Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005# data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Eric Benoist' _publ_contact_author_address ; Laboratoire de Chimie Inorganique Universite Paul Sabatier EA 807 Bat. IIR1 118, route de narbonne Toulouse 31062 FRANCE ; _publ_contact_author_email benoist@chimie.ups-tlse.fr _publ_contact_author_phone ' 0561556104' _publ_contact_author_fax ' 0561556118' loop_ _publ_author_name _publ_author_address E.Benoist ;Laboratoire de chimie inorganique Universite Paul Sabatier 118 route de Narbonne 31062 TOULOUSE cedex3 FRANCE ; 'J.Le Gal' ;Laboratoire de chimie inorganique Universite Paul Sabatier 118 route de Narbonne 31062 TOULOUSE cedex3 FRANCE ; M.Gressier ;Laboratoire de chimie inorganique Universite Paul Sabatier 118 route de Narbonne 31062 TOULOUSE cedex3 FRANCE ; M.Dartiguenave ;Laboratoire de chimie inorganique Universite Paul Sabatier 118 route de Narbonne 31062 TOULOUSE cedex3 FRANCE ; S.Michaud ;Laboratoire de chimie inorganique Universite Paul Sabatier 118 route de Narbonne 31062 TOULOUSE cedex3 FRANCE ; J.Jaud ;CEMES-CNRS 29 rue Jeanne Marvig BP 94347 31055 TOULOUSE cedex4 FRANCE ; ; Tisato ; Fransceco' '4.3.P.I.ICIS-CNR Corso Stati Uniti' Bandoli, Giuliano' ;Dept Pharmaceutical Sciences University Padova Via Marzolo, 5 35131 Padova ITALY ; _publ_section_title ; Synthesis and structural characterization of new oxorhenium and oxotechnetium complexes with XN2S-tetradentate semi-rigid ligands (X = O, S, N) ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 275918' _audit_creation_method maXus _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All diagrams and calculations were performed using maXus (Bruker Nonius, Delft & MacScience, Japan). ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description Parallelipedic _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_colour Colourless _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz # Submission details _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 777.846 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z '-X+ 1/2,-Y,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,-Z' '-X,+Y+ 1/2,-Z+ 1/2' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_cell_setting Orthorhombic _chemical_formula_moiety 'C34 H28 N2 O4 P Re S ' _chemical_formula_sum 'C34 H28 N2 O4 P Re S ' _chemical_name_systematic ; ? ; _cell_length_a 9.600(4) _cell_length_b 14.588(3) _cell_length_c 21.525(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3015.(2) _diffrn_reflns_number 35340 _diffrn_reflns_theta_max 32.00 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_full 32.00 _diffrn_reflns_av_R_equivalents 0.073 _computing_structure_solution 'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.491 _exptl_absorpt_correction_T_max 0.606 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 4.196 _reflns_number_total 9963 _reflns_number_gt 6195 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(7) _refine_ls_number_reflns 9963 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.61839(3) -0.543403(16) -0.908140(10) 0.04114(9) Uani 1 1 d . . . S1 S -0.6583(2) -0.56432(15) -0.80489(8) 0.0667(5) Uani 1 1 d . . . P1 P -0.32070(16) -0.40179(10) -0.69000(7) 0.0332(3) Uani 1 1 d . . . O1 O -0.9231(6) -0.3700(5) -0.8430(4) 0.104(2) Uani 1 1 d . . . O2 O -0.5934(8) -0.3193(4) -1.0210(3) 0.099(2) Uani 1 1 d . . . O3 O -0.4144(5) -0.5625(3) -0.8941(2) 0.0501(12) Uani 1 1 d . . . O4 O -0.6822(5) -0.6316(3) -0.9490(2) 0.0602(13) Uani 1 1 d . . . N1 N -0.7599(6) -0.4454(4) -0.8988(3) 0.0555(14) Uiso 1 1 d . . . N2 N -0.5370(5) -0.4435(3) -0.9603(2) 0.0425(11) Uiso 1 1 d . . . C1 C -0.8200(9) -0.5046(6) -0.7965(4) 0.078(3) Uani 1 1 d . . . C2 C -0.8402(8) -0.4318(6) -0.8477(4) 0.070(2) Uani 1 1 d . . . C3 C -0.7606(8) -0.3769(5) -0.9473(5) 0.071(2) Uani 1 1 d . . . C4 C -0.6262(9) -0.3752(5) -0.9811(3) 0.0608(18) Uani 1 1 d . . . C5 C -0.3939(7) -0.4493(4) -0.9718(3) 0.0424(13) Uani 1 1 d . . . C6 C -0.3135(8) -0.3979(5) -1.0117(3) 0.0551(18) Uani 1 1 d . . . C7 C -0.1661(10) -0.4158(6) -1.0140(4) 0.078(3) Uani 1 1 d . . . C8 C -0.1098(9) -0.4811(6) -0.9758(4) 0.070(2) Uani 1 1 d . . . C9 C -0.1926(9) -0.5294(5) -0.9352(4) 0.068(2) Uani 1 1 d . . . C10 C -0.3325(7) -0.5147(4) -0.9333(3) 0.0404(14) Uani 1 1 d . . . C11 C -0.2056(7) -0.3377(4) -0.6407(3) 0.0370(14) Uani 1 1 d . . . C12 C -0.1257(8) -0.2663(4) -0.6640(3) 0.0514(15) Uani 1 1 d . . . C13 C -0.0355(9) -0.2220(6) -0.6248(3) 0.064(2) Uani 1 1 d . . . C14 C -0.0248(8) -0.2459(5) -0.5636(4) 0.0555(18) Uani 1 1 d . . . C15 C -0.1045(8) -0.3143(4) -0.5399(3) 0.0485(15) Uani 1 1 d . . . C16 C -0.1971(7) -0.3608(4) -0.5785(3) 0.0471(15) Uani 1 1 d . . . C17 C -0.4823(7) -0.4155(4) -0.6500(3) 0.0407(14) Uani 1 1 d . . . C18 C -0.5549(8) -0.4962(5) -0.6529(3) 0.0528(17) Uani 1 1 d . . . C19 C -0.6833(8) -0.5053(5) -0.6242(4) 0.064(2) Uani 1 1 d . . . C20 C -0.7410(8) -0.4327(6) -0.5935(4) 0.070(2) Uani 1 1 d . . . C21 C -0.6679(7) -0.3504(6) -0.5906(4) 0.065(2) Uani 1 1 d . . . C22 C -0.5400(7) -0.3412(5) -0.6188(3) 0.0536(18) Uani 1 1 d . . . C23 C -0.3482(6) -0.3456(3) -0.7628(2) 0.0333(13) Uani 1 1 d . . . C24 C -0.4762(7) -0.3081(4) -0.7774(3) 0.0496(16) Uani 1 1 d . . . C25 C -0.4924(8) -0.2642(5) -0.8346(3) 0.0569(19) Uani 1 1 d . . . C26 C -0.3868(10) -0.2599(4) -0.8759(3) 0.0561(17) Uani 1 1 d . . . C27 C -0.2601(8) -0.2976(4) -0.8614(3) 0.0487(17) Uani 1 1 d . . . C28 C -0.2414(7) -0.3400(4) -0.8055(3) 0.0418(14) Uani 1 1 d . . . C29 C -0.2429(6) -0.5106(4) -0.7064(3) 0.0365(13) Uani 1 1 d . . . C30 C -0.2887(7) -0.5594(4) -0.7584(3) 0.0453(15) Uani 1 1 d . . . C31 C -0.2397(8) -0.6468(5) -0.7701(4) 0.062(2) Uani 1 1 d . . . C32 C -0.1456(8) -0.6860(4) -0.7290(3) 0.0547(18) Uani 1 1 d . . . C33 C -0.0957(9) -0.6377(5) -0.6774(3) 0.065(2) Uani 1 1 d . . . C34 C -0.1461(7) -0.5484(5) -0.6663(3) 0.0504(15) Uani 1 1 d . . . H1A H -0.8959 -0.5474 -0.7979 0.093 Uiso 1 1 d R . . H1B H -0.8199 -0.4739 -0.7570 0.093 Uiso 1 1 d R . . H3A H -0.8295 -0.3935 -0.9776 0.085 Uiso 1 1 d R . . H3B H -0.7835 -0.3183 -0.9298 0.085 Uiso 1 1 d R . . H6 H -0.3598 -0.3519 -1.0361 0.066 Uiso 1 1 d R . . H7 H -0.1065 -0.3820 -1.0416 0.093 Uiso 1 1 d R . . H8 H -0.0113 -0.4924 -0.9771 0.084 Uiso 1 1 d R . . H9 H -0.1511 -0.5726 -0.9072 0.082 Uiso 1 1 d R . . H12 H -0.1364 -0.2478 -0.7066 0.062 Uiso 1 1 d R . . H13 H 0.0217 -0.1732 -0.6405 0.077 Uiso 1 1 d R . . H14 H 0.0399 -0.2136 -0.5376 0.067 Uiso 1 1 d R . . H15 H -0.1002 -0.3304 -0.4967 0.058 Uiso 1 1 d R . . H16 H -0.2539 -0.4103 -0.5635 0.056 Uiso 1 1 d R . . H18 H -0.5156 -0.5486 -0.6734 0.063 Uiso 1 1 d R . . H19 H -0.7311 -0.5628 -0.6279 0.076 Uiso 1 1 d R . . H20 H -0.8290 -0.4393 -0.5728 0.084 Uiso 1 1 d R . . H21 H -0.7096 -0.2990 -0.5699 0.078 Uiso 1 1 d R . . H22 H -0.4881 -0.2850 -0.6180 0.064 Uiso 1 1 d R . . H24 H -0.5509 -0.3104 -0.7477 0.060 Uiso 1 1 d R . . H25 H -0.5818 -0.2396 -0.8456 0.068 Uiso 1 1 d R . . H26 H -0.4028 -0.2293 -0.9147 0.067 Uiso 1 1 d R . . H27 H -0.1849 -0.2923 -0.8906 0.058 Uiso 1 1 d R . . H28 H -0.1540 -0.3683 -0.7957 0.050 Uiso 1 1 d R . . H30 H -0.3536 -0.5311 -0.7864 0.054 Uiso 1 1 d R . . H31 H -0.2724 -0.6797 -0.8059 0.074 Uiso 1 1 d R . . H32 H -0.1106 -0.7467 -0.7362 0.066 Uiso 1 1 d R . . H33 H -0.0334 -0.6661 -0.6482 0.078 Uiso 1 1 d R . . H34 H -0.1113 -0.5134 -0.6319 0.060 Uiso 1 1 d 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 Re1 0.04416(14) 0.04073(14) 0.03853(12) -0.00231(10) -0.00146(12) -0.00324(12) S1 0.0677(13) 0.0896(15) 0.0427(9) 0.0000(8) 0.0108(8) -0.0102(10) P1 0.0321(8) 0.0377(8) 0.0300(7) 0.0014(6) 0.0040(6) 0.0029(6) O1 0.050(4) 0.114(5) 0.149(6) -0.067(5) 0.009(4) 0.022(4) O2 0.097(5) 0.086(4) 0.114(5) 0.059(4) -0.013(4) 0.008(4) O3 0.046(3) 0.054(3) 0.050(3) 0.0042(18) -0.0001(18) 0.006(2) O4 0.072(3) 0.054(3) 0.054(3) -0.015(2) 0.009(2) -0.020(2) C1 0.070(6) 0.088(6) 0.075(6) -0.034(5) 0.014(4) -0.006(5) C2 0.041(4) 0.091(6) 0.079(5) -0.038(5) 0.004(4) -0.005(4) C3 0.041(4) 0.057(5) 0.116(7) 0.002(5) -0.012(4) 0.008(4) C4 0.066(5) 0.061(4) 0.056(4) 0.006(3) -0.024(4) -0.005(4) C5 0.050(3) 0.035(3) 0.042(3) -0.006(2) 0.000(3) -0.004(3) C6 0.061(5) 0.050(4) 0.053(4) 0.000(3) -0.004(3) -0.010(3) C7 0.080(7) 0.089(6) 0.065(5) -0.015(4) 0.016(4) -0.037(5) C8 0.045(4) 0.096(6) 0.069(5) -0.024(4) 0.016(4) -0.007(4) C9 0.075(6) 0.061(5) 0.069(5) -0.025(4) 0.001(4) 0.012(4) C10 0.038(3) 0.050(4) 0.034(3) -0.006(2) 0.001(2) -0.006(3) C11 0.039(3) 0.036(3) 0.036(3) 0.001(2) 0.005(2) 0.008(3) C12 0.051(4) 0.067(4) 0.037(3) 0.005(3) 0.004(3) -0.019(4) C13 0.065(5) 0.083(6) 0.045(4) 0.007(4) 0.011(4) -0.027(4) C14 0.048(4) 0.057(4) 0.062(5) -0.005(3) -0.005(3) -0.007(3) C15 0.057(4) 0.053(4) 0.036(3) -0.002(3) -0.004(3) 0.004(4) C16 0.055(4) 0.044(4) 0.043(4) 0.005(3) 0.004(3) -0.011(3) C17 0.041(4) 0.050(4) 0.031(3) 0.000(2) 0.007(3) 0.006(3) C18 0.054(4) 0.054(4) 0.051(4) -0.006(3) 0.006(3) -0.005(3) C19 0.063(5) 0.045(4) 0.083(5) -0.008(4) 0.029(4) -0.011(4) C20 0.051(4) 0.109(7) 0.050(4) -0.001(4) 0.020(4) -0.012(4) C21 0.051(4) 0.088(5) 0.057(4) -0.023(4) 0.011(4) 0.013(4) C22 0.046(4) 0.062(5) 0.052(4) -0.012(3) 0.010(3) -0.008(3) C23 0.040(4) 0.027(3) 0.033(3) 0.000(2) 0.000(2) 0.001(2) C24 0.051(4) 0.051(4) 0.047(4) 0.003(3) -0.001(3) 0.005(3) C25 0.061(5) 0.064(5) 0.046(4) 0.005(3) -0.009(4) 0.021(4) C26 0.084(5) 0.047(4) 0.037(3) 0.009(2) -0.006(4) 0.002(4) C27 0.061(5) 0.048(4) 0.037(3) 0.000(3) 0.010(3) -0.012(3) C28 0.042(4) 0.045(4) 0.039(3) 0.000(3) 0.005(3) 0.004(3) C29 0.040(3) 0.036(3) 0.033(3) 0.004(2) 0.012(2) 0.005(2) C30 0.042(3) 0.052(4) 0.041(3) -0.002(3) 