# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1296 data_(I) # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source # # symbol number description f' f'' source # 'Au' 2 'Gold ' -2.0133 8.8022 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'O ' 18 'Oxygen ' 0.0106 0.0060 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'N ' 6 'Nitrogen ' 0.0061 0.0033 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 30 'Carbon ' 0.0033 0.0016 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'Cl' 4 'Chlorine ' 0.1484 0.1585 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 24 'Hydrogen ' 0.0000 0.0000 'Int. Tab. C, 4.2.6.8, 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_group # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ calc sof dis Au1 0.15940(2) 0.15079(1) 0.27858(2) 0.0423(1) Uani Au . . . O1 0.0672(5) 0.0122(3) 0.2815(5) 0.0604(13) Uani O . . . N1 0.2440(5) 0.1093(4) 0.0820(6) 0.0498(13) Uani N . . . N2 0.2383(5) 0.2898(3) 0.2736(5) 0.0452(12) Uani N . . . N3 0.1033(5) 0.2344(4) 0.4762(5) 0.0472(13) Uani N . . . C1 0.2372(7) 0.0106(5) -0.0097(7) 0.0605(19) Uani C . . . C2 0.3017(8) -0.0084(6) -0.1401(8) 0.0687(22) Uani C . . . C3 0.3731(8) 0.0720(7) -0.1758(8) 0.0684(21) Uani C . . . C4 0.3793(7) 0.1728(6) -0.0819(7) 0.0619(22) Uani C . . . C5 0.3130(6) 0.1915(5) 0.0476(7) 0.0507(18) Uani C . . . C6 0.3100(6) 0.2947(4) 0.1551(6) 0.0484(15) Uani C . . . C7 0.3659(7) 0.3919(5) 0.1519(8) 0.0624(19) Uani C . . . C8 0.3501(8) 0.4789(5) 0.2709(8) 0.0658(21) Uani C . . . C9 0.2801(7) 0.4686(5) 0.3936(8) 0.0585(18) Uani C . . . C10 0.2221(6) 0.3716(4) 0.3911(6) 0.0475(15) Uani C . . . C11 0.1461(6) 0.3381(5) 0.5081(7) 0.0490(16) Uani C . . . C12 0.1196(7) 0.4039(5) 0.6422(8) 0.0603(19) Uani C . . . C13 0.0478(8) 0.3633(6) 0.7425(8) 0.0674(22) Uani C . . . C14 0.0054(7) 0.2597(6) 0.7074(8) 0.0690(21) Uani C . . . C15 0.0350(6) 0.1950(5) 0.5747(7) 0.0569(17) Uani C . . . Cl1 -0.1864(2) 0.3259(1) 0.0877(2) 0.0557(4) Uani Cl . . . Cl2 0.5761(2) 0.1942(1) 0.5424(2) 0.0588(5) Uani Cl . . . O2 -0.1712(9) 0.3338(6) 0.2509(7) 0.1200(29) Uani O . . . O3 -0.0828(8) 0.3954(7) 0.0651(9) 0.1492(30) Uani O . . . O4 -0.1192(12) 0.2227(6) 0.0322(10) 0.1520(42) Uani O . . . O5 -0.3223(9) 0.3577(11) 0.0086(11) 0.1949(54) Uani O . . . O6 0.4682(8) 0.2624(7) 0.6185(8) 0.1250(31) Uani O . . . O7 0.6691(9) 0.1323(7) 0.6540(11) 0.1493(36) Uani O . . . O8 0.5002(9) 0.1322(6) 0.4099(10) 0.1597(35) Uani O . . . O9 0.6576(10) 0.2662(8) 0.4991(12) 0.1876(39) Uani O . . . H1 0.1893(68) -0.0492(55) 0.0226(71) 0.052(15) Uiso H . . . H2 0.3140(78) -0.0765(59) -0.1910(78) 