Supplementary Information (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_contact_author 'Giuseppe Fachinetti' _publ_contact_author ; Giuseppe Fachinetti Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; _publ_contact_author_phone '+39 050 918223' _publ_contact_author_fax '+39 050 20237' _publ_contact_author_email 'funfac@dcci.unipi.it' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The acylation of an acyl complex resulting in a labile OCO tridentate ligand ; loop_ _publ_author_name _publ_author_address 'Funaioli, Tiziana' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; 'Falchi, Giulia' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; 'Marchetti, Fabio' ; Dipartimento di Ingegneria Chimica, dei Materiali e delle Materie Prime e Metallurgia Universita'' "La Sapienza" di Roma Via del Castro Laurenziano, 7 I-00161 Roma Italy ; 'Fachinetti, Giuseppe' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; #=========================================================================== data_ruprop _database_code_CSD 170235 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dicarbonyl-\m3-propylidindipropionate-trifluoromethansulfonate ruthenium(ii) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(CF3SO3)(CO)2Ru[CEt(OC(O)Et)2]' _chemical_formula_sum 'C12 H15 F3 O9 Ru S' _chemical_formula_weight 493.37 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' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 '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 12.597(2) _cell_length_b 10.299(2) _cell_length_c 14.314(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.640(10) _cell_angle_gamma 90.00 _cell_volume 1818.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 9.965 _cell_measurement_theta_max 24.859 _exptl_crystal_description 'Prism sl. flat. on (-1 0 1)' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.40 mm _exptl_crystal_size_mid 0.36 mm _exptl_crystal_size_min 0.18 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6566 _exptl_absorpt_correction_T_max 0.6755 _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 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4101 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3195 _reflns_number_gt 2367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material ? _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^)+(0.0392P)^2^+0.3254P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3195 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 Ru Ru 0.22175(3) 0.11438(4) 0.13046(3) 0.03420(11) Uani 1 1 d . . . C1 C 0.2388(4) 0.2938(5) 0.1274(4) 0.0497(12) Uani 1 1 d . . . O1 O 0.2493(4) 0.4029(4) 0.1190(4) 0.0806(13) Uani 1 1 d . . . C2 C 0.1073(3) 0.1303(5) 0.0255(3) 0.0407(10) Uani 1 1 d . . . O2 O 0.0376(3) 0.1407(4) -0.0383(3) 0.0615(10) Uani 1 1 d . . . O3 O 0.2133(3) -0.0901(3) 0.1223(2) 0.0436(7) Uani 