# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1401 data_global #=========================================================================== _publ_contact_autor ; Giuseppe Fachinetti Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; _publ_contact_author_phone '050 918223' _publ_contact_author_fax '050 20237' _publ_contact_author_email 'funfac@dcci.unipi.it' _publ_requested_journal 'J. Chem. Soc., Chem. Comm.' _publ_requested_coeditor_name '' _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reactive intermediates from carbonylation of ruthenium(I) carbonyl carboxylates: Isolation, molecular structures and chemical properties of dinuclear unbridged ruthenium carbonyl trifluoroacetates ; loop_ _publ_author_names _publ_author_address 'Funaioli, Tiziana' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; 'Marchetti, Fabio' ; Dipartimento di Ingegneria Chimica, dei Materiali, delle Materie Prime e Metallurgia Universita' "La Sapienza" di Roma Via del Castro Laurenziano, 7 I-00195 Roma Italy ; 'Fachinetti, Giuseppe' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; #============================================================================== data_diru _audit_creation_method SHELXL-97 _chemical_name_systematic ; Pentacarbonylruthenium(0)(ditrifluoroacetato)tricarbonylruthenium(ii) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ru(CO)5Ru(CO)3(OCOCF3)2' _chemical_formula_sum 'C12 F6 O12 Ru2' _chemical_formula_weight 652.26 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' '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' '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)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1510(10) _cell_length_b 15.7400(10) _cell_length_c 15.8570(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.460(10) _cell_angle_gamma 90.00 _cell_volume 2025.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Stick' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max '0.35 mm' _exptl_crystal_size_mid '0.18 mm' _exptl_crystal_size_min '0.09 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.4239 _exptl_absorpt_correction_T_max 0.4889 _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 'Siemens P4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4714 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3565 _reflns_number_gt 2826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0566P)^2^+8.4696P] 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 3565 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.467 _refine_ls_shift/su_mean 