0.062(17) Uiso H . . . H3 0.4119(67) 0.0650(51) -0.2414(67) 0.048(14) Uiso H . . . H4 0.416(11) 0.2404(82) -0.092(11) 0.093(26) Uiso H . . . H7 0.4249(62) 0.4010(48) 0.0718(62) 0.040(12) Uiso H . . . H8 0.3909(53) 0.5433(40) 0.2638(53) 0.0261(96) Uiso H . . . H9 0.2683(64) 0.5315(49) 0.4724(65) 0.042(13) Uiso H . . . H12 0.1452(73) 0.4670(56) 0.6328(73) 0.056(16) Uiso H . . . H13 0.0176(80) 0.4056(62) 0.8551(82) 0.066(18) Uiso H . . . H14 -0.0349(90) 0.2339(69) 0.7695(92) 0.082(22) Uiso H . . . H15 -0.0087(85) 0.1433(66) 0.5312(86) 0.072(20) Uiso H . . . H01 0.13126(0) -0.00231(0) 0.35237(0) 0.0520(0) Uiso H 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 #label U11 U22 U33 U23 U13 U12 Au1 0.0296(1) 0.0277(1) 0.0439(1) 0.0026(0) 0.0099(0) -0.0051(0) O1 0.0495(15) 0.0252(12) 0.0742(19) 0.0091(11) 0.0221(13) -0.0059(13) N1 0.0363(15) 0.0332(16) 0.0493(19) 0.0014(13) 0.0128(13) -0.0045(15) N2 0.0355(14) 0.0288(14) 0.0436(17) 0.0043(12) 0.0093(13) -0.0045(13) N3 0.0341(14) 0.0340(16) 0.0430(17) 0.0005(13) 0.0085(13) -0.0054(14) C1 0.0454(22) 0.0428(23) 0.0522(26) -0.0078(19) 0.0111(19) -0.0091(21) C2 0.0548(27) 0.0486(28) 0.0565(29) -0.0057(23) 0.0142(22) -0.0054(24) C3 0.0530(24) 0.0629(32) 0.0506(24) 0.0080(24) 0.0221(18) -0.0010(23) C4 0.0489(23) 0.0531(27) 0.0482(23) 0.0116(21) 0.0139(18) -0.0051(20) C5 0.0363(18) 0.0375(20) 0.0469(22) 0.0072(16) 0.0098(16) -0.0014(17) C6 0.0378(18) 0.0349(19) 0.0432(20) 0.0088(16) 0.0092(15) -0.0023(16) C7 0.0522(22) 0.0443(22) 0.0586(24) 0.0160(18) 0.0173(18) -0.0107(18) C8 0.0583(26) 0.0350(20) 0.0656(29) 0.0120(18) 0.0103(22) -0.0141(20) C9 0.0489(23) 0.0322(20) 0.0560(26) 0.0063(18) 0.0066(20) -0.0059(19) C10 0.0377(18) 0.0302(18) 0.0429(21) 0.0039(15) 0.0054(16) -0.0033(16) C11 0.0312(17) 0.0377(20) 0.0451(22) 0.0030(16) 0.0058(16) -0.0021(17) C12 0.0487(23) 0.0389(23) 0.0530(26) -0.0001(19) 0.0099(20) -0.0048(20) C13 0.0515(25) 0.0601(32) 0.0472(25) -0.0014(24) 0.0156(19) -0.0031(24) C14 0.0487(23) 0.0647(32) 0.0549(26) 0.0057(22) 0.0196(19) -0.0111(24) C15 0.0453(19) 0.0453(23) 0.0497(22) 0.0051(17) 0.0184(16) -0.0118(18) Cl1 0.0490(5) 0.0393(5) 0.0426(5) 0.0043(4) 0.0068(4) -0.0064(4) Cl2 0.0394(5) 0.0426(5) 0.0564(6) 0.0073(4) 0.0069(4) -0.0052(5) O2 0.1445(49) 0.0914(37) 0.0542(22) 0.0137(35) 0.0280(25) -0.0149(23) O3 0.1391(33) 0.1298(41) 0.1085(36) -0.0165(26) 0.0637(24) -0.0774(32) O4 0.1930(75) 0.0479(28) 0.1053(44) -0.0081(38) 0.0287(46) 0.0141(30) O5 0.0630(32) 0.2580(96) 0.1343(56) 0.0657(46) 0.0115(37) 0.0440(58) O6 0.0816(30) 0.1330(50) 0.0758(30) 0.0179(32) 0.0261(23) 0.0349(32) O7 0.0773(34) 