# Copyright The Royal Society of Chemistry, 1998 data_global _audit_creation_date ? _audit_creation_method 'PARSTCIF' _audit_update_record ? # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_contact_letter ; ; _publ_requested_journal 'J. Chem. Soc. Dalton Trans' _publ_requested_category ? _publ_requested_coeditor_name ? # AUTHOR LIST loop_ _publ_author_name _publ_author_footnote _publ_author_address ? ? ? # TITLE _publ_section_title ; ...... ; _publ_section_title_footnote ; ...... ; # TEXT _publ_section_abstract ; ...... ; _publ_section_comment ; ...... ; _publ_section_acknowledgements ; ...... ; _publ_section_references ; Nardelli, M.(1983). Comput. Chem. 7, 95-98. Nardelli, M.(1991). PARSTCIF. Program for Creating a CIF from the Output of PARST. University of Parma, Italy. Nardelli, M.(1995). J. Appl. Cryst. 28, 659. ; _publ_section_figure_captions ; ...... ; _publ_section_exptl_prep ; ...... ; _publ_section_exptl_refinement ; ...... ; _computing_data_collection 'CAD4 Enraf-Nonius, 1984' _computing_cell_refinement 'CAD4 Enraf-Nonius, 1984' _computing_data_reduction 'MolEN, C.K. Fair, Enraf-Nonius,1990' _computing_structure_solution 'MolEN, 1990' _computing_structure_refinement 'MolEN, 1990' _computing_molecular_graphics 'ORTEP II, Johnson, 1976' _computing_publication_material ; PARST (Nardelli, 1983, 1995); PARSTCIF (Nardelli, 1991) ; #-------------------------- data section of block --------------------------- 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' 2 'Technetium ' -1.4390 0.7593 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'Cl' 2 'Chlorine ' 0.1484 0.1585 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'S ' 4 'Sulphur ' 0.1246 0.1234 '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 ' 6 'Nitrogen ' 0.0061 0.0033 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'C ' 28 'Carbon ' 0.0033 0.0016 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 'H ' 34 '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 0.10733(2) 0.00000(0) 0.25876(2) 0.0354(0) Uani Tc . . . Cl -0.05118(9) -0.09852(5) 0.38273(7) 0.0543(2) Uani Cl . . . S1 -0.12494(8) -0.02391(4) 0.03490(7) 0.0464(2) Uani S . . . S2 -0.2378(1) 0.09981(6) -0.26466(9) 0.0652(2) Uani S . . . O1 0.2719(2) -0.0522(1) 0.2218(2) 0.0518(5) Uani O . . . O2 0.0866(3) 0.2875(1) 0.2370(2) 0.0566(6) Uani O . . . O3 0.1920(3) 0.0887(2) 0.7393(2) 0.0613(6) Uani O . . . O4 0.2626(2) -0.0482(1) 0.6438(2) 0.0464(5) Uani O . . . N1 -0.0130(3) 0.1469(1) 0.0056(2) 0.0431(6) Uani N . . . N2 0.0790(3) 0.1288(1) 0.1708(2) 0.0393(6) Uani N . . . N3 0.1834(3) 0.0731(1) 0.4662(2) 0.0417(5) Uani N . . . C1 -0.1127(3) 0.0793(2) -0.0681(3) 0.0435(7) Uani C . . . C2 -0.3228(4) -0.0143(3) -0.3303(4) 0.0696(11) Uani C . . . C3 0.0196(4) 0.2323(2) -0.0806(3) 0.0568(8) Uani C . . . C4 0.1135(3) 0.2057(2) 0.2767(3) 0.0410(6) Uani C . . . C5 0.1864(3) 0.1758(2) 0.4533(3) 0.0406(6) Uani C . . . C6 0.3622(4) 0.2178(2) 0.5190(4) 0.0618(9) Uani C . . . C7 0.2063(3) 0.0409(2) 0.6257(3) 0.0421(6) Uani C . . . C8 0.2735(4) -0.0880(2) 0.8048(3) 0.0577(8) Uani C . . . C9 0.3355(3) -0.1867(2) 0.8104(3) 0.0507(7) Uani C . . . C10 0.2637(4) -0.2506(2) 0.6866(3) 0.0555(7) Uani C . . . C11 0.3070(4) -0.3459(3) 0.6994(4) 0.0708(10) Uani C . . . C12 0.4286(5) -0.3762(3) 0.8363(4) 0.0839(11) Uani C . . . C13 0.5048(5) -0.3152(3) 0.9561(5) 0.0954(13) Uani C . . . C14 0.4570(5) -0.2199(3) 0.9462(4) 0.0811(12) Uani C . . . H21 -0.3878(34) 0.0016(33) -0.4168(38) 0.0632(78) Uiso H . . . H22 -0.3882(37) -0.0283(35) -0.2589(39) 0.074(11) Uiso H . . . H23 -0.2280(43) -0.0479(28) -0.3201(40) 0.0638(87) Uiso H . . . H31 0.1480(38) 0.2512(29) -0.0161(38) 0.0540(73) Uiso H . . . H32 -0.0754(46) 0.2728(32) -0.0882(46) 0.077(11) Uiso H . . . H33 0.0181(43) 0.2227(31) -0.1759(40) 0.0726(99) Uiso H . . . H5 0.1043(26) 0.2046(18) 0.5053(26) 0.0278(49) Uiso H . . . H61 0.4080(38) 0.2025(25) 0.6295(36) 0.0531(74) Uiso H . . . H62 0.4375(38) 