# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1818 data_[h5-1-(COOEt)-2-Me-4-PhPhC5H2]Ru(CO)2I #------------------------------------------------------------------------------ _audit_creation_date 'Sat May 20 03:36:05 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 511.28 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H15 I O4 Ru ' _chemical_formula_moiety 'C17 H15 I O4 Ru ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.631(3) _cell_length_b 11.246(3) _cell_length_c 8.313(2) _cell_angle_alpha 98.76(2) _cell_angle_beta 101.23(2) _cell_angle_gamma 93.71(3) _cell_volume 868.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 198.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 19.8 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492.00 _exptl_absorpt_coefficient_mu 2.696 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 198.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.51 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -1 1 -1 -1 2 0 0 -2 _diffrn_reflns_number 4230 _reflns_number_total 3990 _reflns_number_gt 3645 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01360 _diffrn_orient_matrix_UB_12 -0.07804 _diffrn_orient_matrix_UB_13 0.04134 _diffrn_orient_matrix_UB_21 0.02078 _diffrn_orient_matrix_UB_22 0.04449 _diffrn_orient_matrix_UB_23 0.11705 _diffrn_orient_matrix_UB_31 -0.10342 _diffrn_orient_matrix_UB_32 0.01015 _diffrn_orient_matrix_UB_33 -0.00846 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.29432(3) 0.10457(2) 0.22384(4) 0.0355(1) Uani 1.00 d . . . Ru(1) Ru 0.24255(3) 0.33890(2) 0.26851(3) 0.01943(9) Uani 1.00 d . . . O(1) O -0.1303(3) 0.3527(3) 0.3754(4) 0.0388(9) Uani 1.00 d . . . O(2) O -0.1458(3) 0.1912(3) 0.1750(4) 0.0337(8) Uani 1.00 d . . . O(3) O 0.5564(3) 0.4204(3) 0.3440(4) 0.0409(9) Uani 1.00 d . . . O(4) O 0.2328(5) 0.3290(4) 0.6262(4) 0.059(1) Uani 1.00 d . . . C(1) C 0.0127(4) 0.3567(4) 0.1746(5) 0.0257(9) Uani 1.00 d . . . C(2) C 0.0661(4) 0.3082(4) 0.0306(4) 0.0275(9) Uani 1.00 d . . . C(3) C 0.1763(4) 0.3935(4) 0.0164(4) 0.0258(9) Uani 1.00 d . . . C(4) C 0.1895(4) 0.4977(3) 0.1457(4) 0.0238(9) Uani 1.00 d . . . C(5) C 0.0889(4) 0.4734(4) 0.2447(4) 0.0246(9) Uani 1.00 d . . . C(6) C -0.0951(4) 0.3012(4) 0.2533(5) 0.0282(9) Uani 1.00 d . . . C(7) C -0.2426(5) 0.1221(5) 0.2516(6) 0.045(1) Uani 1.00 d . . . C(8) C -0.1589(7) 0.0681(5) 0.3853(7) 0.053(2) Uani 1.00 d . . . C(9) C 0.0147(5) 0.1943(4) -0.0909(5) 0.035(1) Uani 1.00 d . . . C(10) C 0.2886(4) 0.6073(3) 0.1691(4) 0.0251(9) Uani 1.00 d . . . C(11) C 0.3132(5) 0.6908(4) 0.3168(5) 0.031(1) Uani 1.00 d . . . C(12) C 0.4090(5) 0.7938(4) 0.3358(6) 0.037(1) Uani 1.00 d . . . C(13) C 0.4776(5) 0.8134(4) 0.2104(6) 0.037(1) Uani 1.00 d . . . C(14) C 0.4544(6) 0.7307(5) 0.0645(6) 0.043(1) Uani 1.00 d . . . C(15) C 0.3603(5) 0.6287(4) 0.0428(5) 0.035(1) Uani 1.00 d . . . C(16) C 0.4394(4) 0.3849(4) 0.3190(4) 0.0263(9) Uani 1.00 d . . . C(17) C 0.2403(5) 0.3314(4) 0.4942(5) 0.032(1) Uani 1.00 d . . . H(1) H 0.2328 0.3836 -0.0656 0.0309 Uiso 1.00 calc . . . H(2) H 0.0746 0.5252 0.3404 0.0295 Uiso 1.00 calc . . . H(3) H -0.3040 0.1745 0.2967 0.0539 Uiso 1.00 calc . . . H(4) H -0.2976 0.0597 0.1696 0.0539 Uiso 1.00 calc . . . H(5) H -0.2214 0.0236 0.4347 0.0638 Uiso 1.00 calc . . . H(6) H -0.0975 0.0157 0.3402 0.0638 Uiso 1.00 calc . . . H(7) H -0.1038 0.1305 0.4673 0.0638 Uiso 1.00 calc . . . H(8) H -0.0597 0.1517 -0.0564 0.0419 Uiso 1.00 calc . . . H(9) H -0.0199 0.2136 -0.1979 0.0419 Uiso 1.00 calc . . . H(10) H 0.0910 0.1452 -0.0955 0.0419 Uiso 1.00 calc . . . H(11) H 0.2654 0.6780 0.4034 0.0378 Uiso 1.00 calc . . . H(12) H 0.4266 0.8506 0.4363 0.0445 Uiso 1.00 calc . . . H(13) H 0.5413 0.8841 0.2242 0.0445 Uiso 1.00 calc . . . H(14) H 0.5032 0.7440 -0.0211 0.0514 Uiso 1.00 calc . . . H(15) H 0.3440 0.5725 -0.0582 0.0417 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0442(2) 0.0235(2) 0.0375(2) 0.0036(1) 0.0057(1) 0.0050(1) Ru(1) 0.0241(2) 0.0228(2) 0.0120(2) 0.0010(1) 0.0063(1) 0.0021(1) O(1) 0.040(2) 0.042(2) 0.040(2) 0.000(1) 0.027(1) -0.001(1) O(2) 0.038(2) 0.035(2) 0.027(1) -0.007(1) 0.011(1) -0.001(1) O(3) 0.029(2) 0.055(2) 0.036(2) -0.001(1) 0.007(1) 0.001(1) O(4) 0.073(3) 0.090(3) 0.016(1) 0.005(2) 0.013(2) 0.013(2) C(1) 0.024(2) 0.033(2) 0.020(2) 0.004(1) 0.004(1) 0.004(1) C(2) 0.032(2) 0.034(2) 0.014(2) 0.000(2) 0.002(1) 0.001(1) C(3) 0.035(2) 0.031(2) 0.013(1) 