Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_section_title ; Water-soluble hydroxyalkylated phosphines: Examples of the differing behaviour toward ruthenium and rhodium ; loop_ _publ_author_name _publ_author_address 'L. Higham' ; Chemistry Department, UCD, Belfield, Dublin 4, Ireland ; 'M.K. Whittlesey' ; School of Chemistry University of Bath Bath BA2 7AY UK ; 'P.T. Wood' ; University Chemical Laboratory Lensfield Road Cambridge CB2 1EW UK ; _publ_contact_author_email lee.higham@ucd.ie _publ_contact_author_phone 0035317162316 _publ_contact_author_fax 0035317062127 _publ_contact_author_name 'Lee Higham' _publ_contact_author_address ; Chemistry Department, UCD, Belfield, Dublin 4, Ireland ; data_1 _database_code_depnum_ccdc_archive 'CCDC 228753' _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H40 Cl2 O6 P4 Ru' _chemical_formula_weight 792.48 _chemical_melting_point ? _chemical_compound_source ? _ccdc_chemical_compound_source_recrystallisation methanol 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' P P 0.1023 0.0942 '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' Ru Ru -1.2594 0.8363 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.283(2) _cell_length_b 10.008(6) _cell_length_c 10.5680(10) _cell_angle_alpha 99.87(2) _cell_angle_beta 105.120(10) _cell_angle_gamma 109.15(2) _cell_volume 859.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method ? _exptl_crystal_F_000 398 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; The unit cell was determined and refined using 37 reflections in a single frame with osscilation angle equal to five degrees. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'area detector' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5570 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.59 _reflns_number_total 2962 _reflns_number_observed 2003 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku Control software' _computing_cell_refinement 'Denzo (Otwinowski, 1987)' _computing_data_reduction 'Scalepack (Otwinowski, 1987)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+0.0000P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0480(77) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2959 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_obs 0.0641 _refine_ls_wR_factor_all 0.2084 _refine_ls_wR_factor_obs 0.1666 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.0000 0.0000 0.0000 0.0541(4) Uani 1 d S . Cl1 Cl -0.0571(2) 0.1220(2) 0.1906(2) 0.0709(5) Uani 1 d . . P1 P -0.1243(2) 0.1086(2) -0.1516(2) 0.0676(5) Uani 1 d . . H1 H -0.2465(100) 0.0289(101) -0.2988(87) 0.100(26) Uiso 1 d . . C1 C -0.0172(9) 0.2323(9) -0.2389(7) 0.069(2) Uani 1 d . . C2 C 0.0153(10) 0.3796(9) -0.2096(9) 0.083(2) Uani 