Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Athanasia Dervisi' _publ_contact_author_address ; School of Chemistry Cardiff University Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email dervisia@cardiff.ac.uk _publ_section_title ; Synthesis and characterisation of benzyl phosphino-thioether and -thiolato Pd(II) complexes and their applications in Suzuki coupling reactions ; loop_ _publ_author_name 'Athanasia Dervisi' 'Despina Koursarou' 'Li-ling Ooi.' P.N.Horton M.B.Hursthouse data_[Pd(1)I]2 _database_code_depnum_ccdc_archive 'CCDC 602963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pd(1)I)2 _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 I2 P2 Pd2 S2' _chemical_formula_sum 'C32 H36 I2 P2 Pd2 S2' _chemical_formula_weight 1013.27 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' I I -0.4742 1.8119 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.50820(10) _cell_length_b 16.0768(2) _cell_length_c 29.9895(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6994.91(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 104895 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'Irregular Block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 3.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.576 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76617 _diffrn_reflns_av_R_equivalents 0.1120 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 30.06 _reflns_number_total 10173 _reflns_number_gt 7732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Large Rint due to poor quality of dataset resulting from a poor quality crystal. 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^)+(0.0282P)^2^+11.7474P] 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 10173 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.7263(2) -0.0551(2) 0.54222(12) 0.0204(7) Uani 1 1 d . . . C2 C 0.7522(3) 0.0228(2) 0.55733(13) 0.0241(8) Uani 1 1 d . . . H2 H 0.7188 0.0486 0.5808 0.029 Uiso 1 1 calc R . . C3 C 0.8273(3) 0.0633(3) 0.53806(14) 0.0310(9) Uani 1 1 d . . . H3 H 0.8452 0.1166 0.5486 0.037 Uiso 1 1 calc R . . C4 C 0.8757(3) 0.0266(3) 0.50381(14) 0.0330(9) Uani 1 1 d . . . H4 H 0.9264 0.0548 0.4907 0.040 Uiso 1 1 calc R . . C5 C 0.8505(3) -0.0512(3) 0.48856(14) 0.0340(10) Uani 1 1 d . . . H5 H 0.8841 -0.0767 0.4650 0.041 Uiso 1 1 calc R . . C6 C 0.7759(3) -0.0924(3) 0.50760(13) 0.0285(8) Uani 1 1 d . . . H6 H 0.7586 -0.1459 0.4971 0.034 Uiso 1 1 calc R . . C7 C 0.6484(3) -0.1919(2) 0.59669(11) 0.0215(7) Uani 1 1 d . . . C8 C 0.7375(3) -0.2217(2) 0.60011(13) 0.0244(8) Uani 1 1 d . . . H8 H 0.7865 -0.1938 0.5854 0.029 Uiso 1 1 calc R . . C9 C 0.7551(3) -0.2928(3) 0.62516(13) 0.0289(9) Uani 1 1 d . . . H9 H 0.8163 -0.3134 0.6274 0.035 Uiso 1 1 calc R . . C10 C 0.6844(3) -0.3332(3) 0.64664(13) 0.0324(9) Uani 1 1 d . . . H10 H 0.6969 -0.3813 0.6640 0.039 Uiso 1 1 calc R . . C11 C 0.5951(3) -0.3038(3) 0.64304(15) 0.0386(11) Uani 1 1 d . . . H11 H 0.5462 -0.3327 0.6573 0.046 Uiso 1 1 calc R . . C12 C 0.5769(3) -0.2325(3) 0.61864(14) 0.0345(10) Uani 1 1 d . . . H12 H 0.5159 -0.2113 0.6169 0.041 Uiso 1 1 calc R . . C13 C 0.5706(2) -0.1500(2) 0.51141(11) 0.0201(7) Uani 1 1 d . . . H13A H 0.5846 -0.1144 0.4854 0.024 Uiso 1 1 calc R . . H13B H 0.5997 -0.2049 0.5064 0.024 Uiso 1 1 calc R . . C14 C 0.4666(2) -0.1611(2) 0.51517(11) 0.0192(7) Uani 1 1 d . . . H14 H 0.4519 -0.2061 0.5371 0.023 Uiso 1 1 calc R . . C15 C 0.4232(2) -0.1810(2) 0.46997(12) 0.0240(8) Uani 1 1 d . . . H15A H 0.3563 -0.1903 0.4741 0.029 Uiso 1 1 calc R . . H15B H 0.4309 -0.1326 0.4500 0.029 Uiso 1 1 calc R . . C16 C 0.4652(3) -0.2573(3) 0.44790(15) 0.0361(10) Uani 1 1 d . . . H16A H 0.5317 -0.2490 0.4443 0.054 Uiso 1 1 calc R . . H16B H 0.4368 -0.2657 0.4186 0.054 Uiso 1 1 calc R . . H16C H 0.4542 -0.3063 0.4666 0.054 Uiso 1 1 calc R . . C17 C 0.2743(3) -0.1206(3) 0.70089(13) 0.0347(10) Uani 1 1 d . . . C18A C 0.3473(12) -0.1709(12) 0.6921(5) 0.028(3) Uani 0.33 1 d P A 1 H18A H 0.3755 -0.1696 0.6636 0.033 Uiso 0.33 1 calc PR A 1 C19A C 0.3807(13) -0.2240(14) 0.7245(5) 0.081(9) Uani 0.50 1 d P A 1 H19A H 0.4313 -0.2592 0.7176 0.097 Uiso 0.50 1 calc PR A 1 C20 C 0.3439(4) -0.2274(5) 0.76568(18) 0.0688(19) Uani 1 1 d . . . H20 H 0.3686 -0.2634 0.7878 0.083 Uiso 1 1 calc R A 1 C21 C 0.2717(5) -0.1786(4) 0.77446(19) 0.0686(19) Uani 1 1 d . A . H21 H 0.2449 -0.1797 0.8034 0.082 Uiso 1 1 calc R . . C22 C 0.2351(4) -0.1263(4) 0.74219(17) 0.0626(18) Uani 1 1 d . A . H22 H 0.1820 -0.0941 0.7489 0.075 Uiso 1 1 calc R . . C23 C 0.1062(3) -0.0510(3) 0.65808(13) 0.0329(9) Uani 1 1 d . . . C24 C 0.0555(4) -0.0264(6) 0.69542(19) 0.082(3) Uani 1 1 d . A . H24 H 0.0867 -0.0110 0.7220 0.099 Uiso 1 1 calc R . . C25 C -0.0402(4) -0.0242(6) 0.6939(2) 0.083(3) Uani 1 1 d . . . H25 H -0.0741 -0.0100 0.7199 0.100 Uiso 1 1 calc R A . C26 C -0.0864(3) -0.0424(3) 0.65483(18) 0.0474(12) Uani 1 1 d . A . H26 H -0.1519 -0.0424 0.6540 0.057 Uiso 1 1 calc R . . C27 C -0.0368(3) -0.0602(3) 0.61776(16) 0.0395(11) Uani 1 1 d . . . H27 H -0.0676 -0.0693 0.5902 0.047 Uiso 1 1 calc R A . C28 C 0.0585(3) -0.0655(3) 0.61952(14) 0.0348(10) Uani 1 1 d . A . H28 H 0.0916 -0.0795 0.5932 0.042 Uiso 1 1 calc R . . C29 C 0.2597(3) 0.0544(3) 0.67918(14) 0.0346(10) Uani 1 1 d . . . H29A H 0.2200 0.0963 0.6645 0.042 Uiso 1 1 calc R A . H29B H 0.2482 0.0568 0.7117 0.042 Uiso 1 1 calc R . . C30 C 0.3612(3) 0.0735(3) 0.66957(12) 0.0287(9) Uani 1 1 d . A . H30 H 0.4008 0.0330 0.6861 0.034 Uiso 1 1 calc R . . C31 C 0.3909(3) 0.1622(3) 0.68150(15) 0.0418(11) Uani 1 1 d . . . H31A H 0.4511 0.1743 0.6673 0.050 Uiso 1 1 calc R A . H31B H 0.3452 0.2021 0.6696 0.050 Uiso 1 1 calc R . . C32 C 0.3993(4) 0.1737(5) 0.73165(19) 0.073(2) Uani 1 1 d . A . H32A H 0.3390 0.1646 0.7456 0.110 Uiso 1 1 calc R . . H32B H 0.4204 0.2303 0.7381 0.110 Uiso 1 1 calc R . . H32C H 0.4438 0.1336 0.7436 0.110 Uiso 1 1 calc R . . I1 I 0.606461(17) 0.008094(17) 0.665542(8) 0.02675(6) Uani 1 1 d . . . I2 I 0.249133(19) -0.217748(18) 0.576944(10) 0.03329(7) Uani 1 1 d . A . P1 P 0.61976(6) -0.10255(6) 0.56200(3) 0.01810(18) Uani 1 1 d . . . P2 P 0.23148(7) -0.05040(8) 0.65787(3) 0.0277(2) Uani 1 1 d . A . Pd1 Pd 0.511778(18) -0.019898(16) 0.592083(9) 0.01702(6) Uani 1 1 d . A . Pd2 Pd 0.309941(18) -0.067593(18) 0.593539(9) 0.01984(6) Uani 1 1 d . . . S1 S 0.37782(6) 0.05853(6) 0.60904(3) 0.02257(18) Uani 