# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs045_0m_Compound_3 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C32 H74 Cl4 N2 O4 P4 Ru2' _chemical_formula_weight 1018.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7890(8) _cell_length_b 10.4080(10) _cell_length_c 13.7962(13) _cell_angle_alpha 91.428(4) _cell_angle_beta 106.792(3) _cell_angle_gamma 114.206(3) _cell_volume 1087.02(18) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9277 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.61 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6665 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18556 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.65 _reflns_number_total 5020 _reflns_number_gt 4575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0221P)^2^+0.4112P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5020 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0510 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _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 Ru1 Ru 0.574963(16) 0.985224(14) 0.643222(10) 0.00906(4) Uani 1 1 d . . . Cl1 Cl 0.83050(5) 0.97749(5) 0.61297(3) 0.01582(9) Uani 1 1 d . . . Cl2 Cl 0.59698(5) 1.17113(4) 0.52863(3) 0.01305(8) Uani 1 1 d . . . P1 P 0.73739(6) 1.15114(5) 0.78361(3) 0.01276(9) Uani 1 1 d . . . P2 P 0.50098(6) 0.78165(5) 0.71019(3) 0.01174(9) Uani 1 1 d . . . O1 O 0.62393(17) 1.19094(15) 0.84452(10) 0.0222(3) Uani 1 1 d . . . O2 O 0.28793(15) 0.69284(13) 0.68350(10) 0.0180(3) Uani 1 1 d . . . N1 N 0.33540(18) 0.99984(15) 0.63666(11) 0.0138(3) Uani 1 1 d . . . H1A H 0.2860 1.0003 0.5674 0.017 Uiso 1 1 calc R . . C1 C 0.8643(2) 1.33134(19) 0.75696(14) 0.0189(4) Uani 1 1 d . . . H1 H 0.7738 1.3547 0.7083 0.023 Uiso 1 1 calc R . . C2 C 0.8902(2) 1.11915(19) 0.89480(13) 0.0171(4) Uani 1 1 d . . . H2 H 0.8303 1.0148 0.8970 0.021 Uiso 1 1 calc R . . C3 C 0.5586(2) 0.76255(19) 0.84793(13) 0.0169(4) Uani 1 1 d . . . H3 H 0.6902 0.8037 0.8775 0.020 Uiso 1 1 calc R . . C4 C 0.5574(2) 0.65466(19) 0.64765(14) 0.0180(4) Uani 1 1 d . . . H4 H 0.5741 0.6906 0.5832 0.022 Uiso 1 1 calc R . . C5 C 0.4451(3) 1.1701(2) 0.80149(15) 0.0244(4) Uani 1 1 d . . . H5A H 0.4382 1.2568 0.8267 0.029 Uiso 1 1 calc R . . H5B H 0.3712 1.0901 0.8294 0.029 Uiso 1 1 calc R . . C6 C 0.3629(2) 1.1393(2) 0.68615(14) 0.0199(4) Uani 1 1 d . . . H6A H 0.2473 1.1428 0.6682 0.024 Uiso 1 1 calc R . . H6B H 0.4392 1.2160 0.6571 0.024 Uiso 1 1 calc R . . C7 C 0.1602(2) 0.7353(2) 0.62170(15) 0.0209(4) Uani 1 1 d . . . H7A H 0.0410 0.6663 0.6198 0.025 Uiso 1 1 calc R . . H7B H 0.1634 0.7311 0.5506 0.025 Uiso 1 1 calc R . . C8 C 0.1891(3) 0.8821(2) 0.65933(17) 0.0260(4) Uani 1 1 d . . . H8A H 0.0785 0.8916 0.6280 0.031 Uiso 1 1 calc R . . H8B H 0.2140 0.8931 0.7345 0.031 Uiso 1 1 calc R . . C9 C 0.9531(3) 1.4507(2) 0.85076(15) 0.0273(4) Uani 1 1 d . . . H9A H 1.0558 1.4431 0.8973 0.041 Uiso 1 1 calc R . . H9B H 0.8687 1.4412 0.8867 0.041 Uiso 1 1 calc R . . H9C H 0.9913 1.5439 0.8280 0.041 Uiso 1 1 calc R . . C10 C 0.9953(3) 1.3419(2) 0.70083(15) 0.0238(4) Uani 1 1 d . . . H10A H 1.0271 1.4304 0.6717 0.036 Uiso 1 1 calc R . . H10B H 0.9407 1.2599 0.6455 0.036 Uiso 1 1 calc R . . H10C H 1.1018 1.3421 0.7493 0.036 Uiso 1 1 calc R . . C11 C 0.9229(3) 1.1945(2) 1.00061(15) 0.0289(5) Uani 1 1 d . . . H11A H 0.9827 1.1547 1.0540 0.043 Uiso 1 1 calc R . . H11B H 0.8098 1.1800 1.0082 0.043 Uiso 1 1 calc R . . H11C H 0.9972 1.2969 1.0073 0.043 Uiso 1 1 calc R . . C12 C 1.0646(3) 1.1433(2) 0.87936(16) 0.0267(4) Uani 1 1 d . . . H12A H 1.1385 1.2461 0.8873 0.040 Uiso 1 1 calc R . . H12B H 1.0410 1.0974 0.8103 0.040 Uiso 1 1 calc R . . H12C H 1.1261 1.1021 0.9305 0.040 Uiso 1 1 calc R . . C13 C 0.4968(3) 0.8488(2) 0.90572(14) 0.0234(4) Uani 1 1 d . . . H13A H 0.3675 0.8051 0.8827 0.035 Uiso 1 1 calc R . . H13B H 0.5413 0.9471 0.8919 0.035 Uiso 1 1 calc R . . H13C H 0.5422 0.8493 0.9796 0.035 Uiso 1 1 calc R . . C14 C 0.4824(3) 0.6084(2) 0.86841(16) 0.0264(4) Uani 1 1 d . . . H14A H 0.5139 0.6085 0.9426 0.040 Uiso 1 1 calc R . . H14B H 0.5311 0.5542 0.8385 0.040 Uiso 1 1 calc R . . H14C H 0.3536 0.5641 0.8372 0.040 Uiso 1 1 calc R . . C15 C 0.7349(3) 0.6594(2) 0.71023(17) 0.0277(5) Uani 1 1 d . . . H15A H 0.7232 0.6140 0.7707 0.042 Uiso 1 1 calc R . . H15B H 0.8239 0.7590 0.7322 0.042 Uiso 1 1 calc R . . H15C H 0.7714 0.6083 0.6679 0.042 Uiso 1 1 calc R . . C16 C 0.4100(3) 0.5018(2) 0.61279(17) 0.0293(5) Uani 1 1 d . . . H16A H 0.4483 0.4433 0.5780 0.044 Uiso 1 1 calc R . . H16B H 0.3036 0.5031 0.5654 0.044 Uiso 1 1 calc R . . H16C H 0.3840 0.4614 0.6727 0.044 Uiso 1 1 calc R . . 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 0.00875(7) 0.01085(7) 0.00858(7) 0.00216(5) 0.00263(5) 0.00533(5) Cl1 0.01226(19) 0.0196(2) 0.0189(2) 0.00402(16) 0.00619(16) 0.00928(16) Cl2 0.01463(19) 0.01238(19) 0.01050(19) 0.00246(14) 0.00219(15) 0.00559(16) P1 0.0128(2) 0.0142(2) 0.0112(2) 0.00033(16) 0.00231(17) 0.00691(17) P2 0.0113(2) 0.0131(2) 0.0119(2) 0.00402(16) 0.00386(17) 0.00621(17) O1 0.0186(7) 0.0338(8) 0.0161(7) -0.0049(6) 0.0028(5) 0.0156(6) O2 0.0106(6) 0.0170(6) 0.0247(7) 0.0084(5) 0.0042(5) 0.0053(5) N1 0.0129(7) 0.0178(7) 0.0138(7) 0.0041(6) 0.0047(6) 0.0093(6) C1 0.0199(9) 0.0128(8) 0.0181(9) 0.0016(7) 0.0004(7) 0.0057(7) C2 0.0176(9) 0.0179(9) 0.0139(9) 0.0025(7) 0.0010(7) 0.0085(7) C3 0.0166(9) 0.0193(9) 0.0140(9) 0.0071(7) 0.0044(7) 0.0073(7) C4 0.0254(10) 0.0149(9) 0.0198(9) 0.0054(7) 0.0111(8) 0.0120(8) C5 0.0235(10) 0.0352(11) 0.0221(10) 0.0003(8) 0.0066(8) 0.0210(9) C6 0.0208(9) 0.0244(10) 0.0214(10) 0.0032(8) 0.0066(8) 0.0167(8) C7 0.0091(8) 0.0236(10) 0.0281(10) 0.0089(8) 0.0052(7) 0.0058(7) C8 0.0188(10) 0.0297(11) 0.0399(12) 0.0141(9) 0.0181(9) 0.0144(9) C9 0.0332(11) 0.0171(9) 0.0232(10) -0.0024(8) -0.0008(9) 0.0099(9) C10 0.0202(10) 0.0186(9) 0.0235(10) 0.0047(8) 0.0045(8) 0.0017(8) C11 0.0325(11) 0.0382(12) 0.0146(10) 0.0001(8) 0.0003(8) 0.0193(10) C12 0.0197(10) 0.0412(12) 0.0211(10) 0.0051(9) 0.0019(8) 0.0184(9) C13 0.0268(10) 0.0319(11) 0.0153(9) 0.0066(8) 0.0099(8) 0.0142(9) C14 0.0308(11) 0.0238(10) 0.0211(10) 0.0118(8) 0.0085(9) 0.0082(9) C15 0.0305(11) 0.0317(11) 0.0348(12) 0.0159(9) 0.0151(9) 0.0232(10) C16 0.0407(12) 0.0165(10) 0.0329(12) 0.0012(8) 0.0158(10) 0.0121(9) _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 N1 2.1489(14) . ? Ru1 P1 2.2328(5) . ? Ru1 P2 2.2540(5) . ? Ru1 Cl1 2.4316(5) . ? Ru1 Cl2 2.5048(5) 2_676 ? Ru1 Cl2 2.5106(5) . ? Cl2 Ru1 2.5047(5) 2_676 ? P1 O1 1.6364(13) . ? P1 C1 1.8582(19) . ? P1 C2 1.8627(18) . ? P2 O2 1.6315(13) . ? P2 C3 1.8581(18) . ? P2 C4 1.8613(18) . ? O1 C5 1.430(2) . ? O2 C7 1.434(2) . ? N1 C6 1.483(2) . ? N1 C8 1.488(2) . ? N1 H1A 0.9300 . ? C1 C10 1.534(3) . ? C1 C9 1.539(3) . ? C1 H1 1.0000 . ? C2 C12 1.527(3) . ? C2 C11 1.531(3) . ? C2 H2 1.0000 . ? C3 C13 1.533(3) . ? C3 C14 1.534(3) . ? C3 H3 1.0000 . ? C4 C15 1.529(3) . ? C4 C16 1.534(3) . ? C4 H4 1.0000 . ? C5 C6 1.509(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.494(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 N1 Ru1 P1 93.64(4) . . ? N1 Ru1 P2 93.42(4) . . ? P1 Ru1 P2 102.065(18) . . ? N1 Ru1 Cl1 167.76(4) . . ? P1 Ru1 Cl1 93.663(17) . . ? P2 Ru1 Cl1 94.645(16) . . ? N1 Ru1 Cl2 86.15(4) . 2_676 ? P1 Ru1 Cl2 171.623(16) . 2_676 ? P2 Ru1 Cl2 86.304(17) . 2_676 ? Cl1 Ru1 Cl2 85.201(15) . 2_676 ? N1 Ru1 Cl2 82.09(4) . . ? P1 Ru1 Cl2 91.999(17) . . ? P2 Ru1 Cl2 165.508(16) . . ? Cl1 Ru1 Cl2 87.848(15) . . ? Cl2 Ru1 Cl2 79.671(16) 2_676 . ? Ru1 Cl2 Ru1 100.330(16) 2_676 . ? O1 P1 C1 99.07(8) . . ? O1 P1 C2 98.40(8) . . ? C1 P1 C2 106.75(8) . . ? O1 P1 Ru1 114.90(5) . . ? C1 P1 Ru1 113.95(6) . . ? C2 P1 Ru1 120.70(6) . . ? O2 P2 C3 95.71(7) . . ? O2 P2 C4 102.58(8) . . ? C3 P2 C4 105.05(8) . . ? O2 P2 Ru1 112.30(5) . . ? C3 P2 Ru1 127.70(6) . . ? C4 P2 Ru1 110.22(6) . . ? C5 O1 P1 126.09(11) . . ? C7 O2 P2 124.51(11) . . ? C6 N1 C8 109.82(14) . . ? C6 N1 Ru1 114.30(11) . . ? C8 N1 Ru1 121.44(11) . . ? C6 N1 H1A 102.8 . . ? C8 N1 H1A 102.8 . . ? Ru1 N1 H1A 102.8 . . ? C10 C1 C9 110.45(16) . . ? C10 C1 P1 115.98(13) . . ? C9 C1 P1 114.21(14) . . ? C10 C1 H1 105.0 . . ? C9 C1 H1 105.0 . . ? P1 C1 H1 105.0 . . ? C12 C2 C11 110.76(16) . . ? C12 C2 P1 112.97(13) . . ? C11 C2 P1 116.23(13) . . ? C12 C2 H2 105.3 . . ? C11 C2 H2 105.3 . . ? P1 C2 H2 105.3 . . ? C13 C3 C14 108.27(15) . . ? C13 C3 P2 109.98(12) . . ? C14 C3 P2 114.88(13) . . ? C13 C3 H3 107.8 . . ? C14 C3 H3 107.8 . . ? P2 C3 H3 107.8 . . ? C15 C4 C16 112.46(16) . . ? C15 C4 P2 112.58(13) . . ? C16 C4 P2 114.71(13) . . ? C15 C4 H4 105.4 . . ? C16 C4 H4 105.4 . . ? P2 C4 H4 105.4 . . ? O1 C5 C6 118.19(16) . . ? O1 C5 H5A 107.8 . . ? C6 C5 H5A 107.8 . . ? O1 C5 H5B 107.8 . . ? C6 C5 H5B 107.8 . . ? H5A C5 H5B 107.1 . . ? N1 C6 C5 115.06(15) . . ? N1 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? N1 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O2 C7 C8 113.72(16) . . ? O2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? O2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C7 114.73(15) . . ? N1 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.468 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 933824' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs061_0m_Compound_4 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16.50 H38 Cl2.50 F3 N O2 P2.50 Ru' _chemical_formula_weight 606.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.3095(13) _cell_length_b 15.5198(12) _cell_length_c 22.333(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4959.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6736 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43884 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11386 _reflns_number_gt 10407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0295P)^2^+4.6159P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(2) _refine_ls_number_reflns 11386 _refine_ls_number_parameters 530 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _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 Ru1 Ru 0.250470(15) 0.736146(15) 0.686709(11) 0.01518(5) Uani 1 1 d . . . Ru2 Ru 0.118380(15) 0.733444(14) 0.811986(11) 0.01467(5) Uani 1 1 d . . . Cl1 Cl 0.14324(6) 0.62438(5) 0.73535(4) 0.01879(16) Uani 1 1 d . A . Cl2 Cl 0.12347(5) 0.82779(4) 0.71876(3) 0.01773(15) Uani 1 1 d . A . Cl3 Cl 0.29143(5) 0.75116(5) 0.79646(4) 0.02469(18) Uani 1 1 d . A . Cl4 Cl 0.49252(10) 0.69956(8) 0.92098(6) 0.0608(3) Uani 1 1 d . . . Cl5 Cl 0.56602(10) 0.83400(9) 0.84474(8) 0.0772(5) Uani 1 1 d . . . P1 P 0.34807(6) 0.84238(5) 0.65800(4) 0.01979(17) Uani 1 1 d . A . P2 P 0.19322(6) 0.69314(5) 0.59684(4) 0.01781(17) Uani 1 1 d . A . P3 P 0.13878(6) 0.64189(5) 0.88951(4) 0.02032(18) Uani 1 1 d . A . P4 P -0.03939(5) 0.74486(5) 0.80913(4) 0.01750(16) Uani 1 1 d . A . P5 P 0.33745(7) 0.02924(6) 0.92096(4) 0.0298(2) Uani 1 1 d . . . F1 F 0.24077(18) 0.05499(18) 0.95091(11) 0.0522(7) Uani 1 1 d . . . F2 F 0.3497(2) -0.04682(15) 0.96878(11) 0.0520(7) Uani 1 1 d . . . F3 F 0.2843(2) -0.03654(19) 0.87761(12) 0.0680(9) Uani 1 1 d . . . F4 F 0.43401(18) 0.00271(16) 0.89043(13) 0.0531(7) Uani 1 1 d . . . F5 F 0.32590(18) 0.10399(16) 0.87271(11) 0.0480(6) Uani 1 1 d . . . F6 F 0.39125(17) 0.09374(14) 0.96412(10) 0.0430(6) Uani 1 1 d . . . O1 O 0.44541(17) 0.80621(16) 0.62884(13) 0.0366(7) Uani 1 1 d D . . O2 O 0.21749(18) 0.59211(15) 0.58378(12) 0.0321(6) Uani 1 1 d D . . O3 O 0.13129(18) 0.68971(15) 0.95467(10) 0.0278(5) Uani 1 1 d . . . O4 O -0.07101(15) 0.84561(13) 0.81170(12) 0.0251(5) Uani 1 1 d . . . N2 N 0.12878(19) 0.84667(16) 0.86710(12) 0.0206(6) Uani 1 1 d . A . H2B H 0.1896 0.8650 0.8598 0.025 Uiso 1 1 calc R . . C1 C 0.0644(2) 0.6897(2) 0.59746(15) 0.0206(7) Uani 1 1 d . . . H1A H 0.0472 0.6788 0.6402 0.025 Uiso 1 1 calc R A . C2 C 0.2241(2) 0.7382(2) 0.52294(14) 0.0243(7) Uani 1 1 d . . . H2A H 0.2098 0.8012 0.5243 0.029 Uiso 1 1 calc R A . C3 C 0.3187(2) 0.9170(2) 0.59662(15) 0.0227(7) Uani 1 1 d . . . H3A H 0.3137 0.8798 0.5602 0.027 Uiso 1 1 calc R A . C4 C 0.3910(3) 0.9101(2) 0.72090(17) 0.0350(9) Uani 1 1 d . . . H4A H 0.3954 0.8707 0.7562 0.042 Uiso 1 1 calc R A . N1 N 0.3608(2) 0.6441(4) 0.6831(3) 0.027(4) Uiso 0.731(7) 1 d PD A 1 H10D H 0.3490 0.6114 0.7172 0.032 Uiso 0.731(7) 1 calc PR A 1 C5 C 0.2717(3) 0.5380(3) 0.6210(2) 0.0240(12) Uani 0.731(7) 1 d PD A 1 H5A H 0.2810 0.4820 0.6007 0.029 Uiso 0.731(7) 1 calc PR A 1 H5B H 0.2370 0.5271 0.6586 0.029 Uiso 0.731(7) 1 calc PR A 1 C6 C 0.3666(3) 0.5763(3) 0.6362(2) 0.0329(14) Uani 0.731(7) 1 d PD A 1 H6A H 0.4085 0.5298 0.6503 0.040 Uiso 0.731(7) 1 calc PR A 1 H6B H 0.3944 0.6014 0.5996 0.040 Uiso 0.731(7) 1 calc PR A 1 C7 C 0.4965(3) 0.7320(3) 0.6456(3) 0.0381(14) Uani 0.731(7) 1 d PD A 1 H7A H 0.5603 0.7502 0.6573 0.046 Uiso 0.731(7) 1 calc PR A 1 H7B H 0.5027 0.6944 0.6100 0.046 Uiso 0.731(7) 1 calc PR A 1 C8 C 0.4552(3) 0.6791(3) 0.6964(2) 0.0303(13) Uani 0.731(7) 1 d PD A 1 H8A H 0.4979 0.6306 0.7054 0.036 Uiso 0.731(7) 1 calc PR A 1 H8B H 0.4514 0.7156 0.7327 0.036 Uiso 0.731(7) 1 calc PR A 1 N1B N 0.3607(4) 0.6409(9) 0.6888(9) 0.015(8) Uiso 0.269(7) 1 d PD A 2 H10E H 0.3718 0.6335 0.7295 0.018 Uiso 0.269(7) 1 calc PR A 2 C5B C 0.2988(7) 0.5493(9) 0.6040(5) 0.022(4) Uiso 0.269(7) 1 d PD A 2 H5BA H 0.3514 0.5707 0.5793 0.027 Uiso 0.269(7) 1 calc PR A 2 H5BB H 0.2909 0.4876 0.5942 0.027 Uiso 0.269(7) 1 calc PR A 2 C6B C 0.3307(8) 0.5538(7) 0.6689(5) 0.019(3) Uiso 0.269(7) 1 d PD A 2 H6BA H 0.2788 0.5343 0.6949 0.022 Uiso 0.269(7) 1 calc PR A 2 H6BB H 0.3833 0.5132 0.6745 0.022 Uiso 0.269(7) 1 calc PR A 2 C7B C 0.4865(11) 0.7535(7) 0.6733(5) 0.039(5) Uiso 0.269(7) 1 d PD A 2 H7BA H 0.4675 0.7739 0.7135 0.047 Uiso 0.269(7) 1 calc PR A 2 H7BB H 0.5554 0.7570 0.6705 0.047 Uiso 0.269(7) 1 calc PR A 2 C8B C 0.4549(7) 0.6609(8) 0.6644(7) 0.029(4) Uiso 0.269(7) 1 d PD A 2 H8BA H 0.4551 0.6480 0.6210 0.035 Uiso 0.269(7) 1 calc PR A 2 H8BB H 0.5010 0.6222 0.6836 0.035 Uiso 0.269(7) 1 calc PR A 2 C9 C 0.0232(2) 0.7784(2) 0.58285(16) 0.0264(8) Uani 1 1 d . A . H9A H -0.0452 0.7750 0.5835 0.040 Uiso 1 1 calc R . . H9B H 0.0441 0.7965 0.5430 0.040 Uiso 1 1 calc R . . H9C H 0.0443 0.8204 0.6127 0.040 Uiso 1 1 calc R . . C10 C 0.0162(3) 0.6178(2) 0.56192(17) 0.0307(8) Uani 1 1 d . A . H10A H -0.0517 0.6233 0.5661 0.046 Uiso 1 1 calc R . . H10B H 0.0362 0.5616 0.5774 0.046 Uiso 1 1 calc R . . H10C H 0.0333 0.6224 0.5196 0.046 Uiso 1 1 calc R . . C11 C 0.1698(3) 0.7004(3) 0.46945(16) 0.0362(9) Uani 1 1 d . A . H11A H 0.1910 0.7279 0.4324 0.054 Uiso 1 1 calc R . . H11B H 0.1029 0.7110 0.4749 0.054 Uiso 1 1 calc R . . H11C H 0.1811 0.6382 0.4671 0.054 Uiso 1 1 calc R . . C12 C 0.3286(3) 0.7295(3) 0.51067(17) 0.0341(9) Uani 1 1 d . A . H12A H 0.3431 0.7541 0.4713 0.051 Uiso 1 1 calc R . . H12B H 0.3461 0.6685 0.5112 0.051 Uiso 1 1 calc R . . H12C H 0.3638 0.7604 0.5416 0.051 Uiso 1 1 calc R . . C13 C 0.2219(3) 0.9575(2) 0.60377(17) 0.0286(8) Uani 1 1 d . A . H13A H 0.2097 0.9964 0.5701 0.043 Uiso 1 1 calc R . . H13B H 0.2194 0.9901 0.6413 0.043 Uiso 1 1 calc R . . H13C H 0.1744 0.9120 0.6045 0.043 Uiso 1 1 calc R . . C14 C 0.3925(3) 0.9845(2) 0.58084(17) 0.0325(9) Uani 1 1 d . A . H14A H 0.3698 1.0203 0.5478 0.049 Uiso 1 1 calc R . . H14B H 0.4504 0.9555 0.5688 0.049 Uiso 1 1 calc R . . H14C H 0.4046 1.0209 0.6159 0.049 Uiso 1 1 calc R . . C15 C 0.3226(3) 0.9799(3) 0.73863(18) 0.0403(11) Uani 1 1 d . A . H15A H 0.3485 1.0132 0.7720 0.060 Uiso 1 1 calc R . . H15B H 0.2635 0.9535 0.7510 0.060 Uiso 1 1 calc R . . H15C H 0.3116 1.0181 0.7044 0.060 Uiso 1 1 calc R . . C16 C 0.4902(3) 0.9473(3) 0.7121(2) 0.0505(12) Uani 1 1 d . A . H16A H 0.5076 0.9815 0.7473 0.076 Uiso 1 1 calc R . . H16B H 0.4911 0.9841 0.6764 0.076 Uiso 1 1 calc R . . H16C H 0.5349 0.9000 0.7070 0.076 Uiso 1 1 calc R . . C17 C -0.1210(2) 0.6946(2) 0.86284(16) 0.0251(7) Uani 1 1 d . . . H17A H -0.1106 0.6309 0.8608 0.030 Uiso 1 1 calc R A . C18 C -0.0882(2) 0.7206(2) 0.73371(15) 0.0238(7) Uani 1 1 d . . . H18A H -0.0363 0.7343 0.7053 0.029 Uiso 1 1 calc R A . C19 C 0.0553(2) 0.5546(2) 0.90450(16) 0.0237(7) Uani 1 1 d . . . H19A H -0.0050 0.5840 0.9140 0.028 Uiso 1 1 calc R A . C20 C 0.2590(3) 0.5953(2) 0.89448(18) 0.0333(9) Uani 1 1 d . . . H20A H 0.3021 0.6417 0.8802 0.040 Uiso 1 1 calc R A . C21 C -0.0328(2) 0.9090(2) 0.85129(17) 0.0269(8) Uani 1 1 d . A . H21A H -0.0474 0.8922 0.8930 0.032 Uiso 1 1 calc R . . H21B H -0.0641 0.9648 0.8434 0.032 Uiso 1 1 calc R . . C22 C 0.0718(2) 0.9218(2) 0.84587(16) 0.0238(7) Uani 1 1 d . . . H22A H 0.0873 0.9333 0.8034 0.029 Uiso 1 1 calc R A . H22B H 0.0898 0.9734 0.8693 0.029 Uiso 1 1 calc R . . C23 C 0.1809(3) 0.7700(2) 0.96030(16) 0.0321(8) Uani 1 1 d . A . H23A H 0.2420 0.7654 0.9397 0.038 Uiso 1 1 calc R . . H23B H 0.1930 0.7819 1.0032 0.038 Uiso 1 1 calc R . . C24 C 0.1255(3) 0.8440(2) 0.93350(15) 0.0268(8) Uani 1 1 d . . . H24A H 0.0595 0.8390 0.9464 0.032 Uiso 1 1 calc R A . H24B H 0.1502 0.8990 0.9494 0.032 Uiso 1 1 calc R . . C25 C -0.1029(3) 0.7224(2) 0.92789(16) 0.0307(8) Uani 1 1 d . A . H25A H -0.1478 0.6938 0.9544 0.046 Uiso 1 1 calc R . . H25B H -0.1102 0.7850 0.9313 0.046 Uiso 1 1 calc R . . H25C H -0.0393 0.7061 0.9395 0.046 Uiso 1 1 calc R . . C26 C -0.2255(2) 0.7107(3) 0.84939(19) 0.0366(9) Uani 1 1 d . A . H26A H -0.2638 0.6817 0.8797 0.055 Uiso 1 1 calc R . . H26B H -0.2408 0.6878 0.8097 0.055 Uiso 1 1 calc R . . H26C H -0.2382 0.7727 0.8503 0.055 Uiso 1 1 calc R . . C27 C -0.1699(2) 0.7762(3) 0.71250(18) 0.0345(9) Uani 1 1 d . A . H27A H -0.1893 0.7577 0.6724 0.052 Uiso 1 1 calc R . . H27B H -0.1505 0.8367 0.7112 0.052 Uiso 1 1 calc R . . H27C H -0.2225 0.7698 0.7403 0.052 Uiso 1 1 calc R . . C28 C -0.1066(3) 0.6244(2) 0.72475(18) 0.0329(9) Uani 1 1 d . A . H28A H -0.1318 0.6147 0.6845 0.049 Uiso 1 1 calc R . . H28B H -0.1518 0.6044 0.7547 0.049 Uiso 1 1 calc R . . H28C H -0.0480 0.5924 0.7293 0.049 Uiso 1 1 calc R . . C29 C 0.0764(3) 0.4980(2) 0.95903(19) 0.0378(10) Uani 1 1 d . A . H29A H 0.0278 0.4539 0.9630 0.057 Uiso 1 1 calc R . . H29B H 0.0777 0.5338 0.9952 0.057 Uiso 1 1 calc R . . H29C H 0.1373 0.4701 0.9538 0.057 Uiso 1 1 calc R . . C30 C 0.0350(3) 0.4995(2) 0.84847(18) 0.0346(9) Uani 1 1 d . A . H30A H -0.0099 0.4542 0.8587 0.052 Uiso 1 1 calc R . . H30B H 0.0932 0.4733 0.8342 0.052 Uiso 1 1 calc R . . H30C H 0.0088 0.5362 0.8169 0.052 Uiso 1 1 calc R . . C31 C 0.2923(3) 0.5726(3) 0.9585(2) 0.0444(11) Uani 1 1 d . A . H31A H 0.3556 0.5486 0.9567 0.067 Uiso 1 1 calc R . . H31B H 0.2499 0.5300 0.9761 0.067 Uiso 1 1 calc R . . H31C H 0.2925 0.6247 0.9832 0.067 Uiso 1 1 calc R . . C32 C 0.2738(3) 0.5201(3) 0.8522(2) 0.0460(12) Uani 1 1 d . A . H32A H 0.3376 0.4982 0.8567 0.069 Uiso 1 1 calc R . . H32B H 0.2641 0.5394 0.8108 0.069 Uiso 1 1 calc R . . H32C H 0.2291 0.4743 0.8617 0.069 Uiso 1 1 calc R . . C33 C 0.4890(3) 0.8086(3) 0.9028(2) 0.0534(12) Uani 1 1 d . . . H33A H 0.5053 0.8430 0.9387 0.064 Uiso 1 1 calc R . . H33B H 0.4246 0.8242 0.8908 0.064 Uiso 1 1 calc R . . 