Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #--------------------------------------------------------------------- _publ_contact_author 'Prof. John A. Gladysz' _publ_contact_author_address ; Prof John A Gladysz Institut fur Organische Chemie Universitat Erlangen-Nurnberg Henkestrasse 42 91054 Erlangen GERMANY ; _publ_contact_author_email gladysz@organik.uni-erlangen.de #--------------------------------------------------------------------- loop_ _publ_author_name 'Brian J. Boone' 'Michael Otto' 'Atta M. Arif' 'John A. Gladysz' _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '?' _journal_coden_Cambridge 186 #------------------------------------------------------------------------- _chemical_name_systematic '?' _chemical_name_common '?' _chemical_formula_moiety '?' _chemical_formula_sum 'C29.50 H33 Cl F3 N O5 P Re S2' _chemical_formula_weight 855.31 _chemical_melting_point ? _ccdc_compound_id '?' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_chemdiag_type '?' _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn ? _exptl_crystal_colour '?' #--------------------------------------------------------------------- _diffrn_radiation_type 'Mo-Ka' _diffrn_measurement_device 'Enraf-Nonius CAD4' _ccdc_temp_data_collection 173 _ccdc_ls_R_squared ? _refine_ls_abs_structure_details '?' _ccdc_disorder '?' _ccdc_comments '?' #--------------------------------------------------------------------- data_boone _database_code_CSD 151132 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29.50 H33 Cl F3 N O5 P Re S2' _chemical_formula_weight 855.31 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.758(2) _cell_length_b 11.121(2) _cell_length_c 14.558(3) _cell_angle_alpha 102.47(2) _cell_angle_beta 102.42(2) _cell_angle_gamma 77.26(2) _cell_volume 1632.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 148(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 4.036 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.4088 _exptl_absorpt_correction_T_max 0.7654 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 148(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 5424 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 23.98 _reflns_number_total 5113 _reflns_number_gt 4614 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction MoleN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material '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^)+(0.0768P)^2^+10.8993P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5113 _refine_ls_number_parameters 404 