0.0956(40) 0.1598(56) 0.0447(31) -0.0266(35) 0.0148(36) O8 0.0949(40) 0.0831(37) 0.1458(52) -0.0476(32) -0.0349(37) 0.0114(35) O9 0.1483(45) 0.1355(46) 0.1992(55) 0.0572(32) 0.0724(34) -0.0513(35) # MOLECULAR GEOMETRY 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 O1 2.000(4) . . yes Au1 N1 2.009(5) . . yes Au1 N2 1.949(5) . . yes Au1 N3 2.008(5) . . yes Au1 H01 2.1557(6) . . no O1 H01 0.776(4) . . no N1 C1 1.351(7) . . yes N1 C5 1.359(8) . . yes N2 C6 1.354(8) . . yes N2 C10 1.345(7) . . yes N3 C11 1.352(7) . . yes N3 C15 1.347(9) . . yes C1 C2 1.37(1) . . yes C1 H1 1.01(7) . . no C2 C3 1.36(1) . . yes C2 H2 0.90(6) . . no C3 C4 1.38(1) . . yes C3 H3 0.73(6) . . no C4 C5 1.375(9) . . yes C4 H4 0.96(*) . . no C5 C6 1.464(7) . . yes C6 C7 1.365(9) . . yes C7 C8 1.394(9) . . yes C7 H7 1.00(6) . . no C8 C9 1.39(1) . . yes C8 H8 0.93(5) . . no C9 C10 1.362(9) . . yes C9 H9 0.97(5) . . no C10 C11 1.488(9) . . yes C11 C12 1.372(8) . . yes C12 C13 1.39(1) . . yes C12 H12 0.86(7) . . no C13 C14 1.35(1) . . yes C13 H13 1.12(7) . . no C14 C15 1.364(9) . . yes C14 H14 0.84(9) . . no C15 H15 0.79(7) . . no Cl1 O2 1.399(6) . . yes Cl1 O3 1.407(9) . . yes Cl1 O4 1.405(8) . . yes Cl1 O5 1.313(8) . . yes Cl2 O6 1.418(7) . . yes Cl2 O7 1.402(9) . . yes Cl2 O8 1.379(8) . . yes Cl2 O9 1.37(1) . . yes 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 O1 Au1 N1 100.0(2) . . . yes O1 Au1 N2 176.9(2) . . . yes O1 Au1 N3 97.4(2) . . . yes O1 Au1 H01 21.1(1) . . . no N1 Au1 N2 81.2(2) . . . yes N1 Au1 N3 162.6(2) . . . yes N1 Au1 H01 105.8(1) . . . no N2 Au1 N3 81.5(2) . . . yes N2 Au1 H01 161.1(1) . . . no N3 Au1 H01 90.4(1) . . . no Au1 O1 H01 90.8(3) . . . no Au1 N1 C1 125.4(4) . . . yes Au1 N1 C5 113.2(4) . . . yes C1 N1 C5 121.4(5) . . . yes Au1 N2 C6 117.2(3) . . . yes Au1 N2 C10 117.4(3) . . . yes C6 N2 C10 125.4(5) . . . yes Au1 N3 C11 113.2(4) . . . yes Au1 N3 C15 126.0(4) . . . yes C11 N3 C15 120.7(5) . . . yes N1 C1 C2 119.9(6) . . . yes N1 C1 H1 119(4) . . . no C2 C1 H1 121(4) . . . no C1 C2 C3 119.8(6) . . . yes C1 C2 H2 121(4) . . . no C3 C2 H2 118(5) . . . no C2 C3 C4 120.0(7) . . . yes C2 C3 H3 124(5) . . . no C4 C3 H3 116(5) . . . no C3 C4 C5 119.8(6) . . . yes C3 C4 H4 132(6) . . . no C5 C4 H4 108(6) . . . no N1 C5 C4 119.1(5) . . . yes N1 C5 C6 115.8(5) . . . yes C4 C5 C6 125.1(5) . . . yes N2 C6 C5 112.7(5) . . . yes N2 C6 C7 117.3(5) . . . yes C5 C6 C7 130.1(5) . . . yes C6 C7 C8 119.0(6) . . . yes C6 C7 H7 122(3) . . . no C8 C7 H7 119(3) . . . no C7 C8 C9 121.6(6) . . . yes C7 C8 H8 116(3) . . . no C9 C8 H8 123(3) . . . no C8 C9 C10 117.8(6) . . . yes