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 0.01610(10) 0.01273(10) 0.01671(11) 0.00028(11) 0.00155(10) 0.00197(9) Ru2 0.01430(10) 0.01109(10) 0.01863(11) -0.00011(11) 0.00247(10) -0.00117(9) Cl1 0.0224(4) 0.0137(3) 0.0203(4) -0.0007(3) 0.0021(3) -0.0010(3) Cl2 0.0184(3) 0.0136(3) 0.0213(4) 0.0008(3) 0.0039(3) 0.0017(3) Cl3 0.0230(4) 0.0250(4) 0.0261(4) 0.0023(3) 0.0025(3) -0.0015(3) Cl4 0.0741(9) 0.0412(6) 0.0673(8) 0.0104(6) -0.0159(7) -0.0107(6) Cl5 0.0519(7) 0.0605(8) 0.1191(13) 0.0305(9) 0.0240(8) 0.0146(6) P1 0.0173(4) 0.0182(4) 0.0240(4) 0.0015(3) 0.0015(3) 0.0001(3) P2 0.0218(4) 0.0133(4) 0.0184(4) -0.0015(3) 0.0017(3) 0.0023(3) P3 0.0204(4) 0.0165(4) 0.0241(5) 0.0024(3) 0.0001(4) -0.0008(3) P4 0.0152(3) 0.0142(4) 0.0232(4) -0.0010(3) 0.0027(3) -0.0002(3) P5 0.0346(5) 0.0290(5) 0.0260(5) -0.0073(4) 0.0041(4) -0.0114(4) F1 0.0416(14) 0.0692(17) 0.0458(15) -0.0007(13) 0.0105(12) 0.0009(13) F2 0.0781(19) 0.0318(12) 0.0460(15) 0.0035(12) 0.0165(14) 0.0043(13) F3 0.083(2) 0.077(2) 0.0443(15) -0.0246(14) 0.0140(15) -0.0608(17) F4 0.0512(15) 0.0404(14) 0.0678(18) -0.0104(13) 0.0309(14) -0.0081(12) F5 0.0616(16) 0.0492(15) 0.0331(13) 0.0054(12) -0.0061(12) -0.0138(12) F6 0.0541(15) 0.0340(12) 0.0410(13) -0.0129(10) -0.0161(12) -0.0025(11) O1 0.0218(12) 0.0267(13) 0.0612(19) 0.0098(13) 0.0118(13) 0.0054(11) O2 0.0407(15) 0.0162(12) 0.0395(16) -0.0073(11) -0.0117(13) 0.0089(11) O3 0.0396(14) 0.0235(12) 0.0202(12) 0.0023(10) -0.0021(11) -0.0053(11) O4 0.0227(11) 0.0169(11) 0.0357(13) -0.0035(11) -0.0003(12) 0.0051(9) N2 0.0229(14) 0.0124(12) 0.0265(15) -0.0036(11) 0.0015(12) -0.0032(11) C1 0.0228(16) 0.0196(16) 0.0194(17) 0.0000(13) -0.0020(13) 0.0020(13) C2 0.0335(18) 0.0186(15) 0.0207(16) -0.0026(14) 0.0058(14) 0.0007(14) C3 0.0296(18) 0.0202(16) 0.0183(17) -0.0014(14) 0.0034(14) -0.0034(14) C4 0.044(2) 0.031(2) 0.029(2) 0.0031(16) -0.0115(18) -0.0139(18) C5 0.028(3) 0.014(2) 0.030(3) -0.001(2) 0.006(3) 0.008(2) C6 0.035(3) 0.023(2) 0.041(3) -0.003(2) 0.002(3) 0.014(2) C7 0.019(2) 0.030(3) 0.065(4) 0.001(3) 0.006(3) 0.005(2) C8 0.024(2) 0.032(3) 0.035(3) 0.004(2) -0.006(2) 0.006(2) C9 0.0265(17) 0.0225(18) 0.0301(19) -0.0023(15) -0.0091(15) 0.0041(14) C10 0.036(2) 0.0239(18) 0.032(2) 0.0013(16) -0.0064(17) -0.0086(16) C11 0.056(3) 0.032(2) 0.0202(19) -0.0003(16) 0.0020(18) -0.0068(19) C12 0.044(2) 0.0253(18) 0.033(2) -0.0060(18) 0.0157(17) 0.0010(18) C13 0.034(2) 0.0221(18) 0.030(2) 0.0015(15) -0.0028(16) 0.0056(15) C14 0.037(2) 0.0299(19) 0.031(2) 0.0060(16) 0.0044(17) -0.0103(17) C15 0.053(3) 0.043(2) 0.025(2) -0.0133(18) 0.0047(19) -0.018(2) C16 0.043(2) 0.050(3) 0.058(3) 0.010(2) -0.018(2) -0.021(2) C17 0.0172(15) 0.0222(16) 0.036(2) 0.0032(15) 0.0104(15) -0.0001(14) C18 0.0174(14) 0.0269(18) 0.0273(18) 0.0002(15) -0.0015(13) -0.0029(13) C19 0.0279(17) 0.0147(15) 0.0284(19) 0.0063(14) 0.0024(15) -0.0022(13) C20 0.0208(17) 0.0309(19) 0.048(2) 0.0121(17) -0.0004(18) 0.0021(16) C21 0.0322(19) 0.0164(16) 0.032(2) -0.0045(14) 0.0038(16) 0.0033(14) C22 0.0313(18) 0.0091(14) 0.0311(19) -0.0027(13) 0.0052(16) -0.0004(13) C23 0.041(2) 0.0293(18) 0.0261(18) -0.0020(17) -0.0061(16) -0.0054(18) C24 0.0359(19) 0.0217(16) 0.0228(18) -0.0044(14) -0.0007(16) -0.0081(16) C25 0.0307(18) 0.030(2) 0.0319(19) 0.0025(16) 0.0119(15) 0.0026(15) C26 0.0187(17) 0.041(2) 0.050(2) 0.0063(19) 0.0091(17) 0.0032(15) C27 0.0285(18) 0.036(2) 0.038(2) 0.0016(19) -0.0048(16) 0.0019(16) C28 0.0295(19) 0.0308(19) 0.039(2) -0.0100(17) -0.0073(17) -0.0037(16) C29 0.040(2) 0.029(2) 0.044(2) 0.0173(18) 0.0083(19) -0.0016(18) C30 0.037(2) 0.0233(18) 0.043(2) 0.0009(17) 0.0059(19) -0.0099(16) C31 0.041(2) 0.044(2) 0.048(3) 0.013(2) -0.015(2) 0.002(2) C32 0.038(2) 0.055(3) 0.045(3) 0.009(2) 0.008(2) 0.026(2) C33 0.053(3) 0.036(2) 0.072(3) 0.004(2) 0.012(3) 0.001(2) _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 N1 2.131(6) . ? Ru1 N1B 2.163(13) . ? Ru1 P1 2.2539(9) . ? Ru1 P2 2.2682(9) . ? Ru1 Cl2 2.4162(8) . ? Ru1 Cl3 2.5309(9) . ? Ru1 Cl1 2.5580(8) . ? Ru2 N2 2.151(3) . ? Ru2 P3 2.2587(9) . ? Ru2 P4 2.2655(8) . ? Ru2 Cl1 2.4332(8) . ? Ru2 Cl3 2.5155(8) . ? Ru2 Cl2 2.5463(8) . ? Cl4 C33 1.740(5) . ? Cl5 C33 1.747(5) . ? P1 O1 1.637(3) . ? P1 C3 1.843(4) . ? P1 C4 1.859(4) . ? P2 O2 1.632(2) . ? P2 C1 1.844(3) . ? P2 C2 1.846(3) . ? P3 O3 1.637(3) . ? P3 C19 1.837(3) . ? P3 C20 1.869(4) . ? P4 O4 1.629(2) . ? P4 C17 1.847(3) . ? P4 C18 1.862(3) . ? P5 F1 1.588(3) . ? P5 F6 1.589(2) . ? P5 F5 1.592(3) . ? P5 F4 1.595(3) . ? P5 F3 1.599(3) . ? P5 F2 1.602(3) . ? O1 C7 1.414(3) . ? O1 C7B 1.414(3) . ? O2 C5 1.414(3) . ? O2 C5B 1.414(3) . ? O3 C23 1.440(4) . ? O4 C21 1.432(4) . ? N2 C24 1.484(4) . ? N2 C22 1.500(4) . ? N2 H2B 0.9300 . ? C1 C9 1.533(4) . ? C1 C10 1.534(5) . ? C1 H1A 1.0000 . ? C2 C12 1.526(5) . ? C2 C11 1.541(5) . ? C2 H2A 1.0000 . ? C3 C14 1.528(5) . ? C3 C13 1.530(5) . ? C3 H3A 1.0000 . ? C4 C15 1.513(6) . ? C4 C16 1.545(6) . ? C4 H4A 1.0000 . ? N1 C6 1.486(3) . ? N1 C8 1.487(3) . ? N1 H10D 0.9300 . ? C5 C6 1.521(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1B C6B 1.487(3) . ? N1B C8B 1.487(4) . ? N1B H10E 0.9300 . ? C5B C6B 1.521(5) . ? C5B H5BA 0.9900 . ? C5B H5BB 0.9900 . ? C6B H6BA 0.9900 . ? C6B H6BB 0.9900 . ? C7B C8B 1.521(5) . ? C7B H7BA 0.9900 . ? C7B H7BB 0.9900 . ? C8B H8BA 0.9900 . ? C8B H8BB 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C25 1.537(5) . ? C17 C26 1.546(5) . ? C17 H17A 1.0000 . ? C18 C27 1.529(5) . ? C18 C28 1.529(5) . ? C18 H18A 1.0000 . ? C19 C29 1.531(5) . ? C19 C30 1.543(5) . ? C19 H19A 1.0000 . ? C20 C32 1.516(6) . ? C20 C31 1.548(5) . ? C20 H20A 1.0000 . ? C21 C22 1.515(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.518(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 N1 Ru1 N1B 3.5(7) . . ? N1 Ru1 P1 91.18(16) . . ? N1B Ru1 P1 93.1(3) . . ? N1 Ru1 P2 92.12(14) . . ? N1B Ru1 P2 94.7(4) . . ? P1 Ru1 P2 100.80(3) . . ? N1 Ru1 Cl2 164.4(2) . . ? N1B Ru1 Cl2 160.9(5) . . ? P1 Ru1 Cl2 96.88(3) . . ? P2 Ru1 Cl2 99.42(3) . . ? N1 Ru1 Cl3 85.79(18) . . ? N1B Ru1 Cl3 82.7(5) . . ? P1 Ru1 Cl3 93.71(3) . . ? P2 Ru1 Cl3 165.39(3) . . ? Cl2 Ru1 Cl3 80.39(3) . . ? N1 Ru1 Cl1 90.33(18) . . ? N1B Ru1 Cl1 88.0(4) . . ? P1 Ru1 Cl1 171.32(3) . . ? P2 Ru1 Cl1 87.68(3) . . ? Cl2 Ru1 Cl1 79.76(3) . . ? Cl3 Ru1 Cl1 77.88(3) . . ? N2 Ru2 P3 93.80(8) . . ? N2 Ru2 P4 91.21(8) . . ? P3 Ru2 P4 101.51(3) . . ? N2 Ru2 Cl1 163.91(8) . . ? P3 Ru2 Cl1 94.74(3) . . ? P4 Ru2 Cl1 100.39(3) . . ? N2 Ru2 Cl3 85.49(8) . . ? P3 Ru2 Cl3 92.70(3) . . ? P4 Ru2 Cl3 165.60(3) . . ? Cl1 Ru2 Cl3 80.51(3) . . ? N2 Ru2 Cl2 89.78(7) . . ? P3 Ru2 Cl2 169.99(3) . . ? P4 Ru2 Cl2 87.74(3) . . ? Cl1 Ru2 Cl2 79.67(3) . . ? Cl3 Ru2 Cl2 78.25(3) . . ? Ru2 Cl1 Ru1 85.11(2) . . ? Ru1 Cl2 Ru2 85.71(2) . . ? Ru2 Cl3 Ru1 84.00(3) . . ? O1 P1 C3 96.54(15) . . ? O1 P1 C4 102.30(18) . . ? C3 P1 C4 106.40(16) . . ? O1 P1 Ru1 112.93(10) . . ? C3 P1 Ru1 122.00(12) . . ? C4 P1 Ru1 113.79(13) . . ? O2 P2 C1 100.72(15) . . ? O2 P2 C2 98.81(15) . . ? C1 P2 C2 104.91(15) . . ? O2 P2 Ru1 111.34(10) . . ? C1 P2 Ru1 111.28(11) . . ? C2 P2 Ru1 126.37(11) . . ? O3 P3 C19 97.46(15) . . ? O3 P3 C20 100.53(16) . . ? C19 P3 C20 107.58(17) . . ? O3 P3 Ru2 112.81(9) . . ? C19 P3 Ru2 121.32(12) . . ? C20 P3 Ru2 114.06(13) . . ? O4 P4 C17 101.95(14) . . ? O4 P4 C18 97.00(14) . . ? C17 P4 C18 105.36(16) . . ? O4 P4 Ru2 110.55(8) . . ? C17 P4 Ru2 125.35(12) . . ? C18 P4 Ru2 112.55(11) . . ? F1 P5 F6 90.46(14) . . ? F1 P5 F5 90.65(15) . . ? F6 P5 F5 90.11(13) . . ? F1 P5 F4 179.41(16) . . ? F6 P5 F4 90.13(14) . . ? F5 P5 F4 89.36(15) . . ? F1 P5 F3 90.09(16) . . ? F6 P5 F3 179.28(18) . . ? F5 P5 F3 90.35(15) . . ? F4 P5 F3 89.33(16) . . ? F1 P5 F2 90.00(15) . . ? F6 P5 F2 90.38(14) . . ? F5 P5 F2 179.18(15) . . ? F4 P5 F2 89.99(15) . . ? F3 P5 F2 89.16(16) . . ? C7 O1 C7B 29.4(6) . . ? C7 O1 P1 127.9(3) . . ? C7B O1 P1 105.8(8) . . ? C5 O2 C5B 23.3(5) . . ? C5 O2 P2 125.6(3) . . ? C5B O2 P2 124.7(6) . . ? C23 O3 P3 116.0(2) . . ? C21 O4 P4 125.2(2) . . ? C24 N2 C22 108.7(3) . . ? C24 N2 Ru2 123.1(2) . . ? C22 N2 Ru2 114.6(2) . . ? C24 N2 H2B 102.4 . . ? C22 N2 H2B 102.4 . . ? Ru2 N2 H2B 102.4 . . ? C9 C1 C10 111.7(3) . . ? C9 C1 P2 110.9(2) . . ? C10 C1 P2 117.9(2) . . ? C9 C1 H1A 105.0 . . ? C10 C1 H1A 105.0 . . ? P2 C1 H1A 105.0 . . ? C12 C2 C11 108.7(3) . . ? C12 C2 P2 111.2(2) . . ? C11 C2 P2 115.3(2) . . ? C12 C2 H2A 107.1 . . ? C11 C2 H2A 107.1 . . ? P2 C2 H2A 107.1 . . ? C14 C3 C13 111.6(3) . . ? C14 C3 P1 116.4(3) . . ? C13 C3 P1 112.8(2) . . ? C14 C3 H3A 104.9 . . ? C13 C3 H3A 104.9 . . ? P1 C3 H3A 104.9 . . ? C15 C4 C16 111.1(3) . . ? C15 C4 P1 112.9(3) . . ? C16 C4 P1 114.8(3) . . ? C15 C4 H4A 105.8 . . ? C16 C4 H4A 105.8 . . ? P1 C4 H4A 105.8 . . ? C6 N1 C8 110.4(4) . . ? C6 N1 Ru1 122.9(4) . . ? C8 N1 Ru1 114.9(4) . . ? C6 N1 H10D 101.6 . . ? C8 N1 H10D 101.6 . . ? Ru1 N1 H10D 101.6 . . ? O2 C5 C6 112.9(4) . . ? O2 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? O2 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C5 112.6(4) . . ? N1 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O1 C7 C8 115.8(4) . . ? O1 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? O1 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C7 113.7(5) . . ? N1 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C6B N1B C8B 110.1(10) . . ? C6B N1B Ru1 113.8(6) . . ? C8B N1B Ru1 120.8(12) . . ? C6B N1B H10E 103.2 . . ? C8B N1B H10E 103.2 . . ? Ru1 N1B H10E 103.2 . . ? O2 C5B C6B 122.0(8) . . ? O2 C5B H5BA 106.8 . . ? C6B C5B H5BA 106.8 . . ? O2 C5B H5BB 106.8 . . ? C6B C5B H5BB 106.8 . . ? H5BA C5B H5BB 106.7 . . ? N1B C6B C5B 114.3(12) . . ? N1B C6B H6BA 108.7 . . ? C5B C6B H6BA 108.7 . . ? N1B C6B H6BB 108.7 . . ? C5B C6B H6BB 108.7 . . ? H6BA C6B H6BB 107.6 . . ? O1 C7B C8B 109.3(9) . . ? O1 C7B H7BA 109.8 . . ? C8B C7B H7BA 109.8 . . ? O1 C7B H7BB 109.8 . . ? C8B C7B H7BB 109.8 . . ? H7BA C7B H7BB 108.3 . . ? N1B C8B C7B 114.7(11) . . ? N1B C8B H8BA 108.6 . . ? C7B C8B H8BA 108.6 . . ? N1B C8B H8BB 108.6 . . ? C7B C8B H8BB 108.6 . . ? H8BA C8B H8BB 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C25 C17 C26 107.5(3) . . ? C25 C17 P4 112.9(2) . . ? C26 C17 P4 114.7(2) . . ? C25 C17 H17A 107.1 . . ? C26 C17 H17A 107.1 . . ? P4 C17 H17A 107.1 . . ? C27 C18 C28 112.3(3) . . ? C27 C18 P4 116.9(3) . . ? C28 C18 P4 112.4(2) . . ? C27 C18 H18A 104.6 . . ? C28 C18 H18A 104.6 . . ? P4 C18 H18A 104.6 . . ? C29 C19 C30 111.4(3) . . ? C29 C19 P3 116.1(3) . . ? C30 C19 P3 112.5(2) . . ? C29 C19 H19A 105.2 . . ? C30 C19 H19A 105.2 . . ? P3 C19 H19A 105.2 . . ? C32 C20 C31 110.9(3) . . ? C32 C20 P3 112.9(3) . . ? C31 C20 P3 115.2(3) . . ? C32 C20 H20A 105.6 . . ? C31 C20 H20A 105.6 . . ? P3 C20 H20A 105.6 . . ? O4 C21 C22 114.7(3) . . ? O4 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? O4 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? N2 C22 C21 114.2(3) . . ? N2 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? N2 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? O3 C23 C24 111.2(3) . . ? O3 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? O3 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N2 C24 C23 113.5(3) . . ? N2 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? N2 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C17 C25 H25A 109.5 . . ? C17 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C17 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 H26A 109.5 . . ? C17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C18 C27 H27A 109.5 . . ? C18 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C18 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C29 H29A 109.5 . . ? C19 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C19 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C19 C30 H30A 109.5 . . ? C19 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C19 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C20 C31 H31A 109.5 . . ? C20 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C20 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C20 C32 H32A 109.5 . . ? C20 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C20 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl4 C33 Cl5 112.0(3) . . ? Cl4 C33 H33A 109.2 . . ? Cl5 C33 H33A 109.2 . . ? Cl4 C33 H33B 109.2 . . ? Cl5 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.047 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 933825' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs047_Compound_6 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C34 H53 Cl N O2 P3 Ru' _chemical_formula_weight 737.20 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.9644(8) _cell_length_b 17.3583(8) _cell_length_c 20.1248(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.167(3) _cell_angle_gamma 90.00 _cell_volume 7672.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3317 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 23.07 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6683 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29264 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_unetI/netI 0.0881 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8769 _reflns_number_gt 5894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0363P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8769 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.239 0.750 219 70 ' ' 2 1.000 0.261 0.250 219 70 ' ' 3 0.500 0.196 0.250 27 3 ' ' 4 0.000 0.304 0.750 27 3 ' ' 5 0.000 0.738 0.750 219 70 ' ' 6 0.500 0.761 0.250 219 70 ' ' 7 0.000 0.696 0.250 27 3 ' ' 8 0.500 0.804 0.750 27 3 ' ' _platon_squeeze_details ;PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: During the refinement of the structure, electron density peaks were located that were believed to be highly disordered solvent molecules (possibly methylene chloride). Attempts made to model the solvent molecule were not successful. The SQUEEZE option in PLATON (Spek, 2009) indicated there was a large solvent cavity 1034.6 Ang^3. In the final cycles of refinement, this contribution (295) to the electron density was removed from the observed data. The density, the F(000) value, the molecular weight and the formula are given without taking into account the results obtained with the SQUEEZE option PLATON (Spek, 2009). Similar treatments of disordered solvent molecules were carried out by St\"ahler et al. (2001), Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). References: Spek, A. L. (2009). Acta Cryst. D65, 148--155. Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). Acta Cryst. E61, m2014-m2017. Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. (2003). Acta Cryst. E59, o975-o977. Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. (2003). Acta Cryst. C59, m84-m86. Stahler, R., Nather, C. & Bensch, W. (2001). Acta Cryst. C57, 26-27. ; 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 0.748283(11) -0.014405(15) 0.562367(12) 0.01361(7) Uani 1 1 d . . . Cl1 Cl 0.80646(4) -0.13664(5) 0.59817(4) 0.02199(18) Uani 1 1 d . . . P1 P 0.83760(4) 0.05139(5) 0.53195(4) 0.01691(19) Uani 1 1 d . . . P2 P 0.64836(4) -0.06352(5) 0.55447(4) 0.0193(2) Uani 1 1 d . . . P3 P 0.74125(4) 0.03211(5) 0.66822(4) 0.01553(18) Uani 1 1 d . . . O1 O 0.83565(10) 0.06959(13) 0.45142(10) 0.0231(5) Uani 1 1 d . . . O2 O 0.63238(11) -0.10083(17) 0.48197(12) 0.0458(8) Uani 1 1 d . . . N1 N 0.76292(12) -0.06399(15) 0.46121(12) 0.0184(6) Uani 1 1 d . . . H1B H 0.8043 -0.0754 0.4624 0.022 Uiso 1 1 calc R . . C1 C 0.91338(14) 0.00484(19) 0.52937(16) 0.0235(8) Uani 1 1 d . . . H1A H 0.9418 0.0428 0.5085 0.028 Uiso 1 1 calc R . . C2 C 0.85591(16) 0.14883(19) 0.56397(17) 0.0258(8) Uani 1 1 d . . . H2A H 0.8529 0.1465 0.6135 0.031 Uiso 1 1 calc R . . C3 C 0.61730(15) -0.13926(19) 0.61018(17) 0.0245(8) Uani 1 1 d . . . H3A H 0.6207 -0.1199 0.6569 0.029 Uiso 1 1 calc R . . C4 C 0.58299(15) 0.0028(2) 0.54762(16) 0.0258(8) Uani 1 1 d . . . H4A H 0.5484 -0.0295 0.5312 0.031 Uiso 1 1 calc R . . C5 C 0.77853(15) 0.0677(2) 0.41580(16) 0.0242(8) Uani 1 1 d . . . H5A H 0.7829 0.0960 0.3734 0.029 Uiso 1 1 calc R . . H5B H 0.7469 0.0939 0.4424 0.029 Uiso 1 1 calc R . . C6 C 0.75891(16) -0.0138(2) 0.40173(16) 0.0263(8) Uani 1 1 d . . . H6A H 0.7164 -0.0134 0.3853 0.032 Uiso 1 1 calc R . . H6B H 0.7849 -0.0354 0.3662 0.032 Uiso 1 1 calc R . . C7 C 0.66874(16) -0.1404(2) 0.43532(17) 0.0293(9) Uani 1 1 d . . . H7A H 0.6620 -0.1169 0.3911 0.035 Uiso 1 1 calc R . . H7B H 0.6543 -0.1944 0.4328 0.035 Uiso 1 1 calc R . . C8 C 0.73574(16) -0.1414(2) 0.44886(17) 0.0268(8) Uani 1 1 d . . . H8A H 0.7435 -0.1744 0.4881 0.032 Uiso 1 1 calc R . . H8B H 0.7566 -0.1652 0.4104 0.032 Uiso 1 1 calc R . . C9 C 0.93803(15) -0.0114(2) 0.59904(17) 0.0306(9) Uani 1 1 d . . . H9A H 0.9782 -0.0357 0.5957 0.046 Uiso 1 1 calc R . . H9B H 0.9101 -0.0461 0.6224 0.046 Uiso 1 1 calc R . . H9C H 0.9416 0.0371 0.6237 0.046 Uiso 1 1 calc R . . C10 C 0.91505(15) -0.0679(2) 0.48597(17) 0.0299(9) Uani 1 1 d . . . H10A H 0.9563 -0.0895 0.4864 0.045 Uiso 1 1 calc R . . H10B H 0.9036 -0.0546 0.4403 0.045 Uiso 1 1 calc R . . H10C H 0.8864 -0.1060 0.5035 0.045 Uiso 1 1 calc R . . C11 C 0.91914(17) 0.1805(2) 0.5473(2) 0.0464(11) Uani 1 1 d . . . H11A H 0.9239 0.2318 0.5669 0.070 Uiso 1 1 calc R . . H11B H 0.9236 0.1840 0.4989 0.070 Uiso 1 1 calc R . . H11C H 0.9504 0.1459 0.5653 0.070 Uiso 1 1 calc R . . C12 C 0.80837(17) 0.2063(2) 0.54007(19) 0.0329(9) Uani 1 1 d . . . H12A H 0.8181 0.2575 0.5575 0.049 Uiso 1 1 calc R . . H12B H 0.7681 0.1905 0.5559 0.049 Uiso 1 1 calc R . . H12C H 0.8083 0.2078 0.4914 0.049 Uiso 1 1 calc R . . C13 C 0.55063(16) -0.1615(2) 0.5980(2) 0.0384(10) Uani 1 1 d . . . H13A H 0.5385 -0.2013 0.6299 0.058 Uiso 1 1 calc R . . H13B H 0.5460 -0.1814 0.5527 0.058 Uiso 1 1 calc R . . H13C H 0.5247 -0.1160 0.6036 0.058 Uiso 1 1 calc R . . C14 C 0.65725(17) -0.2117(2) 0.6046(2) 0.0384(10) Uani 1 1 d . . . H14A H 0.6414 -0.2518 0.6341 0.058 Uiso 1 1 calc R . . H14B H 0.6991 -0.1990 0.6175 0.058 Uiso 1 1 calc R . . H14C H 0.6567 -0.2303 0.5586 0.058 Uiso 1 1 calc R . . C15 C 0.59182(17) 0.0648(2) 0.49502(19) 0.0404(10) Uani 1 1 d . . . H15A H 0.5557 0.0979 0.4933 0.061 Uiso 1 1 calc R . . H15B H 0.5979 0.0405 0.4516 0.061 Uiso 1 1 calc R . . H15C H 0.6276 0.0960 0.5063 0.061 Uiso 1 1 calc R . . C16 C 0.56110(16) 0.0371(2) 0.61337(19) 0.0353(9) Uani 1 1 d . . . H16A H 0.5263 0.0711 0.6051 0.053 Uiso 1 1 calc R . . H16B H 0.5942 0.0667 0.6339 0.053 Uiso 1 1 calc R . . H16C H 0.5488 -0.0046 0.6433 0.053 Uiso 1 1 calc R . . C17 C 0.81378(15) 0.04327(18) 0.71644(14) 0.0171(7) Uani 1 1 d . . . C18 C 0.83867(15) 0.1146(2) 0.73144(16) 0.0254(8) Uani 1 1 d . . . H18A H 0.8180 0.1599 0.7176 0.030 Uiso 1 1 calc R . . C19 C 0.89298(16) 0.1213(2) 0.76613(18) 0.0318(9) Uani 1 1 d . . . H19A H 0.9090 0.1710 0.7757 0.038 Uiso 1 1 calc R . . C20 C 0.92392(17) 0.0569(2) 0.78686(17) 0.0332(9) Uani 1 1 d . . . H20A H 0.9609 0.0617 0.8111 0.040 Uiso 1 1 calc R . . C21 C 0.90058(16) -0.0148(2) 0.77212(18) 0.0331(9) Uani 1 1 d . . . H21A H 0.9213 -0.0598 0.7866 0.040 Uiso 1 1 calc R . . C22 C 0.84682(15) -0.0211(2) 0.73607(17) 0.0268(8) Uani 1 1 d . . . H22A H 0.8322 -0.0708 0.7245 0.032 Uiso 1 1 calc R . . C23 C 0.70754(14) 0.12776(18) 0.68529(15) 0.0179(7) Uani 1 1 d . . . C24 C 0.68132(14) 0.17096(18) 0.63541(16) 0.0191(7) Uani 1 1 d . . . H24A H 0.6810 0.1517 0.5912 0.023 Uiso 1 1 calc R . . C25 C 0.65522(16) 0.24242(19) 0.64875(18) 0.0279(8) Uani 1 1 d . . . H25A H 0.6371 0.2714 0.6138 0.033 Uiso 1 1 calc R . . C26 C 0.65566(16) 0.27079(19) 0.71209(18) 0.0280(9) Uani 1 1 d . . . H26A H 0.6382 0.3198 0.7209 0.034 Uiso 1 1 calc R . . C27 C 0.68135(16) 0.22888(19) 0.76346(17) 0.0245(8) Uani 1 1 d . . . H27A H 0.6814 0.2487 0.8075 0.029 Uiso 1 1 calc R . . C28 C 0.70693(15) 0.15772(18) 0.74990(16) 0.0208(7) Uani 1 1 d . . . H28A H 0.7244 0.1287 0.7851 0.025 Uiso 1 1 calc R . . C29 C 0.69623(14) -0.02747(18) 0.72766(14) 0.0176(7) Uani 1 1 d . . . C30 C 0.71379(15) -0.10354(19) 0.73956(16) 0.0229(8) Uani 1 1 d . . . H30A H 0.7486 -0.1239 0.7179 0.027 Uiso 1 1 calc R . . C31 C 0.68090(17) -0.1497(2) 0.78265(17) 0.0285(8) Uani 1 1 d . . . H31A H 0.6941 -0.2009 0.7912 0.034 Uiso 1 1 calc R . . C32 C 0.62946(17) -0.1224(2) 0.81315(17) 0.0326(9) Uani 1 1 d . . . H32A H 0.6075 -0.1541 0.8432 0.039 Uiso 1 1 calc R . . C33 C 0.61019(17) -0.0491(2) 0.79992(17) 0.0303(9) Uani 1 1 d . . . H33A H 0.5736 -0.0307 0.8193 0.036 Uiso 1 1 calc R . . C34 C 0.64370(15) -0.00125(19) 0.75837(15) 0.0236(8) Uani 1 1 d . . . H34A H 0.6304 0.0501 0.7509 0.028 Uiso 1 1 calc R . . H100 H 0.7175(14) 0.0583(17) 0.5311(15) 0.027(9) Uiso 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 Ru1 0.01484(13) 0.01461(13) 0.01137(12) 0.00005(11) -0.00048(9) 0.00145(11) Cl1 0.0232(4) 0.0207(4) 0.0221(4) 0.0045(3) -0.0005(3) 0.0049(3) P1 0.0159(4) 0.0212(5) 0.0136(4) 0.0008(3) -0.0003(3) -0.0010(3) P2 0.0167(5) 0.0245(5) 0.0167(4) -0.0023(4) -0.0019(4) -0.0001(4) P3 0.0187(4) 0.0157(5) 0.0122(4) -0.0001(3) -0.0006(3) 0.0013(3) O1 0.0237(13) 0.0312(14) 0.0143(12) 0.0028(10) -0.0004(10) -0.0043(10) O2 0.0229(15) 0.080(2) 0.0340(15) -0.0296(15) -0.0004(12) -0.0045(14) N1 0.0201(15) 0.0196(15) 0.0155(14) -0.0024(11) 0.0009(11) 0.0004(12) C1 0.0180(17) 0.026(2) 0.0261(19) 0.0024(15) 0.0026(14) -0.0004(14) C2 0.035(2) 0.0204(19) 0.0218(19) -0.0030(15) -0.0009(16) -0.0061(16) C3 0.0177(18) 0.024(2) 0.032(2) 0.0058(16) -0.0004(15) -0.0048(15) C4 0.0169(17) 0.033(2) 0.0273(19) 0.0065(16) -0.0065(14) 0.0003(15) C5 0.027(2) 0.031(2) 0.0150(17) 0.0072(15) -0.0009(15) -0.0015(16) C6 0.031(2) 0.034(2) 0.0136(17) 0.0052(16) -0.0019(14) -0.0042(17) C7 0.036(2) 0.032(2) 0.0199(19) -0.0082(16) 0.0013(16) -0.0092(17) C8 0.035(2) 0.023(2) 0.0228(19) -0.0080(15) 0.0039(16) 0.0019(16) C9 0.0191(18) 0.044(2) 0.029(2) 0.0029(18) -0.0020(15) 0.0015(17) C10 0.0179(19) 0.040(2) 0.032(2) -0.0013(17) 0.0042(16) 0.0049(16) C11 0.030(2) 0.035(3) 0.074(3) 0.000(2) -0.003(2) -0.0133(19) C12 0.033(2) 0.020(2) 0.045(2) 0.0005(17) 0.0092(18) 0.0000(17) C13 0.029(2) 0.035(2) 0.051(3) 0.010(2) -0.0029(19) -0.0112(18) C14 0.030(2) 0.026(2) 0.060(3) 0.0077(19) 0.001(2) -0.0029(17) C15 0.028(2) 0.045(3) 0.048(3) 0.021(2) -0.0095(19) 0.0013(18) C16 0.023(2) 0.034(2) 0.049(3) -0.0035(19) 0.0006(18) 0.0080(16) C17 0.0241(18) 0.0186(18) 0.0087(15) 0.0007(13) 0.0022(13) 0.0013(14) C18 0.027(2) 0.021(2) 0.028(2) -0.0029(15) -0.0011(16) 0.0017(15) C19 0.028(2) 0.031(2) 0.037(2) -0.0142(17) -0.0018(17) -0.0072(17) C20 0.024(2) 0.054(3) 0.021(2) -0.0030(18) -0.0041(16) -0.0048(19) C21 0.030(2) 0.034(2) 0.036(2) 0.0078(18) -0.0093(17) 0.0034(18) C22 0.0242(19) 0.024(2) 0.032(2) 0.0038(16) -0.0070(15) -0.0048(16) C23 0.0193(17) 0.0167(18) 0.0176(17) 0.0006(13) 0.0010(14) -0.0005(13) C24 0.0227(18) 0.0171(18) 0.0174(17) -0.0039(14) 0.0012(14) -0.0007(14) C25 0.032(2) 0.0173(19) 0.035(2) 0.0040(16) -0.0060(17) 0.0060(15) C26 0.027(2) 0.0129(18) 0.045(2) -0.0101(17) 0.0046(17) 0.0010(15) C27 0.029(2) 0.022(2) 0.0219(18) -0.0090(15) 0.0050(15) 0.0008(15) C28 0.0238(19) 0.0216(19) 0.0170(17) -0.0010(14) 0.0001(14) -0.0002(14) C29 0.0234(18) 0.0198(19) 0.0096(15) 0.0017(13) -0.0009(13) -0.0032(14) C30 0.0249(19) 0.0204(19) 0.0233(19) 0.0015(15) 0.0003(15) 0.0006(15) C31 0.037(2) 0.0182(19) 0.030(2) 0.0083(16) -0.0012(17) -0.0042(16) C32 0.035(2) 0.039(2) 0.025(2) 0.0127(17) 0.0064(17) -0.0078(18) C33 0.030(2) 0.034(2) 0.027(2) 0.0005(17) 0.0103(16) -0.0025(17) C34 0.0281(19) 0.023(2) 0.0196(17) -0.0030(14) 0.0005(14) -0.0023(15) _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 N1 2.234(2) . ? Ru1 P3 2.2838(8) . ? Ru1 P1 2.3526(9) . ? Ru1 P2 2.3595(9) . ? Ru1 Cl1 2.5785(8) . ? Ru1 H100 1.56(3) . ? P1 O1 1.651(2) . ? P1 C1 1.851(3) . ? P1 C2 1.854(3) . ? P2 O2 1.634(2) . ? P2 C4 1.846(3) . ? P2 C3 1.859(3) . ? P3 C23 1.850(3) . ? P3 C29 1.867(3) . ? P3 C17 1.873(3) . ? O1 C5 1.444(4) . ? O2 C7 1.413(4) . ? N1 C6 1.483(4) . ? N1 C8 1.491(4) . ? N1 H1B 0.9300 . ? C1 C9 1.528(4) . ? C1 C10 1.536(5) . ? C1 H1A 1.0000 . ? C2 C12 1.521(5) . ? C2 C11 1.532(5) . ? C2 H2A 1.0000 . ? C3 C13 1.533(4) . ? C3 C14 1.537(5) . ? C3 H3A 1.0000 . ? C4 C15 1.522(5) . ? C4 C16 1.530(5) . ? C4 H4A 1.0000 . ? C5 C6 1.506(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.496(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.386(4) . ? C17 C22 1.389(4) . ? C18 C19 1.385(5) . ? C18 H18A 0.9500 . ? C19 C20 1.373(5) . ? C19 H19A 0.9500 . ? C20 C21 1.378(5) . ? C20 H20A 0.9500 . ? C21 C22 1.388(4) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.378(4) . ? C23 C28 1.400(4) . ? C24 C25 1.393(4) . ? C24 H24A 0.9500 . ? C25 C26 1.367(5) . ? C25 H25A 0.9500 . ? C26 C27 1.383(5) . ? C26 H26A 0.9500 . ? C27 C28 1.384(4) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C34 1.387(4) . ? C29 C30 1.396(4) . ? C30 C31 1.386(4) . ? C30 H30A 0.9500 . ? C31 C32 1.372(5) . ? C31 H31A 0.9500 . ? C32 C33 1.367(5) . ? C32 H32A 0.9500 . ? C33 C34 1.391(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? 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 N1 Ru1 P3 175.11(7) . . ? N1 Ru1 P1 80.07(7) . . ? P3 Ru1 P1 97.46(3) . . ? N1 Ru1 P2 86.32(7) . . ? P3 Ru1 P2 97.19(3) . . ? P1 Ru1 P2 159.08(3) . . ? N1 Ru1 Cl1 82.24(7) . . ? P3 Ru1 Cl1 93.73(3) . . ? P1 Ru1 Cl1 93.40(3) . . ? P2 Ru1 Cl1 100.46(3) . . ? N1 Ru1 H100 90.4(11) . . ? P3 Ru1 H100 93.4(11) . . ? P1 Ru1 H100 82.2(11) . . ? P2 Ru1 H100 82.1(11) . . ? Cl1 Ru1 H100 172.0(11) . . ? O1 P1 C1 94.40(13) . . ? O1 P1 C2 99.88(14) . . ? C1 P1 C2 102.35(16) . . ? O1 P1 Ru1 109.21(9) . . ? C1 P1 Ru1 123.09(11) . . ? C2 P1 Ru1 122.19(12) . . ? O2 P2 C4 90.90(15) . . ? O2 P2 C3 100.37(16) . . ? C4 P2 C3 101.52(15) . . ? O2 P2 Ru1 113.63(10) . . ? C4 P2 Ru1 120.18(12) . . ? C3 P2 Ru1 123.91(11) . . ? C23 P3 C29 99.51(14) . . ? C23 P3 C17 98.70(14) . . ? C29 P3 C17 100.17(14) . . ? C23 P3 Ru1 121.24(10) . . ? C29 P3 Ru1 116.05(10) . . ? C17 P3 Ru1 117.39(10) . . ? C5 O1 P1 120.2(2) . . ? C7 O2 P2 131.8(2) . . ? C6 N1 C8 111.9(2) . . ? C6 N1 Ru1 120.0(2) . . ? C8 N1 Ru1 116.14(19) . . ? C6 N1 H1B 101.7 . . ? C8 N1 H1B 101.7 . . ? Ru1 N1 H1B 101.7 . . ? C9 C1 C10 111.2(3) . . ? C9 C1 P1 111.8(2) . . ? C10 C1 P1 113.4(2) . . ? C9 C1 H1A 106.7 . . ? C10 C1 H1A 106.7 . . ? P1 C1 H1A 106.7 . . ? C12 C2 C11 108.5(3) . . ? C12 C2 P1 109.9(2) . . ? C11 C2 P1 116.6(3) . . ? C12 C2 H2A 107.2 . . ? C11 C2 H2A 107.2 . . ? P1 C2 H2A 107.2 . . ? C13 C3 C14 109.1(3) . . ? C13 C3 P2 115.7(2) . . ? C14 C3 P2 108.9(2) . . ? C13 C3 H3A 107.6 . . ? C14 C3 H3A 107.6 . . ? P2 C3 H3A 107.6 . . ? C15 C4 C16 111.6(3) . . ? C15 C4 P2 113.1(2) . . ? C16 C4 P2 115.1(2) . . ? C15 C4 H4A 105.3 . . ? C16 C4 H4A 105.3 . . ? P2 C4 H4A 105.3 . . ? O1 C5 C6 111.2(3) . . ? O1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N1 C6 C5 112.6(3) . . ? N1 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O2 C7 C8 116.2(3) . . ? O2 C7 H7A 108.2 . . ? C8 C7 H7A 108.2 . . ? O2 C7 H7B 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C7 114.4(3) . . ? N1 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 116.8(3) . . ? C18 C17 P3 122.6(2) . . ? C22 C17 P3 120.5(2) . . ? C19 C18 C17 121.6(3) . . ? C19 C18 H18A 119.2 . . ? C17 C18 H18A 119.2 . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C21 119.1(3) . . ? C19 C20 H20A 120.4 . . ? C21 C20 H20A 120.4 . . ? C20 C21 C22 119.9(3) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C17 121.9(3) . . ? C21 C22 H22A 119.1 . . ? C17 C22 H22A 119.1 . . ? C24 C23 C28 118.0(3) . . ? C24 C23 P3 121.3(2) . . ? C28 C23 P3 120.7(2) . . ? C23 C24 C25 121.0(3) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C27 C28 C23 121.3(3) . . ? C27 C28 H28A 119.4 . . ? C23 C28 H28A 119.4 . . ? C34 C29 C30 117.6(3) . . ? C34 C29 P3 123.1(2) . . ? C30 C29 P3 119.2(2) . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C32 C31 C30 120.8(3) . . ? C32 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? C33 C32 C31 119.3(3) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? C32 C33 C34 120.6(3) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C29 C34 C33 120.9(3) . . ? C29 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.619 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 933826' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs065_0ma_Compound_7 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C21 H42 Cl N O2 P2 Ru S' _chemical_formula_weight 571.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 11.0475(2) _cell_length_b 17.0485(4) _cell_length_c 13.8434(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2607.31(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5545 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.40 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8226 _exptl_absorpt_correction_T_max 0.8893 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17452 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_unetI/netI 0.0273 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3083 _reflns_number_gt 2625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0226P)^2^+1.3750P] 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 3083 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _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 Ru1 Ru 0.718368(18) 0.2500 1.018909(15) 0.01673(7) Uani 1 2 d S . . S1 S 0.50969(6) 0.2500 1.03912(5) 0.02881(17) Uani 1 2 d S . . Cl1 Cl 0.75217(6) 0.2500 1.20462(5) 0.02455(15) Uani 1 2 d S . . P1 P 0.70633(4) 0.11579(3) 0.99824(3) 0.02121(12) Uani 1 1 d . . . O1 O 0.60043(12) 0.07000(8) 1.05990(10) 0.0285(3) Uani 1 1 d . . . N1 N 0.91130(19) 0.2500 0.99363(15) 0.0180(4) Uani 1 2 d S . . C3 C 0.5480(2) 0.10898(13) 1.14133(15) 0.0351(5) Uani 1 1 d . . . H3A H 0.6126 0.1358 1.1782 0.042 Uiso 1 1 calc R . . H3B H 0.5102 0.0696 1.1843 0.042 Uiso 1 1 calc R . . C4 C 0.4544(2) 0.16795(14) 1.1116(2) 0.0469(7) Uani 1 1 d . . . H4A H 0.4161 0.1893 1.1707 0.056 Uiso 1 1 calc R . . H4B H 0.3907 0.1404 1.0745 0.056 Uiso 1 1 calc R . . C2 C 0.83879(18) 0.05275(12) 1.02461(15) 0.0287(4) Uani 1 1 d . . . H2A H 0.9076 0.0717 0.9839 0.034 Uiso 1 1 calc R . . C8 C 0.8754(2) 0.06261(13) 1.13030(16) 0.0366(5) Uani 1 1 d . . . H8A H 0.9455 0.0292 1.1442 0.055 Uiso 1 1 calc R . . H8B H 0.8077 0.0474 1.1720 0.055 Uiso 1 1 calc R . . H8C H 0.8964 0.1176 1.1425 0.055 Uiso 1 1 calc R . . C7 C 0.8197(2) -0.03404(13) 1.00194(18) 0.0401(6) Uani 1 1 d . . . H7A H 0.8934 -0.0634 1.0177 0.060 Uiso 1 1 calc R . . H7B H 0.8013 -0.0403 0.9331 0.060 Uiso 1 1 calc R . . H7C H 0.7520 -0.0542 1.0405 0.060 Uiso 1 1 calc R . . C1 C 0.66077(18) 0.08086(13) 0.87755(14) 0.0285(5) Uani 1 1 d . . . H1A H 0.6537 0.0224 0.8810 0.034 Uiso 1 1 calc R . . C5 C 0.53687(19) 0.11306(14) 0.84723(16) 0.0359(5) Uani 1 1 d . . . H5A H 0.5161 0.0931 0.7829 0.054 Uiso 1 1 calc R . . H5B H 0.5399 0.1705 0.8456 0.054 Uiso 1 1 calc R . . H5C H 0.4754 0.0961 0.8938 0.054 Uiso 1 1 calc R . . C6 C 0.7568(2) 0.10009(15) 0.80160(16) 0.0392(6) Uani 1 1 d . . . H6A H 0.7301 0.0809 0.7384 0.059 Uiso 1 1 calc R . . H6B H 0.8333 0.0747 0.8191 0.059 Uiso 1 1 calc R . . H6C H 0.7686 0.1570 0.7986 0.059 Uiso 1 1 calc R . . C9 C 0.9930(2) 0.2500 1.06658(19) 0.0216(6) Uani 1 2 d S . . H9A H 0.9635 0.2500 1.1310 0.026 Uiso 1 2 calc SR . . C10 C 1.1168(2) 0.2500 1.0525(2) 0.0282(6) Uani 1 2 d S . . H10A H 1.1702 0.2500 1.1063 0.034 Uiso 1 2 calc SR . . C11 C 1.1621(2) 0.2500 0.9599(2) 0.0293(7) Uani 1 2 d S . . H11A H 1.2469 0.2500 0.9484 0.035 Uiso 1 2 calc SR . . C12 C 1.0807(2) 0.2500 0.8846(2) 0.0258(6) Uani 1 2 d S . . H12A H 1.1088 0.2500 0.8197 0.031 Uiso 1 2 calc SR . . C13 C 0.9583(2) 0.2500 0.90378(19) 0.0226(6) Uani 1 2 d S . . H13A H 0.9039 0.2500 0.8506 0.027 Uiso 1 2 calc SR . . H100 H 0.698(3) 0.2500 0.913(2) 0.031(8) Uiso 1 2 d S . . 