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 2.671 _refine_ls_shift/su_mean 0.116 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 Re Re 0.88212(3) 0.56269(3) 0.72467(2) 0.02522(15) Uani 1 1 d . . . S1 S 0.5822(2) 0.5965(2) 0.70209(16) 0.0375(5) Uani 1 1 d . . . P P 0.94352(18) 0.73325(17) 0.84376(14) 0.0226(4) Uani 1 1 d . . . O1 O 0.9343(8) 0.3936(6) 0.8639(5) 0.060(2) Uani 1 1 d . . . O2 O 0.6953(5) 0.6714(5) 0.7348(4) 0.0289(12) Uani 1 1 d . . . N N 0.9093(7) 0.4656(7) 0.8116(5) 0.0357(16) Uani 1 1 d . . . C1 C 0.9833(9) 0.4148(9) 0.6240(7) 0.047(2) Uani 1 1 d . . . H1 H 1.0257 0.3367 0.6419 0.057 Uiso 1 1 calc R . . C2 C 0.8521(9) 0.4433(9) 0.5770(6) 0.044(2) Uani 1 1 d . . . H2 H 0.7910 0.3887 0.5594 0.053 Uiso 1 1 calc R . . C3 C 0.8309(12) 0.5652(10) 0.5620(7) 0.055(3) Uani 1 1 d . . . H3 H 0.7519 0.6076 0.5308 0.066 Uiso 1 1 calc R . . C4 C 0.9413(12) 0.6172(10) 0.5990(7) 0.058(3) Uani 1 1 d . . . H4 H 0.9502 0.6999 0.5978 0.069 Uiso 1 1 calc R . . C5 C 1.0394(11) 0.5236(10) 0.6394(7) 0.054(3) Uani 1 1 d . . . H5 H 1.1250 0.5325 0.6704 0.065 Uiso 1 1 calc R . . C6 C 0.9440(7) 0.8719(7) 0.7959(6) 0.0275(16) Uani 1 1 d . . . C7 C 1.0448(8) 0.9381(7) 0.8209(6) 0.0329(18) Uani 1 1 d . . . H7 H 1.1210 0.9091 0.8628 0.039 Uiso 1 1 calc R . . C8 C 1.0352(10) 1.0465(8) 0.7852(6) 0.041(2) Uani 1 1 d . . . H8 H 1.1048 1.0914 0.8027 0.050 Uiso 1 1 calc R . . C9 C 0.9253(11) 1.0887(8) 0.7245(7) 0.051(3) Uani 1 1 d . . . H9 H 0.9193 1.1626 0.6998 0.062 Uiso 1 1 calc R . . C10 C 0.8221(11) 1.0239(9) 0.6989(8) 0.057(3) Uani 1 1 d . . . H10 H 0.7459 1.0544 0.6576 0.068 Uiso 1 1 calc R . . C11 C 0.8304(9) 0.9165(8) 0.7332(7) 0.043(2) Uani 1 1 d . . . H11 H 0.7606 0.8719 0.7151 0.051 Uiso 1 1 calc R . . C12 C 0.8332(7) 0.7883(7) 0.9305(5) 0.0237(15) Uani 1 1 d . . . C13 C 0.8206(8) 0.7046(8) 0.9850(6) 0.0327(18) Uani 1 1 d . . . H13 H 0.8700 0.6221 0.9772 0.039 Uiso 1 1 calc R . . C14 C 0.7376(8) 0.7392(8) 1.0502(6) 0.037(2) Uani 1 1 d . . . H14 H 0.7317 0.6816 1.0880 0.045 Uiso 1 1 calc R . . C15 C 0.6624(8) 0.8592(8) 1.0605(6) 0.038(2) Uani 1 1 d . . . H15 H 0.6029 0.8828 1.1037 0.046 Uiso 1 1 calc R . . C16 C 0.6751(8) 0.9447(8) 1.0068(6) 0.038(2) Uani 1 1 d . . . H16 H 0.6262 1.0274 1.0149 0.045 Uiso 1 1 calc R . . C17 C 0.7600(7) 0.9078(7) 0.9413(6) 0.0301(17) Uani 1 1 d . . . H17 H 0.7675 0.9653 0.9039 0.036 Uiso 1 1 calc R . . C18 C 1.1005(7) 0.7034(7) 0.9198(5) 0.0235(15) Uani 1 1 d . . . C19 C 1.1946(7) 0.6019(7) 0.8924(6) 0.0314(17) Uani 1 1 d . . . H19 H 1.1754 0.5448 0.8349 