C8 C9 H9 119(3) . . . no C10 C9 H9 123(4) . . . no N2 C10 C9 118.8(5) . . . yes N2 C10 C11 112.3(5) . . . yes C9 C10 C11 128.8(5) . . . yes N3 C11 C10 115.6(5) . . . yes N3 C11 C12 119.7(5) . . . yes C10 C11 C12 124.7(5) . . . yes C11 C12 C13 119.3(6) . . . yes C11 C12 H12 104(4) . . . no C13 C12 H12 136(5) . . . no C12 C13 C14 119.7(7) . . . yes C12 C13 H13 128(4) . . . no C14 C13 H13 112(4) . . . no C13 C14 C15 120.0(7) . . . yes C13 C14 H14 120(6) . . . no C15 C14 H14 120(5) . . . no N3 C15 C14 120.4(6) . . . yes N3 C15 H15 111(6) . . . no C14 C15 H15 125(6) . . . no O2 Cl1 O3 105.7(4) . . . yes O2 Cl1 O4 108.9(4) . . . yes O2 Cl1 O5 115.8(5) . . . yes O3 Cl1 O4 100.5(5) . . . yes O3 Cl1 O5 107.4(5) . . . yes O4 Cl1 O5 116.7(6) . . . yes O6 Cl2 O7 107.1(5) . . . yes O6 Cl2 O8 109.5(5) . . . yes O6 Cl2 O9 104.5(5) . . . yes O7 Cl2 O8 114.4(5) . . . yes O7 Cl2 O9 111.1(6) . . . yes O8 Cl2 O9 109.7(5) . . . yes Au1 H01 O1 68.1(3) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Au1 O1 H01 108.1(3) . . . . no N2 Au1 O1 H01 -138(3) . . . . no N3 Au1 O1 H01 -71.7(3) . . . . no O1 Au1 N1 C1 -1.9(5) . . . . no O1 Au1 N1 C5 178.7(4) . . . . no N2 Au1 N1 C1 -179.0(5) . . . . no N2 Au1 N1 C5 1.6(4) . . . . no N3 Au1 N1 C1 177.1(6) . . . . no N3 Au1 N1 C5 -2.2(9) . . . . no H01 Au1 N1 C1 19.0(5) . . . . no H01 Au1 N1 C5 -160.4(3) . . . . no O1 Au1 N2 C6 -114(3) . . . . no O1 Au1 N2 C10 68(3) . . . . no N1 Au1 N2 C6 -1.4(4) . . . . no N1 Au1 N2 C10 -179.0(4) . . . . no N3 Au1 N2 C6 177.4(4) . . . . no N3 Au1 N2 C10 -0.1(4) . . . . no H01 Au1 N2 C6 112.0(4) . . . . no H01 Au1 N2 C10 -65.6(6) . . . . no O1 Au1 N3 C11 -177.9(4) . . . . no O1 Au1 N3 C15 4.3(5) . . . . no N1 Au1 N3 C11 3.1(8) . . . . no N1 Au1 N3 C15 -174.7(6) . . . . no N2 Au1 N3 C11 -0.7(4) . . . . no N2 Au1 N3 C15 -178.5(5) . . . . no H01 Au1 N3 C11 162.1(4) . . . . no H01 Au1 N3 C15 -15.7(5) . . . . no N1 Au1 H01 O1 -76.7(4) . . . . no N2 Au1 H01 O1 173.8(5) . . . . no N3 Au1 H01 O1 109.7(4) . . . . no Au1 N1 C1 C2 -178.9(5) . . . . no Au1 N1 C1 H1 -1(4) . . . . no C5 N1 C1 C2 0.4(9) . . . . no C5 N1 C1 H1 177(4) . . . . no Au1 N1 C5 C4 178.4(4) . . . . no Au1 N1 C5 C6 -1.6(6) . . . . no C1 N1 C5 C4 -1.0(8) . . . . no C1 N1 C5 C6 179.0(5) . . . . no Au1 N2 C6 C5 0.9(6) . . . . no Au1 N2 C6 C7 -179.7(4) . . . . no C10 N2 C6 C5 178.3(5) . . . . no C10 N2 C6 C7 -2.3(8) . . . . no Au1 N2 C10 C9 178.0(4) . . . . no Au1 N2 C10 C11 0.9(6) . . . . no C6 N2 C10 C9 0.7(8) . . . . no C6 N2 C10 C11 -176.5(5) . . . . no Au1 N3 C11 C10 1.4(6) . . . . no Au1 N3 C11 C12 -177.9(4) . . . . no C15 N3 C11 C10 