# 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 _publ_contact_author_name 'Fornies, Juan' _publ_contact_author_email juan.fornies@unizar.es _publ_section_title ; Synthesis and characterization of neutral and anionic carbonyl derivatives of palladium(II) ; _publ_author_name J.Fornies # Attachment '- structures.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 762684' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 F10 O2 Pd' _chemical_formula_weight 584.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2830(6) _cell_length_b 9.5652(6) _cell_length_c 12.7916(8) _cell_angle_alpha 69.7770(10) _cell_angle_beta 74.2530(10) _cell_angle_gamma 83.9940(10) _cell_volume 1025.72(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4323 _cell_measurement_theta_min 2.269 _cell_measurement_theta_max 23.293 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7583 _exptl_absorpt_correction_T_max 0.9327 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'omega rotations' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6830 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.29 _reflns_number_total 2960 _reflns_number_gt 2663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.611' _computing_cell_refinement 'SAINT+ 6.02' _computing_data_reduction 'SAINT+ 6.02' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL 6.10' _computing_publication_material 'XCIF, SHELXTL 6.10' _refine_special_details ; Refinement of F2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2^, conventional R-factors R are based on F, with F set to zero for negative F2^. The threshold expression of F2^ > 2sigma(F2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2^ 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/[\s2^(Fo2^)+(0.0874P)2^+0.0000P] where P=(Fo2^+2Fc2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2960 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.50756(3) 0.99081(3) 0.25025(2) 0.02060(17) Uani 1 1 d . . . F2 F 0.3158(3) 0.8116(3) 0.1661(2) 0.0332(6) Uani 1 1 d . . . F3 F 0.0465(3) 0.6860(3) 0.2682(2) 0.0414(7) Uani 1 1 d . . . F4 F -0.1061(3) 0.6983(3) 0.4778(2) 0.0438(7) Uani 1 1 d . . . F5 F 0.0131(3) 0.8394(3) 0.5848(2) 0.0357(6) Uani 1 1 d . . . F6 F 0.2838(3) 0.9618(3) 0.48698(19) 0.0324(6) Uani 1 1 d . . . F8 F 0.5559(3) 0.7224(3) 0.46682(19) 0.0311(6) Uani 1 1 d . . . F9 F 0.7005(3) 0.4629(3) 0.4814(2) 0.0370(6) Uani 1 1 d . . . F10 F 0.8158(3) 0.3851(3) 0.2896(2) 0.0398(6) Uani 1 1 d . . . F11 F 0.7888(3) 0.5734(3) 0.0820(2) 0.0382(6) Uani 1 1 d . . . F12 F 0.6523(3) 0.8398(3) 0.06400(19) 0.0356(6) Uani 1 1 d . . . O1 O 0.7167(3) 1.1002(3) 0.1801(2) 0.0266(7) Uani 1 1 d . . . O2 O 0.4219(3) 1.2110(3) 0.2250(3) 0.0255(7) Uani 1 1 d . . . C1 C 0.3109(5) 0.8929(4) 0.3215(4) 0.0203(9) Uani 1 1 d . . . C2 C 0.2446(5) 0.8199(4) 0.2715(3) 0.0255(9) Uani 1 1 d . . . C3 C 0.1066(5) 0.7551(4) 0.3218(4) 0.0286(10) Uani 1 1 d . . . C4 C 0.0286(5) 0.7609(5) 0.4278(4) 0.0309(11) Uani 1 1 d . . . C5 C 0.0903(5) 0.8313(5) 0.4815(4) 0.0265(10) Uani 1 1 d . . . C6 C 0.2290(5) 0.8942(4) 0.4289(3) 0.0248(9) Uani 1 1 d . . . C7 C 0.5972(4) 0.7918(4) 0.2659(4) 0.0206(9) Uani 1 1 d . . . C8 C 0.6127(4) 0.6900(5) 0.3682(3) 0.0240(9) Uani 1 1 d . . . C9 C 0.6861(4) 0.5554(4) 0.3788(4) 0.0260(10) Uani 1 1 d . . . C10 C 0.7461(5) 0.5163(5) 0.2813(4) 0.0286(10) Uani 1 1 d . . . C11 C 0.7310(5) 0.6127(5) 0.1774(4) 0.0269(10) Uani 1 1 d . . . C12 C 0.6595(4) 0.7473(5) 0.1702(3) 0.0258(9) Uani 1 1 d . . . C13 C 0.8539(5) 1.0419(5) 0.2124(4) 0.0350(11) Uani 1 1 d . . . H13A H 0.8741 0.9392 0.2101 0.042 Uiso 1 1 calc R . . H13B H 0.8489 1.0412 0.2909 0.042 Uiso 1 1 calc R . . C14 C 0.9728(5) 1.1464(6) 0.1244(4) 0.0435(12) Uani 1 1 d . . . H14A H 1.0699 1.0937 0.1099 0.052 Uiso 1 1 calc R . . H14B H 0.9859 1.2302 0.1495 0.052 Uiso 1 1 calc R . . C15 C 0.9123(6) 1.2004(7) 0.0189(5) 0.0556(16) Uani 1 1 d . . . H15A H 0.9496 1.3012 -0.0309 0.067 Uiso 1 1 calc R . . H15B H 0.9415 1.1316 -0.0262 0.067 Uiso 1 1 calc R . . C16 C 0.7490(6) 1.2031(6) 0.0646(4) 0.0512(14) Uani 1 1 d . . . H16A H 0.7139 1.3046 0.0643 0.061 Uiso 1 1 calc R . . H16B H 0.6982 1.1729 0.0171 0.061 Uiso 1 1 calc R . . C17 C 0.4301(6) 1.2871(5) 0.3026(4) 0.0397(12) Uani 1 1 d . . . H17A H 0.5353 1.2950 0.3034 0.048 Uiso 1 1 calc R . . H17B H 0.3723 1.2339 0.3818 0.048 Uiso 1 1 calc R . . C18 C 0.3638(6) 1.4376(5) 0.2564(5) 0.0438(12) Uani 1 1 d . . . H18A H 0.3073 1.4739 0.3199 0.053 Uiso 1 1 calc R . . H18B H 0.4430 1.5101 0.2053 0.053 Uiso 1 1 calc R . . C19 C 0.2623(8) 1.4171(6) 0.1910(6) 0.068(2) Uani 1 1 d . . . H19A H 0.1565 1.4233 0.2329 0.082 Uiso 1 1 calc R . . H19B H 0.2796 1.4952 0.1142 0.082 Uiso 1 1 calc R . . C20 C 0.2961(6) 1.2690(6) 0.1790(5) 0.0454(13) Uani 1 1 d . . . H20A H 0.2091 1.2028 0.2218 0.055 Uiso 1 1 calc R . . H20B H 0.3196 1.2768 0.0969 0.055 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 0.0244(2) 0.0125(2) 0.0249(2) -0.00562(16) -0.00781(16) 0.00189(14) F2 0.0385(14) 0.0325(15) 0.0355(14) -0.0180(12) -0.0130(11) 0.0034(11) F3 0.0362(15) 0.0389(16) 0.0621(18) -0.0257(14) -0.0208(13) -0.0020(12) F4 0.0255(14) 0.0366(16) 0.0657(19) -0.0152(14) -0.0055(13) -0.0064(12) F5 0.0353(14) 0.0287(14) 0.0336(14) -0.0074(11) 0.0012(11) 0.0041(11) F6 0.0371(14) 0.0301(14) 0.0318(13) -0.0150(11) -0.0051(11) -0.0018(11) F8 