# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1435 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 # 'Tc' 8 'Technetium ' -1.4390 0.7593 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'O ' 8 'Oxygen ' 0.0106 0.0060 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'N ' 88 'Nitrogen ' 0.0061 0.0033 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 64 'Carbon ' 0.0033 0.0016 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'Cl' 16 'Chlorine ' 0.1484 0.1585 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 192 '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 Tc 0.35031(1) 0.08082(2) -0.00437(1) 0.0216(1) Uani Tc . . . O1 0.46645(7) 0.2659(2) -0.00751(6) 0.0380(4) Uani O . . . N1 0.27842(8) -0.0226(2) -0.00379(7) 0.0333(4) Uani N . . . N2 0.42578(8) -0.0523(2) 0.05147(6) 0.0281(4) Uani N . . . N3 0.35341(8) 0.2591(2) 0.05918(6) 0.0263(4) Uani N . . . N4 0.40680(9) 0.0793(2) 0.13129(6) 0.0292(4) Uani N . . . N5 0.47612(9) -0.1639(2) 0.13690(6) 0.0352(5) Uani N . . . N6 0.37115(8) 0.3571(2) 0.14941(6) 0.0321(5) Uani N . . . N7 0.38398(8) -0.0452(2) -0.06732(6) 0.0287(5) Uani N . . . N8 0.31537(8) 0.2776(2) -0.06128(6) 0.0270(5) Uani N . . . N9 0.34317(8) 0.1526(2) -0.13907(6) 0.0285(4) Uani N . . . N10 0.3902(1) -0.1100(2) -0.15650(7) 0.0400(5) Uani N . . . N11 0.28927(9) 0.4237(2) -0.14483(7) 0.0320(5) Uani N . . . C1 0.43651(9) -0.0483(2) 0.10414(7) 0.0246(5) Uani C . . . C2 0.37672(8) 0.2365(2) 0.11126(7) 0.0246(5) Uani C . . . C3 0.3333(1) 0.5202(3) 0.1328(1) 0.0457(7) Uani C . . . C4 0.4183(1) 0.3592(3) 0.20298(9) 0.0500(8) Uani C . . . C5 0.37398(9) -0.0039(2) -0.11842(7) 0.0253(5) Uani C . . . C6 0.31589(9) 0.2872(2) -0.11306(7) 0.0241(5) Uani C . . . C7 0.2671(1) 0.5810(3) -0.11998(9) 0.0405(6) Uani C . . . C8 0.2929(2) 0.4388(3) -0.2019(1) 0.0642(8) Uani C . . . Cl1 0.53295(3) -0.54221(7) 0.10243(2) 0.0428(2) Uani Cl . . . Cl2 0.39274(3) -0.12381(8) 0.24102(2) 0.0466(2) Uani Cl . . . H10 0.4798(11) 0.3188(33) 0.0221(9) 0.0570(74) Uiso H . . . H20 0.4648(11) 0.3419(33) -0.0296(9) 0.0529(70) Uiso H . . . H2 0.4489(11) -0.1173(28) 0.0404(8) 0.0375(60) Uiso H . . . H3 0.3403(10) 0.3520(29) 0.0513(8) 0.0368(59) Uiso H . . . H4 0.4102(11) 0.0517(28) 0.1630(9) 0.0436(65) Uiso H . . . H51 0.4826(11) -0.1516(31) 0.1720(9) 0.0498(67) Uiso H . . . H52 0.4901(10) -0.2492(28) 0.1230(8) 0.0353(57) Uiso H . . . H7 0.4048(10) -0.1336(28) -0.0609(8) 0.0341(57) Uiso H . . . H8 0.2958(10) 0.3629(28) -0.0498(8) 0.0334(56) Uiso H . . . H9 0.3458(10) 0.1687(27) -0.1711(8) 0.0330(55) Uiso H . . . H101 0.4141(10) -0.1969(28) -0.1453(8) 0.0366(59) Uiso H . . . H102 0.3923(12) -0.0672(30) -0.1865(10) 0.0549(75) Uiso H . . . H31 0.2879(11) 0.4984(34) 0.1080(9) 0.0523(69) Uiso H . . . H32 0.3274(14) 0.5767(36) 0.1671(11) 0.0822(99) Uiso H . . . H33 0.3595(15) 0.6006(38) 0.1158(12) 0.096(11) Uiso H . . . H41 0.4591(17) 0.3014(48) 0.2032(13) 0.122(13) Uiso H . . . H42 0.4204(14) 0.4696(39) 0.2188(11) 0.0823(93) Uiso H . . . H43 0.3996(15) 0.2953(45) 0.2279(12) 0.106(11) Uiso H . . . H71 0.2327(12) 0.5575(31) -0.0972(10) 0.0567(76) Uiso H . . . H72 0.3072(15) 0.6278(40) -0.0871(12) 0.092(10) Uiso H . . . H73 0.2535(13) 0.6622(37) -0.1445(11) 0.0761(88) Uiso H . . . H81 0.2730(15) 0.3342(42) -0.2206(12) 0.096(10) Uiso H . . . H82 0.3418(18) 0.4419(47) -0.2094(14) 0.131(14) Uiso H . . . H83 0.2639(16) 0.5205(48) -0.2188(13) 0.112(12) Uiso H . . . 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 Tc 0.0237(1) 0.0227(1) 0.0187(1) 0.0004(1) 0.0055(1) 0.0049(1) O1 0.0462(7) 0.0334(7) 0.0360(7) 0.0009(6) 0.0121(6) 0.0020(6) N1 0.0325(7) 0.0361(8) 0.0324(8) 0.0014(7) 0.0093(6) -0.0018(7) N2 0.0315(7) 0.0296(8) 0.0245(7) 0.0009(6) 0.0087(5) 0.0124(6) N3 0.0298(7) 0.0238(7) 0.0256(7) 0.0000(6) 0.0065(5) 0.0069(6) N4 0.0386(7) 0.0312(8) 0.0191(6) 0.0013(6) 0.0094(6) 0.0076(7) N5 0.0456(9) 0.0348(8) 0.0240(7) 0.0026(7) 0.0051(6) 0.0141(7) N6 0.0338(8) 0.0325(8) 0.0291(7) -0.0089(7) 0.0048(6) 0.0043(7) N7 0.0385(7) 0.0232(7) 0.0255(7) 0.0026(6) 0.0092(6) 0.0106(6) N8 0.0320(7) 0.0252(7) 0.0252(7) 0.0007(6) 0.0094(5) 0.0093(6) N9 0.0392(7) 0.0276(7) 0.0206(6) 0.0031(6) 0.0104(6) 0.0071(7) N10 0.0675(10) 0.0283(8) 0.0292(7) 0.0019(7) 0.0217(7) 0.0127(8) N11 0.0376(8) 0.0294(8) 0.0298(7) 0.0064(7) 0.0092(6) 0.0093(7) C1 0.0222(7) 0.0254(8) 0.0269(8) 0.0018(7) 0.0066(6) 0.0012(7) C2 0.0217(7) 0.0258(8) 0.0278(8) -0.0031(7) 0.0087(6) -0.0001(7) C3 0.0496(12) 0.0355(10) 0.0476(12) -0.0160(9) 0.0004(10) 0.0114(10) C4 0.0672(15) 0.0476(12) 0.0294(10) -0.0138(10) -0.0022(10) 0.0085(12) C5 0.0279(8) 0.0220(8) 0.0283(8) -0.0009(7) 0.0110(6) 0.0013(7) C6 0.0208(7) 0.0234(8) 0.0281(8) 0.0018(7) 0.0050(6) 0.0018(6) C7 0.0494(11) 0.0275(9) 0.0477(11) 0.0093(9) 0.0175(9) 0.0142(8) C8 0.1055(18) 0.0579(13) 0.0338(10) 0.0204(10) 0.0250(11) 0.0427(12) Cl1 0.0480(3) 0.0316(2) 0.0472(3) 0.0039(2) 0.0067(2) 0.0037(2) Cl2 0.0676(3) 0.0494(3) 0.0265(2) -0.0023(2) 0.0183(2) -0.0052(3) # 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 Tc N1 1.616(2) . . yes Tc N2 2.069(2) . . yes Tc N3 2.080(2) . . yes Tc N7 2.071(2) . . yes Tc N8 2.076(2) . . yes O1 H10 0.83(2) . . no O1 H20 0.79(2) . . no N2 C1 1.292(2) . . yes N2 H2 0.76(2) . . no N3 C2 1.299(2) . . yes N3 H3 0.76(2) . . no N4 C1 1.381(3) . . yes N4 C2 1.375(2) . . yes N4 H4 0.81(2) . . no N5 C1 1.331(2) . . yes N5 H51 0.87(2) . . no N5 H52 0.81(2) . . no N6 C2 1.344(2) . . yes N6 C3 1.457(3) . . yes N6 C4 1.458(3) . . yes N7 C5 1.292(2) . . yes N7 H7 0.78(2) . . no N8 C6 1.303(2) . . yes N8 H8 0.83(2) . . no N9 C5 1.380(2) . . yes N9 C6 1.379(3) . . yes N9 H9 0.82(2) . . no N10 C5 1.338(3) . . yes N10 H101 0.82(2) . . no N10 H102 0.83(2) . . no N11 C6 1.341(2) . . yes N11 C7 1.454(3) . . yes N11 C8 1.453(3) . . yes C3 H31 0.98(2) . . no C3 H32 0.99(3) . . no C3 H33 0.95(3) . . no C4 H41 0.91(3) . . no C4 H42 0.92(3) . . no C4 H43 0.93(3) . . no C7 H71 0.99(2) . . no C7 H72 1.07(2) . . no C7 H73 0.87(2) . . no C8 H81 0.96(3) . . no C8 H82 1.02(3) . . no C8 H83 0.88(3) . . 