# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name F.Cloke S.Caddick O.Esposito P.B.Hitchcock 'de K. Lewis, A.K.' _publ_contact_author_name 'F. Cloke' _publ_contact_author_address ; Departmentl of Chemistry University of Sussex Chichester Building BRIGHTON East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email F.G.CLOKE@SUSSEX.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis and reactivity of alkyl palladium N-heterocyclic carbene complexes ; _publ_requested_category FM data_jul1005 _database_code_depnum_ccdc_archive 'CCDC 633696' _audit_creation_date 2005-07-07T11:05:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H62 Cl2 N4 Pd2' _chemical_formula_sum 'C32 H62 Cl2 N4 Pd2' _chemical_formula_weight 786.56 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1540(3) _cell_length_b 9.7982(2) _cell_length_c 17.5999(4) _cell_angle_alpha 90 _cell_angle_beta 107.560(1) _cell_angle_gamma 90 _cell_volume 1833.85(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28167 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8333 _exptl_absorpt_correction_T_max 0.9667 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.531479E-1 _diffrn_orient_matrix_ub_12 0.164497E-1 _diffrn_orient_matrix_ub_13 0.358077E-1 _diffrn_orient_matrix_ub_21 0.413386E-1 _diffrn_orient_matrix_ub_22 -0.786921E-1 _diffrn_orient_matrix_ub_23 0.340803E-1 _diffrn_orient_matrix_ub_31 0.656441E-1 _diffrn_orient_matrix_ub_32 0.628737E-1 _diffrn_orient_matrix_ub_33 0.332861E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_unetI/netI 0.0337 _diffrn_reflns_number 26967 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 3596 _reflns_number_gt 3084 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0204P)^2^+2.4404P] 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 3596 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.536 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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 Pd Pd 0.632901(19) 0.58754(2) 0.569985(13) 0.01740(8) Uani 1 1 d . . . Cl Cl 0.53863(7) 0.36559(7) 0.55854(5) 0.02829(18) Uani 1 1 d . . . N1 N 0.7722(2) 0.8339(2) 0.53692(14) 0.0186(5) Uani 1 1 d . . . N2 N 0.6472(2) 0.8883(2) 0.60564(14) 0.0198(5) Uani 1 1 d . . . C1 C 0.6894(3) 0.7795(3) 0.57191(16) 0.0174(6) Uani 1 1 d . . . C2 C 0.7817(3) 0.9739(3) 0.55000(19) 0.0277(7) Uani 1 1 d . . . H2 H 0.8338 1.0349 0.5322 0.033 Uiso 1 1 calc R . . C3 C 0.7048(3) 1.0068(3) 0.59188(19) 0.0281(7) Uani 1 1 d . . . H3 H 0.6917 1.0958 0.6093 0.034 Uiso 1 1 calc R . . C4 C 0.8505(3) 0.7628(3) 0.49263(17) 0.0223(6) Uani 1 1 d . . . C5 C 0.8567(3) 0.8537(4) 0.4234(2) 0.0362(8) Uani 1 1 d . . . H5A H 0.7718 0.8668 0.3869 0.054 Uiso 1 1 calc R . . H5B H 0.9096 0.8101 0.395 0.054 Uiso 1 1 calc R . . H5C H 0.8926 0.9424 0.4441 0.054 Uiso 1 1 calc R . . C6 C 0.9816(3) 0.7417(4) 0.5501(2) 0.0393(9) Uani 1 1 d . . . H6A H 1.0166 0.8299 0.5723 0.059 Uiso 1 1 calc R . . H6B H 1.0357 0.7005 0.5217 0.059 Uiso 1 1 calc R . . H6C H 0.9769 0.6811 0.5934 0.059 Uiso 1 1 calc R . . C7 C 0.7947(3) 0.6275(3) 0.4576(2) 0.0344(8) Uani 1 1 d . . . H7A H 0.7096 0.6422 0.4215 0.052 Uiso 1 1 calc R . . H7B H 0.7909 0.5657 0.5006 0.052 Uiso 1 1 calc R . . H7C H 0.8474 0.5869 0.4279 0.052 Uiso 1 1 calc R . . C8 C 0.5586(3) 0.8885(3) 0.65594(18) 0.0241(6) Uani 1 1 d . . . C9 C 0.6367(4) 0.8695(6) 0.7414(2) 0.0755(16) Uani 1 1 d . . . H9A H 0.6791 0.7808 0.7475 0.113 Uiso 1 1 calc R . . H9B H 0.5822 0.8732 0.7758 0.113 Uiso 1 1 calc R . . H9C H 0.6998 0.9423 0.7565 0.113 Uiso 1 1 calc R . . C10 C 0.4581(4) 0.7810(4) 0.6292(3) 0.0678(14) Uani 1 1 d . . . H10A H 0.4973 0.6906 0.6343 0.102 Uiso 1 1 calc R . . H10B H 0.4097 0.7971 0.5734 0.102 Uiso 1 1 calc R . . H10C H 0.4018 0.7854 0.6625 0.102 Uiso 1 1 calc R . . C11 C 0.4931(4) 1.0258(4) 0.6467(3) 0.0499(10) Uani 1 1 d . . . H11A H 0.5561 1.0984 0.663 0.075 Uiso 1 1 calc R . . H11B H 0.4372 1.0285 0.6802 0.075 Uiso 1 1 calc R . . H11C H 0.4438 1.0392 0.5908 0.075 Uiso 1 1 calc R . . C12 C 0.7822(3) 0.5619(3) 0.67304(18) 0.0261(7) Uani 1 1 d . . . H12A H 0.8475 0.6288 0.6706 0.031 Uiso 1 1 calc R . . H12B H 0.7519 0.5895 0.7181 0.031 Uiso 1 1 calc R . . C13 C 0.8487(3) 0.4241(3) 0.69550(17) 0.0218(6) Uani 1 1 d . . . C14 C 0.9788(3) 0.4532(3) 0.7555(2) 0.0324(7) Uani 1 1 d . . . H14A H 0.9681 0.5009 0.802 0.049 Uiso 1 1 calc R . . H14B