# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_address ; Department of Chemistry McMaster University Hamilton Ontario, Canada ; _publ_contact_author_address ; Department of Chemistry McMaster University Hamilton Ontario, Canada ; _publ_contact_author_email emslied@mcmaster.ca _publ_contact_author_fax 1(905)5222509 _publ_contact_author_phone 1(905)5259140 _publ_contact_author_name 'David Emslie' _publ_section_title ; A Study of M-X-BR3 (X=Cl or I) Interactions in Square Planar Group 9 and 10 Transition Metals Complexes: Comparison with Borane-Free Analogues, Solid State Structures, Electrochemistry, and DFT Calculations ; loop_ _publ_author_name 'D.EmslieDavid Emslie' 'Bradley Cowie' 'Simon Oakley' 'Natalie Huk' 'Hilary Jenkins' 'Laura Harrington' 'James Britten' data_de31a _database_code_depnum_ccdc_archive 'CCDC 849792' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common x _chemical_melting_point ? _chemical_formula_moiety 'C47 H48 B Cl2 P Pt S, 2(C H2 Cl2)' _chemical_formula_sum 'C49 H52 B Cl6 P Pt S' _chemical_formula_weight 1122.54 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' B B 0.0013 0.0007 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall '-P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 21.373(2) _cell_length_b 8.9593(9) _cell_length_c 25.330(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4850.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2485 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 19.24 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 3.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5018 _exptl_absorpt_correction_T_max 0.9674 _exptl_absorpt_process_details SADABS _exptl_special_details ; A crystal of suitable size was selected and mounted on a goniometer head, then placed in the cold stream of the diffractometer. Data were collected with Mo K(alpha) radiation from a Siemens rotating anode, with a SMART 1K detector, at -100C. Omega and phi scans were used to ensure complete coverage. A multi-scan absorption correction was applied using the program SADABS (Bruker 2003) and the data were solved in the orthorhombic space group Pna2(1). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'parallel mirrors' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27401 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.48 _reflns_number_total 6568 _reflns_number_gt 4977 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were placed in idealized positions and updated with each cycle of refinement. One of the ligand t-butyl groups exhibited rotational disorder (C20-23) over two positions in a 59:41 ratio. Two molecules of CH2Cl2 were also located and refined as disordered over two positions, one at a ratio of 60:40 and one at 56:44. These solvent molecules were also restrained to approximate isotropic behaviour. The .res file for this complex is shown below and indicates other refinement details. The largest residual peak, at 1.00eA^-3, was associated with the Pt atom. 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^ > 2\s(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. The two molecules of CH2Cl2 within the lattice were refined using the ISOR command because anisotropic refinement of the carbon atoms was not stable. The chlorine atoms in each CH2Cl2 could be refined anisotropically, however for consistency the whole solvent molecule, in both cases, was refined using the ISOR command. ; _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^)+(0.0467P)^2^+1.0362P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(8) _refine_ls_number_reflns 6568 _refine_ls_number_parameters 533 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.014 _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 0.470674(13) 0.64083(4) 0.75046(3) 0.02491(10) Uani 1 1 d . . . S S 0.55165(11) 0.7804(3) 0.77755(9) 0.0257(5) Uani 1 1 d . . . P P 0.53458(11) 0.5357(3) 0.69267(9) 0.0252(6) Uani 1 1 d . . . B B 0.4600(6) 0.6692(18) 0.8829(5) 0.035(4) Uani 1 1 d . . . Cl2 Cl 0.38296(11) 0.5208(3) 0.71705(10) 0.0366(6) Uani 1 1 d . . . Cl1 Cl 0.40995(11) 0.7614(3) 0.81729(9) 0.0321(6) Uani 1 1 d . . . C1 C 0.7296(4) 0.6559(11) 0.7553(5) 0.030(3) Uani 1 1 d . . . H1A H 0.7696 0.6831 0.7687 0.036 Uiso 1 1 calc R . . C2 C 0.7262(4) 0.5356(12) 0.7195(4) 0.031(2) Uani 1 1 d . . . C3 C 0.6661(4) 0.4964(12) 0.7003(3) 0.029(2) Uani 1 1 d . . . H3A H 0.6615 0.4161 0.6761 0.034 Uiso 1 1 calc R . . C4 C 0.6131(4) 0.5769(12) 0.7172(3) 0.025(2) Uani 1 1 d . . . C5 C 0.5273(5) 0.7567(12) 0.8856(4) 0.029(2) Uani 1 1 d . . . C6 C 0.5476(5) 0.7797(13) 0.9380(4) 0.030(3) Uani 1 1 d . A . H6A H 0.5191 0.7602 0.9659 0.036 Uiso 1 1 calc R . . C7 C 0.6067(4) 0.8290(12) 0.9507(4) 0.031(2) Uani 1 1 d . . . C8 C 0.6483(4) 0.8497(12) 0.9099(4) 0.031(2) Uani 1 1 d . A . H8A H 0.6899 0.8787 0.9182 0.037 Uiso 1 1 calc R . . C9 C 0.6809(4) 0.8628(12) 0.8134(4) 0.031(2) Uani 1 1 d . A . C10 C 0.6781(4) 0.7366(12) 0.7722(3) 0.026(2) Uani 1 1 d . . . C11 C 0.6203(4) 0.6897(10) 0.7546(5) 0.026(2) Uani 1 1 d . . . C12 C 0.5708(5) 0.7857(12) 0.8469(3) 0.028(2) Uani 1 1 d . A . C13 C 0.6328(4) 0.8307(11) 0.8582(4) 0.028(2) Uani 1 1 d . . . C14 C 0.6652(5) 1.0142(14) 0.7859(4) 0.042(3) Uani 1 1 d . . . H14A H 0.6957 1.0336 0.7578 0.063 Uiso 1 1 calc R A . H14B H 0.6668 1.0950 0.8119 0.063 Uiso 1 1 calc R . . H14C H 0.6231 1.0090 0.7706 0.063 Uiso 1 1 calc R . . C15 C 0.7462(5) 0.8852(14) 0.8351(4) 0.039(3) Uani 1 1 d . . . H15A H 0.7597 0.7945 0.8535 0.059 Uiso 1 1 calc R A . H15B H 0.7461 0.9693 0.8599 0.059 Uiso 1 1 calc R . . H15C H 0.7751 0.9065 0.8060 0.059 Uiso 1 1 calc R . . C16 C 0.7850(5) 0.4485(13) 0.7048(4) 0.033(2) Uani 1 1 d . . . C17 C 0.7717(5) 0.3194(14) 0.6682(4) 0.045(3) Uani 1 1 d . . . H17A H 0.7420 0.2511 0.6850 0.067 Uiso 1 1 calc R . . H17B H 0.8107 0.2662 0.6606 0.067 Uiso 1 1 calc R . . H17C H 0.7538 0.3572 0.6352 0.067 Uiso 1 1 calc R . . C18 C 0.8326(5) 0.5538(14) 0.6774(4) 0.043(3) Uani 1 1 d . . . H18A H 0.8140 0.5945 0.6451 0.065 Uiso 1 1 calc R . . H18B H 0.8705 0.4977 0.6685 0.065 Uiso 1 1 calc R . . H18C H 0.8434 0.6358 0.7014 0.065 Uiso 1 1 calc R . . C19 C 0.8140(5) 0.3856(13) 0.7556(6) 0.047(3) Uani 1 1 d . . . H19A H 0.7843 0.3176 0.7726 0.071 Uiso 1 1 calc R . . H19B H 0.8239 0.4678 0.7797 0.071 Uiso 1 1 calc R . . H19C H 0.8525 0.3311 0.7469 0.071 Uiso 1 1 calc R . . C20A C 0.6248(5) 0.8562(12) 1.0089(4) 0.047(3) Uani 0.588(12) 1 d PD A 1 C21A C 0.5861(9) 0.987(2) 1.0295(7) 0.079(5) Uani 0.588(12) 1 d PD A 1 H21A H 0.5947 1.0757 1.0081 0.119 Uiso 0.588(12) 1 calc PR A 1 H21B H 0.5973 1.0067 1.0664 0.119 Uiso 0.588(12) 1 calc PR A 1 H21C H 0.5416 0.9621 1.0273 0.119 Uiso 0.588(12) 1 calc PR A 1 C22A C 0.6111(9) 0.718(2) 1.0425(6) 0.079(5) Uani 0.588(12) 1 d PD A 1 H22A H 0.6358 0.6336 1.0294 0.119 Uiso 0.588(12) 1 calc PR A 1 H22B H 0.5664 0.6935 1.0402 0.119 Uiso 0.588(12) 1 calc PR A 1 H22C H 0.6221 0.7381 1.0793 0.119 Uiso 0.588(12) 1 calc PR A 1 C23A C 0.6945(7) 0.893(2) 1.0140(7) 0.079(5) Uani 0.588(12) 1 d PD A 1 H23A H 0.7194 0.8096 1.0008 0.119 Uiso 0.588(12) 1 calc PR A 1 H23B H 0.7047 0.9115 1.0512 0.119 Uiso 0.588(12) 1 calc PR A 1 H23C H 0.7039 0.9830 0.9933 0.119 Uiso 0.588(12) 1 calc PR A 1 C20B C 0.6248(5) 0.8562(12) 1.0089(4) 0.047(3) Uani 0.412(12) 1 d PD A 2 C21B C 0.5667(8) 0.861(3) 1.0445(8) 0.079(5) Uani 0.412(12) 1 d PD A 2 H21D H 0.5396 0.9439 1.0335 0.119 Uiso 0.412(12) 1 calc PR A 2 H21E H 0.5797 0.8765 1.0813 0.119 Uiso 0.412(12) 1 calc PR A 2 H21F H 0.5438 0.7670 1.0416 0.119 Uiso 0.412(12) 1 calc PR A 2 C22B C 0.6668(11) 0.729(2) 1.0267(8) 0.079(5) Uani 0.412(12) 1 d PD A 2 H22D H 0.6439 0.6341 1.0239 0.119 Uiso 0.412(12) 1 calc PR A 2 H22E H 0.6794 0.7446 1.0635 0.119 Uiso 0.412(12) 1 calc PR A 2 H22F H 0.7041 0.7249 1.0043 0.119 Uiso 0.412(12) 1 calc PR A 2 C23B C 0.6596(12) 1.005(2) 1.0140(8) 0.079(5) Uani 0.412(12) 1 d PD A 2 H23D H 0.6324 1.0861 1.0022 0.119 Uiso 0.412(12) 1 calc PR A 2 H23E H 0.6974 1.0020 0.9921 0.119 Uiso 0.412(12) 1 calc PR A 2 H23F H 0.6714 1.0206 1.0510 0.119 Uiso 0.412(12) 1 calc PR A 2 C30 C 0.5310(5) 0.6124(12) 0.6262(4) 0.033(2) Uani 1 1 d . . . C31 C 0.4758(6) 0.5989(19) 0.5980(6) 0.062(4) Uani 1 1 d . . . H31A H 0.4400 0.5550 0.6138 0.074 Uiso 1 1 calc R . . C32 C 0.4736(6) 0.6509(18) 0.5460(5) 0.069(5) Uani 1 1 d . . . H32A H 0.4361 0.6387 0.5263 0.082 Uiso 1 1 calc R . . C33 C 0.5226(7) 0.7172(17) 0.5232(5) 0.062(4) Uani 1 1 d . . . H33A H 0.5197 0.7508 0.4877 0.075 Uiso 1 1 calc R . . C34 C 0.5783(8) 0.7372(16) 0.5516(4) 0.056(4) Uani 1 1 d . . . H34A H 0.6130 0.7877 0.5365 0.067 Uiso 1 1 calc R . . C35 C 0.5809(5) 0.6811(13) 0.6023(4) 0.041(3) Uani 1 1 d . . . H35A H 0.6189 0.6904 0.6215 0.049 Uiso 1 1 calc R . . C24 C 0.5273(4) 0.3359(11) 0.6842(4) 0.027(2) Uani 1 1 d . . . C25 C 0.5003(5) 0.2506(13) 0.7251(4) 0.033(2) Uani 1 1 d . . . H25A H 0.4870 0.2959 0.7571 0.040 Uiso 1 1 calc R . . C26 C 0.4939(5) 0.1004(14) 0.7170(5) 0.043(3) Uani 1 1 d . . . H26A H 0.4745 0.0419 0.7437 0.052 Uiso 1 1 calc R . . C27 C 0.5143(5) 0.0310(13) 0.6720(4) 0.041(3) Uani 1 1 d . . . H27A H 0.5094 -0.0737 0.6680 0.050 Uiso 1 1 calc R . . C28 C 0.5419(5) 0.1137(13) 0.6326(4) 0.040(3) Uani 1 1 d . . . H28A H 0.5567 0.0660 0.6015 0.048 Uiso 1 1 calc R . . C29 C 0.5481(5) 0.2688(16) 0.6385(4) 0.035(3) Uani 1 1 d . . . H29A H 0.5665 0.3270 0.6112 0.042 Uiso 1 1 calc R . . C42 C 0.4687(4) 0.4938(13) 0.8704(4) 0.031(2) Uani 1 1 d . . . C47 C 0.4175(6) 0.3987(12) 0.8591(4) 0.039(3) Uani 1 1 d . . . H47A H 0.3774 0.4416 0.8536 0.047 Uiso 1 1 calc R . . C46 C 0.4242(6) 0.2447(14) 0.8557(4) 0.044(3) Uani 1 1 d . . . H46A H 0.3886 0.1845 0.8486 0.053 Uiso 1 1 calc R . . C45 C 0.4818(7) 0.1783(16) 0.8626(5) 0.054(4) Uani 1 1 d . . . H45A H 0.4860 0.0731 0.8597 0.065 Uiso 1 1 calc R . . C44 C 0.5346(7) 0.2670(18) 0.8740(6) 0.054(4) Uani 1 1 d . . . H44A H 0.5745 0.2226 0.8793 0.065 Uiso 1 1 calc R . . C43 C 0.5269(5) 0.4236(15) 0.8772(4) 0.041(3) Uani 1 1 d . . . H43A H 0.5626 0.4837 0.8842 0.049 Uiso 1 1 calc R . . C36 C 0.4131(4) 0.7082(12) 0.9307(4) 0.030(2) Uani 1 1 d . . . C41 C 0.3954(6) 0.8526(13) 0.9412(5) 0.050(3) Uani 1 1 d . . . H41A H 0.4064 0.9304 0.9175 0.060 Uiso 1 1 calc R . . C40 C 0.3611(6) 0.8854(16) 0.9868(6) 0.061(4) Uani 1 1 d . . . H40A H 0.3526 0.9871 0.9946 0.074 Uiso 1 1 calc R . . C39 C 0.3397(5) 0.7816(17) 1.0197(4) 0.046(3) Uani 1 1 d . . . H39A H 0.3144 0.8073 1.0491 0.055 Uiso 1 1 calc R . . C38 C 0.3558(6) 0.6338(18) 1.0093(4) 0.062(4) Uani 1 1 d . . . H38A H 0.3416 0.5568 1.0321 0.075 Uiso 1 1 calc R . . C37 C 0.3919(5) 0.5991(15) 0.9664(4) 0.048(3) Uani 1 1 d . . . H37A H 0.4030 0.4978 0.9605 0.057 Uiso 1 1 calc R . . C48A C 0.2557(14) 0.601(3) 0.6290(12) 0.065(6) Uani 0.56(2) 1 d PU B 1 H48A H 0.2879 0.5214 0.6295 0.078 Uiso 0.56(2) 1 calc PR B 1 H48B H 0.2655 0.6716 0.6579 0.078 Uiso 0.56(2) 1 calc PR B 1 Cl3A Cl 0.1858(7) 0.5241(19) 0.6407(7) 0.0796(13) Uani 0.56(2) 1 d PU B 1 Cl4A Cl 0.2603(6) 0.6973(14) 0.5677(4) 0.0796(13) Uani 0.56(2) 1 d PU B 1 C48B C 0.2761(10) 0.556(4) 0.6172(10) 0.065(6) Uani 0.44(2) 1 d PDU B 2 H48C H 0.3030 0.6029 0.6443 0.078 Uiso 0.44(2) 1 calc PR B 2 H48D H 0.2918 0.4535 0.6108 0.078 Uiso 0.44(2) 1 calc PR B 2 Cl3B Cl 0.1980(9) 0.548(2) 0.6401(9) 0.0796(13) Uani 0.44(2) 1 d PDU B 2 Cl4B Cl 0.2801(8) 0.6602(18) 0.5581(5) 0.0796(13) Uani 0.44(2) 1 d PDU B 2 C49A C 0.2918(11) 0.649(4) 0.4277(13) 0.135(12) Uiso 0.60(3) 1 d PD C 1 H49A H 0.3288 0.7129 0.4345 0.161 Uiso 0.60(3) 1 calc PR C 1 H49B H 0.2896 0.5737 0.4562 0.161 Uiso 0.60(3) 1 calc PR C 1 Cl5A Cl 0.2236(2) 0.7615(6) 0.4301(2) 0.1143(18) Uani 0.60(3) 1 d PDU C 1 Cl6A Cl 0.3009(3) 0.5618(9) 0.3693(3) 0.151(2) Uani 0.60(3) 1 d PDU C 1 C49B C 0.243(2) 0.5746(13) 0.415(2) 0.135(12) Uiso 0.40(3) 1 d PD C 2 H49C H 0.2568 0.5229 0.4472 0.161 Uiso 0.40(3) 1 calc PR C 2 H49D H 0.2058 0.5228 0.4010 0.161 Uiso 0.40(3) 1 calc PR C 2 Cl5B Cl 0.2236(2) 0.7615(6) 0.4301(2) 0.1143(18) Uani 0.40(3) 1 d PDU C 2 Cl6B Cl 0.3009(3) 0.5618(9) 0.3693(3) 0.151(2) Uani 0.40(3) 1 d PDU C 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 Pt 0.02282(15) 0.02332(18) 0.02860(15) -0.0001(3) -0.0037(3) -0.00020(15) S 0.0245(12) 0.0250(15) 0.0277(11) -0.0025(11) 0.0002(10) -0.0015(10) P 0.0261(13) 0.0241(16) 0.0255(11) -0.0032(10) -0.0042(10) -0.0041(11) B 0.028(7) 0.047(10) 0.032(6) 0.008(6) 0.000(5) 0.000(6) Cl2 0.0275(13) 0.0341(17) 0.0483(14) -0.0024(12) -0.0100(11) -0.0046(11) Cl1 0.0256(12) 0.0333(16) 0.0375(12) -0.0026(11) -0.0008(10) 0.0031(11) C1 0.031(4) 0.032(6) 0.027(6) -0.017(5) 0.001(5) -0.002(4) C2 0.031(6) 0.028(7) 0.034(5) -0.001(5) 0.002(4) 0.002(5) C3 0.038(6) 0.024(6) 0.024(5) -0.003(4) -0.004(4) 0.000(5) C4 0.015(4) 0.033(6) 0.027(5) -0.003(4) 0.004(4) -0.006(4) C5 0.036(6) 0.020(6) 0.033(5) -0.005(4) -0.003(4) 0.002(5) C6 0.036(6) 0.027(7) 0.028(5) 0.000(5) 0.003(4) -0.012(5) C7 0.025(5) 0.033(7) 0.035(5) -0.016(5) 0.004(4) 0.003(5) C8 0.021(5) 0.038(7) 0.033(5) -0.012(5) 0.006(4) -0.015(5) C9 0.023(5) 0.035(7) 0.035(5) -0.009(5) 0.000(4) -0.013(5) C10 0.024(5) 0.028(6) 0.026(4) -0.001(4) -0.004(4) -0.005(4) C11 0.031(4) 0.016(5) 0.030(6) 0.002(5) 0.002(5) -0.004(3) C12 0.034(6) 0.022(6) 0.026(5) -0.003(4) 0.000(4) -0.002(5) C13 0.024(5) 0.022(6) 0.037(5) -0.012(4) 0.001(4) 0.001(4) C14 0.048(7) 0.035(8) 0.044(6) -0.007(5) 0.003(5) -0.012(6) C15 0.035(6) 0.043(9) 0.041(6) -0.014(5) -0.003(5) -0.018(5) C16 0.029(5) 0.035(7) 0.037(5) -0.002(5) 0.000(4) 0.005(5) C17 0.043(7) 0.039(8) 0.052(7) -0.019(5) -0.002(5) 0.019(5) C18 0.020(5) 0.057(9) 0.053(6) 0.001(6) 0.010(5) 0.002(5) C19 0.044(6) 0.046(7) 0.052(8) -0.006(7) -0.016(7) 0.019(5) C20A 0.045(7) 0.064(10) 0.034(5) -0.020(6) -0.005(5) -0.004(6) C21A 0.081(9) 0.119(14) 0.037(5) -0.008(7) -0.002(6) -0.039(8) C22A 0.081(9) 0.119(14) 0.037(5) -0.008(7) -0.002(6) -0.039(8) C23A 0.081(9) 0.119(14) 0.037(5) -0.008(7) -0.002(6) -0.039(8) C20B 0.045(7) 0.064(10) 0.034(5) -0.020(6) -0.005(5) -0.004(6) C21B 0.081(9) 0.119(14) 0.037(5) -0.008(7) -0.002(6) -0.039(8) C22B 0.081(9) 0.119(14) 0.037(5) -0.008(7) -0.002(6) -0.039(8) C23B 0.081(9) 0.119(14) 0.037(5) -0.008(7) -0.002(6) -0.039(8) C30 0.047(6) 0.025(7) 0.027(5) -0.005(4) -0.008(5) 0.004(5) C31 0.062(10) 0.066(11) 0.057(9) 0.041(8) -0.018(7) -0.026(8) C32 0.067(9) 0.101(14) 0.038(6) 0.024(7) -0.016(6) -0.044(9) C33 0.093(11) 0.053(10) 0.041(7) 0.013(6) -0.016(7) -0.009(8) C34 0.085(11) 0.044(10) 0.039(7) 0.012(6) 0.014(7) -0.006(8) C35 0.043(7) 0.040(8) 0.038(5) 0.011(5) -0.002(5) -0.015(6) C24 0.024(5) 0.030(7) 0.026(4) 0.000(4) -0.007(4) 0.003(5) C25 0.034(5) 0.029(7) 0.037(5) -0.001(5) -0.005(4) 0.004(5) C26 0.045(7) 0.035(8) 0.049(6) 0.022(5) 0.009(5) 0.003(5) C27 0.052(7) 0.023(7) 0.049(6) 0.004(5) -0.001(5) 0.006(5) C28 0.044(7) 0.033(8) 0.042(6) -0.005(5) 0.001(5) 0.008(5) C29 0.037(6) 0.042(8) 0.025(5) -0.008(5) 0.006(5) -0.018(6) C42 0.030(5) 0.035(7) 0.028(5) 0.004(4) 0.001(4) -0.009(5) C47 0.053(7) 0.022(7) 0.042(6) 0.005(5) -0.005(5) -0.003(5) C46 0.060(8) 0.038(8) 0.035(5) 0.006(5) -0.003(5) -0.003(6) C45 0.084(11) 0.038(8) 0.040(6) 0.000(5) 0.014(6) -0.001(7) C44 0.067(10) 0.042(10) 0.053(8) 0.020(7) 0.009(7) 0.021(8) C43 0.026(5) 0.044(8) 0.051(6) 0.004(6) -0.001(5) 0.005(5) C36 0.026(5) 0.026(6) 0.039(5) -0.004(5) 0.002(4) -0.002(5) C41 0.058(8) 0.030(7) 0.063(7) -0.002(6) 0.030(6) -0.003(6) C40 0.058(8) 0.043(10) 0.082(9) -0.026(7) 0.026(7) -0.007(7) C39 0.034(6) 0.063(10) 0.041(6) -0.018(6) 0.008(5) -0.003(6) C38 0.048(7) 0.104(14) 0.034(6) 0.011(7) 0.011(5) 0.005(8) C37 0.053(7) 0.049(9) 0.042(6) -0.004(6) 0.004(5) -0.003(6) C48A 0.064(8) 0.059(9) 0.071(8) 0.007(6) -0.009(6) 0.002(6) Cl3A 0.082(4) 0.075(3) 0.0816(19) 0.009(2) 0.004(2) 0.015(2) Cl4A 0.082(4) 0.075(3) 0.0816(19) 0.009(2) 0.004(2) 0.015(2) C48B 0.064(8) 0.059(9) 0.071(8) 0.007(6) -0.009(6) 0.002(6) Cl3B 0.082(4) 0.075(3) 0.0816(19) 0.009(2) 0.004(2) 0.015(2) Cl4B 0.082(4) 0.075(3) 0.0816(19) 0.009(2) 0.004(2) 0.015(2) Cl5A 0.133(4) 0.104(4) 0.106(3) 0.017(3) -0.008(3) 0.021(3) Cl6A 0.140(4) 0.160(5) 0.154(4) -0.016(4) 0.009(4) 0.036(4) Cl5B 0.133(4) 0.104(4) 0.106(3) 0.017(3) -0.008(3) 0.021(3) Cl6B 0.140(4) 0.160(5) 0.154(4) -0.016(4) 0.009(4) 0.036(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P 2.213(2) . ? Pt S 2.243(2) . ? Pt Cl2 2.321(2) . ? Pt Cl1 2.391(2) . ? S C11 1.775(10) . ? S C12 1.805(9) . ? P C24 1.809(11) . ? P C30 1.820(10) . ? P C4 1.827(9) . ? B C36 1.611(17) . ? B C42 1.613(19) . ? B C5 1.638(16) . ? B Cl1 2.142(13) . ? C1 C10 1.384(13) . ? C1 C2 1.411(14) . ? C1 H1A 0.9500 . ? C2 C3 1.419(13) . ? C2 C16 1.524(14) . ? C3 C4 1.409(13) . ? C3 H3A 0.9500 . ? C4 C11 1.395(14) . ? C5 C12 1.376(13) . ? C5 C6 1.413(13) . ? C6 C7 1.377(14) . ? C6 H6A 0.9500 . ? C7 C8 1.376(13) . ? C7 C20A 1.544(13) . ? C8 C13 1.361(13) . ? C8 H8A 0.9500 . ? C9 C15 1.512(13) . ? C9 C10 1.541(14) . ? C9 C13 1.558(13) . ? C9 C14 1.563(16) . ? C10 C11 1.378(12) . ? C12 C13 1.414(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.509(15) . ? C16 C19 1.537(16) . ? C16 C18 1.552(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20A C21A 1.524(12) . ? C20A C22A 1.531(12) . ? C20A C23A 1.533(12) . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C30 C35 1.372(15) . ? C30 C31 1.382(15) . ? C31 C32 1.399(18) . ? C31 H31A 0.9500 . ? C32 C33 1.335(18) . ? C32 H32A 0.9500 . ? C33 C34 1.403(19) . ? C33 H33A 0.9500 . ? C34 C35 1.380(15) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C24 C29 1.377(15) . ? C24 C25 1.411(14) . ? C25 C26 1.368(17) . ? C25 H25A 0.9500 . ? C26 C27 1.370(16) . ? C26 H26A 0.9500 . ? C27 C28 1.376(16) . ? C27 H27A 0.9500 . ? C28 C29 1.404(17) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C42 C43 1.405(14) . ? C42 C47 1.415(15) . ? C47 C46 1.390(16) . ? C47 H47A 0.9500 . ? C46 C45 1.379(17) . ? C46 H46A 0.9500 . ? C45 C44 1.41(2) . ? C45 H45A 0.9500 . ? C44 C43 1.42(2) . ? C44 H44A 0.9500 . ? C43 H43A 0.9500 . ? C36 C41 1.374(15) . ? C36 C37 1.407(16) . ? C41 C40 1.397(16) . ? C41 H41A 0.9500 . ? C40 C39 1.329(18) . ? C40 H40A 0.9500 . ? C39 C38 1.393(18) . ? C39 H39A 0.9500 . ? C38 C37 1.368(16) . ? C38 H38A 0.9500 . ? C37 H37A 0.9500 . ? C48A Cl3A 1.67(3) . ? C48A Cl4A 1.78(3) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C48B Cl4B 1.767(5) . ? C48B Cl3B 1.770(5) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49A Cl6A 1.69(3) . ? C49A Cl5A 1.772(4) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C49B H49C 0.9900 . ? C49B H49D 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 P Pt S 87.90(9) . . ? P Pt Cl2 93.45(9) . . ? S Pt Cl2 173.31(10) . . ? P Pt Cl1 174.75(9) . . ? S Pt Cl1 87.16(9) . . ? Cl2 Pt Cl1 91.66(9) . . ? C11 S C12 98.2(5) . . ? C11 S Pt 106.4(3) . . ? C12 S Pt 119.2(3) . . ? C24 P C30 105.1(5) . . ? C24 P C4 108.6(5) . . ? C30 P C4 106.1(5) . . ? C24 P Pt 116.6(3) . . ? C30 P Pt 115.1(4) . . ? C4 P Pt 104.8(3) . . ? C36 B C42 115.4(10) . . ? C36 B C5 114.2(10) . . ? C42 B C5 111.9(10) . . ? C36 B Cl1 100.8(8) . . ? C42 B Cl1 106.4(8) . . ? C5 B Cl1 106.6(8) . . ? B Cl1 Pt 95.9(4) . . ? C10 C1 C2 123.8(9) . . ? C10 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C1 C2 C3 117.1(9) . . ? C1 C2 C16 120.4(9) . . ? C3 C2 C16 122.4(9) . . ? C4 C3 C2 119.8(9) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C11 C4 C3 119.2(8) . . ? C11 C4 P 118.6(7) . . ? C3 C4 P 122.1(7) . . ? C12 C5 C6 115.6(9) . . ? C12 C5 B 130.9(9) . . ? C6 C5 B 112.3(9) . . ? C7 C6 C5 123.3(9) . . ? C7 C6 H6A 118.4 . . ? C5 C6 H6A 118.4 . . ? C8 C7 C6 117.5(9) . . ? C8 C7 C20A 122.4(8) . . ? C6 C7 C20A 120.2(9) . . ? C13 C8 C7 123.2(9) . . ? C13 C8 H8A 118.4 . . ? C7 C8 H8A 118.4 . . ? C15 C9 C10 112.3(8) . . ? C15 C9 C13 111.7(8) . . ? C10 C9 C13 109.4(8) . . ? C15 C9 C14 104.2(8) . . ? C10 C9 C14 109.0(8) . . ? C13 C9 C14 110.1(8) . . ? C11 C10 C1 117.1(9) . . ? C11 C10 C9 118.5(8) . . ? C1 C10 C9 124.1(8) . . ? C10 C11 C4 122.6(9) . . ? C10 C11 S 119.8(8) . . ? C4 C11 S 117.5(7) . . ? C5 C12 C13 123.0(8) . . ? C5 C12 S 122.3(7) . . ? C13 C12 S 114.6(7) . . ? C8 C13 C12 117.3(9) . . ? C8 C13 C9 121.1(8) . . ? C12 C13 C9 121.6(8) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C2 112.8(9) . . ? C17 C16 C19 108.1(10) . . ? C2 C16 C19 108.4(8) . . ? C17 C16 C18 108.3(9) . . ? C2 C16 C18 109.7(9) . . ? C19 C16 C18 109.4(9) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21A C20A C22A 109.2(6) . . ? C21A C20A C23A 109.3(6) . . ? C22A C20A C23A 108.4(6) . . ? C21A C20A C7 108.2(10) . . ? C22A C20A C7 110.8(10) . . ? C23A C20A C7 110.9(10) . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C20A C23A H23A 109.5 . . ? C20A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C20A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? H21D C21B H21E 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? H22D C22B H22E 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? H23D C23B H23E 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C35 C30 C31 118.3(10) . . ? C35 C30 P 122.9(8) . . ? C31 C30 P 118.7(9) . . ? C30 C31 C32 119.1(12) . . ? C30 C31 H31A 120.4 . . ? C32 C31 H31A 120.4 . . ? C33 C32 C31 122.0(12) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 120.0(12) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 117.8(13) . . ? C35 C34 H34A 121.1 . . ? C33 C34 H34A 121.1 . . ? C30 C35 C34 122.8(11) . . ? C30 C35 H35A 118.6 . . ? C34 C35 H35A 118.6 . . ? C29 C24 C25 120.8(10) . . ? C29 C24 P 120.3(9) . . ? C25 C24 P 118.9(8) . . ? C26 C25 C24 117.6(10) . . ? C26 C25 H25A 121.2 . . ? C24 C25 H25A 121.2 . . ? C25 C26 C27 122.6(11) . . ? C25 C26 H26A 118.7 . . ? C27 C26 H26A 118.7 . . ? C26 C27 C28 119.8(11) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C27 C28 C29 119.7(11) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C24 C29 C28 119.5(11) . . ? C24 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C43 C42 C47 116.1(11) . . ? C43 C42 B 120.9(10) . . ? C47 C42 B 122.5(10) . . ? C46 C47 C42 122.1(11) . . ? C46 C47 H47A 119.0 . . ? C42 C47 H47A 119.0 . . ? C45 C46 C47 120.8(12) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C46 C45 C44 119.9(14) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C45 C44 C43 118.5(13) . . ? C45 C44 H44A 120.7 . . ? C43 C44 H44A 120.7 . . ? C42 C43 C44 122.7(12) . . ? C42 C43 H43A 118.7 . . ? C44 C43 H43A 118.7 . . ? C41 C36 C37 116.1(10) . . ? C41 C36 B 121.5(10) . . ? C37 C36 B 122.2(11) . . ? C36 C41 C40 120.2(11) . . ? C36 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C39 C40 C41 123.4(13) . . ? C39 C40 H40A 118.3 . . ? C41 C40 H40A 118.3 . . ? C40 C39 C38 117.5(11) . . ? C40 C39 H39A 121.3 . . ? C38 C39 H39A 121.3 . . ? C37 C38 C39 120.3(12) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C38 C37 C36 122.3(13) . . ? C38 C37 H37A 118.9 . . ? C36 C37 H37A 118.9 . . ? Cl3A C48A Cl4A 113.8(16) . . ? Cl3A C48A H48A 108.8 . . ? Cl4A C48A H48A 108.8 . . ? Cl3A C48A H48B 108.8 . . ? Cl4A C48A H48B 108.8 . . ? H48A C48A H48B 107.7 . . ? Cl4B C48B Cl3B 110.1(11) . . ? Cl4B C48B H48C 109.6 . . ? Cl3B C48B H48C 109.6 . . ? Cl4B C48B H48D 109.6 . . ? Cl3B C48B H48D 109.6 . . ? H48C C48B H48D 108.2 . . ? Cl6A C49A Cl5A 112.9(14) . . ? Cl6A C49A H49A 109.0 . . ? Cl5A C49A H49A 109.0 . . ? Cl6A C49A H49B 109.0 . . ? Cl5A C49A H49B 109.0 . . ? H49A C49A H49B 107.8 . . ? H49C C49B H49D 107.8 . . ? 