# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1360 #======================================================= # # Gold(I) chloride adducts with bidentate 2-, 3- and 4-pyridyl phosphines. # Solution P31 NMR studies of 2:1 and 1:2 complexes and the # crystal structures of dimeric [(d2pype)Au(mu2-d2pype)]Cl2.14H2O # and monomeric [Au(d4pype)2]Cl.HCL.62O. # # Susan J. Berners-Price, Richard J. Bowen, Trevor W. Hambley and Peter C. Healy # # # submitted to: J. Chem. Soc. Dalton Transactions: paper 8/09285K # # # CIF files for the crystal structures described in the paper: # # 1. [Au(d4pype)2]Cl.HCL.62O - d4pype # 2. [(d2pype)Au(mu2-d2pype)]Cl2.14H2O - d2pype # # #======================================================= data_d4pype #---------------------------------------------------------------------- _audit_creation_date 'Fri Jan 12 11:47:55 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #---------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #---------------------------------------------------------------------- _cell_length_a 12.29(2) _cell_length_b 13.49(3) _cell_length_c 15.00(1) _cell_angle_alpha 90 _cell_angle_beta 95.11(10) _cell_angle_gamma 90 _cell_volume 2477(7) _cell_formula_units_Z 2 _cell_measurement_temperature 294.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 #---------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #---------------------------------------------------------------------- _exptl_crystal_description 'prisms' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_meas ? _chemical_formula_weight 1181.72 _chemical_formula_analytical ? _chemical_formula_sum 'C44 H53 Au Cl2 N8 O6 P4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 3.214 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa_analytical _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_correction_T_min 0.626 #---------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_decay_% -8.80 _diffrn_reflns_number 3550 _reflns_number_total 3385 _reflns_number_observed 2617 _reflns_observed_criterion 'I > 2.5\s(I)' _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 22.58 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.06076 _diffrn_orient_matrix_UB_12 0.04688 _diffrn_orient_matrix_UB_13 0.01890 _diffrn_orient_matrix_UB_21 -0.01891 _diffrn_orient_matrix_UB_22 -0.00428 _diffrn_orient_matrix_UB_23 0.06331 _diffrn_orient_matrix_UB_31 0.05137 _diffrn_orient_matrix_UB_32 -0.05721 _diffrn_orient_matrix_UB_33 0.01052 #---------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Au 0 2 -2.013 8.802 'International Tables' C 0 88 0.003 0.002 'International Tables' H 0 80 0.000 0.000 'International Tables' P 0 8 0.102 0.094 'International Tables' Cl 0 2 0.148 0.159 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 2 0.011 0.006 'International Tables' Na 0 2 0.036 0.025 'International Tables' #---------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Au(1) -0.24100(8) 0 -0.24878(7) 0.0458(3) Uij ? ? Cl(1) -0.1018(8) 0.005(2) -0.8362(6) 0.101(4) Uij ? ? Cl(2) -0.428(1) -0.163(1) -0.7198(7) 0.103(5) Uij ? ? P(1) -0.3674(7) -0.1273(8) -0.2198(5) 0.048(3) Uij ? ? P(2) -0.1158(6) -0.1295(8) -0.2669(5) 0.049(3) Uij ? ? P(3) -0.2449(7) 0.1165(8) -0.3714(5) 0.056(3) Uij ? ? P(4) -0.2534(7) 0.1401(7) -0.1542(5) 0.051(3) Uij ? ? O(1) -0.250(3) -0.328(3) -0.767(3) 0.18(2) Uij ? ? O(2) -0.298(2) 0.039(2) -0.721(2) 0.11(1) Uij ? ? O(3) -0.058(2) -0.208(3) -0.755(2) 0.10(1) Uij ? ? O(4) 0.153(2) -0.007(4) -0.792(2) 0.14(1) Uij ? ? O(5) 0.294(3) -0.013(4) -0.914(3) 0.17(2) Uij ? ? O(6) 0.229(2) 0.022(5) -0.622(2) 0.16(2) Uij ? ? N(11) -0.709(3) -0.146(4) -0.374(2) 0.10(1) Uij ? ? N(12) -0.416(3) -0.137(2) 0.080(2) 0.06(1) Uij ? ? N(21) 0.235(2) -0.140(3) -0.140(2) 0.08(1) Uij ? ? N(22) -0.074(3) -0.165(3) -0.568(2) 0.08(1) Uij ? ? N(31) -0.571(3) 0.119(3) -0.552(2) 0.09(1) Uij ? ? N(32) 0.056(2) 0.086(3) -0.530(2) 0.08(1) Uij ? ? N(41) 0.058(3) 0.249(4) 0.011(2) 0.10(1) Uij ? ? N(42) -0.532(3) 0.111(2) 0.032(2) 0.07(1) Uij ? ? C(1) -0.302(4) -0.240(3) -0.245(2) 0.05(1) Uij ? ? C(2) -0.184(3) -0.236(3) -0.227(2) 0.053(8) Uij ? ? C(3) -0.234(2) 0.234(3) -0.314(2) 0.052(8) Uij ? ? C(4) -0.289(3) 0.244(3) -0.232(2) 0.05(1) Uij ? ? C(111) -0.509(3) -0.134(3) -0.277(2) 0.056(9) Uij ? ? C(112) -0.547(4) -0.052(4) -0.320(3) 0.09(1) Uij ? ? C(113) -0.654(4) -0.061(4) -0.362(3) 0.10(1) Uij ? ? C(115) -0.663(3) -0.224(3) -0.333(3) 0.07(1) Uij ? ? C(116) -0.565(3) -0.219(3) -0.291(2) 0.065(10) Uij ? ? C(121) -0.397(3) -0.133(3) -0.096(2) 0.041(8) Uij ? ? C(122) -0.305(3) -0.147(3) -0.039(2) 0.061(10) Uij ? ? C(123) -0.319(3) -0.148(3) 0.051(2) 0.059(9) Uij ? ? C(125) -0.502(3) -0.130(3) 0.022(2) 0.05(1) Uij ? ? C(126) -0.497(3) -0.128(3) -0.071(3) 0.06(1) Uij ? ? C(211) 0.030(3) -0.135(3) -0.217(2) 0.051(8) Uij ? ? C(212) 0.078(3) -0.051(3) -0.190(2) 0.066(10) Uij ? ? C(213) 0.192(4) -0.059(4) -0.152(3) 0.09(1) Uij ? ? C(215) 0.186(3) -0.215(3) -0.166(3) 0.07(1) Uij ? ? C(216) 0.082(3) -0.219(3) -0.201(2) 0.07(1) Uij ? ? C(221) -0.094(2) -0.147(3) -0.388(2) 0.049(8) Uij ? ? C(222) -0.188(2) -0.160(3) -0.444(2) 0.050(8) Uij ? ? C(223) -0.174(3) -0.170(3) -0.536(2) 0.07(1) Uij ? ? C(225) 0.012(3) -0.151(3) -0.512(2) 0.059(9) Uij ? ? C(226) 0.004(3) -0.149(3) -0.418(3) 0.07(1) Uij ? ? C(311) -0.373(3) 0.127(3) -0.449(2) 0.07(1) Uij ? ? C(312) -0.396(3) 0.040(3) -0.508(2) 0.070(10) Uij ? ? C(313) -0.492(3) 0.045(3) -0.560(3) 0.09(1) Uij ? ? C(315) -0.543(4) 0.187(4) -0.501(3) 0.09(1) Uij ? ? C(316) -0.446(3) 0.207(3) -0.446(3) 0.08(1) Uij ? ? C(321) -0.133(2) 0.109(3) -0.438(2) 0.050(8) Uij ? ? C(322) -0.024(3) 0.110(3) -0.394(2) 0.063(10) Uij ? ? C(323) 0.064(3) 0.099(3) -0.438(2) 0.066(10) Uij ? ? C(325) -0.046(3) 0.084(3) -0.572(2) 0.07(1) Uij ? ? C(326) -0.138(3) 0.097(3) -0.530(2) 0.064(9) Uij ? ? C(411) -0.134(3) 0.185(3) -0.086(2) 0.062(9) Uij ? ? C(412) -0.055(3) 0.120(3) -0.052(2) 0.08(1) Uij ? ? C(413) 0.043(3) 0.153(3) -0.002(2) 0.059(9) Uij ? ? C(415) -0.012(4) 0.305(4) -0.024(3) 0.08(1) Uij ? ? C(416) -0.112(3) 0.284(3) -0.074(3) 0.07(1) Uij ? ? C(421) -0.358(3) 0.134(3) -0.082(2) 0.06(1) Uij ? ? C(422) -0.470(3) 0.138(3) -0.112(3) 0.07(1) Uij ? ? C(423) -0.550(3) 0.127(3) -0.055(2) 0.06(1) Uij ? ? C(425) -0.427(3) 0.103(3) 0.063(3) 0.06(1) Uij ? ? C(426) -0.334(3) 0.117(3) 0.011(2) 0.055(9) Uij ? ? H(11) -0.3292 -0.2914 -0.2098 0.065 Uiso c ? H(12) -0.3190 -0.2545 -0.3066 0.065 Uiso c ? H(21) -0.1547 -0.2929 -0.2536 0.065 Uiso c ? H(22) -0.1678 -0.2388 -0.1639 0.065 Uiso c ? H(31) -0.1585 0.2466 -0.2990 0.062 Uiso c ? H(32) -0.2632 0.2832 -0.3547 0.062 Uiso c ? H(41) -0.3658 0.2444 -0.2469 0.060 Uiso c ? H(42) -0.2674 0.3046 -0.2035 0.060 Uiso c ? H(112) -0.5053 0.0071 -0.3220 0.111 Uiso c ? H(113) -0.6896 -0.0020 -0.3834 0.114 Uiso c ? H(115) -0.7017 -0.2850 -0.3340 0.088 Uiso c ? H(116) -0.5316 -0.2788 -0.2692 0.077 Uiso c ? H(122) -0.2352 -0.1556 -0.0604 0.072 Uiso c ? H(123) -0.2572 -0.1568 0.0930 0.071 Uiso c ? H(125) -0.5718 -0.1260 0.0443 0.062 Uiso c ? H(126) -0.5600 -0.1234 -0.1123 0.075 Uiso c ? H(212) 0.0409 0.0108 -0.1949 0.080 Uiso c ? H(213) 0.2326 -0.0006 -0.1366 0.106 Uiso c ? H(215) 0.2252 -0.2757 -0.1609 0.785 Uiso c ? H(216) 0.0469 -0.2808 -0.2139 0.785 Uiso c ? H(222) -0.2581 -0.1621 -0.4220 0.060 Uiso c ? H(223) -0.2365 -0.1806 -0.5769 0.081 Uiso c ? H(225) 0.0812 -0.1420 -0.5344 0.071 Uiso c ? H(226) 0.0679 -0.1491 -0.3774 0.086 Uiso c ? H(312) -0.3475 -0.0147 -0.5093 0.084 Uiso c ? H(313) -0.5067 -0.0045 -0.6045 0.103 Uiso c ? H(315) -0.5976 0.2364 -0.4977 0.113 Uiso c ? H(316) -0.4322 0.2658 -0.4120 0.095 Uiso c ? H(322) -0.0148 0.1189 -0.3310 0.075 Uiso c ? H(323) 0.1341 0.1000 -0.4058 0.080 Uiso c ? H(325) -0.0536 0.0728 -0.6348 0.085 Uiso c ? H(326) -0.2069 0.0979 -0.5641 0.077 Uiso c ? H(412) -0.0657 0.0510 -0.0619 0.094 Uiso c ? H(413) 0.0963 0.1066 0.0214 0.071 Uiso c ? H(415) 0.0037 0.3736 -0.0161 0.091 Uiso c ? H(416) -0.1603 0.3344 -0.0975 0.082 Uiso c ? H(422) -0.4905 0.1487 -0.1738 0.086 Uiso c ? H(423) -0.6238 0.1312 -0.0797 0.076 Uiso c ? H(425) -0.4119 0.0867 0.1245 0.076 Uiso c ? H(426) -0.2610 0.1149 0.0378 0.066 Uiso c ? 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 Au 0.0431(6) 0.0560(6) 0.0398(5) 0.001(2) 0.0116(4) 0.000(1) Cl(1) 0.104(9) 0.16(1) 0.054(6) -0.049(9) 0.029(5) -0.012(7) Cl(2) 0.101(7) 0.115(9) 0.090(7) 0.00(2) 0.018(5) 0.00(1) P(1) 0.045(4) 0.052(6) 0.047(5) -0.008(5) 0.009(4) 0.000(5) P(2) 0.039(4) 0.067(7) 0.042(5) 0.000(5) 0.008(3) -0.001(5) P(3) 0.047(5) 0.087(8) 0.036(4) -0.003(5) 0.010(4) 0.011(5) P(4) 0.057(5) 0.056(6) 0.039(4) 0.020(5) 0.007(4) -0.014(5) O(1) 0.21(5) 0.09(3) 0.22(5) 0.02(3) -0.07(4) -0.04(3) O(2) 0.12(2) 0.13(3) 0.08(2) -0.04(2) 0.01(2) -0.02(2) O(3) 0.12(2) 0.13(3) 0.06(2) 0.02(2) 0.04(2) 0.02(2) O(4) 0.14(2) 0.17(4) 0.11(2) -0.05(4) 0.05(2) -0.03(3) O(5) 0.19(3) 0.13(4) 0.21(4) -0.06(4) 0.12(3) -0.03(4) O(6) 0.08(2) 0.31(7) 0.10(2) -0.01(4) 0.03(1) -0.07(4) N(11) 0.06(2) 0.17(4) 0.07(2) -0.04(3) 0.00(2) -0.01(3) N(12) 0.11(3) 0.04(2) 0.03(1) 0.01(2) 0.02(2) 0.00(1) N(21) 0.06(2) 0.12(3) 0.08(2) 0.03(2) 0.02(2) 0.00(2) N(22) 0.11(3) 0.10(3) 0.05(2) 0.03(2) 0.03(2) 0.01(2) N(31) 0.09(2) 0.11(3) 0.08(2) -0.01(2) 0.02(2) 0.02(2) N(32) 0.07(2) 0.06(2) 0.10(3) 0.00(2) 0.04(2) 0.00(2) N(41) 0.08(2) 0.16(4) 0.05(2) -0.07(3) 0.02(2) -0.01(2) N(42) 0.06(2) 0.04(2) 0.10(3) 0.00(2) 0.04(2) -0.01(2) #---------------------------------------------------------------------- _refine_special_details ; The crystal used for the data collection was of marginal quality but the best available. Anisotropic thermal parameters were refined for all non-hydrogen atoms except the carbon atoms of the d4pype ligands. Hydrogen atoms were included on the d4pype ligands, constrained at estimated values. Hydrogen atoms were not located on the solvent water molecules or protonated pyridyl rings. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2617 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0780 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0900 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.210 _refine_ls_shift/esd_max 0.0880 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.45 _refine_diff_density_max 3.58 #---------------------------------------------------------------------- _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 AU P1 2.38(1) . . yes AU P2 2.36(1) . . yes AU P3 2.417(9) . . yes AU P4 2.376(9) . . yes P1 C1 1.78(4) . . yes P1 C111 1.87(4) . . yes P1 C121 1.93(3) . . yes P2 C2 1.79(4) . . yes P2 C211 1.88(4) . . yes P2 C221 1.87(3) . . yes P3 C3 1.80(4) . . yes P3 C311 1.88(3) . . yes P3 C321 1.77(3) . . yes P4 C4 1.85(4) . . yes P4 C411 1.82(4) . . yes P4 C421 1.76(4) . . yes N11 C113 1.34(7) . . yes N11 C115 1.32(6) . . yes N12 C123 1.31(5) . . yes N12 C125 1.31(5) . . yes N21 C213 1.22(6) . . yes N21 C215 1.22(5) . . yes N22 C223 1.36(5) . . yes N22 C225 1.30(5) . . yes N31 C313 1.41(6) . . yes N31 C315 1.22(6) . . yes N32 C323 1.39(4) . . yes N32 C325 1.35(4) . . yes N41 C413 1.32(7) . . yes N41 C415 1.23(7) . . yes N42 C423 1.32(4) . . yes N42 C425 1.34(5) . . yes C1 C2 1.45(6) . . yes C1 H11 0.95 . . no C1 H12 0.95 . . no C2 H21 0.95 . . no C2 H22 0.95 . . no C3 C4 1.46(4) . . yes C3 H31 0.95 . . no C3 H32 0.95 . . no C4 H41 0.95 . . no C4 H42 0.95 . . no C111 C112 1.34(6) . . yes C111 C116 1.34(6) . . yes C112 C113 1.41(7) . . yes C112 H112 0.95 . . no C113 H113 0.95 . . no C115 C116 1.31(5) . . yes C115 H115 0.95 . . no C116 H116 0.95 . . no C121 C122 1.37(5) . . yes C121 C126 1.32(5) . . yes C122 C123 1.38(4) . . yes C122 H122 0.95 . . no C123 H123 0.95 . . no C125 C126 1.40(5) . . yes C125 H125 0.95 . . no C126 H126 0.95 . . no C211 C212 1.32(5) . . yes C211 C216 1.31(6) . . yes C212 C213 1.47(6) . . yes C212 H212 0.95 . . no C213 H213 0.95 . . no C215 C216 1.34(5) . . yes C215 H215 0.95 . . no C216 H216 0.95 . . no C221 C222 1.38(4) . . yes C221 C226 1.32(5) . . yes C222 C223 1.41(4) . . yes C222 H222 0.95 . . no C223 H223 0.95 . . no C225 C226 1.42(5) . . yes C225 H225 0.95 . . no C226 H226 0.95 . . no C311 C312 1.48(5) . . yes C311 C316 1.41(6) . . yes C312 C313 1.36(5) . . yes C312 H312 0.95 . . no C313 H313 0.95 . . no C315 C316 1.41(6) . . yes C315 H315 0.95 . . no C316 H316 0.95 . . no C321 C322 1.44(4) . . yes C321 C326 1.39(4) . . yes C322 C323 1.32(5) . . yes C322 H322 0.95 . . no C323 H323 0.95 . . no C325 C326 1.35(5) . . yes C325 H325 0.95 . . no C326 H326 0.95 . . no C411 C412 1.37(5) . . yes C411 C416 1.37(6) . . yes C412 C413 1.43(5) . . yes C412 H412 0.95 . . no C413 H413 0.95 . . no C415 C416 1.41(6) . . yes C415 H415 0.95 . . no C416 H416 0.95 . . no C421 C422 1.41(5) . . yes C421 C426 1.42(4) . . yes C422 C423 1.37(6) . . yes C422 H422 0.95 . . no C423 H423 0.95 . . no C425 C426 1.45(6) . . yes C425 H425 0.95 . . no C426 H426 0.95 . . 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 P1 AU P2 86.0(3) . . . yes P1 AU P3 129.7(3) . . . yes P1 AU P4 112.8(3) . . . yes P2 AU P3 111.3(3) . . . yes P2 AU P4 137.3(3) . . . yes P3 AU P4 86.5(3) . . . yes AU P1 C1 105(2) . . . yes AU P1 C111 123(1) . . . yes AU P1 C121 113(1) . . . yes C1 P1 C111 106(2) . . . yes C1 P1 C121 107(2) . . . yes C111 P1 C121 101(2) . . . yes AU P2 C2 103(1) . . . yes AU P2 C211 126(1) . . . yes AU P2 C221 111(1) . . . yes C2 P2 C211 107(2) . . . yes C2 P2 C221 110(2) . . . yes C211 P2 C221 100(1) . . . yes AU P3 C3 102(1) . . . yes AU P3 C311 119(1) . . . yes AU P3 C321 115(1) . . . yes C3 P3 C311 105(2) . . . yes C3 P3 C321 107(2) . . . yes C311 P3 C321 108(1) . . . yes AU P4 C4 104(1) . . . yes AU P4 C411 121(1) . . . yes AU P4 C421 115(1) . . . yes C4 P4 C411 104(2) . . . yes C4 P4 C421 106(2) . . . yes C411 P4 C421 106(2) . . . yes C113 N11 C115 116(4) . . . yes C123 N12 C125 119(3) . . . yes C213 N21 C215 120(4) . . . yes C223 N22 C225 119(3) . . . yes C313 N31 C315 115(4) . . . yes C323 N32 C325 117(3) . . . yes C413 N41 C415 117(4) . . . yes C423 N42 C425 115(4) . . . yes P1 C1 C2 113(3) . . . yes P1 C1 H11 108.6 . . . no P1 C1 H12 108.6 . . . no C2 C1 H11 108.6 . . . no C2 C1 H12 108.6 . . . no H11 C1 H12 109.5 . . . no P2 C2 C1 117(3) . . . yes P2 C2 H21 107.5 . . . no P2 C2 H22 107.5 . . . no C1 C2 H21 107.5 . . . no C1 C2 H22 107.5 . . . no H21 C2 H22 109.5 . . . no P3 C3 C4 118(3) . . . yes P3 C3 H31 107.4 . . . no P3 C3 H32 107.4 . . . no C4 C3 H31 107.4 . . . no C4 C3 H32 107.4 . . . no H31 C3 H32 109.5 . . . no P4 C4 C3 111(3) . . . yes P4 C4 H41 109.1 . . . no P4 C4 H42 109.1 . . . no C3 C4 H41 109.1 . . . no C3 C4 H42 109.1 . . . no H41 C4 H42 109.5 . . . no P1 C111 C112 117(3) . . . yes P1 C111 C116 124(3) . . . yes C112 C111 C116 118(4) . . . yes C111 C112 C113 114(5) . . . yes C111 C112 H112 122.8 . . . no C113 C112 H112 122.8 . . . no N11 C113 C112 125(5) . . . yes N11 C113 H113 117.5 . . . no C112 C113 H113 117.5 . . . no N11 C115 C116 121(4) . . . yes N11 C115 H115 119.3 . . . no C116 C115 H115 119.3 . . . no C111 C116 C115 124(4) . . . yes C111 C116 H116 118.1 . . . no C115 C116 H116 118.1 . . . no P1 C121 C122 113(3) . . . yes P1 C121 C126 122(3) . . . yes C122 C121 C126 125(3) . . . yes C121 C122 C123 116(3) . . . yes C121 C122 H122 121.8 . . . no C123 C122 H122 121.8 . . . no N12 C123 