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 N1 Tc N2 104.9(1) . . . yes N1 Tc N3 100.9(1) . . . yes N1 Tc N7 101.8(1) . . . yes N1 Tc N8 101.2(1) . . . yes N2 Tc N3 84.2(1) . . . yes N2 Tc N7 89.5(1) . . . yes N2 Tc N8 153.9(1) . . . yes N3 Tc N7 157.2(1) . . . yes N3 Tc N8 90.7(1) . . . yes N7 Tc N8 85.4(1) . . . yes H10 O1 H20 103(2) . . . no Tc N2 C1 128.0(1) . . . yes Tc N2 H2 118(2) . . . no C1 N2 H2 114(2) . . . no Tc N3 C2 129.1(1) . . . yes Tc N3 H3 117(2) . . . no C2 N3 H3 114(1) . . . no C1 N4 C2 128.3(2) . . . yes C1 N4 H4 110(2) . . . no C2 N4 H4 121(2) . . . no C1 N5 H51 120(1) . . . no C1 N5 H52 118(1) . . . no H51 N5 H52 122(2) . . . no C2 N6 C3 119.2(2) . . . yes C2 N6 C4 122.0(2) . . . yes C3 N6 C4 116.0(2) . . . yes Tc N7 C5 129.7(1) . . . yes Tc N7 H7 118(1) . . . no C5 N7 H7 112(1) . . . no Tc N8 C6 130.8(1) . . . yes Tc N8 H8 115(1) . . . no C6 N8 H8 114(1) . . . no C5 N9 C6 129.9(2) . . . yes C5 N9 H9 112(1) . . . no C6 N9 H9 118(1) . . . no C5 N10 H101 116(1) . . . no C5 N10 H102 119(2) . . . no H101 N10 H102 119(2) . . . no C6 N11 C7 119.4(2) . . . yes C6 N11 C8 123.4(2) . . . yes C7 N11 C8 116.1(2) . . . yes N2 C1 N4 121.8(2) . . . yes N2 C1 N5 124.1(2) . . . yes N4 C1 N5 114.1(2) . . . yes N3 C2 N4 120.8(2) . . . yes N3 C2 N6 124.1(2) . . . yes N4 C2 N6 115.0(2) . . . yes N6 C3 H31 112(1) . . . no N6 C3 H32 105(2) . . . no N6 C3 H33 112(2) . . . no H31 C3 H32 111(2) . . . no H31 C3 H33 109(2) . . . no H32 C3 H33 107(2) . . . no N6 C4 H41 113(2) . . . no N6 C4 H42 112(2) . . . no N6 C4 H43 111(2) . . . no H41 C4 H42 118(3) . . . no H41 C4 H43 103(3) . . . no H42 C4 H43 100(3) . . . no N7 C5 N9 122.8(2) . . . yes N7 C5 N10 123.6(2) . . . yes N9 C5 N10 113.6(2) . . . yes N8 C6 N9 121.1(2) . . . yes N8 C6 N11 123.4(2) . . . yes N9 C6 N11 115.5(2) . . . yes N11 C7 H71 114(1) . . . no N11 C7 H72 111(2) . . . no N11 C7 H73 111(2) . . . no H71 C7 H72 95(2) . . . no H71 C7 H73 113(2) . . . no H72 C7 H73 112(2) . . . no N11 C8 H81 108(2) . . . no N11 C8 H82 116(2) . . . no N11 C8 H83 111(2) . . . no H81 C8 H82 103(3) . . . no H81 C8 H83 101(3) . . . no H82 C8 H83 116(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 Tc N2 C1 -74.4(2) . . . . no N1 Tc N2 H2 101(2) . . . . no N3 Tc N2 C1 25.4(2) . . . . no N3 Tc N2 H2 -158(2) . . . . no N7 Tc N2 C1 -176.5(2) . . . . no N7 Tc N2 H2 0(2) . . . . no N8 Tc N2 C1 105.0(2) . . . . no N8 Tc N2 H2 -79(2) . . . . no N1 Tc N3 C2 84.5(2) . . . . no N1 Tc N3 H3 -97(2) . . . . no N2 Tc N3 C2 -19.6(2) . . . . no N2 Tc N3 H3 158(2) . . . . no N7 Tc N3 C2 -94.4(2) . . . . no N7 Tc N3 H3 83(2) . . . . no N8 Tc N3 C2 -174.0(2) . . . . no N8 Tc N3 H3 4(2) . . . . no N1 Tc N7 C5 93.7(2) . . . . no N1 Tc N7 H7 -83(2) . . . . no N2 Tc N7 C5 -161.2(2) . . . . no N2 Tc N7 H7 22(2) . . . . no N3 Tc N7 C5 -87.4(2) . . . . no N3 Tc N7 H7 95(2) . . . . no N8 Tc N7 C5 -6.8(2) . . . . no N8 Tc N7 H7 176(2) . . . . no N1 Tc N8 C6 -98.0(2) . . . . no N1 Tc N8 H8 78(2) . . . . no N2 Tc N8 C6 82.6(2) . . . . no N2 Tc N8 H8 -100(2) . . . . no N3 Tc N8 C6 160.7(2) . . . . no N3 Tc N8 H8 -22(2) . . . . no N7 Tc N8 C6 3.2(2) . . . . no N7 Tc N8 H8 180(2) . . . . no Tc N2 C1 N4 -14.4(3) . . . . no Tc N2 C1 N5 165.4(1) . . . . no H2 N2 C1 N4 170(2) . . . . no H2 N2 C1 N5 -9(2) . . . . no Tc N3 C2 N4 2.6(3) . . . . no Tc N3 C2 N6 -174.5(1) . . . . no H3 N3 C2 N4 -174(2) . . . . no H3 N3 C2 N6 8(2) . . . . no C2 N4 C1 N2 -15.8(3) . . . . no C2 N4 C1 N5 164.3(2) . . . . no H4 N4 C1 N2 166(2) . . . . no H4 N4 C1 N5 -13(2) . . . . no C1 N4 C2 N3 21.9(3) . . . . no C1 N4 C2 N6 -160.8(2) . . . . no H4 N4 C2 N3 -159(2) . . . . no H4 N4 C2 N6 17(2) . . . . no H51 N5 C1 N2 178(2) . . . . no H51 N5 C1 N4 -2(2) . . . . no H52 N5 C1 N2 -8(2) . . . . no H52 N5 C1 N4 171(2) . . . . no C3 N6 C2 N3 3.8(3) . . . . no C3 N6 C2 N4 -173.4(2) . . . . no C4 N6 C2 N3 -156.5(2) . . . . no C4 N6 C2 N4 26.3(3) . . . . no C2 N6 C3 H31 48(2) . . . . no C2 N6 C3 H32 169(2) . . . . no C2 N6 C3 H33 -74(2) . . . . no C4 N6 C3 H31 -150(1) . . . . no C4 N6 C3 H32 -29(2) . . . . no C4 N6 C3 H33 86(2) . . . . no C2 N6 C4 H41 21(2) . . . . no C2 N6 C4 H42 157(2) . . . . no C2 N6 C4 H43 -92(2) . . . . no C3 N6 C4 H41 -139(2) . . . . no C3 N6 C4 H42 -3(2) . . . . no C3 N6 C4 H43 106(2) . . . . no Tc N7 C5 N9 7.6(3) . . . . no Tc N7 C5 N10 -170.2(1) . . . . no H7 N7 C5 N9 -174(2) . . . . no H7 N7 C5 N10 7(2) . . . . no Tc N8 C6 N9 -0.3(3) . . . . no Tc N8 C6 N11 178.2(1) . . . . no H8 N8 C6 N9 -176(2) . . . . no H8 N8 C6 N11 2(2) . . . . no C6 N9 C5 N7 -2.4(3) . . . . no C6 N9 C5 N10 175.6(2) . . . . no H9 N9 C5 N7 171(2) . . . . no H9 N9 C5 N10 -10(2) . . . . no C5 N9 C6 N8 -1.4(3) . . . . no C5 N9 C6 N11 180.0(2) . . . . no H9 N9 C6 N8 -173(2) . . . . no H9 N9 C6 N11 7(2) . . . . no H101 N10 C5 N7 -10(2) . . . . no H101 N10 C5 N9 171(2) . . . . no H102 N10 C5 N7 -163(2) . . . . no H102 N10 C5 N9 18(2) . . . . no C7 N11 C6 N8 8.8(3) . . . . no C7 N11 C6 N9 -172.6(2) . . . . no C8 N11 C6 N8 176.9(2) . . . . no C8 N11 C6 N9 -4.5(3) . . . . no C6 N11 C7 H71 -54(2) . . . . no C6 N11 C7 H72 51(2) . . . . no C6 N11 C7 H73 176(2) . . . . no C8 N11 C7 H71 136(2) . . . . no C8 N11 C7 H72 -117(2) . . . . no C8 N11 C7 H73 7(2) . . . . no C6 N11 C8 H81 55(2) . . . . no C6 N11 C8 H82 -59(2) . . . . no C6 N11 C8 H83 165(2) . . . . no C7 N11 C8 H81 -136(2) . . . . no C7 N11 C8 H82 108(2) . . . . no C7 N11 C8 H83 -25(2) . . . . no # CHEMICAL DATA _chemical_name_systematic ; ..... ; _chemical_formula_analytical 'C8 H24 Cl2 N11 O1 Tc1' _chemical_formula_moiety '[C8 H22 N11 Tc1.