H 1.0279 0.5104 0.7301 0.049 Uiso 1 1 calc R . . H14C H 1.0231 0.3669 0.7726 0.049 Uiso 1 1 calc R . . C15 C 0.8704(3) 0.3492(3) 0.62450(19) 0.0298(7) Uani 1 1 d . . . H15A H 0.7892 0.3301 0.5848 0.045 Uiso 1 1 calc R . . H15B H 0.9144 0.2631 0.6427 0.045 Uiso 1 1 calc R . . H15C H 0.9214 0.4063 0.6005 0.045 Uiso 1 1 calc R . . C16 C 0.7768(3) 0.3327(3) 0.73687(19) 0.0310(7) Uani 1 1 d . . . H16A H 0.6933 0.3127 0.7001 0.046 Uiso 1 1 calc R . . H16B H 0.7678 0.3794 0.7841 0.046 Uiso 1 1 calc R . . H16C H 0.8231 0.2472 0.753 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01667(11) 0.01207(11) 0.02189(12) 0.00102(9) 0.00345(8) -0.00186(9) Cl 0.0253(4) 0.0162(3) 0.0344(4) 0.0066(3) -0.0046(3) -0.0063(3) N1 0.0190(12) 0.0150(12) 0.0227(13) -0.0004(10) 0.0079(10) -0.0023(9) N2 0.0234(12) 0.0134(12) 0.0240(12) -0.0016(10) 0.0093(10) -0.0004(9) C1 0.0166(13) 0.0152(14) 0.0171(14) 0.0001(11) 0.0000(11) 0.0005(11) C2 0.0327(17) 0.0154(15) 0.0380(18) -0.0015(13) 0.0154(15) -0.0074(13) C3 0.0358(18) 0.0139(15) 0.0363(18) -0.0038(13) 0.0135(15) -0.0036(12) C4 0.0222(15) 0.0229(15) 0.0234(15) -0.0005(12) 0.0091(12) -0.0003(12) C5 0.040(2) 0.0388(19) 0.0371(19) 0.0086(16) 0.0235(16) 0.0029(16) C6 0.0283(18) 0.052(2) 0.0354(19) -0.0099(17) 0.0058(15) 0.0112(16) C7 0.045(2) 0.0306(18) 0.0356(19) -0.0113(15) 0.0248(16) -0.0072(15) C8 0.0276(16) 0.0207(16) 0.0282(16) -0.0009(12) 0.0150(13) 0.0046(12) C9 0.069(3) 0.131(5) 0.032(2) 0.021(3) 0.024(2) 0.050(3) C10 0.067(3) 0.058(3) 0.108(4) -0.033(3) 0.071(3) -0.023(2) C11 0.049(2) 0.039(2) 0.072(3) 0.007(2) 0.034(2) 0.0134(18) C12 0.0322(17) 0.0168(15) 0.0234(15) -0.0011(12) -0.0004(13) 0.0002(12) C13 0.0187(14) 0.0228(15) 0.0217(15) 0.0022(12) 0.0028(11) 0.0028(12) C14 0.0241(16) 0.0347(18) 0.0332(18) 0.0046(14) 0.0010(14) -0.0007(14) C15 0.0268(17) 0.0312(17) 0.0342(18) -0.0056(14) 0.0135(14) 0.0039(13) C16 0.0313(18) 0.0332(18) 0.0273(17) 0.0064(14) 0.0070(14) -0.0026(14) #----------------------------------------------------------------------------# # 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 Pd C1 1.980(3) . ? Pd C12 2.075(3) . ? Pd Cl 2.3975(7) . ? Pd Cl 2.5252(7) 3_666 ? Cl Pd 2.5252(7) 3_666 ? N1 C1 1.364(4) . ? N1 C2 1.389(4) . ? N1 C4 1.506(4) . ? N2 C1 1.371(3) . ? N2 C3 1.383(4) . ? N2 C8 1.513(4) . ? C2 C3 1.328(4) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C7 1.515(4) . ? C4 C6 1.520(4) . ? C4 C5 1.527(4) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.505(5) . ? C8 C10 1.507(5) . ? C8 C11 1.516(4) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C13 1.534(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C16 1.526(4) . ? C13 C15 1.530(4) . ? C13 C14 1.542(4) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? 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 C1 Pd C12 86.14(11) . . ? C1 Pd Cl 172.76(8) . . ? C12 Pd Cl 100.36(8) . . ? C1 Pd Cl 89.64(8) . 3_666 ? C12 Pd Cl 175.28(9) . 3_666 ? Cl Pd Cl 83.98(2) . 3_666 ? Pd Cl Pd 96.02(2) . 3_666 ? C1 N1 C2 109.9(2) . . ? C1 N1 C4 129.1(2) . . ? C2 N1 C4 121.0(2) . . ? C1 N2 C3 109.8(2) . . ? C1 N2 C8 128.6(2) . . ? C3 N2 C8 121.5(2) . . ? N1 C1 N2 105.0(2) . . ? N1 C1 Pd 128.2(2) . . ? N2 C1 Pd 126.7(2) . . ? C3 C2 N1 107.5(3) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C2 C3 N2 107.8(3) . . ? C2 C3 H3 126.1 . . ? N2 C3 H3 126.1 . . ? N1 C4 C7 112.6(2) . . ? N1 C4 C6 108.1(2) . . ? C7 C4 C6 110.3(3) . . ? N1 C4 C5 108.4(2) . . ? C7 C4 C5 107.3(3) . . ? C6 C4 C5 110.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 112.2(4) . . ? C9 C8 N2 107.5(3) . . ? C10 C8 N2 111.9(3) . . ? C9 C8 C11 109.4(3) . . ? C10 C8 C11 107.3(3) . . ? N2 C8 C11 108.5(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 Pd 122.01(19) . . ? C13 C12 H12A 106.8 . . ? Pd C12 H12A 106.8 . . ? C13 C12 H12B 106.8 . . ? Pd C12 H12B 106.8 . . ? H12A C12 H12B 106.7 . . ? C16 C13 C15 110.1(2) . . ? C16 C13 C12 110.9(2) . . ? C15 C13 C12 113.3(2) . . ? C16 C13 C14 107.7(2) . . ? C15 C13 C14 107.5(2) . . ? C12 C13 C14 107.2(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? #===END # Attachment 'mar606.cif' data_mar606 _database_code_depnum_ccdc_archive 'CCDC 633697' _audit_creation_date 2006-03-03T15:28:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H94 Cl2 N4 Pd2, 2(C4 H10 O)' _chemical_formula_sum 'C72 H114 Cl2 N4 O2 Pd2' _chemical_formula_weight 1351.37 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.4708(6) _cell_length_b 17.9840(7) _cell_length_c 19.0590(5) _cell_angle_alpha 90 _cell_angle_beta 106.288(2) _cell_angle_gamma 90 _cell_volume 7392.