0.0413(14) 0.0259(13) 0.0277(13) -0.0096(10) -0.0125(11) 0.0043(11) F9 0.0462(15) 0.0208(14) 0.0414(15) -0.0006(11) -0.0218(12) 0.0055(11) F10 0.0423(15) 0.0198(14) 0.0600(17) -0.0168(12) -0.0169(13) 0.0122(11) F11 0.0429(15) 0.0317(15) 0.0419(15) -0.0211(12) -0.0051(12) 0.0070(12) F12 0.0476(16) 0.0285(14) 0.0268(13) -0.0087(11) -0.0069(11) 0.0078(12) O1 0.0244(15) 0.0216(16) 0.0293(16) -0.0020(13) -0.0083(13) 0.0000(12) O2 0.0320(16) 0.0134(15) 0.0359(17) -0.0112(13) -0.0157(14) 0.0081(12) C1 0.023(2) 0.012(2) 0.027(2) -0.0064(17) -0.0103(18) 0.0042(16) C2 0.030(2) 0.018(2) 0.028(2) -0.0084(18) -0.0089(19) 0.0076(18) C3 0.030(2) 0.020(2) 0.044(3) -0.014(2) -0.018(2) 0.0029(19) C4 0.021(2) 0.018(2) 0.050(3) -0.007(2) -0.010(2) 0.0031(18) C5 0.028(2) 0.018(2) 0.031(2) -0.0068(19) -0.008(2) 0.0077(19) C6 0.030(2) 0.016(2) 0.029(2) -0.0084(18) -0.0099(19) 0.0025(18) C7 0.022(2) 0.011(2) 0.028(2) -0.0050(18) -0.0060(18) 0.0006(17) C8 0.025(2) 0.022(2) 0.027(2) -0.0085(18) -0.0078(18) -0.0015(18) C9 0.026(2) 0.018(2) 0.033(2) -0.0021(19) -0.0139(19) -0.0036(18) C10 0.027(2) 0.014(2) 0.045(3) -0.0101(19) -0.013(2) 0.0062(18) C11 0.028(2) 0.023(2) 0.031(2) -0.0134(19) -0.0031(19) -0.0001(19) C12 0.027(2) 0.022(2) 0.025(2) -0.0035(18) -0.0055(18) -0.0026(18) C13 0.029(2) 0.034(3) 0.044(3) -0.010(2) -0.016(2) 0.002(2) C14 0.032(3) 0.041(3) 0.060(3) -0.021(3) -0.009(2) -0.002(2) C15 0.042(3) 0.057(4) 0.045(3) 0.000(3) 0.000(3) 0.008(3) C16 0.049(3) 0.054(4) 0.032(3) 0.014(2) -0.009(2) -0.019(3) C17 0.057(3) 0.023(3) 0.056(3) -0.022(2) -0.032(3) 0.008(2) C18 0.043(3) 0.027(3) 0.068(4) -0.021(3) -0.021(3) 0.005(2) C19 0.105(5) 0.033(3) 0.091(5) -0.028(3) -0.063(4) 0.030(3) C20 0.057(3) 0.036(3) 0.059(3) -0.024(3) -0.039(3) 0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C7 1.962(4) . ? Pd C1 1.976(4) . ? Pd O2 2.120(3) . ? Pd O1 2.121(3) . ? F2 C2 1.357(5) . ? F3 C3 1.349(4) . ? F4 C4 1.338(5) . ? F5 C5 1.345(5) . ? F6 C6 1.355(5) . ? F8 C8 1.356(5) . ? F9 C9 1.339(5) . ? F10 C10 1.335(5) . ? F11 C11 1.355(5) . ? F12 C12 1.356(4) . ? O1 C16 1.435(5) . ? O1 C13 1.443(5) . ? O2 C20 1.424(5) . ? O2 C17 1.440(5) . ? C1 C2 1.373(6) . ? C1 C6 1.381(6) . ? C2 C3 1.372(6) . ? C3 C4 1.370(6) . ? C4 C5 1.366(6) . ? C5 C6 1.373(6) . ? C7 C8 1.369(6) . ? C7 C12 1.393(6) . ? C8 C9 1.374(6) . ? C9 C10 1.381(6) . ? C10 C11 1.365(6) . ? C11 C12 1.371(6) . ? C13 C14 1.504(7) . ? C14 C15 1.508(7) . ? C15 C16 1.470(7) . ? C17 C18 1.491(6) . ? C18 C19 1.485(7) . ? C19 C20 1.470(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Pd C1 87.48(16) . . ? C7 Pd O2 176.57(12) . . ? C1 Pd O2 95.59(14) . . ? C7 Pd O1 93.93(14) . . ? C1 Pd O1 177.31(12) . . ? O2 Pd O1 83.06(11) . . ? C16 O1 C13 110.2(3) . . ? C16 O1 Pd 119.1(3) . . ? C13 O1 Pd 125.5(3) . . ? C20 O2 C17 108.1(3) . . ? C20 O2 Pd 124.8(3) . . ? C17 O2 Pd 120.0(3) . . ? C2 C1 C6 114.8(4) . . ? C2 C1 Pd 124.6(3) . . ? C6 C1 Pd 120.6(3) . . ? F2 C2 C3 116.9(4) . . ? F2 C2 C1 119.6(4) . . ? C3 C2 C1 123.5(4) . . ? F3 C3 C4 119.5(4) . . ? F3 C3 C2 120.9(4) . . ? C4 C3 C2 119.6(4) . . ? F4 C4 C5 120.6(4) . . ? F4 C4 C3 120.3(4) . . ? C5 C4 C3 119.1(4) . . ? F5 C5 C4 119.3(4) . . ? F5 C5 C6 121.0(4) . . ? C4 C5 C6 119.7(4) . . ? F6 C6 C5 116.6(3) . . ? F6 C6 C1 120.1(4) . . ? C5 C6 C1 123.3(4) . . ? C8 C7 C12 114.6(4) . . ? C8 C7 Pd 123.8(3) . . ? C12 C7 Pd 121.5(3) . . ? F8 C8 C7 119.3(4) . . ? F8 C8 C9 116.4(4) . . ? C7 C8 C9 124.3(4) . . ? F9 C9 C8 121.1(4) . . ? F9 C9 C10 120.0(4) . . ? C8 C9 C10 118.9(4) . . ? F10 C10 C11 120.9(4) . . ? F10 C10 C9 120.1(4) . . ? C11 C10 C9 119.0(4) . . ? F11 C11 C10 118.9(4) . . ? F11 C11 C12 120.9(4) . . ? C10 C11 C12 120.2(4) . . ? F12 C12 C11 117.3(4) . . ? F12 C12 C7 119.8(4) . . ? C11 C12 C7 122.9(4) . . ? O1 C13 C14 104.6(4) . . ? C13 C14 C15 103.2(4) . . ? C16 C15 C14 104.4(4) . . ? O1 C16 C15 106.7(4) . . ? O2 C17 C18 104.7(4) . . ? C19 C18 C17 105.1(4) . . ? C20 C19 C18 106.8(4) . . ? O2 C20 C19 107.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.583 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.138 #=== END data_6' _database_code_depnum_ccdc_archive 'CCDC 762685' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H18 Br F10 O P Pd' _chemical_formula_weight 825.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0737(6) _cell_length_b 11.4335(6) _cell_length_c 13.9572(8) _cell_angle_alpha 113.6800(10) _cell_angle_beta 107.8830(10) _cell_angle_gamma 95.5840(10) _cell_volume 1489.99(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4747 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 2.