0.038 Uiso 1 1 calc R . . C20 C 1.3166(8) 0.5838(8) 0.9491(7) 0.039(2) Uani 1 1 d . . . H20 H 1.3801 0.5138 0.9301 0.046 Uiso 1 1 calc R . . C21 C 1.3460(8) 0.6655(7) 1.0315(6) 0.0348(19) Uani 1 1 d . . . H21 H 1.4307 0.6545 1.0685 0.042 Uiso 1 1 calc R . . C22 C 1.2513(8) 0.7649(8) 1.0612(6) 0.0348(19) Uani 1 1 d . . . H22 H 1.2705 0.8204 1.1197 0.042 Uiso 1 1 calc R . . C23 C 1.1298(7) 0.7831(7) 1.0060(5) 0.0262(16) Uani 1 1 d . . . H23 H 1.0654 0.8508 1.0270 0.031 Uiso 1 1 calc R . . C24 C 0.5758(10) 0.5392(12) 0.8061(8) 0.061(3) Uani 1 1 d . . . H24A H 0.6503 0.4721 0.8177 0.091 Uiso 1 1 calc R . . H24B H 0.4956 0.5065 0.7964 0.091 Uiso 1 1 calc R . . H24C H 0.5779 0.6076 0.8613 0.091 Uiso 1 1 calc R . . C25 C 0.4409(9) 0.7233(10) 0.6942(8) 0.051(3) Uani 1 1 d . . . C26 C 0.4499(11) 0.7705(13) 0.6031(10) 0.074(4) Uani 1 1 d . . . H26A H 0.4460 0.7017 0.5483 0.111 Uiso 1 1 calc R . . H26B H 0.5319 0.8001 0.6127 0.111 Uiso 1 1 calc R . . H26C H 0.3775 0.8394 0.5909 0.111 Uiso 1 1 calc R . . C27 C 0.3198(9) 0.6635(12) 0.6759(9) 0.062(3) Uani 1 1 d . . . H27A H 0.3144 0.6344 0.7336 0.094 Uiso 1 1 calc R . . H27B H 0.3254 0.5923 0.6229 0.094 Uiso 1 1 calc R . . H27C H 0.2424 0.7257 0.6595 0.094 Uiso 1 1 calc R . . C28 C 0.4447(12) 0.8229(13) 0.7798(10) 0.084(4) Uani 1 1 d . . . H28A H 0.3737 0.8932 0.7683 0.126 Uiso 1 1 calc R . . H28B H 0.5275 0.8518 0.7932 0.126 Uiso 1 1 calc R . . H28C H 0.4353 0.7898 0.8346 0.126 Uiso 1 1 calc R . . S2 S 0.4185(7) 0.2809(6) 0.6914(4) 0.0634(16) Uani 0.50 1 d PD A 1 F1 F 0.2816(18) 0.1085(19) 0.6752(13) 0.104(6) Uiso 0.50 1 d PD A 1 F2 F 0.4001(18) 0.0745(15) 0.5678(12) 0.093(5) Uiso 0.50 1 d PD A 1 F3 F 0.2320(19) 0.2173(18) 0.5619(14) 0.114(6) Uiso 0.50 1 d PD A 1 O3 O 0.3533(12) 0.3554(11) 0.7644(9) 0.041(3) Uiso 0.50 1 d PD A 1 O4 O 0.436(2) 0.337(2) 0.6228(16) 0.111(7) Uiso 0.50 1 d PD A 1 O5 O 0.518(4) 0.145(4) 0.728(3) 0.24(2) Uiso 0.50 1 d PD A 1 C29 C 0.3275(19) 0.1625(19) 0.6233(14) 0.060(6) Uiso 0.50 1 d PD A 1 S2' S 0.3446(6) 0.2609(6) 0.6980(5) 0.0628(16) Uani 0.50 1 d PD B 2 F1' F 0.541(2) 0.245(2) 0.6295(18) 0.144(9) Uiso 0.50 1 d PD B 2 F2' F 0.4881(18) 0.0693(15) 0.6034(13) 0.096(5) Uiso 0.50 1 d PD B 2 F3' F 0.352(3) 0.184(4) 0.525(2) 0.242(18) Uiso 0.50 1 d PD B 2 O3' O 0.2495(15) 0.1846(17) 0.6946(12) 0.071(5) Uiso 0.50 1 d PD B 2 O4' O 0.306(3) 0.381(2) 0.705(2) 0.129(9) Uiso 0.50 1 d PD B 2 O5' O 0.490(3) 0.206(3) 0.770(2) 0.155(12) Uiso 0.50 1 d PD B 2 C29' C 0.439(2) 0.191(2) 0.6078(17) 0.091 Uiso 0.50 1 d PD B 2 Cl Cl 0.0733(3) 0.8810(2) 0.5223(2) 0.0624(7) Uani 1 1 d . . . C30 C 0.0830(18) 1.0367(17) 0.5195(14) 0.045(4) Uani 0.50 1 d P . . H30A H 0.1430 1.0367 0.4766 0.054 Uiso 0.50 1 calc PR . . H30B H 0.1168 1.0788 0.5844 0.054 Uiso 0.50 1 calc PR . . 