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15174 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8357 _exptl_absorpt_correction_T_max 0.9244 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.335063E-1 _diffrn_orient_matrix_ub_12 -0.199758E-1 _diffrn_orient_matrix_ub_13 0.420605E-1 _diffrn_orient_matrix_ub_21 0.306006E-1 _diffrn_orient_matrix_ub_22 0.340447E-1 _diffrn_orient_matrix_ub_23 -0.127222E-1 _diffrn_orient_matrix_ub_31 -0.95106E-2 _diffrn_orient_matrix_ub_32 0.391642E-1 _diffrn_orient_matrix_ub_33 0.325123E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_unetI/netI 0.0632 _diffrn_reflns_number 24839 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 7207 _reflns_number_gt 5451 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0783P)^2^+50.0248P] 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 7207 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 0.774 _refine_ls_restrained_S_all 0.774 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.946 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' O O 0.0106 0.006 '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 Pd Pd 0.071025(11) 0.621086(15) 0.220905(13) 0.01959(10) Uani 1 1 d . . . Cl1 Cl 0 0.71484(7) 0.25 0.0249(3) Uani 1 2 d S . . Cl2 Cl 0 0.53623(7) 0.25 0.0283(3) Uani 1 2 d S . . N1 N 0.10480(14) 0.70638(17) 0.10597(15) 0.0238(7) Uani 1 1 d . . . N2 N 0.15062(14) 0.75716(18) 0.20901(16) 0.0252(7) Uani 1 1 d . . . C1 C 0.11644(15) 0.6957(2) 0.17970(19) 0.0209(7) Uani 1 1 d . . . C2 C 0.12859(19) 0.7734(2) 0.0904(2) 0.0327(9) Uani 1 1 d . . . H2 H 0.1251 0.7932 0.0433 0.039 Uiso 1 1 calc R . . C3 C 0.15736(19) 0.8048(2) 0.1544(2) 0.0342(9) Uani 1 1 d . . . H3 H 0.1785 0.8511 0.1614 0.041 Uiso 1 1 calc R . . C4 C 0.07627(17) 0.6533(2) 0.04955(18) 0.0253(8) Uani 1 1 d . . . C5 C 0.11542(18) 0.6076(2) 0.0221(2) 0.0305(9) Uani 1 1 d . . . C6 C 0.0876(2) 0.5603(3) -0.0348(2) 0.0402(10) Uani 1 1 d . . . H6 H 0.1129 0.5286 -0.0543 0.048 Uiso 1 1 calc R . . C7 C 0.0240(2) 0.5579(3) -0.0640(2) 0.0444(11) Uani 1 1 d . . . H7 H 0.006 0.525 -0.1032 0.053 Uiso 1 1 calc R . . C8 C -0.0134(2) 0.6031(3) -0.0363(2) 0.0407(11) Uani 1 1 d . . . H8 H -0.0571 0.6009 -0.0567 0.049 Uiso 1 1 calc R . . C9 C 0.01167(18) 0.6526(2) 0.0214(2) 0.0295(9) Uani 1 1 d . . . C10 C 0.1860(2) 0.6106(2) 0.0507(2) 0.0377(10) Uani 1 1 d . . . H10 H 0.197 0.6351 0.0997 0.045 Uiso 1 1 calc R . . C11 C 0.2160(2) 0.5340(3) 0.0598(3) 0.0499(12) Uani 1 1 d . . . H11A H 0.2611 0.5393 0.0785 0.075 Uiso 1 1 calc R . . H11B H 0.2056 0.5087 0.0124 0.075 Uiso 1 1 calc R . . H11C H 0.2005 0.5048 0.0944 0.075 Uiso 1 1 calc R . . C12 C 0.2134(2) 0.6574(3) 0.0002(3) 0.0549(13) Uani 1 1 d . . . H12A H 0.2587 0.6588 0.0197 0.082 Uiso 1 1 calc R . . H12B H 0.1969 0.7081 -0.0026 0.082 Uiso 1 1 calc R . . H12C H 0.2022 0.6353 -0.0487 0.082 Uiso 1 1 calc R . . C13 C -0.03002(18) 0.7046(2) 0.0481(2) 0.0336(9) Uani 1 1 d . . . H13 H -0.0049 0.7272 0.0951 0.04 Uiso 1 1 calc R . . C14 C -0.0850(2) 0.6640(3) 0.0634(3) 0.0468(12) Uani 1 1 d . . . H14A H -0.1106 0.6996 0.0809 0.07 Uiso 1 1 calc R . . H14B H -0.0696 0.6258 0.1008 0.07 Uiso 1 1 calc R . . H14C H -0.1099 0.6405 0.0183 0.07 Uiso 1 1 calc R . . C15 C -0.0517(2) 0.7678(3) -0.0074(3) 0.0558(14) Uani 1 1 d . . . H15A H -0.0786 0.8017 0.0101 0.084 Uiso 1 1 calc R . . H15B H -0.0749 0.7469 -0.0547 0.084 Uiso 1 1 calc R . . H15C H -0.0156 0.7951 -0.0131 0.084 Uiso 1 1 calc R . . C16 C 0.18243(17) 0.7717(2) 0.2852(2) 0.0282(8) Uani 1 1 d . . . C17 C 0.15946(17) 0.8280(2) 0.3216(2) 0.0293(9) Uani 1 1 d . . . C18 C 0.1940(2) 0.8457(3) 0.3926(2) 0.0410(11) Uani 1 1 d . . . H18 H 0.1798 0.8835 0.4187 0.049 Uiso 1 1 calc R . . C19 C 0.2488(2) 0.8089(3) 0.4253(3) 0.0514(13) Uani 1 1 d . . . H19 H 0.2716 0.8214 0.4739 0.062 Uiso 1 1 calc R . . C20 C 0.2702(2) 0.7550(3) 0.3886(2) 0.0459(12) Uani 1 1 d . . . H20 H 0.3078 0.7302 0.4124 0.055 Uiso 1 1 calc R . . C21 C 0.23878(18) 0.7350(2) 0.3169(2) 0.0357(10) Uani 1 1 d . . . C22 C 0.10057(18) 0.8714(2) 0.2872(2) 0.0328(9) Uani 1 1 d . . . H22 H 0.0765 0.8438 0.2427 0.039 Uiso 1 1 calc R . . C23 C 0.0597(2) 0.8783(2) 