0.003(2) 0.007(1) 0.005(1) C(4) 0.029(2) 0.026(2) 0.020(2) 0.008(1) 0.009(1) 0.006(1) C(5) 0.027(2) 0.029(2) 0.019(2) 0.003(1) 0.009(1) 0.001(1) C(6) 0.027(2) 0.032(2) 0.026(2) 0.001(1) 0.007(1) 0.003(2) C(7) 0.041(2) 0.048(3) 0.040(2) -0.017(2) 0.010(2) 0.001(2) C(8) 0.073(4) 0.042(3) 0.051(3) 0.004(2) 0.026(3) 0.013(2) C(9) 0.043(2) 0.040(2) 0.016(2) -0.005(2) 0.003(2) -0.005(2) C(10) 0.034(2) 0.024(2) 0.020(2) 0.004(1) 0.007(1) 0.009(1) C(11) 0.039(2) 0.032(2) 0.023(2) 0.001(2) 0.007(2) 0.006(2) C(12) 0.044(2) 0.028(2) 0.040(2) -0.005(2) 0.013(2) 0.005(2) C(13) 0.040(2) 0.029(2) 0.045(3) -0.001(2) 0.012(2) 0.011(2) C(14) 0.046(2) 0.050(3) 0.041(3) 0.000(2) 0.025(2) 0.015(2) C(15) 0.044(2) 0.034(2) 0.031(2) 0.003(2) 0.020(2) 0.007(2) C(16) 0.030(2) 0.032(2) 0.017(2) 0.004(1) 0.005(1) 0.004(1) C(17) 0.035(2) 0.042(2) 0.022(2) 0.004(2) 0.008(2) 0.006(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 3sigma(F^2^) is used only for calculating R-factors(gt). ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00240|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3645 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_shift/su_max 0.0090 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -2.24 _refine_diff_density_max 1.03 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I(1) Ru(1) 2.6973(4) 1_555 1_555 yes Ru(1) C(1) 2.232(4) 1_555 1_555 yes Ru(1) C(2) 2.308(4) 1_555 1_555 yes Ru(1) C(3) 2.258(4) 1_555 1_555 yes Ru(1) C(4) 2.228(4) 1_555 1_555 yes Ru(1) C(5) 2.187(4) 1_555 1_555 yes Ru(1) C(16) 1.880(4) 1_555 1_555 yes Ru(1) C(17) 1.895(4) 1_555 1_555 yes O(1) C(6) 1.209(5) 1_555 1_555 yes O(2) C(6) 1.320(5) 1_555 1_555 yes O(2) C(7) 1.472(5) 1_555 1_555 yes O(3) C(16) 1.139(5) 1_555 1_555 yes O(4) C(17) 1.118(5) 1_555 1_555 yes C(1) C(2) 1.440(5) 1_555 1_555 yes C(1) C(5) 1.440(5) 1_555 1_555 yes C(1) C(6) 1.484(5) 1_555 1_555 yes C(2) C(3) 1.418(5) 1_555 1_555 yes C(2) C(9) 1.495(5) 1_555 1_555 yes C(3) C(4) 1.445(5) 1_555 1_555 yes C(3) H(1) 0.950 1_555 1_555 no C(4) C(5) 1.427(5) 1_555 1_555 yes C(4) C(10) 1.472(5) 1_555 1_555 yes C(5) H(2) 0.950 1_555 1_555 no C(7) C(8) 1.474(8) 1_555 1_555 yes C(7) H(3) 0.950 1_555 1_555 no C(7) H(4) 0.950 1_555 1_555 no C(8) H(5) 0.950 1_555 1_555 no C(8) H(6) 0.950 1_555 1_555 no C(8) H(7) 0.950 1_555 1_555 no C(9) H(8) 0.950 1_555 1_555 no C(9) H(9) 0.950 1_555 1_555 no C(9) H(10) 0.950 1_555 1_555 no C(10) C(11) 1.397(6) 1_555 1_555 yes C(10) C(15) 1.406(5) 1_555 1_555 yes C(11) C(12) 1.402(6) 1_555 1_555 yes C(11) H(11) 0.950 1_555 1_555 no C(12) C(13) 1.375(6) 1_555 1_555 yes C(12) H(12) 0.950 1_555 1_555 no C(13) C(14) 1.383(7) 1_555 1_555 yes C(13) H(13) 0.950 1_555 1_555 no C(14) C(15) 1.382(7) 1_555 1_555 yes C(14) H(14) 0.950 1_555 1_555 no C(15) H(15) 0.950 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I(1) Ru(1) C(1) 110.5(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(2) 92.1(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(3) 108.53(10) 1_555 1_555 1_555 yes I(1) Ru(1) C(4) 145.86(9) 1_555 1_555 1_555 yes I(1) Ru(1) C(5) 148.6(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(16) 89.7(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(17) 89.1(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(2) 36.9(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(3) 61.5(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(4) 62.8(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(5) 38.0(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(16) 156.7(2) 1_555 1_555 1_555 yes C(1) Ru(1) C(17) 99.6(2) 1_555 1_555 1_555 yes C(2) Ru(1) C(3) 36.2(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(4) 62.1(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(5) 62.5(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(16) 135.3(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(17) 132.8(2) 1_555 1_555 1_555 yes C(3) Ru(1) C(4) 37.6(1) 1_555 1_555 1_555 yes C(3) Ru(1) C(5) 62.5(1) 1_555 1_555 1_555 yes C(3) Ru(1) C(16) 101.9(1) 1_555 1_555 1_555 yes C(3) Ru(1) C(17) 157.4(2) 1_555 1_555 1_555 yes C(4) Ru(1) C(5) 37.7(1) 1_555 1_555 1_555 yes C(4) Ru(1) C(16) 94.0(2) 1_555 1_555 1_555 yes C(4) Ru(1) C(17) 124.6(2) 1_555 1_555 1_555 yes C(5) Ru(1) C(16) 121.2(2) 1_555 1_555 1_555 yes C(5) Ru(1) C(17) 95.1(2) 1_555 1_555 1_555 yes C(16) Ru(1) C(17) 91.9(2) 1_555 1_555 1_555 yes C(6) O(2) C(7) 117.2(3) 1_555 1_555 