0.1905(27) 0.4576(39) 0.0600(82) Uiso H . . . H63 0.3604(45) 0.2898(30) 0.5062(46) 0.077(11) Uiso H . . . H81 0.3517(34) -0.0469(24) 0.8865(35) 0.0503(74) Uiso H . . . H82 0.1645(38) -0.0830(30) 0.8143(39) 0.0609(83) Uiso H . . . H10 0.1813(32) -0.2268(23) 0.5906(34) 0.0426(65) Uiso H . . . H11 0.2559(63) -0.3953(41) 0.6117(64) 0.109(13) Uiso H . . . H12 0.4656(50) -0.4310(39) 0.8456(51) 0.101(14) Uiso H . . . H13 0.5770(40) -0.3234(32) 1.0360(43) 0.0730(96) Uiso H . . . H14 0.5114(45) -0.1886(27) 1.0188(45) 0.0621(82) 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 0.0395(0) 0.0184(0) 0.0263(0) 0.0032(1) 0.0094(0) 0.0004(0) Cl 0.0550(3) 0.0359(2) 0.0371(2) -0.0094(2) 0.0116(2) 0.0071(2) S1 0.0477(2) 0.0252(2) 0.0331(2) -0.0019(2) 0.0041(2) 0.0020(1) S2 0.0667(4) 0.0403(3) 0.0367(2) 0.0086(3) -0.0045(3) 0.0069(2) O1 0.0499(7) 0.0318(7) 0.0431(6) 0.0102(6) 0.0163(5) -0.0007(6) O2 0.0689(10) 0.0199(6) 0.0438(7) 0.0032(6) 0.0126(7) 0.0005(5) O3 0.0736(10) 0.0419(8) 0.0296(6) 0.0029(8) 0.0138(6) -0.0059(6) O4 0.0495(7) 0.0315(7) 0.0285(5) 0.0026(6) 0.0099(5) 0.0032(5) N1 0.0494(8) 0.0226(6) 0.0293(6) 0.0051(6) 0.0092(5) 0.0043(5) N2 0.0444(7) 0.0197(6) 0.0284(6) 0.0035(6) 0.0088(5) 0.0013(5) N3 0.0470(8) 0.0228(6) 0.0281(6) 0.0019(6) 0.0083(5) -0.0018(5) C1 0.0452(9) 0.0269(8) 0.0295(7) 0.0069(7) 0.0076(6) 0.0022(6) C2 0.0516(11) 0.0585(17) 0.0444(11) -0.0076(13) -0.0052(9) -0.0008(12) C3 0.0753(14) 0.0250(8) 0.0357(8) 0.0020(10) 0.0174(8) 0.0069(7) C4 0.0407(8) 0.0209(7) 0.0366(7) 0.0023(6) 0.0121(6) -0.0006(6) C5 0.0387(8) 0.0234(7) 0.0328(7) 0.0015(7) 0.0075(6) -0.0037(6) C6 0.0451(11) 0.0391(11) 0.0559(13) -0.0049(10) 0.0027(10) 0.0026(11) C7 0.0376(8) 0.0317(8) 0.0284(7) -0.0016(7) 0.0055(6) -0.0025(7) C8 0.0679(13) 0.0396(10) 0.0276(7) -0.0033(11) 0.0100(8) 0.0050(8) C9 0.0416(9) 0.0416(10) 0.0359(8) 0.0013(9) 0.0085(7) 0.0135(8) C10 0.0479(10) 0.0417(11) 0.0423(9) 0.0077(9) 0.0129(8) 0.0081(9) C11 0.0711(13) 0.0448(13) 0.0612(11) 0.0122(11) 0.0340(9) 0.0114(11) C12 0.0792(14) 0.0550(14) 0.0778(13) 0.0282(12) 0.0441(10) 0.0335(11) C13 0.0599(16) 0.0824(17) 0.0757(16) 0.0134(15) 0.0043(14) 0.0497(12) C14 0.0577(14) 0.0711(19) 0.0507(13) -0.0043(15) -0.0073(11) 0.0247(13) # 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 CL 2.3401(8) . . no Tc S1 2.3239(6) . . no Tc O1 1.646(2) . . no Tc N2 1.960(2) . . no Tc N3 1.983(2) . . no S1 C1 1.718(2) . . no S2 C1 1.725(2) . . no S2 C2 1.789(4) . . no O2 C4 1.211(3) . . no O3 C7 1.203(3) . . no O4 C7 1.339(3) . . no O4 C8 1.450(3) . . no N1 N2 1.418(3) . . no N1 C1 1.306(3) . . no N1 C3 1.472(3) . . no N2 C4 1.388(3) . . no N3 C5 1.461(3) . . no N3 C7 1.384(3) . . no C2 H21 0.81(2) . . no C2 H22 0.93(3) . . no C2 H23 0.90(3) . . no C3 H31 1.09(3) . . no C3 H32 0.96(4) . . no C3 H33 0.81(3) . . no C4 C5 1.508(3) . . no C5 C6 1.526(4) . . no C5 H5 0.99(2) . . no C6 H61 0.93(2) . . no C6 H62 0.99(3) . . no C6 H63 1.03(4) . . no C8 C9 1.485(4) . . no C8 H81 1.00(2) . . no C8 H82 0.93(3) . . no C9 C10 1.389(4) . . no C9 C14 1.385(4) . . no C10 C11 1.393(5) . . no C10 H10 0.97(2) . . no C11 C12 1.378(4) . . no C11 H11 1.02(5) . . no C12 C13 1.350(5) . . no C12 H12 0.83(5) . . no C13 C14 1.403(6) . . no C13 H13 0.78(3) . . no C14 H14 0.79(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 Cl Tc S1 80.7(0) . . . no Cl Tc O1 113.8(1) . . . no Cl Tc N2 134.4(1) . . . no Cl Tc N3 90.0(1) . . . no S1 Tc O1 108.8(1) . . . no S1 Tc N2 80.8(1) . . . no S1 Tc N3 142.1(1) . . . no O1 Tc N2 111.6(1) . . . no O1 Tc N3 108.7(1) . . . no N2 Tc N3 79.9(1) . . . no Tc S1 C1 98.0(1) . . . no C1 S2 C2 103.2(1) . . . no C7 O4 C8 113.9(2) . . . no N2 N1 C1 115.9(2) . . . no N2 N1 C3 120.8(2) . . . no C1 N1 C3 122.9(2) . . . no Tc N2 N1 121.2(1) . . . no Tc N2 C4 120.3(2) . . . no N1 N2 C4 116.9(2) . . . no Tc N3 C5 117.5(1) . . . no Tc N3 C7 127.8(2) . . . no C5 N3 C7 113.6(2) . . . no S1 C1 S2 121.8(1) . . . no S1 C1 N1 119.9(2) . . . no