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7029 _exptl_absorpt_correction_T_max 0.7569 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'omega rotations' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9935 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4297 _reflns_number_gt 3668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.611' _computing_cell_refinement 'SAINT+ 6.02 ' _computing_data_reduction 'SAINT+ 6.02' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL 6.10' _computing_publication_material 'XCIF, SHELXTL 6.10' _refine_special_details ; Refinement of F2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2^, conventional R-factors R are based on F, with F set to zero for negative F2^. The threshold expression of F2^ > 2sigma(F2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2^ 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/[\s2^(Fo2^)+(0.0444P)2^+0.0000P] where P=(Fo2^+2Fc2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4297 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.77822(3) 1.26350(3) 0.64972(2) 0.01744(11) Uani 1 1 d . . . Br Br 0.54312(4) 1.26468(4) 0.59843(3) 0.02596(13) Uani 1 1 d . . . F2 F 0.8083(2) 1.5624(2) 0.82238(17) 0.0268(5) Uani 1 1 d . . . F3 F 0.8572(2) 1.7893(2) 0.80911(18) 0.0318(6) Uani 1 1 d . . . F4 F 0.8934(2) 1.7875(2) 0.62451(19) 0.0354(6) Uani 1 1 d . . . F5 F 0.8795(2) 1.5566(2) 0.45297(18) 0.0302(5) Uani 1 1 d . . . F6 F 0.8316(2) 1.3289(2) 0.46445(17) 0.0252(5) Uani 1 1 d . . . F8 F 0.9423(2) 1.1228(2) 0.50433(17) 0.0267(5) Uani 1 1 d . . . F9 F 1.2004(2) 1.1468(2) 0.55988(18) 0.0304(5) Uani 1 1 d . . . F10 F 1.37152(19) 1.3079(2) 0.77512(18) 0.0284(5) Uani 1 1 d . . . F11 F 1.2818(2) 1.4489(2) 0.93341(18) 0.0310(6) Uani 1 1 d . . . F12 F 1.0225(2) 1.4269(2) 0.88116(17) 0.0269(5) Uani 1 1 d . . . O O 0.7388(3) 0.9987(3) 0.6572(2) 0.0309(7) Uani 1 1 d . . . C1 C 0.8180(3) 1.4365(3) 0.6438(3) 0.0182(8) Uani 1 1 d . . . C2 C 0.8266(3) 1.5567(4) 0.7287(3) 0.0198(9) Uani 1 1 d . . . C3 C 0.8506(4) 1.6740(4) 0.7244(3) 0.0254(9) Uani 1 1 d . . . C4 C 0.8694(4) 1.6743(4) 0.6304(3) 0.0252(9) Uani 1 1 d . . . C5 C 0.8617(4) 1.5567(4) 0.5439(3) 0.0232(9) Uani 1 1 d . . . C6 C 0.8374(3) 1.4421(4) 0.5526(3) 0.0218(9) Uani 1 1 d . . . C7 C 0.9731(3) 1.2748(3) 0.6906(3) 0.0164(8) Uani 1 1 d . . . C8 C 1.0230(4) 1.2055(4) 0.6127(3) 0.0205(9) Uani 1 1 d . . . C9 C 1.1553(4) 1.2155(4) 0.6381(3) 0.0218(9) Uani 1 1 d . . . C10 C 1.2417(4) 1.2977(4) 0.7471(3) 0.0229(9) Uani 1 1 d . . . C11 C 1.1960(4) 1.3686(4) 0.8272(3) 0.0220(9) Uani 1 1 d . . . C12 C 1.0633(4) 1.3559(4) 0.7974(3) 0.0221(9) Uani 1 1 d . . . C13 C 0.7506(3) 1.0941(4) 0.6543(3) 0.0198(9) Uani 1 1 d . . . P P 0.55679(9) 1.01267(9) 0.22872(8) 0.0174(2) Uani 1 1 d . . . C14 C 0.6669(3) 0.9462(3) 0.1632(3) 0.0180(8) Uani 1 1 d . . . C15 C 0.6197(4) 0.8365(4) 0.0578(3) 0.0214(9) Uani 1 1 d . . . H15 H 0.5282 0.7965 0.0197 0.026 Uiso 1 1 calc R . . C16 C 0.7051(4) 0.7855(4) 0.0085(3) 0.0254(9) Uani 1 1 d . . . H16 H 0.6726 0.7110 -0.0640 0.031 Uiso 1 1 calc R . . C17 C 0.8382(4) 0.8428(4) 0.0646(3) 0.0264(10) Uani 1 1 d . . . H17 H 0.8971 0.8078 0.0304 0.032 Uiso 1 1 calc R . . C18 C 0.8862(4) 0.9503(4) 0.1699(3) 0.0255(9) Uani 1 1 d . . . H18 H 0.9781 0.9884 0.2082 0.031 Uiso 1 1 calc R . . C19 C 0.8016(4) 1.0030(4) 0.2203(3) 0.0231(9) Uani 1 1 d . . . H19 H 0.8348 1.0770 0.2931 0.028 Uiso 1 1 calc R . . C20 C 0.3928(3) 0.9105(4) 0.1431(3) 0.0181(8) Uani 1 1 d . . . C21 C 0.3006(4) 0.9507(4) 0.0789(3) 0.0232(9) Uani 1 1 d . . . H21 H 0.3232 1.0338 0.0802 0.028 Uiso 1 1 calc R . . C22 C 0.1749(4) 0.8690(4) 0.0127(3) 0.0279(10) Uani 1 1 d . . . H22 H 0.1115 0.8958 -0.0320 0.033 Uiso 1 1 calc R . . C23 C 0.1423(4) 0.7492(4) 0.0117(3) 0.0257(9) Uani 1 1 d . . . H23 H 0.0564 0.6933 -0.0342 0.031 Uiso 1 1 calc R . . C24 C 0.2332(4) 0.7096(4) 0.0769(3) 0.0233(9) Uani 1 1 d . . . H24 H 0.2095 0.6275 0.0768 0.028 Uiso 1 1 calc R . . C25 C 0.3588(4) 0.7897(3) 0.1422(3) 0.0200(9) Uani 1 1 d . . . H25 H 0.4219 0.7622 0.1865 0.024 Uiso 1 1 calc R . . C26 C 0.5624(3) 1.1766(4) 0.2458(3) 0.0200(9) Uani 1 1 d . . . C27 C 0.6318(4) 1.2303(4) 0.1977(3) 0.0253(9) Uani 1 1 d . . . H27 H 0.6747 1.1786 0.1531 0.030 Uiso 1 1 calc R . . C28 C 0.6371(4) 1.3588(4) 0.2160(3) 0.0291(10) Uani 1 1 d . . . H28 H 0.6845 1.3959 0.1843 0.035 Uiso 1 1 calc R . . C29 C 0.5743(4) 1.4338(4) 0.2798(3) 0.0298(10) Uani 1 1 d . . . H29 H 0.5781 1.5220 0.2913 0.036 Uiso 1 1 calc R . . C30 C 0.5058(4) 1.3816(4) 0.3274(3) 0.0259(9) Uani 1 1 d . . . H30 H 0.4625 1.4337 0.3713 0.031 Uiso 1 1 calc R . . C31 C 0.5006(4) 1.2537(4) 0.3111(3) 0.0232(9) Uani 1 1 d . . . H31 H 0.4546 1.2182 0.3446 0.028 Uiso 1 1 calc R . . C32 C 0.6051(4) 1.0169(4) 0.3638(3) 0.0201(8) Uani 1 1 d . . . H32A H 0.6024 0.9273 0.3553 0.030 Uiso 1 1 calc R . . H32B H 0.5452 1.0531 0.4001 0.030 Uiso 1 1 calc R . . H32C H 0.6946 1.0728 0.4107 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01636(17) 0.01699(18) 0.01990(17) 0.00819(13) 0.00812(13) 0.00498(12) Br 0.0232(2) 0.0267(2) 0.0302(2) 0.0129(2) 0.01266(19) 0.00783(18) F2 0.0313(13) 0.0266(13) 0.0228(12) 0.0087(10) 0.0134(10) 0.0102(10) F3 0.0388(14) 0.0145(12) 0.0334(13) 0.0035(11) 0.0126(11) 0.0072(10) F4 0.0417(15) 0.0220(13) 0.0423(14) 0.0191(12) 0.0110(12) 0.0034(11) F5 0.0320(13) 0.0342(14) 0.0292(13) 0.0196(11) 0.0121(11) 0.0037(11) F6 0.0301(13) 0.0211(12) 0.0228(12) 0.0065(10) 0.0131(10) 0.0050(10) F8 0.0236(12) 0.0320(13) 0.0198(12) 0.0076(11) 0.0068(10) 0.0104(10) F9 0.0272(13) 0.0421(14) 0.0308(13) 0.0182(11) 0.0172(11) 0.0183(11) F10 0.0168(12) 0.0325(13) 0.0408(14) 0.0203(11) 0.0114(10) 0.0091(10) F11 0.0225(12) 0.0255(13) 0.0306(13) 0.0056(11) 0.0024(10) 0.0034(10) F12 0.0228(12) 0.0258(12) 0.0256(12) 0.0050(10) 0.0096(10) 0.0065(10) O 0.0357(18) 0.0264(17) 0.0379(17) 0.0164(15) 0.0204(14) 0.0104(14) C1 0.015(2) 0.019(2) 0.022(2) 0.0121(18) 0.0055(17) 0.0055(16) C2 0.016(2) 0.025(2) 0.021(2) 0.0122(19) 0.0080(17) 0.0060(17) C3 0.021(2) 0.021(2) 0.027(2) 