1 1 d . A . S2 S 0.41791(6) -0.06039(5) 0.53445(3) 0.01819(16) Uani 1 1 d . A . C19B C 0.405(2) -0.1847(17) 0.7304(9) 0.047(7) Uiso 0.25 1 d P A 2 H19B H 0.4700 -0.1904 0.7319 0.056 Uiso 0.25 1 calc PR A 2 C18C C 0.3340(13) -0.1991(10) 0.6905(6) 0.025(4) Uiso 0.33 1 d P A 3 H18C H 0.3445 -0.2110 0.6599 0.030 Uiso 0.33 1 calc PR A 3 C18B C 0.3648(12) -0.1375(11) 0.6962(6) 0.037(5) Uiso 0.33 1 d P A 2 H18B H 0.3993 -0.1185 0.6713 0.044 Uiso 0.33 1 calc PR A 2 C19C C 0.373(2) -0.2535(18) 0.7211(11) 0.035(6) Uiso 0.25 1 d P A 3 H19C H 0.4125 -0.2992 0.7143 0.042 Uiso 0.25 1 calc PR A 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0177(17) 0.0225(18) 0.0211(17) 0.0032(14) -0.0001(13) 0.0001(14) C2 0.0231(18) 0.0240(19) 0.0253(19) -0.0017(14) 0.0003(14) -0.0015(15) C3 0.027(2) 0.030(2) 0.036(2) -0.0026(17) 0.0016(16) -0.0066(17) C4 0.026(2) 0.037(2) 0.035(2) 0.0081(18) 0.0045(17) -0.0051(18) C5 0.026(2) 0.046(3) 0.030(2) -0.0042(18) 0.0105(16) -0.0026(19) C6 0.0243(19) 0.031(2) 0.030(2) -0.0038(16) 0.0009(15) -0.0036(17) C7 0.0267(19) 0.0181(17) 0.0198(17) -0.0022(13) -0.0009(14) 0.0025(14) C8 0.0219(19) 0.0228(19) 0.029(2) -0.0005(15) -0.0012(14) 0.0030(15) C9 0.033(2) 0.025(2) 0.028(2) -0.0039(15) -0.0047(16) 0.0090(17) C10 0.046(3) 0.0222(19) 0.029(2) 0.0028(16) 0.0037(18) 0.0095(18) C11 0.040(3) 0.036(2) 0.040(3) 0.013(2) 0.0120(19) 0.005(2) C12 0.025(2) 0.038(2) 0.041(2) 0.0148(19) 0.0067(17) 0.0070(18) C13 0.0203(17) 0.0184(17) 0.0217(18) -0.0033(13) -0.0012(13) 0.0031(14) C14 0.0215(17) 0.0164(16) 0.0198(17) -0.0006(13) 0.0016(13) 0.0012(13) C15 0.0157(17) 0.028(2) 0.0278(19) -0.0091(15) -0.0010(14) -0.0018(15) C16 0.025(2) 0.042(3) 0.041(2) -0.022(2) -0.0033(17) 0.0028(19) C17 0.030(2) 0.053(3) 0.021(2) -0.0052(18) 0.0010(16) 0.001(2) C18A 0.033(9) 0.029(11) 0.021(7) 0.002(8) 0.003(6) 0.009(9) C19A 0.083(14) 0.13(2) 0.031(7) -0.016(12) -0.013(7) 0.080(16) C20 0.068(4) 0.100(5) 0.038(3) 0.016(3) -0.010(3) 0.028(4) C21 0.099(5) 0.064(4) 0.042(3) 0.016(3) 0.022(3) 0.022(4) C22 0.084(4) 0.062(4) 0.042(3) 0.018(3) 0.029(3) 0.033(3) C23 0.024(2) 0.051(3) 0.023(2) -0.0018(18) 0.0034(15) -0.0015(19) C24 0.027(3) 0.185(9) 0.035(3) -0.016(4) 0.002(2) 0.009(4) C25 0.025(3) 0.174(9) 0.050(4) -0.015(4) 0.010(2) 0.006(4) C26 0.026(2) 0.056(3) 0.060(3) 0.001(2) -0.001(2) 0.002(2) C27 0.031(2) 0.041(3) 0.046(3) -0.010(2) -0.0085(19) 0.011(2) C28 0.032(2) 0.041(3) 0.031(2) -0.0053(18) -0.0031(17) 0.009(2) C29 0.027(2) 0.051(3) 0.026(2) -0.0158(19) 0.0015(16) 0.007(2) C30 0.029(2) 0.034(2) 0.0235(19) -0.0098(16) 0.0004(15) 0.0029(17) C31 0.042(3) 0.046(3) 0.037(2) -0.019(2) -0.006(2) 0.002(2) C32 0.057(4) 0.103(6) 0.060(4) -0.043(4) 0.000(3) -0.013(4) I1 0.02303(12) 0.03501(14) 0.02222(12) -0.00136(10) -0.00338(9) -0.00215(10) I2 0.02933(14) 0.02752(14) 0.04300(16) -0.00562(11) 0.00878(11) -0.00755(11) P1 0.0161(4) 0.0191(4) 0.0191(4) -0.0001(3) -0.0001(3) 0.0010(3) P2 0.0201(5) 0.0435(6) 0.0196(5) -0.0063(4) 0.0019(4) -0.0016(4) Pd1 0.01608(12) 0.01707(12) 0.01791(13) -0.00109(9) -0.00019(9) 0.00029(10) Pd2 0.01735(13) 0.02447(14) 0.01769(13) -0.00358(10) 0.00119(10) -0.00105(10) S1 0.0215(4) 0.0228(4) 0.0234(4) -0.0050(3) -0.0014(3) 0.0032(4) S2 0.0173(4) 0.0196(4) 0.0177(4) -0.0002(3) -0.0004(3) 0.0010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.383(5) . ? C1 C6 1.399(5) . ? C1 P1 1.823(4) . ? C2 C3 1.395(5) . ? C3 C4 1.377(6) . ? C4 C5 1.382(6) . ? C5 C6 1.391(6) . ? C7 C8 1.382(5) . ? C7 C12 1.391(5) . ? C7 P1 1.822(4) . ? C8 C9 1.391(5) . ? C9 C10 1.374(6) . ? C10 C11 1.383(6) . ? C11 C12 1.386(6) . ? C13 C14 1.524(5) . ? C13 P1 1.842(3) . ? C14 C15 1.528(5) . ? C14 S2 1.859(4) . ? C15 C16 1.521(5) . ? C17 C18B 1.348(19) . ? C17 C18A 1.358(15) . ? C17 C22 1.366(6) . ? C17 C18C 1.562(18) . ? C17 P2 1.824(5) . ? C18A C19A 1.38(2) . ? C19A C20 1.345(17) . ? C20 C21 1.336(8) . ? C20 C19C 1.46(3) . ? C20 C19B 1.54(3) . ? C21 C22 1.387(8) . ? C23 C28 1.368(6) . ? C23 C24 1.397(7) . ? C23 P2 1.817(4) . ? C24 C25 1.390(8) . ? C25 C26 1.380(8) . ? C26 C27 1.355(7) . ? C27 C28 1.386(6) . ? C29 C30 1.533(6) . ? C29 P2 1.847(5) . ? C30 C31 1.532(6) . ? C30 S1 1.847(4) . ? C31 C32 1.520(7) . ? I1 Pd1 2.6349(4) . ? I2 Pd2 2.6179(4) . ? P1 Pd1 2.2436(9) . ? P2 Pd2 2.2570(10) . ? Pd1 S2 2.2947(9) . ? Pd1 S1 2.3719(9) . ? Pd1 Pd2 3.0273(4) . ? Pd2 S1 2.3016(10) . ? Pd2 S2 2.3679(9) . ? C19B C18B 1.40(3) . ? C18C C19C 1.39(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.5(3) . . ? C2 C1 P1 120.2(3) . . ? C6 C1 P1 119.9(3) . . ? C1 C2 C3 119.9(4) . . ? C4 C3 C2 120.5(4) . . ? C3 C4 C5 120.0(4) . . ? C4 C5 C6 120.1(4) . . ? C5 C6 C1 120.1(4) . . ? C8 C7 C12 120.0(4) . . ? C8 C7 P1 122.0(3) . . ? C12 C7 P1 118.0(3) . . ? C7 C8 C9 119.8(4) . . ? C10 C9 C8 120.3(4) . . ? C9 C10 C11 120.1(4) . . ? C10 C11 C12 120.1(4) . . ? C11 C12 C7 119.7(4) . . ? C14 C13 P1 111.8(2) . . ? C13 C14 C15 111.5(3) . . ? C13 C14 S2 107.3(2) . . ? C15 C14 S2 107.6(2) . . ? C16 C15 C14 112.9(3) . . ? C18B C17 C18A 25.9(9) . . ? C18B C17 C22 119.1(9) . . ? C18A C17 C22 117.4(7) . . ? C18B C17 C18C 43.7(9) . . ? C18A C17 C18C 17.8(10) . . ? C22 C17 C18C 111.0(8) . . ? C18B C17 P2 112.5(8) . . ? C18A C17 P2 119.8(7) . . ? C22 C17 P2 122.8(4) . . ? C18C C17 P2 123.2(7) . . ? C17 C18A C19A 120.3(13) . . ? C20 C19A C18A 122.1(13) . . ? C21 C20 C19A 117.9(8) . . ? C21 C20 C19C 125.3(15) . . ? C19A C20 C19C 19.7(16) . . ? C21 C20 C19B 108.9(13) . . ? C19A C20 C19B 28.9(11) . . ? C19C C20 C19B 48.2(15) . . ? C20 C21 C22 121.3(5) . . ? C17 C22 C21 120.9(5) . . ? C28 C23 C24 117.3(4) . . ? C28 C23 P2 120.3(3) . . ? C24 C23 P2 121.9(4) . . ? C25 C24 C23 120.4(5) . . ? C26 C25 C24 120.5(5) . . ? C27 C26 C25 118.9(5) . . ? C26 C27 C28 120.8(4) . . ? C23 C28 C27 121.8(4) . . ? C30 C29 P2 109.3(3) . . ? C31 C30 C29 114.4(4) . . ? C31 C30 S1 108.3(3) . . ? C29 C30 S1 106.5(3) . . ? C32 C31 C30 111.5(5) . . ? C7 P1 C1 108.81(17) . . ? C7 P1 C13 103.41(16) . . ? C1 P1 C13 103.53(16) . . ? C7 P1 Pd1 113.38(12) . . ? C1 P1 Pd1 118.35(13) . . ? C13 P1 Pd1 107.82(11) . . ? C23 P2 C17 109.6(2) . . ? C23 P2 C29 103.0(2) . . ? C17 P2 C29 104.1(2) . . ? C23 P2 Pd2 120.44(13) . . ? C17 P2 Pd2 110.92(14) . . ? C29 P2 Pd2 107.20(14) . . ? P1 Pd1 S2 86.76(3) . . ? P1 Pd1 S1 166.71(3) . . ? S2 Pd1 S1 79.98(3) . . ? P1 Pd1 I1 94.20(2) . . ? S2 Pd1 I1 170.96(3) . . ? S1 Pd1 I1 