# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Nakano, Hiroto' 'Fujita, Reiko' 'Kabuto, Chizuko' 'Okuyama, Yuko' 'Suzuki, Yuichiro' _publ_contact_author_name 'Dr Hiroto Nakano' _publ_contact_author_address ; Chemistry Department Tohoku Pharmaceutical University 4-4-1 Komatsushima, Aoba-ku Sendai Miyagi 981-8558 JAPAN ; _publ_contact_author_email 'HNAKANO@TOHOKU-PHARM.AC.JP' _publ_section_title ; Novel efficient chiral palladium-phosphinooxazolidine catalyst for enantioselective Diels-Alder reaction ; data__nakano-ligand1 _database_code_CSD 180368 # CHEMICAL DATA _chemical_formula_sum 'C36 H33 N O P ' _chemical_formula_moiety 'C36 H33 N O P ' _chemical_formula_weight 526.64 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 9.472(7) _cell_length_b 17.00(1) _cell_length_c 18.07(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2908(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4703 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13560 _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 1.6746 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.6746 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6280 _reflns_number_gt 1113 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.1044 _refine_ls_wR_factor_ref 0.1227 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1113 _refine_ls_number_parameters 158 _refine_ls_goodness_of_fit_ref 2.810 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.37 _refine_diff_density_min -0.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P(1) P -0.4469(5) -0.1597(3) -0.3998(3) 0.042(1) Uiso 1.00 d . . . O(1) O -0.572(1) -0.2317(6) -0.2117(6) 0.054(3) Uiso 1.00 d . . . N(1) N -0.345(1) -0.2800(7) -0.1918(6) 0.029(3) Uiso 1.00 d . . . C(1) C -0.439(2) -0.2428(10) -0.2474(10) 0.053(5) Uiso 1.00 d . . . C(2) C -0.206(2) -0.253(1) -0.200(1) 0.084(7) Uiso 1.00 d . . . C(3) C -0.188(2) -0.174(1) -0.160(1) 0.087(7) Uiso 1.00 d . . . C(4) C -0.325(2) -0.161(1) -0.1226(9) 0.055(5) Uiso 1.00 d . . . C(5) C -0.393(1) -0.2420(8) -0.1238(9) 0.034(4) Uiso 1.00 d . . . C(6) C -0.553(2) -0.2424(10) -0.1335(9) 0.051(5) Uiso 1.00 d . . . C(7) C -0.620(2) -0.3196(9) -0.1123(9) 0.047(5) Uiso 1.00 d . . . C(8) C -0.589(1) -0.3661(8) -0.0532(8) 0.027(4) Uiso 1.00 d . . . C(9) C -0.652(2) -0.435(1) -0.037(1) 0.060(6) Uiso 1.00 d . . . C(10) C -0.760(2) -0.460(1) -0.078(1) 0.063(6) Uiso 1.00 d . . . C(11) C -0.808(2) -0.418(1) -0.137(1) 0.076(7) Uiso 1.00 d . . . C(12) C -0.742(2) -0.348(1) -0.154(1) 0.073(6) Uiso 1.00 d . . . C(13) C -0.631(2) -0.176(1) -0.093(1) 0.059(5) Uiso 1.00 d . . . C(14) C -0.603(2) -0.162(1) -0.0175(10) 0.059(5) Uiso 1.00 d . . . C(15) C -0.675(2) -0.100(1) 0.017(1) 0.081(7) Uiso 1.00 d . . . C(16) C -0.774(2) -0.0566(10) -0.0170(10) 0.047(5) Uiso 1.00 d . . . C(17) C -0.800(2) -0.071(1) -0.092(1) 0.062(6) Uiso 1.00 d . . . C(18) C -0.732(2) -0.132(1) -0.1270(9) 0.047(5) Uiso 1.00 d . . . C(19) C -0.460(2) -0.2984(9) -0.3171(8) 0.034(4) Uiso 1.00 d . . . C(20) C -0.470(2) -0.380(1) -0.3045(10) 0.059(6) Uiso 1.00 d . . . C(21) C -0.472(2) -0.4280(10) -0.3677(10) 0.053(5) Uiso 1.00 d . . . C(22) C -0.478(1) -0.4003(8) -0.4361(8) 0.028(4) Uiso 1.00 d . . . C(23) C -0.471(2) -0.3180(10) -0.4467(10) 0.060(6) Uiso 1.00 d . . . C(24) C -0.467(2) -0.2679(8) -0.3877(9) 0.033(4) Uiso 1.00 d . . . C(25) C -0.622(1) -0.1265(9) -0.3653(8) 0.024(4) Uiso 1.00 d . . . C(26) C -0.743(2) -0.1678(9) -0.3626(8) 0.039(4) Uiso 1.00 d . . . C(27) C -0.867(2) -0.141(1) -0.3348(9) 0.050(5) Uiso 1.00 d . . . C(28) C -0.865(2) -0.061(1) -0.3102(9) 0.047(5) Uiso 1.00 d . . . C(29) C -0.751(2) -0.013(1) -0.313(1) 0.072(6) Uiso 1.00 d . . . C(30) C -0.625(2) -0.046(1) -0.340(1) 0.059(5) Uiso 1.00 d . . . C(31) C -0.466(2) -0.1471(9) -0.5041(8) 0.040(4) Uiso 1.00 d . . . C(32) C -0.594(2) -0.152(1) -0.5374(10) 0.055(5) Uiso 1.00 d . . . C(33) C -0.600(2) -0.1396(9) -0.6157(9) 0.045(5) Uiso 1.00 d . . . C(34) C -0.476(2) -0.1274(8) -0.6548(8) 0.032(4) Uiso 1.00 d . . . C(35) C -0.357(2) -0.124(1) -0.618(1) 0.063(6) Uiso 1.00 d . . . C(36) C -0.343(1) -0.1351(8) -0.5419(9) 0.030(4) Uiso 1.00 d . . . H(1) H -0.4148 -0.1918 -0.2624 0.0783 Uiso 1.00 calc . . . H(2) H -0.1738 -0.2519 -0.2519 0.0952 Uiso 1.00 calc . . . H(3) H -0.1357 -0.2903 -0.1766 0.0952 Uiso 1.00 calc . . . H(4) H -0.1715 -0.1288 -0.2009 0.1031 Uiso 1.00 calc . . . H(5) H -0.1054 -0.1662 -0.1307 0.1031 Uiso 1.00 calc . . . H(6) H -0.3811 -0.1210 -0.1476 0.0812 Uiso 1.00 calc . . . H(7) H -0.3073 -0.1422 -0.0736 0.0812 Uiso 1.00 calc . . . H(8) H -0.3638 -0.2727 -0.0826 0.0784 Uiso 1.00 calc . . . H(9) H -0.5141 -0.3479 -0.0185 0.0640 Uiso 1.00 calc . . . H(10) H -0.6208 -0.4667 0.0059 0.0859 Uiso 1.00 calc . . . H(11) H -0.8076 -0.5098 -0.0656 0.1154 Uiso 1.00 calc . . . H(12) H -0.8894 -0.4310 -0.1703 0.1322 Uiso 1.00 calc . . . H(13) H -0.7788 -0.3133 -0.1904 0.1095 Uiso 1.00 calc . . . H(14) H -0.5425 -0.1995 0.0096 0.0993 Uiso 1.00 calc . . . H(15) H -0.6471 -0.0836 0.0695 0.1009 Uiso 1.00 calc . . . H(16) H -0.8219 -0.0140 0.0096 0.0590 Uiso 1.00 calc . . . H(17) H -0.8668 -0.0381 -0.1128 0.0992 Uiso 1.00 calc . . . H(18) H -0.7556 -0.1398 -0.1792 0.0784 Uiso 1.00 calc . . . H(19) H -0.4835 -0.3987 -0.2519 0.0698 Uiso 1.00 calc . . . H(20) H -0.4746 -0.4856 -0.3593 0.0794 Uiso 1.00 calc . . . H(21) H -0.4762 -0.4363 -0.4792 0.0628 Uiso 1.00 calc . . . H(22) H -0.4677 -0.2965 -0.4974 0.0818 Uiso 1.00 calc . . . H(23) H -0.7366 -0.2204 -0.3845 0.0574 Uiso 1.00 calc . . . H(24) H -0.9465 -0.1721 -0.3345 0.0837 Uiso 1.00 calc . . . H(25) H -0.9576 -0.0395 -0.2927 0.0789 Uiso 1.00 calc . . . H(26) H -0.7521 0.0406 -0.2982 0.0898 Uiso 1.00 calc . . . H(27) H -0.5353 -0.0141 -0.3415 0.0645 Uiso 1.00 calc . . . H(28) H -0.6800 -0.1611 -0.5057 0.0789 Uiso 1.00 calc . . . H(29) H -0.6933 -0.1426 -0.6401 0.0845 Uiso 1.00 calc . . . H(30) H -0.4801 -0.1213 -0.7082 0.0677 Uiso 1.00 calc . . . H(31) H -0.2675 -0.1132 -0.6447 0.0736 Uiso 1.00 calc . . . H(32) H -0.2494 -0.1369 -0.5165 0.0538 Uiso 1.00 calc . . . H(33) H -0.3227 -0.1411 -0.3742 0.0292 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 ? ? ? ? ? ? ? #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P(1) C(24) 1.86(2) . . yes P(1) C(25) 1.86(2) . . yes P(1) C(31) 1.91(3) . . yes O(1) C(1) 1.42(3) . . yes O(1) C(6) 1.43(3) . . yes N(1) C(1) 1.48(3) . . yes N(1) C(2) 1.41(4) . . yes N(1) C(5) 1.46(3) . . yes C(1) C(19) 1.59(3) . . yes C(2) C(3) 1.53(4) . . yes C(3) C(4) 1.48(4) . . yes C(4) C(5) 1.52(3) . . yes C(5) C(6) 1.53(4) . . yes C(6) C(7) 1.50(3) . . yes C(6) C(13) 1.54(4) . . yes C(7) C(8) 1.36(3) . . yes C(7) C(12) 1.46(4) . . yes C(8) C(9) 1.34(3) . . yes C(9) C(10) 1.33(4) . . yes C(10) C(11) 1.36(4) . . yes C(11) C(12) 1.38(4) . . yes C(13) C(14) 1.41(4) . . yes C(13) C(18) 1.37(3) . . yes C(14) C(15) 1.41(4) . . yes C(15) C(16) 1.34(4) . . yes C(16) C(17) 1.39(4) . . yes C(17) C(18) 1.36(4) . . yes C(19) C(20) 1.41(3) . . yes C(19) C(24) 1.38(3) . . yes C(20) C(21) 1.40(3) . . yes C(21) C(22) 1.32(3) . . yes C(22) C(23) 1.41(3) . . yes C(23) C(24) 1.36(3) . . yes C(25) C(26) 1.35(3) . . yes C(25) C(30) 1.44(3) . . yes C(26) C(27) 1.36(3) . . yes C(27) C(28) 1.43(3) . . yes C(28) C(29) 1.36(4) . . yes C(29) C(30) 1.41(4) . . yes C(31) C(32) 1.36(3) . . yes C(31) C(36) 1.37(3) . . yes C(32) C(33) 1.43(3) . . yes C(33) C(34) 1.39(3) . . yes C(34) C(35) 1.30(4) . . yes C(35) C(36) 1.40(3) . . yes P(1) H(33) 1.303 . . no C(1) H(1) 0.936 . . no C(2) H(2) 0.986 . . no C(2) H(3) 1.014 . . no C(3) H(4) 1.082 . . no C(3) H(5) 0.954 . . no C(4) H(6) 0.978 . . no C(4) H(7) 0.957 . . no C(5) H(8) 0.949 . . no C(8) H(9) 0.998 . . no C(9) H(10) 0.990 . . no C(10) H(11) 0.990 . . no C(11) H(12) 1.005 . . no C(12) H(13) 0.956 . . no C(14) H(14) 0.984 . . no C(15) H(15) 1.023 . . no C(16) H(16) 0.980 . . no C(17) H(17) 0.932 . . no C(18) H(18) 0.978 . . no C(20) H(19) 1.010 . . no C(21) H(20) 0.992 . . no C(22) H(21) 0.990 . . no C(23) H(22) 0.985 . . no C(26) H(23) 0.979 . . no C(27) H(24) 0.924 . . no C(28) H(25) 0.995 . . no C(29) H(26) 0.947 . . no C(30) H(27) 1.013 . . no C(32) H(28) 1.007 . . no C(33) H(29) 0.991 . . no C(34) H(30) 0.971 . . no C(35) H(31) 0.988 . . no C(36) H(32) 0.997 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(24) P(1) C(25) 99(1) . . . yes C(24) P(1) C(31) 102(1) . . . yes C(25) P(1) C(31) 102(1) . . . yes C(1) O(1) C(6) 108(2) . . . yes C(1) N(1) C(2) 110(2) . . . yes C(1) N(1) C(5) 101(1) . . . yes C(2) N(1) C(5) 103(2) . . . yes O(1) C(1) N(1) 106(2) . . . yes O(1) C(1) C(19) 109(2) . . . yes N(1) C(1) C(19) 110(2) . . . yes N(1) C(2) C(3) 110(2) . . . yes C(2) C(3) C(4) 104(2) . . . yes C(3) C(4) C(5) 103(2) . . . yes N(1) C(5) C(4) 106(2) . . . yes N(1) C(5) C(6) 101(2) . . . yes C(4) C(5) C(6) 115(2) . . . yes O(1) C(6) C(5) 103(2) . . . yes O(1) C(6) C(7) 108(2) . . . yes O(1) C(6) C(13) 108(2) . . . yes C(5) C(6) C(7) 113(2) . . . yes C(5) C(6) C(13) 114(2) . . . yes C(7) C(6) C(13) 108(2) . . . yes C(6) C(7) C(8) 128(2) . . . yes C(6) C(7) C(12) 119(2) . . . yes C(8) C(7) C(12) 112(2) . . . yes C(7) C(8) C(9) 125(2) . . . yes C(8) C(9) C(10) 119(3) . . . yes C(9) C(10) C(11) 121(3) . . . yes C(10) C(11) C(12) 118(3) . . . yes C(7) C(12) C(11) 122(3) . . . yes C(6) C(13) C(14) 119(2) . . . yes C(6) C(13) C(18) 121(2) . . . yes C(14) C(13) C(18) 118(2) . . . yes C(13) C(14) C(15) 117(3) . . . yes C(14) C(15) C(16) 123(3) . . . yes C(15) C(16) C(17) 117(3) . . . yes C(16) C(17) C(18) 120(2) . . . yes C(13) C(18) C(17) 122(2) . . . yes C(1) C(19) C(20) 117(2) . . . yes C(1) C(19) C(24) 121(2) . . . yes C(20) C(19) C(24) 121(2) . . . yes C(19) C(20) C(21) 116(2) . . . yes C(20) C(21) C(22) 123(2) . . . yes C(21) C(22) C(23) 118(2) . . . yes C(22) C(23) C(24) 120(2) . . . yes