0.007(3) -0.002(3) C31 0.072(5) 0.059(5) 0.054(4) -0.015(3) 0.020(4) 0.007(4) C32 0.068(5) 0.040(3) 0.056(4) 0.002(3) 0.019(4) 0.013(3) C33 0.078(6) 0.067(5) 0.050(4) 0.010(3) 0.009(4) 0.032(4) C34 0.051(4) 0.062(4) 0.038(3) 0.003(3) -0.004(3) 0.012(4) _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 Re1 O4 1.675(4) . ? Re1 N1 1.983(6) . ? Re1 O3 2.000(4) . ? Re1 N2 1.999(5) . ? Re1 S1 2.276(2) . ? S1 C1 1.788(9) . ? P1 C17 1.786(6) . ? P1 C29 1.789(6) . ? P1 C23 1.789(5) . ? P1 C11 1.795(7) . ? O1 C2 1.208(9) . ? O2 C4 1.225(9) . ? O3 C10 1.347(8) . ? N1 C2 1.356(9) . ? N1 C3 1.446(10) . ? N2 C4 1.388(9) . ? N2 C5 1.398(8) . ? C1 C2 1.544(13) . ? C3 C4 1.482(12) . ? C5 C6 1.378(9) . ? C5 C10 1.394(9) . ? C6 C7 1.440(12) . ? C7 C8 1.369(13) . ? C8 C9 1.376(11) . ? C9 C10 1.360(10) . ? C11 C12 1.388(9) . ? C11 C16 1.383(9) . ? C12 C13 1.372(10) . ? C13 C14 1.367(10) . ? C14 C15 1.356(10) . ? C15 C16 1.393(9) . ? C17 C18 1.370(9) . ? C17 C22 1.390(9) . ? C18 C19 1.385(10) . ? C19 C20 1.365(10) . ? C20 C21 1.392(10) . ? C21 C22 1.376(10) . ? C23 C24 1.382(9) . ? C23 C28 1.378(8) . ? C24 C25 1.397(9) . ? C25 C26 1.349(10) . ? C26 C27 1.371(11) . ? C27 C28 1.364(9) . ? C29 C34 1.383(8) . ? C29 C30 1.397(9) . ? C30 C31 1.383(9) . ? C31 C32 1.388(10) . ? C32 C33 1.400(10) . ? C33 C34 1.410(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9601 . ? C3 H3A 0.9600 . ? C3 H3B 0.9594 . ? C6 H6 0.9601 . ? C7 H7 0.9600 . ? C8 H8 0.9600 . ? C9 H9 0.9602 . ? C12 H12 0.9601 . ? C13 H13 0.9598 . ? C14 H14 0.9599 . ? C15 H15 0.9602 . ? C16 H16 0.9600 . ? C18 H18 0.9599 . ? C19 H19 0.9601 . ? C20 H20 0.9600 . ? C21 H21 0.9600 . ? C22 H22 0.9600 . ? C24 H24 0.9600 . ? C25 H25 0.9600 . ? C26 H26 0.9600 . ? C27 H27 0.9600 . ? C28 H28 0.9600 . ? C30 H30 0.9599 . ? C31 H31 0.9599 . ? C32 H32 0.9600 . ? C33 H33 0.9600 . ? C34 H34 0.9600 . ? 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 O4 Re1 N1 110.9(3) . . ? O4 Re1 O3 109.3(2) . . ? N1 Re1 O3 139.1(2) . . ? O4 Re1 N2 114.1(2) . . ? N1 Re1 N2 78.4(2) . . ? O3 Re1 N2 78.6(2) . . ? O4 Re1 S1 110.41(17) . . ? N1 Re1 S1 83.21(17) . . ? O3 Re1 S1 89.95(14) . . ? N2 Re1 S1 135.42(15) . . ? C1 S1 Re1 100.4(3) . . ? C17 P1 C29 111.0(3) . . ? C17 P1 C23 110.3(3) . . ? C29 P1 C23 107.1(2) . . ? C17 P1 C11 107.9(3) . . ? C29 P1 C11 108.8(3) . . ? C23 P1 C11 111.7(3) . . ? C10 O3 Re1 113.9(4) . . ? C2 N1 C3 118.8(7) . . ? C2 N1 Re1 125.2(5) . . ? C3 N1 Re1 115.4(5) . . ? C4 N2 C5 126.4(6) . . ? C4 N2 Re1 117.6(5) . . ? C5 N2 Re1 116.0(4) . . ? C2 C1 S1 111.8(6) . . ? O1 C2 N1 123.5(9) . . ? O1 C2 C1 122.4(8) . . ? N1 C2 C1 114.0(7) . . ? N1 C3 C4 111.2(6) . . ? O2 C4 N2 123.1(8) . . ? O2 C4 C3 125.3(8) . . ? N2 C4 C3 111.6(6) . . ? C6 C5 C10 120.4(6) . . ? C6 C5 N2 128.9(6) . . ? C10 C5 N2 110.6(5) . . ? C5 C6 C7 118.2(7) . . ? C8 C7 C6 119.6(8) . . ? C9 C8 C7 120.6(8) . . ? C8 C9 C10 120.6(8) . . ? O3 C10 C9 120.9(7) . . ? O3 C10 C5 118.6(6) . . ? C9 C10 C5 120.5(7) . . ? C12 C11 C16 120.1(6) . . ? C12 C11 P1 121.1(5) . . ? C16 C11 P1 118.8(5) . . ? C11 C12 C13 118.7(6) . . ? C14 C13 C12 121.4(7) . . ? C15 C14 C13 120.5(7) . . ? C14 C15 C16 119.6(6) . . ? C11 C16 C15 119.7(6) . . ? C18 C17 C22 119.3(6) . . ? C18 C17 P1 