0.0063(19) 0.0052(18) 0.0059(18) C4 0.021(2) 0.018(2) 0.031(2) 0.013(2) 0.0016(18) 0.0023(17) C5 0.018(2) 0.029(2) 0.024(2) 0.015(2) 0.0064(17) 0.0025(18) C6 0.016(2) 0.021(2) 0.024(2) 0.0078(19) 0.0046(17) 0.0041(17) C7 0.019(2) 0.014(2) 0.020(2) 0.0091(17) 0.0105(17) 0.0033(16) C8 0.019(2) 0.018(2) 0.026(2) 0.0126(18) 0.0062(18) 0.0063(17) C9 0.027(2) 0.022(2) 0.028(2) 0.0151(19) 0.0179(19) 0.0124(18) C10 0.017(2) 0.023(2) 0.039(2) 0.021(2) 0.0139(19) 0.0083(18) C11 0.020(2) 0.017(2) 0.024(2) 0.0086(18) 0.0059(18) 0.0002(17) C12 0.023(2) 0.019(2) 0.029(2) 0.0118(19) 0.0141(19) 0.0069(18) C13 0.014(2) 0.026(2) 0.022(2) 0.0104(19) 0.0110(17) 0.0064(18) P 0.0164(5) 0.0167(5) 0.0185(5) 0.0074(4) 0.0067(4) 0.0036(4) C14 0.018(2) 0.020(2) 0.021(2) 0.0126(18) 0.0075(17) 0.0064(17) C15 0.018(2) 0.022(2) 0.022(2) 0.0102(19) 0.0064(17) 0.0036(17) C16 0.029(2) 0.027(2) 0.022(2) 0.0108(19) 0.0125(19) 0.0088(19) C17 0.031(2) 0.028(2) 0.032(2) 0.016(2) 0.021(2) 0.016(2) C18 0.017(2) 0.028(2) 0.037(2) 0.018(2) 0.0122(19) 0.0061(18) C19 0.026(2) 0.019(2) 0.024(2) 0.0099(18) 0.0079(18) 0.0055(18) C20 0.017(2) 0.019(2) 0.0181(19) 0.0064(17) 0.0091(16) 0.0050(16) C21 0.020(2) 0.024(2) 0.028(2) 0.0147(19) 0.0088(18) 0.0045(18) C22 0.021(2) 0.034(3) 0.029(2) 0.016(2) 0.0064(19) 0.0091(19) C23 0.018(2) 0.027(2) 0.024(2) 0.0055(19) 0.0068(18) 0.0008(18) C24 0.025(2) 0.018(2) 0.025(2) 0.0053(18) 0.0132(18) 0.0047(18) C25 0.020(2) 0.019(2) 0.021(2) 0.0081(17) 0.0086(17) 0.0078(17) C26 0.016(2) 0.020(2) 0.020(2) 0.0090(18) 0.0029(17) 0.0016(17) C27 0.025(2) 0.026(2) 0.022(2) 0.0105(19) 0.0079(18) 0.0049(18) C28 0.032(2) 0.024(2) 0.031(2) 0.014(2) 0.010(2) 0.0025(19) C29 0.034(2) 0.018(2) 0.036(2) 0.013(2) 0.010(2) 0.0047(19) C30 0.025(2) 0.021(2) 0.026(2) 0.0057(19) 0.0080(19) 0.0109(19) C31 0.020(2) 0.023(2) 0.027(2) 0.0117(19) 0.0094(18) 0.0054(18) C32 0.020(2) 0.017(2) 0.020(2) 0.0065(17) 0.0064(17) 0.0046(17) _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 C13 1.961(4) . ? Pd C1 2.024(4) . ? Pd C7 2.032(4) . ? Pd Br 2.4821(5) . ? F2 C2 1.361(4) . ? F3 C3 1.348(4) . ? F4 C4 1.335(4) . ? F5 C5 1.343(4) . ? F6 C6 1.360(4) . ? F8 C8 1.356(4) . ? F9 C9 1.334(4) . ? F10 C10 1.348(4) . ? F11 C11 1.347(4) . ? F12 C12 1.365(4) . ? O C13 1.104(4) . ? C1 C2 1.378(5) . ? C1 C6 1.379(5) . ? C2 C3 1.371(5) . ? C3 C4 1.391(5) . ? C4 C5 1.372(5) . ? C5 C6 1.372(5) . ? C7 C12 1.370(5) . ? C7 C8 1.370(5) . ? C8 C9 1.378(5) . ? C9 C10 1.377(5) . ? C10 C11 1.365(5) . ? C11 C12 1.374(5) . ? P C32 1.773(4) . ? P C26 1.784(4) . ? P C14 1.791(4) . ? P C20 1.795(4) . ? C14 C15 1.388(5) . ? C14 C19 1.396(5) . ? C15 C16 1.376(5) . ? C16 C17 1.381(5) . ? C17 C18 1.376(5) . ? C18 C19 1.382(5) . ? C20 C21 1.385(5) . ? C20 C25 1.389(5) . ? C21 C22 1.388(5) . ? C22 C23 1.376(5) . ? C23 C24 1.379(5) . ? C24 C25 1.381(5) . ? C26 C31 1.389(5) . ? C26 C27 1.405(5) . ? C27 C28 1.379(5) . ? C28 C29 1.377(5) . ? C29 C30 1.383(5) . ? C30 C31 1.379(5) . ? 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 C13 Pd C1 176.23(14) . . ? C13 Pd C7 90.18(14) . . ? C1 Pd C7 86.27(13) . . ? C13 Pd Br 93.99(10) . . ? C1 Pd Br 89.56(10) . . ? C7 Pd Br 175.83(10) . . ? C2 C1 C6 114.9(3) . . ? C2 C1 Pd 123.3(3) . . ? C6 C1 Pd 121.8(3) . . ? F2 C2 C3 116.6(3) . . ? F2 C2 C1 119.7(3) . . ? C3 C2 C1 123.7(3) . . ? F3 C3 C2 121.7(3) . . ? F3 C3 C4 119.1(3) . . ? C2 C3 C4 119.2(4) . . ? F4 C4 C5 120.9(3) . . ? F4 C4 C3 120.2(3) . . ? C5 C4 C3 118.9(3) . . ? F5 C5 C4 119.0(3) . . ? F5 C5 C6 121.4(3) . . ? C4 C5 C6 119.5(3) . . ? F6 C6 C5 116.7(3) . . ? F6 C6 C1 119.5(3) . . ? C5 C6 C1 123.8(4) . . ? C12 C7 C8 115.8(3) . . ? C12 C7 Pd 121.8(3) . . ? C8 C7 Pd 122.4(3) . . ? F8 C8 C7 120.6(3) . . ? F8 C8 C9 116.3(3) . . ? C7 C8 C9 123.1(3) . . ? F9 C9 C10 119.8(3) . . ? F9 C9 C8 121.4(3) . . ? C10 C9 C8 118.7(3) . . ? F10 C10 C11 119.8(3) . . ? F10 C10 C9 120.2(3) . . ? C11 C10 C9 120.0(3) . . ? F11 C11 C10 119.3(3) . . ? F11 C11 C12 121.6(3) . . ? C10 C11 C12 119.1(3) . . ? F12 C12 C7 120.0(3) . . ? F12 C12 C11 116.7(3) . . ? C7 C12 C11 123.3(3) . . ? O C13 Pd 177.9(3) . . ? C32 P C26 108.85(17) . . ? C32 P C14 109.08(17) . . ? C26 P C14 110.03(17) . . ? C32 P C20 109.37(17) . . ? C26 P C20 109.77(17) . . ? C14 P C20 109.72(17) . . ? C15 C14 C19 119.8(3) . . ? C15 C14 P 120.6(3) . . ? C19 C14 P 119.5(3) . . ? C16 C15 C14 120.2(4) . . ? C15 C16 C17 119.8(4) . . ? C18 C17 C16 120.5(4) . . ? C17 C18 C19 120.4(4) . . ? C18 C19 C14 119.3(4) . . ? C21 C20 C25 120.0(3) . . ? C21 C20 P 120.9(3) . . ? C25 C20 P 119.1(3) . . ? C20 C21 C22 119.6(4) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C24 120.6(4) . . ? C23 C24 C25 119.8(4) . . ? C24 C25 C20 120.0(4) . . ? C31 C26 C27 119.6(4) . . ? C31 C26 P 119.2(3) . . ? C27 C26 P 121.2(3) . . ? C28 C27 C26 119.3(4) . . ? C29 C28 C27 120.6(4) . . ? C28 C29 C30 120.4(4) . . ? C31 C30 C29 119.8(4) . . ? C30 C31 C26 120.3(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.481 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.082 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 762686' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H38 Cl3 F20 N O2 Pd2' _chemical_formula_weight 1299.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.1282(5) _cell_length_b 18.2509(8) _cell_length_c 29.6036(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9794.