P(1) C(24) C(19) 118(1) . . . yes P(1) C(24) C(23) 121(2) . . . yes C(19) C(24) C(23) 119(2) . . . yes P(1) C(25) C(26) 127(2) . . . yes P(1) C(25) C(30) 114(1) . . . yes C(26) C(25) C(30) 117(2) . . . yes C(25) C(26) C(27) 125(2) . . . yes C(26) C(27) C(28) 115(2) . . . yes C(27) C(28) C(29) 124(2) . . . yes C(28) C(29) C(30) 116(2) . . . yes C(25) C(30) C(29) 120(2) . . . yes P(1) C(31) C(32) 120(2) . . . yes P(1) C(31) C(36) 115(2) . . . yes C(32) C(31) C(36) 123(2) . . . yes C(31) C(32) C(33) 117(2) . . . yes C(32) C(33) C(34) 119(2) . . . yes C(33) C(34) C(35) 118(2) . . . yes C(34) C(35) C(36) 125(3) . . . yes C(31) C(36) C(35) 115(2) . . . yes C(24) P(1) H(33) 107.0 . . . no C(25) P(1) H(33) 127.7 . . . no C(31) P(1) H(33) 114.1 . . . no O(1) C(1) H(1) 103.1 . . . no N(1) C(1) H(1) 116.2 . . . no C(19) C(1) H(1) 110.6 . . . no N(1) C(2) H(2) 113.5 . . . no N(1) C(2) H(3) 111.5 . . . no C(3) C(2) H(2) 113.6 . . . no C(3) C(2) H(3) 105.9 . . . no H(2) C(2) H(3) 101.7 . . . no C(2) C(3) H(4) 108.5 . . . no C(2) C(3) H(5) 119.0 . . . no C(4) C(3) H(4) 109.2 . . . no C(4) C(3) H(5) 116.2 . . . no H(4) C(3) H(5) 99.1 . . . no C(3) C(4) H(6) 111.9 . . . no C(3) C(4) H(7) 108.8 . . . no C(5) C(4) H(6) 113.2 . . . no C(5) C(4) H(7) 113.1 . . . no H(6) C(4) H(7) 106.6 . . . no N(1) C(5) H(8) 109.1 . . . no C(4) C(5) H(8) 111.3 . . . no C(6) C(5) H(8) 112.0 . . . no C(7) C(8) H(9) 117.6 . . . no C(9) C(8) H(9) 116.7 . . . no C(8) C(9) H(10) 120.8 . . . no C(10) C(9) H(10) 119.5 . . . no C(9) C(10) H(11) 119.8 . . . no C(11) C(10) H(11) 118.3 . . . no C(10) C(11) H(12) 127.9 . . . no C(12) C(11) H(12) 113.9 . . . no C(7) C(12) H(13) 116.0 . . . no C(11) C(12) H(13) 121.6 . . . no C(13) C(14) H(14) 118.9 . . . no C(15) C(14) H(14) 123.3 . . . no C(14) C(15) H(15) 119.0 . . . no C(16) C(15) H(15) 117.4 . . . no C(15) C(16) H(16) 120.2 . . . no C(17) C(16) H(16) 121.8 . . . no C(16) C(17) H(17) 114.0 . . . no C(18) C(17) H(17) 125.6 . . . no C(13) C(18) H(18) 120.9 . . . no C(17) C(18) H(18) 116.9 . . . no C(19) C(20) H(19) 118.2 . . . no C(21) C(20) H(19) 125.5 . . . no C(20) C(21) H(20) 116.7 . . . no C(22) C(21) H(20) 119.6 . . . no C(21) C(22) H(21) 121.0 . . . no C(23) C(22) H(21) 120.2 . . . no C(22) C(23) H(22) 119.6 . . . no C(24) C(23) H(22) 119.5 . . . no C(25) C(26) H(23) 114.0 . . . no C(27) C(26) H(23) 121.0 . . . no C(26) C(27) H(24) 120.8 . . . no C(28) C(27) H(24) 123.7 . . . no C(27) C(28) H(25) 115.6 . . . no C(29) C(28) H(25) 119.9 . . . no C(28) C(29) H(26) 123.6 . . . no C(30) C(29) H(26) 119.8 . . . no C(25) C(30) H(27) 119.0 . . . no C(29) C(30) H(27) 120.2 . . . no C(31) C(32) H(28) 118.8 . . . no C(33) C(32) H(28) 123.7 . . . no C(32) C(33) H(29) 117.7 . . . no C(34) C(33) H(29) 122.7 . . . no C(33) C(34) H(30) 119.0 . . . no C(35) C(34) H(30) 122.3 . . . no C(34) C(35) H(31) 120.3 . . . no C(36) C(35) H(31) 114.7 . . . no C(31) C(36) H(32) 121.5 . . . no C(35) C(36) H(32) 122.9 . . . no #------------------------------------------------------------------------------ #===END data_nakano-Pdcomplex-4 _database_code_CSD 180369 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C73.50 H66.50 Cl8.50 N2 O2.50 P2 Pd2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1593.94 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 10.641(3) _cell_length_b 18.805(5) _cell_length_c 34.692(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6942(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15438 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.080 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.928 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53295 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 1.7951 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.7951 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15705 _reflns_number_gt 7688 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0605 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7688 _refine_ls_number_parameters 835 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.0454 _refine_diff_density_max 0.71 _refine_diff_density_min -0.74 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 1.10707(7) 0.17869(4) 0.82487(2) 0.0257(2) Uani 1.00 d . . . Pd(2) Pd 0.54190(10) 0.61011(5) 0.88612(3) 0.0542(3) Uani 1.00 d . . . Cl(1) Cl 1.2105(2) 0.0866(1) 0.79476(7) 0.0383(7) Uani 1.00 d . . . Cl(2) Cl 1.2734(2) 0.2579(2) 0.80659(7) 0.0395(7) Uani 1.00 d . . . Cl(3) Cl 0.5017(4) 0.6062(3) 0.9506(1) 0.094(1) Uani 1.00 d . . . Cl(4) Cl 0.3297(4) 0.5780(2) 0.8752(1) 0.093(1) Uani 1.00 d . . . Cl(5) Cl 0.5928(5) 0.8508(2) 0.7972(2) 0.122(2) Uani 1.00 d . . . Cl(6) Cl 0.6350(7) 0.9312(3) 0.8680(2) 0.160(3) Uani 1.00 d . . . Cl(7) Cl 0.4087(4) 0.9530(2) 0.8262(1) 0.090(1) Uani 1.00 d . . . Cl(8) Cl 0.2751(8) 0.7678(3) 0.8657(2) 0.068(2) Uani 0.50 d P . . Cl(9) Cl 0.124(1) 0.7443(8) 0.9292(4) 0.170(5) Uani 0.50 d P . . Cl(10) Cl 0.314(1) 0.8201(6) 0.9401(3) 0.154(5) Uani 0.50 d P . . P(1) P 0.9455(2) 0.1048(1) 0.83158(7) 0.0313(7) Uani 1.00 d . . . P(2) P 0.7271(4) 0.6570(2) 0.90117(8) 0.0523(9) Uani 1.00 d . . . O(1) O 0.9597(6) 0.2034(3) 0.9114(2) 0.025(2) Uani 1.00 d . . . O(2) O 0.7563(6) 0.5374(3) 0.8330(2) 0.033(2) Uani 1.00 d . . . O(100) O 1.303(2) 0.475(1) 0.9574(6) 0.084(6) Uiso 0.50 d P . . N(1) N 1.0259(7) 0.2614(4) 0.8568(2) 0.023(2) Uani 1.00 d . . . N(2) N 0.5767(7) 0.6010(4) 0.8265(2) 0.038(2) Uani 1.00 d . . . C(1) C 0.9118(8) 0.2471(4) 0.8818(2) 0.021(2) Uani 1.00 d . . . C(2) C 1.0858(8) 0.2301(5) 0.9214(2) 0.024(2) Uani 1.00 d . . . C(3) C 1.1167(9) 0.2810(4) 0.8879(2) 0.023(2) Uani 1.00 d . . . C(4) C 1.0988(10) 0.3614(5) 0.8938(3) 0.033(2) Uani 1.00 d . . . C(5) C 1.0761(9) 0.3880(6) 0.8523(3) 0.039(3) Uani 1.00 d . . . C(6) C 1.0009(8) 0.3280(5) 0.8330(2) 0.030(2) Uani 1.00 d . . . C(7) C 0.7983(8) 0.2143(5) 0.8639(2) 0.025(2) Uani 1.00 d . . . C(8) C 0.6859(8) 0.2485(5) 0.8699(3) 0.030(2) Uani 1.00 d . . . C(9) C 0.5716(9) 0.2215(6) 0.8566(3) 0.038(3) Uani 1.00 d . . . C(10) C 0.5739(9) 0.1567(6) 0.8364(3) 0.040(3) Uani 1.00 d . . . C(11) C 0.6854(9) 0.1230(6) 0.8297(3) 0.041(3) Uani 1.00 d . . . C(12) C 0.8003(9) 0.1499(5) 0.8432(3) 0.031(2) Uani 1.00 d . . . C(13) C 1.0839(9) 0.2692(5) 0.9601(2) 0.028(2) Uani 1.00 d . . . C(14) C 0.9717(10) 0.2887(5) 0.9773(3) 0.034(3) Uani 1.00 d . . . C(15) C 0.972(1) 0.3273(6) 1.0119(3) 0.045(3) Uani 1.00 d . . . C(16) C 1.086(1) 0.3436(6) 1.0292(3) 0.049(3) Uani 1.00 d . . . C(17) C 1.196(1) 0.3243(7) 1.0124(3) 0.054(3) Uani 1.00 d . . . C(18) C 1.196(1) 0.2868(6) 0.9781(3) 0.041(3) Uani 1.00 d . . . C(19) C 1.1680(8) 0.1631(4) 0.9238(2) 0.022(2) Uani 1.00 d . . . C(20) C 1.2740(9) 0.1495(5) 0.9019(2) 0.026(2) Uani 1.00 d . . . C(21) C 1.3344(9) 0.0844(5) 0.9050(3) 0.033(3) Uani 1.00 d . . . C(22) C 1.294(1) 0.0346(5) 0.9297(3) 0.041(3) Uani 1.00 d . . . C(23) C 1.193(1) 0.0459(5) 0.9532(3) 0.040(3) Uani 1.00 d . . . C(24) C 1.1301(9) 0.1100(5) 0.9496(3) 0.031(3) Uani 1.00 d . . . C(25) C 0.9088(10) 0.0663(6) 0.7846(3) 0.040(2) Uani 1.00 d . . . C(26) C 0.906(1) 0.1128(7) 0.7531(3) 0.045(3) Uani 1.00 d . . . C(27) C 0.867(1) 0.0892(7) 0.7177(3) 0.055(3) Uani 1.00 d . . . C(28) C 0.829(1) 0.0198(8) 0.7131(4) 0.063(4) Uani 1.00 d . . . C(29) C 0.828(1) -0.0268(7) 0.7433(4) 0.058(4) Uani 1.00 d . . . C(30) C 0.870(1) -0.0039(7) 0.7799(4) 0.055(3) Uani 1.00 d . . . C(31) C 0.958(1) 0.0321(5) 0.8670(3) 0.039(3) Uani 1.00 d . . . C(32) C 1.051(1) -0.0164(5) 0.8633(3) 0.042(3) Uani 1.00 d . . . C(33) C 1.060(1) -0.0706(6) 0.8901(4) 0.058(4) Uani 1.00 d . . . C(34) C 0.978(2) -0.0769(7) 0.9188(4) 0.072(5) Uani 1.00 d . . . C(35) C 0.883(2) -0.0265(8) 0.9232(5) 0.085(5) Uani 1.00 d . . . C(36) C 0.874(1) 0.0283(6) 0.8966(4) 0.053(4) Uani 1.00 d . . . C(101) C 0.7120(9) 0.5996(5) 0.8147(3) 0.032(2) Uani 1.00 d . . . C(102) C 0.6593(9) 0.4831(5) 0.8279(3) 0.028(2) Uani 1.00 d . . . C(103) C 0.5425(10) 0.5262(5) 0.8147(3) 0.036(2) Uani 1.00 d . . . C(104) C 0.5180(10) 0.5311(6) 0.7707(3) 0.040(3) Uani 1.00 d . . . C(105) C 0.488(1) 0.6105(6) 0.7635(3) 0.051(3) Uani 1.00 d . . . C(106) C 0.501(1) 0.6481(6) 0.8017(3) 0.045(3) Uani 1.00 d . . . C(107) C 0.7861(10) 0.6655(5) 0.8230(3) 0.039(3) Uani 1.00 d . . . C(108) C 0.8382(10) 0.6997(6) 0.7906(3) 0.037(3) Uani 1.00 d . . . C(109) C 0.905(1) 0.7618(6) 0.7940(3) 0.052(3) Uani 1.00 d . . . C(110) C 0.923(1) 0.7909(6) 0.8297(3) 0.060(4) Uani 1.00 d . . . C(111) C 0.872(2) 0.7585(6) 0.8622(3) 0.064(4) Uani 1.00 d . . . C(112) C 0.803(1) 0.6969(6) 0.8589(3) 0.049(3) Uani 1.00 d . . . C(113) C 0.7043(9) 0.4276(5) 0.7982(3) 0.030(2) Uani 1.00 d . . . C(114) C 0.8072(9) 0.4391(5) 0.7751(3) 0.032(3) Uani 1.00 d . . . C(115) C 0.8444(10) 0.3897(6) 0.7484(3) 0.039(3) Uani 1.00 d . . . C(116) C 0.776(1) 0.3270(6) 0.7442(3) 0.041(3) Uani 1.00 d . . . C(117) C 0.672(1) 0.3158(6) 0.7662(3) 0.042(3) Uani 1.00 d . . . C(118) C 0.635(1) 0.3653(5) 0.7935(3) 0.039(3) Uani 1.00 d . . . C(119) C 0.639(1) 0.4461(5) 0.8673(3) 0.035(3) Uani 1.00 d . . . C(120) C 0.739(1) 0.4410(5) 0.8932(3) 0.039(3) Uani 1.00 d . . . C(121) C 0.721(1) 0.4078(6) 0.9290(3) 0.052(3) Uani 1.00 d . . . C(122) C 0.608(2) 0.3808(7) 0.9390(3) 0.059(3) Uani 1.00 d . . . C(123) C 0.511(1) 0.3866(7) 0.9143(3) 0.057(3) Uani 1.00 d . . . C(124) C 0.524(1) 0.4185(6) 0.8784(3) 0.047(3) Uani 1.00 d . . . C(125) C 0.712(2) 0.7316(7) 0.9348(4) 0.090(5) Uani 1.00 d . . . C(126) C 0.610(3) 0.7752(8) 0.9333(5) 0.122(7) Uani 1.00 d . . . C(127) C 0.603(4) 0.8346(10) 0.9587(6) 0.20(1) Uani 1.00 d . . . C(128) C 0.699(4) 0.844(1) 0.9851(7) 0.20(1) Uani 1.00 d . . . C(129) C 0.797(3) 0.803(1) 0.9855(5) 0.18(1) Uani 1.00 d . . . C(130) C 0.809(2) 0.7454(8) 0.9613(4) 0.111(6) Uani 1.00 d . . . C(131) C 0.845(1) 0.6001(6) 0.9228(3) 0.049(3) Uani 