# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email est@soton.ac.uk _publ_contact_author_name 'Eugen Stulz' loop_ _publ_author_name 'Eugen Stulz' 'Jeremy Sanders' 'Andrew Bond' data_P2_Rh3 _database_code_depnum_ccdc_archive 'CCDC 834653' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H74 N4 P2 Rh +, I -, C H2 Cl2' _chemical_formula_sum 'C85 H76 Cl2 I N4 P2 Rh' _chemical_formula_weight 1516.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 26.5305(5) _cell_length_b 12.1202(3) _cell_length_c 22.0169(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.010(2) _cell_angle_gamma 90.00 _cell_volume 7062.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17262 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 22.46 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.950 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 18772 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 22.48 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 4581 _reflns_number_gt 3760 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _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^)+(0.0503P)^2^+5.3690P] 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 4581 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.688 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.122 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 I1 I 0.0000 0.36173(4) 0.2500 0.04011(16) Uani 1 2 d S . . Rh1 Rh 0.2500 0.2500 0.0000 0.01941(15) Uani 1 2 d S . . P1 P 0.21238(4) 0.11526(9) 0.06030(4) 0.0243(3) Uani 1 1 d . . . N1 N 0.24269(12) 0.1369(3) -0.06933(13) 0.0235(8) Uani 1 1 d . . . N2 N 0.32141(12) 0.1899(3) 0.01897(13) 0.0232(8) Uani 1 1 d . . . C1 C 0.20010(15) 0.1281(3) -0.10854(16) 0.0244(10) Uani 1 1 d . . . C2 C 0.20819(15) 0.0473(3) -0.15481(17) 0.0281(10) Uani 1 1 d . . . C3 C 0.25594(15) 0.0068(4) -0.14392(17) 0.0278(10) Uani 1 1 d . . . C4 C 0.27764(14) 0.0626(3) -0.08840(16) 0.0227(9) Uani 1 1 d . . . C5 C 0.32547(15) 0.0457(3) -0.05955(16) 0.0248(10) Uani 1 1 d . . . C6 C 0.34556(14) 0.1038(3) -0.00822(17) 0.0246(10) Uani 1 1 d . . . C7 C 0.39544(15) 0.0879(4) 0.02391(17) 0.0301(10) Uani 1 1 d . . . C8 C 0.40053(15) 0.1680(4) 0.06759(17) 0.0278(10) Uani 1 1 d . . . C9 C 0.35413(14) 0.2300(3) 0.06492(16) 0.0232(9) Uani 1 1 d . . . C10 C 0.34384(15) 0.3119(3) 0.10532(17) 0.0254(10) Uani 1 1 d . . . H10A H 0.3704 0.3295 0.1349 0.030 Uiso 1 1 calc R . . C11 C 0.27949(17) -0.0725(4) -0.18625(19) 0.0414(12) Uani 1 1 d . . . H11A H 0.2558 -0.0869 -0.2215 0.062 Uiso 1 1 calc R . . H11B H 0.2874 -0.1419 -0.1648 0.062 Uiso 1 1 calc R . . H11C H 0.3106 -0.0404 -0.2000 0.062 Uiso 1 1 calc R . . C12 C 0.43324(18) -0.0026(5) 0.0168(2) 0.0532(14) Uani 1 1 d . . . H12A H 0.4589 -0.0004 0.0510 0.080 Uiso 1 1 calc R . . H12B H 0.4495 0.0078 -0.0214 0.080 Uiso 1 1 calc R . . H12C H 0.4160 -0.0741 0.0161 0.080 Uiso 1 1 calc R . . C13 C 0.17098(16) 0.0206(4) -0.20773(18) 0.0370(11) Uani 1 1 d . . . H13A H 0.1363 0.0283 -0.1944 0.044 Uiso 1 1 calc R . . H13B H 0.1756 -0.0573 -0.2197 0.044 Uiso 1 1 calc R . . C14 C 0.1763(2) 0.0932(5) -0.2626(2) 0.0574(15) Uani 1 1 d . . . H14A H 0.1496 0.0754 -0.2941 0.086 Uiso 1 1 calc R . . H14B H 0.2094 0.0807 -0.2786 0.086 Uiso 1 1 calc R . . H14C H 0.1734 0.1708 -0.2508 0.086 Uiso 1 1 calc R . . C15 C 0.44494(16) 0.1919(4) 0.11264(18) 0.0382(12) Uani 1 1 d . . . H15A H 0.4498 0.2727 0.1155 0.046 Uiso 1 1 calc R . . H15B H 0.4758 0.1598 0.0970 0.046 Uiso 1 1 calc R . . C16 C 0.43875(19) 0.1465(5) 0.1760(2) 0.0512(14) Uani 1 1 d . . . H16A H 0.4666 0.1727 0.2039 0.077 Uiso 1 1 calc R . . H16B H 0.4392 0.0656 0.1747 0.077 Uiso 1 1 calc R . . H16C H 0.4065 0.1717 0.1902 0.077 Uiso 1 1 calc R . . C17 C 0.35801(14) -0.0409(3) -0.08600(16) 0.0245(10) Uani 1 1 d . . . C18 C 0.39345(15) -0.0100(4) -0.12633(17) 0.0302(10) Uani 1 1 d . . . H18A H 0.3983 0.0659 -0.1350 0.036 Uiso 1 1 calc R . . C19 C 0.42152(17) -0.0888(4) -0.15385(19) 0.0376(11) Uani 1 1 d . . . H19A H 0.4458 -0.0675 -0.1813 0.045 Uiso 1 1 calc R . . C20 C 0.41414(18) -0.1993(4) -0.1413(2) 0.0421(12) Uani 1 1 d . . . H20A H 0.4331 -0.2538 -0.1608 0.051 Uiso 1 1 calc R . . C21 C 0.37984(18) -0.2308(4) -0.1011(2) 0.0397(12) Uani 1 1 d . . . H21A H 0.3751 -0.3067 -0.0923 0.048 Uiso 1 1 calc R . . C22 C 0.35208(17) -0.1513(4) -0.07322(19) 0.0341(11) Uani 1 1 d . . . H22A H 0.3286 -0.1730 -0.0449 0.041 Uiso 1 1 calc R . . C23 C 0.18266(15) 0.1683(3) 0.12641(17) 0.0261(10) Uani 1 1 d . . . C24 C 0.13062(16) 0.1632(4) 0.12962(18) 0.0340(11) Uani 1 1 d . . . H24A H 0.1103 0.1273 0.0984 0.041 Uiso 1 1 calc R . . C25 C 0.10834(17) 0.2104(4) 0.17847(19) 0.0367(11) Uani 1 1 d . . . H25A H 0.0727 0.2068 0.1805 0.044 Uiso 1 1 calc R . . C26 C 0.13733(17) 0.2624(4) 0.22397(19) 0.0355(11) Uani 1 1 d . . . H26A H 0.1217 0.2943 0.2573 0.043 Uiso 1 1 calc R . . C27 C 0.18901(17) 0.2683(4) 0.22152(18) 0.0331(11) Uani 1 1 d . . . H27A H 0.2090 0.3044 0.2531 0.040 Uiso 1 1 calc R . . C28 C 0.21193(16) 0.2216(4) 0.17277(17) 0.0303(10) Uani 1 1 d . . . H28A H 0.2475 0.2259 0.1710 0.036 Uiso 1 1 calc R . . C29 C 0.25359(15) 0.0020(4) 0.08604(17) 0.0271(10) Uani 1 1 d . . . C30 C 0.24525(18) -0.1050(4) 0.06511(19) 0.0378(11) Uani 1 1 d . . . H30A H 0.2167 -0.1207 0.0380 0.045 Uiso 1 1 calc R . . C31 C 0.2781(2) -0.1885(4) 0.0833(2) 0.0503(14) Uani 1 1 d . . . H31A H 0.2720 -0.2615 0.0689 0.060 Uiso 1 1 calc R . . C32 C 0.3200(2) -0.1666(5) 0.1227(2) 0.0501(14) Uani 1 1 d . . . H32A H 0.3424 -0.2246 0.1354 0.060 Uiso 1 1 calc R . . C33 C 0.32919(18) -0.0602(4) 0.1432(2) 0.0422(12) Uani 1 1 d . . . H33A H 0.3581 -0.0448 0.1697 0.051 Uiso 1 1 calc R . . C34 C 0.29634(16) 0.0234(4) 0.12517(18) 0.0349(11) Uani 1 1 d . . . H34A H 0.3028 0.0964 0.1394 0.042 Uiso 1 1 calc R . . C35 C 0.16214(16) 0.0456(4) 0.02130(18) 0.0300(10) Uani 1 1 d . . . C36 C 0.12743(17) -0.0067(4) -0.00063(18) 0.0327(10) Uani 1 1 d . . . C37 C 0.08700(16) -0.0755(4) -0.02785(19) 0.0344(11) Uani 1 1 d . . . C38 C 0.04532(19) -0.1004(5) 0.0048(2) 0.0542(14) Uani 1 1 d . . . H38A H 0.0416 -0.0687 0.0437 0.065 Uiso 1 1 calc R . . C39 C 0.0090(2) -0.1732(5) -0.0212(3) 0.0721(19) Uani 