Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 04-07-16 _audit_creation_method CRYSTALS_ver_12.20 _publ_contact_author_name 'Prof Jonathan Robin Dilworth' _publ_contact_author_address ; Chemistry Research Lab. University of Oxford 12 Mansfield Road Oxford OX1 3TA UNITED KINGDOM ; _publ_contact_author_email JON.DILWORTH@CHEM.OX.AC.UK _publ_section_title ; Synthesis, Structure and Catalytic Activity of Thioether-phosphane Complexes of Pd(II) and Pt(II) ; loop_ _publ_author_name _publ_author_address J.R.Dilworth ; Central Chemistry Laboratory University of Oxford Mansfield Road Oxford OX1 3QR UK ; 'C.A.Maresca von Beckh W.' ; Central Chemistry Laboratory University of Oxford Mansfield Road Oxford OX1 3QR UK ; S.I.Pascu ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK ; #========================================================================== ######################################## ## denoted [PdClMe(MeS~PPh2)] in text ## ######################################## data_1 _database_code_depnum_ccdc_archive 'CCDC 257327' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 8.7350(10) _cell_angle_alpha 101.530(2) _cell_length_b 9.2150(10) _cell_angle_beta 97.460(2) _cell_length_c 14.7010(10) _cell_angle_gamma 116.200(2) _cell_volume 1007.81(18) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C21 H22 Cl P Pd S ' _chemical_formula_moiety ' C21 H22 Cl P Pd S ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 479.30 _cell_measurement_reflns_used 8187 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.237 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.88 # Sheldrick geometric definitions 0.78 0.88 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 8328 _reflns_number_total 4579 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 4579 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4639 _diffrn_reflns_theta_min 2.679 _diffrn_reflns_theta_max 27.534 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.331 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -11 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -0.80 _refine_diff_density_max 3.13 _refine_ls_number_reflns 3219 _refine_ls_number_restraints 0 _refine_ls_number_parameters 226 #_refine_ls_R_factor_ref 0.0558 _refine_ls_wR_factor_ref 0.0568 _refine_ls_goodness_of_fit_ref 1.0815 #_reflns_number_all 4570 _refine_ls_R_factor_all 0.0848 _refine_ls_wR_factor_all 0.0653 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3219 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_gt 0.0568 _refine_ls_shift/su_max 0.000626 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.03 0.311 1.71 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pd1 Pd 0.28047(5) -0.13322(5) 0.71931(3) 0.0219 1.0000 Uani . . . . . . Cl1 Cl 0.24520(19) -0.40896(16) 0.69938(10) 0.0326 1.0000 Uani . . . . . . S1 S 0.14833(16) -0.20320(14) 0.54967(8) 0.0237 1.0000 Uani . . . . . . P1 P 0.30039(16) 0.11897(14) 0.74832(9) 0.0207 1.0000 Uani . . . . . . C1 C 0.3778(8) -0.0764(7) 0.8652(4) 0.0341 1.0000 Uani . . . . . . C2 C 0.1981(7) -0.3495(6) 0.4763(4) 0.0307 1.0000 Uani . . . . . . C3 C 0.2354(6) -0.0229(6) 0.5064(3) 0.0212 1.0000 Uani . . . . . . C4 C 0.2964(7) -0.0278(7) 0.4231(4) 0.0303 1.0000 Uani . . . . . . C5 C 0.3554(7) 0.1128(7) 0.3894(4) 0.0305 1.0000 Uani . . . . . . C6 C 0.3540(7) 0.2575(7) 0.4372(4) 0.0307 1.0000 Uani . . . . . . C7 C 0.2947(7) 0.2618(6) 0.5208(4) 0.0258 1.0000 Uani . . . . . . C8 C 0.2334(6) 0.1214(6) 0.5563(4) 0.0251 1.0000 Uani . . . . . . C9 C 0.1680(6) 0.1329(6) 0.6455(3) 0.0219 1.0000 Uani . . . . . . C10 C 0.5196(6) 0.2920(6) 0.7688(3) 0.0222 1.0000 Uani . . . . . . C11 C 0.6671(6) 0.2672(6) 0.7867(4) 0.0251 1.0000 Uani . . . . . . C12 C 0.8330(7) 0.3948(7) 0.7932(4) 0.0324 1.0000 Uani . . . . . . C13 C 0.8550(7) 0.5488(7) 0.7830(4) 0.0353 1.0000 Uani . . . . . . C14 C 0.7130(9) 0.5760(7) 0.7684(4) 0.0383 1.0000 Uani . . . . . . C15 C 0.5430(7) 0.4493(6) 0.7608(4) 0.0322 1.0000 Uani . . . . . . C16 C 0.2015(7) 0.1729(7) 0.8423(4) 0.0267 1.0000 Uani . . . . . . C17 C 0.2763(7) 0.3313(7) 0.9091(4) 0.0360 1.0000 Uani . . . . . . C18 C 0.1841(9) 0.3641(8) 0.9734(4) 0.0426 1.0000 Uani . . . . . . C19 C 0.0191(9) 0.2417(8) 0.9725(4) 0.0404 1.0000 Uani . . . . . . C20 C -0.0561(8) 0.0853(8) 0.9058(5) 0.0409 1.0000 Uani . . . . . . C21 C 0.0340(8) 0.0508(7) 0.8419(4) 0.0375 1.0000 Uani . . . . . . H41 H 0.2976 -0.1320 0.3881 0.0355 1.0000 Uiso . . . . . . H51 H 0.3992 0.1095 0.3298 0.0376 1.0000 Uiso . . . . . . H61 H 0.3952 0.3580 0.4121 0.0364 1.0000 Uiso . . . . . . H71 H 0.2959 0.3671 0.5561 0.0320 1.0000 Uiso . . . . . . H91 H 0.1683 0.2435 0.6641 0.0244 1.0000 Uiso . . . . . . H92 H 0.0448 0.0384 0.6307 0.0244 1.0000 Uiso . . . . . . H111 H 0.6517 0.1567 0.7947 0.0293 1.0000 Uiso . . . . . . H121 H 0.9373 0.3762 0.8054 0.0363 1.0000 Uiso . . . . . . H131 H 0.9749 0.6401 0.7862 0.0369 1.0000 Uiso . . . . . . H141 H 0.7312 0.6887 0.7630 0.0418 1.0000 Uiso . . . . . . H151 H 0.4401 0.4703 0.7499 0.0357 1.0000 Uiso . . . . . . H171 H 0.3960 0.4212 0.9108 0.0378 1.0000 Uiso . . . . . . H181 H 0.2382 0.4782 1.0211 0.0466 1.0000 Uiso . . . . . . H191 H -0.0453 0.2660 1.0198 0.0523 1.0000 Uiso . . . . . . H201 H -0.1766 -0.0034 0.9038 0.0467 1.0000 Uiso . . . . . . H211 H -0.0215 -0.0636 0.7945 0.0417 1.0000 Uiso . . . . . . H21 H 0.1536 -0.4561 0.4956 0.0370 1.0000 Uiso . . . . . . H22 H 0.3285 -0.2983 0.4848 0.0370 1.0000 Uiso . . . . . . H23 H 0.1400 -0.3754 0.4075 0.0370 1.0000 Uiso . . . . . . H11 H 0.3872 -0.1741 0.8796 0.0417 1.0000 Uiso . . . . . . H12 H 0.2964 -0.0534 0.9001 0.0417 1.0000 Uiso . . . . . . H13 H 0.4969 0.0258 0.8863 0.0417 1.0000 Uiso . . . . . . 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 0.0244(2) 0.01791(18) 0.0253(2) 0.00695(13) 0.00724(14) 0.01125(14) Cl1 0.0407(7) 0.0256(6) 0.0403(7) 0.0123(5) 0.0129(6) 0.0214(5) S1 0.0268(6) 0.0182(5) 0.0251(6) 0.0039(4) 0.0069(5) 0.0110(5) P1 0.0210(6) 0.0174(5) 0.0235(6) 0.0061(4) 0.0064(5) 0.0086(5) C1 0.041(3) 0.036(3) 0.028(3) 0.011(2) 0.006(2) 0.020(2) C2 0.038(3) 0.022(2) 0.033(3) 0.003(2) 0.009(2) 0.016(2) C3 0.023(2) 0.021(2) 0.021(2) 0.0095(17) 0.0080(18) 0.0099(18) C4 0.029(3) 0.030(2) 0.029(3) 0.003(2) 0.006(2) 0.015(2) C5 0.030(3) 0.039(3) 0.026(2) 0.011(2) 0.010(2) 0.017(2) C6 0.026(2) 0.029(2) 0.036(3) 0.013(2) 0.010(2) 0.010(2) C7 0.028(2) 0.025(2) 0.027(2) 0.0085(19) 0.007(2) 0.014(2) C8 0.020(2) 0.026(2) 0.028(2) 0.0034(19) 0.0036(19) 0.0133(19) C9 0.023(2) 0.021(2) 0.018(2) -0.0035(17) -0.0005(17) 0.0119(18) C10 0.019(2) 0.023(2) 0.019(2) 0.0025(17) 0.0069(17) 0.0071(18) C11 0.021(2) 0.029(2) 0.024(2) 0.0016(18) 0.0048(18) 0.0127(19) C12 0.022(2) 0.036(3) 0.033(3) 0.001(2) 0.007(2) 0.012(2) C13 0.030(3) 0.031(3) 0.031(3) 0.005(2) 0.008(2) 0.005(2) C14 0.049(4) 0.026(2) 0.030(3) 0.012(2) 0.008(3) 0.008(2) C15 0.029(3) 0.023(2) 0.038(3) 0.006(2) 0.001(2) 0.009(2) C16 0.032(3) 0.030(2) 0.027(2) 0.014(2) 0.013(2) 0.019(2) C17 0.029(3) 0.038(3) 0.027(3) -0.006(2) 0.007(2) 0.011(2) C18 0.044(3) 0.042(3) 0.031(3) -0.007(2) 0.011(3) 0.018(3) C19 0.048(3) 0.055(4) 0.028(3) 0.010(3) 0.019(3) 0.031(3) C20 0.036(3) 0.040(3) 0.040(3) 0.011(3) 0.018(3) 0.011(3) C21 0.041(3) 0.026(2) 0.037(3) 0.004(2) 0.014(3) 0.010(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl1 . 2.3717(13) yes Pd1 . S1 . 2.4331(13) yes Pd1 . P1 . 2.2001(12) yes Pd1 . C1 . 2.069(6) yes S1 . C2 . 1.797(5) yes S1 . C3 . 1.781(4) yes P1 . C9 . 1.842(5) yes P1 . C10 . 1.806(5) yes P1 . C16 . 1.821(5) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . C4 . 1.399(7) yes C3 . C8 . 1.393(7) yes C4 . C5 . 1.387(8) yes C4 . H41 . 1.000 no C5 . C6 . 1.383(8) yes C5 . H51 . 1.000 no C6 . C7 . 1.394(7) yes C6 . H61 . 1.000 no C7 . C8 . 1.401(7) yes C7 . H71 . 1.000 no C8 . C9 . 1.499(7) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . C11 . 1.406(7) yes C10 . C15 . 1.404(7) yes C11 . C12 . 1.380(7) yes C11 . H111 . 1.000 no C12 . C13 . 