1.00 d . . . C(132) C 0.827(1) 0.5697(7) 0.9591(3) 0.064(4) Uani 1.00 d . . . C(133) C 0.914(2) 0.5288(9) 0.9761(4) 0.075(5) Uani 1.00 d . . . C(134) C 1.024(1) 0.5132(7) 0.9573(4) 0.067(4) Uani 1.00 d . . . C(135) C 1.048(1) 0.5422(7) 0.9210(4) 0.060(4) Uani 1.00 d . . . C(136) C 0.960(1) 0.5842(6) 0.9045(3) 0.051(3) Uani 1.00 d . . . C(201) C 0.518(2) 0.8873(10) 0.8383(6) 0.120(6) Uani 1.00 d . . . C(202) C 0.245(2) 0.746(1) 0.9112(5) 0.100(5) Uani 0.97 d P . . H(1) H 0.8865 0.2915 0.8931 0.0283 Uiso 1.00 calc . . . H(2) H 1.2009 0.2727 0.8789 0.0292 Uiso 1.00 calc . . . H(3) H 1.0293 0.3713 0.9101 0.0410 Uiso 1.00 calc . . . H(4) H 1.1725 0.3831 0.9049 0.0410 Uiso 1.00 calc . . . H(5) H 1.0296 0.4321 0.8520 0.0532 Uiso 1.00 calc . . . H(6) H 1.1541 0.3967 0.8389 0.0532 Uiso 1.00 calc . . . H(7) H 1.0293 0.3212 0.8069 0.0361 Uiso 1.00 calc . . . H(8) H 0.9139 0.3395 0.8323 0.0361 Uiso 1.00 calc . . . H(9) H 0.6866 0.2935 0.8839 0.0383 Uiso 1.00 calc . . . H(10) H 0.4926 0.2444 0.8620 0.0466 Uiso 1.00 calc . . . H(11) H 0.4965 0.1376 0.8261 0.0445 Uiso 1.00 calc . . . H(12) H 0.6861 0.0781 0.8163 0.0518 Uiso 1.00 calc . . . H(13) H 0.8941 0.2766 0.9644 0.0427 Uiso 1.00 calc . . . H(14) H 0.8908 0.3408 1.0238 0.0554 Uiso 1.00 calc . . . H(15) H 1.0887 0.3704 1.0530 0.0584 Uiso 1.00 calc . . . H(16) H 1.2770 0.3353 1.0250 0.0603 Uiso 1.00 calc . . . H(17) H 1.2755 0.2745 0.9660 0.0532 Uiso 1.00 calc . . . H(18) H 1.3037 0.1867 0.8842 0.0308 Uiso 1.00 calc . . . H(19) H 1.4075 0.0747 0.8891 0.0402 Uiso 1.00 calc . . . H(20) H 1.3380 -0.0096 0.9312 0.0497 Uiso 1.00 calc . . . H(21) H 1.1641 0.0105 0.9715 0.0478 Uiso 1.00 calc . . . H(22) H 1.0572 0.1191 0.9661 0.0394 Uiso 1.00 calc . . . H(23) H 0.9359 0.1621 0.7565 0.0571 Uiso 1.00 calc . . . H(24) H 0.8615 0.1211 0.6962 0.0671 Uiso 1.00 calc . . . H(25) H 0.8063 0.0019 0.6878 0.0822 Uiso 1.00 calc . . . H(26) H 0.7973 -0.0770 0.7408 0.0788 Uiso 1.00 calc . . . H(27) H 0.8725 -0.0363 0.8022 0.0680 Uiso 1.00 calc . . . H(28) H 1.1121 -0.0128 0.8421 0.0478 Uiso 1.00 calc . . . H(29) H 1.1274 -0.1056 0.8888 0.0673 Uiso 1.00 calc . . . H(30) H 0.9841 -0.1154 0.9370 0.0871 Uiso 1.00 calc . . . H(31) H 0.8171 -0.0310 0.9449 0.1040 Uiso 1.00 calc . . . H(32) H 0.8110 0.0675 0.8993 0.0653 Uiso 1.00 calc . . . H(101) H 0.7153 0.5915 0.7871 0.0399 Uiso 1.00 calc . . . H(102) H 0.4682 0.5105 0.8282 0.0444 Uiso 1.00 calc . . . H(103) H 0.5914 0.5165 0.7562 0.0531 Uiso 1.00 calc . . . H(104) H 0.4498 0.5008 0.7627 0.0531 Uiso 1.00 calc . . . H(105) H 0.5431 0.6301 0.7445 0.0648 Uiso 1.00 calc . . . H(106) H 0.4030 0.6154 0.7540 0.0648 Uiso 1.00 calc . . . H(107) H 0.4223 0.6591 0.8133 0.0549 Uiso 1.00 calc . . . H(108) H 0.5454 0.6939 0.7985 0.0549 Uiso 1.00 calc . . . H(109) H 0.8281 0.6775 0.7658 0.0432 Uiso 1.00 calc . . . H(110) H 0.9356 0.7857 0.7714 0.0624 Uiso 1.00 calc . . . H(111) H 0.9702 0.8351 0.8323 0.0721 Uiso 1.00 calc . . . H(112) H 0.8811 0.7804 0.8875 0.0670 Uiso 1.00 calc . . . H(113) H 0.8541 0.4830 0.7777 0.0382 Uiso 1.00 calc . . . H(114) H 0.9186 0.4001 0.7328 0.0488 Uiso 1.00 calc . . . H(115) H 0.8020 0.2902 0.7254 0.0514 Uiso 1.00 calc . . . H(116) H 0.6213 0.2730 0.7636 0.0475 Uiso 1.00 calc . . . H(117) H 0.5592 0.3563 0.8091 0.0506 Uiso 1.00 calc . . . H(118) H 0.5428 0.7664 0.9135 0.1565 Uiso 1.00 calc . . . H(119) H 0.5358 0.8686 0.9578 0.2096 Uiso 1.00 calc . . . H(120) H 0.6884 0.8804 1.0042 0.2229 Uiso 1.00 calc . . . H(121) H 0.8637 0.8159 1.0035 0.2034 Uiso 1.00 calc . . . H(122) H 0.8905 0.7110 0.9633 0.1438 Uiso 1.00 calc . . . H(123) H 0.7461 0.5794 0.9722 0.0749 Uiso 1.00 calc . . . H(124) H 0.8988 0.5103 1.0011 0.0916 Uiso 1.00 calc . . . H(125) H 1.0893 0.4843 0.9704 0.0818 Uiso 1.00 calc . . . H(126) H 1.1271 0.5330 0.9074 0.0695 Uiso 1.00 calc . . . H(127) H 0.9753 0.6036 0.8793 0.0613 Uiso 1.00 calc . . . H(128) H 0.8184 0.4600 0.8866 0.0467 Uiso 1.00 calc . . . H(129) H 0.7897 0.4044 0.9465 0.0619 Uiso 1.00 calc . . . H(130) H 0.5973 0.3579 0.9632 0.0702 Uiso 1.00 calc . . . H(131) H 0.4314 0.3682 0.9217 0.0681 Uiso 1.00 calc . . . H(132) H 0.4534 0.4214 0.8615 0.0564 Uiso 1.00 calc . . . H(201) H 0.4782 0.8476 0.8529 0.1236 Uiso 1.00 calc . . . H(202) H 0.2836 0.7016 0.9180 0.1474 Uiso 0.50 calc P . . H(203) H 1.3618 0.4616 0.9377 0.1008 Uiso 0.50 calc P . . H(204) H 1.3581 0.4763 0.9878 0.0442 Uiso 0.50 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0223(3) 0.0350(4) 0.0198(3) 0.0055(3) 0.0008(3) 0.0015(3) Pd(2) 0.0638(6) 0.0516(6) 0.0473(5) -0.0073(5) 0.0339(5) -0.0087(5) Cl(1) 0.034(1) 0.049(2) 0.031(1) 0.016(1) 0.004(1) -0.002(1) Cl(2) 0.029(1) 0.055(2) 0.034(1) -0.001(1) 0.009(1) 0.008(1) Cl(3) 0.103(3) 0.124(3) 0.055(2) -0.003(3) 0.052(2) 0.003(2) Cl(4) 0.056(2) 0.115(3) 0.107(3) -0.001(2) 0.051(2) -0.021(3) Cl(5) 0.088(3) 0.068(3) 0.210(6) 0.014(2) -0.027(4) -0.019(3) Cl(6) 0.176(6) 0.126(5) 0.177(6) -0.044(4) -0.095(5) 0.034(4) Cl(7) 0.109(3) 0.080(2) 0.082(2) 0.016(2) -0.017(3) -0.002(2) Cl(8) 0.099(6) 0.039(3) 0.067(4) 0.034(4) 0.015(4) 0.008(3) Cl(9) 0.087(7) 0.21(1) 0.21(1) 0.059(8) 0.038(7) 0.17(1) Cl(10) 0.24(1) 0.074(6) 0.149(10) 0.061(8) -0.064(9) -0.002(7) P(1) 0.030(1) 0.033(1) 0.031(1) -0.001(1) 0.000(1) -0.009(1) P(2) 0.087(2) 0.043(2) 0.027(1) -0.022(2) 0.024(1) -0.010(1) O(1) 0.023(3) 0.032(4) 0.019(3) -0.007(3) -0.002(3) 0.003(2) O(2) 0.035(4) 0.031(3) 0.034(4) -0.013(3) 0.008(3) -0.008(3) N(1) 0.023(4) 0.028(3) 0.019(4) -0.001(3) -0.002(2) 0.009(2) N(2) 0.038(4) 0.033(4) 0.042(2) -0.011(3) 0.019(4) -0.008(4) C(1) 0.028(4) 0.017(4) 0.019(4) -0.003(3) 0.004(3) -0.006(3) C(2) 0.021(4) 0.026(4) 0.025(4) 0.001(3) 0.005(4) 0.001(3) C(3) 0.020(4) 0.028(3) 0.022(4) -0.001(4) 0.002(3) 0.002(3) C(4) 0.031(5) 0.031(4) 0.037(4) -0.003(5) -0.005(5) -0.010(4) C(5) 0.040(7) 0.034(5) 0.043(5) -0.007(5) 0.000(4) 0.011(4) C(6) 0.031(5) 0.034(4) 0.027(5) 0.006(4) 0.003(4) 0.014(4) C(7) 0.018(4) 0.036(5) 0.020(4) -0.003(3) 0.001(3) 0.003(3) C(8) 0.018(4) 0.043(6) 0.027(5) -0.002(3) 0.007(4) 0.002(4) C(9) 0.016(4) 0.057(6) 0.040(6) 0.003(4) -0.001(4) -0.002(5) C(10) 0.018(4) 0.063(6) 0.040(6) -0.013(4) 0.002(4) -0.008(4) C(11) 0.028(4) 0.061(7) 0.033(6) -0.005(4) -0.001(4) -0.020(5) C(12) 0.026(3) 0.041(5) 0.025(5) 0.001(3) -0.003(4) -0.007(4) C(13) 0.031(4) 0.032(5) 0.022(4) -0.003(4) 0.003(3) 0.002(3) C(14) 0.031(5) 0.033(6) 0.038(5) -0.001(5) 0.009(4) -0.004(4) C(15) 0.065(6) 0.042(7) 0.029(5) 0.012(6) 0.010(5) 0.003(4) C(16) 0.073(6) 0.045(7) 0.029(5) 0.022(6) -0.007(5) -0.014(5) C(17) 0.053(6) 0.052(7) 0.058(7) 0.005(7) -0.024(5) -0.029(6) C(18) 0.035(6) 0.043(6) 0.044(6) 0.011(5) -0.020(5) -0.004(4) C(19) 0.023(4) 0.020(4) 0.023(4) -0.007(3) -0.008(3) -0.002(3) C(20) 0.030(5) 0.032(4) 0.016(4) 0.001(4) -0.006(3) -0.002(4) C(21) 0.030(5) 0.035(5) 0.033(5) 0.005(4) -0.008(4) -0.010(4) C(22) 0.061(7) 0.026(5) 0.037(6) 0.013(5) -0.017(4) -0.004(4) C(23) 0.059(7) 0.028(5) 0.034(6) -0.004(4) -0.012(4) 0.008(5) C(24) 0.034(6) 0.034(5) 0.025(5) -0.006(4) 0.001(4) 0.012(4) C(25) 0.029(6) 0.055(5) 0.037(4) 0.013(5) -0.001(5) -0.026(3) C(26) 0.035(6) 0.067(7) 0.035(4) 0.005(6) 0.001(5) -0.017(4) C(27) 0.047(8) 0.079(7) 0.038(5) 0.021(6) -0.008(5) -0.025(6) C(28) 0.047(8) 0.076(7) 0.066(8) 0.040(6) -0.014(7) -0.039(6) C(29) 0.036(7) 0.055(8) 0.083(7) 0.008(6) -0.017(7) -0.038(5) C(30) 0.033(7) 0.059(6) 0.073(7) 0.007(5) 0.000(6) -0.023(6) C(31) 0.047(6) 0.022(5) 0.049(6) -0.006(4) 0.002(4) -0.006(3) C(32) 0.048(6) 0.028(5) 0.049(6) -0.001(4) -0.012(5) -0.010(4) C(33) 0.080(9) 0.034(6) 0.062(7) 0.006(6) -0.033(6) 0.002(5) C(34) 0.11(1) 0.046(7) 0.064(8) -0.015(6) -0.012(7) 0.011(7) C(35) 0.11(1) 0.060(9) 0.09(1) -0.004(7) 0.02(1) 0.030(7) C(36) 0.033(7) 0.048(7) 0.078(8) -0.004(5) 0.018(5) 0.008(5) C(101) 0.034(4) 0.031(4) 0.030(5) -0.002(4) 0.008(4) -0.009(4) C(102) 0.032(4) 0.027(5) 0.026(4) -0.008(3) 0.003(4) -0.005(3) C(103) 0.034(5) 0.026(4) 0.047(5) 0.003(4) 0.011(4) -0.004(4) C(104) 0.026(6) 0.047(5) 0.048(5) 0.004(5) 0.001(5) -0.004(5) C(105) 0.059(8) 0.047(5) 0.048(6) 0.007(6) 0.014(6) 0.010(5) C(106) 0.038(7) 0.037(6) 0.062(6) 0.005(5) 0.015(5) -0.006(4) C(107) 0.057(6) 0.033(5) 0.027(4) -0.016(4) 0.017(5) -0.011(4) C(108) 0.038(6) 0.050(6) 0.022(4) -0.007(4) 0.010(4) -0.005(4) C(109) 0.067(8) 0.054(7) 0.035(5) -0.037(6) 0.011(6) 0.000(5) C(110) 0.11(1) 0.035(6) 0.041(5) -0.032(6) -0.001(7) -0.001(4) C(111) 0.11(1) 0.045(7) 0.032(5) -0.032(7) 0.005(7) -0.011(5) C(112) 0.074(8) 0.050(7) 0.022(4) -0.018(5) 0.014(5) -0.004(4) C(113) 0.040(5) 0.028(5) 0.022(5) -0.003(4) 0.001(4) 0.000(4) C(114) 0.030(5) 0.035(6) 0.030(5) 0.007(4) -0.005(3) 0.005(4) C(115) 0.040(6) 0.038(5) 0.039(5) 0.007(4) 0.003(5) -0.004(4) C(116) 0.050(6) 0.037(5) 0.037(5) 0.006(5) -0.001(4) -0.004(5) C(117) 0.047(6) 0.041(6) 0.039(5) -0.005(6) -0.006(4) -0.008(5) C(118) 0.043(7) 0.032(5) 0.042(6) -0.010(4) 0.003(5) -0.006(4) C(119) 0.047(5) 0.032(6) 0.026(4) -0.010(5) 0.011(3) -0.010(4) C(120) 0.049(6) 0.026(5) 0.041(5) -0.011(5) -0.004(4) -0.008(4) C(121) 0.085(8) 0.031(7) 0.039(5) 0.008(6) -0.005(6) -0.008(4) C(122) 0.094(7) 0.056(8) 0.026(5) 0.001(8) 0.021(5) 0.000(5) C(123) 0.071(8) 0.055(7) 0.044(5) -0.014(7) 0.030(5) -0.005(5) C(124) 0.044(6) 0.050(7) 0.047(6) -0.004(5) 0.023(6) 0.001(5) C(125) 0.20(1) 0.036(6) 0.032(7) -0.032(8) 0.046(8) -0.001(4) C(126) 0.25(2) 0.041(8) 0.07(1) 0.04(1) 0.06(1) 0.012(6) C(127) 0.46(4) 0.05(1) 0.09(1) 0.02(2) 0.13(2) -0.010(9) C(128) 0.47(4) 0.06(1) 0.08(1) -0.07(2) 0.16(2) -0.05(1) C(129) 0.40(4) 0.09(1) 0.046(10) -0.14(2) 0.10(2) -0.06(1) C(130) 0.23(2) 0.068(9) 0.035(7) -0.09(1) 0.033(8) -0.012(6) C(131) 0.078(6) 0.041(6) 0.028(5) -0.039(4) 0.014(4) -0.015(4) C(132) 0.088(10) 0.075(9) 0.030(5) -0.049(7) 0.007(6) 0.003(5) C(133) 0.083(10) 0.10(1) 0.039(7) -0.038(7) 