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 P Pt S C11 -18.1(4) . . . . ? Cl1 Pt S C11 160.2(4) . . . . ? P Pt S C12 -127.6(4) . . . . ? Cl1 Pt S C12 50.6(4) . . . . ? S Pt P C24 138.6(3) . . . . ? Cl2 Pt P C24 -48.0(3) . . . . ? S Pt P C30 -97.7(4) . . . . ? Cl2 Pt P C30 75.8(4) . . . . ? S Pt P C4 18.5(3) . . . . ? Cl2 Pt P C4 -168.1(4) . . . . ? C36 B Cl1 Pt -166.3(7) . . . . ? C42 B Cl1 Pt -45.4(7) . . . . ? C5 B Cl1 Pt 74.2(8) . . . . ? S Pt Cl1 B -66.1(4) . . . . ? Cl2 Pt Cl1 B 120.5(4) . . . . ? C10 C1 C2 C3 -0.3(17) . . . . ? C10 C1 C2 C16 -177.4(11) . . . . ? C1 C2 C3 C4 0.1(15) . . . . ? C16 C2 C3 C4 177.1(9) . . . . ? C2 C3 C4 C11 -3.1(15) . . . . ? C2 C3 C4 P 178.3(7) . . . . ? C24 P C4 C11 -141.9(9) . . . . ? C30 P C4 C11 105.6(9) . . . . ? Pt P C4 C11 -16.6(9) . . . . ? C24 P C4 C3 36.7(9) . . . . ? C30 P C4 C3 -75.7(9) . . . . ? Pt P C4 C3 162.0(7) . . . . ? C36 B C5 C12 -159.7(11) . . . . ? C42 B C5 C12 66.7(15) . . . . ? Cl1 B C5 C12 -49.2(15) . . . . ? C36 B C5 C6 33.6(14) . . . . ? C42 B C5 C6 -100.0(11) . . . . ? Cl1 B C5 C6 144.1(8) . . . . ? C12 C5 C6 C7 0.5(16) . . . . ? B C5 C6 C7 169.4(11) . . . . ? C5 C6 C7 C8 -3.1(17) . . . . ? C5 C6 C7 C20A 178.1(10) . . . . ? C6 C7 C8 C13 3.2(17) . . . . ? C20A C7 C8 C13 -178.0(10) . . . . ? C2 C1 C10 C11 3.6(17) . . . . ? C2 C1 C10 C9 176.7(10) . . . . ? C15 C9 C10 C11 170.9(10) . . . . ? C13 C9 C10 C11 46.3(13) . . . . ? C14 C9 C10 C11 -74.1(12) . . . . ? C15 C9 C10 C1 -2.1(15) . . . . ? C13 C9 C10 C1 -126.7(11) . . . . ? C14 C9 C10 C1 112.9(11) . . . . ? C1 C10 C11 C4 -6.8(16) . . . . ? C9 C10 C11 C4 179.7(10) . . . . ? C1 C10 C11 S 176.3(9) . . . . ? C9 C10 C11 S 2.8(14) . . . . ? C3 C4 C11 C10 6.7(17) . . . . ? P C4 C11 C10 -174.6(8) . . . . ? C3 C4 C11 S -176.3(8) . . . . ? P C4 C11 S 2.3(13) . . . . ? C12 S C11 C10 -46.1(10) . . . . ? Pt S C11 C10 -169.9(8) . . . . ? C12 S C11 C4 136.9(10) . . . . ? Pt S C11 C4 13.1(10) . . . . ? C6 C5 C12 C13 2.1(15) . . . . ? B C5 C12 C13 -164.3(11) . . . . ? C6 C5 C12 S -173.9(8) . . . . ? B C5 C12 S 19.8(17) . . . . ? C11 S C12 C5 -138.8(9) . . . . ? Pt S C12 C5 -24.7(10) . . . . ? C11 S C12 C13 44.9(8) . . . . ? Pt S C12 C13 159.0(6) . . . . ? C7 C8 C13 C12 -0.8(16) . . . . ? C7 C8 C13 C9 177.1(10) . . . . ? C5 C12 C13 C8 -2.0(16) . . . . ? S C12 C13 C8 174.3(8) . . . . ? C5 C12 C13 C9 -179.9(10) . . . . ? S C12 C13 C9 -3.7(13) . . . . ? C15 C9 C13 C8 11.1(14) . . . . ? C10 C9 C13 C8 136.1(10) . . . . ? C14 C9 C13 C8 -104.1(11) . . . . ? C15 C9 C13 C12 -171.0(10) . . . . ? C10 C9 C13 C12 -46.1(13) . . . . ? C14 C9 C13 C12 73.7(11) . . . . ? C1 C2 C16 C17 177.2(10) . . . . ? C3 C2 C16 C17 0.2(14) . . . . ? C1 C2 C16 C19 57.5(13) . . . . ? C3 C2 C16 C19 -119.4(10) . . . . ? C1 C2 C16 C18 -61.9(13) . . . . ? C3 C2 C16 C18 121.1(10) . . . . ? C8 C7 C20A C21A 114.8(12) . . . . ? C6 C7 C20A C21A -66.5(13) . . . . ? C8 C7 C20A C22A -125.6(12) . . . . ? C6 C7 C20A C22A 53.2(13) . . . . ? C8 C7 C20A C23A -5.2(14) . . . . ? C6 C7 C20A C23A 173.6(11) . . . . ? C24 P C30 C35 -113.0(10) . . . . ? C4 P C30 C35 1.9(11) . . . . ? Pt P C30 C35 117.4(9) . . . . ? C24 P C30 C31 65.9(12) . . . . ? C4 P C30 C31 -179.2(11) . . . . ? Pt P C30 C31 -63.7(12) . . . . ? C35 C30 C31 C32 2(2) . . . . ? P C30 C31 C32 -176.8(13) . . . . ? C30 C31 C32 C33 -2(3) . . . . ? C31 C32 C33 C34 0(3) . . . . ? C32 C33 C34 C35 3(2) . . . . ? C31 C30 C35 C34 0(2) . . . . ? P C30 C35 C34 179.0(10) . . . . ? C33 C34 C35 C30 -2(2) . . . . ? C30 P C24 C29 29.0(10) . . . . ? C4 P C24 C29 -84.2(9) . . . . ? Pt P C24 C29 157.8(7) . . . . ? C30 P C24 C25 -151.1(8) . . . . ? C4 P C24 C25 95.7(8) . . . . ? Pt P C24 C25 -22.3(8) . . . . ? C29 C24 C25 C26 -1.8(15) . . . . ? P C24 C25 C26 178.3(8) . . . . ? C24 C25 C26 C27 2.0(16) . . . . ? C25 C26 C27 C28 -0.6(18) . . . . ? C26 C27 C28 C29 -0.9(17) . . . . ? C25 C24 C29 C28 0.3(16) . . . . ? P C24 C29 C28 -179.8(8) . . . . ? C27 C28 C29 C24 1.1(17) . . . . ? C36 B C42 C43 -115.7(11) . . . . ? C5 B C42 C43 17.2(14) . . . . ? Cl1 B C42 C43 133.3(9) . . . . ? C36 B C42 C47 55.8(13) . . . . ? C5 B C42 C47 -171.2(9) . . . . ? Cl1 B C42 C47 -55.1(11) . . . . ? C43 C42 C47 C46 1.1(15) . . . . ? B C42 C47 C46 -170.8(10) . . . . ? C42 C47 C46 C45 -1.1(16) . . . . ? C47 C46 C45 C44 1.0(17) . . . . ? C46 C45 C44 C43 -1.0(18) . . . . ? C47 C42 C43 C44 -1.2(15) . . . . ? B C42 C43 C44 170.9(10) . . . . ? C45 C44 C43 C42 1.1(17) . . . . ? C42 B C36 C41 -171.8(10) . . . . ? C5 B C36 C41 56.3(14) . . . . ? Cl1 B C36 C41 -57.6(12) . . . . ? C42 B C36 C37 13.3(15) . . . . ? C5 B C36 C37 -118.6(12) . . . . ? Cl1 B C36 C37 127.4(9) . . . . ? C37 C36 C41 C40 3.3(17) . . . . ? B C36 C41 C40 -171.9(11) . . . . ? C36 C41 C40 C39 -5(2) . . . . ? C41 C40 C39 C38 4(2) . . . . ? C40 C39 C38 C37 -0.5(19) . . . . ? C39 C38 C37 C36 -1.3(19) . . . . ? C41 C36 C37 C38 -0.1(17) . . . . ? B C36 C37 C38 175.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.995 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.132 # Attachment '- 2B DE05 PdCl2(TXPB) NEW.cif' data_de05 _database_code_depnum_ccdc_archive 'CCDC 849793' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H48 B Cl2 P Pd S' _chemical_formula_sum 'C47 H48 B Cl2 P Pd S' _chemical_formula_weight 863.99 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' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 11.2575(5) _cell_length_b 27.0326(13) _cell_length_c 13.7991(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.258(3) _cell_angle_gamma 90.00 _cell_volume 4165.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3135 _cell_measurement_theta_min 23.58 _cell_measurement_theta_max 2.329 _exptl_crystal_description plate _exptl_crystal_colour pale_orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details SADABS _exptl_special_details ; A crystal of suitable size was selected and mounted on a goniometer head, then placed in the cold stream of the diffractometer. Data were collected with Mo K(alpha) radiation from a Siemens rotating anode, with a SMART 1K detector, at -100C. Omega and phi scans were used to ensure complete coverage. Data were corrected for absorption using SADABS then solved by direct methods in the space group P2(1)/c. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'parallel mirrors' _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25320 _diffrn_reflns_av_R_equivalents 0.1524 _diffrn_reflns_av_sigmaI/netI 0.1431 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5445 _reflns_number_gt 3699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were generated in ideal positions and then updated with each cycle of refinement. There was slight (1.0%) twinning, and residual electron density associated with the lattice that is due to a "shadow" of the heavy atom from another microcrystal. 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^)+(0.0938P)^2^+0.0000P] 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 0.0128(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5445 _refine_ls_number_parameters 480 _refine_ls_number_restraints 624 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.2131 _refine_ls_wR_factor_gt 0.1936 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.32441(6) 0.00913(3) 0.75093(7) 0.0169(4) Uani 1 1 d U . . S1 S 0.1355(2) 0.02795(10) 0.6718(2) 0.0160(7) Uani 1 1 d U . . P1 P 0.2485(2) -0.06527(11) 0.7720(2) 0.0168(8) Uani 1 1 d U A . Cl1 Cl 0.5107(2) -0.01857(11) 0.8133(2) 0.0289(8) Uani 1 1 d U . . C1 C -0.1280(9) -0.0206(4) 0.8223(8) 0.020(2) Uani 1 1 d U A 1 H1A H -0.2068 -0.0108 0.8313 0.024 Uiso 1 1 calc R A 1 B1 B 0.2936(11) 0.1294(5) 0.6569(11) 0.023(2) Uani 1 1 d U . . Cl2 Cl 0.3974(2) 0.09070(11) 0.7554(2) 0.0287(8) Uani 1 1 d U . . C2 C -0.0776(9) -0.0601(4) 0.8764(8) 0.019(2) Uani 1 1 d U . . C3 C 0.0345(8) -0.0769(4) 0.8534(8) 0.016(2) Uani 1 1 d U A . H3A H 0.0689 -0.1062 0.8827 0.019 Uiso 1 1 calc R . . C4 C 0.0946(8) -0.0503(4) 0.7879(8) 0.015(2) Uani 1 1 d U . . C5 C 0.1597(9) 0.1303(4) 0.6895(9) 0.022(2) Uani 1 1 d U . . C6 C 0.1109(9) 0.1759(4) 0.7108(8) 0.021(2) Uani 1 1 d U . . H6A H 0.1594 0.2046 0.7086 0.026 Uiso 1 1 calc R . . C7 C -0.0079(9) 0.1821(4) 0.7358(8) 0.019(2) Uani 1 1 d U . . C8 C -0.0789(9) 0.1399(4) 0.7308(8) 0.016(2) Uani 1 1 d U A . H8A H -0.1592 0.1431 0.7442 0.019 Uiso 1 1 calc R . . C9 C -0.1273(8) 0.0500(4) 0.6958(8) 0.019(2) Uani 1 1 d U A . C10 C -0.0695(8) 0.0057(4) 0.7548(8) 0.017(2) Uani 1 1 d U . . C11 C 0.0494(9) -0.0090(4) 0.7428(9) 0.021(2) Uani 1 1 d U A . C12 C 0.0822(8) 0.0885(4) 0.6939(8) 0.016(2) Uani 1 1 d U A . C13 C -0.0393(9) 0.0933(4) 0.7075(8) 0.019(2) Uani 1 1 d U . . C14 C -0.1458(9) 0.0337(4) 0.5855(8) 0.020(3) Uani 1 1 d U . . H14C H -0.0682 0.0251 0.5649 0.030 Uiso 1 1 calc R A . H14B H -0.1815 0.0611 0.5452 0.030 Uiso 1 1 calc R . . H14A H -0.1991 0.0050 0.5776 0.030 Uiso 1 1 calc R . . C15 C -0.2491(9) 0.0622(4) 0.7212(9) 0.030(3) Uani 1 1 d U . . H15C H -0.2427 0.0730 0.7894 0.045 Uiso 1 1 calc R A . H15B H -0.3003 0.0329 0.7121 0.045 Uiso 1 1 calc R . . H15A H -0.2841 0.0889 0.6786 0.045 Uiso 1 1 calc R . . C16 C -0.1415(9) -0.0853(4) 0.9544(9) 0.023(2) Uani 1 1 d U A . C17 C -0.0550(12) -0.1146(5) 1.0245(11) 0.054(4) Uani 1 1 d U . . H17C H 0.0052 -0.0923 1.0583 0.081 Uiso 1 1 calc R A . H17B H -0.0152 -0.1395 0.9882 0.081 Uiso 1 1 calc R . . H17A H -0.0986 -0.1311 1.0725 0.081 Uiso 1 1 calc R . . C18 C -0.2348(12) -0.1210(5) 0.9080(11) 0.057(4) Uani 1 1 d U . . H18C H -0.2763 -0.1362 0.9588 0.086 Uiso 1 1 calc R A . H18B H -0.1960 -0.1468 0.8733 0.086 Uiso 1 1 calc R . . H18A H -0.2928 -0.1032 0.8617 0.086 Uiso 1 1 calc R . . C19 C -0.2001(12) -0.0489(5) 1.0125(11) 0.053(4) Uani 1 1 d U . . H19C H -0.1399 -0.0261 1.0446 0.080 Uiso 1 1 calc R A . H19B H -0.2394 -0.0663 1.0622 0.080 Uiso 1 1 calc R . . H19A H -0.2600 -0.0303 0.9695 0.080 Uiso 1 1 calc R . . C20 C -0.0459(9) 0.2340(4) 0.7639(9) 0.026(3) Uani 1 1 d U . . C21 C 0.0383(11) 0.2501(5) 0.8565(10) 0.049(4) Uani 1 1 d U . . H21C H 0.0169 0.2835 0.8754 0.073 Uiso 1 1 calc R . . H21B H 0.1214 0.2498 0.8424 0.073 Uiso 1 1 calc R . . H21A H 0.0296 0.2271 0.9100 0.073 Uiso 1 1 calc R . . C22 C -0.0338(11) 0.2700(5) 0.6822(10) 0.047(4) Uani 1 1 d U . . H22C H -0.0868 0.2600 0.6237 0.070 Uiso 1 1 calc R . . H22B H 0.0493 0.2703 0.6679 0.070 Uiso 1 1 calc R . . H22A H -0.0560 0.3032 0.7019 0.070 Uiso 1 1 calc R . . C23 C -0.1749(10) 0.2348(4) 0.7871(10) 0.035(3) Uani 1 1 d U . . H23C H -0.2291 0.2260 0.7283 0.053 Uiso 1 1 calc R . . H23B H -0.1945 0.2680 0.8088 0.053 Uiso 1 1 calc R . . H23A H -0.1839 0.2108 0.8389 0.053 Uiso 1 1 calc R . . C24 C 0.2444(8) -0.1063(4) 0.6681(8) 0.016(2) Uani 1 1 d U . . C25 C 0.3535(9) -0.1217(4) 0.6413(9) 0.025(2) Uani 1 1 d U A . H25A H 0.4258 -0.1115 0.6792 0.030 Uiso 1 1 calc R . . C26 C 0.3588(10) -0.1511(4) 0.5620(9) 0.029(3) Uani 1 1 d U . . H26A H 0.4342 -0.1612 0.5449 0.035 Uiso 1 1 calc R A . C27 C 0.2531(9) -0.1664(4) 0.5052(9) 0.029(3) Uani 1 1 d U A . H27A H 0.2558 -0.1865 0.4490 0.035 Uiso 1 1 calc R . . C28 C 0.1453(10) -0.1516(4) 0.5329(9) 0.028(3) Uani 1 1 d U . . H28A H 0.0727 -0.1618 0.4957 0.034 Uiso 1 1 calc R A . C29 C 0.1413(9) -0.1222(4) 0.6142(9) 0.022(2) Uani 1 1 d U A . H29A H 0.0660 -0.1128 0.6329 0.026 Uiso 1 1 calc R . . C30 C 0.3069(9) -0.0990(4) 0.8799(9) 0.020(2) Uani 1 1 d U . . C31 C 0.2971(9) -0.1507(4) 0.8826(9) 0.026(3) Uani 1 1 d U A . H31A H 0.2702 -0.1686 0.8248 0.031 Uiso 1 1 calc R . . C32 C 0.3267(9) -0.1750(5) 0.9693(10) 0.032(3) Uani 1 1 d U . . H32A H 0.3187 -0.2100 0.9714 0.038 Uiso 1 1 calc R A . C33 C 0.3680(9) -0.1497(5) 1.0536(10) 0.033(3) Uani 1 1 d U A . H33A H 0.3877 -0.1669 1.1134 0.039 Uiso 1 1 calc R . . C34 C 0.3800(9) -0.1001(5) 1.0500(10) 0.032(3) Uani 1 1 d U . . H34A H 0.4099 -0.0825 1.1077 0.038 Uiso 1 1 calc R A . C35 C 0.3501(9) -0.0747(4) 0.9649(9) 0.023(2) Uani 1 1 d U A . H35A H 0.3591 -0.0398 0.9643 0.028 Uiso 1 1 calc R . . C36 C 0.3564(9) 0.1836(4) 0.6670(10) 0.029(2) Uani 1 1 d U . . C37 C 0.3924(10) 0.2062(4) 0.7568(10) 0.034(3) Uani 1 1 d U . . H37A H 0.3844 0.1879 0.8143 0.040 Uiso 1 1 calc R . . C38 C 0.4386(10) 0.2532(5) 0.7676(11) 0.041(3) Uani 1 1 d U . . H38A H 0.4599 0.2668 0.8308 0.049 Uiso 1 1 calc R . . C39 C 0.4532(11) 0.2797(5) 0.6867(11) 0.049(3) Uani 1 1 d U . . H39A H 0.4868 0.3120 0.6930 0.059 Uiso 1 1 calc R . . C40 C 0.4200(11) 0.2603(5) 0.5973(12) 0.049(3) Uani 1 1 d U . . H40A H 0.4282 0.2795 0.5408 0.059 Uiso 1 1 calc R . . C41 C 0.3742(10) 0.2130(5) 0.5871(10) 0.038(3) Uani 1 1 d U . . H41A H 0.3542 0.1999 0.5232 0.046 Uiso 1 1 calc R . . C42 C 0.2986(9) 0.1065(4) 0.5536(9) 0.025(2) Uani 1 1 d U . . C43 C 0.2149(10) 0.1191(4) 0.4755(9) 0.027(3) Uani 1 1 d U . . H43A H 0.1477 0.1381 0.4885 0.033 Uiso 1 1 calc R . . C44 C 0.2225(10) 0.1059(4) 0.3795(9) 0.032(3) Uani 1 1 d U . . H44A H 0.1633 0.1167 0.3287 0.039 Uiso 1 1 calc R . . C45 C 0.3163(10) 0.0772(4) 0.3585(9) 0.030(3) Uani 1 1 d U . . H45A H 0.3229 0.0680 0.2930 0.036 Uiso 1 1 calc R . . C46 C 0.4004(10) 0.0618(4) 0.4330(9) 0.030(3) Uani 1 1 d U . . H46A H 0.4652 0.0417 0.4188 0.036 Uiso 1 1 calc R . . C47 C 0.3919(9) 0.0754(4) 0.5285(9) 0.025(2) Uani 1 1 d U . . H47A H 0.4502 0.0635 0.5790 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0149(5) 0.0166(6) 0.0194(6) -0.0018(5) 0.0031(4) -0.0021(4) S1 0.0182(13) 0.0133(16) 0.0164(18) 0.0014(13) 0.0019(13) -0.0016(12) P1 0.0125(14) 0.0206(18) 0.0169(19) -0.0041(15) 0.0005(13) 0.0006(12) Cl1 0.0200(13) 0.0279(19) 0.039(2) 0.0021(16) 0.0026(14) -0.0004(13) C1 0.019(4) 0.019(5) 0.021(5) -0.001(4) -0.001(4) 0.000(4) B1 0.022(4) 0.024(5) 0.023(5) 0.001(4) 0.000(4) 0.001(4) Cl2 0.0257(14) 0.0270(18) 0.031(2) 0.0025(16) -0.0048(14) -0.0073(13) C2 0.021(4) 0.016(4) 0.018(4) 0.000(4) 0.002(4) 0.001(4) C3 0.017(4) 0.011(4) 0.019(5) 0.001(4) 0.000(4) 0.003(4) C4 0.015(4) 0.013(4) 0.017(5) -0.001(4) 0.003(4) 0.003(4) C5 0.028(4) 0.016(4) 0.021(5) 0.003(4) 0.002(4) -0.002(4) C6 0.026(4) 0.018(5) 0.019(5) 0.000(4) -0.001(4) -0.006(4) C7 0.026(4) 0.018(4) 0.014(4) 0.002(4) 0.008(4) -0.002(4) C8 0.020(4) 0.018(4) 0.012(5) 0.004(4) 0.004(4) 0.003(4) C9 0.020(4) 0.021(4) 0.017(5) 0.004(4) 0.003(4) -0.002(4) C10 0.018(4) 0.018(4) 0.013(4) 0.001(4) 0.000(4) 0.000(4) C11 0.025(4) 0.013(4) 0.024(5) 0.000(4) 0.000(4) 0.006(4) C12 0.025(4) 0.008(4) 0.016(5) 0.001(4) 0.005(4) -0.001(4) C13 0.021(4) 0.022(4) 0.014(4) 0.005(4) 0.002(4) -0.001(4) C14 0.025(5) 0.016(5) 0.016(6) -0.001(5) -0.006(5) -0.004(4) C15 0.030(5) 0.031(6) 0.027(6) 0.010(5) -0.001(5) -0.006(5) C16 0.028(4) 0.024(5) 0.019(5) 0.006(4) 0.012(4) 0.003(4) C17 0.059(6) 0.067(7) 0.039(7) 0.019(6) 0.016(6) 0.010(6) C18 0.066(7) 0.055(7) 0.053(7) 0.005(6) 0.017(6) -0.024(6) C19 0.070(7) 0.047(7) 0.046(7) 0.005(6) 0.024(6) 0.009(6) C20 0.029(4) 0.021(5) 0.029(5) 0.001(4) 0.004(4) 0.000(4) C21 0.053(6) 0.042(7) 0.051(7) -0.020(6) 0.005(6) 0.004(6) C22 0.045(6) 0.048(7) 0.051(7) 0.018(6) 0.022(6) 0.007(5) C23 0.043(6) 0.025(6) 0.041(7) -0.005(5) 0.015(5) 0.007(5) C24 0.016(4) 0.015(5) 0.018(5) 0.003(4) 0.006(4) 0.001(4) C25 0.026(4) 0.026(5) 0.022(5) -0.003(4) 0.004(4) 0.004(4) C26 0.033(4) 0.030(5) 0.025(5) -0.005(4) 0.008(4) 0.007(4) C27 0.038(5) 0.028(5) 0.021(5) -0.004(4) 0.001(4) 0.007(4) C28 0.035(4) 0.025(5) 0.025(5) -0.002(4) 0.000(4) -0.003(4) C29 0.028(4) 0.018(5) 0.021(5) 0.001(4) 0.006(4) 0.002(4) C30 0.019(4) 0.022(5) 0.020(5) 0.000(4) 0.002(4) 0.007(4) C31 0.025(4) 0.024(5) 0.027(5) 0.003(4) 0.000(4) 0.000(4) C32 0.027(4) 0.032(5) 0.035(5) 0.007(5) 0.004(4) 0.004(4) C33 0.027(4) 0.038(5) 0.032(5) 0.009(5) 0.004(4) 0.003(4) C34 0.025(4) 0.042(5) 0.028(5) -0.001(5) -0.002(4) -0.001(4) C35 0.022(4) 0.025(5) 0.024(5) -0.001(4) 0.004(4) 0.002(4) C36 0.027(4) 0.028(5) 0.033(5) 0.000(4) 0.007(4) -0.008(4) C37 0.037(5) 0.028(5) 0.035(5) -0.004(5) 0.002(4) -0.010(4) C38 0.043(5) 0.035(5) 0.044(6) -0.009(5) 0.001(5) -0.019(4) C39 0.051(5) 0.042(5) 0.054(6) -0.005(5) 0.006(5) -0.014(5) C40 0.050(5) 0.045(5) 0.053(6) 0.005(5) 0.011(5) -0.013(5) C41 0.037(5) 0.036(5) 0.042(5) 0.003(5) 0.009(5) -0.008(4) C42 0.022(4) 0.026(4) 0.027(5) 0.002(4) 0.006(4) -0.002(4) C43 0.024(4) 0.031(5) 0.027(5) 0.000(5) 0.006(4) -0.002(4) C44 0.034(5) 0.037(5) 0.025(5) -0.003(5) -0.002(5) -0.006(4) C45 0.032(4) 0.036(5) 0.022(5) -0.005(5) 0.012(4) -0.009(4) C46 0.028(4) 0.033(5) 0.032(5) -0.006(5) 0.010(4) -0.005(4) C47 0.025(4) 0.022(5) 0.028(5) -0.005(4) 0.006(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.219(3) . ? Pd1 Cl1 2.290(3) . ? Pd1 S1 2.320(3) . ? Pd1 Cl2 2.352(3) . ? S1 C11 1.770(12) . ? S1 C12 1.784(10) . ? P1 C30 1.798(12) . ? P1 C24 1.809(11) . ? P1 C4 1.819(9) . ? C1 C2 1.383(15) . ? C1 C10 1.400(15) . ? C1 H1A 0.9500 . ? B1 C42 1.562(18) . ? B1 C36 1.626(17) . ? B1 C5 1.626(16) . ? B1 Cl2 1.977(14) . ? C2 C3 1.414(13) . ? C2 C16 1.528(15) . ? C3 C4 1.394(14) . ? C3 H3A 0.9500 . ? C4 C11 1.349(14) . ? C5 C6 1.396(15) . ? C5 C12 1.433(14) . ? C6 C7 1.432(14) . ? C6 H6A 0.9500 . ? C7 C8 1.390(14) . ? C7 C20 1.531(15) . ? C8 C13 1.388(14) . ? C8 H8A 0.9500 . ? C9 C15 1.494(14) . ? C9 C13 1.528(14) . ? C9 C10 1.545(15) . ? C9 C14 1.573(15) . ? C10 C11 1.426(14) . ? C12 C13 1.410(13) . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 C19 1.476(16) . ? C16 C18 1.508(16) . ? C16 C17 1.508(16) . ? C17 H17C 0.9800 . ? C17 H17B 0.9800 . ? C17 H17A 0.9800 . ? C18 H18C 0.9800 . ? C18 H18B 0.9800 . ? C18 H18A 0.9800 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C19 H19A 0.9800 . ? C20 C22 1.510(17) . ? C20 C23 1.526(15) . ? C20 C21 1.553(17) . ? C21 H21C 0.9800 . ? C21 H21B 0.9800 . ? C21 H21A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C23 H23C 0.9800 . ? C23 H23B 0.9800 . ? C23 H23A 0.9800 . ? C24 C29 1.365(14) . ? C24 C25 1.390(14) . ? C25 C26 1.361(16) . ? C25 H25A 0.9500 . ? C26 C27 1.402(15) . ? C26 H26A 0.9500 . ? C27 C28 1.377(15) . ? C27 H27A 0.9500 . ? C28 C29 1.381(16) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.379(15) . ? C30 C31 1.402(15) . ? C31 C32 1.370(16) . ? C31 H31A 0.9500 . ? C32 C33 1.380(17) . ? C32 H32A 0.9500 . ? C33 C34 1.349(16) . ? C33 H33A 0.9500 . ? C34 C35 1.364(16) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C41 1.393(17) . ? C36 C37 1.395(16) . ? C37 C38 1.372(16) . ? C37 H37A 0.9500 . ? C38 C39 1.354(18) . ? C38 H38A 0.9500 . ? C39 C40 1.350(18) . ? C39 H39A 0.9500 . ? C40 C41 1.381(17) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C43 1.382(15) . ? C42 C47 1.422(15) . ? C43 C44 1.385(17) . ? C43 H43A 0.9500 . ? C44 C45 1.371(16) . ? C44 H44A 0.9500 . ? C45 C46 1.370(16) . ? C45 H45A 0.9500 . ? C46 C47 1.383(16) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 Cl1 90.21(10) . . ? P1 Pd1 S1 85.14(10) . . ? Cl1 Pd1 S1 171.79(11) . . ? P1 Pd1 Cl2 170.33(12) . . ? Cl1 Pd1 Cl2 89.78(10) . . ? S1 Pd1 Cl2 95.94(10) . . ? C11 S1 C12 101.7(5) . . ? C11 S1 Pd1 98.6(4) . . ? C12 S1 Pd1 115.4(3) . . ? C30 P1 C24 108.4(5) . . ? C30 P1 C4 105.4(5) . . ? C24 P1 C4 107.6(5) . . ? C30 P1 Pd1 117.5(4) . . ? C24 P1 Pd1 115.1(4) . . ? C4 P1 Pd1 101.7(3) . . ? C2 C1 C10 123.8(10) . . ? C2 C1 H1A 118.1 . . ? C10 C1 H1A 118.1 . . ? C42 B1 C36 111.8(10) . . ? C42 B1 C5 113.6(10) . . ? C36 B1 C5 111.8(10) . . ? C42 B1 Cl2 109.3(8) . . ? C36 B1 Cl2 101.9(8) . . ? C5 B1 Cl2 107.8(8) . . ? B1 Cl2 Pd1 107.7(4) . . ? C1 C2 C3 116.2(10) . . ? C1 C2 C16 121.8(9) . . ? C3 C2 C16 121.9(10) . . ? C4 C3 C2 120.1(10) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C11 C4 C3 122.7(9) . . ? C11 C4 P1 116.0(8) . . ? C3 C4 P1 120.8(8) . . ? C6 C5 C12 115.4(9) . . ? C6 C5 B1 118.3(9) . . ? C12 C5 B1 126.1(10) . . ? C5 C6 C7 123.9(10) . . ? C5 C6 H6A 118.1 . . ? C7 C6 H6A 118.1 . . ? C8 C7 C6 116.2(10) . . ? C8 C7 C20 126.0(9) . . ? C6 C7 C20 117.8(9) . . ? C13 C8 C7 123.9(9) . . ? C13 C8 H8A 118.1 . . ? C7 C8 H8A 118.1 . . ? C15 C9 C13 114.1(9) . . ? C15 C9 C10 112.7(9) . . ? C13 C9 C10 108.3(8) . . ? C15 C9 C14 106.0(9) . . ? C13 C9 C14 108.7(9) . . ? C10 C9 C14 106.8(9) . . ? C1 C10 C11 117.6(10) . . ? C1 C10 C9 122.8(9) . . ? C11 C10 C9 119.6(10) . . ? C4 C11 C10 118.8(10) . . ? C4 C11 S1 121.4(8) . . ? C10 C11 S1 119.7(8) . . ? C13 C12 C5 122.7(9) . . ? C13 C12 S1 117.3(8) . . ? C5 C12 S1 119.8(7) . . ? C8 C13 C12 117.3(9) . . ? C8 C13 C9 119.8(9) . . ? C12 C13 C9 122.9(9) . . ? C9 C14 H14C 109.5 . . ? C9 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C9 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C9 C15 H15C 109.5 . . ? C9 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C9 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C19 C16 C18 108.7(10) . . ? C19 C16 C17 107.4(11) . . ? C18 C16 C17 107.2(11) . . ? C19 C16 C2 111.6(10) . . ? C18 C16 C2 110.5(10) . . ? C17 C16 C2 111.2(9) . . ? C16 C17 H17C 109.5 . . ? C16 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C16 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C16 C18 H18C 109.5 . . ? C16 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? C16 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? C16 C19 H19C 109.5 . . ? C16 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C16 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? C22 C20 C23 109.0(9) . . ? C22 C20 C7 110.4(10) . . ? C23 C20 C7 111.7(9) . . ? C22 C20 C21 109.3(10) . . ? C23 C20 C21 108.8(10) . . ? C7 C20 C21 107.7(9) . . ? C20 C21 H21C 109.5 . . ? C20 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? C20 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? C20 C22 H22C 109.5 . . ? C20 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C20 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C20 C23 H23C 109.5 . . ? C20 C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? C20 C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? C29 C24 C25 118.8(11) . . ? C29 C24 P1 124.0(8) . . ? C25 C24 P1 117.3(8) . . ? C26 C25 C24 121.2(11) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C27 120.2(10) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 118.3(11) . . ? C28 C27 H27A 120.9 . . ? C26 C27 H27A 120.9 . . ? C27 C28 C29 120.9(11) . . ? C27 C28 H28A 119.5 . . ? C29 C28 H28A 119.5 . . ? C24 C29 C28 120.6(10) . . ? C24 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C35 C30 C31 118.2(11) . . ? C35 C30 P1 121.0(9) . . ? C31 C30 P1 120.4(9) . . ? C32 C31 C30 119.4(12) . . ? C32 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C31 C32 C33 121.1(12) . . ? C31 C32 H32A 119.5 . . ? C33 C32 H32A 119.5 . . ? C34 C33 C32 119.2(12) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C33 C34 C35 121.0(12) . . ? C33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C34 C35 C30 121.0(11) . . ? C34 C35 H35A 119.5 . . ? C30 C35 H35A 119.5 . . ? C41 C36 C37 113.6(11) . . ? C41 C36 B1 123.3(12) . . ? C37 C36 B1 123.0(11) . . ? C38 C37 C36 124.4(13) . . ? C38 C37 H37A 117.8 . . ? C36 C37 H37A 117.8 . . ? C39 C38 C37 119.0(14) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C40 C39 C38 119.9(14) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 120.7(15) . . ? C39 C40 H40A 119.7 . . ? C41 C40 H40A 119.7 . . ? C40 C41 C36 122.4(14) . . ? C40 C41 H41A 118.8 . . ? C36 C41 H41A 118.8 . . ? C43 C42 C47 114.1(11) . . ? C43 C42 B1 120.9(10) . . ? C47 C42 B1 124.8(10) . . ? C42 C43 C44 124.3(11) . . ? C42 C43 H43A 117.8 . . ? C44 C43 H43A 117.8 . . ? C45 C44 C43 119.4(12) . . ? C45 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 . . ? C46 C45 C44 119.4(12) . . ? C46 C45 H45A 120.3 . . ? C44 C45 H45A 120.3 . . ? C45 C46 C47 120.7(11) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C46 C47 C42 122.0(11) . . ? C46 C47 H47A 119.0 . . ? C42 C47 H47A 119.0 . . ? 