1 1 d . . . H39A H -0.0196 -0.1916 0.0005 0.086 Uiso 1 1 calc R . . C40 C 0.0142(2) -0.2189(5) -0.0781(3) 0.0679(18) Uani 1 1 d . . . H40A H -0.0104 -0.2690 -0.0952 0.082 Uiso 1 1 calc R . . C41 C 0.0545(2) -0.1916(5) -0.1089(3) 0.0707(18) Uani 1 1 d . . . H41A H 0.0579 -0.2220 -0.1481 0.085 Uiso 1 1 calc R . . C42 C 0.0908(2) -0.1208(5) -0.0846(2) 0.0546(14) Uani 1 1 d . . . H42A H 0.1188 -0.1028 -0.1072 0.065 Uiso 1 1 calc R . . C100 C 0.0000 0.0335(9) 0.2500 0.143(5) Uani 1 2 d S . . H10B H -0.0294 0.0819 0.2394 0.171 Uiso 0.50 1 calc PR . . H10C H 0.0294 0.0819 0.2606 0.171 Uiso 0.50 1 calc PR . . Cl1 Cl 0.01231(14) -0.0398(2) 0.18671(14) 0.1730(13) 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 I1 0.0384(3) 0.0329(3) 0.0505(3) 0.000 0.01327(19) 0.000 Rh1 0.0185(3) 0.0206(3) 0.0187(2) -0.00084(18) -0.00085(17) 0.00230(19) P1 0.0242(6) 0.0254(7) 0.0232(5) 0.0007(4) 0.0004(4) -0.0006(5) N1 0.0253(19) 0.024(2) 0.0208(17) -0.0010(14) 0.0004(14) 0.0004(16) N2 0.0190(18) 0.027(2) 0.0229(17) 0.0005(15) -0.0017(14) 0.0031(16) C1 0.026(2) 0.028(3) 0.019(2) 0.0010(17) -0.0023(17) -0.001(2) C2 0.029(3) 0.027(3) 0.028(2) -0.0024(18) -0.0022(18) -0.001(2) C3 0.031(3) 0.026(3) 0.026(2) -0.0024(18) 0.0010(17) 0.001(2) C4 0.024(2) 0.020(2) 0.024(2) 0.0005(17) 0.0042(17) 0.0033(19) C5 0.025(2) 0.025(2) 0.025(2) 0.0025(18) 0.0051(17) 0.0027(19) C6 0.021(2) 0.026(3) 0.028(2) 0.0020(18) 0.0042(17) 0.0047(19) C7 0.025(2) 0.038(3) 0.027(2) 0.001(2) -0.0007(17) 0.008(2) C8 0.021(2) 0.034(3) 0.028(2) 0.0033(19) -0.0033(17) 0.003(2) C9 0.020(2) 0.023(2) 0.026(2) 0.0026(18) -0.0003(17) 0.0026(19) C10 0.022(2) 0.030(3) 0.024(2) 0.0019(18) -0.0073(16) 0.000(2) C11 0.042(3) 0.041(3) 0.040(3) -0.015(2) -0.007(2) 0.011(2) C12 0.038(3) 0.068(4) 0.052(3) -0.018(3) -0.014(2) 0.028(3) C13 0.036(3) 0.039(3) 0.034(2) -0.014(2) -0.0090(19) 0.006(2) C14 0.065(4) 0.064(4) 0.040(3) -0.001(3) -0.020(2) -0.004(3) C15 0.023(2) 0.053(3) 0.038(3) -0.010(2) -0.0064(19) 0.007(2) C16 0.045(3) 0.063(4) 0.043(3) 0.005(3) -0.014(2) 0.009(3) C17 0.023(2) 0.025(3) 0.025(2) -0.0004(18) -0.0003(17) 0.0039(19) C18 0.029(2) 0.031(3) 0.031(2) 0.0013(19) -0.0003(19) 0.003(2) C19 0.033(3) 0.043(3) 0.038(3) -0.004(2) 0.0114(19) 0.008(2) C20 0.040(3) 0.037(3) 0.050(3) -0.011(2) 0.004(2) 0.015(2) C21 0.047(3) 0.023(3) 0.049(3) 0.001(2) 0.003(2) 0.010(2) C22 0.037(3) 0.032(3) 0.034(2) 0.005(2) 0.0066(19) 0.002(2) C23 0.028(3) 0.025(3) 0.026(2) 0.0044(18) 0.0026(17) 0.003(2) C24 0.028(3) 0.042(3) 0.032(2) -0.001(2) -0.0013(19) 0.004(2) C25 0.027(3) 0.040(3) 0.044(3) 0.001(2) 0.008(2) 0.004(2) C26 0.038(3) 0.039(3) 0.030(2) 0.004(2) 0.012(2) 0.010(2) C27 0.041(3) 0.031(3) 0.027(2) 0.0004(19) 0.0002(19) -0.002(2) C28 0.028(2) 0.033(3) 0.031(2) 0.003(2) 0.0053(19) -0.002(2) C29 0.026(2) 0.029(3) 0.027(2) 0.0064(19) 0.0078(17) 0.006(2) C30 0.046(3) 0.033(3) 0.034(2) 0.000(2) 0.000(2) 0.006(2) C31 0.073(4) 0.033(3) 0.044(3) -0.007(2) -0.003(3) 0.014(3) C32 0.060(4) 0.050(4) 0.041(3) 0.012(2) 0.010(3) 0.026(3) C33 0.042(3) 0.041(3) 0.043(3) 0.014(2) -0.002(2) 0.006(3) C34 0.039(3) 0.026(3) 0.038(2) 0.010(2) 0.000(2) 0.000(2) C35 0.029(3) 0.031(3) 0.030(2) 0.000(2) 0.0021(19) 0.000(2) C36 0.035(3) 0.032(3) 0.031(2) 0.005(2) 0.003(2) 0.001(2) C37 0.031(3) 0.025(3) 0.045(3) 0.003(2) -0.009(2) -0.003(2) C38 0.041(3) 0.070(4) 0.051(3) 0.013(3) -0.003(2) -0.018(3) C39 0.040(3) 0.080(5) 0.094(5) 0.037(4) -0.010(3) -0.025(3) C40 0.058(4) 0.042(4) 0.098(5) 0.005(3) -0.038(4) -0.009(3) C41 0.060(4) 0.063(4) 0.086(4) -0.032(3) -0.021(4) 0.003(4) C42 0.047(3) 0.055(4) 0.061(3) -0.024(3) -0.003(3) -0.004(3) C100 0.252(17) 0.044(7) 0.133(10) 0.000 0.022(10) 0.000 Cl1 0.257(4) 0.0784(17) 0.186(3) -0.0384(17) 0.033(2) 0.037(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 Rh1 N2 2.046(3) 7 ? Rh1 N2 2.046(3) . ? Rh1 N1 2.051(3) 7 ? Rh1 N1 2.051(3) . ? Rh1 P1 2.3688(10) . ? Rh1 P1 2.3688(10) 7 ? P1 C35 1.751(5) . ? P1 C23 1.820(4) . ? P1 C29 1.821(4) . ? N1 C1 1.377(5) . ? N1 C4 1.378(5) . ? N2 C9 1.375(5) . ? N2 C6 1.382(5) . ? C1 C10 1.380(6) 7 ? C1 C2 1.440(6) . ? C2 C3 1.364(6) . ? C2 C13 1.509(5) . ? C3 C4 1.479(5) . ? C3 C11 1.504(6) . ? C4 C5 1.394(5) . ? C5 C6 1.404(5) . ? C5 C17 1.502(6) . ? C6 C7 1.469(5) . ? C7 C8 1.367(6) . ? C7 C12 1.501(6) . ? C8 C9 1.440(6) . ? C8 C15 1.514(6) . ? C9 C10 1.373(6) . ? C10 C1 1.380(6) 7 ? C10 H10A 0.9500 . ? 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 C14 1.510(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.519(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.378(6) . ? C17 C18 1.389(6) . ? C18 C19 1.378(6) . ? C18 H18A 0.9500 . ? C19 C20 1.384(7) . ? C19 H19A 0.9500 . ? C20 C21 1.368(7) . ? C20 H20A 0.9500 . ? C21 C22 1.382(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.389(6) . ? C23 C28 1.397(6) . ? C24 C25 1.387(6) . ? C24 H24A 0.9500 . ? C25 C26 1.372(6) . ? C25 H25A 0.9500 . ? C26 C27 1.378(6) . ? C26 H26A 0.9500 . ? C27 C28 1.391(6) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.389(6) . ? C29 C34 1.400(6) . ? C30 C31 1.377(7) . ? C30 H30A 0.9500 . ? C31 C32 1.387(7) . ? C31 H31A 0.9500 . ? C32 C33 1.382(7) . ? C32 H32A 0.9500 . ? C33 C34 1.377(6) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.192(6) . ? C36 C37 1.455(6) . ? C37 C42 1.374(6) . ? C37 C38 1.393(7) . ? C38 C39 1.399(8) . ? C38 H38A 0.9500 . ? C39 C40 1.385(9) . ? C39 H39A 0.9500 . ? C40 C41 1.347(9) . ? C40 H40A 0.9500 . ? C41 C42 1.369(8) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C100 Cl1 1.703(6) . ? C100 Cl1 1.703(6) 2 ? C100 H10B 0.9900 . ? C100 H10C 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 N2 Rh1 N2 180.00(19) 7 . ? N2 Rh1 N1 87.24(12) 7 7 ? N2 Rh1 N1 92.76(12) . 7 ? N2 Rh1 N1 92.76(12) 7 . ? N2 Rh1 N1 87.24(12) . . ? N1 Rh1 N1 180.00(17) 7 . ? N2 Rh1 P1 86.53(9) 7 . ? N2 Rh1 P1 93.47(9) . . ? N1 Rh1 P1 93.75(9) 7 . ? N1 Rh1 P1 86.25(9) . . ? N2 Rh1 P1 93.47(9) 7 7 ? N2 Rh1 P1 86.53(9) . 7 ? N1 Rh1 P1 86.25(9) 7 7 ? N1 Rh1 P1 93.75(9) . 7 ? P1 Rh1 P1 180.00(7) . 