S2 C1 N1 118.1(2) . . . no S2 C2 H21 98(3) . . . no S2 C2 H22 104(3) . . . no S2 C2 H23 101(3) . . . no H21 C2 H22 106(3) . . . no H21 C2 H23 125(3) . . . no H22 C2 H23 118(3) . . . no N1 C3 H31 104(2) . . . no N1 C3 H32 106(3) . . . no N1 C3 H33 113(3) . . . no H31 C3 H32 124(3) . . . no H31 C3 H33 107(3) . . . no H32 C3 H33 104(4) . . . no O2 C4 N2 125.7(2) . . . no O2 C4 C5 122.4(2) . . . no N2 C4 C5 111.9(2) . . . no N3 C5 C4 110.0(2) . . . no N3 C5 C6 113.3(2) . . . no N3 C5 H5 111(2) . . . no C4 C5 C6 109.7(2) . . . no C4 C5 H5 101(1) . . . no C6 C5 H5 112(1) . . . no C5 C6 H61 111(2) . . . no C5 C6 H62 109(2) . . . no C5 C6 H63 111(2) . . . no H61 C6 H62 107(3) . . . no H61 C6 H63 109(3) . . . no H62 C6 H63 109(3) . . . no O3 C7 O4 123.0(2) . . . no O3 C7 N3 124.7(2) . . . no O4 C7 N3 111.9(2) . . . no O4 C8 C9 109.3(2) . . . no O4 C8 H81 107(2) . . . no O4 C8 H82 103(2) . . . no C9 C8 H81 112(2) . . . no C9 C8 H82 114(2) . . . no H81 C8 H82 111(3) . . . no C8 C9 C10 121.1(3) . . . no C8 C9 C14 120.8(3) . . . no C10 C9 C14 117.9(3) . . . no C9 C10 C11 121.7(3) . . . no C9 C10 H10 118(2) . . . no C11 C10 H10 121(2) . . . no C10 C11 C12 118.7(3) . . . no C10 C11 H11 124(3) . . . no C12 C11 H11 117(3) . . . no C11 C12 C13 120.9(3) . . . no C11 C12 H12 123(3) . . . no C13 C12 H12 116(3) . . . no C12 C13 C14 120.4(4) . . . no C12 C13 H13 130(3) . . . no C14 C13 H13 109(3) . . . no C9 C14 C13 120.3(3) . . . no C9 C14 H14 126(3) . . . no C13 C14 H14 114(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 Cl Tc S1 C1 153.1(1) . . . . no O1 Tc S1 C1 -94.9(1) . . . . no N2 Tc S1 C1 14.9(1) . . . . no N3 Tc S1 C1 75.1(1) . . . . no Cl Tc N2 N1 -87.1(2) . . . . no Cl Tc N2 C4 77.9(2) . . . . no S1 Tc N2 N1 -19.9(2) . . . . no S1 Tc N2 C4 145.1(2) . . . . no O1 Tc N2 N1 86.8(2) . . . . no O1 Tc N2 C4 -108.3(2) . . . . no N3 Tc N2 N1 -167.0(2) . . . . no N3 Tc N2 C4 -2.1(2) . . . . no Cl Tc N3 C5 -137.2(2) . . . . no Cl Tc N3 C7 30.2(2) . . . . no S1 Tc N3 C5 -62.4(2) . . . . no S1 Tc N3 C7 105.0(2) . . . . no O1 Tc N3 C5 107.6(2) . . . . no O1 Tc N3 C7 -85.0(2) . . . . no N2 Tc N3 C5 -1.9(2) . . . . no N2 Tc N3 C7 165.5(2) . . . . no Tc S1 C1 S2 171.4(1) . . . . no Tc S1 C1 N1 -12.2(2) . . . . no C2 S2 C1 S1 -13.3(2) . . . . no C2 S2 C1 N1 170.3(2) . . . . no C1 S2 C2 H21 173(3) . . . . no C1 S2 C2 H22 64(2) . . . . no C1 S2 C2 H23 -57(2) . . . . no C8 O4 C7 O3 11.4(3) . . . . no C8 O4 C7 N3 -174.5(2) . . . . no C7 O4 C8 C9 179.5(2) . . . . no C7 O4 C8 H81 -58(2) . . . . no C7 O4 C8 H82 58(2) . . . . no C1 N1 N2 Tc 17.7(3) . . . . no C1 N1 N2 C4 -147.7(2) . . . . no C3 N1 N2 Tc -155.3(2) . . . . no C3 N1 N2 C4 39.3(3) . . . . no N2 N1 C1 S1 -0.5(3) . . . . no N2 N1 C1 S2 176.0(2) . . . . no C3 N1 C1 S1 172.4(2) . . . . no C3 N1 C1 S2 -11.1(3) . . . . no N2 N1 C3 H31 24(2) . . . . no N2 N1 C3 H32 -106(3) . . . . no N2 N1 C3 H33 140(3) . . . . no C1 N1 C3 H31 -147(2) . . . . no C1 N1 C3 H32 80(3) . . . . no C1 N1 C3 H33 -32(3) . . . . no Tc N2 C4 O2 -173.2(2) . . . . no Tc N2 C4 C5 5.3(3) . . . . no N1 N2 C4 O2 -7.7(3) . . . . no N1 N2 C4 C5 170.9(2) . . . . no Tc N3 C5 C4 4.9(2) . . . . no Tc N3 C5 C6 -118.3(2) . . . . no Tc N3 C5 H5 115(1) . . . . no C7 N3 C5 C4 -164.2(2) . . . . no C7 N3 C5 C6 72.6(3) . . . . no C7 N3 C5 H5 -53(1) . . . . no Tc N3 C7 O3 -151.4(2) . . . . no Tc N3 C7 O4 34.6(3) . . . . no C5 N3 C7 O3 16.3(3) . . . . no C5 N3 C7 O4 -157.6(2) . . . . no O2 C4 C5 N3 172.4(2) . . . . no O2 C4 C5 C6 -62.4(3) . . . . no O2 C4 C5 H5 56(1) . . . . no N2 C4 C5 N3 -6.2(3) . . . . no N2 C4 C5 C6 119.1(2) . . . . no N2 C4 C5 H5 -122(1) . . . . no N3 C5 C6 H61 -58(2) . . . . no N3 C5 C6 H62 58(2) . . . . no N3 C5 C6 H63 179(2) . . . . no C4 C5 C6 H61 177(2) . . . . no C4 C5 C6 H62 -64(2) . . . . no C4 C5 C6 H63 56(2) . . . . no H5 C5 C6 H61 67(3) . . . . no H5 C5 C6 H62 -175(3) . . . . no H5 C5 C6 H63 -54(3) . . . . no O4 C8 C9 C10 -49.2(3) . . . . no O4 C8 