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 Pd1 S1 C11 33.9(4) . . . . ? Cl2 Pd1 S1 C11 -136.4(4) . . . . ? P1 Pd1 S1 C12 141.4(4) . . . . ? Cl2 Pd1 S1 C12 -29.0(4) . . . . ? Cl1 Pd1 P1 C30 37.8(4) . . . . ? S1 Pd1 P1 C30 -148.9(4) . . . . ? Cl1 Pd1 P1 C24 -91.7(4) . . . . ? S1 Pd1 P1 C24 81.5(4) . . . . ? Cl1 Pd1 P1 C4 152.4(4) . . . . ? S1 Pd1 P1 C4 -34.4(4) . . . . ? C42 B1 Cl2 Pd1 -60.4(8) . . . . ? C36 B1 Cl2 Pd1 -178.8(6) . . . . ? C5 B1 Cl2 Pd1 63.5(8) . . . . ? Cl1 Pd1 Cl2 B1 155.5(4) . . . . ? S1 Pd1 Cl2 B1 -18.6(4) . . . . ? C10 C1 C2 C3 -6.4(16) . . . . ? C10 C1 C2 C16 175.6(10) . . . . ? C1 C2 C3 C4 7.5(15) . . . . ? C16 C2 C3 C4 -174.5(10) . . . . ? C2 C3 C4 C11 -1.2(17) . . . . ? C2 C3 C4 P1 170.1(8) . . . . ? C30 P1 C4 C11 151.8(9) . . . . ? C24 P1 C4 C11 -92.7(10) . . . . ? Pd1 P1 C4 C11 28.7(10) . . . . ? C30 P1 C4 C3 -20.0(10) . . . . ? C24 P1 C4 C3 95.5(10) . . . . ? Pd1 P1 C4 C3 -143.2(8) . . . . ? C42 B1 C5 C6 -120.8(12) . . . . ? C36 B1 C5 C6 6.8(15) . . . . ? Cl2 B1 C5 C6 117.9(10) . . . . ? C42 B1 C5 C12 55.6(16) . . . . ? C36 B1 C5 C12 -176.8(11) . . . . ? Cl2 B1 C5 C12 -65.7(14) . . . . ? C12 C5 C6 C7 0.1(17) . . . . ? B1 C5 C6 C7 176.9(11) . . . . ? C5 C6 C7 C8 -4.8(17) . . . . ? C5 C6 C7 C20 176.0(11) . . . . ? C6 C7 C8 C13 2.7(17) . . . . ? C20 C7 C8 C13 -178.2(11) . . . . ? C2 C1 C10 C11 -0.9(17) . . . . ? C2 C1 C10 C9 -179.4(10) . . . . ? C15 C9 C10 C1 1.8(15) . . . . ? C13 C9 C10 C1 129.0(11) . . . . ? C14 C9 C10 C1 -114.2(11) . . . . ? C15 C9 C10 C11 -176.7(10) . . . . ? C13 C9 C10 C11 -49.6(14) . . . . ? C14 C9 C10 C11 67.3(12) . . . . ? C3 C4 C11 C10 -6.4(17) . . . . ? P1 C4 C11 C10 -178.1(8) . . . . ? C3 C4 C11 S1 172.1(9) . . . . ? P1 C4 C11 S1 0.4(14) . . . . ? C1 C10 C11 C4 7.3(16) . . . . ? C9 C10 C11 C4 -174.1(10) . . . . ? C1 C10 C11 S1 -171.2(8) . . . . ? C9 C10 C11 S1 7.4(15) . . . . ? C12 S1 C11 C4 -146.0(10) . . . . ? Pd1 S1 C11 C4 -27.6(10) . . . . ? C12 S1 C11 C10 32.5(10) . . . . ? Pd1 S1 C11 C10 150.9(9) . . . . ? C6 C5 C12 C13 7.1(17) . . . . ? B1 C5 C12 C13 -169.4(11) . . . . ? C6 C5 C12 S1 -178.1(8) . . . . ? B1 C5 C12 S1 5.4(16) . . . . ? C11 S1 C12 C13 -33.6(10) . . . . ? Pd1 S1 C12 C13 -139.2(8) . . . . ? C11 S1 C12 C5 151.3(9) . . . . ? Pd1 S1 C12 C5 45.8(10) . . . . ? C7 C8 C13 C12 3.9(17) . . . . ? C7 C8 C13 C9 -175.0(11) . . . . ? C5 C12 C13 C8 -9.1(17) . . . . ? S1 C12 C13 C8 176.0(8) . . . . ? C5 C12 C13 C9 169.8(11) . . . . ? S1 C12 C13 C9 -5.1(15) . . . . ? C15 C9 C13 C8 -5.7(15) . . . . ? C10 C9 C13 C8 -132.0(10) . . . . ? C14 C9 C13 C8 112.3(11) . . . . ? C15 C9 C13 C12 175.4(10) . . . . ? C10 C9 C13 C12 49.1(14) . . . . ? C14 C9 C13 C12 -66.6(13) . . . . ? C1 C2 C16 C19 -41.1(15) . . . . ? C3 C2 C16 C19 141.0(11) . . . . ? C1 C2 C16 C18 80.1(14) . . . . ? C3 C2 C16 C18 -97.8(13) . . . . ? C1 C2 C16 C17 -161.0(11) . . . . ? C3 C2 C16 C17 21.1(15) . . . . ? C8 C7 C20 C22 -121.3(12) . . . . ? C6 C7 C20 C22 57.7(13) . . . . ? C8 C7 C20 C23 0.1(17) . . . . ? C6 C7 C20 C23 179.2(10) . . . . ? C8 C7 C20 C21 119.5(12) . . . . ? C6 C7 C20 C21 -61.5(13) . . . . ? C30 P1 C24 C29 113.4(10) . . . . ? C4 P1 C24 C29 -0.2(11) . . . . ? Pd1 P1 C24 C29 -112.8(9) . . . . ? C30 P1 C24 C25 -67.8(10) . . . . ? C4 P1 C24 C25 178.6(9) . . . . ? Pd1 P1 C24 C25 66.1(9) . . . . ? C29 C24 C25 C26 1.4(17) . . . . ? P1 C24 C25 C26 -177.5(9) . . . . ? C24 C25 C26 C27 0.1(18) . . . . ? C25 C26 C27 C28 -1.0(18) . . . . ? C26 C27 C28 C29 0.4(18) . . . . ? C25 C24 C29 C28 -2.0(17) . . . . ? P1 C24 C29 C28 176.9(9) . . . . ? C27 C28 C29 C24 1.1(18) . . . . ? C24 P1 C30 C35 162.5(8) . . . . ? C4 P1 C30 C35 -82.5(9) . . . . ? Pd1 P1 C30 C35 29.9(10) . . . . ? C24 P1 C30 C31 -24.7(10) . . . . ? C4 P1 C30 C31 90.3(9) . . . . ? Pd1 P1 C30 C31 -157.3(7) . . . . ? C35 C30 C31 C32 2.1(15) . . . . ? P1 C30 C31 C32 -170.9(8) . . . . ? C30 C31 C32 C33 -1.2(16) . . . . ? C31 C32 C33 C34 -0.5(17) . . . . ? C32 C33 C34 C35 1.2(17) . . . . ? C33 C34 C35 C30 -0.2(17) . . . . ? C31 C30 C35 C34 -1.4(15) . . . . ? P1 C30 C35 C34 171.6(8) . . . . ? C42 B1 C36 C41 20.7(15) . . . . ? C5 B1 C36 C41 -107.9(13) . . . . ? Cl2 B1 C36 C41 137.3(10) . . . . ? C42 B1 C36 C37 -162.4(10) . . . . ? C5 B1 C36 C37 69.0(14) . . . . ? Cl2 B1 C36 C37 -45.8(13) . . . . ? C41 C36 C37 C38 1.5(17) . . . . ? B1 C36 C37 C38 -175.7(11) . . . . ? C36 C37 C38 C39 -1.4(19) . . . . ? C37 C38 C39 C40 1(2) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 C36 2(2) . . . . ? C37 C36 C41 C40 -1.8(17) . . . . ? B1 C36 C41 C40 175.3(11) . . . . ? C36 B1 C42 C43 -82.8(13) . . . . ? C5 B1 C42 C43 44.8(15) . . . . ? Cl2 B1 C42 C43 165.3(9) . . . . ? C36 B1 C42 C47 91.2(14) . . . . ? C5 B1 C42 C47 -141.2(11) . . . . ? Cl2 B1 C42 C47 -20.8(14) . . . . ? C47 C42 C43 C44 -3.9(17) . . . . ? B1 C42 C43 C44 170.7(11) . . . . ? C42 C43 C44 C45 2.1(19) . . . . ? C43 C44 C45 C46 0.3(18) . . . . ? C44 C45 C46 C47 -0.5(18) . . . . ? C45 C46 C47 C42 -1.7(18) . . . . ? C43 C42 C47 C46 3.7(16) . . . . ? B1 C42 C47 C46 -170.6(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.795 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.221 # start Validation Reply Form _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: There was no appreciable diffraction past 45degrees in 2-theta, so this data was "omitted" from least squares calculations. The actual diffraction experiment extended to 55degrees in 2-theta. ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.50 Deg. RESPONSE: After many attempts to grow larger and better quality crystals, this was the best result. The sample did not diffract beyond 45degrees in 2-theta, and background "noise" beyond this level contributed to higher R factors and did nothing to improve the overall structure. ; _vrf_PLAT094_I ; PROBLEM: Ratio of maximum/minimum residual density... 5.35 RESPONSE: There is a "ghost peak" associated with a minor co-crystal. Twinning was modelled for this compound, with BASF = 1.2%. ; # Attachment '- 2B_2CH2Cl2 brad01 PdCl2(TXPB) NEW.cif' data_brad01 _database_code_depnum_ccdc_archive 'CCDC 849794' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (PdCl2(TXPB)) _chemical_melting_point ? _chemical_formula_moiety 'C47 H48 B1 Cl2 P1 Pd1 S1, 2(C H2 Cl2)' _chemical_formula_sum 'C49 H52 B Cl6 P Pd S' _chemical_formula_weight 1033.85 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' B B 0.0013 0.0007 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.3801(14) _cell_length_b 8.9678(6) _cell_length_c 25.2512(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4841.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.439 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.316 _exptl_crystal_size_mid 0.284 _exptl_crystal_size_min 0.118 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7785 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details SADABS _exptl_special_details ; A crystal of suitable size was selected and mounted on a goniometer head, then placed in the cold stream of the diffractometer. Data were collected with Mo K(alpha) radiation from a Siemens rotating anode, with a SMART 1K detector, at -100C. Omega and phi scans were used to ensure complete coverage. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72714 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 30.67 _reflns_number_total 14333 _reflns_number_gt 12392 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; TITL pdcl2_0m in P n a 21 CELL 0.71073 21.3801 8.9678 25.2512 90.000 90.000 90.000 ZERR 4.00 0.0014 0.0006 0.0017 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SFAC C H B CL P PD S UNIT 196 208 4 24 4 4 4 MERG 2 OMIT -3.00 180.00 EXYZ C20A C20B EADP C20A C20B EADP C21A C21B C22A C22B C23A C23B EXYZ CL3A CL3B EXYZ CL4A CL4B EADP CL3A CL3B EADP CL4A CL4B EADP C48A C48B EXYZ CL5A CL5B EXYZ CL6A CL6B EADP CL5A CL5B EADP CL6A CL6B EADP C49A C49B DFIX 1.77 0.005 C48B CL3B DFIX 1.77 0.005 C48A CL4A DFIX 1.77 0.005 C48A CL3A DFIX 1.77 0.005 C49B CL5B DFIX 1.77 0.005 C49A CL5A DFIX 1.77 0.005 C49A CL6A SADI 0.005 C20B C21B C20B C22B C20B C23B BIND C9 S1 BIND Pd1 B1 SIZE 0.12 0.28 0.32 ACTA BOND $H CONF LIST 4 L.S. 4 TEMP 173.00 WGHT 0.063300 1.356000 FVAR 0.25604 0.63703 0.46260 0.43273 PART 1 SAME 0.005 C20B C21B C22B C23B C20A 1 0.624526 0.361835 -0.141912 21.00000 0.03636 0.06609 = 0.02584 0.00858 0.00034 -0.01169 C21A 1 0.692553 0.407032 -0.149328 21.00000 0.06436 0.09320 = 0.03275 0.01386 0.00623 -0.02322 AFIX 33 H21A 2 0.700827 0.422078 -0.186311 21.00000 -1.50000 H21B 2 0.719283 0.329657 -0.135984 21.00000 -1.50000 H21C 2 0.700474 0.497878 -0.130369 21.00000 -1.50000 AFIX 0 C22A 1 0.585342 0.497791 -0.160352 21.00000 0.06436 0.09320 = 0.03275 0.01386 0.00623 -0.02322 AFIX 33 H22A 2 0.541636 0.475482 -0.156724 21.00000 -1.50000 H22B 2 0.594583 0.519150 -0.196775 21.00000 -1.50000 H22C 2 0.595551 0.582897 -0.138973 21.00000 -1.50000 AFIX 0 C23A 1 0.605322 0.237236 -0.178672 21.00000 0.06436 0.09320 = 0.03275 0.01386 0.00623 -0.02322 AFIX 33 H23A 2 0.562869 0.209106 -0.171356 21.00000 -1.50000 H23B 2 0.632265 0.152930 -0.173330 21.00000 -1.50000 H23C 2 0.608620 0.270432 -0.214708 21.00000 -1.50000 AFIX 0 PART 2 C20B 1 0.624526 0.361835 -0.141912 -21.00000 0.03636 0.06609 = 0.02584 0.00858 0.00034 -0.01169 C21B 1 0.666490 0.495910 -0.149941 -21.00000 0.06436 0.09320 = 0.03275 0.01386 0.00623 -0.02322 AFIX 33 H21D 2 0.676591 0.505350 -0.186833 -21.00000 -1.50000 H21E 2 0.704256 0.483178 -0.129880 -21.00000 -1.50000 H21F 2 0.645235 0.584224 -0.138203 -21.00000 -1.50000 AFIX 0 C22B 1 0.571832 0.356756 -0.182040 -21.00000 0.06436 0.09320 = 0.03275 0.01386 0.00623 -0.02322 AFIX 33 H22D 2 0.547179 0.268714 -0.176385 -21.00000 -1.50000 H22E 2 0.589025 0.354897 -0.217154 -21.00000 -1.50000 H22F 2 0.545923 0.443441 -0.177992 -21.00000 -1.50000 AFIX 0 C23B 1 0.661956 0.218742 -0.153530 -21.00000 0.06436 0.09320 = 0.03275 0.01386 0.00623 -0.02322 AFIX 33 H23D 2 0.635983 0.133237 -0.147235 -21.00000 -1.50000 H23E 2 0.697883 0.214670 -0.130772 -21.00000 -1.50000 H23F 2 0.675326 0.219147 -0.189823 -21.00000 -1.50000 AFIX 0 PART 0 PD1 6 0.469713 0.137614 0.115064 11.00000 0.02098 0.02276 = 0.02712 -0.00023 0.00399 -0.00017 CL2 4 0.383964 0.018083 0.151409 11.00000 0.02580 0.03621 = 0.04488 0.00269 0.01069 -0.00411 S1 7 0.551310 0.278869 0.088711 11.00000 0.02271 0.02215 = 0.02618 0.00133 0.00138 -0.00070 CL1 4 0.410244 0.266175 0.048850 11.00000 0.02204 0.03144 = 0.03604 0.00103 0.00108 0.00385 P1 5 0.534567 0.032697 0.173119 11.00000 0.02611 0.02371 = 0.02295 0.00068 0.00335 -0.00238 C1 1 0.729810 0.155358 0.111002 11.00000 0.02249 0.03127 = 0.02840 0.00382 0.00260 -0.00220 AFIX 43 H1A 2 0.769150 0.183188 0.098784 11.00000 -1.20000 AFIX 0 C25 1 0.477070 0.087392 0.269566 11.00000 0.05348 0.06027 = 0.04765 -0.01928 0.01647 -0.01987 AFIX 43 H25A 2 0.442921 0.037985 0.254987 11.00000 -1.20000 AFIX 0 C17 1 0.814600 -0.115650 0.110469 11.00000 0.04427 0.04242 = 0.04674 0.00330 0.00429 0.01197 AFIX 33 H17A 2 0.785457 -0.180930 0.093176 11.00000 -1.50000 H17B 2 0.851697 -0.170297 0.119530 11.00000 -1.50000 H17C 2 0.825303 -0.035187 0.087088 11.00000 -1.50000 AFIX 0 C15 1 0.747318 0.382700 0.032087 11.00000 0.02411 0.04631 = 0.04156 0.01789 -0.00339 -0.01159 AFIX 33 H15A 2 0.748424 0.464508 0.007585 11.00000 -1.50000 H15B 2 0.759294 0.292638 0.014212 11.00000 -1.50000 H15C 2 0.775835 0.401688 0.060669 11.00000 -1.50000 AFIX 0 C2 1 0.725530 0.034695 0.146178 11.00000 0.02811 0.03004 = 0.02874 0.00440 -0.00045 0.00135 C6 1 0.546337 0.285931 -0.071743 11.00000 0.02847 0.03533 = 0.03023 0.00321 -0.00089 -0.00447 AFIX 43 H6A 2 0.518164 0.269410 -0.099185 11.00000 -1.20000 AFIX 0 C29 1 0.581041 0.183851 0.262073 11.00000 0.04239 0.03753 = 0.03446 -0.00382 0.00246 -0.00865 AFIX 43 H29A 2 0.617390 0.198009 0.242478 11.00000 -1.20000 AFIX 0 C7 1 0.606837 0.334355 -0.084695 11.00000 0.02722 0.03512 = 0.02677 0.00475 0.00324 -0.00185 C10 1 0.677973 0.235465 0.093503 11.00000 0.02308 0.02635 = 0.02473 0.00521 -0.00308 -0.00242 C24 1 0.531135 0.109465 0.239449 11.00000 0.04093 0.02316 = 0.02936 -0.00167 0.00133 -0.00361 C18 1 0.831939 0.052195 0.188152 11.00000 0.03271 0.04704 = 0.04895 0.00191 -0.01209 -0.00287 AFIX 33 H18A 2 0.868880 -0.002938 0.197299 11.00000 -1.50000 H18B 2 0.813649 0.093271 0.219660 11.00000 -1.50000 H18C 2 0.842801 0.131521 0.164338 11.00000 -1.50000 AFIX 0 C36 1 0.412751 0.210720 -0.063415 11.00000 0.02071 0.03266 = 0.03263 0.00199 -0.00187 -0.00233 C37 1 0.394265 0.356723 -0.075881 11.00000 0.04062 0.03983 = 0.05857 0.00728 -0.01897 -0.00347 AFIX 43 H37A 2 0.405932 0.433611 -0.053227 11.00000 -1.20000 AFIX 0 C44 1 0.424486 -0.250377 0.011825 11.00000 0.05868 0.03107 = 0.03718 -0.00084 -0.00195 -0.01163 AFIX 43 H44A 2 0.390139 -0.310283 0.019446 11.00000 -1.20000 AFIX 0 C14 1 0.664898 0.513806 0.082599 11.00000 0.04144 0.03035 = 0.04413 0.00543 -0.00934 -0.01107 AFIX 33 H14A 2 0.666864 0.594502 0.057673 11.00000 -1.50000 H14B 2 0.694462 0.530862 0.110564 11.00000 -1.50000 H14C 2 0.623509 0.507936 0.097191 11.00000 -1.50000 AFIX 0 C16 1 0.784669 -0.052343 0.161179 11.00000 0.02477 0.03437 = 0.03501 0.00955 -0.00265 0.00262 C28 1 0.577881 0.237645 0.313370 11.00000 0.07060 0.04486 = 0.03505 -0.00884 -0.00658 -0.00761 AFIX 43 H28A 2 0.611781 0.288424 0.327770 11.00000 -1.20000 AFIX 0 C5 1 0.526057 0.261118 -0.019743 11.00000 0.02263 0.02212 = 0.02862 0.00193 -0.00147 -0.00084 C27 1 0.525233 0.216417 0.342842 11.00000 0.09711 0.05220 = 0.03109 -0.01631 0.00504 -0.00965 AFIX 43 H27A 2 0.523143 0.253182 0.377234 11.00000 -1.20000 AFIX 0 C9 1 0.680807 0.365535 0.054146 11.00000 0.02344 0.02991 = 0.03213 0.00870 -0.00541 -0.00638 C33 1 0.513158 -0.471036 0.194087 11.00000 0.04280 0.02376 = 0.05297 -0.00045 0.00555 0.00237 AFIX 43 H33A 2 0.507856 -0.573219 0.198485 11.00000 -1.20000 AFIX 0 C45 1 0.482390 -0.314642 0.003192 11.00000 0.07925 0.02418 = 0.03860 -0.00382 -0.01197 0.00066 AFIX 43 H45A 2 0.486916 -0.417713 0.004544 11.00000 -1.20000 AFIX 0 C35 1 0.547752 -0.235741 0.227745 11.00000 0.03521 0.03298 = 0.03243 0.00319 -0.00360 -0.00462 AFIX 43 H35A 2 0.565766 -0.179335 0.254625 11.00000 -1.20000 AFIX 0 C46 1 0.533485 -0.225273 -0.007444 11.00000 0.05186 0.02965 = 0.05804 -0.00460 -0.00841 0.01232 AFIX 43 H46A 2 0.572607 -0.268300 -0.012514 11.00000 -1.20000 AFIX 0 C3 1 0.666508 -0.004970 0.165719 11.00000 0.02736 0.03109 = 0.02609 0.00499 -0.00254 -0.00011 AFIX 43 H3A 2 0.662777 -0.082578 0.189943 11.00000 -1.20000 AFIX 0 C41 1 0.392652 0.100062 -0.098960 11.00000 0.03942 0.04462 = 0.03798 -0.00224 -0.00639 0.00583 AFIX 43 H41A 2 0.403492 0.001332 -0.092420 11.00000 -1.20000 AFIX 0 B1 3 0.459776 0.174149 -0.015162 11.00000 0.02440 0.02656 = 0.03090 0.00151 -0.00247 0.00022 C42 1 0.468344 -0.002694 -0.002686 11.00000 0.02958 0.02604 = 0.02773 0.00033 0.00068 -0.00064 C31 1 0.500008 -0.250306 0.141360 11.00000 0.03126 0.03029 = 0.03344 -0.00397 -0.00339 0.00335 AFIX 43 H31A 2 0.486671 -0.204454 0.110315 11.00000 -1.20000 AFIX 0 C8 1 0.648641 0.355886 -0.043541 11.00000 0.02332 0.03563 = 0.02974 0.00914 0.00025 -0.00502 AFIX 43 H8A 2 0.689214 0.385473 -0.051661 11.00000 -1.20000 AFIX 0 C4 1 0.612916 0.072281 0.148791 11.00000 0.02724 0.02526 = 0.02548 0.00443 0.00398 -0.00263 C11 1 0.619330 0.187829 0.112145 11.00000 0.02242 0.02209 = 0.02625 0.00330 0.00009 -0.00116 C12 1 0.570765 0.288248 0.019621 11.00000 0.02194 0.02207 = 0.02630 0.00252 0.00112 -0.00134 C40 1 0.357185 0.133004 -0.143488 11.00000 0.04917 0.06537 = 0.03505 -0.00700 -0.01248 0.00053 AFIX 43 H40A 2 0.344012 0.056788 -0.165835 11.00000 -1.20000 AFIX 0 C47 1 0.526702 -0.070498 -0.010629 11.00000 0.03525 0.02843 = 0.06160 0.00293 -0.00216 0.00253 AFIX 43 H47A 2 0.561399 -0.011625 -0.018126 11.00000 -1.20000 AFIX 0 C13 1 0.632744 0.335259 0.009609 11.00000 0.02463 0.02705 = 0.02962 0.00621 -0.00190 -0.00343 C43 1 0.417471 -0.095987 0.009131 11.00000 0.03687 0.03231 = 0.03606 -0.00109 0.00040 -0.00644 AFIX 43 H43A 2 0.378365 -0.054002 0.015276 11.00000 -1.20000 AFIX 0 C30 1 0.527309 -0.166548 0.181557 11.00000 0.02526 0.02103 = 0.02932 0.00153 0.00374 -0.00267 C39 1 0.341497 0.278915 -0.154559 11.00000 0.03755 0.07702 = 0.03905 0.01400 -0.01187 -0.00289 AFIX 43 H39A 2 0.318877 0.301679 -0.184961 11.00000 -1.20000 AFIX 0 C38 1 0.359532 0.391170 -0.120287 11.00000 0.04929 0.04985 = 0.06504 0.02153 -0.01949 -0.00158 AFIX 43 H38A 2 0.348304 0.489490 -0.127129 11.00000 -1.20000 AFIX 0 C34 1 0.541304 -0.388657 0.233754 11.00000 0.04481 0.02947 = 0.04463 0.01344 0.00353 0.00586 AFIX 43 H34A 2 0.555805 -0.435454 0.264241 11.00000 -1.20000 AFIX 0 C26 1 0.474480 0.139530 0.321411 11.00000 0.07603 0.08366 = 0.04517 -0.01772 0.02990 -0.01864 AFIX 43 H26A 2 0.438902 0.123117 0.341784 11.00000 -1.20000 AFIX 0 C32 1 0.492831 -0.403773 0.148080 11.00000 0.04068 0.02842 = 0.05270 -0.01294 -0.00190 0.00383 AFIX 43 H32A 2 0.474357 -0.460675 0.121558 11.00000 -1.20000 AFIX 0 C19 1 0.770305 -0.184772 0.197758 11.00000 0.03958 0.04358 = 0.05018 0.02117 -0.00038 0.00901 AFIX 33 H19A 2 0.740668 -0.249624 0.180870 11.00000 -1.50000 H19B 2 0.753102 -0.148698 0.230455 11.00000 -1.50000 H19C 2 0.808163 -0.238787 0.204819 11.00000 -1.50000 AFIX 0 PART 3 SAME 0.05 C48B CL3B CL4B C48A 1 0.270433 0.054767 0.250340 31.00000 0.12984 0.03943 = 0.13789 -0.03474 0.09107 -0.03342 AFIX 23 H48A 2 0.297006 0.093039 0.222328 31.00000 -1.20000 H48B 2 0.286281 -0.042119 0.260906 31.00000 -1.20000 AFIX 0 CL3A 4 0.193074 0.036957 0.227052 31.00000 0.10744 0.09093 = 0.07371 -0.00598 0.00133 0.05166 CL4A 4 0.271868 0.177807 0.304996 31.00000 0.15265 0.10789 = 0.11357 -0.04263 0.03680 -0.04545 PART 4 C48B 1 0.269115 0.096829 0.243321 -31.00000 0.12984 0.03943 = 0.13789 -0.03474 0.09107 -0.03342 AFIX 23 H48C 2 0.297307 0.012116 0.242465 -31.00000 -1.20000 H48D 2 0.283264 0.168211 0.217064 -31.00000 -1.20000 AFIX 0 CL3B 4 0.193074 0.036957 0.227052 -31.00000 0.10744 0.09093 = 0.07371 -0.00598 0.00133 0.05166 CL4B 4 0.271868 0.177807 0.304996 -31.00000 0.15265 0.10789 = 0.11357 -0.04263 0.03680 -0.04545 PART 3 C49A 1 0.214063 0.633767 0.933424 41.00000 0.09874 0.16958 = 0.09979 -0.02309 0.00075 -0.02849 AFIX 23 H49A 2 0.177896 0.686024 0.919515 41.00000 -1.20000 H49B 2 0.223914 0.552210 0.909610 41.00000 -1.20000 AFIX 0 CL5A 4 0.197000 0.563058 0.997073 41.00000 0.13151 0.17608 = 0.13612 0.01995 0.00303 -0.04680 CL6A 4 0.278495 0.757365 0.937421 41.00000 0.12661 0.07867 = 0.10159 -0.01798 -0.01176 -0.02053 PART 4 SAME 0.05 C49A CL5A CL6A C49B 1 0.262365 0.568318 0.955297 -41.00000 0.09874 0.16958 = 0.09979 -0.02309 0.00075 -0.02849 AFIX 23 H49C 2 0.254290 0.509896 0.923700 -41.00000 -1.20000 H49D 2 0.298262 0.525739 0.973275 -41.00000 -1.20000 AFIX 0 CL5B 4 0.197000 0.563058 0.997073 -41.00000 0.13151 0.17608 = 0.13612 0.01995 0.00303 -0.04680 CL6B 4 0.278495 0.757365 0.937421 -41.00000 0.12661 0.07867 = 0.10159 -0.01798 -0.01176 -0.02053 HKLF 4 REM pdcl2_0m in P n a 21 REM R1 = 0.0421 for 12392 Fo > 4sig(Fo) and 0.0514 for all 14333 data REM 538 parameters refined using 31 restraints END WGHT 0.0633 1.3566 REM Highest difference peak 1.031, deepest hole -0.672, 1-sigma level 0.085 Q1 1 0.1867 0.4924 0.9308 11.00000 0.05 1.03 Q2 1 0.5117 0.1362 0.1167 11.00000 0.05 0.74 Q3 1 0.4279 0.1414 0.1159 11.00000 0.05 0.66 Q4 1 0.2220 0.0790 0.2123 11.00000 0.05 0.62 Q5 1 0.4732 0.1398 0.1513 11.00000 0.05 0.59 Q6 1 0.2284 0.7712 0.9401 11.00000 0.05 0.57 Q7 1 0.4713 0.1306 0.0795 11.00000 0.05 0.56 Q8 1 0.4788 0.0481 0.1160 11.00000 0.05 0.53 Q9 1 0.2441 0.5747 0.9779 11.00000 0.05 0.50 Q10 1 0.2608 0.2005 0.3008 11.00000 0.05 0.48 Q11 1 0.6797 0.1925 -0.1549 11.00000 0.05 0.48 Q12 1 0.6859 0.4446 -0.1499 11.00000 0.05 0.46 Q13 1 0.2454 0.7388 0.9709 11.00000 0.05 0.45 Q14 1 0.2075 0.0927 0.2515 11.00000 0.05 0.45 Q15 1 0.5041 0.1096 0.1406 11.00000 0.05 0.44 Q16 1 0.4701 0.2285 0.1164 11.00000 0.05 0.42 Q17 1 0.2899 0.1360 0.2795 11.00000 0.05 0.41 Q18 1 0.5685 0.2825 0.0578 11.00000 0.05 0.41 Q19 1 0.2023 0.7318 0.9490 11.00000 0.05 0.39 Q20 1 0.5903 0.5385 -0.1602 11.00000 0.05 0.38 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^ > 2\s(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. There is 0.637(5) disorder for one of the tert-butyl substituents bound to the ligand backbone (C20-C23). In addition, there is 0.46(6) disorder for one of the molecules of CH2Cl2 (C48, CL3, CL4), and 0.43(1) disorder for the other molecule of CH2Cl2 (C49, CL5, CL6). ; _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^)+(0.0633P)^2^+1.3560P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 14333 _refine_ls_number_parameters 538 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 C20A C 0.62453(17) 0.3618(4) -0.14191(15) 0.0428(9) Uani 0.637(5) 1 d PD A 1 C21A C 0.6926(3) 0.4070(12) -0.1493(3) 0.0634(12) Uani 0.637(5) 1 d PD A 1 H21A H 0.7008 0.4221 -0.1863 0.095 Uiso 0.637(5) 1 calc PR A 1 H21B H 0.7193 0.3297 -0.1360 0.095 Uiso 0.637(5) 1 calc PR A 1 H21C H 0.7005 0.4979 -0.1304 0.095 Uiso 0.637(5) 1 calc PR A 1 C22A C 0.5853(3) 0.4978(8) -0.1604(3) 0.0634(12) Uani 0.637(5) 1 d PD A 1 H22A H 0.5416 0.4755 -0.1567 0.095 Uiso 0.637(5) 1 calc PR A 1 H22B H 0.5946 0.5192 -0.1968 0.095 Uiso 0.637(5) 1 calc PR A 1 H22C H 0.5956 0.5829 -0.1390 0.095 Uiso 0.637(5) 1 calc PR A 1 C23A C 0.6053(4) 0.2372(8) -0.1787(3) 0.0634(12) Uani 0.637(5) 1 d PD A 1 H23A H 0.5629 0.2091 -0.1714 0.095 Uiso 0.637(5) 1 calc PR A 1 H23B H 0.6323 0.1529 -0.1733 0.095 Uiso 0.637(5) 1 calc PR A 1 H23C H 0.6086 0.2704 -0.2147 0.095 Uiso 0.637(5) 1 calc PR A 1 C20B C 0.62453(17) 0.3618(4) -0.14191(15) 0.0428(9) Uani 0.363(5) 1 d PD A 2 C21B C 0.6665(6) 0.4959(12) -0.1499(5) 0.0634(12) Uani 0.363(5) 1 d PD A 2 H21D H 0.6766 0.5054 -0.1868 0.095 Uiso 0.363(5) 1 calc PR A 2 H21E H 0.7043 0.4832 -0.1299 0.095 Uiso 0.363(5) 1 calc PR A 2 H21F H 0.6452 0.5842 -0.1382 0.095 Uiso 0.363(5) 1 calc PR A 2 C22B C 0.5718(5) 0.3568(14) -0.1820(4) 0.0634(12) Uani 0.363(5) 1 d PD A 2 H22D H 0.5472 0.2687 -0.1764 0.095 Uiso 0.363(5) 1 calc PR A 2 H22E H 0.5890 0.3549 -0.2172 0.095 Uiso 0.363(5) 1 calc PR A 2 H22F H 0.5459 0.4434 -0.1780 0.095 Uiso 0.363(5) 1 calc PR A 2 C23B C 0.6620(5) 0.2187(9) -0.1535(5) 0.0634(12) Uani 0.363(5) 1 d PD A 2 H23D H 0.6360 0.1332 -0.1472 0.095 Uiso 0.363(5) 1 calc PR A 2 H23E H 0.6979 0.2147 -0.1308 0.095 Uiso 