0.023 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 Ru1 Ru -0.11269(7) 0.70928(4) 0.32655(4) 0.04309(18) Uani 1 1 d . . . Ru2 Ru 0.12085(7) 0.69353(4) 0.20441(4) 0.03994(17) Uani 1 1 d . . . C1 C -0.2808(11) 0.7098(6) 0.4119(5) 0.061(2) Uani 1 1 d . . . O1 O -0.3738(9) 0.7086(5) 0.4585(5) 0.093(2) Uani 1 1 d . . . C2 C -0.2682(9) 0.7269(5) 0.2255(5) 0.0472(17) Uani 1 1 d . . . O2 O -0.3542(7) 0.7387(4) 0.1676(4) 0.0615(14) Uani 1 1 d . . . C3 C -0.0708(11) 0.8321(6) 0.3314(5) 0.058(2) Uani 1 1 d . . . O3 O -0.0454(11) 0.9026(4) 0.3308(4) 0.090(2) Uani 1 1 d . . . C4 C 0.0814(10) 0.6910(6) 0.4078(5) 0.057(2) Uani 1 1 d . . . O4 O 0.1919(8) 0.6793(5) 0.4538(4) 0.084(2) Uani 1 1 d . . . C5 C -0.1314(10) 0.5844(5) 0.3078(5) 0.0531(18) Uani 1 1 d . . . O5 O -0.1427(8) 0.5143(4) 0.3014(4) 0.0715(17) Uani 1 1 d . . . C6 C 0.0316(9) 0.7885(5) 0.1452(5) 0.0488(17) Uani 1 1 d . . . O6 O -0.0172(8) 0.8477(4) 0.1093(4) 0.0696(17) Uani 1 1 d . . . C7 C 0.2711(9) 0.7658(5) 0.2681(5) 0.0521(18) Uani 1 1 d . . . O7 O 0.3598(8) 0.8101(4) 0.3049(5) 0.082(2) Uani 1 1 d . . . C8 C 0.2714(9) 0.6742(5) 0.1163(5) 0.0501(17) Uani 1 1 d . . . O8 O 0.3540(7) 0.6681(5) 0.0645(4) 0.0729(18) Uani 1 1 d . . . O9 O 0.2065(6) 0.5837(3) 0.2720(3) 0.0503(12) Uani 1 1 d . . . C9 C 0.3582(9) 0.5710(5) 0.2936(5) 0.0526(18) Uani 1 1 d . A . O10 O 0.4748(7) 0.6153(4) 0.2807(5) 0.082(2) Uani 1 1 d . . . C10 C 0.3921(12) 0.4879(7) 0.3416(8) 0.086(3) Uani 1 1 d . . . F1A F 0.5433(9) 0.4726(8) 0.3670(8) 0.102(4) Uiso 0.591(16) 1 d PG A 1 F2A F 0.3031(13) 0.4859(8) 0.4122(7) 0.101(4) Uiso 0.591(16) 1 d PG A 1 F3A F 0.3293(16) 0.4195(9) 0.2952(7) 0.125(6) Uiso 0.591(16) 1 d PG A 1 F1B F 0.5195(17) 0.5004(10) 0.4029(10) 0.089(5) Uiso 0.409(16) 1 d PG A 2 F2B F 0.2755(13) 0.4508(10) 0.3682(11) 0.092(6) Uiso 0.409(16) 1 d PG A 2 F3B F 0.467(3) 0.4333(15) 0.2846(10) 0.158(10) Uiso 0.409(16) 1 d PG A 2 O11 O -0.0513(6) 0.6079(3) 0.1440(3) 0.0468(11) Uani 1 1 d . . . C11 C -0.1040(8) 0.6163(5) 0.0674(5) 0.0444(16) Uani 1 1 d . B . O12 O -0.0644(8) 0.6687(4) 0.0163(4) 0.0685(16) Uani 1 1 d . . . C12 C -0.2374(10) 0.5501(5) 0.0387(6) 0.060(2) Uani 1 1 d . . . F4A F -0.3216(14) 0.5734(7) -0.0354(5) 0.100(4) Uiso 0.609(13) 1 d PG B 1 F5A F -0.1725(11) 0.4753(6) 0.0285(7) 0.091(4) Uiso 0.609(13) 1 d PG B 1 F6A F -0.3514(12) 0.5428(6) 0.0949(5) 0.084(3) Uiso 0.609(13) 1 d PG B 1 F4B F -0.1793(17) 0.5011(9) -0.0264(9) 0.083(5) Uiso 0.391(13) 1 d PG B 2 F5B F -0.276(2) 0.4965(11) 0.0956(7) 0.104(6) Uiso 0.391(13) 1 d PG B 2 F6B F -0.3732(19) 