(H2O)^++^], 2Cl^-^' _chemical_formula_structural ? _chemical_formula_sum 'C8 H24 Cl2 N11 O1 Tc1 ' _chemical_formula_weight 460.16 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 19.620(3) _cell_length_b 7.576(1) _cell_length_c 25.074(3) _cell_angle_alpha 90.00(0) _cell_angle_beta 102.40(1) _cell_angle_gamma 90.00(0) _cell_volume 3640.1(9) _cell_formula_units_Z 8.00 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M ' C 2/c ' _symmetry_Int_Tables_number 15 _exptl_crystal_description ; prismatic ; _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.6793 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872.0 _exptl_absorpt_coefficient_mu 1.1057 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Plillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.0 # 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' _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 4367 _reflns_number_gt 3918 _reflns_threshold_expression 'I>3sigma(I)' _diffrn_reflns_av_R_equivalents 0.007 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_number 4488 _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) + (0.01F^2^)^2^)' _refine_ls_weighting_details ? _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_abs_structure_details ; ...... ; _refine_ls_number_reflns 3918 _refine_ls_number_parameters 304 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.021 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.027 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.34 _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 0.14 _refine_diff_density_min -0.11 _refine_diff_density_rms ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' 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 N4 H4 Cl2 0.81(2) 2.45(2) 3.215(2) 158(2) 1_555 yes N5 H51 Cl2 0.87(2) 2.73(2) 3.379(2) 133(2) 1_555 yes N5 H52 Cl1 0.81(2) 2.47(2) 3.259(2) 166(2) 1_555 yes O1 H10 Cl1 0.83(2) 2.31(2) 3.142(2) 172(2) 1_565 yes O1 H20 Cl1 0.79(2) 2.38(2) 3.171(2) 172(2) 2_655 yes N2 H2 O1 0.76(2) 2.30(2) 3.050(2) 168(2) 2_655 yes N10 H102 Cl2 0.83(2) 2.32(2) 3.130(2) 164(2) 6_554 yes N9 H9 Cl2 0.82(2) 2.59(2) 3.360(2) 157(2) 6_554 yes N10 H101 Cl1 0.82(2) 2.38(2) 3.190(2) 169(2) 2_645 yes #===END data_(II) # 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 # 'Tc' 4 'Technetium ' -1.4390 0.7593 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'O ' 8 'Oxygen ' 0.0106 0.0060 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'N ' 40 'Nitrogen ' 0.0061 0.0033 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 132 'Carbon ' 0.0033 0.0016 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'B ' 4 'Boron ' 0.0013 0.0007 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 176 '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 Tc 0.33812(2) 0.19764(2) 0.12819(1) 0.0300(1) Uani Tc . 0.8 . O1 0.2774(2) 0.1110(2) 0.1533(1) 0.0480(8) Uani O . 0.8 . Tc' 0.40078(9) 0.27506(7) 0.10652(5) 0.0321(3) Uani Tc . 0.2 . O1' 0.4720(11) 0.3589(7) 0.0880(6) 0.0596(36) Uani O . 0.2 . N1 0.4447(2) 0.2480(2) 0.2058(1) 0.0455(8) Uani N . . . N2 0.2365(2) 0.2954(2) 0.1476(1) 0.0494(8) Uani N . . . N3 0.3198(2) 0.3373(2) 0.2624(1) 0.0382(7) Uani N . . . N4 0.4957(2) 0.2984(2) 0.3180(1) 0.0641(10) Uani N . . . N5 0.1470(2) 0.3922(2) 0.2128(1) 0.0420(7) Uani N . . . N6 0.2889(2) 0.2258(2) 0.0271(1) 0.0447(8) Uani N . . . N7 0.4863(2) 0.1629(2) 0.0916(1) 0.0420(7) Uani N . . . N8 0.4264(2) 0.1483(2) -0.0328(1) 0.0362(7) Uani N . . . N9 0.2608(2) 0.2003(2) -0.0918(1) 0.0525(9) Uani N . . . N10 0.5956(2) 0.0885(2) 0.0178(1) 0.0394(7) Uani N . . . C1 0.4171(2) 0.2944(2) 0.2598(1) 0.0397(8) Uani C . . . C2 0.2355(2) 0.3404(2) 0.2070(1) 0.0356(7) Uani C . . . C3 0.1470(3) 0.4489(2) 0.2738(2) 0.0652(12) Uani C . . . C4 0.0426(3) 0.3953(2) 0.1609(2) 0.0607(11) Uani C . . . C5 0.3273(2) 0.1911(2) -0.0309(1) 0.0369(7) Uani C . . . C6 0.5011(2) 0.1346(2) 0.0261(1) 0.0330(7) Uani C . . . C7 0.6170(3) 0.0580(2) -0.0515(2) 0.0518(8) Uani C . . . C8 0.6816(3) 0.0653(2) 0.0768(2) 0.0571(11) Uani C . . . B1 0.8828(3) 0.2307(2) 0.4001(2) 0.0413(9) Uani B . . . C9 0.9272(3) 0.2880(2) 0.4701(2) 0.0446(9) Uani C . . . C10 0.9024(3) 0.2702(2) 0.5393(2) 0.0548(10) Uani C . . . C11 0.9469(4) 0.3179(3) 0.5981(2) 0.0659(13) Uani C . . . C12 1.0180(3) 0.3834(3) 0.5913(2) 0.0685(13) Uani C . . . C13 1.0485(3) 0.4027(2) 0.5245(2) 0.0631(12) Uani C . . . C14 1.0037(3) 0.3556(2) 0.4668(2) 0.0535(10) Uani C . . . C15 0.8288(2) 0.2857(2) 0.3306(2) 0.0384(8) Uani C . . . C16 0.7889(3) 0.2456(2) 0.2673(2) 0.0459(9) Uani C . . . C17 0.7411(3) 0.2861(2) 0.2069(2) 0.0510(10) Uani C . . . C18 0.7299(3) 0.3726(2) 0.2074(2) 0.0600(12) Uani C . . . C19 0.7674(3) 0.4152(2) 0.2686(2) 0.0554(10) Uani C . . . C20 0.8158(2) 0.3734(2) 0.3283(2) 0.0444(9) Uani C . . . C21 0.7783(3) 0.1656(2) 0.4155(2) 0.0438(9) Uani C . . . C22 0.7785(3) 0.0795(2) 0.3996(2) 0.0555(11) Uani C . . . C23 0.6864(4) 0.0273(2) 0.4096(2) 0.0659(13) Uani C . . . C24 0.5894(4) 0.0579(3) 0.4358(2) 0.0752(13) Uani C . . . C25 0.5858(3) 0.1416(3) 0.4511(2) 0.0754(14) Uani C . . . C26 0.6773(3) 0.1941(2) 0.4416(2) 0.0597(12) Uani C . . . C27 0.9989(3) 0.1778(2) 0.3833(2) 0.0432(8) Uani C . . . C28 1.0561(3) 0.1262(2) 0.4356(2) 