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 0.01401(11) 0.02173(12) 0.01446(11) 0.000 0.00003(8) 0.000 S1 0.0161(3) 0.0461(5) 0.0243(4) 0.000 0.0023(3) 0.000 Cl1 0.0240(3) 0.0333(4) 0.0164(3) 0.000 -0.0007(2) 0.000 P1 0.0175(2) 0.0229(3) 0.0232(3) -0.00009(19) 0.00080(19) -0.00201(19) O1 0.0246(7) 0.0256(8) 0.0354(8) 0.0014(6) 0.0084(6) -0.0044(6) N1 0.0188(11) 0.0165(11) 0.0185(11) 0.000 -0.0013(8) 0.000 C3 0.0408(13) 0.0381(13) 0.0264(11) -0.0001(9) 0.0106(9) -0.0161(10) C4 0.0368(13) 0.0317(13) 0.0724(18) -0.0083(12) 0.0311(13) -0.0072(10) C2 0.0205(9) 0.0258(11) 0.0398(12) 0.0006(9) 0.0013(9) 0.0009(8) C8 0.0372(12) 0.0294(12) 0.0432(14) 0.0086(10) -0.0077(10) 0.0028(10) C7 0.0321(12) 0.0282(12) 0.0599(16) -0.0049(11) 0.0005(11) 0.0047(9) C1 0.0269(10) 0.0301(11) 0.0285(11) -0.0064(9) -0.0013(9) -0.0070(9) C5 0.0317(11) 0.0448(14) 0.0312(12) -0.0037(10) -0.0079(9) -0.0070(10) C6 0.0400(13) 0.0494(14) 0.0283(12) -0.0137(10) 0.0050(10) -0.0093(11) C9 0.0216(13) 0.0239(14) 0.0194(13) 0.000 -0.0023(11) 0.000 C10 0.0196(13) 0.0367(17) 0.0285(15) 0.000 -0.0056(12) 0.000 C11 0.0163(13) 0.0331(17) 0.0387(18) 0.000 0.0017(12) 0.000 C12 0.0228(14) 0.0316(16) 0.0230(14) 0.000 0.0054(11) 0.000 C13 0.0215(13) 0.0267(15) 0.0197(13) 0.000 -0.0025(11) 0.000 _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 N1 2.160(2) . ? Ru1 P1 2.3098(5) . ? Ru1 P1 2.3099(5) 7_565 ? Ru1 S1 2.3222(7) . ? Ru1 Cl1 2.5979(7) . ? Ru1 H100 1.49(3) . ? S1 C4 1.827(2) . ? S1 C4 1.827(2) 7_565 ? P1 O1 1.6452(14) . ? P1 C1 1.844(2) . ? P1 C2 1.852(2) . ? O1 C3 1.431(2) . ? N1 C13 1.348(3) . ? N1 C9 1.354(3) . ? C3 C4 1.500(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C2 C8 1.527(3) . ? C2 C7 1.527(3) . ? C2 H2A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C1 C6 1.529(3) . ? C1 C5 1.533(3) . ? C1 H1A 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C9 C10 1.381(4) . ? C9 H9A 0.9500 . ? C10 C11 1.376(4) . ? C10 H10A 0.9500 . ? C11 C12 1.377(4) . ? C11 H11A 0.9500 . ? C12 C13 1.379(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? 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 N1 Ru1 P1 92.105(14) . . ? N1 Ru1 P1 92.104(14) . 7_565 ? P1 Ru1 P1 164.30(3) . 7_565 ? N1 Ru1 S1 177.59(6) . . ? P1 Ru1 S1 87.580(13) . . ? P1 Ru1 S1 87.582(13) 7_565 . ? N1 Ru1 Cl1 91.06(6) . . ? P1 Ru1 Cl1 97.518(13) . . ? P1 Ru1 Cl1 97.517(13) 7_565 . ? S1 Ru1 Cl1 91.35(2) . . ? N1 Ru1 H100 89.5(11) . . ? P1 Ru1 H100 82.46(5) . . ? P1 Ru1 H100 82.46(5) 7_565 . ? S1 Ru1 H100 88.1(11) . . ? Cl1 Ru1 H100 179.5(11) . . ? C4 S1 C4 99.92(15) . 7_565 ? C4 S1 Ru1 113.47(8) . . ? C4 S1 Ru1 113.47(8) 7_565 . ? O1 P1 C1 97.05(8) . . ? O1 P1 C2 100.62(9) . . ? C1 P1 C2 101.94(10) . . ? O1 P1 Ru1 116.53(5) . . ? C1 P1 Ru1 116.61(7) . . ? C2 P1 Ru1 120.33(7) . . ? C3 O1 P1 118.44(13) . . ? C13 N1 C9 115.6(2) . . ? C13 N1 Ru1 121.97(17) . . ? C9 N1 Ru1 122.46(17) . . ? O1 C3 C4 112.00(18) . . ? O1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 S1 115.67(15) . . ? C3 C4 H4A 108.4 . . ? S1 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? S1 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C8 C2 C7 109.89(18) . . ? C8 C2 P1 109.51(14) . . ? C7 C2 P1 114.36(15) . . ? C8 C2 H2A 107.6 . . ? C7 C2 H2A 107.6 . . ? P1 C2 H2A 107.6 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C1 C5 110.76(18) . . ? C6 C1 P1 111.37(14) . . ? C5 C1 P1 112.09(14) . . ? C6 C1 H1A 107.5 . . ? C5 C1 H1A 107.5 . . ? P1 C1 H1A 107.5 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C9 C10 123.7(3) . . ? N1 C9 H9A 118.2 . . ? C10 C9 H9A 118.2 . . ? C11 C10 C9 119.5(3) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C10 C11 C12 117.9(3) . . ? C10 C11 H11A 121.1 . . ? C12 C11 H11A 121.1 . . ? C11 C12 C13 119.6(3) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? N1 C13 C12 123.8(3) . . ? N1 C13 H13A 118.1 . . ? C12 C13 H13A 118.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.373 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.066 _database_code_depnum_ccdc_archive 'CCDC 933827' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs055_0m_Compound_8 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C40 H57 B N O2 P2 Ru' _chemical_formula_weight 757.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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 13.6707(6) _cell_length_b 13.3994(5) _cell_length_c 21.0170(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.0960(10) _cell_angle_gamma 90.00 _cell_volume 3844.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8932 _exptl_absorpt_correction_T_max 0.9068 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33195 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_unetI/netI 0.0347 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8808 _reflns_number_gt 7230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0284P)^2^+2.1953P] 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 8808 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _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 Ru1 Ru 0.048739(10) 0.135166(11) 0.219166(7) 0.01537(5) Uani 1 1 d . . . P1 P -0.07282(3) 0.25241(4) 0.22881(2) 0.01853(11) Uani 1 1 d . . . P2 P 0.08616(4) 0.13712(4) 0.32557(2) 0.01866(10) Uani 1 1 d . . . O1 O -0.05197(9) 0.35763(10) 0.26505(7) 0.0228(3) Uani 1 1 d . . . O2 O 0.02913(10) 0.22660(10) 0.35895(6) 0.0225(3) Uani 1 1 d . . . N1 N 0.08632(13) 0.43466(13) 0.37676(9) 0.0281(4) Uani 1 1 d . . . C1 C -0.17754(14) 0.21382(16) 0.27583(10) 0.0244(4) Uani 1 1 d . . . H1 H -0.1470 0.1827 0.3153 0.029 Uiso 1 1 calc R . . C9 C -0.23849(16) 0.13044(17) 0.24341(11) 0.0321(5) Uani 1 1 d . . . H9A H -0.2874 0.1068 0.2723 0.048 Uiso 1 1 calc R . . H9B H -0.1954 0.0751 0.2329 0.048 Uiso 1 1 calc R . . H9C H -0.2717 0.1561 0.2043 0.048 Uiso 1 1 calc R . . C10 C -0.24388(16) 0.29712(19) 0.29971(12) 0.0367(6) Uani 1 1 d . . . H10A H -0.2856 0.3228 0.2640 0.055 Uiso 1 1 calc R . . H10B H -0.2032 0.3514 0.3179 0.055 Uiso 1 1 calc R . . H10C H -0.2850 0.2703 0.3324 0.055 Uiso 1 1 calc R . . C5 C 0.03267(15) 0.42024(15) 0.26154(10) 0.0261(4) Uani 1 1 d . . . H5A H 0.0260 0.4628 0.2231 0.031 Uiso 1 1 calc R . . H5B H 0.0920 0.3786 0.2586 0.031 Uiso 1 1 calc R . . C6 C 0.04224(15) 0.48481(16) 0.32048(10) 0.0266(4) Uani 1 1 d . . . H6A H 0.0824 0.5439 0.3111 0.032 Uiso 1 1 calc R . . H6B H -0.0237 0.5089 0.3304 0.032 Uiso 1 1 calc R . . C8 C 0.01993(16) 0.37940(16) 0.41629(10) 0.0292(5) Uani 1 1 d . . . H8A H -0.0479 0.3861 0.3978 0.035 Uiso 1 1 calc R . . H8B H 0.0222 0.4091 0.4595 0.035 Uiso 1 1 calc R . . C7 C 0.04570(16) 0.26972(16) 0.42161(9) 0.0263(4) Uani 1 1 d . . . H7A H 0.1151 0.2615 0.4366 0.032 Uiso 1 1 calc R . . H7B H 0.0040 0.2364 0.4523 0.032 Uiso 1 1 calc R . . C4 C 0.21619(14) 0.15579(16) 0.35188(10) 0.0249(4) Uani 1 1 d . . . H4 H 0.2199 0.1550 0.3995 0.030 Uiso 1 1 calc R . . C15 C 0.25465(15) 0.25733(17) 0.33126(10) 0.0287(5) Uani 1 1 d . . . H15A H 0.3227 0.2654 0.3476 0.043 Uiso 1 1 calc R . . H15B H 0.2144 0.3104 0.3484 0.043 Uiso 1 1 calc R . . H15C H 0.2515 0.2612 0.2846 0.043 Uiso 1 1 calc R . . C16 C 0.28116(16) 0.07042(18) 0.33001(11) 0.0334(5) Uani 1 1 d . . . H16A H 0.2843 0.0726 0.2836 0.050 Uiso 1 1 calc R . . H16B H 0.2534 0.0064 0.3426 0.050 Uiso 1 1 calc R . . H16C H 0.3473 0.0777 0.3499 0.050 Uiso 1 1 calc R . . C3 C 0.05346(16) 0.02297(16) 0.37024(10) 0.0269(4) Uani 1 1 d . . . H3 H 0.0768 -0.0352 0.3454 0.032 Uiso 1 1 calc R . . C13 C 0.09995(18) 0.01246(19) 0.43785(10) 0.0367(5) Uani 1 1 d . . . H13A H 0.0793 0.0684 0.4640 0.055 Uiso 1 1 calc R . . H13B H 0.1715 0.0128 0.4363 0.055 Uiso 1 1 calc R . . H13C H 0.0788 -0.0505 0.4565 0.055 Uiso 1 1 calc R . . C14 C -0.05808(17) 0.01263(18) 0.37153(11) 0.0336(5) Uani 1 1 d . . . H14A H -0.0742 -0.0514 0.3909 0.050 Uiso 1 1 calc R . . H14B H -0.0871 0.0154 0.3279 0.050 Uiso 1 1 calc R . . H14C H -0.0842 0.0673 0.3966 0.050 Uiso 1 1 calc R . . C2 C -0.12221(15) 0.29167(16) 0.14901(10) 0.0248(4) Uani 1 1 d . . . H2 H -0.1413 0.2296 0.1251 0.030 Uiso 1 1 calc R . . C11 C -0.21315(17) 0.35868(18) 0.14819(12) 0.0374(6) Uani 1 1 d . . . H11A H -0.1997 0.4170 0.1754 0.056 Uiso 1 1 calc R . . H11B H -0.2683 0.3211 0.1641 0.056 Uiso 1 1 calc R . . H11C H -0.2297 0.3808 0.1045 0.056 Uiso 1 1 calc R . . C12 C -0.04234(17) 0.34284(17) 0.11228(10) 0.0312(5) Uani 1 1 d . . . H12A H -0.0609 0.3419 0.0666 0.047 Uiso 1 1 calc R . . H12B H 0.0198 0.3073 0.1200 0.047 Uiso 1 1 calc R . . H12C H -0.0348 0.4121 0.1267 0.047 Uiso 1 1 calc R . . C22 C 0.16197(14) 0.03799(14) 0.17278(9) 0.0183(4) Uani 1 1 d . . . H22 H 0.2326 0.0471 0.1866 0.022 Uiso 1 1 calc R . . C21 C 0.10393(15) -0.02180(14) 0.21044(9) 0.0217(4) Uani 1 1 d . . . H21 H 0.1344 -0.0563 0.2488 0.026 Uiso 1 1 calc R . . C20 C 0.00113(15) -0.02686(15) 0.19782(10) 0.0237(4) Uani 1 1 d . . . H20 H -0.0413 -0.0636 0.2272 0.028 Uiso 1 1 calc R . . C19 C -0.04006(14) 0.03460(15) 0.15013(9) 0.0235(4) Uani 1 1 d . . . H19 H -0.1129 0.0424 0.1458 0.028 Uiso 1 1 calc R . . C18 C 0.01976(14) 0.09440(15) 0.11196(9) 0.0195(4) Uani 1 1 d . . . H18 H -0.0128 0.1451 0.0830 0.023 Uiso 1 1 calc R . . C17 C 0.12306(13) 0.09515(14) 0.11987(9) 0.0170(4) Uani 1 1 d . . . C35 C 0.14378(14) 0.22303(16) 0.01963(10) 0.0242(4) Uani 1 1 d . . . C36 C 0.16903(17) 0.32369(18) 0.02425(12) 0.0375(6) Uani 1 1 d . . . H36 H 0.2182 0.3435 0.0554 0.045 Uiso 1 1 calc R . . C37 C 0.1246(2) 0.3965(2) -0.01530(16) 0.0597(9) Uani 1 1 d . . . H37 H 0.1435 0.4645 -0.0108 0.072 Uiso 1 1 calc R . . C38 C 0.0532(2) 0.3690(2) -0.06092(16) 0.0655(10) Uani 1 1 d . . . H38 H 0.0225 0.4181 -0.0879 0.079 Uiso 1 1 calc R . . C39 C 0.02672(19) 0.2708(2) -0.06715(13) 0.0506(7) Uani 1 1 d . . . H39 H -0.0223 0.2518 -0.0986 0.061 Uiso 1 1 calc R . . C40 C 0.07125(16) 0.19865(18) -0.02762(10) 0.0323(5) Uani 1 1 d . . . H40 H 0.0519 0.1309 -0.0328 0.039 Uiso 1 1 calc R . . C29 C 0.21484(13) 0.03716(15) 0.02072(9) 0.0193(4) Uani 1 1 d . . . C34 C 0.26148(15) 0.04784(17) -0.03716(9) 0.0262(5) Uani 1 1 d . . . H34 H 0.2742 0.1132 -0.0521 0.031 Uiso 1 1 calc R . . C33 C 0.28953(15) -0.03292(18) -0.07310(10) 0.0309(5) Uani 1 1 d . . . H33 H 0.3233 -0.0223 -0.1109 0.037 Uiso 1 1 calc R . . C32 C 0.26837(15) -0.12933(18) -0.05399(10) 0.0301(5) Uani 1 1 d . . . H32 H 0.2891 -0.1850 -0.0777 0.036 Uiso 1 1 calc R . . C31 C 0.21678(15) -0.14317(16) -0.00005(10) 0.0271(5) Uani 1 1 d . . . H31 H 0.1985 -0.2085 0.0122 0.033 Uiso 1 1 calc R . . C30 C 0.19148(14) -0.06124(15) 0.03646(9) 0.0217(4) Uani 1 1 d . . . H30 H 0.1568 -0.0727 0.0737 0.026 Uiso 1 1 calc R . . C23 C 0.30105(14) 0.17782(14) 0.09741(9) 0.0191(4) Uani 1 1 d . . . C28 C 0.38862(14) 0.17459(16) 0.06556(10) 0.0252(4) Uani 1 1 d . . . H28 H 0.3873 0.1467 0.0240 0.030 Uiso 1 1 calc R . . C27 C 0.47747(15) 0.21048(17) 0.09217(10) 0.0290(5) Uani 1 1 d . . . H27 H 0.5345 0.2077 0.0683 0.035 Uiso 1 1 calc R . . C26 C 0.48304(15) 0.24998(15) 0.15283(10) 0.0264(5) Uani 1 1 d . . . H26 H 0.5437 0.2732 0.1715 0.032 Uiso 1 1 calc R . . C25 C 0.39866(15) 0.25501(15) 0.18579(11) 0.0271(5) Uani 1 1 d . . . H25 H 0.4012 0.2814 0.2278 0.033 Uiso 1 1 calc R . . C24 C 0.30971(14) 0.22172(15) 0.15793(10) 0.0241(4) Uani 1 1 d . . . H24 H 0.2523 0.2292 0.1811 0.029 Uiso 1 1 calc R . . B1 B 0.19561(15) 0.13654(17) 0.06519(10) 0.0179(4) Uani 1 1 d . . . H100 H 0.1086(16) 0.2330(17) 0.2253(10) 0.035(6) Uiso 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 Ru1 0.01397(7) 0.01390(8) 0.01828(8) -0.00176(6) 0.00133(5) -0.00055(6) P1 0.0149(2) 0.0162(2) 0.0244(3) -0.0043(2) 0.00012(19) -0.00037(19) P2 0.0179(2) 0.0187(2) 0.0195(2) -0.0021(2) 0.00191(18) 0.0011(2) O1 0.0183(7) 0.0179(7) 0.0323(8) -0.0079(6) 0.0014(6) -0.0011(6) O2 0.0222(7) 0.0233(7) 0.0221(7) -0.0072(6) 0.0013(6) 0.0022(6) N1 0.0244(9) 0.0257(10) 0.0341(10) -0.0055(8) 0.0009(8) -0.0020(7) C1 0.0185(10) 0.0261(11) 0.0289(11) -0.0042(9) 0.0044(8) -0.0016(8) C9 0.0245(11) 0.0313(12) 0.0412(13) -0.0086(11) 0.0072(9) -0.0065(10) C10 0.0245(11) 0.0407(14) 0.0458(14) -0.0161(11) 0.0109(10) 0.0004(10) C5 0.0257(10) 0.0202(10) 0.0327(11) -0.0052(9) 0.0029(9) -0.0065(8) C6 0.0248(10) 0.0184(10) 0.0369(12) -0.0071(9) 0.0035(9) -0.0033(8) C8 0.0296(11) 0.0296(12) 0.0287(11) -0.0112(9) 0.0048(9) 0.0008(9) C7 0.0284(11) 0.0297(12) 0.0211(10) -0.0075(9) 0.0039(8) 0.0003(9) C4 0.0211(10) 0.0325(12) 0.0206(10) -0.0051(8) -0.0024(8) 0.0026(8) C15 0.0184(10) 0.0390(13) 0.0281(11) -0.0066(10) -0.0022(8) -0.0035(9) C16 0.0250(11) 0.0431(14) 0.0316(12) -0.0052(10) -0.0038(9) 0.0101(10) C3 0.0347(12) 0.0228(11) 0.0237(10) 0.0016(9) 0.0065(9) 0.0008(9) C13 0.0468(14) 0.0363(13) 0.0276(12) 0.0089(10) 0.0059(10) 0.0051(11) C14 0.0375(13) 0.0299(12) 0.0345(12) 0.0050(10) 0.0104(10) -0.0066(10) C2 0.0229(10) 0.0224(10) 0.0285(11) -0.0031(9) -0.0042(8) 0.0052(8) C11 0.0325(12) 0.0338(13) 0.0449(14) -0.0027(11) -0.0065(10) 0.0137(10) C12 0.0361(12) 0.0280(12) 0.0290(11) 0.0033(9) -0.0020(9) 0.0030(9) C22 0.0194(9) 0.0161(9) 0.0194(9) -0.0030(7) 0.0021(7) 0.0021(7) C21 0.0284(10) 0.0145(9) 0.0227(10) -0.0025(8) 0.0050(8) 0.0043(8) C20 0.0293(11) 0.0154(10) 0.0270(10) -0.0059(8) 0.0088(8) -0.0075(8) C19 0.0184(10) 0.0238(11) 0.0286(11) -0.0106(9) 0.0044(8) -0.0041(8) C18 0.0180(9) 0.0192(9) 0.0214(10) -0.0048(8) 0.0010(7) 0.0009(8) C17 0.0183(9) 0.0147(9) 0.0180(9) -0.0038(7) 0.0020(7) 0.0007(7) C35 0.0205(10) 0.0255(11) 0.0268(10) 0.0079(9) 0.0023(8) 0.0005(8) C36 0.0285(12) 0.0284(12) 0.0543(15) 0.0145(11) -0.0079(11) -0.0025(10) C37 0.0478(17) 0.0319(14) 0.097(2) 0.0330(16) -0.0150(16) -0.0052(12) C38 0.0476(17) 0.0583(19) 0.088(2) 0.0503(18) -0.0213(16) -0.0039(15) C39 0.0361(14) 0.0604(19) 0.0531(16) 0.0278(14) -0.0175(12) -0.0025(13) C40 0.0278(11) 0.0361(13) 0.0325(12) 0.0094(10) -0.0033(9) 0.0005(10) C29 0.0144(9) 0.0239(10) 0.0194(9) -0.0007(8) -0.0013(7) 0.0015(8) C34 0.0234(10) 0.0330(12) 0.0221(10) -0.0023(9) 0.0006(8) -0.0072(9) C33 0.0203(10) 0.0483(15) 0.0244(11) -0.0120(10) 0.0046(8) -0.0074(10) C32 0.0190(10) 0.0381(13) 0.0329(12) -0.0178(10) -0.0022(8) 0.0026(9) C31 0.0256(10) 0.0255(11) 0.0295(11) -0.0042(9) -0.0063(8) 0.0013(9) C30 0.0205(10) 0.0250(11) 0.0196(9) -0.0011(8) 0.0001(8) 0.0017(8) C23 0.0175(9) 0.0148(9) 0.0248(10) 0.0038(8) 0.0001(7) 0.0019(7) C28 0.0199(10) 0.0321(11) 0.0237(10) 0.0029(9) 0.0025(8) -0.0012(9) C27 0.0190(10) 0.0375(13) 0.0309(11) 0.0047(10) 0.0045(8) -0.0016(9) C26 0.0199(10) 0.0224(11) 0.0365(12) 0.0012(9) -0.0019(9) -0.0035(8) C25 0.0256(11) 0.0206(10) 0.0351(12) -0.0096(9) 0.0017(9) -0.0031(8) C24 0.0187(10) 0.0211(10) 0.0329(11) -0.0055(9) 0.0048(8) -0.0011(8) B1 0.0156(10) 0.0186(10) 0.0196(10) 0.0023(9) 0.0015(8) 0.0001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C21 2.2453(19) . ? Ru1 P2 2.2670(5) . ? Ru1 C22 2.2815(18) . ? Ru1 C19 2.2813(19) . ? Ru1 P1 2.3037(5) . ? Ru1 C20 2.3037(19) . ? Ru1 C18 2.3314(18) . ? Ru1 C17 2.4299(18) . ? Ru1 H100 1.55(2) . ? P1 O1 1.6205(14) . ? P1 C2 1.850(2) . ? P1 C1 1.856(2) . ? P2 O2 1.6114(14) . ? P2 C4 1.850(2) . ? P2 C3 1.862(2) . ? O1 C5 1.434(2) . ? O2 C7 1.445(2) . ? N1 C6 1.462(3) . ? N1 C8 1.464(3) . ? C1 C9 1.531(3) . ? C1 C10 1.539(3) . ? C1 H1 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C5 C6 1.511(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C7 1.514(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C4 C15 1.530(3) . ? C4 C16 1.534(3) . ? C4 H4 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C3 C14 1.533(3) . ? C3 C13 1.531(3) . ? C3 H3 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C2 C12 1.533(3) . ? C2 C11 1.533(3) . ? C2 H2 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C22 C21 1.402(3) . ? C22 C17 1.429(3) . ? C22 H22 1.0000 . ? C21 C20 1.418(3) . ? C21 H21 1.0000 . ? C20 C19 1.392(3) . ? C20 H20 1.0000 . ? C19 C18 1.423(3) . ? C19 H19 1.0000 . ? C18 C17 1.413(3) . ? C18 H18 1.0000 . ? C17 B1 1.654(3) . ? C35 C36 1.394(3) . ? C35 C40 1.403(3) . ? C35 B1 1.640(3) . ? C36 C37 1.399(3) . ? C36 H36 0.9500 . ? C37 C38 1.381(4) . ? C37 H37 0.9500 . ? C38 C39 1.369(4) . ? C38 H38 0.9500 . ? C39 C40 1.393(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C29 C30 1.400(3) . ? C29 C34 1.411(3) . ? C29 B1 1.656(3) . ? C34 C33 1.386(3) . ? C34 H34 0.9500 . ? C33 C32 1.388(3) . ? C33 H33 0.9500 . ? C32 C31 1.380(3) . ? C32 H32 0.9500 . ? C31 C30 1.394(3) . ? C31 H31 0.9500 . ? C30 H30 0.9500 . ? C23 C24 1.401(3) . ? C23 C28 1.403(3) . ? C23 B1 1.654(3) . ? C28 C27 1.395(3) . ? C28 H28 0.9500 . ? C27 C26 1.379(3) . ? C27 H27 0.9500 . ? C26 C25 1.379(3) . ? C26 H26 0.9500 . ? C25 C24 1.394(3) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? 