0.363(5) 1 calc PR A 2 H23F H 0.6753 0.2191 -0.1898 0.095 Uiso 0.363(5) 1 calc PR A 2 Pd1 Pd 0.469713(9) 0.13761(2) 0.115064(11) 0.02362(6) Uani 1 1 d . . . Cl2 Cl 0.38396(4) 0.01808(9) 0.15141(4) 0.03563(18) Uani 1 1 d . . . S1 S 0.55131(4) 0.27887(7) 0.08871(3) 0.02368(14) Uani 1 1 d . . . Cl1 Cl 0.41024(4) 0.26617(8) 0.04885(3) 0.02984(15) Uani 1 1 d . . . P1 P 0.53457(4) 0.03270(8) 0.17312(3) 0.02426(15) Uani 1 1 d . . . C1 C 0.72981(14) 0.1554(3) 0.11100(16) 0.0274(6) Uani 1 1 d . . . H1A H 0.7692 0.1832 0.0988 0.033 Uiso 1 1 calc R . . C25 C 0.4771(2) 0.0874(6) 0.2696(2) 0.0538(12) Uani 1 1 d . . . H25A H 0.4429 0.0380 0.2550 0.065 Uiso 1 1 calc R . . C17 C 0.81460(19) -0.1156(4) 0.1105(2) 0.0445(9) Uani 1 1 d . . . H17A H 0.7855 -0.1809 0.0932 0.067 Uiso 1 1 calc R . . H17B H 0.8517 -0.1703 0.1195 0.067 Uiso 1 1 calc R . . H17C H 0.8253 -0.0352 0.0871 0.067 Uiso 1 1 calc R . . C15 C 0.74732(17) 0.3827(4) 0.03209(16) 0.0373(8) Uani 1 1 d . . . H15A H 0.7484 0.4645 0.0076 0.056 Uiso 1 1 calc R . . H15B H 0.7593 0.2926 0.0142 0.056 Uiso 1 1 calc R . . H15C H 0.7758 0.4017 0.0607 0.056 Uiso 1 1 calc R . . C2 C 0.72553(15) 0.0347(3) 0.14618(14) 0.0290(6) Uani 1 1 d . . . C6 C 0.54634(16) 0.2859(4) -0.07174(14) 0.0313(7) Uani 1 1 d . A . H6A H 0.5182 0.2694 -0.0992 0.038 Uiso 1 1 calc R . . C29 C 0.58104(19) 0.1839(4) 0.26207(16) 0.0381(8) Uani 1 1 d . . . H29A H 0.6174 0.1980 0.2425 0.046 Uiso 1 1 calc R . . C7 C 0.60684(16) 0.3344(4) -0.08469(14) 0.0297(6) Uani 1 1 d . . . C10 C 0.67797(14) 0.2355(3) 0.09350(13) 0.0247(6) Uani 1 1 d . . . C24 C 0.53113(17) 0.1095(4) 0.23945(14) 0.0311(7) Uani 1 1 d . . . C18 C 0.83194(18) 0.0522(4) 0.18815(17) 0.0429(9) Uani 1 1 d . . . H18A H 0.8689 -0.0029 0.1973 0.064 Uiso 1 1 calc R . . H18B H 0.8136 0.0933 0.2197 0.064 Uiso 1 1 calc R . . H18C H 0.8428 0.1315 0.1643 0.064 Uiso 1 1 calc R . . C36 C 0.41275(15) 0.2107(3) -0.06341(14) 0.0287(6) Uani 1 1 d . . . C37 C 0.3943(2) 0.3567(4) -0.0759(2) 0.0463(10) Uani 1 1 d . . . H37A H 0.4059 0.4336 -0.0532 0.056 Uiso 1 1 calc R . . C44 C 0.4245(2) -0.2504(4) 0.01183(16) 0.0423(9) Uani 1 1 d . . . H44A H 0.3901 -0.3103 0.0194 0.051 Uiso 1 1 calc R . . C14 C 0.66490(18) 0.5138(4) 0.08260(16) 0.0386(8) Uani 1 1 d . . . H14A H 0.6669 0.5945 0.0577 0.058 Uiso 1 1 calc R . . H14B H 0.6945 0.5309 0.1106 0.058 Uiso 1 1 calc R . . H14C H 0.6235 0.5079 0.0972 0.058 Uiso 1 1 calc R . . C16 C 0.78467(15) -0.0523(4) 0.16118(14) 0.0314(7) Uani 1 1 d . . . C28 C 0.5779(3) 0.2376(5) 0.31337(17) 0.0502(11) Uani 1 1 d . . . H28A H 0.6118 0.2884 0.3278 0.060 Uiso 1 1 calc R . . C5 C 0.52606(14) 0.2611(3) -0.01974(13) 0.0245(6) Uani 1 1 d . . . C27 C 0.5252(3) 0.2164(5) 0.34284(19) 0.0601(14) Uani 1 1 d . . . H27A H 0.5231 0.2532 0.3772 0.072 Uiso 1 1 calc R . . C9 C 0.68081(15) 0.3655(3) 0.05415(14) 0.0285(6) Uani 1 1 d . A . C33 C 0.51316(19) -0.4710(4) 0.19409(17) 0.0398(8) Uani 1 1 d . . . H33A H 0.5079 -0.5732 0.1985 0.048 Uiso 1 1 calc R . . C45 C 0.4824(2) -0.3146(4) 0.00319(17) 0.0473(10) Uani 1 1 d . . . H45A H 0.4869 -0.4177 0.0045 0.057 Uiso 1 1 calc R . . C35 C 0.54775(19) -0.2357(4) 0.22775(15) 0.0335(7) Uani 1 1 d . . . H35A H 0.5658 -0.1793 0.2546 0.040 Uiso 1 1 calc R . . C46 C 0.5335(2) -0.2253(4) -0.0074(2) 0.0465(11) Uani 1 1 d . . . H46A H 0.5726 -0.2683 -0.0125 0.056 Uiso 1 1 calc R . . C3 C 0.66651(15) -0.0050(4) 0.16572(13) 0.0282(6) Uani 1 1 d . . . H3A H 0.6628 -0.0826 0.1899 0.034 Uiso 1 1 calc R . . C41 C 0.39265(19) 0.1001(5) -0.09896(16) 0.0407(8) Uani 1 1 d . . . H41A H 0.4035 0.0013 -0.0924 0.049 Uiso 1 1 calc R . . B1 B 0.45978(17) 0.1741(4) -0.01516(16) 0.0273(7) Uani 1 1 d . A . C42 C 0.46834(15) -0.0027(3) -0.00269(14) 0.0278(6) Uani 1 1 d . . . C31 C 0.50001(17) -0.2503(4) 0.14136(14) 0.0317(7) Uani 1 1 d . . . H31A H 0.4867 -0.2045 0.1103 0.038 Uiso 1 1 calc R . . C8 C 0.64864(16) 0.3559(3) -0.04354(14) 0.0296(7) Uani 1 1 d . A . H8A H 0.6892 0.3855 -0.0517 0.035 Uiso 1 1 calc R . . C4 C 0.61292(15) 0.0723(3) 0.14879(13) 0.0260(6) Uani 1 1 d . . . C11 C 0.61933(13) 0.1878(3) 0.11214(15) 0.0236(5) Uani 1 1 d . . . C12 C 0.57077(14) 0.2882(3) 0.01962(12) 0.0234(6) Uani 1 1 d . A . C40 C 0.3572(2) 0.1330(5) -0.14349(18) 0.0499(10) Uani 1 1 d . . . H40A H 0.3440 0.0568 -0.1658 0.060 Uiso 1 1 calc R . . C47 C 0.52670(18) -0.0705(4) -0.01063(19) 0.0418(9) Uani 1 1 d . A . H47A H 0.5614 -0.0116 -0.0181 0.050 Uiso 1 1 calc R . . C13 C 0.63274(15) 0.3353(3) 0.00961(13) 0.0271(6) Uani 1 1 d . . . C43 C 0.41747(18) -0.0960(4) 0.00913(15) 0.0351(7) Uani 1 1 d . A . H43A H 0.3784 -0.0540 0.0153 0.042 Uiso 1 1 calc R . . C30 C 0.52731(14) -0.1665(3) 0.18156(14) 0.0252(6) Uani 1 1 d . . . C39 C 0.3415(2) 0.2789(5) -0.15456(18) 0.0512(11) Uani 1 1 d . . . H39A H 0.3189 0.3017 -0.1850 0.061 Uiso 1 1 calc R . . C38 C 0.3595(2) 0.3912(5) -0.1203(2) 0.0547(12) Uani 1 1 d . . . H38A H 0.3483 0.4895 -0.1271 0.066 Uiso 1 1 calc R . . C34 C 0.54130(19) -0.3887(4) 0.23375(17) 0.0396(9) Uani 1 1 d . . . H34A H 0.5558 -0.4355 0.2642 0.048 Uiso 1 1 calc R . . C26 C 0.4745(3) 0.1395(6) 0.3214(2) 0.0683(17) Uani 1 1 d . . . H26A H 0.4389 0.1231 0.3418 0.082 Uiso 1 1 calc R . . C32 C 0.49283(19) -0.4038(4) 0.14808(18) 0.0406(8) Uani 1 1 d . . . H32A H 0.4744 -0.4607 0.1216 0.049 Uiso 1 1 calc R . . C19 C 0.77030(19) -0.1848(4) 0.19776(17) 0.0444(9) Uani 1 1 d . . . H19A H 0.7407 -0.2496 0.1809 0.067 Uiso 1 1 calc R . . H19B H 0.7531 -0.1487 0.2305 0.067 Uiso 1 1 calc R . . H19C H 0.8082 -0.2388 0.2048 0.067 Uiso 1 1 calc R . . C48A C 0.2704(4) 0.055(3) 0.2503(9) 0.102(5) Uani 0.46(5) 1 d PD B 3 H48A H 0.2970 0.0930 0.2223 0.123 Uiso 0.46(5) 1 calc PR B 3 H48B H 0.2863 -0.0421 0.2609 0.123 Uiso 0.46(5) 1 calc PR B 3 Cl3A Cl 0.19307(9) 0.03696(19) 0.22705(7) 0.0907(5) Uani 0.46(5) 1 d PD B 3 Cl4A Cl 0.27187(13) 0.1778(3) 0.30500(10) 0.1247(8) Uani 0.46(5) 1 d PD B 3 C48B C 0.2691(5) 0.097(4) 0.2433(8) 0.102(5) Uani 0.54(5) 1 d PD B 4 H48C H 0.2973 0.0121 0.2425 0.123 Uiso 0.54(5) 1 calc PR B 4 H48D H 0.2833 0.1682 0.2171 0.123 Uiso 0.54(5) 1 calc PR B 4 Cl3B Cl 0.19307(9) 0.03696(19) 0.22705(7) 0.0907(5) Uani 0.54(5) 1 d PD B 4 Cl4B Cl 0.27187(13) 0.1778(3) 0.30500(10) 0.1247(8) Uani 0.54(5) 1 d PD B 4 C49A C 0.2141(8) 0.634(2) 0.9334(3) 0.123(5) Uani 0.433(12) 1 d PD C 3 H49A H 0.1779 0.6860 0.9195 0.147 Uiso 0.433(12) 1 calc PR C 3 H49B H 0.2239 0.5522 0.9096 0.147 Uiso 0.433(12) 1 calc PR C 3 Cl5A Cl 0.19700(14) 0.5631(4) 0.99707(13) 0.1479(10) Uani 0.433(12) 1 d PD C 3 Cl6A Cl 0.27849(10) 0.75736(18) 0.93742(9) 0.1023(6) Uani 0.433(12) 1 d PD C 3 C49B C 0.2624(5) 0.568(2) 0.9553(6) 0.123(5) Uani 0.567(12) 1 d PD C 4 H49C H 0.2543 0.5099 0.9237 0.147 Uiso 0.567(12) 1 calc PR C 4 H49D H 0.2983 0.5257 0.9733 0.147 Uiso 0.567(12) 1 calc PR C 4 Cl5B Cl 0.19700(14) 0.5631(4) 0.99707(13) 0.1479(10) Uani 0.567(12) 1 d PD C 4 Cl6B Cl 0.27849(10) 0.75736(18) 0.93742(9) 0.1023(6) Uani 0.567(12) 1 d PD C 4 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 C20A 0.036(2) 0.066(3) 0.0258(18) 0.0086(16) 0.0003(15) -0.0117(17) C21A 0.064(3) 0.093(3) 0.0328(17) 0.014(2) 0.0062(18) -0.023(2) C22A 0.064(3) 0.093(3) 0.0328(17) 0.014(2) 0.0062(18) -0.023(2) C23A 0.064(3) 0.093(3) 0.0328(17) 0.014(2) 0.0062(18) -0.023(2) C20B 0.036(2) 0.066(3) 0.0258(18) 0.0086(16) 0.0003(15) -0.0117(17) C21B 0.064(3) 0.093(3) 0.0328(17) 0.014(2) 0.0062(18) -0.023(2) C22B 0.064(3) 0.093(3) 0.0328(17) 0.014(2) 0.0062(18) -0.023(2) C23B 0.064(3) 0.093(3) 0.0328(17) 0.014(2) 0.0062(18) -0.023(2) Pd1 0.02098(10) 0.02276(9) 0.02712(10) -0.00023(10) 0.00399(11) -0.00017(7) Cl2 0.0258(4) 0.0362(4) 0.0449(5) 0.0027(3) 0.0107(3) -0.0041(3) S1 0.0227(3) 0.0222(3) 0.0262(4) 0.0013(3) 0.0014(3) -0.0007(2) Cl1 0.0220(3) 0.0314(3) 0.0360(4) 0.0010(3) 0.0011(3) 0.0038(3) P1 0.0261(4) 0.0237(3) 0.0230(4) 0.0007(3) 0.0034(3) -0.0024(3) C1 0.0225(13) 0.0313(13) 0.0284(16) 0.0038(13) 0.0026(15) -0.0022(9) C25 0.053(3) 0.060(3) 0.048(3) -0.019(2) 0.016(2) -0.020(2) C17 0.044(2) 0.0424(17) 0.047(2) 0.0033(18) 0.004(2) 0.0120(14) C15 0.0241(17) 0.0463(19) 0.042(2) 0.0179(15) -0.0034(14) -0.0116(13) C2 0.0281(16) 0.0300(14) 0.0287(16) 0.0044(12) -0.0005(13) 0.0014(11) C6 0.0285(17) 0.0353(16) 0.0302(17) 0.0032(13) -0.0009(13) -0.0045(12) C29 0.042(2) 0.0375(17) 0.0345(19) -0.0038(14) 0.0025(16) -0.0086(15) C7 0.0272(16) 0.0351(15) 0.0268(16) 0.0048(12) 0.0032(13) -0.0018(12) C10 0.0231(14) 0.0263(13) 0.0247(14) 0.0052(10) -0.0031(12) -0.0024(10) C24 0.041(2) 0.0232(13) 0.0294(17) -0.0017(11) 0.0013(14) -0.0036(12) C18 0.033(2) 0.047(2) 0.049(2) 0.0019(17) -0.0121(17) -0.0029(15) C36 0.0207(15) 0.0327(15) 0.0326(17) 0.0020(12) -0.0019(13) -0.0023(11) C37 0.041(2) 0.0398(19) 0.059(3) 0.0073(17) -0.019(2) -0.0035(15) C44 0.059(3) 0.0311(16) 0.037(2) -0.0008(14) -0.0019(18) -0.0116(16) C14 0.041(2) 0.0304(15) 0.044(2) 0.0054(14) -0.0093(17) -0.0111(13) C16 0.0248(15) 0.0344(15) 0.0350(18) 0.0096(12) -0.0026(13) 0.0026(11) C28 0.071(3) 0.045(2) 0.035(2) -0.0088(17) -0.007(2) -0.008(2) C5 0.0226(15) 0.0221(12) 0.0286(15) 0.0019(10) -0.0015(12) -0.0008(10) C27 0.097(4) 0.052(3) 0.031(2) -0.0163(18) 0.005(2) -0.010(2) C9 0.0234(15) 0.0299(14) 0.0321(17) 0.0087(12) -0.0054(13) -0.0064(11) C33 0.043(2) 0.0238(15) 0.053(2) -0.0005(14) 0.0056(18) 0.0024(13) C45 0.079(3) 0.0242(15) 0.039(2) -0.0038(14) -0.012(2) 0.0007(17) C35 0.0352(19) 0.0330(16) 0.0324(19) 0.0032(13) -0.0036(15) -0.0046(14) C46 0.052(3) 0.0297(18) 0.058(3) -0.0046(17) -0.008(2) 0.0123(16) C3 0.0274(15) 0.0311(14) 0.0261(16) 0.0050(11) -0.0025(12) -0.0001(11) C41 0.039(2) 0.0446(18) 0.038(2) -0.0022(15) -0.0064(17) 0.0058(15) B1 0.0244(18) 0.0266(15) 0.0309(19) 0.0015(13) -0.0025(14) 0.0002(12) C42 0.0296(16) 0.0260(14) 0.0277(16) 0.0003(11) 0.0007(12) -0.0006(11) C31 0.0313(17) 0.0303(14) 0.0334(17) -0.0040(12) -0.0034(14) 0.0034(12) C8 0.0233(16) 0.0356(16) 0.0297(17) 0.0091(12) 0.0002(13) -0.0050(11) C4 0.0272(15) 0.0253(13) 0.0255(15) 0.0044(11) 0.0040(12) -0.0026(10) C11 0.0224(12) 0.0221(10) 0.0262(14) 0.0033(13) 0.0001(14) -0.0012(9) C12 0.0219(14) 0.0221(12) 0.0263(15) 0.0025(10) 0.0011(11) -0.0013(10) C40 0.049(3) 0.065(3) 0.035(2) -0.0070(18) -0.0125(19) 0.0005(19) C47 0.035(2) 0.0284(17) 0.062(3) 0.0029(16) -0.0022(17) 0.0025(13) C13 0.0246(15) 0.0270(13) 0.0296(16) 0.0062(11) -0.0019(12) -0.0034(11) C43 0.0369(19) 0.0323(15) 0.0361(19) -0.0011(13) 0.0004(15) -0.0064(13) C30 0.0253(15) 0.0210(12) 0.0293(16) 0.0015(11) 0.0037(12) -0.0027(10) C39 0.038(2) 0.077(3) 0.039(2) 0.014(2) -0.0119(18) -0.003(2) C38 0.049(3) 0.050(2) 0.065(3) 0.022(2) -0.019(2) -0.0016(19) C34 0.045(2) 0.0295(16) 0.045(2) 0.0134(14) 0.0035(17) 0.0059(14) C26 0.076(4) 0.084(4) 0.045(3) -0.018(2) 0.030(3) -0.019(3) C32 0.041(2) 0.0284(14) 0.053(2) -0.0129(15) -0.0019(18) 0.0038(14) C19 0.040(2) 0.0436(19) 0.050(2) 0.0212(17) -0.0004(18) 0.0090(16) C48A 0.130(7) 0.039(9) 0.138(8) -0.035(7) 0.091(6) -0.033(5) Cl3A 0.1074(13) 0.0909(10) 0.0737(10) -0.0060(8) 0.0013(9) 0.0517(10) Cl4A 0.153(2) 0.1079(13) 0.1136(16) -0.0426(12) 0.0368(15) -0.0455(14) C48B 0.130(7) 0.039(9) 0.138(8) -0.035(7) 0.091(6) -0.033(5) Cl3B 0.1074(13) 0.0909(10) 0.0737(10) -0.0060(8) 0.0013(9) 0.0517(10) Cl4B 0.153(2) 0.1079(13) 0.1136(16) -0.0426(12) 0.0368(15) -0.0455(14) C49A 0.099(10) 0.170(13) 0.100(10) -0.023(9) 0.001(7) -0.028(9) Cl5A 0.132(2) 0.176(2) 0.136(2) 0.0199(19) 0.0030(17) -0.047(2) Cl6A 0.1266(17) 0.0787(10) 0.1016(14) -0.0180(9) -0.0118(11) -0.0205(11) C49B 0.099(10) 0.170(13) 0.100(10) -0.023(9) 0.001(7) -0.028(9) Cl5B 0.132(2) 0.176(2) 0.136(2) 0.0199(19) 0.0030(17) -0.047(2) Cl6B 0.1266(17) 0.0787(10) 0.1016(14) -0.0180(9) -0.0118(11) -0.0205(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C20A C23A 1.510(5) . ? C20A C7 1.514(5) . ? C20A C21A 1.521(5) . ? C20A C22A 1.551(5) . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23B H23D 0.9600 . ? C23B H23E 0.9600 . ? C23B H23F 0.9600 . ? Pd1 P1 2.2264(8) . ? Pd1 S1 2.2563(7) . ? Pd1 Cl2 2.3135(8) . ? Pd1 Cl1 2.3961(8) . ? Pd1 B1 3.311(4) . ? S1 C11 1.770(3) . ? S1 C12 1.795(3) . ? S1 C9 3.005(3) . ? Cl1 B1 2.101(4) . ? P1 C30 1.806(3) . ? P1 C24 1.812(4) . ? P1 C4 1.819(3) . ? C1 C10 1.393(4) . ? C1 C2 1.403(4) . ? C1 H1A 0.9300 . ? C25 C26 1.391(7) . ? C25 C24 1.398(6) . ? C25 H25A 0.9300 . ? C17 C16 1.540(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C15 C9 1.535(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C2 C3 1.401(5) . ? C2 C16 1.533(4) . ? C6 C5 1.401(5) . ? C6 C7 1.403(5) . ? C6 H6A 0.9300 . ? C29 C24 1.382(5) . ? C29 C28 1.384(6) . ? C29 H29A 0.9300 . ? C7 C8 1.384(5) . ? C10 C11 1.406(4) . ? C10 C9 1.534(4) . ? C18 C16 1.538(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C36 C37 1.403(5) . ? C36 C41 1.405(5) . ? C36 B1 1.613(5) . ? C37 C38 1.380(6) . ? C37 H37A 0.9300 . ? C44 C45 1.383(7) . ? C44 C43 1.394(5) . ? C44 H44A 0.9300 . ? C14 C9 1.549(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 C19 1.536(5) . ? C28 C27 1.363(7) . ? C28 H28A 0.9300 . ? C5 C12 1.400(4) . ? C5 B1 1.622(5) . ? C27 C26 1.395(8) . ? C27 H27A 0.9300 . ? C9 C13 1.547(5) . ? C33 C32 1.379(6) . ? C33 C34 1.382(6) . ? C33 H33A 0.9300 . ? C45 C46 1.381(7) . ? C45 H45A 0.9300 . ? C35 C34 1.387(5) . ? C35 C30 1.392(5) . ? C35 H35A 0.9300 . ? C46 C47 1.398(6) . ? C46 H46A 0.9300 . ? C3 C4 1.406(4) . ? C3 H3A 0.9300 . ? C41 C40 1.388(6) . ? C41 H41A 0.9300 . ? B1 C42 1.627(5) . ? C42 C47 1.402(5) . ? C42 C43 1.404(5) . ? C31 C30 1.391(5) . ? C31 C32 1.395(5) . ? C31 H31A 0.9300 . ? C8 C13 1.397(5) . ? C8 H8A 0.9300 . ? C4 C11 1.396(4) . ? C12 C13 1.413(4) . ? C40 C39 1.379(6) . ? C40 H40A 0.9300 . ? C47 H47A 0.9300 . ? C43 H43A 0.9300 . ? C39 C38 1.382(7) . ? C39 H39A 0.9300 . ? C38 H38A 0.9300 . ? C34 H34A 0.9300 . ? C26 H26A 0.9300 . ? C32 H32A 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C48A Cl3A 1.763(5) . ? C48A Cl4A 1.767(5) . ? C48A H48A 0.9700 . ? C48A H48B 0.9700 . ? C48B H48C 0.9700 . ? C48B H48D 0.9700 . ? C49A Cl5A 1.766(5) . ? C49A Cl6A 1.771(5) . ? C49A H49A 0.9700 . ? C49A H49B 0.9700 . ? C49B H49C 0.9700 . ? C49B H49D 0.9700 . ? 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 C23A C20A C7 113.5(4) . . ? C23A C20A C21A 112.4(5) . . ? C7 C20A C21A 113.6(4) . . ? C23A C20A C22A 104.5(5) . . ? C7 C20A C22A 106.2(4) . . ? C21A C20A C22A 105.7(5) . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C20A C23A H23A 109.5 . . ? C20A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C20A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? H21D C21B H21E 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? H22D C22B H22E 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? H23D C23B H23E 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? P1 Pd1 S1 87.13(3) . . ? P1 Pd1 Cl2 92.09(3) . . ? S1 Pd1 Cl2 171.82(3) . . ? P1 Pd1 Cl1 173.35(3) . . ? S1 Pd1 Cl1 86.24(3) . . ? Cl2 Pd1 Cl1 94.55(3) . . ? P1 Pd1 B1 137.36(7) . . ? S1 Pd1 B1 72.61(7) . . ? Cl2 Pd1 B1 112.89(7) . . ? Cl1 Pd1 B1 39.23(7) . . ? C11 S1 C12 98.98(16) . . ? C11 S1 Pd1 106.13(9) . . ? C12 S1 Pd1 119.47(10) . . ? C11 S1 C9 57.27(11) . . ? C12 S1 C9 59.49(12) . . ? Pd1 S1 C9 160.59(6) . . ? B1 Cl1 Pd1 94.61(11) . . ? C30 P1 C24 105.26(16) . . ? C30 P1 C4 108.18(14) . . ? C24 P1 C4 105.98(16) . . ? C30 P1 Pd1 116.25(11) . . ? C24 P1 Pd1 115.01(12) . . ? C4 P1 Pd1 105.58(11) . . ? C10 C1 C2 123.1(3) . . ? C10 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C16 121.8(3) . . ? C1 C2 C16 119.7(3) . . ? C5 C6 C7 123.6(3) . . ? C5 C6 H6A 118.2 . . ? C7 C6 H6A 118.2 . . ? C24 C29 C28 121.2(4) . . ? C24 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C8 C7 C6 117.6(3) . . ? C8 C7 C20A 122.2(3) . . ? C6 C7 C20A 120.2(3) . . ? C1 C10 C11 116.5(3) . . ? C1 C10 C9 124.5(3) . . ? C11 C10 C9 118.9(3) . . ? C29 C24 C25 118.8(4) . . ? C29 C24 P1 122.3(3) . . ? C25 C24 P1 118.8(3) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C37 C36 C41 115.4(3) . . ? C37 C36 B1 122.3(3) . . ? C41 C36 B1 122.0(3) . . ? C38 C37 C36 122.9(4) . . ? C38 C37 H37A 118.6 . . ? C36 C37 H37A 118.6 . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 C16 C19 112.2(3) . . ? C2 C16 C18 109.9(3) . . ? C19 C16 C18 109.7(3) . . ? C2 C16 C17 109.0(3) . . ? C19 C16 C17 107.3(3) . . ? C18 C16 C17 108.7(3) . . ? C27 C28 C29 120.2(4) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C12 C5 C6 115.2(3) . . ? C12 C5 B1 129.0(3) . . ? C6 C5 B1 114.4(3) . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C10 C9 C15 110.4(3) . . ? C10 C9 C13 108.1(2) . . ? C15 C9 C13 111.7(3) . . ? C10 C9 C14 110.1(3) . . ? C15 C9 C14 106.6(3) . . ? C13 C9 C14 110.0(3) . . ? C10 C9 S1 65.08(16) . . ? C15 C9 S1 170.0(2) . . ? C13 C9 S1 63.51(16) . . ? C14 C9 S1 83.40(19) . . ? C32 C33 C34 120.9(3) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C46 C45 C44 119.8(3) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C34 C35 C30 120.1(4) . . ? C34 C35 H35A 120.0 . . ? C30 C35 H35A 119.9 . . ? C45 C46 C47 120.3(4) . . ? C45 C46 H46A 119.8 . . ? C47 C46 H46A 119.8 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C40 C41 C36 122.3(4) . . ? C40 C41 H41A 118.9 . . ? C36 C41 H41A 118.9 . . ? C36 B1 C5 113.1(3) . . ? C36 B1 C42 114.5(3) . . ? C5 B1 C42 112.6(3) . . ? C36 B1 Cl1 100.8(2) . . ? C5 B1 Cl1 107.8(2) . . ? C42 B1 Cl1 106.9(2) . . ? C36 B1 Pd1 144.1(2) . . ? C5 B1 Pd1 93.6(2) . . ? C42 B1 Pd1 72.79(18) . . ? Cl1 B1 Pd1 46.16(8) . . ? C47 C42 C43 117.5(3) . . ? C47 C42 B1 119.7(3) . . ? C43 C42 B1 122.3(3) . . ? C30 C31 C32 119.3(3) . . ? C30 C31 H31A 120.3 . . ? C32 C31 H31A 120.3 . . ? C7 C8 C13 123.1(3) . . ? C7 C8 H8A 118.5 . . ? C13 C8 H8A 118.5 . . ? C11 C4 C3 119.2(3) . . ? C11 C4 P1 117.3(2) . . ? C3 C4 P1 123.5(2) . . ? C4 C11 C10 122.4(3) . . ? C4 C11 S1 118.9(2) . . ? C10 C11 S1 118.7(2) . . ? C5 C12 C13 124.4(3) . . ? C5 C12 S1 121.6(2) . . ? C13 C12 S1 113.9(2) . . ? C39 C40 C41 119.9(4) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C46 C47 C42 121.0(4) . . ? C46 C47 H47A 119.5 . . ? C42 C47 H47A 119.5 . . ? C8 C13 C12 116.1(3) . . ? C8 C13 C9 120.9(3) . . ? C12 C13 C9 123.0(3) . . ? C44 C43 C42 121.2(4) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C31 C30 C35 120.2(3) . . ? C31 C30 P1 119.0(3) . . ? C35 C30 P1 120.9(3) . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C37 C38 C39 119.7(4) . . ? C37 C38 H38A 120.1 . . ? C39 C38 H38A 120.1 . . ? C33 C34 C35 119.5(4) . . ? C33 C34 H34A 120.2 . . ? C35 C34 H34A 120.2 . . ? C25 C26 C27 120.0(5) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Cl3A C48A Cl4A 109.5(4) . . ? Cl3A C48A H48A 109.8 . . ? Cl4A C48A H48A 109.8 . . ? Cl3A C48A H48B 109.8 . . ? Cl4A C48A H48B 109.8 . . ? H48A C48A H48B 108.2 . . ? H48C C48B H48D 107.9 . . ? Cl5A C49A Cl6A 109.5(4) . . ? Cl5A C49A H49A 109.8 . . ? Cl6A C49A H49A 109.8 . . ? Cl5A C49A H49B 109.8 . . ? Cl6A C49A H49B 109.8 . . ? H49A C49A H49B 108.2 . . ? H49C C49B H49D 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 S1 C11 17.89(12) . . . . ? Cl1 Pd1 S1 C11 -161.61(12) . . . . ? B1 Pd1 S1 C11 -124.06(14) . . . . ? P1 Pd1 S1 C12 128.39(11) . . . . ? Cl1 Pd1 S1 C12 -51.12(11) . . . . ? B1 Pd1 S1 C12 -13.57(13) . . . . ? P1 Pd1 S1 C9 47.1(2) . . . . ? Cl1 Pd1 S1 C9 -132.4(2) . . . . ? B1 Pd1 S1 C9 -94.9(2) . . . . ? S1 Pd1 Cl1 B1 66.87(10) . . . . ? Cl2 Pd1 Cl1 B1 -121.30(10) . . . . ? S1 Pd1 P1 C30 -139.27(12) . . . . ? Cl2 Pd1 P1 C30 48.88(12) . . . . ? B1 Pd1 P1 C30 -79.01(15) . . . . ? S1 Pd1 P1 C24 97.09(12) . . . . ? Cl2 Pd1 P1 C24 -74.76(12) . . . . ? B1 Pd1 P1 C24 157.35(15) . . . . ? S1 Pd1 P1 C4 -19.36(10) . . . . ? Cl2 Pd1 P1 C4 168.79(11) . . . . ? B1 Pd1 P1 C4 40.90(14) . . . . ? C10 C1 C2 C3 -1.6(5) . . . . ? C10 C1 C2 C16 176.9(3) . . . . ? C5 C6 C7 C8 1.2(5) . . . . ? C5 C6 C7 C20A -178.6(3) . . . . ? C23A C20A C7 C8 132.9(5) . . . . ? C21A C20A C7 C8 2.9(6) . . . . ? C22A C20A C7 C8 -112.9(4) . . . . ? C23A C20A C7 C6 -47.3(6) . . . . ? C21A C20A C7 C6 -177.4(5) . . . . ? C22A C20A C7 C6 66.9(5) . . . . ? C2 C1 C10 C11 -1.2(5) . . . . ? C2 C1 C10 C9 -178.6(3) . . . . ? C28 C29 C24 C25 -0.8(6) . . . . ? C28 C29 C24 P1 -178.1(3) . . . . ? C26 C25 C24 C29 -0.3(7) . . . . ? C26 C25 C24 P1 177.1(4) . . . . ? C30 P1 C24 C29 115.8(3) . . . . ? C4 P1 C24 C29 1.3(3) . . . . ? Pd1 P1 C24 C29 -115.0(3) . . . . ? C30 P1 C24 C25 -61.6(4) . . . . ? C4 P1 C24 C25 -176.1(4) . . . . ? Pd1 P1 C24 C25 67.7(4) . . . . ? C41 C36 C37 C38 -0.9(7) . . . . ? B1 C36 C37 C38 172.9(4) . . . . ? C3 C2 C16 C19 1.3(5) . . . . ? C1 C2 C16 C19 -177.1(3) . . . . ? C3 C2 C16 C18 -121.0(4) . . . . ? C1 C2 C16 C18 60.5(4) . . . . ? C3 C2 C16 C17 120.0(4) . . . . ? C1 C2 C16 C17 -58.4(4) . . . . ? C24 C29 C28 C27 0.7(7) . . . . ? C7 C6 C5 C12 0.1(5) . . . . ? C7 C6 C5 B1 -168.1(3) . . . . ? C29 C28 C27 C26 0.4(8) . . . . ? C1 C10 C9 C15 6.5(5) . . . . ? C11 C10 C9 C15 -170.8(3) . . . . ? C1 C10 C9 C13 128.9(3) . . . . ? C11 C10 C9 C13 -48.4(4) . . . . ? C1 C10 C9 C14 -110.9(4) . . . . ? C11 C10 C9 C14 71.8(4) . . . . ? C1 C10 C9 S1 176.9(4) . . . . ? C11 C10 C9 S1 -0.4(2) . . . . ? C11 S1 C9 C10 0.3(2) . . . . ? C12 S1 C9 C10 -126.1(2) . . . . ? Pd1 S1 C9 C10 -33.5(3) . . . . ? C11 S1 C9 C13 128.3(2) . . . . ? C12 S1 C9 C13 1.84(17) . . . . ? Pd1 S1 C9 C13 94.5(3) . . . . ? C11 S1 C9 C14 -115.5(2) . . . . ? C12 S1 C9 C14 118.1(2) . . . . ? Pd1 S1 C9 C14 -149.3(2) . . . . ? C43 C44 C45 C46 0.8(6) . . . . ? C44 C45 C46 C47 -1.4(7) . . . . ? C1 C2 C3 C4 2.0(5) . . . . ? C16 C2 C3 C4 -176.5(3) . . . . ? C37 C36 C41 C40 0.3(6) . . . . ? B1 C36 C41 C40 -173.6(4) . . . . ? C37 C36 B1 C5 -56.5(5) . . . . ? C41 C36 B1 C5 116.9(4) . . . . ? C37 C36 B1 C42 172.7(4) . . . . ? C41 C36 B1 C42 -13.9(5) . . . . ? C37 C36 B1 Cl1 58.3(4) . . . . ? C41 C36 B1 Cl1 -128.2(3) . . . . ? C37 C36 B1 Pd1 78.4(5) . . . . ? C41 C36 B1 Pd1 -108.2(4) . . . . ? C12 C5 B1 C36 161.8(3) . . . . ? C6 C5 B1 C36 -32.0(4) . . . . ? C12 C5 B1 C42 -66.4(4) . . . . ? C6 C5 B1 C42 99.8(3) . . . . ? C12 C5 B1 Cl1 51.2(4) . . . . ? C6 C5 B1 Cl1 -142.6(2) . . . . ? C12 C5 B1 Pd1 6.4(3) . . . . ? C6 C5 B1 Pd1 172.6(2) . . . . ? Pd1 Cl1 B1 C36 163.83(18) . . . . ? Pd1 Cl1 B1 C5 -77.4(2) . . . . ? Pd1 Cl1 B1 C42 43.9(2) . . . . ? P1 Pd1 B1 C36 160.9(3) . . . . ? S1 Pd1 B1 C36 -133.8(4) . . . . ? Cl2 Pd1 B1 C36 39.8(4) . . . . ? Cl1 Pd1 B1 C36 -27.8(3) . . . . ? P1 Pd1 B1 C5 -59.8(2) . . . . ? S1 Pd1 B1 C5 5.50(16) . . . . ? Cl2 Pd1 B1 C5 179.05(15) . . . . ? Cl1 Pd1 B1 C5 111.4(2) . . . . ? P1 Pd1 B1 C42 52.7(2) . . . . ? S1 Pd1 B1 C42 118.06(17) . . . . ? Cl2 Pd1 B1 C42 -68.39(18) . . . . ? Cl1 Pd1 B1 C42 -136.0(2) . . . . ? P1 Pd1 B1 Cl1 -171.27(4) . . . . ? S1 Pd1 B1 Cl1 -105.94(9) . . . . ? Cl2 Pd1 B1 Cl1 67.60(10) . . . . ? C36 B1 C42 C47 114.6(4) . . . . ? C5 B1 C42 C47 -16.5(5) . . . . ? Cl1 B1 C42 C47 -134.7(3) . . . . ? Pd1 B1 C42 C47 -103.1(3) . . . . ? C36 B1 C42 C43 -56.7(5) . . . . ? C5 B1 C42 C43 172.3(3) . . . . ? Cl1 B1 C42 C43 54.0(4) . . . . ? Pd1 B1 C42 C43 85.6(3) . . . . ? C6 C7 C8 C13 -1.6(5) . . . . ? C20A C7 C8 C13 178.1(3) . . . . ? C2 C3 C4 C11 0.4(5) . . . . ? C2 C3 C4 P1 -178.3(3) . . . . ? C30 P1 C4 C11 143.4(3) . . . . ? C24 P1 C4 C11 -104.1(3) . . . . ? Pd1 P1 C4 C11 18.3(3) . . . . ? C30 P1 C4 C3 -37.9(3) . . . . ? C24 P1 C4 C3 74.6(3) . . . . ? Pd1 P1 C4 C3 -162.9(3) . . . . ? C3 C4 C11 C10 -3.5(5) . . . . ? P1 C4 C11 C10 175.3(3) . . . . ? C3 C4 C11 S1 177.1(2) . . . . ? P1 C4 C11 S1 -4.1(4) . . . . ? C1 C10 C11 C4 3.8(5) . . . . ? C9 C10 C11 C4 -178.7(3) . . . . ? C1 C10 C11 S1 -176.8(3) . . . . ? C9 C10 C11 S1 0.7(4) . . . . ? C12 S1 C11 C4 -136.4(3) . . . . ? Pd1 S1 C11 C4 -12.0(3) . . . . ? C9 S1 C11 C4 179.1(3) . . . . ? C12 S1 C11 C10 44.2(3) . . . . ? Pd1 S1 C11 C10 168.5(2) . . . . ? C9 S1 C11 C10 -0.4(2) . . . . ? C6 C5 C12 C13 -0.9(4) . . . . ? B1 C5 C12 C13 165.2(3) . . . . ? C6 C5 C12 S1 174.3(2) . . . . ? B1 C5 C12 S1 -19.6(4) . . . . ? C11 S1 C12 C5 139.1(2) . . . . ? Pd1 S1 C12 C5 24.8(3) . . . . ? C9 S1 C12 C5 -177.6(3) . . . . ? C11 S1 C12 C13 -45.2(2) . . . . ? Pd1 S1 C12 C13 -159.56(18) . . . . ? C9 S1 C12 C13 -1.97(19) . . . . ? C36 C41 C40 C39 1.2(7) . . . . ? C45 C46 C47 C42 0.6(7) . . . . ? C43 C42 C47 C46 0.7(6) . . . . ? B1 C42 C47 C46 -171.0(4) . . . . ? C7 C8 C13 C12 0.9(5) . . . . ? C7 C8 C13 C9 -178.1(3) . . . . ? C5 C12 C13 C8 0.5(4) . . . . ? S1 C12 C13 C8 -175.0(2) . . . . ? C5 C12 C13 C9 179.5(3) . . . . ? S1 C12 C13 C9 3.9(4) . . . . ? C10 C9 C13 C8 -134.7(3) . . . . ? C15 C9 C13 C8 -13.0(4) . . . . ? C14 C9 C13 C8 105.1(4) . . . . ? S1 C9 C13 C8 176.5(3) . . . . ? C10 C9 C13 C12 46.4(4) . . . . ? C15 C9 C13 C12 168.0(3) . . . . ? C14 C9 C13 C12 -73.9(4) . . . . ? S1 C9 C13 C12 -2.4(2) . . . . ? C45 C44 C43 C42 0.5(6) . . . . ? C47 C42 C43 C44 -1.2(5) . . . . ? B1 C42 C43 C44 170.2(3) . . . . ? C32 C31 C30 C35 0.6(5) . . . . ? C32 C31 C30 P1 -178.5(3) . . . . ? C34 C35 C30 C31 0.4(5) . . . . ? C34 C35 C30 P1 179.4(3) . . . . ? C24 P1 C30 C31 150.5(3) . . . . ? C4 P1 C30 C31 -96.5(3) . . . . ? Pd1 P1 C30 C31 22.0(3) . . . . ? C24 P1 C30 C35 -28.5(3) . . . . ? C4 P1 C30 C35 84.4(3) . . . . ? Pd1 P1 C30 C35 -157.1(3) . . . . ? C41 C40 C39 C38 -2.0(7) . . . . ? C36 C37 C38 C39 0.1(8) . . . . ? C40 C39 C38 C37 1.4(8) . . . . ? C32 C33 C34 C35 1.6(6) . . . . ? C30 C35 C34 C33 -1.5(6) . . . . ? C24 C25 C26 C27 1.4(9) . . . . ? C28 C27 C26 C25 -1.4(9) . . . . ? C34 C33 C32 C31 -0.7(6) . . . . ? C30 C31 C32 C33 -0.