0.3395(2) 0.0404(10) Uani 1 1 d . . . H23A H 0.022 0.9061 0.3155 0.061 Uiso 1 1 calc R . . H23B H 0.0826 0.9046 0.3839 0.061 Uiso 1 1 calc R . . H23C H 0.0484 0.8286 0.3525 0.061 Uiso 1 1 calc R . . C24 C 0.1161(2) 0.9489(3) 0.2632(3) 0.0463(11) Uani 1 1 d . . . H24A H 0.0775 0.9759 0.2408 0.069 Uiso 1 1 calc R . . H24B H 0.1399 0.9437 0.2275 0.069 Uiso 1 1 calc R . . H24C H 0.1407 0.9764 0.3058 0.069 Uiso 1 1 calc R . . C25 C 0.2670(2) 0.6801(3) 0.2751(3) 0.0448(11) Uani 1 1 d . . . H25 H 0.2326 0.6482 0.2454 0.054 Uiso 1 1 calc R . . C26 C 0.2970(2) 0.7185(3) 0.2224(3) 0.0629(15) Uani 1 1 d . . . H26A H 0.3143 0.681 0.1963 0.094 Uiso 1 1 calc R . . H26B H 0.3303 0.7513 0.2498 0.094 Uiso 1 1 calc R . . H26C H 0.2658 0.748 0.1871 0.094 Uiso 1 1 calc R . . C27 C 0.3152(2) 0.6285(3) 0.3250(4) 0.0679(18) Uani 1 1 d . . . H27A H 0.3314 0.594 0.295 0.102 Uiso 1 1 calc R . . H27B H 0.2956 0.6002 0.3565 0.102 Uiso 1 1 calc R . . H27C H 0.3493 0.6583 0.3554 0.102 Uiso 1 1 calc R . . C28 C 0.12625(16) 0.5388(2) 0.1984(2) 0.0249(8) Uani 1 1 d . . . H28A H 0.1011 0.5097 0.1564 0.03 Uiso 1 1 calc R . . H28B H 0.1599 0.5628 0.1825 0.03 Uiso 1 1 calc R . . C29 C 0.15626(19) 0.4836(3) 0.2605(2) 0.0389(10) Uani 1 1 d . . . C30 C 0.1732(2) 0.5231(3) 0.3347(2) 0.0551(14) Uani 1 1 d . . . H30A H 0.1997 0.566 0.3332 0.083 Uiso 1 1 calc R . . H30B H 0.1953 0.4885 0.3728 0.083 Uiso 1 1 calc R . . H30C H 0.1352 0.5401 0.3455 0.083 Uiso 1 1 calc R . . C31 C 0.2164(2) 0.4547(3) 0.2467(3) 0.0544(14) Uani 1 1 d . . . H31A H 0.244 0.4967 0.2457 0.082 Uiso 1 1 calc R . . H31B H 0.2066 0.4286 0.1997 0.082 Uiso 1 1 calc R . . H31C H 0.2371 0.4204 0.286 0.082 Uiso 1 1 calc R . . C32 C 0.1151(2) 0.4163(3) 0.2619(3) 0.0598(15) Uani 1 1 d . . . H32A H 0.1361 0.3834 0.3023 0.09 Uiso 1 1 calc R . . H32B H 0.1073 0.3893 0.2156 0.09 Uiso 1 1 calc R . . H32C H 0.0757 0.4331 0.2689 0.09 Uiso 1 1 calc R . . O O 0.0793(3) 0.8595(2) -0.0699(2) 0.0899(15) Uani 1 1 d . A 1 C33 C 0.0692(7) 0.9353(4) -0.0631(6) 0.164(5) Uani 1 1 d . A 1 H33A H 0.0242 0.9445 -0.0721 0.197 Uiso 1 1 calc R A 1 H33B H 0.0834 0.9631 -0.1002 0.197 Uiso 1 1 calc R A 1 C34 C 0.1027(7) 0.9624(5) 0.0107(6) 0.187(6) Uani 1 1 d . A 1 H34A H 0.0947 1.0157 0.0142 0.281 Uiso 1 1 calc R A 1 H34B H 0.1473 0.9542 0.0193 0.281 Uiso 1 1 calc R A 1 H34C H 0.0882 0.9353 0.0474 0.281 Uiso 1 1 calc R A 1 C35 C 0.0494(4) 0.8297(4) -0.1395(4) 0.096(2) Uani 1 1 d . A 1 H35A H 0.0635 0.8562 -0.1774 0.116 Uiso 1 1 calc R A 1 H35B H 0.004 0.8368 -0.1501 0.116 Uiso 1 1 calc R A 1 C36 C 0.0633(4) 0.7504(4) -0.1413(3) 0.090(2) Uani 1 1 d . A 1 H36A H 0.042 0.7301 -0.1895 0.135 Uiso 1 1 calc R A 1 H36B H 0.0492 0.7243 -0.1037 0.135 Uiso 1 1 calc R A 1 H36C H 0.1082 0.7436 -0.1318 0.135 Uiso 1 1 calc R A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01779(15) 0.01872(16) 0.02242(15) 0.00091(11) 0.00589(10) 0.00001(11) Cl1 0.0235(6) 0.0194(6) 0.0336(7) 0 0.0110(5) 0 Cl2 0.0280(7) 0.0199(6) 0.0430(7) 0 0.0194(6) 0 N1 0.0259(16) 0.0233(17) 0.0220(15) 0.0015(12) 0.0064(12) -0.0033(13) N2 0.0242(16) 0.0248(17) 0.0251(15) -0.0007(13) 0.0043(12) -0.0048(13) C1 0.0157(16) 0.0207(19) 0.0264(18) -0.0023(14) 0.0058(14) 0.0016(14) C2 0.044(2) 0.024(2) 0.030(2) 0.0026(16) 0.0103(17) -0.0067(18) C3 0.043(2) 0.024(2) 0.037(2) -0.0005(17) 0.0123(18) -0.0112(18) C4 0.033(2) 0.0232(19) 0.0192(17) 0.0010(15) 0.0064(15) -0.0039(16) C5 0.034(2) 0.030(2) 0.030(2) 0.0010(16) 0.0132(16) -0.0080(17) C6 0.049(3) 0.040(3) 0.037(2) -0.0105(19) 0.022(2) -0.005(2) C7 0.047(3) 0.048(3) 0.038(2) -0.021(2) 0.012(2) -0.015(2) C8 0.033(2) 0.052(3) 0.034(2) -0.012(2) 0.0049(18) -0.014(2) C9 0.029(2) 0.033(2) 0.0259(19) 0.0022(16) 0.0058(16) -0.0030(17) C10 0.035(2) 0.041(3) 0.041(2) -0.0046(19) 0.0162(18) 0.0000(19) C11 0.049(3) 0.055(3) 0.050(3) 0.003(2) 0.022(2) 0.012(2) C12 0.043(3) 0.051(3) 0.079(4) -0.001(3) 0.030(3) -0.008(2) C13 0.029(2) 0.038(2) 0.030(2) -0.0018(18) 0.0032(16) -0.0014(18) C14 0.033(2) 0.060(3) 0.045(3) -0.006(2) 0.007(2) -0.005(2) C15 0.057(3) 0.056(3) 0.047(3) 0.006(2) 0.004(2) 0.015(3) C16 0.0247(19) 0.030(2) 0.0260(19) -0.0034(16) 0.0010(15) -0.0067(16) C17 0.0265(19) 0.029(2) 0.030(2) 0.0003(16) 0.0050(16) -0.0081(17) C18 0.037(2) 0.046(3) 0.039(2) -0.016(2) 0.0097(19) -0.011(2) C19 0.044(3) 0.066(4) 0.036(2) -0.007(2) -0.002(2) -0.011(3) C20 0.030(2) 0.050(3) 