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 Re 0.0285(2) 0.0222(2) 0.0260(2) 0.00128(12) 0.00346(12) -0.01124(12) S1 0.0331(11) 0.0398(12) 0.0411(12) 0.0080(9) -0.0024(9) -0.0181(9) P 0.0215(9) 0.0204(9) 0.0267(10) 0.0031(7) 0.0039(8) -0.0067(7) O1 0.076(5) 0.040(4) 0.066(5) 0.024(4) -0.006(4) -0.015(3) O2 0.025(3) 0.029(3) 0.034(3) 0.004(2) 0.000(2) -0.015(2) N 0.052(4) 0.034(4) 0.023(3) 0.009(3) -0.006(3) -0.020(3) C1 0.045(5) 0.042(5) 0.043(5) -0.012(4) 0.002(4) -0.010(4) C2 0.046(5) 0.045(5) 0.037(5) -0.003(4) 0.000(4) -0.017(4) C3 0.077(7) 0.048(6) 0.036(5) 0.001(4) 0.016(5) -0.003(5) C4 0.088(8) 0.045(6) 0.046(6) -0.006(5) 0.029(6) -0.024(6) C5 0.060(6) 0.066(7) 0.039(5) -0.016(5) 0.025(5) -0.026(5) C6 0.032(4) 0.017(4) 0.034(4) 0.003(3) 0.008(3) -0.006(3) C7 0.044(5) 0.032(4) 0.028(4) 0.007(3) 0.005(4) -0.017(4) C8 0.066(6) 0.032(5) 0.033(5) 0.002(4) 0.009(4) -0.028(4) C9 0.094(8) 0.029(5) 0.038(5) 0.007(4) 0.007(5) -0.027(5) C10 0.073(7) 0.038(5) 0.054(6) 0.024(5) -0.018(5) -0.013(5) C11 0.042(5) 0.041(5) 0.045(5) 0.015(4) -0.010(4) -0.018(4) C12 0.020(4) 0.026(4) 0.025(4) 0.001(3) 0.001(3) -0.010(3) C13 0.034(4) 0.026(4) 0.037(5) 0.007(3) 0.006(4) -0.003(3) C14 0.045(5) 0.038(5) 0.036(5) 0.007(4) 0.013(4) -0.016(4) C15 0.028(4) 0.048(5) 0.039(5) -0.003(4) 0.013(4) -0.012(4) C16 0.030(4) 0.029(4) 0.050(5) 0.001(4) 0.007(4) 0.000(3) C17 0.027(4) 0.025(4) 0.035(4) 0.000(3) 0.001(3) -0.007(3) C18 0.020(4) 0.022(4) 0.029(4) 0.007(3) 0.002(3) -0.006(3) C19 0.028(4) 0.029(4) 0.035(4) 0.002(3) 0.006(3) -0.005(3) C20 0.025(4) 0.034(5) 0.054(6) 0.008(4) 0.013(4) 0.007(3) C21 0.023(4) 0.030(4) 0.052(5) 0.020(4) -0.005(4) -0.006(3) C22 0.034(4) 0.027(4) 0.038(5) 0.006(3) -0.004(4) -0.006(3) C23 0.021(4) 0.023(4) 0.032(4) 0.005(3) 0.001(3) -0.002(3) C24 0.048(6) 0.086(8) 0.067(7) 0.047(6) -0.001(5) -0.028(6) C25 0.027(5) 0.050(6) 0.072(7) 0.018(5) -0.007(4) -0.006(4) C26 0.055(7) 0.082(9) 0.099(10) 0.055(8) -0.007(7) -0.023(6) C27 0.033(5) 0.087(8) 0.071(7) 0.026(6) -0.010(5) -0.026(5) C28 0.045(7) 0.089(10) 0.091(10) -0.025(8) -0.002(6) -0.011(6) S2 0.056(4) 0.084(4) 0.042(3) -0.017(3) 0.016(3) -0.015(3) S2' 0.046(3) 0.068(4) 0.067(4) -0.015(3) 0.019(3) -0.012(3) Cl 0.0780(19) 0.0361(13) 0.0619(16) 0.0124(11) -0.0022(14) 0.0023(12) C30 0.043(10) 