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 C21 Ru1 P2 91.86(5) . . ? C21 Ru1 C22 36.07(7) . . ? P2 Ru1 C22 107.81(5) . . ? C21 Ru1 C19 64.17(7) . . ? P2 Ru1 C19 135.91(5) . . ? C22 Ru1 C19 74.99(7) . . ? C21 Ru1 P1 153.27(5) . . ? P2 Ru1 P1 91.766(18) . . ? C22 Ru1 P1 159.41(5) . . ? C19 Ru1 P1 95.57(5) . . ? C21 Ru1 C20 36.29(7) . . ? P2 Ru1 C20 104.44(5) . . ? C22 Ru1 C20 64.53(7) . . ? C19 Ru1 C20 35.36(7) . . ? P1 Ru1 C20 117.53(5) . . ? C21 Ru1 C18 75.04(7) . . ? P2 Ru1 C18 166.78(5) . . ? C22 Ru1 C18 62.42(7) . . ? C19 Ru1 C18 35.92(7) . . ? P1 Ru1 C18 99.15(5) . . ? C20 Ru1 C18 63.86(7) . . ? C21 Ru1 C17 64.23(7) . . ? P2 Ru1 C17 140.10(4) . . ? C22 Ru1 C17 35.14(6) . . ? C19 Ru1 C17 63.65(7) . . ? P1 Ru1 C17 124.27(5) . . ? C20 Ru1 C17 75.62(7) . . ? C18 Ru1 C17 34.45(6) . . ? C21 Ru1 H100 128.5(8) . . ? P2 Ru1 H100 79.5(8) . . ? C22 Ru1 H100 98.7(8) . . ? C19 Ru1 H100 144.5(8) . . ? P1 Ru1 H100 78.2(8) . . ? C20 Ru1 H100 163.2(8) . . ? C18 Ru1 H100 109.9(8) . . ? C17 Ru1 H100 90.9(8) . . ? O1 P1 C2 103.00(9) . . ? O1 P1 C1 96.50(8) . . ? C2 P1 C1 107.91(9) . . ? O1 P1 Ru1 121.68(5) . . ? C2 P1 Ru1 110.11(7) . . ? C1 P1 Ru1 115.95(7) . . ? O2 P2 C4 104.42(8) . . ? O2 P2 C3 104.87(9) . . ? C4 P2 C3 102.32(10) . . ? O2 P2 Ru1 110.45(5) . . ? C4 P2 Ru1 117.29(7) . . ? C3 P2 Ru1 116.13(7) . . ? C5 O1 P1 127.35(12) . . ? C7 O2 P2 129.70(13) . . ? C6 N1 C8 116.78(17) . . ? C9 C1 C10 110.98(17) . . ? C9 C1 P1 112.52(14) . . ? C10 C1 P1 117.16(16) . . ? C9 C1 H1 105.0 . . ? C10 C1 H1 105.0 . . ? P1 C1 H1 105.0 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C5 C6 109.10(17) . . ? O1 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? O1 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N1 C6 C5 114.44(18) . . ? N1 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? N1 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? N1 C8 C7 112.58(17) . . ? N1 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? O2 C7 C8 107.24(17) . . ? O2 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O2 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C15 C4 C16 111.41(18) . . ? C15 C4 P2 112.03(14) . . ? C16 C4 P2 111.85(14) . . ? C15 C4 H4 107.1 . . ? C16 C4 H4 107.1 . . ? P2 C4 H4 107.1 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C3 C13 109.80(18) . . ? C14 C3 P2 110.45(15) . . ? C13 C3 P2 116.39(16) . . ? C14 C3 H3 106.5 . . ? C13 C3 H3 106.5 . . ? P2 C3 H3 106.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C2 C11 109.37(18) . . ? C12 C2 P1 110.41(14) . . ? C11 C2 P1 115.65(15) . . ? C12 C2 H2 107.0 . . ? C11 C2 H2 107.0 . . ? P1 C2 H2 107.0 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 C22 C17 123.18(17) . . ? C21 C22 Ru1 70.56(11) . . ? C17 C22 Ru1 78.11(11) . . ? C21 C22 H22 118.2 . . ? C17 C22 H22 118.2 . . ? Ru1 C22 H22 118.2 . . ? C22 C21 C20 120.48(18) . . ? C22 C21 Ru1 73.37(11) . . ? C20 C21 Ru1 74.10(11) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? Ru1 C21 H21 119.6 . . ? C19 C20 C21 117.68(18) . . ? C19 C20 Ru1 71.44(11) . . ? C21 C20 Ru1 69.61(11) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? Ru1 C20 H20 120.7 . . ? C20 C19 C18 121.09(18) . . ? C20 C19 Ru1 73.20(11) . . ? C18 C19 Ru1 73.96(11) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? Ru1 C19 H19 119.3 . . ? C17 C18 C19 122.61(18) . . ? C17 C18 Ru1 76.59(11) . . ? C19 C18 Ru1 70.12(11) . . ? C17 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? Ru1 C18 H18 118.4 . . ? C18 C17 C22 114.54(17) . . ? C18 C17 B1 123.63(16) . . ? C22 C17 B1 120.56(16) . . ? C18 C17 Ru1 68.96(10) . . ? C22 C17 Ru1 66.75(10) . . ? B1 C17 Ru1 144.80(13) . . ? C36 C35 C40 115.9(2) . . ? C36 C35 B1 123.05(18) . . ? C40 C35 B1 121.01(19) . . ? C35 C36 C37 122.4(2) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C38 C37 C36 119.7(3) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C37 119.7(2) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 120.4(2) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 122.0(2) . . ? C39 C40 H40 119.0 . . ? C35 C40 H40 119.0 . . ? C30 C29 C34 114.74(18) . . ? C30 C29 B1 125.36(17) . . ? C34 C29 B1 119.86(17) . . ? C33 C34 C29 122.8(2) . . ? C33 C34 H34 118.6 . . ? C29 C34 H34 118.6 . . ? C34 C33 C32 120.1(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C31 C32 C33 119.1(2) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C30 C29 123.03(19) . . ? C31 C30 H30 118.5 . . ? C29 C30 H30 118.5 . . ? C24 C23 C28 114.43(17) . . ? C24 C23 B1 122.76(17) . . ? C28 C23 B1 122.78(17) . . ? C27 C28 C23 123.0(2) . . ? C27 C28 H28 118.5 . . ? C23 C28 H28 118.5 . . ? C26 C27 C28 120.4(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C25 C26 C27 118.51(19) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C24 C23 123.01(19) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C35 B1 C17 112.73(15) . . ? C35 B1 C23 110.01(16) . . ? C17 B1 C23 111.70(15) . . ? C35 B1 C29 108.39(16) . . ? C17 B1 C29 104.00(15) . . ? C23 B1 C29 109.79(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.772 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 933828' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs074_0m_Compound_9 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C43 H60 B O2 P2 Ru S' _chemical_formula_weight 814.79 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' B B 0.0013 0.0007 '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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1172(16) _cell_length_b 13.3573(17) _cell_length_c 13.6408(15) _cell_angle_alpha 86.498(6) _cell_angle_beta 86.588(6) _cell_angle_gamma 71.613(6) _cell_volume 2261.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9667 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.14 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6665 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31611 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7948 _reflns_number_gt 6684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0382P)^2^+0.2441P] 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 7948 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.002 _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 Ru1 Ru 0.785410(17) 0.775421(16) 0.647423(14) 0.01733(8) Uani 1 1 d . . . S1 S 1.06666(7) 0.88300(6) 0.89732(6) 0.0364(2) Uani 1 1 d . . . P1 P 0.73679(6) 0.93030(5) 0.72814(5) 0.01921(16) Uani 1 1 d . . . P2 P 0.88162(6) 0.68396(5) 0.77486(5) 0.02042(16) Uani 1 1 d . . . B1 B 0.8227(3) 0.8179(2) 0.3733(2) 0.0230(7) Uani 1 1 d . . . O1 O 0.82788(14) 0.96455(14) 0.77971(12) 0.0214(4) Uani 1 1 d . . . O2 O 0.89122(15) 0.76253(14) 0.85658(12) 0.0231(4) Uani 1 1 d . . . C1 C 0.6510(2) 0.9371(2) 0.84134(19) 0.0252(6) Uani 1 1 d . . . H1 H 0.6941 0.8797 0.8867 0.030 Uiso 1 1 calc R . . C2 C 0.6765(2) 1.0477(2) 0.6458(2) 0.0256(6) Uani 1 1 d . . . H2 H 0.7140 1.0316 0.5799 0.031 Uiso 1 1 calc R . . C3 C 0.8231(2) 0.5881(2) 0.84080(19) 0.0259(6) Uani 1 1 d . . . H3 H 0.8064 0.5458 0.7896 0.031 Uiso 1 1 calc R . . C4 C 1.0211(2) 0.6024(2) 0.7486(2) 0.0267(6) Uani 1 1 d . . . H4 H 1.0497 0.5659 0.8121 0.032 Uiso 1 1 calc R . . C5 C 0.9310(2) 0.9604(2) 0.7365(2) 0.0266(6) Uani 1 1 d . . . H5A H 0.9228 1.0114 0.6794 0.032 Uiso 1 1 calc R . . H5B H 0.9689 0.8887 0.7134 0.032 Uiso 1 1 calc R . . C6 C 0.9941(3) 0.9876(2) 0.8137(2) 0.0322(7) Uani 1 1 d . . . H6A H 0.9436 1.0433 0.8534 0.039 Uiso 1 1 calc R . . H6B H 1.0464 1.0189 0.7797 0.039 Uiso 1 1 calc R . . C7 C 0.9499(3) 0.7427(2) 0.94534(19) 0.0291(7) Uani 1 1 d . . . H7A H 1.0206 0.6884 0.9348 0.035 Uiso 1 1 calc R . . H7B H 0.9094 0.7165 0.9990 0.035 Uiso 1 1 calc R . . C8 C 0.9650(3) 0.8445(2) 0.9723(2) 0.0346(7) Uani 1 1 d . . . H8A H 0.9848 0.8376 1.0419 0.041 Uiso 1 1 calc R . . H8B H 0.8956 0.9016 0.9669 0.041 Uiso 1 1 calc R . . C9 C 0.5472(2) 0.9114(3) 0.8296(2) 0.0344(7) Uani 1 1 d . . . H9A H 0.5196 0.8929 0.8942 0.052 Uiso 1 1 calc R . . H9B H 0.5615 0.8517 0.7869 0.052 Uiso 1 1 calc R . . H9C H 0.4937 0.9731 0.8003 0.052 Uiso 1 1 calc R . . C10 C 0.6287(3) 1.0388(2) 0.8965(2) 0.0371(8) Uani 1 1 d . . . H10A H 0.5767 1.0969 0.8611 0.056 Uiso 1 1 calc R . . H10B H 0.6959 1.0555 0.9007 0.056 Uiso 1 1 calc R . . H10C H 0.5994 1.0291 0.9628 0.056 Uiso 1 1 calc R . . C11 C 0.6949(3) 1.1488(2) 0.6757(2) 0.0369(8) Uani 1 1 d . . . H11A H 0.6697 1.2045 0.6244 0.055 Uiso 1 1 calc R . . H11B H 0.7718 1.1356 0.6840 0.055 Uiso 1 1 calc R . . H11C H 0.6549 1.1712 0.7377 0.055 Uiso 1 1 calc R . . C12 C 0.5573(2) 1.0697(2) 0.6303(2) 0.0344(7) Uani 1 1 d . . . H12A H 0.5154 1.1010 0.6889 0.052 Uiso 1 1 calc R . . H12B H 0.5437 1.0034 0.6186 0.052 Uiso 1 1 calc R . . H12C H 0.5360 1.1188 0.5733 0.052 Uiso 1 1 calc R . . C13 C 0.7167(3) 0.6460(2) 0.8923(2) 0.0358(8) Uani 1 1 d . . . H13A H 0.6816 0.5947 0.9189 0.054 Uiso 1 1 calc R . . H13B H 0.6701 0.6952 0.8452 0.054 Uiso 1 1 calc R . . H13C H 0.7297 0.6852 0.9461 0.054 Uiso 1 1 calc R . . C14 C 0.8944(3) 0.5095(2) 0.9132(2) 0.0380(8) Uani 1 1 d . . . H14A H 0.9138 0.5477 0.9644 0.057 Uiso 1 1 calc R . . H14B H 0.9598 0.4671 0.8784 0.057 Uiso 1 1 calc R . . H14C H 0.8554 0.4630 0.9435 0.057 Uiso 1 1 calc R . . C15 C 1.0944(2) 0.6668(2) 0.7114(2) 0.0325(7) Uani 1 1 d . . . H15A H 1.1681 0.6196 0.7021 0.049 Uiso 1 1 calc R . . H15B H 1.0927 0.7189 0.7596 0.049 Uiso 1 1 calc R . . H15C H 1.0693 0.7034 0.6487 0.049 Uiso 1 1 calc R . . C16 C 1.0267(2) 0.5165(2) 0.6779(2) 0.0327(7) Uani 1 1 d . . . H16A H 1.0087 0.5487 0.6121 0.049 Uiso 1 1 calc R . . H16B H 0.9754 0.4795 0.7006 0.049 Uiso 1 1 calc R . . H16C H 1.0996 0.4662 0.6755 0.049 Uiso 1 1 calc R . . C17 C 0.7746(2) 0.7742(2) 0.47541(18) 0.0199(6) Uani 1 1 d . . . C18 C 0.6761(2) 0.8337(2) 0.51792(18) 0.0216(6) Uani 1 1 d . . . H18 H 0.6498 0.9113 0.5014 0.026 Uiso 1 1 calc R . . C19 C 0.6200(2) 0.7923(2) 0.59406(19) 0.0264(6) Uani 1 1 d . . . H19 H 0.5550 0.8409 0.6278 0.032 Uiso 1 1 calc R . . C20 C 0.6614(2) 0.6887(2) 0.6302(2) 0.0273(7) Uani 1 1 d . . . H20 H 0.6268 0.6623 0.6892 0.033 Uiso 1 1 calc R . . C21 C 0.7632(3) 0.6282(2) 0.59216(19) 0.0284(7) Uani 1 1 d . . . H21 H 0.8007 0.5581 0.6246 0.034 Uiso 1 1 calc R . . C22 C 0.8175(2) 0.6702(2) 0.51749(18) 0.0228(6) Uani 1 1 d . . . H22 H 0.8937 0.6293 0.4996 0.027 Uiso 1 1 calc R . . C23 C 0.9511(2) 0.7594(2) 0.35282(19) 0.0227(6) Uani 1 1 d . . . C24 C 0.9977(2) 0.7430(2) 0.2579(2) 0.0273(7) Uani 1 1 d . . . H24 H 0.9523 0.7642 0.2037 0.033 Uiso 1 1 calc R . . C25 C 1.1065(3) 0.6975(2) 0.2393(2) 0.0356(8) Uani 1 1 d . . . H25 H 1.1349 0.6895 0.1735 0.043 Uiso 1 1 calc R . . C26 C 1.1745(3) 0.6634(2) 0.3170(2) 0.0376(8) Uani 1 1 d . . . H26 H 1.2494 0.6306 0.3049 0.045 Uiso 1 1 calc R . . C27 C 1.1323(2) 0.6777(2) 0.4118(2) 0.0324(7) Uani 1 1 d . . . H27 H 1.1780 0.6546 0.4657 0.039 Uiso 1 1 calc R . . C28 C 1.0232(2) 0.7257(2) 0.4284(2) 0.0276(7) Uani 1 1 d . . . H28 H 0.9960 0.7362 0.4944 0.033 Uiso 1 1 calc R . . C29 C 0.7546(2) 0.7910(2) 0.28616(19) 0.0255(6) Uani 1 1 d . . . C30 C 0.7049(2) 0.7122(2) 0.2970(2) 0.0289(7) Uani 1 1 d . . . H30 H 0.7098 0.6728 0.3579 0.035 Uiso 1 1 calc R . . C31 C 0.6490(3) 0.6890(3) 0.2233(2) 0.0396(8) Uani 1 1 d . . . H31 H 0.6169 0.6345 0.2342 0.048 Uiso 1 1 calc R . . C32 C 0.6398(3) 0.7443(3) 0.1346(2) 0.0445(9) Uani 1 1 d . . . H32 H 0.6006 0.7293 0.0841 0.053 Uiso 1 1 calc R . . C33 C 0.6879(3) 0.8215(3) 0.1197(2) 0.0434(9) Uani 1 1 d . . . H33 H 0.6825 0.8599 0.0583 0.052 Uiso 1 1 calc R . . C34 C 0.7446(3) 0.8443(3) 0.1936(2) 0.0354(8) Uani 1 1 d . . . H34 H 0.7777 0.8978 0.1810 0.042 Uiso 1 1 calc R . . C35 C 0.8000(2) 0.9453(2) 0.37979(18) 0.0214(6) Uani 1 1 d . . . C36 C 0.7079(2) 1.0214(2) 0.3448(2) 0.0301(7) Uani 1 1 d . . . H36 H 0.6558 0.9988 0.3151 0.036 Uiso 1 1 calc R . . C37 C 0.6901(3) 1.1285(2) 0.3520(2) 0.0381(8) Uani 1 1 d . . . H37 H 0.6269 1.1777 0.3267 0.046 Uiso 1 1 calc R . . C38 C 0.7627(3) 1.1642(2) 0.3954(2) 0.0382(8) Uani 1 1 d . . . H38 H 0.7508 1.2378 0.3989 0.046 Uiso 1 1 calc R . . C39 C 0.8526(2) 1.0926(2) 0.4335(2) 0.0317(7) Uani 1 1 d . . . H39 H 0.9027 1.1161 0.4657 0.038 Uiso 1 1 calc R . . C40 C 0.8698(2) 0.9855(2) 0.4246(2) 0.0270(7) Uani 1 1 d . . . H40 H 0.9331 0.9371 0.4508 0.032 Uiso 1 1 calc R . . C41 C 0.5941(5) 0.4838(6) 0.4322(5) 0.144(6) Uiso 0.50 1 d PG A -1 H41A H 0.6609 0.4773 0.3980 0.173 Uiso 0.50 1 calc PR A -1 C41A C 0.5731(5) 0.3945(5) 0.4742(6) 0.132(6) Uiso 0.50 1 d PG A -1 H41B H 0.6255 0.3270 0.4686 0.159 Uiso 0.50 1 calc PR A -1 C42 C 0.4753(5) 0.4039(4) 0.5243(5) 0.055(2) Uiso 0.50 1 d PG A -1 H42A H 0.4609 0.3429 0.5530 0.066 Uiso 0.50 1 calc PR A -1 C42A C 0.3986(4) 0.5027(4) 0.5325(4) 0.0399(17) Uiso 0.50 1 d PG A -1 H42B H 0.3318 0.5091 0.5667 0.048 Uiso 0.50 1 calc PR A -1 C43 C 0.4196(4) 0.5920(4) 0.4905(4) 0.050(2) Uiso 0.50 1 d PG A -1 H43A H 0.3672 0.6595 0.4961 0.060 Uiso 0.50 1 calc PR A -1 C43A C 0.5174(5) 0.5825(5) 0.4404(5) 0.064(3) Uiso 0.50 1 d PG A -1 H43B H 0.5318 0.6436 0.4117 0.077 Uiso 0.50 1 calc PR A -1 H100 H 0.888(2) 0.817(2) 0.633(2) 0.044(9) Uiso 1 1 d . B -1 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 0.01932(13) 0.01781(12) 0.01532(12) -0.00034(8) -0.00101(8) -0.00649(9) S1 0.0362(5) 0.0396(5) 0.0381(4) -0.0015(4) -0.0116(4) -0.0171(4) P1 0.0203(4) 0.0179(4) 0.0183(3) -0.0005(3) 0.0004(3) -0.0046(3) P2 0.0252(4) 0.0174(4) 0.0186(4) -0.0006(3) -0.0038(3) -0.0061(3) B1 0.0232(18) 0.0255(17) 0.0190(16) -0.0018(13) 0.0016(13) -0.0061(13) O1 0.0218(10) 0.0212(10) 0.0219(10) -0.0037(8) -0.0003(8) -0.0076(8) O2 0.0302(11) 0.0207(10) 0.0180(9) -0.0010(7) -0.0085(8) -0.0061(8) C1 0.0262(16) 0.0268(16) 0.0199(14) -0.0008(11) 0.0030(12) -0.0051(12) C2 0.0302(17) 0.0214(15) 0.0225(14) 0.0036(11) -0.0007(12) -0.0049(12) C3 0.0375(18) 0.0221(15) 0.0200(14) 0.0022(11) -0.0048(12) -0.0119(13) C4 0.0281(17) 0.0212(15) 0.0279(15) -0.0020(12) -0.0072(13) -0.0021(12) C5 0.0266(17) 0.0284(16) 0.0268(15) -0.0016(12) 0.0001(12) -0.0115(13) C6 0.0368(19) 0.0321(17) 0.0328(17) -0.0009(13) -0.0003(14) -0.0183(14) C7 0.0397(19) 0.0298(16) 0.0195(14) 0.0020(12) -0.0103(13) -0.0124(14) C8 0.051(2) 0.0379(18) 0.0212(15) -0.0003(13) -0.0098(14) -0.0212(16) C9 0.0264(17) 0.046(2) 0.0282(16) -0.0019(14) 0.0099(13) -0.0103(14) C10 0.042(2) 0.0342(18) 0.0288(16) -0.0085(13) 0.0086(14) -0.0035(15) C11 0.046(2) 0.0212(16) 0.0410(18) 0.0049(13) -0.0062(15) -0.0078(14) C12 0.0311(18) 0.0287(17) 0.0370(17) 0.0036(13) -0.0029(14) -0.0009(13) C13 0.046(2) 0.0350(18) 0.0292(16) 0.0050(13) 0.0035(14) -0.0196(15) C14 0.057(2) 0.0290(17) 0.0295(17) 0.0070(13) -0.0106(15) -0.0164(15) C15 0.0263(17) 0.0318(17) 0.0382(17) -0.0069(13) -0.0028(14) -0.0063(13) C16 0.0327(18) 0.0240(16) 0.0369(17) -0.0046(13) -0.0029(14) -0.0014(13) C17 0.0234(15) 0.0230(14) 0.0171(13) -0.0025(11) -0.0062(11) -0.0111(12) C18 0.0231(15) 0.0273(15) 0.0165(13) -0.0002(11) -0.0060(11) -0.0099(12) C19 0.0254(16) 0.0378(18) 0.0190(14) -0.0029(12) -0.0017(12) -0.0136(13) C20 0.0353(18) 0.0361(18) 0.0196(14) 0.0015(12) -0.0049(13) -0.0239(14) C21 0.0414(19) 0.0269(16) 0.0223(15) 0.0033(12) -0.0106(13) -0.0174(14) C22 0.0300(17) 0.0220(15) 0.0177(14) -0.0048(11) -0.0043(12) -0.0088(12) C23 0.0269(16) 0.0154(14) 0.0268(15) -0.0023(11) 0.0015(12) -0.0081(11) C24 0.0314(18) 0.0248(16) 0.0266(15) 0.0003(12) 0.0036(13) -0.0112(13) C25 0.039(2) 0.0309(17) 0.0391(18) -0.0093(14) 0.0151(15) -0.0158(15) C26 0.0283(18) 0.0232(16) 0.062(2) -0.0114(15) 0.0096(16) -0.0091(13) C27 0.0256(17) 0.0296(17) 0.0413(18) -0.0041(13) -0.0032(14) -0.0067(13) C28 0.0253(17) 0.0256(16) 0.0311(16) -0.0056(12) 0.0002(13) -0.0062(12) C29 0.0240(16) 0.0298(16) 0.0199(14) -0.0052(12) 0.0019(12) -0.0042(12) C30 0.0258(17) 0.0341(17) 0.0265(16) -0.0062(12) 0.0000(13) -0.0083(13) C31 0.0336(19) 0.051(2) 0.0389(19) -0.0162(16) -0.0014(15) -0.0179(16) C32 0.034(2) 0.069(3) 0.0296(18) -0.0182(17) -0.0065(15) -0.0104(18) C33 0.045(2) 0.060(2) 0.0173(16) -0.0036(15) -0.0051(14) -0.0033(18) C34 0.040(2) 0.0403(19) 0.0227(16) -0.0001(13) 0.0002(14) -0.0091(15) C35 0.0201(15) 0.0251(15) 0.0190(14) 0.0013(11) 0.0032(11) -0.0083(12) C36 0.0256(17) 0.0301(17) 0.0363(17) 0.0029(13) -0.0028(13) -0.0116(13) C37 0.0262(18) 0.0266(17) 0.057(2) 0.0083(15) -0.0025(15) -0.0041(14) C38 0.0323(19) 0.0208(16) 0.061(2) 0.0010(14) 0.0043(16) -0.0099(14) C39 0.0266(17) 0.0305(17) 0.0411(18) -0.0050(14) 0.0005(14) -0.0130(13) C40 0.0238(16) 0.0287(16) 0.0269(15) 0.0002(12) 0.0006(12) -0.0067(13) _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 C21 2.256(3) . ? Ru1 C22 2.266(2) . ? Ru1 P2 2.2662(7) . ? Ru1 C19 2.269(3) . ? Ru1 C18 2.283(3) . ? Ru1 P1 2.2938(7) . ? Ru1 C20 2.305(3) . ? Ru1 C17 2.360(2) . ? Ru1 H100 1.61(3) . ? S1 C6 1.804(3) . ? S1 C8 1.815(3) . ? P1 O1 1.6174(19) . ? P1 C1 1.845(3) . ? P1 C2 1.858(3) . ? P2 O2 1.6134(18) . ? P2 C4 1.837(3) . ? P2 C3 1.853(3) . ? B1 C23 1.634(4) . ? B1 C35 1.641(4) . ? B1 C17 1.645(4) . ? B1 C29 1.649(4) . ? O1 C5 1.429(3) . ? O2 C7 1.439(3) . ? C1 C9 1.525(4) . ? C1 C10 1.531(4) . ? C1 H1 1.0000 . ? C2 C12 1.523(4) . ? C2 C11 1.527(4) . ? C2 H2 1.0000 . ? C3 C13 1.520(4) . ? C3 C14 1.522(4) . ? C3 H3 1.0000 . ? C4 C16 1.525(4) . ? C4 C15 1.527(4) . ? C4 H4 1.0000 . ? C5 C6 1.506(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.505(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.399(4) . ? C17 C22 1.422(4) . ? C18 C19 1.422(4) . ? C18 H18 1.0000 . ? C19 C20 1.388(4) . ? C19 H19 1.0000 . ? C20 C21 1.412(4) . ? C20 H20 1.0000 . ? C21 C22 1.399(4) . ? C21 H21 1.0000 . ? C22 H22 1.0000 . ? C23 C28 1.396(4) . ? C23 C24 1.398(4) . ? C24 C25 1.378(4) . ? C24 H24 0.9500 . ? C25 C26 1.387(5) . ? C25 H25 0.9500 . ? C26 C27 1.376(4) . ? C26 H26 0.9500 . ? C27 C28 1.382(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.399(4) . ? C29 C34 1.403(4) . ? C30 C31 1.384(4) . ? C30 H30 0.9500 . ? C31 C32 1.370(5) . ? C31 H31 0.9500 . ? C32 C33 1.367(5) . ? C32 H32 0.9500 . ? C33 C34 1.390(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.385(4) . ? C35 C36 1.398(4) . ? C36 C37 1.383(4) . ? C36 H36 0.9500 . ? C37 C38 1.368(5) . ? C37 H37 0.9500 . ? C38 C39 1.370(4) . ? C38 H38 0.9500 . ? C39 C40 1.388(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C41A 1.3900 . ? C41 C43A 1.3900 . ? C41 H41A 0.9500 . ? C41A C42 1.3900 . ? C41A H41B 0.9500 . ? C42 C42A 1.3900 . ? C42 H42A 0.9500 . ? C42A C43 1.3900 . ? C42A H42B 0.9500 . ? C43 C43A 1.3900 . ? C43 H43A 0.9500 . ? C43A H43B 0.9500 . ? 