99.04(2) . . ? P1 Pd1 Pd2 122.09(3) . . ? S2 Pd1 Pd2 50.57(2) . . ? S1 Pd1 Pd2 48.62(2) . . ? I1 Pd1 Pd2 122.378(12) . . ? P2 Pd2 S1 86.28(4) . . ? P2 Pd2 S2 165.31(4) . . ? S1 Pd2 S2 79.92(3) . . ? P2 Pd2 I2 96.05(3) . . ? S1 Pd2 I2 174.24(3) . . ? S2 Pd2 I2 97.23(2) . . ? P2 Pd2 Pd1 117.98(3) . . ? S1 Pd2 Pd1 50.65(2) . . ? S2 Pd2 Pd1 48.47(2) . . ? I2 Pd2 Pd1 123.834(13) . . ? C30 S1 Pd2 104.93(14) . . ? C30 S1 Pd1 112.76(14) . . ? Pd2 S1 Pd1 80.73(3) . . ? C14 S2 Pd1 104.84(11) . . ? C14 S2 Pd2 116.19(12) . . ? Pd1 S2 Pd2 80.96(3) . . ? C18B C19B C20 120(2) . . ? C19C C18C C17 127.1(19) . . ? C17 C18B C19B 115.9(18) . . ? C18C C19C C20 108(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.991 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.158 #===END data_Pd(3)Cl2.CHCl3 _database_code_depnum_ccdc_archive 'CCDC 602964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Pd(3)Cl2.CHCl3 _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Cl5 P Pd S' _chemical_formula_sum 'C24 H26 Cl5 P Pd S' _chemical_formula_weight 661.13 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 14.7145(2) _cell_length_b 13.2355(2) _cell_length_c 14.8381(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.7700(10) _cell_angle_gamma 90.00 _cell_volume 2664.56(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25254 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.034 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7467 _exptl_absorpt_correction_T_max 0.7742 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39701 _diffrn_reflns_av_R_equivalents 0.0873 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7770 _reflns_number_gt 6398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdiff-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0268P)^2^+2.9514P] 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 7770 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.26874(16) 1.03760(18) -0.02473(16) 0.0173(4) Uani 1 1 d . . . C2 C 0.19413(17) 1.08669(18) -0.10101(17) 0.0213(5) Uani 1 1 d . . . H2 H 0.1270 1.0738 -0.1128 0.026 Uiso 1 1 calc R . . C3 C 0.21837(19) 1.1549(2) -0.16005(18) 0.0268(5) Uani 1 1 d . . . H3 H 0.1678 1.1882 -0.2123 0.032 Uiso 1 1 calc R . . C4 C 0.31659(19) 1.1737(2) -0.14204(19) 0.0275(5) Uani 1 1 d . . . H4 H 0.3331 1.2200 -0.1822 0.033 Uiso 1 1 calc R . . C5 C 0.39062(19) 1.1257(2) -0.06627(19) 0.0280(6) Uani 1 1 d . . . H5 H 0.4577 1.1391 -0.0546 0.034 Uiso 1 1 calc R . . C6 C 0.36719(17) 1.05774(19) -0.00691(17) 0.0222(5) Uani 1 1 d . . . H6 H 0.4182 1.0252 0.0456 0.027 Uiso 1 1 calc R . . C7 C 0.34449(16) 0.88190(18) 0.12542(16) 0.0179(4) Uani 1 1 d . . . C8 C 0.40885(18) 0.9325(2) 0.20864(17) 0.0250(5) Uani 1 1 d . . . H8 H 0.3940 0.9989 0.2230 0.030 Uiso 1 1 calc R . . C9 C 0.49460(19) 0.8847(2) 0.26989(19) 0.0313(6) Uani 1 1 d . . . H9 H 0.5395 0.9194 0.3253 0.038 Uiso 1 1 calc R . . C10 C 0.51500(19) 0.7868(2) 0.25061(19) 0.0310(6) Uani 1 1 d . . . H10 H 0.5728 0.7539 0.2939 0.037 Uiso 1 1 calc R . . C11 C 0.45176(19) 0.7369(2) 0.16892(19) 0.0296(6) Uani 1 1 d . . . H11 H 0.4663 0.6699 0.1559 0.036 Uiso 1 1 calc R . . C12 C 0.36676(18) 0.78440(19) 0.10545(18) 0.0238(5) Uani 1 1 d . . . H12 H 0.3239 0.7503 0.0485 0.029 Uiso 1 1 calc R . . C13 C 0.15750(16) 0.85523(17) -0.04447(15) 0.0169(4) Uani 1 1 d . . . H13A H 0.1081 0.8923 -0.0997 0.020 Uiso 1 1 calc R . . H13B H 0.1999 0.8166 -0.0702 0.020 Uiso 1 1 calc R . . C14 C 0.10429(16) 0.78153(17) -0.00253(15) 0.0165(4) Uani 1 1 d . . . H14 H 0.1536 0.7345 0.0437 0.020 Uiso 1 1 calc R . . C15 C 0.02798(18) 0.71988(18) -0.08439(17) 0.0227(5) Uani 1 1 d . . . H15A H -0.0202 0.7672 -0.1299 0.027 Uiso 1 1 calc R . . H15B H 0.0621 0.6850 -0.1214 0.027 Uiso 1 1 calc R . . C16 C -0.0281(2) 0.6416(2) -0.0515(2) 0.0358(7) Uani 1 1 d . . . H16A H 0.0187 0.5964 -0.0035 0.054 Uiso 1 1 calc R . . H16B H -0.0706 0.6022 -0.1080 0.054 Uiso 1 1 calc R . . H16C H -0.0687 0.6757 -0.0216 0.054 Uiso 1 1 calc R . . C17 C 0.05658(18) 0.77509(19) 0.17011(17) 0.0225(5) Uani 1 1 d . . . H17A H 0.0346 0.8138 0.2152 0.027 Uiso 1 1 calc R . . H17B H 0.0112 0.7171 0.1454 0.027 Uiso 1 1 calc R . . C18 C 0.15824(18) 0.73530(19) 0.22675(16) 0.0222(5) Uani 1 1 d . . . C19 C 0.1806(2) 0.6345(2) 0.21756(18) 0.0296(6) Uani 1 1 d . . . H19 H 0.1311 0.5908 0.1754 0.036 Uiso 1 1 calc R . . C20 C 0.2751(2) 0.5973(2) 0.2698(2) 0.0373(7) Uani 1 1 d . . . H20 H 0.2900 0.5287 0.2627 0.045 Uiso 1 1 calc R . . C21 C 0.3471(2) 0.6602(3) 0.3321(2) 0.0385(7) Uani 1 1 d . . . H21 H 0.4114 0.6347 0.3678 0.046 Uiso 1 1 calc R . . C22 C 0.3258(2) 0.7601(2) 0.34263(19) 0.0330(6) Uani 1 1 d . . . H22 H 0.3752 0.8031 0.3859 0.040 Uiso 1 1 calc R . . C23 C 0.23192(19) 0.7976(2) 0.28987(17) 0.0262(5) Uani 1 1 d . . . H23 H 0.2177 0.8665 0.2968 0.031 Uiso 1 1 calc R . . C24 C 0.2685(2) 0.4335(2) -0.0459(2) 0.0326(6) Uani 1 1 d . . . H24 H 0.2177 0.4240 -0.1135 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.05690(4) 1.02990(5) 0.23323(4) 0.02215(12) Uani 1 1 d . . . Cl2 Cl 0.23876(4) 1.14001(4) 0.17629(4) 0.02428(12) Uani 1 1 d . . . Cl3 Cl 0.26702(5) 0.32809(5) 0.02509(6) 0.03758(16) Uani 1 1 d . . . Cl4 Cl 0.38456(6) 0.44863(8) -0.05236(6) 0.0553(2) Uani 1 1 d . . . Cl5 Cl 0.23903(9) 0.54223(7) 0.00543(8) 0.0655(3) Uani 1 1 d . . . P1 P 0.23305(4) 0.94575(4) 0.04576(4) 0.01456(11) Uani 1 1 d . . . Pd1 Pd 0.144272(12) 0.994778(12) 0.129005(11) 0.01493(5) Uani 1 1 d . . . S1 S 0.04587(4) 0.85699(4) 0.06575(4) 0.01684(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0182(10) 0.0192(11) 0.0150(10) 0.0018(8) 0.0070(8) -0.0009(9) C2 0.0171(10) 0.0236(12) 0.0229(12) 0.0032(9) 0.0073(9) 0.0005(9) C3 0.0257(12) 0.0279(13) 0.0249(12) 0.0104(10) 0.0079(10) 0.0054(10) C4 0.0293(13) 0.0276(13) 0.0292(13) 0.0092(10) 0.0153(11) 0.0005(11) C5 0.0209(12) 0.0314(14) 0.0339(14) 0.0093(11) 0.0129(11) -0.0030(10) C6 0.0171(11) 0.0242(12) 0.0223(12) 0.0060(9) 0.0043(9) 0.0003(9) C7 0.0166(10) 0.0234(11) 0.0149(10) 0.0035(8) 0.0074(8) 0.0001(9) C8 0.0234(12) 0.0290(13) 0.0177(11) 0.0006(9) 0.0026(9) 0.0013(10) C9 0.0217(12) 0.0457(17) 0.0209(12) 0.0040(11) 0.0021(10) 0.0033(12) C10 0.0207(12) 0.0451(17) 0.0275(13) 0.0148(12) 0.0098(10) 0.0100(12) C11 0.0297(13) 0.0299(14) 0.0332(14) 0.0095(11) 0.0165(11) 0.0100(11) C12 0.0247(12) 0.0253(12) 0.0229(12) 0.0041(10) 0.0106(10) 0.0023(10) C13 