0.043(11) 0.048(11) -0.003(8) 0.005(9) -0.021(8) _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 Re N 1.773(7) . ? Re O2 2.122(5) . ? Re C1 2.212(9) . ? Re C5 2.222(9) . ? Re C2 2.268(9) . ? Re C4 2.295(10) . ? Re C3 2.318(10) . ? Re P 2.383(2) . ? S1 O2 1.558(5) . ? S1 C24 1.784(10) . ? S1 C25 1.834(10) . ? P C18 1.816(7) . ? P C6 1.826(7) . ? P C12 1.835(8) . ? O1 N 1.171(9) . ? C1 C2 1.429(13) . ? C1 C5 1.424(14) . ? C2 C3 1.382(14) . ? C3 C4 1.388(16) . ? C4 C5 1.434(16) . ? C6 C7 1.385(11) . ? C6 C11 1.421(12) . ? C7 C8 1.388(12) . ? C8 C9 1.373(14) . ? C9 C10 1.396(16) . ? C10 C11 1.369(13) . ? C12 C17 1.384(11) . ? C12 C13 1.392(11) . ? C13 C14 1.379(12) . ? C14 C15 1.396(12) . ? C15 C16 1.398(13) . ? C16 C17 1.397(12) . ? C18 C23 1.389(11) . ? C18 C19 1.390(11) . ? C19 C20 1.390(12) . ? C20 C21 1.364(13) . ? C21 C22 1.390(12) . ? C22 C23 1.378(11) . ? C25 C28 1.477(16) . ? C25 C27 1.539(13) . ? C25 C26 1.557(16) . ? S2 O4 1.35(2) . ? S2 O3 1.411(12) . ? S2 O5 1.76(3) . ? S2 C29 1.81(2) . ? F1 C29 1.29(2) . ? F2 C29 1.35(2) . ? F3 C29 1.34(2) . ? S2' O4' 1.30(2) . ? S2' O3' 1.453(15) . ? S2' O5' 1.75(3) . ? S2' C29' 1.78(2) . ? F1' C29' 1.30(2) . ? F2' C29' 1.34(2) . ? F3' C29' 1.35(3) . ? Cl C30 1.767(19) . ? Cl C30 1.776(19) 2_576 ? C30 Cl 1.776(19) 2_576 ? 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 N Re O2 103.9(3) . . ? N Re C1 93.2(4) . . ? O2 Re C1 140.2(3) . . ? N Re C5 113.8(4) . . ? O2 Re C5 142.1(4) . . ? C1 Re C5 37.5(4) . . ? N Re C2 108.9(3) . . ? O2 Re C2 103.1(3) . . ? C1 Re C2 37.2(3) . . ? C5 Re C2 61.9(4) . . ? N Re C4 150.6(4) . . ? O2 Re C4 105.1(3) . . ? C1 Re C4 61.0(4) . . ? C5 Re C4 37.0(4) . . ? C2 Re C4 59.8(4) . . ? N Re C3 143.8(3) . . ? O2 Re C3 87.2(3) . . ? C1 Re C3 59.8(4) . . ? C5 Re C3 60.2(4) . . ? C2 Re C3 35.0(4) . . ? C4 Re C3 35.0(4) . . ? N Re P 91.4(2) . . ? O2 Re P 81.21(15) . . ? C1 Re P 134.7(2) . . ? C5 Re P 100.8(3) . . ? C2 Re P 157.2(3) . . ? C4 Re P 97.4(3) . . ? C3 Re P 124.6(3) . . ? O2 S1 C24 104.0(4) . . ? O2 S1 C25 101.5(4) . . ? C24 S1 C25 103.4(5) . . ? C18 P C6 105.2(3) . . ? C18 P C12 102.6(3) . . ? C6 P C12 104.7(3) . . ? C18 P Re 116.8(2) . . ? C6 P Re 113.7(3) . . ? C12 P Re 112.5(2) . . ? S1 O2 Re 115.0(3) . . ? O1 N Re 173.9(8) . . ? C2 C1 C5 108.2(9) . . ? C2 C1 Re 73.6(5) . . ? C5 C1 Re 71.7(5) . . ? C3 C2 C1 107.0(9) . . ? C3 C2 Re 74.4(5) . . ? C1 C2 Re 69.3(5) . . ? C2 C3 C4 110.6(10) . . ? C2 C3 Re 70.5(6) . . ? C4 C3 Re 71.6(6) . . ? C3 C4 C5 107.7(9) . . ? C3 C4 Re 73.4(6) . . ? C5 C4 Re 