Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Sarath D. Perera' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mustaffa Ahmad' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Bernard L. Shaw' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof B Shaw' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email B.L.SHAW@CHEM.LEEDS.AC.UK _publ_requested_journal 'J. Chem Soc., Dalton Trans.' _publ_contact_letter ; The following 3 sets of data are included in a paper which we are about to submit to J. Chem Soc., Dalton Trans. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Uni-, bi- and ter-dentate complexes formed from PPh2CH2C(R)=NNHC(=O)Ph (R = But or Ph) and Pd or Pt: Crystal structures of [PdCl{PPh2CH2C(But) =NN=C(Ph)O}], [Pt{PPh2CH=C(Ph)NN=C(Ph)O}{PPh2CH2C(Ph)=NNHC(=O)Ph] and [Pd{PPh2CH=C(But)NHNC(=O)Ph}2] ; data_sp31 _database_code_CSD 174213 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H26 Cl N2 O P Pd' _chemical_formula_weight 543.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pna21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 19.4346(8) _cell_length_b 9.6142(6) _cell_length_c 12.4346(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2323.38(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22.5 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.003 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5618 _exptl_absorpt_correction_T_max 0.7019 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90.0 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5612 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4110 _reflns_number_gt 4069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0259P)^2^+0.5313P] 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 SHELXL _refine_ls_extinction_coef 0.00148(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.038(16) _refine_ls_number_reflns 4110 _refine_ls_number_parameters 284 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0161 _refine_ls_R_factor_gt 0.0158 _refine_ls_wR_factor_ref 0.0424 _refine_ls_wR_factor_gt 0.0421 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.809316(6) 0.790792(13) 0.999262(15) 0.01927(5) Uani 1 1 d . . . Cl1 Cl 0.70765(3) 0.89081(6) 1.05641(5) 0.03267(12) Uani 1 1 d . . . P1 P 0.76802(3) 0.67528(5) 0.86146(4) 0.02114(11) Uani 1 1 d D . . C111 C 0.71787(10) 0.7616(2) 0.76002(16) 0.0229(4) Uani 1 1 d D . . C112 C 0.68266(12) 0.6860(3) 0.6820(2) 0.0325(5) Uani 1 1 d D . . H112 H 0.6813 0.5873 0.6848 0.039 Uiso 1 1 calc R . . C113 C 0.64945(14) 0.7580(3) 0.5995(2) 0.0417(6) Uani 1 1 d D . . H113 H 0.6255 0.7078 0.5453 0.050 Uiso 1 1 calc R . . C114 C 0.65109(12) 0.9012(3) 0.59607(19) 0.0392(6) Uani 1 1 d D . . H114 H 0.6283 0.9492 0.5396 0.047 Uiso 1 1 calc R . . C115 C 0.68538(12) 0.9747(3) 0.6736(2) 0.0407(6) Uani 1 1 d D . . H115 H 0.6862 1.0735 0.6709 0.049 Uiso 1 1 calc R . . C116 C 0.71903(12) 0.9055(2) 0.75628(18) 0.0327(5) Uani 1 1 d D . . H116 H 0.7428 0.9566 0.8101 0.039 Uiso 1 1 calc R . . C121 C 0.72564(10) 0.5153(2) 0.89965(15) 0.0251(4) Uani 1 1 d D . . C122 C 0.67941(12) 0.5200(2) 0.9849(2) 0.0350(5) Uani 1 1 d D . . H122 H 0.6690 0.6065 1.0179 0.042 Uiso 1 1 calc R . . C123 C 0.64834(15) 0.3991(3) 1.0221(2) 0.0450(6) Uani 1 1 d D . . H123 H 0.6165 0.4035 1.0800 0.054 Uiso 1 1 calc R . . C124 C 0.66336(18) 0.2741(3) 0.9759(2) 0.0486(8) Uani 1 1 d D . . H124 H 0.6429 0.1912 1.0025 0.058 Uiso 1 1 calc R . . C125 C 0.7083(2) 0.2686(3) 0.8906(3) 0.0623(9) Uani 1 1 d D . . H125 H 0.7187 0.1814 0.8584 0.075 Uiso 1 1 calc R . . C126 C 0.73877(16) 0.3883(3) 0.8508(2) 0.0469(7) Uani 1 1 d D . . H126 H 0.7686 0.3834 0.7904 0.056 Uiso 1 1 calc R . . O1 O 0.87166(7) 0.86347(15) 1.12161(11) 0.0267(3) Uani 1 1 d . . . C2 C 0.93304(11) 0.8140(2) 1.10705(17) 0.0228(4) Uani 1 1 d D . . C21 C 0.98714(11) 0.8505(2) 1.18738(17) 0.0254(4) Uani 1 1 d D . . C22 C 0.96814(12) 0.9142(3) 1.2835(2) 0.0352(5) Uani 1 1 d D . . H22 H 0.9211 0.9330 1.2980 0.042 Uiso 1 1 calc R . . C23 C 1.01850(14) 0.9501(3) 1.3584(2) 0.0434(6) Uani 1 1 d D . . H23 H 1.0056 0.9923 1.4245 0.052 Uiso 1 1 calc R . . C24 C 1.08718(14) 0.9246(3) 1.33705(19) 0.0392(6) Uani 1 1 d D . . H24 H 1.1214 0.9516 1.3874 0.047 Uiso 1 1 calc R . . C25 C 1.10600(13) 0.8596(3) 1.2418(2) 0.0380(5) Uani 1 1 d D . . H25 H 1.1531 0.8407 1.2277 0.046 Uiso 1 1 calc R . . C26 C 1.05659(12) 0.8221(3) 1.16779(19) 0.0331(5) Uani 1 1 d D . . H26 H 1.0698 0.7769 1.1031 0.040 Uiso 1 1 calc R . . N3 N 0.95295(9) 0.73344(18) 1.02640(13) 0.0236(4) Uani 1 1 d . . . N4 N 0.89912(9) 0.71179(15) 0.95368(14) 0.0203(3) Uani 1 1 d . . . C5 C 0.91035(10) 0.6463(2) 0.86391(16) 0.0214(4) Uani 1 1 d . . . C51 C 0.97989(11) 0.5884(2) 0.82744(17) 0.0261(4) Uani 1 1 d . . . C52 C 1.03670(15) 0.6980(3) 0.8340(3) 0.0540(8) Uani 1 1 d . . . H52A H 1.0229 0.7805 0.7931 0.081 Uiso 1 1 calc R . . H52B H 1.0793 0.6600 0.8038 0.081 Uiso 1 1 calc R . . H52C H 1.0443 0.7237 0.9094 0.081 Uiso 1 1 calc R . . C53 C 0.99751(16) 0.4610(3) 0.8961(2) 0.0509(7) Uani 1 1 d . . . H53A H 0.9601 0.3930 0.8913 0.076 Uiso 1 1 calc R . . H53B H 1.0035 0.4896 0.9712 0.076 Uiso 1 1 calc R . . H53C H 1.0402 0.4189 0.8698 0.076 Uiso 1 1 calc R . . C54 C 0.97582(13) 0.5424(3) 0.70898(19) 0.0395(6) Uani 1 1 d . . . H54A H 0.9620 0.6217 0.6643 0.059 Uiso 1 1 calc R . . H54B H 0.9419 0.4677 0.7017 0.059 Uiso 1 1 calc R . . H54C H 1.0210 0.5087 0.6856 0.059 Uiso 1 1 calc R . . C6 C 0.84868(11) 0.6302(3) 0.79220(17) 0.0313(5) Uani 1 1 d . . . H6A H 0.8461 0.5327 0.7668 0.038 Uiso 1 1 calc R . . H6B H 0.8542 0.6908 0.7284 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01977(8) 0.02043(8) 0.01762(8) -0.00297(7) 0.00041(7) 0.00149(5) Cl1 0.0259(2) 0.0368(3) 0.0353(3) -0.0103(2) 0.0031(2) 0.0069(2) P1 0.0203(2) 0.0243(2) 0.0189(2) -0.0030(2) -0.00173(19) 0.0024(2) C111 0.0196(10) 0.0294(10) 0.0197(10) 0.0014(9) 0.0020(8) 0.0010(8) C112 0.0366(13) 0.0331(12) 0.0278(12) -0.0069(10) -0.0061(10) 0.0052(9) C113 0.0434(14) 0.0551(15) 0.0267(12) -0.0082(11) -0.0114(10) 0.0076(13) C114 0.0353(12) 0.0540(16) 0.0284(11) 0.0146(11) 0.0016(10) 0.0096(11) C115 0.0439(14) 0.0304(13) 0.0479(15) 0.0142(12) -0.0023(11) -0.0007(10) C116 0.0341(12) 0.0303(12) 0.0337(13) 0.0035(10) -0.0049(10) -0.0054(9) C121 0.0311(10) 0.0232(10) 0.0209(10) -0.0013(8) -0.0075(8) 