C122 121(3) . . . yes N12 C123 H123 119.3 . . . no C122 C123 H123 119.3 . . . no N12 C125 C126 124(4) . . . yes N12 C125 H125 118.1 . . . no C126 C125 H125 118.1 . . . no C121 C126 C125 114(3) . . . yes C121 C126 H126 123.0 . . . no C125 C126 H126 123.0 . . . no P2 C211 C212 118(3) . . . yes P2 C211 C216 123(3) . . . yes C212 C211 C216 119(3) . . . yes C211 C212 C213 116(4) . . . yes C211 C212 H212 122.0 . . . no C213 C212 H212 122.0 . . . no N21 C213 C212 121(4) . . . yes N21 C213 H213 119.7 . . . no C212 C213 H213 119.7 . . . no N21 C215 C216 126(4) . . . yes N21 C215 H215 117.1 . . . no C216 C215 H215 117.1 . . . no C211 C216 C215 118(4) . . . yes C211 C216 H216 121.0 . . . no C215 C216 H216 121.0 . . . no P2 C221 C222 115(2) . . . yes P2 C221 C226 123(3) . . . yes C222 C221 C226 122(3) . . . yes C221 C222 C223 116(3) . . . yes C221 C222 H222 122.0 . . . no C223 C222 H222 122.0 . . . no N22 C223 C222 122(3) . . . yes N22 C223 H223 118.9 . . . no C222 C223 H223 118.9 . . . no N22 C225 C226 121(3) . . . yes N22 C225 H225 119.4 . . . no C226 C225 H225 119.4 . . . no C221 C226 C225 119(3) . . . yes C221 C226 H226 120.6 . . . no C225 C226 H226 120.6 . . . no P3 C311 C312 115(3) . . . yes P3 C311 C316 123(3) . . . yes C312 C311 C316 123(3) . . . yes C311 C312 C313 114(4) . . . yes C311 C312 H312 122.8 . . . no C313 C312 H312 122.8 . . . no N31 C313 C312 124(4) . . . yes N31 C313 H313 118.0 . . . no C312 C313 H313 118.0 . . . no N31 C315 C316 133(5) . . . yes N31 C315 H315 113.5 . . . no C316 C315 H315 113.5 . . . no C311 C316 C315 110(4) . . . yes C311 C316 H316 125.0 . . . no C315 C316 H316 125.0 . . . no P3 C321 C322 119(2) . . . yes P3 C321 C326 127(2) . . . yes C322 C321 C326 114(3) . . . yes C321 C322 C323 123(3) . . . yes C321 C322 H322 118.7 . . . no C323 C322 H322 118.7 . . . no N32 C323 C322 121(3) . . . yes N32 C323 H323 119.3 . . . no C322 C323 H323 119.3 . . . no N32 C325 C326 124(3) . . . yes N32 C325 H325 118.0 . . . no C326 C325 H325 118.0 . . . no C321 C326 C325 121(3) . . . yes C321 C326 H326 119.5 . . . no C325 C326 H326 119.5 . . . no P4 C411 C412 120(3) . . . yes P4 C411 C416 123(3) . . . yes C412 C411 C416 117(3) . . . yes C411 C412 C413 122(4) . . . yes C411 C412 H412 119.0 . . . no C413 C412 H412 119.0 . . . no N41 C413 C412 119(4) . . . yes N41 C413 H413 120.6 . . . no C412 C413 H413 120.6 . . . no N41 C415 C416 130(5) . . . yes N41 C415 H415 114.8 . . . no C416 C415 H415 114.8 . . . no C411 C416 C415 115(4) . . . yes C411 C416 H416 122.7 . . . no C415 C416 H416 122.7 . . . no P4 C421 C422 123(3) . . . yes P4 C421 C426 121(3) . . . yes C422 C421 C426 116(3) . . . yes C421 C422 C423 122(4) . . . yes C421 C422 H422 118.9 . . . no C423 C422 H422 118.9 . . . no N42 C423 C422 125(4) . . . yes N42 C423 H423 117.7 . . . no C422 C423 H423 117.7 . . . no N42 C425 C426 126(4) . . . yes N42 C425 H425 117.1 . . . no C426 C425 H425 117.1 . . . no C421 C426 C425 116(3) . . . yes C421 C426 H426 121.8 . . . no C425 C426 H426 121.8 . . . no #---------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag CL1 N12 3.04(3) . 1_554 no CL1 O2 3.16(3) . . no CL1 O1 3.24(4) . . no CL1 C316 3.51(5) . 2_444 no CL2 O2 3.12(3) . . no CL2 O4 3.15(3) . . no CL2 O3 3.15(5) . . no O1 O3 2.85(5) . . no O1 C213 3.44(7) . 2_544 no O1 C423 3.52(5) . 2_444 no O2 C115 3.34(5) . 2_454 no O2 C326 3.42(4) . . no O2 C312 3.51(4) . . no O2 C313 3.54(5) . . no O2 C425 3.58(5) . 1_554 no O3 N22 2.89(4) . . no O3 C322 3.41(5) . 2_544 no O3 C416 3.45(5) . 2_544 no O3 C415 3.50(6) . 2_544 no O4 O5 2.63(5) . . no O4 O6 2.67(4) . . no O4 C416 3.47(6) . 2_544 no O5 N42 2.89(6) . 1_654 no O5 C125 3.18(6) . 1_654 no O5 C423 3.53(6) . 1_654 no O5 C416 3.53(6) . 2_544 no O6 N32 2.77(4) . . no O6 N31 2.90(5) . 1_655 no O6 C313 3.49(4) . 1_655 no N11 C226 3.53(5) . 1_455 no N12 C423 3.23(5) . 2_445 no N12 C422 3.39(5) . 2_445 no N21 C126 3.37(4) . 1_655 no N21 C115 3.45(5) . 1_655 no N22 C323 3.19(6) . 2_544 no N22 C322 3.33(6) . 2_544 no N41 C122 3.34(5) . 2 no N41 C2 3.47(4) . 2 no N41 C216 3.48(5) . 2 no N42 C126 3.58(5) . 2_455 no C115 C215 3.25(6) . 1_455 no C123 C423 3.44(6) . 2_445 no C125 C423 3.37(6) . 2_445 no C125 C422 3.44(6) . 2_445 no C216 C415 3.57(6) . 2_545 no C223 C323 3.43(6) . 2_544 no C225 C322 3.53(6) . 2_544 no C225 C323 3.56(6) . 2_544 no #=========================================================END data_d2pype #---------------------------------------------------------------------- _audit_creation_date 'Fri Jan 12 11:47:03 1996' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #---------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #---------------------------------------------------------------------- _cell_length_a 22.519(5) _cell_length_b 17.937(6) _cell_length_c 26.565(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10730(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294.2 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 18.5 _cell_measurement_theta_max 24.6 #---------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2-y,1/2+z' '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' '1/2+x,1/2+y,1/2-z' '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' #---------------------------------------------------------------------- _exptl_crystal_description 'plates' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_meas ? _chemical_formula_weight 2326.56 _chemical_formula_analytical ? _chemical_formula_sum 'C88 H108 Au2 Cl2 N16 O14 P8 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4688 _exptl_absorpt_coefficient_mu 6.926 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_T_min 0.613 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 294.