1_555 yes Ru(1) C(1) C(2) 74.4(2) 1_555 1_555 1_555 yes Ru(1) C(1) C(5) 69.3(2) 1_555 1_555 1_555 yes Ru(1) C(1) C(6) 119.2(3) 1_555 1_555 1_555 yes C(2) C(1) C(5) 108.4(3) 1_555 1_555 1_555 yes C(2) C(1) C(6) 129.5(4) 1_555 1_555 1_555 yes C(5) C(1) C(6) 122.0(3) 1_555 1_555 1_555 yes Ru(1) C(2) C(1) 68.7(2) 1_555 1_555 1_555 yes Ru(1) C(2) C(3) 70.0(2) 1_555 1_555 1_555 yes Ru(1) C(2) C(9) 128.9(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 106.9(3) 1_555 1_555 1_555 yes C(1) C(2) C(9) 128.7(4) 1_555 1_555 1_555 yes C(3) C(2) C(9) 124.3(3) 1_555 1_555 1_555 yes Ru(1) C(3) C(2) 73.8(2) 1_555 1_555 1_555 yes Ru(1) C(3) C(4) 70.1(2) 1_555 1_555 1_555 yes Ru(1) C(3) H(1) 122.51 1_555 1_555 1_555 no C(2) C(3) C(4) 109.6(3) 1_555 1_555 1_555 yes C(2) C(3) H(1) 125.19 1_555 1_555 1_555 no C(4) C(3) H(1) 125.19 1_555 1_555 1_555 no Ru(1) C(4) C(3) 72.3(2) 1_555 1_555 1_555 yes Ru(1) C(4) C(5) 69.6(2) 1_555 1_555 1_555 yes Ru(1) C(4) C(10) 123.1(3) 1_555 1_555 1_555 yes C(3) C(4) C(5) 106.8(3) 1_555 1_555 1_555 yes C(3) C(4) C(10) 126.0(3) 1_555 1_555 1_555 yes O(1) C(6) O(2) 125.1(4) 1_555 1_555 1_555 yes O(1) C(6) C(1) 122.6(4) 1_555 1_555 1_555 yes O(2) C(6) C(1) 112.3(3) 1_555 1_555 1_555 yes O(2) C(7) C(8) 109.5(4) 1_555 1_555 1_555 yes O(2) C(7) H(3) 109.46 1_555 1_555 1_555 no O(2) C(7) H(4) 109.46 1_555 1_555 1_555 no C(8) C(7) H(3) 109.47 1_555 1_555 1_555 no C(8) C(7) H(4) 109.45 1_555 1_555 1_555 no H(3) C(7) H(4) 109.46 1_555 1_555 1_555 no C(7) C(8) H(5) 109.48 1_555 1_555 1_555 no C(7) C(8) H(6) 109.49 1_555 1_555 1_555 no C(7) C(8) H(7) 109.46 1_555 1_555 1_555 no H(5) C(8) H(6) 109.48 1_555 1_555 1_555 no H(5) C(8) H(7) 109.46 1_555 1_555 1_555 no H(6) C(8) H(7) 109.46 1_555 1_555 1_555 no C(2) C(9) H(8) 109.47 1_555 1_555 1_555 no C(2) C(9) H(9) 109.48 1_555 1_555 1_555 no C(2) C(9) H(10) 109.48 1_555 1_555 1_555 no H(8) C(9) H(9) 109.47 1_555 1_555 1_555 no C(12) C(11) H(11) 120.33 1_555 1_555 1_555 no C(11) C(12) C(13) 120.7(4) 1_555 1_555 1_555 yes C(11) C(12) H(12) 119.66 1_555 1_555 1_555 no C(13) C(12) H(12) 119.66 1_555 1_555 1_555 no C(12) C(13) C(14) 120.3(4) 1_555 1_555 1_555 yes C(12) C(13) H(13) 119.87 1_555 1_555 1_555 no C(14) C(13) H(13) 119.87 1_555 1_555 1_555 no C(13) C(14) C(15) 120.1(4) 1_555 1_555 1_555 yes C(13) C(14) H(14) 119.96 1_555 1_555 1_555 no C(15) C(14) H(14) 119.93 1_555 1_555 1_555 no C(10) C(15) C(14) 120.5(4) 1_555 1_555 1_555 yes C(10) C(15) H(15) 119.75 1_555 1_555 1_555 no C(14) C(15) H(15) 119.76 1_555 1_555 1_555 no Ru(1) C(16) O(3) 174.7(4) 1_555 1_555 1_555 yes Ru(1) C(17) O(4) 176.8(4) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ _publ_contact_author_name ' Shigetoshi Takahashi' _publ_contact_author_address ; 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; _publ_contact_author_email ' takahahsi@sanken.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-(0)6-6879-8455 ' _publ_contact_author_phone ' +81-(0)6-6879-8459 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chem. Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; Multiple Ligand Transfer Reaction to Planar-Chiral Cyclopentadienylruthenium Complexes Inducing Metal-Centered Chirality ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #===END data_[h5-1-(COOEt)-2,4-Me2PhC5H2]Ru(CO)(PMe3)I #------------------------------------------------------------------------------ _audit_creation_date 'Sat May 20 03:39:20 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 497.27 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H22 I O3 P Ru ' _chemical_formula_moiety 'C14 H22 I O3 P Ru ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.067(2) _cell_length_b 9.951(2) _cell_length_c 18.322(1) _cell_angle_alpha 90 _cell_angle_beta 100.410(8) _cell_angle_gamma 90 _cell_volume 1805.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.3 _cell_measurement_theta_max 17.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.650 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.500 _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968.00 _exptl_absorpt_coefficient_mu 2.671 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 223.