0.5871(9) 0.0016(11) 0.099(6) Uiso 0.391(13) 1 d PG B 2 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 Ru1 0.0396(3) 0.0486(3) 0.0414(3) -0.0046(2) 0.0054(2) -0.0068(3) Ru2 0.0360(3) 0.0420(3) 0.0419(3) -0.0016(2) 0.0043(2) -0.0059(2) C1 0.055(5) 0.071(6) 0.057(5) -0.008(4) 0.010(4) -0.009(4) O1 0.075(5) 0.131(7) 0.080(5) -0.016(4) 0.041(4) -0.021(5) C2 0.040(4) 0.047(4) 0.055(5) -0.006(3) 0.005(4) -0.004(3) O2 0.051(3) 0.068(4) 0.063(4) 0.000(3) -0.007(3) -0.006(3) C3 0.063(5) 0.066(5) 0.047(4) -0.010(4) 0.005(4) -0.012(4) O3 0.132(7) 0.058(4) 0.079(5) -0.008(3) 0.011(4) -0.025(4) C4 0.053(5) 0.071(5) 0.047(4) -0.006(4) 0.006(4) -0.009(4) O4 0.063(4) 0.128(6) 0.057(4) -0.003(4) -0.010(3) 0.006(4) C5 0.049(5) 0.051(5) 0.061(5) 0.007(4) 0.011(4) -0.009(4) O5 0.068(4) 0.054(4) 0.094(5) 0.011(3) 0.016(3) -0.004(3) C6 0.049(4) 0.051(4) 0.046(4) -0.005(3) 0.006(3) -0.004(4) O6 0.085(4) 0.053(3) 0.072(4) 0.009(3) 0.015(3) 0.013(3) C7 0.044(4) 0.054(4) 0.059(5) 0.000(4) 0.005(4) -0.012(4) O7 0.074(4) 0.079(4) 0.092(5) -0.021(4) -0.004(4) -0.033(4) C8 0.040(4) 0.054(4) 0.057(5) -0.006(3) 0.005(3) -0.003(3) O8 0.051(3) 0.103(5) 0.068(4) -0.018(4) 0.019(3) -0.003(3) O9 0.037(3) 0.052(3) 0.062(3) 0.007(2) 0.000(2) -0.007(2) C9 0.039(4) 0.050(4) 0.068(5) 0.001(4) 0.000(3) -0.005(3) O10 0.044(3) 0.076(4) 0.123(6) 0.027(4) -0.002(3) -0.015(3) C10 0.048(5) 0.095(8) 0.113(9) 0.031(7) -0.003(5) -0.006(5) O11 0.042(3) 0.052(3) 0.046(3) -0.005(2) 0.000(2) -0.009(2) C11 0.036(4) 0.044(4) 0.052(4) -0.006(3) 0.003(3) 0.002(3) O12 0.081(4) 0.070(4) 0.052(3) 0.002(3) -0.009(3) -0.012(3) C12 0.051(5) 0.060(5) 0.067(5) -0.013(4) -0.010(4) 0.003(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 Ru1 C4 1.964(9) . ? Ru1 C3 1.964(9) . ? Ru1 C2 1.966(8) . ? Ru1 C5 1.991(9) . ? Ru1 C1 2.016(8) . ? Ru1 Ru2 2.8526(8) . ? Ru2 C6 1.875(8) . ? Ru2 C7 1.891(8) . ? Ru2 C8 1.969(8) . ? Ru2 O11 2.109(5) . ? Ru2 O9 2.118(5) . ? C1 O1 1.107(10) . ? C2 O2 1.116(9) . ? C3 O3 1.128(10) . ? C4 O4 1.119(10) . ? C5 O5 1.112(10) . ? C6 O6 1.143(9) . ? C7 O7 1.127(9) . ? C8 O8 1.113(9) . ? O9 C9 1.267(9) . ? C9 O10 1.212(9) . ? C9 C10 1.525(13) . ? C10 F2B 1.224(14) . ? C10 F1A 1.283(12) . ? C10 F1B 1.367(15) . ? C10 F3A 1.375(15) . ? C10 F2A 1.391(14) . ? C10 F3B 1.425(18) . ? O11 C11 1.257(8) . ? C11 O12 1.222(9) . ? C11 C12 1.543(10) . ? C12 F5B 1.295(14) . ? C12 F5A 1.307(11) . ? C12 F6B 1.337(14) . ? C12 F6A 1.352(11) . ? C12 F4A 1.355(11) . ? C12 F4B 1.406(13) . ? 