# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Werner Thiel' _publ_contact_author_email THIEL@CHEMIE.UNI-KL.DE _publ_section_title ; A facile access to a novel two dentate enatiomerically pure P,N-donor ligand ; loop_ _publ_author_name 'Werner Thiel' 'Christoph K. Seubert' 'Yu Sun' # Attachment 'Compound5.cif' data_0811o _database_code_depnum_ccdc_archive 'CCDC 713118' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Cl2 N3 O3 P Pd' _chemical_formula_weight 706.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.0871(3) _cell_length_b 13.8105(5) _cell_length_c 13.5808(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.325(3) _cell_angle_gamma 90.00 _cell_volume 1492.24(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9756 _cell_measurement_theta_min 4.5842 _cell_measurement_theta_max 62.7430 _exptl_crystal_description 'transparent block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 7.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58696 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S Ultra' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16618 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.60 _diffrn_reflns_theta_max 62.83 _reflns_number_total 4115 _reflns_number_gt 3904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(5) _refine_ls_number_reflns 4115 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.1471(5) 0.8804(3) 0.6970(3) 0.0361(10) Uani 1 1 d . . . H1 H 0.1174 0.9364 0.7305 0.043 Uiso 1 1 calc R . . C2 C 0.0715(5) 0.7916(3) 0.6962(3) 0.0356(9) Uani 1 1 d . . . H2 H -0.0196 0.7742 0.7281 0.043 Uiso 1 1 calc R . . C3 C 0.1562(3) 0.7318(4) 0.63865(19) 0.0250(6) Uani 1 1 d . . . C4 C 0.3710(5) 0.9542(3) 0.6161(3) 0.0374(9) Uani 1 1 d . . . H4A H 0.3016 0.9961 0.5670 0.056 Uiso 1 1 calc R . . H4B H 0.4640 0.9277 0.5871 0.056 Uiso 1 1 calc R . . H4C H 0.4161 0.9919 0.6760 0.056 Uiso 1 1 calc R . . C5 C 0.1322(4) 0.6294(3) 0.6153(2) 0.0251(8) Uani 1 1 d . . . C6 C 0.1375(4) 0.5902(3) 0.5217(2) 0.0254(7) Uani 1 1 d . . . C7 C 0.1199(5) 0.4923(3) 0.5019(3) 0.0357(9) Uani 1 1 d . . . H7 H 0.1293 0.4677 0.4378 0.043 Uiso 1 1 calc R . . C8 C 0.0883(5) 0.4304(3) 0.5767(3) 0.0423(10) Uani 1 1 d . . . H8 H 0.0757 0.3629 0.5643 0.051 Uiso 1 1 calc R . . C9 C 0.0752(5) 0.4677(3) 0.6697(3) 0.0388(10) Uani 1 1 d . . . H9 H 0.0505 0.4258 0.7206 0.047 Uiso 1 1 calc R . . C10 C 0.0978(5) 0.5661(3) 0.6890(3) 0.0321(10) Uani 1 1 d . . . H10 H 0.0897 0.5906 0.7533 0.038 Uiso 1 1 calc R . . C11 C 0.2690(4) 0.6237(3) 0.2453(3) 0.0250(8) Uani 1 1 d . . . C12 C 0.2299(4) 0.6984(3) 0.1797(2) 0.0247(8) Uani 1 1 d . . . C13 C 0.1034(4) 0.6793(3) 0.0914(2) 0.0262(7) Uani 1 1 d . . . C14 C 0.0405(5) 0.5830(3) 0.0738(3) 0.0289(8) Uani 1 1 d . . . C15 C 0.0981(5) 0.5099(3) 0.1428(3) 0.0308(8) Uani 1 1 d . . . H15 H 0.0591 0.4455 0.1293 0.037 Uiso 1 1 calc R . . C16 C 0.2084(4) 0.5286(3) 0.2287(2) 0.0280(8) Uani 1 1 d . . . H16 H 0.2436 0.4788 0.2760 0.034 Uiso 1 1 calc R . . C17 C 0.0341(4) 0.7539(3) 0.0255(2) 0.0305(9) Uani 1 1 d . . . H17 H 0.0725 0.8186 0.0376 0.037 Uiso 1 1 calc R . . C18 C -0.0885(4) 0.7336(4) -0.0560(2) 0.0359(7) Uani 1 1 d . . . H18 H -0.1349 0.7845 -0.0994 0.043 Uiso 1 1 calc R . . C19 C -0.1459(5) 0.6383(3) -0.0757(3) 0.0397(10) Uani 1 1 d . . . H19 H -0.2280 0.6248 -0.1334 0.048 Uiso 1 1 calc R . . C20 C -0.0844(5) 0.5655(3) -0.0125(3) 0.0362(9) Uani 1 1 d . . . H20 H -0.1256 0.5016 -0.0261 0.043 Uiso 1 1 calc R . . C21 C 0.3019(4) 0.8401(3) 0.2901(3) 0.0250(8) Uani 1 1 d . . . C22 C 0.3075(4) 0.7956(3) 0.2004(2) 0.0243(8) Uani 1 1 d . . . C23 C 0.3955(4) 0.8446(3) 0.1319(3) 0.0296(8) Uani 1 1 d . . . C24 C 0.4635(5) 0.9385(3) 0.1571(3) 0.0356(9) Uani 1 1 d . . . C25 C 0.4453(5) 0.9811(3) 0.2491(3) 0.0359(9) Uani 1 1 d . . . H25 H 0.4881 1.0444 0.2648 0.043 Uiso 1 1 calc R . . C26 C 0.3671(5) 0.9329(3) 0.3160(3) 0.0321(8) Uani 1 1 d . . . H26 H 0.3572 0.9614 0.3783 0.039 Uiso 1 1 calc R . . C27 C 0.4223(5) 0.8009(3) 0.0409(3) 0.0376(10) Uani 1 1 d . . . H27 H 0.3829 0.7371 0.0242 0.045 Uiso 1 1 calc R . . C28 C 0.5057(5) 0.8517(4) -0.0226(3) 0.0501(12) Uani 1 1 d . . . H28 H 0.5207 0.8230 -0.0840 0.060 Uiso 1 1 calc R . . C29 C 0.5689(5) 0.9449(4) 0.0017(4) 0.0539(13) Uani 1 1 d . . . H29 H 0.6256 0.9788 -0.0433 0.065 Uiso 1 1 calc R . . C30 C 0.5493(5) 0.9866(4) 0.0888(3) 0.0445(11) Uani 1 1 d . . . H30 H 0.5939 1.0495 0.1048 0.053 Uiso 1 1 calc R . . N1 N 0.2688(4) 0.8752(2) 0.6432(2) 0.0269(7) Uani 1 1 d . . . N2 N 0.2770(3) 0.7848(2) 0.6073(2) 0.0234(6) Uani 1 1 d . . . O1 O 0.1462(3) 0.65189(19) 0.43950(16) 0.0271(5) Uani 1 1 d . . . O2 O 0.3809(3) 0.64043(18) 0.33689(16) 0.0252(5) Uani 1 1 d . . . O3 O 0.2198(3) 0.79353(17) 0.35893(16) 0.0245(5) Uani 1 1 d . . . P1 P 0.31268(10) 0.70273(6) 0.41982(6) 0.0217(2) Uani 1 1 d . . . Cl1 Cl 0.63934(10) 0.77133(7) 0.71630(6) 0.0325(2) Uani 1 1 d . . . Cl2 Cl 0.71549(11) 0.68234(8) 0.50030(7) 0.0358(2) Uani 1 1 d . . . Pd1 Pd 0.48518(2) 0.73542(2) 0.558201(14) 0.02043(7) Uani 1 1 d . . . C31 C 0.7803(5) 0.7430(5) 0.2382(3) 0.0485(11) Uani 1 1 d . . . H31A H 0.7200 0.7679 0.2893 0.073 Uiso 1 1 calc R . . H31B H 0.7675 0.7884 0.1818 0.073 Uiso 1 1 calc R . . H31C H 0.8998 0.7360 0.2669 0.073 Uiso 1 1 calc R . . C32 C 0.7121(5) 0.6501(4) 0.2036(3) 0.0407(10) Uani 1 1 d . . . N3 N 0.6572(6) 0.5772(3) 0.1771(3) 0.0600(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(2) 0.039(3) 0.042(2) -0.0070(19) 0.0138(18) 0.0039(19) C2 0.0281(19) 0.045(3) 0.038(2) -0.0038(18) 0.0165(16) -0.0003(19) C3 0.0192(14) 0.0338(18) 0.0218(13) 0.000(2) 0.0030(11) -0.001(2) C4 0.041(2) 0.030(2) 0.044(2) -0.0010(17) 0.0147(18) -0.0003(17) C5 0.0150(16) 0.030(2) 0.0289(17) 0.0043(15) 0.0016(13) -0.0032(14) C6 0.0196(16) 0.031(2) 0.0247(17) 0.0040(15) 0.0022(13) -0.0053(15) C7 0.036(2) 0.035(2) 0.035(2) -0.0046(17) 0.0033(17) -0.0065(18) C8 0.042(2) 0.026(2) 0.059(3) 0.0033(19) 0.011(2) -0.0090(19) C9 0.040(2) 0.038(2) 0.040(2) 0.0150(18) 0.0092(18) -0.0076(19) C10 0.028(2) 0.043(3) 0.0252(19) 0.0049(16) 0.0055(16) -0.0052(17) C11 0.0208(17) 0.034(2) 0.0221(17) -0.0054(15) 0.0078(15) 0.0046(15) C12 0.0267(18) 0.029(2) 0.0192(15) -0.0004(13) 0.0070(14) 0.0026(14) C13 0.0276(17) 0.032(2) 0.0198(15) -0.0003(15) 0.0055(14) 0.0010(16) C14 0.0295(19) 0.036(2) 0.0223(16) -0.0002(15) 0.0067(14) 0.0035(17) C15 0.036(2) 0.027(2) 0.0310(19) -0.0036(15) 0.0102(16) -0.0004(16) C16 0.0298(18) 0.030(2) 0.0245(17) 0.0008(15) 0.0066(15) 0.0092(16) C17 0.0335(17) 0.034(3) 0.0236(16) 0.0050(15) 0.0038(14) -0.0030(15) C18 0.0375(18) 0.040(2) 0.0273(15) 0.009(2) -0.0028(13) 0.000(2) C19 0.040(2) 0.049(3) 0.0246(18) 