179.3(5) . . . . no C15 N3 C11 C12 0.0(8) . . . . no Au1 N3 C15 C14 178.7(5) . . . . no Au1 N3 C15 H15 -20(6) . . . . no C11 N3 C15 C14 1.1(9) . . . . no C11 N3 C15 H15 161(6) . . . . no N1 C1 C2 C3 0(1) . . . . no N1 C1 C2 H2 168(5) . . . . no H1 C1 C2 C3 -175(4) . . . . no H1 C1 C2 H2 -8(7) . . . . no C1 C2 C3 C4 0(1) . . . . no C1 C2 C3 H3 177(6) . . . . no H2 C2 C3 C4 -168(5) . . . . no H2 C2 C3 H3 9(8) . . . . no C2 C3 C4 C5 0(1) . . . . no C2 C3 C4 H4 -173(8) . . . . no H3 C3 C4 C5 -177(5) . . . . no H3 C3 C4 H4 8(*) . . . . no C3 C4 C5 N1 0.8(9) . . . . no C3 C4 C5 C6 -179.2(6) . . . . no H4 C4 C5 N1 176(6) . . . . no H4 C4 C5 C6 -3(6) . . . . no N1 C5 C6 N2 0.5(7) . . . . no N1 C5 C6 C7 -178.8(6) . . . . no C4 C5 C6 N2 -179.4(6) . . . . no C4 C5 C6 C7 1(1) . . . . no N2 C6 C7 C8 1.6(9) . . . . no N2 C6 C7 H7 177(4) . . . . no C5 C6 C7 C8 -179.1(6) . . . . no C5 C6 C7 H7 -3(4) . . . . no C6 C7 C8 C9 1(1) . . . . no C6 C7 C8 H8 180(3) . . . . no H7 C7 C8 C9 -174(4) . . . . no H7 C7 C8 H8 4(5) . . . . no C7 C8 C9 C10 -1(1) . . . . no C7 C8 C9 H9 -177(4) . . . . no H8 C8 C9 C10 179(4) . . . . no H8 C8 C9 H9 3(5) . . . . no C8 C9 C10 N2 1.7(9) . . . . no C8 C9 C10 C11 178.3(6) . . . . no H9 C9 C10 N2 177(4) . . . . no H9 C9 C10 C11 -5(4) . . . . no N2 C10 C11 N3 -1.5(7) . . . . no N2 C10 C11 C12 177.8(6) . . . . no C9 C10 C11 N3 -178.3(6) . . . . no C9 C10 C11 C12 1(1) . . . . no N3 C11 C12 C13 -0.7(9) . . . . no N3 C11 C12 H12 -172(5) . . . . no C10 C11 C12 C13 -179.9(6) . . . . no C10 C11 C12 H12 7(5) . . . . no C11 C12 C13 C14 0(1) . . . . no C11 C12 C13 H13 -179(5) . . . . no H12 C12 C13 C14 170(6) . . . . no H12 C12 C13 H13 -9(8) . . . . no C12 C13 C14 C15 1(1) . . . . no C12 C13 C14 H14 178(7) . . . . no H13 C13 C14 C15 -178(4) . . . . no H13 C13 C14 H14 -1(8) . . . . no C13 C14 C15 N3 0(1) . . . . no C13 C14 C15 H15 -157(7) . . . . no H14 C14 C15 N3 -177(7) . . . . no H14 C14 C15 H15 25(*) . . . . no # CHEMICAL DATA _chemical_name_systematic ; ..... ; _chemical_formula_analytical 'Au1 Cl2 H12 C15 N3 O9' _chemical_formula_moiety '(Au1 C15 H12 O1 N3)^++^ 2(Cl1 O4)^-^' _chemical_formula_structural ? _chemical_formula_sum 'Au1 Cl2 H12 C15 N3 O9 ' _chemical_formula_weight 646.15 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 9.006(1) _cell_length_b 12.361(4) _cell_length_c 8.790(2) _cell_angle_alpha 99.13(2) _cell_angle_beta 102.86(2) _cell_angle_gamma 82.93(2) _cell_volume 938.0(4) _cell_formula_units_Z 2.00 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 14 _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M ' P-1 ' _symmetry_Int_Tables_number 2 _exptl_crystal_description ; plated ; _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.2878 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616.0 _exptl_absorpt_coefficient_mu 8.185 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.99 # EXPERIMENTAL DATA _diffrn_special_details ; ....... ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _reflns_number_total 4532 _reflns_number_gt 3882 _reflns_threshold_expression '>3sigma (I)' _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_number 4822 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_reduction_process ; ...... ; # REFINEMENT DATA _refine_special_details ; ...... ; _atom_sites_solution_primary 'Patterson' _atom_sites_solution_secondary 'Fourier' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_structure_factor_coef 'F' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme 'calc w= 4F^2^/(\s^2^(I) + (0.05F^2^)^2^)' _refine_ls_weighting_details ? _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 3882 _refine_ls_number_parameters 315 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.301 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max 0.03 _refine_ls_shift/su_mean ? _refine_diff_density_max 1.470 _refine_diff_density_min -0.520 _refine_diff_density_rms ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance # # This is the complete list of first-neighbour intramolecular distances # less than 4.00 Angstrom. # # lab1 lab2 distance Au1 C1 3.001(6) Au1 C5 2.834(7) Au1 C6 2.836(6) Au1 C10 2.832(5) Au1 C11 2.829(5) Au1 C15 3.004(6) Au1 CL1 3.790(2) Au1 CL2 3.997(2) Au1 O2 3.498(8) Au1 O3 3.972(8) Au1 O4 3.069(8) Au1 O6 3.808(6) Au1 O8 3.023(8) Au1 H1 3.096(61) Au1 H15 2.971(86) O1 N1 3.071(7) O1 N2 3.947(6) O1 N3 3.010(6) O1 C1 3.258(9) O1 C15 3.187(7) O1 O4 3.673(9) O1 H1 2.706(66) O1 H15 2.679(75) N1 N2 2.576(6) N1 N3 3.971(7) N1 C2 2.359(8) N1 C3 2.722(9) N1 C4 2.357(9) N1 C6 2.391(7) N1 C7 3.708(8) N1 C10 3.901(7) N1 O4 3.359(10) N1 O8 3.264(9) N1 H1 2.037(67) N1 H2 3.162(67) N1 H3 3.447(64) N1 H4 3.133(112) N1 H01 3.323(5) N2 N3 2.583(7) N2 C1 3.922(7) N2 C4 3.654(8) N2 C5 2.346(7) N2 C7 2.321(9) N2 C8 2.661(8) N2 C9 2.330(7) N2 C11 2.355(8) N2 C12 3.654(8) N2 C15 3.925(9) N2 CL1 3.811(4) N2 CL2 3.611(4) N2 O2 3.626(9) N2 O3 3.300(8) N2 O4 3.551(10) N2 O6 3.310(8) N2 O8 3.024(9) N2 O9 3.855(9) N2 H4 3.830(101) N2 H7 3.245(65) N2 H8 3.593(53) N2 H9 3.222(56) N2 H12 3.742(63) N3 C6 3.915(8) N3 C9 3.709(9) N3 C10 2.404(8) N3 C12 2.356(7) N3 C13 2.722(8) N3 C14 2.352(9) N3 O2 3.064(8) N3 O4 3.960(9) N3 O6 3.285(8) N3 O8 3.780(9) N3 H12 3.013(65) N3 H13 3.831(71) N3 