# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Werner Oberhauser' _publ_contact_author_email WERNER.OBERHAUSER@ICCOM.CNR.IT _publ_section_title ; Chemoselective methoxycarbonylation of terminal alkynes catalyzed by Pd(II)-TROPP complexes ; loop_ _publ_author_name 'Werner Oberhauser' 'Lorenzo Bettucci' 'Claudio Bianchini' 'Hansjorg Grutzmacher' 'Matthias Vogt' # Attachment '10a.cif' data_trop180k _database_code_depnum_ccdc_archive 'CCDC 696684' #TrackingRef '10a.cif' _audit_creation_date 2010-04-19T18:43:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic '[Pd(CH2CH2COCH3)(trop)](PF6)' _chemical_formula_sum 'C34 H31 F6 O P2 Pd' _chemical_formula_moiety 'C31 H28 O P Pd,(P F6), 0.5 (C6 H6)' _chemical_formula_weight 737.93 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9962(5) _cell_length_b 8.9054(2) _cell_length_c 21.4435(5) _cell_angle_alpha 90 _cell_angle_beta 110.763(3) _cell_angle_gamma 90 _cell_volume 3213.42(14) _cell_formula_units_Z 4 _cell_measurement_temperature 180.2(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.849 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180.2(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur 3, Oxford diffraction' _diffrn_reflns_av_unetI/netI 0.0629 _diffrn_reflns_number 10409 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 32.48 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.895 _reflns_number_total 10409 _reflns_number_gt 6560 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR-97 (J. Appl. Cryst. 1999, 32, 115)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.1666P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10409 _refine_ls_number_parameters 383 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.089 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.576 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.111 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.247155(14) 0.43560(3) 0.802247(11) 0.02894(9) Uani 1 1 d . . . P1 P 0.19970(5) 0.55814(9) 0.70732(4) 0.02668(16) Uani 1 1 d . . . P2 P 0.19299(7) 0.81877(12) 0.47970(5) 0.0494(3) Uani 1 1 d . . . O1 O 0.27803(15) 0.2985(3) 0.88898(11) 0.0382(5) Uani 1 1 d . . . F1 F 0.2654(3) 0.7395(4) 0.4694(3) 0.1306(16) Uani 1 1 d . . . F2 F 0.1360(2) 0.7373(5) 0.41617(13) 0.1045(12) Uani 1 1 d . . . F3 F 0.1200(2) 0.8924(4) 0.49430(19) 0.0910(10) Uani 1 1 d . . . F4 F 0.2519(2) 0.8905(4) 0.54791(17) 0.0935(10) Uani 1 1 d . . . F5 F 0.2054(4) 0.9596(5) 0.4428(3) 0.156(2) Uani 1 1 d . . . F6 F 0.1819(2) 0.6775(3) 0.52174(15) 0.0860(9) Uani 1 1 d . . . C1 C 0.2845(2) 0.6557(4) 0.69370(16) 0.0316(6) Uani 1 1 d . . . H1 H 0.2644 0.7016 0.6493 0.038 Uiso 1 1 calc R . . C2 C 0.3512(2) 0.5510(4) 0.69597(17) 0.0357(7) Uani 1 1 d . . . C3 C 0.3696(3) 0.5345(5) 0.6384(2) 0.0511(10) Uani 1 1 d . . . H3 H 0.3424 0.5907 0.6006 0.061 Uiso 1 1 calc R . . C4 C 0.4285(3) 0.4346(5) 0.6372(3) 0.0626(13) Uani 1 1 d . . . H4 H 0.4424 0.4284 0.5994 0.075 Uiso 1 1 calc R . . C5 C 0.4658(3) 0.3458(6) 0.6907(3) 0.0662(13) Uani 1 1 d . . . H5 H 0.5026 0.2747 0.6884 0.079 Uiso 1 1 calc R . . C6 C 0.4489(2) 0.3615(5) 0.7489(2) 0.0552(10) Uani 1 1 d . . . H6 H 0.4759 0.3022 0.7857 0.066 Uiso 1 1 calc R . . C7 C 0.3920(2) 0.4651(4) 0.75310(19) 0.0386(8) Uani 1 1 d . . . C8 C 0.3793(2) 0.4775(4) 0.81656(18) 0.0393(8) Uani 1 1 d . . . H8 H 0.3892 0.3912 0.8427 0.047 Uiso 1 1 calc R . . C9 C 0.3547(2) 0.5999(4) 0.84214(16) 0.0371(7) Uani 1 1 d . . . H9 H 0.3464 0.5857 0.8821 0.045 Uiso 1 1 calc R . . C10 C 0.3400(2) 0.7502(4) 0.81389(16) 0.0351(7) Uani 1 1 d . . . C11 C 0.3569(2) 0.8711(5) 0.8582(2) 0.0465(9) Uani 1 1 d . . . H11 H 0.3729 0.8522 0.9037 0.056 Uiso 1 1 calc R . . C12 C 0.3506(3) 1.0184(5) 0.8362(2) 0.0511(10) Uani 1 1 d . . . H12 H 0.364 1.0973 0.8665 0.061 Uiso 1 1 calc R . . C13 C 0.3242(3) 1.0461(4) 0.7690(3) 0.0554(11) Uani 1 1 d . . . H13 H 0.3194 1.1447 0.7538 0.067 Uiso 1 1 calc R . . C14 C 0.3046(2) 0.9292(4) 0.7235(2) 0.0431(8) Uani 1 1 d . . . H14 H 0.2865 0.9503 0.678 0.052 Uiso 1 1 calc R . . C15 C 0.31155(19) 0.7812(4) 0.74463(16) 0.0333(7) Uani 1 1 d . . . C16 C 0.13370(18) 0.7111(3) 0.70490(15) 0.0294(6) Uani 1 1 d . . . C17 C 0.1177(2) 0.7477(4) 0.76223(16) 0.0332(7) Uani 1 1 d . . . H17 H 0.137 0.687 0.7998 0.04 Uiso 1 1 calc R . . C18 C 0.0729(2) 0.8742(4) 0.76342(18) 0.0415(8) Uani 1 1 d . . . H18 H 0.0631 0.8991 0.8019 0.05 Uiso 1 1 calc R . . C19 C 0.0431(2) 0.9633(4) 0.7070(2) 0.0421(8) Uani 1 1 d . . . H19 H 0.0127 1.0473 0.7077 0.051 Uiso 1 1 calc R . . C20 C 0.0579(2) 0.9289(4) 0.6496(2) 0.0420(8) Uani 1 1 d . . . H20 H 0.0378 0.9896 0.6121 0.05 Uiso 1 1 calc R . . C21 C 0.1031(2) 0.8029(4) 0.64844(15) 0.0345(7) Uani 1 1 d . . . H21 H 0.113 0.7794 0.6099 0.041 Uiso 1 1 calc R . . C22 C 0.1519(2) 0.4378(3) 0.63664(15) 0.0317(7) Uani 1 1 d . . . C23 C 0.0719(2) 0.4463(4) 0.60102(18) 0.0410(8) Uani 1 1 d . . . H23 H 0.0418 0.5219 0.6105 0.049 Uiso 1 1 calc R . . C24 C 0.0348(3) 0.3415(5) 0.55025(18) 0.0517(10) Uani 1 1 d . . . H24 H -0.0194 0.3475 0.5263 0.062 Uiso 1 1 calc R . . C25 C 0.0800(3) 0.2296(5) 0.53639(18) 0.0535(11) Uani 1 1 d . . . H25 H 0.056 0.1604 0.5028 0.064 Uiso 1 1 calc R . . C26 C 0.1593(3) 0.2203(5) 0.57180(19) 0.0506(10) Uani 1 1 d . . . H26 H 0.1892 0.1453 0.5617 0.061 Uiso 1 1 calc R . . C27 C 0.1964(2) 0.3221(4) 0.62311(17) 0.0394(8) Uani 1 1 d . . . H27 H 0.2503 0.3128 0.648 0.047 Uiso 1 1 calc R . . C28 C 0.1422(2) 0.3220(4) 0.77880(17) 0.0399(8) Uani 1 1 d . . . H28A H 0.0976 0.3881 0.7572 0.048 Uiso 1 1 calc R . . H28B H 0.1404 0.2387 0.7492 0.048 Uiso 1 1 calc R . . C29 C 0.1398(2) 0.2653(5) 0.84540(19) 0.0461(9) Uani 1 1 d . . . H29A H 0.114 0.34 0.8637 0.055 Uiso 1 1 calc R . . H29B H 0.1083 0.1742 0.8378 0.055 Uiso 1 1 calc R . . C30 C 0.2193(2) 0.2344(4) 0.89393(17) 0.0400(8) Uani 1 1 d . . . C31 C 0.2310(3) 0.1264(5) 0.9501(2) 0.0675(14) Uani 1 1 d . . . H31A H 0.2822 0.1427 0.9838 0.101 Uiso 1 1 calc R . . H31B H 0.2279 0.0255 0.9336 0.101 Uiso 1 1 calc R . . H31C H 0.1903 0.1418 0.9688 0.101 Uiso 1 1 calc R . . C32 C 0.5333(7) 0.3643(14) 0.9697(6) 0.175(4) Uiso 1 1 d D . . H32 H 0.5559 0.2892 0.9521 0.21 Uiso 1 1 calc R . . C33 C 0.4702(6) 0.3545(11) 0.9942(5) 0.150(3) Uiso 1 1 d D . . H33 H 0.4444 0.2631 0.9922 0.18 Uiso 1 1 calc R . . C34 C 0.4464(6) 0.4757(10) 1.0205(4) 0.132(3) Uiso 1 1 d D . . H34 H 0.4064 0.4508 1.0367 0.158 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02858(14) 0.02933(14) 0.02847(12) 0.00276(9) 0.00956(9) -0.00080(10) P1 0.0245(4) 0.0291(4) 0.0262(3) 0.0005(3) 0.0086(3) 0.0013(3) P2 0.0691(7) 0.0420(5) 0.0423(5) -0.0024(4) 0.0263(5) -0.0025(5) O1 0.0448(14) 0.0367(13) 0.0368(11) 0.0069(10) 0.0189(11) 0.0041(11) F1 0.117(3) 0.110(3) 0.215(4) -0.080(3) 0.120(3) -0.034(2) F2 0.123(3) 0.142(3) 0.0430(14) -0.0288(17) 0.0229(17) -0.031(3) F3 0.075(2) 0.0654(18) 0.128(3) -0.0298(19) 0.030(2) 0.0112(17) F4 0.082(2) 0.108(2) 0.083(2) -0.0393(19) 0.0200(18) -0.009(2) F5 0.194(5) 0.109(3) 0.160(4) 0.077(3) 0.058(4) -0.038(3) F6 0.116(3) 0.0685(19) 0.0766(18) 0.0208(15) 0.0382(19) 0.0039(17) C1 0.0299(16) 0.0334(17) 0.0346(15) 0.0038(12) 0.0153(13) -0.0003(13) C2 0.0308(17) 0.0369(18) 0.0430(17) 0.0002(14) 0.0176(14) -0.0044(14) C3 0.045(2) 0.066(3) 0.052(2) -0.0021(19) 0.0290(19) 0.006(2) C4 0.053(3) 0.073(3) 0.082(3) 0.005(2) 0.049(3) 0.011(2) C5 0.042(2) 0.069(3) 0.099(4) 0.000(3) 0.039(3) 0.016(2) C6 0.034(2) 0.053(2) 0.082(3) 0.007(2) 0.024(2) 0.0119(18) C7 0.0226(16) 0.0413(19) 0.0499(19) 0.0082(15) 0.0105(15) -0.0004(14) C8 0.0318(17) 0.0404(19) 0.0416(17) 0.0100(15) 0.0081(15) -0.0035(15) C9 0.0300(17) 0.048(2) 0.0286(14) 0.0022(13) 0.0047(13) -0.0085(15) C10 0.0282(16) 0.0381(17) 0.0404(16) -0.0001(14) 0.0137(14) -0.0036(14) C11 0.038(2) 0.053(2) 0.053(2) -0.0140(18) 0.0210(17) -0.0083(18) C12 0.047(2) 0.037(2) 0.069(3) -0.0167(19) 0.019(2) -0.0033(18) C13 0.049(2) 0.032(2) 0.082(3) -0.0029(19) 0.018(2) -0.0011(17) C14 0.041(2) 0.0366(19) 0.051(2) 0.0117(15) 0.0154(17) 0.0051(16) C15 0.0243(15) 0.0364(18) 0.0424(16) 0.0008(13) 0.0158(14) -0.0014(13) C16 0.0234(14) 0.0310(16) 0.0355(14) -0.0015(12) 0.0127(12) -0.0010(12) C17 0.0306(16) 0.0385(17) 0.0334(15) 0.0017(13) 0.0151(13) 0.0033(14) C18 0.0383(19) 0.046(2) 0.0430(18) -0.0103(16) 0.0184(16) 0.0036(17) C19 0.0336(18) 0.0342(18) 0.060(2) -0.0054(16) 0.0182(17) 0.0026(15) C20 0.0348(18) 0.0350(18) 0.055(2) 0.0113(15) 0.0144(17) 0.0046(15) C21 0.0315(16) 0.0387(18) 0.0331(15) 0.0044(13) 0.0114(13) 0.0035(14) C22 0.0376(18) 0.0291(16) 0.0286(13) 0.0031(12) 0.0119(13) 0.0008(13) C23 0.0372(19) 0.0393(19) 0.0396(17) -0.0015(14) 0.0052(15) 0.0004(15) C24 0.044(2) 0.053(2) 0.0391(19) 0.0011(16) -0.0085(17) -0.0093(19) C25 0.072(3) 0.041(2) 0.0360(18) -0.0028(15) 0.0051(19) -0.008(2) C26 0.065(3) 0.040(2) 0.049(2) -0.0075(16) 0.023(2) 0.0008(19) C27 0.041(2) 0.0352(18) 0.0408(17) -0.0038(14) 0.0128(15) 0.0030(15) C28 0.0334(18) 0.046(2) 