0.0183(10) 0.0196(11) 0.0137(10) -0.0013(8) 0.0072(8) -0.0024(9) C14 0.0175(10) 0.0163(10) 0.0147(10) -0.0012(8) 0.0053(8) -0.0007(8) C15 0.0253(12) 0.0204(12) 0.0191(11) -0.0034(9) 0.0050(9) -0.0049(10) C16 0.0402(16) 0.0322(15) 0.0317(15) -0.0027(12) 0.0103(12) -0.0185(13) C17 0.0252(12) 0.0259(12) 0.0201(11) 0.0046(9) 0.0127(10) -0.0026(10) C18 0.0276(12) 0.0259(12) 0.0160(11) 0.0080(9) 0.0117(9) 0.0020(10) C19 0.0408(15) 0.0275(14) 0.0224(12) 0.0063(10) 0.0142(11) 0.0021(12) C20 0.0505(18) 0.0338(15) 0.0355(15) 0.0145(12) 0.0252(14) 0.0170(14) C21 0.0319(15) 0.056(2) 0.0304(15) 0.0208(14) 0.0148(12) 0.0130(14) C22 0.0281(13) 0.0479(18) 0.0234(13) 0.0115(12) 0.0104(11) -0.0018(13) C23 0.0281(13) 0.0309(13) 0.0204(12) 0.0072(10) 0.0102(10) -0.0012(11) C24 0.0292(14) 0.0333(15) 0.0266(13) 0.0014(11) 0.0012(11) -0.0023(12) Cl1 0.0195(3) 0.0300(3) 0.0180(3) -0.0022(2) 0.0084(2) 0.0044(2) Cl2 0.0266(3) 0.0190(3) 0.0264(3) -0.0090(2) 0.0094(2) -0.0071(2) Cl3 0.0355(4) 0.0303(4) 0.0440(4) 0.0025(3) 0.0121(3) -0.0011(3) Cl4 0.0416(4) 0.0843(7) 0.0421(5) -0.0008(4) 0.0185(4) -0.0182(5) Cl5 0.0977(8) 0.0326(4) 0.0743(7) 0.0009(4) 0.0422(6) 0.0128(5) P1 0.0142(2) 0.0166(3) 0.0127(2) 0.0005(2) 0.0049(2) -0.0010(2) Pd1 0.01538(8) 0.01631(9) 0.01261(8) -0.00119(6) 0.00488(6) 0.00047(6) S1 0.0155(2) 0.0194(3) 0.0159(2) 0.0006(2) 0.0064(2) -0.0006(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 C1 C6 1.394(3) . ? C1 C2 1.395(3) . ? C1 P1 1.809(2) . ? C2 C3 1.397(3) . ? C2 H2 0.9500 . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.391(3) . ? C7 C8 1.402(3) . ? C7 P1 1.817(2) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 C11 1.378(4) . ? C10 H10 0.9500 . ? C11 C12 1.391(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.526(3) . ? C13 P1 1.820(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.532(3) . ? C14 S1 1.854(2) . ? C14 H14 1.0000 . ? C15 C16 1.518(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.499(3) . ? C17 S1 1.846(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.394(4) . ? C18 C23 1.396(4) . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.381(4) . ? C21 H21 0.9500 . ? C22 C23 1.389(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 Cl3 1.753(3) . ? C24 Cl5 1.759(3) . ? C24 Cl4 1.759(3) . ? C24 H24 1.0000 . ? Cl1 Pd1 2.4082(6) . ? Cl2 Pd1 2.3163(6) . ? P1 Pd1 2.2141(6) . ? Pd1 S1 2.2916(6) . ? 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 C6 C1 C2 119.9(2) . . ? C6 C1 P1 122.13(17) . . ? C2 C1 P1 117.94(17) . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 119.8(2) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C7 C8 119.7(2) . . ? C12 C7 P1 121.38(18) . . ? C8 C7 P1 118.88(18) . . ? C9 C8 C7 119.5(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.9(2) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 P1 112.61(15) . . ? C14 C13 H13A 109.1 . . ? P1 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? P1 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 110.58(18) . . ? C13 C14 S1 107.34(15) . . ? C15 C14 S1 111.57(16) . . ? C13 C14 H14 109.1 . . ? C15 C14 H14 109.1 . . ? S1 C14 H14 109.1 . . ? C16 C15 C14 115.5(2) . . ? C16 C15 H15A 108.4 . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C14 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 114.78(16) . . ? C18 C17 H17A 108.6 . . ? S1 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? S1 C17 H17B 108.6 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C23 118.7(2) . . ? C19 C18 C17 120.2(2) . . ? C23 C18 C17 121.1(2) . . ? C20 C19 C18 120.4(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C18 120.8(3) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? Cl3 C24 Cl5 109.19(16) . . ? Cl3 C24 Cl4 111.18(15) . . ? Cl5 C24 Cl4 109.75(16) . . ? Cl3 C24 H24 108.9 . . ? Cl5 C24 H24 108.9 . . ? Cl4 C24 H24 108.9 . . ? C1 P1 C7 107.33(10) . . ? C1 P1 C13 104.38(10) . . ? C7 P1 C13 108.24(11) . . ? C1 P1 Pd1 119.45(8) . . ? C7 P1 Pd1 110.62(7) . . ? C13 P1 Pd1 106.21(7) . . ? P1 Pd1 S1 87.36(2) . . ? P1 Pd1 Cl2 89.86(2) . . ? S1 Pd1 Cl2 174.01(2) . . ? P1 Pd1 Cl1 172.61(2) . . ? S1 Pd1 Cl1 90.40(2) . . ? Cl2 Pd1 Cl1 93.00(2) . . ? C17 S1 C14 103.59(11) . . ? C17 S1 Pd1 106.76(8) . . ? C14 S1 Pd1 107.42(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.8(4) . . . . ? P1 C1 C2 C3 -177.2(2) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? P1 C1 C6 C5 177.0(2) . . . . ? C12 C7 C8 C9 0.4(4) . . . . ? P1 C7 C8 C9 -179.7(2) . . . . ? C7 C8 C9 C10 -1.9(4) . . . . ? C8 C9 C10 C11 1.9(4) . . . . ? C9 C10 C11 C12 -0.3(4) . . . . ? C10 C11 C12 C7 -1.2(4) . . . . ? C8 C7 C12 C11 1.1(4) . . . . ? P1 C7 C12 C11 -178.80(19) . . . . ? P1 C13 C14 C15 169.80(16) . . . . ? P1 C13 C14 S1 47.89(18) . . . . ? C13 C14 C15 C16 178.4(2) . . . . ? S1 C14 C15 C16 -62.2(3) . . . . ? S1 C17 C18 C19 -106.0(2) . . . . ? S1 C17 C18 C23 74.4(3) . . . . ? C23 C18 C19 C20 -0.6(4) . . . . ? C17 C18 C19 C20 179.8(2) . . . . ? C18 C19 C20 C21 0.7(4) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C20 C21 C22 C23 -0.5(4) . . . . ? C21 C22 C23 C18 0.6(4) . . . . ? C19 C18 C23 C22 0.0(4) . . . . ? C17 C18 C23 C22 179.6(2) . . . . ? C6 C1 P1 C7 -6.7(2) . . . . ? C2 C1 P1 C7 171.31(19) . . . . ? C6 C1 P1 C13 -121.4(2) . . . . ? C2 C1 P1 C13 56.6(2) . . . . ? C6 C1 P1 Pd1 120.19(19) . . . . ? C2 C1 P1 Pd1 -61.8(2) . . . . ? C12 C7 P1 C1 -104.2(2) . . . . ? C8 C7 P1 C1 75.9(2) . . . . ? C12 C7 P1 C13 7.9(2) . . . . ? C8 C7 P1 C13 -171.97(18) . . . . ? C12 C7 P1 Pd1 123.90(18) . . . . ? C8 C7 P1 Pd1 -56.0(2) . . . . ? C14 C13 P1 C1 -169.54(16) . . . . ? C14 C13 P1 C7 76.36(18) . . . . ? C14 C13 P1 Pd1 -42.45(17) . . . . ? C1 P1 Pd1 S1 133.55(9) . . . . ? C7 P1 Pd1 S1 -101.14(8) . . . . ? C13 P1 Pd1 S1 16.09(8) . . . . ? C1 P1 Pd1 Cl2 -41.13(9) . . . . ? C7 P1 Pd1 Cl2 84.17(8) . . . . ? C13 P1 Pd1 Cl2 -158.60(8) . . . . ? C1 P1 Pd1 Cl1 -154.00(17) . . . . ? C7 P1 Pd1 Cl1 -28.7(2) . . . . ? C13 P1 Pd1 Cl1 88.53(18) . . . . ? C18 C17 S1 C14 51.1(2) . . . . ? C18 C17 S1 Pd1 -62.15(19) . . . . ? C13 C14 S1 C17 -144.63(15) . . . . ? C15 C14 S1 C17 94.08(17) . . . . ? C13 C14 S1 Pd1 -31.87(15) . . . . ? C15 C14 S1 Pd1 -153.16(14) . . . . ? P1 Pd1 S1 C17 116.84(9) . . . . ? Cl2 Pd1 S1 C17 179(17) . . . . ? Cl1 Pd1 S1 C17 -56.12(9) . . . . ? P1 Pd1 S1 C14 6.25(7) . . . . ? Cl2 Pd1 S1 C14 68.7(2) . . . . ? Cl1 Pd1 S1 C14 -166.71(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.851 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.150 #==END data_[Pd(4)Cl2] _database_code_depnum_ccdc_archive 'CCDC 602965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pd(4)Cl2) _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 Cl2 P Pd S' _chemical_formula_sum 'C25 H29 Cl2 P Pd S' _chemical_formula_weight 569.81 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' Pd Pd -0.9988 1.0072 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.029(2) _cell_length_b 12.600(2) _cell_length_c 14.870(3) _cell_angle_alpha 90.000 _cell_angle_beta 109.835(1) _cell_angle_gamma 90.000 _cell_volume 2472.56(72) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26893 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6939 _exptl_absorpt_correction_T_max 0.7660 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40943 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.40 _reflns_number_total 5613 _reflns_number_gt 4634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0320P)^2^+4.2020P] 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 5613 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3009(2) 0.4048(2) 0.4087(2) 0.0226(6) Uani 1 1 d . . . H1A H 0.2305 0.3971 0.3642 0.027 Uiso 1 1 calc R . . H1B H 0.3278 0.4730 0.3947 0.027 Uiso 1 1 calc R . . C2 C 0.3649(2) 0.3143(2) 0.3928(2) 0.0229(6) Uani 1 1 d . . . H2 H 0.3314 0.2453 0.3972 0.027 Uiso 1 1 calc R . . C3 C 0.3763(3) 0.3227(3) 0.2942(2) 0.0296(7) Uani 1 1 d . . . H3A H 0.3078 0.3259 0.2453 0.036 Uiso 1 1 calc R . . H3B H 0.4108 0.3905 0.2912 0.036 Uiso 1 1 calc R . . C4 C 0.4347(3) 0.2332(3) 0.2675(3) 0.0414(9) Uani 1 1 d . . . H4A H 0.5054 0.2343 0.3104 0.062 Uiso 1 1 calc R . . H4B H 0.4325 0.2427 0.2014 0.062 Uiso 1 1 calc R . . H4C H 0.4039 0.1649 0.2735 0.062 Uiso 1 1 calc R . . C5 C 0.5243(2) 0.1799(3) 0.5149(2) 0.0275(7) Uani 1 1 d . . . H5A H 0.5315 0.1476 0.4568 0.033 Uiso 1 1 calc R . . H5B H 0.5913 0.1761 0.5662 0.033 Uiso 1 1 calc R . . C6 C 0.4499(2) 0.1155(2) 0.5444(2) 0.0232(6) Uani 1 1 d . . . C7 C 0.3706(2) 0.0626(2) 0.4771(2) 0.0244(7) Uani 1 1 d . . . H7 H 0.3652 0.0646 0.4117 0.029 Uiso 1 1 calc R . . C8 C 0.2988(2) 0.0064(2) 0.5039(2) 0.0249(7) Uani 1 1 d . . . C9 C 0.3093(2) 0.0034(2) 0.6002(2) 0.0254(7) Uani 1 1 d . . . H9 H 0.2605 -0.0339 0.6192 0.031 Uiso 1 1 calc R . . C10 C 0.3892(2) 0.0534(3) 0.6694(2) 0.0269(7) Uani 1 1 d . . . C11 C 0.4589(2) 0.1102(2) 0.6409(2) 0.0250(7) Uani 1 1 d . . . H11 H 0.5132 0.1458 0.6874 0.030 Uiso 1 1 calc R . . C12 C 0.2121(3) -0.0485(3) 0.4296(2) 0.0347(8) Uani 1 1 d . . . H12A H 0.2332 -0.1199 0.4180 0.052 Uiso 1 1 calc R . . H12B H 0.1922 -0.0077 0.3700 0.052 Uiso 1 1 calc R . . H12C H 0.1544 -0.0538 0.4524 0.052 Uiso 1 1 calc R . . C13 C 0.3990(3) 0.0476(3) 0.7734(3) 0.0427(9) Uani 1 1 d . . . H13A H 0.4322 -0.0191 0.8008 0.064 Uiso 1 1 calc R . . H13B H 0.3315 0.0505 0.7792 0.064 Uiso 1 1 calc R . . H13C H 0.4396 0.1075 0.8079 0.064 Uiso 1 1 calc R . . C14 C 0.2173(2) 0.3019(2) 0.5436(2) 0.0212(6) Uani 1 1 d . . . C15 C 0.2154(2) 0.2775(3) 0.6347(2) 0.0266(7) Uani 1 1 d . . . H15 H 0.2582 0.3148 0.6889 0.032 Uiso 1 1 calc R . . C16 C 0.1512(2) 0.1990(3) 0.6460(2) 0.0301(7) Uani 1 1 d . . . H16 H 0.1501 0.1828 0.7080 0.036 Uiso 1 1 calc R . . C17 C 0.0891(2) 0.1443(3) 0.5680(3) 0.0306(8) Uani 1 1 d . . . H17 H 0.0452 0.0906 0.5763 0.037 Uiso 1 1 calc R . . C18 C 0.0905(2) 0.1676(3) 0.4777(2) 0.0284(7) Uani 1 1 d . . . H18 H 0.0473 0.1298 0.4240 0.034 Uiso 1 1 calc R . . C19 C 0.1545(2) 0.2456(2) 0.4648(2) 0.0244(7) Uani 1 1 d . . . H19 H 0.1555 0.2608 0.4026 0.029 Uiso 1 1 calc R . . C20 C 0.2396(2) 0.5304(2) 0.5401(2) 0.0211(6) Uani 1 1 d . . . C21 C 0.2974(2) 0.6180(2) 0.5845(2) 0.0267(7) Uani 1 1 d . . . H21 H 0.3687 0.6115 0.6140 0.032 Uiso 1 1 calc R . . C22 C 0.2503(2) 0.7142(3) 0.5856(3) 0.0310(7) Uani 1 1 d . . . H22 H 0.2895 0.7740 0.6157 0.037 Uiso 1 1 calc R . . C23 C 0.1464(3) 0.7239(3) 0.5429(2) 0.0312(8) Uani 1 1 d . . . H23 H 0.1143 0.7899 0.5448 0.037 Uiso 1 1 calc R . . C24 C 0.0889(2) 0.6376(3) 0.4973(2) 0.0288(7) Uani 1 1 d . . . H24 H 0.0178 0.6448 0.4669 0.035 Uiso 1 1 calc R . . C25 C 0.1355(2) 0.5407(3) 0.4963(2) 0.0254(7) Uani 1 1 d . . . H25 H 0.0962 0.4813 0.4656 0.031 Uiso 1 1 calc R . . Pd1 Pd 0.460910(16) 0.381382(18) 0.623645(16) 0.01937(8) Uani 1 1 d . . . P1 P 0.30097(6) 0.40629(6) 0.53163(5) 0.01902(16) Uani 1 1 d . . . S1 S 0.48883(6) 0.32086(6) 0.49004(5) 0.02204(16) Uani 1 1 d . . . Cl1 Cl 0.42733(6) 0.44857(6) 0.75583(5) 0.02589(17) Uani 1 1 d . . . Cl2 Cl 0.63598(5) 0.34622(6) 0.71136(5) 0.02587(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0234(15) 0.0245(16) 0.0202(15) 0.0041(12) 0.0078(12) 0.0015(13) C2 0.0235(15) 0.0238(16) 0.0224(15) 0.0014(12) 0.0094(12) -0.0007(13) C3 0.0349(18) 0.0338(19) 0.0235(16) 0.0003(14) 0.0142(14) -0.0025(15) C4 0.050(2) 0.049(2) 0.0320(19) -0.0071(17) 0.0235(17) 0.0007(19) C5 0.0282(17) 0.0234(17) 0.0353(18) 0.0014(13) 0.0165(14) 0.0084(13) C6 0.0259(15) 0.0174(14) 0.0269(16) 0.0000(12) 0.0097(13) 0.0070(13) C7 0.0325(17) 0.0188(15) 0.0223(15) 0.0007(12) 0.0100(13) 0.0082(13) C8 0.0287(16) 0.0151(15) 0.0268(16) 0.0022(12) 0.0040(13) 0.0051(13) C9 0.0261(16) 0.0180(15) 0.0344(17) 0.0059(13) 0.0131(13) 0.0047(13) C10 0.0342(17) 0.0248(17) 0.0229(16) 0.0034(13) 0.0110(13) 0.0088(14) C11 0.0269(16) 0.0202(16) 0.0253(16) 0.0002(12) 0.0057(13) 0.0039(13) C12 0.041(2) 0.0206(17) 0.0354(19) 0.0004(14) 0.0040(15) -0.0007(15) C13 0.053(2) 0.047(2) 0.0292(19) 0.0031(17) 0.0149(17) -0.0006(19) C14 0.0200(15) 0.0191(15) 0.0249(15) 0.0024(12) 0.0083(12) 0.0057(12) C15 0.0262(16) 0.0279(17) 0.0254(16) 0.0021(13) 0.0083(13) 0.0012(14) C16 0.0278(17) 0.0344(19) 0.0312(17) 0.0124(15) 0.0141(14) 0.0055(15) C17 0.0202(16) 0.0239(17) 0.047(2) 0.0071(15) 0.0111(14) -0.0003(13) C18 0.0202(15) 0.0220(16) 0.0404(19) -0.0063(14) 0.0068(14) 0.0020(13) C19 0.0224(15) 0.0256(16) 0.0245(16) -0.0002(13) 0.0069(12) 0.0043(13) C20 0.0226(15) 0.0202(15) 0.0231(15) 0.0041(12) 0.0112(12) 0.0011(12) C21 0.0209(15) 0.0237(16) 0.0369(18) 0.0037(14) 0.0115(13) 0.0033(13) C22 0.0273(17) 0.0185(16) 0.048(2) 0.0035(14) 0.0141(15) 0.0003(13) C23 0.0345(18) 0.0197(16) 0.043(2) 0.0102(14) 0.0182(15) 0.0109(14) C24 0.0218(16) 0.0320(18) 0.0322(17) 0.0082(14) 0.0089(13) 0.0059(14) C25 0.0226(15) 0.0257(17) 0.0266(16) 0.0022(13) 0.0065(12) 0.0021(13) Pd1 0.01824(12) 0.01768(12) 0.02118(12) 0.00010(9) 0.00538(9) 0.00185(9) P1 0.0188(4) 0.0190(4) 0.0197(4) 0.0020(3) 0.0072(3) 0.0032(3) S1 0.0212(4) 0.0216(4) 0.0258(4) 0.0012(3) 0.0111(3) 0.0008(3) Cl1 0.0288(4) 0.0283(4) 0.0179(3) -0.0050(3) 0.0043(3) 0.0066(3) Cl2 0.0175(3) 0.0259(4) 0.0291(4) 0.0001(3) 0.0012(3) 0.0007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.519(4) . ? C1 P1 1.827(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.532(4) . ? C2 S1 1.847(3) . ? C2 H2 1.0000 . ? C3 C4 1.524(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.501(4) . ? C5 S1 1.848(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.388(4) . ? C6 C11 1.398(4) . ? C7 C8 1.395(5) . ? C7 H7 0.9500 . ? C8 C9 1.390(4) . ? C8 C12 1.506(4) . ? C9 C10 1.389(4) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 C13 1.508(5) . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.397(4) . ? C14 C15 1.397(4) . ? C14 P1 1.812(3) . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.376(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.389(4) . ? C20 C21 1.395(4) . ? C20 P1 1.811(3) . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.384(5) . ? C22 H22 0.9500 . ? C23 C24 1.385(5) . ? C23 H23 0.9500 . ? C24 C25 1.388(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? Pd1 P1 2.2185(8) . ? Pd1 S1 2.2825(8) . ? Pd1 Cl1 2.3304(7) . ? Pd1 Cl2 2.3991(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 P1 111.4(2) . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 C3 110.9(3) . . ? C1 C2 S1 107.1(2) . . ? C3 C2 S1 111.7(2) . . ? C1 C2 H2 109.0 . . ? C3 C2 H2 109.0 . . ? S1 C2 H2 109.0 . . ? C4 C3 C2 116.0(3) . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? C2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 S1 114.3(2) . . ? C6 C5 H5A 108.7 . . ? S1 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? S1 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C11 119.2(3) . . ? C7 C6 C5 121.0(3) . . ? C11 C6 C5 119.8(3) . . ? C6 C7 C8 121.2(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 118.2(3) . . ? C9 C8 C12 121.4(3) . . ? C7 C8 C12 120.4(3) . . ? C10 C9 C8 121.9(3) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 118.8(3) . . ? C9 C10 C13 120.5(3) . . ? C11 C10 C13 120.7(3) . . ? C10 C11 C6 120.6(3) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.2(3) . . ? C19 C14 P1 122.1(2) . . ? C15 C14 P1 118.7(2) . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 119.8(3) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? C25 C20 C21 119.9(3) . . ? C25 C20 P1 119.8(2) . . ? C21 C20 P1 120.2(2) . . ? C22 C21 C20 119.7(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C20 120.1(3) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? P1 Pd1 S1 86.95(3) . . ? P1 Pd1 Cl1 90.99(3) . . ? S1 Pd1 Cl1 177.47(3) . . ? P1 Pd1 Cl2 174.88(3) . . ? S1 Pd1 Cl2 88.00(3) . . ? Cl1 Pd1 Cl2 94.08(3) . . ? C20 P1 C14 106.32(13) . . ? C20 P1 C1 103.90(14) . . ? C14 P1 C1 108.09(14) . . ? C20 P1 Pd1 118.98(10) . . ? C14 P1 Pd1 112.96(10) . . ? C1 P1 Pd1 105.81(10) . . ? C2 S1 C5 103.38(15) . . ? C2 S1 Pd1 107.60(10) . . ? C5 S1 Pd1 105.16(11) . . ? 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 P1 C1 C2 C3 -172.2(2) . . . . ? P1 C1 C2 S1 -50.1(2) . . . . ? C1 C2 C3 C4 -177.1(3) . . . . ? S1 C2 C3 C4 63.6(3) . . . . ? S1 C5 C6 C7 90.8(3) . . . . ? S1 C5 C6 C11 -87.9(3) . . . . ? C11 C6 C7 C8 1.5(4) . . . . ? C5 C6 C7 C8 -177.2(3) . . . . ? C6 C7 C8 C9 -0.9(4) . . . . ? C6 C7 C8 C12 178.7(3) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C12 C8 C9 C10 179.7(3) . . . . ? C8 C9 C10 C11 1.6(5) . . . . ? C8 C9 C10 C13 -179.3(3) . . . . ? C9 C10 C11 C6 -1.0(5) . . . . ? C13 C10 C11 C6 179.9(3) . . . . ? C7 C6 C11 C10 -0.5(4) . . . . ? C5 C6 C11 C10 178.2(3) . . . . ? C19 C14 C15 C16 -0.5(5) . . . . ? P1 C14 C15 C16 179.1(2) . . . . ? C14 C15 C16 C17 0.2(5) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 C19 0.2(5) . . . . ? C17 C18 C19 C14 -0.6(5) . . . . ? C15 C14 C19 C18 0.8(4) . . . . ? P1 C14 C19 C18 -178.9(2) . . . . ? C25 C20 C21 C22 0.7(5) . . . . ? P1 C20 C21 C22 176.1(3) . . . . ? C20 C21 C22 C23 0.1(5) . . . . ? C21 C22 C23 C24 -1.2(5) . . . . ? C22 C23 C24 C25 1.4(5) . . . . ? C23 C24 C25 C20 -0.5(5) . . . . ? C21 C20 C25 C24 -0.5(5) . . . . ? P1 C20 C25 C24 -175.9(2) . . . . ? C25 C20 P1 C14 -39.9(3) . . . . ? C21 C20 P1 C14 144.8(3) . . . . ? C25 C20 P1 C1 74.1(3) . . . . ? C21 C20 P1 C1 -101.3(3) . . . . ? C25 C20 P1 Pd1 -168.7(2) . . . . ? C21 C20 P1 Pd1 16.0(3) . . . . ? C19 C14 P1 C20 101.9(3) . . . . ? C15 C14 P1 C20 -77.7(3) . . . . ? C19 C14 P1 C1 -9.1(3) . . . . ? C15 C14 P1 C1 171.2(2) . . . . ? C19 C14 P1 Pd1 -125.8(2) . . . . ? C15 C14 P1 Pd1 54.5(3) . . . . ? C2 C1 P1 C20 170.8(2) . . . . ? C2 C1 P1 C14 -76.6(2) . . . . ? C2 C1 P1 Pd1 44.7(2) . . . . ? S1 Pd1 P1 C20 -133.50(11) . . . . ? Cl1 Pd1 P1 C20 45.03(11) . . . . ? Cl2 Pd1 P1 C20 -143.0(3) . . . . ? S1 Pd1 P1 C14 100.80(11) . . . . ? Cl1 Pd1 P1 C14 -80.67(11) . . . . ? Cl2 Pd1 P1 C14 91.3(3) . . . . ? S1 Pd1 P1 C1 -17.26(11) . . . . ? Cl1 Pd1 P1 C1 161.27(11) . . . . ? Cl2 Pd1 P1 C1 -26.8(4) . . . . ? C1 C2 S1 C5 144.4(2) . . . . ? C3 C2 S1 C5 -94.0(2) . . . . ? C1 C2 S1 Pd1 33.4(2) . . . . ? C3 C2 S1 Pd1 155.0(2) . . . . ? C6 C5 S1 C2 -59.3(3) . . . . ? C6 C5 S1 Pd1 53.5(2) . . . . ? P1 Pd1 S1 C2 -6.16(11) . . . . ? Cl1 Pd1 S1 C2 -41.6(7) . . . . ? Cl2 Pd1 S1 C2 173.00(11) . . . . ? P1 Pd1 S1 C5 -115.89(11) . . . . ? Cl1 Pd1 S1 C5 -151.3(7) . . . . ? Cl2 Pd1 S1 C5 63.27(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.724 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.121 #===END data_[Pd(5)Cl2] _database_code_depnum_ccdc_archive 'CCDC 602966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. A. Dervisi ; _chemical_name_common 'Dr. A. Dervisi' _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Cl2 P Pd S' _chemical_formula_sum 'C27 H27 Cl2 P Pd S' _chemical_formula_weight 591.82 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9134(3) _cell_length_b 11.6302(5) _cell_length_c 11.7817(4) _cell_angle_alpha 102.154(2) _cell_angle_beta 99.477(2) _cell_angle_gamma 103.735(2) _cell_volume 1256.57(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5554 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Slab _exptl_crystal_colour 