1.388(8) yes C12 . H121 . 1.000 no C13 . C14 . 1.369(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.398(8) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.393(7) yes C16 . C21 . 1.396(8) yes C17 . C18 . 1.390(8) yes C17 . H171 . 1.000 no C18 . C19 . 1.380(9) yes C18 . H181 . 1.000 no C19 . C20 . 1.379(9) yes C19 . H191 . 1.000 no C20 . C21 . 1.377(8) yes C20 . H201 . 1.000 no C21 . H211 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Pd1 . S1 . 91.05(5) yes Cl1 . Pd1 . P1 . 174.74(5) yes S1 . Pd1 . P1 . 92.09(4) yes Cl1 . Pd1 . C1 . 89.51(16) yes S1 . Pd1 . C1 . 176.44(18) yes P1 . Pd1 . C1 . 87.10(16) yes Pd1 . S1 . C2 . 112.37(19) yes Pd1 . S1 . C3 . 111.61(16) yes C2 . S1 . C3 . 103.7(2) yes Pd1 . P1 . C9 . 110.48(15) yes Pd1 . P1 . C10 . 115.19(16) yes C9 . P1 . C10 . 105.1(2) yes Pd1 . P1 . C16 . 116.29(17) yes C9 . P1 . C16 . 99.8(2) yes C10 . P1 . C16 . 108.4(2) yes Pd1 . C1 . H11 . 109.468 no Pd1 . C1 . H12 . 109.468 no H11 . C1 . H12 . 109.476 no Pd1 . C1 . H13 . 109.467 no H11 . C1 . H13 . 109.474 no H12 . C1 . H13 . 109.475 no S1 . C2 . H21 . 109.467 no S1 . C2 . H22 . 109.466 no H21 . C2 . H22 . 109.474 no S1 . C2 . H23 . 109.468 no H21 . C2 . H23 . 109.476 no H22 . C2 . H23 . 109.476 no S1 . C3 . C4 . 121.4(4) yes S1 . C3 . C8 . 117.6(4) yes C4 . C3 . C8 . 120.9(4) yes C3 . C4 . C5 . 119.6(5) yes C3 . C4 . H41 . 120.196 no C5 . C4 . H41 . 120.196 no C4 . C5 . C6 . 120.7(5) yes C4 . C5 . H51 . 119.665 no C6 . C5 . H51 . 119.669 no C5 . C6 . C7 . 119.3(5) yes C5 . C6 . H61 . 120.351 no C7 . C6 . H61 . 120.351 no C6 . C7 . C8 . 121.3(5) yes C6 . C7 . H71 . 119.332 no C8 . C7 . H71 . 119.333 no C7 . C8 . C3 . 118.2(5) yes C7 . C8 . C9 . 118.8(4) yes C3 . C8 . C9 . 123.1(4) yes C8 . C9 . P1 . 114.4(3) yes C8 . C9 . H91 . 108.231 no P1 . C9 . H91 . 108.232 no C8 . C9 . H92 . 108.231 no P1 . C9 . H92 . 108.232 no H91 . C9 . H92 . 109.466 no P1 . C10 . C11 . 120.4(4) yes P1 . C10 . C15 . 120.1(4) yes C11 . C10 . C15 . 119.5(4) yes C10 . C11 . C12 . 120.3(5) yes C10 . C11 . H111 . 119.845 no C12 . C11 . H111 . 119.843 no C11 . C12 . C13 . 120.0(5) yes C11 . C12 . H121 . 119.985 no C13 . C12 . H121 . 119.987 no C12 . C13 . C14 . 120.2(5) yes C12 . C13 . H131 . 119.922 no C14 . C13 . H131 . 119.920 no C13 . C14 . C15 . 121.3(5) yes C13 . C14 . H141 . 119.355 no C15 . C14 . H141 . 119.355 no C10 . C15 . C14 . 118.7(5) yes C10 . C15 . H151 . 120.644 no C14 . C15 . H151 . 120.645 no P1 . C16 . C17 . 124.1(4) yes P1 . C16 . C21 . 117.2(4) yes C17 . C16 . C21 . 118.5(5) yes C16 . C17 . C18 . 119.8(5) yes C16 . C17 . H171 . 120.090 no C18 . C17 . H171 . 120.090 no C17 . C18 . C19 . 121.0(5) yes C17 . C18 . H181 . 119.504 no C19 . C18 . H181 . 119.502 no C18 . C19 . C20 . 119.3(5) yes C18 . C19 . H191 . 120.335 no C20 . C19 . H191 . 120.333 no C19 . C20 . C21 . 120.3(6) yes C19 . C20 . H201 . 119.843 no C21 . C20 . H201 . 119.843 no C16 . C21 . C20 . 121.0(5) yes C16 . C21 . H211 . 119.476 no C20 . C21 . H211 . 119.477 no #===END ######################################## ## denoted [PtMe2(MeS~PPh2)] in text ## ######################################## data_2 _database_code_depnum_ccdc_archive 'CCDC 257328' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 8.7885(2) _cell_angle_alpha 90 _cell_length_b 15.0806(3) _cell_angle_beta 104.9820(8) _cell_length_c 16.1036(4) _cell_angle_gamma 90 _cell_volume 2061.75(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'Pt ' -2.3520 8.3880 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C22 H25 P1 Pt1 S1 ' _chemical_formula_moiety ' C22 H25 P1 Pt1 S1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 547.57 _cell_measurement_reflns_used 3755 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 6.986 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.094 _exptl_absorpt_correction_T_max 0.247 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 7962 _reflns_number_total 4666 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 4666 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4722 _diffrn_reflns_theta_min 2.701 _diffrn_reflns_theta_max 27.470 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.921 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -1.26 _refine_diff_density_max 1.11 _refine_ls_number_reflns 4256 _refine_ls_number_restraints 0 _refine_ls_number_parameters 226 #_refine_ls_R_factor_ref 0.0210 _refine_ls_wR_factor_ref 0.0268 _refine_ls_goodness_of_fit_ref 1.0168 #_reflns_number_all 4661 _refine_ls_R_factor_all 0.0236 _refine_ls_wR_factor_all 0.0289 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4256 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_gt 0.0268 _refine_ls_shift/su_max 0.003813 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.89 -0.165 1.57 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.653629(8) 0.334603(5) 0.334515(5) 0.0215 1.0000 Uani . . . . 3 . S1 S 0.80956(7) 0.38215(4) 0.46824(4) 0.0316 1.0000 Uani . . . . 3 . P1 P 0.70510(7) 0.46193(4) 0.27288(4) 0.0235 1.0000 Uani . . . . 3 . C1 C 0.6150(3) 0.21141(16) 0.38634(18) 0.0342 1.0000 Uani . . . . 3 . C2 C 0.5195(3) 0.28913(19) 0.21774(16) 0.0349 1.0000 Uani . . . . 3 . C3 C 0.7556(5) 0.32786(19) 0.5562(2) 0.0507 1.0000 Uani . . . . 3 . C4 C 0.7624(3) 0.49537(16) 0.48257(15) 0.0279 1.0000 Uani . . . . 3 . C5 C 0.7013(3) 0.52268(17) 0.54977(16) 0.0326 1.0000 Uani . . . . 3 . C6 C 0.6724(3) 0.61203(19) 0.55953(18) 0.0376 1.0000 Uani . . . . 3 . C7 C 0.7017(4) 0.67334(17) 0.5018(2) 0.0363 1.0000 Uani . . . . 3 . C8 C 0.7599(3) 0.64574(18) 0.43358(18) 0.0331 1.0000 Uani . . . . 3 . C9 C 0.7932(3) 0.55703(16) 0.42362(15) 0.0265 1.0000 Uani . . . . 3 . C10 C 0.8560(3) 0.52851(16) 0.34901(16) 0.0293 1.0000 Uani . . . . 3 . C11 C 0.5479(3) 0.54250(16) 0.23583(14) 0.0263 1.0000 Uani . . . . 3 . C12 C 0.3962(3) 0.52235(16) 0.24040(15) 0.0287 1.0000 Uani . . . . 3 . C13 C 0.2761(3) 0.58500(19) 0.21684(17) 0.0349 1.0000 Uani . . . . 3 . C14 C 0.3087(4) 0.66834(17) 0.1884(2) 0.0395 1.0000 Uani . . . . 3 . C15 C 0.4590(4) 0.6882(2) 0.1824(2) 0.0424 1.0000 Uani . . . . 3 . C16 C 0.5790(3) 0.62617(18) 0.20634(18) 0.0361 1.0000 Uani . . . . 3 . C17 C 0.7905(3) 0.44706(16) 0.18193(17) 0.0314 1.0000 Uani . . . . 3 . C18 C 0.9402(4) 0.4092(2) 0.1970(2) 0.0465 1.0000 Uani . . . . 3 . C19 C 1.0059(5) 0.3932(3) 0.1285(3) 0.0611 1.0000 Uani . . . . 3 . C20 C 0.9224(5) 0.4134(2) 0.0455(3) 0.0584 1.0000 Uani . . . . 3 . C21 C 0.7749(6) 0.4493(3) 0.0303(2) 0.0622 1.0000 Uani . . . . 3 . C22 C 0.7083(4) 0.4665(2) 0.09843(19) 0.0478 1.0000 Uani . . . . 3 . H51 H 0.6784 0.4782 0.5909 0.0380 1.0000 Uiso . . . . 3 . H61 H 0.6302 0.6321 0.6084 0.0450 1.0000 Uiso . . . . 3 . H71 H 0.6810 0.7377 0.5090 0.0434 1.0000 Uiso . . . . 3 . H81 H 0.7780 0.6903 0.3912 0.0396 1.0000 Uiso . . . . 3 . H101 H 0.8822 0.5822 0.3189 0.0357 1.0000 Uiso . . . . 3 . H102 H 0.9531 0.4920 0.3708 0.0357 1.0000 Uiso . . . . 3 . H121 H 0.3728 0.4625 0.2608 0.0346 1.0000 Uiso . . . . 3 . H131 H 0.1671 0.5702 0.2204 0.0428 1.0000 Uiso . . . . 3 . H141 H 0.2233 0.7138 0.1722 0.0480 1.0000 Uiso . . . . 3 . H151 H 0.4814 0.7477 0.1607 0.0516 1.0000 Uiso . . . . 3 . H161 H 0.6878 0.6413 0.2025 0.0445 1.0000 Uiso . . . . 3 . H181 H 1.0001 0.3937 0.2569 0.0592 1.0000 Uiso . . . . 3 . H191 H 1.1137 0.3669 0.1394 0.0797 1.0000 Uiso . . . . 3 . H201 H 0.9700 0.4017 -0.0035 0.0788 1.0000 Uiso . . . . 3 . H211 H 0.7145 0.4632 -0.0299 0.0803 1.0000 Uiso . . . . 3 . H221 H 0.6006 0.4931 0.0868 0.0600 1.0000 Uiso . . . . 3 . H31 H 0.8245 0.3498 0.6119 0.0553 1.0000 Uiso . . . . 3 . H32 H 0.6431 0.3413 0.5536 0.0553 1.0000 Uiso . . . . 3 . H33 H 0.7694 0.2623 0.5519 0.0553 1.0000 Uiso . . . . 3 . H11 H 0.5465 0.1740 0.3403 0.0433 1.0000 Uiso . . . . 3 . H12 H 0.7182 0.1809 0.4098 0.0433 1.0000 Uiso . . . . 3 . H13 H 0.5618 0.2207 0.4336 0.0433 1.0000 Uiso . . . . 3 . H21 H 0.5124 0.3362 0.1732 0.0422 1.0000 Uiso . . . . 3 . H22 H 0.5696 0.2349 0.2007 0.0422 1.0000 Uiso . . . . 