0.0561(11) Uani C . . . C29 1.1568(3) 0.0810(3) 0.4269(2) 0.0728(13) Uani C . . . C30 1.2044(3) 0.0892(3) 0.3633(2) 0.0731(13) Uani C . . . C31 1.1497(3) 0.1385(3) 0.3114(2) 0.0677(12) Uani C . . . C32 1.0499(3) 0.1830(2) 0.3206(2) 0.0516(9) Uani C . . . O2 0.5929(2) 0.0911(2) 0.2447(1) 0.0693(9) Uani O . . . C33 0.5075(4) 0.0304(3) 0.2498(2) 0.0804(14) Uani C . . . H1 0.5015(23) 0.2275(17) 0.2132(14) 0.0379(74) Uiso H . . . H2 0.1900(24) 0.2987(16) 0.1242(14) 0.0378(77) Uiso H . . . H41 0.4881(32) 0.3182(21) 0.3557(19) 0.076(11) Uiso H . . . H42 0.5633(24) 0.2600(18) 0.3278(14) 0.0436(78) Uiso H . . . H60 0.2171(40) 0.2574(30) 0.0119(23) 0.125(16) Uiso H . . . H70 0.5427(22) 0.1430(16) 0.1251(13) 0.0341(71) Uiso H . . . H910 0.2804(29) 0.1781(20) -0.1352(17) 0.0625(99) Uiso H . . . H920 0.1987(24) 0.2297(18) -0.0892(14) 0.0460(80) Uiso H . . . H310 0.12560(0) 0.51507(0) 0.26528(0) 0.0710(0) Uiso H . . . H320 0.22816(0) 0.46068(0) 0.30829(0) 0.1230(0) Uiso H . . . H330 0.08912(0) 0.41464(0) 0.29275(0) 0.0848(0) Uiso H . . . H410 -0.02563(0) 0.42053(0) 0.17299(0) 0.1019(0) Uiso H . . . H420 -0.00621(0) 0.34768(0) 0.17976(0) 0.1164(0) Uiso H . . . H430 0.06736(0) 0.39708(0) 0.11313(0) 0.0957(0) Uiso H . . . H710 0.65467(0) 0.01106(0) -0.04501(0) 0.0718(0) Uiso H . . . H720 0.54653(0) 0.03108(0) -0.06923(0) 0.0976(0) Uiso H . . . H730 0.65584(0) 0.10073(0) -0.07092(0) 0.0744(0) Uiso H . . . H810 0.70901(0) 0.10591(0) 0.10456(0) 0.0829(0) Uiso H . . . H820 0.73830(0) 0.04820(0) 0.04750(0) 0.0743(0) Uiso H . . . H830 0.67010(0) 0.01690(0) 0.10460(0) 0.1299(0) Uiso H . . . H10 0.8490(25) 0.2270(19) 0.5502(15) 0.0483(83) Uiso H . . . H11 0.9509(39) 0.3104(26) 0.6397(23) 0.114(16) Uiso H . . . H12 1.0634(31) 0.4198(23) 0.6388(18) 0.080(12) Uiso H . . . H13 1.0965(29) 0.4391(21) 0.5166(18) 0.069(10) Uiso H . . . H14 1.0150(25) 0.3613(18) 0.4323(15) 0.0519(87) Uiso H . . . H16 0.7893(24) 0.1951(16) 0.2626(14) 0.0385(78) Uiso H . . . H17 0.7148(24) 0.2481(18) 0.1668(14) 0.0452(80) Uiso H . . . H18 0.6966(29) 0.4033(21) 0.1603(17) 0.071(11) Uiso H . . . H19 0.7650(22) 0.4662(16) 0.2681(14) 0.0369(74) Uiso H . . . H20 0.8415(21) 0.4094(16) 0.3694(12) 0.0310(68) Uiso H . . . H22 0.8592(35) 0.0493(27) 0.3837(22) 0.112(15) Uiso H . . . H23 0.7146(45) -0.0219(34) 0.4203(27) 0.159(21) Uiso H . . . H24 0.5267(43) 0.0177(31) 0.4446(27) 0.146(18) Uiso H . . . H25 0.5154(32) 0.1616(23) 0.4719(18) 0.080(11) Uiso H . . . H26 0.6657(29) 0.2447(22) 0.4627(17) 0.067(10) Uiso H . . . H28 1.0138(31) 0.1155(22) 0.4765(17) 0.078(11) Uiso H . . . H29 1.1865(28) 0.0421(21) 0.4723(17) 0.069(11) Uiso H . . . H30 1.2615(29) 0.0558(21) 0.3627(18) 0.071(11) Uiso H . . . H31 1.1647(23) 0.1449(17) 0.2812(14) 0.0396(75) Uiso H . . . H32 1.0081(31) 0.2296(23) 0.2868(18) 0.078(11) Uiso H . . . H200 0.6358(29) 0.1019(21) 0.2896(17) 0.074(11) Uiso H . . . H331 0.46005(0) 0.03467(0) 0.21114(0) 0.0778(0) Uiso H . . . H332 0.53142(0) -0.00997(0) 0.28360(0) 0.1470(0) Uiso H . . . H333 0.43998(0) 0.01884(0) 0.27364(0) 0.1033(0) Uiso H . . . 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 Tc 0.0272(1) 0.0398(1) 0.0231(1) 0.0000(1) 0.0035(1) 0.0021(1) O1 0.0459(13) 0.0503(14) 0.0495(13) 0.0064(12) 0.0126(11) -0.0027(12) Tc' 0.0324(5) 0.0378(5) 0.0263(5) -0.0082(4) 0.0049(4) 0.0046(5) O1' 0.0795(72) 0.0466(59) 0.0576(57) -0.0081(50) 0.0278(52) 0.0015(57) N1 0.0325(11) 0.0698(16) 0.0334(11) -0.0141(11) 0.0003(9) 0.0144(11) N2 0.0420(12) 0.0681(16) 0.0344(11) -0.0153(11) -0.0105(10) 0.0222(12) N3 0.0346(11) 0.0519(13) 0.0281(10) -0.0085(10) 0.0034(9) 0.0000(11) N4 0.0458(14) 0.1082(22) 0.0347(12) -0.0265(13) -0.0093(11) 0.0212(14) N5 0.0350(11) 0.0504(13) 0.0407(11) -0.0079(11) 0.0047(9) 0.0066(11) N6 0.0424(12) 0.0629(14) 0.0277(10) -0.0052(11) -0.0006(10) 0.0151(12) N7 0.0349(11) 0.0600(14) 0.0296(10) -0.0067(11) -0.0017(9) 0.0110(11) N8 0.0371(11) 0.0468(13) 0.0254(9) 0.0004(9) 0.0071(8) 0.0032(10) N9 0.0458(13) 0.0831(19) 0.0279(11) 0.0000(12) 0.0016(10) 0.0150(13) N10 0.0358(11) 0.0466(13) 0.0373(11) -0.0021(10) 0.0105(9) 0.0040(11) C1 0.0343(13) 0.0555(17) 0.0284(12) -0.0077(12) 0.0007(11) 0.0023(13) C2 0.0325(12) 0.0431(14) 0.0317(12) -0.0009(12) 0.0056(10) 0.0002(12) C3 0.0631(19) 0.0772(22) 0.0554(18) -0.0200(16) 0.0080(16) 0.0200(18) C4 0.0413(16) 0.0716(21) 0.0653(19) -0.0172(17) -0.0093(15) 0.0149(16) C5 0.0394(13) 0.0431(14) 0.0283(11) 0.0008(11) 0.0048(10) -0.0052(12) C6 0.0337(12) 0.0356(13) 0.0310(11) -0.0015(10) 0.0091(10) -0.0025(11) C7 0.0633(17) 0.0529(17) 0.0447(14) -0.0013(14) 0.0284(12) 0.0087(15) C8 0.0379(15) 0.0700(20) 0.0615(19) -0.0122(17) -0.0022(14) 0.0143(15) B1 0.0411(16) 0.0482(17) 0.0358(14) 0.0065(14) 0.0095(13) 0.0099(15) C9 0.0420(14) 0.0477(16) 0.0443(15) 0.0029(13) 0.0063(12) 0.0116(13) C10 0.0665(19) 0.0557(18) 0.0427(15) 0.0039(15) 0.0087(15) 0.0115(17) C11 0.0751(23) 0.0805(24) 0.0411(16) -0.0056(16) 0.0029(16) 0.0163(20) C12 0.0567(19) 0.0796(23) 0.0656(20) -0.0216(18) -0.0074(17) 0.0170(19) C13 0.0462(17) 0.0661(22) 0.0755(22) -0.0094(19) 0.0015(16) -0.0025(17) C14 0.0445(16) 0.0655(20) 0.0513(16) 0.0020(16) 0.0089(14) -0.0006(16) C15 0.0309(12) 0.0440(15) 0.0418(13) 0.0057(12) 0.0102(11) 0.0036(12) C16 0.0410(15) 0.0452(16) 0.0508(16) 0.0043(14) 0.0026(13) -0.0003(13) C17 0.0419(15) 0.0640(20) 0.0456(16) 0.0039(15) -0.0002(13) -0.0025(15) C18 0.0546(18) 0.0686(21) 0.0559(18) 0.0197(16) 0.0031(15) 0.0091(17) C19 0.0553(18) 0.0444(16) 0.0675(19) 0.0110(15) 0.0110(16) 0.0096(15) C20 0.0376(13) 0.0484(16) 0.0499(15) 0.0010(13) 0.0157(11) 0.0082(13) C21 0.0435(15) 0.0471(15) 0.0411(14) 0.0076(13) 0.0060(12) 