0.0419(17) -0.0032(15) 0.0154(15) -0.0123(16) C29 0.047(2) 0.047(2) 0.051(2) 0.0026(17) 0.0257(18) -0.0081(18) C30 0.056(2) 0.0274(16) 0.0435(18) 0.0021(14) 0.0256(17) 0.0013(16) C31 0.096(4) 0.053(3) 0.068(3) 0.028(2) 0.047(3) 0.009(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C28 2.042(3) . ? Pd1 O1 2.127(2) . ? Pd1 P1 2.1981(8) . ? Pd1 C8 2.318(4) . ? Pd1 C9 2.333(3) . ? P1 C16 1.796(3) . ? P1 C22 1.806(3) . ? P1 C1 1.867(3) . ? P2 F5 1.541(3) . ? P2 F2 1.563(3) . ? P2 F1 1.566(4) . ? P2 F3 1.595(3) . ? P2 F6 1.601(3) . ? P2 F4 1.604(3) . ? O1 C30 1.239(4) . ? C1 C2 1.506(5) . ? C1 C15 1.517(5) . ? C1 H1 0.98 . ? C2 C3 1.396(5) . ? C2 C7 1.410(5) . ? C3 C4 1.390(6) . ? C3 H3 0.93 . ? C4 C5 1.359(7) . ? C4 H4 0.93 . ? C5 C6 1.393(6) . ? C5 H5 0.93 . ? C6 C7 1.406(5) . ? C6 H6 0.93 . ? C7 C8 1.462(5) . ? C8 C9 1.363(5) . ? C8 H8 0.93 . ? C9 C10 1.454(5) . ? C9 H9 0.93 . ? C10 C11 1.397(5) . ? C10 C15 1.416(5) . ? C11 C12 1.385(6) . ? C11 H11 0.93 . ? C12 C13 1.370(7) . ? C12 H12 0.93 . ? C13 C14 1.385(6) . ? C13 H13 0.93 . ? C14 C15 1.385(5) . ? C14 H14 0.93 . ? C16 C17 1.397(4) . ? C16 C21 1.402(4) . ? C17 C18 1.390(5) . ? C17 H17 0.93 . ? C18 C19 1.387(5) . ? C18 H18 0.93 . ? C19 C20 1.382(5) . ? C19 H19 0.93 . ? C20 C21 1.391(5) . ? C20 H20 0.93 . ? C21 H21 0.93 . ? C22 C23 1.373(5) . ? C22 C27 1.397(5) . ? C23 C24 1.410(5) . ? C23 H23 0.93 . ? C24 C25 1.383(6) . ? C24 H24 0.93 . ? C25 C26 1.361(6) . ? C25 H25 0.93 . ? C26 C27 1.399(5) . ? C26 H26 0.93 . ? C27 H27 0.93 . ? C28 C29 1.530(5) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29 C30 1.466(6) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 C31 1.497(5) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C32 C33 1.412(8) . ? C32 C34 1.468(14) 3_667 ? C32 H32 0.93 . ? C33 C34 1.356(8) . ? C33 H33 0.93 . ? C34 C32 1.468(14) 3_667 ? C34 H34 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Pd1 O1 82.14(13) . . ? C28 Pd1 P1 89.77(10) . . ? O1 Pd1 P1 171.85(7) . . ? C28 Pd1 C8 158.20(15) . . ? O1 Pd1 C8 92.23(11) . . ? P1 Pd1 C8 94.95(9) . . ? C28 Pd1 C9 167.27(14) . . ? O1 Pd1 C9 96.53(11) . . ? P1 Pd1 C9 91.58(9) . . ? C8 Pd1 C9 34.08(13) . . ? C16 P1 C22 108.22(15) . . ? C16 P1 C1 102.23(15) . . ? C22 P1 C1 108.49(15) . . ? C16 P1 Pd1 116.05(10) . . ? C22 P1 Pd1 113.31(10) . . ? C1 P1 Pd1 107.76(11) . . ? F5 P2 F2 95.7(3) . . ? F5 P2 F1 90.9(3) . . ? F2 P2 F1 89.4(2) . . ? F5 P2 F3 92.6(3) . . ? F2 P2 F3 91.7(2) . . ? F1 P2 F3 176.2(3) . . ? F5 P2 F6 176.9(3) . . ? F2 P2 F6 87.25(19) . . ? F1 P2 F6 90.1(2) . . ? F3 P2 F6 86.4(2) . . ? F5 P2 F4 88.6(3) . . ? F2 P2 F4 175.6(2) . . ? F1 P2 F4 89.7(2) . . ? F3 P2 F4 88.93(19) . . ? F6 P2 F4 88.5(2) . . ? C30 O1 Pd1 111.9(2) . . ? C2 C1 C15 112.6(3) . . ? C2 C1 P1 113.1(2) . . ? C15 C1 P1 107.5(2) . . ? C2 C1 H1 107.8 . . ? C15 C1 H1 107.8 . . ? P1 C1 H1 107.8 . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 118.2(3) . . ? C7 C2 C1 121.8(3) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 121.3(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 117.9(4) . . ? C6 C7 C8 117.9(3) . . ? C2 C7 C8 124.3(3) . . ? C9 C8 C7 128.0(3) . . ? C9 C8 Pd1 73.6(2) . . ? C7 C8 Pd1 110.9(2) . . ? C9 C8 H8 116 . . ? C7 C8 H8 116 . . ? Pd1 C8 H8 85.2 . . ? C8 C9 C10 127.3(3) . . ? C8 C9 Pd1 72.3(2) . . ? C10 C9 Pd1 114.8(2) . . ? C8 C9 H9 116.4 . . ? C10 C9 H9 116.4 . . ? Pd1 C9 H9 82.5 . . ? C11 C10 C15 118.3(3) . . ? C11 C10 C9 117.5(3) . . ? C15 C10 C9 124.1(3) . . ? C12 C11 C10 121.8(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 119.0(4) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 120.9(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 120.9(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 119.1(3) . . ? C14 C15 C1 119.8(3) . . ? C10 C15 C1 121.0(3) . . ? C17 C16 C21 118.9(3) . . ? C17 C16 P1 119.5(2) . . ? C21 C16 P1 121.4(2) . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.6(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C21 C16 120.5(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C23 C22 C27 119.4(3) . . ? C23 C22 P1 121.8(3) . . ? C27 C22 P1 118.3(3) . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.4(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.9(4) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.5(4) . . ? C22 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 Pd1 105.3(2) . . ? C29 C28 H28A 110.7 . . ? Pd1 C28 H28A 110.7 . . ? C29 C28 H28B 110.7 . . ? Pd1 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? C30 C29 C28 112.4(3) . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? O1 C30 C29 120.0(3) . . ? O1 C30 C31 119.0(4) . . ? C29 C30 C31 121.0(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C34 101.5(10) . 3_667 ? C33 C32 H32 129.2 . . ? C34 C32 H32 129.2 3_667 . ? C34 C33 C32 121.3(11) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.3 . . ? C33 C34 C32 137.1(9) . 3_667 ? C33 C34 H34 111.4 . . ? C32 C34 H34 111.4 3_667 . ? _chemical_name_common (Pd(CH2CH2COCH3)(trop))(PF6) # Attachment '7a.cif' data_tropos _database_code_depnum_ccdc_archive 'CCDC 696685' #TrackingRef '7a.cif' _audit_creation_date 2010-04-20T15:12:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic '[PdClMe(trop)]' _chemical_formula_sum 'C28.50 H25 Cl2 P Pd' _chemical_formula_moiety 'C27 H24 Cl P Pd, 0.5(C H2 Cl2)' _chemical_formula_weight 575.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.907(5) _cell_length_b 19.718(5) _cell_length_c 15.161(5) _cell_angle_alpha 90 _cell_angle_beta 92.175(5) _cell_angle_gamma 90 _cell_volume 2660.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.840 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_reflns_av_unetI/netI 0.125 _diffrn_reflns_number 4654 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 4654 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR-97 (J. Appl. Cryst. 1999, 32, 115)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4654 _refine_ls_number_parameters 293 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1759 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.881 _refine_diff_density_min -0.48 _refine_diff_density_rms 0.105 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.82926(9) 0.18363(4) 0.01140(5) 0.0580(3) Uani 1 1 d . . . Cl1 Cl 0.8881(4) 0.11745(16) -0.11421(17) 0.0891(9) Uani 1 1 d . . . P1 P 0.7678(2) 0.24695(12) 0.12458(15) 0.0474(6) Uani 1 1 d . . . C1 C 0.9376(8) 0.2541(4) 0.2003(5) 0.046(2) Uani 1 1 d . . . H1 H 0.9095 0.2824 0.2502 0.055 Uiso 1 1 calc R . . C2 C 1.0618(9) 0.2902(5) 0.1557(6) 0.049(2) Uani 1 1 d . . . C3 C 1.1108(10) 0.3530(5) 0.1837(7) 0.064(3) Uani 1 1 d . . . H3 H 1.0659 0.3728 0.2317 0.077 Uiso 1 1 calc R . . C4 C 1.2232(12) 0.3880(6) 0.1436(9) 0.088(4) Uani 1 1 d . . . H4 H 1.2555 0.4299 0.165 0.106 Uiso 1 1 calc R . . C5 C 1.2872(12) 0.3591(7) 0.0709(10) 0.094(4) Uani 1 1 d . . . H5 H 1.3624 0.3825 0.0428 0.113 Uiso 1 1 calc R . . C6 C 1.2418(11) 0.2959(6) 0.0387(7) 0.073(3) Uani 1 1 d . . . H6 H 1.2862 0.2772 -0.0102 0.087 Uiso 1 1 calc R . . C7 C 1.1275(9) 0.2608(5) 0.0814(6) 0.056(2) Uani 1 1 d . . . C8 C 1.0901(10) 0.1945(6) 0.0464(6) 0.065(3) Uani 1 1 d . . . H8 H 1.1027 0.1891 -0.0138 0.079 Uiso 1 1 calc R . . C9 C 1.0386(10) 0.1383(5) 0.0893(6) 0.059(2) Uani 1 1 d . . . H9 H 1.0163 0.1006 0.0545 0.07 Uiso 1 1 calc R . . C10 C 1.0149(9) 0.1312(5) 0.1838(6) 0.053(2) Uani 1 1 d . . . C11 C 1.0293(10) 0.0668(5) 0.2205(7) 0.062(3) Uani 1 1 d . . . H11 H 1.0445 0.0297 0.184 0.075 Uiso 1 1 calc R . . C12 C 1.0216(11) 0.0571(5) 0.3104(8) 0.068(3) Uani 1 1 d . . . H12 H 1.035 0.0141 0.3347 0.082 Uiso 1 1 calc R . . C13 C 0.9937(11) 0.1118(6) 0.3634(7) 0.072(3) Uani 1 1 d . . . H13 H 0.9898 0.1056 0.4241 0.087 Uiso 1 1 calc R . . C14 C 0.9716(10) 0.1753(5) 0.3286(6) 0.058(2) Uani 1 1 d . . . H14 H 0.9528 0.2118 0.3654 0.07 Uiso 1 1 calc R . . C15 C 0.9776(9) 0.1850(5) 0.2370(5) 0.046(2) Uani 1 1 d . . . C16 C 0.6216(9) 0.2123(5) 0.1895(6) 0.051(2) Uani 1 1 d . . . C17 C 0.6235(14) 0.1447(6) 0.2103(10) 0.105(5) Uani 1 1 d . . . H17 H 0.7004 0.1175 0.1903 0.126 Uiso 1 1 calc R . . C18 C 0.5125(18) 0.1159(7) 0.2606(12) 0.143(7) Uani 1 1 d . . . H18 H 0.5174 0.0699 0.2736 0.172 Uiso 1 1 calc R . . C19 C 0.3988(12) 0.1528(7) 0.2909(8) 0.080(3) Uani 1 1 d . . . H19 H 0.3236 0.1323 0.3225 0.095 Uiso 1 1 calc R . . C20 C 0.3956(12) 0.2192(7) 0.2750(7) 0.083(3) Uani 1 1 d . . . H20 H 0.3193 0.2456 0.2973 0.1 Uiso 1 1 calc R . . C21 C 0.5073(11) 0.2499(6) 0.2245(6) 0.071(3) Uani 1 1 d . . . H21 H 0.5038 0.2964 0.2147 0.086 Uiso 1 1 calc R . . C22 C 0.7218(9) 0.3347(4) 0.1031(6) 0.047(2) Uani 1 1 d . . . C23 C 0.7034(10) 0.3797(5) 0.1715(6) 0.058(2) Uani 1 1 d . . . H23 H 0.7101 0.3641 0.2294 0.07 Uiso 1 1 calc R . . C24 C 0.6751(12) 0.4481(6) 0.1552(8) 0.078(3) Uani 1 1 d . . . H24 H 0.6642 0.4777 0.2022 0.094 Uiso 1 1 calc R . . C25 C 0.6635(12) 0.4717(6) 0.0721(9) 0.076(3) Uani 1 1 d . . . H25 H 0.644 