0.007(6) 0.017(7) C(134) 0.078(9) 0.062(9) 0.060(7) -0.021(8) -0.006(6) 0.008(6) C(135) 0.072(9) 0.048(8) 0.060(7) -0.012(6) 0.021(7) -0.006(5) C(136) 0.083(7) 0.033(6) 0.036(6) -0.023(5) 0.019(5) -0.006(4) C(201) 0.11(1) 0.08(1) 0.18(1) 0.005(6) -0.022(7) 0.031(9) C(202) 0.111(10) 0.12(1) 0.068(7) 0.04(1) 0.015(9) 0.018(8) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Cl(1) 2.302(3) . . yes Pd(1) Cl(2) 2.398(3) . . yes Pd(1) P(1) 2.224(3) . . yes Pd(1) N(1) 2.096(8) . . yes Pd(2) Cl(3) 2.280(3) . . yes Pd(2) Cl(4) 2.368(4) . . yes Pd(2) P(2) 2.221(4) . . yes Pd(2) N(2) 2.108(9) . . yes Cl(5) C(201) 1.77(2) . . yes Cl(6) C(201) 1.81(2) . . yes Cl(7) C(201) 1.75(2) . . yes Cl(8) C(202) 1.66(2) . . yes Cl(9) C(202) 1.42(2) . . yes Cl(10) C(202) 1.87(2) . . yes P(1) C(12) 1.81(1) . . yes P(1) C(25) 1.827(10) . . yes P(1) C(31) 1.84(1) . . yes P(2) C(112) 1.83(1) . . yes P(2) C(125) 1.83(1) . . yes P(2) C(131) 1.81(1) . . yes O(1) C(1) 1.41(1) . . yes O(1) C(2) 1.47(1) . . yes O(2) C(101) 1.41(1) . . yes O(2) C(102) 1.46(1) . . yes N(1) C(1) 1.52(1) . . yes N(1) C(3) 1.50(1) . . yes N(1) C(6) 1.52(1) . . yes N(2) C(101) 1.50(1) . . yes N(2) C(103) 1.51(1) . . yes N(2) C(106) 1.48(1) . . yes C(1) C(7) 1.49(1) . . yes C(2) C(3) 1.54(1) . . yes C(2) C(13) 1.53(1) . . yes C(2) C(19) 1.54(1) . . yes C(3) C(4) 1.54(1) . . yes C(4) C(5) 1.54(1) . . yes C(5) C(6) 1.54(1) . . yes C(7) C(8) 1.37(1) . . yes C(7) C(12) 1.41(1) . . yes C(8) C(9) 1.40(1) . . yes C(9) C(10) 1.41(2) . . yes C(10) C(11) 1.37(1) . . yes C(11) C(12) 1.40(1) . . yes C(13) C(14) 1.38(1) . . yes C(13) C(18) 1.39(1) . . yes C(14) C(15) 1.40(1) . . yes C(15) C(16) 1.39(2) . . yes C(16) C(17) 1.36(2) . . yes C(17) C(18) 1.38(2) . . yes C(19) C(20) 1.38(1) . . yes C(19) C(24) 1.40(1) . . yes C(20) C(21) 1.39(1) . . yes C(21) C(22) 1.34(2) . . yes C(22) C(23) 1.37(2) . . yes C(23) C(24) 1.38(1) . . yes C(25) C(26) 1.40(2) . . yes C(25) C(30) 1.39(2) . . yes C(26) C(27) 1.37(1) . . yes C(27) C(28) 1.38(2) . . yes C(28) C(29) 1.37(2) . . yes C(29) C(30) 1.41(2) . . yes C(31) C(32) 1.36(2) . . yes C(31) C(36) 1.36(2) . . yes C(32) C(33) 1.38(2) . . yes C(33) C(34) 1.33(2) . . yes C(34) C(35) 1.40(2) . . yes C(35) C(36) 1.39(2) . . yes C(101) C(107) 1.50(1) . . yes C(102) C(103) 1.55(1) . . yes C(102) C(113) 1.54(1) . . yes C(102) C(119) 1.55(1) . . yes C(103) C(104) 1.55(1) . . yes C(104) C(105) 1.55(2) . . yes C(105) C(106) 1.51(2) . . yes C(107) C(108) 1.41(1) . . yes C(107) C(112) 1.39(1) . . yes C(108) C(109) 1.37(2) . . yes C(109) C(110) 1.37(2) . . yes C(110) C(111) 1.39(2) . . yes C(111) C(112) 1.38(2) . . yes C(113) C(114) 1.37(1) . . yes C(113) C(118) 1.39(1) . . yes C(114) C(115) 1.37(1) . . yes C(115) C(116) 1.39(2) . . yes C(116) C(117) 1.36(2) . . yes C(117) C(118) 1.38(1) . . yes C(119) C(120) 1.39(2) . . yes C(119) C(124) 1.38(1) . . yes C(120) C(121) 1.40(2) . . yes C(121) C(122) 1.35(2) . . yes C(122) C(123) 1.35(2) . . yes C(123) C(124) 1.39(2) . . yes C(125) C(126) 1.36(3) . . yes C(125) C(130) 1.41(3) . . yes C(126) C(127) 1.42(3) . . yes C(127) C(128) 1.39(5) . . yes C(128) C(129) 1.30(5) . . yes C(129) C(130) 1.38(2) . . yes C(131) C(132) 1.40(2) . . yes C(131) C(136) 1.41(2) . . yes C(132) C(133) 1.34(2) . . yes C(133) C(134) 1.37(2) . . yes C(134) C(135) 1.39(2) . . yes C(135) C(136) 1.35(2) . . yes O(100) H(203) 0.965 . . no O(100) H(204) 1.208 . . no C(1) H(1) 0.962 . . no C(3) H(2) 0.962 . . no C(4) H(3) 0.948 . . no C(4) H(4) 0.965 . . no C(5) H(5) 0.967 . . no C(5) H(6) 0.965 . . no C(6) H(7) 0.966 . . no C(6) H(8) 0.951 . . no C(8) H(9) 0.975 . . no C(9) H(10) 0.962 . . no C(10) H(11) 0.967 . . no C(11) H(12) 0.965 . . no C(14) H(13) 0.966 . . no C(15) H(14) 0.989 . . no C(16) H(15) 0.968 . . no C(17) H(16) 0.989 . . no C(18) H(17) 0.974 . . no C(20) H(18) 0.981 . . no C(21) H(19) 0.972 . . no C(22) H(20) 0.955 . . no C(23) H(21) 0.970 . . no C(24) H(22) 0.978 . . no C(26) H(23) 0.988 . . no C(27) H(24) 0.958 . . no C(28) H(25) 0.970 . . no C(29) H(26) 1.004 . . no C(30) H(27) 0.985 . . no C(32) H(28) 0.980 . . no C(33) H(29) 0.975 . . no C(34) H(30) 0.962 . . no C(35) H(31) 1.030 . . no C(36) H(32) 1.000 . . no C(101) H(101) 0.968 . . no C(103) H(102) 0.964 . . no C(104) H(103) 0.968 . . no C(104) H(104) 0.965 . . no C(105) H(105) 0.956 . . no C(105) H(106) 0.969 . . no C(106) H(107) 0.952 . . no C(106) H(108) 0.988 . . no C(108) H(109) 0.965 . . no C(109) H(110) 0.961 . . no C(110) H(111) 0.977 . . no C(111) H(112) 0.974 . . no C(114) H(113) 0.970 . . no C(115) H(114) 0.977 . . no C(116) H(115) 0.989 . . no C(117) H(116) 0.972 . . no C(118) H(117) 0.986 . . no C(120) H(128) 0.951 . . no C(121) H(129) 0.951 . . no C(122) H(130) 0.950 . . no C(123) H(131) 0.950 . . no C(124) H(132) 0.953 . . no C(126) H(118) 1.002 . . no C(127) H(119) 0.960 . . no C(128) H(120) 0.957 . . no C(129) H(121) 0.975 . . no C(130) H(122) 1.081 . . no C(132) H(123) 0.987 . . no C(133) H(124) 0.950 . . no C(134) H(125) 0.990 . . no C(135) H(126) 0.983 . . no C(136) H(127) 0.964 . . no C(201) H(201) 0.998 . . no C(202) H(202) 0.968 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Pd(1) Cl(2) 89.7(1) . . . yes Cl(1) Pd(1) P(1) 87.0(1) . . . yes Cl(1) Pd(1) N(1) 174.3(2) . . . yes Cl(2) Pd(1) P(1) 170.60(10) . . . yes Cl(2) Pd(1) N(1) 89.0(2) . . . yes P(1) Pd(1) N(1) 95.2(2) . . . yes Cl(3) Pd(2) Cl(4) 88.3(2) . . . yes Cl(3) Pd(2) P(2) 87.0(1) . . . yes Cl(3) Pd(2) N(2) 173.5(3) . . . yes Cl(4) Pd(2) P(2) 170.0(1) . . . yes Cl(4) Pd(2) N(2) 89.4(2) . . . yes P(2) Pd(2) N(2) 96.1(2) . . . yes Pd(1) P(1) C(12) 113.0(4) . . . yes Pd(1) P(1) C(25) 108.6(4) . . . yes Pd(1) P(1) C(31) 118.6(4) . . . yes C(12) P(1) C(25) 101.7(5) . . . yes C(12) P(1) C(31) 105.1(5) . . . yes C(25) P(1) C(31) 108.5(5) . . . yes Pd(2) P(2) C(112) 111.4(4) . . . yes Pd(2) P(2) C(125) 111.9(7) . . . yes Pd(2) P(2) C(131) 118.4(4) . . . yes C(112) P(2) C(125) 103.6(5) . . . yes C(112) P(2) C(131) 105.6(6) . . . yes C(125) P(2) C(131) 104.6(8) . . . yes C(1) O(1) C(2) 107.5(6) . . . yes C(101) O(2) C(102) 106.8(7) . . . yes Pd(1) N(1) C(1) 120.0(5) . . . yes Pd(1) N(1) C(3) 107.3(5) . . . yes Pd(1) N(1) C(6) 113.3(5) . . . yes C(1) N(1) C(3) 98.5(6) . . . yes C(1) N(1) C(6) 108.4(7) . . . yes C(3) N(1) C(6) 107.6(7) . . . yes Pd(2) N(2) C(101) 116.1(6) . . . yes Pd(2) N(2) C(103) 107.4(6) . . . yes Pd(2) N(2) C(106) 115.3(6) . . . yes C(101) N(2) C(103) 98.1(7) . . . yes C(101) N(2) C(106) 112.1(8) . . . yes C(103) N(2) C(106) 105.7(8) . . . yes O(1) C(1) N(1) 103.3(7) . . . yes O(1) C(1) C(7) 110.8(7) . . . yes N(1) C(1) C(7) 119.0(7) . . . yes O(1) C(2) C(3) 103.3(7) . . . yes O(1) C(2) C(13) 110.9(7) . . . yes O(1) C(2) C(19) 104.6(7) . . . yes C(3) C(2) C(13) 111.4(7) . . . yes C(3) C(2) C(19) 115.4(7) . . . yes C(13) C(2) C(19) 110.7(7) . . . yes N(1) C(3) C(2) 104.7(7) . . . yes N(1) C(3) C(4) 105.0(8) . . . yes C(2) C(3) C(4) 119.0(8) . . . yes C(3) C(4) C(5) 102.3(8) . . . yes C(4) C(5) C(6) 104.4(8) . . . yes N(1) C(6) C(5) 106.1(7) . . . yes C(1) C(7) C(8) 116.6(9) . . . yes C(1) C(7) C(12) 123.8(8) . . . yes C(8) C(7) C(12) 119.5(9) . . . yes C(7) C(8) C(9) 122.6(10) . . . yes C(8) C(9) C(10) 117.7(9) . . . yes C(9) C(10) C(11) 120.2(9) . . . yes C(10) C(11) C(12) 122.3(10) . . . yes P(1) C(12) C(7) 122.0(7) . . . yes P(1) C(12) C(11) 120.1(8) . . . yes C(7) C(12) C(11) 117.8(9) . . . yes C(2) C(13) C(14) 121.2(9) . . . yes C(2) C(13) C(18) 119.9(9) . . . yes C(14) C(13) C(18) 119.0(9) . . . yes C(13) C(14) C(15) 120(1) . . . yes C(14) C(15) C(16) 118(1) . . . yes C(15) C(16) C(17) 120.6(10) . . . yes C(16) C(17) C(18) 120(1) . . . yes C(13) C(18) C(17) 120(1) . . . yes C(2) C(19) C(20) 125.8(8) . . . yes C(2) C(19) C(24) 117.1(8) . . . yes C(20) C(19) C(24) 117.1(9) . . . yes C(19) C(20) C(21) 119.8(9) . . . yes C(20) C(21) C(22) 121(1) . . . yes C(21) C(22) C(23) 121(1) . . . yes C(22) C(23) C(24) 117.5(10) . . . yes C(19) C(24) C(23) 122.7(9) . . . yes P(1) C(25) C(26) 117.0(8) . . . yes P(1) C(25) C(30) 122.9(10) . . . yes C(26) C(25) C(30) 119(1) . . . yes C(25) C(26) C(27) 120(1) . . . yes C(26) C(27) C(28) 119(1) . . . yes C(27) C(28) C(29) 121(1) . . . yes C(28) C(29) C(30) 119(1) . . . yes C(25) C(30) C(29) 119(1) . . . yes P(1) C(31) C(32) 119.1(9) . . . yes P(1) C(31) C(36) 119.8(9) . . . yes C(32) C(31) C(36) 121(1) . . . yes C(31) C(32) C(33) 118(1) . . . yes C(32) C(33) C(34) 121(1) . . . yes C(33) C(34) C(35) 119(1) . . . yes C(34) C(35) C(36) 118(1) . . . yes C(31) C(36) C(35) 119(1) . . . yes O(2) C(101) N(2) 102.3(7) . . . yes O(2) C(101) C(107) 115.0(9) . . . yes N(2) C(101) C(107) 116.0(8) . . . yes O(2) C(102) C(103) 103.6(7) . . . yes O(2) C(102) C(113) 109.5(8) . . . yes O(2) C(102) C(119) 107.9(8) . . . yes C(103) C(102) C(113) 113.9(8) . . . yes C(103) C(102) C(119) 112.5(8) . . . yes C(113) C(102) C(119) 109.3(8) . . . yes N(2) C(103) C(102) 102.4(8) . . . yes N(2) C(103) C(104) 104.5(8) . . . yes C(102) C(103) C(104) 117.1(8) . . . yes C(103) C(104) C(105) 104.5(9) . . . yes C(104) C(105) C(106) 107.1(10) . . . yes N(2) C(106) C(105) 106.2(9) . . . yes C(101) C(107) C(108) 115.6(9) . . . yes C(101) C(107) C(112) 126.3(9) . . . yes C(108) C(107) C(112) 118.0(9) . . . yes C(107) C(108) C(109) 121.6(9) . . . yes C(108) C(109) C(110) 119(1) . . . yes C(109) C(110) C(111) 120(1) . . . yes C(110) C(111) C(112) 120(1) . . . yes P(2) C(112) C(107) 119.1(8) . . . yes P(2) C(112) C(111) 120.8(8) . . . yes C(107) C(112) C(111) 120.1(10) . . . yes C(102) C(113) C(114) 122.1(9) . . . yes C(102) C(113) C(118) 118.8(9) . . . yes C(114) C(113) C(118) 119.1(9) . . . yes C(113) C(114) C(115) 121(1) . . . yes C(114) C(115) C(116) 119(1) . . . yes C(115) C(116) C(117) 119(1) . . . yes C(116) C(117) C(118) 120(1) . . . yes