7 ? C35 P1 C23 101.83(19) . . ? C35 P1 C29 102.1(2) . . ? C23 P1 C29 107.56(17) . . ? C35 P1 Rh1 113.18(14) . . ? C23 P1 Rh1 115.32(14) . . ? C29 P1 Rh1 115.27(13) . . ? C1 N1 C4 107.4(3) . . ? C1 N1 Rh1 123.3(3) . . ? C4 N1 Rh1 129.2(2) . . ? C9 N2 C6 107.3(3) . . ? C9 N2 Rh1 123.5(3) . . ? C6 N2 Rh1 129.1(2) . . ? N1 C1 C10 125.9(3) . 7 ? N1 C1 C2 109.9(3) . . ? C10 C1 C2 124.3(3) 7 . ? C3 C2 C1 107.6(3) . . ? C3 C2 C13 127.4(4) . . ? C1 C2 C13 124.8(4) . . ? C2 C3 C4 106.5(3) . . ? C2 C3 C11 122.8(3) . . ? C4 C3 C11 130.5(4) . . ? N1 C4 C5 124.6(3) . . ? N1 C4 C3 108.6(3) . . ? C5 C4 C3 126.8(4) . . ? C4 C5 C6 125.1(4) . . ? C4 C5 C17 117.1(3) . . ? C6 C5 C17 117.8(3) . . ? N2 C6 C5 124.4(3) . . ? N2 C6 C7 108.6(3) . . ? C5 C6 C7 126.9(4) . . ? C8 C7 C6 106.7(4) . . ? C8 C7 C12 124.0(4) . . ? C6 C7 C12 129.2(4) . . ? C7 C8 C9 107.5(3) . . ? C7 C8 C15 129.1(4) . . ? C9 C8 C15 123.4(4) . . ? C10 C9 N2 126.1(4) . . ? C10 C9 C8 124.0(3) . . ? N2 C9 C8 109.8(3) . . ? C9 C10 C1 128.4(4) . 7 ? C9 C10 H10A 115.8 . . ? C1 C10 H10A 115.8 7 . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 C13 C14 113.6(4) . . ? C2 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C2 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C15 C16 113.8(4) . . ? C8 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C8 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 119.0(4) . . ? C22 C17 C5 121.5(4) . . ? C18 C17 C5 119.5(4) . . ? C19 C18 C17 120.3(4) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C17 C22 C21 120.9(4) . . ? C17 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C24 C23 C28 119.2(4) . . ? C24 C23 P1 120.8(3) . . ? C28 C23 P1 119.9(3) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C23 120.1(4) . . ? C27 C28 H28A 119.9 . . ? C23 C28 H28A 119.9 . . ? C30 C29 C34 118.7(4) . . ? C30 C29 P1 121.5(3) . . ? C34 C29 P1 119.7(3) . . ? C31 C30 C29 120.5(4) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C30 C31 C32 120.3(5) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C33 C32 C31 119.8(5) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C29 120.7(4) . . ? C33 C34 H34A 119.7 . . ? C29 C34 H34A 119.7 . . ? C36 C35 P1 174.3(4) . . ? C35 C36 C37 176.8(5) . . ? C42 C37 C38 119.5(4) . . ? C42 C37 C36 120.3(4) . . ? C38 C37 C36 120.1(4) . . ? C37 C38 C39 118.3(5) . . ? C37 C38 H38A 120.8 . . ? C39 C38 H38A 120.8 . . ? C40 C39 C38 120.8(6) . . ? C40 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? C41 C40 C39 119.3(5) . . ? C41 C40 H40A 120.3 . . ? C39 C40 H40A 120.3 . . ? C40 C41 C42 121.2(6) . . ? C40 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C41 C42 C37 120.8(6) . . ? C41 C42 H42A 119.6 . . ? C37 C42 H42A 119.6 . . ? Cl1 C100 Cl1 117.1(6) . 2 ? Cl1 C100 H10B 108.0 . . ? Cl1 C100 H10B 108.0 2 . ? Cl1 C100 H10C 108.0 . . ? Cl1 C100 H10C 108.0 2 . ? H10B C100 H10C 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Rh1 P1 C35 51.85(18) 7 . . . ? N2 Rh1 P1 C35 -128.15(18) . . . . ? N1 Rh1 P1 C35 138.84(18) 7 . . . ? N1 Rh1 P1 C35 -41.16(18) . . . . ? N2 Rh1 P1 C23 -64.85(16) 7 . . . ? N2 Rh1 P1 C23 115.15(16) . . . . ? N1 Rh1 P1 C23 22.15(17) 7 . . . ? N1 Rh1 P1 C23 -157.85(17) . . . . ? N2 Rh1 P1 C29 168.82(17) 7 . . . ? N2 Rh1 P1 C29 -11.18(17) . . . . ? N1 Rh1 P1 C29 -104.18(17) 7 . . . ? N1 Rh1 P1 C29 75.82(17) . . . . ? N2 Rh1 N1 C1 1.9(3) 7 . . . ? N2 Rh1 N1 C1 -178.1(3) . . . . ? P1 Rh1 N1 C1 88.3(3) . . . . ? P1 Rh1 N1 C1 -91.7(3) 7 . . . ? N2 Rh1 N1 C4 177.6(3) 7 . . . ? N2 Rh1 N1 C4 -2.4(3) . . . . ? P1 Rh1 N1 C4 -96.0(3) . . . . ? P1 Rh1 N1 C4 84.0(3) 7 . . . ? N1 Rh1 N2 C9 -0.7(3) 7 . . . ? N1 Rh1 N2 C9 179.3(3) . . . . ? P1 Rh1 N2 C9 -94.6(3) . . . . ? P1 Rh1 N2 C9 85.4(3) 7 . . . ? N1 Rh1 N2 C6 177.3(3) 7 . . . ? N1 Rh1 N2 C6 -2.7(3) . . . . ? P1 Rh1 N2 C6 83.4(3) . . . . ? P1 Rh1 N2 C6 -96.6(3) 7 . . . ? C4 N1 C1 C10 179.9(4) . . . 7 ? Rh1 N1 C1 C10 -3.6(5) . . . 7 ? C4 N1 C1 C2 -1.0(4) . . . . ? Rh1 N1 C1 C2 175.5(3) . . . . ? N1 C1 C2 C3 -0.2(5) . . . . ? C10 C1 C2 C3 179.0(4) 7 . . . ? N1 C1 C2 C13 -176.1(4) . . . . ? C10 C1 C2 C13 3.0(7) 7 . . . ? C1 C2 C3 C4 1.2(5) . . . . ? C13 C2 C3 C4 177.0(4) . . . . ? C1 C2 C3 C11 -174.5(4) . . . . ? C13 C2 C3 C11 1.4(7) . . . . ? C1 N1 C4 C5 -178.9(4) . . . . ? Rh1 N1 C4 C5 4.9(6) . . . . ? C1 N1 C4 C3 1.8(4) . . . . ? Rh1 N1 C4 C3 -174.5(3) . . . . ? C2 C3 C4 N1 -1.9(4) . . . . ? C11 C3 C4 N1 173.4(4) . . . . ? C2 C3 C4 C5 178.8(4) . . . . ? C11 C3 C4 C5 -6.0(7) . . . . ? N1 C4 C5 C6 -2.0(6) . . . . ? C3 C4 C5 C6 177.2(4) . . . . ? N1 C4 C5 C17 178.5(3) . . . . ? C3 C4 C5 C17 -2.3(6) . . . . ? C9 N2 C6 C5 -176.0(4) . . . . ? Rh1 N2 C6 C5 5.8(6) . . . . ? C9 N2 C6 C7 1.7(4) . . . . ? Rh1 N2 C6 C7 -176.5(3) . . . . ? C4 C5 C6 N2 -3.4(6) . . . . ? C17 C5 C6 N2 176.1(3) . . . . ? C4 C5 C6 C7 179.3(4) . . . . ? C17 C5 C6 C7 -1.2(6) . . . . ? N2 C6 C7 C8 -2.6(5) . . . . ? C5 C6 C7 C8 175.0(4) . . . . ? N2 C6 C7 C12 172.0(4) . . . . ? C5 C6 C7 C12 -10.3(7) . . . . ? C6 C7 C8 C9 2.4(5) . . . . ? C12 C7 C8 C9 -172.6(4) . . . . ? C6 C7 C8 C15 -178.3(4) . . . . ? C12 C7 C8 C15 6.7(7) . . . . ? C6 N2 C9 C10 -176.2(4) . . . . ? Rh1 N2 C9 C10 2.1(6) . . . . ? C6 N2 C9 C8 -0.2(4) . . . . ? Rh1 N2 C9 C8 178.2(3) . . . . ? C7 C8 C9 C10 174.7(4) . . . . ? C15 C8 C9 C10 -4.7(6) . . . . ? C7 C8 C9 N2 -1.5(5) . . . . ? C15 C8 C9 N2 179.2(4) . . . . ? N2 C9 C10 C1 -0.9(7) . . . 7 ? C8 C9 C10 C1 -176.4(4) . . . 