0.0009(18) -0.0093(16) -0.007(2) C20 0.042(2) 0.035(2) 0.0299(19) -0.0064(17) 0.0032(17) -0.0060(18) C21 0.0230(18) 0.029(2) 0.0217(18) 0.0055(15) 0.0010(15) 0.0015(15) C22 0.0198(17) 0.031(2) 0.0213(17) 0.0036(15) 0.0017(14) 0.0017(15) C23 0.0222(17) 0.038(2) 0.0272(18) 0.0088(16) 0.0012(14) 0.0009(16) C24 0.0239(18) 0.043(3) 0.038(2) 0.0148(18) 0.0012(16) -0.0015(18) C25 0.032(2) 0.032(2) 0.041(2) 0.0082(17) -0.0036(17) -0.0059(17) C26 0.034(2) 0.032(2) 0.0284(18) 0.0017(16) -0.0009(16) 0.0023(17) C27 0.0316(19) 0.059(3) 0.0230(18) 0.0051(17) 0.0067(15) -0.0016(19) C28 0.038(2) 0.083(4) 0.031(2) 0.012(2) 0.0124(18) 0.001(2) C29 0.037(2) 0.076(4) 0.050(3) 0.031(3) 0.012(2) -0.005(2) C30 0.034(2) 0.052(3) 0.045(3) 0.021(2) 0.0011(18) -0.008(2) N1 0.0263(15) 0.0273(17) 0.0285(14) -0.0034(12) 0.0085(12) 0.0000(13) N2 0.0212(13) 0.0263(16) 0.0230(14) 0.0004(12) 0.0051(11) -0.0023(13) O1 0.0251(12) 0.0324(14) 0.0228(11) 0.0018(10) 0.0014(9) -0.0046(11) O2 0.0258(12) 0.0295(14) 0.0196(11) -0.0005(10) 0.0018(10) 0.0087(11) O3 0.0245(12) 0.0289(14) 0.0208(11) 0.0034(10) 0.0060(9) 0.0049(11) P1 0.0213(4) 0.0259(5) 0.0175(4) 0.0010(3) 0.0025(3) 0.0012(3) Cl1 0.0282(4) 0.0449(5) 0.0225(4) -0.0021(3) -0.0011(3) -0.0012(4) Cl2 0.0229(4) 0.0471(6) 0.0381(4) -0.0128(4) 0.0075(4) 0.0033(4) Pd1 0.01877(11) 0.02473(12) 0.01780(10) 0.00046(11) 0.00326(7) -0.00076(12) C31 0.0365(19) 0.059(3) 0.049(2) -0.007(3) 0.0041(16) 0.001(3) C32 0.043(2) 0.050(3) 0.030(2) 0.0046(19) 0.0078(17) 0.002(2) N3 0.076(3) 0.057(3) 0.048(2) -0.003(2) 0.014(2) -0.003(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 C1 N1 1.329(5) . ? C1 C2 1.369(6) . ? C1 H1 0.9500 . ? C2 C3 1.397(5) . ? C2 H2 0.9500 . ? C3 N2 1.349(5) . ? C3 C5 1.456(6) . ? C4 N1 1.455(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.390(5) . ? C5 C10 1.394(5) . ? C6 C7 1.380(6) . ? C6 O1 1.416(4) . ? C7 C8 1.386(6) . ? C7 H7 0.9500 . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 C10 1.390(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.363(5) . ? C11 C16 1.407(5) . ? C11 O2 1.419(4) . ? C12 C13 1.454(5) . ? C12 C22 1.486(5) . ? C13 C17 1.413(5) . ? C13 C14 1.429(5) . ? C14 C15 1.399(5) . ? C14 C20 1.424(5) . ? C15 C16 1.360(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C18 C19 1.404(7) . ? C18 H18 0.9500 . ? C19 C20 1.357(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.372(5) . ? C21 O3 1.397(4) . ? C21 C26 1.406(6) . ? C22 C23 1.439(5) . ? C23 C24 1.425(6) . ? C23 C27 1.426(5) . ? C24 C25 1.413(6) . ? C24 C30 1.419(5) . ? C25 C26 1.369(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.379(6) . ? C27 H27 0.9500 . ? C28 C29 1.402(7) . ? C28 H28 0.9500 . ? C29 C30 1.351(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? N1 N2 1.346(4) . ? N2 Pd1 2.037(3) . ? O1 P1 1.583(2) . ? O2 P1 1.592(2) . ? O3 P1 1.612(2) . ? P1 Pd1 2.1776(8) . ? Cl1 Pd1 2.3347(8) . ? Cl2 Pd1 2.2693(9) . ? C31 C32 1.442(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.132(6) . ? 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 C1 C2 108.7(4) . . ? N1 C1 H1 125.6 . . ? C2 C1 H1 125.6 . . ? C1 C2 C3 105.7(3) . . ? C1 C2 H2 127.2 . . ? C3 C2 H2 127.2 . . ? N2 C3 C2 108.2(4) . . ? N2 C3 C5 122.3(3) . . ? C2 C3 C5 129.5(3) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 117.1(4) . . ? C6 C5 C3 123.6(3) . . ? C10 C5 C3 119.3(3) . . ? C7 C6 C5 122.7(3) . . ? C7 C6 O1 117.0(3) . . ? C5 C6 O1 120.0(3) . . ? C6 C7 C8 119.2(4) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 119.5(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C5 120.9(4) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? C12 C11 C16 124.6(3) . . ? C12 C11 O2 119.1(3) . . ? C16 C11 O2 116.2(3) . . ? C11 C12 C13 116.6(3) . . ? C11 C12 C22 121.3(3) . . ? C13 C12 C22 122.1(3) . . ? C17 C13 C14 119.0(3) . . ? C17 C13 C12 122.0(3) . . ? C14 C13 C12 118.9(3) . . ? C15 C14 C20 122.1(4) . . ? C15 C14 C13 119.6(3) . . ? C20 C14 C13 118.3(3) . . ? C16 C15 C14 121.7(4) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C11 118.1(3) . . ? C15 C16 H16 120.9 . . ? C11 C16 H16 120.9 . . ? C18 C17 C13 120.5(4) . . ? C18 C17 H17 119.8 . . ? C13 C17 H17 119.8 . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C14 121.4(4) . . ? C19 C20 H20 119.3 . . ? C14 C20 H20 119.3 . . ? C22 C21 O3 118.9(3) . . ? C22 C21 C26 124.0(3) . . ? O3 C21 C26 117.0(3) . . ? C21 C22 C23 117.5(3) . . ? C21 C22 C12 119.5(3) . . ? C23 C22 C12 122.9(3) . . ? C24 C23 C27 118.8(3) . . ? C24 C23 C22 119.2(3) . . ? C27 C23 C22 122.0(4) . . ? C25 C24 C30 121.5(4) . . ? C25 C24 C23 119.6(3) . . ? C30 C24 C23 118.8(4) . . ? C26 C25 C24 121.2(4) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 118.3(4) . . ? C25 C26 H26 120.8 . . ? C21 C26 H26 120.8 . . ? C28 C27 C23 119.6(4) . . ? C28 C27 H27 120.2 . . ? C23 C27 H27 120.2 . . ? C27 C28 C29 121.2(4) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C24 121.3(4) . . ? C29 C30 H30 119.3 . . ? C24 C30 H30 119.3 . . ? C1 N1 N2 109.8(3) . . ? C1 N1 C4 127.5(3) . . ? N2 N1 C4 122.4(3) . . ? N1 N2 C3 107.6(3) . . ? N1 N2 Pd1 121.8(2) . . ? C3 N2 Pd1 127.6(3) . . ? C6 O1 P1 124.3(2) . . ? C11 O2 P1 117.4(2) . . ? C21 O3 P1 117.9(2) . . ? O1 P1 O2 107.01(13) . . ? O1 P1 O3 95.71(13) . . ? O2 P1 O3 104.25(12) . . ? O1 P1 Pd1 112.27(9) . . ? O2 P1 Pd1 118.23(9) . . ? O3 P1 Pd1 116.68(9) . . ? N2 Pd1 P1 84.98(8) . . ? N2 Pd1 Cl2 178.71(9) . . ? P1 Pd1 Cl2 94.16(3) . . ? N2 Pd1 Cl1 87.96(8) . . ? P1 Pd1 Cl1 172.57(3) . . ? Cl2 Pd1 Cl1 92.93(3) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C31 179.2(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 62.83 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.251 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.056 # Attachment 'Compound6.cif' data_0872o _database_code_depnum_ccdc_archive 'CCDC 713119' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H47 Cl2 N2 O3.50 P Ru' _chemical_formula_weight 922.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' _cell_length_a 15.80010(10) _cell_length_b 15.80010(10) _cell_length_c 35.7434(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8923.10(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19132 _cell_measurement_theta_min 3.7255 _cell_measurement_theta_max 62.4439 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 4.