C(113) C(118) C(117) 119(1) . . . yes C(102) C(119) C(120) 119.5(9) . . . yes C(102) C(119) C(124) 122.5(10) . . . yes C(120) C(119) C(124) 118(1) . . . yes C(119) C(120) C(121) 120(1) . . . yes C(120) C(121) C(122) 120(1) . . . yes C(121) C(122) C(123) 119(1) . . . yes C(122) C(123) C(124) 122(1) . . . yes C(119) C(124) C(123) 119(1) . . . yes P(2) C(125) C(126) 120(1) . . . yes P(2) C(125) C(130) 119(1) . . . yes C(126) C(125) C(130) 120(1) . . . yes C(125) C(126) C(127) 119(2) . . . yes C(126) C(127) C(128) 118(3) . . . yes C(127) C(128) C(129) 121(1) . . . yes C(128) C(129) C(130) 122(3) . . . yes C(125) C(130) C(129) 118(2) . . . yes P(2) C(131) C(132) 121(1) . . . yes P(2) C(131) C(136) 122.7(9) . . . yes C(132) C(131) C(136) 115(1) . . . yes C(131) C(132) C(133) 122(1) . . . yes C(132) C(133) C(134) 120(1) . . . yes C(133) C(134) C(135) 119(1) . . . yes C(134) C(135) C(136) 119(1) . . . yes C(131) C(136) C(135) 122(1) . . . yes Cl(5) C(201) Cl(6) 108(1) . . . yes Cl(5) C(201) Cl(7) 112(1) . . . yes Cl(6) C(201) Cl(7) 105(1) . . . yes Cl(8) C(202) Cl(9) 126(1) . . . yes Cl(8) C(202) Cl(10) 104(1) . . . yes Cl(9) C(202) Cl(10) 98(1) . . . yes H(203) O(100) H(204) 107.8 . . . no O(1) C(1) H(1) 108.0 . . . no N(1) C(1) H(1) 107.7 . . . no C(7) C(1) H(1) 107.6 . . . no N(1) C(3) H(2) 109.0 . . . no C(2) C(3) H(2) 110.2 . . . no C(4) C(3) H(2) 108.5 . . . no C(3) C(4) H(3) 111.7 . . . no C(3) C(4) H(4) 111.6 . . . no C(5) C(4) H(3) 111.6 . . . no C(5) C(4) H(4) 111.1 . . . no H(3) C(4) H(4) 108.4 . . . no C(4) C(5) H(5) 111.6 . . . no C(4) C(5) H(6) 111.7 . . . no C(6) C(5) H(5) 111.1 . . . no C(6) C(5) H(6) 111.3 . . . no H(5) C(5) H(6) 106.8 . . . no N(1) C(6) H(7) 110.3 . . . no N(1) C(6) H(8) 111.8 . . . no C(5) C(6) H(7) 110.1 . . . no C(5) C(6) H(8) 110.5 . . . no H(7) C(6) H(8) 108.0 . . . no C(7) C(8) H(9) 118.4 . . . no C(9) C(8) H(9) 119.1 . . . no C(8) C(9) H(10) 122.3 . . . no C(10) C(9) H(10) 120.0 . . . no C(9) C(10) H(11) 119.4 . . . no C(11) C(10) H(11) 120.4 . . . no C(10) C(11) H(12) 119.7 . . . no C(12) C(11) H(12) 118.0 . . . no C(13) C(14) H(13) 118.4 . . . no C(15) C(14) H(13) 121.2 . . . no C(14) C(15) H(14) 119.4 . . . no C(16) C(15) H(14) 121.7 . . . no C(15) C(16) H(15) 120.4 . . . no C(17) C(16) H(15) 118.9 . . . no C(16) C(17) H(16) 120.2 . . . no C(18) C(17) H(16) 119.3 . . . no C(13) C(18) H(17) 119.7 . . . no C(17) C(18) H(17) 119.6 . . . no C(19) C(20) H(18) 118.3 . . . no C(21) C(20) H(18) 122.0 . . . no C(20) C(21) H(19) 119.5 . . . no C(22) C(21) H(19) 119.2 . . . no C(21) C(22) H(20) 119.1 . . . no C(23) C(22) H(20) 119.3 . . . no C(22) C(23) H(21) 122.2 . . . no C(24) C(23) H(21) 120.3 . . . no C(19) C(24) H(22) 118.4 . . . no C(23) C(24) H(22) 118.9 . . . no C(25) C(26) H(23) 119.1 . . . no C(27) C(26) H(23) 120.5 . . . no C(26) C(27) H(24) 120.9 . . . no C(28) C(27) H(24) 119.1 . . . no C(27) C(28) H(25) 120.4 . . . no C(29) C(28) H(25) 118.1 . . . no C(28) C(29) H(26) 122.5 . . . no C(30) C(29) H(26) 118.1 . . . no C(25) C(30) H(27) 119.1 . . . no C(29) C(30) H(27) 121.7 . . . no C(31) C(32) H(28) 120.6 . . . no C(33) C(32) H(28) 120.8 . . . no C(32) C(33) H(29) 121.0 . . . no C(34) C(33) H(29) 117.2 . . . no C(33) C(34) H(30) 120.9 . . . no C(35) C(34) H(30) 119.3 . . . no C(34) C(35) H(31) 120.9 . . . no C(36) C(35) H(31) 120.2 . . . no C(31) C(36) H(32) 118.0 . . . no C(35) C(36) H(32) 122.0 . . . no O(2) C(101) H(101) 107.7 . . . no N(2) C(101) H(101) 107.9 . . . no C(107) C(101) H(101) 107.5 . . . no N(2) C(103) H(102) 110.6 . . . no C(102) C(103) H(102) 110.8 . . . no C(104) C(103) H(102) 110.9 . . . no C(103) C(104) H(103) 111.0 . . . no C(103) C(104) H(104) 112.0 . . . no C(105) C(104) H(103) 110.9 . . . no C(105) C(104) H(104) 111.7 . . . no H(103) C(104) H(104) 106.8 . . . no C(104) C(105) H(105) 110.9 . . . no C(104) C(105) H(106) 109.9 . . . no C(106) C(105) H(105) 111.7 . . . no C(106) C(105) H(106) 109.9 . . . no H(105) C(105) H(106) 107.3 . . . no N(2) C(106) H(107) 111.3 . . . no N(2) C(106) H(108) 109.0 . . . no C(105) C(106) H(107) 113.3 . . . no C(105) C(106) H(108) 110.8 . . . no H(107) C(106) H(108) 106.2 . . . no C(107) C(108) H(109) 118.2 . . . no C(109) C(108) H(109) 120.1 . . . no C(108) C(109) H(110) 120.3 . . . no C(110) C(109) H(110) 120.3 . . . no C(109) C(110) H(111) 119.7 . . . no C(111) C(110) H(111) 120.1 . . . no C(110) C(111) H(112) 120.3 . . . no C(112) C(111) H(112) 119.0 . . . no C(113) C(114) H(113) 119.3 . . . no C(115) C(114) H(113) 119.5 . . . no C(114) C(115) H(114) 118.2 . . . no C(116) C(115) H(114) 122.1 . . . no C(115) C(116) H(115) 121.0 . . . no C(117) C(116) H(115) 119.3 . . . no C(116) C(117) H(116) 121.7 . . . no C(118) C(117) H(116) 117.6 . . . no C(113) C(118) H(117) 120.8 . . . no C(117) C(118) H(117) 119.5 . . . no C(119) C(120) H(128) 120.0 . . . no C(121) C(120) H(128) 119.9 . . . no C(120) C(121) H(129) 119.6 . . . no C(122) C(121) H(129) 119.6 . . . no C(121) C(122) H(130) 120.3 . . . no C(123) C(122) H(130) 120.4 . . . no C(122) C(123) H(131) 118.9 . . . no C(124) C(123) H(131) 119.1 . . . no C(119) C(124) H(132) 120.2 . . . no C(123) C(124) H(132) 120.1 . . . no C(125) C(126) H(118) 119.5 . . . no C(127) C(126) H(118) 121.2 . . . no C(126) C(127) H(119) 122.7 . . . no C(128) C(127) H(119) 118.9 . . . no C(127) C(128) H(120) 117.5 . . . no C(129) C(128) H(120) 120.9 . . . no C(128) C(129) H(121) 116.2 . . . no C(130) C(129) H(121) 121.1 . . . no C(125) C(130) H(122) 121.5 . . . no C(129) C(130) H(122) 120.4 . . . no C(131) C(132) H(123) 117.3 . . . no C(133) C(132) H(123) 120.3 . . . no C(132) C(133) H(124) 119.4 . . . no C(134) C(133) H(124) 120.3 . . . no C(133) C(134) H(125) 119.5 . . . no C(135) C(134) H(125) 120.6 . . . no C(134) C(135) H(126) 121.1 . . . no C(136) C(135) H(126) 119.6 . . . no C(131) C(136) H(127) 118.4 . . . no C(135) C(136) H(127) 119.2 . . . no Cl(5) C(201) H(201) 108.1 . . . no Cl(6) C(201) H(201) 110.1 . . . no Cl(7) C(201) H(201) 111.6 . . . no Cl(8) C(202) H(202) 111.0 . . . no Cl(9) C(202) H(202) 104.8 . . . no Cl(10) C(202) H(202) 110.1 . . . no #------------------------------------------------------------------------------ #===END data_nakano-Pdcomplex-5 _database_code_CSD 180370 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C74 H66 Cl10 N2 O2 P2 Pd2 ' _chemical_formula_moiety 'C74 H66 Cl10 N2 O2 P2 Pd2 ' _chemical_formula_weight 1644.63 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz x,y,z _cell_length_a 10.841(3) _cell_length_b 12.860(3) _cell_length_c 13.625(3) _cell_angle_alpha 100.916(3) _cell_angle_beta 96.331(3) _cell_angle_gamma 104.576(3) _cell_volume 1780.0(8) _cell_formula_units_Z 1 _cell_measurement_reflns_used 7748 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.864 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 16413 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 1.3949 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.3949 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 4.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 4.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11363 _reflns_number_gt 10276 _reflns_threshold_expression F^2^>4.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0334 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 10276 _refine_ls_number_parameters 830 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.0633 _refine_diff_density_max 0.49 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd -0.0001(7) -0.0004(6) -0.0022(5) 0.02204(9) Uani 1.00 d . . . Pd(2) Pd 0.2720(7) -0.4721(6) 0.4321(5) 0.02092(9) Uani 1.00 d . . . Cl(1) Cl -0.0916(7) 0.1243(6) 0.0950(6) 0.0376(4) Uani 1.00 d . . . Cl(2) Cl 0.0157(7) -0.0836(6) 0.1307(5) 0.0396(4) Uani 1.00 d . . . Cl(3) Cl 0.4244(7) -0.5455(6) 0.5139(5) 0.0322(3) Uani 1.00 d . . . Cl(4) Cl 0.2385(7) -0.3884(6) 0.5871(5) 0.0323(3) Uani 1.00 d . . . Cl(5) Cl 0.2472(7) 0.5188(6) 0.8256(6) 0.0840(8) Uani 1.00 d . . . Cl(6) Cl 0.4297(7) 0.4024(6) 0.7835(6) 0.118(1) Uani 1.00 d . . . Cl(7) Cl 0.1781(8) 0.3154(7) 0.6711(6) 0.191(1) Uani 1.00 d . . . Cl(8) Cl 0.7313(7) 0.0565(6) 0.3279(6) 0.0762(6) Uani 1.00 d . . . Cl(9) Cl 0.9561(7) 0.2434(6) 0.4063(6) 0.0784(7) Uani 1.00 d . . . Cl(10) Cl 0.9715(7) 0.0277(6) 0.4132(6) 0.0798(7) Uani 1.00 d . . . P(1) P 0.0965(7) -0.1194(6) -0.0819(5) 0.0229(3) Uani 1.00 d . . . P(101) P 0.1436(7) -0.3792(6) 0.3714(5) 0.0210(3) Uani 1.00 d . . . O(1) O -0.1087(7) 0.0188(6) -0.2992(6) 0.0213(8) Uani 1.00 d . . . O(101) O 0.3453(7) -0.5228(6) 0.1312(6) 0.0210(8) Uani 1.00 d . . . N(1) N -0.0169(7) 0.0686(7) -0.1287(6) 0.0204(8) Uani 1.00 d . . . N(101) N 0.2886(7) -0.5487(7) 0.2852(6) 0.0198(8) Uani 1.00 d . . . C(1) C 0.1015(8) 0.1638(7) -0.1206(7) 0.031(1) Uani 1.00 d . . . C(2) C 0.0648(9) 0.2635(7) -0.0797(7) 0.042(1) Uani 1.00 d . . . C(3) C -0.0720(9) 0.2386(7) -0.1371(7) 0.039(1) Uani 1.00 d . . . C(4) C -0.1328(8) 0.1161(7) -0.1441(6) 0.024(1) Uani 1.00 d . . . C(5) C -0.2105(8) 0.0462(7) -0.2466(6) 0.0213(10) Uani 1.00 d . . . C(6) C -0.0377(8) -0.0171(7) -0.2256(6) 0.021(1) Uani 1.00 d . . . C(7) C 0.0856(8) -0.0361(7) -0.2561(6) 0.024(1) Uani 1.00 d . . . C(8) C 0.1268(8) -0.0096(7) -0.3430(6) 0.029(1) Uani 1.00 d . . . C(9) C 0.2403(8) -0.0312(7) -0.3704(6) 0.031(1) Uani 1.00 d . . . C(10) C 0.3102(8) -0.0788(8) -0.3104(7) 0.034(1) Uani 1.00 d . . . C(11) C 0.2710(8) -0.1023(7) -0.2216(7) 0.029(1) Uani 1.00 d . . . C(12) C 0.1570(8) -0.0825(7) -0.1940(6) 0.023(1) Uani 1.00 d . . . C(13) C -0.3051(8) -0.0618(7) -0.2404(6) 0.024(1) Uani 1.00 d . . . C(14) C -0.3479(8) -0.1456(7) -0.3279(6) 0.030(1) Uani 1.00 d . . . C(15) C -0.4299(8) -0.2462(7) -0.3271(7) 0.042(1) Uani 1.00 d . . . C(16) C -0.4717(8) -0.2658(8) -0.2391(8) 0.045(1) Uani 1.00 d . . . C(17) C -0.4321(8) -0.1849(8) -0.1522(7) 0.043(1) Uani 1.00 d . . . C(18) C -0.3483(8) -0.0826(7) -0.1511(7) 0.035(1) Uani 1.00 d . . . C(19) C -0.2776(8) 0.1104(7) -0.3073(6) 0.023(1) Uani 1.00 d . . . C(20) C -0.3970(8) 0.1227(7) -0.2854(6) 0.032(1) Uani 1.00 d . . . C(21) C -0.4572(8) 0.1861(8) -0.3337(7) 0.039(1) Uani 1.00 d . . . C(22) C -0.4026(9) 0.2381(8) -0.4040(7) 0.045(2) Uani 1.00 d . . . C(23) C -0.2865(9) 0.2248(8) -0.4260(7) 0.049(2) Uani 1.00 d . . . C(24) C -0.2242(8) 0.1610(8) -0.3785(7) 0.041(2) Uani 1.00 d . . . C(25) C 0.2380(8) -0.1272(7) -0.0024(7) 0.026(1) Uani 1.00 d . . . C(26) C 0.3365(9) -0.0322(8) 0.0364(7) 0.041(2) Uani 1.00 d . . . C(27) C 0.4477(9) -0.0320(8) 0.0967(7) 0.047(2) Uani 1.00 d . . . C(28) C 0.4578(8) -0.1313(8) 0.1197(7) 0.041(1) Uani 1.00 d . . . C(29) C 0.3607(8) -0.2266(8) 0.0805(7) 0.041(1) Uani 1.00 d . . . C(30) C 0.2495(8) -0.2261(7) 0.0190(7) 0.033(1) Uani 1.00 d . . . C(31) C -0.0123(8) -0.2567(7) -0.1315(7) 0.027(1) Uani 1.00 d . . . C(32) C 0.0190(8) -0.3328(8) -0.2048(7) 0.037(1) Uani 1.00 d . . . C(33) C -0.0658(9) -0.4348(8) -0.2459(7) 0.047(2) Uani 1.00 d . . . C(34) C -0.1861(9) -0.4616(8) -0.2157(7) 0.049(2) Uani 1.00 d . . . C(35) C -0.2197(8) -0.3873(8) -0.1451(7) 0.045(2) Uani 1.00 d . . . C(36) C -0.1337(8) -0.2849(7) -0.1026(7) 0.037(1) Uani 1.00 d . . . C(101) C 0.1814(8) -0.6544(7) 0.2495(6) 0.027(1) Uani 1.00 d . . . C(102) C 0.2371(8) -0.7381(7) 0.2896(7) 0.033(1) Uani 1.00 d . . . C(103) C 0.3737(8) -0.7083(7) 0.2645(7) 0.037(1) Uani 1.00 d . . . C(104) C 0.4128(8) -0.5835(7) 0.2761(6) 0.024(1) Uani 1.00 d . . . C(105) C 0.4609(8) -0.5391(7) 0.1840(6) 0.0218(10) Uani 1.00 d . . . C(106) C 0.2895(8) -0.4749(7) 0.2114(6) 0.020(1) Uani 1.00 d . . . C(107) C 0.1585(8) -0.4658(7) 0.1712(6) 0.0202(10) Uani 1.00 d . . . C(108) C 0.1173(8) -0.4908(7) 0.0676(6) 0.024(1) Uani 1.00 d . . . C(109) C -0.0029(8) -0.4822(7) 0.0276(6) 0.027(1) Uani 1.00 d . . . C(110) C -0.0820(8) -0.4474(7) 0.0930(7) 0.030(1) Uani 1.00 d . . . C(111) C -0.0398(8) -0.4199(7) 0.1956(7) 0.028(1) Uani 1.00 d . . . C(112) C 0.0804(8) -0.4276(7) 0.2371(6) 0.0207(10) Uani 1.00 d . . . C(113) C 0.5640(8) -0.4271(7) 0.2100(7) 0.0234(10) Uani 1.00 d . . . C(114) C 0.6158(8) -0.3648(8) 0.3065(7) 0.036(1) Uani 1.00 d . . . C(115) C 0.7068(9) -0.2642(8) 0.3215(7) 0.050(2) Uani 1.00 d . . . C(116) C 0.7489(8) -0.2231(7) 0.2413(7) 0.045(1) Uani 1.00 d . . . C(117) C 0.6959(9) -0.2839(8) 0.1456(7) 0.043(1) Uani 1.00 d . . . C(118) C 0.6052(8) -0.3835(7) 0.1288(7) 0.034(1) Uani 1.00 d . . . C(119) C 0.5089(8) -0.6215(7) 0.1136(7) 0.024(1) Uani 1.00 d . . . C(120) C 0.6238(8) -0.6415(8) 0.1486(7) 0.035(1) Uani 1.00 d . . . C(121) C 0.6674(8) -0.7207(8) 0.0893(7) 0.047(2) Uani 1.00 d . . . C(122) C 0.5981(9) -0.7788(8) -0.0037(7) 0.048(2) Uani 1.00 d . . . C(123) C 0.4850(9) -0.7573(8) -0.0399(7) 0.044(2) Uani 1.00 d . . . C(124) C 0.4397(8) -0.6797(7) 0.0195(7) 0.034(1) Uani 1.00 d . . . C(125) C 0.0021(8) -0.3801(7) 0.4319(7) 0.026(1) Uani 1.00 d . . . C(126) C -0.0934(8) -0.4805(7) 0.4148(7) 0.036(1) Uani 1.00 d . . . C(127) C -0.1995(8) -0.4868(8) 0.4653(7) 0.044(2) Uani 1.00 d . . . C(128) C -0.2105(8) -0.3963(8) 0.5307(7) 0.046(2) Uani 1.00 d . . . C(129) C -0.1164(8) -0.2981(8) 0.5471(7) 0.046(1) Uani 1.00 d . . . C(130) C -0.0087(8) -0.2889(7) 0.4973(7) 0.035(1) Uani 1.00 d . . . C(131) C 0.2370(8) -0.2375(7) 0.3819(6) 0.024(1) Uani 1.00 d . . . C(132) C 0.1880(8) -0.1695(7) 0.3294(7) 0.035(1) Uani 1.00 d . . . C(133) C 0.2642(9) -0.0637(8) 0.3329(7) 0.042(1) Uani 1.00 d . . . C(134) C 0.3869(9) -0.0252(7) 0.3866(7) 0.040(1) Uani 1.00 d . . . C(135) C 0.4364(8) -0.0923(7) 0.4396(7) 0.038(1) Uani 1.00 d . . . C(136) C 0.3626(8) -0.1974(7) 0.4369(7) 0.030(1) Uani 1.00 d . . . C(201) C 0.295(1) 0.4326(9) 0.7298(8) 0.074(2) Uani 1.00 d . . . C(202) C 0.9007(9) 0.1037(8) 0.3436(7) 0.053(1) Uani 1.00 d . . . H(1) H -0.1680 0.0987 -0.0845 0.0172 Uiso 1.00 calc . . . H(2) H 0.1716 0.1500 -0.0776 0.0502 Uiso 1.00 calc . . . H(3) H 0.1139 0.1598 -0.1940 0.0371 Uiso 1.00 calc . . . H(4) H 0.0538 0.2699 -0.0008 0.0654 Uiso 1.00 calc . . . H(5) H 0.1204 0.3325 -0.0959 0.0564 Uiso 1.00 calc . . . H(6) H -0.1187 0.2822 -0.1070 0.0366 Uiso 1.00 calc . . . H(7) H -0.0678 0.2519 -0.1945 0.0472 Uiso 1.00 calc . . . H(8) H 0.0929 0.0363 -0.3679 0.0536 Uiso 1.00 calc . . . H(9) H 0.2693 -0.0141 -0.4294 0.0264 Uiso 1.00 calc . . . H(10) H 0.3850 -0.0910 -0.3217 0.0513 Uiso 1.00 calc . . . H(11) H 0.3194 -0.1303 -0.1831 0.0177 Uiso 1.00 calc . . . H(12) H -0.3250 -0.1327 -0.3873 0.0212 Uiso 1.00 calc . . . H(13) H -0.4595 -0.2987 -0.3848 0.0382 Uiso 1.00 calc . . . H(14) H -0.5342 -0.3466 -0.2381 0.0549 Uiso 1.00 calc . . . H(15) H -0.4550 -0.1897 -0.0934 0.0418 Uiso 1.00 calc . . . H(16) H -0.4356 0.0935 -0.2344 0.0346 Uiso 1.00 calc . . . H(17) H -0.5383 0.1880 -0.3192 0.0383 Uiso 1.00 calc . . . H(18) H -0.4508 0.2864 -0.4414 0.0382 Uiso 1.00 calc . . . H(19) H -0.2516 0.2513 -0.4758 0.0391 Uiso 1.00 calc . . . H(20) H -0.1601 0.1490 -0.3911 0.0686 Uiso 1.00 calc . . . H(21) H 0.3380 0.0229 0.0094 0.0543 Uiso 1.00 calc . . . H(22) H 0.5107 0.0376 0.1200 0.0594 Uiso 1.00 calc . . . H(23) H 0.5282 -0.1324 0.1648 0.0637 Uiso 1.00 calc . . . H(24) H 0.3698 -0.3018 0.0916 0.0353 Uiso 1.00 calc . . . H(25) H 0.1741 -0.2928 -0.0064 0.0406 Uiso 1.00 calc . . . H(26) H 0.0910 -0.3233 -0.2238 0.0391 Uiso 1.00 calc . . . H(27) H -0.0508 -0.4850 -0.2970 0.0632 Uiso 1.00 calc . . . H(28) H -0.2433 -0.5346 -0.2444 0.0814 Uiso 1.00 calc . . . H(29) H -0.3115 -0.4094 -0.1166 0.0436 Uiso 1.00 calc . . . H(30) H -0.1561 -0.2207 -0.0452 0.0446 Uiso 1.00 calc . . . H(31) H -0.0939 -0.0897 -0.2159 0.0339 Uiso 1.00 calc . . . H(32) H -0.3086 -0.0229 -0.0771 0.0367 Uiso 1.00 calc . . . H(101) H 0.3492 -0.3955 0.2471 0.0205 Uiso 1.00 calc . . . H(102) H 0.4675 -0.5476 0.3399 0.0156 Uiso 1.00 calc . . . H(103) H 0.1086 -0.6467 0.2800 0.0293 Uiso 1.00 calc . . . H(104) H 0.1728 -0.6781 0.1774 0.0221 Uiso 1.00 calc . . . H(105) H 0.2403 -0.7256 0.3588 0.0279 Uiso 1.00 calc . . . H(106) H 0.1849 -0.8145 0.2582 0.0347 Uiso 1.00 calc . . . H(107) H 0.4311 -0.7285 0.3107 0.0442 Uiso 1.00 calc . . . H(108) H 0.3747 -0.7446 0.1974 0.0442 Uiso 1.00 calc . . . H(109) H 0.5954 -0.3815 0.3636 0.0346 Uiso 1.00 calc . . . H(110) H 0.7409 -0.2340 0.3820 0.0451 Uiso 1.00 calc . . . H(111) H 0.8176 -0.1539 0.2584 0.0438 Uiso 1.00 calc . . . H(112) H 0.7102 -0.2645 0.0919 0.0639 Uiso 1.00 calc . . . H(113) H 0.5738 -0.4216 0.0673 0.0458 Uiso 1.00 calc . . . H(114) H 0.6752 -0.6033 0.2111 0.0364 Uiso 1.00 calc . . . H(115) H 0.7341 -0.7344 0.1139 0.0586 Uiso 1.00 calc . . . H(116) H 0.6253 -0.8350 -0.0406 0.0492 Uiso 1.00 calc . . . H(117) H 0.4448 -0.7905 -0.0980 0.0243 Uiso 1.00 calc . . . H(118) H 0.3585 -0.6634 -0.0117 0.0357 Uiso 1.00 calc . . . H(119) H -0.0829 -0.5400 0.3696 0.0298 Uiso 1.00 calc . . . H(120) H -0.2576 -0.5515 0.4572 0.0663 Uiso 1.00 calc . . . H(121) H -0.2883 -0.4051 0.5594 0.0767 Uiso 1.00 calc . . . H(122) H -0.1186 -0.2302 0.5945 0.0412 Uiso 1.00 calc . . . H(123) H 0.0610 -0.2159 0.5106 0.0277 Uiso 1.00 calc . . . H(124) H 0.1096 -0.1932 0.2960 0.0468 Uiso 1.00 calc . . . H(125) H 0.2332 -0.0253 0.3014 0.0874 Uiso 1.00 calc . . . H(126) H 0.4382 0.0441 0.3885 0.0375 Uiso 1.00 calc . . . H(127) H 0.5262 -0.0596 0.4749 0.0488 Uiso 1.00 calc . . . H(128) H 0.3999 -0.2445 0.4804 0.0484 Uiso 1.00 calc . . . H(129) H 0.1717 -0.5142 0.0229 0.0284 Uiso 1.00 calc . . . H(130) H -0.0325 -0.5035 -0.0447 0.0330 Uiso 1.00 calc . . . H(131) H -0.1658 -0.4429 0.0638 0.0461 Uiso 1.00 calc . . . H(132) H -0.0970 -0.4006 0.2404 0.0343 Uiso 1.00 calc . . . H(133) H 0.3242 0.4767 0.6981 0.0252 Uiso 1.00 calc . . . H(134) H 0.9284 0.0888 0.2892 0.0390 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0221(2) 0.0290(2) 0.0181(2) 0.0106(2) 0.0030(1) 0.0082(2) Pd(2) 0.0201(2) 0.0277(2) 0.0195(2) 0.0116(1) 0.0056(1) 0.0084(2) Cl(1) 0.0492(7) 0.0526(8) 0.0206(6) 0.0309(7) 0.0088(5) 0.0071(6) Cl(2) 0.0428(7) 0.0587(9) 0.0299(7) 0.0228(7) 0.0106(6) 0.0258(6) Cl(3) 0.0341(6) 0.0448(7) 0.0281(6) 0.0241(6) 0.0061(5) 0.0145(6) Cl(4) 0.0353(6) 0.0481(8) 0.0192(5) 0.0220(6) 0.0059(5) 0.0068(5) Cl(5) 0.127(2) 0.091(1) 0.081(1) 0.065(1) 0.075(1) 0.051(1) Cl(6) 0.186(3) 0.143(2) 0.084(2) 0.130(2) 0.030(2) 0.048(2) Cl(7) 0.239(4) 0.151(3) 0.078(2) -0.127(3) 0.015(2) 0.026(2) Cl(8) 0.0537(10) 0.093(2) 0.073(1) 0.0251(10) 0.0047(9) -0.007(1) Cl(9) 0.087(1) 0.058(1) 0.096(2) 0.0083(10) 0.060(1) 0.018(1) Cl(10) 0.101(2) 0.093(2) 0.048(1) 0.043(1) -0.0149(10) 0.0139(10) P(1) 0.0211(5) 0.0263(6) 0.0251(6) 0.0104(5) 0.0034(4) 0.0102(5) P(101) 0.0197(5) 0.0285(6) 0.0189(6) 0.0134(5) 0.0047(4) 0.0055(5) O(1) 0.020(1) 0.027(2) 0.019(2) 0.012(1) 0.003(1) 0.005(1) O(101) 0.019(1) 0.029(2) 0.020(2) 0.014(1) 0.008(1) 0.007(1) N(1) 0.019(2) 0.022(2) 0.018(2) 0.006(1) 0.000(1) 0.003(1) N(101) 0.017(2) 0.022(2) 0.024(2) 0.008(1) 0.007(1) 0.008(1) C(1) 0.029(2) 0.029(2) 0.028(3) -0.004(2) -0.003(2) 0.010(2) C(2) 0.043(3) 0.033(3) 0.044(3) 0.005(2) 0.011(2) 0.003(2) C(3) 0.055(3) 0.024(2) 0.036(3) 0.015(2) -0.005(2) 0.003(2) C(4) 0.031(2) 0.026(2) 0.020(2) 0.017(2) 0.004(2) 0.006(2) C(5) 0.023(2) 0.023(2) 0.020(2) 0.012(2) 0.005(1) 0.003(2) C(6) 0.024(2) 0.024(2) 0.017(2) 0.009(2) 0.005(2) 0.007(2) C(7) 0.021(2) 0.022(2) 0.029(2) 0.007(2) 0.004(2) 0.006(2) C(8) 0.029(2) 0.036(3) 0.025(2) 0.013(2) 0.004(2) 0.012(2) C(9) 0.034(2) 0.040(3) 0.023(2) 0.012(2) 0.015(2) 0.008(2) C(10) 0.021(2) 0.049(3) 0.034(3) 0.013(2) 0.010(2) 0.009(2) C(11) 0.022(2) 0.038(3) 0.033(2) 0.014(2) 0.004(2) 0.011(2) C(12) 0.020(2) 0.025(2) 0.026(2) 0.008(2) 0.003(2) 0.008(2) C(13) 0.018(2) 0.025(2) 0.033(2) 0.011(2) 0.003(2) 0.009(2) C(14) 0.020(2) 0.036(2) 0.032(2) 