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.06 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 -2 0 -2 -1 2 -1 0 _diffrn_reflns_number 4352 _reflns_number_total 4122 _reflns_number_gt 3889 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.011 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.09965 _diffrn_orient_matrix_UB_12 -0.01634 _diffrn_orient_matrix_UB_13 0.00986 _diffrn_orient_matrix_UB_21 -0.01642 _diffrn_orient_matrix_UB_22 -0.09915 _diffrn_orient_matrix_UB_23 -0.00108 _diffrn_orient_matrix_UB_31 -0.00023 _diffrn_orient_matrix_UB_32 -0.00099 _diffrn_orient_matrix_UB_33 -0.05460 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.00058(3) 0.10502(3) 0.17866(1) 0.0380(1) Uani 1.00 d . . . Ru(1) Ru -0.16902(3) 0.20754(3) 0.06010(2) 0.02538(10) Uani 1.00 d . . . P(1) P -0.2041(1) 0.38714(9) 0.13364(6) 0.0318(2) Uani 1.00 d . . . O(1) O -0.4622(4) 0.0110(3) 0.1447(2) 0.0495(9) Uani 1.00 d . . . O(2) O -0.5321(3) 0.2130(3) 0.0983(2) 0.0401(8) Uani 1.00 d . . . O(3) O 0.0550(4) 0.3557(4) 0.0083(2) 0.057(1) Uani 1.00 d . . . C(1) C -0.3700(4) 0.1039(3) 0.0454(2) 0.0299(9) Uani 1.00 d . . . C(2) C -0.2767(4) 0.0032(4) 0.0335(2) 0.0333(9) Uani 1.00 d . . . C(3) C -0.2161(4) 0.0447(4) -0.0270(2) 0.0365(10) Uani 1.00 d . . . C(4) C -0.2751(4) 0.1694(4) -0.0554(2) 0.0359(10) Uani 1.00 d . . . C(5) C -0.3692(4) 0.2074(4) -0.0100(2) 0.0335(9) Uani 1.00 d . . . C(6) C -0.2469(5) -0.1278(4) 0.0737(3) 0.043(1) Uani 1.00 d . . . C(7) C -0.2492(6) 0.2382(6) -0.1239(2) 0.052(1) Uani 1.00 d . . . C(8) C -0.0285(4) 0.3000(4) 0.0305(2) 0.0343(10) Uani 1.00 d . . . C(9) C -0.4570(4) 0.1007(4) 0.1020(2) 0.0345(10) Uani 1.00 d . . . C(10) C -0.6240(5) 0.2222(6) 0.1525(3) 0.054(1) Uani 1.00 d . . . C(11) C -0.6719(6) 0.3627(7) 0.1533(4) 0.065(2) Uani 1.00 d . . . C(12) C -0.3315(6) 0.5061(5) 0.0898(3) 0.051(1) Uani 1.00 d . . . C(13) C -0.0607(6) 0.4954(5) 0.1655(3) 0.051(1) Uani 1.00 d . . . C(14) C -0.2627(5) 0.3449(5) 0.2191(2) 0.043(1) Uani 1.00 d . . . H(1) H -0.1475 -0.0027 -0.0457 0.0438 Uiso 1.00 calc . . . H(2) H -0.4222 0.2870 -0.0151 0.0402 Uiso 1.00 calc . . . H(3) H -0.2987 -0.1342 0.1121 0.0514 Uiso 1.00 calc . . . H(4) H -0.2697 -0.2000 0.0398 0.0514 Uiso 1.00 calc . . . H(5) H -0.1535 -0.1323 0.0946 0.0514 Uiso 1.00 calc . . . H(6) H -0.1797 0.1923 -0.1426 0.0624 Uiso 1.00 calc . . . H(7) H -0.3295 0.2378 -0.1603 0.0624 Uiso 1.00 calc . . . H(8) H -0.2222 0.3284 -0.1124 0.0624 Uiso 1.00 calc . . . H(9) H -0.6986 0.1636 0.1383 0.0647 Uiso 1.00 calc . . . H(10) H -0.5771 0.1979 0.2004 0.0647 Uiso 1.00 calc . . . H(11) H -0.5968 0.4209 0.1671 0.0781 Uiso 1.00 calc . . . H(12) H -0.7188 0.3864 0.1053 0.0781 Uiso 1.00 calc . . . H(13) H -0.7309 0.3710 0.1881 0.0781 Uiso 1.00 calc . . . H(14) H -0.3485 0.5703 0.1253 0.0610 Uiso 1.00 calc . . . H(15) H -0.2998 0.5508 0.0504 0.0610 Uiso 1.00 calc . . . H(16) H -0.4125 0.4593 0.0706 0.0610 Uiso 1.00 calc . . . H(17) H 0.0130 0.4429 0.1899 0.0614 Uiso 1.00 calc . . . H(18) H -0.0354 0.5399 0.1242 0.0614 Uiso 1.00 calc . . . H(19) H -0.0843 0.5602 0.1990 0.0614 Uiso 1.00 calc . . . H(20) H -0.2867 0.4247 0.2420 0.0516 Uiso 1.00 calc . . . H(21) H -0.3393 0.2876 0.2082 0.0516 Uiso 1.00 calc . . . H(22) H -0.1927 0.3000 0.2519 0.0516 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0335(2) 0.0474(2) 0.0319(2) 0.00257(9) 0.0023(1) 0.00741(10) Ru(1) 0.0296(2) 0.0258(2) 0.0214(2) 0.00106(9) 0.0060(1) -0.00083(9) P(1) 0.0384(5) 0.0289(5) 0.0292(5) -0.0030(3) 0.0093(4) -0.0065(3) O(1) 0.057(2) 0.049(2) 0.046(2) 0.009(1) 0.018(2) 0.006(1) O(2) 0.034(1) 0.045(2) 0.042(2) 0.006(1) 0.010(1) -0.002(1) O(3) 0.061(2) 0.057(2) 0.062(2) -0.010(2) 0.032(2) 0.000(2) C(1) 0.033(2) 0.029(2) 0.027(2) -0.001(1) 0.004(1) -0.002(1) C(2) 0.038(2) 0.027(2) 0.035(2) -0.002(1) 0.007(2) -0.004(1) C(3) 0.045(2) 0.034(2) 0.030(2) 0.000(2) 0.006(2) -0.011(2) C(4) 0.044(2) 0.042(2) 0.019(2) 0.000(2) 0.001(1) -0.003(2) C(5) 0.037(2) 0.029(2) 0.031(2) -0.003(1) -0.002(2) 0.002(1) C(6) 0.059(3) 0.023(2) 0.047(2) 0.003(2) 0.013(2) 0.001(2) C(7) 0.076(3) 0.057(3) 0.022(2) 0.002(3) 0.009(2) 0.007(2) C(8) 0.038(2) 0.033(2) 0.033(2) 0.001(1) 0.009(2) -0.003(1) C(9) 0.032(2) 0.040(2) 0.032(2) 0.000(1) 0.007(2) -0.007(1) C(10) 0.042(2) 0.064(3) 0.060(3) -0.008(2) 0.023(2) -0.011(2) C(11) 0.047(3) 0.081(4) 0.068(4) 0.013(3) 0.011(3) -0.027(3) C(12) 0.068(3) 0.036(2) 0.049(3) 0.011(2) 0.011(2) -0.002(2) C(13) 0.058(3) 0.052(3) 0.047(3) -0.021(2) 0.018(2) -0.019(2) C(14) 0.048(2) 0.050(2) 0.033(2) -0.004(2) 0.015(2) -0.012(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 3sigma(F^2^) is used only for calculating R-factors(gt). ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00126|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3889 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.779 _refine_ls_shift/su_max 0.0770 _refine_ls_shift/su_mean 0.0180 _refine_diff_density_min -1.37 _refine_diff_density_max 0.36 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I(1) Ru(1) 2.7082(4) 1_555 1_555 yes Ru(1) P(1) 2.3036(9) 1_555 1_555 yes Ru(1) C(1) 2.244(4) 1_555 1_555 yes Ru(1) C(2) 2.314(4) 1_555 1_555 yes Ru(1) C(3) 2.264(4) 1_555 1_555 yes Ru(1) C(4) 2.224(4) 1_555 1_555 yes Ru(1) C(5) 2.185(4) 1_555 1_555 yes Ru(1) C(8) 1.849(4) 1_555 1_555 yes P(1) C(12) 1.822(5) 1_555 1_555 yes P(1) C(13) 1.811(5) 1_555 1_555 yes P(1) C(14) 1.820(4) 1_555 1_555 yes O(1) C(9) 1.195(5) 1_555 1_555 yes O(2) C(9) 1.344(5) 1_555 1_555 yes O(2) C(10) 1.477(6) 1_555 1_555 yes O(3) C(8) 1.141(5) 1_555 1_555 yes C(1) C(2) 1.417(5) 1_555 1_555 yes C(1) C(5) 1.447(5) 1_555 1_555 yes C(1) C(9) 1.473(5) 1_555 1_555 yes C(2) C(3) 1.420(6) 1_555 1_555 yes C(2) C(6) 1.501(6) 1_555 1_555 yes C(3) C(4) 1.433(6) 1_555 1_555 yes C(3) H(1) 0.950 1_555 1_555 no C(4) C(5) 1.420(6) 1_555 1_555 yes C(4) C(7) 1.493(6) 1_555 1_555 yes C(5) H(2) 0.950 1_555 1_555 no C(6) H(3) 0.950 1_555 1_555 no C(6) H(4) 0.950 1_555 1_555 no C(6) H(5) 0.950 1_555 1_555 no C(7) H(6) 0.949 1_555 1_555 no C(7) H(7) 0.951 1_555 1_555 no C(7) H(8) 0.950 1_555 1_555 no C(10) C(11) 1.480(9) 1_555 1_555 yes C(10) H(9) 0.950 1_555 1_555 no C(10) H(10) 0.950 1_555 1_555 no C(11) H(11) 0.950 1_555 1_555 no C(11) H(12) 0.950 1_555 1_555 no C(11) H(13) 0.950 1_555 1_555 no C(12) H(14) 0.950 1_555 1_555 no C(12) H(15) 0.950 1_555 1_555 no C(12) H(16) 0.950 1_555 1_555 no C(13) H(17) 0.950 1_555 1_555 no C(13) H(18) 0.950 1_555 1_555 no C(13) H(19) 0.950 1_555 1_555 no C(14) H(20) 0.950 1_555 1_555 no C(14) H(21) 0.951 1_555 1_555 no C(14) H(22) 0.950 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I(1) Ru(1) P(1) 87.94(3) 1_555 1_555 1_555 yes I(1) Ru(1) C(1) 110.32(10) 1_555 1_555 1_555 yes I(1) Ru(1) C(2) 92.4(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(3) 108.5(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(4) 145.5(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(5) 148.4(1) 1_555 1_555 1_555 yes I(1) Ru(1) C(8) 91.0(1) 1_555 1_555 1_555 yes P(1) Ru(1) C(1) 101.34(10) 1_555 1_555 1_555 yes P(1) Ru(1) C(2) 133.6(1) 1_555 1_555 1_555 yes P(1) Ru(1) C(3) 158.9(1) 1_555 1_555 1_555 yes P(1) Ru(1) C(4) 126.2(1) 1_555 1_555 1_555 yes P(1) Ru(1) C(5) 97.0(1) 1_555 1_555 1_555 yes P(1) Ru(1) C(8) 89.5(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(2) 36.2(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(3) 61.1(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(4) 62.6(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(5) 38.1(1) 1_555 1_555 1_555 yes C(1) Ru(1) C(8) 156.2(2) 1_555 1_555 1_555 yes C(2) Ru(1) C(3) 36.1(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(4) 61.6(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(5) 61.9(1) 1_555 1_555 1_555 yes C(2) Ru(1) C(8) 136.8(2) 1_555 1_555 1_555 yes C(3) Ru(1) C(4) 37.2(2) 1_555 1_555 1_555 yes C(3) Ru(1) C(5) 62.1(1) 1_555 1_555 1_555 yes C(3) Ru(1) C(8) 102.9(2) 1_555 1_555 1_555 yes C(4) Ru(1) C(5) 37.6(2) 1_555 1_555 1_555 yes C(4) Ru(1) C(8) 93.8(2) 1_555 1_555 1_555 yes C(5) Ru(1) C(8) 120.1(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(12) 114.6(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(13) 116.9(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(14) 115.6(2) 1_555 1_555 1_555 yes C(12) P(1) C(13) 102.3(3) 1_555 1_555 1_555 yes C(12) P(1) C(14) 102.6(2) 1_555 1_555 1_555 yes C(13) P(1) C(14) 102.9(2) 1_555 1_555 1_555 yes C(9) O(2) C(10) 115.7(4) 1_555 1_555 1_555 yes Ru(1) C(1) C(2) 74.6(2) 1_555 1_555 1_555 yes Ru(1) C(1) C(5) 68.7(2) 1_555 1_555 1_555 yes Ru(1) C(1) C(9) 124.3(3) 1_555 1_555 1_555 yes C(2) C(1) C(5) 107.9(3) 1_555 1_555 1_555 yes C(2) C(1) C(9) 126.0(3) 1_555 1_555 1_555 yes C(5) C(1) C(9) 126.0(3) 1_555 1_555 1_555 yes Ru(1) C(2) C(1) 69.2(2) 1_555 1_555 1_555 yes Ru(1) C(2) C(3) 70.0(2) 1_555 1_555 1_555 yes Ru(1) C(2) C(6) 128.0(3) 1_555 1_555 1_555 yes C(1) C(2) C(3) 107.7(3) 1_555 1_555 1_555 yes C(1) C(2) C(6) 128.2(4) 1_555 1_555 1_555 yes C(3) C(2) C(6) 124.0(4) 1_555 1_555 1_555 yes Ru(1) C(3) C(2) 73.9(2) 1_555 1_555 