0.046(3) 0.002(2) -0.0087(19) -0.005(2) C21 0.026(2) 0.032(2) 0.044(2) -0.0006(19) 0.0013(17) -0.0056(18) C22 0.030(2) 0.028(2) 0.039(2) -0.0070(18) 0.0084(17) -0.0063(18) C23 0.041(2) 0.034(2) 0.050(3) -0.016(2) 0.018(2) -0.007(2) C24 0.040(3) 0.032(3) 0.067(3) 0.003(2) 0.015(2) -0.003(2) C25 0.029(2) 0.042(3) 0.057(3) -0.012(2) 0.000(2) -0.001(2) C26 0.047(3) 0.058(4) 0.091(4) -0.019(3) 0.032(3) -0.006(3) C27 0.035(3) 0.046(3) 0.107(5) -0.017(3) -0.006(3) 0.009(2) C28 0.0222(18) 0.022(2) 0.0314(19) 0.0013(15) 0.0084(15) -0.0008(15) C29 0.032(2) 0.038(3) 0.052(3) 0.015(2) 0.0208(19) 0.0135(19) C30 0.045(3) 0.079(4) 0.041(3) 0.023(3) 0.012(2) 0.018(3) C31 0.048(3) 0.053(3) 0.072(3) 0.029(3) 0.032(3) 0.027(2) C32 0.056(3) 0.036(3) 0.100(4) 0.030(3) 0.044(3) 0.019(2) O 0.153(5) 0.056(3) 0.071(3) 0.021(2) 0.048(3) 0.008(3) C33 0.332(17) 0.052(5) 0.123(8) 0.039(5) 0.089(10) 0.043(7) C34 0.38(2) 0.055(5) 0.121(8) 0.001(5) 0.063(11) -0.003(8) C35 0.142(7) 0.092(6) 0.062(4) 0.034(4) 0.039(4) 0.034(5) C36 0.131(6) 0.085(5) 0.060(4) 0.010(3) 0.038(4) 0.012(5) #----------------------------------------------------------------------------# # 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 Pd C1 1.977(4) . ? Pd C28 2.053(4) . ? Pd Cl2 2.3832(9) . ? Pd Cl1 2.4887(9) . ? Cl1 Pd 2.4887(9) 2 ? Cl2 Pd 2.3832(9) 2 ? N1 C1 1.369(4) . ? N1 C2 1.383(5) . ? N1 C4 1.446(5) . ? N2 C1 1.373(5) . ? N2 C3 1.388(5) . ? N2 C16 1.452(4) . ? C2 C3 1.336(5) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C9 1.399(5) . ? C4 C5 1.407(6) . ? C5 C6 1.383(6) . ? C5 C10 1.526(6) . ? C6 C7 1.382(6) . ? C6 H6 0.95 . ? C7 C8 1.376(6) . ? C7 H7 0.95 . ? C8 C9 1.404(6) . ? C8 H8 0.95 . ? C9 C13 1.509(6) . ? C10 C11 1.521(6) . ? C10 C12 1.532(6) . ? C10 H10 1 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.532(6) . ? C13 C15 1.536(6) . ? C13 H13 1 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C21 1.405(5) . ? C16 C17 1.405(6) . ? C17 C18 1.394(5) . ? C17 C22 1.517(6) . ? C18 C19 1.382(7) . ? C18 H18 0.95 . ? C19 C20 1.361(7) . ? C19 H19 0.95 . ? C20 C21 1.398(6) . ? C20 H20 0.95 . ? C21 C25 1.515(6) . ? C22 C24 1.538(6) . ? C22 C23 1.539(6) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.525(7) . ? C25 C27 1.537(7) . ? C25 H25 1 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.546(5) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C32 1.527(7) . ? C29 C30 1.532(7) . ? C29 C31 1.538(6) . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? O C33 1.394(9) . ? O C35 1.413(8) . ? C33 C34 1.479(13) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.464(10) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? 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 C1 Pd C28 89.81(14) . . ? C1 Pd Cl2 168.82(10) . . ? C28 Pd Cl2 94.03(11) . . ? C1 Pd Cl1 93.65(10) . . ? C28 Pd Cl1 176.49(10) . . ? Cl2 Pd Cl1 82.46(3) . . ? Pd Cl1 Pd 94.71(4) . 2 ? Pd Cl2 Pd 100.37(5) . 2 ? C1 N1 C2 111.6(3) . . ? C1 N1 C4 126.0(3) . . ? C2 N1 C4 122.2(3) . . ? C1 N2 C3 111.0(3) . . ? C1 N2 C16 127.9(3) . . ? C3 N2 C16 120.8(3) . . ? N1 C1 N2 103.2(3) . . ? N1 C1 Pd 122.1(2) . . ? N2 C1 Pd 132.6(3) . . ? C3 C2 N1 106.9(3) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 107.3(3) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C9 C4 C5 122.8(3) . . ? C9 C4 N1 119.1(3) . . ? C5 C4 N1 117.9(3) . . ? C6 C5 C4 117.3(4) . . ? C6 C5 C10 119.8(4) . . ? C4 C5 C10 122.8(3) . . ? C7 C6 C5 121.6(4) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7 120 . . ? C6 C7 H7 120 . . ? C7 C8 C9 121.4(4) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C4 C9 C8 116.8(4) . . ? C4 C9 C13 122.7(3) . . ? C8 C9 C13 120.4(4) . . ? C11 C10 C5 113.0(4) . . ? C11 C10 C12 109.0(4) . . ? C5 C10 C12 110.9(4) . . ? C11 C10 H10 107.9 . . ? C5 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 112.2(4) . . ? C9 C13 C15 109.5(4) . . ? C14 C13 C15 111.5(4) . . ? C9 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.5(3) . . ? C21 C16 N2 118.5(4) . . ? C17 C16 N2 118.5(3) . . ? C18 C17 C16 117.5(4) . . ? C18 C17 C22 118.9(4) . . ? C16 C17 C22 123.6(3) . . ? C19 C18 C17 120.8(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.5(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 122.1(4) . . ? C19 C20 H20 119 . . ? C21 C20 H20 119 . . ? C20 C21 C16 116.5(4) . . ? C20 C21 C25 120.7(4) . . ? C16 C21 C25 122.6(4) . . ? C17 C22 C24 110.6(3) . . ? C17 C22 C23 111.6(4) . . ? C24 C22 C23 110.2(4) . . ? C17 C22 H22 108.1 . . ? C24 C22 H22 108.1 . . ? C23 C22 H22 108.