0.0024(8) C122 0.0400(11) 0.0286(10) 0.0364(15) -0.0045(11) 0.0030(11) -0.0047(9) C123 0.0545(15) 0.0403(13) 0.0400(17) 0.0014(10) 0.0032(11) -0.0129(11) C124 0.074(2) 0.0315(13) 0.0399(19) 0.0067(10) -0.0092(13) -0.0148(12) C125 0.106(3) 0.0210(13) 0.060(2) -0.0100(13) 0.002(2) 0.0021(15) C126 0.0704(19) 0.0300(12) 0.0401(14) -0.0080(11) 0.0109(13) 0.0036(12) O1 0.0258(7) 0.0298(8) 0.0244(7) -0.0080(6) -0.0021(6) 0.0026(6) C2 0.0255(10) 0.0223(10) 0.0206(10) 0.0012(8) -0.0019(8) -0.0025(8) C21 0.0296(11) 0.0228(10) 0.0239(10) 0.0006(8) -0.0050(9) -0.0016(8) C22 0.0374(12) 0.0352(12) 0.0330(12) -0.0094(9) -0.0074(10) 0.0050(10) C23 0.0586(16) 0.0395(14) 0.0322(12) -0.0128(11) -0.0150(11) 0.0036(12) C24 0.0462(14) 0.0361(12) 0.0353(13) 0.0035(10) -0.0227(11) -0.0092(11) C25 0.0293(12) 0.0451(14) 0.0396(13) 0.0082(11) -0.0057(10) -0.0095(10) C26 0.0313(12) 0.0405(13) 0.0275(12) 0.0012(9) -0.0026(9) -0.0079(10) N3 0.0226(8) 0.0288(9) 0.0194(11) -0.0025(6) -0.0016(6) 0.0002(7) N4 0.0201(8) 0.0207(8) 0.0201(8) -0.0015(6) 0.0000(7) -0.0010(6) C5 0.0230(10) 0.0214(10) 0.0199(9) 0.0024(8) 0.0012(8) -0.0012(7) C51 0.0217(10) 0.0308(11) 0.0259(11) -0.0053(9) 0.0048(8) 0.0026(8) C52 0.0361(15) 0.0639(19) 0.0619(19) -0.0309(14) 0.0238(14) -0.0181(12) C53 0.0567(15) 0.0513(16) 0.0448(15) 0.0087(12) 0.0125(13) 0.0298(14) C54 0.0328(12) 0.0537(15) 0.0320(12) -0.0139(11) 0.0071(10) 0.0054(11) C6 0.0237(10) 0.0471(13) 0.0231(11) -0.0080(9) 0.0000(9) 0.0043(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 Pd N4 1.9859(17) . ? Pd O1 2.0666(14) . ? Pd P1 2.1940(5) . ? Pd Cl1 2.3095(5) . ? P1 C111 1.797(2) . ? P1 C121 1.808(2) . ? P1 C6 1.840(2) . ? C111 C116 1.384(3) . ? C111 C112 1.392(3) . ? C112 C113 1.395(3) . ? C113 C114 1.378(4) . ? C114 C115 1.369(4) . ? C115 C116 1.389(3) . ? C121 C126 1.388(3) . ? C121 C122 1.390(3) . ? C122 C123 1.389(3) . ? C123 C124 1.364(4) . ? C124 C125 1.376(5) . ? C125 C126 1.385(4) . ? O1 C2 1.297(3) . ? C2 N3 1.325(3) . ? C2 C21 1.492(3) . ? C21 C22 1.393(3) . ? C21 C26 1.398(3) . ? C22 C23 1.394(3) . ? C23 C24 1.383(4) . ? C24 C25 1.388(4) . ? C25 C26 1.378(3) . ? N3 N4 1.398(2) . ? N4 C5 1.300(3) . ? C5 C6 1.502(3) . ? C5 C51 1.531(3) . ? C51 C52 1.529(3) . ? C51 C53 1.532(3) . ? C51 C54 1.540(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 N4 Pd O1 79.87(6) . . ? N4 Pd P1 84.55(5) . . ? O1 Pd P1 163.85(4) . . ? N4 Pd Cl1 177.32(5) . . ? O1 Pd Cl1 97.72(4) . . ? P1 Pd Cl1 97.94(2) . . ? C111 P1 C121 109.27(9) . . ? C111 P1 C6 104.02(10) . . ? C121 P1 C6 108.09(11) . . ? C111 P1 Pd 120.85(7) . . ? C121 P1 Pd 113.09(6) . . ? C6 P1 Pd 99.97(7) . . ? C116 C111 C112 120.4(2) . . ? C116 C111 P1 118.44(17) . . ? C112 C111 P1 120.98(17) . . ? C111 C112 C113 118.7(2) . . ? C114 C113 C112 120.5(2) . . ? C115 C114 C113 120.4(2) . . ? C114 C115 C116 120.2(2) . . ? C111 C116 C115 119.8(2) . . ? C126 C121 C122 118.7(2) . . ? C126 C121 P1 123.38(17) . . ? C122 C121 P1 117.87(16) . . ? C123 C122 C121 120.6(2) . . ? C124 C123 C122 120.2(2) . . ? C123 C124 C125 119.7(2) . . ? C124 C125 C126 121.0(3) . . ? C125 C126 C121 119.8(2) . . ? C2 O1 Pd 108.21(12) . . ? O1 C2 N3 126.07(19) . . ? O1 C2 C21 117.94(18) . . ? N3 C2 C21 115.99(19) . . ? C22 C21 C26 119.4(2) . . ? C22 C21 C2 119.4(2) . . ? C26 C21 C2 121.2(2) . . ? C21 C22 C23 119.7(2) . . ? C24 C23 C22 120.4(2) . . ? C23 C24 C25 119.9(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C21 120.4(2) . . ? C2 N3 N4 110.97(17) . . ? C5 N4 N3 120.11(17) . . ? C5 N4 Pd 125.29(15) . . ? N3 N4 Pd 114.58(12) . . ? N4 C5 C6 115.21(18) . . ? N4 C5 C51 125.37(18) . . ? C6 C5 C51 119.41(17) . . ? C52 C51 C5 111.78(19) . . ? C52 C51 C53 111.1(2) . . ? C5 C51 C53 108.88(18) . . ? C52 C51 C54 106.6(2) . . ? C5 C51 C54 110.03(18) . . ? C53 C51 C54 108.4(2) . . ? C5 C6 P1 112.18(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.267 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.040 #==END data_sp32 _database_code_CSD 174214 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H46 Cl2 N4 O2 P2 Pt' _chemical_formula_weight 1122.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 12.614(2) _cell_length_b 13.671(2) _cell_length_c 15.754(3) _cell_angle_alpha 100.260(9) _cell_angle_beta 99.334(9) _cell_angle_gamma 110.682(7) _cell_volume 2425.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 17.5 _cell_measurement_theta_max 20.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 3.116 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3105 _exptl_absorpt_correction_T_max 0.5890 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90.0 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method \w-\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9663 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8527 _reflns_number_gt 7943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0207P)^2^+4.3144P] 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 8527 _refine_ls_number_parameters 598 _refine_ls_number_restraints 218 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.078 _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 Pt Pt 0.208837(9) 0.176900(9) 0.204610(8) 0.01620(4) Uani 1 1 d . . . P1 P 0.13004(7) 0.07057(6) 0.28940(5) 0.01898(16) Uani 1 1 d D . . C111 C 0.1162(3) 0.1361(2) 0.3957(2) 0.0232(7) Uani 1 1 d D . . C112 C 0.0126(3) 0.1451(3) 0.4068(2) 0.0312(8) Uani 1 1 d D . . H112 H -0.0566 0.1093 0.3603 0.037 Uiso 1 1 calc R . . C113 C 0.0110(4) 0.2073(3) 0.4870(3) 0.0414(9) Uani 1 1 d D . . H113 H -0.0592 0.2148 0.4947 0.050 Uiso 1 1 calc R . . C114 C 0.1112(4) 0.2579(3) 0.5549(3) 0.0445(10) Uani 1 1 d D . . H114 H 0.1095 0.3004 0.6090 0.053 Uiso 1 1 calc R . . C115 C 0.2137(4) 0.2477(3) 0.5454(2) 0.0416(9) Uani 1 1 d D . . H115 H 0.2820 0.2822 0.5929 0.050 Uiso 1 1 calc R . . C116 C 0.2166(3) 0.1863(3) 0.4657(2) 0.0321(8) Uani 1 1 d D . . H116 H 0.2869 0.1786 0.4590 0.039 Uiso 1 1 calc R . . C121 C -0.0123(3) -0.0375(2) 0.2360(2) 0.0216(7) Uani 1 1 d D . . C122 C -0.0561(3) -0.0601(3) 0.1444(2) 0.0245(7) Uani 1 1 d D . . H122 H -0.0114 -0.0189 0.1105 0.029 Uiso 1 1 calc R . . C123 C -0.1646(3) -0.1426(3) 0.1024(2) 0.0295(8) Uani 1 1 d D . . H123 H -0.1938 -0.1580 0.0399 0.035 Uiso 1 1 calc R . . C124 C -0.2302(3) -0.2025(3) 0.1521(2) 0.0320(8) Uani 1 1 d D . . H124 H -0.3053 -0.2576 0.1239 0.038 Uiso 1 1 calc R . . C125 C -0.1863(3) -0.1818(3) 0.2426(3) 0.0326(8) Uani 1 1 d D . . H125 H -0.2310 -0.2238 0.2761 0.039 Uiso 1 1 calc R . . C126 C -0.0777(3) -0.1006(3) 0.2848(2) 0.0280(7) Uani 1 1 d D . . H126 H -0.0477 -0.0877 0.3469 0.034 Uiso 1 1 calc R . . C2 C 0.2350(3) 0.0134(3) 0.3103(2) 0.0235(7) Uani 1 1 d . . . H2 H 0.2314 -0.0318 0.3501 0.028 Uiso 1 1 calc R . . C3 C 0.3218(3) 0.0384(2) 0.2654(2) 0.0211(6) Uani 1 1 d D . . C31 C 0.4144(3) -0.0054(2) 0.2764(2) 0.0223(7) Uani 1 1 d D . . C32 C 0.4294(3) -0.0710(3) 0.2047(2) 0.0298(8) Uani 1 1 d D . . H32 H 0.3829 -0.0853 0.1465 0.036 Uiso 1 1 calc R . . C33 C 0.5119(3) -0.1154(3) 0.2182(3) 0.0371(9) Uani 1 1 d D . . H33 H 0.5205 -0.1616 0.1695 0.045 Uiso 1 1 calc R . . C34 C 0.5818(3) -0.0929(3) 0.3020(3) 0.0428(10) Uani 1 1 d D . . H34 H 0.6384 -0.1235 0.3107 0.051 Uiso 1 1 calc R . . C35 C 0.5699(4) -0.0260(4) 0.3732(3) 0.0485(11) Uani 1 1 d D . . H35 H 0.6193 -0.0093 0.4307 0.058 Uiso 1 1 calc R . . C36 C 0.4850(3) 0.0170(3) 0.3607(3) 0.0378(9) Uani 1 1 d D . . H36 H 0.4755 0.0616 0.4099 0.045 Uiso 1 1 calc R . . N4 N 0.3213(2) 0.1055(2) 0.21085(17) 0.0203(5) Uani 1 1 d . . . N5 N 0.4092(2) 0.1385(2) 0.16660(17) 0.0199(5) Uani 1 1 d . . . C6 C 0.3992(3) 0.2116(2) 0.1271(2) 0.0190(6) Uani 1 1 d D . . C61 C 0.4849(3) 0.2589(2) 0.0771(2) 0.0198(6) Uani 1 1 d D . . C62 C 0.5774(3) 0.2266(3) 0.0720(2) 0.0285(7) Uani 1 1 d D . . H62 H 0.5853 0.1732 0.1008 0.034 Uiso 1 1 calc R . . C63 C 0.6578(3) 0.2720(3) 0.0254(3) 0.0339(8) Uani 1 1 d D . . H63 H 0.7208 0.2497 0.0226 0.041 Uiso 1 1 calc R . . C64 C 0.6476(3) 0.3493(3) -0.0171(3) 0.0361(9) Uani 1 1 d D . . H64 H 0.7029 0.3797 -0.0492 0.043 Uiso 1 1 calc R . . C65 C 0.5563(3) 0.3824(3) -0.0127(2) 0.0321(8) Uani 1 1 d D . . H65 H 0.5491 0.4357 -0.0418 0.039 Uiso 1 1 calc R . . C66 C 0.4757(3) 0.3376(3) 0.0340(2) 0.0260(7) Uani 1 1 d D . . H66 H 0.4133 0.3607 0.0369 0.031 Uiso 1 1 calc R . . O6 O 0.31504(18) 0.25030(16) 0.12924(14) 0.0200(4) Uani 1 1 d . . . P2 P 0.09574(6) 0.27265(6) 0.19140(5) 0.01668(15) Uani 1 1 d D . . C211 C -0.0581(3) 0.1894(2) 0.1405(2) 0.0219(7) Uani 1 1 d D . . C212 C -0.0909(3) 0.1412(3) 0.0495(2) 0.0283(7) Uani 1 1 d D . . H212 H -0.0357 0.1597 0.0145 0.034 Uiso 1 1 calc R . . C213 C -0.2043(3) 0.0659(3) 0.0097(3) 0.0375(9) Uani 1 1 d D . . H213 H -0.2263 0.0328 -0.0523 0.045 Uiso 1 1 calc R . . C214 C -0.2846(3) 0.0394(3) 0.0605(3) 0.0416(10) Uani 1 1 d D . . H214 H -0.3619 -0.0122 0.0333 0.050 Uiso 1 1 calc R . . C215 C -0.2533(3) 0.0873(3) 0.1503(3) 0.0376(9) Uani 1 1 d D . . H215 H -0.3090 0.0686 0.1848 0.045 Uiso 1 1 calc R . . C216 C -0.1405(3) 0.1627(3) 0.1905(2) 0.0286(7) Uani 1 1 d D . . H216 H -0.1196 0.1962 0.2524 0.034 Uiso 1 1 calc R . . C221 C 0.1058(3) 0.3644(2) 0.2938(2) 0.0212(6) Uani 1 1 d D . . C222 C 0.0269(3) 0.4137(3) 0.3019(2) 0.0277(7) Uani 1 1 d D . . H222 H -0.0377 0.3967 0.2535 0.033 Uiso 1 1 calc R . . C223 C 0.0424(3) 0.4874(3) 0.3806(2) 0.0349(8) Uani 1 1 d D . . H223 H -0.0112 0.5213 0.3855 0.042 Uiso 1 1 calc R . . C224 C 0.1351(3) 0.5118(3) 0.4516(2) 0.0366(9) Uani 1 1 d D . . H224 H 0.1453 0.5624 0.5053 0.044 Uiso 1 1 calc R . . C225 C 0.2132(3) 0.4629(3) 0.4448(2) 0.0346(8) Uani 1 1 d D . . H225 H 0.2768 0.4795 0.4940 0.042 Uiso 1 1 calc R . . C226 C 0.1991(3) 0.3896(3) 0.3665(2) 0.0257(7) Uani 1 1 d D . . H226 H 0.2533 0.3563 0.3622 0.031 Uiso 1 1 calc R . . C7 C 0.1404(3) 0.3600(2) 0.1139(2) 0.0198(6) Uani 1 1 d . . . H7A H 0.1971 0.3399 0.0859 0.024 Uiso 1 1 calc R . . H7B H 0.0707 0.3436 0.0659 0.024 Uiso 1 1 calc R . . C8 C 0.1943(3) 0.4804(2) 0.1550(2) 0.0200(6) Uani 1 1 d D . . C81 C 0.1214(3) 0.5453(3) 0.1464(2) 0.0213(6) Uani 1 1 d D . . C82 C 0.0010(3) 0.4971(3) 0.1126(2) 0.0282(7) Uani 1 1 d D . . H82 H -0.0368 0.4206 0.0925 0.034 Uiso 1 1 calc R . . C83 C -0.0648(3) 0.5603(3) 0.1078(3) 0.0346(8) Uani 1 1 d D . . H83 H -0.1473 0.5265 0.0854 0.042 Uiso 1 1 calc R . . C84 C -0.0108(3) 0.6713(3) 0.1353(3) 0.0388(9) Uani 1 1 d D . . H84 H -0.0558 0.7140 0.1321 0.047 Uiso 1 1 calc R . . C85 C 0.1091(4) 0.7203(3) 0.1676(3) 0.0406(9) Uani 1 1 d D . . H85 H 0.1466 0.7969 0.1861 0.049 Uiso 1 1 calc R . . C86 C 0.1746(3) 0.6582(3) 0.1733(2) 0.0291(7) Uani 1 1 d D . . H86 H 0.2570 0.6927 0.1957 0.035 Uiso 1 1 calc R . . N9 N 0.3019(2) 0.5347(2) 0.19739(18) 0.0234(6) Uani 1 1 d . . . N10 N 0.3760(2) 0.4829(2) 0.21076(19) 0.0243(6) Uani 1 1 d . . . H10 H 0.354(3) 0.414(3) 0.195(2) 0.029 Uiso 1 1 d . . . C11 C 0.4941(3) 0.5450(3) 0.2431(2) 0.0267(7) Uani 1 1 d D . . C12 C 0.5665(3) 0.4829(3) 0.2643(2) 0.0254(7) Uani 1 1 d D . . C13 C 0.5322(3) 0.3986(3) 0.3055(2) 0.0303(8) Uani 1 1 d D . . H13 H 0.4591 0.3782 0.3209 0.036 Uiso 1 1 calc R . . C14 C 0.6040(3) 0.3444(3) 0.3240(2) 0.0356(8) Uani 1 1 d D . . H14 H 0.5805 0.2874 0.3525 0.043 Uiso 1 1 calc R . . C15 C 0.7091(3) 0.3733(3) 0.3011(3) 0.0385(9) Uani 1 1 d D . . H15 H 0.7578 0.3355 0.3133 0.046 Uiso 1 1 calc R . . C16 C 0.7451(3) 0.4574(3) 0.2603(3) 0.0388(9) Uani 1 1 d D . . H16 H 0.8179 0.4770 0.2445 0.047 Uiso 1 1 calc R . . C17 C 0.6745(3) 0.5123(3) 0.2429(2) 0.0311(8) Uani 1 1 d D . . H17 H 0.6996 0.5708 0.2161 0.037 Uiso 1 1 calc R . . O11 O 0.5361(2) 0.6427(2) 0.2535(2) 0.0408(7) Uani 1 1 d . . . C1S C 0.3595(4) 0.7122(4) 0.3841(3) 0.0626(14) Uani 1 1 d . . . H1S1 H 0.3024 0.6391 0.3502 0.075 Uiso 1 1 calc R . . H1S2 H 0.3960 0.7498 0.3416 0.075 Uiso 1 1 calc R . . Cl1 Cl 0.28586(16) 0.78407(12) 0.43530(12) 0.0893(5) Uani 1 1 d . . . Cl2 Cl 0.46734(12) 0.70049(15) 0.46181(10) 0.0875(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01495(6) 0.01539(6) 0.02046(7) 0.00587(4) 0.00601(4) 0.00717(5) P1 0.0183(4) 0.0184(4) 0.0221(4) 0.0076(3) 0.0070(3) 0.0074(3) C111 0.0273(17) 0.0205(16) 0.0223(16) 0.0084(13) 0.0090(13) 0.0073(13) C112 0.0335(19) 0.036(2) 0.0297(19) 0.0110(15) 0.0113(15) 0.0169(16) C113 0.051(2) 0.045(2) 0.042(2) 0.0149(19) 0.028(2) 0.027(2) C114 0.064(3) 0.043(2) 0.026(2) 0.0041(17) 0.0167(19) 0.021(2) C115 0.047(2) 0.042(2) 0.0263(19) 0.0069(17) 0.0050(17) 0.0090(19) C116 0.0300(19) 0.034(2) 0.0306(19) 0.0101(16) 0.0066(15) 0.0107(16) C121 0.0188(15) 0.0179(15) 0.0297(17) 0.0065(13) 0.0077(13) 0.0082(13) C122 0.0275(17) 0.0207(16) 0.0277(17) 0.0082(13) 0.0076(14) 0.0111(14) C123 