68.7(6) . . ? C1 C5 C4 106.4(9) . . ? C1 C5 Re 70.9(5) . . ? C4 C5 Re 74.3(6) . . ? C7 C6 C11 119.1(7) . . ? C7 C6 P 123.9(6) . . ? C11 C6 P 117.0(6) . . ? C6 C7 C8 120.5(8) . . ? C9 C8 C7 120.0(8) . . ? C8 C9 C10 120.4(8) . . ? C11 C10 C9 120.2(9) . . ? C10 C11 C6 119.8(8) . . ? C17 C12 C13 119.2(7) . . ? C17 C12 P 122.5(6) . . ? C13 C12 P 118.2(6) . . ? C14 C13 C12 121.2(8) . . ? C13 C14 C15 119.7(8) . . ? C14 C15 C16 119.7(8) . . ? C17 C16 C15 119.7(8) . . ? C12 C17 C16 120.5(8) . . ? C23 C18 C19 118.7(7) . . ? C23 C18 P 120.5(6) . . ? C19 C18 P 120.8(6) . . ? C20 C19 C18 120.2(8) . . ? C21 C20 C19 120.7(7) . . ? C20 C21 C22 119.6(7) . . ? C23 C22 C21 120.1(8) . . ? C22 C23 C18 120.7(7) . . ? C28 C25 C27 112.0(10) . . ? C28 C25 C26 112.4(11) . . ? C27 C25 C26 109.8(9) . . ? C28 C25 S1 112.9(8) . . ? C27 C25 S1 107.2(7) . . ? C26 C25 S1 101.8(8) . . ? O4 S2 O3 118.2(12) . . ? O4 S2 O5 125.5(17) . . ? O3 S2 O5 111.5(15) . . ? O4 S2 C29 102.5(12) . . ? O3 S2 C29 110.2(9) . . ? O5 S2 C29 79.2(17) . . ? F1 C29 F3 110.6(18) . . ? F1 C29 F2 108.9(19) . . ? F3 C29 F2 104.8(18) . . ? F1 C29 S2 113.8(16) . . ? F3 C29 S2 107.4(15) . . ? F2 C29 S2 110.9(14) . . ? O4' S2' O3' 118.2(14) . . ? O4' S2' O5' 118.0(16) . . ? O3' S2' O5' 109.7(13) . . ? O4' S2' C29' 114.7(14) . . ? O3' S2' C29' 109.6(11) . . ? O5' S2' C29' 80.8(15) . . ? F1' C29' F3' 128(3) . . ? F1' C29' F2' 105(2) . . ? F3' C29' F2' 98(2) . . ? F1' C29' S2' 106.2(18) . . ? F3' C29' S2' 104(2) . . ? F2' C29' S2' 116.0(17) . . ? C30 Cl C30 70.5(9) . 2_576 ? Cl C30 Cl 109.5(9) . 2_576 ? 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 N Re P C18 54.2(4) . . . . ? O2 Re P C18 158.1(3) . . . . ? C1 Re P C18 -41.7(5) . . . . ? C5 Re P C18 -60.4(4) . . . . ? C2 Re P C18 -99.1(7) . . . . ? C4 Re P C18 -97.7(4) . . . . ? C3 Re P C18 -121.6(4) . . . . ? N Re P C6 177.0(4) . . . . ? O2 Re P C6 -79.1(3) . . . . ? C1 Re P C6 81.1(5) . . . . ? C5 Re P C6 62.4(4) . . . . ? C2 Re P C6 23.7(7) . . . . ? C4 Re P C6 25.1(4) . . . . ? C3 Re P C6 1.3(4) . . . . ? N Re P C12 -64.1(4) . . . . ? O2 Re P C12 39.8(3) . . . . ? C1 Re P C12 -160.0(5) . . . . ? C5 Re P C12 -178.7(4) . . . . ? C2 Re P C12 142.6(7) . . . . ? C4 Re P C12 144.0(4) . . . . ? C3 Re P C12 120.2(4) . . . . ? C24 S1 O2 Re 85.7(5) . . . . ? C25 S1 O2 Re -167.1(4) . . . . ? N Re O2 S1 -67.3(4) . . . . ? C1 Re O2 S1 45.5(6) . . . . ? C5 Re O2 S1 107.0(5) . . . . ? C2 Re O2 S1 46.3(4) . . . . ? C4 Re O2 S1 108.1(4) . . . . ? C3 Re O2 S1 77.7(4) . . . . ? P Re O2 S1 -156.6(3) . . . . ? O2 Re