7 ? C3 C2 C13 C14 -87.6(6) . . . . ? C1 C2 C13 C14 87.6(5) . . . . ? C7 C8 C15 C16 -100.0(5) . . . . ? C9 C8 C15 C16 79.2(5) . . . . ? C4 C5 C17 C22 -81.2(5) . . . . ? C6 C5 C17 C22 99.2(5) . . . . ? C4 C5 C17 C18 95.9(5) . . . . ? C6 C5 C17 C18 -83.6(5) . . . . ? C22 C17 C18 C19 1.1(6) . . . . ? C5 C17 C18 C19 -176.1(4) . . . . ? C17 C18 C19 C20 0.2(6) . . . . ? C18 C19 C20 C21 -1.1(7) . . . . ? C19 C20 C21 C22 0.6(7) . . . . ? C18 C17 C22 C21 -1.7(6) . . . . ? C5 C17 C22 C21 175.5(4) . . . . ? C20 C21 C22 C17 0.8(7) . . . . ? C35 P1 C23 C24 -10.3(4) . . . . ? C29 P1 C23 C24 -117.1(4) . . . . ? Rh1 P1 C23 C24 112.7(3) . . . . ? C35 P1 C23 C28 174.1(3) . . . . ? C29 P1 C23 C28 67.2(4) . . . . ? Rh1 P1 C23 C28 -62.9(3) . . . . ? C28 C23 C24 C25 -0.1(6) . . . . ? P1 C23 C24 C25 -175.8(3) . . . . ? C23 C24 C25 C26 -0.1(7) . . . . ? C24 C25 C26 C27 0.2(7) . . . . ? C25 C26 C27 C28 0.0(7) . . . . ? C26 C27 C28 C23 -0.2(6) . . . . ? C24 C23 C28 C27 0.3(6) . . . . ? P1 C23 C28 C27 176.0(3) . . . . ? C35 P1 C29 C30 10.3(4) . . . . ? C23 P1 C29 C30 117.0(3) . . . . ? Rh1 P1 C29 C30 -112.8(3) . . . . ? C35 P1 C29 C34 -173.3(3) . . . . ? C23 P1 C29 C34 -66.6(4) . . . . ? Rh1 P1 C29 C34 63.6(3) . . . . ? C34 C29 C30 C31 1.0(6) . . . . ? P1 C29 C30 C31 177.4(4) . . . . ? C29 C30 C31 C32 -0.3(7) . . . . ? C30 C31 C32 C33 -0.6(7) . . . . ? C31 C32 C33 C34 0.8(7) . . . . ? C32 C33 C34 C29 -0.1(7) . . . . ? C30 C29 C34 C33 -0.8(6) . . . . ? P1 C29 C34 C33 -177.3(3) . . . . ? C42 C37 C38 C39 1.4(8) . . . . ? C36 C37 C38 C39 -175.5(5) . . . . ? C37 C38 C39 C40 -0.4(8) . . . . ? C38 C39 C40 C41 -0.8(9) . . . . ? C39 C40 C41 C42 1.0(9) . . . . ? C40 C41 C42 C37 0.0(9) . . . . ? C38 C37 C42 C41 -1.2(8) . . . . ? C36 C37 C42 C41 175.6(5) . . . . ? #============================================================================= data_P2_Rh5 _database_code_depnum_ccdc_archive 'CCDC 834654' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C116 H122 N4 P2 Rh +, I -, C5 H12' _chemical_formula_sum 'C121 H134 I N4 P2 Rh' _chemical_formula_weight 1936.07 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' I I -0.4742 1.8119 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0257(3) _cell_length_b 15.2154(3) _cell_length_c 16.3438(5) _cell_angle_alpha 102.144(1) _cell_angle_beta 98.439(1) _cell_angle_gamma 111.559(1) _cell_volume 2635.21(12) _cell_formula_units_Z 1 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 21879 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description lath _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; Complex sited on centre of symmetry. Therefore, one iodide per cell on a general position - refined with half site occupancy. When iodide is not present, the space is filled by a pentane molecule - also refined with half occupancy. Some C atoms of tert-butyl groups might be split, but little information gained by doing so - left with relatively large ellipsoids. ; _diffrn_ambient_temperature 220(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 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 21481 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 24.71 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 8901 _reflns_number_gt 7512 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _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^)+(0.1164P)^2^+7.9928P] 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 8901 _refine_ls_number_parameters 581 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.1859 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.178 _refine_diff_density_min -1.649 _refine_diff_density_rms 0.119 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 Rh1 Rh 0.0000 0.0000 0.0000 0.02064(18) Uani 1 2 d S . 1 P1 P 0.19936(11) 0.01532(8) 0.06242(8) 0.0268(3) Uani 1 1 d . A 1 N1 N 0.0746(3) 0.0769(3) -0.0808(2) 0.0216(8) Uani 1 1 d U B 1 N2 N 0.0327(3) 0.1293(3) 0.0880(2) 0.0237(8) Uani 1 1 d U B 1 C1 C 0.0865(4) 0.0377(3) -0.1611(3) 0.0261(10) Uani 1 1 d . . 1 C2 C 0.1443(5) 0.1177(4) -0.1966(3) 0.0360(12) Uani 1 1 d . B 1 H2A H 0.1631 0.1113 -0.2508 0.043 Uiso 1 1 calc R B 1 C3 C 0.1663(5) 0.2021(4) -0.1388(3) 0.0369(12) Uani 1 1 d . B 1 H3A H 0.2044 0.2658 -0.1447 0.044 Uiso 1 1 calc R B 1 C4 C 0.1210(4) 0.1785(3) -0.0651(3) 0.0271(10) Uani 1 1 d . B 1 C5 C 0.1242(4) 0.2467(3) 0.0077(3) 0.0288(10) Uani 1 1 d . B 1 C6 C 0.0816(4) 0.2220(3) 0.0788(3) 0.0254(9) Uani 1 1 d . B 1 C7 C 0.0841(5) 0.2915(3) 0.1547(3) 0.0309(11) Uani 1 1 d . B 1 H7A H 0.1117 0.3600 0.1642 0.037 Uiso 1 1 calc R B 1 C8 C 0.0401(5) 0.2412(3) 0.2097(3) 0.0303(10) Uani 1 1 d . B 1 H8A H 0.0322 0.2680 0.2647 0.036 Uiso 1 1 calc R B 1 C9 C 0.0074(4) 0.1388(3) 0.1687(3) 0.0251(9) Uani 1 1 d . B 1 C10 C -0.0460(5) 0.0620(3) 0.2037(3) 0.0302(10) Uani 1 1 d . . 1 C11 C 0.1770(5) 0.3533(3) 0.0096(3) 0.0307(10) Uani 1 1 d . B 1 C12 C 0.1241(5) 0.3840(4) -0.0540(3) 0.0345(11) Uani 1 1 d . B 1 H12A H 0.0528 0.3382 -0.0963 0.041 Uiso 1 1 calc R B 1 C13 C 0.1751(5) 0.4820(4) -0.0559(4) 0.0376(12) Uani 1 1 d . B 1 C14 C 0.2791(5) 0.5481(4) 0.0085(4) 0.0416(13) Uani 1 1 d . B 1 H14A H 0.3141 0.6143 0.0081 0.050 Uiso 1 1 calc R B 1 C15 C 0.3337(5) 0.5199(4) 0.0740(4) 0.0378(12) Uani 1 1 d . B 1 C16 C 0.2821(5) 0.4216(3) 0.0723(3) 0.0333(11) Uani 1 1 d . B 1 H16A H 0.3191 0.4005 0.1144 0.040 Uiso 1 1 calc R B 1 C17 C 0.1178(6) 0.5118(4) -0.1310(4) 0.0494(15) Uani 1 1 d . B 1 C18 C 0.1298(11) 0.4545(8) -0.2167(5) 0.093(3) Uani 1 1 d . B 1 H18A H 0.2163 0.4711 -0.2147 0.140 Uiso 1 1 calc R B 1 H18B H 0.0936 0.4723 -0.2642 0.140 Uiso 1 1 calc R B 1 H18C H 0.0872 0.3842 -0.2250 0.140 Uiso 1 1 calc R B 1 C19 C 0.1781(9) 0.6226(6) -0.1194(7) 0.101(3) Uani 1 1 d . B 1 H19A H 0.2658 0.6432 -0.1147 0.151 Uiso 1 1 calc R B 1 H19B H 0.1654 0.6577 -0.0673 0.151 Uiso 1 1 calc R B 1 H19C H 0.1414 0.6373 -0.1688 0.151 Uiso 1 1 calc R B 1 C20 C -0.0214(7) 0.4812(5) -0.1385(5) 0.0661(19) Uani 1 1 d . B 1 H20A H -0.0617 0.4105 -0.1478 0.099 Uiso 1 1 calc R B 1 H20B H -0.0565 0.4984 -0.1868 0.099 Uiso 1 1 calc R B 1 H20C H -0.0336 0.5153 -0.0857 0.099 Uiso 1 1 calc R B 1 C21 C 0.4481(6) 0.5931(4) 0.1472(4) 0.0500(15) Uani 1 1 d . B 1 C22 C 0.5003(7) 0.6969(5) 0.1331(6) 0.072(2) Uani 1 1 d . B 1 H22A H 0.5714 0.7409 0.1802 0.107 Uiso 1 1 calc R B 1 H22B H 0.4374 0.7226 0.1313 0.107 Uiso 1 1 calc R B 1 H22C H 0.5248 0.6921 0.0789 0.107 Uiso 1 1 calc R B 1 C23 C 0.4078(8) 0.6043(6) 0.2319(5) 0.076(2) Uani 1 1 d . B 1 H23A H 0.3748 0.5405 0.2428 0.115 Uiso 1 1 calc R B 1 H23B H 0.3449 0.6298 0.2278 0.115 Uiso 1 1 calc R B 1 H23C H 0.4783 0.6497 0.2789 0.115 Uiso 1 1 calc R B 1 C24 C 0.5489(7) 0.5558(5) 0.1520(6) 0.077(2) Uani 1 1 d . B 1 H24A H 0.5178 0.4912 0.1614 0.115 Uiso 1 1 calc R B 1 H24B H 0.6188 0.6012 0.1994 0.115 Uiso 1 1 calc R B 1 H24C H 0.5746 0.5512 0.0983 0.115 Uiso 1 1 calc R B 1 C25 C -0.0618(5) 0.0884(4) 0.2944(3) 0.0367(12) Uani 1 1 d . C 1 C26 C 0.0422(6) 0.1351(4) 0.3629(3) 0.0420(13) Uani 1 1 d . C 1 H26A H 0.1210 0.1507 0.3524 0.050 Uiso 1 1 calc R C 1 