1 d . . H2 H -0.0154(10) 0.4223(9) -0.1413(9) 0.100 Uiso 1 calc R . C3 C 0.0948(13) 0.4683(11) -0.2811(11) 0.105(3) Uani 1 d . . H3 H 0.1160(13) 0.5685(11) -0.2598(11) 0.126 Uiso 1 calc R . C4 C 0.1394(15) 0.4081(13) -0.3796(11) 0.114(3) Uani 1 d . . H4 H 0.1932(15) 0.4658(13) -0.4265(11) 0.137 Uiso 1 calc R . C5 C 0.1040(14) 0.2590(15) -0.4100(11) 0.117(3) Uani 1 d . . H5 H 0.1336(14) 0.2160(15) -0.4789(11) 0.140 Uiso 1 calc R . C6 C 0.0261(11) 0.1722(10) -0.3410(9) 0.090(2) Uani 1 d . . H6 H 0.0028(11) 0.0717(10) -0.3643(9) 0.108 Uiso 1 calc R . C7 C -0.2402(11) 0.2064(12) -0.0829(11) 0.099(3) Uani 1 d . . H7A H -0.2998(11) 0.1477(12) -0.0350(11) 0.118 Uiso 1 calc R . H7B H -0.1644(11) 0.2998(12) -0.0174(11) 0.118 Uiso 1 calc R . O1 O -0.3484(10) 0.2323(10) -0.1845(8) 0.123(2) Uani 1 d . . P2 P -0.2505(2) -0.2091(2) -0.0790(2) 0.0617(5) Uani 1 d . . C11 C -0.4068(9) -0.2311(8) -0.2378(8) 0.071(2) Uani 1 d . . C12 C -0.3979(11) -0.2877(11) -0.3638(8) 0.091(3) Uani 1 d . . H12 H -0.3185(11) -0.3238(11) -0.3684(8) 0.110 Uiso 1 calc R . C13 C -0.5085(14) -0.2901(14) -0.4832(9) 0.111(3) Uani 1 d . . H13 H -0.4991(14) -0.3251(14) -0.5668(9) 0.134 Uiso 1 calc R . C14 C -0.6294(12) -0.2427(14) -0.4810(10) 0.110(3) Uani 1 d . . H14 H -0.7028(12) -0.2462(14) -0.5617(10) 0.132 Uiso 1 calc R . C15 C -0.6410(11) -0.1897(12) -0.3572(10) 0.097(3) Uani 1 d . . H15 H -0.7225(11) -0.1560(12) -0.3540(10) 0.116 Uiso 1 calc R . C16 C -0.5316(10) -0.1855(10) -0.2351(9) 0.080(2) Uani 1 d . . H16 H -0.5431(10) -0.1519(10) -0.1521(9) 0.096 Uiso 1 calc R . C17 C -0.2312(11) -0.3890(10) -0.1253(10) 0.092(2) Uani 1 d . . H17A H -0.1864(11) -0.3915(10) -0.1986(10) 0.110 Uiso 1 calc R . H17B H -0.1564(11) -0.3980(10) -0.0471(10) 0.110 Uiso 1 calc R . O2 O -0.3833(9) -0.5106(8) -0.1678(9) 0.126(3) Uani 1 d . . C18 C -0.3671(10) -0.2449(10) 0.0378(9) 0.080(2) Uani 1 d . . H18 H -0.3006(10) -0.2691(10) 0.1116(9) 0.096 Uiso 1 calc R . O3 O -0.3872(9) -0.1212(10) 0.1011(8) 0.079(2) Uani 0.67 d P . O13 O -0.5136(22) -0.3565(22) -0.0094(18) 0.091(5) Uani 0.33 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0615(6) 0.0551(5) 0.0577(5) 0.0225(3) 0.0264(3) 0.0296(4) Cl1 0.0872(12) 0.0701(11) 0.0726(11) 0.0234(8) 0.0416(9) 0.0391(9) P1 0.0719(12) 0.0712(12) 0.0760(11) 0.0363(10) 0.0300(9) 0.0366(10) C1 0.070(5) 0.077(5) 0.066(4) 0.030(4) 0.023(3) 0.033(4) C2 0.097(6) 0.073(5) 0.084(5) 0.033(4) 0.033(4) 0.031(5) C3 0.124(8) 0.072(6) 0.117(7) 0.040(5) 0.044(6) 0.025(6) C4 0.152(10) 0.098(8) 0.111(8) 0.058(6) 0.068(7) 0.038(7) C5 0.148(9) 0.127(9) 0.092(7) 0.041(6) 0.072(6) 0.046(7) C6 0.122(7) 0.075(5) 0.078(5) 0.023(4) 0.043(5) 0.036(5) C7 0.090(6) 0.131(8) 0.140(8) 0.095(7) 0.066(6) 0.074(6) O1 0.133(6) 