0.0306(19) 0.0234(17) 0.0315(19) 0.0036(14) -0.0015(15) 0.0127(15) C124 0.0205(17) 0.0218(17) 0.049(2) 0.0023(16) 0.0013(16) 0.0086(14) C125 0.0240(18) 0.0269(18) 0.048(2) 0.0105(16) 0.0158(16) 0.0075(15) C126 0.0268(18) 0.0272(18) 0.0290(18) 0.0089(14) 0.0091(14) 0.0078(14) C2 0.0254(17) 0.0229(16) 0.0273(17) 0.0130(14) 0.0079(14) 0.0117(14) C3 0.0227(16) 0.0179(15) 0.0231(16) 0.0038(12) 0.0030(13) 0.0102(13) C31 0.0211(16) 0.0156(15) 0.0327(18) 0.0100(13) 0.0083(14) 0.0076(13) C32 0.0286(18) 0.0264(18) 0.036(2) 0.0057(15) 0.0075(15) 0.0143(15) C33 0.035(2) 0.0283(19) 0.055(2) 0.0078(17) 0.0181(18) 0.0196(16) C34 0.035(2) 0.040(2) 0.067(3) 0.018(2) 0.013(2) 0.0279(18) C35 0.045(2) 0.058(3) 0.047(2) 0.013(2) -0.004(2) 0.033(2) C36 0.041(2) 0.042(2) 0.036(2) 0.0049(17) 0.0042(17) 0.0279(18) N4 0.0181(13) 0.0202(13) 0.0263(14) 0.0078(11) 0.0077(11) 0.0100(11) N5 0.0160(13) 0.0179(13) 0.0251(14) 0.0040(11) 0.0049(11) 0.0067(10) C6 0.0167(15) 0.0183(15) 0.0212(16) 0.0039(12) 0.0057(12) 0.0060(12) C61 0.0187(15) 0.0177(15) 0.0205(15) 0.0019(12) 0.0063(12) 0.0049(12) C62 0.0265(18) 0.0276(18) 0.037(2) 0.0110(15) 0.0136(15) 0.0134(15) C63 0.0283(19) 0.034(2) 0.045(2) 0.0104(17) 0.0203(17) 0.0148(16) C64 0.035(2) 0.032(2) 0.041(2) 0.0102(17) 0.0208(17) 0.0071(16) C65 0.039(2) 0.0285(18) 0.0322(19) 0.0150(15) 0.0149(16) 0.0104(16) C66 0.0252(17) 0.0253(17) 0.0294(18) 0.0084(14) 0.0087(14) 0.0108(14) O6 0.0190(11) 0.0196(11) 0.0277(12) 0.0092(9) 0.0106(9) 0.0113(9) P2 0.0153(4) 0.0162(4) 0.0199(4) 0.0045(3) 0.0052(3) 0.0074(3) C211 0.0170(15) 0.0161(15) 0.0326(18) 0.0051(13) 0.0032(13) 0.0085(12) C212 0.0263(17) 0.0219(17) 0.0347(19) 0.0040(14) 0.0033(15) 0.0106(14) C213 0.033(2) 0.0255(18) 0.045(2) -0.0009(16) -0.0079(17) 0.0128(16) C214 0.0207(18) 0.0233(18) 0.069(3) 0.0049(19) -0.0037(18) 0.0052(15) C215 0.0232(18) 0.0298(19) 0.064(3) 0.0200(19) 0.0135(18) 0.0098(15) C216 0.0196(16) 0.0259(17) 0.044(2) 0.0126(15) 0.0087(15) 0.0106(14) C221 0.0210(16) 0.0178(15) 0.0247(16) 0.0045(13) 0.0088(13) 0.0067(13) C222 0.0270(18) 0.0309(18) 0.0314(19) 0.0107(15) 0.0112(15) 0.0155(15) C223 0.040(2) 0.033(2) 0.039(2) 0.0046(16) 0.0192(17) 0.0204(17) C224 0.049(2) 0.0296(19) 0.0271(19) -0.0002(15) 0.0135(17) 0.0126(17) C225 0.037(2) 0.0303(19) 0.0267(19) 0.0032(15) 0.0020(16) 0.0058(16) C226 0.0238(17) 0.0250(17) 0.0267(17) 0.0071(14) 0.0065(14) 0.0075(14) C7 0.0208(15) 0.0194(15) 0.0220(16) 0.0069(12) 0.0076(13) 0.0095(13) C8 0.0232(16) 0.0185(15) 0.0223(16) 0.0083(13) 0.0105(13) 0.0091(13) C81 0.0251(16) 0.0234(16) 0.0221(16) 0.0103(13) 0.0115(13) 0.0126(13) C82 0.0279(18) 0.0260(17) 0.0343(19) 0.0108(15) 0.0096(15) 0.0122(15) C83 0.0279(19) 0.041(2) 0.044(2) 0.0168(18) 0.0120(16) 0.0209(17) C84 0.043(2) 0.042(2) 0.047(2) 0.0129(18) 0.0149(18) 0.0326(19) C85 0.047(2) 0.0264(19) 0.054(3) 0.0074(18) 0.0101(19) 0.0224(18) C86 0.0298(18) 0.0237(17) 0.0359(19) 0.0072(15) 0.0078(15) 0.0131(15) N9 0.0232(14) 0.0200(13) 0.0305(15) 0.0073(11) 0.0092(12) 0.0111(11) N10 0.0198(14) 0.0174(13) 0.0345(16) 0.0057(12) 0.0048(12) 0.0072(11) C11 0.0216(16) 0.0243(18) 0.0306(18) 0.0018(14) 0.0045(14) 0.0083(14) C12 0.0221(16) 0.0231(16) 0.0249(17) -0.0011(13) 0.0009(13) 0.0073(13) C13 0.0271(18) 0.0334(19) 0.0267(18) 0.0042(15) 0.0044(14) 0.0101(15) C14 0.041(2) 0.033(2) 0.031(2) 0.0087(16) 0.0001(16) 0.0168(17) C15 0.036(2) 0.041(2) 0.040(2) 0.0026(18) -0.0005(17) 0.0249(18) C16 0.0257(19) 0.046(2) 0.044(2) 0.0049(18) 0.0074(17) 0.0172(17) C17 0.0245(18) 0.0293(18) 0.036(2) 0.0053(15) 0.0050(15) 0.0092(15) O11 0.0257(13) 0.0228(13) 0.0664(19) 0.0067(12) 0.0037(13) 0.0063(11) C1S 0.060(3) 0.063(3) 0.041(3) 0.001(2) 0.014(2) 0.003(2) Cl1 0.1032(12) 0.0560(8) 0.0976(12) 0.0044(8) 0.0379(10) 0.0199(8) Cl2 0.0537(8) 0.1200(13) 0.0660(9) 0.0227(9) 0.0106(7) 0.0098(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 Pt N4 1.985(2) . ? Pt O6 2.050(2) . ? Pt P1 2.2332(8) . ? Pt P2 2.2609(8) . ? P1 C2 1.777(3) . ? P1 C111 1.818(3) . ? P1 C121 1.819(3) . ? C111 C112 1.391(4) . ? C111 C116 1.398(5) . ? C112 C113 1.399(5) . ? C112 H112 0.9500 . ? C113 C114 1.379(6) . ? C113 H113 0.9500 . ? C114 C115 1.378(6) . ? C114 H114 0.9500 . ? C115 C116 1.393(5) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.393(4) . ? C121 C126 1.399(4) . ? C122 C123 1.391(4) . ? C122 H122 0.9500 . ? C123 C124 1.388(5) . ? C123 H123 0.9500 . ? C124 C125 1.381(5) . ? C124 H124 0.9500 . ? C125 C126 1.386(5) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C2 C3 1.374(4) . ? C2 H2 0.9500 . ? C3 N4 1.365(4) . ? C3 C31 1.489(4) . ? C31 C36 1.389(5) . ? C31 C32 1.395(5) . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 C34 1.378(6) . ? C33 H33 0.9500 . ? C34 C35 1.380(6) . ? C34 H34 0.9500 . ? C35 C36 1.395(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N4 N5 1.389(4) . ? N5 C6 1.299(4) . ? C6 O6 1.346(4) . ? C6 C61 1.472(4) . ? C61 C62 1.395(4) . ? C61 C66 1.399(4) . ? C62 C63 1.383(5) . ? C62 H62 0.9500 . ? C63 C64 1.379(5) . ? C63 H63 0.9500 . ? C64 C65 1.384(5) . ? C64 H64 0.9500 . ? C65 C66 1.383(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? P2 C221 1.814(3) . ? P2 C211 1.820(3) . ? P2 C7 1.872(3) . ? C211 C216 1.391(4) . ? C211 C212 1.394(4) . ? C212 C213 1.392(5) . ? C212 H212 0.9500 . ? C213 C214 1.380(5) . ? C213 H213 0.9500 . ? C214 C215 1.375(5) . ? C214 H214 0.9500 . ? C215 C216 1.388(5) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.394(4) . ? C221 C226 1.397(4) . ? C222 C223 1.389(5) . ? C222 H222 0.9500 . ? C223 C224 1.377(5) . ? C223 H223 0.9500 . ? C224 C225 1.380(5) . ? C224 H224 0.9500 . ? C225 C226 1.386(5) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C7 C8 1.509(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N9 1.287(4) . ? C8 C81 1.492(4) . ? C81 C82 1.390(5) . ? C81 C86 1.399(5) . ? C82 C83 1.397(5) . ? C82 H82 0.9500 . ? C83 C84 1.376(5) . ? C83 H83 0.9500 . ? C84 C85 1.381(6) . ? C84 H84 0.9500 . ? C85 C86 1.382(5) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? N9 N10 1.371(4) . ? N10 C11 1.381(4) . ? N10 H10 0.85(4) . ? C11 O11 1.218(4) . ? C11 C12 1.489(5) . ? C12 C17 1.393(5) . ? C12 C13 1.393(5) . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.371(6) . ? C14 H14 0.9500 . ? C15 C16 1.390(6) . ? C15 H15 0.9500 . ? C16 C17 1.377(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C1S Cl2 1.749(6) . ? C1S Cl1 1.755(5) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? 