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11919 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 24.8 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6533 _exptl_absorpt_correction_T_max 0.8081 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Gon. KM4/Xcalibur, det.: Sapphire3' _diffrn_measurement_method 'w scans' _diffrn_detector_area_resol_mean 16.0655 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27465 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 25.06 _reflns_number_total 8559 _reflns_number_gt 7140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0534P)^2^+20.9225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8559 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.446884(16) 0.088966(17) 0.731092(10) 0.01633(10) Uani 1 1 d . . . Pd2 Pd 0.367401(16) -0.047670(17) 0.794952(10) 0.01697(10) Uani 1 1 d . . . Cl1 Cl 0.39341(6) 0.08083(5) 0.80543(3) 0.0201(2) Uani 1 1 d . . . F2 F 0.41996(13) 0.24742(13) 0.76494(8) 0.0249(6) Uani 1 1 d . . . F3 F 0.32440(14) 0.35296(13) 0.74040(8) 0.0277(6) Uani 1 1 d . . . F4 F 0.22340(14) 0.32762(14) 0.67440(9) 0.0294(6) Uani 1 1 d . . . F5 F 0.21922(14) 0.19518(14) 0.63217(9) 0.0314(6) Uani 1 1 d . . . F6 F 0.31342(13) 0.08887(13) 0.65531(8) 0.0247(5) Uani 1 1 d . . . F8 F 0.52176(14) 0.21800(13) 0.67193(9) 0.0270(6) Uani 1 1 d . . . F9 F 0.55610(15) 0.22377(14) 0.58383(10) 0.0383(7) Uani 1 1 d . . . F10 F 0.52918(17) 0.10625(16) 0.52935(9) 0.0404(7) Uani 1 1 d . . . F11 F 0.47080(16) -0.01812(14) 0.56436(9) 0.0353(7) Uani 1 1 d . . . F12 F 0.43722(14) -0.02689(13) 0.65316(8) 0.0259(6) Uani 1 1 d . . . F14 F 0.52124(13) -0.13687(14) 0.80460(8) 0.0253(5) Uani 1 1 d . . . F15 F 0.60057(15) -0.17373(15) 0.87778(9) 0.0366(7) Uani 1 1 d . . . F16 F 0.55603(16) -0.13100(17) 0.96150(9) 0.0428(7) Uani 1 1 d . . . F17 F 0.43027(16) -0.05043(17) 0.97136(9) 0.0398(7) Uani 1 1 d . . . F18 F 0.34829(14) -0.01596(14) 0.89917(9) 0.0296(6) Uani 1 1 d . . . F20 F 0.27884(14) -0.16870(14) 0.85305(9) 0.0299(6) Uani 1 1 d . . . F21 F 0.25873(15) -0.31234(14) 0.83820(9) 0.0346(6) Uani 1 1 d . . . F22 F 0.32432(15) -0.38019(13) 0.76685(9) 0.0310(6) Uani 1 1 d . . . F23 F 0.40928(16) -0.30144(15) 0.70919(9) 0.0347(7) Uani 1 1 d . . . F24 F 0.42730(13) -0.15495(14) 0.71978(8) 0.0265(6) Uani 1 1 d . . . O1 O 0.57944(18) -0.00929(18) 0.75786(12) 0.0350(8) Uani 1 1 d . . . O2 O 0.25740(19) -0.01565(19) 0.71709(12) 0.0376(8) Uani 1 1 d . . . C1 C 0.3702(2) 0.1635(2) 0.71185(13) 0.0162(8) Uani 1 1 d . . . C2 C 0.3699(2) 0.2321(2) 0.73225(13) 0.0184(9) Uani 1 1 d . . . C3 C 0.3217(2) 0.2873(2) 0.72036(14) 0.0203(9) Uani 1 1 d . . . C4 C 0.2708(2) 0.2743(2) 0.68629(14) 0.0205(9) Uani 1 1 d . . . C5 C 0.2691(2) 0.2076(2) 0.66544(15) 0.0229(9) Uani 1 1 d . . . C6 C 0.3182(2) 0.1534(2) 0.67798(14) 0.0196(9) Uani 1 1 d . . . C7 C 0.4799(2) 0.0948(2) 0.66636(14) 0.0208(9) Uani 1 1 d . . . C8 C 0.5098(2) 0.1572(2) 0.64678(14) 0.0209(9) Uani 1 1 d . . . C9 C 0.5273(2) 0.1623(2) 0.60138(15) 0.0257(10) Uani 1 1 d . . . C10 C 0.5137(3) 0.1029(3) 0.57372(15) 0.0289(11) Uani 1 1 d . . . C11 C 0.4841(2) 0.0401(2) 0.59180(15) 0.0252(10) Uani 1 1 d . . . C12 C 0.4677(2) 0.0369(2) 0.63720(15) 0.0215(9) Uani 1 1 d . . . C13 C 0.4312(2) -0.0755(2) 0.84839(14) 0.0190(9) Uani 1 1 d . . . C14 C 0.4962(2) -0.1150(2) 0.84522(14) 0.0203(9) Uani 1 1 d . . . C15 C 0.5380(2) -0.1344(2) 0.88271(16) 0.0273(10) Uani 1 1 d . . . C16 C 0.5161(3) -0.1131(3) 0.92466(16) 0.0300(11) Uani 1 1 d . . . C17 C 0.4522(2) -0.0723(3) 0.92960(15) 0.0270(10) Uani 1 1 d . . . C18 C 0.4112(2) -0.0552(2) 0.89165(14) 0.0220(9) Uani 1 1 d . . . C19 C 0.3529(2) -0.1563(2) 0.78681(14) 0.0180(9) Uani 1 1 d . . . C20 C 0.3114(2) -0.1991(2) 0.81612(14) 0.0203(9) Uani 1 1 d . . . C21 C 0.3007(2) -0.2733(2) 0.80976(14) 0.0224(9) Uani 1 1 d . . . C22 C 0.3333(2) -0.3079(2) 0.77358(14) 0.0211(9) Uani 1 1 d . . . C23 C 0.3763(2) -0.2673(2) 0.74457(14) 0.0221(9) Uani 1 1 d . . . C24 C 0.3850(2) -0.1932(2) 0.75141(14) 0.0192(9) Uani 1 1 d . . . C25 C 0.5299(2) 0.0236(2) 0.74791(15) 0.0239(9) Uani 1 1 d . . . C26 C 0.2990(2) -0.0269(2) 0.74430(16) 0.0239(10) Uani 1 1 d . . . N N 0.52288(18) -0.25591(18) 0.58942(11) 0.0164(7) Uani 1 1 d . . . C27 C 0.4684(2) -0.2134(2) 0.56044(14) 0.0198(9) Uani 1 1 d . . . H27A H 0.4507 -0.2460 0.5360 0.024 Uiso 1 1 calc R . . H27B H 0.4949 -0.1722 0.5460 0.024 Uiso 1 1 calc R . . C28 C 0.4014(2) -0.1826(2) 0.58522(14) 0.0191(9) Uani 1 1 d . . . H28A H 0.4172 -0.1451 0.6074 0.023 Uiso 1 1 calc R . . H28B H 0.3756 -0.2223 0.6017 0.023 Uiso 1 1 calc R . . C29 C 0.3494(2) -0.1481(3) 0.54991(15) 0.0238(10) Uani 1 1 d . . . H29A H 0.3769 -0.1109 0.5324 0.029 Uiso 1 1 calc R . . H29B H 0.3328 -0.1866 0.5287 0.029 Uiso 1 1 calc R . . C30 C 0.2824(3) -0.1123(3) 0.57149(16) 0.0332(11) Uani 1 1 d . . . H30A H 0.2509 -0.0914 0.5479 0.050 Uiso 1 1 calc R . . H30B H 0.2986 -0.0733 0.5920 0.050 Uiso 1 1 calc R . . H30C H 0.2545 -0.1491 0.5885 0.050 Uiso 1 1 calc R . . C31 C 0.4851(2) -0.3197(2) 0.61302(13) 0.0171(8) Uani 1 1 d . . . H31A H 0.5236 -0.3490 0.6284 0.020 Uiso 1 1 calc R . . H31B H 0.4526 -0.2994 0.6368 0.020 Uiso 1 1 calc R . . C32 C 0.4393(2) -0.3715(2) 0.58426(15) 0.0236(9) Uani 1 1 d . . . H32A H 0.4701 -0.3928 0.5600 0.028 Uiso 