C9 C14 136.3(3) . . . . no H81 C8 C9 C10 -166(2) . . . . no H81 C8 C9 C14 18(2) . . . . no H82 C8 C9 C10 66(2) . . . . no H82 C8 C9 C14 -108(2) . . . . no C8 C9 C10 C11 -172.5(3) . . . . no C8 C9 C10 H10 7(2) . . . . no C14 C9 C10 C11 2.2(5) . . . . no C14 C9 C10 H10 -177(2) . . . . no C8 C9 C14 C13 174.8(3) . . . . no C8 C9 C14 H14 -11(3) . . . . no C10 C9 C14 C13 0.2(5) . . . . no C10 C9 C14 H14 174(3) . . . . no C9 C10 C11 C12 -2.3(5) . . . . no C9 C10 C11 H11 179(4) . . . . no H10 C10 C11 C12 178(2) . . . . no H10 C10 C11 H11 0(4) . . . . no C10 C11 C12 C13 -0.1(5) . . . . no C10 C11 C12 H12 -173(4) . . . . no H11 C11 C12 C13 179(3) . . . . no H11 C11 C12 H12 5(5) . . . . no C11 C12 C13 C14 2.4(6) . . . . no C11 C12 C13 H13 -176(4) . . . . no H12 C12 C13 C14 177(4) . . . . no H12 C12 C13 H13 -2(5) . . . . no C12 C13 C14 C9 -2.5(6) . . . . no C12 C13 C14 H14 -176(3) . . . . no H13 C13 C14 C9 177(3) . . . . no H13 C13 C14 H14 3(4) . . . . no # CHEMICAL DATA _chemical_name_systematic ; ..... ; _chemical_formula_analytical 'Tc1 Cl1 S2 O4 N3 C14 H17' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'Tc1 Cl1 S2 O4 N3 C14 H17 ' _chemical_formula_weight 489.79 _chemical_melting_point ? _chemical_compound_source ; ...... ; # CRYSTAL DATA _cell_length_a 8.238(1) _cell_length_b 14.169(1) _cell_length_c 8.427(1) _cell_angle_alpha 90.00(0) _cell_angle_beta 105.54(1) _cell_angle_gamma 90.00(0) _cell_volume 947.7(2) _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 10 _cell_measurement_theta_max 13 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M ' P21 ' _symmetry_Int_Tables_number 4 _exptl_crystal_description ; ...... ; _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.7164 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 492.0 _exptl_absorpt_coefficient_mu 1.1444 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.9524 _exptl_absorpt_correction_T_max 0.9973 # 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 3026 _reflns_number_gt 2688 _reflns_threshold_expression '>3sigma(I)' _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_number 2857 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 30 _diffrn_reflns_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 'isotropic' _refine_ls_structure_factor_coef 'F' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme 'calc w= 4F^2^/(\s^2^(I) + (0.02F^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 2688 _refine_ls_number_parameters 293 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.017 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.021 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.331 _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 0.34 _refine_diff_density_min -0.24 _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 3.50 Angstrom. # # lab1 lab2 distance Tc O4 3.226(2) Tc N1 2.955(2) Tc C1 3.076(2) Tc C4 2.918(2) Tc C5 2.957(2) Tc C7 3.035(2) Cl S1 3.021(1) Cl O1 3.360(2) Cl O4 2.997(2) Cl N3 3.068(2) Cl C7 3.204(2) Cl H10 2.871(28) S1 S2 3.009(1) S1 O1 3.251(2) S1 N1 2.625(2) S1 N2 2.790(2) S1 C2 3.076(3) S1 H22 2.822(28) S1 H23 2.902(33) S2 N1 2.608(2) S2 C3 2.944(3) S2 H21 2.064(37) S2 H22 2.206(45) S2 H23 2.150(40) S2 H32 2.991(42) S2 H33 2.681(38) O1 N2 2.988(3) O1 N3 2.955(3) O2 N1 2.755(3) O2 N2 2.314(3) O2 C3 2.700(3) O2 C5 2.387(3) O2 C6 2.981(3) O2 H31 2.376(35) O2 H32 2.716(35) O2 H33 3.495(34) O2 H5 2.517(23) O2 H62 3.290(30) O2 H63 2.737(33) O3 O4 2.236(3) O3 N3 2.294(3) O3 C5 2.697(3) O3 C6 3.187(4) O3 C8 2.613(4) O3 H5 2.519(23) O3 H61 2.740(35) O3 H81 2.467(31) O3 H82 2.538(41) O4 N3 2.257(3) O4 C9 2.394(3) O4 C10 2.890(4) O4 H81 1.980(28) O4 H82 1.893(37) O4 H10 2.625(32) N1 C4 2.392(3) N1 H31 2.027(38) N1 H32 1.963(43) N1 H33 1.941(39) N2 N3 2.533(3) N2 C1 2.309(3) N2 C3 2.514(3) N2 C5 2.401(3) N2 C6 3.461(3) N2 H31 2.508(38) N2 H32 3.009(40) N2 H33 3.125(36) N2 H5 2.971(23) N2 H62 3.392(28) N3 C4 2.433(3) N3 C6 2.495(4) N3 H5 2.030(26) N3 