3 . H23 H 0.4113 0.2742 0.2227 0.0422 1.0000 Uiso . . . . 3 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01839(7) 0.01968(7) 0.02664(7) -0.00450(2) 0.00640(4) -0.00076(2) S1 0.0264(3) 0.0275(3) 0.0336(3) -0.0016(2) -0.0057(2) 0.0038(2) P1 0.0221(3) 0.0236(3) 0.0262(3) -0.0045(2) 0.0091(2) -0.0033(2) C1 0.0400(13) 0.0234(10) 0.0449(14) 0.0017(10) 0.0213(11) 0.0018(10) C2 0.0381(13) 0.0380(13) 0.0293(11) -0.0114(10) 0.0098(10) -0.0118(11) C3 0.072(2) 0.0366(15) 0.0300(14) 0.0099(10) -0.0116(14) 0.0043(13) C4 0.0233(10) 0.0272(11) 0.0284(10) -0.0042(9) -0.0018(8) -0.0011(8) C5 0.0332(12) 0.0361(13) 0.0259(11) -0.0017(9) 0.0027(9) 0.0010(10) C6 0.0395(14) 0.0416(14) 0.0314(12) -0.0064(10) 0.0085(10) 0.0069(11) C7 0.0399(15) 0.0315(13) 0.0371(14) -0.0088(10) 0.0093(12) 0.0013(10) C8 0.0356(13) 0.0295(11) 0.0340(12) -0.0053(10) 0.0088(10) -0.0051(10) C9 0.0198(10) 0.0306(11) 0.0272(10) -0.0068(9) 0.0029(8) -0.0041(8) C10 0.0239(10) 0.0303(11) 0.0349(12) -0.0085(9) 0.0099(9) -0.0053(9) C11 0.0311(11) 0.0260(10) 0.0234(10) -0.0032(8) 0.0100(9) -0.0011(9) C12 0.0300(11) 0.0300(11) 0.0265(11) 0.0028(8) 0.0081(9) 0.0008(9) C13 0.0306(12) 0.0422(14) 0.0342(12) 0.0047(10) 0.0124(10) 0.0062(10) C14 0.0504(18) 0.0353(15) 0.0343(14) 0.0059(10) 0.0136(13) 0.0109(11) C15 0.0562(18) 0.0274(12) 0.0453(16) 0.0064(11) 0.0161(13) 0.0004(12) C16 0.0395(14) 0.0313(13) 0.0404(14) 0.0021(10) 0.0159(11) -0.0049(11) C17 0.0361(13) 0.0251(11) 0.0388(12) -0.0085(9) 0.0200(10) -0.0103(10) C18 0.0419(16) 0.0464(16) 0.0598(18) -0.0079(14) 0.0285(15) 0.0042(13) C19 0.057(2) 0.0528(19) 0.090(3) -0.0251(19) 0.048(2) -0.0057(16) C20 0.088(3) 0.0420(16) 0.067(2) -0.0224(15) 0.059(2) -0.0164(16) C21 0.097(3) 0.059(2) 0.0445(17) -0.0095(15) 0.0441(19) -0.001(2) C22 0.0617(19) 0.0562(18) 0.0321(14) -0.0072(12) 0.0242(13) 0.0013(15) _refine_ls_extinction_coef 95.500 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 . 2.3460(6) yes Pt1 . P1 . 2.2603(6) yes Pt1 . C1 . 2.100(2) yes Pt1 . C2 . 2.062(2) yes S1 . C3 . 1.803(4) yes S1 . C4 . 1.786(2) yes P1 . C10 . 1.852(2) yes P1 . C11 . 1.821(2) yes P1 . C17 . 1.824(2) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C4 . C5 . 1.389(4) yes C4 . C9 . 1.405(4) yes C5 . C6 . 1.388(4) yes C5 . H51 . 1.000 no C6 . C7 . 1.382(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.390(4) yes C7 . H71 . 1.000 no C8 . C9 . 1.388(4) yes C8 . H81 . 1.000 no C9 . C10 . 1.508(3) yes C10 . H101 . 1.000 no C10 . H102 . 1.000 no C11 . C12 . 1.388(3) yes C11 . C16 . 1.400(3) yes C12 . C13 . 1.394(3) yes C12 . H121 . 1.000 no C13 . C14 . 1.393(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.382(5) yes C14 . H141 . 1.000 no C15 . C16 . 1.388(4) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C17 . C18 . 1.397(4) yes C17 . C22 . 1.383(4) yes C18 . C19 . 1.392(5) yes C18 . H181 . 1.000 no C19 . C20 . 1.382(6) yes C19 . H191 . 1.000 no C20 . C21 . 1.367(6) yes C20 . H201 . 1.000 no C21 . C22 . 1.394(4) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pt1 . P1 . 90.44(2) yes S1 . Pt1 . C1 . 91.25(8) yes P1 . Pt1 . C1 . 175.84(7) yes S1 . Pt1 . C2 . 178.30(8) yes P1 . Pt1 . C2 . 90.81(8) yes C1 . Pt1 . C2 . 87.43(11) yes Pt1 . S1 . C3 . 111.88(11) yes Pt1 . S1 . C4 . 108.11(7) yes C3 . S1 . C4 . 102.45(14) yes Pt1 . P1 . C10 . 111.11(9) yes Pt1 . P1 . C11 . 119.33(8) yes C10 . P1 . C11 . 102.00(11) yes Pt1 . P1 . C17 . 114.76(8) yes C10 . P1 . C17 . 103.04(11) yes C11 . P1 . C17 . 104.69(12) yes Pt1 . C1 . H11 . 109.463 no Pt1 . C1 . H12 . 109.467 no H11 . C1 . H12 . 109.469 no Pt1 . C1 . H13 . 109.471 no H11 . C1 . H13 . 109.476 no H12 . C1 . H13 . 109.482 no Pt1 . C2 . H21 . 109.469 no Pt1 . C2 . H22 . 109.473 no H21 . C2 . H22 . 109.475 no Pt1 . C2 . H23 . 109.468 no H21 . C2 . H23 . 109.468 no H22 . C2 . H23 . 109.474 no S1 . C3 . H31 . 109.463 no S1 . C3 . H32 . 109.470 no H31 . C3 . H32 . 109.484 no S1 . C3 . H33 . 109.461 no H31 . C3 . H33 . 109.469 no H32 . C3 . H33 . 109.481 no S1 . C4 . C5 . 122.3(2) yes S1 . C4 . C9 . 116.98(19) yes C5 . C4 . C9 . 120.8(2) yes C4 . C5 . C6 . 119.7(2) yes C4 . C5 . H51 . 120.153 no C6 . C5 . H51 . 120.154 no C5 . C6 . C7 . 120.1(2) yes C5 . C6 . H61 . 119.951 no C7 . C6 . H61 . 119.944 no C6 . C7 . C8 . 120.1(2) yes C6 . C7 . H71 . 119.926 no C8 . C7 . H71 . 119.924 no C7 . C8 . C9 . 120.8(3) yes C7 . C8 . H81 . 119.610 no C9 . C8 . H81 . 119.600 no C4 . C9 . C8 . 118.5(2) yes C4 . C9 . C10 . 121.6(2) yes C8 . C9 . C10 . 119.9(2) yes C9 . C10 . P1 . 109.59(15) yes C9 . C10 . H101 . 109.437 no P1 . C10 . H101 . 109.442 no C9 . C10 . H102 . 109.440 no P1 . C10 . H102 . 109.445 no H101 . C10 . H102 . 109.469 no P1 . C11 . C12 . 119.63(18) yes P1 . C11 . C16 . 120.95(19) yes C12 . C11 . C16 . 119.4(2) yes C11 . C12 . C13 . 120.5(2) yes C11 . C12 . H121 . 119.767 no C13 . C12 . H121 . 119.770 no C12 . C13 . C14 . 119.7(3) yes C12 . C13 . H131 . 120.130 no C14 . C13 . H131 . 120.134 no C13 . C14 . C15 . 120.0(3) yes C13 . C14 . H141 . 119.998 no C15 . C14 . H141 . 119.996 no C14 . C15 . C16 . 120.4(3) yes C14 . C15 . H151 . 119.809 no C16 . C15 . H151 . 119.789 no C11 . C16 . C15 . 120.0(3) yes C11 . C16 . H161 . 119.986 no C15 . C16 . H161 . 119.986 no P1 . C17 . C18 . 118.4(2) yes P1 . C17 . C22 . 122.3(2) yes C18 . C17 . C22 . 119.1(3) yes C17 . C18 . C19 . 119.9(3) yes C17 . C18 . H181 . 120.052 no C19 . C18 . H181 . 120.052 no C18 . C19 . C20 . 120.2(3) yes C18 . C19 . H191 . 119.915 no C20 . C19 . H191 . 119.910 no C19 . C20 . C21 . 120.1(3) yes C19 . C20 . H201 . 119.924 no C21 . C20 . H201 . 119.956 no C20 . C21 . C22 . 120.3(4) yes C20 . C21 . H211 . 119.848 no C22 . C21 . H211 . 119.853 no C21 . C22 . C17 . 120.4(3) yes C21 . C22 . H221 . 119.819 no C17 . C22 . H221 . 119.817 no #===END ######################################## ## denoted [PdCl2(MeS~PPh2)] in text ## ######################################## data_3 _database_code_depnum_ccdc_archive 'CCDC 257329' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.3529(2) _cell_angle_alpha 86.8988(8) _cell_length_b 11.5466(2) _cell_angle_beta 78.5238(8) _cell_length_c 19.6892(4) _cell_angle_gamma 87.2643(7) _cell_volume 2301.59(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C42 H42 Cl8 P2 Pd2 S2 ' _chemical_formula_moiety ' C42 H42 Cl8 P2 Pd2 S2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1169.30 _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.437 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.75 # Sheldrick geometric definitions 0.65 0.75 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 19293 _reflns_number_total 10514 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 10514 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10550 _diffrn_reflns_theta_min 1.056 _diffrn_reflns_theta_max 27.476 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.476 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.68 _refine_diff_density_max 0.92 _refine_ls_number_reflns 6679 _refine_ls_number_restraints 0 _refine_ls_number_parameters 505 #_refine_ls_R_factor_ref 0.0308 _refine_ls_wR_factor_ref 0.0335 _refine_ls_goodness_of_fit_ref 1.0776 #_reflns_number_all 10480 _refine_ls_R_factor_all 0.0633 _refine_ls_wR_factor_all 0.0633 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6679 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_gt 0.0335 _refine_ls_shift/su_max 0.003406 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.305 0.742E-01 0.869E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) SIR97: a new tool for crystal structure determination and refinement.J. App. Cryst. 