0.011(2) 0.002(2) 0.000(2) C(15) 0.026(2) 0.031(2) 0.062(3) 0.011(2) -0.009(2) 0.000(3) C(16) 0.026(2) 0.038(3) 0.072(3) 0.005(2) -0.002(2) 0.025(2) C(17) 0.030(3) 0.050(3) 0.061(3) 0.012(2) 0.015(2) 0.030(2) C(18) 0.035(3) 0.040(3) 0.036(3) 0.018(2) 0.010(2) 0.011(2) C(19) 0.025(2) 0.027(2) 0.018(2) 0.013(2) -0.003(2) 0.000(2) C(20) 0.030(2) 0.039(3) 0.033(3) 0.019(2) 0.008(2) 0.008(2) C(21) 0.037(3) 0.044(3) 0.043(3) 0.029(2) 0.004(2) 0.008(2) C(22) 0.060(3) 0.054(4) 0.032(3) 0.039(3) -0.003(2) 0.010(2) C(23) 0.069(4) 0.068(4) 0.038(3) 0.047(3) 0.023(3) 0.032(3) C(24) 0.045(3) 0.060(4) 0.037(3) 0.032(3) 0.021(2) 0.028(3) C(25) 0.023(2) 0.035(2) 0.025(3) 0.010(2) 0.002(2) 0.014(2) C(26) 0.039(3) 0.030(3) 0.053(4) 0.012(2) -0.011(2) 0.013(3) C(27) 0.037(3) 0.042(3) 0.050(4) 0.005(3) -0.018(2) 0.003(3) C(28) 0.033(2) 0.054(3) 0.038(3) 0.019(2) -0.006(2) 0.015(3) C(29) 0.033(2) 0.051(3) 0.045(3) 0.017(2) 0.000(2) 0.025(3) C(30) 0.028(2) 0.030(3) 0.042(3) 0.009(2) 0.003(2) 0.015(2) C(31) 0.026(2) 0.028(2) 0.028(2) 0.006(2) 0.002(2) 0.016(2) C(32) 0.041(3) 0.039(3) 0.033(3) 0.015(2) 0.006(2) 0.009(2) C(33) 0.060(3) 0.041(3) 0.031(3) 0.011(2) -0.003(3) -0.001(3) C(34) 0.050(3) 0.036(3) 0.044(3) -0.003(2) -0.019(2) 0.005(2) C(35) 0.032(3) 0.045(3) 0.053(4) 0.003(2) -0.005(2) 0.016(2) C(36) 0.028(2) 0.041(3) 0.044(3) 0.011(2) 0.008(2) 0.014(2) C(101) 0.028(2) 0.022(2) 0.029(3) 0.003(2) 0.004(2) 0.004(2) C(102) 0.036(2) 0.022(3) 0.042(3) 0.008(2) 0.012(2) 0.011(2) C(103) 0.043(3) 0.032(2) 0.052(3) 0.021(2) 0.026(3) 0.024(3) C(104) 0.021(2) 0.031(2) 0.027(2) 0.018(2) 0.009(2) 0.010(2) C(105) 0.019(2) 0.026(2) 0.025(2) 0.013(2) 0.005(2) 0.007(2) C(106) 0.019(2) 0.025(2) 0.021(2) 0.013(2) 0.009(2) 0.008(2) C(107) 0.017(2) 0.023(2) 0.024(2) 0.008(2) 0.005(1) 0.009(2) C(108) 0.025(2) 0.028(2) 0.021(2) 0.012(2) 0.007(2) 0.007(2) C(109) 0.029(2) 0.030(3) 0.023(2) 0.012(2) -0.002(2) 0.004(2) C(110) 0.021(2) 0.037(3) 0.033(2) 0.012(2) 0.001(2) 0.009(2) C(111) 0.020(2) 0.038(3) 0.030(2) 0.015(2) 0.007(2) 0.009(2) C(112) 0.021(2) 0.024(2) 0.022(2) 0.012(2) 0.006(1) 0.006(2) C(113) 0.014(2) 0.026(2) 0.035(2) 0.010(1) 0.005(2) 0.010(2) C(114) 0.034(3) 0.039(3) 0.034(2) 0.010(2) 0.004(2) 0.010(2) C(115) 0.036(3) 0.043(3) 0.058(4) 0.001(2) -0.012(2) 0.002(3) C(116) 0.027(3) 0.036(3) 0.073(3) 0.010(2) 0.013(2) 0.011(2) C(117) 0.043(3) 0.034(3) 0.063(3) 0.017(2) 0.031(2) 0.019(2) C(118) 0.035(2) 0.037(3) 0.038(3) 0.014(2) 0.018(2) 0.011(2) C(119) 0.026(2) 0.025(2) 0.030(2) 0.015(2) 0.015(2) 0.008(2) C(120) 0.027(2) 0.042(3) 0.040(3) 0.017(2) 0.005(2) 0.010(2) C(121) 0.039(3) 0.055(4) 0.061(3) 0.033(3) 0.018(2) 0.011(3) C(122) 0.057(3) 0.042(3) 0.056(3) 0.032(3) 0.028(2) 0.007(3) C(123) 0.054(3) 0.044(3) 0.035(3) 0.020(3) 0.013(2) -0.001(3) C(124) 0.033(3) 0.041(3) 0.031(2) 0.017(2) 0.007(2) 0.008(2) C(125) 0.022(2) 0.042(2) 0.023(2) 0.020(2) 0.009(2) 0.012(2) C(126) 0.027(2) 0.044(3) 0.044(3) 0.015(2) 0.012(2) 0.019(3) C(127) 0.029(3) 0.066(4) 0.050(3) 0.017(3) 0.018(2) 0.033(3) C(128) 0.026(2) 0.085(4) 0.039(3) 0.027(2) 0.013(2) 0.020(3) C(129) 0.035(3) 0.077(4) 0.027(3) 0.030(2) 0.010(2) -0.005(3) C(130) 0.027(2) 0.049(3) 0.028(3) 0.016(2) 0.004(2) -0.002(2) C(131) 0.025(2) 0.029(2) 0.020(2) 0.011(1) 0.008(2) 0.004(2) C(132) 0.032(3) 0.034(2) 0.039(3) 0.011(2) -0.006(2) 0.010(2) C(133) 0.050(3) 0.036(3) 0.044(3) 0.013(2) 0.001(2) 0.018(3) C(134) 0.044(3) 0.034(3) 0.039(3) 0.002(2) 0.011(2) 0.013(2) C(135) 0.027(2) 0.040(2) 0.045(3) 0.006(2) 0.007(2) 0.012(2) C(136) 0.024(2) 0.036(2) 0.031(3) 0.011(2) 0.006(2) 0.010(2) C(201) 0.136(4) 0.056(3) 0.056(4) 0.034(2) 0.055(3) 0.043(2) C(202) 0.059(2) 0.068(3) 0.037(3) 0.024(3) 0.020(3) 0.010(2) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Cl(1) 2.366(1) . . yes Pd(1) Cl(2) 2.283(1) . . yes Pd(1) P(1) 2.246(1) . . yes Pd(1) N(1) 2.093(4) . . yes Pd(2) Cl(3) 2.375(1) . . yes Pd(2) Cl(4) 2.293(1) . . yes Pd(2) P(101) 2.237(1) . . yes Pd(2) N(101) 2.105(4) . . yes Cl(5) C(201) 1.760(7) . . yes Cl(6) C(201) 1.723(9) . . yes Cl(7) C(201) 1.696(9) . . yes Cl(8) C(202) 1.757(7) . . yes Cl(9) C(202) 1.755(7) . . yes Cl(10) C(202) 1.736(7) . . yes P(1) C(12) 1.824(4) . . yes P(1) C(25) 1.813(5) . . yes P(1) C(31) 1.814(5) . . yes P(101) C(112) 1.812(4) . . yes P(101) C(125) 1.818(4) . . yes P(101) C(131) 1.818(5) . . yes O(1) C(5) 1.459(4) . . yes O(1) C(6) 1.413(5) . . yes O(101) C(105) 1.457(4) . . yes O(101) C(106) 1.420(4) . . yes N(1) C(1) 1.511(6) . . yes N(1) C(4) 1.541(5) . . yes N(1) C(6) 1.506(5) . . yes N(101) C(101) 1.505(6) . . yes N(101) C(104) 1.531(4) . . yes N(101) C(106) 1.507(5) . . yes C(1) C(2) 1.466(7) . . yes C(2) C(3) 1.524(7) . . yes C(3) C(4) 1.526(7) . . yes C(4) C(5) 1.533(6) . . yes C(5) C(13) 1.528(6) . . yes C(5) C(19) 1.525(5) . . yes C(6) C(7) 1.506(5) . . yes C(7) C(8) 1.382(6) . . yes C(7) C(12) 1.397(6) . . yes C(8) C(9) 1.402(6) . . yes C(9) C(10) 1.380(7) . . yes C(10) C(11) 1.385(7) . . yes C(11) C(12) 1.400(5) . . yes C(13) C(14) 1.392(6) . . yes C(13) C(18) 1.398(7) . . yes C(14) C(15) 1.375(7) . . yes C(15) C(16) 1.372(8) . . yes C(16) C(17) 1.365(9) . . yes C(17) C(18) 1.395(7) . . yes C(19) C(20) 1.401(6) . . yes C(19) C(24) 1.368(7) . . yes C(20) C(21) 1.378(6) . . yes C(21) C(22) 1.373(8) . . yes C(22) C(23) 1.370(8) . . yes C(23) C(24) 1.390(7) . . yes C(25) C(26) 1.373(7) . . yes C(25) C(30) 1.389(6) . . yes C(26) C(27) 1.382(7) . . yes C(27) C(28) 1.398(8) . . yes C(28) C(29) 1.369(8) . . yes C(29) C(30) 1.392(6) . . yes C(31) C(32) 1.395(7) . . yes C(31) C(36) 1.395(6) . . yes C(32) C(33) 1.371(8) . . yes C(33) C(34) 1.391(9) . . yes C(34) C(35) 1.370(9) . . yes C(35) C(36) 1.383(7) . . yes C(101) C(102) 1.516(6) . . yes C(102) C(103) 1.528(6) . . yes C(103) C(104) 1.526(7) . . yes C(104) C(105) 1.563(6) . . yes C(105) C(113) 1.536(6) . . yes C(105) C(119) 1.521(5) . . yes C(106) C(107) 1.506(5) . . yes C(107) C(108) 1.384(6) . . yes C(107) C(112) 1.405(5) . . yes C(108) C(109) 1.395(6) . . yes C(109) C(110) 1.393(6) . . yes C(110) C(111) 1.371(7) . . yes C(111) C(112) 1.397(5) . . yes C(113) C(114) 1.378(7) . . yes C(113) C(118) 1.398(7) . . yes C(114) C(115) 1.379(8) . . yes C(115) C(116) 1.373(9) . . yes C(116) C(117) 1.366(8) . . yes C(117) C(118) 1.366(7) . . yes C(119) C(120) 1.387(6) . . yes C(119) C(124) 1.382(7) . . yes C(120) C(121) 1.388(7) . . yes C(121) C(122) 1.371(8) . . yes C(122) C(123) 1.383(8) . . yes C(123) C(124) 1.386(7) . . yes C(125) C(126) 1.397(7) . . yes C(125) C(130) 1.370(7) . . yes C(126) C(127) 1.397(6) . . yes C(127) C(128) 1.365(8) . . yes C(128) C(129) 1.372(8) . . yes C(129) C(130) 1.405(6) . . yes C(131) C(132) 1.395(6) . . yes C(131) C(136) 1.399(6) . . yes C(132) C(133) 1.391(8) . . yes C(133) C(134) 1.366(8) . . yes C(134) C(135) 1.392(7) . . yes C(135) C(136) 1.377(7) . . yes C(1) H(2) 0.980 . . no C(1) H(3) 1.018 . . no C(2) H(4) 1.085 . . no C(2) H(5) 1.016 . . no C(3) H(6) 0.918 . . no C(3) H(7) 0.835 . . no C(4) H(1) 0.975 . . no C(6) H(31) 1.018 . . no C(8) H(8) 0.869 . . no C(9) H(9) 0.938 . . no C(10) H(10) 0.888 . . no C(11) H(11) 0.886 . . no C(14) H(12) 0.905 . . no C(15) H(13) 0.901 . . no C(16) H(14) 1.092 . . no C(17) H(15) 0.874 . . no C(18) H(32) 1.112 . . no C(20) H(16) 0.940 . . no C(21) H(17) 0.926 . . no C(22) H(18) 1.069 . . no C(23) H(19) 0.894 . . no C(24) H(20) 0.779 . . no C(26) H(21) 0.855 . . no C(27) H(22) 0.951 . . no C(28) H(23) 0.930 . . no C(29) H(24) 1.034 . . no C(30) H(25) 0.998 . . no C(32) H(26) 0.836 . . no C(33) H(27) 0.914 . . no C(34) H(28) 0.966 . . no C(35) H(29) 1.098 . . no C(36) H(30) 1.119 . . no C(101) H(103) 0.949 . . no C(101) H(104) 0.958 . . no C(102) H(105) 0.921 . . no C(102) H(106) 0.989 . . no C(103) H(107) 0.953 . . no C(103) H(108) 0.946 . . no C(104) H(102) 0.957 . . no C(106) H(101) 1.053 . . no C(108) H(129) 0.953 . . no C(109) H(130) 0.965 . . no C(110) H(131) 0.971 . . no C(111) H(132) 0.961 . . no C(114) H(109) 0.882 . . no C(115) H(110) 0.841 . . no C(116) H(111) 0.975 . . no C(117) H(112) 0.834 . . no C(118) H(113) 0.870 . . no C(120) H(114) 0.936 . . no C(121) H(115) 0.837 . . no C(122) H(116) 0.929 . . no C(123) H(117) 0.837 . . no C(124) H(118) 1.021 . . no C(126) H(119) 0.927 . . no C(127) H(120) 0.888 . . no C(128) H(121) 0.959 . . no C(129) H(122) 0.991 . . no C(130) H(123) 1.017 . . no C(132) H(124) 0.868 . . no C(133) H(125) 0.821 . . no C(134) H(126) 0.918 . . no C(135) H(127) 0.985 . . no C(136) H(128) 1.043 . . no C(201) H(133) 0.800 . . no C(202) H(134) 0.837 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Pd(1) Cl(2) 89.27(5) . . . yes Cl(1) Pd(1) P(1) 175.04(5) . . . yes Cl(1) Pd(1) N(1) 92.83(10) . . . yes Cl(2) Pd(1) P(1) 86.48(4) . . . yes Cl(2) Pd(1) N(1) 177.3(1) . . . yes P(1) Pd(1) N(1) 91.50(9) . . . yes Cl(3) Pd(2) Cl(4) 89.83(4) . . . yes Cl(3) Pd(2) P(101) 171.45(5) . . . yes Cl(3) Pd(2) N(101) 94.11(9) . . . yes Cl(4) Pd(2) P(101) 84.27(4) . . . yes Cl(4) Pd(2) N(101) 175.65(9) . . . yes P(101) Pd(2) N(101) 92.01(9) . . . yes Pd(1) P(1) C(12) 113.8(1) . . . yes Pd(1) P(1) C(25) 112.4(2) . . . yes Pd(1) P(1) C(31) 112.9(1) . . . yes C(12) P(1) C(25) 104.2(2) . . . yes C(12) P(1) C(31) 103.1(2) . . . yes C(25) P(1) C(31) 109.7(2) . . . yes Pd(2) P(101) C(112) 114.5(1) . . . yes Pd(2) P(101) C(125) 114.6(2) . . . yes Pd(2) P(101) C(131) 109.4(1) . . . yes C(112) P(101) C(125) 104.9(2) . . . yes C(112) P(101) C(131) 103.2(2) . . . yes C(125) P(101) C(131) 109.5(2) . . . yes C(5) O(1) C(6) 102.1(3) . . . yes C(105) O(101) C(106) 103.2(3) . . . yes Pd(1) N(1) C(1) 109.5(2) . . . yes Pd(1) N(1) C(4) 116.4(2) . . . yes Pd(1) N(1) C(6) 111.0(2) . . . yes C(1) N(1) C(4) 105.4(3) . . . yes C(1) N(1) C(6) 111.7(3) . . . yes C(4) N(1) C(6) 102.6(3) . . . yes Pd(2) N(101) C(101) 