1 1 d . . . C3 C 0.2622(3) -0.1329(4) 0.0631(3) 0.0391(10) Uani 1 1 d . . . C4 C 0.2500(4) -0.2720(5) 0.0315(4) 0.0532(13) Uani 1 1 d . . . H4A H 0.2783 -0.3269 0.0859 0.069 Uiso 1 1 calc R . . H4B H 0.1733 -0.2909 0.0118 0.069 Uiso 1 1 calc R . . C5 C 0.3050(5) -0.3082(6) -0.0483(5) 0.0758(19) Uani 1 1 d . . . H5A H 0.2926 -0.3985 -0.0635 0.099 Uiso 1 1 calc R . . H5B H 0.3815 -0.2928 -0.0292 0.099 Uiso 1 1 calc R . . H5C H 0.2763 -0.2566 -0.1035 0.099 Uiso 1 1 calc R . . O4 O 0.3247(3) -0.0602(3) 0.0210(2) 0.0428(7) Uani 1 1 d . . . C6 C 0.3383(3) 0.0769(4) 0.0545(3) 0.0377(10) Uani 1 1 d . . . C7 C 0.3652(4) 0.1518(5) -0.0286(4) 0.0512(12) Uani 1 1 d . . . H7A H 0.4285 0.1130 -0.0462 0.067 Uiso 1 1 calc R . . H7B H 0.3840 0.2401 -0.0081 0.067 Uiso 1 1 calc R . . C8 C 0.2742(5) 0.1559(7) -0.1160(4) 0.0737(19) Uani 1 1 d . . . H8A H 0.2969 0.2055 -0.1653 0.096 Uiso 1 1 calc R . . H8B H 0.2115 0.1956 -0.0997 0.096 Uiso 1 1 calc R . . H8C H 0.2567 0.0690 -0.1383 0.096 Uiso 1 1 calc R . . O5 O 0.4439(2) 0.0704(4) 0.1235(2) 0.0460(8) Uani 1 1 d . . . C9 C 0.4412(4) 0.0724(5) 0.2143(3) 0.0442(11) Uani 1 1 d . . . C10 C 0.5494(4) 0.0607(6) 0.2805(4) 0.0624(15) Uani 1 1 d . . . H10A H 0.5895 0.1405 0.2780 0.081 Uiso 1 1 calc R . . H10B H 0.5898 -0.0091 0.2583 0.081 Uiso 1 1 calc R . . C11 C 0.5421(5) 0.0344(7) 0.3820(4) 0.077(2) Uani 1 1 d . . . H11A H 0.6137 0.0277 0.4205 0.100 Uiso 1 1 calc R . . H11B H 0.5038 -0.0456 0.3854 0.100 Uiso 1 1 calc R . . H11C H 0.5039 0.1041 0.4053 0.100 Uiso 1 1 calc R . . O6 O 0.3563(2) 0.0874(3) 0.2429(2) 0.0460(8) Uani 1 1 d . . . O7 O 0.1235(3) 0.1058(4) 0.2391(2) 0.0537(9) Uani 1 1 d . . . O8 O -0.0546(3) 0.1584(5) 0.1483(3) 0.0845(15) Uani 1 1 d . . . O9 O 0.0163(4) 0.2677(4) 0.2997(4) 0.0813(14) Uani 1 1 d . . . S S 0.01559(10) 0.15586(13) 0.24013(10) 0.0496(3) Uani 1 1 d . . . C12 C -0.0386(5) 0.0277(6) 0.3043(4) 0.0654(16) Uani 1 1 d . . . F1 F -0.0332(4) -0.0857(4) 0.2648(4) 0.1063(15) Uani 1 1 d . . . F2 F -0.1421(3) 0.0513(5) 0.3054(3) 0.1054(15) Uani 1 1 d . . . F3 F 0.0158(4) 0.0177(5) 0.3930(3) 0.0976(14) Uani 1 1 d . . . 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 Ru 0.03237(17) 0.03180(17) 0.03892(18) -0.00032(18) 0.00838(12) 0.00223(17) C1 0.053(3) 0.043(3) 0.054(3) -0.010(2) 0.010(2) 0.000(2) O1 0.096(3) 0.033(2) 0.108(4) -0.006(2) 0.009(3) -0.006(2) C2 0.037(2) 0.041(3) 0.046(2) 0.002(2) 0.0119(19) -0.001(2) O2 0.0472(19) 0.078(3) 0.054(2) 0.005(2) -0.0016(17) -0.0006(19) O3 0.0473(17) 0.0336(18) 0.0539(18) 0.0022(15) 0.0199(15) 0.0014(15) C3 0.040(2) 0.034(2) 0.041(2) 0.000(2) 0.0034(19) 0.0036(19) C4 0.055(3) 0.038(3) 0.065(3) -0.011(2) 0.006(3) 0.000(2) C5 0.078(4) 0.058(4) 0.094(5) -0.028(4) 0.026(4) 0.001(3) O4 0.0441(17) 0.0380(16) 0.0492(18) -0.0067(15) 0.0160(14) -0.0002(14) C6 0.032(2) 0.037(2) 0.043(2) -0.0027(19) 