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51880 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S Ultra' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27147 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 62.59 _reflns_number_total 6661 _reflns_number_gt 6109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+13.6162P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(11) _chemical_absolute_configuration ad _refine_ls_number_reflns 6661 _refine_ls_number_parameters 622 _refine_ls_number_restraints 321 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.106 _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 C1 C 0.6077(4) 0.1670(5) 0.47388(16) 0.0568(17) Uani 1 1 d . . . H1 H 0.6427 0.1407 0.4921 0.068 Uiso 1 1 calc R . . C2 C 0.5555(4) 0.1270(4) 0.44906(15) 0.0427(14) Uani 1 1 d . . . H2 H 0.5471 0.0678 0.4462 0.051 Uiso 1 1 calc R . . C3 C 0.5171(3) 0.1922(3) 0.42865(14) 0.0361(13) Uani 1 1 d . . . C4 C 0.6457(5) 0.3211(5) 0.4859(2) 0.078(2) Uani 1 1 d . . . H4A H 0.6473 0.3117 0.5130 0.117 Uiso 1 1 calc R . . H4B H 0.6163 0.3743 0.4806 0.117 Uiso 1 1 calc R . . H4C H 0.7036 0.3239 0.4762 0.117 Uiso 1 1 calc R . . C5 C 0.4534(4) 0.1878(3) 0.39836(15) 0.0385(14) Uani 1 1 d . . . C6 C 0.4612(3) 0.1348(3) 0.36762(14) 0.0302(12) Uani 1 1 d . . . C7 C 0.4016(4) 0.1335(4) 0.33922(15) 0.0397(14) Uani 1 1 d . . . H7 H 0.4083 0.0966 0.3184 0.048 Uiso 1 1 calc R . . C8 C 0.3324(4) 0.1861(4) 0.34145(15) 0.0467(14) Uani 1 1 d . . . H8 H 0.2913 0.1861 0.3220 0.056 Uiso 1 1 calc R . . C9 C 0.3229(4) 0.2384(4) 0.37157(18) 0.0517(16) Uani 1 1 d . . . H9 H 0.2743 0.2736 0.3732 0.062 Uiso 1 1 calc R . . C10 C 0.3823(4) 0.2410(4) 0.39966(18) 0.0500(16) Uani 1 1 d . . . H10 H 0.3753 0.2790 0.4200 0.060 Uiso 1 1 calc R . . C11 C 0.6029(3) -0.0862(3) 0.37020(13) 0.0268(11) Uani 1 1 d . . . C12 C 0.5642(3) -0.1461(3) 0.34808(13) 0.0285(11) Uani 1 1 d . . . C13 C 0.5121(3) -0.2073(3) 0.36597(14) 0.0306(12) Uani 1 1 d . . . C14 C 0.5079(3) -0.2079(3) 0.40547(15) 0.0334(13) Uani 1 1 d . . . C15 C 0.5558(3) -0.1494(3) 0.42696(13) 0.0294(12) Uani 1 1 d . . . H15 H 0.5557 -0.1524 0.4535 0.035 Uiso 1 1 calc R . . C16 C 0.6017(3) -0.0892(3) 0.40896(13) 0.0279(11) Uani 1 1 d . . . H16 H 0.6332 -0.0490 0.4230 0.033 Uiso 1 1 calc R . . C17 C 0.4605(4) -0.2645(3) 0.34577(16) 0.0376(14) Uani 1 1 d . . . H17 H 0.4628 -0.2650 0.3192 0.045 Uiso 1 1 calc R . . C18 C 0.4072(4) -0.3193(4) 0.36395(17) 0.0505(16) Uani 1 1 d . . . H18 H 0.3726 -0.3569 0.3500 0.061 Uiso 1 1 calc R . . C19 C 0.4038(4) -0.3198(4) 0.40344(18) 0.0518(17) Uani 1 1 d . . . H19 H 0.3672 -0.3583 0.4159 0.062 Uiso 1 1 calc R . . C20 C 0.4523(4) -0.2658(4) 0.42368(16) 0.0415(14) Uani 1 1 d . . . H20 H 0.4492 -0.2666 0.4502 0.050 Uiso 1 1 calc R . . C21 C 0.5509(3) -0.0692(3) 0.28788(13) 0.0277(11) Uani 1 1 d . . . C22 C 0.5732(3) -0.1418(3) 0.30624(13) 0.0284(11) Uani 1 1 d . . . C23 C 0.6062(3) -0.2103(3) 0.28487(14) 0.0315(12) Uani 1 1 d . . . C24 C 0.6098(3) -0.2025(4) 0.24503(14) 0.0369(13) Uani 1 1 d . . . C25 C 0.5802(4) -0.1283(4) 0.22788(15) 0.0394(14) Uani 1 1 d . . . H25 H 0.5792 -0.1245 0.2014 0.047 Uiso 1 1 calc R . . C26 C 0.5526(3) -0.0613(3) 0.24893(13) 0.0339(12) Uani 1 1 d . . . H26 H 0.5348 -0.0103 0.2372 0.041 Uiso 1 1 calc R . . C27 C 0.6400(4) -0.2841(4) 0.30163(16) 0.0426(14) Uani 1 1 d . . . H27 H 0.6387 -0.2899 0.3281 0.051 Uiso 1 1 calc R . . C28 C 0.6746(4) -0.3475(4) 0.28015(16) 0.0500(15) Uani 1 1 d . . . H28 H 0.6968 -0.3968 0.2918 0.060 Uiso 1 1 calc R . . C29 C 0.6772(4) -0.3398(4) 0.24105(16) 0.0528(16) Uani 1 1 d . . . H29 H 0.7018 -0.3835 0.2264 0.063 Uiso 1 1 calc R . . C30 C 0.6449(4) -0.2702(4) 0.22412(16) 0.0478(16) Uani 1 1 d . . . H30 H 0.6458 -0.2667 0.1976 0.057 Uiso 1 1 calc R . . C31 C 0.6645(4) 0.2937(4) 0.32394(16) 0.0490(16) Uani 1 1 d . . . C32 C 0.7382(4) 0.2812(4) 0.29993(16) 0.0492(17) Uani 1 1 d . . . H32 H 0.7452 0.3161 0.2785 0.059 Uiso 1 1 calc R . . C33 C 0.7969(4) 0.2212(4) 0.30740(16) 0.0454(15) Uani 1 1 d . . . H33 H 0.8436 0.2152 0.2909 0.055 Uiso 1 1 calc R . . C34 C 0.7917(4) 0.1662(5) 0.33917(16) 0.0574(19) Uani 1 1 d . . . C35 C 0.7220(4) 0.1821(4) 0.36373(15) 0.0530(19) Uani 1 1 d . . . H35 H 0.7167 0.1492 0.3859 0.064 Uiso 1 1 calc R . . C36 C 0.6607(5) 0.2453(4) 0.35613(16) 0.0517(17) Uani 1 1 d . . . H36 H 0.6161 0.2545 0.3735 0.062 Uiso 1 1 calc R . . C37 C 0.5998(5) 0.3613(4) 0.3137(2) 0.063(2) Uani 1 1 d . . . H37 H 0.5873 0.3543 0.2865 0.076 Uiso 1 1 calc R . . C38 C 0.5166(5) 0.3555(5) 0.3340(2) 0.074(2) Uani 1 1 d . . . H38A H 0.4959 0.2970 0.3331 0.112 Uiso 1 1 calc R . . H38B H 0.4754 0.3930 0.3220 0.112 Uiso 1 1 calc R . . H38C H 0.5243 0.3726 0.3601 0.112 Uiso 1 1 calc R . . C39 C 0.6403(7) 0.4491(5) 0.3185(3) 0.130(5) Uani 1 1 d . . . H39A H 0.6041 0.4920 0.3068 0.196 Uiso 1 1 calc R . . H39B H 0.6961 0.4497 0.3065 0.196 Uiso 1 1 calc R . . H39C H 0.6466 0.4617 0.3452 0.196 Uiso 1 1 calc R . . C40 C 0.8543(5) 0.0990(5) 0.3459(2) 0.066(2) Uani 1 1 d . . . H40A H 0.9018 0.1221 0.3603 0.100 Uiso 1 1 calc R . . H40B H 0.8751 0.0773 0.3220 0.100 Uiso 1 1 calc R . . H40C H 0.8278 0.0529 0.3601 0.100 Uiso 1 1 calc R . . N1 N 0.6003(4) 0.2506(4) 0.46781(13) 0.0542(14) Uani 1 1 d . . . N2 N 0.5449(3) 0.2681(3) 0.43998(13) 0.0477(12) Uani 1 1 d . . . O1 O 0.5298(2) 0.0781(2) 0.36784(9) 0.0278(8) Uani 1 1 d . . . O2 O 0.6464(2) -0.0177(2) 0.35344(9) 0.0263(7) Uani 1 1 d . . . O3 O 0.52437(19) 0.0005(2) 0.30834(8) 0.0282(7) Uani 1 1 d . . . P1 P 0.59050(8) 0.05428(8) 0.33367(3) 0.0264(3) Uani 1 1 d . . . Cl1 Cl 0.72905(9) 0.04585(9) 0.27081(3) 0.0386(3) Uani 1 1 d . . . Cl2 Cl 0.56237(8) 0.17768(9) 0.26235(4) 0.0395(3) Uani 1 1 d . . . Ru1 Ru 0.67150(3) 0.15583(3) 0.308907(10) 0.03384(12) Uani 1 1 d . . . C41A C 0.4054(9) 0.6894(9) 0.2315(4) 0.138(6) Uani 0.806(13) 1 d PDU A 1 H41A H 0.4523 0.7218 0.2430 0.166 Uiso 0.806(13) 1 calc PR A 1 H41B H 0.4168 0.6830 0.2044 0.166 Uiso 0.806(13) 1 calc PR A 1 C42A C 0.3225(10) 0.7338(9) 0.2377(4) 0.183(8) Uani 0.806(13) 1 d PDU A 1 H42A H 0.2944 0.7444 0.2134 0.220 Uiso 0.806(13) 1 calc PR A 1 H42B H 0.3322 0.7889 0.2501 0.220 Uiso 0.806(13) 1 calc PR A 1 O4A O 0.3969(8) 0.6031(8) 0.2500 0.158(6) Uani 0.806(13) 2 d SPDU A 1 C41B C 0.460(3) 0.589(4) 0.2186(8) 0.146(12) Uani 0.194(13) 1 d PDU A 2 H41C H 0.4382 0.5596 0.1961 0.175 Uiso 0.194(13) 1 calc PR A 2 H41D H 0.5145 0.6165 0.2127 0.175 Uiso 0.194(13) 1 calc PR A 2 C42B C 0.394(5) 0.655(4) 0.2341(18) 0.141(12) Uani 0.194(13) 1 d PDU A 2 H42C H 0.4226 0.7053 0.2443 0.170 Uiso 0.194(13) 1 calc PR A 2 H42D H 0.3541 0.6727 0.2142 0.170 Uiso 0.194(13) 1 calc PR A 2 O4B O 0.466(3) 0.534(3) 0.2500 0.146(13) Uani 0.194(13) 2 d SPDU A 2 C43A C 0.3512(19) 0.4595(17) 0.4387(7) 0.107(7) Uani 0.423(12) 1 d PDU B 1 C44A C 0.3171(14) 0.4636(15) 0.4035(7) 0.096(7) Uani 0.423(12) 1 d PDU B 1 H44A H 0.3497 0.4748 0.3818 0.116 Uiso 0.423(12) 1 calc PR B 1 C45A C 0.2325(13) 0.4501(12) 0.4026(7) 0.085(5) Uani 0.423(12) 1 