N O1 152(6) . . . . ? C1 Re N O1 8(6) . . . . ? C5 Re N O1 -24(6) . . . . ? C2 Re N O1 42(6) . . . . ? C4 Re N O1 -19(7) . . . . ? C3 Re N O1 47(7) . . . . ? P Re N O1 -127(6) . . . . ? N Re C1 C2 117.6(6) . . . . ? O2 Re C1 C2 1.2(8) . . . . ? C5 Re C1 C2 -116.2(9) . . . . ? C4 Re C1 C2 -77.3(7) . . . . ? C3 Re C1 C2 -36.8(6) . . . . ? P Re C1 C2 -147.3(5) . . . . ? N Re C1 C5 -126.2(7) . . . . ? O2 Re C1 C5 117.4(6) . . . . ? C2 Re C1 C5 116.2(9) . . . . ? C4 Re C1 C5 38.9(7) . . . . ? C3 Re C1 C5 79.3(7) . . . . ? P Re C1 C5 -31.1(8) . . . . ? C5 C1 C2 C3 1.7(11) . . . . ? Re C1 C2 C3 65.4(7) . . . . ? C5 C1 C2 Re -63.8(6) . . . . ? N Re C2 C3 175.2(6) . . . . ? O2 Re C2 C3 65.3(7) . . . . ? C1 Re C2 C3 -115.5(9) . . . . ? C5 Re C2 C3 -77.3(7) . . . . ? C4 Re C2 C3 -34.8(7) . . . . ? P Re C2 C3 -33.2(10) . . . . ? N Re C2 C1 -69.3(6) . . . . ? O2 Re C2 C1 -179.2(6) . . . . ? C5 Re C2 C1 38.2(6) . . . . ? C4 Re C2 C1 80.7(7) . . . . ? C3 Re C2 C1 115.5(9) . . . . ? P Re C2 C1 82.3(8) . . . . ? C1 C2 C3 C4 -1.3(11) . . . . ? Re C2 C3 C4 60.7(7) . . . . ? C1 C2 C3 Re -62.0(6) . . . . ? N Re C3 C2 -7.7(10) . . . . ? O2 Re C3 C2 -117.6(6) . . . . ? C1 Re C3 C2 39.1(6) . . . . ? C5 Re C3 C2 82.6(7) . . . . ? C4 Re C3 C2 120.7(10) . . . . ? P Re C3 C2 165.1(5) . . . . ? N Re C3 C4 -128.4(7) . . . . ? O2 Re C3 C4 121.7(6) . . . . ? C1 Re C3 C4 -81.5(7) . . . . ? C5 Re C3 C4 -38.0(6) . . . . ? C2 Re C3 C4 -120.7(10) . . . . ? P Re C3 C4 44.4(7) . . . . ? C2 C3 C4 C5 0.5(11) . . . . ? Re C3 C4 C5 60.5(7) . . . . ? C2 C3 C4 Re -60.0(7) . . . . ? N Re C4 C3 109.3(9) . . . . ? O2 Re C4 C3 -61.7(6) . . . . ? C1 Re C4 C3 77.8(6) . . . . ? C5 Re C4 C3 117.2(9) . . . . ? C2 Re C4 C3 34.8(6) . . . . ? P Re C4 C3 -144.5(6) . . . . ? N Re C4 C5 -7.9(10) . . . . ? O2 Re C4 C5 -178.9(5) . . . . ? C1 Re C4 C5 -39.4(6) . . . . ? C2 Re C4 C5 -82.4(6) . . . . ? C3 Re C4 C5 -117.2(9) . . . . ? P Re C4 C5 98.3(6) . . . . ? C2 C1 C5 C4 -1.4(11) . . . . ? Re C1 C5 C4 -66.3(6) . . . . ? C2 C1 C5 Re 65.0(7) . . . . ? C3 C4 C5 C1 0.6(11) . . . . ? Re C4 C5 C1 64.0(6) . . . . ? C3 C4 C5 Re -63.5(7) . . . . ? N Re C5 C1 61.7(7) . . . . ? O2 Re C5 C1 -112.4(7) . . . . ? C2 Re C5 C1 -37.9(6) . . . . ? C4 Re C5 C1 -114.1(9) . . . . ? C3 Re C5 C1 -78.1(6) . . . . ? P Re C5 C1 158.0(6) . . . . ? N Re C5 C4 175.8(5) . . . . ? O2 Re C5 C4 1.7(8) . . . . ? C1 Re C5 C4 114.1(9) . . . . ? C2 Re C5 C4 76.2(6) . . . . ? C3 Re C5 C4 36.0(6) . . . . ? P Re C5 C4 -87.9(6) . . . . ? C18 P C6 C7 -3.2(8) . . . . ? C12 P C6 C7 