0.0069(14) C22 0.0581(18) 0.0515(18) 0.0571(18) 0.0070(15) 0.0075(15) 0.0022(16) C23 0.0774(23) 0.0568(20) 0.0622(20) 0.0115(17) 0.0033(18) -0.0081(19) C24 0.0727(22) 0.0808(24) 0.0735(22) 0.0220(19) 0.0146(18) -0.0189(20) C25 0.0531(18) 0.0938(28) 0.0846(23) 0.0160(22) 0.0296(16) 0.0044(20) C26 0.0541(18) 0.0561(19) 0.0721(20) 0.0109(16) 0.0210(15) 0.0078(16) C27 0.0374(14) 0.0491(16) 0.0428(14) -0.0056(13) 0.0034(12) 0.0038(13) C28 0.0526(17) 0.0629(20) 0.0519(17) 0.0012(16) 0.0026(15) 0.0131(16) C29 0.0610(20) 0.0701(23) 0.0825(25) -0.0061(20) -0.0102(19) 0.0254(18) C30 0.0498(17) 0.0777(23) 0.0904(25) -0.0260(20) 0.0028(17) 0.0226(17) C31 0.0565(18) 0.0923(26) 0.0576(17) -0.0252(17) 0.0199(14) 0.0052(19) C32 0.0432(16) 0.0615(19) 0.0497(16) -0.0139(14) 0.0045(13) 0.0030(15) O2 0.0603(14) 0.0820(16) 0.0630(14) 0.0126(13) -0.0031(12) -0.0032(14) C33 0.0769(25) 0.0780(25) 0.0833(26) 0.0149(22) -0.0026(22) -0.0145(22) # 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 Tc O1 1.645(3) . . yes Tc Tc' 1.512(1) . . yes Tc N1 1.973(2) . . yes Tc N2 2.012(3) . . yes Tc N6 1.984(2) . . yes Tc N7 2.006(3) . . yes Tc' O1' 1.63(1) . . yes Tc' N1 1.939(3) . . yes Tc' N2 2.167(3) . . yes Tc' N6 2.022(3) . . yes Tc' N7 2.078(3) . . yes N1 C1 1.333(4) . . yes N1 H1 0.73(2) . . yes N2 C2 1.337(4) . . yes N2 H2 0.66(2) . . yes N3 C1 1.324(4) . . yes N3 C2 1.347(3) . . yes N4 C1 1.343(4) . . yes N4 H41 0.80(3) . . yes N4 H42 0.99(2) . . yes N5 C2 1.331(4) . . yes N5 C3 1.467(4) . . yes N5 C4 1.465(4) . . yes N6 C5 1.353(4) . . yes N6 H60 0.99(4) . . yes N7 C6 1.352(4) . . yes N7 H70 0.91(2) . . yes N8 C5 1.340(4) . . yes N8 C6 1.345(3) . . yes N9 C5 1.318(4) . . yes N9 H910 0.95(3) . . yes N9 H920 0.87(2) . . yes N10 C6 1.342(4) . . yes N10 C7 1.451(4) . . yes N10 C8 1.454(4) . . yes C3 H310 1.089(4) . . yes C3 H320 1.095(4) . . yes C3 H330 0.967(4) . . yes C4 H410 0.939(4) . . yes C4 H420 1.035(4) . . yes C4 H430 0.983(4) . . yes C7 H710 0.866(3) . . yes C7 H720 0.947(3) . . yes C7 H730 0.917(3) . . yes C8 H810 0.869(4) . . yes C8 H820 0.951(4) . . yes C8 H830 0.952(4) . . yes B1 C9 1.641(4) . . yes B1 C15 1.641(4) . . yes B1 C21 1.646(5) . . yes B1 C27 1.651(5) . . yes C9 C10 1.406(5) . . yes C9 C14 1.400(5) . . yes C10 C11 1.395(5) . . yes C10 H10 0.96(3) . . yes C11 C12 1.344(6) . . yes C11 H11 0.79(4) . . yes C12 C13 1.390(6) . . yes C12 H12 1.14(3) . . yes C13 C14 1.375(5) . . yes C13 H13 0.83(3) . . yes C14 H14 0.69(2) . . yes C15 C16 1.389(4) . . yes C15 C20 1.405(4) . . yes C16 C17 1.371(4) . . yes C16 H16 0.81(2) . . yes C17 C18 1.384(5) . . yes C17 H17 0.99(2) . . yes C18 C19 1.369(5) . . yes C18 H18 1.05(3) . . yes C19 C20 1.372(5) . . yes C19 H19 0.81(2) . . yes C20 H20 0.98(2) . . yes C21 C22 1.404(5) . . yes C21 C26 1.400(5) . . yes C22 C23 1.384(5) . . yes C22 H22 1.12(4) . . yes C23 C24 1.371(6) . . yes C23 H23 0.86(5) . . yes C24 C25 1.366(6) . . yes C24 H24 1.00(5) . . yes C25 C26 1.380(6) . . yes C25 H25 1.00(3) . . yes C26 H26 0.92(3) . . yes C27 C28 1.392(4) . . yes C27 C32 1.393(5) . . yes C28 C29 1.397(5) . . yes C28 H28 0.98(3) . . yes C29 C30 1.392(6) . . yes C29 H29 1.08(3) . . yes C30 C31 1.355(5) . . yes C30 H30 0.85(3) . . yes C31 C32 1.385(5) . . yes C31 H31 0.63(2) . . yes C32 H32 1.06(3) . . yes O2 C33 1.396(5) . . yes O2 H200 0.95(3) . . yes C33 H331 0.864(4) . . yes C33 H332 0.925(4) . . yes C33 H333 0.967(5) . . 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 Tc Tc' 176.6(1) . . . yes O1 Tc N1 112.1(1) . . . yes O1 Tc N2 108.4(1) . . . yes O1 Tc N6 112.7(1) . . . yes O1 Tc N7 106.4(1) . . . yes Tc' Tc N1 66.1(1) . . . yes Tc' Tc N2 74.3(1) . . . yes Tc' Tc N6 69.2(1) . . . yes Tc' Tc N7 70.8(1) . . . yes N1 Tc N2 82.9(1) . . . yes N1 Tc N6 135.2(1) . . . yes N1 Tc N7 83.4(1) . . . yes N2 Tc N6 84.0(1) . . . yes N2 Tc N7 145.2(1) . . . yes N6 Tc N7 83.5(1) . . . yes Tc Tc' O1' 176.6(4) . . . yes Tc Tc' N1 68.5(1) . . . yes Tc Tc' N2 63.4(1) . . . yes Tc Tc' N6 66.5(1) . . . yes Tc Tc' N7 65.7(1) . . . yes O1' Tc' N1 108.1(4) . . . yes O1' Tc' N2 116.4(4) . . . yes O1' Tc' N6 116.9(4) . . . yes O1' Tc' N7 114.4(4) . . . yes N1 Tc' N2 79.8(1) . . . yes N1 Tc' N6 134.9(1) . . . yes N1 Tc' N7 82.4(1) . . . yes N2 Tc' N6 79.2(1) . . . yes N2 Tc' N7 129.1(1) . . . yes N6 Tc' N7 80.7(1) . . . yes Tc N1 Tc' 45.5(1) . . . yes Tc N1 C1 127.7(2) . . . yes Tc N1 H1 115(2) . . . no Tc' N1 C1 124.3(2) . . . yes Tc' N1 H1 114(2) . . . no C1 N1 H1 113(2) . . . no Tc N2 Tc' 42.2(1) . . . yes Tc N2 C2 129.4(2) . . . yes Tc N2 H2 113(2) . . . no Tc' N2 C2 118.8(2) . . . yes Tc' N2 H2 117(2) . . . no C2 N2 H2 116(2) . . . no C1 N3 C2 122.1(2) . . . yes C1 N4 H41 128(3) . . . no C1 N4 H42 124(2) . . . no H41 N4 H42 104(3) . . . no C2 N5 C3 121.4(3) . . . yes C2 N5 C4 123.1(2) . . . yes C3 N5 C4 115.5(3) . . . yes Tc N6 Tc' 44.3(1) . . . yes Tc N6 C5 127.5(2) . . . yes Tc N6 H60 122(3) . . . no Tc' N6 C5 121.3(2) . . . yes Tc' N6 H60 118(3) . . . no C5 N6 H60 109(3) . . . no Tc N7 Tc' 43.4(1) . . . yes Tc N7 C6 128.3(2) . . . yes Tc N7 H70 115(2) . . . no Tc' N7 C6 121.8(2) . . . yes Tc' N7 H70 121(2) . . . no C6 N7 H70 111(2) . . . no C5 N8 C6 121.8(2) . . . yes C5 N9 H910 123(2) . . . no C5 N9 H920 114(2) . . . no H910 N9 H920 123(3) . . . no C6 N10 C7 121.4(2) . . . yes C6 N10 C8 122.8(2) . . . yes C7 N10 C8 115.8(2) . . . yes N1 C1 N3 126.8(3) . . . yes N1 C1 N4 117.1(2) . . . yes N3 C1 N4 116.2(3) . . . yes N2 C2 N3 123.9(2) . . . yes N2 C2 N5 119.2(3) . . . yes N3 C2 N5 116.9(2) . . . yes N5 C3 H310 120.0(3) . . . no N5 C3 H320 119.6(3) . . . no N5 C3 H330 90.7(3) . . . no H310 C3 