C27 C 0.0298(6) 0.1593(4) 0.4479(4) 0.0471(14) Uani 1 1 d . C 1 C28 C -0.0877(7) 0.1355(5) 0.4600(4) 0.0621(18) Uani 1 1 d . C 1 H28A H -0.0968 0.1525 0.5166 0.074 Uiso 1 1 calc R C 1 C29 C -0.1932(7) 0.0876(7) 0.3925(4) 0.071(2) Uani 1 1 d . C 1 C30 C -0.1771(6) 0.0656(5) 0.3096(4) 0.0496(15) Uani 1 1 d . C 1 H30A H -0.2467 0.0343 0.2625 0.059 Uiso 1 1 calc R C 1 C31 C 0.1414(8) 0.2118(6) 0.5256(4) 0.078(3) Uani 1 1 d . C 1 C32 C 0.2612(9) 0.2447(8) 0.5004(5) 0.105(4) Uani 1 1 d . C 1 H32A H 0.2702 0.1876 0.4677 0.157 Uiso 1 1 calc R C 1 H32B H 0.3285 0.2789 0.5519 0.157 Uiso 1 1 calc R C 1 H32C H 0.2627 0.2888 0.4651 0.157 Uiso 1 1 calc R C 1 C33 C 0.1354(13) 0.3068(10) 0.5770(9) 0.175(7) Uani 1 1 d . C 1 H33A H 0.2059 0.3409 0.6265 0.262 Uiso 1 1 calc R C 1 H33B H 0.0599 0.2897 0.5967 0.262 Uiso 1 1 calc R C 1 H33C H 0.1366 0.3493 0.5402 0.262 Uiso 1 1 calc R C 1 C34 C 0.1370(13) 0.1470(12) 0.5829(9) 0.199(9) Uani 1 1 d . C 1 H34A H 0.1411 0.0870 0.5516 0.298 Uiso 1 1 calc R C 1 H34B H 0.0606 0.1305 0.6013 0.298 Uiso 1 1 calc R C 1 H34C H 0.2064 0.1813 0.6331 0.298 Uiso 1 1 calc R C 1 C35 C -0.3270(11) 0.0597(14) 0.4049(6) 0.135(6) Uani 1 1 d . C 1 C36 C -0.3730(16) 0.1311(17) 0.3744(8) 0.202(10) Uani 1 1 d . C 1 H36A H -0.3203 0.1980 0.4095 0.303 Uiso 1 1 calc R C 1 H36B H -0.4569 0.1152 0.3799 0.303 Uiso 1 1 calc R C 1 H36C H -0.3711 0.1255 0.3144 0.303 Uiso 1 1 calc R C 1 C37 C -0.4126(10) -0.0453(14) 0.3516(9) 0.173(8) Uani 1 1 d . C 1 H37A H -0.4134 -0.0522 0.2911 0.259 Uiso 1 1 calc R C 1 H37B H -0.4953 -0.0597 0.3590 0.259 Uiso 1 1 calc R C 1 H37C H -0.3835 -0.0911 0.3706 0.259 Uiso 1 1 calc R C 1 C38 C -0.3235(13) 0.0728(19) 0.5038(8) 0.244(13) Uani 1 1 d . C 1 H38A H -0.2731 0.1411 0.5364 0.367 Uiso 1 1 calc R C 1 H38B H -0.2885 0.0308 0.5243 0.367 Uiso 1 1 calc R C 1 H38C H -0.4066 0.0544 0.5116 0.367 Uiso 1 1 calc R C 1 C39 C 0.2052(4) -0.0613(4) 0.1328(3) 0.0328(11) Uani 1 1 d . A 1 C40 C 0.1890(8) -0.0324(6) 0.2153(4) 0.0649(19) Uani 1 1 d . A 1 H40A H 0.1797 0.0268 0.2334 0.078 Uiso 1 1 calc R A 1 C41 C 0.1865(9) -0.0903(7) 0.2714(5) 0.083(3) Uani 1 1 d . A 1 H41A H 0.1727 -0.0712 0.3262 0.099 Uiso 1 1 calc R A 1 C42 C 0.2041(8) -0.1747(6) 0.2468(6) 0.075(2) Uani 1 1 d . A 1 H42A H 0.2062 -0.2123 0.2854 0.091 Uiso 1 1 calc R A 1 C43 C 0.2188(7) -0.2043(5) 0.1656(6) 0.065(2) Uani 1 1 d . A 1 H43A H 0.2293 -0.2630 0.1482 0.078 Uiso 1 1 calc R A 1 C44 C 0.2182(6) -0.1487(5) 0.1091(5) 0.0530(15) Uani 1 1 d . A 1 H44A H 0.2268 -0.1709 0.0532 0.064 Uiso 1 1 calc R A 1 C45 C 0.2888(4) -0.0020(4) -0.0146(3) 0.0333(11) Uani 1 1 d . A 1 C46 C 0.2588(5) -0.0940(4) -0.0708(3) 0.0414(13) Uani 1 1 d . A 1 H46A H 0.1883 -0.1483 -0.0710 0.050 Uiso 1 1 calc R A 1 C47 C 0.3321(6) -0.1069(6) -0.1269(4) 0.0558(16) Uani 1 1 d . A 1 H47A H 0.3117 -0.1699 -0.1637 0.067 Uiso 1 1 calc R A 1 C48 C 0.4329(7) -0.0288(6) -0.1286(5) 0.0639(19) Uani 1 1 d . A 1 H48A H 0.4837 -0.0385 -0.1650 0.077 Uiso 1 1 calc R A 1 C49 C 0.4604(6) 0.0635(6) -0.0777(5) 0.0600(19) Uani 1 1 d . A 1 H49A H 0.5274 0.1176 -0.0820 0.072 Uiso 1 1 calc R A 1 C50 C 0.3909(5) 0.0792(5) -0.0192(4) 0.0473(14) Uani 1 1 d . A 1 H50A H 0.4119 0.1429 0.0165 0.057 Uiso 1 1 calc R A 1 C51 C 0.2895(5) 0.1332(4) 0.1319(3) 0.0379(12) Uani 1 1 d . A 1 C52 C 0.3520(5) 0.2089(4) 0.1878(4) 0.0450(13) Uani 1 1 d . A 1 C53 C 0.4293(6) 0.2968(4) 0.2560(4) 0.0479(15) Uani 1 1 d . A 1 C54 C 0.5571(7) 0.3276(5) 0.2738(5) 0.069(2) Uani 1 1 d . A 1 H54A H 0.5924 0.2932 0.2393 0.082 Uiso 1 1 calc R A 1 C55 C 0.6313(8) 0.4097(7) 0.3430(6) 0.093(3) Uani 1 1 d . A 1 H55A H 0.7173 0.4302 0.3558 0.112 Uiso 1 1 calc R A 1 C56 C 0.5806(10) 0.4611(6) 0.3928(5) 0.094(3) Uani 1 1 d . A 1 H56A H 0.6319 0.5155 0.4404 0.113 Uiso 1 1 calc R A 1 C57 C 0.4552(10) 0.4336(6) 0.3737(5) 0.089(3) Uani 1 1 d . A 1 H57A H 0.4212 0.4704 0.4071 0.107 Uiso 1 1 calc R A 1 C58 C 0.3791(8) 0.3516(5) 0.3053(5) 0.0667(19) Uani 1 1 d . A 1 H58A H 0.2934 0.3330 0.2921 0.080 Uiso 1 1 calc R A 1 I1 I 0.0452(4) 0.4480(2) 0.40662(15) 0.225(2) Uani 0.50 1 d P D 1 C1S C 0.218(2) 0.6687(13) 0.3934(17) 0.127(4) Uiso 0.50 1 d PD E 2 H1S1 H 0.2883 0.7306 0.4233 0.190 Uiso 0.50 1 calc PR E 2 H1S2 H 0.1449 0.6706 0.4107 0.190 Uiso 0.50 1 calc PR E 2 H1S3 H 0.2053 0.6588 0.3315 0.190 Uiso 0.50 1 calc PR E 2 C2S C 0.2417(16) 0.5851(13) 0.4159(14) 0.127(4) Uiso 0.50 1 d PD E 2 H2S1 H 0.3173 0.5856 0.3999 0.152 Uiso 0.50 1 calc PR E 2 H2S2 H 0.2564 0.5970 0.4786 0.152 Uiso 0.50 1 calc PR E 2 C3S C 0.1404(18) 0.4852(12) 0.3736(15) 0.127(4) Uiso 0.50 1 d PD E 2 H3S1 H 0.1749 0.4357 0.3671 0.152 Uiso 0.50 1 calc PR E 2 H3S2 H 0.1003 0.4827 0.3159 0.152 Uiso 0.50 1 calc PR E 2 C4S C 0.043(2) 0.461(2) 0.4281(16) 0.127(4) Uiso 0.50 1 d PD E 2 H4S1 H 0.0768 0.4471 0.4799 0.152 Uiso 0.50 1 calc PR E 2 H4S2 H 0.0224 0.5173 0.4464 0.152 Uiso 0.50 1 calc PR E 2 C5S C -0.0743(17) 0.3697(17) 0.3729(17) 0.127(4) Uiso 0.50 1 d PD E 2 H5S1 H -0.1354 0.3544 0.4065 0.190 Uiso 0.50 1 calc PR E 2 H5S2 H -0.0536 0.3137 0.3557 0.190 Uiso 0.50 1 calc PR E 2 H5S3 H -0.1076 0.3837 0.3219 0.190 Uiso 0.50 1 calc PR E 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 Rh1 0.0229(3) 0.0165(3) 0.0197(3) 0.00669(18) 0.00370(19) 0.0048(2) P1 0.0245(6) 0.0231(6) 0.0269(6) 0.0063(5) 0.0011(5) 0.0058(5) N1 0.0223(11) 0.0220(11) 0.0205(11) 0.0080(8) 0.0084(8) 0.0070(8) N2 0.0241(11) 0.0233(11) 0.0234(11) 0.0077(8) 0.0058(8) 0.0088(8) C1 0.032(2) 0.025(2) 0.022(2) 0.0116(18) 0.0113(19) 0.0076(19) C2 0.047(3) 0.033(3) 0.030(3) 0.015(2) 0.020(2) 0.011(2) C3 0.044(3) 0.026(2) 0.039(3) 0.016(2) 0.013(2) 0.008(2) C4 0.028(2) 0.021(2) 0.029(2) 0.0116(19) 0.0042(19) 0.0051(19) C5 0.030(2) 0.019(2) 0.034(3) 0.0092(19) 0.004(2) 0.0076(19) C6 0.025(2) 0.022(2) 0.029(2) 0.0075(18) 0.0023(18) 0.0106(18) C7 0.038(3) 0.018(2) 0.033(3) 0.0047(19) 0.008(2) 0.010(2) C8 0.038(3) 0.025(2) 0.025(2) 0.0020(19) 0.008(2) 0.012(2) C9 0.028(2) 0.020(2) 0.023(2) 0.0036(17) 0.0020(18) 0.0076(18) C10 0.035(3) 0.029(2) 0.024(2) 0.0085(19) 0.006(2) 0.011(2) C11 0.039(3) 0.022(2) 0.033(3) 0.013(2) 0.014(2) 0.011(2) C12 0.043(3) 0.026(2) 0.038(3) 0.012(2) 0.014(2) 0.016(2) C13 0.052(3) 