32, 115-119 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pd1 Pd 0.68163(3) 0.08862(2) 0.198314(14) 0.0182 1.0000 Uani . . . . . . Pd2 Pd 1.11318(3) 0.23324(2) 0.356172(14) 0.0182 1.0000 Uani . . . . . . P1 P 0.56655(9) 0.23446(8) 0.15470(5) 0.0180 1.0000 Uani . . . . . . P2 P 1.00223(9) 0.36362(8) 0.29779(5) 0.0179 1.0000 Uani . . . . . . S1 S 0.50083(9) 0.05850(8) 0.28506(5) 0.0229 1.0000 Uani . . . . . . S2 S 0.97104(10) 0.09647(8) 0.33970(5) 0.0247 1.0000 Uani . . . . . . C1 C 0.3921(4) 0.2391(3) 0.19863(19) 0.0230 1.0000 Uani . . . . . . C2 C 0.3298(4) 0.1233(3) 0.20188(19) 0.0213 1.0000 Uani . . . . . . C3 C 0.3715(4) 0.0297(3) 0.24223(19) 0.0231 1.0000 Uani . . . . . . C4 C 0.3092(4) -0.0763(4) 0.2489(2) 0.0291 1.0000 Uani . . . . . . C5 C 0.2039(4) -0.0885(4) 0.2167(2) 0.0334 1.0000 Uani . . . . . . C6 C 0.1612(4) 0.0023(4) 0.1763(2) 0.0334 1.0000 Uani . . . . . . C7 C 0.2260(4) 0.1066(3) 0.1684(2) 0.0256 1.0000 Uani . . . . . . C8 C 0.5175(4) -0.0727(4) 0.3361(2) 0.0330 1.0000 Uani . . . . . . C9 C 0.6195(4) 0.3812(3) 0.16028(18) 0.0191 1.0000 Uani . . . . . . C10 C 0.7318(4) 0.4194(3) 0.1141(2) 0.0260 1.0000 Uani . . . . . . C11 C 0.7780(4) 0.5287(4) 0.1192(2) 0.0287 1.0000 Uani . . . . . . C12 C 0.7128(4) 0.6021(3) 0.1697(2) 0.0294 1.0000 Uani . . . . . . C13 C 0.6007(5) 0.5648(4) 0.2150(2) 0.0314 1.0000 Uani . . . . . . C14 C 0.5537(4) 0.4549(3) 0.21101(19) 0.0252 1.0000 Uani . . . . . . C15 C 0.5596(3) 0.2226(3) 0.06403(18) 0.0202 1.0000 Uani . . . . . . C16 C 0.4961(4) 0.3118(4) 0.0314(2) 0.0277 1.0000 Uani . . . . . . C17 C 0.4798(4) 0.3028(4) -0.0361(2) 0.0336 1.0000 Uani . . . . . . C18 C 0.5255(5) 0.2040(4) -0.0715(2) 0.0367 1.0000 Uani . . . . . . C19 C 0.5892(5) 0.1159(4) -0.0396(2) 0.0348 1.0000 Uani . . . . . . C20 C 0.6060(4) 0.1239(3) 0.0283(2) 0.0265 1.0000 Uani . . . . . . C21 C 0.8551(4) 0.3021(4) 0.27613(19) 0.0247 1.0000 Uani . . . . . . C22 C 0.7662(4) 0.2503(3) 0.33912(18) 0.0215 1.0000 Uani . . . . . . C23 C 0.8099(4) 0.1524(3) 0.37474(19) 0.0222 1.0000 Uani . . . . . . C24 C 0.7276(4) 0.1014(3) 0.4320(2) 0.0276 1.0000 Uani . . . . . . C25 C 0.6005(4) 0.1484(4) 0.4539(2) 0.0313 1.0000 Uani . . . . . . C26 C 0.5565(4) 0.2450(4) 0.4188(2) 0.0293 1.0000 Uani . . . . . . C27 C 0.6401(4) 0.2970(3) 0.3627(2) 0.0256 1.0000 Uani . . . . . . C28 C 0.9852(5) -0.0343(4) 0.3915(3) 0.0376 1.0000 Uani . . . . . . C29 C 0.9375(4) 0.4875(3) 0.34724(19) 0.0217 1.0000 Uani . . . . . . C30 C 0.9222(4) 0.4802(3) 0.41956(19) 0.0241 1.0000 Uani . . . . . . C31 C 0.8695(4) 0.5742(4) 0.4582(2) 0.0299 1.0000 Uani . . . . . . C32 C 0.8304(4) 0.6750(4) 0.4257(2) 0.0317 1.0000 Uani . . . . . . C33 C 0.8432(5) 0.6826(4) 0.3543(2) 0.0355 1.0000 Uani . . . . . . C34 C 0.8968(4) 0.5891(4) 0.3151(2) 0.0283 1.0000 Uani . . . . . . C35 C 1.0912(4) 0.4235(3) 0.21553(18) 0.0199 1.0000 Uani . . . . . . C36 C 1.1801(4) 0.5118(3) 0.2154(2) 0.0257 1.0000 Uani . . . . . . C37 C 1.2511(4) 0.5567(4) 0.1534(2) 0.0301 1.0000 Uani . . . . . . C38 C 1.2342(4) 0.5150(4) 0.0910(2) 0.0309 1.0000 Uani . . . . . . C39 C 1.1458(4) 0.4294(4) 0.0903(2) 0.0289 1.0000 Uani . . . . . . C40 C 1.0749(4) 0.3832(3) 0.15261(19) 0.0230 1.0000 Uani . . . . . . C41 C 0.9622(4) -0.1336(3) 0.0582(2) 0.0320 1.0000 Uani . . . . . . C42 C 0.6527(6) 0.3906(5) 0.5549(3) 0.0486 1.0000 Uani . . . . . . Cl1 Cl 0.80205(10) -0.07181(9) 0.23558(5) 0.0312 1.0000 Uani . . . . . . Cl2 Cl 0.86308(9) 0.14346(8) 0.11560(5) 0.0243 1.0000 Uani . . . . . . Cl3 Cl 1.22548(10) 0.10490(9) 0.42358(5) 0.0297 1.0000 Uani . . . . . . Cl4 Cl 1.26133(9) 0.37675(8) 0.35855(4) 0.0233 1.0000 Uani . . . . . . Cl5 Cl 1.04300(12) -0.26281(10) 0.08150(8) 0.0493 1.0000 Uani . . . . . . Cl6 Cl 0.82494(12) -0.16089(11) 0.02180(7) 0.0454 1.0000 Uani . . . . . . Cl7 Cl 0.7569(2) 0.29953(17) 0.59519(12) 0.0868 1.0000 Uani . . . . . . Cl8 Cl 0.48504(16) 0.37096(13) 0.59056(8) 0.0603 1.0000 Uani . . . . . . H11 H 0.3862 0.2641 0.2470 0.0270 1.0000 Uiso . . . . . . H12 H 0.3425 0.2968 0.1728 0.0270 1.0000 Uiso . . . . . . H41 H 0.3407 -0.1429 0.2768 0.0346 1.0000 Uiso . . . . . . H51 H 0.1577 -0.1636 0.2227 0.0398 1.0000 Uiso . . . . . . H61 H 0.0850 -0.0073 0.1531 0.0406 1.0000 Uiso . . . . . . H71 H 0.1973 0.1711 0.1380 0.0308 1.0000 Uiso . . . . . . H101 H 0.7790 0.3676 0.0773 0.0305 1.0000 Uiso . . . . . . H111 H 0.8588 0.5549 0.0862 0.0349 1.0000 Uiso . . . . . . H121 H 0.7463 0.6809 0.1733 0.0373 1.0000 Uiso . . . . . . H131 H 0.5529 0.6176 0.2511 0.0383 1.0000 Uiso . . . . . . H141 H 0.4732 0.4289 0.2443 0.0308 1.0000 Uiso . . . . . . H161 H 0.4622 0.3830 0.0569 0.0330 1.0000 Uiso . . . . . . H171 H 0.4348 0.3676 -0.0593 0.0412 1.0000 Uiso . . . . . . H181 H 0.5124 0.1966 -0.1200 0.0445 1.0000 Uiso . . . . . . H191 H 0.6239 0.0453 -0.0656 0.0414 1.0000 Uiso . . . . . . H201 H 0.6512 0.0589 0.0512 0.0318 1.0000 Uiso . . . . . . H211 H 0.8842 0.2401 0.2422 0.0302 1.0000 Uiso . . . . . . H212 H 0.8047 0.3651 0.2546 0.0302 1.0000 Uiso . . . . . . H241 H 0.7594 0.0316 0.4572 0.0330 1.0000 Uiso . . . . . . H251 H 0.5408 0.1123 0.4950 0.0374 1.0000 Uiso . . . . . . H261 H 0.4645 0.2772 0.4339 0.0350 1.0000 Uiso . . . . . . H271 H 0.6093 0.3688 0.3390 0.0315 1.0000 Uiso . . . . . . H301 H 0.9494 0.4070 0.4434 0.0292 1.0000 Uiso . . . . . . H311 H 0.8597 0.5690 0.5098 0.0358 1.0000 Uiso . . . . . . H321 H 0.7927 0.7427 0.4537 0.0368 1.0000 Uiso . . . . . . H331 H 0.8139 0.7554 0.3309 0.0421 1.0000 Uiso . . . . . . H341 H 0.9061 0.5949 0.2635 0.0339 1.0000 Uiso . . . . . . H361 H 1.1919 0.5423 0.2603 0.0306 1.0000 Uiso . . . . . . H371 H 1.3146 0.6193 0.1534 0.0348 1.0000 Uiso . . . . . . H381 H 1.2863 0.5472 0.0463 0.0350 1.0000 Uiso . . . . . . H391 H 1.1328 0.4007 0.0452 0.0335 1.0000 Uiso . . . . . . H401 H 1.0118 0.3206 0.1521 0.0275 1.0000 Uiso . . . . . . H411 H 1.0259 -0.0875 0.0235 0.0382 1.0000 Uiso . . . . . . H412 H 0.9316 -0.0880 0.1006 0.0382 1.0000 Uiso . . . . . . H421 H 0.6732 0.4730 0.5601 0.0588 1.0000 Uiso . . . . . . H422 H 0.6691 0.3741 0.5045 0.0588 1.0000 Uiso . . . . . . H81 H 0.5893 -0.0652 0.3626 0.0396 1.0000 Uiso . . . . . . H82 H 0.4325 -0.0869 0.3691 0.0396 1.0000 Uiso . . . . . . H83 H 0.5400 -0.1392 0.3048 0.0396 1.0000 Uiso . . . . . . H281 H 1.0738 -0.0729 0.3756 0.0447 1.0000 Uiso . . . . . . H282 H 0.9748 -0.0151 0.4412 0.0447 1.0000 Uiso . . . . . . H283 H 0.9148 -0.0878 0.3864 0.0447 1.0000 Uiso . . . . . . 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 0.01741(14) 0.01848(14) 0.01854(13) 0.00045(11) -0.00368(10) -0.00100(11) Pd2 0.01849(14) 0.01855(14) 0.01711(13) 0.00053(10) -0.00294(10) -0.00106(11) P1 0.0170(4) 0.0182(4) 0.0181(4) -0.0005(3) -0.0018(3) 0.0001(4) P2 0.0193(4) 0.0181(4) 0.0166(4) 0.0012(3) -0.0047(3) -0.0026(4) S1 0.0221(5) 0.0276(5) 0.0190(4) 0.0014(4) -0.0033(4) -0.0058(4) S2 0.0261(5) 0.0195(4) 0.0277(5) -0.0026(4) -0.0029(4) -0.0031(4) C1 0.0195(18) 0.0232(19) 0.0248(19) -0.0038(15) -0.0006(15) 0.0030(15) C2 0.0181(18) 0.0230(18) 0.0210(18) -0.0069(15) 0.0015(14) 0.0004(14) C3 0.0208(18) 0.028(2) 0.0203(18) -0.0050(15) -0.0016(14) -0.0040(15) C4 0.029(2) 0.028(2) 0.030(2) -0.0012(17) -0.0031(17) -0.0050(17) C5 0.030(2) 0.031(2) 0.038(2) -0.0085(19) -0.0013(18) -0.0092(18) C6 0.024(2) 0.040(2) 0.038(2) -0.0122(19) -0.0066(18) -0.0001(18) C7 0.0198(18) 0.031(2) 0.027(2) -0.0066(16) -0.0056(15) 0.0057(16) C8 0.032(2) 0.037(2) 0.030(2) 0.0130(18) -0.0085(18) -0.0081(18) C9 0.0197(17) 0.0180(17) 0.0204(17) 0.0005(14) -0.0060(14) -0.0024(14) C10 0.026(2) 0.0243(19) 0.0256(19) 0.0023(16) -0.0028(16) 0.0033(16) C11 0.028(2) 0.027(2) 0.032(2) 0.0084(17) -0.0099(17) -0.0074(17) C12 0.039(2) 0.023(2) 0.031(2) 0.0016(16) -0.0182(18) -0.0062(17) C13 0.042(2) 0.024(2) 0.030(2) -0.0057(17) -0.0101(19) 0.0003(18) C14 0.031(2) 0.026(2) 0.0196(18) -0.0009(15) -0.0092(15) -0.0003(16) C15 0.0160(17) 0.0234(18) 0.0205(17) -0.0021(14) -0.0011(14) -0.0032(14) C16 0.025(2) 0.034(2) 0.0233(19) 0.0006(17) -0.0045(16) 0.0024(17) C17 0.029(2) 0.046(3) 0.028(2) 0.0063(19) -0.0121(17) -0.0054(19) C18 0.037(2) 0.055(3) 0.0195(19) -0.0029(19) -0.0050(17) -0.015(2) C19 0.038(2) 0.042(2) 0.024(2) -0.0121(18) 0.0010(18) -0.010(2) C20 0.026(2) 0.026(2) 0.027(2) -0.0022(16) -0.0043(16) -0.0039(16) C21 0.026(2) 0.033(2) 0.0161(17) 0.0004(15) -0.0071(15) -0.0050(16) C22 0.0230(19) 0.0256(19) 