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 N4 Pt O6 78.79(9) . . ? N4 Pt P1 83.62(8) . . ? O6 Pt P1 162.42(6) . . ? N4 Pt P2 173.28(8) . . ? O6 Pt P2 94.70(6) . . ? P1 Pt P2 102.88(3) . . ? C2 P1 C111 108.35(15) . . ? C2 P1 C121 109.15(14) . . ? C111 P1 C121 105.86(14) . . ? C2 P1 Pt 100.21(11) . . ? C111 P1 Pt 117.26(10) . . ? C121 P1 Pt 115.58(11) . . ? C112 C111 C116 119.6(3) . . ? C112 C111 P1 122.2(3) . . ? C116 C111 P1 117.9(2) . . ? C111 C112 C113 119.6(3) . . ? C111 C112 H112 120.2 . . ? C113 C112 H112 120.2 . . ? C114 C113 C112 120.0(4) . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C115 C114 C113 121.0(4) . . ? C115 C114 H114 119.5 . . ? C113 C114 H114 119.5 . . ? C114 C115 C116 119.5(4) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? C115 C116 C111 120.2(3) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C122 C121 C126 119.2(3) . . ? C122 C121 P1 119.7(2) . . ? C126 C121 P1 121.1(2) . . ? C123 C122 C121 120.5(3) . . ? C123 C122 H122 119.7 . . ? C121 C122 H122 119.7 . . ? C124 C123 C122 119.7(3) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C125 C124 C123 120.0(3) . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C124 C125 C126 120.6(3) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? C125 C126 C121 119.9(3) . . ? C125 C126 H126 120.1 . . ? C121 C126 H126 120.1 . . ? C3 C2 P1 115.9(2) . . ? C3 C2 H2 122.0 . . ? P1 C2 H2 122.0 . . ? N4 C3 C2 118.0(3) . . ? N4 C3 C31 120.9(3) . . ? C2 C3 C31 121.2(3) . . ? C36 C31 C32 119.3(3) . . ? C36 C31 C3 119.1(3) . . ? C32 C31 C3 121.6(3) . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.2(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 119.8(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 120.2(4) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C3 N4 N5 121.3(2) . . ? C3 N4 Pt 121.6(2) . . ? N5 N4 Pt 116.57(18) . . ? C6 N5 N4 111.0(2) . . ? N5 C6 O6 124.3(3) . . ? N5 C6 C61 119.9(3) . . ? O6 C6 C61 115.9(3) . . ? C62 C61 C66 118.4(3) . . ? C62 C61 C6 120.8(3) . . ? C66 C61 C6 120.8(3) . . ? C63 C62 C61 120.3(3) . . ? C63 C62 H62 119.8 . . ? C61 C62 H62 119.8 . . ? C64 C63 C62 120.7(3) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 119.8(3) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C66 C65 C64 119.9(3) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.8(3) . . ? C65 C66 H66 119.6 . . ? C61 C66 H66 119.6 . . ? C6 O6 Pt 109.34(18) . . ? C221 P2 C211 108.08(14) . . ? C221 P2 C7 105.29(14) . . ? C211 P2 C7 103.88(14) . . ? C221 P2 Pt 115.22(10) . . ? C211 P2 Pt 113.84(10) . . ? C7 P2 Pt 109.61(10) . . ? C216 C211 C212 119.1(3) . . ? C216 C211 P2 122.3(3) . . ? C212 C211 P2 118.1(2) . . ? C213 C212 C211 120.2(3) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C214 C213 C212 119.9(4) . . ? C214 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? C215 C214 C213 120.3(3) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C214 C215 C216 120.2(4) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C216 C211 120.2(3) . . ? C215 C216 H216 119.9 . . ? C211 C216 H216 119.9 . . ? C222 C221 C226 118.7(3) . . ? C222 C221 P2 122.9(2) . . ? C226 C221 P2 118.4(2) . . ? C223 C222 C221 120.3(3) . . ? C223 C222 H222 119.9 . . ? C221 C222 H222 119.9 . . ? C224 C223 C222 120.4(3) . . ? C224 C223 H223 119.8 . . ? C222 C223 H223 119.8 . . ? C223 C224 C225 120.0(3) . . ? C223 C224 H224 120.0 . . ? C225 C224 H224 120.0 . . ? C224 C225 C226 120.2(3) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C225 C226 C221 120.4(3) . . ? C225 C226 H226 119.8 . . ? C221 C226 H226 119.8 . . ? C8 C7 P2 116.0(2) . . ? C8 C7 H7A 108.3 . . ? P2 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? P2 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N9 C8 C81 115.3(3) . . ? N9 C8 C7 124.9(3) . . ? C81 C8 C7 119.7(3) . . ? C82 C81 C86 118.2(3) . . ? C82 C81 C8 122.1(3) . . ? C86 C81 C8 119.7(3) . . ? C81 C82 C83 120.5(3) . . ? C81 C82 H82 119.7 . . ? C83 C82 H82 119.7 . . ? C84 C83 C82 120.3(3) . . ? C84 C83 H83 119.9 . . ? C82 C83 H83 119.9 . . ? C83 C84 C85 119.8(3) . . ? C83 C84 H84 120.1 . . ? C85 C84 H84 120.1 . . ? C84 C85 C86 120.2(4) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C85 C86 C81 121.0(3) . . ? C85 C86 H86 119.5 . . ? C81 C86 H86 119.5 . . ? C8 N9 N10 120.2(3) . . ? N9 N10 C11 118.2(3) . . ? N9 N10 H10 123(3) . . ? C11 N10 H10 118(3) . . ? O11 C11 N10 123.0(3) . . ? O11 C11 C12 122.5(3) . . ? N10 C11 C12 114.5(3) . . ? C17 C12 C13 118.9(3) . . ? C17 C12 C11 117.9(3) . . ? C13 C12 C11 123.2(3) . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C12 120.6(4) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? Cl2 C1S Cl1 111.9(3) . . ? Cl2 C1S H1S1 109.2 . . ? Cl1 C1S H1S1 109.2 . . ? Cl2 C1S H1S2 109.2 . . ? Cl1 C1S H1S2 109.2 . . ? H1S1 C1S H1S2 107.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.954 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.080 #==END data_sp33 _database_code_CSD 174215 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H54 Cl2 N4 O2 P2 Pd' _chemical_formula_weight 994.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 25.162(2) _cell_length_b 19.489(2) _cell_length_c 19.329(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9478.6(16) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 17.5 _cell_measurement_theta_max 20.0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.68 _exptl_crystal_size_min 0.68 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.6517 _exptl_absorpt_correction_T_max 0.6794 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90.0 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method \w-\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8502 _diffrn_reflns_av_R_equivalents 0.0101 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.99 _reflns_number_total 8340 _reflns_number_gt 6888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0251P)^2^+14.0243P] 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 8340 _refine_ls_number_parameters 571 _refine_ls_number_restraints 223 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.369935(7) 0.066924(9) 0.239766(10) 0.02219(6) Uani 1 1 d . . . P1 P 0.42102(2) 0.15395(3) 0.27920(3) 0.02354(14) Uani 