0.5174 0.0618 0.091 Uiso 1 1 calc R . . C26 C 0.6800(11) 0.4289(6) 0.0030(8) 0.077(3) Uani 1 1 d . . . H26 H 0.6728 0.4457 -0.0543 0.093 Uiso 1 1 calc R . . C27 C 0.7081(11) 0.3593(6) 0.0169(7) 0.069(3) Uani 1 1 d . . . H27 H 0.7174 0.3301 -0.0308 0.082 Uiso 1 1 calc R . . C28 C 0.6052(11) 0.1955(6) -0.0345(7) 0.083(4) Uani 1 1 d . . . H28A H 0.6011 0.227 -0.0829 0.125 Uiso 1 1 calc R . . H28B H 0.5462 0.2125 0.0123 0.125 Uiso 1 1 calc R . . H28C H 0.566 0.1525 -0.054 0.125 Uiso 1 1 calc R . . Cl2 Cl 0.5744(18) -0.0009(10) -0.0475(9) 0.281(8) Uiso 0.5 1 d PD . . Cl3 Cl 0.630(3) -0.0491(17) 0.1309(13) 0.477(18) Uiso 0.5 1 d PD . . C29 C 0.7157(19) -0.0125(15) 0.0386(14) 0.108(9) Uiso 0.5 1 d PD . . H29A H 0.7943 -0.0421 0.0184 0.13 Uiso 0.5 1 calc PR . . H29B H 0.7604 0.0308 0.0548 0.13 Uiso 0.5 1 calc PR . . 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 0.0593(5) 0.0594(5) 0.0551(4) -0.0040(4) 0.0006(3) 0.0118(4) Cl1 0.112(2) 0.094(2) 0.0621(15) -0.0164(15) 0.0059(15) 0.0190(19) P1 0.0385(12) 0.0470(14) 0.0570(13) 0.0038(11) 0.0029(10) 0.0023(11) C1 0.037(5) 0.041(5) 0.060(5) 0.011(4) 0.012(4) -0.001(4) C2 0.040(5) 0.045(5) 0.061(5) 0.015(4) -0.001(4) -0.001(4) C3 0.054(6) 0.054(7) 0.086(7) 0.007(6) 0.010(5) -0.003(5) C4 0.067(8) 0.068(8) 0.132(10) 0.020(8) 0.015(7) -0.030(6) C5 0.048(7) 0.103(11) 0.132(11) 0.063(9) -0.003(7) -0.010(7) C6 0.056(6) 0.092(9) 0.072(7) 0.029(6) 0.020(5) -0.002(6) C7 0.042(5) 0.060(7) 0.067(6) 0.016(5) 0.003(4) 0.002(5) C8 0.054(6) 0.085(9) 0.059(5) -0.006(6) 0.022(5) 0.015(6) C9 0.051(6) 0.056(6) 0.069(6) -0.006(5) -0.003(5) 0.016(5) C10 0.039(5) 0.052(6) 0.066(6) 0.005(5) -0.002(4) 0.011(4) C11 0.050(6) 0.057(7) 0.080(7) 0.003(6) -0.001(5) 0.010(5) C12 0.057(6) 0.043(6) 0.104(8) 0.019(6) -0.003(6) 0.005(5) C13 0.059(6) 0.078(8) 0.080(7) 0.029(7) -0.002(5) -0.003(6) C14 0.051(6) 0.057(6) 0.067(6) 0.002(5) 0.001(4) 0.005(5) C15 0.039(5) 0.045(5) 0.055(5) 0.011(5) 0.006(4) 0.002(4) C16 0.028(5) 0.052(6) 0.074(6) 0.006(5) 0.000(4) 0.002(4) C17 0.085(9) 0.055(8) 0.178(14) 0.005(8) 0.056(9) -0.011(7) C18 0.121(12) 0.067(9) 0.25(2) 0.018(11) 0.067(13) -0.020(9) C19 0.048(7) 0.079(9) 0.113(9) 0.010(7) 0.020(6) -0.017(6) C20 0.058(7) 0.107(11) 0.085(8) -0.002(7) 0.015(6) -0.012(7) C21 0.071(7) 0.060(7) 0.083(7) 0.006(6) 0.015(6) -0.005(6) C22 0.037(5) 0.040(5) 0.065(5) 0.006(4) 0.010(4) 0.006(4) C23 0.056(6) 0.043(6) 0.075(6) 0.002(5) -0.001(5) 0.001(5) C24 0.069(7) 0.052(7) 0.111(9) -0.024(7) -0.022(7) 0.001(6) C25 0.060(7) 0.050(7) 0.119(10) 0.018(7) 0.008(7) 0.012(5) C26 0.057(7) 0.076(8) 0.100(9) 0.036(7) 0.014(6) 0.010(6) C27 0.064(6) 0.075(8) 0.068(6) 0.018(6) 0.024(5) 0.019(6) C28 0.060(6) 0.099(9) 0.089(7) -0.034(7) -0.031(5) 0.033(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C28 2.102(9) . ? Pd1 P1 2.208(2) . ? Pd1 C9 2.346(9) . ? Pd1 C8 2.373(10) . ? Pd1 Cl1 2.383(3) . ? P1 C16 1.797(9) . ? P1 C22 1.805(8) . ? P1 C1 1.869(8) . ? C1 C2 1.498(11) . ? C1 C15 1.510(11) . ? C1 H1 0.98 . ? C2 C3 1.376(13) . ? C2 C7 1.413(12) . ? C3 C4 1.376(13) . ? C3 H3 0.93 . ? C4 C5 1.382(17) . ? C4 H4 0.93 . ? C5 C6 1.393(16) . ? C5 H5 0.93 . ? C6 C7 1.409(12) . ? C6 H6 0.93 . ? C7 C8 1.445(13) . ? C8 C9 1.373(13) . ? C8 H8 0.93 . ? C9 C10 1.462(12) . ? C9 H9 0.93 . ? C10 C15 1.381(12) . ? C10 C11 1.390(13) . ? C11 C12 1.380(13) . ? C11 H11 0.93 . ? C12 C13 1.373(14) . ? C12 H12 0.93 . ? C13 C14 1.370(13) . ? C13 H13 0.93 . ? C14 C15 1.404(12) . ? C14 H14 0.93 . ? C16 C17 1.368(14) . ? C16 C21 1.382(12) . ? C17 C18 1.392(16) . ? C17 H17 0.93 . ? C18 C19 1.342(17) . ? C18 H18 0.93 . ? C19 C20 1.331(15) . ? C19 H19 0.93 . ? C20 C21 1.415(13) . ? C20 H20 0.93 . ? C21 H21 0.93 . ? C22 C23 1.379(12) . ? C22 C27 1.395(12) . ? C23 C24 1.393(13) . ? C23 H23 0.93 . ? C24 C25 1.344(15) . ? C24 H24 0.93 . ? C25 C26 1.357(15) . ? C25 H25 0.93 . ? C26 C27 1.409(15) . ? C26 H26 0.93 . ? C27 H27 0.93 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? Cl2 C29 1.793(10) . ? Cl2 Cl2 2.00(3) 3_655 ? Cl2 Cl3 2.39(3) 3_655 ? Cl3 C29 1.775(10) . ? Cl3 Cl2 2.39(3) 3_655 ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Pd1 P1 86.2(3) . . ? C28 Pd1 C9 159.4(4) . . ? P1 Pd1 C9 92.3(2) . . ? C28 Pd1 C8 166.7(4) . . ? P1 Pd1 C8 92.6(2) . . ? C9 Pd1 C8 33.8(3) . . ? C28 Pd1 Cl1 91.8(3) . . ? P1 Pd1 Cl1 177.75(10) . . ? C9 Pd1 Cl1 90.0(2) . . ? C8 Pd1 Cl1 89.1(2) . . ? C16 P1 C22 107.4(4) . . ? C16 P1 C1 106.2(4) . . ? C22 P1 C1 102.2(4) . . ? C16 P1 