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.67 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.031 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.085 # end Validation Reply Form # Attachment '- 2H_2CH2Cl2 de060m PdCl2(TXPH) NEW.cif' data_de060m _database_code_depnum_ccdc_archive 'CCDC 849795' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H39 Cl2 P Pd S, 2(C H2 Cl2)' _chemical_formula_sum 'C37 H43 Cl6 P Pd S' _chemical_formula_weight 869.84 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1463(18) _cell_length_b 12.547(2) _cell_length_c 13.883(2) _cell_angle_alpha 76.402(10) _cell_angle_beta 74.583(10) _cell_angle_gamma 81.960(10) _cell_volume 1975.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2538 _cell_measurement_theta_min 5.04 _cell_measurement_theta_max 49.61 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 885 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details SADABS _exptl_special_details ; A crystal of suitable size was selected and mounted on a goniometer head, then placed in the cold stream of the diffractometer. Data were collected with Mo K(alpha) radiation from a Siemens rotating anode, with a SMART 1K detector, at -100C. Omega and phi scans were used to ensure complete coverage. The data were corrected for absorption using SADABS (Bruker AXS 2003) and solved by direct methods in the triclinic space group P-1. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'parallel mirrors' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13584 _diffrn_reflns_av_R_equivalents 0.1027 _diffrn_reflns_av_sigmaI/netI 0.2146 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 24.75 _reflns_number_total 6736 _reflns_number_gt 3307 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were placed in idealized positions and updated with each cycle of refinement. Both of the ligand t-butyl groups exhibited rotational disorder (C16-19 and C20-23) over two positions; C16-19 in 54:46 ratio, and C20-23 in a 87:13 ratio. Two molecules of CH2Cl2 were also located and refined. The .res file for this complex is shown below and indicates other refinement details. The largest residual peak, at 0.66eA^-3, was associated with the Pd atom. 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^ > 2\s(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^)+(0.0787P)^2^+4.2189P] 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 0.0028(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6736 _refine_ls_number_parameters 412 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1966 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.60683(7) 0.38320(8) 0.17107(7) 0.0246(3) Uani 1 1 d . . . S1 S 0.4316(2) 0.4532(2) 0.1480(2) 0.0276(7) Uani 1 1 d . . . P1 P 0.6330(2) 0.5469(3) 0.1918(2) 0.0292(8) Uani 1 1 d . A . Cl2 Cl 0.7898(2) 0.3250(3) 0.1909(2) 0.0437(9) Uani 1 1 d . . . C1 C 0.2816(8) 0.7388(9) 0.2171(8) 0.030(3) Uani 1 1 d . A . H1A H 0.2065 0.7746 0.2298 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.5818(2) 0.2214(3) 0.1220(3) 0.0458(9) Uani 1 1 d . . . C2 C 0.3726(9) 0.7958(9) 0.2197(9) 0.035(3) Uani 1 1 d . . . C3 C 0.4813(8) 0.7373(10) 0.2118(9) 0.034(3) Uani 1 1 d . A . H3A H 0.5436 0.7709 0.2184 0.041 Uiso 1 1 calc R . . Cl3 Cl 0.5403(5) 0.1897(6) 0.4351(5) 0.156(3) Uani 1 1 d . . . C4 C 0.4984(7) 0.6291(9) 0.1941(8) 0.024(3) Uani 1 1 d . . . Cl4 Cl 0.6751(6) -0.0178(6) 0.4289(6) 0.205(4) Uani 1 1 d . . . C5 C 0.3210(8) 0.2831(9) 0.2899(8) 0.029(3) Uani 1 1 d . . . H5A H 0.3933 0.2416 0.2806 0.035 Uiso 1 1 calc R . . Cl5 Cl 0.8080(7) -0.0589(7) 0.0740(7) 0.203(4) Uani 1 1 d . . . C6 C 0.2250(8) 0.2349(10) 0.3570(8) 0.033(3) Uani 1 1 d . B . H6A H 0.2313 0.1606 0.3926 0.039 Uiso 1 1 calc R . . Cl6 Cl 0.9337(6) 0.0001(7) 0.1959(6) 0.180(3) Uani 1 1 d . . . C7 C 0.1197(8) 0.2976(10) 0.3710(9) 0.031(3) Uani 1 1 d . . . C8 C 0.1127(8) 0.4038(9) 0.3188(8) 0.029(3) Uani 1 1 d . A . H8A H 0.0402 0.4449 0.3283 0.035 Uiso 1 1 calc R . . C9 C 0.1960(8) 0.5739(9) 0.1929(9) 0.031(3) Uani 1 1 d . A . C10 C 0.2944(8) 0.6341(9) 0.1972(8) 0.028(3) Uani 1 1 d . . . C11 C 0.4047(7) 0.5823(9) 0.1857(8) 0.024(3) Uani 1 1 d . A . C12 C 0.3121(7) 0.3890(9) 0.2377(8) 0.024(3) Uani 1 1 d . A . C13 C 0.2066(7) 0.4550(9) 0.2521(8) 0.023(3) Uani 1 1 d . . . C14 C 0.2059(8) 0.5755(9) 0.0796(9) 0.035(3) Uani 1 1 d . . . H14C H 0.2793 0.5376 0.0511 0.052 Uiso 1 1 calc R A . H14B H 0.2016 0.6518 0.0418 0.052 Uiso 1 1 calc R . . H14A H 0.1430 0.5380 0.0739 0.052 Uiso 1 1 calc R . . C15 C 0.0781(8) 0.6350(9) 0.2349(9) 0.034(3) Uani 1 1 d . . . H15C H 0.0742 0.7104 0.1949 0.051 Uiso 1 1 calc R A . H15B H 0.0702 0.6367 0.3066 0.051 Uiso 1 1 calc R . . H15A H 0.0161 0.5962 0.2295 0.051 Uiso 1 1 calc R . . C16A C 0.3579(9) 0.9146(10) 0.2267(11) 0.045(4) Uani 0.46(3) 1 d PD A 1 C17A C 0.453(3) 0.943(3) 0.270(3) 0.090(5) Uani 0.46(3) 1 d PD A 1 H17A H 0.4419 1.0215 0.2732 0.134 Uiso 0.46(3) 1 calc PR A 1 H17B H 0.5284 0.9283 0.2255 0.134 Uiso 0.46(3) 1 calc PR A 1 H17C H 0.4492 0.8986 0.3388 0.134 Uiso 0.46(3) 1 calc PR A 1 C18A C 0.396(3) 0.967(3) 0.1173(18) 0.090(5) Uani 0.46(3) 1 d PD A 1 H18A H 0.3912 1.0468 0.1099 0.134 Uiso 0.46(3) 1 calc PR A 1 H18B H 0.3456 0.9486 0.0794 0.134 Uiso 0.46(3) 1 calc PR A 1 H18C H 0.4747 0.9395 0.0902 0.134 Uiso 0.46(3) 1 calc PR A 1 C19A C 0.2423(17) 0.960(3) 0.278(3) 0.090(5) Uani 0.46(3) 1 d PD A 1 H19A H 0.2445 1.0375 0.2774 0.134 Uiso 0.46(3) 1 calc PR A 1 H19B H 0.2207 0.9188 0.3489 0.134 Uiso 0.46(3) 1 calc PR A 1 H19C H 0.1858 0.9519 0.2418 0.134 Uiso 0.46(3) 1 calc PR A 1 C16B C 0.3579(9) 0.9146(10) 0.2267(11) 0.045(4) Uani 0.54(3) 1 d PD A 2 C17B C 0.399(3) 0.918(2) 0.323(2) 0.090(5) Uani 0.54(3) 1 d PD A 2 H17D H 0.3921 0.9945 0.3311 0.134 Uiso 0.54(3) 1 calc PR A 2 H17E H 0.4792 0.8885 0.3146 0.134 Uiso 0.54(3) 1 calc PR A 2 H17F H 0.3516 0.8739 0.3835 0.134 Uiso 0.54(3) 1 calc PR A 2 C18B C 0.437(2) 0.985(2) 0.145(2) 0.090(5) Uani 0.54(3) 1 d PD A 2 H18D H 0.4228 1.0607 0.1545 0.134 Uiso 0.54(3) 1 calc PR A 2 H18E H 0.4258 0.9818 0.0784 0.134 Uiso 0.54(3) 1 calc PR A 2 H18F H 0.5166 0.9579 0.1474 0.134 Uiso 0.54(3) 1 calc PR A 2 C19B C 0.2345(14) 0.957(2) 0.239(3) 0.090(5) Uani 0.54(3) 1 d PD A 2 H19D H 0.2261 1.0347 0.2429 0.134 Uiso 0.54(3) 1 calc PR A 2 H19E H 0.1884 0.9147 0.3016 0.134 Uiso 0.54(3) 1 calc PR A 2 H19F H 0.2083 0.9493 0.1801 0.134 Uiso 0.54(3) 1 calc PR A 2 C20A C 0.0136(9) 0.2420(10) 0.4410(9) 0.036(3) Uani 0.135(13) 1 d PD B 1 C21A C 0.043(6) 0.125(3) 0.500(6) 0.062(3) Uani 0.135(13) 1 d PD B 1 H21A H -0.0282 0.0935 0.5421 0.093 Uiso 0.135(13) 1 calc PR B 1 H21B H 0.0931 0.1287 0.5430 0.093 Uiso 0.135(13) 1 calc PR B 1 H21C H 0.0814 0.0785 0.4507 0.093 Uiso 0.135(13) 1 calc PR B 1 C22A C -0.072(5) 0.241(7) 0.380(5) 0.062(3) Uani 0.135(13) 1 d PD B 1 H22A H -0.1401 0.2065 0.4250 0.093 Uiso 0.135(13) 1 calc PR B 1 H22B H -0.0377 0.2000 0.3259 0.093 Uiso 0.135(13) 1 calc PR B 1 H22C H -0.0947 0.3171 0.3489 0.093 Uiso 0.135(13) 1 calc PR B 1 C23A C -0.041(7) 0.317(6) 0.516(5) 0.062(3) Uani 0.135(13) 1 d PD B 1 H23A H -0.1097 0.2862 0.5631 0.093 Uiso 0.135(13) 1 calc PR B 1 H23B H -0.0626 0.3902 0.4775 0.093 Uiso 0.135(13) 1 calc PR B 1 H23C H 0.0137 0.3243 0.5539 0.093 Uiso 0.135(13) 1 calc PR B 1 C20B C 0.0136(9) 0.2420(10) 0.4410(9) 0.036(3) Uani 0.865(13) 1 d PD B 2 C21B C 0.0376(11) 0.1889(14) 0.5469(12) 0.062(3) Uani 0.865(13) 1 d PD B 2 H21D H -0.0300 0.1534 0.5917 0.093 Uiso 0.865(13) 1 calc PR B 2 H21E H 0.0547 0.2460 0.5771 0.093 Uiso 0.865(13) 1 calc PR B 2 H21F H 0.1032 0.1339 0.5388 0.093 Uiso 0.865(13) 1 calc PR B 2 C22B C -0.0174(12) 0.1549(13) 0.3958(13) 0.062(3) Uani 0.865(13) 1 d PD B 2 H22D H -0.0851 0.1208 0.4420 0.093 Uiso 0.865(13) 1 calc PR B 2 H22E H 0.0470 0.0986 0.3867 0.093 Uiso 0.865(13) 1 calc PR B 2 H22F H -0.0340 0.1889 0.3295 0.093 Uiso 0.865(13) 1 calc PR B 2 C23B C -0.0941(11) 0.3223(12) 0.4595(14) 0.062(3) Uani 0.865(13) 1 d PD B 2 H23D H -0.1583 0.2822 0.5053 0.093 Uiso 0.865(13) 1 calc PR B 2 H23E H -0.1134 0.3563 0.3942 0.093 Uiso 0.865(13) 1 calc PR B 2 H23F H -0.0794 0.3796 0.4907 0.093 Uiso 0.865(13) 1 calc PR B 2 C24 C 0.6702(9) 0.5537(11) 0.3082(9) 0.037(3) Uani 1 1 d . . . C25 C 0.6402(9) 0.4692(13) 0.3930(11) 0.055(4) Uani 1 1 d . A . H25A H 0.6119 0.4054 0.3858 0.066 Uiso 1 1 calc R . . C26 C 0.6513(11) 0.4771(15) 0.4883(11) 0.066(5) Uani 1 1 d . . . H26A H 0.6260 0.4225 0.5477 0.079 Uiso 1 1 calc R A . C27 C 0.7013(12) 0.5693(16) 0.4921(12) 0.064(5) Uani 1 1 d . A . H27A H 0.7171 0.5734 0.5546 0.077 Uiso 1 1 calc R . . C28 C 0.7278(12) 0.6514(15) 0.4122(15) 0.074(5) Uani 1 1 d . . . H28A H 0.7561 0.7151 0.4196 0.089 Uiso 1 1 calc R A . C29 C 0.7143(10) 0.6446(12) 0.3177(11) 0.050(4) Uani 1 1 d . A . H29A H 0.7353 0.7024 0.2600 0.060 Uiso 1 1 calc R . . C30 C 0.7351(8) 0.6210(9) 0.0863(9) 0.030(3) Uani 1 1 d . . . C31 C 0.8514(8) 0.5997(10) 0.0815(9) 0.032(3) Uani 1 1 d . A . H31A H 0.8775 0.5507 0.1359 0.038 Uiso 1 1 calc R . . C32 C 0.9289(9) 0.6506(11) -0.0035(10) 0.043(3) Uani 1 1 d . . . H32A H 1.0086 0.6368 -0.0071 0.051 Uiso 1 1 calc R A . C33 C 0.8914(9) 0.7218(10) -0.0839(10) 0.041(3) Uani 1 1 d . A . H33A H 0.9448 0.7563 -0.1426 0.049 Uiso 1 1 calc R . . C34 C 0.7766(10) 0.7409(10) -0.0767(9) 0.042(3) Uani 1 1 d . . . H34A H 0.7507 0.7900 -0.1311 0.051 Uiso 1 1 calc R A . C35 C 0.6973(9) 0.6920(9) 0.0062(9) 0.030(3) Uani 1 1 d . A . H35A H 0.6177 0.7063 0.0089 0.036 Uiso 1 1 calc R . . C37 C 0.8526(16) 0.0471(15) 0.1082(17) 0.123(8) Uani 1 1 d . . . H37B H 0.7848 0.0934 0.1375 0.147 Uiso 1 1 calc R . . H37A H 0.8982 0.0934 0.0467 0.147 Uiso 1 1 calc R . . C36 C 0.6474(18) 0.1054(16) 0.3697(18) 0.142(9) Uani 1 1 d . . . H36B H 0.6257 0.1005 0.3071 0.171 Uiso 1 1 calc R . . H36A H 0.7192 0.1428 0.3477 0.171 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0175(4) 0.0277(6) 0.0263(6) -0.0091(4) -0.0003(4) 0.0025(3) S1 0.0218(13) 0.0296(19) 0.0306(19) -0.0109(16) -0.0015(13) -0.0009(13) P1 0.0203(13) 0.040(2) 0.029(2) -0.0133(17) -0.0047(13) 0.0005(14) Cl2 0.0277(14) 0.055(2) 0.044(2) -0.0077(19) -0.0076(15) 0.0027(15) C1 0.025(5) 0.025(7) 0.037(8) -0.002(6) -0.002(5) -0.010(5) Cl1 0.0352(15) 0.039(2) 0.062(2) -0.0217(18) -0.0012(15) 0.0000(14) C2 0.033(6) 0.030(7) 0.036(8) -0.004(6) -0.005(6) 0.002(5) C3 0.020(5) 0.041(8) 0.041(8) -0.008(7) -0.007(5) -0.004(5) Cl3 0.124(4) 0.166(6) 0.149(6) 0.031(5) -0.048(4) 0.005(4) C4 0.015(5) 0.032(7) 0.024(7) -0.008(6) 0.001(5) -0.003(5) Cl4 0.155(6) 0.190(8) 0.187(8) 0.060(6) -0.024(5) 0.053(5) C5 0.028(6) 0.030(7) 0.029(7) -0.002(6) -0.010(5) 0.000(5) Cl5 0.194(7) 0.216(9) 0.266(10) -0.158(8) -0.101(7) 0.030(6) C6 0.038(6) 0.031(7) 0.027(7) -0.009(6) -0.004(6) 0.001(5) Cl6 0.159(6) 0.225(8) 0.185(8) -0.065(6) -0.101(6) 0.042(5) C7 0.031(6) 0.034(8) 0.026(7) -0.011(6) -0.001(5) -0.004(5) C8 0.032(6) 0.031(7) 0.034(8) -0.007(6) -0.024(6) 0.004(5) C9 0.021(5) 0.029(7) 0.046(8) -0.012(6) -0.012(5) 0.002(5) C10 0.017(5) 0.033(7) 0.028(7) -0.007(6) 0.003(5) -0.004(5) C11 0.013(5) 0.039(7) 0.018(6) -0.009(6) 0.002(4) -0.003(5) C12 0.017(5) 0.037(7) 0.018(7) -0.018(6) 0.002(5) 0.002(5) C13 0.019(5) 0.026(7) 0.025(7) -0.007(6) -0.004(5) -0.005(5) C14 0.030(6) 0.034(7) 0.040(8) -0.009(6) -0.012(6) 0.004(5) C15 0.028(5) 0.028(7) 0.049(9) -0.014(7) -0.014(6) 0.005(5) C16A 0.031(6) 0.033(8) 0.066(10) -0.018(8) 0.001(6) -0.003(6) C17A 0.064(8) 0.049(8) 0.148(16) -0.038(10) 0.002(8) -0.004(6) C18A 0.064(8) 0.049(8) 0.148(16) -0.038(10) 0.002(8) -0.004(6) C19A 0.064(8) 0.049(8) 0.148(16) -0.038(10) 0.002(8) -0.004(6) C16B 0.031(6) 0.033(8) 0.066(10) -0.018(8) 0.001(6) -0.003(6) C17B 0.064(8) 0.049(8) 0.148(16) -0.038(10) 0.002(8) -0.004(6) C18B 0.064(8) 0.049(8) 0.148(16) -0.038(10) 0.002(8) -0.004(6) C19B 0.064(8) 0.049(8) 0.148(16) -0.038(10) 0.002(8) -0.004(6) C20A 0.034(6) 0.041(8) 0.034(8) -0.009(7) -0.002(6) -0.013(6) C21A 0.037(5) 0.063(7) 0.073(8) -0.007(6) 0.014(5) -0.022(5) C22A 0.037(5) 0.063(7) 0.073(8) -0.007(6) 0.014(5) -0.022(5) C23A 0.037(5) 0.063(7) 0.073(8) -0.007(6) 0.014(5) -0.022(5) C20B 0.034(6) 0.041(8) 0.034(8) -0.009(7) -0.002(6) -0.013(6) C21B 0.037(5) 0.063(7) 0.073(8) -0.007(6) 0.014(5) -0.022(5) C22B 0.037(5) 0.063(7) 0.073(8) -0.007(6) 0.014(5) -0.022(5) C23B 0.037(5) 0.063(7) 0.073(8) -0.007(6) 0.014(5) -0.022(5) C24 0.033(6) 0.056(9) 0.027(8) -0.019(7) -0.015(6) 0.011(6) C25 0.037(7) 0.098(13) 0.035(9) -0.030(9) -0.010(7) 0.007(7) C26 0.038(7) 0.098(14) 0.042(10) -0.002(10) 0.001(7) 0.013(8) C27 0.062(9) 0.108(15) 0.032(10) -0.036(10) -0.021(8) 0.021(10) C28 0.059(9) 0.085(14) 0.090(15) -0.032(12) -0.032(10) 0.006(9) C29 0.055(8) 0.065(10) 0.045(10) -0.022(8) -0.024(7) -0.011(7) C30 0.024(5) 0.029(7) 0.040(8) -0.016(6) -0.002(5) -0.006(5) C31 0.028(5) 0.046(8) 0.026(7) -0.014(6) -0.005(5) -0.012(6) C32 0.024(6) 0.067(10) 0.040(9) -0.006(8) -0.013(6) -0.010(6) C33 0.031(6) 0.057(9) 0.036(8) -0.021(7) 0.008(6) -0.018(6) C34 0.063(8) 0.036(8) 0.029(8) 0.001(7) -0.018(7) -0.004(7) C35 0.029(6) 0.034(7) 0.025(7) -0.004(6) -0.009(6) 0.002(5) C37 0.131(16) 0.087(15) 0.19(2) -0.085(16) -0.086(16) 0.049(12) C36 0.128(17) 0.114(19) 0.15(2) 0.026(17) -0.036(16) 0.028(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.216(3) . ? Pd1 S1 2.260(3) . ? Pd1 Cl2 2.308(3) . ? Pd1 Cl1 2.369(3) . ? S1 C11 1.779(11) . ? S1 C12 1.789(10) . ? P1 C4 1.803(9) . ? P1 C30 1.808(11) . ? P1 C24 1.813(12) . ? C1 C10 1.384(14) . ? C1 C2 1.410(14) . ? C1 H1A 0.9500 . ? C2 C3 1.409(14) . ? C2 C16A 1.499(15) . ? C3 C4 1.414(14) . ? C3 H3A 0.9500 . ? Cl3 C36 1.75(2) . ? C4 C11 1.394(13) . ? Cl4 C36 1.606(18) . ? C5 C12 1.360(14) . ? C5 C6 1.396(14) . ? C5 H5A 0.9500 . ? Cl5 C37 1.710(17) . ? C6 C7 1.398(14) . ? C6 H6A 0.9500 . ? Cl6 C37 1.714(18) . ? C7 C8 1.362(14) . ? C7 C20A 1.535(14) . ? C8 C13 1.390(14) . ? C8 H8A 0.9500 . ? C9 C10 1.521(14) . ? C9 C13 1.531(14) . ? C9 C14 1.540(15) . ? C9 C15 1.561(13) . ? C10 C11 1.392(13) . ? C12 C13 1.419(13) . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16A C18A 1.48(2) . ? C16A C19A 1.495(17) . ? C16A C17A 1.56(2) . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20A C22A 1.51(3) . ? C20A C23A 1.53(2) . ? C20A C21A 1.54(3) . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24 C29 1.372(16) . ? C24 C25 1.392(17) . ? C25 C26 1.391(18) . ? C25 H25A 0.9500 . ? C26 C27 1.40(2) . ? C26 H26A 0.9500 . ? C27 C28 1.33(2) . ? C27 H27A 0.9500 . ? C28 C29 1.388(19) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.388(13) . ? C30 C35 1.390(14) . ? C31 C32 1.381(15) . ? C31 H31A 0.9500 . ? C32 C33 1.392(16) . ? C32 H32A 0.9500 . ? C33 C34 1.362(15) . ? C33 H33A 0.9500 . ? C34 C35 1.368(15) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C37 H37B 0.9900 . ? C37 H37A 0.9900 . ? C36 H36B 0.9900 . ? C36 H36A 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 P1 Pd1 S1 87.98(11) . . ? P1 Pd1 Cl2 88.10(11) . . ? S1 Pd1 Cl2 175.72(13) . . ? P1 Pd1 Cl1 171.14(13) . . ? S1 Pd1 Cl1 89.19(11) . . ? Cl2 Pd1 Cl1 94.44(11) . . ? C11 S1 C12 97.3(5) . . ? C11 S1 Pd1 106.5(3) . . ? C12 S1 Pd1 116.2(4) . . ? C4 P1 C30 105.1(5) . . ? C4 P1 C24 105.3(5) . . ? C30 P1 C24 107.3(6) . . ? C4 P1 Pd1 106.7(3) . . ? C30 P1 Pd1 113.6(4) . . ? C24 P1 Pd1 117.8(5) . . ? C10 C1 C2 124.4(10) . . ? C10 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C3 C2 C1 117.1(11) . . ? C3 C2 C16A 120.2(10) . . ? C1 C2 C16A 122.7(10) . . ? C2 C3 C4 120.5(10) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C11 C4 C3 118.1(9) . . ? C11 C4 P1 119.3(8) . . ? C3 C4 P1 122.5(7) . . ? C12 C5 C6 120.7(10) . . ? C12 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C7 118.9(11) . . ? C5 C6 H6A 120.5 . . ? C7 C6 H6A 120.5 . . ? C8 C7 C6 119.5(10) . . ? C8 C7 C20A 122.0(10) . . ? C6 C7 C20A 118.5(10) . . ? C7 C8 C13 123.2(10) . . ? C7 C8 H8A 118.4 . . ? C13 C8 H8A 118.4 . . ? C10 C9 C13 109.3(8) . . ? C10 C9 C14 107.3(9) . . ? C13 C9 C14 109.9(9) . . ? C10 C9 C15 110.8(9) . . ? C13 C9 C15 111.7(9) . . ? C14 C9 C15 107.7(8) . . ? C1 C10 C11 115.6(9) . . ? C1 C10 C9 124.0(9) . . ? C11 C10 C9 120.3(10) . . ? C10 C11 C4 124.0(10) . . ? C10 C11 S1 118.5(8) . . ? C4 C11 S1 117.3(7) . . ? C5 C12 C13 121.4(9) . . ? C5 C12 S1 122.3(7) . . ? C13 C12 S1 116.3(8) . . ? C8 C13 C12 116.2(10) . . ? C8 C13 C9 122.1(9) . . ? C12 C13 C9 121.5(9) . . ? C9 C14 H14C 109.5 . . ? C9 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C9 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C9 C15 H15C 109.5 . . ? C9 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C9 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C18A C16A C19A 113.6(15) . . ? C18A C16A C2 100.2(18) . . ? C19A C16A C2 117.9(17) . . ? C18A C16A C17A 101.2(15) . . ? C19A C16A C17A 111.0(16) . . ? C2 C16A C17A 111.2(14) . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C16A C18A H18A 109.5 . . ? C16A C18A H18B 109.4 . . ? H18A C18A H18B 109.5 . . ? C16A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C16A C19A H19A 109.5 . . ? C16A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C16A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? H17D C17B H17E 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? H18D C18B H18E 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? H19D C19B H19E 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C22A C20A C23A 107(3) . . ? C22A C20A C7 110(3) . . ? C23A C20A C7 105(3) . . ? C22A C20A C21A 111(3) . . ? C23A C20A C21A 110(3) . . ? C7 C20A C21A 113(3) . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20A C22A H22A 109.5 . . ? C20A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C20A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C20A C23A H23A 109.5 . . ? C20A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C20A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? H21D C21B H21E 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? H22D C22B H22E 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? H23D C23B H23E 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C29 C24 C25 119.8(12) . . ? C29 C24 P1 121.9(11) . . ? C25 C24 P1 117.9(10) . . ? C26 C25 C24 120.7(15) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C25 C26 C27 116.7(15) . . ? C25 C26 H26A 121.7 . . ? C27 C26 H26A 121.7 . . ? C28 C27 C26 122.7(15) . . ? C28 C27 H27A 118.6 . . ? C26 C27 H27A 118.6 . . ? C27 C28 C29 120.3(16) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C24 C29 C28 119.5(14) . . ? C24 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C31 C30 C35 120.3(10) . . ? C31 C30 P1 119.7(9) . . ? C35 C30 P1 119.7(8) . . ? C32 C31 C30 119.1(11) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.4 . . ? C31 C32 C33 120.8(10) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C34 C33 C32 118.5(11) . . ? C34 C33 H33A 120.7 . . ? C32 C33 H33A 120.7 . . ? C33 C34 C35 122.4(12) . . ? C33 C34 H34A 118.8 . . ? C35 C34 H34A 118.8 . . ? C34 C35 C30 118.8(10) . . ? C34 C35 H35A 120.6 . . ? C30 C35 H35A 120.6 . . ? Cl5 C37 Cl6 111.7(11) . . ? Cl5 C37 H37B 109.3 . . ? Cl6 C37 H37B 109.3 . . ? Cl5 C37 H37A 109.3 . . ? Cl6 C37 H37A 109.3 . . ? H37B C37 H37A 107.9 . . ? Cl4 C36 Cl3 118.0(14) . . ? Cl4 C36 H36B 107.8 . . ? Cl3 C36 H36B 107.8 . . ? Cl4 C36 H36A 107.8 . . ? Cl3 C36 H36A 107.8 . . ? H36B C36 H36A 107.1 . . ? 