1_555 yes Ru(1) C(3) C(4) 69.9(2) 1_555 1_555 1_555 yes Ru(1) C(3) H(1) 122.4(3) 1_555 1_555 1_555 no C(2) C(3) C(4) 109.1(3) 1_555 1_555 1_555 yes C(2) C(3) H(1) 125.5(4) 1_555 1_555 1_555 no C(4) C(3) H(1) 125.5(4) 1_555 1_555 1_555 no Ru(1) C(4) C(3) 72.9(2) 1_555 1_555 1_555 yes Ru(1) C(4) C(5) 69.7(2) 1_555 1_555 1_555 yes Ru(1) C(4) C(7) 126.5(3) 1_555 1_555 1_555 yes C(3) C(4) C(5) 107.1(3) 1_555 1_555 1_555 yes C(3) C(4) C(7) 125.3(4) 1_555 1_555 1_555 yes C(5) C(4) C(7) 127.3(4) 1_555 1_555 1_555 yes Ru(1) C(5) C(1) 73.1(2) 1_555 1_555 1_555 yes Ru(1) C(5) C(4) 72.7(2) 1_555 1_555 1_555 yes Ru(1) C(5) H(2) 120.0(3) 1_555 1_555 1_555 no C(1) C(5) C(4) 108.1(3) 1_555 1_555 1_555 yes C(1) C(5) H(2) 126.0(4) 1_555 1_555 1_555 no C(4) C(5) H(2) 125.9(4) 1_555 1_555 1_555 no C(2) C(6) H(3) 109.5(4) 1_555 1_555 1_555 no C(2) C(6) H(4) 109.5(4) 1_555 1_555 1_555 no C(2) C(6) H(5) 109.5(4) 1_555 1_555 1_555 no H(3) C(6) H(4) 109.4(5) 1_555 1_555 1_555 no H(3) C(6) H(5) 109.5(5) 1_555 1_555 1_555 no H(4) C(6) H(5) 109.5(4) 1_555 1_555 1_555 no C(4) C(7) H(6) 109.5(5) 1_555 1_555 1_555 no C(4) C(7) H(7) 109.4(5) 1_555 1_555 1_555 no C(4) C(7) H(8) 109.5(4) 1_555 1_555 1_555 no H(6) C(7) H(7) 109.5(5) 1_555 1_555 1_555 no H(6) C(7) H(8) 109.5(6) 1_555 1_555 1_555 no H(7) C(7) H(8) 109.4(5) 1_555 1_555 1_555 no Ru(1) C(8) O(3) 176.3(4) 1_555 1_555 1_555 yes O(1) C(9) O(2) 124.3(4) 1_555 1_555 1_555 yes O(1) C(9) C(1) 125.4(4) 1_555 1_555 1_555 yes O(2) C(9) C(1) 110.4(3) 1_555 1_555 1_555 yes O(2) C(10) C(11) 108.1(5) 1_555 1_555 1_555 yes O(2) C(10) H(9) 109.8(5) 1_555 1_555 1_555 no O(2) C(10) H(10) 109.8(4) 1_555 1_555 1_555 no C(11) C(10) H(9) 109.9(5) 1_555 1_555 1_555 no C(11) C(10) H(10) 109.8(5) 1_555 1_555 1_555 no H(9) C(10) H(10) 109.5(5) 1_555 1_555 1_555 no C(10) C(11) H(11) 109.5(5) 1_555 1_555 1_555 no C(10) C(11) H(12) 109.5(5) 1_555 1_555 1_555 no C(10) C(11) H(13) 109.5(7) 1_555 1_555 1_555 no H(11) C(11) H(12) 109.4(7) 1_555 1_555 1_555 no H(11) C(11) H(13) 109.5(6) 1_555 1_555 1_555 no H(12) C(11) H(13) 109.5(5) 1_555 1_555 1_555 no P(1) C(12) H(14) 109.5(4) 1_555 1_555 1_555 no P(1) C(12) H(15) 109.4(4) 1_555 1_555 1_555 no P(1) C(12) H(16) 109.5(4) 1_555 1_555 1_555 no H(14) C(12) H(15) 109.5(5) 1_555 1_555 1_555 no H(14) C(12) H(16) 109.5(6) 1_555 1_555 1_555 no H(15) C(12) H(16) 109.5(5) 1_555 1_555 1_555 no P(1) C(13) H(17) 109.5(4) 1_555 1_555 1_555 no P(1) C(13) H(18) 109.5(4) 1_555 1_555 1_555 no P(1) C(13) H(19) 109.5(4) 1_555 1_555 1_555 no H(17) C(13) H(18) 109.4(5) 1_555 1_555 1_555 no H(17) C(13) H(19) 109.5(5) 1_555 1_555 1_555 no H(18) C(13) H(19) 109.5(5) 1_555 1_555 1_555 no P(1) C(14) H(20) 109.5(4) 1_555 1_555 1_555 no P(1) C(14) H(21) 109.5(3) 1_555 1_555 1_555 no P(1) C(14) H(22) 109.5(3) 1_555 1_555 1_555 no H(20) C(14) H(21) 109.4(4) 1_555 1_555 1_555 no H(20) C(14) H(22) 109.5(4) 1_555 1_555 1_555 no H(21) C(14) H(22) 109.4(5) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I(1) Ru(1) P(1) C(12) -174.8(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) P(1) C(13) 65.6(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) P(1) C(14) -55.8(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(1) C(2) -64.4(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(1) C(5) 178.9(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(1) C(9) 59.0(3) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(2) C(1) 122.2(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(2) C(3) -118.8(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(2) C(6) -0.7(4) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(3) C(2) 67.4(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(3) C(4) -174.7(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(4) C(3) 8.9(4) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(4) C(5) 125.2(2) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(4) C(7) -112.8(4) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(5) C(1) -2.0(3) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(5) C(4) -117.7(3) 1_555 1_555 1_555 1_555 yes I(1) Ru(1) C(8) O(3) 144(5) 1_555 1_555 1_555 1_555 yes Ru(1) C(1) C(2) C(3) -59.6(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(1) C(2) C(6) 122.6(4) 1_555 1_555 1_555 1_555 yes Ru(1) C(1) C(5) C(4) 64.8(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(1) C(9) O(1) -97.2(5) 1_555 1_555 1_555 1_555 yes