H320 95.0(3) . . . no H310 C3 H330 116.4(4) . . . no H320 C3 H330 117.3(4) . . . no N5 C4 H410 120.0(3) . . . no N5 C4 H420 100.6(3) . . . no N5 C4 H430 108.1(3) . . . no H410 C4 H420 73.6(3) . . . no H410 C4 H430 124.1(4) . . . no H420 C4 H430 125.0(3) . . . no N6 C5 N8 126.7(3) . . . yes N6 C5 N9 116.9(2) . . . yes N8 C5 N9 116.4(3) . . . yes N7 C6 N8 124.6(2) . . . yes N7 C6 N10 119.1(2) . . . yes N8 C6 N10 116.3(2) . . . yes N10 C7 H710 107.3(3) . . . no N10 C7 H720 103.7(3) . . . no N10 C7 H730 105.1(3) . . . no H710 C7 H720 93.4(3) . . . no H710 C7 H730 115.7(4) . . . no H720 C7 H730 129.6(4) . . . no N10 C8 H810 116.3(3) . . . no N10 C8 H820 94.6(3) . . . no N10 C8 H830 120.2(3) . . . no H810 C8 H820 109.8(4) . . . no H810 C8 H830 109.4(4) . . . no H820 C8 H830 104.2(3) . . . no C9 B1 C15 113.8(2) . . . yes C9 B1 C21 111.8(3) . . . yes C9 B1 C27 104.8(2) . . . yes C15 B1 C21 105.2(2) . . . yes C15 B1 C27 110.9(2) . . . yes C21 B1 C27 110.3(2) . . . yes B1 C9 C10 124.2(3) . . . yes B1 C9 C14 122.0(3) . . . yes C10 C9 C14 113.5(3) . . . yes C9 C10 C11 122.6(3) . . . yes C9 C10 H10 124(2) . . . no C11 C10 H10 114(2) . . . no C10 C11 C12 121.1(4) . . . yes C10 C11 H11 133(3) . . . no C12 C11 H11 104(3) . . . no C11 C12 C13 119.1(3) . . . yes C11 C12 H12 123(2) . . . no C13 C12 H12 117(2) . . . no C12 C13 C14 119.3(3) . . . yes C12 C13 H13 125(2) . . . no C14 C13 H13 116(2) . . . no C9 C14 C13 124.4(3) . . . yes C9 C14 H14 110(2) . . . no C13 C14 H14 126(2) . . . no B1 C15 C16 120.2(3) . . . yes B1 C15 C20 125.8(3) . . . yes C16 C15 C20 114.0(3) . . . yes C15 C16 C17 124.3(3) . . . yes C15 C16 H16 123(2) . . . no C17 C16 H16 113(2) . . . no C16 C17 C18 119.4(3) . . . yes C16 C17 H17 114(2) . . . no C18 C17 H17 126(2) . . . no C17 C18 C19 118.6(3) . . . yes C17 C18 H18 119(2) . . . no C19 C18 H18 122(2) . . . no C18 C19 C20 121.0(3) . . . yes C18 C19 H19 119(2) . . . no C20 C19 H19 120(2) . . . no C15 C20 C19 122.7(3) . . . yes C15 C20 H20 122(1) . . . no C19 C20 H20 115(1) . . . no B1 C21 C22 123.7(3) . . . yes B1 C21 C26 121.5(3) . . . yes C22 C21 C26 114.6(3) . . . yes C21 C22 C23 122.3(3) . . . yes C21 C22 H22 120(2) . . . no C23 C22 H22 117(2) . . . no C22 C23 C24 121.1(4) . . . yes C22 C23 H23 107(4) . . . no C24 C23 H23 123(4) . . . no C23 C24 C25 118.2(4) . . . yes C23 C24 H24 119(3) . . . no C25 C24 H24 123(3) . . . no C24 C25 C26 121.2(4) . . . yes C24 C25 H25 116(2) . . . no C26 C25 H25 122(2) . . . no C21 C26 C25 122.6(3) . . . yes C21 C26 H26 128(2) . . . no C25 C26 H26 109(2) . . . no B1 C27 C28 119.6(3) . . . yes B1 C27 C32 125.1(3) . . . yes C28 C27 C32 115.3(3) . . . yes C27 C28 C29 123.6(3) . . . yes C27 C28 H28 115(2) . . . no C29 C28 H28 121(2) . . . no C28 C29 C30 118.6(3) . . . yes C28 C29 H29 113(2) . . . no C30 C29 H29 128(2) . . . no C29 C30 C31 119.0(4) . . . yes C29 C30 H30 110(2) . . . no C31 C30 H30 130(2) . . . no C30 C31 C32 121.9(3) . . . yes C30 C31 H31 127(2) . . . no C32 C31 H31 111(2) . . . no C27 C32 C31 121.7(3) . . . yes C27 C32 H32 110(2) . . . no C31 C32 H32 127(2) . . . no C33 O2 H200 111(2) . . . no O2 C33 H331 105.6(4) . . . no O2 C33 H332 111.9(4) . . . no O2 C33 H333 141.7(4) . . . no H331 C33 H332 138.5(5) . . . no H331 C33 H333 86.8(4) . . . no H332 C33 H333 74.7(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 O1 Tc Tc' O1' -57(7) . . . . no O1 Tc Tc' N1 -55(2) . . . . no O1 Tc Tc' N2 -144(2) . . . . no O1 Tc Tc' N6 125(2) . . . . no O1 Tc Tc' N7 35(2) . . . . no N1 Tc Tc' O1' 0(7) . . . . no N1 Tc Tc' N2 -89.1(1) . . . . no N1 Tc Tc' N6 -178.6(1) . . . . no N1 Tc Tc' N7 91.2(1) . . . . no N2 Tc Tc' O1' 88(7) . . . . no N2 Tc Tc' N1 89.1(1) . . . . no N2 Tc Tc' N6 -89.5(1) . . . . no N2 Tc Tc' N7 -179.6(1) . . . . no N6 Tc Tc' O1' 177(7) . . . . no N6 Tc Tc' N1 178.6(1) . . . . no N6 Tc Tc' N2 89.5(1) . . . . no N6 Tc Tc' N7 -90.2(1) . . . . no N7 Tc Tc' O1' -92(7) . . . . no N7 Tc Tc' N1 -91.2(1) . . . . no N7 Tc Tc' N2 179.6(1) . . . . no N7 Tc Tc' N6 90.2(1) . . . . no O1 Tc N1 Tc' 177.0(1) . . . . no O1 Tc N1 C1 -79.1(3) . . . . no O1 Tc N1 H1 77(2) . . . . no Tc' Tc N1 C1 103.9(3) . . . . no Tc' Tc N1 H1 -99(2) . . . . no N2 Tc N1 Tc' -76.0(1) . . . . no N2 Tc N1 C1 27.9(3) . . . . no N2 Tc N1 H1 -175(2) . . . . no N6 Tc N1 Tc' -1.9(2) . . . . no N6 Tc N1 C1 102.0(3) . . . . no N6 Tc N1 H1 -101(2) . . . . no N7 Tc N1 Tc' 71.9(1) . . . . no N7 Tc N1 C1 175.8(3) . . . . no N7 Tc N1 H1 -27(2) . . . . no O1 Tc N2 Tc' 178.0(1) . . . . no O1 Tc N2 C2 86.7(3) . . . . no O1 Tc N2 H2 -76(3) . . . . no Tc' Tc N2 C2 -91.3(3) . . . . no Tc' Tc N2 H2 106(3) . . . . no N1 Tc N2 Tc' 67.1(1) . . . . no N1 Tc N2 C2 -24.2(3) . . . . no N1 Tc N2 H2 173(3) . . . . no N6 Tc N2 Tc' -70.0(1) . . . . no N6 Tc N2 C2 -161.3(3) . . . . no N6 Tc N2 H2 35(3) . . . . no N7 Tc N2 Tc' -0.6(2) . . . . no N7 Tc N2 C2 -91.9(3) . . . . no N7 Tc N2 H2 105(3) . . . . no O1 Tc N6 Tc' -177.0(1) . . . . no O1 Tc N6 C5 -78.3(3) . . . . no O1 Tc N6 H60 85(3) . . . . no Tc' Tc N6 C5 98.7(3) . . . . no Tc' Tc N6 H60 -97(3) . . . . no N1 Tc N6 Tc' 1.9(2) . . . . no N1 Tc N6 C5 100.6(3) . . . . no N1 Tc N6 H60 -95(3) . . . . no N2 Tc N6 Tc' 75.5(1) . . . . no N2 Tc N6 C5 174.2(3) . . . . no N2 Tc N6 H60 -21(3) . . . . no N7 Tc N6 Tc' -71.9(1) . . . . no N7 Tc N6 C5 26.8(2) . . . . no N7 Tc N6 H60 -169(3) . . . . no O1 Tc N7 Tc' -178.0(1) . . . . no O1 Tc N7 C6 83.8(3) . . . . no O1 Tc N7 H70 -68(2) . . . . no Tc' Tc N7 C6 -98.2(2) . . . . no Tc' Tc N7 H70 109(2) . . . . no N1 Tc N7 Tc' -66.9(1) . . . . no N1 Tc N7 C6 -165.1(3) . . . . no N1 Tc N7 H70 43(2) . . . . no N2 Tc N7 Tc' 