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 C21 Ru1 C22 36.04(10) . . ? C21 Ru1 P2 92.09(7) . . ? C22 Ru1 P2 108.87(7) . . ? C21 Ru1 C19 63.91(11) . . ? C22 Ru1 C19 75.36(10) . . ? P2 Ru1 C19 133.72(7) . . ? C21 Ru1 C18 75.28(10) . . ? C22 Ru1 C18 63.04(10) . . ? P2 Ru1 C18 166.72(7) . . ? C19 Ru1 C18 36.40(9) . . ? C21 Ru1 P1 155.93(8) . . ? C22 Ru1 P1 157.24(7) . . ? P2 Ru1 P1 92.15(3) . . ? C19 Ru1 P1 96.66(8) . . ? C18 Ru1 P1 97.79(7) . . ? C21 Ru1 C20 36.05(11) . . ? C22 Ru1 C20 64.65(10) . . ? P2 Ru1 C20 102.96(7) . . ? C19 Ru1 C20 35.33(10) . . ? C18 Ru1 C20 64.38(10) . . ? P1 Ru1 C20 120.10(8) . . ? C21 Ru1 C17 64.86(9) . . ? C22 Ru1 C17 35.73(9) . . ? P2 Ru1 C17 141.86(7) . . ? C19 Ru1 C17 64.68(9) . . ? C18 Ru1 C17 35.02(9) . . ? P1 Ru1 C17 121.57(7) . . ? C20 Ru1 C17 76.65(9) . . ? C21 Ru1 H100 129.3(11) . . ? C22 Ru1 H100 99.4(10) . . ? P2 Ru1 H100 80.9(11) . . ? C19 Ru1 H100 145.2(11) . . ? C18 Ru1 H100 110.2(10) . . ? P1 Ru1 H100 74.8(11) . . ? C20 Ru1 H100 164.0(10) . . ? C17 Ru1 H100 90.7(10) . . ? C6 S1 C8 105.84(15) . . ? O1 P1 C1 94.52(11) . . ? O1 P1 C2 101.85(12) . . ? C1 P1 C2 109.38(13) . . ? O1 P1 Ru1 119.34(7) . . ? C1 P1 Ru1 117.00(9) . . ? C2 P1 Ru1 112.55(9) . . ? O2 P2 C4 104.20(12) . . ? O2 P2 C3 105.84(11) . . ? C4 P2 C3 102.29(13) . . ? O2 P2 Ru1 110.98(7) . . ? C4 P2 Ru1 117.97(9) . . ? C3 P2 Ru1 114.32(9) . . ? C23 B1 C35 109.6(2) . . ? C23 B1 C17 113.2(2) . . ? C35 B1 C17 108.4(2) . . ? C23 B1 C29 109.7(2) . . ? C35 B1 C29 111.8(2) . . ? C17 B1 C29 104.2(2) . . ? C5 O1 P1 125.59(16) . . ? C7 O2 P2 131.28(17) . . ? C9 C1 C10 110.8(2) . . ? C9 C1 P1 115.02(19) . . ? C10 C1 P1 114.6(2) . . ? C9 C1 H1 105.1 . . ? C10 C1 H1 105.1 . . ? P1 C1 H1 105.1 . . ? C12 C2 C11 109.1(2) . . ? C12 C2 P1 114.2(2) . . ? C11 C2 P1 114.2(2) . . ? C12 C2 H2 106.2 . . ? C11 C2 H2 106.2 . . ? P1 C2 H2 106.2 . . ? C13 C3 C14 109.5(2) . . ? C13 C3 P2 110.20(19) . . ? C14 C3 P2 116.6(2) . . ? C13 C3 H3 106.7 . . ? C14 C3 H3 106.7 . . ? P2 C3 H3 106.7 . . ? C16 C4 C15 110.8(2) . . ? C16 C4 P2 111.4(2) . . ? C15 C4 P2 113.26(19) . . ? C16 C4 H4 107.0 . . ? C15 C4 H4 107.0 . . ? P2 C4 H4 107.0 . . ? O1 C5 C6 107.8(2) . . ? O1 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? O1 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? C5 C6 S1 118.0(2) . . ? C5 C6 H6A 107.8 . . ? S1 C6 H6A 107.8 . . ? C5 C6 H6B 107.8 . . ? S1 C6 H6B 107.8 . . ? H6A C6 H6B 107.1 . . ? O2 C7 C8 108.2(2) . . ? O2 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O2 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C7 C8 S1 114.6(2) . . ? C7 C8 H8A 108.6 . . ? S1 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? S1 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 114.9(2) . . ? C18 C17 B1 120.2(2) . . ? C22 C17 B1 124.2(2) . . ? C18 C17 Ru1 69.47(14) . . ? C22 C17 Ru1 68.51(14) . . ? B1 C17 Ru1 140.15(18) . . ? C17 C18 C19 122.9(3) . . ? C17 C18 Ru1 75.51(15) . . ? C19 C18 Ru1 71.26(15) . . ? C17 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? Ru1 C18 H18 118.2 . . ? C20 C19 C18 120.9(3) . . ? C20 C19 Ru1 73.74(16) . . ? C18 C19 Ru1 72.34(15) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? Ru1 C19 H19 119.3 . . ? C19 C20 C21 117.6(3) . . ? C19 C20 Ru1 70.93(16) . . ? C21 C20 Ru1 70.07(16) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? Ru1 C20 H20 120.8 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 Ru1 72.39(15) . . ? C20 C21 Ru1 73.88(16) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? Ru1 C21 H21 119.4 . . ? C21 C22 C17 122.8(3) . . ? C21 C22 Ru1 71.57(15) . . ? C17 C22 Ru1 75.76(15) . . ? C21 C22 H22 118.3 . . ? C17 C22 H22 118.3 . . ? Ru1 C22 H22 118.3 . . ? C28 C23 C24 115.0(3) . . ? C28 C23 B1 122.7(2) . . ? C24 C23 B1 122.3(2) . . ? C25 C24 C23 123.0(3) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.2(3) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 119.8(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 123.1(3) . . ? C27 C28 H28 118.5 . . ? C23 C28 H28 118.5 . . ? C30 C29 C34 114.6(3) . . ? C30 C29 B1 123.3(2) . . ? C34 C29 B1 122.1(3) . . ? C31 C30 C29 123.1(3) . . ? C31 C30 H30 118.5 . . ? C29 C30 H30 118.5 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 119.1(3) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 120.7(3) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 122.3(3) . . ? C33 C34 H34 118.8 . . ? C29 C34 H34 118.8 . . ? C40 C35 C36 114.8(3) . . ? C40 C35 B1 121.8(2) . . ? C36 C35 B1 123.4(3) . . ? C37 C36 C35 122.3(3) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 119.3(3) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C40 119.3(3) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C35 C40 C39 123.7(3) . . ? C35 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? C41A C41 C43A 120.0 . . ? C41A C41 H41A 120.0 . . ? C43A C41 H41A 120.0 . . ? C41 C41A C42 120.0 . . ? C41 C41A H41B 120.0 . . ? C42 C41A H41B 120.0 . . ? C42A C42 C41A 120.0 . . ? C42A C42 H42A 120.0 . . ? C41A C42 H42A 120.0 . . ? C42 C42A C43 120.0 . . ? C42 C42A H42B 120.0 . . ? C43 C42A H42B 120.0 . . ? C43A C43 C42A 120.0 . . ? C43A C43 H43A 120.0 . . ? C42A C43 H43A 120.0 . . ? C43 C43A C41 120.0 . . ? C43 C43A H43B 120.0 . . ? C41 C43A H43B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.084 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 933829' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs092_0m_Compound_11 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C60 H56 B F20 N2 O2 P3 Ru' _chemical_formula_weight 1421.86 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7350(6) _cell_length_b 14.0486(7) _cell_length_c 16.8712(9) _cell_angle_alpha 92.955(2) _cell_angle_beta 92.820(2) _cell_angle_gamma 92.267(2) _cell_volume 3008.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8518 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.58 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6937 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50571 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_unetI/netI 0.0742 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.58 _reflns_number_total 13678 _reflns_number_gt 9277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0379P)^2^+5.9348P] 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 13678 _refine_ls_number_parameters 807 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.005 _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 Ru1 Ru 0.74225(2) 0.82261(2) 0.717578(17) 0.02431(9) Uani 1 1 d . . . P1 P 0.59545(7) 0.90037(7) 0.67037(5) 0.0235(2) Uani 1 1 d . . . P2 P 0.89908(9) 0.74010(10) 0.70897(6) 0.0443(3) Uani 1 1 d . . . P3 P 0.82028(7) 0.94912(7) 0.79386(5) 0.0221(2) Uani 1 1 d . . . F1 F 0.6304(3) 0.72361(17) 0.12059(13) 0.0591(8) Uani 1 1 d . . . F2 F 0.6891(2) 0.90691(18) 0.11717(15) 0.0566(8) Uani 1 1 d . . . F3 F 0.77043(19) 1.00475(17) 0.25179(17) 0.0507(7) Uani 1 1 d . . . F4 F 0.79388(19) 0.91145(16) 0.38889(15) 0.0452(6) Uani 1 1 d . . . F5 F 0.74684(17) 0.72730(14) 0.39189(12) 0.0293(5) Uani 1 1 d . . . F6 F 0.8701(2) 0.60205(18) 0.30520(14) 0.0466(7) Uani 1 1 d . . . F7 F 0.9576(2) 0.5075(2) 0.42162(15) 0.0531(7) Uani 1 1 d . . . F8 F 0.8388(2) 0.38592(18) 0.50545(14) 0.0498(7) Uani 1 1 d . . . F9 F 0.6272(2) 0.36674(19) 0.47055(16) 0.0608(8) Uani 1 1 d . . . F10 F 0.5377(2) 0.46136(18) 0.35614(16) 0.0562(8) Uani 1 1 d . . . F11 F 0.52251(18) 0.66502(16) 0.37132(12) 0.0366(5) Uani 1 1 d . . . F12 F 0.3153(2) 0.6851(2) 0.36290(17) 0.0574(7) Uani 1 1 d . . . F13 F 0.1983(3) 0.6277(2) 0.2284(2) 0.0836(11) Uani 1 1 d . . . F14 F 0.2969(3) 0.5548(3) 0.0999(2) 0.1134(17) Uani 1 1 d . . . F15 F 0.5021(3) 0.5438(2) 0.10309(16) 0.0794(11) Uani 1 1 d . . . F16 F 0.8333(3) 0.6585(2) 0.13962(17) 0.0741(10) Uani 1 1 d . . . F17 F 0.9159(4) 0.5486(3) 0.0320(2) 0.129(2) Uani 1 1 d . . . F18 F 0.8453(4) 0.3647(3) 0.00151(17) 0.129(2) Uani 1 1 d . . . F19 F 0.6820(4) 0.2952(2) 0.0851(2) 0.1136(17) Uani 1 1 d . . . F20 F 0.5964(3) 0.40614(18) 0.19472(19) 0.0692(10) Uani 1 1 d . . . O1 O 0.5519(2) 0.8483(2) 0.58493(15) 0.0344(7) Uani 1 1 d . . . O2 O 0.8865(3) 0.6591(3) 0.6386(2) 0.0841(15) Uani 1 1 d . . . N1 N 0.6638(3) 0.6985(2) 0.64613(18) 0.0317(8) Uani 1 1 d . . . H1B H 0.5963 0.6968 0.6648 0.038 Uiso 1 1 calc R . . N2 N 0.6739(2) 0.7594(2) 0.81608(18) 0.0270(7) Uani 1 1 d . . . C1 C 0.6123(3) 1.0272(3) 0.6445(2) 0.0296(9) Uani 1 1 d . . . H1A H 0.6683 1.0570 0.6825 0.035 Uiso 1 1 calc R . . C2 C 0.4675(3) 0.8912(3) 0.7176(2) 0.0268(8) Uani 1 1 d . . . H2A H 0.4168 0.9300 0.6872 0.032 Uiso 1 1 calc R . . C3 C 1.0103(5) 0.8197(5) 0.6676(3) 0.0760(19) Uani 1 1 d . . . H3A H 1.0016 0.8858 0.6905 0.091 Uiso 1 1 calc R . . C4 C 0.9689(4) 0.6810(3) 0.7891(3) 0.0486(13) Uani 1 1 d . . . H4A H 1.0107 0.7312 0.8226 0.058 Uiso 1 1 calc R . . C5 C 0.6234(3) 0.8010(3) 0.5339(2) 0.0382(11) Uani 1 1 d . . . H5A H 0.6909 0.8387 0.5354 0.046 Uiso 1 1 calc R . . H5B H 0.5934 0.7975 0.4785 0.046 Uiso 1 1 calc R . . C6 C 0.6434(4) 0.7012(3) 0.5594(2) 0.0417(11) Uani 1 1 d . . . H6A H 0.5814 0.6587 0.5430 0.050 Uiso 1 1 calc R . . H6B H 0.7046 0.6767 0.5321 0.050 Uiso 1 1 calc R . . C7 C 0.8077(5) 0.5825(4) 0.6336(3) 0.072(2) Uani 1 1 d . . . H7A H 0.8366 0.5283 0.6615 0.087 Uiso 1 1 calc R . . H7B H 0.7951 0.5612 0.5769 0.087 Uiso 1 1 calc R . . C8 C 0.7028(4) 0.6040(3) 0.6670(3) 0.0522(13) Uani 1 1 d . . . H8A H 0.6502 0.5536 0.6470 0.063 Uiso 1 1 calc R . . H8B H 0.7094 0.6019 0.7256 0.063 Uiso 1 1 calc R . . C9 C 0.6536(3) 1.0356(3) 0.5611(2) 0.0428(11) Uani 1 1 d . . . H9A H 0.6616 1.1030 0.5496 0.064 Uiso 1 1 calc R . . H9B H 0.6036 1.0029 0.5218 0.064 Uiso 1 1 calc R . . H9C H 0.7219 1.0061 0.5587 0.064 Uiso 1 1 calc R . . C10 C 0.5160(3) 1.0884(3) 0.6521(2) 0.0357(10) Uani 1 1 d . . . H10A H 0.5338 1.1534 0.6373 0.054 Uiso 1 1 calc R . . H10B H 0.4947 1.0901 0.7072 0.054 Uiso 1 1 calc R . . H10C H 0.4580 1.0609 0.6168 0.054 Uiso 1 1 calc R . . C11 C 0.4745(3) 0.9307(3) 0.8035(2) 0.0296(9) Uani 1 1 d . . . H11A H 0.4051 0.9246 0.8259 0.044 Uiso 1 1 calc R . . H11B H 0.4979 0.9981 0.8055 0.044 Uiso 1 1 calc R . . H11C H 0.5249 0.8948 0.8345 0.044 Uiso 1 1 calc R . . C12 C 0.4233(3) 0.7879(3) 0.7133(3) 0.0375(10) Uani 1 1 d . . . H12A H 0.3556 0.7851 0.7385 0.056 Uiso 1 1 calc R . . H12B H 0.4728 0.7477 0.7411 0.056 Uiso 1 1 calc R . . H12C H 0.4132 0.7647 0.6575 0.056 Uiso 1 1 calc R . . C13 C 1.1204(5) 0.7979(6) 0.6853(4) 0.107(3) Uani 1 1 d . . . H13A H 1.1667 0.8446 0.6614 0.160 Uiso 1 1 calc R . . H13B H 1.1333 0.7337 0.6633 0.160 Uiso 1 1 calc R . . H13C H 1.1347 0.8008 0.7430 0.160 Uiso 1 1 calc R . . C14 C 0.9841(5) 0.8225(7) 0.5775(4) 0.123(3) Uani 1 1 d . . . H14A H 1.0375 0.8624 0.5536 0.184 Uiso 1 1 calc R . . H14B H 0.9148 0.8493 0.5686 0.184 Uiso 1 1 calc R . . H14C H 0.9832 0.7577 0.5530 0.184 Uiso 1 1 calc R . . C15 C 0.8921(4) 0.6309(4) 0.8429(3) 0.0591(15) Uani 1 1 d . . . H15A H 0.9321 0.6003 0.8850 0.089 Uiso 1 1 calc R . . H15B H 0.8485 0.5825 0.8112 0.089 Uiso 1 1 calc R . . H15C H 0.8469 0.6781 0.8669 0.089 Uiso 1 1 calc R . . C16 C 1.0462(5) 0.6065(5) 0.7593(3) 0.084(2) Uani 1 1 d . . . H16A H 1.0809 0.5781 0.8050 0.127 Uiso 1 1 calc R . . H16B H 1.0992 0.6377 0.7282 0.127 Uiso 1 1 calc R . . H16C H 1.0073 0.5564 0.7259 0.127 Uiso 1 1 calc R . . C17 C 0.7335(3) 1.0206(2) 0.8577(2) 0.0200(7) Uani 1 1 d . . . C18 C 0.6955(3) 0.9857(3) 0.9268(2) 0.0233(8) Uani 1 1 d . . . H18A H 0.7167 0.9253 0.9430 0.028 Uiso 1 1 calc R . . C19 C 0.6276(3) 1.0367(3) 0.9726(2) 0.0318(9) Uani 1 1 d . . . H19A H 0.6036 1.0115 1.0200 0.038 Uiso 1 1 calc R . . C20 C 0.5943(3) 1.1244(3) 0.9497(2) 0.0385(10) Uani 1 1 d . . . H20A H 0.5472 1.1593 0.9807 0.046 Uiso 1 1 calc R . . C21 C 0.6309(3) 1.1601(3) 0.8809(3) 0.0385(10) Uani 1 1 d . . . H21A H 0.6084 1.2200 0.8644 0.046 Uiso 1 1 calc R . . C22 C 0.7000(3) 1.1097(3) 0.8359(2) 0.0286(8) Uani 1 1 d . . . H22A H 0.7252 1.1361 0.7893 0.034 Uiso 1 1 calc R . . C23 C 0.8883(3) 1.0476(3) 0.7461(2) 0.0348(10) Uani 1 1 d . . . C24 C 0.9319(3) 1.1269(3) 0.7910(3) 0.0455(12) Uani 1 1 d . . . H24A H 0.9292 1.1290 0.8473 0.055 Uiso 1 1 calc R . . C25 C 0.9790(4) 1.2026(4) 0.7545(4) 0.0686(18) Uani 1 1 d . . . H25A H 1.0082 1.2565 0.7855 0.082 Uiso 1 1 calc R . . C26 C 0.9832(4) 1.1989(6) 0.6727(5) 0.096(3) Uani 1 1 d . . . H26A H 1.0157 1.2503 0.6474 0.115 Uiso 1 1 calc R . . C27 C 0.9412(4) 1.1225(6) 0.6285(4) 0.093(3) Uani 1 1 d . . . H27A H 0.9435 1.1212 0.5723 0.112 Uiso 1 1 calc R . . C28 C 0.8947(3) 1.0460(4) 0.6645(3) 0.0551(14) Uani 1 1 d . . . H28A H 0.8671 0.9921 0.6328 0.066 Uiso 1 1 calc R . . C29 C 0.9240(3) 0.9157(3) 0.8668(2) 0.0225(8) Uani 1 1 d . . . C30 C 0.9009(3) 0.8538(3) 0.9258(2) 0.0274(8) Uani 1 1 d . . . H30A H 0.8301 0.8314 0.9302 0.033 Uiso 1 1 calc R . . C31 C 0.9782(3) 0.8238(3) 0.9786(2) 0.0331(9) Uani 1 1 d . . . H31A H 0.9601 0.7817 1.0186 0.040 Uiso 1 1 calc R . . C32 C 1.0821(3) 0.8553(3) 0.9728(2) 0.0376(10) Uani 1 1 d . . . H32A H 1.1352 0.8358 1.0093 0.045 Uiso 1 1 calc R . . C33 C 1.1076(3) 0.9148(3) 0.9141(2) 0.0373(10) Uani 1 1 d . . . H33A H 1.1788 0.9354 0.9091 0.045 Uiso 1 1 calc R . . C34 C 1.0298(3) 0.9453(3) 0.8617(2) 0.0282(8) Uani 1 1 d . . . H34A H 1.0486 0.9869 0.8217 0.034 Uiso 1 1 calc R . . C35 C 0.6390(3) 0.7237(3) 0.8688(2) 0.0297(9) Uani 1 1 d . . . C36 C 0.5983(4) 0.6788(3) 0.9379(2) 0.0531(13) Uani 1 1 d . . . H36A H 0.6258 0.6149 0.9412 0.080 Uiso 1 1 calc R . . H36B H 0.5213 0.6739 0.9326 0.080 Uiso 1 1 calc R . . H36C H 0.6206 0.7175 0.9862 0.080 Uiso 1 1 calc R . . C37 C 0.6896(3) 0.7130(3) 0.2550(2) 0.0277(9) Uani 1 1 d . . . C38 C 0.6738(4) 0.7669(3) 0.1890(2) 0.0371(10) Uani 1 1 d . . . C39 C 0.7018(4) 0.8621(3) 0.1859(2) 0.0396(11) Uani 1 1 d . . . C40 C 0.7436(3) 0.9113(3) 0.2528(3) 0.0356(10) Uani 1 1 d . . . C41 C 0.7563(3) 0.8640(3) 0.3213(2) 0.0303(9) Uani 1 1 d . . . C42 C 0.7302(3) 0.7674(3) 0.3209(2) 0.0248(8) Uani 1 1 d . . . C43 C 0.6987(4) 0.5404(3) 0.3254(2) 0.0321(9) Uani 1 1 d . . . C44 C 0.8058(4) 0.5458(3) 0.3462(2) 0.0353(10) Uani 1 1 d . . . C45 C 0.8535(4) 0.4969(3) 0.4056(2) 0.0370(10) Uani 1 1 d . . . C46 C 0.7936(4) 0.4361(3) 0.4482(2) 0.0373(10) Uani 1 1 d . . . C47 C 0.6880(4) 0.4266(3) 0.4299(2) 0.0414(11) Uani 1 1 d . . . C48 C 0.6427(4) 0.4777(3) 0.3700(2) 0.0385(10) Uani 1 1 d . . . C49 C 0.5251(4) 0.6002(3) 0.2392(2) 0.0361(10) Uani 1 1 d . . . C50 C 0.4695(4) 0.6377(3) 0.3020(2) 0.0350(10) Uani 1 1 d . . . C51 C 0.3628(4) 0.6484(3) 0.2994(3) 0.0411(11) Uani 1 1 d . . . C52 C 0.3035(4) 0.6191(3) 0.2311(4) 0.0584(15) Uani 1 1 d . . . C53 C 0.3540(5) 0.5831(3) 0.1672(3) 0.0686(19) Uani 1 1 d . . . C54 C 0.4606(5) 0.5756(3) 0.1714(3) 0.0566(15) Uani 1 1 d . . . C55 C 0.7079(4) 0.5396(3) 0.1733(2) 0.0486(13) Uani 1 1 d . . . C56 C 0.7905(5) 0.5703(4) 0.1293(3) 0.0651(18) Uani 1 1 d . . . C57 C 0.8358(6) 0.5131(4) 0.0709(3) 0.089(3) Uani 1 1 d . . . C58 C 0.8001(7) 0.4210(5) 0.0557(3) 0.098(3) Uani 1 1 d . . . C59 C 0.7194(6) 0.3870(4) 0.0977(3) 0.081(2) Uani 1 1 d . . . C60 C 0.6761(6) 0.4457(4) 0.1550(3) 0.0640(18) Uani 1 1 d . . . B1 B 0.6544(4) 0.5986(3) 0.2484(3) 0.0354(12) Uani 1 1 d . . . H100 H 0.783(3) 0.860(3) 0.640(2) 0.033(11) Uiso 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 Ru1 0.01985(15) 0.03634(18) 0.01672(15) -0.00257(12) -0.00279(11) 0.01063(13) P1 0.0201(5) 0.0315(5) 0.0184(5) -0.0049(4) -0.0031(4) 0.0086(4) P2 0.0296(6) 0.0774(9) 0.0253(6) -0.0146(6) -0.0078(4) 0.0300(6) P3 0.0169(4) 0.0314(5) 0.0183(5) 0.0050(4) 0.0005(4) 0.0023(4) F1 0.123(3) 0.0371(15) 0.0187(12) 0.0028(10) -0.0049(14) 0.0292(16) F2 0.082(2) 0.0479(16) 0.0466(16) 0.0283(13) 0.0233(14) 0.0298(15) F3 0.0387(14) 0.0287(13) 0.087(2) 0.0202(13) 0.0136(14) -0.0007(11) F4 0.0414(15) 0.0316(13) 0.0602(17) -0.0054(12) -0.0060(12) -0.0068(11) F5 0.0371(13) 0.0286(12) 0.0220(11) -0.0010(9) 0.0018(9) 0.0024(10) F6 0.0573(16) 0.0482(15) 0.0394(14) 0.0169(12) 0.0216(12) 0.0236(13) F7 0.0517(17) 0.0688(19) 0.0430(15) 0.0166(13) 0.0087(13) 0.0294(14) F8 0.0743(19) 0.0469(15) 0.0289(13) 0.0127(11) -0.0098(12) 0.0149(14) F9 0.081(2) 0.0469(16) 0.0531(17) 0.0318(14) -0.0219(15) -0.0178(15) F10 0.0678(19) 0.0406(15) 0.0572(17) 0.0235(13) -0.0316(14) -0.0208(14) F11 0.0398(14) 0.0451(14) 0.0236(12) -0.0011(10) -0.0003(10) -0.0073(11) F12 0.0446(16) 0.074(2) 0.0546(18) 0.0192(15) -0.0001(13) -0.0018(15) F13 0.069(2) 0.059(2) 0.118(3) 0.0064(19) -0.055(2) 0.0127(17) F14 0.146(3) 0.081(2) 0.102(3) -0.040(2) -0.102(3) 0.057(2) F15 0.141(3) 0.0563(18) 0.0372(16) -0.0221(14) -0.0460(18) 0.0483(19) F16 0.130(3) 0.0501(18) 0.0520(18) 0.0215(14) 0.0552(18) 0.0433(19) F17 0.237(5) 0.110(3) 0.060(2) 0.042(2) 0.089(3) 0.118(3) F18 0.242(5) 0.116(3) 0.0342(17) -0.0233(18) -0.012(2) 0.139(3) F19 0.182(4) 0.054(2) 0.096(3) -0.0499(19) -0.075(3) 0.061(2) F20 0.114(3) 0.0252(15) 0.063(2) -0.0126(14) -0.0425(19) 0.0131(16) O1 0.0322(15) 0.0458(17) 0.0240(14) -0.0120(12) -0.0098(11) 