1 1 d D . . C111 C 0.46514(10) 0.14724(13) 0.35403(13) 0.0262(6) Uani 1 1 d D . . C112 C 0.44377(11) 0.15411(15) 0.42019(14) 0.0337(6) Uani 1 1 d D . . H112 H 0.4066 0.1606 0.4258 0.040 Uiso 1 1 calc R . . C113 C 0.47639(12) 0.15150(17) 0.47781(15) 0.0423(7) Uani 1 1 d D . . H113 H 0.4616 0.1572 0.5227 0.051 Uiso 1 1 calc R . . C114 C 0.53038(12) 0.14063(16) 0.47042(15) 0.0387(7) Uani 1 1 d D . . H114 H 0.5526 0.1384 0.5101 0.046 Uiso 1 1 calc R . . C115 C 0.55176(11) 0.13304(14) 0.40539(14) 0.0333(6) Uani 1 1 d D . . H115 H 0.5888 0.1252 0.4004 0.040 Uiso 1 1 calc R . . C116 C 0.51982(10) 0.13665(13) 0.34723(14) 0.0290(6) Uani 1 1 d D . . H116 H 0.5351 0.1319 0.3025 0.035 Uiso 1 1 calc R . . C121 C 0.46715(10) 0.18262(13) 0.21188(13) 0.0253(5) Uani 1 1 d D . . C122 C 0.47584(11) 0.25192(14) 0.20099(14) 0.0324(6) Uani 1 1 d D . . H122 H 0.4570 0.2849 0.2276 0.039 Uiso 1 1 calc R . . C123 C 0.51207(12) 0.27330(16) 0.15138(15) 0.0397(7) Uani 1 1 d D . . H123 H 0.5177 0.3209 0.1440 0.048 Uiso 1 1 calc R . . C124 C 0.53984(12) 0.22610(16) 0.11273(16) 0.0421(7) Uani 1 1 d D . . H124 H 0.5645 0.2412 0.0788 0.051 Uiso 1 1 calc R . . C125 C 0.53185(12) 0.15686(17) 0.12325(16) 0.0422(7) Uani 1 1 d D . . H125 H 0.5512 0.1242 0.0969 0.051 Uiso 1 1 calc R . . C126 C 0.49544(11) 0.13504(15) 0.17243(14) 0.0349(6) Uani 1 1 d D . . H126 H 0.4897 0.0873 0.1793 0.042 Uiso 1 1 calc R . . C2 C 0.37912(10) 0.22169(14) 0.30242(14) 0.0288(6) Uani 1 1 d . . . H2 H 0.3926 0.2529 0.3359 0.035 Uiso 1 1 calc R . . C3 C 0.32930(10) 0.23492(13) 0.27801(13) 0.0263(6) Uani 1 1 d . . . C31 C 0.29761(11) 0.29624(14) 0.30745(15) 0.0336(6) Uani 1 1 d . . . C32 C 0.28874(13) 0.28585(18) 0.38547(16) 0.0453(8) Uani 1 1 d . . . H32A H 0.3231 0.2808 0.4086 0.068 Uiso 1 1 calc R . . H32B H 0.2674 0.2445 0.3930 0.068 Uiso 1 1 calc R . . H32C H 0.2700 0.3257 0.4045 0.068 Uiso 1 1 calc R . . C33 C 0.33034(13) 0.36192(15) 0.29559(18) 0.0440(8) Uani 1 1 d . . . H33A H 0.3381 0.3668 0.2462 0.066 Uiso 1 1 calc R . . H33B H 0.3637 0.3590 0.3215 0.066 Uiso 1 1 calc R . . H33C H 0.3100 0.4018 0.3115 0.066 Uiso 1 1 calc R . . C34 C 0.24363(11) 0.30575(16) 0.27197(17) 0.0412(7) Uani 1 1 d . . . H34A H 0.2489 0.3116 0.2221 0.062 Uiso 1 1 calc R . . H34B H 0.2260 0.3465 0.2908 0.062 Uiso 1 1 calc R . . H34C H 0.2215 0.2652 0.2803 0.062 Uiso 1 1 calc R . . N5 N 0.30556(9) 0.19883(12) 0.22823(12) 0.0291(5) Uani 1 1 d . . . H5 H 0.2769(12) 0.2084(16) 0.2155(16) 0.035 Uiso 1 1 d . . . N6 N 0.33195(8) 0.14959(11) 0.18880(11) 0.0273(5) Uani 1 1 d . . . O6 O 0.26605(8) 0.17278(11) 0.11017(11) 0.0405(5) Uani 1 1 d . . . C6 C 0.30803(11) 0.14262(14) 0.12611(14) 0.0308(6) Uani 1 1 d D . . C61 C 0.33682(12) 0.10122(14) 0.07281(14) 0.0353(7) Uani 1 1 d D . . C62 C 0.39117(14) 0.1036(2) 0.06696(18) 0.0601(10) Uani 1 1 d D . . H62 H 0.4113 0.1275 0.1008 0.072 Uiso 1 1 calc R . . C63 C 0.41730(19) 0.0716(3) 0.0125(2) 0.0871(16) Uani 1 1 d D . . H63 H 0.4549 0.0743 0.0090 0.105 Uiso 1 1 calc R . . C64 C 0.3888(2) 0.0362(2) -0.0361(2) 0.0762(13) Uani 1 1 d D . . H64 H 0.4066 0.0139 -0.0732 0.091 Uiso 1 1 calc R . . C65 C 0.3347(2) 0.0333(2) -0.03115(19) 0.0679(12) Uani 1 1 d D . . H65 H 0.3148 0.0093 -0.0652 0.082 Uiso 1 1 calc R . . C66 C 0.30847(15) 0.06523(17) 0.02344(18) 0.0522(9) Uani 1 1 d D . . H66 H 0.2709 0.0623 0.0268 0.063 Uiso 1 1 calc R . . P7 P 0.41097(3) -0.02628(3) 0.28478(4) 0.02653(15) Uani 1 1 d D . . C711 C 0.48087(10) -0.02626(13) 0.31075(15) 0.0304(6) Uani 1 1 d D . . C712 C 0.51952(11) -0.02559(14) 0.25858(17) 0.0374(7) Uani 1 1 d D . . H712 H 0.5089 -0.0249 0.2114 0.045 Uiso 1 1 calc R . . C713 C 0.57308(12) -0.02598(16) 0.27507(19) 0.0460(8) Uani 1 1 d D . . H713 H 0.5989 -0.0243 0.2393 0.055 Uiso 1 1 calc R . . C714 C 0.58913(12) -0.02888(16) 0.3435(2) 0.0487(9) Uani 1 1 d D . . H714 H 0.6259 -0.0301 0.3547 0.058 Uiso 1 1 calc R . . C715 C 0.55158(12) -0.02991(15) 0.39512(18) 0.0437(8) Uani 1 1 d D . . H715 H 0.5626 -0.0319 0.4421 0.052 Uiso 1 1 calc R . . C716 C 0.49755(11) -0.02807(14) 0.37955(16) 0.0354(7) Uani 1 1 d D . . H716 H 0.4721 -0.0280 0.4158 0.042 Uiso 1 1 calc R . . C721 C 0.37721(10) -0.05886(14) 0.36212(14) 0.0295(6) Uani 1 1 d D . . C722 C 0.36740(10) -0.12912(15) 0.36833(15) 0.0333(6) Uani 1 1 d D . . H722 H 0.3771 -0.1594 0.3319 0.040 Uiso 1 1 calc R . . C723 C 0.34353(11) -0.15470(16) 0.42746(17) 0.0411(7) Uani 1 1 d D . . H723 H 0.3369 -0.2025 0.4312 0.049 Uiso 1 1 calc R . . C724 C 0.32934(11) -0.11203(17) 0.48085(16) 0.0430(8) Uani 1 1 d D . . H724 H 0.3130 -0.1302 0.5212 0.052 Uiso 1 1 calc R . . C725 C 0.33905(12) -0.04205(18) 0.47547(16) 0.0437(8) Uani 1 1 d D . . H725 H 0.3295 -0.0122 0.5123 0.052 Uiso 1 1 calc R . . C726 C 0.36277(11) -0.01572(16) 0.41602(15) 0.0375(7) Uani 1 1 d D . . H726 H 0.3691 0.0322 0.4123 0.045 Uiso 1 1 calc R . . C8 C 0.41092(12) -0.08957(14) 0.22021(14) 0.0334(6) Uani 1 1 d . . . H8 H 0.4375 -0.1240 0.2243 0.040 Uiso 1 1 calc R . . C9 C 0.37753(11) -0.09554(14) 0.16489(14) 0.0308(6) Uani 1 1 d . . . C91 C 0.38744(12) -0.15133(16) 0.10973(16) 0.0390(7) Uani 1 1 d . . . C92 C 0.3527(2) -0.1431(2) 0.0456(2) 0.0873(16) Uani 1 1 d . . . H92A H 0.3606 -0.1800 0.0128 0.131 Uiso 1 1 calc R . . H92B H 0.3600 -0.0986 0.0239 0.131 Uiso 1 1 calc R . . H92C H 0.3152 -0.1453 0.0590 0.131 Uiso 1 1 calc R . . C93 C 0.44495(17) -0.1518(3) 0.0875(3) 0.0973(19) Uani 1 1 d . . . H93A H 0.4676 -0.1615 0.1276 0.146 Uiso 1 1 calc R . . H93B H 0.4543 -0.1068 0.0683 0.146 Uiso 1 1 calc R . . H93C H 0.4503 -0.1872 0.0523 0.146 Uiso 1 1 calc R . . C94 C 0.3734(2) -0.22000(19) 0.1423(3) 0.0898(17) Uani 1 1 d . . . H94A H 0.3974 -0.2291 0.1812 0.135 Uiso 1 1 calc R . . H94B H 0.3770 -0.2565 0.1077 0.135 Uiso 1 1 calc R . . H94C H 0.3366 -0.2187 0.1591 0.135 Uiso 1 1 calc R . . N10 N 0.33450(10) -0.05649(12) 0.15498(13) 0.0328(5) Uani 1 1 d . . . H10 H 0.3165(13) -0.0630(16) 0.1223(17) 0.039 Uiso 1 1 d . . . N11 N 0.31587(8) -0.00853(11) 0.20278(12) 0.0286(5) Uani 1 1 d . . . O12 O 0.23749(8) -0.02601(11) 0.14519(11) 0.0445(5) Uani 1 1 d . . . C12 C 0.26338(11) 0.00259(14) 0.19199(14) 0.0309(6) Uani 1 1 d D . . C131 C 0.23583(10) 0.05034(14) 0.24069(14) 0.0304(6) Uani 1 1 d D . . C132 C 0.25062(11) 0.05714(15) 0.30961(15) 0.0362(7) Uani 1 1 d D . . H132 H 0.2806 0.0328 