121.1(5) . . ? C22 C17 P1 119.4(5) . . ? C17 C18 C19 120.9(7) . . ? C20 C19 C18 120.2(7) . . ? C19 C20 C21 119.1(7) . . ? C20 C21 C22 120.9(7) . . ? C17 C22 C21 119.5(7) . . ? C24 C23 C28 119.2(5) . . ? C24 C23 P1 120.7(5) . . ? C28 C23 P1 120.1(4) . . ? C23 C24 C25 118.7(6) . . ? C26 C25 C24 121.2(7) . . ? C25 C26 C27 119.9(6) . . ? C28 C27 C26 119.9(6) . . ? C27 C28 C23 121.1(6) . . ? C34 C29 C30 120.6(6) . . ? C34 C29 P1 120.7(5) . . ? C30 C29 P1 118.6(5) . . ? C31 C30 C29 120.6(7) . . ? C30 C31 C32 119.0(7) . . ? C31 C32 C33 121.5(6) . . ? C32 C33 C34 118.7(7) . . ? C29 C34 C33 119.6(6) . . ? C2 C1 H1A 109.1 . . ? S1 C1 H1A 109.8 . . ? C2 C1 H1B 108.1 . . ? S1 C1 H1B 108.5 . . ? H1A C1 H1B 109.5 . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 105.7 . . ? N1 C3 H3B 109.5 . . ? C4 C3 H3B 112.2 . . ? H3A C3 H3B 109.5 . . ? C5 C6 H6 117.5 . . ? C7 C6 H6 124.3 . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 120.9 . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.4 . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.6 . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 121.5 . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.5 . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 119.0 . . ? C14 C15 H15 121.3 . . ? C16 C15 H15 119.0 . . ? C11 C16 H16 118.4 . . ? C15 C16 H16 121.8 . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 118.6 . . ? C20 C19 H19 121.6 . . ? C18 C19 H19 118.2 . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.6 . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 H22 117.9 . . ? C21 C22 H22 122.6 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 121.3 . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.2 . . ? C25 C26 H26 118.4 . . ? C27 C26 H26 121.7 . . ? C28 C27 H27 121.0 . . ? C26 C27 H27 119.1 . . ? C27 C28 H28 120.3 . . ? C23 C28 H28 118.5 . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 121.2 . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 118.2 . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 120.2 . . ? C29 C34 H34 120.2 . . ? C33 C34 H34 120.1 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.175 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.120 #===END data_[TcO(Ph-ON2S)]- _database_code_depnum_ccdc_archive 'CCDC 275919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 N3 O4 S Tc' _chemical_formula_weight 592.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.114(2) _cell_length_b 18.383(4) _cell_length_c 17.360(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.32(3) _cell_angle_gamma 90.00 _cell_volume 2908(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 6.1 _cell_measurement_theta_max 8.6 _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type 'psi-scan method' _exptl_absorpt_correction_T_min 0.345 _exptl_absorpt_correction_T_max 0.562 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nicolet R3m/V diffractometer' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 7250 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 29.55 _reflns_number_total 7250 _reflns_number_gt 3700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3/P4 vers.4.27 (Nicolet, 1991)' _computing_cell_refinement 'P3/P4 vers.4.27 (Nicolet, 