0.150(7) 0.124(5) 0.061(5) 0.055(4) 0.082(5) P2 0.0654(11) 0.0588(10) 0.0666(10) 0.0216(8) 0.0270(8) 0.0260(9) C11 0.072(5) 0.063(4) 0.075(5) 0.021(4) 0.024(3) 0.021(4) C12 0.096(6) 0.107(7) 0.075(5) 0.017(5) 0.033(4) 0.048(5) C13 0.127(9) 0.144(10) 0.059(5) 0.018(5) 0.027(5) 0.056(7) C14 0.081(6) 0.142(10) 0.090(7) 0.034(6) 0.008(5) 0.039(6) C15 0.079(6) 0.115(8) 0.101(7) 0.040(6) 0.023(5) 0.046(5) C16 0.076(5) 0.093(6) 0.081(5) 0.030(4) 0.034(4) 0.036(4) C17 0.094(6) 0.070(5) 0.108(6) 0.028(5) 0.039(5) 0.024(5) O2 0.122(6) 0.085(5) 0.159(7) 0.034(5) 0.039(5) 0.034(4) C18 0.084(6) 0.091(6) 0.077(5) 0.033(4) 0.034(4) 0.039(5) O3 0.062(4) 0.097(6) 0.086(5) 0.029(4) 0.033(4) 0.033(4) O13 0.086(12) 0.094(13) 0.084(11) 0.025(9) 0.033(9) 0.022(10) _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 P1 2.352(2) 2 ? Ru1 P1 2.352(2) . ? Ru1 P2 2.383(2) . ? Ru1 P2 2.383(2) 2 ? Ru1 Cl1 2.443(2) . ? Ru1 Cl1 2.443(2) 2 ? P1 H1 1.55(8) . ? P1 C1 1.853(8) . ? P1 C7 1.871(9) . ? C1 C6 1.360(11) . ? C1 C2 1.365(11) . ? C2 C3 1.413(12) . ? C3 C4 1.339(15) . ? C4 C5 1.38(2) . ? C5 C6 1.375(13) . ? C7 O1 1.390(11) . ? P2 C11 1.834(8) . ? P2 C18 1.849(8) . ? P2 C17 1.863(9) . ? C11 C16 1.382(11) . ? C11 C12 1.389(11) . ? C12 C13 1.394(13) . ? C13 C14 1.358(14) . ? C14 C15 1.370(14) . ? C15 C16 1.402(12) . ? C17 O2 1.426(11) . ? C18 O13 1.34(2) . ? C18 O3 1.395(12) . ? 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 P1 Ru1 P1 180.0 2 . ? P1 Ru1 P2 91.45(7) 2 . ? P1 Ru1 P2 88.55(7) . . ? P1 Ru1 P2 88.55(7) 2 2 ? P1 Ru1 P2 91.45(7) . 2 ? P2 Ru1 P2 180.0 . 2 ? P1 Ru1 Cl1 87.09(7) 2 . ? P1 Ru1 Cl1 92.91(7) . . ? P2 Ru1 Cl1 94.26(7) . . ? P2 Ru1 Cl1 85.74(7) 2 . ? P1 Ru1 Cl1 92.92(7) 2 2 ? P1 Ru1 Cl1 87.08(7) . 2 ? P2 Ru1 Cl1 85.74(7) . 2 ? P2 Ru1 Cl1 94.26(7) 2 2 ? Cl1 Ru1 Cl1 180.0 . 2 ? H1 P1 C1 82.5(34) . . ? H1 P1 C7 99.2(31) . . ? C1 P1 C7 104.3(4) . . ? H1 P1 Ru1 126.5(34) . . ? C1 P1 Ru1 124.1(2) . . ? C7 P1 Ru1 114.1(3) . . ? C6 C1 C2 118.2(8) . . ? C6 C1 P1 118.2(6) . . ? C2 C1 P1 123.5(6) . . ? C1 C2 C3 121.1(9) . . ? C4 C3 C2 120.0(9) . . ? C3 C4 C5 118.6(9) . . ? C6 C5 C4 121.6(10) . . ? C1 C6 C5 120.5(9) . . ? O1 C7 P1 112.7(7) . . ? C11 P2 C18 102.5(4) . . ? C11 P2 C17 98.9(4) . . ? C18 P2 C17 100.3(4) . . ? C11 P2 Ru1 118.8(3) . . ? C18 P2 Ru1 118.8(3) . . ? C17 P2 Ru1 114.2(3) . . ? C16 C11 C12 118.5(7) . . ? C16 C11 P2 120.9(6) . . ? C12 C11 P2 120.5(6) . . ? C11 C12 C13 119.8(8) . . ? C14 C13 C12 121.9(9) . . ? C13 C14 C15 118.6(8) . . ? C14 C15 C16 121.0(9) . . ? C11 C16 C15 120.2(8) . . ? O2 C17 P2 112.0(6) . . ? O13 C18 O3 106.5(11) . . ? O13 C18 P2 119.0(9) . . ? O3 C18 P2 113.5(6) . . ? _refine_diff_density_max 0.624 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.115