0.0172(17) -0.0028(14) -0.0054(14) -0.0057(15) C23 0.0190(18) 0.0258(19) 0.0217(18) -0.0038(15) -0.0018(14) -0.0064(15) C24 0.034(2) 0.0223(19) 0.026(2) 0.0027(16) -0.0046(17) -0.0092(16) C25 0.027(2) 0.040(2) 0.027(2) 0.0015(18) -0.0025(17) -0.0122(18) C26 0.0218(19) 0.042(2) 0.0234(19) -0.0061(17) -0.0019(16) -0.0017(17) C27 0.026(2) 0.027(2) 0.0257(19) 0.0007(16) -0.0098(16) -0.0029(16) C28 0.039(3) 0.019(2) 0.053(3) 0.0044(19) -0.007(2) -0.0016(18) C29 0.0198(18) 0.0253(19) 0.0189(17) -0.0012(14) -0.0002(14) -0.0053(15) C30 0.0228(19) 0.029(2) 0.0206(18) 0.0001(15) -0.0058(15) -0.0026(16) C31 0.028(2) 0.040(2) 0.0219(19) -0.0073(17) -0.0025(16) -0.0031(18) C32 0.031(2) 0.028(2) 0.032(2) -0.0096(17) 0.0038(17) -0.0038(17) C33 0.042(3) 0.022(2) 0.041(2) 0.0005(18) -0.007(2) 0.0055(18) C34 0.033(2) 0.028(2) 0.0241(19) 0.0045(16) -0.0065(17) -0.0012(17) C35 0.0199(17) 0.0195(17) 0.0183(17) -0.0001(14) -0.0002(14) 0.0022(14) C36 0.0238(19) 0.027(2) 0.0257(19) 0.0019(16) -0.0042(15) -0.0014(16) C37 0.026(2) 0.030(2) 0.031(2) 0.0079(17) -0.0010(17) 0.0015(17) C38 0.028(2) 0.031(2) 0.029(2) 0.0108(17) 0.0020(17) 0.0061(17) C39 0.034(2) 0.032(2) 0.0172(18) 0.0002(16) -0.0003(16) 0.0068(18) C40 0.027(2) 0.0207(18) 0.0213(18) -0.0012(14) -0.0057(15) 0.0037(15) C41 0.034(2) 0.020(2) 0.042(2) 0.0004(18) -0.0068(19) -0.0003(17) C42 0.066(4) 0.045(3) 0.036(3) -0.003(2) -0.007(2) -0.026(3) Cl1 0.0287(5) 0.0307(5) 0.0331(5) 0.0077(4) -0.0070(4) 0.0042(4) Cl2 0.0204(4) 0.0243(4) 0.0257(4) -0.0004(4) 0.0010(3) -0.0005(3) Cl3 0.0285(5) 0.0289(5) 0.0308(5) 0.0076(4) -0.0073(4) 0.0037(4) Cl4 0.0225(4) 0.0270(5) 0.0207(4) -0.0024(3) -0.0042(3) -0.0045(4) Cl5 0.0398(6) 0.0281(5) 0.0818(9) 0.0128(6) -0.0206(6) 0.0005(5) Cl6 0.0420(6) 0.0443(7) 0.0557(7) -0.0101(6) -0.0232(6) 0.0050(5) Cl7 0.0734(11) 0.0707(11) 0.1150(16) 0.0202(11) -0.0186(11) -0.0177(9) Cl8 0.0647(9) 0.0566(8) 0.0523(8) -0.0080(6) 0.0097(7) -0.0127(7) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . P1 . 2.2475(10) yes Pd1 . S1 . 2.295(1) yes Pd1 . Cl1 . 2.3496(10) yes Pd1 . Cl2 . 2.3166(9) yes Pd2 . P2 . 2.2540(10) yes Pd2 . S2 . 2.2873(10) yes Pd2 . Cl3 . 2.3549(10) yes Pd2 . Cl4 . 2.3195(9) yes P1 . C1 . 1.840(4) yes P1 . C9 . 1.821(4) yes P1 . C15 . 1.814(4) yes P2 . C21 . 1.844(4) yes P2 . C29 . 1.801(4) yes P2 . C35 . 1.816(4) yes S1 . C3 . 1.771(4) yes S1 . C8 . 1.792(4) yes S2 . C23 . 1.779(4) yes S2 . C28 . 1.792(4) yes C1 . C2 . 1.505(5) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C3 . 1.408(6) yes C2 . C7 . 1.394(5) yes C3 . C4 . 1.399(6) yes C4 . C5 . 1.382(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.391(7) yes C5 . H51 . 1.000 no C6 . C7 . 1.393(6) yes C6 . H61 . 1.000 no C7 . H71 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C9 . C10 . 1.400(5) yes C9 . C14 . 1.397(5) yes C10 . C11 . 1.385(6) yes C10 . H101 . 1.000 no C11 . C12 . 1.390(6) yes C11 . H111 . 1.000 no C12 . C13 . 1.387(6) yes C12 . H121 . 1.000 no C13 . C14 . 1.391(6) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.392(5) yes C15 . C20 . 1.388(5) yes C16 . C17 . 1.382(6) yes C16 . H161 . 1.000 no C17 . C18 . 1.383(7) yes C17 . H171 . 1.000 no C18 . C19 . 1.377(7) yes C18 . H181 . 1.000 no C19 . C20 . 1.389(6) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.504(5) yes C21 . H211 . 1.000 no C21 . H212 . 1.000 no C22 . C23 . 1.402(5) yes C22 . C27 . 1.388(5) yes C23 . C24 . 1.392(5) yes C24 . C25 . 1.394(6) yes C24 . H241 . 1.000 no C25 . C26 . 1.387(6) yes C25 . H251 . 1.000 no C26 . C27 . 1.388(6) yes C26 . H261 . 1.000 no C27 . H271 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C29 . C30 . 1.399(5) yes C29 . C34 . 1.391(6) yes C30 . C31 . 1.387(6) yes C30 . H301 . 1.000 no C31 . C32 . 1.380(6) yes C31 . H311 . 1.000 no C32 . C33 . 1.384(6) yes C32 . H321 . 1.000 no C33 . C34 . 1.390(6) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no C35 . C36 . 1.405(5) yes C35 . C40 . 1.390(5) yes C36 . C37 . 1.383(5) yes C36 . H361 . 1.000 no C37 . C38 . 1.389(6) yes C37 . H371 . 1.000 no C38 . C39 . 1.381(6) yes C38 . H381 . 1.000 no C39 . C40 . 1.391(5) yes C39 . H391 . 1.000 no C40 . H401 . 1.000 no C41 . Cl5 . 1.759(4) yes C41 . Cl6 . 1.762(5) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no C42 . Cl7 . 1.744(6) yes C42 . Cl8 . 1.759(6) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Pd1 . S1 . 88.51(4) yes P1 . Pd1 . Cl1 . 175.32(4) yes S1 . Pd1 . Cl1 . 93.46(4) yes P1 . Pd1 . Cl2 . 87.48(3) yes S1 . Pd1 . Cl2 . 172.54(4) yes Cl1 . Pd1 . Cl2 . 91.01(4) yes P2 . Pd2 . S2 . 88.34(4) yes P2 . Pd2 . Cl3 . 176.18(4) yes S2 . Pd2 . Cl3 . 93.57(4) yes P2 . Pd2 . Cl4 . 87.40(3) yes S2 . Pd2 . Cl4 . 173.09(4) yes Cl3 . Pd2 . Cl4 . 91.00(4) yes Pd1 . P1 . C1 . 111.71(13) yes Pd1 . P1 . C9 . 117.12(12) yes C1 . P1 . C9 . 104.06(17) yes Pd1 . P1 . C15 . 114.17(12) yes C1 . P1 . C15 . 103.73(17) yes C9 . P1 . C15 . 104.70(17) yes Pd2 . P2 . C21 . 111.96(13) yes Pd2 . P2 . C29 . 113.18(13) yes C21 . P2 . C29 . 103.97(18) yes Pd2 . P2 . C35 . 117.00(12) yes C21 . P2 . C35 . 104.30(17) yes C29 . P2 . C35 . 105.22(17) yes Pd1 . S1 . C3 . 105.38(12) yes Pd1 . S1 . C8 . 112.54(15) yes C3 . S1 . C8 . 103.22(19) yes Pd2 . S2 . C23 . 106.08(12) yes Pd2 . S2 . C28 . 112.45(16) yes C23 . S2 . C28 . 103.3(2) yes P1 . C1 . C2 . 112.7(2) yes P1 . C1 . H11 . 108.671 no C2 . C1 . H11 . 108.672 no P1 . C1 . H12 . 108.669 no C2 . C1 . H12 . 108.670 no H11 . C1 . H12 . 109.466 no C1 . C2 . C3 . 120.1(3) yes C1 . C2 . C7 . 121.6(3) yes C3 . C2 . C7 . 118.1(3) yes S1 . C3 . C2 . 115.6(3) yes S1 . C3 . C4 . 123.7(3) yes C2 . C3 . C4 . 120.7(4) yes C3 . C4 . C5 . 119.6(4) yes C3 . C4 . H41 . 120.211 no C5 . C4 . H41 . 120.211 no C4 . C5 . C6 . 120.9(4) yes C4 . C5 . H51 . 119.561 no C6 . C5 . H51 . 119.565 no C5 . C6 . C7 . 119.2(4) yes C5 . C6 . H61 . 120.398 no C7 . C6 . H61 . 120.398 no C2 . C7 . C6 . 121.5(4) yes C2 . C7 . H71 . 119.273 no C6 . C7 . H71 . 119.274 no S1 . C8 . H81 . 109.462 no S1 . C8 . H82 . 109.461 no H81 . C8 . H82 . 109.483 no S1 . C8 . H83 . 109.459 no H81 . C8 . H83 . 109.481 no H82 . C8 . H83 . 109.480 no P1 . C9 . C10 . 119.0(3) yes P1 . C9 . C14 . 121.7(3) yes C10 . C9 . C14 . 119.2(3) yes C9 . C10 . C11 . 120.3(4) yes C9 . C10 . H101 . 119.832 no C11 . C10 . H101 . 119.827 no C10 . C11 . C12 . 120.5(4) yes C10 . C11 . H111 . 119.744 no C12 . C11 . H111 . 119.743 no C11 . C12 . C13 . 119.2(4) yes C11 . C12 . H121 . 120.399 no C13 . C12 . H121 . 120.403 no C12 . C13 . C14 . 121.0(4) yes C12 . C13 . H131 . 119.494 no C14 . C13 . H131 . 119.493 no C9 . C14 . C13 . 119.7(4) yes C9 . C14 . H141 . 120.153 no C13 . C14 . H141 . 120.153 no P1 . C15 . C16 . 118.5(3) yes P1 . C15 . C20 . 122.0(3) yes C16 . C15 . C20 . 119.3(3) yes C15 . C16 . C17 . 120.6(4) yes C15 . C16 . H161 . 119.722 no C17 . C16 . H161 . 119.724 no C16 . C17 . C18 . 120.0(4) yes C16 . C17 . H171 . 120.018 no C18 . C17 . H171 . 120.019 no C17 . C18 . C19 . 119.7(4) yes C17 . C18 . H181 . 120.159 no C19 . C18 . H181 . 120.159 no C18 . C19 . C20 . 120.9(4) yes C18 . C19 . H191 . 119.567 no C20 . C19 . H191 . 119.570 no C19 . C20 . C15 . 119.6(4) yes C19 . C20 . H201 . 120.200 no C15 . C20 . H201 . 120.204 no P2 . C21 . C22 . 112.1(3) yes P2 . C21 . H211 . 108.822 no C22 . C21 . H211 . 108.820 no P2 . C21 . H212 . 108.820 no C22 . C21 . H212 . 108.819 no H211 . C21 . H212 . 109.467 no C21 . C22 . C23 . 119.9(3) yes C21 . C22 . C27 . 121.3(4) yes C23 . C22 . C27 . 118.9(3) yes S2 . C23 . C22 . 115.8(3) yes S2 . C23 . C24 . 123.4(3) yes C22 . C23 . C24 . 120.7(4) yes C23 . C24 . C25 . 119.4(4) yes C23 . C24 . H241 . 120.309 no C25 . C24 . H241 . 120.307 no C24 . C25 . C26 . 120.2(4) yes C24 . C25 . H251 . 119.875 no C26 . C25 . H251 . 119.881 no C25 . C26 . C27 . 120.0(4) yes C25 . C26 . H261 . 119.999 no C27 . C26 . H261 . 119.997 no C22 . C27 . C26 . 120.7(4) yes C22 . C27 . H271 . 119.627 no C26 . C27 . H271 . 119.626 no S2 . C28 . H281 . 109.461 no S2 . C28 . H282 . 