0.3267 0.043 Uiso 1 1 calc R . . C133 C 0.22179(12) 0.09931(17) 0.35344(17) 0.0453(8) Uani 1 1 d D . . H133 H 0.2324 0.1041 0.4003 0.054 Uiso 1 1 calc R . . C134 C 0.17783(12) 0.13437(17) 0.32964(18) 0.0464(8) Uani 1 1 d D . . H134 H 0.1580 0.1628 0.3601 0.056 Uiso 1 1 calc R . . C135 C 0.16295(12) 0.12785(17) 0.26152(18) 0.0456(8) Uani 1 1 d D . . H135 H 0.1328 0.1520 0.2449 0.055 Uiso 1 1 calc R . . C136 C 0.19156(11) 0.08637(16) 0.21700(17) 0.0383(7) Uani 1 1 d D . . H136 H 0.1810 0.0824 0.1700 0.046 Uiso 1 1 calc R . . C1S C 0.30659(13) 0.17207(17) 0.58453(18) 0.0475(8) Uani 1 1 d D . . H1S1 H 0.2950 0.1381 0.6195 0.057 Uiso 1 1 calc R . . H1S2 H 0.2814 0.2111 0.5858 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.37070(4) 0.20145(5) 0.60523(6) 0.0620(3) Uani 1 1 d D . . Cl2 Cl 0.30519(5) 0.13419(6) 0.50210(5) 0.0728(3) Uani 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 Pd 0.02082(10) 0.02090(10) 0.02484(11) -0.00046(8) -0.00091(8) -0.00053(7) P1 0.0208(3) 0.0243(3) 0.0256(3) -0.0017(3) -0.0001(3) -0.0013(3) C111 0.0267(13) 0.0252(13) 0.0266(13) -0.0008(11) -0.0025(11) -0.0042(11) C112 0.0290(14) 0.0413(17) 0.0309(15) 0.0011(13) 0.0041(12) -0.0040(13) C113 0.0472(18) 0.054(2) 0.0261(15) -0.0013(14) 0.0012(13) -0.0017(15) C114 0.0406(17) 0.0408(17) 0.0347(16) 0.0023(13) -0.0123(13) -0.0049(14) C115 0.0274(14) 0.0316(15) 0.0408(16) 0.0011(12) -0.0046(12) -0.0028(12) C116 0.0268(14) 0.0288(14) 0.0314(14) -0.0012(12) 0.0005(11) -0.0032(11) C121 0.0216(12) 0.0298(14) 0.0246(13) 0.0035(11) -0.0029(10) -0.0015(11) C122 0.0345(15) 0.0296(14) 0.0333(15) 0.0011(12) -0.0029(12) -0.0021(12) C123 0.0435(17) 0.0339(16) 0.0417(17) 0.0109(14) 0.0012(14) -0.0070(13) C124 0.0394(17) 0.053(2) 0.0344(16) 0.0100(15) 0.0077(14) -0.0073(15) C125 0.0399(17) 0.0478(19) 0.0390(17) 0.0005(14) 0.0111(14) 0.0055(15) C126 0.0399(16) 0.0294(15) 0.0352(16) 0.0038(12) 0.0048(13) 0.0011(13) C2 0.0271(14) 0.0283(14) 0.0311(14) -0.0056(11) 0.0002(11) -0.0002(11) C3 0.0240(13) 0.0257(14) 0.0291(14) 0.0001(11) 0.0063(11) -0.0005(11) C31 0.0308(15) 0.0305(15) 0.0394(16) -0.0046(13) 0.0073(12) 0.0034(12) C32 0.0433(18) 0.051(2) 0.0414(18) -0.0070(15) 0.0109(14) 0.0093(15) C33 0.0445(18) 0.0282(16) 0.059(2) -0.0052(14) 0.0076(16) 0.0027(14) C34 0.0324(16) 0.0380(17) 0.0532(19) -0.0022(15) 0.0053(14) 0.0100(13) N5 0.0232(11) 0.0272(12) 0.0369(13) -0.0032(10) -0.0020(10) 0.0036(10) N6 0.0267(11) 0.0249(11) 0.0302(12) -0.0010(9) -0.0032(9) 0.0012(9) O6 0.0343(11) 0.0414(12) 0.0458(12) 0.0020(10) -0.0147(9) 0.0036(9) C6 0.0302(14) 0.0263(14) 0.0359(15) 0.0043(12) -0.0062(12) -0.0063(12) C61 0.0452(17) 0.0323(15) 0.0284(15) 0.0032(12) -0.0084(13) -0.0001(13) C62 0.051(2) 0.089(3) 0.0410(19) -0.021(2) 0.0048(16) -0.010(2) C63 0.070(3) 0.130(4) 0.062(3) -0.039(3) 0.020(2) -0.004(3) C64 0.105(4) 0.080(3) 0.043(2) -0.018(2) 0.009(2) 0.014(3) C65 0.112(4) 0.051(2) 0.041(2) -0.0138(17) -0.028(2) 0.008(2) C66 0.064(2) 0.0429(19) 0.050(2) -0.0051(16) -0.0219(17) 0.0033(17) P7 0.0270(3) 0.0242(4) 0.0284(4) 0.0014(3) -0.0008(3) 0.0023(3) C711 0.0290(14) 0.0222(13) 0.0399(16) 0.0054(12) -0.0012(12) 0.0032(11) C712 0.0342(15) 0.0318(15) 0.0463(18) 0.0039(13) 0.0054(13) 0.0064(12) C713 0.0309(16) 0.0379(18) 0.069(2) 0.0032(16) 0.0111(16) 0.0067(13) C714 0.0272(15) 0.0321(17) 0.087(3) 0.0067(17) -0.0065(17) 0.0029(13) C715 0.0403(17) 0.0325(16) 0.058(2) 0.0112(15) -0.0137(16) -0.0035(14) C716 0.0317(15) 0.0304(15) 0.0439(17) 0.0060(13) -0.0046(13) -0.0044(12) C721 0.0215(13) 0.0354(15) 0.0315(14) 0.0052(12) -0.0033(11) -0.0023(11) C722 0.0255(14) 0.0352(15) 0.0392(16) 0.0052(13) -0.0056(12) -0.0017(12) C723 0.0272(15) 0.0414(17) 0.055(2) 0.0165(15) -0.0062(14) -0.0049(13) C724 0.0258(15) 0.063(2) 0.0401(18) 0.0175(16) -0.0016(13) -0.0043(14) C725 0.0353(17) 0.062(2) 0.0334(16) -0.0016(15) 0.0013(13) -0.0014(15) C726 0.0360(16) 0.0387(16) 0.0378(16) 0.0002(13) 0.0016(13) -0.0037(13) C8 0.0391(16) 0.0253(14) 0.0356(16) -0.0018(12) 0.0011(13) 0.0088(12) C9 0.0348(15) 0.0247(14) 0.0329(15) -0.0015(12) 0.0056(12) -0.0007(12) C91 0.0435(17) 0.0348(16) 0.0388(17) -0.0097(13) 0.0064(14) 0.0064(14) C92 0.121(4) 0.078(3) 0.063(3) -0.042(2) -0.031(3) 0.037(3) C93 0.058(3) 0.142(5) 0.093(3) -0.070(3) 0.031(2) -0.016(3) C94 0.146(5) 0.034(2) 0.089(3) -0.015(2) 0.041(3) -0.001(2) N10 0.0346(13) 0.0305(13) 0.0333(13) -0.0095(11) -0.0048(10) -0.0003(11) N11 0.0260(11) 0.0257(12) 0.0340(12) -0.0061(10) -0.0017(10) -0.0016(9) O12 0.0329(11) 0.0495(13) 0.0512(13) -0.0169(11) -0.0101(10) -0.0055(10) C12 0.0298(15) 0.0262(14) 0.0367(15) 0.0003(12) -0.0031(12) -0.0045(11) C131 0.0230(13) 0.0287(14) 0.0394(15) -0.0019(12) -0.0010(11) -0.0080(11) C132 0.0277(14) 0.0416(17) 0.0394(16) 0.0037(14) 0.0001(13) -0.0013(12) C133 0.0433(18) 0.054(2) 0.0386(17) -0.0068(15) 0.0084(14) -0.0066(16) C134 0.0346(17) 0.0446(19) 0.060(2) -0.0080(16) 0.0160(15) -0.0016(14) C135 0.0279(15) 0.0437(18) 0.065(2) 0.0013(16) 0.0024(15) 0.0050(13) C136 0.0289(15) 0.0416(17) 0.0444(17) 0.0002(14) -0.0032(13) -0.0037(13) C1S 0.0503(19) 0.0395(18) 0.053(2) -0.0068(15) 0.0059(16) -0.0040(15) Cl1 0.0474(5) 0.0558(5) 0.0827(7) -0.0200(5) -0.0028(5) 0.0028(4) Cl2 0.0831(7) 0.0889(8) 0.0463(5) -0.0131(5) 0.0042(5) -0.0206(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N6 2.117(2) . ? Pd N11 2.127(2) . ? Pd P1 2.2605(7) . ? Pd P7 2.2633(7) . ? P1 C2 1.748(3) . ? P1 C111 1.828(3) . ? P1 C121 1.831(3) . ? C111 C112 1.394(4) . ? C111 C116 1.397(3) . ? C112 C113 1.384(4) . ? C112 H112 0.9500 . ? C113 C114 1.382(4) . ? C113 H113 0.9500 . ? C114 C115 1.375(4) . ? C114 H114 0.9500 . ? C115 C116 1.384(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.384(4) . ? C121 C126 1.396(4) . ? C122 C123 1.387(4) . ? C122 H122 0.9500 . ? C123 C124 1.376(4) . ? C123 H123 0.9500 . ? C124 C125 1.379(4) . ? C124 H124 0.9500 . ? C125 C126 1.387(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C2 C3 1.364(4) . ? C2 H2 0.9500 . ? C3 N5 1.333(3) . ? C3 C31 1.545(4) . ? C31 C34 1.533(4) . ? C31 C32 1.538(4) . ? C31 C33 1.539(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N5 N6 1.394(3) . ? N5 H5 0.79(3) . ? N6 C6 1.360(3) . ? O6 C6 1.247(3) . ? C6 C61 1.496(4) . ? C61 C62 1.373(4) . ? C61 C66 1.383(4) . ? C62 C63 1.389(5) . ? C62 H62 0.9500 . ? C63 C64 1.368(6) . ? C63 