0.0064(18) -0.0015(18) C7 0.045(2) 0.055(3) 0.058(3) 0.006(2) 0.020(2) -0.006(2) C8 0.064(3) 0.102(5) 0.057(3) 0.025(3) 0.017(3) -0.005(4) O5 0.0301(14) 0.057(2) 0.0503(18) 0.0011(16) 0.0069(13) -0.0002(14) C9 0.041(2) 0.037(2) 0.052(3) -0.001(2) 0.003(2) -0.003(2) C10 0.042(3) 0.064(3) 0.073(4) -0.002(3) -0.009(3) 0.004(3) C11 0.075(4) 0.075(5) 0.066(4) -0.012(3) -0.020(3) 0.013(4) O6 0.0412(16) 0.052(2) 0.0434(17) 0.0004(15) 0.0046(14) 0.0053(15) O7 0.0460(17) 0.071(2) 0.0474(18) 0.009(2) 0.0185(14) 0.0163(19) O8 0.055(2) 0.127(4) 0.071(3) 0.034(3) 0.014(2) 0.030(3) O9 0.090(3) 0.048(2) 0.116(4) -0.011(3) 0.046(3) 0.010(2) S 0.0476(6) 0.0495(7) 0.0575(7) 0.0091(6) 0.0243(6) 0.0119(6) C12 0.065(4) 0.064(4) 0.068(4) 0.004(3) 0.016(3) -0.012(3) F1 0.133(4) 0.055(3) 0.126(4) -0.014(2) 0.014(3) -0.029(2) F2 0.069(2) 0.125(4) 0.132(4) 0.023(3) 0.044(2) -0.016(3) F3 0.108(3) 0.120(4) 0.061(2) 0.025(2) 0.009(2) -0.036(3) _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 Ru C1 1.861(6) . ? Ru C2 1.868(4) . ? Ru C6 2.033(4) . ? Ru O6 2.107(3) . ? Ru O3 2.111(3) . ? Ru O7 2.176(3) . ? C1 O1 1.141(7) . ? C2 O2 1.137(5) . ? O3 C3 1.225(5) . ? C3 O4 1.317(5) . ? C3 C4 1.501(6) . ? C4 C5 1.498(8) . ? O4 C6 1.489(5) . ? C6 O5 1.490(5) . ? C6 C7 1.513(6) . ? C7 C8 1.518(7) . ? O5 C9 1.308(6) . ? C9 O6 1.229(6) . ? C9 C10 1.499(6) . ? C10 C11 1.500(8) . ? O7 S 1.457(3) . ? O8 S 1.429(4) . ? O9 S 1.432(5) . ? S C12 1.818(6) . ? C12 F1 1.305(8) . ? C12 F3 1.319(7) . ? C12 F2 1.329(7) . ? 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 C1 Ru C2 88.2(2) . . ? C1 Ru C6 94.4(2) . . ? C2 Ru C6 96.35(18) . . ? C1 Ru O6 94.01(19) . . ? C2 Ru O6 175.88(17) . . ? C6 Ru O6 80.02(15) . . ? C1 Ru O3 173.57(18) . . ? C2 Ru O3 91.20(18) . . ? C6 Ru O3 79.29(15) . . ? O6 Ru O3 86.24(13) . . ? C1 Ru O7 98.2(2) . . ? C2 Ru O7 96.91(16) . . ? C6 Ru O7 161.97(16) . . ? O6 Ru O7 86.24(12) . . ? O3 Ru O7 88.26(14) . . ? O1 C1 Ru 175.3(5) . . ? O2 C2 Ru 179.6(5) . . ? C3 O3 Ru 111.7(3) . . ? O3 C3 O4 122.8(4) . . ? O3 C3 C4 121.1(4) . . ? O4 C3 C4 116.0(4) . . ? C5 C4 C3 115.6(5) . . ? C3 O4 C6 115.6(3) . . ? O4 C6 O5 101.6(3) . . ? O4 C6 C7 105.0(4) . . ? O5 C6 C7 103.4(3) . . ? O4 C6 Ru 107.7(3) . . ? O5 C6 Ru 107.4(3) . . ? C7 C6 Ru 128.6(3) . . ? C6 C7 C8 114.2(4) . . ? C9 O5 C6 117.3(3) . . ? O6 C9 O5 122.1(4) . . ? O6 C9 C10 122.8(5) . . ? O5 C9 C10 115.0(4) . . ? C9 C10 C11 113.6(5) . . ? C9 O6 Ru 112.5(3) . . ? S O7 Ru 131.2(2) . . ? O8 S O9 117.5(3) . . ? O8 S O7 113.7(2) . . ? O9 S O7 113.4(3) . . ? O8 S C12 104.6(3) . . ? O9 S C12 104.0(3) . . ? O7 S C12 101.2(3) . . ? F1 C12 F3 106.6(6) . . ? F1 C12 F2 107.8(6) . . ? F3 C12 F2 108.8(5) . . ? F1 C12 S 111.9(4) . . ? F3 C12 S 111.6(4) . . ? F2 C12 S 110.0(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.790 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.079 #======END