0.032(3) 0.046(3) 0.023(2) 0.031(3) 0.023(2) C14 0.054(3) 0.024(2) 0.054(3) 0.018(2) 0.025(3) 0.015(2) C15 0.040(3) 0.024(2) 0.048(3) 0.010(2) 0.018(2) 0.010(2) C16 0.031(3) 0.025(2) 0.043(3) 0.012(2) 0.011(2) 0.008(2) C17 0.066(4) 0.042(3) 0.057(4) 0.031(3) 0.021(3) 0.029(3) C18 0.152(9) 0.125(8) 0.060(5) 0.051(5) 0.042(5) 0.101(7) C19 0.109(7) 0.061(5) 0.135(8) 0.069(6) 0.003(6) 0.027(5) C20 0.075(5) 0.063(4) 0.072(5) 0.037(4) 0.013(4) 0.034(4) C21 0.044(3) 0.025(3) 0.066(4) 0.006(3) 0.010(3) 0.003(2) C22 0.062(4) 0.032(3) 0.100(6) 0.016(3) 0.012(4) 0.001(3) C23 0.075(5) 0.060(4) 0.059(4) -0.004(4) 0.008(4) 0.003(4) C24 0.048(4) 0.043(4) 0.112(7) 0.005(4) -0.009(4) 0.009(3) C25 0.052(3) 0.028(2) 0.030(3) 0.012(2) 0.012(2) 0.013(2) C26 0.055(3) 0.031(3) 0.028(3) 0.008(2) 0.004(2) 0.007(2) C27 0.071(4) 0.033(3) 0.030(3) 0.010(2) 0.012(3) 0.013(3) C28 0.090(5) 0.078(5) 0.028(3) 0.019(3) 0.029(3) 0.038(4) C29 0.078(5) 0.114(6) 0.039(4) 0.033(4) 0.027(3) 0.049(5) C30 0.050(3) 0.073(4) 0.034(3) 0.023(3) 0.017(3) 0.028(3) C31 0.089(6) 0.071(5) 0.028(3) 0.012(3) -0.002(3) -0.008(4) C32 0.083(6) 0.117(8) 0.047(4) 0.014(5) -0.016(4) -0.013(5) C33 0.143(11) 0.133(11) 0.127(11) -0.075(9) 0.013(9) -0.006(9) C34 0.140(11) 0.209(15) 0.139(11) 0.132(11) -0.068(9) -0.052(10) C35 0.097(8) 0.292(18) 0.049(5) 0.065(8) 0.049(5) 0.095(11) C36 0.194(16) 0.40(3) 0.086(8) 0.030(13) 0.042(9) 0.23(2) C37 0.062(6) 0.29(2) 0.116(10) 0.082(13) 0.031(7) 0.006(10) C38 0.114(10) 0.56(4) 0.077(8) 0.107(15) 0.062(8) 0.137(17) C39 0.027(2) 0.042(3) 0.034(3) 0.016(2) 0.008(2) 0.016(2) C40 0.095(6) 0.070(4) 0.040(4) 0.022(3) 0.013(3) 0.043(4) C41 0.110(7) 0.112(7) 0.042(4) 0.042(4) 0.021(4) 0.052(6) C42 0.078(5) 0.087(6) 0.077(5) 0.059(5) 0.010(4) 0.034(4) C43 0.060(4) 0.059(4) 0.101(6) 0.052(4) 0.028(4) 0.034(3) C44 0.059(4) 0.048(3) 0.062(4) 0.031(3) 0.023(3) 0.023(3) C45 0.028(2) 0.047(3) 0.031(3) 0.019(2) 0.013(2) 0.016(2) C46 0.044(3) 0.049(3) 0.034(3) 0.014(2) 0.005(2) 0.023(3) C47 0.059(4) 0.075(4) 0.048(4) 0.018(3) 0.013(3) 0.043(4) C48 0.063(4) 0.098(6) 0.055(4) 0.036(4) 0.019(3) 0.050(4) C49 0.037(3) 0.097(6) 0.071(5) 0.057(4) 0.031(3) 0.030(3) C50 0.034(3) 0.053(3) 0.055(4) 0.029(3) 0.011(3) 0.012(3) C51 0.028(3) 0.030(3) 0.040(3) 0.000(2) -0.004(2) 0.005(2) C52 0.038(3) 0.041(3) 0.047(3) 0.009(3) 0.001(3) 0.011(3) C53 0.051(3) 0.032(3) 0.038(3) 0.003(2) -0.007(3) 0.003(3) C54 0.052(4) 0.058(4) 0.064(4) 0.000(3) -0.003(3) 0.004(3) C55 0.063(5) 0.074(6) 0.079(6) -0.002(5) -0.014(4) -0.017(4) C56 0.106(8) 0.052(5) 0.056(5) -0.012(4) -0.005(5) -0.017(5) C57 0.119(8) 0.058(5) 0.055(5) -0.010(4) 0.009(5) 0.018(5) C58 0.074(5) 0.058(4) 0.052(4) -0.001(3) 0.000(3) 0.024(4) I1 0.461(6) 0.1376(19) 0.0926(14) 0.0018(12) 0.014(2) 0.180(3) _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 Rh1 N1 2.035(3) . ? Rh1 N1 2.035(3) 2 ? Rh1 N2 2.041(4) 2 ? Rh1 N2 2.041(4) . ? Rh1 P1 2.3694(12) 2 ? Rh1 P1 2.3694(12) . ? P1 C51 1.741(5) . ? P1 C45 1.810(5) . ? P1 C39 1.813(5) . ? N1 C1 1.374(6) . ? N1 C4 1.387(6) . ? N2 C6 1.364(6) . ? N2 C9 1.388(6) . ? C1 C10 1.392(7) 2 ? C1 C2 1.448(6) . ? C2 C3 1.333(7) . ? C2 H2A 0.9400 . ? C3 C4 1.451(7) . ? C3 H3A 0.9400 . ? C4 C5 1.389(7) . ? C5 C6 1.405(7) . ? C5 C11 1.500(6) . ? C6 C7 1.439(6) . ? C7 C8 1.343(7) . ? C7 H7A 0.9400 . ? C8 C9 1.437(6) . ? C8 H8A 0.9400 . ? C9 C10 1.393(7) . ? C10 C1 1.392(7) 2 ? C10 C25 1.510(7) . ? C11 C12 1.389(7) . ? C11 C16 1.390(7) . ? C12 C13 1.397(7) . ? C12 H12A 0.9400 . ? C13 C14 1.389(8) . ? C13 C17 1.550(8) . ? C14 C15 1.398(8) . ? C14 H14A 0.9400 . ? C15 C16 1.385(7) . ? C15 C21 1.547(8) . ? C16 H16A 0.9400 . ? C17 C19 1.526(9) . ? C17 C20 1.541(10) . ? C17 C18 1.544(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C24 1.514(10) . ? C21 C23 1.529(10) . ? C21 C22 1.552(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C30 1.374(8) . ? C25 C26 1.386(8) . ? C26 C27 1.406(8) . ? C26 H26A 0.9400 . ? C27 C28 1.379(10) . ? C27 C31 1.528(9) . ? C28 C29 1.389(10) . ? C28 H28A 0.9400 . ? C29 C30 1.386(9) . ? C29 C35 1.562(13) . ? C30 H30A 0.9400 . ? C31 C34 1.489(13) . ? C31 C32 1.493(13) . ? C31 C33 1.543(15) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 C37 1.52(2) . ? C35 C36 1.52(2) . ? C35 C38 1.579(13) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C44 1.377(8) . ? C39 C40 1.393(9) . ? C40 C41 1.394(10) . ? C40 H40A 0.9400 . ? C41 C42 1.366(12) . ? C41 H41A 0.9400 . ? C42 C43 1.366(11) . ? C42 H42A 0.9400 . ? C43 C44 1.378(9) . ? C43 H43A 0.9400 . ? C44 H44A 0.9400 . ? C45 C46 1.387(8) . ? C45 C50 1.411(7) . ? C46 C47 1.395(9) . ? C46 H46A 0.9400 . ? C47 C48 1.359(10) . ? C47 H47A 0.9400 . ? C48 C49 1.364(11) . ? C48 H48A 0.9400 . ? C49 C50 1.398(9) . ? C49 H49A 0.9400 . ? C50 H50A 0.9400 . ? C51 C52 1.203(7) . ? C52 C53 1.432(8) . ? C53 C58 1.393(10) . ? C53 C54 1.395(10) . ? C54 C55 1.387(10) . ? C54 H54A 0.9400 . ? C55 C56 1.369(14) . ? C55 H55A 0.9400 . ? C56 C57 1.375(15) . ? C56 H56A 0.9400 . ? C57 C58 1.384(10) . ? C57 H57A 0.9400 . ? C58 H58A 0.9400 . ? C1S C2S 1.506(10) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C1S H1S3 0.9700 . ? C2S C3S 1.490(10) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C3S C4S 1.559(10) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C4S C5S 1.545(10) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C5S H5S1 0.9700 . ? C5S H5S2 0.9700 . ? C5S H5S3 0.9700 . ? 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 Rh1 N1 180.0(3) . 2 ? N1 Rh1 N2 90.28(14) . 2 ? N1 Rh1 N2 89.72(14) 2 2 ? N1 Rh1 N2 89.72(14) . . ? N1 Rh1 N2 90.28(14) 2 . ? N2 Rh1 N2 180.0(3) 2 . ? N1 Rh1 P1 91.34(10) . 2 ? N1 Rh1 P1 88.66(10) 2 2 ? N2 Rh1 P1 89.48(10) 2 2 ? N2 Rh1 P1 90.52(10) . 2 ? N1 Rh1 P1 88.66(10) . . ? N1 Rh1 P1 91.34(10) 2 . ? N2 Rh1 P1 90.52(10) 2 . ? N2 Rh1 P1 89.48(10) . . ? P1 Rh1 P1 180.00(6) 2 . ? C51 P1 C45 104.3(3) . . ? C51 P1 C39 101.7(3) . . ? C45 P1 C39 107.9(2) . . ? C51 P1 Rh1 111.32(18) . . ? C45 P1 Rh1 114.43(16) . . ? C39 P1 Rh1 115.80(16) . . ? C1 N1 C4 107.6(4) . . ? C1 N1 Rh1 126.3(3) . . ? C4 N1 Rh1 126.1(3) . . ? C6 N2 C9 107.0(4) . . ? C6 N2 Rh1 127.2(3) . . ? C9 N2 Rh1 125.9(3) . . ? N1 C1 C10 126.5(4) . 