109.458 no H281 . C28 . H282 . 109.486 no S2 . C28 . H283 . 109.457 no H281 . C28 . H283 . 109.485 no H282 . C28 . H283 . 109.481 no P2 . C29 . C30 . 119.7(3) yes P2 . C29 . C34 . 121.1(3) yes C30 . C29 . C34 . 119.2(4) yes C29 . C30 . C31 . 120.1(4) yes C29 . C30 . H301 . 119.957 no C31 . C30 . H301 . 119.959 no C30 . C31 . C32 . 120.3(4) yes C30 . C31 . H311 . 119.874 no C32 . C31 . H311 . 119.867 no C31 . C32 . C33 . 120.1(4) yes C31 . C32 . H321 . 119.936 no C33 . C32 . H321 . 119.929 no C32 . C33 . C34 . 120.0(4) yes C32 . C33 . H331 . 119.981 no C34 . C33 . H331 . 119.982 no C29 . C34 . C33 . 120.3(4) yes C29 . C34 . H341 . 119.849 no C33 . C34 . H341 . 119.845 no P2 . C35 . C36 . 119.2(3) yes P2 . C35 . C40 . 121.7(3) yes C36 . C35 . C40 . 119.1(3) yes C35 . C36 . C37 . 120.1(4) yes C35 . C36 . H361 . 119.952 no C37 . C36 . H361 . 119.957 no C36 . C37 . C38 . 120.0(4) yes C36 . C37 . H371 . 119.983 no C38 . C37 . H371 . 119.985 no C37 . C38 . C39 . 120.4(4) yes C37 . C38 . H381 . 119.783 no C39 . C38 . H381 . 119.784 no C38 . C39 . C40 . 119.8(4) yes C38 . C39 . H391 . 120.111 no C40 . C39 . H391 . 120.115 no C39 . C40 . C35 . 120.5(4) yes C39 . C40 . H401 . 119.735 no C35 . C40 . H401 . 119.737 no Cl5 . C41 . Cl6 . 111.9(2) yes Cl5 . C41 . H411 . 108.854 no Cl6 . C41 . H411 . 108.852 no Cl5 . C41 . H412 . 108.854 no Cl6 . C41 . H412 . 108.852 no H411 . C41 . H412 . 109.467 no Cl7 . C42 . Cl8 . 112.5(3) yes Cl7 . C42 . H421 . 108.713 no Cl8 . C42 . H421 . 108.709 no Cl7 . C42 . H422 . 108.714 no Cl8 . C42 . H422 . 108.710 no H421 . C42 . H422 . 109.468 no #===END ######################################## ## denoted [PdCl2(tBuS~PPh2)] in text ## ######################################## data_4 _database_code_depnum_ccdc_archive 'CCDC 257330' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 12.5554(4) _cell_angle_alpha 90 _cell_length_b 15.0824(5) _cell_angle_beta 109.7231(14) _cell_length_c 12.7084(4) _cell_angle_gamma 90 _cell_volume 2265.35(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C23 H25 Cl2 P1 Pd1 S1 ' _chemical_formula_moiety ' C23 H25 Cl2 P1 Pd1 S1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 541.80 _cell_measurement_reflns_used 4756 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.225 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.96 # Sheldrick geometric definitions 0.83 0.96 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 9161 _reflns_number_total 5117 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 5117 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5202 _diffrn_reflns_theta_min 5.107 _diffrn_reflns_theta_max 27.496 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.70 _refine_diff_density_max 0.59 _refine_ls_number_reflns 3429 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 #_refine_ls_R_factor_ref 0.0317 _refine_ls_wR_factor_ref 0.0337 _refine_ls_goodness_of_fit_ref 1.1108 #_reflns_number_all 5117 _refine_ls_R_factor_all 0.0609 _refine_ls_wR_factor_all 0.0561 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3429 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_gt 0.0337 _refine_ls_shift/su_max 0.001123 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.361 0.682E-01 0.941E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pd1 Pd 0.80754(2) 0.319915(18) 0.12368(2) 0.0175 1.0000 Uani . . . . . . Cl1 Cl 0.86620(8) 0.18543(6) 0.06395(7) 0.0268 1.0000 Uani . . . . . . Cl2 Cl 0.83882(8) 0.26352(6) 0.30108(7) 0.0248 1.0000 Uani . . . . . . S1 S 0.79688(7) 0.37982(6) -0.04583(7) 0.0192 1.0000 Uani . . . . . . P1 P 0.75841(7) 0.44311(6) 0.19203(7) 0.0187 1.0000 Uani . . . . . . C1 C 0.6933(3) 0.5266(2) 0.0851(3) 0.0221 1.0000 Uani . . . . . . C2 C 0.7694(3) 0.5555(2) 0.0224(3) 0.0211 1.0000 Uani . . . . . . C3 C 0.8019(3) 0.6442(3) 0.0282(3) 0.0277 1.0000 Uani . . . . . . C4 C 0.8716(3) 0.6758(3) -0.0276(3) 0.0300 1.0000 Uani . . . . . . C5 C 0.9109(3) 0.6185(3) -0.0912(3) 0.0274 1.0000 Uani . . . . . . C6 C 0.8826(3) 0.5290(3) -0.0964(3) 0.0234 1.0000 Uani . . . . . . C7 C 0.8129(3) 0.4972(2) -0.0400(3) 0.0197 1.0000 Uani . . . . . . C8 C 0.6611(3) 0.3584(3) -0.1637(3) 0.0234 1.0000 Uani . . . . . . C9 C 0.5604(3) 0.4054(3) -0.1485(3) 0.0283 1.0000 Uani . . . . . . C10 C 0.6451(3) 0.2582(3) -0.1664(3) 0.0326 1.0000 Uani . . . . . . C11 C 0.6808(4) 0.3911(3) -0.2692(3) 0.0349 1.0000 Uani . . . . . . C12 C 0.6502(3) 0.4214(2) 0.2536(3) 0.0228 1.0000 Uani . . . . . . C13 C 0.6542(3) 0.4554(3) 0.3567(3) 0.0302 1.0000 Uani . . . . . . C14 C 0.5686(4) 0.4341(4) 0.3993(4) 0.0423 1.0000 Uani . . . . . . C15 C 0.4801(4) 0.3800(3) 0.3411(4) 0.0433 1.0000 Uani . . . . . . C16 C 0.4758(4) 0.3461(3) 0.2379(4) 0.0417 1.0000 Uani . . . . . . C17 C 0.5595(4) 0.3672(3) 0.1937(3) 0.0321 1.0000 Uani . . . . . . C18 C 0.8773(3) 0.5009(2) 0.2894(3) 0.0218 1.0000 Uani . . . . . . C19 C 0.8640(4) 0.5849(3) 0.3285(3) 0.0305 1.0000 Uani . . . . . . C20 C 0.9576(4) 0.6300(3) 0.3992(4) 0.0383 1.0000 Uani . . . . . . C21 C 1.0641(4) 0.5925(3) 0.4293(3) 0.0376 1.0000 Uani . . . . . . C22 C 1.0779(3) 0.5100(3) 0.3897(3) 0.0327 1.0000 Uani . . . . . . C23 C 0.9846(3) 0.4631(3) 0.3212(3) 0.0260 1.0000 Uani . . . . . . H11 H 0.6739 0.5796 0.1223 0.0267 1.0000 Uiso . U . . . . H12 H 0.6227 0.5010 0.0307 0.0267 1.0000 Uiso . U . . . . H31 H 0.7740 0.6862 0.0740 0.0334 1.0000 Uiso . U . . . . H41 H 0.8935 0.7398 -0.0219 0.0356 1.0000 Uiso . U . . . . H51 H 0.9595 0.6414 -0.1334 0.0327 1.0000 Uiso . U . . . . H61 H 0.9126 0.4873 -0.1409 0.0280 1.0000 Uiso . U . . . . H91 H 0.4907 0.3917 -0.2134 0.0324 1.0000 Uiso . U . . . . H92 H 0.5739 0.4709 -0.1444 0.0324 1.0000 Uiso . U . . . . H93 H 0.5501 0.3847 -0.0778 0.0324 1.0000 Uiso . . . . . . H101 H 0.5737 0.2422 -0.2279 0.0370 1.0000 Uiso . U . . . . H102 H 0.7107 0.2288 -0.1798 0.0370 1.0000 Uiso . U . . . . H103 H 0.6404 0.2378 -0.0932 0.0370 1.0000 Uiso . . . . . . H111 H 0.6109 0.3814 -0.3352 0.0410 1.0000 Uiso . U . . . . H112 H 0.6993 0.4558 -0.2616 0.0410 1.0000 Uiso . U . . . . H113 H 0.7452 0.3577 -0.2798 0.0410 1.0000 Uiso . . . . . . H131 H 0.7180 0.4948 0.3999 0.0371 1.0000 Uiso . U . . . . H141 H 0.5715 0.4585 0.4734 0.0537 1.0000 Uiso . U . . . . H151 H 0.4194 0.3652 0.3727 0.0565 1.0000 Uiso . U . . . . H161 H 0.4120 0.3064 0.1954 0.0533 1.0000 Uiso . U . . . . H171 H 0.5551 0.3437 0.1188 0.0412 1.0000 Uiso . U . . . . H191 H 0.7873 0.6128 0.3059 0.0344 1.0000 Uiso . U . . . . H201 H 0.9477 0.6899 0.4284 0.0438 1.0000 Uiso . U . . . . H211 H 1.1310 0.6253 0.4798 0.0422 1.0000 Uiso . U . . . . H221 H 1.1552 0.4835 0.4102 0.0389 1.0000 Uiso . U . . . . H231 H 0.9948 0.4022 0.2948 0.0311 1.0000 Uiso . U . . . . 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 0.01907(12) 0.01711(13) 0.01638(12) 0.00026(10) 0.00609(9) 0.00022(11) Cl1 0.0345(5) 0.0222(4) 0.0244(4) -0.0009(3) 0.0108(3) 0.0053(4) Cl2 0.0308(5) 0.0238(4) 0.0202(4) 0.0043(3) 0.0093(3) 0.0021(3) S1 0.0200(4) 0.0210(4) 0.0162(4) -0.0002(3) 0.0056(3) -0.0002(3) P1 0.0212(4) 0.0186(4) 0.0175(4) 0.0000(3) 0.0079(3) -0.0001(3) C1 0.0229(17) 0.0232(18) 0.0207(16) 0.0006(14) 0.0082(14) 0.0021(14) C2 0.0227(17) 0.0220(18) 0.0162(16) 0.0034(13) 0.0034(13) 0.0008(14) C3 0.036(2) 0.0256(19) 0.0220(18) 0.0007(15) 0.0103(16) 0.0003(16) C4 0.035(2) 0.0242(19) 0.0302(19) 0.0038(16) 0.0099(16) -0.0031(17) C5 0.0263(19) 0.031(2) 0.0246(18) 0.0086(16) 0.0078(15) -0.0016(16) C6 0.0211(17) 0.030(2) 0.0184(16) 0.0032(14) 0.0062(13) 0.0015(15) C7 0.0186(16) 0.0222(17) 0.0164(15) 0.0009(13) 0.0036(13) 0.0003(13) C8 0.0212(17) 0.0289(19) 0.0157(16) -0.0029(14) 0.0004(13) 0.0003(15) C9 0.0217(18) 0.031(2) 0.0283(19) -0.0033(16) 0.0033(15) -0.0015(15) C10 0.029(2) 0.031(2) 0.032(2) -0.0089(17) 0.0033(17) 0.0007(17) C11 0.036(2) 0.047(3) 0.0201(18) 0.0008(17) 0.0062(16) -0.0039(19) C12 0.0273(18) 0.0184(17) 0.0247(18) 0.0037(14) 0.0114(14) 0.0029(14) C13 0.0328(19) 0.038(2) 0.0218(18) 0.0023(16) 0.0119(15) 0.0076(18) C14 0.040(2) 0.065(3) 0.029(2) 0.011(2) 0.0211(19) 0.017(2) C15 0.038(2) 0.052(3) 0.051(3) 0.020(2) 0.030(2) 0.010(2) C16 0.039(2) 0.037(2) 0.058(3) 0.003(2) 0.027(2) -0.0032(19) C17 0.039(2) 0.029(2) 0.035(2) -0.0056(17) 0.0212(18) -0.0051(18) C18 0.0271(18) 0.0212(17) 0.0161(16) 0.0026(13) 0.0058(14) -0.0023(14) C19 0.039(2) 0.024(2) 0.0231(18) -0.0028(15) 0.0032(16) 0.0030(17) C20 0.058(3) 0.022(2) 0.030(2) -0.0030(16) 0.008(2) -0.0036(19) C21 0.043(2) 0.038(2) 0.0245(19) -0.0039(17) 0.0019(18) -0.015(2) C22 0.0253(19) 0.046(3) 0.0254(19) -0.0018(17) 0.0073(16) -0.0063(18) C23 0.0260(18) 0.029(2) 0.0231(18) -0.0018(15) 0.0081(15) -0.0013(16) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl1 . 