0.0187(13) O2 0.051(2) 0.132(4) 0.062(2) -0.070(2) -0.0283(18) 0.051(2) N1 0.0368(19) 0.0340(19) 0.0236(17) -0.0076(14) -0.0088(14) 0.0162(15) N2 0.0280(17) 0.0269(17) 0.0252(17) -0.0031(14) -0.0088(14) 0.0074(14) C1 0.024(2) 0.039(2) 0.025(2) 0.0012(17) -0.0057(16) 0.0083(17) C2 0.0197(18) 0.028(2) 0.032(2) -0.0050(16) -0.0046(15) 0.0037(16) C3 0.064(4) 0.117(5) 0.047(3) -0.017(3) 0.000(3) 0.036(4) C4 0.050(3) 0.059(3) 0.036(2) -0.017(2) -0.016(2) 0.035(2) C5 0.045(3) 0.051(3) 0.0193(19) -0.0078(18) -0.0059(17) 0.023(2) C6 0.049(3) 0.048(3) 0.026(2) -0.0157(19) -0.0099(19) 0.019(2) C7 0.088(4) 0.083(4) 0.045(3) -0.031(3) -0.028(3) 0.067(4) C8 0.068(3) 0.043(3) 0.044(3) -0.011(2) -0.017(2) 0.032(2) C9 0.042(3) 0.057(3) 0.031(2) 0.013(2) 0.0001(19) 0.013(2) C10 0.035(2) 0.035(2) 0.038(2) 0.0083(18) -0.0016(18) 0.0112(19) C11 0.026(2) 0.034(2) 0.030(2) -0.0007(17) 0.0058(16) 0.0057(17) C12 0.026(2) 0.033(2) 0.052(3) -0.007(2) -0.0036(19) -0.0005(18) C13 0.049(4) 0.145(7) 0.118(6) -0.071(5) 0.004(4) 0.010(4) C14 0.075(5) 0.236(10) 0.063(4) -0.004(5) 0.040(4) 0.047(6) C15 0.081(4) 0.051(3) 0.044(3) -0.009(2) -0.024(3) 0.036(3) C16 0.083(4) 0.107(5) 0.064(4) -0.025(3) -0.018(3) 0.076(4) C17 0.0157(17) 0.0199(18) 0.0238(18) -0.0010(14) -0.0020(14) -0.0005(14) C18 0.0217(18) 0.0247(19) 0.0234(18) 0.0024(15) -0.0018(14) 0.0027(15) C19 0.030(2) 0.044(2) 0.0216(19) -0.0009(17) 0.0009(16) 0.0041(18) C20 0.040(2) 0.039(2) 0.036(2) -0.0134(19) 0.0035(19) 0.010(2) C21 0.042(3) 0.020(2) 0.053(3) -0.0030(19) -0.003(2) 0.0077(18) C22 0.029(2) 0.025(2) 0.031(2) 0.0051(16) -0.0007(17) -0.0021(16) C23 0.0154(18) 0.054(3) 0.038(2) 0.024(2) 0.0038(17) 0.0045(18) C24 0.026(2) 0.044(3) 0.069(3) 0.023(2) 0.001(2) -0.004(2) C25 0.028(3) 0.059(3) 0.122(5) 0.049(4) 0.002(3) -0.004(2) C26 0.027(3) 0.131(7) 0.139(7) 0.109(6) 0.012(4) -0.007(3) C27 0.039(3) 0.174(8) 0.075(4) 0.087(5) 0.013(3) -0.008(4) C28 0.024(2) 0.104(4) 0.042(3) 0.039(3) 0.007(2) 0.004(3) C29 0.0232(18) 0.0280(19) 0.0160(17) -0.0031(14) -0.0013(14) 0.0048(15) C30 0.026(2) 0.031(2) 0.0251(19) -0.0022(16) 0.0007(16) 0.0048(16) C31 0.041(2) 0.034(2) 0.024(2) 0.0022(17) -0.0044(17) 0.0063(19) C32 0.036(2) 0.042(3) 0.032(2) -0.0027(19) -0.0170(18) 0.006(2) C33 0.025(2) 0.045(3) 0.041(2) 0.001(2) -0.0079(18) 0.0017(19) C34 0.0223(19) 0.035(2) 0.027(2) 0.0015(17) -0.0016(16) 0.0009(17) C35 0.039(2) 0.028(2) 0.021(2) -0.0019(16) -0.0068(17) 0.0055(18) C36 0.089(4) 0.049(3) 0.022(2) 0.006(2) 0.006(2) 0.007(3) C37 0.040(2) 0.024(2) 0.0200(18) 0.0032(15) 0.0085(16) 0.0097(17) C38 0.057(3) 0.032(2) 0.023(2) 0.0010(17) 0.0061(19) 0.020(2) C39 0.050(3) 0.039(2) 0.035(2) 0.020(2) 0.021(2) 0.025(2) C40 0.027(2) 0.026(2) 0.057(3) 0.012(2) 0.018(2) 0.0064(17) C41 0.0185(19) 0.027(2) 0.046(2) -0.0004(18) 0.0067(17) 0.0007(16) C42 0.0264(19) 0.0251(19) 0.0246(19) 0.0055(15) 0.0093(15) 0.0057(16) C43 0.059(3) 0.0186(19) 0.0177(18) -0.0028(15) -0.0060(18) 0.0073(19) C44 0.058(3) 0.029(2) 0.021(2) 0.0037(16) 0.0101(19) 0.016(2) C45 0.048(3) 0.039(2) 0.026(2) -0.0003(18) 0.0026(19) 0.021(2) C46 0.065(3) 0.028(2) 0.0190(19) 0.0020(16) -0.005(2) 0.013(2) C47 0.072(3) 0.026(2) 0.025(2) 0.0073(17) -0.011(2) -0.005(2) C48 0.060(3) 0.024(2) 0.030(2) 0.0018(17) -0.015(2) -0.003(2) C49 0.065(3) 0.0151(19) 0.027(2) 0.0038(16) -0.015(2) 0.0030(19) C50 0.051(3) 0.023(2) 0.029(2) 0.0072(17) -0.0151(19) -0.0074(19) C51 0.049(3) 0.028(2) 0.046(3) 0.017(2) -0.009(2) -0.003(2) C52 0.060(3) 0.032(3) 0.080(4) 0.015(3) -0.042(3) 0.006(2) C53 0.103(5) 0.036(3) 0.061(3) -0.007(2) -0.059(3) 0.024(3) C54 0.103(4) 0.027(2) 0.037(3) -0.004(2) -0.033(3) 0.021(3) C55 0.097(4) 0.030(2) 0.019(2) -0.0017(18) -0.011(2) 0.030(2) C56 0.132(5) 0.050(3) 0.020(2) 0.011(2) 0.018(3) 0.053(3) C57 0.175(7) 0.074(4) 0.028(3) 0.021(3) 0.028(4) 0.084(5) C58 0.194(8) 0.081(5) 0.024(3) -0.013(3) -0.016(4) 0.102(5) C59 0.153(7) 0.043(3) 0.042(3) -0.024(3) -0.048(4) 0.058(4) C60 0.125(5) 0.035(3) 0.030(3) -0.006(2) -0.032(3) 0.034(3) B1 0.066(3) 0.022(2) 0.018(2) 0.0002(17) -0.008(2) 0.013(2) _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 N2 2.131(3) . ? Ru1 N1 2.240(3) . ? Ru1 P3 2.3024(10) . ? Ru1 P1 2.3297(9) . ? Ru1 P2 2.3554(11) . ? Ru1 H100 1.53(4) . ? P1 O1 1.644(3) . ? P1 C2 1.851(4) . ? P1 C1 1.863(4) . ? P2 O2 1.599(3) . ? P2 C4 1.834(4) . ? P2 C3 1.948(7) . ? P3 C23 1.844(4) . ? P3 C29 1.851(4) . ? P3 C17 1.867(3) . ? F1 C38 1.358(5) . ? F2 C39 1.353(4) . ? F3 C40 1.344(4) . ? F4 C41 1.348(4) . ? F5 C42 1.361(4) . ? F6 C44 1.353(5) . ? F7 C45 1.340(5) . ? F8 C46 1.346(4) . ? F9 C47 1.356(5) . ? F10 C48 1.354(5) . ? F11 C50 1.352(4) . ? F12 C51 1.345(5) . ? F13 C52 1.349(6) . ? F14 C53 1.351(5) . ? F15 C54 1.354(6) . ? F16 C56 1.334(7) . ? F17 C57 1.334(8) . ? F18 C58 1.344(6) . ? F19 C59 1.359(7) . ? F20 C60 1.360(7) . ? O1 C5 1.441(4) . ? O2 C7 1.438(8) . ? N1 C6 1.475(5) . ? N1 C8 1.489(5) . ? N1 H1B 0.9300 . ? N2 C35 1.143(5) . ? C1 C10 1.532(5) . ? C1 C9 1.534(5) . ? C1 H1A 1.0000 . ? C2 C11 1.523(5) . ? C2 C12 1.534(5) . ? C2 H2A 1.0000 . ? C3 C13 1.467(8) . ? C3 C14 1.543(8) . ? C3 H3A 1.0000 . ? C4 C15 1.542(7) . ? C4 C16 1.546(6) . ? C4 H4A 1.0000 . ? C5 C6 1.516(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.511(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.388(5) . ? C17 C22 1.400(5) . ? C18 C19 1.385(5) . ? C18 H18A 0.9500 . ? C19 C20 1.385(6) . ? C19 H19A 0.9500 . ? C20 C21 1.382(6) . ? C20 H20A 0.9500 . ? C21 C22 1.383(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.382(6) . ? C23 C24 1.395(6) . ? C24 C25 1.388(6) . ? C24 H24A 0.9500 . ? C25 C26 1.382(9) . ? C25 H25A 0.9500 . ? C26 C27 1.351(11) . ? C26 H26A 0.9500 . ? C27 C28 1.388(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.391(5) . ? C29 C34 1.402(5) . ? C30 C31 1.388(5) . ? C30 H30A 0.9500 . ? C31 C32 1.388(6) . ? C31 H31A 0.9500 . ? C32 C33 1.372(6) . ? C32 H32A 0.9500 . ? C33 C34 1.390(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.462(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.383(5) . ? C37 C38 1.390(5) . ? C37 B1 1.648(6) . ? C38 C39 1.375(6) . ? C39 C40 1.366(6) . ? C40 C41 1.370(6) . ? C41 C42 1.384(5) . ? C43 C48 1.387(6) . ? C43 C44 1.390(6) . ? C43 B1 1.658(6) . ? C44 C45 1.375(5) . ? C45 C46 1.376(6) . ? C46 C47 1.364(6) . ? C47 C48 1.386(6) . ? C49 C50 1.395(6) . ? C49 C54 1.396(6) . ? C49 B1 1.647(7) . ? C50 C51 1.371(6) . ? C51 C52 1.382(6) . ? C52 C53 1.367(8) . ? C53 C54 1.364(8) . ? C55 C60 1.379(7) . ? C55 C56 1.384(8) . ? C55 B1 1.668(6) . ? C56 C57 1.400(6) . ? C57 C58 1.361(10) . ? C58 C59 1.361(11) . ? C59 C60 1.387(8) . ? 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 N2 Ru1 N1 84.68(12) . . ? N2 Ru1 P3 93.81(8) . . ? N1 Ru1 P3 178.46(9) . . ? N2 Ru1 P1 98.17(8) . . ? N1 Ru1 P1 82.47(8) . . ? P3 Ru1 P1 97.44(3) . . ? N2 Ru1 P2 101.46(9) . . ? N1 Ru1 P2 86.54(9) . . ? P3 Ru1 P2 94.09(4) . . ? P1 Ru1 P2 156.46(4) . . ? N2 Ru1 H100 173.2(14) . . ? N1 Ru1 H100 88.7(14) . . ? P3 Ru1 H100 92.8(14) . . ? P1 Ru1 H100 79.5(14) . . ? P2 Ru1 H100 79.5(14) . . ? O1 P1 C2 95.16(15) . . ? O1 P1 C1 101.83(16) . . ? C2 P1 C1 105.66(17) . . ? O1 P1 Ru1 109.10(10) . . ? C2 P1 Ru1 122.09(13) . . ? C1 P1 Ru1 118.66(12) . . ? O2 P2 C4 103.3(2) . . ? O2 P2 C3 99.1(3) . . ? C4 P2 C3 102.6(2) . . ? O2 P2 Ru1 110.01(13) . . ? C4 P2 Ru1 126.98(15) . . ? C3 P2 Ru1 111.14(19) . . ? C23 P3 C29 101.14(17) . . ? C23 P3 C17 98.95(18) . . ? C29 P3 C17 102.03(15) . . ? C23 P3 Ru1 120.15(15) . . ? C29 P3 Ru1 114.41(12) . . ? C17 P3 Ru1 117.18(11) . . ? C5 O1 P1 120.2(2) . . ? C7 O2 P2 124.5(3) . . ? C6 N1 C8 110.5(3) . . ? C6 N1 Ru1 121.4(3) . . ? C8 N1 Ru1 114.3(2) . . ? C6 N1 H1B 102.5 . . ? C8 N1 H1B 102.5 . . ? Ru1 N1 H1B 102.5 . . ? C35 N2 Ru1 178.3(3) . . ? C10 C1 C9 108.9(3) . . ? C10 C1 P1 116.5(3) . . ? C9 C1 P1 111.7(3) . . ? C10 C1 H1A 106.4 . . ? C9 C1 H1A 106.4 . . ? P1 C1 H1A 106.4 . . ? C11 C2 C12 109.8(3) . . ? C11 C2 P1 112.4(3) . . ? C12 C2 P1 111.2(3) . . ? C11 C2 H2A 107.7 . . ? C12 C2 H2A 107.7 . . ? P1 C2 H2A 107.7 . . ? C13 C3 C14 112.2(5) . . ? C13 C3 P2 119.1(5) . . ? C14 C3 P2 106.0(5) . . ? C13 C3 H3A 106.2 . . ? C14 C3 H3A 106.2 . . ? P2 C3 H3A 106.2 . . ? C15 C4 C16 107.9(5) . . ? C15 C4 P2 111.7(3) . . ? C16 C4 P2 113.8(3) . . ? C15 C4 H4A 107.7 . . ? C16 C4 H4A 107.7 . . ? P2 C4 H4A 107.7 . . ? O1 C5 C6 111.3(4) . . ? O1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N1 C6 C5 112.3(3) . . ? N1 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? O2 C7 C8 116.8(4) . . ? O2 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? O2 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C7 113.5(5) . . ? N1 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 117.3(3) . . ? C18 C17 P3 121.4(3) . . ? C22 C17 P3 121.2(3) . . ? C19 C18 C17 121.7(3) . . ? C19 C18 H18A 119.2 . . ? C17 C18 H18A 119.2 . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 118.8(4) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C21 C22 C17 121.1(4) . . ? C21 C22 H22A 119.4 . . ? C17 C22 H22A 119.4 . . ? C28 C23 C24 118.2(4) . . ? C28 C23 P3 120.8(4) . . ? C24 C23 P3 121.0(3) . . ? C25 C24 C23 120.7(5) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C26 C25 C24 119.4(6) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C27 C26 C25 120.4(5) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 120.6(6) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C23 C28 C27 120.6(6) . . ? C23 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C34 117.0(3) . . ? C30 C29 P3 120.8(3) . . ? C34 C29 P3 122.1(3) . . ? C31 C30 C29 121.8(4) . . ? C31 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C33 C32 C31 119.6(4) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C34 120.4(4) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C33 C34 C29 121.3(4) . . ? C33 C34 H34A 119.3 . . ? C29 C34 H34A 119.3 . . ? N2 C35 C36 177.8(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 112.4(3) . . ? C42 C37 B1 128.3(3) . . ? C38 C37 B1 119.2(3) . . ? F1 C38 C39 115.9(4) . . ? F1 C38 C37 119.0(4) . . ? C39 C38 C37 125.1(4) . . ? F2 C39 C40 120.0(4) . . ? F2 C39 C38 120.6(4) . . ? C40 C39 C38 119.5(4) . . ? F3 C40 C39 120.8(4) . . ? F3 C40 C41 120.5(4) . . ? C39 C40 C41 118.7(4) . . ? F4 C41 C40 120.0(4) . . ? F4 C41 C42 120.3(4) . . ? C40 C41 C42 119.7(4) . . ? F5 C42 C37 120.7(3) . . ? F5 C42 C41 114.9(3) . . ? C37 C42 C41 124.5(4) . . ? C48 C43 C44 113.0(4) . . ? C48 C43 B1 127.7(4) . . ? C44 C43 B1 119.1(4) . . ? F6 C44 C45 116.2(4) . . ? F6 C44 C43 118.9(3) . . ? C45 C44 C43 124.9(4) . . ? F7 C45 C44 120.5(4) . . ? F7 C45 C46 120.1(4) . . ? C44 C45 C46 119.4(4) . . ? F8 C46 C47 120.9(4) . . ? F8 C46 C45 120.5(4) . . ? C47 C46 C45 118.6(4) . . ? F9 C47 C46 119.8(4) . . ? F9 C47 C48 119.8(4) . . ? C46 C47 C48 120.4(4) . . ? F10 C48 C47 115.2(4) . . ? F10 C48 C43 121.0(4) . . ? C47 C48 C43 123.8(4) . . ? C50 C49 C54 112.7(4) . . ? C50 C49 B1 119.5(3) . . ? C54 C49 B1 127.5(4) . . ? F11 C50 C51 116.3(4) . . ? F11 C50 C49 118.9(4) . . ? C51 C50 C49 124.8(4) . . ? F12 C51 C50 120.9(4) . . ? F12 C51 C52 119.8(4) . . ? C50 C51 C52 119.2(5) . . ? F13 C52 C53 121.6(5) . . ? F13 C52 C51 119.8(5) . . ? C53 C52 C51 118.6(5) . . ? F14 C53 C54 120.5(6) . . ? F14 C53 C52 119.1(6) . . ? C54 C53 C52 120.4(4) . . ? F15 C54 C53 115.0(4) . . ? F15 C54 C49 120.8(5) . . ? C53 C54 C49 124.2(5) . . ? C60 C55 C56 113.0(5) . . ? C60 C55 B1 119.0(5) . . ? C56 C55 B1 127.6(4) . . ? F16 C56 C55 121.8(4) . . ? F16 C56 C57 114.5(6) . . ? C55 C56 C57 123.8(6) . . ? F17 C57 C58 120.4(6) . . ? F17 C57 C56 119.5(6) . . ? C58 C57 C56 120.0(7) . . ? F18 C58 C57 120.4(8) . . ? F18 C58 C59 121.0(7) . . ? C57 C58 C59 118.6(5) . . ? F19 C59 C58 120.6(6) . . ? F19 C59 C60 119.5(8) . . ? C58 C59 C60 119.9(6) . . ? F20 C60 C55 119.0(5) . . ? F20 C60 C59 116.3(6) . . ? C55 C60 C59 124.7(7) . . ? C49 B1 C37 102.6(3) . . ? C49 B1 C43 113.8(4) . . ? C37 B1 C43 113.1(3) . . ? C49 B1 C55 113.7(4) . . ? C37 B1 C55 112.7(4) . . ? C43 B1 C55 101.5(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.293 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 933830' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs086_0m_Compound_14 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C17 H38 Cl N O3 P2 Ru' _chemical_formula_weight 502.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.4105(7) _cell_length_b 20.4109(8) _cell_length_c 15.1460(6) _cell_angle_alpha 90.00 _cell_angle_beta 126.0750(10) _cell_angle_gamma 90.00 _cell_volume 4600.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6868 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35094 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_unetI/netI 0.0220 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5287 _reflns_number_gt 4698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0192P)^2^+5.2099P] 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 5287 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _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 Ru1 Ru 0.313855(8) 0.230522(6) 0.829708(10) 0.01601(4) Uani 1 1 d . . . Cl1 Cl 0.37105(3) 0.24588(2) 1.02784(3) 0.02380(9) Uani 1 1 d . . . P1 P 0.29585(3) 0.11808(2) 0.83386(3) 0.01842(9) Uani 1 1 d . . . P2 P 0.32204(3) 0.33813(2) 0.78523(3) 0.01861(9) Uani 1 1 d . . . O1 O 0.19384(8) 0.09400(6) 0.78304(10) 0.0273(3) Uani 1 1 d . . . O2 O 0.25096(8) 0.39051(6) 0.77700(10) 0.0244(3) Uani 1 1 d . . . O3 O 0.49685(9) 0.21514(7) 0.88271(13) 0.0400(3) Uani 1 1 d . . . N1 N 0.18259(9) 0.24889(7) 0.80062(11) 0.0204(3) Uani 1 1 d . . . H1B H 0.1961 0.2473 0.8702 0.024 Uiso 1 1 calc R . . C1 C 0.35828(12) 0.07960(9) 0.97016(14) 0.0276(4) Uani 1 1 d . . . H1A H 0.3384 0.1031 1.0105 0.033 Uiso 1 1 calc R . . C2 C 0.31046(12) 0.06380(8) 0.74827(14) 0.0263(4) Uani 1 1 d . . . H2A H 0.3057 0.0177 0.7666 0.032 Uiso 1 1 calc R . . C3 C 0.42982(12) 0.38218(8) 0.87634(14) 0.0270(4) Uani 1 1 d . . . H3A H 0.4789 0.3520 0.8922 0.032 Uiso 1 1 calc R . . C4 C 0.29494(11) 0.34998(8) 0.64858(13) 0.0231(3) Uani 1 1 d . . . H4A H 0.3019 0.3977 0.6402 0.028 Uiso 1 1 calc R . . C5 C 0.13705(12) 0.13359(9) 0.79732(16) 0.0301(4) Uani 1 1 d . . . H5A H 0.1683 0.1418 0.8763 0.036 Uiso 1 1 calc R . . H5B H 0.0815 0.1088 0.7708 0.036 Uiso 1 1 calc R . . C6 C 0.11164(11) 0.19820(9) 0.73897(14) 0.0277(4) Uani 1 1 d . . . H6A H 0.0997 0.1919 0.6667 0.033 Uiso 1 1 calc R . . H6B H 0.0555 0.2140 0.7266 0.033 Uiso 1 1 calc R . . C7 C 0.20230(12) 0.37062(9) 0.81987(15) 0.0284(4) Uani 1 1 d . . . H7A H 0.1670 0.4083 0.8168 0.034 Uiso 1 1 calc R . . H7B H 0.2458 0.3582 0.8975 0.034 Uiso 1 1 calc R . . C8 C 0.13950(11) 0.31383(9) 0.75860(15) 0.0269(4) Uani 1 1 d . . . H8A H 0.0881 0.3171 0.7630 0.032 Uiso 1 1 calc R . . H8B H 0.1155 0.3171 0.6806 0.032 Uiso 1 1 calc R . . C9 C 0.45963(13) 0.08970(10) 1.03762(15) 0.0380(5) Uani 1 1 d . . . H9A H 0.4885 0.0682 1.1087 0.057 Uiso 1 1 calc R . . H9B H 0.4731 0.1367 1.0486 0.057 Uiso 1 1 calc R . . H9C H 0.4825 0.0707 0.9990 0.057 Uiso 1 1 calc R . . C10 C 0.33440(17) 0.00782(10) 0.96795(17) 0.0472(6) Uani 1 1 d . . . H10A H 0.3697 -0.0094 1.0427 0.071 Uiso 1 1 calc R . . H10B H 0.3479 -0.0173 0.9242 0.071 Uiso 1 1 calc R . . H10C H 0.2702 0.0041 0.9356 0.071 Uiso 1 1 calc R . . C11 C 0.23518(14) 0.07425(11) 0.62728(15) 0.0399(5) Uani 1 1 d . . . H11A H 0.2440 0.0447 0.5833 0.060 Uiso 1 1 calc R . . H11B H 0.2362 0.1198 0.6074 0.060 Uiso 1 1 calc R . . H11C H 0.1771 0.0650 0.6136 0.060 Uiso 1 1 calc R . . C12 C 0.40163(14) 0.07081(12) 0.76817(18) 0.0432(5) Uani 1 1 d . . . H12A H 0.4050 0.0404 0.7207 0.065 Uiso 1 1 calc R . . H12B H 0.4496 0.0607 0.8447 0.065 Uiso 1 1 calc R . . H12C H 0.4088 0.1158 0.7519 0.065 Uiso 1 1 calc R . . C13 C 0.44426(14) 0.39661(10) 0.98471(15) 0.0384(5) Uani 1 1 d . . . H13A H 0.5016 0.4195 1.0337 0.058 Uiso 1 1 calc R . . H13B H 0.4453 0.3554 1.0186 0.058 Uiso 1 1 calc R . . H13C H 0.3951 0.4242 0.9714 0.058 Uiso 1 1 calc R . . C14 C 0.43873(14) 0.44528(10) 0.82885(17) 0.0371(5) Uani 1 1 d . . . H14A H 0.4980 0.4647 0.8817 0.056 Uiso 1 1 calc R . . H14B H 0.3919 0.4763 0.8134 0.056 Uiso 1 1 calc R . . H14C H 0.4320 0.4352 0.7611 0.056 Uiso 1 1 calc R . . C15 C 0.36105(13) 0.31270(10) 0.63710(15) 0.0319(4) Uani 1 1 d . . . H15A H 0.3454 0.3197 0.5637 0.048 Uiso 1 1 calc R . . H15B H 0.3580 0.2658 0.6485 0.048 Uiso 1 1 calc R . . H15C H 0.4222 0.3287 0.6917 0.048 Uiso 1 1 calc R . . C16 C 0.19774(12) 0.33114(9) 0.55818(14) 0.0288(4) Uani 1 1 d . . . H16A H 0.1861 0.3377 0.4868 0.043 Uiso 1 1 calc R . . H16B H 0.1568 0.3586 0.5635 0.043 Uiso 1 1 calc R . . H16C H 0.1880 0.2850 0.5663 0.043 Uiso 1 1 calc R . . C17 C 0.42549(12) 0.21934(8) 0.86090(14) 0.0236(4) Uani 1 1 d . . . H38 H 0.2669(12) 0.2173(9) 0.7070(15) 0.026(5) Uiso 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 Ru1 0.01295(7) 0.01656(7) 0.01621(6) 0.00010(5) 0.00730(5) 0.00119(5) Cl1 0.02011(19) 0.0298(2) 0.01785(18) -0.00240(15) 0.00918(16) 0.00003(16) P1 0.0179(2) 0.0181(2) 0.01823(19) -0.00094(15) 0.01012(17) -0.00189(16) P2 0.0165(2) 0.0162(2) 0.01970(19) -0.00048(15) 0.00876(17) 0.00162(15) O1 0.0210(6) 0.0271(7) 0.0336(7) -0.0106(5) 