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 C4 Ru1 C3 89.6(4) . . ? C4 Ru1 C2 166.4(3) . . ? C3 Ru1 C2 89.4(3) . . ? C4 Ru1 C5 89.9(3) . . ? C3 Ru1 C5 171.2(3) . . ? C2 Ru1 C5 89.0(3) . . ? C4 Ru1 C1 96.7(3) . . ? C3 Ru1 C1 95.5(3) . . ? C2 Ru1 C1 96.9(3) . . ? C5 Ru1 C1 93.3(3) . . ? C4 Ru1 Ru2 83.4(2) . . ? C3 Ru1 Ru2 89.3(2) . . ? C2 Ru1 Ru2 83.1(2) . . ? C5 Ru1 Ru2 81.9(2) . . ? C1 Ru1 Ru2 175.2(3) . . ? C6 Ru2 C7 89.3(3) . . ? C6 Ru2 C8 90.4(3) . . ? C7 Ru2 C8 93.2(3) . . ? C6 Ru2 O11 94.2(3) . . ? C7 Ru2 O11 174.8(3) . . ? C8 Ru2 O11 90.7(3) . . ? C6 Ru2 O9 176.4(3) . . ? C7 Ru2 O9 93.2(3) . . ? C8 Ru2 O9 92.0(3) . . ? O11 Ru2 O9 83.18(19) . . ? C6 Ru2 Ru1 91.0(2) . . ? C7 Ru2 Ru1 91.5(2) . . ? C8 Ru2 Ru1 175.1(2) . . ? O11 Ru2 Ru1 84.58(13) . . ? O9 Ru2 Ru1 86.35(14) . . ? O1 C1 Ru1 178.7(8) . . ? O2 C2 Ru1 178.2(7) . . ? O3 C3 Ru1 177.2(8) . . ? O4 C4 Ru1 179.0(8) . . ? O5 C5 Ru1 176.5(7) . . ? O6 C6 Ru2 177.5(7) . . ? O7 C7 Ru2 178.6(8) . . ? O8 C8 Ru2 175.7(8) . . ? C9 O9 Ru2 122.1(5) . . ? O10 C9 O9 128.7(8) . . ? O10 C9 C10 118.1(8) . . ? O9 C9 C10 113.3(7) . . ? F2B C10 F1A 123.9(12) . . ? F2B C10 F1B 112.7(11) . . ? F1A C10 F1B 33.0(7) . . ? F2B C10 F3A 63.2(9) . . ? F1A C10 F3A 108.5(10) . . ? F1B C10 F3A 135.3(12) . . ? F2B C10 F2A 39.7(8) . . ? F1A C10 F2A 107.6(9) . . ? F1B C10 F2A 81.4(9) . . ? F3A C10 F2A 102.5(8) . . ? F2B C10 F3B 108.9(12) . . ? F1A C10 F3B 68.2(10) . . ? F1B C10 F3B 101.2(10) . . ? F3A C10 F3B 49.3(9) . . ? F2A C10 F3B 141.6(14) . . ? F2B C10 C9 118.1(11) . . ? F1A C10 C9 116.1(10) . . ? F1B C10 C9 108.7(11) . . ? F3A C10 C9 111.3(10) . . ? F2A C10 C9 109.8(10) . . ? F3B C10 C9 105.5(13) . . ? C11 O11 Ru2 121.6(5) . . ? O12 C11 O11 128.7(7) . . ? O12 C11 C12 119.0(7) . . ? O11 C11 C12 112.4(7) . . ? F5B C12 F5A 68.2(8) . . ? F5B C12 F6B 110.2(10) . . ? F5A C12 F6B 131.7(11) . . ? F5B C12 F6A 42.1(8) . . ? F5A C12 F6A 108.5(8) . . ? F6B C12 F6A 74.6(8) . . ? F5B C12 F4A 130.1(11) . . ? F5A C12 F4A 108.3(7) . . ? F6B C12 F4A 33.8(7) . . ? F6A C12 F4A 105.8(7) . . ? F5B C12 F4B 106.0(9) . . ? F5A C12 F4B 41.1(6) . . ? F6B C12 F4B 103.7(9) . . ? F6A C12 F4B 137.6(10) . . ? F4A C12 F4B 71.9(7) . . ? F5B C12 C11 116.4(10) . . ? F5A C12 C11 111.3(8) . . ? F6B C12 C11 111.5(10) . . ? F6A C12 C11 111.9(7) . . ? F4A C12 C11 110.9(8) . . ? F4B C12 C11 108.0(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.360 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.116 #==END data_rct _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[tetracarbonyl(trifluoroacetato)ruthenium(i)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ru(CO)4(OCOCF3)]2' _chemical_formula_sum 'C6 F3 O6 Ru' _chemical_formula_weight 326.13 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' '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pccn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 9.0200(10) _cell_length_b 12.716(2) _cell_length_c 17.748(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2035.