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 112.2(4) . . ? C21 C25 C27 113.2(4) . . ? C26 C25 C27 108.4(4) . . ? C21 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 Pd 117.6(3) . . ? C29 C28 H28A 107.9 . . ? Pd C28 H28A 107.9 . . ? C29 C28 H28B 107.9 . . ? Pd C28 H28B 107.9 . . ? H28A C28 H28B 107.2 . . ? C32 C29 C30 110.2(4) . . ? C32 C29 C31 107.5(4) . . ? C30 C29 C31 108.2(4) . . ? C32 C29 C28 112.7(4) . . ? C30 C29 C28 110.5(4) . . ? C31 C29 C28 107.6(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O C35 114.2(6) . . ? O C33 C34 111.0(8) . . ? O C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? O C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O C35 C36 110.0(6) . . ? O C35 H35A 109.7 . . ? C36 C35 H35A 109.7 . . ? O C35 H35B 109.7 . . ? C36 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? #===END # Attachment 'oct406.cif' data_oct406 _database_code_depnum_ccdc_archive 'CCDC 633698' _audit_creation_date 2006-10-06T11:32:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H40 Cl N3 O Pd' _chemical_formula_sum 'C20 H40 Cl N3 O Pd' _chemical_formula_weight 480.4 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.6642(3) _cell_length_b 23.1895(5) _cell_length_c 10.4673(3) _cell_angle_alpha 90 _cell_angle_beta 95.324(1) _cell_angle_gamma 90 _cell_volume 2335.69(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18355 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.9978 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.209329E-1 _diffrn_orient_matrix_ub_12 -0.374554E-1 _diffrn_orient_matrix_ub_13 0.450499E-1 _diffrn_orient_matrix_ub_21 0.326795E-1 _diffrn_orient_matrix_ub_22 0.213514E-1 _diffrn_orient_matrix_ub_23 0.801752E-1 _diffrn_orient_matrix_ub_31 -0.964046E-1 _diffrn_orient_matrix_ub_32 -0.8951E-3 _diffrn_orient_matrix_ub_33 0.273633E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_unetI/netI 0.0623 _diffrn_reflns_number 21525 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 4570 _reflns_number_gt 3366 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C16 neopentyl group is disordered over two resolved orientations which were included with isotropic C atoms, and restrained to have similar geometries using the SAME instruction . 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^)+(0.0748P)^2^+11.7021P] 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 4570 _refine_ls_number_parameters 243 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.108 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.82 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.902 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 Pd Pd 0.21753(4) 0.189087(15) 0.83447(3) 0.02354(14) Uani 1 1 d . . . Cl Cl 0.10609(15) 0.23765(6) 0.64010(13) 0.0403(3) Uani 1 1 d . A . O O 0.3808(5) 0.38746(16) 0.8609(4) 0.0442(10) Uani 1 1 d . . . N1 N 0.1476(4) 0.07097(17) 0.7197(4) 0.0290(9) Uani 1 1 d . . . N2 N -0.0197(5) 0.10355(18) 0.8244(4) 0.0313(10) Uani 1 1 d . . . N3 N 0.3268(4) 0.26556(16) 0.8934(4) 0.0248(9) Uani 1 1 d . A . H3X H 0.3855 0.2568 0.9662 0.03 Uiso 1 1 calc R . . C1 C 0.1097(5) 0.1179(2) 0.7885(4) 0.0256(11) Uani 1 1 d . A . C2 C 0.0465(7) 0.0282(2) 0.7206(6) 0.0446(15) Uani 1 1 d . A . H2 H 0.0505 -0.0091 0.6835 0.054 Uiso 1 1 calc R . . C3 C -0.0554(7) 0.0488(2) 0.7824(6) 0.0434(15) Uani 1 1 d . A . H3 H -0.1392 0.0292 0.7957 0.052 Uiso 1 1 calc R . . C4 C 0.2702(6) 0.0620(2) 0.6448(5) 0.0349(12) Uani 1 1 d . A . C5 C 0.2159(7) 0.0407(3) 0.5111(6) 0.0485(16) Uani 1 1 d . . . H5A H 0.1677 0.0039 0.5186 0.073 Uiso 1 1 calc R A . H5B H 0.2941 0.0355 0.4589 0.073 Uiso 1 1 calc R . . H5C H 0.1512 0.0692 0.4702 0.073 Uiso 1 1 calc R . . C6 C 0.3641(7) 0.0159(3) 0.7122(6) 0.0496(16) Uani 1 1 d . . . H6A H 0.3098 -0.0191 0.7233 0.074 Uiso 1 1 calc R A . H6B H 0.4019 0.0303 0.7964 0.074 Uiso 1 1 calc R . . H6C H 0.4405 0.0072 0.6601 0.074 Uiso 1 1 calc R . . C7 C 0.3513(6) 0.1171(3) 0.6285(6) 0.0437(14) Uani 1 1 d . . . H7A H 0.3892 0.1312 0.7128 0.065 Uiso 1 1 calc R A . H7B H 0.2895 0.1463 0.5866 0.065 Uiso 1 1 calc R . . H7C H 0.4276 0.1093 0.5754 0.065 Uiso 1 1 calc R . . C8 C -0.1239(6) 0.1394(3) 0.8897(5) 0.0371(13) Uani 1 1 d . A . C9 C -0.1685(8) 