2.3686(9) yes Pd1 . Cl2 . 2.3157(9) yes Pd1 . S1 . 2.2979(9) yes Pd1 . P1 . 2.2247(9) yes S1 . C7 . 1.780(4) yes S1 . C8 . 1.879(3) yes P1 . C1 . 1.830(4) yes P1 . C12 . 1.812(4) yes P1 . C18 . 1.809(4) yes C1 . C2 . 1.500(5) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C3 . 1.393(5) yes C2 . C7 . 1.412(5) yes C3 . C4 . 1.384(5) yes C3 . H31 . 1.000 no C4 . C5 . 1.383(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.392(5) yes C5 . H51 . 1.000 no C6 . C7 . 1.390(5) yes C6 . H61 . 1.000 no C8 . C9 . 1.519(5) yes C8 . C10 . 1.523(6) yes C8 . C11 . 1.525(5) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . C13 . 1.392(5) yes C12 . C17 . 1.399(5) yes C13 . C14 . 1.394(6) yes C13 . H131 . 1.000 no C14 . C15 . 1.375(7) yes C14 . H141 . 1.000 no C15 . C16 . 1.392(7) yes C15 . H151 . 1.000 no C16 . C17 . 1.385(6) yes C16 . H161 . 1.000 no C17 . H171 . 1.000 no C18 . C19 . 1.391(5) yes C18 . C23 . 1.392(5) yes C19 . C20 . 1.393(6) yes C19 . H191 . 1.000 no C20 . C21 . 1.381(7) yes C20 . H201 . 1.000 no C21 . C22 . 1.376(6) yes C21 . H211 . 1.000 no C22 . C23 . 1.393(5) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Pd1 . Cl2 . 91.64(3) yes Cl1 . Pd1 . S1 . 87.84(3) yes Cl2 . Pd1 . S1 . 173.81(3) yes Cl1 . Pd1 . P1 . 175.99(3) yes Cl2 . Pd1 . P1 . 84.54(3) yes S1 . Pd1 . P1 . 95.83(3) yes Pd1 . S1 . C7 . 112.45(12) yes Pd1 . S1 . C8 . 115.45(12) yes C7 . S1 . C8 . 105.30(16) yes Pd1 . P1 . C1 . 113.44(12) yes Pd1 . P1 . C12 . 111.38(12) yes C1 . P1 . C12 . 103.47(16) yes Pd1 . P1 . C18 . 113.32(13) yes C1 . P1 . C18 . 103.60(16) yes C12 . P1 . C18 . 110.99(17) yes P1 . C1 . C2 . 112.9(2) yes P1 . C1 . H11 . 108.598 no C2 . C1 . H11 . 108.597 no P1 . C1 . H12 . 108.598 no C2 . C1 . H12 . 108.597 no H11 . C1 . H12 . 109.466 no C1 . C2 . C3 . 118.6(3) yes C1 . C2 . C7 . 123.6(3) yes C3 . C2 . C7 . 117.7(3) yes C2 . C3 . C4 . 121.9(4) yes C2 . C3 . H31 . 119.055 no C4 . C3 . H31 . 119.055 no C3 . C4 . C5 . 119.7(4) yes C3 . C4 . H41 . 120.127 no C5 . C4 . H41 . 120.126 no C4 . C5 . C6 . 119.9(3) yes C4 . C5 . H51 . 120.061 no C6 . C5 . H51 . 120.061 no C5 . C6 . C7 . 120.3(3) yes C5 . C6 . H61 . 119.839 no C7 . C6 . H61 . 119.839 no S1 . C7 . C2 . 125.6(3) yes S1 . C7 . C6 . 113.8(3) yes C2 . C7 . C6 . 120.4(3) yes S1 . C8 . C9 . 112.9(2) yes S1 . C8 . C10 . 105.5(3) yes C9 . C8 . C10 . 110.9(3) yes S1 . C8 . C11 . 105.8(3) yes C9 . C8 . C11 . 110.4(3) yes C10 . C8 . C11 . 111.2(3) yes C8 . C9 . H91 . 109.467 no C8 . C9 . H92 . 109.467 no H91 . C9 . H92 . 109.476 no C8 . C9 . H93 . 109.467 no H91 . C9 . H93 . 109.475 no H92 . C9 . H93 . 109.476 no C8 . C10 . H101 . 109.467 no C8 . C10 . H102 . 109.467 no H101 . C10 . H102 . 109.475 no C8 . C10 . H103 . 109.467 no H101 . C10 . H103 . 109.476 no H102 . C10 . H103 . 109.476 no C8 . C11 . H111 . 109.466 no C8 . C11 . H112 . 109.467 no H111 . C11 . H112 . 109.475 no C8 . C11 . H113 . 109.467 no H111 . C11 . H113 . 109.476 no H112 . C11 . H113 . 109.476 no P1 . C12 . C13 . 123.1(3) yes P1 . C12 . C17 . 117.5(3) yes C13 . C12 . C17 . 119.4(4) yes C12 . C13 . C14 . 119.6(4) yes C12 . C13 . H131 . 120.217 no C14 . C13 . H131 . 120.219 no C13 . C14 . C15 . 121.0(4) yes C13 . C14 . H141 . 119.479 no C15 . C14 . H141 . 119.480 no C14 . C15 . C16 . 119.5(4) yes C14 . C15 . H151 . 120.244 no C16 . C15 . H151 . 120.244 no C15 . C16 . C17 . 120.3(4) yes C15 . C16 . H161 . 119.867 no C17 . C16 . H161 . 119.864 no C12 . C17 . C16 . 120.2(4) yes C12 . C17 . H171 . 119.908 no C16 . C17 . H171 . 119.910 no P1 . C18 . C19 . 120.8(3) yes P1 . C18 . C23 . 119.7(3) yes C19 . C18 . C23 . 119.4(3) yes C18 . C19 . C20 . 119.9(4) yes C18 . C19 . H191 . 120.057 no C20 . C19 . H191 . 120.058 no C19 . C20 . C21 . 120.4(4) yes C19 . C20 . H201 . 119.808 no C21 . C20 . H201 . 119.806 no C20 . C21 . C22 . 119.9(4) yes C20 . C21 . H211 . 120.035 no C22 . C21 . H211 . 120.035 no C21 . C22 . C23 . 120.3(4) yes C21 . C22 . H221 . 119.829 no C23 . C22 . H221 . 119.828 no C22 . C23 . C18 . 120.0(4) yes C22 . C23 . H231 . 119.989 no C18 . C23 . H231 . 119.987 no #===END ####################################### ## denoted [PdCl2(PhS~PPh2)] in text ## ####################################### data_5 _database_code_depnum_ccdc_archive 'CCDC 257331' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 9.8876(3) _cell_angle_alpha 90 _cell_length_b 13.0573(4) _cell_angle_beta 96.6649(12) _cell_length_c 17.6637(6) _cell_angle_gamma 90 _cell_volume 2265.07(12) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Pd ' -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C25 H21 Cl2 P1 Pd1 S1 ' _chemical_formula_moiety ' C25 H21 Cl2 P1 Pd1 S1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 561.79 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.05 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.229 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.98 # Sheldrick geometric definitions 0.94 0.98 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 8928 _reflns_number_total 5335 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 5118 # Number of reflections without Friedels Law is 5335 # Theoretical number of reflections is about 5210 _diffrn_reflns_theta_min 5.110 _diffrn_reflns_theta_max 27.513 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _refine_diff_density_min -1.18 _refine_diff_density_max 0.98 _refine_ls_number_reflns 3808 _refine_ls_number_restraints 0 _refine_ls_number_parameters 271 #_refine_ls_R_factor_ref 0.0500 _refine_ls_wR_factor_ref 0.0534 _refine_ls_goodness_of_fit_ref 1.0609 #_reflns_number_all 5118 _refine_ls_R_factor_all 0.0733 _refine_ls_wR_factor_all 0.0637 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3808 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_gt 0.0534 _refine_ls_shift/su_max 0.000458 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.93 0.610 1.60 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pd1 Pd 0.45887(3) 0.36909(2) 0.291024(17) 0.0249 1.0000 Uani . . . . . . Cl2 Cl 0.44184(10) 0.41679(7) 0.16285(5) 0.0264 1.0000 Uani . . . . . . P1 P 0.30078(11) 0.24862(7) 0.25912(6) 0.0240 1.0000 Uani . . . . . . C1 C 0.2928(4) 0.1578(3) 0.3381(2) 0.0268 1.0000 Uani . . . . . . C2 C 0.2541(5) 0.2061(3) 0.4094(2) 0.0311 1.0000 Uani . . . . . . C7 C 0.3358(5) 0.2802(3) 0.4503(2) 0.0332 1.0000 Uani . . . . . . S1 S 0.48741(12) 0.32742(8) 0.41837(6) 0.0319 1.0000 Uani . . . . . . C8 C 0.5978(5) 0.2176(3) 0.4274(2) 0.0332 1.0000 Uani . . . . . . C9 C 0.6917(5) 0.2047(4) 0.3753(3) 0.0396 1.0000 Uani . . . . . . C10 C 0.7804(5) 0.1210(4) 0.3843(3) 0.0443 1.0000 Uani . . . . . . C11 C 0.7769(5) 0.0541(4) 0.4452(3) 0.0434 1.0000 Uani . . . . . . C12 C 0.6843(6) 0.0699(4) 0.4969(3) 0.0459 1.0000 Uani . . . . . . C13 C 0.5931(6) 0.1512(4) 0.4892(3) 0.0395 1.0000 Uani . . . . . . C6 C 0.3013(6) 0.3200(4) 0.5179(3) 0.0396 1.0000 Uani . . . . . . C5 C 0.1821(6) 0.2885(4) 0.5456(3) 0.0473 1.0000 Uani . . . . . . C4 C 0.0981(6) 0.2182(4) 0.5051(3) 0.0416 1.0000 Uani . . . . . . C3 C 0.1338(5) 0.1767(4) 0.4381(3) 0.0358 1.0000 Uani . . . . . . C14 C 0.1277(4) 0.2924(3) 0.2334(2) 0.0269 1.0000 Uani . . . . . . C19 C 0.1017(5) 0.3910(3) 0.2043(3) 0.0381 1.0000 Uani . . . . . . C18 C -0.0321(5) 0.4210(4) 0.1820(4) 0.0499 1.0000 Uani . . . . . . C17 C -0.1379(5) 