1991)' _computing_data_reduction 'P3/P4 vers.4.27 (Nicolet, 1991)' _computing_structure_solution 'SHELXTL NT vers.5.10 (Bruker, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT vers.5.10 (Bruker, 1999)' _computing_publication_material 'SHELXTL NT vers.5.10 (Bruker, 1999)' _refine_special_details ; C26 splitted into two postitions,each with occupancy 0.5 Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7250 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tc1 Tc 0.14921(3) 0.790970(17) 0.096371(18) 0.05788(12) Uani 1 1 d . . . S1 S 0.15719(11) 0.81190(6) -0.03270(6) 0.0657(3) Uani 1 1 d . . . O1 O 0.1465(3) 1.01056(16) 0.05154(17) 0.0830(8) Uani 1 1 d . . . O2 O -0.0971(4) 0.87390(19) 0.26816(17) 0.0936(10) Uani 1 1 d . . . O3 O 0.0349(3) 0.70119(13) 0.07396(15) 0.0648(7) Uani 1 1 d . . . O4 O 0.3140(3) 0.77087(15) 0.13203(17) 0.0783(8) Uani 1 1 d . . . N1 N 0.1187(3) 0.89646(17) 0.10030(17) 0.0609(8) Uani 1 1 d . . . N2 N -0.0052(3) 0.79815(17) 0.17471(17) 0.0583(7) Uani 1 1 d . . . N3 N 0.1700(3) 0.75573(18) 0.43115(16) 0.0596(8) Uani 1 1 d . . . C1 C 0.1856(4) 0.9100(2) -0.0321(2) 0.0705(11) Uani 1 1 d . . . H1A H 0.2875 0.9201 -0.0431 0.085 Uiso 1 1 calc R . . H1B H 0.1255 0.9317 -0.0728 0.085 Uiso 1 1 calc R . . C2 C 0.1488(4) 0.9448(2) 0.0431(2) 0.0635(10) Uani 1 1 d . . . C3 C 0.0570(5) 0.9241(2) 0.1711(2) 0.0751(12) Uani 1 1 d . . . H3A H -0.0092 0.9641 0.1593 0.090 Uiso 1 1 calc R . . H3B H 0.1350 0.9420 0.2049 0.090 Uiso 1 1 calc R . . C4 C -0.0255(4) 0.8638(2) 0.2108(2) 0.0686(11) Uani 1 1 d . . . C5 C -0.0870(4) 0.7340(2) 0.1871(2) 0.0612(10) Uani 1 1 d . . . C6 C -0.1850(4) 0.7187(3) 0.2444(2) 0.0764(12) Uani 1 1 d . . . H6A H -0.2056 0.7530 0.2820 0.092 Uiso 1 1 calc R . . C7 C -0.2517(5) 0.6511(3) 0.2448(3) 0.0973(16) Uani 1 1 d . . . H7A H -0.3174 0.6403 0.2833 0.117 Uiso 1 1 calc R . . C8 C -0.2241(6) 0.5997(3) 0.1901(3) 0.0958(16) Uani 1 1 d . . . H8A H -0.2708 0.5548 0.1917 0.115 Uiso 1 1 calc R . . C9 C -0.1261(5) 0.6147(2) 0.1324(3) 0.0794(12) Uani 1 1 d . . . H9A H -0.1068 0.5801 0.0948 0.095 Uiso 1 1 calc R . . C10 C -0.0569(4) 0.6822(2) 0.1312(2) 0.0635(10) Uani 1 1 d . . . C11 C 0.2057(4) 0.7102(2) 0.5024(2) 0.0647(10) Uani 1 1 d . . . H11A H 0.3016 0.6884 0.4961 0.078 Uiso 1 1 calc R . . H11B H 0.2131 0.7427 0.5464 0.078 Uiso 1 1 calc R . . C12 C 0.0992(4) 0.6507(2) 0.5210(2) 0.0593(9) Uani 1 1 d . . . H12A H 0.0942 0.6160 0.4790 0.071 Uiso 1 1 calc R . . H12B H 0.0021 0.6712 0.5273 0.071 Uiso 1 1 calc R . . C13 C 0.1487(4) 0.6126(2) 0.5948(2) 0.0699(11) Uani 1 1 d . . . H13A H 0.2449 0.5915 0.5874 0.084 Uiso 1 1 calc R . . H13B H 0.1579 0.6484 0.6357 0.084 Uiso 1 1 calc R . . C14 C 0.0457(5) 0.5538(2) 0.6195(3) 0.0858(13) Uani 1 1 d . . . H14A H 0.0837 0.5312 0.6656 0.129 Uiso 1 1 calc R . . H14B H 0.0361 0.5181 0.5794 0.129 Uiso 1 1 calc R . . H14C H -0.0488 0.5746 0.6292 0.129 Uiso 1 1 calc R . . C15 C 0.0240(4) 0.7947(2) 0.4378(2) 0.0643(10) Uani 1 1 d . . . H15A H 0.0057 0.8216 0.3905 0.077 Uiso 1 1 calc R . . H15B H -0.0524 0.7581 0.4413 0.077 Uiso 1 1 calc R . . C16 C 0.0086(5) 0.8456(3) 0.5032(3) 0.0914(14) Uani 1 1 d . . . H16A H 0.0900 0.8796 0.5046 0.110 Uiso 1 1 calc R . . H16B H 0.0095 0.8188 0.5514 0.110 Uiso 