d PDU B 1 H45A H 0.2013 0.4496 0.3799 0.102 Uiso 0.423(12) 1 calc PR B 1 C46A C 0.1953(18) 0.437(2) 0.4361(7) 0.105(7) Uani 0.423(12) 1 d PDU B 1 H46A H 0.1352 0.4358 0.4350 0.126 Uiso 0.423(12) 1 calc PR B 1 C47A C 0.2262(17) 0.4266(18) 0.4701(7) 0.136(8) Uani 0.423(12) 1 d PDU B 1 H47A H 0.1944 0.4083 0.4911 0.164 Uiso 0.423(12) 1 calc PR B 1 C48A C 0.3088(16) 0.4451(13) 0.4706(7) 0.109(6) Uani 0.423(12) 1 d PDU B 1 H48A H 0.3378 0.4481 0.4938 0.131 Uiso 0.423(12) 1 calc PR B 1 C49A C 0.446(2) 0.478(3) 0.4421(12) 0.227(17) Uani 0.423(12) 1 d PDU B 1 H49A H 0.4573 0.5093 0.4652 0.340 Uiso 0.423(12) 1 calc PR B 1 H49B H 0.4652 0.5113 0.4206 0.340 Uiso 0.423(12) 1 calc PR B 1 H49C H 0.4777 0.4241 0.4427 0.340 Uiso 0.423(12) 1 calc PR B 1 C43B C 0.3347(14) 0.4560(13) 0.4233(5) 0.098(5) Uani 0.577(12) 1 d PDU B 2 C44B C 0.3190(9) 0.4727(11) 0.3865(4) 0.084(5) Uani 0.577(12) 1 d PDU B 2 H44B H 0.3646 0.4896 0.3709 0.101 Uiso 0.577(12) 1 calc PR B 2 C45B C 0.2371(9) 0.4657(8) 0.3709(4) 0.090(4) Uani 0.577(12) 1 d PDU B 2 H45B H 0.2287 0.4792 0.3453 0.107 Uiso 0.577(12) 1 calc PR B 2 C46B C 0.1705(10) 0.4402(9) 0.3918(5) 0.100(5) Uani 0.577(12) 1 d PDU B 2 H46B H 0.1153 0.4347 0.3815 0.120 Uiso 0.577(12) 1 calc PR B 2 C47B C 0.1879(15) 0.4218(19) 0.4302(6) 0.120(6) Uani 0.577(12) 1 d PDU B 2 H47B H 0.1428 0.4013 0.4453 0.144 Uiso 0.577(12) 1 calc PR B 2 C48B C 0.2681(12) 0.4323(11) 0.4472(5) 0.111(5) Uani 0.577(12) 1 d PDU B 2 H48B H 0.2764 0.4239 0.4733 0.133 Uiso 0.577(12) 1 calc PR B 2 C49B C 0.4159(16) 0.4647(13) 0.4388(7) 0.159(8) Uani 0.577(12) 1 d PDU B 2 H49D H 0.4484 0.4128 0.4345 0.238 Uiso 0.577(12) 1 calc PR B 2 H49E H 0.4111 0.4748 0.4658 0.238 Uiso 0.577(12) 1 calc PR B 2 H49F H 0.4449 0.5126 0.4271 0.238 Uiso 0.577(12) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.070(5) 0.063(5) 0.037(3) 0.006(3) -0.001(3) 0.016(4) C2 0.060(4) 0.034(3) 0.034(3) 0.004(2) -0.004(3) -0.001(3) C3 0.037(3) 0.037(3) 0.035(3) -0.002(2) 0.005(2) 0.000(3) C4 0.078(5) 0.074(5) 0.083(5) -0.030(4) -0.038(4) 0.011(5) C5 0.046(4) 0.034(3) 0.036(3) 0.004(2) 0.003(3) 0.003(3) C6 0.031(3) 0.028(3) 0.031(3) 0.008(2) 0.002(2) -0.005(2) C7 0.044(3) 0.038(3) 0.037(3) 0.000(2) 0.001(3) -0.005(3) C8 0.042(4) 0.051(4) 0.047(3) 0.005(3) -0.004(3) 0.011(3) C9 0.043(4) 0.043(4) 0.070(4) -0.002(3) 0.006(3) 0.010(3) C10 0.049(4) 0.048(4) 0.053(4) -0.009(3) 0.007(3) 0.010(3) C11 0.023(3) 0.027(3) 0.031(3) 0.006(2) 0.002(2) 0.001(2) C12 0.029(3) 0.026(3) 0.031(3) 0.005(2) -0.001(2) 0.002(2) C13 0.029(3) 0.030(3) 0.033(3) 0.001(2) 0.003(2) 0.002(2) C14 0.030(3) 0.033(3) 0.037(3) 0.004(2) 0.006(2) 0.005(2) C15 0.032(3) 0.033(3) 0.023(2) 0.000(2) 0.002(2) 0.010(2) C16 0.031(3) 0.027(3) 0.025(2) -0.002(2) -0.001(2) 0.003(2) C17 0.041(4) 0.031(3) 0.041(3) -0.001(2) -0.001(3) -0.007(3) C18 0.053(4) 0.042(4) 0.056(4) 0.004(3) 0.001(3) -0.011(3) C19 0.047(4) 0.050(4) 0.058(4) 0.013(3) 0.009(3) -0.014(3) C20 0.047(4) 0.035(3) 0.043(3) 0.010(3) 0.007(3) -0.003(3) C21 0.026(3) 0.030(3) 0.027(3) -0.001(2) -0.008(2) -0.008(2) C22 0.026(3) 0.035(3) 0.025(3) -0.001(2) 0.002(2) -0.005(2) C23 0.035(3) 0.026(3) 0.033(3) -0.001(2) -0.002(2) -0.002(2) C24 0.034(3) 0.046(4) 0.031(3) -0.006(3) -0.001(2) -0.006(3) C25 0.041(3) 0.052(4) 0.025(3) 0.001(3) -0.003(2) -0.010(3) C26 0.036(3) 0.040(3) 0.026(3) 0.005(2) -0.007(2) -0.003(2) C27 0.048(4) 0.039(3) 0.041(3) 0.000(3) 0.002(3) 0.004(3) C28 0.061(4) 0.035(3) 0.055(4) -0.007(3) 0.000(3) 0.008(3) C29 0.065(4) 0.046(4) 0.048(3) -0.015(3) 0.003(3) 0.009(4) C30 0.051(4) 0.058(4) 0.035(3) -0.018(3) -0.001(3) -0.003(3) C31 0.059(4) 0.039(3) 0.049(4) -0.007(3) 0.010(3) -0.024(3) C32 0.067(5) 0.044(4) 0.037(3) 0.001(3) 0.008(3) -0.033(3) C33 0.050(4) 0.051(4) 0.035(3) -0.003(3) -0.001(3) -0.029(3) C34 0.061(4) 0.070(5) 0.041(4) 0.008(3) -0.016(3) -0.040(4) C35 0.073(5) 0.065(5) 0.021(3) -0.003(3) -0.004(3) -0.047(4) C36 0.065(5) 0.050(4) 0.040(3) -0.011(3) 0.009(3) -0.028(4) C37 0.086(5) 0.034(4) 0.069(5) -0.010(3) 0.018(4) -0.019(4) C38 0.086(6) 0.059(5) 0.078(5) 0.012(4) 0.002(4) -0.013(4) C39 0.122(9) 0.045(5) 0.224(12) -0.029(6) 0.064(9) -0.032(5) C40 0.055(5) 0.072(5) 0.072(5) 0.015(4) -0.020(4) -0.025(4) N1 0.064(4) 0.061(4) 0.037(3) -0.012(3) -0.007(3) 0.014(3) N2 0.059(3) 0.046(3) 0.038(3) -0.005(2) -0.005(3) 0.007(2) O1 0.035(2) 0.0251(19) 0.0236(17) 0.0008(14) 0.0014(14) 0.0001(15) O2 0.0238(19) 0.0262(18) 0.0291(18) 0.0042(14) 0.0003(14) -0.0013(15) O3 0.0269(19) 0.0301(19) 0.0277(17) 0.0004(15) -0.0062(15) -0.0027(14) P1 0.0291(7) 0.0269(7) 0.0232(6) 0.0033(5) -0.0013(5) -0.0056(5) Cl1 0.0394(8) 0.0455(9) 0.0310(7) 0.0013(6) 0.0003(6) -0.0044(6) Cl2 0.0431(8) 0.0382(8) 0.0373(7) 0.0079(6) 0.0010(6) -0.0044(6) Ru1 0.0426(3) 0.0351(2) 0.02380(18) 0.00119(17) 0.00156(17) -0.01699(19) C41A 0.162(11) 0.176(11) 0.077(8) -0.026(8) 0.003(8) -0.147(9) C42A 0.31(2) 0.124(12) 0.118(14) 0.008(10) -0.061(14) 0.002(14) O4A 0.155(8) 0.155(8) 0.163(15) -0.024(7) -0.024(7) -0.021(11) C41B 0.13(2) 0.19(2) 0.13(3) -0.025(18) -0.02(2) -0.05(2) C42B 0.18(2) 0.14(2) 0.10(2) 0.00(2) -0.01(2) -0.04(2) O4B 0.133(17) 0.133(17) 0.17(3) -0.016(17) -0.016(17) -0.04(2) C43A 0.091(12) 0.052(12) 0.178(15) -0.022(16) -0.015(10) 0.001(13) C44A 0.105(11) 0.049(12) 0.134(14) 0.019(16) 0.021(12) 0.004(12) C45A 0.098(10) 0.042(9) 0.115(11) -0.022(10) 0.003(10) 0.016(10) C46A 0.086(11) 0.070(15) 0.159(12) -0.011(14) 0.030(9) 0.032(12) C47A 0.179(15) 0.105(15) 0.125(12) -0.005(15) 0.043(13) -0.008(16) C48A 0.172(15) 0.046(11) 0.110(13) -0.043(11) -0.026(11) 0.017(13) C49A 0.085(15) 0.20(4) 0.39(4) 0.00(4) -0.052(16) 0.01(2) C43B 0.109(9) 0.045(9) 0.141(11) -0.003(11) -0.002(9) 0.004(10) C44B 0.083(7) 0.067(11) 0.102(9) -0.041(9) 0.037(7) -0.009(8) C45B 0.100(9) 0.057(9) 0.112(10) -0.049(8) 0.018(7) 0.001(7) C46B 0.063(8) 0.044(7) 0.193(12) -0.016(9) 0.013(8) 0.006(7) C47B 0.128(10) 0.053(11) 0.180(11) -0.015(11) 0.049(10) -0.011(10) C48B 0.163(11) 0.056(9) 0.113(11) 0.011(10) 0.026(8) -0.003(10) C49B 0.129(12) 0.035(10) 0.31(2) -0.002(14) -0.087(15) 0.024(12) _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 C1 N1 1.343(9) . ? C1 C2 1.366(8) . ? C1 H1 0.9500 . ? C2 C3 1.400(8) . ? C2 H2 0.9500 . ? C3 N2 1.340(7) . ? C3 C5 1.480(8) . ? C4 N1 1.474(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.387(7) . ? C5 C10 1.403(8) . ? C6 C7 1.385(7) . ? C6 O1 1.406(6) . ? C7 C8 1.376(8) . ? C7 H7 0.9500 . ? C8 C9 1.366(8) . ? C8 H8 0.9500 . ? C9 C10 1.375(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.376(7) . ? C11 C16 1.386(6) . ? C11 O2 1.416(6) . ? C12 C13 1.423(7) . ? C12 C22 1.503(7) . ? C13 C14 1.414(7) . ? C13 