H14 3.104(90) N3 H15 1.787(89) N3 H01 2.957(4) C1 C3 2.363(11) C1 C4 2.731(10) C1 C5 2.362(9) C1 C6 3.659(8) C1 O4 3.931(11) C1 H2 1.986(69) C1 H3 3.033(69) C1 H4 3.671(111) C1 H01 3.551(7) C2 C4 2.373(10) C2 C5 2.744(9) C2 H1 2.080(73) C2 H3 1.862(71) C2 H4 3.296(105) C3 C5 2.384(9) C3 C6 3.765(9) C3 H1 3.279(74) C3 H2 1.950(76) C3 H4 2.147(99) C4 C6 2.520(8) C4 C7 3.136(9) C4 H1 3.736(74) C4 H2 3.166(72) C4 H3 1.823(57) C4 H7 2.963(56) C5 C7 2.565(8) C5 C8 3.791(8) C5 C10 3.642(8) C5 O4 3.838(12) C5 O8 3.401(10) C5 H1 3.261(70) C5 H2 3.629(67) C5 H3 3.016(59) C5 H4 1.899(110) C5 H7 2.853(62) C6 C8 2.377(8) C6 C9 2.787(8) C6 C10 2.399(8) C6 C11 3.662(9) C6 Cl2 3.981(6) C6 O3 3.560(9) C6 O4 3.947(11) C6 O8 3.295(10) C6 O9 3.863(10) C6 H4 2.524(99) C6 H7 2.076(65) C6 H8 3.193(49) C6 H9 3.753(55) C7 C9 2.434(10) C7 C10 2.761(10) C7 O3 3.938(10) C7 O9 3.945(11) C7 H4 2.691(91) C7 H8 1.986(47) C7 H9 3.297(57) C8 C10 2.360(10) C8 C11 3.794(10) C8 H7 2.067(56) C8 H9 2.049(60) C9 C11 2.570(10) C9 C12 3.122(11) C9 O3 3.942(9) C9 O6 3.510(10) C9 O9 3.990(10) C9 H7 3.320(59) C9 H8 2.054(56) C9 H12 2.656(73) C10 C12 2.533(9) C10 C13 3.783(10) C10 C15 3.666(9) C10 Cl2 3.749(5) C10 O2 3.545(9) C10 O3 3.522(8) C10 O6 2.979(9) C10 O8 3.633(9) C10 O9 3.932(10) C10 H7 3.757(63) C10 H8 3.221(56) C10 H9 2.052(59) C10 H12 2.458(65) C11 C13 2.380(10) C11 C14 2.728(10) C11 C15 2.345(9) C11 O2 3.226(8) C11 O6 2.932(8) C11 O8 3.990(9) C11 H9 2.839(65) C11 H12 1.785(63) C11 H13 3.445(76) C11 H14 3.566(95) C11 H15 2.982(87) C12 C14 2.366(11) C12 C15 2.720(9) C12 O2 3.879(9) C12 O6 3.433(9) C12 H9 2.944(68) C12 H13 2.257(80) C12 H14 3.125(95) C12 H15 3.477(81) C13 C15 2.351(9) C13 H12 2.095(77) C13 H14 1.914(93) C13 H15 3.070(74) C14 H12 3.205(75) C14 H13 2.048(70) C14 H15 1.933(72) C15 O2 3.592(9) C15 H12 3.550(70) C15 H13 3.304(69) C15 H14 1.924(85) C15 H01 3.040(6) O2 O3 2.237(12) O2 O4 2.282(10) O2 O5 2.299(11) O2 H15 3.626(79) O3 O4 2.163(12) O3 O5 2.193(12) O4 O5 2.316(13) O6 O7 2.269(10) O6 O8 2.284(11) O6 O9 2.201(13) O6 H9 3.848(59) O6 H12 3.623(63) O7 O8 2.338(12) O7 O9 2.283(15) O8 O9 2.244(12) O8 H01 3.796(9) H1 H2 2.355(101) H1 H3 3.899(101) H1 H01 3.013(65) H2 H3 2.198(105) H3 H4 2.351(110) H4 H7 2.257(106) H7 H8 2.278(70) H8 H9 2.372(84) H9 H12 2.264(101) H12 H13 2.720(112) H12 H14 3.936(121) H13 H14 2.209(112) H13 H15 3.955(100) H14 H15 2.260(108) H15 H01 2.593(76) loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag #D H A D-H H..A D..A D-H..A A site sym Flg O1 H01 O7 0.777(4) 2.263(7) 2.798(8) 126.8(4) 2_656 ? # -x,-y,-z # x,+y,+z+1 # -x+1,-y,-z+1 # -x+1,-y,-z+1