H61 2.705(31) N3 H62 2.690(35) N3 H63 3.378(41) C1 C2 2.755(4) C1 C3 2.441(4) C1 C4 3.496(3) C1 H21 3.379(30) C1 H22 2.848(35) C1 H23 2.753(35) C1 H31 3.199(37) C1 H32 2.769(45) C1 H33 2.576(42) C3 C4 2.925(3) C4 C6 2.481(3) C4 H31 2.638(34) C4 H32 3.196(36) C4 H5 1.948(23) C4 H61 3.296(26) C4 H62 2.705(28) C4 H63 2.682(35) C5 C7 2.381(3) C5 H61 2.056(27) C5 H62 2.070(32) C5 H63 2.126(40) C6 C7 3.060(4) C6 H5 2.105(22) C7 C8 2.339(4) C7 H5 2.581(25) C7 H61 2.825(35) C7 H62 3.402(37) C7 H81 2.530(29) C7 H82 2.452(39) C8 C10 2.502(4) C8 C14 2.496(5) C8 H10 2.639(30) C8 H14 2.689(34) C9 C11 2.430(5) C9 C12 2.785(5) C9 C13 2.418(5) C9 H81 2.075(34) C9 H82 2.042(38) C9 H10 2.027(25) C9 H11 3.374(57) C9 H13 3.049(37) C9 H14 1.955(33) C10 C12 2.384(5) C10 C13 2.743(4) C10 C14 2.376(4) C10 H81 3.323(33) C10 H82 2.818(40) C10 H11 2.141(58) C10 H12 3.146(50) C10 H14 3.117(33) C11 C13 2.374(5) C11 C14 2.768(5) C11 H10 2.062(30) C11 H12 1.953(44) C11 H13 3.117(31) C12 C14 2.388(6) C12 H10 3.265(28) C12 H11 2.058(47) C12 H13 1.946(33) C12 H14 3.056(38) C13 H11 3.275(48) C13 H12 1.872(52) C13 H14 1.867(39) C14 H81 2.604(34) C14 H82 3.061(35) C14 H10 3.241(24) C14 H12 3.115(55) C14 H13 1.817(41) H21 H22 1.397(49) H21 H23 1.521(46) H22 H23 1.564(52) H31 H32 1.803(47) H31 H33 1.533(42) H32 H33 1.396(59) H5 H61 2.440(35) H5 H62 2.886(40) H5 H63 2.429(46) H61 H62 1.541(48) H61 H63 1.595(52) H62 H63 1.641(57) H81 H82 1.583(41) H81 H14 2.494(48) H82 H10 2.805(50) H82 H14 3.277(46) H10 H11 2.460(66) H11 H12 2.302(60) H12 H13 2.225(61) H13 H14 1.980(59) loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' #=END data_(II) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Tc P S2 O3 N4 C34 H36' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Tc P S2 O3 N4 C34 H36' _chemical_formula_weight 741.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Tc' 'Tc' -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.0400(10) _cell_length_b 14.2840(10) _cell_length_c 24.256(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3478.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description ? _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method ? _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type 'psi-scan method' _exptl_absorpt_correction_T_min 0.9834 _exptl_absorpt_correction_T_max 0.9985 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4659 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 28 _reflns_number_total 4659 _reflns_number_observed 3665 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Enraf-Nonius, 1984' _computing_cell_refinement 'CAD4 Enraf-Nonius, 1984' _computing_data_reduction 'MolEN, Enraf-Nonius, 1990' _computing_structure_solution 'MolEN, Enraf-Nonius, 1990'' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP II, Johnson, 1976' _computing_publication_material 'PARST, Nardelli, 1985' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+6.2133P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(9) _refine_ls_number_reflns 4659 _refine_ls_number_parameters 287 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_obs 0.0643 _refine_ls_wR_factor_all 0.1931 _refine_ls_wR_factor_obs 0.1805 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.177 _refine_ls_restrained_S_all 1.112 _refine_ls_restrained_S_obs 1.180 _refine_ls_shift/esd_max 0.05 _refine_ls_shift/esd_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tc1 Tc -0.15790(7) 0.11487(5) 0.35598(3) 0.0568(2) Uani 1 d . . P1 P -0.3196(2) 0.03740(15) 0.29650(10) 0.0556(5) Uani 1 d . . S1 S -0.2121(3) 0.2619(2) 0.31556(13) 0.0794(8) Uani 1 d . . S2 S -0.0936(6) 0.4491(2) 0.3477(2) 0.137(2) Uani 1 d . . O1 O -0.1725(11) 0.2446(7) 0.5053(4) 0.118(3) Uani 1 d . . O2 O -0.3027(9) -0.0884(5) 0.3872(3) 0.085(2) Uani 1 d . . N1 N -0.0279(9) 0.0737(6) 0.3246(4) 0.075(2) Uani 1 d . . N2 N -0.0767(11) 0.2984(6) 0.4064(4) 0.082(3) Uani 1 d . . N3 N -0.1014(9) 0.2037(6) 0.4178(3) 0.071(2) Uani 