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 2.018 _cell_measurement_theta_max 13.635 _exptl_crystal_description 'Prismatic splinter' _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max '0.28 mm' _exptl_crystal_size_mid '0.21 mm' _exptl_crystal_size_min '0.13 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.595 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2849 _exptl_absorpt_correction_T_max 0.3341 _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 'Siemens P4' _diffrn_measurement_method '\w/2\q 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 2140 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 23.98 _reflns_number_total 1595 _reflns_number_gt 964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0782P)^2^+2.2272P] 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 1595 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.22857(8) 0.86045(8) 0.15997(5) 0.0704(4) Uani 1 1 d . . . C1 C 0.0423(12) 0.8356(10) 0.2047(6) 0.081(3) Uani 1 1 d . . . O1 O -0.0689(9) 0.8179(8) 0.2324(5) 0.106(3) Uani 1 1 d . . . C2 C 0.2039(13) 1.0152(13) 0.1555(8) 0.093(4) Uani 1 1 d . . . O2 O 0.1914(11) 1.1028(10) 0.1522(7) 0.121(3) Uani 1 1 d . . . C3 C 0.1408(11) 0.8396(10) 0.0609(6) 0.077(3) Uani 1 1 d . . . O3 O 0.0853(10) 0.8275(8) 0.0040(5) 0.115(3) Uani 1 1 d . . . C4 C 0.3173(12) 0.8655(10) 0.2599(6) 0.083(3) Uani 1 1 d . . . O4 O 0.3643(10) 0.8655(9) 0.3197(5) 0.115(3) Uani 1 1 d . . . O5 O 0.4339(7) 0.8721(6) 0.1043(4) 0.0747(19) Uani 1 1 d . . . C5 C 0.5399(11) 0.9287(11) 0.1266(7) 0.079(3) Uani 1 1 d . A . O6 O 0.5503(11) 0.9766(9) 0.1832(6) 0.121(4) Uani 1 1 d . . . C6 C 0.6679(12) 0.9341(13) 0.0706(8) 0.103(4) Uani 1 1 d . . . F1A F 0.6762(16) 1.0335(8) 0.0449(8) 0.133(6) Uiso 0.630(16) 1 d PG A 1 F2A F 0.7964(15) 0.9117(11) 0.1035(7) 0.132(6) Uiso 0.630(16) 1 d PG A 1 F3A F 0.6525(13) 0.8715(9) 0.0108(6) 0.112(5) Uiso 0.630(16) 1 d PG A 1 F1B F 0.725(3) 0.8136(11) 0.0725(13) 0.150(11) Uiso 0.370(16) 1 d PG . 