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 Pd1 S1 C11 -12.0(4) . . . . ? Cl1 Pd1 S1 C11 176.4(4) . . . . ? P1 Pd1 S1 C12 -119.1(4) . . . . ? Cl1 Pd1 S1 C12 69.3(4) . . . . ? S1 Pd1 P1 C4 6.9(4) . . . . ? Cl2 Pd1 P1 C4 -174.9(4) . . . . ? S1 Pd1 P1 C30 -108.5(4) . . . . ? Cl2 Pd1 P1 C30 69.8(4) . . . . ? S1 Pd1 P1 C24 124.8(4) . . . . ? Cl2 Pd1 P1 C24 -56.9(4) . . . . ? C10 C1 C2 C3 -6.7(17) . . . . ? C10 C1 C2 C16A 171.1(11) . . . . ? C1 C2 C3 C4 4.7(16) . . . . ? C16A C2 C3 C4 -173.1(11) . . . . ? C2 C3 C4 C11 -0.5(16) . . . . ? C2 C3 C4 P1 -175.7(8) . . . . ? C30 P1 C4 C11 122.3(9) . . . . ? C24 P1 C4 C11 -124.6(9) . . . . ? Pd1 P1 C4 C11 1.3(9) . . . . ? C30 P1 C4 C3 -62.6(10) . . . . ? C24 P1 C4 C3 50.5(11) . . . . ? Pd1 P1 C4 C3 176.4(8) . . . . ? C12 C5 C6 C7 -1.0(16) . . . . ? C5 C6 C7 C8 0.3(16) . . . . ? C5 C6 C7 C20A 177.1(10) . . . . ? C6 C7 C8 C13 -1.0(17) . . . . ? C20A C7 C8 C13 -177.6(10) . . . . ? C2 C1 C10 C11 4.0(17) . . . . ? C2 C1 C10 C9 -179.0(11) . . . . ? C13 C9 C10 C1 -135.0(11) . . . . ? C14 C9 C10 C1 105.8(12) . . . . ? C15 C9 C10 C1 -11.4(16) . . . . ? C13 C9 C10 C11 41.9(14) . . . . ? C14 C9 C10 C11 -77.3(12) . . . . ? C15 C9 C10 C11 165.5(10) . . . . ? C1 C10 C11 C4 0.7(16) . . . . ? C9 C10 C11 C4 -176.4(10) . . . . ? C1 C10 C11 S1 -174.1(8) . . . . ? C9 C10 C11 S1 8.7(14) . . . . ? C3 C4 C11 C10 -2.4(16) . . . . ? P1 C4 C11 C10 172.9(8) . . . . ? C3 C4 C11 S1 172.5(8) . . . . ? P1 C4 C11 S1 -12.1(12) . . . . ? C12 S1 C11 C10 -48.1(9) . . . . ? Pd1 S1 C11 C10 -168.3(8) . . . . ? C12 S1 C11 C4 136.7(8) . . . . ? Pd1 S1 C11 C4 16.6(9) . . . . ? C6 C5 C12 C13 2.2(17) . . . . ? C6 C5 C12 S1 -178.1(8) . . . . ? C11 S1 C12 C5 -137.4(9) . . . . ? Pd1 S1 C12 C5 -24.9(11) . . . . ? C11 S1 C12 C13 42.3(8) . . . . ? Pd1 S1 C12 C13 154.8(7) . . . . ? C7 C8 C13 C12 2.1(16) . . . . ? C7 C8 C13 C9 178.9(10) . . . . ? C5 C12 C13 C8 -2.7(15) . . . . ? S1 C12 C13 C8 177.6(8) . . . . ? C5 C12 C13 C9 -179.5(10) . . . . ? S1 C12 C13 C9 0.8(13) . . . . ? C10 C9 C13 C8 136.0(10) . . . . ? C14 C9 C13 C8 -106.5(11) . . . . ? C15 C9 C13 C8 13.0(14) . . . . ? C10 C9 C13 C12 -47.4(14) . . . . ? C14 C9 C13 C12 70.1(12) . . . . ? C15 C9 C13 C12 -170.4(9) . . . . ? C3 C2 C16A C18A 82(2) . . . . ? C1 C2 C16A C18A -96(2) . . . . ? C3 C2 C16A C19A -154.3(19) . . . . ? C1 C2 C16A C19A 28(2) . . . . ? C3 C2 C16A C17A -24(2) . . . . ? C1 C2 C16A C17A 158(2) . . . . ? C8 C7 C20A C22A 60(4) . . . . ? C6 C7 C20A C22A -117(4) . . . . ? C8 C7 C20A C23A -54(4) . . . . ? C6 C7 C20A C23A 129(4) . . . . ? C8 C7 C20A C21A -175(4) . . . . ? C6 C7 C20A C21A 8(4) . . . . ? C4 P1 C24 C29 -77.1(10) . . . . ? C30 P1 C24 C29 34.5(11) . . . . ? Pd1 P1 C24 C29 164.2(8) . . . . ? C4 P1 C24 C25 95.4(9) . . . . ? C30 P1 C24 C25 -153.1(9) . . . . ? Pd1 P1 C24 C25 -23.4(10) . . . . ? C29 C24 C25 C26 1.9(17) . . . . ? P1 C24 C25 C26 -170.7(9) . . . . ? C24 C25 C26 C27 -4.6(18) . . . . ? C25 C26 C27 C28 6(2) . . . . ? C26 C27 C28 C29 -5(2) . . . . ? C25 C24 C29 C28 -0.4(18) . . . . ? P1 C24 C29 C28 171.9(10) . . . . ? C27 C28 C29 C24 2(2) . . . . ? C4 P1 C30 C31 160.4(9) . . . . ? C24 P1 C30 C31 48.8(10) . . . . ? Pd1 P1 C30 C31 -83.3(9) . . . . ? C4 P1 C30 C35 -25.1(10) . . . . ? C24 P1 C30 C35 -136.7(9) . . . . ? Pd1 P1 C30 C35 91.2(9) . . . . ? C35 C30 C31 C32 0.5(17) . . . . ? P1 C30 C31 C32 175.0(9) . . . . ? C30 C31 C32 C33 -0.5(18) . . . . ? C31 C32 C33 C34 0.5(18) . . . . ? C32 C33 C34 C35 -0.6(18) . . . . ? C33 C34 C35 C30 0.6(18) . . . . ? C31 C30 C35 C34 -0.6(17) . . . . ? P1 C30 C35 C34 -175.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.664 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.140 # Attachment '- 4B_1_31CH2Cl2 so02 PtI2(TXPB) NEW.cif' data_so02 _database_code_depnum_ccdc_archive 'CCDC 849796' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H48 B I2 P Pt S, 1.31(C H2 Cl2)' _chemical_formula_sum 'C48.31 H50.62 B Cl2.62 I2 P Pt S' _chemical_formula_weight 1246.93 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' B B 0.0013 0.0007 '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' I I -0.4742 1.8119 '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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.18(2) _cell_length_b 9.043(8) _cell_length_c 24.75(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4964(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 512 _cell_measurement_theta_min 6.173 _cell_measurement_theta_max 37.558 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2410 _exptl_absorpt_coefficient_mu 4.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details SADABS _exptl_special_details ; Several attempts to grow high-quality crystals were made; the best crystal from the lot was chosen. A crystal of suitable size was selected and mounted on a goniometer head, then placed in the cold stream of the diffractometer. Data were collected with Mo K(alpha) radiation from a Siemens rotating anode, with a SMART 1K detector, at -100C. Omega and phi scans were used to ensure complete coverage. Data were corrected for absorption using the program SADABS (Bruker AXS 2003) and solved in the orthorhombic space group Pna2(1). The Rint for this sample was greater than 0.1; data were checked to confirm space group choice using PLATON addsym. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'parallel mirrors' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34768 _diffrn_reflns_av_R_equivalents 0.1803 _diffrn_reflns_av_sigmaI/netI 0.2059 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.36 _reflns_number_total 9159 _reflns_number_gt 5008 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were placed in idealized positions and updated with each cycle of refinement. Two molecules of CH2Cl2 were located and refined with occupancies of 0.60 and 0.70. No void calculation was applied. The .res file for this complex is shown below and indicates other refinement details. The largest residual peak, at 1.26eA^-3, was associated with the Pt atom. Other residual peaks were associated with Pt and/or the I ligands. TITL so02 in Pna2(1) CELL 0.71073 22.1810 9.0433 24.7456 90.000 90.000 90.000 ZERR 4.00 0.0226 0.0082 0.0198 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H B P S CL I PT UNIT 193 202 4 4 4 10 8 4 MERG 2 OMIT -3.00 180.00 ISOR 0.01 C15 C42 C12 C11 ISOR 0.05 C10 C43 ISOR 0.01 C5 C4 C7 C13 ISOR 0.01 C49 ISOR 0.01 CL3 CL4 ISOR 0.01 C48 ISOR 0.01 CL1 CL2 SUMP 1.31 0.01 1 2 1 3 DFIX 1.77 0.005 C49 CL3 DFIX 1.77 0.005 C49 CL4 DFIX 1.77 0.005 C48 CL1 DFIX 1.77 0.005 C48 CL2 DFIX 2.9 0.005 CL1 CL2 DFIX 2.9 0.005 CL3 CL4 EADP CL1 CL2 EADP CL3 CL4 SIMU 0.01 BIND I1 B1 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -100.00 WGHT 0.053500 18.704201 EXTI 0.001011 FVAR 0.17196 0.60023 0.70195 PT1 8 0.538502 0.362258 0.686804 11.00000 0.01924 0.02722 = 0.02461 0.00244 -0.00047 -0.00001 I1 7 0.605025 0.209378 0.755212 11.00000 0.02342 0.03679 = 0.03083 0.00304 0.00034 0.00108 S1 5 0.459094 0.230861 0.716196 11.00000 0.02484 0.02616 = 0.02675 0.00368 -0.00540 0.00077 P1 4 0.476215 0.476007 0.630108 11.00000 0.01752 0.02545 = 0.02587 0.00331 0.00383 -0.00248 C1 1 0.288296 0.352696 0.689622 11.00000 0.03017 0.03634 = 0.03217 0.00204 0.00552 0.00623 AFIX 43 H1A 2 0.249031 0.319164 0.698837 11.00000 -1.20000 AFIX 0 B1 3 0.533571 0.348659 0.830710 11.00000 0.03403 0.04155 = 0.02903 -0.00077 -0.00389 -0.00283 I2 7 0.633243 0.481906 0.643995 11.00000 0.02349 0.04344 = 0.04766 0.01136 0.00484 -0.00307 C2 1 0.292802 0.479132 0.658170 11.00000 0.02878 0.02894 = 0.03001 -0.00057 0.00646 0.00186 C3 1 0.351282 0.516441 0.636617 11.00000 0.02596 0.02579 = 0.02296 0.00275 -0.00333 -0.00158 AFIX 43 H3A 2 0.355807 0.594370 0.611194 11.00000 -1.20000 AFIX 0 C4 1 0.400888 0.435242 0.654059 11.00000 0.02118 0.02837 = 0.02349 0.00333 0.00499 -0.00503 C5 1 0.474613 0.251142 0.829556 11.00000 0.02281 0.03263 = 0.02746 -0.00115 -0.00205 -0.00473 C6 1 0.452531 0.215446 0.881711 11.00000 0.02293 0.03490 = 0.02936 -0.00094 0.00064 -0.00656 AFIX 43 H6A 2 0.478634 0.224527 0.911966 11.00000 -1.20000 AFIX 0 C7 1 0.392297 0.166384 0.889898 11.00000 0.02862 0.03921 = 0.03309 -0.00255 0.00545 -0.00296 C8 1 0.357396 0.145976 0.845265 11.00000 0.03293 0.03066 = 0.03514 -0.00168 0.00802 -0.00672 AFIX 43 H8A 2 0.316888 0.115181 0.850631 11.00000 -1.20000 AFIX 0 C9 1 0.336274 0.135890 0.745266 11.00000 0.03203 0.03112 = 0.03027 0.00606 0.00971 -0.00037 C13 1 0.376558 0.166725 0.793023 11.00000 0.02654 0.02624 = 0.02919 0.00168 0.00967 -0.00135 C12 1 0.435507 0.223421 0.785073 11.00000 0.02105 0.02642 = 0.02394 0.00436 0.01004 -0.00243 C11 1 0.396861 0.318140 0.691680 11.00000 0.03132 0.03492 = 0.02694 0.00640 0.00314 0.00191 C10 1 0.336605 0.272305 0.708444 11.00000 0.03103 0.03023 = 0.02270 0.00298 0.00371 0.00026 C14 1 0.353064 -0.004613 0.714219 11.00000 0.05320 0.03181 = 0.03607 -0.00715 -0.01937 0.00756 AFIX 33 H14A 2 0.395133 0.001760 0.702344 11.00000 -1.50000 H14B 2 0.326751 -0.014772 0.682623 11.00000 -1.50000 H14C 2 0.348057 -0.090773 0.737816 11.00000 -1.50000 AFIX 0 C15 1 0.269164 0.114517 0.764154 11.00000 0.04017 0.03508 = 0.03336 0.01967 -0.00360 -0.00796 AFIX 33 H15A 2 0.255938 0.202374 0.784078 11.00000 -1.50000 H15B 2 0.266450 0.027575 0.787669 11.00000 -1.50000 H15C 2 0.243271 0.100279 0.732489 11.00000 -1.50000 AFIX 0 C16 1 0.238376 0.568250 0.643401 11.00000 0.03376 0.03293 = 0.03530 0.01039 0.00717 0.00640 C17 1 0.250670 0.693761 0.603124 11.00000 0.03524 0.04121 = 0.03201 0.01049 0.01745 0.01161 AFIX 33 H17A 2 0.279178 0.764122 0.619068 11.00000 -1.50000 H17B 2 0.212817 0.744682 0.594703 11.00000 -1.50000 H17C 2 0.267862 0.652615 0.569886 11.00000 -1.50000 AFIX 0 C18 1 0.189198 0.463938 0.616454 11.00000 0.03115 0.04583 = 0.03088 0.00900 -0.00259 -0.01103 AFIX 33 H18A 2 0.178628 0.384390 0.641624 11.00000 -1.50000 H18B 2 0.205542 0.421169 0.583145 11.00000 -1.50000 H18C 2 0.153090 0.521915 0.607973 11.00000 -1.50000 AFIX 0 C19 1 0.213521 0.627752 0.693231 11.00000 0.04140 0.05182 = 0.04395 0.03122 0.01841 0.02580 AFIX 33 H19A 2 0.243178 0.693217 0.710242 11.00000 -1.50000 H19B 2 0.203837 0.546362 0.717896 11.00000 -1.50000 H19C 2 0.176796 0.683784 0.685143 11.00000 -1.50000 AFIX 0 C20 1 0.374303 0.129557 0.947117 11.00000 0.03799 0.05672 = 0.02669 0.00866 0.00132 0.00137 C21 1 0.405892 -0.013655 0.965026 11.00000 0.06897 0.07257 = 0.03616 0.02112 0.01074 0.01555 AFIX 33 H21A 2 0.395252 -0.035455 1.002629 11.00000 -1.50000 H21B 2 0.449657 -0.001273 0.962032 11.00000 -1.50000 H21C 2 0.392898 -0.095505 0.941831 11.00000 -1.50000 AFIX 0 C22 1 0.390328 0.248623 0.986390 11.00000 0.05105 0.08310 = 0.02644 -0.00598 0.00257 0.00008 AFIX 33 H22A 2 0.379809 0.216714 1.023044 11.00000 -1.50000 H22B 2 0.367980 0.338859 0.977466 11.00000 -1.50000 H22C 2 0.433711 0.268430 0.984433 11.00000 -1.50000 AFIX 0 C23 1 0.306392 0.092623 0.951068 11.00000 0.05406 0.09924 = 0.02734 0.00367 0.01051 -0.01891 AFIX 33 H23A 2 0.296397 0.065876 0.988385 11.00000 -1.50000 H23B 2 0.297058 0.009471 0.927090 11.00000 -1.50000 H23C 2 0.282674 0.179111 0.940234 11.00000 -1.50000 AFIX 0 C24 1 0.482045 0.675933 0.620269 11.00000 0.03073 0.02938 = 0.03252 -0.00041 -0.00044 0.00847 C25 1 0.511451 0.756623 0.660997 11.00000 0.03320 0.03071 = 0.03019 -0.00355 -0.00052 0.00666 AFIX 43 H25A 2 0.524946 0.709842 0.693173 11.00000 -1.20000 AFIX 0 C26 1 0.520159 0.907081 0.652692 11.00000 0.04136 0.03301 = 0.03541 -0.00758 -0.00860 0.00173 AFIX 43 H26A 2 0.541503 0.963783 0.678738 11.00000 -1.20000 AFIX 0 C27 1 0.499075 0.971166 0.609106 11.00000 0.04188 0.03349 = 0.04554 -0.00177 -0.00354 0.00580 AFIX 43 H27A 2 0.505208 1.074324 0.604375 11.00000 -1.20000 AFIX 0 C28 1 0.468776 0.894769 0.570553 11.00000 0.03854 0.03543 = 0.04675 0.00974 -0.00248 0.00699 AFIX 43 H28A 2 0.452917 0.944958 0.539970 11.00000 -1.20000 AFIX 0 C29 1 0.460887 0.741751 0.575876 11.00000 0.03353 0.03382 = 0.04245 0.00602 -0.00733 0.00242 AFIX 43 H29A 2 0.440990 0.686268 0.548589 11.00000 -1.20000 AFIX 0 C30 1 0.477554 0.400279 0.564140 11.00000 0.04762 0.03504 = 0.02484 0.00158 0.00353 0.00648 C31 1 0.525739 0.433582 0.528072 11.00000 0.05360 0.04812 = 0.02789 -0.00252 0.00308 0.00124 AFIX 43 H31A 2 0.558233 0.495503 0.538723 11.00000 -1.20000 AFIX 0 C32 1 0.523227 0.369709 0.474883 11.00000 0.05924 0.05759 = 0.03041 -0.00044 -0.00167 0.00576 AFIX 43 H32A 2 0.556137 0.387149 0.451155 11.00000 -1.20000 AFIX 0 C33 1 0.478311 0.288887 0.457120 11.00000 0.05849 0.04530 = 0.03359 -0.01259 -0.00905 0.00469 AFIX 43 H33A 2 0.478082 0.252992 0.421040 11.00000 -1.20000 AFIX 0 C34 1 0.432849 0.257963 0.490748 11.00000 0.05344 0.03710 = 0.03741 -0.00878 -0.00791 -0.00417 AFIX 43 H34A 2 0.401209 0.196566 0.477861 11.00000 -1.20000 AFIX 0 C35 1 0.429136 0.310449 0.543561 11.00000 0.04540 0.02958 = 0.03168 -0.00598 -0.00091 -0.00405 AFIX 43 H35A 2 0.395321 0.287426 0.565569 11.00000 -1.20000 AFIX 0 C36 1 0.580847 0.298850 0.882450 11.00000 0.02061 0.04698 = 0.02828 0.00062 -0.00784 0.00127 C37 1 0.593118 0.155728 0.897859 11.00000 0.02695 0.04849 = 0.03400 0.00132 -0.01080 -0.00548 AFIX 43 H37A 2 0.574228 0.076826 0.878999 11.00000 -1.20000 AFIX 0 C38 1 0.629479 0.125012 0.937128 11.00000 0.03148 0.04689 = 0.03383 0.01236 -0.00336 -0.00900 AFIX 43 H38A 2 0.639626 0.024726 0.944050 11.00000 -1.20000 AFIX 0 C39 1 0.654433 0.236958 0.969930 11.00000 0.02726 0.05772 = 0.03106 0.00730 -0.00103 -0.00334 AFIX 43 H39A 2 0.677312 0.215264 1.001401 11.00000 -1.20000 AFIX 0 C40 1 0.643777 0.375279 0.953836 11.00000 0.02886 0.05758 = 0.03399 -0.01020 -0.00044 -0.00514 AFIX 43 H40A 2 0.662920 0.451912 0.973713 11.00000 -1.20000 AFIX 0 C41 1 0.608459 0.417231 0.912066 11.00000 0.02337 0.05319 = 0.03362 -0.00670 -0.00334 0.00720 AFIX 43 H41A 2 0.602336 0.518158 0.902940 11.00000 -1.20000 AFIX 0 C42 1 0.534612 0.505980 0.814492 11.00000 0.03556 0.03507 = 0.02553 -0.00074 -0.00506 -0.00626 C43 1 0.477494 0.581975 0.815417 11.00000 0.04176 0.03949 = 0.03529 -0.00044 -0.01228 -0.00582 AFIX 43 H43A 2 0.441860 0.526163 0.821550 11.00000 -1.20000 AFIX 0 C44 1 0.472270 0.741309 0.807300 11.00000 0.04494 0.04062 = 0.04459 -0.00135 -0.01791 0.00279 AFIX 43 H44A 2 0.433997 0.788451 0.807512 11.00000 -1.20000 AFIX 0 C45 1 0.523025 0.819552 0.799520 11.00000 0.05370 0.03972 = 0.04511 0.00383 -0.00840 -0.00340 AFIX 43 H45A 2 0.521961 0.924450 0.797688 11.00000 -1.20000 AFIX 0 C46 1 0.575962 0.745011 0.794329 11.00000 0.04488 0.04174 = 0.04153 0.00467 -0.00185 -0.00491 AFIX 43 H46A 2 0.610909 0.799720 0.784694 11.00000 -1.20000 AFIX 0 C47 1 0.581996 0.593579 0.802278 11.00000 0.04104 0.04477 = 0.03873 -0.00271 -0.00121 -0.00482 AFIX 43 H47A 2 0.620826 0.550171 0.799002 11.00000 -1.20000 AFIX 0 C48 1 0.807886 0.966049 0.832186 21.00000 0.06286 0.06453 = 0.07193 0.00943 -0.00280 -0.00222 AFIX 23 H48A 2 0.839177 1.011235 0.855450 21.00000 -1.20000 H48B 2 0.816994 0.991766 0.794165 21.00000 -1.20000 AFIX 0 CL1 6 0.736137 1.035854 0.850092 21.00000 0.18971 0.19049 = 0.18151 0.00483 0.01464 0.00183 CL2 6 0.808692 0.771646 0.840200 21.00000 0.18971 0.19049 = 0.18151 0.00483 0.01464 0.00183 C49 1 0.238157 0.080296 0.525244 31.00000 0.20584 AFIX 23 H49A 2 0.233225 -0.013277 0.504956 31.00000 -1.20000 H49B 2 0.201069 0.097476 0.546597 31.00000 -1.20000 AFIX 0 CL3 6 0.300982 0.066785 0.569023 31.00000 0.16483 0.15540 = 0.13783 0.00894 0.01690 0.00289 CL4 6 0.249327 0.228202 0.479638 31.00000 0.16483 0.15540 = 0.13783 0.00894 0.01690 0.00289 HKLF 4 REM so02 in Pna2(1) REM R1 = 0.0652 for 5008 Fo > 4sig(Fo) and 0.1661 for all 9159 data REM 518 parameters refined using 398 restraints END WGHT 0.0535 18.7595 REM Highest difference peak 1.743, deepest hole -1.368, 1-sigma level 0.249 Q1 1 0.5891 0.3000 0.6511 11.00000 0.05 1.26 Q2 1 0.3043 0.1950 0.8010 11.00000 0.05 1.15 Q3 1 0.6702 0.4756 0.6874 11.00000 0.05 1.13 Q4 1 0.2806 0.1371 0.8134 11.00000 0.05 1.05 Q5 1 0.7099 0.7609 0.8859 11.00000 0.05 1.03 Q6 1 0.4342 0.1431 0.7470 11.00000 0.05 1.02 Q7 1 0.2016 0.1619 0.4906 11.00000 0.05 1.01 Q8 1 0.5969 0.3451 0.7215 11.00000 0.05 1.01 Q9 1 0.5500 0.6427 0.6343 11.00000 0.05 1.01 Q10 1 0.4421 1.1441 0.6260 11.00000 0.05 1.00 Q11 1 0.5991 0.3857 0.7262 11.00000 0.05 1.00 Q12 1 0.5313 0.4129 0.6319 11.00000 0.05 1.00 Q13 1 0.4306 0.3382 0.6617 11.00000 0.05 0.98 Q14 1 0.3821 0.3578 0.6867 11.00000 0.05 0.97 Q15 1 0.5809 0.4911 0.6895 11.00000 0.05 0.96 Q16 1 0.4026 0.2170 0.6888 11.00000 0.05 0.94 Q17 1 0.2871 0.1850 0.8390 11.00000 0.05 0.93 Q18 1 0.5344 0.4073 0.7409 11.00000 0.05 0.93 Q19 1 0.7202 0.3665 0.6470 11.00000 0.05 0.92 Q20 1 0.5807 0.8304 0.6119 11.00000 0.05 0.92 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^ > 2\s(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. The two molecules of CH2Cl2 within the lattice were refined using the ISOR command, however the carbon atom of one of the molecules of CH2Cl2 was left isotropic. This is because anisotropic refinement of the carbon atoms was unstable. The chlorine atoms in each CH2Cl2 could be refined anisotropically, however for consistency the whole solvent molecule, in both cases, was refined using the ISOR command, with the exception being C49. The Rint for this structure is higher than 0.1, suggesting the choice of space group may potentially be incorrect. However, Platon ADDSYM was employed and did not suggest any alternative space group. ; _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^)+(0.0535P)^2^+18.7042P] 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 0.00101(8) _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 0.003(11) _refine_ls_number_reflns 9159 _refine_ls_number_parameters 518 _refine_ls_number_restraints 398 _refine_ls_R_factor_all 0.1661 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.53850(3) 0.36226(7) 0.68680(3) 0.02369(19) Uani 1 1 d . . . I1 I 0.60503(6) 0.20938(14) 0.75521(5) 0.0303(3) Uani 1 1 d . . . S1 S 0.4591(2) 0.2309(5) 0.71620(18) 0.0259(11) Uani 1 1 d . . . P1 P 0.4762(2) 0.4760(5) 0.63011(18) 0.0229(12) Uani 1 1 d . . . C1 C 0.2883(8) 0.3527(19) 0.6896(9) 0.033(3) Uani 1 1 d U . . H1A H 0.2490 0.3192 0.6988 0.039 Uiso 1 1 calc R . . B1 B 0.5336(11) 0.349(3) 0.8307(8) 0.035(4) Uani 1 1 d U . . I2 I 0.63324(6) 0.48191(15) 0.64399(6) 0.0382(4) Uani 1 1 d . . . C2 C 0.2928(9) 0.479(2) 0.6582(7) 0.029(3) Uani 1 1 d U . . C3 C 0.3513(7) 0.5164(19) 0.6366(7) 0.025(3) Uani 1 1 d U . . H3A H 0.3558 0.5944 0.6112 0.030 Uiso 1 1 calc R . . C4 C 0.4009(8) 0.4352(19) 0.6541(6) 0.024(3) Uani 1 1 d U . . C5 C 0.4746(8) 0.251(2) 0.8296(7) 0.028(3) Uani 1 1 d U . . C6 C 0.4525(8) 0.215(2) 0.8817(7) 0.029(3) Uani 1 1 d U . . H6A H 0.4786 0.2245 0.9120 0.035 Uiso 1 1 calc R . . C7 C 0.3923(9) 0.166(2) 0.8899(7) 0.034(3) Uani 1 1 d U . . C8 C 0.3574(9) 0.146(2) 0.8453(7) 0.033(3) Uani 1 1 d U . . H8A H 0.3169 0.1152 0.8506 0.039 Uiso 1 1 calc R . . C9 C 0.3363(9) 0.136(2) 0.7453(7) 0.031(3) Uani 1 1 d U . . C13 C 0.3766(9) 0.1667(19) 0.7930(7) 0.027(3) Uani 1 1 d U . . C12 C 0.4355(8) 0.223(2) 0.7851(7) 0.024(3) Uani 1 1 d U . . C11 C 0.3969(8) 0.3181(19) 0.6917(8) 0.031(3) Uani 1 1 d U . . C10 C 0.3366(9) 0.272(2) 0.7084(7) 0.028(3) Uani 1 1 d U . . C14 C 0.3531(9) -0.005(2) 0.7142(8) 0.040(5) Uani 1 1 d U . . H14A H 0.3951 0.0018 0.7023 0.061 Uiso 1 1 calc R . . H14B H 0.3268 -0.0148 0.6826 0.061 Uiso 1 1 calc R . . H14C H 0.3481 -0.0908 0.7378 0.061 Uiso 1 1 calc R . . C15 C 0.2692(9) 0.115(2) 0.7642(7) 0.036(5) Uani 1 1 d U . . H15A H 0.2559 0.2024 0.7841 0.054 Uiso 1 1 calc R . . H15B H 0.2664 0.0276 0.7877 0.054 Uiso 1 1 calc R . . H15C H 0.2433 0.1003 0.7325 0.054 Uiso 1 1 calc R . . C16 C 0.2384(9) 0.568(2) 0.6434(8) 0.034(3) Uani 1 1 d U . . C17 C 0.2507(9) 0.694(2) 0.6031(7) 0.036(5) Uani 1 1 d U . . H17A H 0.2792 0.7641 0.6191 0.054 Uiso 1 1 calc R . . H17B H 0.2128 0.7447 0.5947 0.054 Uiso 1 1 calc R . . H17C H 0.2679 0.6526 0.5699 0.054 Uiso 1 1 calc R . . C18 C 0.1892(8) 0.464(2) 0.6165(7) 0.036(5) Uani 1 1 d U . . H18A H 0.1786 0.3844 0.6416 0.054 Uiso 1 1 calc R . . H18B H 0.2055 0.4212 0.5831 0.054 Uiso 1 1 calc R . . H18C H 0.1531 0.5219 0.6080 0.054 Uiso 1 1 calc R . . C19 C 0.2135(9) 0.628(2) 0.6932(9) 0.046(5) Uani 1 1 d U . . H19A H 0.2432 0.6932 0.7102 0.069 Uiso 1 1 calc R . . H19B H 0.2038 0.5464 0.7179 0.069 Uiso 1 1 calc R . . H19C H 0.1768 0.6838 0.6851 0.069 Uiso 1 1 calc R . . C20 C 0.3743(10) 0.130(2) 0.9471(7) 0.040(4) Uani 1 1 d U . . C21 C 0.4059(11) -0.014(3) 0.9650(8) 0.059(6) Uani 1 1 d U . . H21A H 0.3953 -0.0355 1.0026 0.089 Uiso 1 1 calc R . . H21B H 0.4497 -0.0013 0.9620 0.089 Uiso 1 1 calc R . . H21C H 0.3929 -0.0955 0.9418 0.089 Uiso 1 1 calc R . . C22 C 0.3903(11) 0.249(3) 0.9864(7) 0.054(6) Uani 1 1 d U . . H22A H 0.3798 0.2167 1.0230 0.080 Uiso 1 1 calc R . . H22B H 0.3680 0.3389 0.9775 0.080 Uiso 1 1 calc R . . H22C H 0.4337 0.2684 0.9844 0.080 Uiso 1 1 calc R . . C23 C 0.3064(11) 0.093(3) 0.9511(8) 0.060(6) Uani 1 1 d U . . H23A H 0.2964 0.0659 0.9884 0.090 Uiso 1 1 calc R . . H23B H 0.2971 0.0095 0.9271 0.090 Uiso 1 1 calc R . . H23C H 0.2827 0.1791 0.9402 0.090 Uiso 1 1 calc R . . C24 C 0.4820(9) 0.676(2) 0.6203(7) 0.031(4) Uani 1 1 d U . . C25 C 0.5115(9) 0.757(2) 0.6610(7) 0.031(4) Uani 1 1 d U . . H25A H 0.5249 0.7098 0.6932 0.038 Uiso 1 1 calc R . . C26 C 0.5202(9) 0.907(2) 0.6527(8) 0.037(4) Uani 1 1 d U . . H26A H 0.5415 0.9638 0.6787 0.044 Uiso 1 1 calc R . . C27 C 0.4991(9) 0.971(2) 0.6091(8) 0.040(4) Uani 1 1 d U . . H27A H 0.5052 1.0743 0.6044 0.048 Uiso 1 1 calc R . . C28 C 0.4688(9) 0.895(2) 0.5706(8) 0.040(4) Uani 1 1 d U . . H28A H 0.4529 0.9450 0.5400 0.048 Uiso 1 1 calc R . . C29 C 0.4609(9) 0.742(2) 0.5759(8) 0.037(4) Uani 1 1 d U . . H29A H 0.4410 0.6863 0.5486 0.044 Uiso 1 1 calc R . . C30 C 0.4776(10) 0.400(2) 0.5641(7) 0.036(4) Uani 1 1 d U . . C31 C 0.5257(10) 0.434(2) 0.5281(7) 0.043(4) Uani 1 1 d U . . H31A H 0.5582 0.4955 0.5387 0.052 Uiso 1 1 calc R . . C32 C 0.5232(11) 0.370(2) 0.4749(8) 0.049(4) Uani 1 1 d U . . H32A H 0.5561 0.3871 0.4512 0.059 Uiso 1 1 calc R . . C33 C 0.4783(11) 0.289(2) 0.4571(8) 0.046(4) Uani 1 1 d U . . H33A H 0.4781 0.2530 0.4210 0.055 Uiso 1 1 calc R . . C34 C 0.4328(11) 0.258(2) 0.4907(8) 0.043(4) Uani 1 1 d U . . H34A H 0.4012 0.1966 0.4779 0.051 Uiso 1 1 calc R . . C35 C 0.4291(10) 0.310(2) 0.5436(7) 0.036(4) Uani 1 1 d U . . H35A H 0.3953 0.2874 0.5656 0.043 Uiso 1 1 calc R . . C36 C 0.5808(9) 0.299(2) 0.8825(7) 0.032(4) Uani 1 1 d U . . C37 C 0.5931(8) 0.156(2) 0.8979(7) 0.036(4) Uani 1 1 d U . . H37A H 0.5742 0.0768 0.8790 0.044 Uiso 1 1 calc R . . C38 C 0.6295(9) 0.125(2) 0.9371(7) 0.037(4) Uani 1 1 d U . . H38A H 0.6396 0.0247 0.9441 0.045 Uiso 1 1 calc R . . C39 C 0.6544(9) 0.237(2) 0.9699(8) 0.039(4) Uani 1 1 d U . . H39A H 0.6773 0.2153 1.0014 0.046 Uiso 1 1 calc R . . C40 C 0.6438(9) 0.375(2) 0.9538(7) 0.040(4) Uani 1 1 d U . . H40A H 0.6629 0.4519 0.9737 0.048 Uiso 1 1 calc R . . C41 C 0.6085(9) 0.417(2) 0.9121(7) 0.037(4) Uani 1 1 d U . . H41A H 0.6023 0.5182 0.9029 0.044 Uiso 1 1 calc R . . C42 C 0.5346(9) 0.506(2) 0.8145(7) 0.032(3) Uani 1 1 d U . . C43 C 0.4775(10) 0.582(2) 0.8154(7) 0.039(4) Uani 1 1 d U . . H43A H 0.4419 0.5262 0.8215 0.047 Uiso 1 1 calc R . . C44 C 0.4723(11) 0.741(2) 0.8073(8) 0.043(4) Uani 1 1 d U . . H44A H 0.4340 0.7885 0.8075 0.052 Uiso 1 1 calc R . . C45 C 0.5230(10) 0.820(2) 0.7995(8) 0.046(4) Uani 1 1 d U . . H45A H 0.5220 0.9245 0.7977 0.055 Uiso 1 1 calc R . . C46 C 0.5760(11) 0.745(2) 0.7943(8) 0.043(4) Uani 1 1 d U . . H46A H 0.6109 0.7997 0.7847 0.051 Uiso 1 1 calc R . . C47 C 0.5820(10) 0.594(2) 0.8023(7) 0.042(4) Uani 1 1 d U . . H47A H 0.6208 0.5502 0.7990 0.050 Uiso 1 1 calc R . . C48 C 0.8079(10) 0.966(2) 0.8322(16) 0.066(13) Uani 0.600(13) 1 d PDU . . H48A H 0.8392 1.0112 0.8555 0.080 Uiso 0.600(13) 1 calc PR . . H48B H 0.8170 0.9918 0.7942 0.080 Uiso 0.600(13) 1 calc PR . . Cl1 Cl 0.7361(9) 1.036(2) 0.8501(8) 0.187(8) Uani 0.600(13) 1 d PDU . . Cl2 Cl 0.8087(10) 0.7716(19) 0.8402(8) 0.187(8) Uani 0.600(13) 1 d PDU . . C49 C 0.2382(15) 0.080(5) 0.5252(18) 0.21(3) Uiso 0.702(13) 1 d PD . . H49A H 0.2332 -0.0133 0.5050 0.247 Uiso 0.702(13) 1 calc PR . . H49B H 0.2011 0.0975 0.5466 0.247 Uiso 0.702(13) 1 calc PR . . Cl3 Cl 0.3010(8) 0.0668(17) 0.5690(5) 0.153(5) Uani 0.702(13) 1 d PDU . . Cl4 Cl 0.2493(8) 0.2282(18) 0.4796(5) 0.153(5) Uani 0.702(13) 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0192(4) 0.0272(4) 0.0246(3) 0.0024(4) -0.0005(5) 0.0000(4) I1 0.0234(7) 0.0368(8) 0.0308(6) 0.0030(6) 0.0003(7) 0.0011(6) S1 0.025(3) 0.026(3) 0.027(2) 0.004(2) -0.005(2) 0.001(2) P1 0.018(3) 0.025(3) 0.026(3) 0.003(2) 0.004(2) -0.002(2) C1 0.030(7) 0.036(7) 