2 ? N1 C1 C2 108.5(4) . . ? C10 C1 C2 124.9(4) 2 . ? C3 C2 C1 107.9(4) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? C2 C3 C4 108.1(4) . . ? C2 C3 H3A 126.0 . . ? C4 C3 H3A 126.0 . . ? N1 C4 C5 126.8(4) . . ? N1 C4 C3 107.9(4) . . ? C5 C4 C3 125.4(4) . . ? C4 C5 C6 124.2(4) . . ? C4 C5 C11 117.3(4) . . ? C6 C5 C11 118.5(4) . . ? N2 C6 C5 126.0(4) . . ? N2 C6 C7 109.0(4) . . ? C5 C6 C7 125.0(4) . . ? C8 C7 C6 107.9(4) . . ? C8 C7 H7A 126.0 . . ? C6 C7 H7A 126.0 . . ? C7 C8 C9 107.3(4) . . ? C7 C8 H8A 126.4 . . ? C9 C8 H8A 126.4 . . ? N2 C9 C10 126.2(4) . . ? N2 C9 C8 108.8(4) . . ? C10 C9 C8 125.0(4) . . ? C1 C10 C9 124.8(4) 2 . ? C1 C10 C25 117.3(4) 2 . ? C9 C10 C25 117.9(4) . . ? C12 C11 C16 119.2(4) . . ? C12 C11 C5 120.0(4) . . ? C16 C11 C5 120.7(4) . . ? C11 C12 C13 121.1(5) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C14 C13 C12 117.9(5) . . ? C14 C13 C17 122.6(5) . . ? C12 C13 C17 119.4(5) . . ? C13 C14 C15 122.5(5) . . ? C13 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C16 C15 C14 117.7(5) . . ? C16 C15 C21 119.2(5) . . ? C14 C15 C21 123.0(5) . . ? C15 C16 C11 121.6(5) . . ? C15 C16 H16A 119.2 . . ? C11 C16 H16A 119.2 . . ? C19 C17 C20 108.4(6) . . ? C19 C17 C18 110.1(7) . . ? C20 C17 C18 106.5(7) . . ? C19 C17 C13 112.5(6) . . ? C20 C17 C13 110.4(5) . . ? C18 C17 C13 108.8(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C23 111.0(7) . . ? C24 C21 C15 110.4(5) . . ? C23 C21 C15 108.0(5) . . ? C24 C21 C22 108.5(6) . . ? C23 C21 C22 107.4(6) . . ? C15 C21 C22 111.6(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 120.0(5) . . ? C30 C25 C10 120.9(5) . . ? C26 C25 C10 119.0(5) . . ? C25 C26 C27 120.1(6) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 117.8(6) . . ? C28 C27 C31 120.0(6) . . ? C26 C27 C31 122.2(6) . . ? C27 C28 C29 123.1(6) . . ? C27 C28 H28A 118.5 . . ? C29 C28 H28A 118.5 . . ? C30 C29 C28 117.3(7) . . ? C30 C29 C35 118.8(7) . . ? C28 C29 C35 123.8(7) . . ? C25 C30 C29 121.6(6) . . ? C25 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? C34 C31 C32 111.3(10) . . ? C34 C31 C27 109.6(7) . . ? C32 C31 C27 112.9(6) . . ? C34 C31 C33 108.4(11) . . ? C32 C31 C33 105.8(8) . . ? C27 C31 C33 108.6(9) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C36 109.2(11) . . ? C37 C35 C29 111.4(10) . . ? C36 C35 C29 106.9(12) . . ? C37 C35 C38 110.5(14) . . ? C36 C35 C38 109.5(13) . . ? C29 C35 C38 109.3(9) . . ? 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 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C39 C40 117.5(5) . . ? C44 C39 P1 124.7(4) . . ? C40 C39 P1 117.7(4) . . ? C39 C40 C41 120.8(7) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C42 C41 C40 120.1(8) . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C41 C42 C43 119.6(6) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C42 C43 C44 120.6(7) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? C39 C44 C43 121.4(7) . . ? C39 C44 H44A 119.3 . . ? C43 C44 H44A 119.3 . . ? C46 C45 C50 118.4(5) . . ? C46 C45 P1 121.5(4) . . ? C50 C45 P1 120.2(4) . . ? C45 C46 C47 120.7(6) . . ? C45 C46 H46A 119.7 . . ? C47 C46 H46A 119.7 . . ? C48 C47 C46 120.4(7) . . ? C48 C47 H47A 119.8 . . ? C46 C47 H47A 119.8 . . ? C47 C48 C49 120.2(7) . . ? C47 C48 H48A 119.9 . . ? C49 C48 H48A 119.9 . . ? C48 C49 C50 121.1(6) . . ? C48 C49 H49A 119.4 . . ? C50 C49 H49A 119.4 . . ? C49 C50 C45 119.1(6) . . ? C49 C50 H50A 120.5 . . ? C45 C50 H50A 120.5 . . ? C52 C51 P1 171.8(5) . . ? C51 C52 C53 177.5(6) . . ? C58 C53 C54 119.4(6) . . ? C58 C53 C52 121.1(6) . . ? C54 C53 C52 119.4(6) . . ? C55 C54 C53 119.2(8) . . ? C55 C54 H54A 120.4 . . ? C53 C54 H54A 120.4 . . ? C56 C55 C54 120.8(9) . . ? C56 C55 H55A 119.6 . . ? C54 C55 H55A 119.6 . . ? C55 C56 C57 120.4(7) . . ? C55 C56 H56A 119.8 . . ? C57 C56 H56A 119.8 . . ? C56 C57 C58 119.9(9) . . ? C56 C57 H57A 120.0 . . ? C58 C57 H57A 120.0 . . ? C57 C58 C53 120.1(8) . . ? C57 C58 H58A 119.9 . . ? C53 C58 H58A 119.9 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3S C2S C1S 115.0(10) . . ? C3S C2S H2S1 108.5 . . ? C1S C2S H2S1 108.5 . . ? C3S C2S H2S2 108.5 . . ? C1S C2S H2S2 108.5 . . ? H2S1 C2S H2S2 107.5 . . ? C2S C3S C4S 110.9(9) . . ? C2S C3S H3S1 109.5 . . ? C4S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? C4S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 108.1 . . ? C5S C4S C3S 109.2(9) . . ? C5S C4S H4S1 109.8 . . ? C3S C4S H4S1 109.8 . . ? C5S C4S H4S2 109.8 . . ? C3S C4S H4S2 109.8 . . ? H4S1 C4S H4S2 108.3 . . ? C4S C5S H5S1 109.5 . . ? C4S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? C4S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 P1 C51 76.6(2) . . . . ? N1 Rh1 P1 C51 -103.4(2) 2 . . . ? N2 Rh1 P1 C51 166.9(2) 2 . . . ? N2 Rh1 P1 C51 -13.1(2) . . . . ? N1 Rh1 P1 C45 -41.4(2) . . . . ? N1 Rh1 P1 C45 138.6(2) 2 . . . ? N2 Rh1 P1 C45 48.9(2) 2 . . . ? N2 Rh1 P1 C45 -131.1(2) . . . . ? N1 Rh1 P1 C39 -167.9(2) . . . . ? N1 Rh1 P1 C39 12.1(2) 2 . . . ? N2 Rh1 P1 C39 -77.6(2) 2 . . . ? N2 Rh1 P1 C39 102.4(2) . . . . ? N2 Rh1 N1 C1 0.2(4) 2 . . . ? N2 Rh1 N1 C1 -179.8(4) . . . . ? P1 Rh1 N1 C1 -89.3(4) 2 . . . ? P1 Rh1 N1 C1 90.7(4) . . . . ? N2 Rh1 N1 C4 179.2(4) 2 . . . ? N2 Rh1 N1 C4 -0.8(4) . . . . ? P1 Rh1 N1 C4 89.7(3) 2 . . . ? P1 Rh1 N1 C4 -90.3(3) . . . . ? N1 Rh1 N2 C6 2.5(4) . . . . ? N1 Rh1 N2 C6 -177.5(4) 2 . . . ? P1 Rh1 N2 C6 -88.8(4) 2 . . . ? P1 Rh1 N2 C6 91.2(4) . . . . ? N1 Rh1 N2 C9 -178.3(4) . . . . ? N1 Rh1 N2 C9 1.7(4) 2 . . . ? P1 Rh1 N2 C9 90.4(3) 2 . . . ? P1 Rh1 N2 C9 -89.6(3) . . . . ? C4 N1 C1 C10 -176.7(5) . . . 2 ? Rh1 N1 C1 C10 2.4(7) . . . 2 ? C4 N1 C1 C2 0.9(5) . . . . ? Rh1 N1 C1 C2 -179.9(3) . . . . ? N1 C1 C2 C3 0.1(6) . . . . ? C10 C1 C2 C3 177.8(5) 2 . . . ? C1 C2 C3 C4 -1.1(6) . . . . ? C1 N1 C4 C5 178.4(5) . . . . ? Rh1 N1 C4 C5 -0.8(7) . . . . ? C1 N1 C4 C3 -1.6(5) . . . . ? Rh1 N1 C4 C3 179.3(3) . . . . ? C2 C3 C4 N1 1.7(6) . . . . ? C2 C3 C4 C5 -178.3(5) . . . . ? N1 C4 C5 C6 1.2(8) . . . . ? C3 C4 C5 C6 -178.8(5) . . . . ? N1 C4 C5 C11 -178.9(4) . . . . ? C3 C4 C5 C11 1.0(7) . . . . ? C9 N2 C6 C5 177.8(4) . . . . ? Rh1 N2 C6 C5 -2.9(7) . . . . ? C9 N2 C6 C7 -1.6(5) . . . . ? Rh1 N2 C6 C7 177.7(3) . . . . ? C4 C5 C6 N2 0.8(8) . . . . ? C11 C5 C6 N2 -179.1(4) . . . . ? C4 C5 C6 C7 -180.0(5) . . . . ? C11 C5 C6 C7 0.2(7) . . . . ? N2 C6 C7 C8 1.6(5) . . . . ? C5 C6 C7 C8 -177.8(4) . . . . ? C6 C7 C8 C9 -0.8(5) . . . . ? C6 N2 C9 C10 178.5(4) . . . . ? Rh1 N2 C9 C10 -0.8(7) . . . . ? C6 N2 C9 C8 1.1(5) . . . . ? Rh1 N2 C9 C8 -178.2(3) . . . . ? C7 C8 C9 N2 -0.1(5) . . . . ? C7 C8 C9 C10 -177.6(5) . . . . ? N2 C9 C10 C1 -2.3(8) . . . 