C17 1.416(7) . ? C14 C15 1.419(7) . ? C14 C20 1.426(8) . ? C15 C16 1.359(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.370(8) . ? C17 H17 0.9500 . ? C18 C19 1.412(8) . ? C18 H18 0.9500 . ? C19 C20 1.356(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.368(7) . ? C21 O3 1.386(6) . ? C21 C26 1.398(7) . ? C22 C23 1.424(7) . ? C23 C27 1.415(7) . ? C23 C24 1.430(7) . ? C24 C25 1.403(8) . ? C24 C30 1.418(8) . ? C25 C26 1.369(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.376(8) . ? C27 H27 0.9500 . ? C28 C29 1.404(8) . ? C28 H28 0.9500 . ? C29 C30 1.354(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.383(8) . ? C31 C32 1.460(9) . ? C31 C37 1.522(9) . ? C31 Ru1 2.247(6) . ? C32 C33 1.353(9) . ? C32 Ru1 2.266(6) . ? C32 H32 0.9500 . ? C33 C34 1.431(8) . ? C33 Ru1 2.235(5) . ? C33 H33 0.9500 . ? C34 C35 1.430(9) . ? C34 C40 1.472(10) . ? C34 Ru1 2.191(6) . ? C35 C36 1.418(10) . ? C35 Ru1 2.156(5) . ? C35 H35 0.9500 . ? C36 Ru1 2.208(6) . ? C36 H36 0.9500 . ? C37 C38 1.504(10) . ? C37 C39 1.538(9) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1 N2 1.353(7) . ? O1 P1 1.598(3) . ? O2 P1 1.605(3) . ? O3 P1 1.623(3) . ? P1 Ru1 2.2351(13) . ? Cl1 Ru1 2.3876(15) . ? Cl2 Ru1 2.4211(14) . ? C41A C42A 1.502(15) . ? C41A O4A 1.521(13) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C42A C42A 1.535(18) 5_665 ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? O4A C41A 1.521(13) 5_665 ? C41B O4B 1.430(19) . ? C41B C42B 1.57(2) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42B C42B 1.57(2) 5_665 ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? O4B C41B 1.430(19) 5_665 ? C43A C48A 1.341(17) . ? C43A C44A 1.368(16) . ? C43A C49A 1.54(4) . ? C44A C45A 1.354(17) . ? C44A H44A 0.9500 . ? C45A C46A 1.347(16) . ? C45A H45A 0.9500 . ? C46A C47A 1.320(16) . ? C46A H46A 0.9500 . ? C47A C48A 1.337(17) . ? C47A H47A 0.9500 . ? C48A H48A 0.9500 . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? C43B C44B 1.363(13) . ? C43B C49B 1.41(3) . ? C43B C48B 1.407(15) . ? C44B C45B 1.414(14) . ? C44B H44B 0.9500 . ? C45B C46B 1.350(13) . ? C45B H45B 0.9500 . ? C46B C47B 1.433(14) . ? C46B H46B 0.9500 . ? C47B C48B 1.414(15) . ? C47B H47B 0.9500 . ? C48B H48B 0.9500 . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 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 C1 C2 107.3(6) . . ? N1 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? C1 C2 C3 105.1(5) . . ? C1 C2 H2 127.5 . . ? C3 C2 H2 127.5 . . ? N2 C3 C2 111.0(5) . . ? N2 C3 C5 119.1(5) . . ? C2 C3 C5 129.9(5) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 117.4(5) . . ? C6 C5 C3 123.2(5) . . ? C10 C5 C3 119.5(5) . . ? C7 C6 C5 121.9(5) . . ? C7 C6 O1 121.3(5) . . ? C5 C6 O1 116.7(5) . . ? C8 C7 C6 119.3(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 C7 119.9(6) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 121.2(6) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C5 120.3(6) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C12 C11 C16 123.0(5) . . ? C12 C11 O2 119.9(4) . . ? C16 C11 O2 117.1(4) . . ? C11 C12 C13 117.8(4) . . ? C11 C12 C22 120.0(4) . . ? C13 C12 C22 122.1(4) . . ? C14 C13 C17 118.6(5) . . ? C14 C13 C12 118.7(5) . . ? C17 C13 C12 122.6(5) . . ? C13 C14 C15 120.7(5) . . ? C13 C14 C20 119.3(5) . . ? C15 C14 C20 119.9(5) . . ? C16 C15 C14 119.0(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C11 120.3(5) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C18 C17 C13 121.0(5) . . ? C18 C17 H17 119.5 . . ? C13 C17 H17 119.5 . . ? C17 C18 C19 120.1(6) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.5(6) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C14 120.5(5) . . ? C19 C20 H20 119.7 . . ? C14 C20 H20 119.7 . . ? C22 C21 O3 119.4(4) . . ? C22 C21 C26 123.2(5) . . ? O3 C21 C26 117.4(4) . . ? C21 C22 C23 118.3(4) . . ? C21 C22 C12 119.4(4) . . ? C23 C22 C12 122.3(4) . . ? C27 C23 C22 122.5(5) . . ? C27 C23 C24 118.5(5) . . ? C22 C23 C24 118.9(5) . . ? C25 C24 C30 122.0(5) . . ? C25 C24 C23 119.6(5) . . ? C30 C24 C23 118.4(5) . . ? C26 C25 C24 120.8(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 119.0(5) . . ? C25 C26 H26 120.5 . . ? C21 C26 H26 120.5 . . ? C28 C27 C23 120.9(5) . . ? C28 C27 H27 119.5 . . ? C23 C27 H27 119.5 . . ? C27 C28 C29 120.2(6) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.3(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C24 121.6(5) . . ? C29 C30 H30 119.2 . . ? C24 C30 H30 119.2 . . ? C36 C31 C32 116.7(7) . . ? C36 C31 C37 123.9(6) . . ? C32 C31 C37 119.3(5) . . ? C36 C31 Ru1 70.4(3) . . ? C32 C31 Ru1 71.9(3) . . ? C37 C31 Ru1 130.9(4) . . ? C33 C32 C31 121.7(6) . . ? C33 C32 Ru1 71.2(4) . . ? C31 C32 Ru1 70.4(3) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? Ru1 C32 H32 132.4 . . ? C32 C33 C34 122.8(6) . . ? C32 C33 Ru1 73.8(4) . . ? C34 C33 Ru1 69.5(3) . . ? C32 C33 H33 118.6 . . ? C34 C33 H33 118.6 . . ? Ru1 C33 H33 131.1 . . ? C35 C34 C33 115.2(7) . . ? C35 C34 C40 122.9(6) . . ? C33 C34 C40 121.9(6) . . ? C35 C34 Ru1 69.5(3) . . ? C33 C34 Ru1 72.8(3) . . ? C40 C34 Ru1 127.6(5) . . ? C36 C35 C34 122.1(6) . . ? C36 C35 Ru1 73.0(3) . . ? C34 C35 Ru1 72.1(3) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? Ru1 C35 H35 128.2 . . ? C31 C36 C35 121.3(6) . . ? C31 C36 Ru1 73.5(3) . . ? C35 C36 Ru1 69.1(3) . . ? C31 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? Ru1 C36 H36 130.9 . . ? C38 C37 C31 115.4(6) . . ? C38 C37 C39 111.4(6) . . ? C31 C37 C39 109.1(7) . . ? C38 C37 H37 106.8 . . ? C31 C37 H37 106.8 . . ? C39 C37 H37 106.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 N1 N2 112.1(5) . . ? C1 N1 C4 129.0(6) . . ? N2 N1 C4 118.9(5) . . ? C3 N2 N1 104.6(5) . . ? C6 O1 P1 127.5(3) . . ? C11 O2 P1 117.4(3) . . ? C21 O3 P1 121.0(3) . . ? O1 P1 O2 99.26(18) . . ? O1 P1 O3 99.43(17) . . ? O2 P1 O3 103.23(17) . . ? O1 P1 Ru1 118.48(13) . . ? O2 P1 Ru1 111.59(13) . . ? O3 P1 Ru1 121.59(12) . . ? C35 Ru1 C34 38.4(2) . . ? C35 Ru1 C36 37.9(3) . . ? C34 Ru1 C36 69.0(3) . . ? C35 Ru1 C33 66.7(2) . . ? C34 Ru1 C33 37.7(2) . . ? C36 Ru1 C33 78.0(2) . . ? C35 Ru1 P1 89.44(15) . . ? C34 Ru1 P1 110.77(17) . . ? C36 Ru1 P1 96.46(16) . . ? C33 Ru1 P1 148.08(17) . . ? C35 Ru1 C31 67.3(3) . . ? C34 Ru1 C31 81.5(3) . . ? C36 Ru1 C31 36.2(2) . . ? C33 Ru1 C31 66.5(2) . . ? P1 Ru1 C31 124.99(16) . . ? C35 Ru1 C32 77.8(2) . . ? C34 Ru1 C32 66.5(3) . . ? C36 Ru1 C32 65.5(2) . . ? C33 Ru1 C32 35.0(2) . . ? P1 Ru1 C32 161.75(16) . . ? C31 Ru1 C32 37.7(2) . . ? C35 Ru1 Cl1 121.1(2) . . ? C34 Ru1 Cl1 90.4(2) . . ? C36 Ru1 Cl1 158.6(2) . . ? C33 Ru1 Cl1 89.13(17) . . ? P1 Ru1 Cl1 85.50(5) . . ? C31 Ru1 Cl1 149.41(16) . . ? C32 Ru1 Cl1 112.22(17) . . ? C35 Ru1 Cl2 149.4(2) . . ? C34 Ru1 Cl2 161.02(17) . . ? C36 Ru1 Cl2 112.3(2) . . ? C33 Ru1 Cl2 123.30(16) . . ? P1 Ru1 Cl2 88.09(5) . . ? C31 Ru1 Cl2 89.50(18) . . ? C32 Ru1 Cl2 96.28(18) . . ? Cl1 Ru1 Cl2 89.02(5) . . ? C42A C41A O4A 106.2(12) . . ? C42A C41A H41A 110.5 . . ? O4A C41A H41A 110.5 . . ? C42A C41A H41B 110.5 . . ? O4A C41A H41B 110.5 . . ? H41A C41A H41B 108.7 . . ? C41A C42A C42A 108.6(6) . 