1 1 calc R . . H32B H 0.3979 -0.3446 0.5701 0.028 Uiso 1 1 calc R . . C33 C 0.4096(2) -0.4321(2) 0.61473(15) 0.0243(10) Uani 1 1 d . . . H33A H 0.3880 -0.4098 0.6422 0.029 Uiso 1 1 calc R . . H33B H 0.4511 -0.4638 0.6243 0.029 Uiso 1 1 calc R . . C34 C 0.3513(3) -0.4791(3) 0.59153(19) 0.0372(12) Uani 1 1 d . . . H34A H 0.3342 -0.5171 0.6124 0.056 Uiso 1 1 calc R . . H34B H 0.3726 -0.5021 0.5646 0.056 Uiso 1 1 calc R . . H34C H 0.3095 -0.4482 0.5827 0.056 Uiso 1 1 calc R . . C35 C 0.5829(2) -0.2826(2) 0.55738(13) 0.0192(9) Uani 1 1 d . . . H35A H 0.5605 -0.3181 0.5361 0.023 Uiso 1 1 calc R . . H35B H 0.6004 -0.2403 0.5394 0.023 Uiso 1 1 calc R . . C36 C 0.6491(2) -0.3187(2) 0.57922(14) 0.0209(9) Uani 1 1 d . . . H36A H 0.6325 -0.3546 0.6021 0.025 Uiso 1 1 calc R . . H36B H 0.6796 -0.2812 0.5946 0.025 Uiso 1 1 calc R . . C37 C 0.6953(2) -0.3577(2) 0.54280(15) 0.0232(9) Uani 1 1 d . . . H37A H 0.6674 -0.4001 0.5310 0.028 Uiso 1 1 calc R . . H37B H 0.7043 -0.3235 0.5174 0.028 Uiso 1 1 calc R . . C38 C 0.7692(2) -0.3840(3) 0.56160(16) 0.0285(10) Uani 1 1 d . . . H38A H 0.7973 -0.4082 0.5376 0.043 Uiso 1 1 calc R . . H38B H 0.7604 -0.4188 0.5862 0.043 Uiso 1 1 calc R . . H38C H 0.7972 -0.3420 0.5730 0.043 Uiso 1 1 calc R . . C39 C 0.5546(2) -0.2088(2) 0.62716(13) 0.0190(9) Uani 1 1 d . . . H39A H 0.5133 -0.1926 0.6466 0.023 Uiso 1 1 calc R . . H39B H 0.5872 -0.2400 0.6459 0.023 Uiso 1 1 calc R . . C40 C 0.5978(2) -0.1416(2) 0.61297(14) 0.0219(9) Uani 1 1 d . . . H40A H 0.5681 -0.1118 0.5918 0.026 Uiso 1 1 calc R . . H40B H 0.6436 -0.1567 0.5973 0.026 Uiso 1 1 calc R . . C41 C 0.6169(2) -0.0964(2) 0.65481(15) 0.0258(10) Uani 1 1 d . . . H41A H 0.5706 -0.0817 0.6701 0.031 Uiso 1 1 calc R . . H41B H 0.6452 -0.1274 0.6761 0.031 Uiso 1 1 calc R . . C42 C 0.6616(3) -0.0281(2) 0.64414(17) 0.0303(11) Uani 1 1 d . . . H42A H 0.6718 -0.0014 0.6722 0.045 Uiso 1 1 calc R . . H42B H 0.6335 0.0033 0.6235 0.045 Uiso 1 1 calc R . . H42C H 0.7082 -0.0423 0.6298 0.045 Uiso 1 1 calc R . . Cl2 Cl 0.21888(12) 0.17096(10) 0.47599(8) 0.0838(6) Uani 1 1 d . . . Cl3 Cl 0.34158(12) 0.07649(15) 0.50526(8) 0.0987(8) Uani 1 1 d . . . C43 C 0.2542(3) 0.0828(3) 0.4812(2) 0.0498(15) Uani 1 1 d . . . H43A H 0.2560 0.0603 0.4509 0.060 Uiso 1 1 calc R . . H43B H 0.2196 0.0536 0.4998 0.060 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 0.01865(17) 0.01541(17) 0.01494(17) -0.00020(12) -0.00159(11) 0.00125(12) Pd2 0.01872(17) 0.01608(18) 0.01612(17) -0.00019(13) -0.00109(12) 0.00084(12) Cl1 0.0268(5) 0.0172(5) 0.0161(5) -0.0009(4) -0.0005(4) 0.0000(4) F2 0.0289(14) 0.0240(13) 0.0219(13) -0.0039(10) -0.0070(10) 0.0032(10) F3 0.0355(15) 0.0190(13) 0.0286(14) -0.0045(11) -0.0018(11) 0.0072(11) F4 0.0294(14) 0.0295(15) 0.0293(15) 0.0060(12) -0.0027(11) 0.0130(11) F5 0.0291(14) 0.0355(15) 0.0297(15) 0.0015(12) -0.0147(11) 0.0029(11) F6 0.0251(13) 0.0212(13) 0.0276(14) -0.0022(11) -0.0073(10) -0.0017(10) F8 0.0294(14) 0.0196(13) 0.0320(15) -0.0037(11) -0.0013(11) -0.0046(10) F9 0.0462(17) 0.0272(15) 0.0414(17) 0.0117(13) 0.0147(13) -0.0010(12) F10 0.0562(19) 0.0470(18) 0.0181(14) 0.0070(13) 0.0112(12) 0.0092(14) F11 0.0532(18) 0.0299(15) 0.0228(14) -0.0091(12) -0.0009(12) 0.0051(13) F12 0.0392(15) 0.0162(12) 0.0223(13) -0.0018(10) 0.0049(11) 0.0008(10) F14 0.0244(13) 0.0286(14) 0.0229(13) -0.0013(11) 0.0030(10) 0.0036(10) F15 0.0313(15) 0.0402(16) 0.0383(17) 0.0056(13) -0.0066(12) 0.0133(12) F16 0.0447(18) 0.057(2) 0.0266(15) 0.0152(14) -0.0150(12) 0.0013(14) F17 0.0455(17) 0.059(2) 0.0149(13) -0.0013(13) 0.0027(11) -0.0035(14) F18 0.0253(14) 0.0344(15) 0.0290(15) -0.0060(12) 0.0008(10) 0.0068(11) F20 0.0295(14) 0.0255(14) 0.0346(15) -0.0090(12) 0.0162(11) 0.0004(11) F21 0.0414(16) 0.0278(15) 0.0346(15) 0.0039(12) 0.0165(12) -0.0076(12) F22 0.0421(16) 0.0181(13) 0.0328(15) -0.0022(11) 0.0030(12) -0.0037(11) F23 0.0497(18) 0.0319(15) 0.0225(14) -0.0082(12) 0.0116(12) -0.0010(13) F24 0.0297(14) 0.0295(14) 0.0203(13) -0.0053(11) 0.0102(10) -0.0050(11) O1 0.0299(19) 0.0308(19) 0.044(2) 0.0111(16) -0.0006(15) 0.0058(15) O2 0.035(2) 0.033(2) 0.044(2) 0.0125(17) -0.0168(17) -0.0060(15) C1 0.016(2) 0.019(2) 0.013(2) -0.0001(16) 0.0019(15) 0.0001(16) C2 0.017(2) 0.022(2) 0.017(2) 0.0011(17) -0.0030(16) -0.0023(16) C3 0.024(2) 0.017(2) 0.020(2) 0.0005(17) 0.0046(17) 0.0009(17) C4 0.019(2) 0.020(2) 0.022(2) 0.0071(18) 0.0023(16) 0.0050(16) C5 0.019(2) 0.028(3) 0.022(2) 0.0044(19) -0.0043(17) 0.0010(17) C6 0.022(2) 0.020(2) 0.016(2) -0.0014(17) 0.0024(16) -0.0022(17) C7 0.025(2) 0.019(2) 0.019(2) 0.0039(17) -0.0068(17) 0.0048(17) C8 0.019(2) 0.016(2) 0.028(2) 0.0018(18) -0.0032(17) 0.0016(16) C9 0.025(2) 0.022(2) 0.030(3) 0.008(2) 0.0048(18) 0.0020(18) C10 0.029(3) 0.037(3) 0.021(2) 0.004(2) 0.0051(18) 0.015(2) C11 0.030(2) 0.023(2) 0.022(2) -0.0004(19) -0.0013(18) 0.0030(19) C12 0.025(2) 0.015(2) 0.024(2) 0.0020(18) -0.0004(17) 0.0032(17) C13 0.018(2) 0.019(2) 0.020(2) 0.0035(17) -0.0018(16) -0.0041(16) C14 0.025(2) 0.020(2) 0.016(2) 0.0011(17) 0.0017(16) -0.0023(17) C15 0.023(2) 0.027(2) 0.032(3) 0.009(2) -0.0024(19) 0.0043(18) C16 0.036(3) 0.029(3) 0.025(2) 0.012(2) -0.008(2) -0.004(2) C17 0.030(3) 0.035(3) 0.015(2) -0.0001(19) 0.0032(17) -0.0067(19) C18 0.021(2) 0.022(2) 0.022(2) -0.0001(18) 0.0023(17) 0.0028(17) C19 0.020(2) 0.016(2) 