0.032(6) 0.002(7) 0.006(7) 0.006(6) B1 0.034(7) 0.042(7) 0.029(6) -0.001(7) -0.004(7) -0.003(7) I2 0.0235(7) 0.0434(9) 0.0477(7) 0.0114(7) 0.0048(7) -0.0031(7) C2 0.029(6) 0.029(6) 0.030(6) -0.001(5) 0.006(6) 0.002(6) C3 0.026(7) 0.026(7) 0.023(6) 0.003(6) -0.003(6) -0.002(6) C4 0.021(6) 0.028(6) 0.023(6) 0.003(5) 0.005(5) -0.005(5) C5 0.023(6) 0.033(6) 0.027(5) -0.001(5) -0.002(5) -0.005(5) C6 0.023(7) 0.035(7) 0.029(6) -0.001(6) 0.001(6) -0.007(6) C7 0.029(6) 0.039(6) 0.033(5) -0.003(5) 0.005(5) -0.003(5) C8 0.033(7) 0.031(7) 0.035(6) -0.002(6) 0.008(6) -0.007(6) C9 0.032(6) 0.031(6) 0.030(6) 0.006(6) 0.010(6) 0.000(6) C13 0.027(6) 0.026(5) 0.029(5) 0.002(5) 0.010(5) -0.001(5) C12 0.021(6) 0.026(6) 0.024(5) 0.004(5) 0.010(5) -0.002(5) C11 0.031(6) 0.035(6) 0.027(6) 0.006(6) 0.003(6) 0.002(5) C10 0.031(6) 0.030(6) 0.023(5) 0.003(5) 0.004(6) 0.000(6) C14 0.053(12) 0.032(11) 0.036(9) -0.007(9) -0.019(10) 0.008(10) C15 0.040(8) 0.035(8) 0.033(7) 0.020(7) -0.004(7) -0.008(7) C16 0.034(7) 0.033(7) 0.035(7) 0.010(6) 0.007(7) 0.006(6) C17 0.035(11) 0.041(11) 0.032(9) 0.010(8) 0.017(9) 0.012(9) C18 0.031(11) 0.046(12) 0.031(10) 0.009(9) -0.003(9) -0.011(9) C19 0.041(11) 0.052(11) 0.044(11) 0.031(10) 0.018(11) 0.026(10) C20 0.038(8) 0.057(8) 0.027(7) 0.009(7) 0.001(7) 0.001(7) C21 0.069(14) 0.073(14) 0.036(10) 0.021(10) 0.011(11) 0.016(12) C22 0.051(13) 0.083(15) 0.026(10) -0.006(10) 0.003(10) 0.000(12) C23 0.054(13) 0.099(15) 0.027(10) 0.004(10) 0.011(11) -0.019(12) C24 0.031(8) 0.029(8) 0.033(7) 0.000(6) 0.000(7) 0.008(6) C25 0.033(8) 0.031(8) 0.030(7) -0.004(6) -0.001(6) 0.007(7) C26 0.041(8) 0.033(8) 0.035(7) -0.008(6) -0.009(7) 0.002(7) C27 0.042(9) 0.033(8) 0.046(8) -0.002(7) -0.004(7) 0.006(7) C28 0.039(8) 0.035(8) 0.047(8) 0.010(6) -0.002(7) 0.007(7) C29 0.034(8) 0.034(8) 0.042(7) 0.006(6) -0.007(7) 0.002(7) C30 0.048(9) 0.035(8) 0.025(7) 0.002(6) 0.004(7) 0.006(7) C31 0.054(10) 0.048(8) 0.028(7) -0.003(7) 0.003(7) 0.001(7) C32 0.059(10) 0.058(9) 0.030(7) 0.000(7) -0.002(7) 0.006(8) C33 0.058(10) 0.045(9) 0.034(7) -0.013(7) -0.009(7) 0.005(8) C34 0.053(10) 0.037(8) 0.037(8) -0.009(7) -0.008(7) -0.004(8) C35 0.045(9) 0.030(8) 0.032(7) -0.006(6) -0.001(7) -0.004(7) C36 0.021(8) 0.047(8) 0.028(7) 0.001(7) -0.008(7) 0.001(7) C37 0.027(8) 0.048(8) 0.034(7) 0.001(7) -0.011(7) -0.005(7) C38 0.031(8) 0.047(8) 0.034(7) 0.012(7) -0.003(7) -0.009(7) C39 0.027(8) 0.058(9) 0.031(7) 0.007(7) -0.001(7) -0.003(8) C40 0.029(8) 0.058(9) 0.034(7) -0.010(7) 0.000(7) -0.005(8) C41 0.023(8) 0.053(9) 0.034(7) -0.007(7) -0.003(7) 0.007(7) C42 0.036(6) 0.035(6) 0.026(5) -0.001(5) -0.005(5) -0.006(5) C43 0.042(8) 0.039(7) 0.035(7) 0.000(6) -0.012(7) -0.006(7) C44 0.045(9) 0.041(8) 0.045(7) -0.001(7) -0.018(7) 0.003(7) C45 0.054(9) 0.040(9) 0.045(7) 0.004(7) -0.008(8) -0.003(7) C46 0.045(9) 0.042(9) 0.042(7) 0.005(7) -0.002(8) -0.005(7) C47 0.041(8) 0.045(8) 0.039(7) -0.003(7) -0.001(7) -0.005(7) C48 0.063(15) 0.065(15) 0.072(15) 0.009(9) -0.003(9) -0.002(9) Cl1 0.190(10) 0.190(9) 0.182(9) 0.005(6) 0.015(6) 0.002(6) Cl2 0.190(10) 0.190(9) 0.182(9) 0.005(6) 0.015(6) 0.002(6) Cl3 0.165(8) 0.155(7) 0.138(7) 0.009(5) 0.017(5) 0.003(6) Cl4 0.165(8) 0.155(7) 0.138(7) 0.009(5) 0.017(5) 0.003(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.222(5) . ? Pt1 S1 2.246(5) . ? Pt1 I2 2.590(2) . ? Pt1 I1 2.637(2) . ? I1 B1 2.75(2) . ? S1 C11 1.702(18) . ? S1 C12 1.784(17) . ? P1 C30 1.770(18) . ? P1 C4 1.811(18) . ? P1 C24 1.829(19) . ? C1 C10 1.38(2) . ? C1 C2 1.39(2) . ? C1 H1A 0.9500 . ? B1 C42 1.48(3) . ? B1 C5 1.58(3) . ? B1 C36 1.72(3) . ? C2 C3 1.44(2) . ? C2 C16 1.50(3) . ? C3 C4 1.39(2) . ? C3 H3A 0.9500 . ? C4 C11 1.41(2) . ? C5 C6 1.42(2) . ? C5 C12 1.42(2) . ? C6 C7 1.42(2) . ? C6 H6A 0.9500 . ? C7 C8 1.36(2) . ? C7 C20 1.51(2) . ? C8 C13 1.37(2) . ? C8 H8A 0.9500 . ? C9 C13 1.51(3) . ? C9 C14 1.53(2) . ? C9 C10 1.53(2) . ? C9 C15 1.57(2) . ? C13 C12 1.42(2) . ? C11 C10 1.46(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C19 1.45(3) . ? C16 C17 1.53(2) . ? C16 C18 1.59(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.49(3) . ? C20 C21 1.54(3) . ? C20 C23 1.55(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.33(3) . ? C24 C25 1.40(2) . ? C25 C26 1.39(2) . ? C25 H25A 0.9500 . ? C26 C27 1.31(2) . ? C26 H26A 0.9500 . ? C27 C28 1.36(3) . ? C27 H27A 0.9500 . ? C28 C29 1.40(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.42(3) . ? C30 C35 1.44(3) . ? C31 C32 1.44(3) . ? C31 H31A 0.9500 . ? C32 C33 1.31(3) . ? C32 H32A 0.9500 . ? C33 C34 1.34(3) . ? C33 H33A 0.9500 . ? C34 C35 1.39(3) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.38(3) . ? C36 C41 1.43(3) . ? C37 C38 1.29(2) . ? C37 H37A 0.9500 . ? C38 C39 1.41(3) . ? C38 H38A 0.9500 . ? C39 C40 1.33(3) . ? C39 H39A 0.9500 . ? C40 C41 1.35(2) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C47 1.35(3) . ? C42 C43 1.44(3) . ? C43 C44 1.46(3) . ? C43 H43A 0.9500 . ? C44 C45 1.34(3) . ? C44 H44A 0.9500 . ? C45 C46 1.36(3) . ? C45 H45A 0.9500 . ? C46 C47 1.39(3) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 Cl1 1.769(5) . ? C48 Cl2 1.769(5) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 Cl4 1.768(5) . ? C49 Cl3 1.769(5) . ? C49 H49A 0.9900 . ? C49 H49B 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 P1 Pt1 S1 87.81(18) . . ? P1 Pt1 I2 93.03(14) . . ? S1 Pt1 I2 171.81(13) . . ? P1 Pt1 I1 174.96(13) . . ? S1 Pt1 I1 87.34(14) . . ? I2 Pt1 I1 91.58(8) . . ? Pt1 I1 B1 82.7(5) . . ? C11 S1 C12 96.9(9) . . ? C11 S1 Pt1 106.0(6) . . ? C12 S1 Pt1 124.0(6) . . ? C30 P1 C4 103.8(9) . . ? C30 P1 C24 105.0(9) . . ? C4 P1 C24 108.1(9) . . ? C30 P1 Pt1 113.1(7) . . ? C4 P1 Pt1 105.8(6) . . ? C24 P1 Pt1 119.9(6) . . ? C10 C1 C2 124.7(18) . . ? C10 C1 H1A 117.6 . . ? C2 C1 H1A 117.6 . . ? C42 B1 C5 123(2) . . ? C42 B1 C36 116.5(18) . . ? C5 B1 C36 111.9(16) . . ? C42 B1 I1 104.3(13) . . ? C5 B1 I1 102.1(13) . . ? C36 B1 I1 92.0(12) . . ? C1 C2 C3 117.7(17) . . ? C1 C2 C16 121.5(17) . . ? C3 C2 C16 120.6(16) . . ? C4 C3 C2 118.2(16) . . ? C4 C3 H3A 120.9 . . ? C2 C3 H3A 120.9 . . ? C3 C4 C11 123.4(17) . . ? C3 C4 P1 121.4(13) . . ? C11 C4 P1 115.3(14) . . ? C6 C5 C12 117.0(17) . . ? C6 C5 B1 113.4(16) . . ? C12 C5 B1 128.1(16) . . ? C5 C6 C7 121.7(17) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C8 C7 C6 117.4(17) . . ? C8 C7 C20 125.5(18) . . ? C6 C7 C20 116.8(17) . . ? C7 C8 C13 124.7(19) . . ? C7 C8 H8A 117.7 . . ? C13 C8 H8A 117.7 . . ? C13 C9 C14 113.7(16) . . ? C13 C9 C10 108.3(15) . . ? C14 C9 C10 111.6(14) . . ? C13 C9 C15 110.5(14) . . ? C14 C9 C15 106.1(16) . . ? C10 C9 C15 106.3(15) . . ? C8 C13 C12 117.7(17) . . ? C8 C13 C9 121.9(17) . . ? C12 C13 C9 120.3(15) . . ? C13 C12 C5 121.2(15) . . ? C13 C12 S1 114.6(13) . . ? C5 C12 S1 123.6(14) . . ? C4 C11 C10 117.3(16) . . ? C4 C11 S1 122.1(14) . . ? C10 C11 S1 120.6(14) . . ? C1 C10 C11 117.8(16) . . ? C1 C10 C9 128.5(18) . . ? C11 C10 C9 113.7(16) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C2 107.3(16) . . ? C19 C16 C17 110.1(15) . . ? C2 C16 C17 114.4(16) . . ? C19 C16 C18 108.4(16) . . ? C2 C16 C18 109.7(15) . . ? C17 C16 C18 106.8(16) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C7 112.9(18) . . ? C22 C20 C21 108.1(18) . . ? C7 C20 C21 109.6(17) . . ? C22 C20 C23 110.3(18) . . ? C7 C20 C23 111.4(17) . . ? C21 C20 C23 104.1(18) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 121.5(18) . . ? C29 C24 P1 121.7(16) . . ? C25 C24 P1 116.8(14) . . ? C26 C25 C24 117.8(17) . . ? C26 C25 H25A 121.1 . . ? C24 C25 H25A 121.1 . . ? C27 C26 C25 120.3(19) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 122(2) . . ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C27 C28 C29 119.9(19) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C24 C29 C28 118(2) . . ? C24 C29 H29A 120.9 . . ? C28 C29 H29A 120.9 . . ? C31 C30 C35 117.2(17) . . ? C31 C30 P1 120.6(16) . . ? C35 C30 P1 122.1(15) . . ? C30 C31 C32 117(2) . . ? C30 C31 H31A 121.3 . . ? C32 C31 H31A 121.3 . . ? C33 C32 C31 124(2) . . ? C33 C32 H32A 118.0 . . ? C31 C32 H32A 118.0 . . ? C32 C33 C34 119(2) . . ? C32 C33 H33A 120.6 . . ? C34 C33 H33A 120.6 . . ? C33 C34 C35 124(2) . . ? C33 C34 H34A 118.1 . . ? C35 C34 H34A 118.1 . . ? C34 C35 C30 119(2) . . ? C34 C35 H35A 120.7 . . ? C30 C35 H35A 120.7 . . ? C37 C36 C41 118.4(17) . . ? C37 C36 B1 125.1(18) . . ? C41 C36 B1 116.5(18) . . ? C38 C37 C36 122(2) . . ? C38 C37 H37A 118.9 . . ? C36 C37 H37A 118.9 . . ? C37 C38 C39 122(2) . . ? C37 C38 H38A 119.2 . . ? C39 C38 H38A 119.2 . . ? C40 C39 C38 115.6(19) . . ? C40 C39 H39A 122.2 . . ? C38 C39 H39A 122.2 . . ? C39 C40 C41 126(2) . . ? C39 C40 H40A 116.8 . . ? C41 C40 H40A 116.8 . . ? C40 C41 C36 115(2) . . ? C40 C41 H41A 122.3 . . ? C36 C41 H41A 122.3 . . ? C47 C42 C43 114.1(19) . . ? C47 C42 B1 130(2) . . ? C43 C42 B1 116.2(19) . . ? C42 C43 C44 123(2) . . ? C42 C43 H43A 118.7 . . ? C44 C43 H43A 118.7 . . ? C45 C44 C43 118(2) . . ? C45 C44 H44A 120.9 . . ? C43 C44 H44A 120.9 . . ? C44 C45 C46 118(2) . . ? C44 C45 H45A 120.8 . . ? C46 C45 H45A 120.8 . . ? C45 C46 C47 124(2) . . ? C45 C46 H46A 118.0 . . ? C47 C46 H46A 118.0 . . ? C42 C47 C46 122(2) . . ? C42 C47 H47A 118.8 . . ? C46 C47 H47A 118.8 . . ? Cl1 C48 Cl2 109.6(4) . . ? Cl1 C48 H48A 109.7 . . ? Cl2 C48 H48A 109.7 . . ? Cl1 C48 H48B 109.7 . . ? Cl2 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? Cl4 C49 Cl3 109.4(4) . . ? Cl4 C49 H49A 109.8 . . ? Cl3 C49 H49A 109.8 . . ? Cl4 C49 H49B 109.8 . . ? Cl3 C49 H49B 109.8 . . ? H49A C49 H49B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Pt1 I1 B1 -64.0(5) . . . . ? I2 Pt1 I1 B1 124.1(5) . . . . ? P1 Pt1 S1 C11 -13.6(8) . . . . ? I1 Pt1 S1 C11 167.8(8) . . . . ? P1 Pt1 S1 C12 -123.7(8) . . . . ? I1 Pt1 S1 C12 57.7(8) . . . . ? S1 Pt1 P1 C30 -97.6(8) . . . . ? I2 Pt1 P1 C30 74.2(8) . . . . ? S1 Pt1 P1 C4 15.4(6) . . . . ? I2 Pt1 P1 C4 -172.8(6) . . . . ? S1 Pt1 P1 C24 137.7(7) . . . . ? I2 Pt1 P1 C24 -50.5(7) . . . . ? Pt1 I1 B1 C42 -48.3(13) . . . . ? Pt1 I1 B1 C5 80.7(12) . . . . ? Pt1 I1 B1 C36 -166.3(11) . . . . ? C10 C1 C2 C3 10(3) . . . . ? C10 C1 C2 C16 -174.4(19) . . . . ? C1 C2 C3 C4 -8(3) . . . . ? C16 C2 C3 C4 176.4(16) . . . . ? C2 C3 C4 C11 0(3) . . . . ? C2 C3 C4 P1 -179.0(13) . . . . ? C30 P1 C4 C3 -76.6(16) . . . . ? C24 P1 C4 C3 34.5(17) . . . . ? Pt1 P1 C4 C3 164.1(13) . . . . ? C30 P1 C4 C11 104.3(15) . . . . ? C24 P1 C4 C11 -144.6(14) . . . . ? Pt1 P1 C4 C11 -15.0(15) . . . . ? C42 B1 C5 C6 -109(2) . . . . ? C36 B1 C5 C6 37(2) . . . . ? I1 B1 C5 C6 134.5(14) . . . . ? C42 B1 C5 C12 56(3) . . . . ? C36 B1 C5 C12 -157.2(18) . . . . ? I1 B1 C5 C12 -60(2) . . . . ? C12 C5 C6 C7 -5(3) . . . . ? B1 C5 C6 C7 161.8(18) . . . . ? C5 C6 C7 C8 4(3) . . . . ? C5 C6 C7 C20 179.1(18) . . . . ? C6 C7 C8 C13 1(3) . . . . ? C20 C7 C8 C13 -173.4(19) . . . . ? C7 C8 C13 C12 -5(3) . . . . ? C7 C8 C13 C9 177.4(18) . . . . ? C14 C9 C13 C8 -107(2) . . . . ? C10 C9 C13 C8 128.8(18) . . . . ? C15 C9 C13 C8 13(2) . . . . ? C14 C9 C13 C12 76(2) . . . . ? C10 C9 C13 C12 -49(2) . . . . ? C15 C9 C13 C12 -165.2(16) . . . . ? C8 C13 C12 C5 3(3) . . . . ? C9 C13 C12 C5 -179.0(17) . . . . ? C8 C13 C12 S1 174.5(14) . . . . ? C9 C13 C12 S1 -7(2) . . . . ? C6 C5 C12 C13 2(3) . . . . ? B1 C5 C12 C13 -163.2(19) . . . . ? C6 C5 C12 S1 -169.0(14) . . . . ? B1 C5 C12 S1 26(3) . . . . ? C11 S1 C12 C13 49.9(15) . . . . ? Pt1 S1 C12 C13 164.5(11) . . . . ? C11 S1 C12 C5 -138.7(17) . . . . ? Pt1 S1 C12 C5 -24.1(19) . . . . ? C3 C4 C11 C10 6(3) . . . . ? P1 C4 C11 C10 -174.6(14) . . . . ? C3 C4 C11 S1 -174.7(14) . . . . ? P1 C4 C11 S1 4(2) . . . . ? C12 S1 C11 C4 136.7(17) . . . . ? Pt1 S1 C11 C4 8.4(18) . . . . ? C12 S1 C11 C10 -44.2(17) . . . . ? Pt1 S1 C11 C10 -172.6(14) . . . . ? C2 C1 C10 C11 -4(3) . . . . ? C2 C1 C10 C9 177.1(18) . . . . ? C4 C11 C10 C1 -5(3) . . . . ? S1 C11 C10 C1 176.3(16) . . . . ? C4 C11 C10 C9 174.8(16) . . . . ? S1 C11 C10 C9 -4(2) . . . . ? C13 C9 C10 C1 -126(2) . . . . ? C14 C9 C10 C1 108(2) . . . . ? C15 C9 C10 C1 -7(3) . . . . ? C13 C9 C10 C11 55(2) . . . . ? C14 C9 C10 C11 -71(2) . . . . ? C15 C9 C10 C11 173.8(15) . . . . ? C1 C2 C16 C19 64(2) . . . . ? C3 C2 C16 C19 -120.4(18) . . . . ? C1 C2 C16 C17 -173.2(18) . . . . ? C3 C2 C16 C17 2(3) . . . . ? C1 C2 C16 C18 -53(2) . . . . ? C3 C2 C16 C18 122.0(17) . . . . ? C8 C7 C20 C22 -136(2) . . . . ? C6 C7 C20 C22 50(2) . . . . ? C8 C7 C20 C21 104(2) . . . . ? C6 C7 C20 C21 -71(2) . . . . ? C8 C7 C20 C23 -11(3) . . . . ? C6 C7 C20 C23 174.5(18) . . . . ? C30 P1 C24 C29 29(2) . . . . ? C4 P1 C24 C29 -80.9(18) . . . . ? Pt1 P1 C24 C29 157.8(15) . . . . ? C30 P1 C24 C25 -148.9(15) . . . . ? C4 P1 C24 C25 100.8(15) . . . . ? Pt1 P1 C24 C25 -20.4(17) . . . . ? C29 C24 C25 C26 -3(3) . . . . ? P1 C24 C25 C26 175.6(14) . . . . ? C24 C25 C26 C27 3(3) . . . . ? C25 C26 C27 C28 -1(3) . . . . ? C26 C27 C28 C29 -2(3) . . . . ? C25 C24 C29 C28 0(3) . . . . ? P1 C24 C29 C28 -178.0(15) . . . . ? C27 C28 C29 C24 2(3) . . . . ? C4 P1 C30 C31 168.4(16) . . . . ? C24 P1 C30 C31 55.0(18) . . . . ? Pt1 P1 C30 C31 -77.4(17) . . . . ? C4 P1 C30 C35 -8.0(18) . . . . ? C24 P1 C30 C35 -121.4(17) . . . . ? Pt1 P1 C30 C35 106.2(16) . . . . ? C35 C30 C31 C32 -3(3) . . . . ? P1 C30 C31 C32 -179.1(15) . . . . ? C30 C31 C32 C33 3(3) . . . . ? C31 C32 C33 C34 -3(4) . . . . ? C32 C33 C34 C35 2(4) . . . . ? C33 C34 C35 C30 -2(3) . . . . ? C31 C30 C35 C34 2(3) . . . . ? P1 C30 C35 C34 178.4(15) . . . . ? C42 B1 C36 C37 -170(2) . . . . ? C5 B1 C36 C37 41(3) . . . . ? I1 B1 C36 C37 -63(2) . . . . ? C42 B1 C36 C41 11(3) . . . . ? C5 B1 C36 C41 -137.7(18) . . . . ? I1 B1 C36 C41 118.5(15) . . . . ? C41 C36 C37 C38 -2(3) . . . . ? B1 C36 C37 C38 179.7(18) . . . . ? C36 C37 C38 C39 6(3) . . . . ? C37 C38 C39 C40 -8(3) . . . . ? C38 C39 C40 C41 5(3) . . . . ? C39 C40 C41 C36 -1(3) . . . . ? C37 C36 C41 C40 -1(3) . . . . ? B1 C36 C41 C40 177.7(17) . . . . ? C5 B1 C42 C47 -164.2(19) . . . . ? C36 B1 C42 C47 50(3) . . . . ? I1 B1 C42 C47 -49(2) . . . . ? C5 B1 C42 C43 21(3) . . . . ? C36 B1 C42 C43 -124.4(19) . . . . ? I1 B1 C42 C43 136.0(14) . . . . ? C47 C42 C43 C44 -4(3) . . . . ? B1 C42 C43 C44 171.9(17) . . . . ? C42 C43 C44 C45 -1(3) . . . . ? C43 C44 C45 C46 6(3) . . . . ? C44 C45 C46 C47 -7(3) . . . . ? C43 C42 C47 C46 3(3) . . . . ? B1 C42 C47 C46 -171.6(19) . . . . ? C45 C46 C47 C42 2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.743 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.249 # Attachment '- 4H_1_50CH2Cl2 so04 PtI2(TXPH) NEW_squeeze.cif' data_so04 _database_code_depnum_ccdc_archive 'CCDC 849797' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of G ttingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H39 I2 P Pt S, 1.5(C H2 Cl2)' _chemical_formula_sum 'C36.50 H42 Cl3 I2 P Pt S' _chemical_formula_weight 1098.97 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' I I -0.4742 1.8119 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.451(2) _cell_length_b 12.803(2) _cell_length_c 13.852(2) _cell_angle_alpha 75.815(2) _cell_angle_beta 74.648(2) _cell_angle_gamma 80.524(4) _cell_volume 2052.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1077 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 18.93 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 5.230 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7443 _exptl_absorpt_correction_T_max 0.8589 _exptl_absorpt_process_details SADABS _exptl_special_details ; A crystal of suitable size was selected and mounted on a goniometer head, then placed in the cold stream of the diffractometer. Data were collected with Mo K(alpha) radiation from a Siemens rotating anode, with a SMART 1K detector, at -100C. Omega and phi scans were used to ensure complete coverage. The data were corrected for absorption using the program SADABS (Bruker AXS, 2003) and solved in the triclinic space group P-1. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'parallel mirrors' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17425 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.1939 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.35 _reflns_number_total 9987 _reflns_number_gt 4809 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were placed in idealized positions and updated with each cycle of refinement. One of the ligand t-butyl groups exhibited rotational disorder (C16-19) over two positions in a 57:43 ratio. Two molecules of CH2Cl2 were also located and one of these was refined as disordered over two positions in a ratio of 62:38, while the second only had a 0.57 occupancy. No void calculation was made. The .res file for this complex is shown below and indicates other refinement details. The largest residual peak, at 2.58eA^-3, is found in the lattice, marginally associated with one of the phenyl rings of the ligand. Presumably this peak is due to a Pt "shadow" from another microcrystal of the compound. Reference for the squeeze routine: Sluiz, P.V.D.; Spek, A.L. Acta Cryst. 1990, A46, 194. TITL SO04 in P-1 CELL 0.71073 12.4506 12.8031 13.8525 75.815 74.648 80.524 ZERR 2.00 0.0021 0.0021 0.0023 0.002 0.002 0.004 LATT 1 SFAC C H P S CL I PT UNIT 73 84 2 2 6 4 2 MERG 2 OMIT -3.00 180.00 ISOR 0.01 C36A C36B ISOR 0.01 CL1A CL1B CL2A CL2B EADP C36A C36B EADP CL1A CL1B CL2A CL2B EADP C16A C16B EXYZ C16A C16B EADP C17A C17B C18A C18B C19A C19B SADI 0.005 C16A C17A C16A C18A C16A C19A DFIX 1.77 0.005 C36A CL2A DFIX 1.77 0.005 C36A CL1A DFIX 1.77 0.005 C36B CL1B DFIX 1.77 0.005 C36B CL2B DELU_* SIMU_* 0.1 SIZE 0.03 0.05 0.06 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -100.00 WGHT 0.054000 FVAR 2.34812 0.56806 0.39188 0.40579 PT1 7 0.602018 0.877407 0.172266 11.00000 0.01995 0.03508 = 0.02310 -0.00893 -0.00212 -0.00328 I2 6 0.799964 0.797878 0.202383 11.00000 0.02530 0.05363 = 0.04216 -0.01433 -0.01047 0.00413 S1 4 0.429276 0.947578 0.150567 11.00000 0.02073 0.03526 = 0.02265 -0.00966 -0.00248 -0.00412 P1 3 0.622406 1.035901 0.201800 11.00000 0.02058 0.03699 = 0.02046 -0.00908 -0.00197 -0.00359 C1 1 0.277858 1.228629 0.219944 11.00000 0.03092 0.03384 = 0.02626 -0.00331 0.00206 -0.00457 AFIX 43 H1A 2 0.204307 1.265393 0.230579 11.00000 -1.20000 AFIX 0 I1 6 0.585729 0.707707 0.100370 11.00000 0.03088 0.03892 = 0.04242 -0.01685 -0.00529 -0.00111 C2 1 0.364695 1.281986 0.224009 11.00000 0.03448 0.03843 = 0.03655 -0.00574 -0.00474 -0.00396 C3 1 0.471149 1.224627 0.217314 11.00000 0.03478 0.03489 = 0.01811 -0.00299 -0.00460 -0.00607 AFIX 43 H3A 2 0.530896 1.257896 0.223907 11.00000 -1.20000 AFIX 0 C4 1 0.490980 1.118146 0.200921 11.00000 0.02702 0.03416 = 0.01935 0.00254 -0.00231 -0.00875 C5 1 0.328562 0.778961 0.293324 11.00000 0.02256 0.03842 = 0.03781 -0.00869 -0.00999 0.00023 AFIX 43 H5A 2 0.400214 0.738280 0.284680 11.00000 -1.20000 AFIX 0 C6 1 0.235050 0.731676 0.360606 11.00000 0.03212 0.03978 = 0.02706 -0.00306 -0.00414 -0.00816 AFIX 43 H6A 2 0.243552 0.658012 0.395157 11.00000 -1.20000 AFIX 0 C7 1 0.128886 0.791678 0.377689 11.00000 0.02924 0.03583 = 0.02343 -0.01089 0.00461 -0.00931 C8 1 0.118919 0.898117 0.325765 11.00000 0.02839 0.04095 = 0.02109 -0.01423 0.00147 0.00196 AFIX 43 H8A 2 0.047715 0.939197 0.338332 11.00000 -1.20000 AFIX 0 C9 1 0.196769 1.067048 0.196259 11.00000 0.02637 0.03169 = 0.02169 -0.00114 -0.00850 0.00140 C10 1 0.291945 1.125509 0.201403 11.00000 0.02632 0.03834 = 0.01860 -0.00054 -0.00283 -0.00777 C11 1 0.401806 1.072106 0.190964 11.00000 0.02785 0.03242 = 0.01321 -0.00140 -0.00250 -0.00662 C12 1 0.316214 0.884463 0.239865 11.00000 0.01953 0.03119 = 0.02825 -0.01500 -0.00800 -0.00059 C13 1 0.209318 0.949475 0.254620 11.00000 0.02274 0.02732 = 0.02906 -0.01069 -0.00281 0.00072 C14 1 0.202062 1.069715 0.083162 11.00000 0.03288 0.06382 = 0.02335 -0.01201 -0.00618 -0.01377 AFIX 33 H14A 2 0.273837 1.032669 0.052713 11.00000 -1.50000 H14B 2 0.195078 1.145126 0.045621 11.00000 -1.50000 H14C 2 0.140631 1.033046 0.079307 11.00000 -1.50000 AFIX 0 C15 1 0.082074 1.127738 0.238955 11.00000 0.02366 0.03492 = 0.03807 -0.01358 -0.00813 0.00429 AFIX 33 H15A 2 0.075045 1.128131 0.311023 11.00000 -1.50000 H15B 2 0.021581 1.090968 0.233366 11.00000 -1.50000 H15C 2 0.077125 1.202464 0.199453 11.00000 -1.50000 AFIX 0 PART 1 C16A 1 0.348811 1.403393 0.226681 41.00000 0.04787 0.03597 = 0.08472 -0.02493 -0.00064 -0.00578 C17A 1 0.326636 1.474837 0.125895 41.00000 0.06060 0.03405 = 0.09550 -0.02182 -0.00817 0.00426 AFIX 33 H17A 2 0.316013 1.551182 0.130486 41.00000 -1.50000 H17B 2 0.259045 1.455859 0.113549 41.00000 -1.50000 H17C 2 0.390696 1.463072 0.069317 41.00000 -1.50000 AFIX 0 C18A 1 0.453477 1.442167 0.239540 41.00000 0.06060 0.03405 = 0.09550 -0.02182 -0.00817 0.00426 AFIX 33 H18A 2 0.439203 1.519553 0.240459 41.00000 -1.50000 H18B 2 0.516684 1.430351 0.182283 41.00000 -1.50000 H18C 2 0.471376 1.401356 0.304089 41.00000 -1.50000 AFIX 0 C19A 1 0.252731 1.421055 0.318687 41.00000 0.06060 0.03405 = 0.09550 -0.02182 -0.00817 0.00426 AFIX 33 H19A 2 0.240244 1.498014 0.321301 41.00000 -1.50000 H19B 2 0.272221 1.378214 0.381927 41.00000 -1.50000 H19C 2 0.184326 1.398224 0.311633 41.00000 -1.50000 AFIX 0 PART 2 SAME 0.01 C16A C17A C18A C19A C16B 1 0.348811 1.403393 0.226681 -41.00000 0.04787 0.03597 = 0.08472 -0.02493 -0.00064 -0.00578 C17B 1 0.416224 1.464237 0.123574 -41.00000 0.06060 0.03405 = 0.09550 -0.02182 -0.00817 0.00426 AFIX 33 H17D 2 0.406611 1.541941 0.122796 -41.00000 -1.50000 H17E 2 0.389063 1.452245 0.067322 -41.00000 -1.50000 H17F 2 0.495764 1.437122 0.115197 -41.00000 -1.50000 AFIX 0 C18B 1 0.400496 1.422085 0.308659 -41.00000 0.06060 0.03405 = 0.09550 -0.02182 -0.00817 0.00426 AFIX 33 H18D 2 0.389490 1.499460 0.309501 -41.00000 -1.50000 H18E 2 0.480844 1.397723 0.293286 -41.00000 -1.50000 H18F 2 0.364324 1.381067 0.375803 -41.00000 -1.50000 AFIX 0 C19B 1 0.226292 1.452776 0.244823 -41.00000 0.06060 0.03405 = 0.09550 -0.02182 -0.00817 0.00426 AFIX 33 H19D 2 0.222504 1.529804 0.244965 -41.00000 -1.50000 H19E 2 0.184116 1.415168 0.311022 -41.00000 -1.50000 H19F 2 0.193883 1.444944 0.190085 -41.00000 -1.50000 AFIX 0 PART 0 C20 1 0.026895 0.735914 0.450145 11.00000 0.02935 0.04262 = 0.03663 -0.00837 -0.00914 -0.00807 C21 1 -0.080749 0.816943 0.465286 11.00000 0.03814 0.05990 = 0.04055 -0.00917 0.01181 -0.00579 AFIX 33 H21A 2 -0.099143 0.848702 0.398927 11.00000 -1.50000 H21B 2 -0.067943 0.874574 0.494932 11.00000 -1.50000 H21C 2 -0.143022 0.778637 0.511544 11.00000 -1.50000 AFIX 0 C22 1 0.002188 0.647208 0.407871 11.00000 0.05579 0.04837 = 0.08309 -0.02725 0.00068 -0.02152 AFIX 33 H22A 2 0.068891 0.594915 0.397130 11.00000 -1.50000 H22B 2 -0.018596 0.678516 0.342470 11.00000 -1.50000 H22C 2 -0.059823 0.610414 0.456477 11.00000 -1.50000 AFIX 0 C23 1 0.050242 0.690406 0.556770 11.00000 0.04028 0.06803 = 0.03083 0.00227 0.00953 -0.00719 AFIX 33 H23A 2 0.118363 0.639328 0.551219 11.00000 -1.50000 H23B 2 -0.013155 0.652882 0.601821 11.00000 -1.50000 H23C 2 0.060427 0.749948 0.585356 11.00000 -1.50000 AFIX 0 C24 1 0.653214 1.036498 0.321947 11.00000 0.02271 0.05604 = 0.02276 -0.01495 -0.00624 -0.00402 C25 1 0.629487 0.949350 0.404749 11.00000 0.02321 