5_665 ? C41A C42A H42A 110.0 . . ? C42A C42A H42A 110.0 5_665 . ? C41A C42A H42B 110.0 . . ? C42A C42A H42B 110.0 5_665 . ? H42A C42A H42B 108.4 . . ? C41A O4A C41A 110.3(16) 5_665 . ? O4B C41B C42B 100(2) . . ? O4B C41B H41C 111.7 . . ? C42B C41B H41C 111.7 . . ? O4B C41B H41D 111.7 . . ? C42B C41B H41D 111.7 . . ? H41C C41B H41D 109.5 . . ? C42B C42B C41B 105.0(19) 5_665 . ? C42B C42B H42C 110.7 5_665 . ? C41B C42B H42C 110.7 . . ? C42B C42B H42D 110.7 5_665 . ? C41B C42B H42D 110.7 . . ? H42C C42B H42D 108.8 . . ? C41B O4B C41B 122(3) . 5_665 ? C48A C43A C44A 126(2) . . ? C48A C43A C49A 116.9(15) . . ? C44A C43A C49A 116.8(15) . . ? C45A C44A C43A 113.7(14) . . ? C45A C44A H44A 123.1 . . ? C43A C44A H44A 123.1 . . ? C46A C45A C44A 115.7(14) . . ? C46A C45A H45A 122.2 . . ? C44A C45A H45A 122.2 . . ? C47A C46A C45A 132(2) . . ? C47A C46A H46A 113.8 . . ? C45A C46A H46A 113.8 . . ? C46A C47A C48A 110(2) . . ? C46A C47A H47A 124.9 . . ? C48A C47A H47A 124.9 . . ? C47A C48A C43A 121(2) . . ? C47A C48A H48A 119.6 . . ? C43A C48A H48A 119.6 . . ? C44B C43B C49B 121.9(13) . . ? C44B C43B C48B 120.1(16) . . ? C49B C43B C48B 118.0(13) . . ? C43B C44B C45B 122.1(11) . . ? C43B C44B H44B 118.9 . . ? C45B C44B H44B 118.9 . . ? C46B C45B C44B 121.2(11) . . ? C46B C45B H45B 119.4 . . ? C44B C45B H45B 119.4 . . ? C45B C46B C47B 116.1(16) . . ? C45B C46B H46B 121.9 . . ? C47B C46B H46B 121.9 . . ? C48B C47B C46B 124.1(17) . . ? C48B C47B H47B 118.0 . . ? C46B C47B H47B 118.0 . . ? C43B C48B C47B 116.1(16) . . ? C43B C48B H48B 122.0 . . ? C47B C48B H48B 122.0 . . ? C43B C49B H49D 109.5 . . ? C43B C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? C43B C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 62.59 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.550 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.065 # Attachment '7_New.cif' data_08185o _database_code_depnum_ccdc_archive 'CCDC 713120' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H36 Cl5 N2 O7 P Ru' _chemical_formula_weight 978.01 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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.4579(2) _cell_length_b 15.0138(2) _cell_length_c 12.2822(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.677(2) _cell_angle_gamma 90.00 _cell_volume 2076.29(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9852 _cell_measurement_theta_min 3.0084 _cell_measurement_theta_max 32.4127 _exptl_crystal_description 'transparent block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93125 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S Ultra' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 16.1399 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30506 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 32.51 _reflns_number_total 12948 _reflns_number_gt 9320 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0541P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_number_reflns 12948 _refine_ls_number_parameters 518 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 C1 C 0.5431(4) 0.5385(3) 0.3800(3) 0.0345(9) Uani 1 1 d . . . H1 H 0.6088 0.5014 0.4088 0.041 Uiso 1 1 calc R . . C2 C 0.4289(4) 0.5103(3) 0.3451(3) 0.0348(9) Uani 1 1 d . . . H2 H 0.3997 0.4512 0.3464 0.042 Uiso 1 1 calc R . . C3 C 0.3642(3) 0.5861(3) 0.3071(3) 0.0300(8) Uani 1 1 d . . . C4 C 0.6553(4) 0.6786(3) 0.3765(4) 0.0410(10) Uani 1 1 d . . . H4A H 0.6890 0.6883 0.4549 0.062 Uiso 1 1 calc R . . H4B H 0.6370 0.7361 0.3397 0.062 Uiso 1 1 calc R . . H4C H 0.7128 0.6465 0.3412 0.062 Uiso 1 1 calc R . . C5 C 0.2417(4) 0.5892(3) 0.2440(4) 0.0317(9) Uani 1 1 d . . . C6 C 0.1504(3) 0.6411(3) 0.2733(3) 0.0310(8) Uani 1 1 d . . . C7 C 0.0411(4) 0.6466(3) 0.2052(4) 0.0402(10) Uani 1 1 d . . . H7 H -0.0192 0.6831 0.2253 0.048 Uiso 1 1 calc R . . C8 C 0.0188(4) 0.5983(3) 0.1060(4) 0.0471(11) Uani 1 1 d . . . H8 H -0.0559 0.6029 0.0576 0.057 Uiso 1 1 calc R . . C9 C 0.1069(4) 0.5435(3) 0.0791(4) 0.0480(12) Uani 1 1 d . . . H9 H 0.0915 0.5086 0.0136 0.058 Uiso 1 1 calc R . . C10 C 0.2171(4) 0.5398(3) 0.1475(4) 0.0364(10) Uani 1 1 d . . . H10 H 0.2770 0.5025 0.1279 0.044 Uiso 1 1 calc R . . C11 C 0.0966(3) 0.8407(2) 0.4959(3) 0.0250(7) Uani 1 1 d . . . C12 C 0.1297(3) 0.8331(2) 0.6084(3) 0.0238(7) Uani 1 1 d . . . C13 C 0.0350(3) 0.8220(2) 0.6712(3) 0.0273(8) Uani 1 1 d . . . C14 C -0.0845(3) 0.8254(3) 0.6144(4) 0.0318(8) Uani 1 1 d . . . C15 C -0.1098(3) 0.8376(3) 0.4977(4) 0.0343(9) Uani 1 1 d . . . H15 H -0.1901 0.8414 0.4605 0.041 Uiso 1 1 calc R . . C16 C -0.0213(3) 0.8438(3) 0.4386(3) 0.0331(8) Uani 1 1 d . . . H16 H -0.0387 0.8501 0.3603 0.040 Uiso 1 1 calc R . . C17 C 0.0573(3) 0.8026(3) 0.7859(3) 0.0328(8) Uani 1 1 d . . . H17 H 0.1369 0.7969 0.8243 0.039 Uiso 1 1 calc R . . C18 C -0.0338(3) 0.7921(4) 0.8425(3) 0.0409(8) Uani 1 1 d . . . H18 H -0.0175 0.7791 0.9195 0.049 Uiso 1 1 calc R . . C19 C -0.1528(3) 0.8005(4) 0.7856(4) 0.0414(10) Uani 1 1 d . . . H19 H -0.2159 0.7957 0.8257 0.050 Uiso 1 1 calc R . . C20 C -0.1776(3) 0.8155(3) 0.6751(4) 0.0363(10) Uani 1 1 d . . . H20 H -0.2579 0.8194 0.6380 0.044 Uiso 1 1 calc R . . C21 C 0.3360(3) 0.7774(2) 0.6263(3) 0.0277(9) Uani 1 1 d . . . C22 C 0.2568(3) 0.8327(2) 0.6621(3) 0.0245(7) Uani 1 1 d . . . C23 C 0.3005(3) 0.8900(3) 0.7546(3) 0.0276(8) Uani 1 1 d . . . C24 C 0.4168(3) 0.8771(3) 0.8164(3) 0.0326(8) Uani 1 1 d . . . C25 C 0.4896(3) 0.8109(3) 0.7808(3) 0.0366(11) Uani 1 1 d . . . H25 H 0.5658 0.7993 0.8240 0.044 Uiso 1 1 calc R . . C26 C 0.4530(3) 0.7643(3) 0.6873(4) 0.0343(9) Uani 1 1 d . . . H26 H 0.5048 0.7229 0.6622 0.041 Uiso 1 1 calc R . . C27 C 0.2340(4) 0.9637(3) 0.7836(4) 0.0348(9) Uani 1 1 d . . . H27 H 0.1576 0.9757 0.7411 0.042 Uiso 1 1 calc R . . C28 C 0.2788(4) 1.0180(3) 0.8723(4) 0.0394(10) Uani 1 1 d . . . H28 H 0.2334 1.0667 0.8910 0.047 Uiso 1 1 calc R . . C29 C 0.3925(4) 1.0004(3) 0.9347(4) 0.0455(12) Uani 1 1 d . . . H29 H 0.4225 1.0365 0.9971 0.055 Uiso 1 1 calc R . . C30 C 0.4587(4) 0.9339(3) 0.9076(4) 0.0405(10) Uani 1 1 d . . . H30 H 0.5357 0.9243 0.9502 0.049 Uiso 1 1 calc R . . C31 C 0.2962(3) 0.9175(2) 0.2109(3) 0.0289(8) Uani 1 1 d . . . C32 C 0.2359(3) 0.8385(3) 0.1623(3) 