H63 0.9500 . ? C64 C65 1.366(6) . ? C64 H64 0.9500 . ? C65 C66 1.392(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? P7 C8 1.755(3) . ? P7 C711 1.829(3) . ? P7 C721 1.833(3) . ? C711 C716 1.395(4) . ? C711 C712 1.401(4) . ? C712 C713 1.385(4) . ? C712 H712 0.9500 . ? C713 C714 1.384(5) . ? C713 H713 0.9500 . ? C714 C715 1.374(4) . ? C714 H714 0.9500 . ? C715 C716 1.393(4) . ? C715 H715 0.9500 . ? C716 H716 0.9500 . ? C721 C726 1.387(4) . ? C721 C722 1.396(4) . ? C722 C723 1.384(4) . ? C722 H722 0.9500 . ? C723 C724 1.372(4) . ? C723 H723 0.9500 . ? C724 C725 1.389(4) . ? C724 H724 0.9500 . ? C725 C726 1.393(4) . ? C725 H725 0.9500 . ? C726 H726 0.9500 . ? C8 C9 1.365(4) . ? C8 H8 0.9500 . ? C9 N10 1.337(4) . ? C9 C91 1.543(4) . ? C91 C93 1.509(5) . ? C91 C94 1.521(5) . ? C91 C92 1.525(5) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? N10 N11 1.395(3) . ? N10 H10 0.79(3) . ? N11 C12 1.355(3) . ? O12 C12 1.246(3) . ? C12 C131 1.494(4) . ? C131 C132 1.390(4) . ? C131 C136 1.394(4) . ? C132 C133 1.385(4) . ? C132 H132 0.9500 . ? C133 C134 1.379(4) . ? C133 H133 0.9500 . ? C134 C135 1.375(5) . ? C134 H134 0.9500 . ? C135 C136 1.383(4) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? C1S Cl2 1.756(3) . ? C1S Cl1 1.758(3) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? 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 N6 Pd N11 94.64(8) . . ? N6 Pd P1 80.94(6) . . ? N11 Pd P1 174.71(6) . . ? N6 Pd P7 174.78(6) . . ? N11 Pd P7 82.31(6) . . ? P1 Pd P7 102.31(3) . . ? C2 P1 C111 102.54(12) . . ? C2 P1 C121 109.53(12) . . ? C111 P1 C121 101.48(11) . . ? C2 P1 Pd 108.08(9) . . ? C111 P1 Pd 123.95(8) . . ? C121 P1 Pd 110.47(8) . . ? C112 C111 C116 118.7(2) . . ? C112 C111 P1 119.0(2) . . ? C116 C111 P1 122.3(2) . . ? C113 C112 C111 120.4(3) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C114 C113 C112 120.3(3) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 119.7(3) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C115 C116 120.7(3) . . ? C114 C115 H115 119.7 . . ? C116 C115 H115 119.7 . . ? C115 C116 C111 120.2(3) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C122 C121 C126 119.0(2) . . ? C122 C121 P1 120.4(2) . . ? C126 C121 P1 120.6(2) . . ? C121 C122 C123 120.1(3) . . ? C121 C122 H122 119.9 . . ? C123 C122 H122 119.9 . . ? C124 C123 C122 120.6(3) . . ? C124 C123 H123 119.7 . . ? C122 C123 H123 119.7 . . ? C123 C124 C125 120.0(3) . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C124 C125 C126 119.8(3) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C125 C126 C121 120.5(3) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C3 C2 P1 127.5(2) . . ? C3 C2 H2 116.3 . . ? P1 C2 H2 116.3 . . ? N5 C3 C2 124.2(2) . . ? N5 C3 C31 116.3(2) . . ? C2 C3 C31 119.5(2) . . ? C34 C31 C32 109.0(2) . . ? C34 C31 C33 107.9(2) . . ? C32 C31 C33 109.5(3) . . ? C34 C31 C3 112.7(2) . . ? C32 C31 C3 109.5(2) . . ? C33 C31 C3 108.2(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C3 N5 N6 123.0(2) . . ? C3 N5 H5 121(2) . . ? N6 N5 H5 115(2) . . ? C6 N6 N5 110.2(2) . . ? C6 N6 Pd 122.59(18) . . ? N5 N6 Pd 118.99(16) . . ? O6 C6 N6 123.2(3) . . ? O6 C6 C61 119.6(2) . . ? N6 C6 C61 117.0(2) . . ? C62 C61 C66 118.3(3) . . ? C62 C61 C6 121.4(3) . . ? C66 C61 C6 119.9(3) . . ? C61 C62 C63 121.3(4) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C64 C63 C62 119.9(4) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 119.7(4) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C64 C65 C66 120.5(4) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C61 C66 C65 120.4(4) . . ? C61 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C8 P7 C711 101.31(13) . . ? C8 P7 C721 109.65(13) . . ? C711 P7 C721 102.82(12) . . ? C8 P7 Pd 106.88(10) . . ? C711 P7 Pd 122.96(9) . . ? C721 P7 Pd 112.34(9) . . ? C716 C711 C712 118.5(3) . . ? C716 C711 P7 123.4(2) . . ? C712 C711 P7 118.0(2) . . ? C713 C712 C711 120.6(3) . . ? C713 C712 H712 119.7 . . ? C711 C712 H712 119.7 . . ? C714 C713 C712 120.3(3) . . ? C714 C713 H713 119.9 . . ? C712 C713 H713 119.9 . . ? C715 C714 C713 119.6(3) . . ? C715 C714 H714 120.2 . . ? C713 C714 H714 120.2 . . ? C714 C715 C716 120.9(3) . . ? C714 C715 H715 119.5 . . ? C716 C715 H715 119.5 . . ? C715 C716 C711 120.0(3) . . ? C715 C716 H716 120.0 . . ? C711 C716 H716 120.0 . . ? C726 C721 C722 118.9(3) . . ? C726 C721 P7 121.6(2) . . ? C722 C721 P7 119.5(2) . . ? C723 C722 C721 120.1(3) . . ? C723 C722 H722 120.0 . . ? C721 C722 H722 120.0 . . ? C724 C723 C722 121.0(3) . . ? C724 C723 H723 119.5 . . ? C722 C723 H723 119.5 . . ? C723 C724 C725 119.5(3) . . ? C723 C724 H724 120.2 . . ? C725 C724 H724 120.2 . . ? C724 C725 C726 119.9(3) . . ? C724 C725 H725 120.0 . . ? C726 C725 H725 120.0 . . ? C721 C726 C725 120.6(3) . . ? C721 C726 H726 119.7 . . ? C725 C726 H726 119.7 . . ? C9 C8 P7 128.1(2) . . ? C9 C8 H8 115.9 . . ? P7 C8 H8 115.9 . . ? N10 C9 C8 124.2(3) . . ? N10 C9 C91 115.6(2) . . ? C8 C9 C91 120.1(3) . . ? C93 C91 C94 109.6(4) . . ? C93 C91 C92 108.6(3) . . ? C94 C91 C92 107.2(4) . . ? C93 C91 C9 110.8(3) . . ? C94 C91 C9 107.2(3) . . ? C92 C91 C9 113.2(3) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 H94A 109.5 . . ? C91 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C91 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C9 N10 N11 123.9(2) . . ? C9 N10 H10 119(2) . . ? N11 N10 H10 117(2) . . ? C12 N11 N10 109.4(2) . . ? C12 N11 Pd 124.38(18) . . ? N10 N11 Pd 118.08(16) . . ? O12 C12 N11 123.4(3) . . ? O12 C12 C131 119.6(2) . . ? N11 C12 C131 117.1(2) . . ? C132 C131 C136 118.7(3) . . ? C132 C131 C12 122.6(3) . . ? C136 C131 C12 118.5(3) . . ? C133 C132 C131 120.2(3) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C134 C133 C132 120.7(3) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C135 C134 C133 119.5(3) . . ? C135 C134 H134 120.3 . . ? C133 C134 H134 120.3 . . ? C134 C135 C136 120.5(3) . . ? C134 C135 H135 119.7 . . ? C136 C135 H135 119.7 . . ? C135 C136 C131 120.4(3) . . ? C135 C136 H136 119.8 . . ? C131 C136 H136 119.8 . . ? Cl2 C1S Cl1 111.21(19) . . ? Cl2 C1S H1S1 109.4 . . ? Cl1 C1S H1S1 109.4 . . ? Cl2 C1S H1S2 109.4 . . ? Cl1 C1S H1S2 109.4 . . ? H1S1 C1S H1S2 108.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.492 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.061