0.019(2) -0.0002(17) -0.0009(16) 0.0010(16) C20 0.021(2) 0.021(2) 0.019(2) -0.0029(18) 0.0046(16) 0.0049(17) C21 0.023(2) 0.025(2) 0.019(2) 0.0060(18) 0.0007(17) -0.0016(17) C22 0.027(2) 0.015(2) 0.021(2) 0.0005(17) -0.0027(18) 0.0004(17) C23 0.025(2) 0.026(2) 0.015(2) -0.0044(18) 0.0032(17) 0.0043(17) C24 0.022(2) 0.024(2) 0.012(2) 0.0068(17) 0.0019(16) -0.0029(17) C25 0.030(3) 0.022(2) 0.020(2) 0.0006(19) 0.0039(19) 0.0012(19) C26 0.027(2) 0.017(2) 0.028(3) 0.0034(19) -0.001(2) -0.0062(17) N 0.0172(17) 0.0201(18) 0.0120(17) 0.0017(14) 0.0021(13) 0.0002(14) C27 0.018(2) 0.024(2) 0.017(2) 0.0023(18) -0.0019(16) 0.0031(17) C28 0.017(2) 0.022(2) 0.018(2) 0.0033(18) 0.0005(16) 0.0010(16) C29 0.022(2) 0.029(2) 0.021(2) -0.0002(19) 0.0010(17) 0.0059(18) C30 0.028(3) 0.043(3) 0.029(3) 0.003(2) 0.0005(19) 0.016(2) C31 0.019(2) 0.019(2) 0.014(2) 0.0015(17) 0.0003(15) -0.0023(16) C32 0.026(2) 0.024(2) 0.021(2) -0.0032(19) -0.0047(17) -0.0009(18) C33 0.020(2) 0.023(2) 0.030(2) -0.0030(19) -0.0018(18) -0.0018(17) C34 0.033(3) 0.027(3) 0.052(3) 0.000(2) -0.004(2) -0.004(2) C35 0.019(2) 0.025(2) 0.014(2) -0.0006(17) 0.0038(16) 0.0028(17) C36 0.018(2) 0.025(2) 0.020(2) 0.0025(18) 0.0004(16) 0.0020(17) C37 0.022(2) 0.026(2) 0.022(2) 0.0035(19) 0.0021(17) 0.0044(17) C38 0.023(2) 0.031(3) 0.031(3) 0.003(2) 0.0052(18) 0.0082(19) C39 0.022(2) 0.021(2) 0.014(2) -0.0035(17) 0.0004(16) 0.0007(17) C40 0.025(2) 0.020(2) 0.020(2) 0.0009(18) -0.0003(17) -0.0042(17) C41 0.026(2) 0.026(2) 0.025(2) -0.005(2) 0.0010(18) -0.0028(18) C42 0.032(3) 0.024(2) 0.035(3) -0.004(2) 0.002(2) 0.0004(19) Cl2 0.0967(15) 0.0444(10) 0.1103(17) 0.0015(10) 0.0305(12) -0.0087(9) Cl3 0.0758(13) 0.139(2) 0.0816(14) 0.0497(14) -0.0375(11) -0.0434(13) C43 0.045(3) 0.054(4) 0.051(4) 0.007(3) -0.002(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C25 1.983(5) . ? Pd1 C7 2.010(4) . ? Pd1 C1 2.027(4) . ? Pd1 Cl1 2.4092(10) . ? Pd2 C26 1.982(5) . ? Pd2 C19 2.015(4) . ? Pd2 C13 2.024(4) . ? Pd2 Cl1 2.4122(10) . ? F2 C2 1.356(5) . ? F3 C3 1.339(5) . ? F4 C4 1.345(5) . ? F5 C5 1.356(5) . ? F6 C6 1.358(5) . ? F8 C8 1.353(5) . ? F9 C9 1.342(5) . ? F10 C10 1.344(5) . ? F11 C11 1.358(5) . ? F12 C12 1.373(5) . ? F14 C14 1.346(5) . ? F15 C15 1.350(5) . ? F16 C16 1.349(5) . ? F17 C17 1.359(5) . ? F18 C18 1.365(5) . ? F20 C20 1.361(5) . ? F21 C21 1.340(5) . ? F22 C22 1.344(5) . ? F23 C23 1.357(5) . ? F24 C24 1.397(5) . ? O1 C25 1.121(5) . ? O2 C26 1.122(5) . ? C1 C6 1.389(6) . ? C1 C2 1.391(6) . ? C2 C3 1.378(6) . ? C3 C4 1.388(6) . ? C4 C5 1.366(6) . ? C5 C6 1.381(6) . ? C7 C12 1.382(6) . ? C7 C8 1.388(6) . ? C8 C9 1.384(6) . ? C9 C10 1.380(7) . ? C10 C11 1.375(6) . ? C11 C12 1.378(6) . ? C13 C18 1.382(6) . ? C13 C14 1.384(6) . ? C14 C15 1.391(6) . ? C15 C16 1.361(7) . ? C16 C17 1.384(7) . ? C17 C18 1.383(6) . ? C19 C24 1.374(6) . ? C19 C20 1.389(6) . ? C20 C21 1.380(6) . ? C21 C22 1.377(6) . ? C22 C23 1.377(6) . ? C23 C24 1.378(6) . ? N C31 1.521(5) . ? N C27 1.521(5) . ? N C39 1.522(5) . ? N C35 1.523(5) . ? C27 C28 1.525(6) . ? C28 C29 1.542(6) . ? C29 C30 1.520(6) . ? C31 C32 1.519(6) . ? C32 C33 1.525(6) . ? C33 C34 1.525(6) . ? C35 C36 1.515(6) . ? C36 C37 1.539(6) . ? C37 C38 1.528(6) . ? C39 C40 1.514(6) . ? C40 C41 1.528(6) . ? C41 C42 1.520(6) . ? Cl2 C43 1.738(6) . ? Cl3 C43 1.740(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 Pd1 C7 92.62(17) . . ? C25 Pd1 C1 173.99(17) . . ? C7 Pd1 C1 84.28(16) . . ? C25 Pd1 Cl1 92.23(13) . . ? C7 Pd1 Cl1 173.55(12) . . ? C1 Pd1 Cl1 91.26(11) . . ? C26 Pd2 C19 90.90(17) . . ? C26 Pd2 C13 175.15(16) . . ? C19 Pd2 C13 85.48(16) . . ? C26 Pd2 Cl1 91.94(12) . . ? C19 Pd2 Cl1 176.19(12) . . ? C13 Pd2 Cl1 91.82(12) . . ? Pd1 Cl1 Pd2 91.21(3) . . ? C6 C1 C2 115.5(4) . . ? C6 C1 Pd1 125.4(3) . . ? C2 C1 Pd1 119.0(3) . . ? F2 C2 C3 117.1(4) . . ? F2 C2 C1 119.5(4) . . ? C3 C2 C1 123.3(4) . . ? F3 C3 C2 121.2(4) . . ? F3 C3 C4 119.9(4) . . ? C2 C3 C4 118.9(4) . . ? F4 C4 C5 120.8(4) . . ? F4 C4 C3 119.5(4) . . ? C5 C4 C3 119.7(4) . . ? F5 C5 C4 119.5(4) . . ? F5 C5 C6 120.3(4) . . ? C4 C5 C6 120.2(4) . . ? F6 C6 C5 116.6(4) . . ? F6 C6 C1 121.0(4) . . ? C5 C6 C1 122.4(4) . . ? C12 C7 C8 115.4(4) . . ? C12 C7 Pd1 120.5(3) . . ? C8 C7 Pd1 123.9(3) . . ? F8 C8 C9 116.3(4) . . ? F8 C8 C7 120.3(4) . . ? C9 C8 C7 123.3(4) . . ? F9 C9 C10 119.7(4) . . ? F9 C9 C8 121.4(4) . . ? C10 C9 C8 118.9(4) . . ? F10 C10 C11 120.0(4) . . ? F10 C10 C9 120.5(4) . . ? C11 C10 C9 119.6(4) . . ? F11 C11 C10 119.2(4) . . ? F11 C11 C12 120.9(4) . . ? C10 C11 C12 119.9(4) . . ? F12 C12 C11 117.2(4) . . ? F12 C12 C7 119.9(4) . . ? C11 C12 C7 122.9(4) . . ? C18 C13 C14 115.2(4) . . ? C18 C13 Pd2 120.5(3) . . ? C14 C13 Pd2 124.3(3) . . ? F14 C14 C13 120.1(4) . . ? F14 C14 C15 117.0(4) . . ? C13 C14 C15 122.9(4) . . ? F15 C15 C16 119.8(4) . . ? F15 C15 C14 120.5(4) . . ? C16 C15 C14 119.7(4) . . ? F16 C16 C15 120.8(4) . . ? F16 C16 C17 119.6(4) . . ? C15 C16 C17 119.7(4) . . ? F17 C17 C18 121.0(4) . . ? F17 C17 C16 120.0(4) . . ? C18 C17 C16 119.0(4) . . ? F18 C18 C13 120.7(4) . . ? F18 C18 C17 115.8(4) . . ? C13 C18 C17 123.5(4) . . ? C24 C19 C20 115.5(4) . . ? C24 C19 Pd2 121.1(3) . . ? C20 C19 Pd2 123.3(3) . . ? F20 C20 C21 116.7(4) . . ? F20 C20 C19 120.5(4) . . ? C21 C20 C19 122.8(4) . . ? F21 C21 C22 119.2(4) . . ? F21 C21 C20 121.0(4) . . ? C22 