0.0301(8) Uani 1 1 d . . . H32 H 0.1533 0.8320 0.1615 0.036 Uiso 1 1 calc R . . C33 C 0.2955(3) 0.7726(2) 0.1171(3) 0.0299(9) Uani 1 1 d . . . H33 H 0.2530 0.7216 0.0859 0.036 Uiso 1 1 calc R . . C34 C 0.4204(3) 0.7790(3) 0.1161(3) 0.0329(9) Uani 1 1 d . . . C35 C 0.4812(4) 0.8542(3) 0.1663(3) 0.0352(9) Uani 1 1 d . . . H35 H 0.5642 0.8601 0.1688 0.042 Uiso 1 1 calc R . . C36 C 0.4186(3) 0.9208(3) 0.2129(3) 0.0325(8) Uani 1 1 d . . . H36 H 0.4619 0.9705 0.2473 0.039 Uiso 1 1 calc R . . C37 C 0.2283(5) 0.9931(3) 0.2506(4) 0.0433(13) Uani 1 1 d . . . H37 H 0.1662 0.9664 0.2880 0.052 Uiso 1 1 calc R . . C38 C 0.3017(7) 1.0547(4) 0.3316(6) 0.097(3) Uani 1 1 d . . . H38A H 0.3479 1.0200 0.3923 0.145 Uiso 1 1 calc R . . H38B H 0.2494 1.0960 0.3616 0.145 Uiso 1 1 calc R . . H38C H 0.3558 1.0885 0.2941 0.145 Uiso 1 1 calc R . . C39 C 0.1651(5) 1.0441(3) 0.1502(4) 0.0492(13) Uani 1 1 d . . . H39A H 0.2239 1.0706 0.1113 0.074 Uiso 1 1 calc R . . H39B H 0.1165 1.0913 0.1742 0.074 Uiso 1 1 calc R . . H39C H 0.1140 1.0033 0.1002 0.074 Uiso 1 1 calc R . . C40 C 0.4829(5) 0.7048(3) 0.0682(4) 0.0480(11) Uani 1 1 d . . . H40A H 0.5689 0.7113 0.0923 0.072 Uiso 1 1 calc R . . H40B H 0.4632 0.7072 -0.0129 0.072 Uiso 1 1 calc R . . H40C H 0.4574 0.6474 0.0939 0.072 Uiso 1 1 calc R . . C41 C 0.2037(10) 0.5392(6) 0.7229(9) 0.121(3) Uani 1 1 d . . . H41 H 0.1803 0.4822 0.7552 0.146 Uiso 1 1 calc R . . N1 N 0.5468(3) 0.6262(2) 0.3672(3) 0.0291(7) Uani 1 1 d . . . N2 N 0.4374(3) 0.6585(2) 0.3217(2) 0.0249(6) Uani 1 1 d . . . O1 O 0.1660(2) 0.68723(18) 0.3729(2) 0.0330(6) Uani 1 1 d . . . O2 O 0.1855(2) 0.84874(16) 0.4306(2) 0.0262(5) Uani 1 1 d . . . O3 O 0.3057(2) 0.72518(16) 0.5329(2) 0.0272(5) Uani 1 1 d . . . O4 O 0.7775(3) 0.8051(3) 0.2079(3) 0.0607(10) Uani 1 1 d . . . O5 O 0.9311(3) 0.8512(2) 0.1205(3) 0.0550(9) Uani 1 1 d . . . O6 O 0.7984(4) 0.7411(3) 0.0405(4) 0.0670(11) Uani 1 1 d . . . O7 O 0.7348(3) 0.8871(3) 0.0442(3) 0.0620(10) Uani 1 1 d . . . P1 P 0.26051(8) 0.76342(6) 0.41046(8) 0.02404(19) Uani 1 1 d . . . Cl1 Cl 0.51200(8) 0.84514(6) 0.45401(8) 0.0334(2) Uani 1 1 d . . . Cl2 Cl 0.81039(8) 0.82105(7) 0.10375(9) 0.0367(2) Uani 1 1 d . . . Cl3 Cl 0.3034(2) 0.5124(2) 0.6352(3) 0.1428(10) Uani 1 1 d . . . Cl4 Cl 0.2839(5) 0.6024(3) 0.8317(4) 0.1921(17) Uani 1 1 d . . . Cl5 Cl 0.0786(3) 0.58617(19) 0.6509(4) 0.1679(14) Uani 1 1 d . . . Ru1 Ru 0.38353(2) 0.793002(16) 0.29114(2) 0.02274(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(2) 0.035(2) 0.027(2) 0.0021(16) 0.0036(18) 0.0144(17) C2 0.046(2) 0.0246(19) 0.034(2) 0.0028(15) 0.0061(19) 0.0031(16) C3 0.037(2) 0.0282(19) 0.0263(19) -0.0010(14) 0.0100(16) 0.0029(15) C4 0.027(2) 0.044(2) 0.050(3) 0.002(2) 0.0027(19) 0.0027(17) C5 0.031(2) 0.030(2) 0.035(2) -0.0013(18) 0.0064(19) -0.0067(16) C6 0.034(2) 0.0286(19) 0.032(2) -0.0055(15) 0.0121(17) -0.0044(15) C7 0.029(2) 0.038(2) 0.053(3) -0.0115(19) 0.008(2) 0.0021(16) C8 0.028(2) 0.060(3) 0.051(3) -0.018(2) 0.001(2) -0.0083(19) C9 0.043(3) 0.050(3) 0.052(3) -0.027(2) 0.012(2) -0.008(2) C10 0.031(2) 0.033(2) 0.046(3) -0.0145(18) 0.0079(19) -0.0039(16) C11 0.0231(17) 0.0236(17) 0.0282(18) -0.0018(14) 0.0048(14) 0.0002(13) C12 0.0233(17) 0.0211(16) 0.0277(18) 0.0000(13) 0.0068(15) -0.0011(13) C13 0.0198(16) 0.0269(18) 0.035(2) -0.0018(13) 0.0039(15) 0.0005(12) C14 0.0236(18) 0.0301(18) 0.042(2) -0.0081(15) 0.0055(16) 0.0010(14) C15 0.0236(18) 0.033(2) 0.043(2) -0.0047(17) -0.0025(17) 0.0021(15) C16 0.032(2) 0.035(2) 0.029(2) 0.0006(16) -0.0035(16) 0.0018(16) C17 0.0257(16) 0.039(2) 0.0343(18) -0.0013(19) 0.0073(14) -0.0051(18) C18 0.0387(19) 0.043(2) 0.044(2) -0.002(3) 0.0152(16) -0.002(3) C19 0.0296(17) 0.044(3) 0.057(2) -0.009(3) 0.0224(18) -0.007(2) C20 0.0225(17) 0.042(3) 0.047(2) -0.0041(16) 0.0130(17) -0.0031(14) C21 0.0284(17) 0.031(3) 0.0246(16) 0.0107(14) 0.0073(14) 0.0043(14) C22 0.0193(16) 0.0303(17) 0.0245(17) 0.0040(14) 0.0056(14) 0.0007(13) C23 0.0259(18) 0.039(2) 0.0192(17) 0.0072(14) 0.0076(14) -0.0073(14) C24 0.0248(18) 0.051(2) 0.0224(19) 0.0107(16) 0.0056(15) -0.0032(16) C25 0.0210(16) 0.061(3) 0.0265(18) 0.0155(17) 0.0005(14) 0.0028(16) C26 0.0249(18) 0.044(2) 0.036(2) 0.0143(16) 0.0105(17) 0.0102(15) C27 0.035(2) 0.034(2) 0.040(2) 0.0005(17) 0.0189(19) -0.0017(16) C28 0.043(2) 0.044(3) 0.034(2) -0.0030(18) 0.014(2) -0.0091(19) C29 0.054(3) 0.058(3) 0.025(2) -0.0079(18) 0.010(2) -0.029(2) C30 0.034(2) 0.060(3) 0.026(2) 0.0071(18) 0.0006(17) -0.016(2) C31 0.037(2) 0.0249(18) 0.0242(18) 0.0062(14) 0.0049(16) 0.0013(15) C32 0.0280(19) 0.037(2) 0.0248(19) 0.0082(16) 0.0028(15) 0.0030(15) C33 0.039(2) 0.023(2) 0.0249(18) 0.0007(12) 0.0007(16) -0.0031(13) C34 0.0409(19) 0.039(3) 0.0211(16) 0.0041(15) 0.0110(15) 0.0075(17) C35 0.034(2) 0.038(2) 0.035(2) 0.0081(17) 0.0117(18) -0.0007(17) C36 0.037(2) 0.0276(19) 0.032(2) 0.0080(15) 0.0024(17) -0.0050(15) C37 0.069(4) 0.031(3) 0.032(3) 0.0086(19) 0.014(2) 0.015(2) C38 0.139(7) 0.064(4) 0.066(4) -0.032(3) -0.037(4) 0.048(4) C39 0.068(3) 0.035(2) 0.042(3) 0.0068(19) 0.004(3) 0.025(2) C40 0.062(3) 0.047(3) 0.039(3) 0.0053(19) 0.020(2) 0.011(2) C41 0.154(9) 0.074(5) 0.141(9) 0.000(5) 0.040(7) -0.002(5) N1 0.0283(16) 0.0345(18) 0.0247(16) 0.0022(12) 0.0059(13) 0.0046(13) N2 0.0239(15) 0.0317(16) 0.0196(14) 0.0014(11) 0.0057(12) 0.0020(12) O1 0.0326(14) 0.0337(14) 0.0357(15) -0.0094(12) 0.0142(12) -0.0086(11) O2 0.0286(13) 0.0294(13) 0.0210(12) 0.0000(10) 0.0054(10) 0.0067(10) O3 0.0325(14) 0.0247(13) 0.0256(13) 0.0044(10) 0.0087(11) 0.0046(10) O4 0.0443(16) 0.108(3) 0.0319(15) 0.004(2) 0.0115(13) -0.012(2) O5 0.0271(15) 0.067(2) 0.072(2) 0.0119(18) 0.0115(16) -0.0035(14) O6 0.067(3) 0.062(2) 0.076(3) -0.006(2) 0.026(2) -0.006(2) O7 0.0396(19) 0.071(2) 0.072(3) 0.022(2) 0.0011(18) 0.0138(17) P1 0.0275(5) 0.0224(4) 0.0233(4) -0.0004(3) 0.0074(4) 0.0009(3) Cl1 0.0363(5) 0.0362(5) 0.0259(4) -0.0012(4) 0.0011(4) -0.0072(4) Cl2 0.0250(4) 0.0487(6) 0.0376(5) 0.0089(4) 0.0090(4) 0.0006(4) Cl3 0.1062(17) 0.132(2) 0.188(3) -0.019(2) 0.0228(19) 0.0062(15) Cl4 0.280(5) 0.154(3) 0.149(3) 0.002(2) 0.056(3) -0.068(3) Cl5 0.153(2) 0.0983(18) 0.268(4) -0.018(2) 0.078(3) 0.0230(17) Ru1 0.02350(12) 0.02286(12) 0.02226(11) 0.00095(14) 0.00526(9) -0.00022(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.328(5) . ? C1 C2 1.366(6) . ? C1 H1 0.9500 . ? C2 C3 1.390(5) . ? C2 H2 0.9500 . ? C3 N2 1.364(5) . ? C3 C5 1.473(6) . ? C4 N1 1.457(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.382(6) . ? C5 C6 1.403(6) . ? C6 C7 1.374(6) . ? C6 O1 1.388(5) . ? C7 C8 1.400(7) . ? C7 H7 0.9500 . ? C8 C9 1.389(6) . ? C8 H8 0.9500 . ? C9 C10 