1 d . . N4 N -0.2062(9) 0.0405(6) 0.4256(3) 0.067(2) Uani 1 d . . C1 C -0.1250(12) 0.3310(7) 0.3608(5) 0.087(3) Uani 1 d . . C2 C -0.1691(5) 0.4664(3) 0.2806(2) 0.148(7) Uani 1 d . . H2A H -0.1573(5) 0.5303(3) 0.2694(2) 0.150 Uiso 1 calc R . H2B H -0.2625(5) 0.4524(3) 0.2826(2) 0.150 Uiso 1 calc R . H2C H -0.1274(5) 0.4257(3) 0.2542(2) 0.150 Uiso 1 calc R . C3 C 0.0228(5) 0.3464(3) 0.4425(2) 0.115(5) Uani 1 d R . H3A H 0.0419(5) 0.3077(3) 0.4738(2) 0.130 Uiso 1 calc R . H3B H -0.0129(5) 0.4052(3) 0.4547(2) 0.130 Uiso 1 calc R . H3C H 0.1032(5) 0.3571(3) 0.4220(2) 0.130 Uiso 1 calc R . C4 C -0.1503(5) 0.1867(3) 0.4687(2) 0.078(3) Uani 1 d R . C5 C -0.1742(5) 0.0825(3) 0.4805(2) 0.079(3) Uani 1 d R . H5 H -0.2440(5) 0.0718(3) 0.5080(2) 0.100 Uiso 1 calc R 1 C6 C -0.0214(5) 0.0444(3) 0.5016(2) 0.100(8) Uiso 0.50 d PRD 1 H6 H 0.0477(5) 0.0622(3) 0.4751(2) 0.140 Uiso 0.50 calc PR 1 C7 C -0.0068(5) 0.0992(3) 0.5551(2) 0.153(14) Uiso 0.50 d PRD 1 H7A H 0.0037(5) 0.1645(3) 0.5468(2) 0.200 Uiso 0.50 calc PR 1 H7B H 0.0701(5) 0.0772(3) 0.5748(2) 0.200 Uiso 0.50 calc PR 1 H7C H -0.0848(5) 0.0904(3) 0.5773(2) 0.200 Uiso 0.50 calc PR 1 C8 C -0.0393(5) -0.0600(3) 0.5029(2) 0.240(28) Uiso 0.50 d PRD 1 H8A H -0.0469(5) -0.0833(3) 0.4659(2) 0.220 Uiso 0.50 calc PR 1 H8B H -0.1186(5) -0.0751(3) 0.5231(2) 0.220 Uiso 0.50 calc PR 1 H8C H 0.0362(5) -0.0883(3) 0.5206(2) 0.220 Uiso 0.50 calc PR 1 C6' C -0.0636(5) 0.0367(3) 0.5090(2) 0.077(6) Uiso 0.50 d PRD 2 H6' H -0.0654(5) -0.0295(3) 0.4984(2) 0.150 Uiso 0.50 calc PR 2 C7' C -0.0658(5) 0.0402(3) 0.5741(2) 0.138(12) Uiso 0.50 d PRD 2 H7A' H 0.0109(5) 0.0082(3) 0.5883(2) 0.130 Uiso 0.50 calc PR 2 H7B' H -0.1452(5) 0.0104(3) 0.5874(2) 0.130 Uiso 0.50 calc PR 2 H7C' H -0.0644(5) 0.1043(3) 0.5861(2) 0.130 Uiso 0.50 calc PR 2 C8' C 0.0825(5) 0.0803(3) 0.4877(2) 0.190(19) Uiso 0.50 d PRD 2 H8A' H 0.1538(5) 0.0494(3) 0.5068(2) 0.180 Uiso 0.50 calc PR 2 H8B' H 0.0856(5) 0.1462(3) 0.4953(2) 0.180 Uiso 0.50 calc PR 2 H8C' H 0.0918(5) 0.0702(3) 0.4488(2) 0.180 Uiso 0.50 calc PR 2 C9 C -0.2795(5) -0.0402(3) 0.4257(2) 0.088(3) Uani 1 d R . O3 O -0.2843(5) -0.0790(3) 0.4825(2) 0.087(4) Uiso 0.50 d PRD 1 C10 C -0.3560(5) -0.1735(3) 0.4822(2) 0.101(8) Uiso 0.50 d PRD 1 H10A H -0.3016(5) -0.2215(3) 0.4994(2) 0.120 Uiso 0.50 calc PR 1 H10B H -0.3774(5) -0.1927(3) 0.4449(2) 0.120 Uiso 0.50 calc PR 1 C11 C -0.4845(14) -0.1557(13) 0.5162(7) 0.058(5) Uiso 0.50 d PGD 1 C12 C -0.5164(18) -0.2107(13) 0.5616(7) 0.112(9) Uiso 0.50 d PGD 1 H12 H -0.4584(25) -0.2575(18) 0.5730(11) 0.140 Uiso 0.50 calc PR 1 C13 C -0.6350(22) -0.1956(19) 0.5898(8) 0.146(15) Uiso 0.50 d PGD 1 H13 H -0.6563(32) -0.2324(25) 0.6201(11) 0.170 Uiso 0.50 calc PR 1 C14 C -0.7217(18) -0.1256(20) 0.5726(10) 0.127(10) Uiso 0.50 d PGD 1 H14 H -0.8011(22) -0.1156(28) 0.5915(14) 0.170 Uiso 0.50 calc PR 1 C15 C -0.6899(21) -0.0706(16) 0.5272(11) 0.171(17) Uiso 0.50 d PGD 1 H15 H -0.7479(29) -0.0238(21) 0.5157(15) 0.170 Uiso 0.50 calc PR 1 C16 C -0.5713(22) -0.0857(14) 0.4990(8) 0.186(20) Uiso 0.50 d PGD 1 H16 H -0.5499(32) -0.0489(20) 0.4686(11) 0.210 Uiso 0.50 calc PR 1 O3' O -0.3614(19) -0.0486(12) 0.4709(7) 0.101(5) Uiso 0.50 d PD 2 C10' C -0.4320(41) -0.1416(22) 0.4564(12) 0.177(17) Uiso 0.50 d PD 2 H10C H -0.5076(41) -0.1310(22) 0.4323(12) 0.200 Uiso 0.50 calc PR 2 H10D H -0.3712(41) -0.1851(22) 0.4389(12) 0.200 Uiso 0.50 calc PR 2 C11' C -0.4764(27) -0.1770(17) 0.5121(9) 0.143(18) Uiso 0.50 d PGD 2 C12' C -0.5838(30) -0.1301(17) 0.5353(13) 0.176(17) Uiso 0.50 d PGD 2 H12' H -0.6144(42) -0.0747(20) 0.5196(18) 0.140 Uiso 0.50 calc PR 2 C13' C -0.6455(29) -0.1658(25) 0.5821(13) 0.225(29) Uiso 0.50 d PGD 2 H13' H -0.7174(37) -0.1344(33) 0.5977(18) 0.260 Uiso 0.50 calc PR 2 C14' C -0.5997(33) -0.2485(25) 0.6056(10) 0.182(19) Uiso 0.50 d PGD 2 H14' H -0.6410(45) -0.2724(34) 0.6370(13) 0.180 Uiso 0.50 calc PR 2 C15' C -0.4923(31) -0.2954(18) 0.5824(10) 0.161(15) Uiso 0.50 d PGD 2 H15' H -0.4616(44) -0.3508(21) 0.5981(15) 0.170 Uiso 0.50 calc PR 2 C16' C -0.4306(24) -0.2597(17) 0.5356(11) 0.147(13) Uiso 0.50 d PGD 2 H16' H -0.3587(31) -0.2912(24) 0.5200(16) 0.160 Uiso 0.50 calc PR 2 C17 C -0.3540(11) 0.1066(6) 0.2343(4) 0.068(2) Uani 1 d . . C18 C -0.2517(3) 0.1150(2) 0.19624(12) 0.090(3) Uani 1 d . . H18 H -0.1684(3) 0.0892(2) 0.20337(12) 0.110 Uiso 1 calc R . C19 C -0.2760(3) 0.1633(2) 0.14651(12) 0.131(6) Uani 1 d R . H19 H -0.2089(3) 0.1677(2) 0.12022(12) 0.150 Uiso 1 calc R . C20 C -0.3961(3) 0.2034(2) 0.13654(12) 0.121(6) Uani 1 d R . H20 H -0.4100(3) 0.2339(2) 0.10314(12) 0.150 Uiso 1 calc R . C21 C -0.4977(3) 0.2003(2) 0.17432(12) 0.105(4) Uani 1 d R . H21 H -0.5775(3) 0.2314(2) 0.16748(12) 0.140 Uiso 1 calc R . C22 C -0.4794(3) 0.1480(2) 0.22516(12) 0.078(3) Uani 1 d R . H22 H -0.5479(3) 0.1421(2) 0.25071(12) 0.090 Uiso 1 calc R . C23 C -0.4795(3) 0.0250(2) 0.32892(12) 0.061(2) Uani 1 d R . C24 C -0.5659(3) -0.0503(2) 0.31835(12) 0.082(3) Uani 1 d R . H24 H -0.5399(3) -0.0981(2) 0.29461(12) 0.100 Uiso 1 calc R . C25 C -0.6926(3) -0.0533(2) 0.34395(12) 0.103(4) Uani 1 d R . H25 H -0.7504(3) -0.1027(2) 0.33673(12) 0.120 Uiso 1 calc R . C26 C -0.7311(3) 0.0193(2) 0.38072(12) 0.106(5) Uani 1 d R . H26 H -0.8142(3) 0.0170(2) 0.39766(12) 0.120 Uiso 1 calc R . C27 C -0.6459(3) 0.0939(2) 0.39162(12) 0.087(4) Uani 1 d R . H27 H -0.6709(3) 0.1406(2) 0.41626(12) 0.100 Uiso 1 calc R . C28 C -0.5212(3) 0.0979(2) 0.36492(12) 0.070(3) Uani 1 d R . H28 H -0.4656(3) 0.1489(2) 0.37094(12) 0.085 Uiso 1 calc R . C29 C -0.2751(3) -0.0731(2) 0.26379(12) 0.063(2) Uani 1 d R . C30 C -0.3483(3) -0.1049(2) 0.21948(12) 0.076(3) Uani 1 d R . H30 H -0.4226(3) -0.0714(2) 0.20786(12) 0.092 Uiso 1 calc R . C31 C -0.3117(3) -0.1882(2) 0.19139(12) 0.085(3) Uani 1 d R . H31 H -0.3610(3) -0.2097(2) 0.16148(12) 0.100 Uiso 1 calc R . C32 C -0.2004(3) -0.2370(2) 0.20969(12) 0.096(4) Uani 1 d R . H32 H -0.1749(3) -0.2912(2) 0.19128(12) 0.115 Uiso 1 calc R . C33 C -0.1278(3) -0.2077(2) 0.25368(12) 0.095(4) Uani 1 d R . H33 H -0.0545(3) -0.2423(2) 0.26522(12) 0.110 Uiso 1 calc R . C34 C -0.1642(3) -0.1230(2) 0.28267(12) 0.079(3) Uani 1 d R . H34 H -0.1153(3) -0.1023(2) 0.31290(12) 0.094 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tc1 0.0541(3) 0.0524(3) 0.0638(4) -0.0085(3) -0.0091(4) -0.0005(4) P1 0.0565(13) 0.0439(10) 0.0664(12) -0.0062(9) -0.0083(11) 0.0029(10) S1 0.090(2) 0.0552(13) 0.093(2) -0.0015(13) -0.026(2) -0.0093(13) S2 0.192(5) 0.061(2) 0.158(4) -0.001(2) -0.049(4) -0.037(2) O1 0.133(8) 0.097(5) 0.126(6) -0.063(5) 0.030(7) -0.008(6) O2 0.120(7) 0.052(4) 0.082(4) 0.000(3) -0.032(5) -0.006(4) N1 0.064(5) 0.078(5) 0.083(6) -0.017(5) -0.005(4) 0.001(4) N2 0.102(7) 0.058(5) 0.086(6) -0.010(4) -0.030(6) -0.012(5) N3 0.079(5) 0.060(4) 0.076(5) -0.014(4) -0.016(5) -0.005(4) N4 0.073(5) 0.064(5) 0.065(4) -0.007(4) -0.003(4) -0.004(4) C1 0.099(8) 0.055(5) 0.107(8) -0.009(6) -0.026(8) -0.016(5) C2 0.167(16) 0.072(8) 0.204(17) 0.033(10) -0.029(17) -0.018(11) C3 0.145(13) 0.086(8) 0.113(10) -0.025(7) -0.032(10) -0.044(9) C4 0.082(7) 0.073(6) 0.081(6) -0.026(5) 0.009(6) 0.001(6) C5 0.079(7) 0.082(6) 0.077(6) -0.032(5) 0.014(6) -0.012(6) C9 0.112(9) 0.073(7) 0.079(7) 0.003(6) -0.002(7) -0.010(7) C17 0.082(6) 0.052(4) 0.072(5) -0.007(4) -0.017(5) 0.000(5) C18 0.095(8) 0.089(8) 0.085(7) 0.019(7) 0.005(6) -0.004(8) C19 0.170(16) 0.120(12) 0.104(10) 0.034(10) 0.023(12) -0.029(12) C20 0.174(16) 0.092(9) 0.099(10) 0.018(8) -0.049(11) -0.011(10) C21 0.127(12) 0.086(8) 0.104(10) 0.007(8) -0.027(9) 0.025(9) C22 0.093(7) 0.062(6) 0.079(6) -0.001(5) -0.019(6) 0.012(6) C23 0.062(5) 0.059(5) 0.063(5) 0.005(4) -0.007(4) 0.001(4) C24 0.067(6) 0.074(7) 0.106(8) 0.006(6) -0.002(6) -0.013(5) C25 0.089(9) 0.111(10) 0.108(10) 0.015(8) 0.003(8) -0.022(8) C26 0.074(7) 0.141(13) 0.102(9) 0.045(9) 0.001(7) -0.009(9) C27 0.102(8) 0.108(9) 0.050(5) 0.014(5) 0.011(6) 0.038(8) C28 0.074(6) 0.073(6) 0.063(6) -0.005(5) 