Ru(1) C(1) C(9) O(2) 83.7(4) 1_555 1_555 1_555 1_555 yes Ru(1) C(2) C(1) C(5) 61.0(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(2) C(1) C(9) -121.5(4) 1_555 1_555 1_555 1_555 yes Ru(1) C(2) C(3) C(4) -61.4(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(3) C(2) C(1) 59.1(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(3) C(2) C(6) -123.0(4) 1_555 1_555 1_555 1_555 yes Ru(1) C(3) C(4) C(5) -61.7(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(3) C(4) C(7) 123.0(4) 1_555 1_555 1_555 1_555 yes Ru(1) C(4) C(3) C(2) 63.9(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(4) C(5) C(1) -65.1(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(5) C(1) C(2) -64.9(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(5) C(1) C(9) 117.7(4) 1_555 1_555 1_555 1_555 yes Ru(1) C(5) C(4) C(3) 63.8(3) 1_555 1_555 1_555 1_555 yes Ru(1) C(5) C(4) C(7) -121.0(5) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(1) C(2) -156.4(2) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(1) C(5) 86.9(2) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(1) C(9) -33.0(3) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(2) C(1) 32.8(3) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(2) C(3) 151.8(2) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(2) C(6) -90.1(4) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(3) C(2) -72.3(4) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(3) C(4) 45.6(4) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(4) C(3) -161.4(2) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(4) C(5) -45.2(3) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(4) C(7) 76.9(4) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(5) C(1) -99.5(2) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(5) C(4) 144.8(2) 1_555 1_555 1_555 1_555 yes P(1) Ru(1) C(8) O(3) -127(5) 1_555 1_555 1_555 1_555 yes O(1) C(9) O(2) C(10) 0.9(6) 1_555 1_555 1_555 1_555 yes O(1) C(9) C(1) C(2) -1.5(7) 1_555 1_555 1_555 1_555 yes O(1) C(9) C(1) C(5) 175.5(4) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(1) C(2) 179.4(4) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(1) C(5) -3.6(6) 1_555 1_555 1_555 1_555 yes O(3) C(8) Ru(1) C(1) -9(5) 1_555 1_555 1_555 1_555 yes O(3) C(8) Ru(1) C(2) 49(5) 1_555 1_555 1_555 1_555 yes O(3) C(8) Ru(1) C(3) 35(5) 1_555 1_555 1_555 1_555 yes O(3) C(8) Ru(1) C(4) -1(5) 1_555 1_555 1_555 1_555 yes O(3) C(8) Ru(1) C(5) -29(5) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) P(1) C(12) -64.5(2) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) P(1) C(13) 175.9(2) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) P(1) C(14) 54.5(2) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(2) C(3) 119.0(3) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(2) C(6) -122.9(5) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(3) C(2) -36.1(2) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(3) C(4) 81.8(3) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(4) C(3) -77.5(2) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(4) C(5) 38.8(2) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(4) C(7) 160.9(4) 1_555 1_555 1_555 1_555 yes C(1) Ru(1) C(5) C(4) -115.7(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) Ru(1) C(3) -119.0(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) Ru(1) C(4) -81.6(2) 1_555 1_555 1_555 1_555 yes C(1) C(2) Ru(1) C(5) -38.7(2) 1_555 1_555 1_555 1_555 yes C(1) C(2) Ru(1) C(8) -143.8(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -2.3(5) 1_555 1_555 1_555 1_555 yes C(1) C(5) Ru(1) C(2) 36.7(2) 1_555 1_555 1_555 1_555 yes C(1) C(5) Ru(1) C(3) 77.8(2) 1_555 1_555 1_555 1_555 yes C(1) C(5) Ru(1) C(4) 115.7(3) 1_555 1_555 1_555 1_555 yes C(1) C(5) Ru(1) C(8) 167.0(2) 1_555 1_555 1_555 1_555 yes C(1) C(5) C(4) C(3) -1.3(4) 1_555 1_555 1_555 1_555 yes C(1) C(5) C(4) C(7) 173.9(4) 1_555 1_555 1_555 1_555 yes C(1) C(9) O(2) C(10) -179.9(4) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) P(1) C(12) -83.5(3) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) P(1) C(13) 156.9(3) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) P(1) C(14) 35.5(2) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(1) C(5) -116.7(3) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(1) C(9) 123.4(4) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(3) C(4) 117.9(4) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(4) C(3) -36.3(2) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(4) C(5) 79.9(2) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(4) C(7) -158.0(4) 1_555 1_555 1_555 1_555 yes C(2) Ru(1) C(5) C(4) -79.0(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) Ru(1) C(3) 36.1(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) Ru(1) C(4) 78.5(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) Ru(1) C(5) 116.