1 1 calc R . . C17 C -0.1361(7) 0.8869(4) 0.4931(4) 0.137(2) Uani 1 1 d . . . H17A H -0.1351 0.9121 0.4440 0.165 Uiso 1 1 calc R . . H17B H -0.2152 0.8516 0.4904 0.165 Uiso 1 1 calc R . . C18 C -0.1673(13) 0.9362(6) 0.5489(8) 0.291(7) Uani 1 1 d . . . H18A H -0.2592 0.9594 0.5365 0.437 Uiso 1 1 calc R . . H18B H -0.0910 0.9722 0.5518 0.437 Uiso 1 1 calc R . . H18C H -0.1738 0.9118 0.5976 0.437 Uiso 1 1 calc R . . C19 C 0.2947(4) 0.8093(3) 0.4238(2) 0.0752(12) Uani 1 1 d . . . H19A H 0.3854 0.7821 0.4199 0.090 Uiso 1 1 calc R . . H19B H 0.3015 0.8378 0.4707 0.090 Uiso 1 1 calc R . . C20 C 0.2831(5) 0.8610(3) 0.3562(3) 0.0907(14) Uani 1 1 d . . . H20A H 0.1996 0.8930 0.3625 0.109 Uiso 1 1 calc R . . H20B H 0.2676 0.8336 0.3090 0.109 Uiso 1 1 calc R . . C21 C 0.4218(7) 0.9058(4) 0.3508(4) 0.144(3) Uani 1 1 d . . . H21A H 0.4040 0.9459 0.3156 0.173 Uiso 1 1 calc R . . H21B H 0.4458 0.9261 0.4011 0.173 Uiso 1 1 calc R . . C22 C 0.5405(8) 0.8658(5) 0.3257(5) 0.207(4) Uani 1 1 d . . . H22A H 0.6248 0.8969 0.3227 0.311 Uiso 1 1 calc R . . H22B H 0.5178 0.8459 0.2757 0.311 Uiso 1 1 calc R . . H22C H 0.5609 0.8269 0.3613 0.311 Uiso 1 1 calc R . . C23 C 0.1566(4) 0.7083(2) 0.3610(2) 0.0680(11) Uani 1 1 d . . . H23A H 0.1266 0.7385 0.3176 0.082 Uiso 1 1 calc R . . H23B H 0.0787 0.6734 0.3691 0.082 Uiso 1 1 calc R . . C24 C 0.2939(5) 0.6665(3) 0.3388(3) 0.0892(14) Uani 1 1 d . . . H24A H 0.3723 0.7007 0.3289 0.107 Uiso 1 1 calc R . . H24B H 0.3254 0.6358 0.3815 0.107 Uiso 1 1 calc R . . C25 C 0.2664(9) 0.6197(4) 0.2678(3) 0.127(2) Uani 1 1 d . . . C26 C 0.1714(12) 0.5735(6) 0.2738(6) 0.088(3) Uiso 0.50 1 d P . . C26' C 0.3724(12) 0.5846(6) 0.2263(6) 0.103(3) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tc1 0.04397(17) 0.0593(2) 0.0699(2) 0.00862(16) -0.00897(13) 0.00318(14) S1 0.0586(6) 0.0691(6) 0.0694(6) 0.0047(5) 0.0007(5) 0.0022(5) O1 0.095(2) 0.0593(18) 0.094(2) 0.0047(16) -0.0216(17) -0.0075(16) O2 0.100(2) 0.112(3) 0.0692(19) -0.0121(18) 0.0073(17) 0.004(2) O3 0.0604(15) 0.0581(16) 0.0757(17) 0.0036(13) -0.0035(13) -0.0023(12) O4 0.0508(15) 0.081(2) 0.103(2) 0.0216(16) -0.0139(14) 0.0055(13) N1 0.0604(18) 0.063(2) 0.0585(18) 0.0020(16) -0.0117(15) 0.0000(15) N2 0.0509(16) 0.064(2) 0.0591(18) 0.0040(15) -0.0058(13) -0.0007(15) N3 0.0465(16) 0.075(2) 0.0564(17) 0.0122(16) -0.0099(13) -0.0066(15) C1 0.064(2) 0.072(3) 0.075(3) 0.019(2) -0.003(2) -0.001(2) C2 0.059(2) 0.058(2) 0.073(3) 0.010(2) -0.0194(19) -0.0017(18) C3 0.082(3) 0.074(3) 0.069(3) -0.005(2) -0.020(2) 0.003(2) C4 0.064(2) 0.078(3) 0.062(2) -0.004(2) -0.014(2) 0.004(2) C5 0.048(2) 0.076(3) 0.058(2) 0.012(2) -0.0134(17) -0.0016(18) C6 0.064(2) 0.100(4) 0.065(3) 0.011(2) -0.007(2) -0.009(2) C7 0.076(3) 0.129(5) 0.087(3) 0.030(3) -0.006(3) -0.028(3) C8 0.087(3) 0.100(4) 0.100(4) 0.030(3) -0.013(3) -0.036(3) C9 0.073(3) 0.077(3) 0.086(3) 0.012(2) -0.015(2) -0.015(2) C10 0.049(2) 0.068(2) 0.072(3) 0.017(2) -0.0136(19) -0.0068(18) C11 0.052(2) 0.082(3) 0.059(2) 0.016(2) -0.0100(17) -0.010(2) C12 0.0508(19) 0.065(2) 0.061(2) 0.0022(18) -0.0033(16) -0.0048(18) C13 0.066(2) 0.076(3) 0.067(2) 0.010(2) -0.0047(19) -0.005(2) C14 0.088(3) 0.081(3) 0.089(3) 0.020(3) 0.006(2) -0.004(3) C15 0.0476(19) 