0.1050(3) 1.0036(7) 0.0594(18) Uani 1 1 d . . . H9A H -0.2172 0.07 0.9725 0.089 Uiso 1 1 calc R A . H9B H -0.2306 0.1286 1.0509 0.089 Uiso 1 1 calc R . . H9C H -0.0862 0.0945 1.0606 0.089 Uiso 1 1 calc R . . C10 C -0.2470(8) 0.1510(4) 0.7914(7) 0.080(3) Uani 1 1 d . . . H10A H -0.2842 0.1143 0.7568 0.12 Uiso 1 1 calc R A . H10B H -0.2165 0.1746 0.7215 0.12 Uiso 1 1 calc R . . H10C H -0.3194 0.1716 0.8327 0.12 Uiso 1 1 calc R . . C11 C -0.0676(7) 0.1973(3) 0.9370(7) 0.0524(17) Uani 1 1 d . . . H11A H 0.013 0.1913 0.9996 0.079 Uiso 1 1 calc R A . H11B H -0.1398 0.2183 0.9775 0.079 Uiso 1 1 calc R . . H11C H -0.0394 0.2197 0.8643 0.079 Uiso 1 1 calc R . . C12 C 0.4139(6) 0.2880(2) 0.7948(5) 0.0341(12) Uani 1 1 d . . . H12A H 0.3556 0.2929 0.7126 0.041 Uiso 1 1 calc R A . H12B H 0.4876 0.2596 0.7809 0.041 Uiso 1 1 calc R . . C13 C 0.4806(6) 0.3455(2) 0.8351(5) 0.0404(14) Uani 1 1 d . A . H13A H 0.5456 0.3397 0.9129 0.049 Uiso 1 1 calc R . . H13B H 0.535 0.3597 0.766 0.049 Uiso 1 1 calc R . . C14 C 0.2312(6) 0.3118(2) 0.9280(5) 0.0312(11) Uani 1 1 d . . . H14A H 0.1817 0.2987 1.0014 0.037 Uiso 1 1 calc R A . H14B H 0.1609 0.3187 0.8546 0.037 Uiso 1 1 calc R . . C15 C 0.3055(7) 0.3678(2) 0.9633(6) 0.0416(14) Uani 1 1 d . A . H15A H 0.2367 0.3975 0.9829 0.05 Uiso 1 1 calc R . . H15B H 0.3704 0.362 1.0412 0.05 Uiso 1 1 calc R . . C16 C 0.3575(6) 0.1443(3) 0.9594(6) 0.0239(15) Uiso 0.757(7) 1 d PD A 1 H16A H 0.3757 0.1073 0.9169 0.029 Uiso 0.757(7) 1 calc PR A 1 H16B H 0.4457 0.1663 0.9644 0.029 Uiso 0.757(7) 1 calc PR A 1 C17 C 0.3309(7) 0.1294(3) 1.0993(7) 0.0275(18) Uiso 0.757(7) 1 d PD A 1 C18 C 0.2213(7) 0.0818(3) 1.1006(7) 0.0364(18) Uiso 0.757(7) 1 d PD A 1 H18A H 0.2478 0.0493 1.0484 0.055 Uiso 0.757(7) 1 calc PR A 1 H18B H 0.131 0.0968 1.0654 0.055 Uiso 0.757(7) 1 calc PR A 1 H18C H 0.215 0.0689 1.189 0.055 Uiso 0.757(7) 1 calc PR A 1 C19 C 0.4691(8) 0.1049(3) 1.1640(8) 0.042(2) Uiso 0.757(7) 1 d PD A 1 H19A H 0.4946 0.0702 1.1184 0.064 Uiso 0.757(7) 1 calc PR A 1 H19B H 0.4576 0.0952 1.2536 0.064 Uiso 0.757(7) 1 calc PR A 1 H19C H 0.5425 0.1339 1.1611 0.064 Uiso 0.757(7) 1 calc PR A 1 C20 C 0.2918(7) 0.1817(3) 1.1733(7) 0.0339(17) Uiso 0.757(7) 1 d PD A 1 H20A H 0.3666 0.2103 1.1747 0.051 Uiso 0.757(7) 1 calc PR A 1 H20B H 0.2777 0.1705 1.2614 0.051 Uiso 0.757(7) 1 calc PR A 1 H20C H 0.2058 0.1984 1.132 0.051 Uiso 0.757(7) 1 calc PR A 1 C16A C 0.2423(18) 0.1626(7) 1.0279(18) 0.025(5) Uiso 0.243(7) 1 d PD A 2 H16C H 0.268 0.1974 1.0796 0.029 Uiso 0.243(7) 1 calc PR A 2 H16D H 0.1495 0.1505 1.0506 0.029 Uiso 0.243(7) 1 calc PR A 2 C17A C 0.3458(17) 0.1142(7) 1.0765(16) 0.019(5) Uiso 0.243(7) 1 d PD A 2 C18A C 0.273(2) 0.0558(8) 1.055(2) 0.031(5) Uiso 0.243(7) 1 d PD A 2 H18D H 0.1741 0.06 1.0685 0.046 Uiso 0.243(7) 1 calc PR A 2 H18E H 0.3159 0.0275 1.1158 0.046 Uiso 0.243(7) 1 calc PR A 2 H18F H 0.2812 0.0427 0.9671 0.046 Uiso 0.243(7) 1 calc PR A 2 C19A C 0.374(2) 0.1222(9) 1.2234(16) 0.038(6) Uiso 0.243(7) 1 d PD A 2 H19D H 0.2864 0.1198 1.263 0.057 Uiso 0.243(7) 1 calc PR A 2 H19E H 0.4167 0.1601 1.2416 0.057 Uiso 0.243(7) 1 calc PR A 2 H19F H 0.4373 0.0919 1.2585 0.057 Uiso 0.243(7) 1 calc PR A 2 C20A C 0.4797(19) 0.1167(9) 1.016(2) 0.036(6) Uiso 0.243(7) 1 d PD A 2 H20D H 0.4626 0.1082 0.9245 0.054 Uiso 0.243(7) 1 calc PR A 2 H20E H 0.5443 0.0881 1.057 0.054 Uiso 0.243(7) 1 calc PR A 2 H20F H 0.52 0.1553 1.0279 0.054 Uiso 0.243(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0305(2) 0.01686(19) 0.0220(2) 0.00050(15) -0.00448(14) -0.00174(17) Cl 0.0500(8) 0.0335(7) 0.0333(7) 0.0055(5) -0.0183(6) -0.0035(6) O 0.065(3) 0.026(2) 0.042(2) 0.0048(17) 0.006(2) -0.0075(19) N1 0.033(2) 0.020(2) 0.032(2) -0.0044(17) -0.0050(18) 0.0003(18) N2 0.033(2) 0.029(2) 0.032(2) -0.0003(18) 0.0018(19) -0.0033(19) N3 0.030(2) 0.022(2) 0.021(2) 0.0037(16) -0.0042(17) -0.0033(17) C1 0.033(3) 0.021(2) 0.021(2) -0.0001(19) -0.005(2) 0.000(2) C2 0.058(4) 0.022(3) 0.051(4) -0.010(3) -0.006(3) -0.008(3) C3 0.050(4) 0.028(3) 0.050(4) -0.002(3) -0.005(3) -0.018(3) C4 0.045(3) 0.027(3) 0.032(3) -0.006(2) -0.001(2) 0.011(2) C5 0.065(4) 0.039(3) 0.040(3) -0.008(3) -0.003(3) 0.014(3) C6 0.054(4) 0.043(3) 0.049(4) -0.008(3) -0.009(3) 0.019(3) C7 0.046(4) 0.045(3) 0.042(3) -0.003(3) 0.014(3) 0.005(3) C8 0.033(3) 0.054(3) 0.024(3) -0.002(2) 0.002(2) 0.001(3) C9 0.070(5) 0.063(4) 0.049(4) 0.006(3) 