0.004(5) 0.007(5) C29 0.065(5) 0.045(4) 0.077(6) -0.006(4) -0.003(5) 0.003(4) C30 0.085(6) 0.055(5) 0.090(6) -0.022(5) -0.003(6) -0.007(6) C31 0.105(9) 0.063(6) 0.086(7) -0.019(5) -0.006(7) -0.015(6) C32 0.120(10) 0.060(6) 0.108(9) -0.024(6) 0.022(8) 0.004(7) C33 0.098(9) 0.057(6) 0.128(10) -0.009(6) -0.009(8) 0.020(6) C34 0.084(6) 0.064(5) 0.088(6) -0.012(5) -0.016(6) 0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tc1 N1 1.621(9) . ? Tc1 N3 2.044(8) . ? Tc1 N4 2.054(8) . ? Tc1 S1 2.381(3) . ? Tc1 P1 2.437(2) . ? P1 C23 1.796(4) . ? P1 C29 1.822(4) . ? P1 C17 1.836(9) . ? S1 C1 1.716(11) . ? S2 C1 1.746(11) . ? S2 C2 1.811(7) . ? O1 C4 1.235(9) . ? O2 C9 1.184(8) . ? N2 C1 1.294(14) . ? N2 N3 1.403(12) . ? N2 C3 1.494(10) . ? N3 C4 1.352(10) . ? N4 C9 1.368(9) . ? N4 C5 1.495(9) . ? C4 C5 1.53 . ? C5 C6' 1.46 . ? C5 C6 1.71 . ? C6 C8 1.50 . ? C6 C7 1.52 . ? C6' C7' 1.58 . ? C6' C8' 1.68 . ? C9 O3' 1.37(2) . ? C9 O3 1.49 . ? O3 C10 1.53 . ? C10 C11 1.552(14) . ? C11 C12 1.39 . ? C11 C16 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? O3' C10' 1.54(3) . ? C10' C11' 1.51(2) . ? C11' C12' 1.39 . ? C11' C16' 1.39 . ? C12' C13' 1.39 . ? C13' C14' 1.39 . ? C14' C15' 1.39 . ? C15' C16' 1.39 . ? C17 C18 1.386(11) . ? C17 C22 1.409(11) . ? C18 C19 1.41 . ? C19 C20 1.36 . ? C20 C21 1.37 . ? C21 C22 1.45 . ? C23 C24 1.41 . ? C23 C28 1.42 . ? C24 C25 1.42 . ? C25 C26 1.42 . ? C26 C27 1.39 . ? C27 C28 1.41 . ? C29 C30 1.38 . ? C29 C34 1.40 . ? C30 C31 1.42 . ? C31 C32 1.39 . ? C32 C33 1.36 . ? C33 C34 1.45 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Tc1 N3 110.2(4) . . ? N1 Tc1 N4 112.9(4) . . ? N3 Tc1 N4 77.5(3) . . ? N1 Tc1 S1 108.1(4) . . ? N3 Tc1 S1 79.5(3) . . ? N4 Tc1 S1 137.8(3) . . ? N1 Tc1 P1 95.4(3) . . ? N3 Tc1 P1 154.2(3) . . ? N4 Tc1 P1 95.4(2) . . ? S1 Tc1 P1 90.25(9) . . ? C23 P1 C29 109.0(2) . . ? C23 P1 C17 104.2(4) . . ? C29 P1 C17 98.9(3) . . ? C23 P1 Tc1 112.38(14) . . ? C29 P1 Tc1 119.17(15) . . ? C17 P1 Tc1 111.6(3) . . ? C1 S1 Tc1 97.3(4) . . ? C1 S2 C2 102.7(5) . . ? C1 N2 N3 116.6(8) . . ? C1 N2 C3 125.9(8) . . ? N3 N2 C3 116.5(8) . . ? C4 N3 N2 114.7(7) . . ? C4 N3 Tc1 117.2(5) . . ? N2 N3 Tc1 120.3(7) . . ? C9 N4 C5 116.9(6) . . ? C9 N4 Tc1 124.3(5) . . ? C5 N4 Tc1 118.3(5) . . ? N2 C1 S1 122.1(8) . . ? N2 C1 S2 115.8(8) . . ? S1 C1 S2 122.1(8) . . ? O1 C4 N3 127.0(7) . . ? O1 C4 C5 119.2(6) . . ? N3 C4 C5 113.7(4) . . ? C6' C5 N4 113.9(4) . . ? C6' C5 C4 113.8 . . ? N4 C5 C4 104.9(4) . . ? N4 C5 C6 109.4(4) . . ? C4 C5 C6 103.0 . . ? C8 C6 C7 120.3 . . ? C8 C6 C5 102.5 . . ? C7 C6 C5 100.3 . . ? C5 C6' C7' 116.6 . . ? C5 C6' C8' 110.6 . . ? C7' C6' C8' 108.0 . . ? O2 C9 N4 126.5(6) . . ? O2 C9 O3' 117.4(9) . . ? N4 C9 O3' 113.4(9) . . ? O2 C9 O3 120.6(4) . . ? N4 C9 O3 109.4(4) . . ? C9 O3 C10 109.9 . . ? O3 C10 C11 104.1(7) . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 121.2(12) . . ? C16 C11 C10 118.7(12) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C9 O3' C10' 99.7(16) . . ? C11' C10' O3' 102.8(19) . . ? C12' C11' C16' 120.0 . . ? C12' C11' C10' 115.5(18) . . ? C16' C11' C10' 123.7(18) . . ? C11' C12' C13' 120.0 . . ? C14' C13' C12' 120.0 . . ? C15' C14' C13' 120.0 . . ? C14' C15' C16' 120.0 . . ? C15' C16' C11' 120.0 . . ? C18 C17 C22 121.4(7) . . ? C18 C17 P1 117.0(6) . . ? C22 C17 P1 121.6(7) . . ? C17 C18 C19 118.9(4) . . ? C20 C19 C18 120.9 . . ? C19 C20 C21 121.9 . . ? C20 C21 C22 119.3 . . ? C17 C22 C21 117.6(4) . . ? C24 C23 C28 119.4 . . ? C24 C23 P1 123.14(11) . . ? C28 C23 P1 117.40(11) . . ? C23 C24 C25 119.8 . . ? C24 C25 C26 119.8 . . ? C27 C26 C25 120.7 . . ? C26 C27 C28 119.3 . . ? C27 C28 C23 120.9 . . ? C30 C29 C34 120.7 . . ? C30 C29 P1 119.60(12) . . ? C34 C29 P1 119.61(12) . . ? C29 C30 C31 120.8 . . ? C32 C31 C30 118.4 . . ? C33 C32 C31 121.9 . . ? C32 C33 C34 120.2 . . ? C29 C34 C33 117.9 . . ? _refine_diff_density_max 0.662 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.085