0.6(2) . . . . no N2 Tc N7 C6 -97.6(3) . . . . no N2 Tc N7 H70 110(2) . . . . no N6 Tc N7 Tc' 70.2(1) . . . . no N6 Tc N7 C6 -28.0(2) . . . . no N6 Tc N7 H70 180(2) . . . . no Tc Tc' N1 C1 -111.5(2) . . . . no Tc Tc' N1 H1 103(2) . . . . no O1' Tc' N1 Tc 179.9(4) . . . . no O1' Tc' N1 C1 68.4(5) . . . . no O1' Tc' N1 H1 -76(2) . . . . no N2 Tc' N1 Tc 65.3(1) . . . . no N2 Tc' N1 C1 -46.2(2) . . . . no N2 Tc' N1 H1 168(2) . . . . no N6 Tc' N1 Tc 1.9(2) . . . . no N6 Tc' N1 C1 -109.7(3) . . . . no N6 Tc' N1 H1 104(2) . . . . no N7 Tc' N1 Tc -66.9(1) . . . . no N7 Tc' N1 C1 -178.4(3) . . . . no N7 Tc' N1 H1 36(2) . . . . no Tc Tc' N2 C2 118.1(2) . . . . no Tc Tc' N2 H2 -94(3) . . . . no O1' Tc' N2 Tc -176.2(5) . . . . no O1' Tc' N2 C2 -58.0(5) . . . . no O1' Tc' N2 H2 89(3) . . . . no N1 Tc' N2 Tc -70.9(1) . . . . no N1 Tc' N2 C2 47.2(2) . . . . no N1 Tc' N2 H2 -165(3) . . . . no N6 Tc' N2 Tc 68.9(1) . . . . no N6 Tc' N2 C2 -172.9(2) . . . . no N6 Tc' N2 H2 -25(3) . . . . no N7 Tc' N2 Tc 0.4(1) . . . . no N7 Tc' N2 C2 118.6(2) . . . . no N7 Tc' N2 H2 -94(3) . . . . no Tc Tc' N6 C5 -113.4(2) . . . . no Tc Tc' N6 H60 109(3) . . . . no O1' Tc' N6 Tc -179.8(5) . . . . no O1' Tc' N6 C5 66.8(5) . . . . no O1' Tc' N6 H60 -70(3) . . . . no N1 Tc' N6 Tc -1.9(2) . . . . no N1 Tc' N6 C5 -115.3(2) . . . . no N1 Tc' N6 H60 107(3) . . . . no N2 Tc' N6 Tc -65.5(1) . . . . no N2 Tc' N6 C5 -178.9(2) . . . . no N2 Tc' N6 H60 43(3) . . . . no N7 Tc' N6 Tc 67.5(1) . . . . no N7 Tc' N6 C5 -45.9(2) . . . . no N7 Tc' N6 H60 176(3) . . . . no Tc Tc' N7 C6 113.9(2) . . . . no Tc Tc' N7 H70 -94(2) . . . . no O1' Tc' N7 Tc 176.2(4) . . . . no O1' Tc' N7 C6 -69.9(5) . . . . no O1' Tc' N7 H70 81(2) . . . . no N1 Tc' N7 Tc 69.8(1) . . . . no N1 Tc' N7 C6 -176.3(2) . . . . no N1 Tc' N7 H70 -24(2) . . . . no N2 Tc' N7 Tc -0.4(1) . . . . no N2 Tc' N7 C6 113.5(2) . . . . no N2 Tc' N7 H70 -94(2) . . . . no N6 Tc' N7 Tc -68.3(1) . . . . no N6 Tc' N7 C6 45.6(2) . . . . no N6 Tc' N7 H70 -162(2) . . . . no Tc N1 C1 N3 -21.8(4) . . . . no Tc N1 C1 N4 158.1(2) . . . . no Tc' N1 C1 N3 35.1(4) . . . . no Tc' N1 C1 N4 -144.9(2) . . . . no H1 N1 C1 N3 -178(2) . . . . no H1 N1 C1 N4 1(2) . . . . no Tc N2 C2 N3 12.9(4) . . . . no Tc N2 C2 N5 -167.4(2) . . . . no Tc' N2 C2 N3 -37.2(3) . . . . no Tc' N2 C2 N5 142.5(2) . . . . no H2 N2 C2 N3 176(3) . . . . no H2 N2 C2 N5 -4(3) . . . . no C2 N3 C1 N1 -1.9(4) . . . . no C2 N3 C1 N4 178.1(3) . . . . no C1 N3 C2 N2 6.3(4) . . . . no C1 N3 C2 N5 -173.3(3) . . . . no H41 N4 C1 N1 -170(3) . . . . no H41 N4 C1 N3 9(3) . . . . no H42 N4 C1 N1 -13(2) . . . . no H42 N4 C1 N3 166(2) . . . . no C3 N5 C2 N2 -174.1(3) . . . . no C3 N5 C2 N3 5.6(4) . . . . no C4 N5 C2 N2 7.7(4) . . . . no C4 N5 C2 N3 -172.6(3) . . . . no C2 N5 C3 H310 131.5(3) . . . . no C2 N5 C3 H320 15.2(5) . . . . no C2 N5 C3 H330 -107.1(3) . . . . no C4 N5 C3 H310 -50.2(4) . . . . no C4 N5 C3 H320 -166.4(3) . . . . no C4 N5 C3 H330 71.2(3) . . . . no C2 N5 C4 H410 162.5(3) . . . . no C2 N5 C4 H420 85.3(3) . . . . no C2 N5 C4 H430 -47.1(4) . . . . no C3 N5 C4 H410 -15.9(5) . . . . no C3 N5 C4 H420 -93.0(3) . . . . no C3 N5 C4 H430 134.6(3) . . . . no Tc N6 C5 N8 -19.8(4) . . . . no Tc N6 C5 N9 160.4(2) . . . . no Tc' N6 C5 N8 34.2(4) . . . . no Tc' N6 C5 N9 -145.6(2) . . . . no H60 N6 C5 N8 175(3) . . . . no H60 N6 C5 N9 -4(3) . . . . no Tc N7 C6 N8 21.5(4) . . . . no Tc N7 C6 N10 -157.6(2) . . . . no Tc' N7 C6 N8 -31.7(4) . . . . no Tc' N7 C6 N10 149.2(2) . . . . no H70 N7 C6 N8 175(2) . . . . no H70 N7 C6 N10 -3(2) . . . . no C6 N8 C5 N6 0.4(4) . . . . no C6 N8 C5 N9 -179.8(3) . . . . no C5 N8 C6 N7 -1.3(4) . . . . no C5 N8 C6 N10 177.9(2) . . . . no H910 N9 C5 N6 -179(2) . . . . no H910 N9 C5 N8 0(2) . . . . no H920 N9 C5 N6 2(2) . . . . no H920 N9 C5 N8 -177(2) . . . . no C7 N10 C6 N7 -178.8(3) . . . . no C7 N10 C6 N8 2.0(4) . . . . no C8 N10 C6 N7 2.0(4) . . . . no C8 N10 C6 N8 -177.3(3) . . . . no C6 N10 C7 H710 -149.6(3) . . . . no C6 N10 C7 H720 -51.5(4) . . . . no C6 N10 C7 H730 86.7(3) . . . . no C8 N10 C7 H710 29.8(4) . . . . no C8 N10 C7 H720 127.8(3) . . . . no C8 N10 C7 H730 -93.9(3) . . . . no C6 N10 C8 H810 -51.1(5) . . . . no C6 N10 C8 H820 -165.9(3) . . . . no C6 N10 C8 H830 84.7(4) . . . . no C7 N10 C8 H810 129.6(3) . . . . no C7 N10 C8 H820 14.8(3) . . . . no C7 N10 C8 H830 -94.6(4) . . . . no N5 C4 H410 H420 -93.0(3) . . . . no H430 C4 H410 H420 121.5(5) . . . . no N5 C4 H420 H410 118.4(3) . . . . no H430 C4 H420 H410 -120.5(5) . . . . no C15 B1 C9 C10 134.4(3) . . . . no C15 B1 C9 C14 -52.0(4) . . . . no C21 B1 C9 C10 15.3(4) . . . . no C21 B1 C9 C14 -171.0(3) . . . . no C27 B1 C9 C10 -104.2(3) . . . . no C27 B1 C9 C14 69.4(3) . . . . no C9 B1 C15 C16 179.3(3) . . . . no C9 B1 C15 C20 -2.1(4) . . . . no C21 B1 C15 C16 -58.0(3) . . . . no C21 B1 C15 C20 120.7(3) . . . . no C27 B1 C15 C16 61.4(3) . . . . no C27 B1 C15 C20 -120.0(3) . . . . no C9 B1 C21 C22 -130.6(3) . . . . no C9 B1 C21 C26 53.9(4) . . . . no C15 B1 C21 C22 105.4(3) . . . . no C15 B1 C21 C26 -70.1(4) . . . . no C27 B1 C21 C22 -14.4(4) . . . . no C27 B1 C21 C26 170.2(3) . . . . no C9 B1 C27 C28 57.7(3) . . . . no C9 B1 C27 C32 -119.2(3) . . . . no C15 B1 C27 C28 -179.0(3) . . . . no C15 B1 C27 C32 4.1(4) . . . . no C21 B1 C27 C28 -62.8(4) . . . . no C21 B1 C27 C32 120.3(3) . . . . no B1 C9 C10 C11 176.4(3) . . . . no B1 C9 C10 H10 -7(2) . . . . no C14 C9 C10 C11 2.3(5) . . . . no C14 C9 C10 H10 178(2) . . . . no B1 C9 C14 C13 -176.3(3) . . . . no B1 C9 C14 H14 4(3) . . . . no C10 C9 C14 C13 -2.0(5) . . . . no C10 C9 C14 H14 178(3) . . . . no C9 C10 C11 C12 -0.9(6) . . . . no C9 C10 C11 H11 -165(4) . . . . no H10 C10 C11 C12 -176(2) . . . . no H10 C10 C11 H11 18(5) . . . . no C10 C11 C12 C13 -0.9(6) . . . . no C10 C11 C12 H12 -173(2) . . . . no H11 C11 C12 C13 168(3) . . . . no H11 C11 C12 H12 -4(4) . . . . no C11 C12 C13 C14 1.3(6) . . . . no C11 C12 C13 H13 -173(3) . . . . no H12 C12 C13 C14 174(2) . . . . no H12 C12 C13 H13 0(4) . . . . no C12 C13 C14 C9 0.3(6) . . . . no C12 C13 C14 H14 -179(3) . . . . no H13 C13 C14 C9 176(3) . . . . no H13 C13 C14 H14 -3(4) . . . . no B1 C15 C16 C17 179.1(3) . . . . no B1 C15 C16 H16 1(2) . . . . no C20 C15 C16 C17 0.3(4) . . . . no C20 C15 C16 H16 -176(2) . . . . no B1 C15 C20 C19 -178.5(3) . . . . no B1 C15 C20 H20 2(2) . . . . no C16 C15 C20 C19 0.2(4) . . . . no C16 C15 C20 H20 -178(2) . . . . no C15 C16 C17 C18 -0.5(5) . . . . no C15 C16 C17 H17 -177(2) . . . . no H16 C16 C17 C18 177(2) . . . . no H16 C16 C17 H17 0(3) . . . . no C16 C17 C18 C19 0.2(5) . . . . no C16 C17 C18 H18 177(2) . . . . no H17 C17 C18 C19 178(2) . . . . no H17 C17 C18 H18 -4(3) . . . . no C17 C18 C19 C20 0.3(5) . . . . no C17 C18 C19 H19 176(2) . . . . no H18 C18 C19 C20 -176(2) . . . . no H18 C18 C19 H19 0(3) . . . . no C18 C19 C20 C15 -0.5(5) . . . . no C18 C19 C20 H20 179(2) . . . . no H19 C19 C20 C15 -175(2) . . . . no H19 C19 C20 H20 3(3) . . . . no B1 C21 C22 C23 -176.4(3) . . . . no B1 C21 C22 H22 10(2) . . . . no C26 C21 C22 C23 -0.6(5) . . . . no C26 C21 C22 H22 -173(2) . . . . no B1 C21 C26 C25 176.2(3) . . . . no B1 C21 C26 H26 -16(3) . . . . no C22 C21 C26 C25 0.3(5) . . . . no C22 C21 C26 H26 167(3) . . . . no C21 C22 C23 C24 0.2(6) . . . . no C21 C22 C23 H23 -147(4) . . . . no H22 C22 C23 C24 174(2) . . . . no H22 C22 C23 H23 25(4) . . . . no C22 C23 C24 C25 0.6(6) . . . . no C22 C23 C24 H24 -176(3) . . . . no H23 C23 C24 C25 144(4) . . . . no H23 C23 C24 H24 -32(5) . . . . no C23 C24 C25 C26 -0.8(6) . . . . no C23 C24 C25 H25 -177(2) . . . . no H24 C24 C25 C26 176(3) . . . . no H24 C24 C25 H25 0(4) . . . . no C24 C25 C26 C21 0.4(6) . . . . no C24 C25 C26 H26 -168(2) . . . . no H25 C25 C26 C21 177(2) . . . . no H25 C25 C26 H26 8(3) . . . . no B1 C27 C28 C29 -178.1(3) . . . . no B1 C27 C28 H28 12(2) . . . . no C32 C27 C28 C29 -0.9(5) . . . . no C32 C27 C28 H28 -170(2) . . . . no B1 C27 C32 C31 178.0(3) . . . . no B1 C27 C32 H32 5(2) . . . . no C28 C27 C32 C31 0.9(5) . . . . no C28 C27 C32 H32 -171(2) . . . . no C27 C28 C29 C30 1.5(6) . . . . no C27 C28 C29 H29 -176(2) . . . . no H28 C28 C29 C30 171(2) . . . . no H28 C28 C29 H29 -7(3) . . . . no C28 C29 C30 C31 -2.1(6) . . . . no C28 C29 C30 H30 -174(2) . . . . no H29 C29 C30 C31 177(2) . . . . no H29 C29 C30 H30 4(3) . . . . no C29 C30 C31 C32 2.2(6) . . . . no C29 C30 C31 H31 -178(3) . . . . no H30 C30 C31 C32 173(3) . . . . no H30 C30 C31 H31 -6(4) . . . . no C30 C31 C32 C27 -1.6(6) . . . . no C30 C31 C32 H32 170(2) . . . . no H31 C31 C32 C27 179(3) . . . . no H31 C31 C32 H32 -8(4) . . . . no H200 O2 C33 H331 164(2) . . . . no H200 O2 C33 H332 -34(2) . . . . no H200 O2 C33 H333 58(2) . . . . no O2 C33 H332 H333 140.1(5) . . . . no H331 C33 H332 H333 -66.7(7) . . . . no O2 C33 H333 H332 -106.2(7) . . . . no H331 C33 H333 H332 142.4(5) . . . . no # CHEMICAL DATA _chemical_name_systematic ; ..... ; _chemical_formula_analytical 'C33 H44 B1 N10 O2 Tc1' _chemical_formula_moiety '[C8 H20 N10 O1 Tc1]+.[C24 H20 B1]-.C1 H4 O1' _chemical_formula_structural ? _chemical_formula_sum ' C33 H44 B1 N10 O2 Tc1 ' _chemical_formula_weight 722.49 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 11.589(2) _cell_length_b 15.918(2) _cell_length_c 18.962(4) _cell_angle_alpha 90.00(0) _cell_angle_beta 96.97(1) _cell_angle_gamma 90.00(0) _cell_volume 3472.(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 295 _cell_measurement_radiation 'Mo K\a' _cell_measurement_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M ' P21/c ' _symmetry_Int_Tables_number 14 _exptl_crystal_description ; prismatic ; _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_diffrn 1.3821 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504.0 _exptl_absorpt_coefficient_mu 0.4602 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '[North, Phillips & Mathews, 1968]' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1. # 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_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _reflns_number_total 7561 _reflns_number_gt 6172 _reflns_threshold_expression 'I>3sima(I)' _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_number 7792 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 27 _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 'mixed' _refine_ls_structure_factor_coef 'F' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme 'calc w= 4F^2^/(\s^2^(I) + (0.04F^2^)^2^)' _refine_ls_weighting_details ? _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_abs_structure_details ; ...... ; _refine_ls_number_reflns 6172 _refine_ls_number_parameters 558 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.062 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.23 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max 0.02 _refine_ls_shift/su_mean ? _refine_diff_density_max 0.043 _refine_diff_density_min -0.035 _refine_diff_density_rms ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' 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 N1 H1 O2 0.73(3) 2.46(3) 3.069(4) 142(3) 1_555 ? N7 H70 O2 0.91(2) 2.42(2) 3.223(3) 147(2) 1_555 ? N4 H41 N8 0.80(4) 2.37(4) 3.151(3) 165(3) 4_555 ? N9 H910 N3 0.95(3) 2.06(3) 2.987(3) 165(3) 4_554 ? #===END