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.61 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -5 1 -3 -5 -1 -2 -5 -2 _diffrn_reflns_number 8730 _reflns_number_total 8701 _reflns_number_observed 3411 _reflns_observed_criterion 'I > 2.5\s(I)' _diffrn_reflns_av_R_equivalents 0.371 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 60.44 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.03937 _diffrn_orient_matrix_UB_12 -0.02481 _diffrn_orient_matrix_UB_13 -0.00481 _diffrn_orient_matrix_UB_21 0.01706 _diffrn_orient_matrix_UB_22 -0.04802 _diffrn_orient_matrix_UB_23 0.01252 _diffrn_orient_matrix_UB_31 -0.01145 _diffrn_orient_matrix_UB_32 0.01368 _diffrn_orient_matrix_UB_33 0.03517 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 352 0.018 0.009 'International Tables' H 0 256 0.000 0.000 'International Tables' P 0 32 0.295 0.434 'International Tables' N 0 128 0.031 0.018 'International Tables' Au 0 8 -4.420 7.298 'International Tables' O 0 128 0.049 0.032 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Au(1) 0.02962(4) 0.33803(5) 0.47512(4) 0.0548(3) Uij ? ? P(1) -0.0150(3) 0.3249(3) 0.3929(2) 0.063(2) Uij ? ? P(2) 0.0439(3) 0.2032(3) 0.4696(3) 0.066(2) Uij ? ? P(3) -0.0357(3) 0.3668(3) 0.5427(2) 0.052(2) Uij ? ? P(4) 0.1172(2) 0.4107(3) 0.4790(2) 0.051(2) Uij ? ? O(1) 0.119(2) 0.039(2) 0.143(1) 0.30(2) Uij ? ? O(2) 0.277(2) 0.236(2) 0.246(2) 0.36(2) Uij ? ? O(3) -0.146(2) 0.361(3) 0.706(2) 0.37(2) Uij ? ? O(4) -0.321(1) 0.344(2) 0.673(1) 0.25(1) Uij ? ? O(5) -0.389(2) 0.475(2) 0.670(2) 0.34(2) Uij ? ? O(6) 0.171(2) 0.134(2) 0.706(1) 0.28(2) Uij ? ? O(7) 0.025(2) 0.018(3) 0.647(2) 0.40(2) Uij ? ? O(8) 0.0000 0.113(3) 0.7500 0.33(3) Uij ? ? O(9) 0.106(2) 0.188(2) 0.804(1) 0.28(2) Uij ? ? O(10) 0.128(2) -0.148(2) 0.710(1) 0.29(2) Uij ? ? N(112) -0.0908(10) 0.436(1) 0.3828(7) 0.080(9) Uij ? ? N(122) 0.037(2) 0.429(2) 0.343(1) 0.13(1) Uij ? ? N(212) -0.024(1) 0.157(1) 0.5489(9) 0.087(8) Uij ? ? N(222) 0.118(1) 0.155(1) 0.5399(9) 0.084(9) Uij ? ? N(312) 0.009(1) 0.269(1) 0.6077(9) 0.100(10) Uij ? ? N(322) -0.1182(10) 0.278(1) 0.4980(9) 0.089(9) Uij ? ? N(412) 0.2179(9) 0.431(1) 0.5332(8) 0.074(8) Uij ? ? N(422) 0.1943(9) 0.472(2) 0.4116(9) 0.11(1) Uij ? ? C(1) -0.023(1) 0.227(1) 0.3850(10) 0.09(1) Uij ? ? C(2) 0.036(1) 0.184(1) 0.4038(9) 0.078(9) Uij ? ? C(3) -0.0597(9) 0.461(1) 0.5545(8) 0.046(7) Uij ? ? C(4) 0.1005(9) 0.509(1) 0.4893(8) 0.056(8) Uij ? ? C(111) -0.088(1) 0.362(1) 0.3772(8) 0.061(9) Uij ? ? C(113) -0.145(1) 0.470(2) 0.370(1) 0.09(1) Uij ? ? C(114) -0.192(1) 0.429(2) 0.357(1) 0.09(1) Uij ? ? C(115) -0.187(1) 0.351(2) 0.352(1) 0.10(1) Uij ? ? C(116) -0.135(1) 0.317(1) 0.3630(8) 0.069(9) Uij ? ? C(121) 0.027(1) 0.357(1) 0.339(1) 0.071(9) Uij ? ? C(123) 0.063(3) 0.453(4) 0.315(2) 0.27(4) Uij ? ? C(124) 0.086(2) 0.437(3) 0.279(3) 0.20(3) Uij ? ? C(125) 0.087(1) 0.359(3) 0.264(1) 0.15(2) Uij ? ? C(126) 0.052(1) 0.314(1) 0.300(1) 0.08(1) Uij ? ? C(211) -0.011(1) 0.140(1) 0.500(1) 0.07(1) Uij ? ? C(213) -0.063(2) 0.115(2) 0.576(1) 0.11(1) Uij ? ? C(214) -0.095(2) 0.061(2) 0.548(2) 0.13(2) Uij ? ? C(215) -0.084(2) 0.046(2) 0.499(2) 0.12(1) Uij ? ? C(216) -0.042(1) 0.088(2) 0.475(1) 0.09(1) Uij ? ? C(221) 0.112(1) 0.158(1) 0.492(1) 0.063(9) Uij ? ? C(223) 0.169(2) 0.127(2) 0.558(1) 0.10(1) Uij ? ? C(224) 0.214(2) 0.102(2) 0.528(2) 0.12(2) Uij ? ? C(225) 0.209(2) 0.104(2) 0.479(2) 0.14(2) Uij ? ? C(226) 0.155(1) 0.138(1) 0.457(1) 0.09(1) Uij ? ? C(311) -0.0026(10) 0.341(2) 0.6023(9) 0.062(8) Uij ? ? C(313) 0.039(2) 0.246(2) 0.646(2) 0.13(2) Uij ? ? C(314) 0.062(2) 0.295(2) 0.684(1) 0.15(2) Uij ? ? C(315) 0.049(1) 0.370(2) 0.680(1) 0.10(1) Uij ? ? C(316) 0.018(1) 0.395(1) 0.6372(10) 0.08(1) Uij ? ? C(321) -0.105(1) 0.311(1) 0.542(1) 0.068(9) Uij ? ? C(323) -0.168(2) 0.237(2) 0.499(1) 0.11(1) Uij ? ? C(324) -0.204(2) 0.228(2) 0.537(2) 0.11(2) Uij ? ? C(325) -0.191(2) 0.260(2) 0.577(2) 0.14(2) Uij ? ? C(326) -0.139(1) 0.307(2) 0.585(1) 0.11(1) Uij ? ? C(411) 0.169(1) 0.389(1) 0.5308(9) 0.055(8) Uij ? ? C(413) 0.254(1) 0.416(1) 0.569(1) 0.074(9) Uij ? ? C(414) 0.245(1) 0.362(2) 0.6049(9) 0.073(10) Uij ? ? C(415) 0.195(1) 0.318(2) 0.6025(10) 0.08(1) Uij ? ? C(416) 0.1567(10) 0.332(1) 0.5636(9) 0.067(9) Uij ? ? C(421) 0.1650(10) 0.410(2) 0.4242(9) 0.059(8) Uij ? ? C(423) 0.230(2) 0.459(3) 0.366(2) 0.16(2) Uij ? ? C(424) 0.229(2) 0.391(4) 0.347(2) 0.17(3) Uij ? ? C(425) 0.195(3) 0.343(3) 0.356(2) 0.20(3) Uij ? ? C(426) 0.167(1) 0.346(2) 0.397(1) 0.09(1) Uij ? ? H(11) -0.0564 0.2094 0.4045 0.112 Uiso c ? H(12) -0.0292 0.2158 0.3497 0.112 Uiso c ? H(21) 0.0710 0.2029 0.3859 0.093 Uiso c ? H(22) 0.0328 0.1311 0.3984 0.093 Uiso c ? H(31) -0.0822 0.4628 0.5868 0.054 Uiso c ? H(32) -0.0248 0.4937 0.5593 0.054 Uiso c ? H(41) 0.0789 0.5155 0.5225 0.064 Uiso c ? H(42) 0.1368 0.5389 0.4926 0.064 Uiso c ? H(113) -0.1479 0.5235 0.3716 0.105 Uiso c ? H(114) -0.2292 0.4536 0.3507 0.110 Uiso c ? H(115) -0.2215 0.3221 0.3411 0.116 Uiso c ? H(116) -0.1304 0.2629 0.3610 0.0827 Uiso c ? H(123) 0.0746 0.5129 0.3154 0.190 Uiso c ? H(124) 0.1089 0.4593 0.2469 0.186 Uiso c ? H(125) 0.1055 0.3260 0.2383 0.157 Uiso c ? H(126) 0.0443 0.2594 0.2999 0.095 Uiso c ? H(213) -0.0697 0.1227 0.6118 0.138 Uiso c ? H(214) -0.1261 0.0325 0.5643 0.152 Uiso c ? H(215) -0.1043 0.0056 0.4811 0.139 Uiso c ? H(216) -0.0347 0.0801 0.4394 0.106 Uiso c ? H(223) 0.1750 0.1258 0.5945 0.119 Uiso c ? H(224) 0.2497 0.0819 0.5435 0.147 Uiso c ? H(225) 0.2397 0.0835 0.4570 0.167 Uiso c ? H(226) 0.1501 0.1460 0.4213 0.111 Uiso c ? H(313) 0.0474 0.1930 0.6498 0.151 Uiso c ? H(314) 0.0855 0.2771 0.7116 0.183 Uiso c ? H(315) 0.0612 0.4052 0.7057 0.123 Uiso c ? H(316) 0.0107 0.4480 0.6318 0.097 Uiso c ? H(323) -0.1781 0.2117 0.4675 0.134 Uiso c ? H(324) -0.2386 0.1963 0.5340 0.135 Uiso c ? H(325) -0.2183 0.2526 0.6052 0.164 Uiso c ? H(326) -0.1294 0.3321 0.6164 0.134 Uiso c ? H(413) 0.2907 0.4439 0.5715 0.089 Uiso c ? H(414) 0.2729 0.3550 0.6321 0.088 Uiso c ? H(415) 0.1867 0.2786 0.6268 0.098 Uiso c ? H(416) 0.1213 0.3021 0.5593 0.080 Uiso c ? H(423) 0.2522 0.4994 0.3501 0.196 Uiso c ? H(424) 0.2606 0.3803 0.3232 0.211 Uiso c ? H(425) 0.1901 0.3020 0.3319 0.240 Uiso c ? H(426) 0.1472 0.3021 0.4099 0.102 Uiso c ? 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 Au(1) 0.0531(6) 0.0471(5) 0.0642(6) -0.0023(5) -0.0042(6) -0.0042(6) P(1) 0.065(5) 0.054(4) 0.069(4) 0.001(3) -0.005(3) -0.007(3) P(2) 0.066(5) 0.045(3) 0.086(5) 0.006(3) -0.012(4) -0.008(4) P(3) 0.050(4) 0.044(3) 0.063(4) -0.006(3) -0.005(3) 0.003(3) P(4) 0.045(4) 0.048(3) 0.060(4) 0.003(3) -0.001(3) -0.002(3) N(112) 0.07(2) 0.09(2) 0.07(2) 0.00(1) -0.01(1) 0.00(1) N(122) 0.13(3) 0.15(3) 0.10(2) 0.01(2) 0.08(2) 0.05(2) N(212) 0.10(2) 0.07(1) 0.09(2) -0.01(2) -0.03(2) 0.01(2) N(222) 0.09(2) 0.09(2) 0.07(2) 0.01(1) -0.02(1) 0.00(1) N(312) 0.12(2) 0.07(2) 0.11(2) 0.01(1) -0.04(2) 0.05(2) N(322) 0.07(2) 0.07(2) 0.13(2) -0.02(1) -0.02(1) -0.02(1) N(412) 0.05(1) 0.06(1) 0.11(2) 0.01(1) -0.02(1) 0.00(1) N(422) 0.05(2) 0.17(3) 0.10(2) -0.02(2) 0.02(1) 0.02(2) C(1) 0.11(2) 0.09(2) 0.09(2) -0.01(2) -0.04(2) -0.02(2) C(2) 0.09(2) 0.06(2) 0.09(2) 0.00(1) -0.03(2) -0.02(1) C(3) 0.04(1) 0.04(1) 0.06(1) 0.00(1) -0.01(1) 0.00(1) C(4) 0.04(1) 0.04(1) 0.08(2) 0.00(1) 0.01(1) 0.00(1) C(111) 0.08(2) 0.06(2) 0.05(2) -0.01(1) -0.02(1) 0.01(1) C(113) 0.07(2) 0.10(2) 0.09(2) 0.01(2) -0.01(2) -0.02(2) C(114) 0.09(3) 0.12(3) 0.08(2) 0.05(2) 0.00(2) -0.01(2) C(115) 0.05(2) 0.15(3) 0.08(2) -0.01(2) -0.02(2) 0.00(2) C(116) 0.07(2) 0.08(2) 0.05(2) 0.00(2) -0.01(1) -0.01(1) C(121) 0.08(2) 0.05(2) 0.09(2) -0.02(1) -0.04(2) 0.01(1) C(123) 0.17(6) 0.35(9) 0.29(8) 0.16(6) -0.09(5) -0.26(7) C(124) 0.12(4) 0.18(4) 0.31(7) -0.06(4) -0.07(4) 0.18(5) C(125) 0.08(3) 0.35(6) 0.03(2) 0.07(4) 0.02(2) -0.05(3) C(126) 0.09(2) 0.08(2) 0.08(2) 0.02(2) -0.02(2) -0.04(2) C(211) 0.07(2) 0.04(2) 0.11(2) -0.01(1) -0.02(2) 0.00(2) C(213) 0.13(3) 0.07(2) 0.14(3) -0.04(2) 0.01(2) 0.02(2) C(214) 0.11(3) 0.08(3) 0.19(4) -0.03(2) -0.02(3) 0.04(3) C(215) 0.10(3) 0.09(3) 0.16(3) -0.01(2) -0.01(3) -0.03(3) C(216) 0.07(2) 0.06(2) 0.13(3) 0.01(2) 0.00(2) 0.01(2) C(221) 0.06(2) 0.04(1) 0.09(2) 0.02(1) 0.00(1) -0.01(2) C(223) 0.12(3) 0.08(2) 0.10(3) 0.00(2) -0.04(2) 0.02(2) C(224) 0.09(3) 0.09(2) 0.18(4) 0.02(2) -0.02(3) -0.01(3) C(225) 0.08(3) 0.18(4) 0.16(4) 0.00(3) 0.04(3) -0.02(4) C(226) 0.08(2) 0.09(2) 0.12(3) 0.02(2) -0.02(2) -0.02(2) C(311) 0.05(1) 0.07(2) 0.07(2) -0.01(1) 0.00(1) 0.04(2) C(313) 0.15(3) 0.05(2) 0.18(4) 0.02(2) -0.01(3) -0.01(2) C(314) 0.23(5) 0.09(3) 0.13(3) 0.09(3) -0.01(3) 0.07(3) C(315) 0.06(2) 0.15(3) 0.09(2) -0.02(2) -0.02(2) -0.04(2) C(316) 0.10(2) 0.07(2) 0.07(2) 0.00(2) -0.02(2) 0.01(2) C(321) 0.06(2) 0.06(2) 0.09(2) -0.01(1) 0.00(2) 0.01(1) C(323) 0.10(3) 0.09(2) 0.15(3) -0.02(2) -0.04(2) -0.04(2) C(324) 0.10(3) 0.09(3) 0.14(4) -0.03(2) 0.00(3) -0.02(3) C(325) 0.11(3) 0.16(4) 0.14(4) -0.05(3) 0.07(3) 0.03(3) C(326) 0.10(3) 0.15(3) 0.08(2) -0.04(2) 0.01(2) 0.01(2) C(411) 0.06(2) 0.04(1) 0.06(2) 0.01(1) 0.01(1) -0.01(1) C(413) 0.06(2) 0.07(2) 0.09(2) 0.01(1) -0.02(2) 0.01(2) C(414) 0.05(2) 0.10(2) 0.07(2) 0.03(2) -0.03(1) -0.01(2) C(415) 0.05(2) 0.12(3) 0.08(2) 0.01(2) -0.02(2) 0.00(2) C(416) 0.04(2) 0.08(2) 0.08(2) 0.00(1) 0.00(1) 0.02(2) C(421) 0.04(2) 0.07(2) 0.07(2) 0.01(1) 0.02(1) 0.00(2) C(423) 0.10(3) 0.24(6) 0.14(4) -0.05(4) 0.02(3) 0.11(4) C(424) 0.10(4) 0.31(9) 0.10(3) 0.12(5) -0.02(3) -0.11(5) C(425) 0.25(7) 0.16(4) 0.20(5) -0.05(4) -0.18(5) 0.07(5) C(426) 0.12(3) 0.09(2) 0.04(2) 0.04(2) -0.01(2) 0.02(2) #-------------------------------------------------------------------- _refine_special_details ; The crystal used for the data collection was of marginal quality but the best available. Anisotropic thermal parameters were refined for all non-hydrogen atoms. The results also show evidence for disorder in the peripheral carbon atoms of the pyridyl rings. Hydrogen atoms were included on the d2pype ligands, constrained at estimated values. The pyridyl nitrogen atoms were assigned on the basis of slightly shorter C-N bonds. However, the marginal quality of the structure determination makes this assignment tentative only. 10 solvent/anion sites identified, one of which is located on a two fold axis. The electron densities of all these sites were similar and none could be definitely assigned as chloride ions. All such sites were modelled as water which, after allowing for the two chloride counterions, leads to an estimate of 14 water molecules per dimer. Hydrogen atoms were not located on the solvent water molecules. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3411 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0860 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 3.040 _refine_ls_shift/su_max 0.7110 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.91 _refine_diff_density_max 1.26 #-------------------------------------------------------------------- _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 AU1 P1 2.416(6) . . yes AU1 P2 2.444(5) . . yes AU1 P3 2.378(6) . . yes AU1 P4 2.366(5) . . yes P1 C1 1.78(2) . . yes P1 C111 1.82(2) . . yes P1 C121 1.81(3) . . yes P2 C2 1.79(3) . . yes P2 C211 1.86(2) . . yes P2 C221 1.83(2) . . yes P3 C3 1.80(2) . . yes P3 C311 1.81(3) . . yes P3 C321 1.85(2) . . yes P4 C4 1.82(2) . . yes P4 C411 1.85(2) . . yes P4 C421 1.81(2) . . yes N112 C111 1.34(3) . . yes N112 C113 1.41(3) . . yes N122 C121 1.32(4) . . yes N122 C123 1.04(7) . . yes N212 C211 1.37(4) . . yes N212 C213 1.36(4) . . yes N222 C221 1.28(4) . . yes N222 C223 1.34(5) . . yes N312 C311 1.33(4) . . yes N312 C313 1.29(5) . . yes N322 C321 1.34(3) . . yes N322 C323 1.34(5) . . yes N412 C411 1.34(3) . . yes N412 C413 1.28(3) . . yes N422 C421 1.34(5) . . yes N422 C423 1.47(6) . . yes C1 C2 1.62(3) . . yes C1 H11 0.97 . . no C1 H12 0.97 . . no C2 H21 0.98 . . no C2 H22 0.96 . . no C3 C4 1.58(3) . 5_566 yes C3 H31 1.00 . . no C3 H32 0.99 . . no C4 H41 1.01 . . no C4 H42 0.98 . . no C111 C116 1.38(3) . . yes C113 C114 1.33(4) . . yes C113 H113 0.96 . . no C114 C115 1.41(5) . . yes C114 H114 0.96 . . no C115 C116 1.35(3) . . yes C115 H115 0.98 . . no C116 H116 0.98 . . no C121 C126 1.41(3) . . yes C123 C124 1.12(9) . . yes C123 H123 1.11 . . no C124 C125 1.45(8) . . yes C124 H124 1.07 . . no C125 C126 1.48(4) . . yes C125 H125 1.00 . . no C126 H126 0.99 . . no C211 C216 1.34(4) . . yes C213 C214 1.42(6) . . yes C213 H213 0.97 . . no C214 C215 1.35(7) . . yes C214 H214 0.97 . . no C215 C216 1.37(5) . . yes C215 H215 0.98 . . no C216 H216 0.97 . . no C221 C226 1.39(3) . . yes C223 C224 1.37(6) . . yes C223 H223 0.98 . . no C224 C225 1.31(8) . . yes C224 H224 0.97 . . no C225 C226 1.48(5) . . yes C225 H225 0.98 . . no C226 H226 0.97 . . no C311 C316 1.42(4) . . yes C313 C314 1.44(6) . . yes C313 H313 0.97 . . no C314 C315 1.38(5) . . yes C314 H314 0.96 . . no C315 C316 1.41(4) . . yes C315 H315 0.97 . . no C316 H316 0.98 . . no C321 C326 1.38(4) . . yes C323 C324 1.30(6) . . yes C323 H323 0.98 . . no C324 C325 1.24(7) . . yes C324 H324 0.97 . . no C325 C326 1.46(5) . . yes C325 H325 0.98 . . no C326 H326 0.97 . . no C411 C416 1.37(3) . . yes C413 C414 1.37(4) . . yes C413 H413 0.97 . . no C414 C415 1.38(4) . . yes C414 H414 0.97 . . no C415 C416 1.37(3) . . yes C415 H415 0.98 . . no C416 H416 0.97 . . no C421 C426 1.36(5) . . yes C423 C424 1.32(9) . . yes C423 H423 0.98 . . no C424 C425 1.18(9) . . yes C424 H424 0.97 . . no C425 C426 1.26(6) . . yes C425 H425 0.98 . . no C426 H426 0.97 . . 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 P1 AU1 P2 84.5(2) . . . yes P1 AU1 P3 116.5(2) . . . yes P1 AU1 P4 116.1(2) . . . yes P2 AU1 P3 110.0(2) . . . yes P2 AU1 P4 116.0(2) . . . yes P3 AU1 P4 111.3(2) . . . yes AU1 P1 C1 104.2(9) . . . yes AU1 P1 C111 123.1(7) . . . yes AU1 P1 C121 117.8(8) . . . yes C1 P1 C111 104(1) . . . yes C1 P1 C121 106(1) . . . yes C111 P1 C121 100(1) . . . yes AU1 P2 C2 103.6(7) . . . yes AU1 P2 C211 119.3(7) . . . yes AU1 P2 C221 121.9(7) . . . yes C2 P2 C211 104(1) . . . yes C2 P2 C221 108(1) . . . yes C211 P2 C221 98(1) . . . yes AU1 P3 C3 121.4(7) . . . yes AU1 P3 C311 110.5(8) . . . yes AU1 P3 C321 113.3(8) . . . yes C3 P3 C311 102(1) . . . yes C3 P3 C321 104.8(9) . . . yes C311 P3 C321 103(1) . . . yes AU1 P4 C4 111.5(7) . . . yes AU1 P4 C411 116.3(7) . . . yes AU1 P4 C421 117.2(9) . . . yes C4 P4 C411 102.9(9) . . . yes C4 P4 C421 104(1) . . . yes C411 P4 C421 103(1) . . . yes C111 N112 C113 116(2) . . . yes C121 N122 C123 116(5) . . . yes C211 N212 C213 121(2) . . . yes C221 N222 C223 118(2) . . . yes C311 N312 C313 120(3) . . . yes C321 N322 C323 114(2) . . . yes C411 N412 C413 116(2) . . . yes C421 N422 C423 110(3) . . . yes P1 C1 C2 111(1) . . . yes P1 C1 H11 109.8 . . . no P1 C1 H12 109.5 . . . no C2 C1 H11 108.6 . . . no C2 C1 H12 108.6 . . . no H11 C1 H12 109.8 . . . no P2 C2 C1 107(2) . . . yes P2 C2 H21 109.1 . . . no P2 C2 H22 110.0 . . . no C1 C2 H21 110.2 . . . no C1 C2 H22 111.3 . . . no H21 C2 H22 109.2 . . . no P3 C3 C4 111(1) . . 