104.6(7) . . . . ? Re P C6 C7 -132.2(6) . . . . ? C18 P C6 C11 -179.9(7) . . . . ? C12 P C6 C11 -72.1(7) . . . . ? Re P C6 C11 51.2(7) . . . . ? C11 C6 C7 C8 0.0(12) . . . . ? P C6 C7 C8 -176.7(6) . . . . ? C6 C7 C8 C9 -0.1(13) . . . . ? C7 C8 C9 C10 0.5(15) . . . . ? C8 C9 C10 C11 -0.9(17) . . . . ? C9 C10 C11 C6 0.8(17) . . . . ? C7 C6 C11 C10 -0.3(14) . . . . ? P C6 C11 C10 176.5(8) . . . . ? C18 P C12 C17 116.6(6) . . . . ? C6 P C12 C17 6.9(7) . . . . ? Re P C12 C17 -117.1(6) . . . . ? C18 P C12 C13 -65.4(6) . . . . ? C6 P C12 C13 -175.0(6) . . . . ? Re P C12 C13 61.0(6) . . . . ? C17 C12 C13 C14 -0.7(12) . . . . ? P C12 C13 C14 -178.8(6) . . . . ? C12 C13 C14 C15 1.5(13) . . . . ? C13 C14 C15 C16 -2.2(13) . . . . ? C14 C15 C16 C17 2.0(13) . . . . ? C13 C12 C17 C16 0.5(11) . . . . ? P C12 C17 C16 178.6(6) . . . . ? C15 C16 C17 C12 -1.2(12) . . . . ? C6 P C18 C23 70.6(7) . . . . ? C12 P C18 C23 -38.7(7) . . . . ? Re P C18 C23 -162.2(5) . . . . ? C6 P C18 C19 -108.3(6) . . . . ? C12 P C18 C19 142.4(6) . . . . ? Re P C18 C19 18.9(7) . . . . ? C23 C18 C19 C20 -2.2(12) . . . . ? P C18 C19 C20 176.8(6) . . . . ? C18 C19 C20 C21 -0.5(13) . . . . ? C19 C20 C21 C22 2.7(13) . . . . ? C20 C21 C22 C23 -2.2(13) . . . . ? C21 C22 C23 C18 -0.6(12) . . . . ? C19 C18 C23 C22 2.7(11) . . . . ? P C18 C23 C22 -176.2(6) . . . . ? O2 S1 C25 C28 -48.3(10) . . . . ? C24 S1 C25 C28 59.2(10) . . . . ? O2 S1 C25 C27 -172.2(7) . . . . ? C24 S1 C25 C27 -64.6(9) . . . . ? O2 S1 C25 C26 72.4(7) . . . . ? C24 S1 C25 C26 -180.0(7) . . . . ? O4 S2 C29 F1 -170.0(19) . . . . ? O3 S2 C29 F1 -43.3(19) . . . . ? O5 S2 C29 F1 66(2) . . . . ? O4 S2 C29 F3 -47.2(18) . . . . ? O3 S2 C29 F3 79.5(16) . . . . ? O5 S2 C29 F3 -171(2) . . . . ? O4 S2 C29 F2 66.8(19) . . . . ? O3 S2 C29 F2 -166.5(14) . . . . ? O5 S2 C29 F2 -57(2) . . . . ? O4' S2' C29' F1' 60(2) . . . . ? O3' S2' C29' F1' -164.6(18) . . . . ? O5' S2' C29' F1' -57(2) . . . . ? O4' S2' C29' F3' -78(3) . . . . ? O3' S2' C29' F3' 58(2) . . . . ? O5' S2' C29' F3' 166(2) . . . . ? O4' S2' C29' F2' 175(2) . . . . ? O3' S2' C29' F2' -49(2) . . . . ? O5' S2' C29' F2' 59(2) . . . . ? C30 Cl C30 Cl 0.0 2_576 . . 2_576 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.706 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.168 \|/ @ @ #--------------------------oOOo-(_)-oOOo--------------------------- Dr. Frank Hampel * Tel: (49)-(0)9131-85-22988 Institut fuer Organische Chemie * Fax: (49)-(0)9131-85-26865 Henkestr. 42, D-91054 Erlangen * email: hampel@organik.uni-erlangen.de