2 F2B F 0.6389(17) 0.9399(14) 0.0039(8) 0.085(6) Uiso 0.370(16) 1 d PG A 2 F3B F 0.793(2) 0.9736(15) 0.0939(9) 0.098(7) Uiso 0.370(16) 1 d PG A 2 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 0.0461(5) 0.1034(7) 0.0615(5) -0.0039(5) -0.0007(4) 0.0001(4) C1 0.054(6) 0.118(10) 0.071(6) 0.009(7) -0.002(5) 0.001(6) O1 0.063(5) 0.157(9) 0.099(6) 0.009(6) 0.016(4) 0.003(5) C2 0.063(7) 0.113(10) 0.101(9) -0.003(9) 0.004(7) 0.011(7) O2 0.089(6) 0.115(8) 0.157(9) -0.007(7) 0.006(6) 0.019(6) C3 0.062(6) 0.102(9) 0.067(6) 0.010(6) -0.011(5) -0.013(6) O3 0.110(7) 0.158(9) 0.076(5) 0.018(6) -0.023(5) -0.043(6) C4 0.064(6) 0.115(9) 0.069(7) -0.023(7) -0.001(5) 0.017(6) O4 0.082(6) 0.183(10) 0.079(5) -0.024(6) -0.009(4) 0.003(6) O5 0.051(4) 0.097(5) 0.076(4) -0.006(4) 0.001(3) -0.013(4) C5 0.054(6) 0.113(10) 0.070(6) 0.005(7) -0.006(5) -0.002(7) O6 0.095(6) 0.167(10) 0.101(6) -0.038(7) 0.006(5) -0.044(6) C6 0.052(6) 0.139(12) 0.119(10) -0.003(10) -0.025(7) 0.003(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 Ru C1 1.885(11) . ? Ru C4 1.946(12) . ? Ru C3 1.947(11) . ? Ru C2 1.982(16) . ? Ru O5 2.104(6) . ? Ru Ru 2.836(2) 2_565 ? C1 O1 1.140(13) . ? C2 O2 1.120(15) . ? C3 O3 1.137(12) . ? C4 O4 1.142(12) . ? O5 C5 1.261(13) . ? C5 O6 1.178(14) . ? C5 C6 1.525(17) . ? C6 F2B 1.216(17) . ? C6 F3B 1.299(19) . ? C6 F2A 1.329(14) . ? C6 F3A 1.336(16) . ? C6 F1A 1.346(17) . ? C6 F1B 1.62(2) . ? F1B F1B 1.68(3) 2_665 ? 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 C4 89.3(5) . . ? C1 Ru C3 89.7(4) . . ? C4 Ru C3 174.1(5) . . ? C1 Ru C2 94.7(5) . . ? C4 Ru C2 92.8(5) . . ? C3 Ru C2 93.1(5) . . ? C1 Ru O5 173.7(4) . . ? C4 Ru O5 93.6(4) . . ? C3 Ru O5 86.8(3) . . ? C2 Ru O5 90.6(4) . . ? C1 Ru Ru 87.5(4) . 2_565 ? C4 Ru Ru 88.7(4) . 2_565 ? C3 Ru Ru 85.4(4) . 2_565 ? C2 Ru Ru 177.3(4) . 2_565 ? O5 Ru Ru 87.1(2) . 2_565 ? O1 C1 Ru 178.0(11) . . ? O2 C2 Ru 179.0(14) . . ? O3 C3 Ru 177.8(10) . . ? O4 C4 Ru 176.9(12) . . ? C5 O5 Ru 124.1(7) . . ? O6 C5 O5 128.5(11) . . ? O6 C5 C6 118.2(11) . . ? O5 C5 C6 113.3(11) . . ? F2B C6 F3B 118.2(16) . . ? F2B C6 F2A 128.9(15) . . ? F3B C6 F2A 35.7(9) . . ? F2B C6 F3A 40.3(9) . . ? F3B C6 F3A 125.0(14) . . ? F2A C6 F3A 108.2(11) . . ? F2B C6 F1A 68.0(12) . . ? F3B C6 F1A 72.4(12) . . ? F2A C6 F1A 107.6(11) . . ? F3A C6 F1A 107.2(11) . . ? F2B C6 C5 118.4(12) . . ? F3B C6 C5 117.8(14) . . ? F2A C6 C5 111.4(12) . . ? F3A C6 C5 114.4(12) . . ? F1A C6 C5 107.8(13) . . ? F2B C6 F1B 98.3(13) . . ? F3B C6 F1B 94.9(11) . . ? F2A C6 F1B 60.8(10) . . ? F3A C6 F1B 58.9(10) . . ? F1A C6 F1B 151.6(15) . . ? C5 C6 F1B 100.6(14) . . ? C6 F1B F1B 177(2) . 2_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.856 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.103 #==END