Pd1 114.6(3) . . ? C22 P1 Pd1 117.6(3) . . ? C1 P1 Pd1 107.5(3) . . ? C2 C1 C15 115.3(7) . . ? C2 C1 P1 110.6(6) . . ? C15 C1 P1 109.4(6) . . ? C2 C1 H1 107 . . ? C15 C1 H1 107 . . ? P1 C1 H1 107 . . ? C3 C2 C7 118.6(8) . . ? C3 C2 C1 121.3(8) . . ? C7 C2 C1 120.0(8) . . ? C4 C3 C2 122.9(10) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 118.3(11) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C4 C5 C6 121.7(11) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 119.0(11) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C2 119.5(10) . . ? C6 C7 C8 115.9(9) . . ? C2 C7 C8 124.5(8) . . ? C9 C8 C7 129.2(9) . . ? C9 C8 Pd1 72.0(5) . . ? C7 C8 Pd1 112.0(6) . . ? C9 C8 H8 115.4 . . ? C7 C8 H8 115.4 . . ? Pd1 C8 H8 85.6 . . ? C8 C9 C10 127.3(9) . . ? C8 C9 Pd1 74.2(5) . . ? C10 C9 Pd1 112.8(6) . . ? C8 C9 H9 116.3 . . ? C10 C9 H9 116.3 . . ? Pd1 C9 H9 82.5 . . ? C15 C10 C11 119.2(8) . . ? C15 C10 C9 123.0(8) . . ? C11 C10 C9 117.8(9) . . ? C12 C11 C10 121.0(10) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C11 119.0(10) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 121.3(10) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.7(9) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C10 C15 C14 119.5(8) . . ? C10 C15 C1 122.4(7) . . ? C14 C15 C1 118.0(8) . . ? C17 C16 C21 115.9(9) . . ? C17 C16 P1 119.6(8) . . ? C21 C16 P1 124.4(8) . . ? C16 C17 C18 121.3(12) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 121.9(13) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C20 C19 C18 118.8(11) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C19 C20 C21 120.6(12) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 121.4(11) . . ? C16 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C27 118.2(8) . . ? C23 C22 P1 120.9(7) . . ? C27 C22 P1 120.9(7) . . ? C22 C23 C24 121.0(10) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 120.6(10) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.1(10) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 121.0(10) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.1(10) . . ? C22 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? Pd1 C28 H28A 109.5 . . ? Pd1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Pd1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 Cl2 Cl2 86.8(10) . 3_655 ? C29 Cl2 Cl3 159.7(16) . 3_655 ? Cl2 Cl2 Cl3 82.1(9) 3_655 3_655 ? C29 Cl3 Cl2 76.0(9) . 3_655 ? Cl3 C29 Cl2 108.3(8) . . ? Cl3 C29 H29A 110 . . ? Cl2 C29 H29A 110 . . ? Cl3 C29 H29B 110 . . ? Cl2 C29 H29B 110 . . ? H29A C29 H29B 108.4 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _chemical_name_common (PdClMe(trop)) # Attachment '1a-7a-10a.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-03-03 at 11:56:17 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : tropos6-170k # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_tropos6-170k _database_code_depnum_ccdc_archive 'CCDC 739871' #TrackingRef '1a-7a-10a.cif' #TrackingRef '1a-7a-10a.cif' _audit_creation_date 2009-03-03T11:56:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic '[PdCl2(Tropp)]' _chemical_formula_sum 'C28 H23 Cl3 P Pd' _chemical_formula_moiety 'C27 H21 Cl2 P Pd, 0.5(C2 H4 Cl2)' _chemical_formula_weight 603.18 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group-name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6468(6) _cell_length_b 14.0728(8) _cell_length_c 20.6612(12) _cell_angle_alpha 90 _cell_angle_beta 95.573(6) _cell_angle_gamma 90 _cell_volume 2502.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type 'empirical, SADABS' _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.892 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur 3, Oxford diffraction' _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.1382 _diffrn_reflns_number 6900 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 30.67 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.89 _reflns_number_total 6900 _reflns_number_gt 3929 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SIR-97 (J. Appl. Cryst.1999, 32, 115)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6900 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.257 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.132 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.87055(4) 0.46814(3) 0.165966(14) 0.01922(9) Uani 1 1 d . . . Cl1 Cl 0.92346(14) 0.60088(8) 0.10249(5) 0.0309(3) Uani 1 1 d . . . Cl2 Cl 0.63180(13) 0.52839(9) 0.18833(5) 