0.0160(5) -0.0074(5) O2 0.0250(6) 0.0187(6) 0.0303(6) 0.0031(5) 0.0167(5) 0.0060(5) O3 0.0230(7) 0.0358(8) 0.0626(10) 0.0101(7) 0.0261(7) 0.0071(6) N1 0.0148(6) 0.0254(7) 0.0187(6) 0.0005(5) 0.0086(6) 0.0023(6) C1 0.0341(10) 0.0233(9) 0.0219(8) 0.0010(7) 0.0145(8) -0.0048(8) C2 0.0348(10) 0.0195(9) 0.0284(9) -0.0023(7) 0.0207(8) -0.0004(7) C3 0.0200(8) 0.0190(9) 0.0315(9) -0.0039(7) 0.0094(7) -0.0018(7) C4 0.0233(9) 0.0214(9) 0.0228(8) 0.0028(6) 0.0126(7) 0.0010(7) C5 0.0238(9) 0.0338(10) 0.0381(10) -0.0088(8) 0.0213(8) -0.0083(8) C6 0.0138(8) 0.0362(10) 0.0279(9) -0.0059(8) 0.0094(7) -0.0027(7) C7 0.0318(10) 0.0270(10) 0.0334(9) 0.0039(7) 0.0230(8) 0.0118(8) C8 0.0199(8) 0.0305(10) 0.0306(9) 0.0089(7) 0.0150(7) 0.0099(7) C9 0.0331(11) 0.0306(11) 0.0279(9) 0.0058(8) 0.0054(8) 0.0005(8) C10 0.0625(15) 0.0323(11) 0.0350(11) 0.0063(9) 0.0222(11) -0.0153(10) C11 0.0428(12) 0.0519(13) 0.0260(9) -0.0105(9) 0.0208(9) -0.0045(10) C12 0.0395(12) 0.0533(14) 0.0436(12) -0.0080(10) 0.0283(10) 0.0082(10) C13 0.0374(11) 0.0289(10) 0.0273(9) -0.0061(8) 0.0070(9) -0.0096(9) C14 0.0351(11) 0.0281(10) 0.0426(11) -0.0051(8) 0.0198(9) -0.0105(8) C15 0.0329(10) 0.0378(11) 0.0303(9) 0.0024(8) 0.0216(8) 0.0037(8) C16 0.0272(9) 0.0319(10) 0.0200(8) 0.0042(7) 0.0098(7) 0.0011(8) C17 0.0233(9) 0.0172(8) 0.0279(8) 0.0035(6) 0.0137(7) 0.0019(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 Ru1 C17 1.8319(18) . ? Ru1 N1 2.2184(14) . ? Ru1 P1 2.3249(4) . ? Ru1 P2 2.3282(4) . ? Ru1 Cl1 2.5477(4) . ? Ru1 H38 1.543(18) . ? P1 O1 1.6306(12) . ? P1 C2 1.8416(17) . ? P1 C1 1.8454(17) . ? P2 O2 1.6366(12) . ? P2 C4 1.8372(17) . ? P2 C3 1.8508(17) . ? O1 C5 1.435(2) . ? O2 C7 1.440(2) . ? O3 C17 1.154(2) . ? N1 C8 1.482(2) . ? N1 C6 1.487(2) . ? N1 H1B 0.9300 . ? C1 C9 1.524(3) . ? C1 C10 1.524(3) . ? C1 H1A 1.0000 . ? C2 C12 1.527(3) . ? C2 C11 1.527(3) . ? C2 H2A 1.0000 . ? C3 C13 1.529(3) . ? C3 C14 1.530(3) . ? C3 H3A 1.0000 . ? C4 C16 1.529(2) . ? C4 C15 1.530(2) . ? C4 H4A 1.0000 . ? C5 C6 1.501(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.509(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 C17 Ru1 N1 176.25(7) . . ? C17 Ru1 P1 91.51(5) . . ? N1 Ru1 P1 90.93(4) . . ? C17 Ru1 P2 86.46(5) . . ? N1 Ru1 P2 91.81(4) . . ? P1 Ru1 P2 166.818(15) . . ? C17 Ru1 Cl1 95.09(6) . . ? N1 Ru1 Cl1 81.92(4) . . ? P1 Ru1 Cl1 93.221(14) . . ? P2 Ru1 Cl1 99.930(15) . . ? C17 Ru1 H38 92.1(7) . . ? N1 Ru1 H38 91.0(7) . . ? P1 Ru1 H38 82.6(7) . . ? P2 Ru1 H38 84.4(7) . . ? Cl1 Ru1 H38 171.8(7) . . ? O1 P1 C2 95.24(7) . . ? O1 P1 C1 100.68(8) . . ? C2 P1 C1 106.17(8) . . ? O1 P1 Ru1 115.33(5) . . ? C2 P1 Ru1 119.51(6) . . ? C1 P1 Ru1 116.46(6) . . ? O2 P2 C4 98.84(7) . . ? O2 P2 C3 101.40(7) . . ? C4 P2 C3 103.69(8) . . ? O2 P2 Ru1 116.95(5) . . ? C4 P2 Ru1 115.42(6) . . ? C3 P2 Ru1 117.79(6) . . ? C5 O1 P1 119.86(11) . . ? C7 O2 P2 117.60(10) . . ? C8 N1 C6 107.60(13) . . ? C8 N1 Ru1 118.78(11) . . ? C6 N1 Ru1 117.28(10) . . ? C8 N1 H1B 103.7 . . ? C6 N1 H1B 103.7 . . ? Ru1 N1 H1B 103.7 . . ? C9 C1 C10 111.60(17) . . ? C9 C1 P1 113.74(13) . . ? C10 C1 P1 113.76(13) . . ? C9 C1 H1A 105.6 . . ? C10 C1 H1A 105.6 . . ? P1 C1 H1A 105.6 . . ? C12 C2 C11 109.82(16) . . ? C12 C2 P1 113.82(13) . . ? C11 C2 P1 110.79(13) . . ? C12 C2 H2A 107.4 . . ? C11 C2 H2A 107.4 . . ? P1 C2 H2A 107.4 . . ? C13 C3 C14 110.09(15) . . ? C13 C3 P2 109.04(13) . . ? C14 C3 P2 115.02(13) . . ? C13 C3 H3A 107.5 . . ? C14 C3 H3A 107.5 . . ? P2 C3 H3A 107.5 . . ? C16 C4 C15 111.29(15) . . ? C16 C4 P2 111.95(12) . . ? C15 C4 P2 110.87(12) . . ? C16 C4 H4A 107.5 . . ? C15 C4 H4A 107.5 . . ? P2 C4 H4A 107.5 . . ? O1 C5 C6 114.10(15) . . ? O1 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? O1 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N1 C6 C5 112.81(14) . . ? N1 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 C8 113.20(14) . . ? O2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? O2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C7 113.59(14) . . ? N1 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 Ru1 176.84(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.413 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.055 _database_code_depnum_ccdc_archive 'CCDC 933831' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mjs088_0m_Compound_16 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C23 H43 Cl2 F6 N O3 P3 Ru S' _chemical_formula_weight 792.52 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8302(15) _cell_length_b 13.451(2) _cell_length_c 15.359(2) _cell_angle_alpha 81.154(7) _cell_angle_beta 74.718(7) _cell_angle_gamma 74.475(7) _cell_volume 1688.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5384 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.07 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 0.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6614 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22788 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_unetI/netI 0.0614 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5897 _reflns_number_gt 4520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1823P)^2^+7.1002P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5897 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.2672 _refine_ls_wR_factor_gt 0.2465 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _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 Ru1 Ru 0.85176(8) 0.74612(5) 0.73642(4) 0.0213(3) Uani 1 1 d . . . P1 P 0.8349(3) 0.71929(17) 0.59131(14) 0.0256(5) Uani 1 1 d . . . P2 P 0.8192(3) 0.75371(18) 0.89293(14) 0.0275(5) Uani 1 1 d . . . P3 P 0.0550(3) 0.79130(19) 0.20047(16) 0.0354(6) Uani 1 1 d . . . S1 S 1.0443(3) 0.58806(19) 0.74989(19) 0.0456(7) Uani 1 1 d . . . Cl1 Cl 0.4603(5) 0.4992(3) 0.8464(3) 0.0871(11) Uani 1 1 d . . . N1 N 0.6730(8) 0.8900(6) 0.7321(5) 0.0277(16) Uani 1 1 d . . . Cl2 Cl 0.4567(6) 0.3803(4) 0.7048(4) 0.1149(18) Uani 1 1 d . . . O1 O 0.8933(8) 0.6007(5) 0.5647(4) 0.0354(15) Uani 1 1 d . . . F1 F -0.0315(9) 0.8669(5) 0.1295(4) 0.0600(18) Uani 1 1 d . . . F2 F -0.0264(10) 0.8778(6) 0.2699(4) 0.078(2) Uani 1 1 d . . . F4 F 0.1386(8) 0.7066(5) 0.1309(5) 0.0604(17) Uani 1 1 d . . . O2 O 0.8305(9) 0.6416(5) 0.9514(4) 0.0452(18) Uani 1 1 d . . . C22 C 0.7115(11) 0.9831(7) 0.7215(5) 0.0284(19) Uani 1 1 d . . . H22A H 0.8216 0.9838 0.7136 0.034 Uiso 1 1 calc R . . C3 C 0.9674(11) 0.7961(7) 0.9330(6) 0.031(2) Uani 1 1 d . . . H3A H 0.9364 0.7882 1.0008 0.038 Uiso 1 1 calc R . . C18 C 0.5160(10) 0.8920(8) 0.7446(6) 0.036(2) Uani 1 1 d . . . H18A H 0.4854 0.8280 0.7531 0.043 Uiso 1 1 calc R . . F6 F 0.2059(8) 0.8403(6) 0.1663(6) 0.077(2) Uani 1 1 d . . . C2 C 0.6298(12) 0.7528(9) 0.5695(7) 0.046(3) Uani 1 1 d . . . H2A H 0.5747 0.8243 0.5876 0.056 Uiso 1 1 calc R . . C17 C 1.0273(11) 0.8123(7) 0.6978(6) 0.0292(19) Uani 1 1 d . . . C19 C 0.3967(12) 0.9829(8) 0.7457(7) 0.043(2) Uani 1 1 d . . . H19A H 0.2870 0.9808 0.7541 0.051 Uiso 1 1 calc R . . F3 F 0.1382(11) 0.7163(7) 0.2732(5) 0.100(3) Uani 1 1 d . . . C21 C 0.5994(12) 1.0759(7) 0.7218(6) 0.038(2) Uani 1 1 d . . . H21A H 0.6319 1.1393 0.7133 0.045 Uiso 1 1 calc R . . C14 C 1.1353(12) 0.7253(9) 0.9039(7) 0.046(3) Uani 1 1 d . . . H14A H 1.2133 0.7487 0.9261 0.070 Uiso 1 1 calc R . . H14B H 1.1672 0.7277 0.8377 0.070 Uiso 1 1 calc R . . H14C H 1.1333 0.6541 0.9294 0.070 Uiso 1 1 calc R . . F5 F -0.0947(9) 0.7412(6) 0.2325(8) 0.121(4) Uani 1 1 d . . . C5 C 0.9144(13) 0.5121(7) 0.6334(7) 0.042(2) Uani 1 1 d . . . H5A H 0.9203 0.4478 0.6075 0.050 Uiso 1 1 calc R . . H5B H 0.8203 0.5222 0.6859 0.050 Uiso 1 1 calc R . . C13 C 0.9639(14) 0.9111(8) 0.9042(7) 0.043(2) Uani 1 1 d . . . H13A H 1.0447 0.9306 0.9270 0.065 Uiso 1 1 calc R . . H13B H 0.8563 0.9534 0.9293 0.065 Uiso 1 1 calc R . . H13C H 0.9885 0.9225 0.8379 0.065 Uiso 1 1 calc R . . C6 C 1.0638(13) 0.5019(8) 0.6636(7) 0.046(3) Uani 1 1 d . . . H6A H 1.1492 0.5160 0.6102 0.056 Uiso 1 1 calc R . . H6B H 1.0999 0.4294 0.6882 0.056 Uiso 1 1 calc R . . C20 C 0.4385(12) 1.0763(8) 0.7344(6) 0.043(3) Uani 1 1 d . . . H20A H 0.3585 1.1396 0.7354 0.051 Uiso 1 1 calc R . . C1 C 0.9573(14) 0.7770(8) 0.4922(6) 0.047(3) Uani 1 1 d . . . H1A H 0.9336 0.7583 0.4374 0.057 Uiso 1 1 calc R . . O3 O 1.1371(8) 0.8482(6) 0.6760(5) 0.0424(16) Uani 1 1 d . . . C4 C 0.6232(12) 0.8306(11) 0.9525(6) 0.051(3) Uani 1 1 d . . . H4A H 0.5990 0.8979 0.9148 0.061 Uiso 1 1 calc R . . C12 C 0.5302(13) 0.6786(11) 0.6268(8) 0.058(3) Uani 1 1 d . . . H12A H 0.4221 0.6977 0.6146 0.087 Uiso 1 1 calc R . . H12B H 0.5210 0.6829 0.6911 0.087 Uiso 1 1 calc R . . H12C H 0.5836 0.6076 0.6113 0.087 Uiso 1 1 calc R . . C10 C 1.1392(15) 0.7331(13) 0.4866(7) 0.071(4) Uani 1 1 d . . . H10A H 1.2015 0.7653 0.4323 0.106 Uiso 1 1 calc R . . H10B H 1.1661 0.6580 0.4833 0.106 Uiso 1 1 calc R . . H10C H 1.1657 0.7480 0.5405 0.106 Uiso 1 1 calc R . . C16 C 0.6176(14) 0.8568(12) 1.0484(7) 0.067(4) Uani 1 1 d . . . H16A H 0.5096 0.8979 1.0745 0.101 Uiso 1 1 calc R . . H16B H 0.6979 0.8966 1.0439 0.101 Uiso 1 1 calc R . . H16C H 0.6419 0.7925 1.0872 0.101 Uiso 1 1 calc R . . C15 C 0.4901(14) 0.7754(14) 0.9570(8) 0.080(5) Uani 1 1 d . . . H15A H 0.3858 0.8165 0.9883 0.121 Uiso 1 1 calc R . . H15B H 0.5137 0.7070 0.9903 0.121 Uiso 1 1 calc R . . H15C H 0.4857 0.7675 0.8955 0.121 Uiso 1 1 calc R . . C7 C 0.825(2) 0.5535(9) 0.9120(8) 0.072(5) Uani 1 1 d . . . H7A H 0.7406 0.5750 0.8768 0.087 Uiso 1 1 calc R . . H7B H 0.7926 0.5012 0.9613 0.087 Uiso 1 1 calc R . . C8 C 0.980(2) 0.5045(9) 0.8516(9) 0.092(6) Uani 1 1 d . . . H8A H 0.9689 0.4401 0.8328 0.111 Uiso 1 1 calc R . . H8B H 1.0655 0.4849 0.8861 0.111 Uiso 1 1 calc R . . C9 C 0.911(2) 0.8943(10) 0.4901(8) 0.090(6) Uani 1 1 d . . . H9A H 0.9773 0.9238 0.4360 0.135 Uiso 1 1 calc R . . H9B H 0.9278 0.9152 0.5444 0.135 Uiso 1 1 calc R . . H9C H 0.7963 0.9197 0.4885 0.135 Uiso 1 1 calc R . . C11 C 0.6297(16) 0.7511(13) 0.4702(8) 0.072(4) Uani 1 1 d . . . H11A H 0.5181 0.7694 0.4634 0.108 Uiso 1 1 calc R . . H11B H 0.6832 0.6815 0.4510 0.108 Uiso 1 1 calc R . . H11C H 0.6879 0.8011 0.4326 0.108 Uiso 1 1 calc R . . C23 C 0.490(3) 0.3823(15) 0.8069(12) 0.144(10) Uani 1 1 d . . . H23B H 0.6038 0.3445 0.8054 0.172 Uiso 1 1 calc R . . H23A H 0.4205 0.3425 0.8517 0.172 Uiso 1 1 calc R . . 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 0.0286(4) 0.0215(4) 0.0160(4) -0.0029(2) -0.0061(3) -0.0080(3) P1 0.0336(12) 0.0268(12) 0.0183(11) -0.0065(9) -0.0078(9) -0.0059(9) P2 0.0338(12) 0.0365(13) 0.0182(11) -0.0020(9) -0.0078(9) -0.0169(10) P3 0.0441(14) 0.0321(14) 0.0252(12) -0.0004(10) -0.0086(10) -0.0019(11) S1 0.0639(17) 0.0241(13) 0.0577(17) -0.0078(11) -0.0389(14) 0.0009(11) Cl1 0.112(3) 0.073(3) 0.090(3) 0.001(2) -0.039(2) -0.035(2) N1 0.033(4) 0.029(4) 0.020(4) -0.008(3) -0.005(3) -0.004(3) Cl2 0.115(3) 0.095(3) 0.153(4) -0.055(3) -0.091(3) 0.028(3) O1 0.046(4) 0.032(4) 0.030(3) -0.010(3) -0.013(3) -0.004(3) F1 0.095(5) 0.039(3) 0.058(4) 0.000(3) -0.052(4) -0.004(3) F2 0.099(6) 0.071(5) 0.038(4) -0.018(3) -0.019(4) 0.033(4) F4 0.070(4) 0.047(4) 0.064(4) -0.024(3) -0.015(3) -0.004(3) O2 0.089(5) 0.044(4) 0.021(3) 0.009(3) -0.024(3) -0.041(4) C22 0.043(5) 0.030(5) 0.014(4) 0.000(3) -0.008(3) -0.011(4) C3 0.047(5) 0.029(5) 0.025(4) 0.002(4) -0.014(4) -0.017(4) C18 0.028(5) 0.046(6) 0.034(5) -0.013(4) -0.005(4) -0.008(4) F6 0.052(4) 0.072(5) 0.118(6) -0.036(5) -0.018(4) -0.021(4) C2 0.039(5) 0.058(7) 0.048(6) -0.028(5) -0.023(5) 0.005(5) C17 0.033(5) 0.033(5) 0.022(4) -0.013(4) -0.004(4) -0.005(4) C19 0.034(5) 0.052(7) 0.039(6) -0.016(5) -0.011(4) 0.005(5) F3 0.124(7) 0.084(6) 0.043(4) 0.005(4) -0.027(4) 0.056(5) C21 0.057(6) 0.023(5) 0.032(5) -0.007(4) -0.016(4) -0.001(4) C14 0.036(5) 0.066(7) 0.045(6) -0.006(5) -0.023(5) -0.013(5) F5 0.047(4) 0.038(4) 0.234(13) 0.021(6) 0.018(5) -0.006(3) C5 0.065(7) 0.019(5) 0.042(6) -0.007(4) -0.015(5) -0.008(4) C13 0.070(7) 0.034(6) 0.034(5) -0.005(4) -0.014(5) -0.025(5) C6 0.062(7) 0.026(5) 0.051(6) -0.009(4) -0.024(5) 0.003(5) C20 0.050(6) 0.041(6) 0.033(5) -0.020(4) -0.015(4) 0.013(5) C1 0.079(8) 0.048(6) 0.019(5) -0.004(4) -0.002(5) -0.032(6) O3 0.036(4) 0.052(4) 0.044(4) -0.013(3) -0.004(3) -0.020(3) C4 0.043(6) 0.090(9) 0.022(5) -0.017(5) -0.002(4) -0.019(6) C12 0.041(6) 0.084(9) 0.061(7) -0.026(7) -0.016(5) -0.020(6) C10 0.074(8) 0.122(13) 0.031(6) -0.014(7) 0.006(5) -0.061(9) C16 0.056(7) 0.123(12) 0.026(6) -0.034(7) 0.004(5) -0.026(7) C15 0.041(6) 0.182(17) 0.034(6) -0.023(8) 0.003(5) -0.060(9) C7 0.163(14) 0.044(7) 0.047(7) 0.025(6) -0.053(8) -0.075(9) C8 0.217(19) 0.020(6) 0.051(8) 0.001(5) -0.063(10) -0.017(8) C9 0.200(18) 0.062(9) 0.022(6) 0.010(5) -0.014(8) -0.074(11) C11 0.069(8) 0.115(12) 0.035(6) -0.013(7) -0.024(6) -0.013(8) C23 0.24(3) 0.078(13) 0.081(13) -0.015(10) -0.074(15) 0.048(15) _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 C17 1.908(9) . ? Ru1 N1 2.150(7) . ? Ru1 P2 2.359(2) . ? Ru1 S1 2.360(3) . ? Ru1 P1 2.360(2) . ? P1 O1 1.621(6) . ? P1 C1 1.819(10) . ? P1 C2 1.853(9) . ? P2 O2 1.625(7) . ? P2 C3 1.830(9) . ? P2 C4 1.845(11) . ? P3 F5 1.573(8) . ? P3 F6 1.575(7) . ? P3 F1 1.578(6) . ? P3 F4 1.579(7) . ? P3 F3 1.579(7) . ? P3 F2 1.592(7) . ? S1 C8 1.832(14) . ? S1 C6 1.837(10) . ? Cl1 C23 1.70(2) . ? N1 C18 1.342(11) . ? N1 C22 1.358(11) . ? Cl2 C23 1.676(18) . ? O1 C5 1.472(11) . ? O2 C7 1.428(13) . ? C22 C21 1.371(13) . ? C22 H22A 0.9500 . ? C3 C14 1.526(14) . ? C3 C13 1.536(13) . ? C3 H3A 1.0000 . ? C18 C19 1.383(14) . ? C18 H18A 0.9500 . ? C2 C12 1.528(17) . ? C2 C11 1.530(14) . ? C2 H2A 1.0000 . ? C17 O3 1.147(11) . ? C19 C20 1.375(16) . ? C19 H19A 0.9500 . ? C21 C20 1.381(14) . ? C21 H21A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C5 C6 1.477(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C20 H20A 0.9500 . ? C1 C9 1.517(17) . ? C1 C10 1.540(18) . ? C1 H1A 1.0000 . ? C4 C15 1.531(16) . ? C4 C16 1.551(13) . ? C4 H4A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C7 C8 1.49(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C23 H23B 0.9900 . ? C23 H23A 0.9900 . ? 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 C17 Ru1 N1 93.1(3) . . ? C17 Ru1 P2 95.9(2) . . ? N1 Ru1 P2 89.77(19) . . ? C17 Ru1 S1 87.7(3) . . ? N1 Ru1 S1 176.85(19) . . ? P2 Ru1 S1 87.11(9) . . ? C17 Ru1 P1 97.3(2) . . ? N1 Ru1 P1 89.68(18) . . ? P2 Ru1 P1 166.81(8) . . ? S1 Ru1 P1 93.25(8) . . ? O1 P1 C1 98.1(4) . . ? O1 P1 C2 99.1(4) . . ? C1 P1 C2 104.8(5) . . ? O1 P1 Ru1 116.5(2) . . ? C1 P1 Ru1 118.7(3) . . ? C2 P1 Ru1 116.5(3) . . ? O2 P2 C3 98.3(4) . . ? O2 P2 C4 102.3(5) . . ? C3 P2 C4 103.7(5) . . ? O2 P2 Ru1 113.8(3) . . ? C3 P2 Ru1 120.0(3) . . ? C4 P2 Ru1 116.0(3) . . ? F5 P3 F6 178.7(6) . . ? F5 P3 F1 89.2(5) . . ? F6 P3 F1 90.4(4) . . ? F5 P3 F4 89.3(5) . . ? F6 P3 F4 89.4(4) . . ? F1 P3 F4 92.2(4) . . ? F5 P3 F3 90.1(6) . . ? F6 P3 F3 90.4(5) . . ? F1 P3 F3 178.8(4) . . ? F4 P3 F3 88.7(4) . . ? F5 P3 F2 91.8(5) . . ? F6 P3 F2 89.4(5) . . ? F1 P3 F2 87.7(4) . . ? F4 P3 F2 178.8(5) . . ? F3 P3 F2 91.4(4) . . ? C8 S1 C6 98.9(5) . . ? C8 S1 Ru1 112.9(6) . . ? C6 S1 Ru1 112.6(3) . . ? C18 N1 C22 116.7(8) . . ? C18 N1 Ru1 121.3(6) . . ? C22 N1 Ru1 122.0(6) . . ? C5 O1 P1 121.9(5) . . ? C7 O2 P2 120.4(6) . . ? N1 C22 C21 123.3(9) . . ? N1 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? C14 C3 C13 112.8(8) . . ? C14 C3 P2 110.4(6) . . ? C13 C3 P2 112.0(6) . . ? C14 C3 H3A 107.1 . . ? C13 C3 H3A 107.1 . . ? P2 C3 H3A 107.1 . . ? N1 C18 C19 123.0(9) . . ? N1 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C12 C2 C11 108.2(10) . . ? C12 C2 P1 110.6(8) . . ? C11 C2 P1 113.6(8) . . ? C12 C2 H2A 108.1 . . ? C11 C2 H2A 108.1 . . ? P1 C2 H2A 108.1 . . ? O3 C17 Ru1 176.9(8) . . ? C20 C19 C18 119.3(9) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C22 C21 C20 119.1(9) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C5 C6 110.3(8) . . ? O1 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? O1 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C6 S1 114.8(7) . . ? C5 C6 H6A 108.6 . . ? S1 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? S1 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C19 C20 C21 118.6(9) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? C9 C1 C10 111.9(11) . . ? C9 C1 P1 110.8(8) . . ? C10 C1 P1 111.6(8) . . ? C9 C1 H1A 107.4 . . ? C10 C1 H1A 107.4 . . ? P1 C1 H1A 107.4 . . ? C15 C4 C16 110.3(9) . . ? C15 C4 P2 109.4(9) . . ? C16 C4 P2 115.2(8) . . ? C15 C4 H4A 107.2 . . ? C16 C4 H4A 107.2 . . ? P2 C4 H4A 107.2 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C7 C8 114.4(11) . . ? O2 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? O2 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 S1 113.6(9) . . ? C7 C8 H8A 108.8 . . ? S1 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? S1 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Cl2 C23 Cl1 118.4(10) . . ? Cl2 C23 H23B 107.7 . . ? Cl1 C23 H23B 107.7 . . ? Cl2 C23 H23A 107.7 . . ? Cl1 C23 H23A 107.7 . . ? H23B C23 H23A 107.1 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.477 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.247 _database_code_depnum_ccdc_archive 'CCDC 933832'