C21 C20 119.8(4) . . ? F22 C22 C21 121.0(4) . . ? F22 C22 C23 120.3(4) . . ? C21 C22 C23 118.7(4) . . ? F23 C23 C22 118.9(4) . . ? F23 C23 C24 120.9(4) . . ? C22 C23 C24 120.1(4) . . ? C19 C24 C23 123.0(4) . . ? C19 C24 F24 120.0(4) . . ? C23 C24 F24 117.0(4) . . ? O1 C25 Pd1 175.5(4) . . ? O2 C26 Pd2 176.5(4) . . ? C31 N C27 110.9(3) . . ? C31 N C39 105.4(3) . . ? C27 N C39 111.8(3) . . ? C31 N C35 111.2(3) . . ? C27 N C35 106.0(3) . . ? C39 N C35 111.6(3) . . ? N C27 C28 115.7(3) . . ? C27 C28 C29 108.1(3) . . ? C30 C29 C28 112.3(4) . . ? C32 C31 N 117.7(3) . . ? C31 C32 C33 108.2(3) . . ? C32 C33 C34 112.7(4) . . ? C36 C35 N 116.1(3) . . ? C35 C36 C37 109.5(3) . . ? C38 C37 C36 111.5(4) . . ? C40 C39 N 116.7(3) . . ? C39 C40 C41 109.2(3) . . ? C42 C41 C40 113.3(4) . . ? Cl2 C43 Cl3 115.7(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.186 _refine_diff_density_min -0.911 _refine_diff_density_rms 0.108 #=== END data_cis-[Pt(C6Cl5)2(CO)2] _database_code_depnum_ccdc_archive 'CCDC 762687' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H6 Cl10 O5 Pt' _chemical_formula_weight 803.78 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 20.206(2) _cell_length_b 12.5190(15) _cell_length_c 11.8245(13) _cell_angle_alpha 90.00 _cell_angle_beta 122.900(10) _cell_angle_gamma 90.00 _cell_volume 2511.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 21.7 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 6.675 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1351 _exptl_absorpt_correction_T_max 0.2394 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'enraf nonius CAD4' _diffrn_measurement_method 'w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1844 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max -3 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1844 _reflns_number_gt 1748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+15.0558P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1844 _refine_ls_number_parameters 141 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.0000 0.06374(3) 0.7500 0.03499(17) Uani 1 2 d S . . Cl1 Cl 0.08405(13) 0.2405(2) 1.0092(2) 0.0581(5) Uani 1 1 d . . . Cl2 Cl 0.19826(14) 0.4220(2) 1.0475(3) 0.0674(6) Uani 1 1 d . . . Cl3 Cl 0.25310(15) 0.4461(2) 0.8480(3) 0.0737(7) Uani 1 1 d . . . Cl4 Cl 0.19919(15) 0.2796(2) 0.6178(3) 0.0752(7) Uani 1 1 d . . . Cl5 Cl 0.08193(12) 0.10005(18) 0.5744(2) 0.0526(5) Uani 1 1 d . . . O1 O 0.1315(4) -0.0972(6) 0.8224(9) 0.0725(19) Uani 1 1 d . . . C1 C 0.0826(4) 0.1810(6) 0.7887(8) 0.0383(14) Uani 1 1 d . . . C2 C 0.1120(4) 0.2528(6) 0.8944(8) 0.0424(16) Uani 1 1 d . . . C3 C 0.1650(4) 0.3343(6) 0.9160(8) 0.0467(17) Uani 1 1 d . . . C4 C 0.1900(4) 0.3445(7) 0.8263(9) 0.0507(19) Uani 1 1 d . . . C5 C 0.1646(4) 0.2727(7) 0.7239(8) 0.0465(17) Uani 1 1 d . . . C6 C 0.1111(4) 0.1914(6) 0.7038(7) 0.0405(15) Uani 1 1 d . . . C7 C 0.0831(5) -0.0401(7) 0.7943(9) 0.0466(17) Uani 1 1 d . . . O2 O 0.0147(4) 0.4988(7) 0.6569(9) 0.086(2) Uani 1 1 d . . . O3 O 0.0181(11) 0.7094(11) 0.736(2) 0.086(5) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0393(2) 0.0311(2) 0.0457(3) 0.000 0.03035(18) 0.000 Cl1 0.0639(11) 0.0713(14) 0.0496(11) -0.0119(10) 0.0376(10) -0.0097(10) Cl2 0.0636(12) 0.0584(14) 0.0637(15) -0.0206(11) 0.0238(11) -0.0128(9) Cl3 0.0654(13) 0.0647(16) 0.0816(17) 0.0044(12) 0.0338(12) -0.0279(11) Cl4 0.0767(14) 0.0940(19) 0.0810(17) 0.0018(14) 0.0598(14) -0.0226(13) Cl5 0.0621(11) 0.0566(12) 0.0590(12) -0.0110(9) 0.0459(10) -0.0076(9) O1 0.075(4) 0.058(4) 0.111(6) 0.014(4) 0.068(4) 0.025(3) C1 0.034(3) 0.039(4) 0.045(4) 0.003(3) 0.024(3) -0.002(3) C2 0.040(3) 0.042(4) 0.048(4) 0.000(3) 0.026(3) 0.001(3) C3 0.045(4) 0.038(4) 0.048(4) -0.003(3) 0.019(3) -0.002(3) C4 0.040(3) 0.045(5) 0.061(5) 0.013(4) 0.023(3) -0.008(3) C5 0.042(4) 0.050(4) 0.053(5) 0.007(4) 0.030(3) -0.003(3) C6 0.040(3) 0.047(4) 0.042(4) 0.000(3) 0.027(3) 0.001(3) C7 0.047(4) 0.044(4) 0.059(5) -0.001(4) 0.036(4) -0.001(3) O2 0.064(4) 0.086(6) 0.090(6) -0.022(5) 0.029(4) 0.017(4) O3 0.130(11) 0.022(6) 0.135(12) -0.019(6) 0.091(9) -0.022(6) _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 Pt C7 1.956(8) 2_556 ? Pt C7 1.956(8) . ? Pt C1 2.078(7) . ? Pt C1 2.078(7) 2_556 ? Cl1 C2 1.737(7) . ? Cl2 C3 1.715(8) . ? Cl3 C4 1.719(7) . ? Cl4 C5 1.738(8) . ? Cl5 C6 1.737(8) . ? O1 C7 1.108(10) . ? C1 C2 1.385(11) . ? C1 C6 1.409(9) . ? C2 C3 1.398(10) . ? C3 C4 1.407(12) . ? C4 C5 1.364(12) . ? C5 C6 1.409(11) . ? 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 C7 Pt C7 96.7(5) 2_556 . ? C7 Pt C1 176.3(3) 2_556 . ? C7 Pt C1 86.6(3) . . ? C7 Pt C1 86.6(3) 2_556 2_556 ? C7 Pt C1 176.3(3) . 2_556 ? C1 Pt C1 90.1(4) . 2_556 ? C2 C1 C6 116.2(6) . . ? C2 C1 Pt 123.9(5) . . ? C6 C1 Pt 119.9(6) . . ? C1 C2 C3 123.3(7) . . ? C1 C2 Cl1 119.0(5) . . ? C3 C2 Cl1 117.7(6) . . ? C2 C3 C4 118.8(7) . . ? C2 C3 Cl2 121.1(6) . . ? C4 C3 Cl2 120.1(6) . . ? C5 C4 C3 119.6(7) . . ? C5 C4 Cl3 120.7(6) . . ? C3 C4 Cl3 119.7(7) . . ? C4 C5 C6 120.6(7) . . ? C4 C5 Cl4 120.2(6) . . ? C6 C5 Cl4 119.1(6) . . ? C5 C6 C1 121.4(7) . . ? C5 C6 Cl5 119.1(5) . . ? C1 C6 Cl5 119.5(6) . . ? O1 C7 Pt 178.1(9) . . ? _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.835 _refine_diff_density_max 0.972 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.138