0.0291(2) Uani 1 1 d . . . Cl3 Cl 0.6791(2) 0.40797(15) -0.02825(7) 0.0801(6) Uani 1 1 d . . . P1 P 0.81628(13) 0.34243(8) 0.22573(5) 0.0172(2) Uani 1 1 d . . . C1 C 0.9748(5) 0.2540(3) 0.22289(17) 0.0158(9) Uani 1 1 d . . . H1 H 0.9466 0.1969 0.2481 0.019 Uiso 1 1 calc R . . C2 C 1.1212(5) 0.2960(3) 0.25735(18) 0.0176(9) Uani 1 1 d . . . C3 C 1.1857(5) 0.2543(3) 0.31509(19) 0.0250(10) Uani 1 1 d . . . H3 H 1.1417 0.1981 0.331 0.03 Uiso 1 1 calc R . . C4 C 1.3147(6) 0.2957(4) 0.3491(2) 0.0311(11) Uani 1 1 d . . . H4 H 1.3601 0.2665 0.3878 0.037 Uiso 1 1 calc R . . C5 C 1.3776(5) 0.3777(4) 0.3279(2) 0.0333(12) Uani 1 1 d . . . H5 H 1.4668 0.4046 0.3514 0.04 Uiso 1 1 calc R . . C6 C 1.3105(5) 0.4217(4) 0.2718(2) 0.0301(11) Uani 1 1 d . . . H6 H 1.3523 0.4799 0.258 0.036 Uiso 1 1 calc R . . C7 C 1.1829(5) 0.3814(3) 0.23563(19) 0.0217(10) Uani 1 1 d . . . C8 C 1.1239(5) 0.4290(3) 0.17498(19) 0.0239(10) Uani 1 1 d . . . H8 H 1.1363 0.4961 0.1742 0.029 Uiso 1 1 calc R . . C9 C 1.0522(5) 0.3883(3) 0.1185(2) 0.0243(10) Uani 1 1 d . . . H9 H 1.0213 0.4311 0.0841 0.029 Uiso 1 1 calc R . . C10 C 1.0187(5) 0.2889(3) 0.10556(19) 0.0203(9) Uani 1 1 d . . . C11 C 1.0203(5) 0.2575(3) 0.04163(19) 0.0256(10) Uani 1 1 d . . . H11 H 1.037 0.3018 0.0083 0.031 Uiso 1 1 calc R . . C12 C 0.9981(6) 0.1637(3) 0.0263(2) 0.0318(12) Uani 1 1 d . . . H12 H 1.0014 0.1438 -0.0175 0.038 Uiso 1 1 calc R . . C13 C 0.9710(5) 0.0969(3) 0.0733(2) 0.0298(11) Uani 1 1 d . . . H13 H 0.9581 0.0316 0.0625 0.036 Uiso 1 1 calc R . . C14 C 0.9633(5) 0.1286(3) 0.13677(19) 0.0235(10) Uani 1 1 d . . . H14 H 0.9402 0.0843 0.1692 0.028 Uiso 1 1 calc R . . C15 C 0.9883(5) 0.2230(3) 0.15388(18) 0.0183(9) Uani 1 1 d . . . C16 C 0.6436(5) 0.2790(3) 0.19402(18) 0.0188(9) Uani 1 1 d . . . C17 C 0.6006(6) 0.2870(4) 0.1275(2) 0.0318(12) Uani 1 1 d . . . H17 H 0.6573 0.3272 0.1014 0.038 Uiso 1 1 calc R . . C18 C 0.4736(6) 0.2354(4) 0.0995(2) 0.0396(13) Uani 1 1 d . . . H18 H 0.4443 0.2404 0.0542 0.048 Uiso 1 1 calc R . . C19 C 0.3904(5) 0.1777(3) 0.1366(2) 0.0337(12) Uani 1 1 d . . . H19 H 0.3036 0.1431 0.1171 0.04 Uiso 1 1 calc R . . C20 C 0.4328(5) 0.1699(3) 0.2022(2) 0.0292(11) Uani 1 1 d . . . H20 H 0.376 0.1291 0.2278 0.035 Uiso 1 1 calc R . . C21 C 0.5572(5) 0.2209(3) 0.2313(2) 0.0254(10) Uani 1 1 d . . . H21 H 0.5838 0.2163 0.2769 0.03 Uiso 1 1 calc R . . C22 C 0.8183(5) 0.3668(3) 0.31209(18) 0.0182(9) Uani 1 1 d . . . C23 C 0.8116(5) 0.2921(3) 0.35625(18) 0.0224(10) Uani 1 1 d . . . H23 H 0.7979 0.2287 0.3409 0.027 Uiso 1 1 calc R . . C24 C 0.8248(5) 0.3103(3) 0.42209(19) 0.0287(11) Uani 1 1 d . . . H24 H 0.817 0.2598 0.4521 0.034 Uiso 1 1 calc R . . C25 C 0.8495(6) 0.4025(4) 0.4446(2) 0.0309(11) Uani 1 1 d . . . H25 H 0.8591 0.4149 0.4901 0.037 Uiso 1 1 calc R . . C26 C 0.8601(5) 0.4761(4) 0.40115(19) 0.0307(11) Uani 1 1 d . . . H26 H 0.878 0.5391 0.4166 0.037 Uiso 1 1 calc R . . C27 C 0.8447(5) 0.4581(3) 0.33486(19) 0.0246(10) Uani 1 1 d . . . H27 H 0.8524 0.5089 0.305 0.03 Uiso 1 1 calc R . . C28 C 0.5722(6) 0.5132(5) -0.0121(3) 0.068(2) Uani 1 1 d . . . H28A H 0.634 0.5529 0.0204 0.081 Uiso 1 1 calc R . . H28B H 0.5513 0.5507 -0.0526 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01955(17) 0.01882(16) 0.01922(15) 0.00317(15) 0.00154(11) 0.00040(18) Cl1 0.0389(7) 0.0237(6) 0.0316(6) 0.0082(5) 0.0110(5) 0.0023(6) Cl2 0.0245(6) 0.0287(6) 0.0346(6) 0.0033(5) 0.0045(4) 0.0056(6) Cl3 0.0826(14) 0.1028(15) 0.0564(10) 0.0107(9) 0.0147(9) 0.0550(12) P1 0.0150(6) 0.0193(6) 0.0171(5) 0.0010(4) 0.0000(4) -0.0007(5) C1 0.016(2) 0.014(2) 0.0180(19) 0.0018(16) 0.0018(16) -0.0015(18) C2 0.011(2) 0.017(2) 0.024(2) 0.0013(17) 0.0001(17) 0.0008(19) C3 0.023(3) 0.026(3) 0.025(2) -0.0010(19) -0.0011(19) -0.001(2) C4 0.026(3) 0.037(3) 0.028(2) -0.004(2) -0.008(2) 0.008(2) C5 0.015(3) 0.039(3) 0.043(3) -0.008(2) -0.009(2) 0.002(2) C6 0.021(3) 0.031(3) 0.039(3) -0.005(2) 0.000(2) -0.002(2) C7 0.016(2) 0.023(2) 0.026(2) -0.0011(18) 0.0003(18) 0.002(2) C8 0.024(3) 0.021(2) 0.027(2) 0.0019(18) 0.0063(19) 0.003(2) C9 0.023(3) 0.025(2) 0.025(2) 0.0072(19) 0.0063(19) 0.010(2) C10 0.015(2) 0.022(2) 0.022(2) 0.0013(17) -0.0020(17) 0.005(2) C11 0.031(3) 0.027(2) 0.019(2) 0.0038(18) 0.0031(19) 0.010(2) C12 0.037(3) 0.037(3) 0.021(2) -0.007(2) 0.001(2) 0.008(3) C13 0.031(3) 0.027(3) 0.030(2) -0.004(2) 0.000(2) 0.000(2) C14 0.023(3) 0.024(2) 0.022(2) 0.0004(18) -0.0014(18) 0.000(2) C15 0.014(2) 0.021(2) 0.019(2) 0.0010(17) -0.0019(16) 