'Light Orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8250 _exptl_absorpt_correction_T_max 0.9465 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24762 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0346 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5748 _reflns_number_gt 4902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0252P)^2^+1.1836P] 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 SHELXL _refine_ls_extinction_coef 0.0047(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5748 _refine_ls_number_parameters 420 _refine_ls_number_restraints 625 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0381(3) 0.2486(3) 0.5889(2) 0.0450(7) Uani 1 1 d U B . H1A H 1.0969 0.3340 0.6274 0.054 Uiso 1 1 calc R . . H1B H 1.1023 0.1987 0.5660 0.054 Uiso 1 1 calc R . . C2 C 0.9306(3) 0.2452(3) 0.4777(3) 0.0609(9) Uani 1 1 d U . . H2 H 0.8615 0.2868 0.5083 0.073 Uiso 1 1 calc R A 1 C3 C 0.9946(9) 0.3187(9) 0.3999(8) 0.050(2) Uani 0.515(9) 1 d PU B 1 H3A H 1.0496 0.4025 0.4478 0.060 Uiso 0.515(9) 1 calc PR B 1 H3B H 0.9188 0.3250 0.3373 0.060 Uiso 0.515(9) 1 calc PR B 1 C4 C 1.0916(8) 0.2530(7) 0.3443(5) 0.054(2) Uani 0.515(9) 1 d PU B 1 H4A H 1.1725 0.2563 0.4064 0.081 Uiso 0.515(9) 1 calc PR B 1 H4B H 1.1266 0.2927 0.2851 0.081 Uiso 0.515(9) 1 calc PR B 1 H4C H 1.0385 0.1672 0.3054 0.081 Uiso 0.515(9) 1 calc PR B 1 C5 C 0.8662(3) 0.3075(3) 0.7536(2) 0.0423(6) Uani 1 1 d U B . C6 C 0.7210(3) 0.2895(3) 0.7277(3) 0.0665(10) Uani 1 1 d U . . H6 H 0.6595 0.2120 0.6819 0.080 Uiso 1 1 calc R . . C7 C 0.6642(4) 0.3843(3) 0.7683(4) 0.0857(14) Uani 1 1 d U . . H7 H 0.5639 0.3715 0.7495 0.103 Uiso 1 1 calc R . . C8 C 0.7516(4) 0.4959(3) 0.8351(3) 0.0711(11) Uani 1 1 d U . . H8 H 0.7122 0.5606 0.8626 0.085 Uiso 1 1 calc R . . C9 C 0.8964(4) 0.5143(3) 0.8623(3) 0.0679(10) Uani 1 1 d U . . H9 H 0.9573 0.5917 0.9090 0.081 Uiso 1 1 calc R . . C10 C 0.9532(3) 0.4208(3) 0.8220(3) 0.0569(8) Uani 1 1 d U . . H10 H 1.0536 0.4341 0.8413 0.068 Uiso 1 1 calc R . . C11 C 1.0764(3) 0.1851(2) 0.8162(2) 0.0353(5) Uani 1 1 d U B . C12 C 1.0368(3) 0.1640(3) 0.9192(2) 0.0420(6) Uani 1 1 d U . . H12 H 0.9394 0.1483 0.9232 0.050 Uiso 1 1 calc R . . C13 C 1.1379(3) 0.1655(3) 1.0162(2) 0.0443(7) Uani 1 1 d U . . H13 H 1.1095 0.1495 1.0858 0.053 Uiso 1 1 calc R . . C14 C 1.2790(3) 0.1902(3) 1.0118(2) 0.0479(7) Uani 1 1 d U . . H14 H 1.3486 0.1922 1.0786 0.057 Uiso 1 1 calc R . . C15 C 1.3192(3) 0.2120(3) 0.9103(3) 0.0578(8) Uani 1 1 d U . . H15 H 1.4171 0.2298 0.9076 0.069 Uiso 1 1 calc R . . C16 C 1.2185(3) 0.2083(3) 0.8118(3) 0.0479(7) Uani 1 1 d U . . H16 H 1.2471 0.2217 0.7415 0.058 Uiso 1 1 calc R . . C17 C 0.6462(5) 0.0799(5) 0.3423(4) 0.0409(11) Uani 0.658(5) 1 d PDU B 1 H17A H 0.5836 -0.0042 0.3038 0.049 Uiso 0.658(5) 1 calc PR B 1 H17B H 0.6025 0.1185 0.4042 0.049 Uiso 0.658(5) 1 calc PR B 1 C18 C 0.6551(4) 0.1521(4) 0.2504(3) 0.0340(10) Uani 0.658(5) 1 d PDU B 1 C19 C 0.6756(15) 0.0966(8) 0.1442(8) 0.0466(17) Uani 0.658(5) 1 d PDU B 1 H19 H 0.6783 0.0138 0.1275 0.056 Uiso 0.658(5) 1 calc PR B 1 C20 C 0.6938(19) 0.1672(9) 0.0554(9) 0.064(2) Uani 0.658(5) 1 d PDU B 1 H20 H 0.7107 0.1308 -0.0190 0.077 Uiso 0.658(5) 1 calc PR B 1 C21 C 0.6865(6) 0.2825(7) 0.0797(6) 0.0701(18) Uani 0.658(5) 1 d PDU B 1 H21 H 0.6978 0.3276 0.0217 0.084 Uiso 0.658(5) 1 calc PR B 1 C22 C 0.664(3) 0.3353(15) 0.1830(17) 0.063(2) Uani 0.658(5) 1 d PDU B 1 C23 C 0.6560(15) 0.4617(10) 0.2075(11) 0.098(3) Uani 0.658(5) 1 d PDU B 1 H23 H 0.6643 0.5062 0.1487 0.117 Uiso 0.658(5) 1 calc PR B 1 C24 C 0.6369(9) 0.5142(9) 0.3146(12) 0.114(3) Uani 0.658(5) 1 d PDU B 1 H24 H 0.6353 0.5974 0.3302 0.137 Uiso 0.658(5) 1 calc PR B 1 C25 C 0.6190(11) 0.4528(8) 0.4057(10) 0.099(3) Uani 0.658(5) 1 d PDU B 1 H25 H 0.6102 0.4937 0.4817 0.119 Uiso 0.658(5) 1 calc PR B 1 C26 C 0.6154(18) 0.3354(11) 0.3788(9) 0.077(3) Uani 0.658(5) 1 d PDU B 1 H26 H 0.5903 0.2898 0.4340 0.092 Uiso 0.658(5) 1 calc PR B 1 C27 C 0.6463(6) 0.2732(5) 0.2740(5) 0.0435(12) Uani 0.658(5) 1 d PDU B 1 P1 P 0.94238(7) 0.18812(6) 0.69281(6) 0.03411(15) Uani 1 1 d U . . S1 S 0.8238(2) 0.0713(2) 0.41445(19) 0.0348(4) Uani 0.658(5) 1 d PDU B 1 Cl1 Cl 0.61931(7) -0.16308(7) 0.44996(6) 0.04799(18) Uani 1 1 d U . . Cl2 Cl 0.72675(8) -0.03868(7) 0.74835(6) 0.04806(18) Uani 1 1 d U . . Pd1 Pd 0.780097(19) 0.017890(18) 0.581792(16) 0.03299(8) Uani 1 1 d U B . C33 C 1.0138(10) 0.2661(9) 0.3720(8) 0.049(2) Uani 0.485(9) 1 d PU B 2 H33A H 1.0926 0.2273 0.3745 0.059 Uiso 0.485(9) 1 calc PR B 2 H33B H 0.9477 0.2319 0.2927 0.059 Uiso 0.485(9) 1 calc PR B 2 C34 C 1.0709(12) 0.4052(9) 0.3992(8) 0.108(4) Uani 0.485(9) 1 d PU B 2 H34A H 0.9923 0.4398 0.3775 0.162 Uiso 0.485(9) 1 calc PR B 2 H34B H 1.1426 0.4261 0.3531 0.162 Uiso 0.485(9) 1 calc PR B 2 H34C H 1.1144 0.4390 0.4845 0.162 Uiso 0.485(9) 1 calc PR B 2 C37 C 0.6346(8) 0.1414(10) 0.3883(9) 0.044(2) Uani 0.342(5) 1 d PDU B 2 H37A H 0.5689 0.0665 0.3308 0.053 Uiso 0.342(5) 1 calc PR B 2 H37B H 0.5961 0.1553 0.4608 0.053 Uiso 0.342(5) 1 calc PR B 2 C38 C 0.6360(9) 0.2492(8) 0.3342(8) 0.042(2) Uani 0.342(5) 1 d PDU B 2 C39 C 0.625(3) 0.3530(16) 0.4029(12) 0.045(3) Uani 0.342(5) 1 d PDU B 2 H39 H 0.6222 0.3601 0.4843 0.054 Uiso 0.342(5) 1 calc PR B 2 C40 C 0.6154(19) 0.4579(15) 0.3484(11) 0.056(3) Uani 0.342(5) 1 d PDU B 2 H40 H 0.5941 0.5274 0.3918 0.067 Uiso 0.342(5) 1 calc PR B 2 C41 C 0.637(2) 0.4528(13) 0.2399(11) 0.044(3) Uani 0.342(5) 1 d PDU B 2 H41 H 0.6374 0.5205 0.2068 0.053 Uiso 0.342(5) 1 calc PR B 2 C42 C 0.659(5) 0.351(2) 0.177(2) 0.039(3) Uani 0.342(5) 1 d PDU B 2 C43 C 0.6801(9) 0.3417(10) 0.0541(8) 0.052(2) Uani 0.342(5) 1 d PDU B 2 H43 H 0.6822 0.4095 0.0206 0.063 Uiso 0.342(5) 1 calc PR B 2 C44 C 0.6966(9) 0.2376(10) -0.0101(9) 0.058(2) Uani 0.342(5) 1 d PDU B 2 H44 H 0.7147 0.2352 -0.0872 0.070 Uiso 0.342(5) 1 calc PR B 2 C45 C 0.688(4) 0.1297(15) 0.0334(15) 0.050(3) Uani 0.342(5) 1 d PDU B 2 H45 H 0.6924 0.0557 -0.0164 0.060 Uiso 0.342(5) 1 calc PR B 2 C46 C 0.673(3) 0.1355(13) 0.1442(14) 0.040(3) Uani 0.342(5) 1 d PDU B 2 H46 H 0.6731 0.0662 0.1749 0.048 Uiso 0.342(5) 1 calc PR B 2 C47 C 0.6563(11) 0.2435(9) 0.2189(8) 0.039(2) Uani 0.342(5) 1 d PDU B 2 S37 S 0.8113(4) 0.1142(4) 0.4287(4) 0.0309(7) Uani 0.342(5) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0319(13) 0.0567(18) 0.0463(15) 0.0282(14) 0.0012(11) 0.0048(12) C2 