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) Ru(1) C(8) 87.9(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(5) C(4) -0.1(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) Ru(1) C(4) -117.9(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) Ru(1) C(5) -79.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) Ru(1) C(8) 162.9(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 2.2(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(7) -173.1(4) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) P(1) C(12) -32.7(4) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) P(1) C(13) -152.3(4) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) P(1) C(14) 86.3(4) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) C(1) C(5) -80.6(2) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) C(1) C(9) 159.5(4) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) C(2) C(6) 118.1(5) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) C(4) C(5) 116.2(3) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) C(4) C(7) -121.7(5) 1_555 1_555 1_555 1_555 yes C(3) Ru(1) C(5) C(4) -37.9(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) Ru(1) C(4) 37.4(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) Ru(1) C(5) 80.3(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) Ru(1) C(8) -24.8(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(5) 1.4(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(9) 178.9(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) Ru(1) C(5) -116.2(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) Ru(1) C(8) 106.3(3) 1_555 1_555 1_555 1_555 yes C(4) Ru(1) P(1) C(12) -0.3(2) 1_555 1_555 1_555 1_555 yes C(4) Ru(1) P(1) C(13) -119.9(3) 1_555 1_555 1_555 1_555 yes C(4) Ru(1) P(1) C(14) 118.7(2) 1_555 1_555 1_555 1_555 yes C(4) Ru(1) C(1) C(5) -38.2(2) 1_555 1_555 1_555 1_555 yes C(4) Ru(1) C(1) C(9) -158.1(4) 1_555 1_555 1_555 1_555 yes C(4) Ru(1) C(2) C(6) 155.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) Ru(1) C(5) 38.2(2) 1_555 1_555 1_555 1_555 yes C(4) C(3) Ru(1) C(8) -79.2(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(6) 175.6(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) Ru(1) C(8) 51.3(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(1) C(9) -177.5(4) 1_555 1_555 1_555 1_555 yes C(5) Ru(1) P(1) C(12) -26.1(2) 1_555 1_555 1_555 1_555 yes C(5) Ru(1) P(1) C(13) -145.7(2) 1_555 1_555 1_555 1_555 yes C(5) Ru(1) P(1) C(14) 92.9(2) 1_555 1_555 1_555 1_555 yes C(5) Ru(1) C(1) C(9) -119.9(4) 1_555 1_555 1_555 1_555 yes C(5) Ru(1) C(2) C(6) -161.6(4) 1_555 1_555 1_555 1_555 yes C(5) Ru(1) C(4) C(7) 122.1(5) 1_555 1_555 1_555 1_555 yes C(5) C(1) Ru(1) C(8) -28.8(5) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(2) C(6) -176.3(4) 1_555 1_555 1_555 1_555 yes C(5) C(4) Ru(1) C(8) -137.4(2) 1_555 1_555 1_555 1_555 yes C(6) C(2) Ru(1) C(8) 93.3(4) 1_555 1_555 1_555 1_555 yes C(6) C(2) C(1) C(9) 1.1(7) 1_555 1_555 1_555 1_555 yes C(7) C(4) Ru(1) C(8) -15.4(4) 1_555 1_555 1_555 1_555 yes C(8) Ru(1) P(1) C(12) 94.1(2) 1_555 1_555 1_555 1_555 yes C(8) Ru(1) P(1) C(13) -25.5(2) 1_555 1_555 1_555 1_555 yes C(8) Ru(1) P(1) C(14) -146.8(2) 1_555 1_555 1_555 1_555 yes C(8) Ru(1) C(1) C(9) -148.7(4) 1_555 1_555 1_555 1_555 yes C(9) O(2) C(10) C(11) 166.1(4) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ _publ_contact_author_name ' Shigetoshi Takahashi' _publ_contact_author_address ; 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; _publ_contact_author_email ' takahahsi@sanken.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-(0)6-6879-8455 ' _publ_contact_author_phone ' +81-(0)6-6879-8459 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chem. Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; Multiple Ligand Transfer Reaction to Planar-Chiral Cyclopentadienylruthenium Complexes Inducing Metal-Centered Chirality ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #===END