0.003(2) C16 0.014(2) 0.019(2) 0.023(2) -0.0010(17) 0.0013(17) -0.0022(19) C17 0.030(3) 0.039(3) 0.026(2) 0.005(2) -0.003(2) -0.008(3) C18 0.036(3) 0.049(3) 0.031(3) -0.004(2) -0.011(2) -0.006(3) C19 0.016(3) 0.035(3) 0.048(3) -0.010(2) -0.006(2) -0.005(2) C20 0.022(3) 0.024(3) 0.042(3) -0.003(2) 0.006(2) -0.003(2) C21 0.019(2) 0.030(3) 0.026(2) 0.0016(19) -0.0010(18) -0.003(2) C22 0.014(2) 0.022(2) 0.019(2) 0.0006(17) -0.0003(16) -0.0013(19) C23 0.018(2) 0.027(2) 0.021(2) -0.0016(18) 0.0012(18) 0.001(2) C24 0.033(3) 0.033(3) 0.020(2) 0.0065(19) 0.0005(19) -0.004(2) C25 0.035(3) 0.039(3) 0.018(2) -0.006(2) -0.001(2) -0.003(3) C26 0.039(3) 0.027(3) 0.025(2) -0.003(2) 0.000(2) -0.004(3) C27 0.023(2) 0.027(2) 0.024(2) 0.0043(19) 0.0020(17) -0.003(2) C28 0.046(4) 0.095(6) 0.060(4) 0.020(4) -0.005(3) 0.008(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2332(11) . ? Pd1 C9 2.234(4) . ? Pd1 C8 2.249(4) . ? Pd1 Cl2 2.3194(12) . ? Pd1 Cl1 2.3527(11) . ? Cl3 C28 1.793(7) . ? P1 C16 1.807(4) . ? P1 C22 1.815(4) . ? P1 C1 1.856(4) . ? C1 C15 1.507(5) . ? C1 C2 1.511(5) . ? C1 H1 1 . ? C2 C3 1.396(5) . ? C2 C7 1.406(6) . ? C3 C4 1.387(6) . ? C3 H3 0.95 . ? C4 C5 1.366(7) . ? C4 H4 0.95 . ? C5 C6 1.390(6) . ? C5 H5 0.95 . ? C6 C7 1.393(6) . ? C6 H6 0.95 . ? C7 C8 1.468(6) . ? C8 C9 1.391(6) . ? C8 H8 0.95 . ? C9 C10 1.448(6) . ? C9 H9 0.95 . ? C10 C11 1.394(5) . ? C10 C15 1.406(5) . ? C11 C12 1.367(6) . ? C11 H11 0.95 . ? C12 C13 1.388(6) . ? C12 H12 0.95 . ? C13 C14 1.392(5) . ? C13 H13 0.95 . ? C14 C15 1.387(6) . ? C14 H14 0.95 . ? C16 C21 1.389(5) . ? C16 C17 1.394(5) . ? C17 C18 1.394(6) . ? C17 H17 0.95 . ? C18 C19 1.368(7) . ? C18 H18 0.95 . ? C19 C20 1.373(6) . ? C19 H19 0.95 . ? C20 C21 1.381(6) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C27 1.381(6) . ? C22 C23 1.397(5) . ? C23 C24 1.378(5) . ? C23 H23 0.95 . ? C24 C25 1.388(6) . ? C24 H24 0.95 . ? C25 C26 1.380(6) . ? C25 H25 0.95 . ? C26 C27 1.386(5) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 C28 1.438(11) 3_665 ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 C9 92.23(12) . . ? P1 Pd1 C8 90.89(11) . . ? C9 Pd1 C8 36.15(15) . . ? P1 Pd1 Cl2 86.59(4) . . ? C9 Pd1 Cl2 161.56(12) . . ? C8 Pd1 Cl2 162.13(11) . . ? P1 Pd1 Cl1 179.08(5) . . ? C9 Pd1 Cl1 88.36(12) . . ? C8 Pd1 Cl1 90.00(11) . . ? Cl2 Pd1 Cl1 92.62(4) . . ? C16 P1 C22 112.23(19) . . ? C16 P1 C1 104.10(18) . . ? C22 P1 C1 102.77(17) . . ? C16 P1 Pd1 113.68(13) . . ? C22 P1 Pd1 114.30(14) . . ? C1 P1 Pd1 108.55(13) . . ? C15 C1 C2 114.9(3) . . ? C15 C1 P1 110.5(3) . . ? C2 C1 P1 108.1(3) . . ? C15 C1 H1 107.7 . . ? C2 C1 H1 107.7 . . ? P1 C1 H1 107.7 . . ? C3 C2 C7 119.9(4) . . ? C3 C2 C1 119.1(4) . . ? C7 C2 C1 120.7(3) . . ? C4 C3 C2 119.4(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 121.2(4) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 120.7(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 118.9(4) . . ? C6 C7 C8 117.6(4) . . ? C2 C7 C8 123.5(4) . . ? C9 C8 C7 128.2(4) . . ? C9 C8 Pd1 71.3(2) . . ? C7 C8 Pd1 115.9(3) . . ? C9 C8 H8 115.9 . . ? C7 C8 H8 115.9 . . ? Pd1 C8 H8 82.3 . . ? C8 C9 C10 128.1(4) . . ? C8 C9 Pd1 72.5(2) . . ? C10 C9 Pd1 115.5(3) . . ? C8 C9 H9 115.9 . . ? C10 C9 H9 115.9 . . ? Pd1 C9 H9 81.4 . . ? C11 C10 C15 118.9(4) . . ? C11 C10 C9 117.5(4) . . ? C15 C10 C9 123.7(4) . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 118.0(4) . . ? C12 C13 H13 121 . . ? C14 C13 H13 121 . . ? C15 C14 C13 121.7(4) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C10 119.1(4) . . ? C14 C15 C1 119.6(4) . . ? C10 C15 C1 121.2(4) . . ? C21 C16 C17 119.2(4) . . ? C21 C16 P1 124.0(3) . . ? C17 C16 P1 116.7(3) . . ? C18 C17 C16 119.3(4) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C21 120.7(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 120.1(4) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C27 C22 C23 119.6(4) . . ? C27 C22 P1 119.7(3) . . ? C23 C22 P1 120.2(3) . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24 120 . . ? C25 C24 H24 120 . . ? C26 C25 C24 120.0(4) . . ? C26 C25 H25 120 . . ? C24 C25 H25 120 . . ? C25 C26 C27 120.1(4) . . ? C25 C26 H26 120 . . ? C27 C26 H26 120 . . ? C22 C27 C26 120.2(4) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C28 C28 Cl3 109.4(7) 3_665 . ? C28 C28 H28A 109.8 3_665 . ? Cl3 C28 H28A 109.8 . . ? C28 C28 H28B 109.8 3_665 . ? Cl3 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? _chemical_name_common (PdCl2(Tropp))