108.8(2) . . . yes Pd(2) N(101) C(104) 115.5(3) . . . yes Pd(2) N(101) C(106) 112.9(2) . . . yes C(101) N(101) C(104) 104.7(3) . . . yes C(101) N(101) C(106) 111.5(3) . . . yes C(104) N(101) C(106) 103.1(3) . . . yes N(1) C(1) C(2) 105.7(4) . . . yes C(1) C(2) C(3) 102.1(4) . . . yes C(2) C(3) C(4) 105.1(4) . . . yes N(1) C(4) C(3) 104.5(3) . . . yes N(1) C(4) C(5) 103.7(3) . . . yes C(3) C(4) C(5) 117.5(4) . . . yes O(1) C(5) C(4) 101.7(3) . . . yes O(1) C(5) C(13) 107.9(3) . . . yes O(1) C(5) C(19) 108.2(3) . . . yes C(4) C(5) C(13) 114.4(4) . . . yes C(4) C(5) C(19) 113.2(3) . . . yes C(13) C(5) C(19) 110.8(3) . . . yes O(1) C(6) N(1) 105.5(3) . . . yes O(1) C(6) C(7) 112.8(3) . . . yes N(1) C(6) C(7) 113.6(3) . . . yes C(6) C(7) C(8) 121.5(4) . . . yes C(6) C(7) C(12) 117.8(4) . . . yes C(8) C(7) C(12) 120.7(4) . . . yes C(7) C(8) C(9) 119.9(4) . . . yes C(8) C(9) C(10) 119.7(4) . . . yes C(9) C(10) C(11) 120.5(4) . . . yes C(10) C(11) C(12) 120.4(4) . . . yes P(1) C(12) C(7) 119.2(3) . . . yes P(1) C(12) C(11) 122.0(3) . . . yes C(7) C(12) C(11) 118.8(4) . . . yes C(5) C(13) C(14) 118.2(4) . . . yes C(5) C(13) C(18) 123.8(4) . . . yes C(14) C(13) C(18) 118.0(4) . . . yes C(13) C(14) C(15) 121.3(5) . . . yes C(14) C(15) C(16) 120.2(5) . . . yes C(15) C(16) C(17) 119.8(5) . . . yes C(16) C(17) C(18) 120.9(5) . . . yes C(13) C(18) C(17) 119.7(5) . . . yes C(5) C(19) C(20) 118.1(4) . . . yes C(5) C(19) C(24) 123.3(4) . . . yes C(20) C(19) C(24) 118.4(4) . . . yes C(19) C(20) C(21) 120.2(5) . . . yes C(20) C(21) C(22) 121.3(4) . . . yes C(21) C(22) C(23) 118.3(4) . . . yes C(22) C(23) C(24) 121.4(5) . . . yes C(19) C(24) C(23) 120.4(4) . . . yes P(1) C(25) C(26) 118.4(4) . . . yes P(1) C(25) C(30) 121.9(4) . . . yes C(26) C(25) C(30) 119.7(4) . . . yes C(25) C(26) C(27) 121.6(5) . . . yes C(26) C(27) C(28) 118.5(5) . . . yes C(27) C(28) C(29) 120.2(4) . . . yes C(28) C(29) C(30) 120.8(5) . . . yes C(25) C(30) C(29) 119.1(4) . . . yes P(1) C(31) C(32) 120.9(4) . . . yes P(1) C(31) C(36) 120.2(4) . . . yes C(32) C(31) C(36) 118.7(5) . . . yes C(31) C(32) C(33) 121.0(5) . . . yes C(32) C(33) C(34) 119.5(5) . . . yes C(33) C(34) C(35) 120.5(5) . . . yes C(34) C(35) C(36) 120.1(5) . . . yes C(31) C(36) C(35) 120.3(5) . . . yes N(101) C(101) C(102) 103.4(3) . . . yes C(101) C(102) C(103) 101.5(4) . . . yes C(102) C(103) C(104) 105.7(3) . . . yes N(101) C(104) C(103) 105.7(3) . . . yes N(101) C(104) C(105) 103.7(3) . . . yes C(103) C(104) C(105) 116.9(4) . . . yes O(101) C(105) C(104) 103.1(3) . . . yes O(101) C(105) C(113) 106.5(3) . . . yes O(101) C(105) C(119) 109.6(3) . . . yes C(104) C(105) C(113) 115.9(4) . . . yes C(104) C(105) C(119) 112.6(3) . . . yes C(113) C(105) C(119) 108.6(3) . . . yes O(101) C(106) N(101) 104.2(3) . . . yes O(101) C(106) C(107) 110.4(3) . . . yes N(101) C(106) C(107) 114.8(3) . . . yes C(106) C(107) C(108) 119.2(3) . . . yes C(106) C(107) C(112) 121.0(4) . . . yes C(108) C(107) C(112) 119.7(3) . . . yes C(107) C(108) C(109) 120.9(4) . . . yes C(108) C(109) C(110) 119.5(4) . . . yes C(109) C(110) C(111) 119.7(4) . . . yes C(110) C(111) C(112) 121.7(4) . . . yes P(101) C(112) C(107) 119.2(3) . . . yes P(101) C(112) C(111) 122.0(3) . . . yes C(107) C(112) C(111) 118.6(4) . . . yes C(105) C(113) C(114) 125.3(4) . . . yes C(105) C(113) C(118) 117.1(4) . . . yes C(114) C(113) C(118) 117.6(4) . . . yes C(113) C(114) C(115) 120.6(5) . . . yes C(114) C(115) C(116) 121.4(5) . . . yes C(115) C(116) C(117) 118.1(5) . . . yes C(116) C(117) C(118) 121.6(5) . . . yes C(113) C(118) C(117) 120.7(5) . . . yes C(105) C(119) C(120) 117.8(4) . . . yes C(105) C(119) C(124) 122.5(4) . . . yes C(120) C(119) C(124) 119.6(4) . . . yes C(119) C(120) C(121) 119.7(5) . . . yes C(120) C(121) C(122) 120.6(5) . . . yes C(121) C(122) C(123) 119.9(4) . . . yes C(122) C(123) C(124) 119.9(5) . . . yes C(119) C(124) C(123) 120.3(4) . . . yes P(101) C(125) C(126) 117.3(4) . . . yes P(101) C(125) C(130) 122.3(4) . . . yes C(126) C(125) C(130) 120.2(4) . . . yes C(125) C(126) C(127) 119.3(5) . . . yes C(126) C(127) C(128) 120.7(5) . . . yes C(127) C(128) C(129) 119.7(4) . . . yes C(128) C(129) C(130) 121.0(5) . . . yes C(125) C(130) C(129) 119.1(5) . . . yes P(101) C(131) C(132) 120.4(3) . . . yes P(101) C(131) C(136) 120.5(3) . . . yes C(132) C(131) C(136) 118.9(4) . . . yes C(131) C(132) C(133) 119.7(4) . . . yes C(132) C(133) C(134) 121.1(5) . . . yes C(133) C(134) C(135) 119.6(5) . . . yes C(134) C(135) C(136) 120.2(5) . . . yes C(131) C(136) C(135) 120.6(4) . . . yes Cl(5) C(201) Cl(6) 107.6(4) . . . yes Cl(5) C(201) Cl(7) 114.1(5) . . . yes Cl(6) C(201) Cl(7) 110.9(4) . . . yes Cl(8) C(202) Cl(9) 110.8(3) . . . yes Cl(8) C(202) Cl(10) 110.6(4) . . . yes Cl(9) C(202) Cl(10) 108.8(4) . . . yes N(1) C(1) H(2) 106.5 . . . no N(1) C(1) H(3) 103.1 . . . no C(2) C(1) H(2) 115.2 . . . no C(2) C(1) H(3) 110.8 . . . no H(2) C(1) H(3) 114.4 . . . no C(1) C(2) H(4) 111.5 . . . no C(1) C(2) H(5) 113.0 . . . no C(3) C(2) H(4) 105.0 . . . no C(3) C(2) H(5) 108.5 . . . no H(4) C(2) H(5) 115.5 . . . no C(2) C(3) H(6) 113.1 . . . no C(2) C(3) H(7) 108.8 . . . no C(4) C(3) H(6) 112.7 . . . no C(4) C(3) H(7) 111.4 . . . no H(6) C(3) H(7) 105.7 . . . no N(1) C(4) H(1) 96.1 . . . no C(3) C(4) H(1) 115.1 . . . no C(5) C(4) H(1) 115.8 . . . no O(1) C(6) H(31) 108.2 . . . no N(1) C(6) H(31) 108.3 . . . no C(7) C(6) H(31) 108.2 . . . no C(7) C(8) H(8) 116.0 . . . no C(9) C(8) H(8) 121.8 . . . no C(8) C(9) H(9) 120.9 . . . no C(10) C(9) H(9) 119.5 . . . no C(9) C(10) H(10) 124.0 . . . no C(11) C(10) H(10) 115.3 . . . no C(10) C(11) H(11) 118.7 . . . no C(12) C(11) H(11) 120.9 . . . no C(13) C(14) H(12) 119.6 . . . no C(15) C(14) H(12) 119.0 . . . no C(14) C(15) H(13) 120.4 . . . no C(16) C(15) H(13) 119.3 . . . no C(15) C(16) H(14) 120.1 . . . no C(17) C(16) H(14) 120.1 . . . no C(16) C(17) H(15) 126.0 . . . no C(18) C(17) H(15) 113.1 . . . no C(13) C(18) H(32) 121.3 . . . no C(17) C(18) H(32) 118.6 . . . no C(19) C(20) H(16) 122.0 . . . no C(21) C(20) H(16) 117.7 . . . no C(20) C(21) H(17) 116.6 . . . no C(22) C(21) H(17) 122.0 . . . no C(21) C(22) H(18) 120.5 . . . no C(23) C(22) H(18) 121.2 . . . no C(22) C(23) H(19) 121.1 . . . no C(24) C(23) H(19) 117.2 . . . no C(19) C(24) H(20) 115.3 . . . no C(23) C(24) H(20) 124.3 . . . no C(25) C(26) H(21) 117.9 . . . no C(27) C(26) H(21) 118.2 . . . no C(26) C(27) H(22) 115.7 . . . no C(28) C(27) H(22) 125.8 . . . no C(27) C(28) H(23) 120.2 . . . no C(29) C(28) H(23) 119.4 . . . no C(28) C(29) H(24) 121.3 . . . no C(30) C(29) H(24) 117.8 . . . no C(25) C(30) H(25) 117.9 . . . no C(29) C(30) H(25) 122.8 . . . no C(31) C(32) H(26) 124.3 . . . no C(33) C(32) H(26) 114.6 . . . no C(32) C(33) H(27) 123.3 . . . no C(34) C(33) H(27) 117.0 . . . no C(33) C(34) H(28) 117.9 . . . no C(35) C(34) H(28) 121.5 . . . no C(34) C(35) H(29) 121.2 . . . no C(36) C(35) H(29) 118.5 . . . no C(31) C(36) H(30) 116.4 . . . no C(35) C(36) H(30) 123.3 . . . no N(101) C(101) H(103) 109.1 . . . no N(101) C(101) H(104) 108.9 . . . no C(102) C(101) H(103) 109.9 . . . no C(102) C(101) H(104) 103.6 . . . no H(103) C(101) H(104) 120.5 . . . no C(101) C(102) H(105) 109.2 . . . no C(101) C(102) H(106) 111.8 . . . no C(103) C(102) H(105) 110.1 . . . no C(103) C(102) H(106) 114.6 . . . no H(105) C(102) H(106) 109.3 . . . no C(102) C(103) H(107) 110.1 . . . no C(102) C(103) H(108) 110.6 . . . no C(104) C(103) H(107) 110.2 . . . no C(104) C(103) H(108) 110.7 . . . no H(107) C(103) H(108) 109.5 . . . no N(101) C(104) H(102) 104.2 . . . no C(103) C(104) H(102) 110.5 . . . no C(105) C(104) H(102) 114.3 . . . no O(101) C(106) H(101) 110.0 . . . no N(101) C(106) H(101) 108.6 . . . no C(107) C(106) H(101) 108.7 . . . no C(107) C(108) H(129) 119.6 . . . no C(109) C(108) H(129) 119.6 . . . no C(108) C(109) H(130) 120.1 . . . no C(110) C(109) H(130) 120.4 . . . no C(109) C(110) H(131) 118.3 . . . no C(111) C(110) H(131) 122.0 . . . no C(110) C(111) H(132) 119.2 . . . no C(112) C(111) H(132) 118.9 . . . no C(113) C(114) H(109) 126.4 . . . no C(115) C(114) H(109) 112.9 . . . no C(114) C(115) H(110) 115.8 . . . no C(116) C(115) H(110) 122.4 . . . no C(115) C(116) H(111) 116.3 . . . no C(117) C(116) H(111) 125.6 . . . no C(116) C(117) H(112) 125.8 . . . no C(118) C(117) H(112) 112.5 . . . no C(113) C(118) H(113) 118.9 . . . no C(117) C(118) H(113) 120.3 . . . no C(119) C(120) H(114) 122.9 . . . no C(121) C(120) H(114) 117.3 . . . no C(120) C(121) H(115) 117.8 . . . no C(122) C(121) H(115) 121.5 . . . no C(121) C(122) H(116) 119.6 . . . no C(123) C(122) H(116) 120.4 . . . no C(122) C(123) H(117) 119.8 . . . no C(124) C(123) H(117) 120.3 . . . no C(119) C(124) H(118) 122.3 . . . no C(123) C(124) H(118) 117.3 . . . no C(125) C(126) H(119) 117.6 . . . no C(127) C(126) H(119) 123.1 . . . no C(126) C(127) H(120) 119.1 . . . no C(128) C(127) H(120) 120.1 . . . no C(127) C(128) H(121) 116.5 . . . no C(129) C(128) H(121) 123.7 . . . no C(128) C(129) H(122) 123.2 . . . no C(130) C(129) H(122) 115.8 . . . no C(125) C(130) H(123) 120.6 . . . no C(129) C(130) H(123) 120.3 . . . no C(131) C(132) H(124) 119.6 . . . no C(133) C(132) H(124) 120.8 . . . no C(132) C(133) H(125) 117.9 . . . no C(134) C(133) H(125) 121.0 . . . no C(133) C(134) H(126) 121.7 . . . no C(135) C(134) H(126) 118.8 . . . no C(134) C(135) H(127) 114.8 . . . no C(136) C(135) H(127) 124.9 . . . no C(131) C(136) H(128) 120.6 . . . no C(135) C(136) H(128) 118.7 . . . no Cl(5) C(201) H(133) 99.4 . . . no Cl(6) C(201) H(133) 103.6 . . . no Cl(7) C(201) H(133) 120.0 . . . no Cl(8) C(202) H(134) 112.2 . . . no Cl(9) C(202) H(134) 114.1 . . . no Cl(10) C(202) H(134) 99.7 . . . no #------------------------------------------------------------------------------ #===END