0.0344(15) 0.090(2) 0.0613(19) 0.0529(19) -0.0009(13) 0.0028(15) C3 0.031(4) 0.077(6) 0.057(5) 0.042(5) 0.009(3) 0.024(4) C4 0.043(4) 0.086(5) 0.043(3) 0.032(3) 0.010(3) 0.025(3) C5 0.0381(14) 0.0393(15) 0.0462(15) 0.0135(12) -0.0048(12) 0.0125(12) C6 0.0429(17) 0.0426(18) 0.095(3) -0.0057(17) -0.0150(17) 0.0180(14) C7 0.048(2) 0.055(2) 0.130(4) -0.011(2) -0.017(2) 0.0277(17) C8 0.065(2) 0.049(2) 0.086(3) -0.0022(18) -0.0106(19) 0.0286(17) C9 0.062(2) 0.0413(18) 0.080(2) -0.0045(17) -0.0128(18) 0.0143(15) C10 0.0421(16) 0.0481(18) 0.066(2) 0.0029(15) -0.0065(14) 0.0091(13) C11 0.0353(13) 0.0353(14) 0.0323(12) 0.0106(11) -0.0016(10) 0.0088(11) C12 0.0368(14) 0.0488(17) 0.0368(14) 0.0148(12) 0.0009(11) 0.0074(12) C13 0.0503(16) 0.0458(17) 0.0318(13) 0.0149(12) -0.0029(12) 0.0083(13) C14 0.0456(16) 0.0516(18) 0.0390(15) 0.0131(13) -0.0105(12) 0.0123(13) C15 0.0354(15) 0.086(3) 0.0519(18) 0.0279(17) -0.0025(13) 0.0176(16) C16 0.0371(15) 0.069(2) 0.0401(15) 0.0206(14) 0.0020(12) 0.0174(14) C17 0.037(2) 0.048(3) 0.036(2) 0.016(2) -0.0012(18) 0.011(2) C18 0.0283(19) 0.042(2) 0.0309(19) 0.0123(16) 0.0004(15) 0.0091(16) C19 0.049(3) 0.054(4) 0.038(3) 0.009(3) 0.006(2) 0.021(4) C20 0.042(4) 0.106(7) 0.032(4) 0.020(5) 0.001(4) 0.003(7) C21 0.036(3) 0.101(5) 0.072(4) 0.064(4) -0.010(3) -0.004(3) C22 0.028(4) 0.063(5) 0.098(5) 0.048(4) -0.006(4) 0.006(4) C23 0.040(4) 0.071(5) 0.175(9) 0.059(5) -0.004(7) -0.002(3) C24 0.049(4) 0.068(5) 0.222(10) 0.037(5) 0.017(6) 0.019(4) C25 0.065(4) 0.059(4) 0.156(8) -0.009(5) 0.032(7) 0.013(4) C26 0.060(6) 0.057(4) 0.098(6) -0.010(4) 0.026(6) 0.010(4) C27 0.028(2) 0.044(3) 0.055(4) 0.010(3) 0.004(3) 0.0091(19) P1 0.0297(3) 0.0385(4) 0.0332(3) 0.0143(3) -0.0008(3) 0.0087(3) S1 0.0345(7) 0.0421(11) 0.0275(7) 0.0117(8) 0.0026(5) 0.0113(7) Cl1 0.0346(3) 0.0590(5) 0.0368(3) 0.0016(3) 0.0021(3) 0.0015(3) Cl2 0.0485(4) 0.0559(4) 0.0309(3) 0.0190(3) -0.0001(3) -0.0023(3) Pd1 0.02973(12) 0.04186(14) 0.02619(11) 0.01170(8) 0.00139(7) 0.00873(8) C33 0.034(5) 0.074(6) 0.049(5) 0.041(5) 0.006(3) 0.013(4) C34 0.132(9) 0.081(6) 0.079(6) 0.049(5) -0.003(6) -0.037(6) C37 0.025(4) 0.060(6) 0.050(5) 0.030(5) 0.002(4) 0.010(4) C38 0.029(4) 0.056(5) 0.044(5) 0.021(4) 0.009(4) 0.012(4) C39 0.040(6) 0.058(7) 0.032(4) 0.016(5) 0.002(4) 0.006(7) C40 0.047(6) 0.069(7) 0.065(6) 0.028(6) 0.024(6) 0.024(6) C41 0.048(8) 0.055(6) 0.038(5) 0.020(4) 0.012(4) 0.024(6) C42 0.023(7) 0.041(6) 0.056(6) 0.026(4) 0.001(5) 0.006(6) C43 0.020(4) 0.084(6) 0.050(5) 0.024(4) 0.005(4) 0.008(4) C44 0.038(5) 0.093(7) 0.048(5) 0.030(4) 0.010(4) 0.016(5) C45 0.042(7) 0.067(7) 0.028(6) 0.006(5) -0.006(6) 0.004(8) C46 0.031(5) 0.048(7) 0.041(5) 0.021(5) -0.005(4) 0.013(7) C47 0.027(4) 0.059(5) 0.037(5) 0.021(4) 0.008(4) 0.015(4) S37 0.0277(12) 0.043(2) 0.0251(12) 0.0134(14) 0.0046(8) 0.0124(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.534(4) . ? C1 P1 1.823(3) . ? C2 C3 1.495(9) . ? C2 C33 1.631(10) . ? C2 S37 1.613(6) . ? C2 S1 1.963(4) . ? C3 C4 1.512(10) . ? C5 C6 1.377(4) . ? C5 C10 1.383(4) . ? C5 P1 1.808(3) . ? C6 C7 1.386(5) . ? C7 C8 1.366(5) . ? C8 C9 1.372(5) . ? C9 C10 1.374(5) . ? C11 C16 1.382(4) . ? C11 C12 1.387(4) . ? C11 P1 1.813(2) . ? C12 C13 1.385(4) . ? C13 C14 1.371(4) . ? C14 C15 1.375(4) . ? C15 C16 1.386(4) . ? C17 C18 1.506(5) . ? C17 S1 1.859(5) . ? C18 C19 1.353(8) . ? C18 C27 1.403(6) . ? C19 C20 1.467(12) . ? C20 C21 1.333(11) . ? C21 C22 1.323(19) . ? C22 C27 1.425(10) . ? C22 C23 1.461(17) . ? C23 C24 1.345(12) . ? C24 C25 1.421(13) . ? C25 C26 1.326(13) . ? C26 C27 1.412(10) . ? P1 Pd1 2.2187(7) . ? S1 Pd1 2.265(2) . ? Cl1 Pd1 2.3660(7) . ? Cl2 Pd1 2.2986(7) . ? Pd1 S37 2.339(4) . ? C33 C34 1.525(13) . ? C37 C38 1.520(11) . ? C37 S37 1.857(8) . ? C38 C39 1.345(15) . ? C38 C47 1.396(10) . ? C39 C40 1.507(17) . ? C40 C41 1.322(13) . ? C41 C42 1.34(2) . ? C42 C47 1.433(13) . ? C42 C43 1.48(2) . ? C43 C44 1.347(13) . ? C44 C45 1.442(17) . ? C45 C46 1.327(19) . ? C46 C47 1.435(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 P1 109.33(19) . . ? C3 C2 C1 113.6(4) . . ? C1 C2 C33 109.3(4) . . ? C3 C2 S37 124.4(5) . . ? C1 C2 S37 111.3(3) . . ? C33 C2 S37 107.6(4) . . ? C3 C2 S1 121.6(5) . . ? C1 C2 S1 104.2(2) . . ? C33 C2 S1 100.6(4) . . ? C2 C3 C4 107.0(6) . . ? C6 C5 C10 118.8(3) . . ? C6 C5 P1 120.6(2) . . ? C10 C5 P1 120.6(2) . . ? C5 C6 C7 120.2(3) . . ? C8 C7 C6 120.4(3) . . ? C7 C8 C9 119.8(3) . . ? C8 C9 C10 120.0(3) . . ? C9 C10 C5 120.8(3) . . ? C16 C11 C12 119.1(2) . . ? C16 C11 P1 121.4(2) . . ? C12 C11 P1 119.5(2) . . ? C13 C12 C11 120.6(3) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 119.8(3) . . ? C14 C15 C16 120.7(3) . . ? C11 C16 C15 119.9(3) . . ? C18 C17 S1 112.5(3) . . ? C19 C18 C27 120.9(5) . . ? C19 C18 C17 117.2(5) . . ? C27 C18 C17 121.8(4) . . ? C18 C19 C20 118.6(6) . . ? C21 C20 C19 119.7(8) . . ? C22 C21 C20 121.2(7) . . ? C21 C22 C27 122.3(11) . . ? C21 C22 C23 120.3(9) . . ? C27 C22 C23 117.4(14) . . ? C24 C23 C22 119.0(11) . . ? C23 C24 C25 123.9(9) . . ? C26 C25 C24 116.4(10) . . ? C25 C26 C27 124.7(11) . . ? C18 C27 C22 117.1(9) . . ? C18 C27 C26 124.8(7) . . ? C22 C27 C26 118.0(10) . . ? C5 P1 C11 105.03(12) . . ? C5 P1 C1 104.33(14) . . ? C11 P1 C1 106.55(12) . . ? C5 P1 Pd1 113.32(9) . . ? C11 P1 Pd1 121.32(9) . . ? C1 P1 Pd1 104.91(10) . . ? C17 S1 C2 102.1(2) . . ? C17 S1 Pd1 101.85(17) . . ? C2 S1 Pd1 101.87(13) . . ? P1 Pd1 S1 90.14(6) . . ? P1 Pd1 Cl2 91.45(2) . . ? S1 Pd1 Cl2 177.85(6) . . ? P1 Pd1 S37 82.95(11) . . ? S1 Pd1 S37 13.37(8) . . ? Cl2 Pd1 S37 166.13(11) . . ? P1 Pd1 Cl1 174.78(3) . . ? S1 Pd1 Cl1 85.31(6) . . ? Cl2 Pd1 Cl1 93.16(3) . . ? S37 Pd1 Cl1 93.08(11) . . ? C34 C33 C2 103.8(8) . . ? C38 C37 S37 114.8(6) . . ? C39 C38 C47 120.7(9) . . ? C39 C38 C37 118.1(10) . . ? C47 C38 C37 121.2(8) . . ? C38 C39 C40 118.8(11) . . ? C41 C40 C39 119.7(13) . . ? C42 C41 C40 119.5(12) . . ? C41 C42 C47 123.8(15) . . ? C41 C42 C43 120.5(10) . . ? C47 C42 C43 115.7(17) . . ? C44 C43 C42 120.1(11) . . ? C43 C44 C45 122.6(11) . . ? C46 C45 C44 118.9(13) . . ? C45 C46 C47 121.7(12) . . ? C38 C47 C42 117.0(12) . . ? C38 C47 C46 122.2(9) . . ? C42 C47 C46 120.8(12) . . ? C2 S37 C37 108.4(4) . . ? C2 S37 Pd1 111.3(2) . . ? C37 S37 Pd1 101.3(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.515 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.068 #===END