0.3558(4) 0.1885(3) 0.0412 1.0000 Uani . . . . . . C16 C -0.1134(5) 0.2577(4) 0.2153(3) 0.0450 1.0000 Uani . . . . . . C15 C 0.0197(5) 0.2257(4) 0.2381(3) 0.0423 1.0000 Uani . . . . . . C20 C 0.3394(4) 0.1636(3) 0.1840(2) 0.0285 1.0000 Uani . . . . . . C21 C 0.4633(5) 0.1135(4) 0.1918(3) 0.0361 1.0000 Uani . . . . . . C22 C 0.4921(5) 0.0368(4) 0.1408(3) 0.0410 1.0000 Uani . . . . . . C23 C 0.3964(6) 0.0130(4) 0.0799(3) 0.0421 1.0000 Uani . . . . . . C24 C 0.2728(7) 0.0633(5) 0.0710(3) 0.0596 1.0000 Uani . . . . . . C25 C 0.2429(6) 0.1384(4) 0.1224(3) 0.0513 1.0000 Uani . . . . . . Cl1 Cl 0.63551(12) 0.48799(9) 0.32471(7) 0.0409 1.0000 Uani . . . . . . H11 H 0.3845 0.1254 0.3501 0.0318 1.0000 Uiso . . . . . . H12 H 0.2241 0.1039 0.3213 0.0318 1.0000 Uiso . . . . . . H91 H 0.6958 0.2541 0.3324 0.0467 1.0000 Uiso . . . . . . H101 H 0.8468 0.1091 0.3466 0.0517 1.0000 Uiso . . . . . . H111 H 0.8412 -0.0052 0.4516 0.0507 1.0000 Uiso . . . . . . H121 H 0.6829 0.0218 0.5408 0.0533 1.0000 Uiso . . . . . . H131 H 0.5261 0.1618 0.5267 0.0464 1.0000 Uiso . . . . . . H61 H 0.3618 0.3715 0.5468 0.0470 1.0000 Uiso . . . . . . H51 H 0.1572 0.3166 0.5948 0.0572 1.0000 Uiso . . . . . . H41 H 0.0109 0.1972 0.5243 0.0506 1.0000 Uiso . . . . . . H31 H 0.0727 0.1250 0.4098 0.0429 1.0000 Uiso . . . . . . H191 H 0.1786 0.4394 0.1996 0.0462 1.0000 Uiso . . . . . . H181 H -0.0509 0.4913 0.1609 0.0586 1.0000 Uiso . . . . . . H171 H -0.2336 0.3794 0.1738 0.0488 1.0000 Uiso . . . . . . H161 H -0.1910 0.2094 0.2183 0.0535 1.0000 Uiso . . . . . . H151 H 0.0373 0.1546 0.2580 0.0495 1.0000 Uiso . . . . . . H211 H 0.5338 0.1325 0.2347 0.0433 1.0000 Uiso . . . . . . H221 H 0.5810 -0.0004 0.1483 0.0495 1.0000 Uiso . . . . . . H231 H 0.4167 -0.0406 0.0424 0.0510 1.0000 Uiso . . . . . . H241 H 0.2039 0.0455 0.0271 0.0691 1.0000 Uiso . . . . . . H251 H 0.1529 0.1743 0.1153 0.0591 1.0000 Uiso . . . . . . 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 0.02660(17) 0.02187(16) 0.02472(16) -0.00063(11) -0.00330(10) 0.00013(12) Cl2 0.0277(5) 0.0273(5) 0.0239(4) 0.0060(3) 0.0016(3) -0.0009(4) P1 0.0289(5) 0.0217(4) 0.0204(5) -0.0003(4) -0.0014(4) -0.0023(4) C1 0.039(2) 0.0216(17) 0.0190(17) 0.0026(14) -0.0008(15) -0.0016(16) C2 0.043(2) 0.0269(19) 0.0221(18) 0.0047(15) -0.0013(16) 0.0068(17) C7 0.047(3) 0.028(2) 0.0238(19) 0.0013(16) -0.0006(17) 0.0066(19) S1 0.0413(6) 0.0268(5) 0.0249(5) -0.0028(4) -0.0080(4) 0.0011(4) C8 0.037(2) 0.031(2) 0.028(2) -0.0027(17) -0.0120(17) 0.0008(18) C9 0.038(2) 0.040(2) 0.039(2) 0.002(2) -0.0041(19) -0.001(2) C10 0.034(2) 0.046(3) 0.049(3) 0.005(2) -0.010(2) 0.007(2) C11 0.038(3) 0.040(3) 0.049(3) 0.003(2) -0.010(2) 0.006(2) C12 0.053(3) 0.037(2) 0.043(3) 0.011(2) -0.013(2) 0.007(2) C13 0.052(3) 0.032(2) 0.033(2) 0.0019(18) -0.007(2) 0.005(2) C6 0.062(3) 0.030(2) 0.025(2) -0.0028(17) -0.001(2) 0.012(2) C5 0.062(3) 0.052(3) 0.028(2) 0.005(2) 0.010(2) 0.023(3) C4 0.051(3) 0.047(3) 0.029(2) 0.011(2) 0.0121(19) 0.010(2) C3 0.035(2) 0.040(2) 0.032(2) 0.0113(19) 0.0034(18) 0.0050(19) C14 0.0282(19) 0.0307(19) 0.0209(17) -0.0013(15) -0.0015(14) -0.0012(16) C19 0.024(2) 0.0242(19) 0.067(3) 0.000(2) 0.010(2) 0.0004(16) C18 0.033(2) 0.027(2) 0.086(4) -0.006(2) -0.007(3) 0.0047(19) C17 0.028(2) 0.054(3) 0.039(2) -0.011(2) -0.0037(18) 0.005(2) C16 0.033(2) 0.058(3) 0.042(3) 0.016(2) -0.001(2) -0.012(2) C15 0.030(2) 0.047(3) 0.047(3) 0.013(2) -0.0088(19) -0.006(2) C20 0.037(2) 0.0256(18) 0.0227(18) -0.0032(15) 0.0018(16) -0.0036(17) C21 0.028(2) 0.047(3) 0.033(2) -0.0081(19) 0.0039(17) -0.0043(19) C22 0.031(2) 0.049(3) 0.044(3) -0.013(2) 0.0078(19) 0.003(2) C23 0.056(3) 0.039(2) 0.032(2) -0.0109(19) 0.011(2) -0.004(2) C24 0.065(4) 0.062(3) 0.046(3) -0.030(3) -0.019(3) 0.020(3) C25 0.057(3) 0.049(3) 0.041(3) -0.020(2) -0.021(2) 0.013(3) Cl1 0.0324(6) 0.0382(6) 0.0502(7) -0.0085(5) -0.0039(5) -0.0074(4) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl2 . 2.3353(9) yes Pd1 . P1 . 2.2429(10) yes Pd1 . S1 . 2.2997(11) yes Pd1 . Cl1 . 2.3608(11) yes P1 . C1 . 1.840(4) yes P1 . C14 . 1.812(4) yes P1 . C20 . 1.805(4) yes C1 . C2 . 1.497(6) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C7 . 1.406(6) yes C2 . C3 . 1.400(7) yes C7 . S1 . 1.773(5) yes C7 . C6 . 1.381(6) yes S1 . C8 . 1.798(5) yes C8 . C9 . 1.392(7) yes C8 . C13 . 1.399(7) yes C9 . C10 . 1.399(7) yes C9 . H91 . 1.000 no C10 . C11 . 1.388(8) yes C10 . H101 . 1.000 no C11 . C12 . 1.382(8) yes C11 . H111 . 1.000 no C12 . C13 . 1.388(7) yes C12 . H121 . 1.000 no C13 . H131 . 1.000 no C6 . C5 . 1.390(8) yes C6 . H61 . 1.000 no C5 . C4 . 1.380(8) yes C5 . H51 . 1.000 no C4 . C3 . 1.385(7) yes C4 . H41 . 1.000 no C3 . H31 . 1.000 no C14 . C19 . 1.398(6) yes C14 . C15 . 1.388(6) yes C19 . C18 . 1.393(7) yes C19 . H191 . 1.000 no C18 . C17 . 1.363(8) yes C18 . H181 . 1.000 no C17 . C16 . 1.378(8) yes C17 . H171 . 1.000 no C16 . C15 . 1.395(7) yes C16 . H161 . 1.000 no C15 . H151 . 1.000 no C20 . C21 . 1.381(7) yes C20 . C25 . 1.401(6) yes C21 . C22 . 1.398(7) yes C21 . H211 . 1.000 no C22 . C23 . 1.383(7) yes C22 . H221 . 1.000 no C23 . C24 . 1.380(8) yes C23 . H231 . 1.000 no C24 . C25 . 1.390(7) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 . Pd1 . P1 . 88.49(4) yes Cl2 . Pd1 . S1 . 176.64(4) yes P1 . Pd1 . S1 . 94.74(4) yes Cl2 . Pd1 . Cl1 . 92.12(4) yes P1 . Pd1 . Cl1 . 176.50(4) yes S1 . Pd1 . Cl1 . 84.60(4) yes Pd1 . P1 . C1 . 110.57(13) yes Pd1 . P1 . C14 . 116.89(14) yes C1 . P1 . C14 . 105.75(19) yes Pd1 . P1 . C20 . 114.56(15) yes C1 . P1 . C20 . 101.08(19) yes C14 . P1 . C20 . 106.50(19) yes P1 . C1 . C2 . 113.8(3) yes P1 . C1 . H11 . 108.375 no C2 . C1 . H11 . 108.375 no P1 . C1 . H12 . 108.375 no C2 . C1 . H12 . 108.375 no H11 . C1 . H12 . 109.467 no C1 . C2 . C7 . 122.3(4) yes C1 . C2 . C3 . 120.0(4) yes C7 . C2 . C3 . 117.7(4) yes C2 . C7 . S1 . 122.2(3) yes C2 . C7 . C6 . 121.3(5) yes S1 . C7 . C6 . 116.6(4) yes C7 . S1 . Pd1 . 112.40(14) yes C7 . S1 . C8 . 102.8(2) yes Pd1 . S1 . C8 . 106.27(15) yes S1 . C8 . C9 . 118.8(4) yes S1 . C8 . C13 . 119.3(4) yes C9 . C8 . C13 . 121.7(4) yes C8 . C9 . C10 . 118.5(5) yes C8 . C9 . H91 . 120.762 no C10 . C9 . H91 . 120.762 no C9 . C10 . C11 . 120.5(5) yes C9 . C10 . H101 . 119.732 no C11 . C10 . H101 . 119.732 no C10 . C11 . C12 . 119.7(5) yes C10 . C11 . H111 . 120.150 no C12 . C11 . H111 . 120.150 no C11 . C12 . C13 . 121.5(5) yes C11 . C12 . H121 . 119.251 no C13 . C12 . H121 . 119.251 no C8 . C13 . C12 . 118.0(5) yes C8 . C13 . H131 . 120.987 no C12 . C13 . H131 . 120.987 no C7 . C6 . C5 . 119.8(5) yes C7 . C6 . H61 . 120.085 no C5 . C6 . H61 . 120.085 no C6 . C5 . C4 . 119.9(5) yes C6 . C5 . H51 . 120.053 no C4 . C5 . H51 . 120.054 no C5 . C4 . C3 . 120.4(5) yes C5 . C4 . H41 . 119.816 no C3 . C4 . H41 . 119.816 no C2 . C3 . C4 . 120.9(5) yes C2 . C3 . H31 . 119.532 no C4 . C3 . H31 . 119.532 no P1 . C14 . C19 . 120.7(3) yes P1 . C14 . C15 . 119.8(3) yes C19 . C14 . C15 . 119.4(4) yes C14 . C19 . C18 . 119.4(4) yes C14 . C19 . H191 . 120.310 no C18 . C19 . H191 . 120.310 no C19 . C18 . C17 . 120.9(5) yes C19 . C18 . H181 . 119.537 no C17 . C18 . H181 . 119.537 no C18 . C17 . C16 . 120.2(4) yes C18 . C17 . H171 . 119.907 no C16 . C17 . H171 . 119.907 no C17 . C16 . C15 . 120.1(5) yes C17 . C16 . H161 . 119.966 no C15 . C16 . H161 . 119.966 no C16 . C15 . C14 . 120.0(4) yes C16 . C15 . H151 . 119.996 no C14 . C15 . H151 . 119.996 no P1 . C20 . C21 . 118.6(3) yes P1 . C20 . C25 . 122.2(4) yes C21 . C20 . C25 . 118.8(4) yes C20 . C21 . C22 . 121.3(4) yes C20 . C21 . H211 . 119.337 no C22 . C21 . H211 . 119.336 no C21 . C22 . C23 . 119.3(5) yes C21 . C22 . H221 . 120.342 no C23 . C22 . H221 . 120.342 no C22 . C23 . C24 . 119.9(5) yes C22 . C23 . H231 . 120.056 no C24 . C23 . H231 . 120.056 no C23 . C24 . C25 . 121.0(5) yes C23 . C24 . H241 . 119.520 no C25 . C24 . H241 . 119.520 no C20 . C25 . C24 . 119.6(5) yes C20 . C25 . H251 . 120.184 no C24 . C25 . H251 . 120.185 no #===END