1.382(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.368(5) . ? C11 C16 1.404(5) . ? C11 O2 1.414(4) . ? C12 C13 1.452(5) . ? C12 C22 1.484(5) . ? C13 C17 1.415(6) . ? C13 C14 1.419(5) . ? C14 C20 1.418(5) . ? C14 C15 1.420(6) . ? C15 C16 1.355(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.365(5) . ? C17 H17 0.9500 . ? C18 C19 1.418(6) . ? C18 H18 0.9500 . ? C19 C20 1.353(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.361(5) . ? C21 O3 1.380(5) . ? C21 C26 1.423(5) . ? C22 C23 1.439(5) . ? C23 C24 1.419(5) . ? C23 C27 1.426(5) . ? C24 C25 1.417(6) . ? C24 C30 1.418(6) . ? C25 C26 1.344(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.381(6) . ? C27 H27 0.9500 . ? C28 C29 1.409(7) . ? C28 H28 0.9500 . ? C29 C30 1.333(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.400(6) . ? C31 C32 1.443(6) . ? C31 C37 1.507(6) . ? C31 Ru1 2.258(4) . ? C32 C33 1.377(5) . ? C32 Ru1 2.200(4) . ? C32 H32 0.9500 . ? C33 C34 1.437(5) . ? C33 Ru1 2.209(4) . ? C33 H33 0.9500 . ? C34 C35 1.408(6) . ? C34 C40 1.502(6) . ? C34 Ru1 2.276(3) . ? C35 C36 1.413(6) . ? C35 Ru1 2.255(4) . ? C35 H35 0.9500 . ? C36 Ru1 2.216(4) . ? C36 H36 0.9500 . ? C37 C38 1.498(8) . ? C37 C39 1.518(7) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 Cl5 1.692(11) . ? C41 Cl4 1.754(11) . ? C41 Cl3 1.755(11) . ? C41 H41 1.0000 . ? N1 N2 1.363(4) . ? N2 Ru1 2.125(3) . ? O1 P1 1.584(3) . ? O2 P1 1.587(3) . ? O3 P1 1.603(3) . ? O4 Cl2 1.420(3) . ? O5 Cl2 1.434(3) . ? O6 Cl2 1.422(4) . ? O7 Cl2 1.426(3) . ? P1 Ru1 2.2577(10) . ? Cl1 Ru1 2.3853(9) . ? 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 C1 C2 108.6(3) . . ? N1 C1 H1 125.7 . . ? C2 C1 H1 125.7 . . ? C1 C2 C3 105.8(3) . . ? C1 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? N2 C3 C2 109.3(4) . . ? N2 C3 C5 123.2(3) . . ? C2 C3 C5 126.8(4) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 118.4(4) . . ? C10 C5 C3 117.2(4) . . ? C6 C5 C3 124.4(4) . . ? C7 C6 O1 117.4(3) . . ? C7 C6 C5 121.0(4) . . ? O1 C6 C5 121.5(4) . . ? C6 C7 C8 119.9(4) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 119.3(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 120.2(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C5 121.2(4) . . ? C9 C10 H10 119.4 . . ? C5 C10 H10 119.4 . . ? C12 C11 C16 124.8(3) . . ? C12 C11 O2 119.1(3) . . ? C16 C11 O2 116.1(3) . . ? C11 C12 C13 116.8(3) . . ? C11 C12 C22 121.0(3) . . ? C13 C12 C22 122.1(3) . . ? C17 C13 C14 118.5(3) . . ? C17 C13 C12 122.6(3) . . ? C14 C13 C12 118.9(4) . . ? C20 C14 C13 119.3(4) . . ? C20 C14 C15 120.8(4) . . ? C13 C14 C15 119.9(4) . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 118.4(4) . . ? C15 C16 H16 120.8 . . ? C11 C16 H16 120.8 . . ? C18 C17 C13 121.1(4) . . ? C18 C17 H17 119.4 . . ? C13 C17 H17 119.4 . . ? C17 C18 C19 119.7(4) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C14 120.5(4) . . ? C19 C20 H20 119.8 . . ? C14 C20 H20 119.8 . . ? C22 C21 O3 122.3(3) . . ? C22 C21 C26 122.3(4) . . ? O3 C21 C26 115.3(3) . . ? C21 C22 C23 117.7(3) . . ? C21 C22 C12 121.2(3) . . ? C23 C22 C12 121.2(3) . . ? C24 C23 C27 117.7(4) . . ? C24 C23 C22 119.7(3) . . ? C27 C23 C22 122.5(3) . . ? C25 C24 C30 122.2(4) . . ? C25 C24 C23 118.6(4) . . ? C30 C24 C23 119.2(4) . . ? C26 C25 C24 121.4(3) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C21 119.5(4) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? C28 C27 C23 121.2(4) . . ? C28 C27 H27 119.4 . . ? C23 C27 H27 119.4 . . ? C27 C28 C29 119.3(4) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 121.1(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C24 121.5(4) . . ? C29 C30 H30 119.3 . . ? C24 C30 H30 119.3 . . ? C36 C31 C32 116.0(3) . . ? C36 C31 C37 122.9(4) . . ? C32 C31 C37 121.1(4) . . ? C36 C31 Ru1 70.2(2) . . ? C32 C31 Ru1 68.9(2) . . ? C37 C31 Ru1 134.1(3) . . ? C33 C32 C31 121.5(3) . . ? C33 C32 Ru1 72.2(2) . . ? C31 C32 Ru1 73.3(2) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? Ru1 C32 H32 127.4 . . ? C32 C33 C34 121.6(3) . . ? C32 C33 Ru1 71.4(2) . . ? C34 C33 Ru1 73.9(2) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? Ru1 C33 H33 127.7 . . ? C35 C34 C33 117.6(3) . . ? C35 C34 C40 122.2(4) . . ? C33 C34 C40 120.1(4) . . ? C35 C34 Ru1 71.1(2) . . ? C33 C34 Ru1 68.8(2) . . ? C40 C34 Ru1 128.6(3) . . ? C34 C35 C36 119.9(4) . . ? C34 C35 Ru1 72.7(2) . . ? C36 C35 Ru1 70.1(2) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? Ru1 C35 H35 129.5 . . ? C31 C36 C35 123.4(4) . . ? C31 C36 Ru1 73.4(2) . . ? C35 C36 Ru1 73.1(2) . . ? C31 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? Ru1 C36 H36 127.4 . . ? C38 C37 C31 114.9(5) . . ? C38 C37 C39 110.6(4) . . ? C31 C37 C39 108.3(4) . . ? C38 C37 H37 107.6 . . ? C31 C37 H37 107.6 . . ? C39 C37 H37 107.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Cl5 C41 Cl4 116.5(6) . . ? Cl5 C41 Cl3 111.1(6) . . ? Cl4 C41 Cl3 106.4(6) . . ? Cl5 C41 H41 107.5 . . ? Cl4 C41 H41 107.5 . . ? Cl3 C41 H41 107.5 . . ? C1 N1 N2 110.7(3) . . ? C1 N1 C4 124.9(3) . . ? N2 N1 C4 123.1(3) . . ? N1 N2 C3 105.5(3) . . ? N1 N2 Ru1 128.7(2) . . ? C3 N2 Ru1 125.6(2) . . ? C6 O1 P1 125.9(2) . . ? C11 O2 P1 119.1(2) . . ? C21 O3 P1 124.4(2) . . ? O1 P1 O2 105.49(14) . . ? O1 P1 O3 95.69(14) . . ? O2 P1 O3 103.48(14) . . ? O1 P1 Ru1 115.37(11) . . ? O2 P1 Ru1 111.31(10) . . ? O3 P1 Ru1 123.19(10) . . ? O4 Cl2 O6 109.6(3) . . ? O4 Cl2 O7 110.0(2) . . ? O6 Cl2 O7 108.5(3) . . ? O4 Cl2 O5 109.5(2) . . ? O6 Cl2 O5 109.7(2) . . ? O7 Cl2 O5 109.4(2) . . ? N2 Ru1 C32 125.60(13) . . ? N2 Ru1 C33 96.01(12) . . ? C32 Ru1 C33 36.39(14) . . ? N2 Ru1 C36 146.05(13) . . ? C32 Ru1 C36 66.17(14) . . ? C33 Ru1 C36 77.74(14) . . ? N2 Ru1 C35 110.04(13) . . ? C32 Ru1 C35 78.26(14) . . ? C33 Ru1 C35 66.03(15) . . ? C36 Ru1 C35 36.82(15) . . ? N2 Ru1 P1 83.93(8) . . ? C32 Ru1 P1 92.22(10) . . ? C33 Ru1 P1 111.88(11) . . ? C36 Ru1 P1 129.58(11) . . ? C35 Ru1 P1 165.90(11) . . ? N2 Ru1 C31 162.64(12) . . ? C32 Ru1 C31 37.76(14) . . ? C33 Ru1 C31 66.84(13) . . ? C36 Ru1 C31 36.44(14) . . ? C35 Ru1 C31 66.53(14) . . ? P1 Ru1 C31 99.59(10) . . ? N2 Ru1 C34 88.87(13) . . ? C32 Ru1 C34 66.54(14) . . ? C33 Ru1 C34 37.32(14) . . ? C36 Ru1 C34 65.80(15) . . ? C35 Ru1 C34 36.19(15) . . ? P1 Ru1 C34 147.38(11) . . ? C31 Ru1 C34 79.00(14) . . ? N2 Ru1 Cl1 92.85(9) . . ? C32 Ru1 Cl1 140.70(11) . . ? C33 Ru1 Cl1 163.15(10) . . ? C36 Ru1 Cl1 86.91(11) . . ? C35 Ru1 Cl1 97.45(11) . . ? P1 Ru1 Cl1 83.26(3) . . ? C31 Ru1 Cl1 104.43(10) . . ? C34 Ru1 Cl1 128.96(10) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 32.51 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.026 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.092