0.06924 = 0.02129 -0.00722 0.00449 0.00460 AFIX 43 H25A 2 0.602216 0.887592 0.396889 11.00000 -1.20000 AFIX 0 C26 1 0.646238 0.954063 0.498703 11.00000 0.03977 0.09206 = 0.01986 -0.00501 -0.00193 0.00520 AFIX 43 H26A 2 0.626528 0.896737 0.556194 11.00000 -1.20000 AFIX 0 C27 1 0.689572 1.037875 0.509332 11.00000 0.05642 0.12441 = 0.02919 -0.03044 -0.00765 -0.00067 AFIX 43 H27A 2 0.702579 1.037630 0.573942 11.00000 -1.20000 AFIX 0 C28 1 0.715758 1.123782 0.430499 11.00000 0.08179 0.09000 = 0.06289 -0.03504 -0.04542 -0.00984 AFIX 43 H28A 2 0.746820 1.182460 0.440013 11.00000 -1.20000 AFIX 0 C29 1 0.696336 1.124830 0.334602 11.00000 0.04494 0.08199 = 0.02799 -0.02205 -0.00843 -0.01895 AFIX 43 H29A 2 0.712423 1.185005 0.279185 11.00000 -1.20000 AFIX 0 C30 1 0.722044 1.113494 0.099607 11.00000 0.02157 0.04079 = 0.02300 -0.00938 -0.00699 -0.00490 C31 1 0.836287 1.094709 0.098146 11.00000 0.01821 0.05751 = 0.04008 -0.00116 -0.01100 -0.00314 AFIX 43 H31A 2 0.861799 1.045644 0.153076 11.00000 -1.20000 AFIX 0 C32 1 0.911579 1.148151 0.016124 11.00000 0.02000 0.05782 = 0.04437 -0.00793 -0.00162 -0.00300 AFIX 43 H32A 2 0.988613 1.139259 0.016993 11.00000 -1.20000 AFIX 0 C33 1 0.876934 1.213617 -0.066248 11.00000 0.03352 0.04803 = 0.04412 -0.00443 -0.00132 -0.01244 AFIX 43 H33A 2 0.929810 1.246466 -0.124330 11.00000 -1.20000 AFIX 0 C34 1 0.762379 1.231651 -0.063905 11.00000 0.03320 0.04767 = 0.03769 0.00027 -0.00598 -0.01129 AFIX 43 H34A 2 0.737177 1.279570 -0.119579 11.00000 -1.20000 AFIX 0 C35 1 0.686806 1.181306 0.017214 11.00000 0.01900 0.04769 = 0.02273 -0.01012 -0.00433 -0.00224 AFIX 43 H35A 2 0.609469 1.192866 0.017155 11.00000 -1.20000 AFIX 0 PART 1 SAME 0.01 C36B CL1B CL2B C36A 1 0.849103 0.515599 0.150689 31.00000 0.19667 0.20514 = 0.20229 -0.04260 -0.05674 -0.02188 AFIX 23 H36A 2 0.810635 0.569021 0.192965 31.00000 -1.20000 H36B 2 0.834970 0.542648 0.081342 31.00000 -1.20000 AFIX 0 CL1A 5 0.994944 0.501482 0.142597 31.00000 0.20029 0.19034 = 0.20331 -0.03294 -0.05864 -0.00998 CL2A 5 0.795191 0.389327 0.205994 31.00000 0.20029 0.19034 = 0.20331 -0.03294 -0.05864 -0.00998 PART 2 C36B 1 0.878892 0.502985 0.088693 -31.00000 0.19667 0.20514 = 0.20229 -0.04260 -0.05674 -0.02188 AFIX 23 H36C 2 0.832343 0.572125 0.097337 -31.00000 -1.20000 H36D 2 0.924373 0.512618 0.017323 -31.00000 -1.20000 AFIX 0 CL1B 5 0.967802 0.467646 0.175094 -31.00000 0.20029 0.19034 = 0.20331 -0.03294 -0.05864 -0.00998 CL2B 5 0.791946 0.398626 0.113579 -31.00000 0.20029 0.19034 = 0.20331 -0.03294 -0.05864 -0.00998 HKLF 4 REM SO04 in P-1 REM R1 = 0.0673 for 4809 Fo > 4sig(Fo) and 0.1518 for all 9987 data REM 391 parameters refined using 514 restraints END WGHT 0.0541 0.0000 REM Highest difference peak 2.389, deepest hole -2.485, 1-sigma level 0.248 Q1 1 -0.2147 0.7735 0.4843 11.00000 0.05 2.39 Q2 1 0.5882 1.0090 0.1316 11.00000 0.05 1.91 Q3 1 0.3811 1.0853 0.1064 11.00000 0.05 1.73 Q4 1 -0.0316 0.7023 0.5158 11.00000 0.05 1.32 Q5 1 0.6069 0.9478 0.1695 11.00000 0.05 1.20 Q6 1 0.6049 1.1877 0.2031 11.00000 0.05 1.14 Q7 1 0.5677 0.8355 0.0901 11.00000 0.05 1.14 Q8 1 0.5319 0.8145 0.1644 11.00000 0.05 1.09 Q9 1 0.8365 0.6750 0.2290 11.00000 0.05 1.06 Q10 1 0.9810 0.4931 0.1692 11.00000 0.05 1.02 Q11 1 0.6270 0.8958 0.2650 11.00000 0.05 1.01 Q12 1 0.5040 0.9082 0.1283 11.00000 0.05 1.01 Q13 1 0.7299 0.8950 0.1387 11.00000 0.05 1.01 Q14 1 0.6992 0.8370 0.2041 11.00000 0.05 1.00 Q15 1 0.5897 0.8840 0.1382 11.00000 0.05 0.93 Q16 1 0.8769 0.4415 0.2668 11.00000 0.05 0.92 Q17 1 0.4643 1.2913 0.0562 11.00000 0.05 0.92 Q18 1 0.8671 1.0370 0.1846 11.00000 0.05 0.90 Q19 1 0.7032 0.6581 0.1219 11.00000 0.05 0.90 Q20 1 -0.0409 0.6162 0.4859 11.00000 0.05 0.89 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^ > 2\s(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. The molecule of CH2Cl2 within the lattice was refined using the ISOR command. This is because anisotropic refinement of the carbon atom was unstable. The chlorine atoms could be refined anisotropically, however for consistency the whole solvent molecule was refined using the ISOR command. ; _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^)+(0.0540P)^2^+0.0000P] 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 9987 _refine_ls_number_parameters 391 _refine_ls_number_restraints 514 _refine_ls_R_factor_all 0.1518 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.60202(3) 0.87741(4) 0.17227(4) 0.02608(14) Uani 1 1 d U . . I2 I 0.79996(6) 0.79788(8) 0.20238(7) 0.0401(2) Uani 1 1 d U . . S1 S 0.4293(2) 0.9476(2) 0.1506(2) 0.0260(6) Uani 1 1 d U . . P1 P 0.6224(2) 1.0359(3) 0.2018(2) 0.0260(7) Uani 1 1 d U A . C1 C 0.2779(9) 1.2286(10) 0.2199(8) 0.032(3) Uani 1 1 d U A . H1A H 0.2043 1.2654 0.2306 0.039 Uiso 1 1 calc R . . I1 I 0.58573(6) 0.70771(7) 0.10037(7) 0.0369(2) Uani 1 1 d U . . C2 C 0.3647(10) 1.2820(10) 0.2240(10) 0.038(3) Uani 1 1 d U . . C3 C 0.4711(9) 1.2246(10) 0.2173(8) 0.030(2) Uani 1 1 d U A . H3A H 0.5309 1.2579 0.2239 0.036 Uiso 1 1 calc R . . C4 C 0.4910(9) 1.1181(10) 0.2009(8) 0.028(2) Uani 1 1 d U . . C5 C 0.3286(9) 0.7790(10) 0.2933(9) 0.033(3) Uani 1 1 d U . . H5A H 0.4002 0.7383 0.2847 0.039 Uiso 1 1 calc R . . C6 C 0.2351(9) 0.7317(10) 0.3606(9) 0.034(3) Uani 1 1 d U . . H6A H 0.2436 0.6580 0.3952 0.040 Uiso 1 1 calc R . . C7 C 0.1289(9) 0.7917(10) 0.3777(8) 0.030(2) Uani 1 1 d U . . C8 C 0.1189(9) 0.8981(10) 0.3258(8) 0.031(2) Uani 1 1 d U A . H8A H 0.0477 0.9392 0.3383 0.037 Uiso 1 1 calc R . . C9 C 0.1968(9) 1.0670(9) 0.1963(8) 0.027(2) Uani 1 1 d U A . C10 C 0.2919(9) 1.1255(10) 0.2014(8) 0.029(2) Uani 1 1 d U . . C11 C 0.4018(8) 1.0721(9) 0.1910(8) 0.025(2) Uani 1 1 d U A . C12 C 0.3162(8) 0.8845(9) 0.2399(8) 0.025(2) Uani 1 1 d U A . C13 C 0.2093(8) 0.9495(9) 0.2546(8) 0.027(2) Uani 1 1 d U . . C14 C 0.2021(9) 1.0697(11) 0.0832(9) 0.039(3) Uani 1 1 d U . . H14A H 0.2738 1.0327 0.0527 0.058 Uiso 1 1 calc R A . H14B H 0.1951 1.1451 0.0456 0.058 Uiso 1 1 calc R . . H14C H 0.1406 1.0330 0.0793 0.058 Uiso 1 1 calc R . . C15 C 0.0821(8) 1.1277(10) 0.2390(9) 0.032(3) Uani 1 1 d U . . H15A H 0.0750 1.1281 0.3110 0.048 Uiso 1 1 calc R A . H15B H 0.0216 1.0910 0.2334 0.048 Uiso 1 1 calc R . . H15C H 0.0771 1.2025 0.1995 0.048 Uiso 1 1 calc R . . C16A C 0.3488(10) 1.4034(11) 0.2267(10) 0.057(3) Uani 0.406(14) 1 d PDU A 1 C17A C 0.327(3) 1.475(2) 0.1259(18) 0.065(3) Uani 0.406(14) 1 d PDU A 1 H17A H 0.3160 1.5512 0.1305 0.098 Uiso 0.406(14) 1 calc PR A 1 H17B H 0.2590 1.4559 0.1135 0.098 Uiso 0.406(14) 1 calc PR A 1 H17C H 0.3907 1.4631 0.0693 0.098 Uiso 0.406(14) 1 calc PR A 1 C18A C 0.4535(19) 1.442(3) 0.240(3) 0.065(3) Uani 0.406(14) 1 d PDU A 1 H18A H 0.4392 1.5196 0.2405 0.098 Uiso 0.406(14) 1 calc PR A 1 H18B H 0.5167 1.4304 0.1823 0.098 Uiso 0.406(14) 1 calc PR A 1 H18C H 0.4714 1.4014 0.3041 0.098 Uiso 0.406(14) 1 calc PR A 1 C19A C 0.253(2) 1.421(3) 0.319(2) 0.065(3) Uani 0.406(14) 1 d PDU A 1 H19A H 0.2402 1.4980 0.3213 0.098 Uiso 0.406(14) 1 calc PR A 1 H19B H 0.2722 1.3782 0.3819 0.098 Uiso 0.406(14) 1 calc PR A 1 H19C H 0.1843 1.3982 0.3116 0.098 Uiso 0.406(14) 1 calc PR A 1 C16B C 0.3488(10) 1.4034(11) 0.2267(10) 0.057(3) Uani 0.594(14) 1 d PDU A 2 C17B C 0.416(2) 1.4642(18) 0.1236(16) 0.065(3) Uani 0.594(14) 1 d PDU A 2 H17D H 0.4066 1.5419 0.1228 0.098 Uiso 0.594(14) 1 calc PR A 2 H17E H 0.3891 1.4522 0.0673 0.098 Uiso 0.594(14) 1 calc PR A 2 H17F H 0.4958 1.4371 0.1152 0.098 Uiso 0.594(14) 1 calc PR A 2 C18B C 0.400(2) 1.4221(19) 0.3087(18) 0.065(3) Uani 0.594(14) 1 d PDU A 2 H18D H 0.3895 1.4995 0.3095 0.098 Uiso 0.594(14) 1 calc PR A 2 H18E H 0.4808 1.3977 0.2933 0.098 Uiso 0.594(14) 1 calc PR A 2 H18F H 0.3643 1.3811 0.3758 0.098 Uiso 0.594(14) 1 calc PR A 2 C19B C 0.2263(14) 1.4528(18) 0.245(2) 0.065(3) Uani 0.594(14) 1 d PDU A 2 H19D H 0.2225 1.5298 0.2450 0.098 Uiso 0.594(14) 1 calc PR A 2 H19E H 0.1841 1.4152 0.3110 0.098 Uiso 0.594(14) 1 calc PR A 2 H19F H 0.1939 1.4449 0.1901 0.098 Uiso 0.594(14) 1 calc PR A 2 C20 C 0.0269(9) 0.7359(10) 0.4501(9) 0.035(3) Uani 1 1 d U . . C21 C -0.0807(10) 0.8169(11) 0.4653(10) 0.051(3) Uani 1 1 d U . . H21A H -0.0991 0.8487 0.3989 0.076 Uiso 1 1 calc R . . H21B H -0.0679 0.8746 0.4949 0.076 Uiso 1 1 calc R . . H21C H -0.1430 0.7786 0.5115 0.076 Uiso 1 1 calc R . . C22 C 0.0022(11) 0.6472(11) 0.4079(12) 0.061(4) Uani 1 1 d U . . H22A H 0.0689 0.5949 0.3971 0.092 Uiso 1 1 calc R . . H22B H -0.0186 0.6785 0.3425 0.092 Uiso 1 1 calc R . . H22C H -0.0598 0.6104 0.4565 0.092 Uiso 1 1 calc R . . C23 C 0.0502(10) 0.6904(12) 0.5568(9) 0.052(4) Uani 1 1 d U . . H23A H 0.1184 0.6393 0.5512 0.078 Uiso 1 1 calc R . . H23B H -0.0132 0.6529 0.6018 0.078 Uiso 1 1 calc R . . H23C H 0.0604 0.7499 0.5854 0.078 Uiso 1 1 calc R . . C24 C 0.6532(9) 1.0365(11) 0.3219(9) 0.032(3) Uani 1 1 d U . . C25 C 0.6295(9) 0.9493(12) 0.4047(9) 0.041(3) Uani 1 1 d U A . H25A H 0.6022 0.8876 0.3969 0.050 Uiso 1 1 calc R . . C26 C 0.6462(10) 0.9541(14) 0.4987(10) 0.054(4) Uani 1 1 d U . . H26A H 0.6265 0.8967 0.5562 0.065 Uiso 1 1 calc R A . C27 C 0.6896(12) 1.0379(16) 0.5093(12) 0.069(4) Uani 1 1 d U A . H27A H 0.7026 1.0376 0.5739 0.083 Uiso 1 1 calc R . . C28 C 0.7158(13) 1.1238(15) 0.4305(13) 0.069(4) Uani 1 1 d U . . H28A H 0.7468 1.1825 0.4400 0.083 Uiso 1 1 calc R A . C29 C 0.6963(10) 1.1248(13) 0.3346(10) 0.048(3) Uani 1 1 d U A . H29A H 0.7124 1.1850 0.2792 0.058 Uiso 1 1 calc R . . C30 C 0.7220(8) 1.1135(10) 0.0996(8) 0.027(2) Uani 1 1 d U . . C31 C 0.8363(9) 1.0947(11) 0.0981(10) 0.040(3) Uani 1 1 d U A . H31A H 0.8618 1.0456 0.1531 0.047 Uiso 1 1 calc R . . C32 C 0.9116(9) 1.1482(11) 0.0161(10) 0.043(3) Uani 1 1 d U . . H32A H 0.9886 1.1393 0.0170 0.051 Uiso 1 1 calc R A . C33 C 0.8769(10) 1.2136(11) -0.0662(10) 0.043(3) Uani 1 1 d U A . H33A H 0.9298 1.2465 -0.1243 0.052 Uiso 1 1 calc R . . C34 C 0.7624(9) 1.2317(11) -0.0639(10) 0.041(3) Uani 1 1 d U . . H34A H 0.7372 1.2796 -0.1196 0.049 Uiso 1 1 calc R A . C35 C 0.6868(9) 1.1813(10) 0.0172(8) 0.030(3) Uani 1 1 d U A . H35A H 0.6095 1.1929 0.0172 0.036 Uiso 1 1 calc R . . C36A C 0.849(3) 0.516(2) 0.151(6) 0.199(7) Uani 0.392(13) 1 d PDU B 1 H36A H 0.8106 0.5690 0.1930 0.239 Uiso 0.392(13) 1 calc PR B 1 H36B H 0.8350 0.5426 0.0813 0.239 Uiso 0.392(13) 1 calc PR B 1 Cl1A Cl 0.995(2) 0.501(3) 0.143(3) 0.199(4) Uani 0.392(13) 1 d PDU B 1 Cl2A Cl 0.7952(19) 0.389(2) 0.206(2) 0.199(4) Uani 0.392(13) 1 d PDU B 1 C36B C 0.879(3) 0.503(2) 0.089(3) 0.199(7) Uani 0.608(13) 1 d PDU B 2 H36C H 0.8323 0.5721 0.0973 0.239 Uiso 0.608(13) 1 calc PR B 2 H36D H 0.9244 0.5126 0.0173 0.239 Uiso 0.608(13) 1 calc PR B 2 Cl1B Cl 0.9678(16) 0.4676(17) 0.1751(17) 0.199(4) Uani 0.608(13) 1 d PDU B 2 Cl2B Cl 0.7919(13) 0.3986(14) 0.1136(16) 0.199(4) Uani 0.608(13) 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 Pt1 0.0200(2) 0.0351(3) 0.0231(2) -0.0089(2) -0.00212(17) -0.00328(19) I2 0.0253(4) 0.0536(6) 0.0422(5) -0.0143(5) -0.0105(4) 0.0041(4) S1 0.0207(13) 0.0353(18) 0.0226(15) -0.0097(13) -0.0025(11) -0.0041(12) P1 0.0206(13) 0.0370(19) 0.0205(15) -0.0091(14) -0.0020(12) -0.0036(13) C1 0.031(5) 0.034(6) 0.026(6) -0.003(5) 0.002(5) -0.005(4) I1 0.0309(4) 0.0389(5) 0.0424(5) -0.0169(4) -0.0053(4) -0.0011(4) C2 0.034(5) 0.038(5) 0.037(7) -0.006(5) -0.005(5) -0.004(4) C3 0.035(5) 0.035(6) 0.018(6) -0.003(5) -0.005(5) -0.006(4) C4 0.027(4) 0.034(5) 0.019(6) 0.003(5) -0.002(4) -0.009(4) C5 0.023(5) 0.038(6) 0.038(7) -0.009(5) -0.010(5) 0.000(4) C6 0.032(5) 0.040(7) 0.027(7) -0.003(5) -0.004(5) -0.008(4) C7 0.029(5) 0.036(6) 0.023(6) -0.011(5) 0.005(4) -0.009(4) C8 0.028(5) 0.041(6) 0.021(6) -0.014(5) 0.001(4) 0.002(5) C9 0.026(5) 0.032(5) 0.022(5) -0.001(5) -0.009(4) 0.001(4) C10 0.026(4) 0.038(6) 0.019(6) -0.001(5) -0.003(4) -0.008(4) C11 0.028(4) 0.032(5) 0.013(5) -0.001(5) -0.003(4) -0.007(4) C12 0.020(4) 0.031(5) 0.028(6) -0.015(4) -0.008(4) -0.001(4) C13 0.023(5) 0.027(5) 0.029(6) -0.011(4) -0.003(4) 0.001(4) C14 0.033(6) 0.064(9) 0.023(5) -0.012(5) -0.006(5) -0.014(6) C15 0.024(5) 0.035(7) 0.038(7) -0.014(6) -0.008(5) 0.004(4) C16A 0.048(7) 0.036(6) 0.085(9) -0.025(6) -0.001(6) -0.006(5) C17A 0.061(6) 0.034(6) 0.096(9) -0.022(5) -0.008(6) 0.004(5) C18A 0.061(6) 0.034(6) 0.096(9) -0.022(5) -0.008(6) 0.004(5) C19A 0.061(6) 0.034(6) 0.096(9) -0.022(5) -0.008(6) 0.004(5) C16B 0.048(7) 0.036(6) 0.085(9) -0.025(6) -0.001(6) -0.006(5) C17B 0.061(6) 0.034(6) 0.096(9) -0.022(5) -0.008(6) 0.004(5) C18B 0.061(6) 0.034(6) 0.096(9) -0.022(5) -0.008(6) 0.004(5) C19B 0.061(6) 0.034(6) 0.096(9) -0.022(5) -0.008(6) 0.004(5) C20 0.029(5) 0.043(7) 0.037(6) -0.008(5) -0.009(5) -0.008(5) C21 0.038(6) 0.060(9) 0.041(8) -0.009(7) 0.012(5) -0.006(5) C22 0.056(9) 0.048(9) 0.083(11) -0.027(8) 0.001(8) -0.022(7) C23 0.040(7) 0.068(11) 0.031(6) 0.002(6) 0.010(5) -0.007(6) C24 0.023(5) 0.056(8) 0.023(5) -0.015(5) -0.006(4) -0.004(5) C25 0.023(6) 0.069(8) 0.021(5) -0.007(5) 0.004(5) 0.005(6) C26 0.040(7) 0.092(11) 0.020(6) -0.005(7) -0.002(6) 0.005(7) C27 0.056(9) 0.124(14) 0.029(7) -0.030(7) -0.008(7) -0.001(9) C28 0.082(11) 0.090(12) 0.063(9) -0.035(7) -0.045(9) -0.010(9) C29 0.045(7) 0.082(10) 0.028(6) -0.022(6) -0.008(6) -0.019(7) C30 0.022(4) 0.041(7) 0.023(5) -0.009(4) -0.007(4) -0.005(5) C31 0.018(5) 0.058(9) 0.040(7) -0.001(6) -0.011(5) -0.003(5) C32 0.020(5) 0.058(9) 0.044(8) -0.008(6) -0.002(5) -0.003(5) C33 0.034(5) 0.048(9) 0.044(7) -0.004(6) -0.001(5) -0.012(6) C34 0.033(6) 0.048(9) 0.038(7) 0.000(6) -0.006(5) -0.011(6) C35 0.019(5) 0.048(8) 0.023(6) -0.010(5) -0.004(4) -0.002(5) C36A 0.197(8) 0.205(9) 0.202(10) -0.043(6) -0.057(7) -0.022(6) Cl1A 0.200(5) 0.190(5) 0.203(6) -0.033(4) -0.059(4) -0.010(4) Cl2A 0.200(5) 0.190(5) 0.203(6) -0.033(4) -0.059(4) -0.010(4) C36B 0.197(8) 0.205(9) 0.202(10) -0.043(6) -0.057(7) -0.022(6) Cl1B 0.200(5) 0.190(5) 0.203(6) -0.033(4) -0.059(4) -0.010(4) Cl2B 0.200(5) 0.190(5) 0.203(6) -0.033(4) -0.059(4) -0.010(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.232(3) . ? Pt1 S1 2.258(3) . ? Pt1 I2 2.6067(10) . ? Pt1 I1 2.6582(10) . ? S1 C12 1.768(10) . ? S1 C11 1.769(12) . ? P1 C4 1.795(12) . ? P1 C24 1.806(11) . ? P1 C30 1.821(11) . ? C1 C10 1.381(16) . ? C1 C2 1.390(15) . ? C1 H1A 0.9500 . ? C2 C3 1.397(16) . ? C2 C16A 1.543(18) . ? C3 C4 1.408(16) . ? C3 H3A 0.9500 . ? C4 C11 1.391(14) . ? C5 C12 1.378(16) . ? C5 C6 1.404(14) . ? C5 H5A 0.9500 . ? C6 C7 1.408(16) . ? C6 H6A 0.9500 . ? C7 C8 1.379(16) . ? C7 C20 1.550(15) . ? C8 C13 1.417(14) . ? C8 H8A 0.9500 . ? C9 C10 1.527(14) . ? C9 C13 1.529(15) . ? C9 C14 1.543(15) . ? C9 C15 1.551(15) . ? C10 C11 1.412(15) . ? C12 C13 1.442(14) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16A C19A 1.533(12) . ? C16A C18A 1.535(12) . ? C16A C17A 1.535(12) . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20 C22 1.505(16) . ? C20 C23 1.535(17) . ? C20 C21 1.554(17) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.395(16) . ? C24 C25 1.396(16) . ? C25 C26 1.388(17) . ? C25 H25A 0.9500 . ? C26 C27 1.33(2) . ? C26 H26A 0.9500 . ? C27 C28 1.36(2) . ? C27 H27A 0.9500 . ? C28 C29 1.408(17) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.379(15) . ? C30 C31 1.399(14) . ? C31 C32 1.380(15) . ? C31 H31A 0.9500 . ? C32 C33 1.365(17) . ? C32 H32A 0.9500 . ? C33 C34 1.400(16) . ? C33 H33A 0.9500 . ? C34 C35 1.360(15) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36A Cl2A 1.769(5) . ? C36A Cl1A 1.771(5) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C36B Cl2B 1.769(5) . ? C36B Cl1B 1.770(5) . ? C36B H36C 0.9900 . ? C36B H36D 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 P1 Pt1 S1 88.17(11) . . ? P1 Pt1 I2 90.87(8) . . ? S1 Pt1 I2 178.37(8) . . ? P1 Pt1 I1 169.24(8) . . ? S1 Pt1 I1 89.55(8) . . ? I2 Pt1 I1 91.62(3) . . ? C12 S1 C11 97.1(5) . . ? C12 S1 Pt1 116.0(4) . . ? C11 S1 Pt1 106.0(4) . . ? C4 P1 C24 105.5(5) . . ? C4 P1 C30 103.8(5) . . ? C24 P1 C30 107.8(5) . . ? C4 P1 Pt1 106.5(4) . . ? C24 P1 Pt1 118.2(4) . . ? C30 P1 Pt1 113.8(4) . . ? C10 C1 C2 124.0(11) . . ? C10 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C1 C2 C3 118.0(12) . . ? C1 C2 C16A 122.1(11) . . ? C3 C2 C16A 119.7(10) . . ? C2 C3 C4 120.8(10) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C11 C4 C3 118.1(11) . . ? C11 C4 P1 118.5(9) . . ? C3 C4 P1 123.2(8) . . ? C12 C5 C6 119.9(11) . . ? C12 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C7 121.1(12) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C8 C7 C6 118.2(10) . . ? C8 C7 C20 122.2(11) . . ? C6 C7 C20 119.6(11) . . ? C7 C8 C13 123.5(11) . . ? C7 C8 H8A 118.3 . . ? C13 C8 H8A 118.3 . . ? C10 C9 C13 109.5(9) . . ? C10 C9 C14 109.1(9) . . ? C13 C9 C14 109.6(10) . . ? C10 C9 C15 110.1(9) . . ? C13 C9 C15 111.9(9) . . ? C14 C9 C15 106.6(9) . . ? C1 C10 C11 115.9(10) . . ? C1 C10 C9 124.1(10) . . ? C11 C10 C9 119.9(10) . . ? C4 C11 C10 122.9(11) . . ? C4 C11 S1 118.7(9) . . ? C10 C11 S1 118.1(8) . . ? C5 C12 C13 121.2(10) . . ? C5 C12 S1 122.3(8) . . ? C13 C12 S1 116.5(9) . . ? C8 C13 C12 116.2(10) . . ? C8 C13 C9 123.0(10) . . ? C12 C13 C9 120.9(9) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19A C16A C18A 107.8(17) . . ? C19A C16A C17A 111.8(18) . . ? C18A C16A C17A 104.9(16) . . ? C19A C16A C2 108.0(15) . . ? C18A C16A C2 112.7(15) . . ? C17A C16A C2 111.6(15) . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C16A C18A H18A 109.5 . . ? C16A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C16A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C16A C19A H19A 109.5 . . ? C16A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C16A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? H17D C17B H17E 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? H18D C18B H18E 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? H19D C19B H19E 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C22 C20 C23 110.5(12) . . ? C22 C20 C7 110.7(10) . . ? C23 C20 C7 109.5(9) . . ? C22 C20 C21 107.6(10) . . ? C23 C20 C21 106.3(11) . . ? C7 C20 C21 112.0(11) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 119.3(11) . . ? C29 C24 P1 120.9(10) . . ? C25 C24 P1 119.7(9) . . ? C26 C25 C24 119.2(13) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C27 C26 C25 120.9(15) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 122.0(15) . . ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C27 C28 C29 119.3(15) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? C24 C29 C28 119.2(14) . . ? C24 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C35 C30 C31 119.6(10) . . ? C35 C30 P1 119.8(8) . . ? C31 C30 P1 120.1(9) . . ? C32 C31 C30 119.3(12) . . ? C32 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C33 C32 C31 120.9(11) . . ? C33 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C32 C33 C34 119.0(12) . . ? C32 C33 H33A 120.5 . . ? C34 C33 H33A 120.5 . . ? C35 C34 C33 120.7(12) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C30 120.2(10) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? Cl2A C36A Cl1A 110.1(12) . . ? Cl2A C36A H36A 109.6 . . ? Cl1A C36A H36A 109.6 . . ? Cl2A C36A H36B 109.6 . . ? Cl1A C36A H36B 109.6 . . ? H36A C36A H36B 108.2 . . ? Cl2B C36B Cl1B 108.9(10) . . ? Cl2B C36B H36C 109.9 . . ? Cl1B C36B H36C 109.9 . . ? Cl2B C36B H36D 109.9 . . ? Cl1B C36B H36D 109.9 . . ? H36C C36B H36D 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 S1 C12 -116.5(4) . . . . ? I1 Pt1 S1 C12 74.0(4) . . . . ? P1 Pt1 S1 C11 -10.1(4) . . . . ? I1 Pt1 S1 C11 -179.6(4) . . . . ? S1 Pt1 P1 C4 4.3(4) . . . . ? I2 Pt1 P1 C4 -174.4(4) . . . . ? I1 Pt1 P1 C4 82.2(5) . . . . ? S1 Pt1 P1 C24 122.6(4) . . . . ? I2 Pt1 P1 C24 -56.0(4) . . . . ? I1 Pt1 P1 C24 -159.5(5) . . . . ? S1 Pt1 P1 C30 -109.4(4) . . . . ? I2 Pt1 P1 C30 71.9(4) . . . . ? I1 Pt1 P1 C30 -31.5(6) . . . . ? C10 C1 C2 C3 -5.5(19) . . . . ? C10 C1 C2 C16A 169.4(11) . . . . ? C1 C2 C3 C4 3.7(18) . . . . ? C16A C2 C3 C4 -171.4(11) . . . . ? C2 C3 C4 C11 0.4(17) . . . . ? C2 C3 C4 P1 -174.8(9) . . . . ? C24 P1 C4 C11 -121.8(9) . . . . ? C30 P1 C4 C11 125.0(9) . . . . ? Pt1 P1 C4 C11 4.6(9) . . . . ? C24 P1 C4 C3 53.4(11) . . . . ? C30 P1 C4 C3 -59.8(10) . . . . ? Pt1 P1 C4 C3 179.8(8) . . . . ? C12 C5 C6 C7 -2.5(17) . . . . ? C5 C6 C7 C8 0.6(17) . . . . ? C5 C6 C7 C20 178.3(10) . . . . ? C6 C7 C8 C13 1.4(17) . . . . ? C20 C7 C8 C13 -176.3(10) . . . . ? C2 C1 C10 C11 2.9(17) . . . . ? C2 C1 C10 C9 -179.6(11) . . . . ? C13 C9 C10 C1 -136.5(11) . . . . ? C14 C9 C10 C1 103.6(13) . . . . ? C15 C9 C10 C1 -13.0(15) . . . . ? C13 C9 C10 C11 40.9(13) . . . . ? C14 C9 C10 C11 -79.0(13) . . . . ? C15 C9 C10 C11 164.3(10) . . . . ? C3 C4 C11 C10 -3.1(16) . . . . ? P1 C4 C11 C10 172.4(9) . . . . ? C3 C4 C11 S1 170.2(8) . . . . ? P1 C4 C11 S1 -14.4(12) . . . . ? C1 C10 C11 C4 1.5(16) . . . . ? C9 C10 C11 C4 -176.1(10) . . . . ? C1 C10 C11 S1 -171.8(8) . . . . ? C9 C10 C11 S1 10.6(14) . . . . ? C12 S1 C11 C4 136.1(9) . . . . ? Pt1 S1 C11 C4 16.5(9) . . . . ? C12 S1 C11 C10 -50.3(9) . . . . ? Pt1 S1 C11 C10 -169.9(8) . . . . ? C6 C5 C12 C13 2.5(16) . . . . ? C6 C5 C12 S1 -177.7(8) . . . . ? C11 S1 C12 C5 -135.4(10) . . . . ? Pt1 S1 C12 C5 -23.7(10) . . . . ? C11 S1 C12 C13 44.4(9) . . . . ? Pt1 S1 C12 C13 156.0(7) . . . . ? C7 C8 C13 C12 -1.3(16) . . . . ? C7 C8 C13 C9 179.0(10) . . . . ? C5 C12 C13 C8 -0.7(15) . . . . ? S1 C12 C13 C8 179.6(8) . . . . ? C5 C12 C13 C9 179.0(10) . . . . ? S1 C12 C13 C9 -0.7(14) . . . . ? C10 C9 C13 C8 133.2(11) . . . . ? C14 C9 C13 C8 -107.2(11) . . . . ? C15 C9 C13 C8 10.9(15) . . . . ? C10 C9 C13 C12 -46.5(13) . . . . ? C14 C9 C13 C12 73.1(12) . . . . ? C15 C9 C13 C12 -168.8(9) . . . . ? C1 C2 C16A C19A 57(2) . . . . ? C3 C2 C16A C19A -128.7(19) . . . . ? C1 C2 C16A C18A 175.5(18) . . . . ? C3 C2 C16A C18A -10(2) . . . . ? C1 C2 C16A C17A -66.8(19) . . . . ? C3 C2 C16A C17A 108.0(18) . . . . ? C8 C7 C20 C22 113.7(13) . . . . ? C6 C7 C20 C22 -63.9(15) . . . . ? C8 C7 C20 C23 -124.1(13) . . . . ? C6 C7 C20 C23 58.3(14) . . . . ? C8 C7 C20 C21 -6.4(16) . . . . ? C6 C7 C20 C21 176.0(11) . . . . ? C4 P1 C24 C29 -78.7(10) . . . . ? C30 P1 C24 C29 31.7(11) . . . . ? Pt1 P1 C24 C29 162.5(9) . . . . ? C4 P1 C24 C25 98.8(10) . . . . ? C30 P1 C24 C25 -150.8(9) . . . . ? Pt1 P1 C24 C25 -20.1(11) . . . . ? C29 C24 C25 C26 1.9(17) . . . . ? P1 C24 C25 C26 -175.6(9) . . . . ? C24 C25 C26 C27 -3(2) . . . . ? C25 C26 C27 C28 2(2) . . . . ? C26 C27 C28 C29 0(3) . . . . ? C25 C24 C29 C28 0.5(19) . . . . ? P1 C24 C29 C28 177.9(11) . . . . ? C27 C28 C29 C24 -2(2) . . . . ? C4 P1 C30 C35 -28.8(11) . . . . ? C24 P1 C30 C35 -140.4(10) . . . . ? Pt1 P1 C30 C35 86.5(10) . . . . ? C4 P1 C30 C31 159.0(10) . . . . ? C24 P1 C30 C31 47.4(11) . . . . ? Pt1 P1 C30 C31 -85.7(10) . . . . ? C35 C30 C31 C32 2.8(18) . . . . ? P1 C30 C31 C32 175.1(10) . . . . ? C30 C31 C32 C33 -4(2) . . . . ? C31 C32 C33 C34 4(2) . . . . ? C32 C33 C34 C35 -3(2) . . . . ? C33 C34 C35 C30 1.5(19) . . . . ? C31 C30 C35 C34 -1.6(18) . . . . ? P1 C30 C35 C34 -173.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.389 _refine_diff_density_min -2.485 _refine_diff_density_rms 0.248 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.500 204 96 ' ' _platon_squeeze_details ; ;