0.073(3) 0.072(2) 0.008(2) -0.0057(17) 0.0008(19) C16 0.086(3) 0.094(4) 0.094(3) -0.004(3) 0.010(3) -0.004(3) C17 0.116(5) 0.106(5) 0.191(7) -0.040(5) 0.049(5) 0.013(4) C18 0.281(15) 0.176(10) 0.423(19) -0.048(11) 0.114(13) 0.013(10) C19 0.051(2) 0.100(3) 0.074(3) 0.023(2) -0.0074(19) -0.019(2) C20 0.067(3) 0.102(4) 0.103(3) 0.036(3) -0.001(2) -0.005(3) C21 0.087(4) 0.168(7) 0.178(6) 0.089(5) 0.022(4) -0.007(4) C22 0.107(5) 0.263(11) 0.253(10) 0.142(8) 0.035(6) -0.001(6) C23 0.057(2) 0.088(3) 0.058(2) 0.010(2) -0.0107(17) 0.005(2) C24 0.079(3) 0.085(3) 0.104(4) 0.021(3) 0.005(3) 0.006(3) C25 0.176(6) 0.134(5) 0.072(3) 0.013(3) 0.018(4) 0.072(5) _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 O4 1.653(2) . ? Tc1 N1 1.960(3) . ? Tc1 N2 1.984(3) . ? Tc1 O3 1.986(2) . ? Tc1 S1 2.2764(12) . ? S1 C1 1.822(4) . ? O1 C2 1.219(4) . ? O2 C4 1.216(5) . ? O3 C10 1.359(4) . ? N1 C2 1.365(5) . ? N1 C3 1.454(5) . ? N2 C4 1.375(5) . ? N2 C5 1.414(5) . ? N3 C23 1.501(5) . ? N3 C19 1.511(5) . ? N3 C15 1.518(4) . ? N3 C11 1.522(4) . ? C1 C2 1.497(5) . ? C3 C4 1.514(6) . ? C5 C6 1.383(5) . ? C5 C10 1.391(6) . ? C6 C7 1.383(6) . ? C7 C8 1.366(7) . ? C8 C9 1.386(6) . ? C9 C10 1.393(5) . ? C11 C12 1.503(5) . ? C12 C13 1.519(5) . ? C13 C14 1.500(5) . ? C15 C16 1.481(6) . ? C16 C17 1.528(7) . ? C17 C18 1.362(10) . ? C19 C20 1.512(5) . ? C20 C21 1.513(7) . ? C21 C22 1.386(9) . ? C23 C24 1.525(6) . ? C24 C25 1.520(7) . ? C25 C26 1.219(11) . ? C25 C26' 1.378(12) . ? C26 C26' 2.037(15) . ? 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 O4 Tc1 N1 109.66(13) . . ? O4 Tc1 N2 114.26(13) . . ? N1 Tc1 N2 78.86(13) . . ? O4 Tc1 O3 110.84(12) . . ? N1 Tc1 O3 139.01(11) . . ? N2 Tc1 O3 79.19(12) . . ? O4 Tc1 S1 110.91(11) . . ? N1 Tc1 S1 82.81(9) . . ? N2 Tc1 S1 134.66(9) . . ? O3 Tc1 S1 88.64(8) . . ? C1 S1 Tc1 99.74(13) . . ? C10 O3 Tc1 113.5(2) . . ? C2 N1 C3 118.4(3) . . ? C2 N1 Tc1 125.9(3) . . ? C3 N1 Tc1 115.6(3) . . ? C4 N2 C5 125.9(3) . . ? C4 N2 Tc1 118.5(3) . . ? C5 N2 Tc1 115.7(3) . . ? C23 N3 C19 110.9(3) . . ? C23 N3 C15 106.3(3) . . ? C19 N3 C15 111.2(3) . . ? C23 N3 C11 110.6(3) . . ? C19 N3 C11 106.2(3) . . ? C15 N3 C11 111.6(3) . . ? C2 C1 S1 113.1(3) . . ? O1 C2 N1 123.6(4) . . ? O1 C2 C1 122.2(4) . . ? N1 C2 C1 114.2(3) . . ? N1 C3 C4 109.6(3) . . ? O2 C4 N2 126.0(4) . . ? O2 C4 C3 122.9(4) . . ? N2 C4 C3 111.1(4) . . ? C6 C5 C10 120.2(4) . . ? C6 C5 N2 129.1(4) . . ? C10 C5 N2 110.6(3) . . ? C5 C6 C7 118.5(5) . . ? C8 C7 C6 122.0(5) . . ? C7 C8 C9 119.8(5) . . ? C8 C9 C10 119.2(5) . . ? O3 C10 C5 117.9(3) . . ? O3 C10 C9 121.8(4) . . ? C5 C10 C9 120.2(4) . . ? C12 C11 N3 116.6(3) . . ? C11 C12 C13 109.7(3) . . ? C14 C13 C12 113.4(3) . . ? C16 C15 N3 117.1(3) . . ? C15 C16 C17 108.8(4) . . ? C18 C17 C16 116.3(8) . . ? N3 C19 C20 115.9(3) . . ? C19 C20 C21 110.2(4) . . ? C22 C21 C20 113.0(7) . . ? N3 C23 C24 116.4(3) . . ? C25 C24 C23 111.6(4) . . ? C26 C25 C26' 103.1(9) . . ? C26 C25 C24 115.4(7) . . ? C26' C25 C24 125.8(8) . . ? C25 C26 C26' 41.2(5) . . ? C25 C26' C26 35.6(5) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 29.55 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.758 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.065 #===END