5_566 yes P3 C3 H31 109.4 . . . no P3 C3 H32 109.9 . . . no C4 C3 H31 109.1 5_566 . . no C4 C3 H32 110.8 5_566 . . no H31 C3 H32 105.9 . . . no P4 C4 C3 110(1) . . 5_566 yes P4 C4 H41 109.9 . . . no P4 C4 H42 111.7 . . . no C3 C4 H41 108.8 5_566 . . no C3 C4 H42 111.4 5_566 . . no H41 C4 H42 105.0 . . . no P1 C111 N112 112(2) . . . yes P1 C111 C116 123(1) . . . yes N112 C111 C116 125(2) . . . yes N112 C113 C114 121(3) . . . yes N112 C113 H113 118.7 . . . no C114 C113 H113 120.5 . . . no C113 C114 C115 121(3) . . . yes C113 C114 H114 118.9 . . . no C115 C114 H114 120.6 . . . no C114 C115 C116 120(2) . . . yes C114 C115 H115 119.4 . . . no C116 C115 H115 120.9 . . . no C111 C116 C115 117(2) . . . yes C111 C116 H116 120.9 . . . no C115 C116 H116 121.9 . . . no P1 C121 N122 110(2) . . . yes P1 C121 C126 128(2) . . . yes N122 C121 C126 122(2) . . . yes N122 C123 C124 140(8) . . . yes N122 C123 H123 121.9 . . . no C124 C123 H123 98.5 . . . no C123 C124 C125 119(6) . . . yes C123 C124 H124 143.3 . . . no C125 C124 H124 97.7 . . . no C124 C125 C126 110(3) . . . yes C124 C125 H125 140.0 . . . no C126 C125 H125 110.0 . . . no C121 C126 C125 113(2) . . . yes C121 C126 H126 118.1 . . . no C125 C126 H126 128.9 . . . no P2 C211 N212 115(2) . . . yes P2 C211 C216 124(2) . . . yes N212 C211 C216 121(2) . . . yes N212 C213 C214 115(3) . . . yes N212 C213 H213 122.5 . . . no C214 C213 H213 122.1 . . . no C213 C214 C215 123(4) . . . yes C213 C214 H214 119.5 . . . no C215 C214 H214 117.2 . . . no C214 C215 C216 118(4) . . . yes C214 C215 H215 121.9 . . . no C216 C215 H215 120.3 . . . no C211 C216 C215 121(3) . . . yes C211 C216 H216 119.7 . . . no C215 C216 H216 119.4 . . . no P2 C221 N222 115(2) . . . yes P2 C221 C226 119(2) . . . yes N222 C221 C226 125(2) . . . yes N222 C223 C224 123(3) . . . yes N222 C223 H223 118.7 . . . no C224 C223 H223 117.9 . . . no C223 C224 C225 121(4) . . . yes C223 C224 H224 119.2 . . . no C225 C224 H224 120.2 . . . no C224 C225 C226 118(4) . . . yes C224 C225 H225 121.6 . . . no C226 C225 H225 120.0 . . . no C221 C226 C225 114(3) . . . yes C221 C226 H226 122.6 . . . no C225 C226 H226 122.9 . . . no P3 C311 N312 115(2) . . . yes P3 C311 C316 122(2) . . . yes N312 C311 C316 122(2) . . . yes N312 C313 C314 123(3) . . . yes N312 C313 H313 119.7 . . . no C314 C313 H313 117.0 . . . no C313 C314 C315 118(3) . . . yes C313 C314 H314 122.1 . . . no C315 C314 H314 120.1 . . . no C314 C315 C316 119(3) . . . yes C314 C315 H315 121.3 . . . no C316 C315 H315 120.1 . . . no C311 C316 C315 118(2) . . . yes C311 C316 H316 120.9 . . . no C315 C316 H316 120.9 . . . no P3 C321 N322 116(2) . . . yes P3 C321 C326 119(2) . . . yes N322 C321 C326 125(2) . . . yes N322 C323 C324 127(3) . . . yes N322 C323 H323 115.6 . . . no C324 C323 H323 117.4 . . . no C323 C324 C325 117(4) . . . yes C323 C324 H324 120.6 . . . no C325 C324 H324 122.1 . . . no C324 C325 C326 126(4) . . . yes C324 C325 H325 116.4 . . . no C326 C325 H325 118.1 . . . no C321 C326 C325 111(3) . . . yes C321 C326 H326 124.3 . . . no C325 C326 H326 124.8 . . . no P4 C411 N412 116(2) . . . yes P4 C411 C416 120(2) . . . yes N412 C411 C416 124(2) . . . yes N412 C413 C414 125(2) . . . yes N412 C413 H413 119.0 . . . no C414 C413 H413 116.3 . . . no C413 C414 C415 120(2) . . . yes C413 C414 H414 121.0 . . . no C415 C414 H414 119.5 . . . no C414 C415 C416 116(3) . . . yes C414 C415 H415 122.8 . . . no C416 C415 H415 120.8 . . . no C411 C416 C415 119(2) . . . yes C411 C416 H416 120.3 . . . no C415 C416 H416 120.4 . . . no P4 C421 N422 119(2) . . . yes P4 C421 C426 117(2) . . . yes N422 C421 C426 124(2) . . . yes N422 C423 C424 117(5) . . . yes N422 C423 H423 121.2 . . . no C424 C423 H423 121.9 . . . no C423 C424 C425 128(5) . . . yes C423 C424 H424 114.8 . . . no C425 C424 H424 117.7 . . . no C424 C425 C426 118(5) . . . yes C424 C425 H425 119.3 . . . no C426 C425 H425 122.7 . . . no C421 C426 C425 121(4) . . . yes C421 C426 H426 119.0 . . . no C425 C426 H426 120.1 . . . no #-------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 O7 2.35(6) . 8_554 no O1 O10 2.65(5) . 8_554 no O1 C413 3.56(5) . 2_554 no O2 O3 2.77(7) . 3_556 no O2 O6 2.82(5) . 2_554 no O2 O9 3.34(6) . 2_554 no O2 O4 3.40(5) . 3_556 no O3 O9 3.24(6) . 4_556 no O3 C326 3.36(6) . . no O4 O5 2.81(5) . . no O4 O10 3.32(4) . 6_456 no O4 C425 3.46(6) . 3_456 no O4 C226 3.51(4) . 3_456 no O5 O7 3.22(6) . 7_455 no O6 O9 3.14(5) . . no O6 C115 3.56(5) . 3_556 no O7 C213 3.24(6) . . no O7 O8 3.27(6) . . no O8 O9 3.09(5) . . no O8 O9 3.09(5) . 4_556 no O9 C213 3.58(4) . 4_556 no N412 C224 3.43(4) . 7 no C126 C126 3.54(5) . 4 no C224 C413 3.58(4) . 7_545 no #================================================================END