0.026(4) -0.013(4) C10 0.052(4) 0.130(8) 0.055(5) -0.028(5) -0.014(4) 0.039(5) C11 0.059(4) 0.047(4) 0.055(4) -0.008(3) 0.029(3) -0.003(3) C12 0.034(3) 0.036(3) 0.033(3) 0.003(2) 0.004(2) -0.005(2) C13 0.046(3) 0.042(3) 0.033(3) 0.006(2) 0.003(3) -0.018(3) C14 0.043(3) 0.019(2) 0.032(3) -0.004(2) 0.006(2) 0.000(2) C15 0.062(4) 0.025(3) 0.039(3) -0.009(2) 0.010(3) -0.007(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 Pd C1 1.988(5) . ? Pd C16 2.072(6) . ? Pd C16A 2.109(18) . ? Pd N3 2.126(4) . ? Pd Cl 2.4821(13) . ? O C13 1.413(7) . ? O C15 1.425(7) . ? N1 C1 1.373(6) . ? N1 C2 1.393(7) . ? N1 C4 1.495(7) . ? N2 C3 1.378(7) . ? N2 C1 1.379(7) . ? N2 C8 1.517(7) . ? N3 C14 1.482(6) . ? N3 C12 1.485(6) . ? N3 H3X 0.93 . ? C2 C3 1.317(9) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C7 1.516(8) . ? C4 C5 1.530(8) . ? C4 C6 1.531(7) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C11 1.515(8) . ? C8 C10 1.522(8) . ? C8 C9 1.529(8) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C13 1.525(7) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.514(7) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.549(9) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C20 1.507(10) . ? C17 C18 1.530(9) . ? C17 C19 1.548(10) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C16A C17A 1.556(16) . ? C16A H16C 0.99 . ? C16A H16D 0.99 . ? C17A C20A 1.492(17) . ? C17A C18A 1.535(17) . ? C17A C19A 1.548(17) . ? C18A H18D 0.98 . ? C18A H18E 0.98 . ? C18A H18F 0.98 . ? C19A H19D 0.98 . ? C19A H19E 0.98 . ? C19A H19F 0.98 . ? C20A H20D 0.98 . ? C20A H20E 0.98 . ? C20A H20F 0.98 . ? 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 C1 Pd C16 91.9(2) . . ? C1 Pd C16A 90.0(5) . . ? C16 Pd C16A 40.4(5) . . ? C1 Pd N3 176.70(18) . . ? C16 Pd N3 87.6(2) . . ? C16A Pd N3 87.5(5) . . ? C1 Pd Cl 90.03(14) . . ? C16 Pd Cl 162.41(18) . . ? C16A Pd Cl 157.2(5) . . ? N3 Pd Cl 91.45(11) . . ? C13 O C15 109.2(4) . . ? C1 N1 C2 109.8(4) . . ? C1 N1 C4 130.4(4) . . ? C2 N1 C4 119.7(4) . . ? C3 N2 C1 110.0(5) . . ? C3 N2 C8 119.4(5) . . ? C1 N2 C8 130.4(4) . . ? C14 N3 C12 108.9(4) . . ? C14 N3 Pd 111.7(3) . . ? C12 N3 Pd 112.9(3) . . ? C14 N3 H3X 107.7 . . ? C12 N3 H3X 107.7 . . ? Pd N3 H3X 107.7 . . ? N1 C1 N2 104.2(4) . . ? N1 C1 Pd 128.7(4) . . ? N2 C1 Pd 127.0(4) . . ? C3 C2 N1 107.6(5) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C2 C3 N2 108.3(5) . . ? C2 C3 H3 125.8 . . ? N2 C3 H3 125.8 . . ? N1 C4 C7 112.7(4) . . ? N1 C4 C5 107.6(5) . . ? C7 C4 C5 107.8(5) . . ? N1 C4 C6 108.6(5) . . ? C7 C4 C6 110.5(5) . . ? C5 C4 C6 109.5(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C8 N2 113.5(5) . . ? C11 C8 C10 107.4(6) . . ? N2 C8 C10 107.6(5) . . ? C11 C8 C9 109.0(5) . . ? N2 C8 C9 108.3(5) . . ? C10 C8 C9 111.1(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 111.5(4) . . ? N3 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N3 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108 . . ? O C13 C12 112.1(5) . . ? O C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? O C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N3 C14 C15 112.9(4) . . ? N3 C14 H14A 109 . . ? C15 C14 H14A 109 . . ? N3 C14 H14B 109 . . ? C15 C14 H14B 109 . . ? H14A C14 H14B 107.8 . . ? O C15 C14 110.8(4) . . ? O C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? O C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 Pd 123.5(4) . . ? C17 C16 H16A 106.4 . . ? Pd C16 H16A 106.4 . . ? C17 C16 H16B 106.4 . . ? Pd C16 H16B 106.4 . . ? H16A C16 H16B 106.5 . . ? C20 C17 C18 111.7(6) . . ? C20 C17 C19 108.5(6) . . ? C18 C17 C19 107.6(6) . . ? C20 C17 C16 112.2(6) . . ? C18 C17 C16 110.2(6) . . ? C19 C17 C16 106.4(6) . . ? C17A C16A Pd 122.4(12) . . ? C17A C16A H16C 106.7 . . ? Pd C16A H16C 106.7 . . ? C17A C16A H16D 106.7 . . ? Pd C16A H16D 106.7 . . ? H16C C16A H16D 106.6 . . ? C20A C17A C18A 112.2(15) . . ? C20A C17A C19A 109.6(14) . . ? C18A C17A C19A 106.7(14) . . ? C20A C17A C16A 113.0(14) . . ? C18A C17A C16A 108.3(13) . . ? C19A C17A C16A 106.7(14) . . ? C17A C18A H18D 109.5 . . ? C17A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17A C19A H19D 109.5 . . ? C17A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C17A C20A H20D 109.5 . . ? C17A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C17A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? #===END