2 ? C8 C9 C10 C1 174.7(5) . . . 2 ? N2 C9 C10 C25 177.9(4) . . . . ? C8 C9 C10 C25 -5.1(7) . . . . ? C4 C5 C11 C12 59.5(6) . . . . ? C6 C5 C11 C12 -120.7(5) . . . . ? C4 C5 C11 C16 -117.7(5) . . . . ? C6 C5 C11 C16 62.2(7) . . . . ? C16 C11 C12 C13 0.3(8) . . . . ? C5 C11 C12 C13 -176.9(5) . . . . ? C11 C12 C13 C14 -1.1(8) . . . . ? C11 C12 C13 C17 176.4(5) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C17 C13 C14 C15 -177.2(5) . . . . ? C13 C14 C15 C16 1.4(8) . . . . ? C13 C14 C15 C21 -178.8(5) . . . . ? C14 C15 C16 C11 -2.3(8) . . . . ? C21 C15 C16 C11 177.9(5) . . . . ? C12 C11 C16 C15 1.5(8) . . . . ? C5 C11 C16 C15 178.6(5) . . . . ? C14 C13 C17 C19 -7.1(9) . . . . ? C12 C13 C17 C19 175.5(7) . . . . ? C14 C13 C17 C20 -128.3(6) . . . . ? C12 C13 C17 C20 54.3(7) . . . . ? C14 C13 C17 C18 115.2(7) . . . . ? C12 C13 C17 C18 -62.2(8) . . . . ? C16 C15 C21 C24 53.5(8) . . . . ? C14 C15 C21 C24 -126.4(6) . . . . ? C16 C15 C21 C23 -68.0(7) . . . . ? C14 C15 C21 C23 112.2(7) . . . . ? C16 C15 C21 C22 174.2(6) . . . . ? C14 C15 C21 C22 -5.6(8) . . . . ? C1 C10 C25 C30 -67.9(7) 2 . . . ? C9 C10 C25 C30 111.9(6) . . . . ? C1 C10 C25 C26 111.3(5) 2 . . . ? C9 C10 C25 C26 -68.9(6) . . . . ? C30 C25 C26 C27 0.0(8) . . . . ? C10 C25 C26 C27 -179.2(5) . . . . ? C25 C26 C27 C28 -0.3(8) . . . . ? C25 C26 C27 C31 -179.4(6) . . . . ? C26 C27 C28 C29 1.2(10) . . . . ? C31 C27 C28 C29 -179.8(7) . . . . ? C27 C28 C29 C30 -1.6(12) . . . . ? C27 C28 C29 C35 179.8(10) . . . . ? C26 C25 C30 C29 -0.4(9) . . . . ? C10 C25 C30 C29 178.8(6) . . . . ? C28 C29 C30 C25 1.2(11) . . . . ? C35 C29 C30 C25 179.9(9) . . . . ? C28 C27 C31 C34 63.4(13) . . . . ? C26 C27 C31 C34 -117.6(11) . . . . ? C28 C27 C31 C32 -171.9(8) . . . . ? C26 C27 C31 C32 7.1(11) . . . . ? C28 C27 C31 C33 -54.9(10) . . . . ? C26 C27 C31 C33 124.1(9) . . . . ? C30 C29 C35 C37 46.7(14) . . . . ? C28 C29 C35 C37 -134.7(10) . . . . ? C30 C29 C35 C36 -72.4(13) . . . . ? C28 C29 C35 C36 106.1(11) . . . . ? C30 C29 C35 C38 169.1(13) . . . . ? C28 C29 C35 C38 -12(2) . . . . ? C51 P1 C39 C44 -138.8(5) . . . . ? C45 P1 C39 C44 -29.4(6) . . . . ? Rh1 P1 C39 C44 100.4(5) . . . . ? C51 P1 C39 C40 44.7(5) . . . . ? C45 P1 C39 C40 154.2(5) . . . . ? Rh1 P1 C39 C40 -76.1(5) . . . . ? C44 C39 C40 C41 0.2(11) . . . . ? P1 C39 C40 C41 176.9(6) . . . . ? C39 C40 C41 C42 2.2(13) . . . . ? C40 C41 C42 C43 -2.9(13) . . . . ? C41 C42 C43 C44 1.2(12) . . . . ? C40 C39 C44 C43 -1.8(9) . . . . ? P1 C39 C44 C43 -178.3(5) . . . . ? C42 C43 C44 C39 1.2(11) . . . . ? C51 P1 C45 C46 167.6(4) . . . . ? C39 P1 C45 C46 60.0(5) . . . . ? Rh1 P1 C45 C46 -70.5(4) . . . . ? C51 P1 C45 C50 -13.1(5) . . . . ? C39 P1 C45 C50 -120.7(4) . . . . ? Rh1 P1 C45 C50 108.8(4) . . . . ? C50 C45 C46 C47 3.7(8) . . . . ? P1 C45 C46 C47 -176.9(4) . . . . ? C45 C46 C47 C48 -1.4(9) . . . . ? C46 C47 C48 C49 -2.5(10) . . . . ? C47 C48 C49 C50 3.9(10) . . . . ? C48 C49 C50 C45 -1.5(9) . . . . ? C46 C45 C50 C49 -2.3(8) . . . . ? P1 C45 C50 C49 178.4(4) . . . . ? C58 C53 C54 C55 3.1(11) . . . . ? C52 C53 C54 C55 -176.4(7) . . . . ? C53 C54 C55 C56 -0.9(14) . . . . ? C54 C55 C56 C57 -1.6(15) . . . . ? C55 C56 C57 C58 2.0(15) . . . . ? C56 C57 C58 C53 0.2(13) . . . . ? C54 C53 C58 C57 -2.7(11) . . . . ? C52 C53 C58 C57 176.7(7) . . . . ? C1S C2S C3S C4S -87(3) . . . . ? C2S C3S C4S C5S 166(2) . . . . ? #============================================================================= data_P2_Ru2 _database_code_depnum_ccdc_archive 'CCDC 834655' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H74 N4 P2 Ru' _chemical_formula_sum 'C76 H74 N4 P2 Ru' _chemical_formula_weight 1206.40 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5833(3) _cell_length_b 12.2478(3) _cell_length_c 13.1535(3) _cell_angle_alpha 96.180(1) _cell_angle_beta 110.866(1) _cell_angle_gamma 113.422(1) _cell_volume 1530.93(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25482 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 18951 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0465 _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 17 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 6976 _reflns_number_gt 6232 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _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^)+(0.0283P)^2^+1.1653P] 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 6976 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.451 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.085 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 0.0000 0.0000 0.0000 0.01805(7) Uani 1 2 d S . . P1 P 0.17148(5) 0.14971(4) -0.04033(4) 0.02168(11) Uani 1 1 d . . . N1 N -0.06889(16) -0.11019(13) -0.16036(13) 0.0194(3) Uani 1 1 d . . . N2 N 0.13295(16) -0.07302(13) 0.06535(13) 0.0196(3) Uani 1 1 d . . . C1 C -0.1680(2) -0.11421(17) -0.25871(16) 0.0224(4) Uani 1 1 d . . . C2 C -0.1914(2) -0.20636(18) -0.35362(17) 0.0265(4) Uani 1 1 d . . . C3 C -0.1070(2) -0.25807(17) -0.30978(17) 0.0245(4) Uani 1 1 d . . . C4 C -0.02975(19) -0.19716(16) -0.18828(16) 0.0208(4) Uani 1 1 d . . . C5 C 0.0695(2) -0.22081(17) -0.11037(17) 0.0227(4) Uani 1 1 d . . . H5A H 0.0857 -0.2845 -0.1403 0.027 Uiso 1 1 calc R . . C6 C 0.14768(19) -0.16220(16) 0.00595(16) 0.0209(4) Uani 1 1 d . . . C7 C 0.2567(2) -0.18442(17) 0.08369(17) 0.0237(4) Uani 1 1 d . . . C8 C 0.3038(2) -0.10961(17) 0.18920(17) 0.0239(4) Uani 1 1 d . . . C9 C 0.22518(19) -0.04056(17) 0.17700(16) 0.0215(4) Uani 1 1 d . . . C10 C 0.2402(2) 0.04551(17) 0.26510(17) 0.0238(4) Uani 1 1 d . . . H10A H 0.3080 0.0592 0.3387 0.029 Uiso 1 1 calc R . . C11 C -0.2901(3) -0.2348(2) -0.47549(19) 0.0387(5) Uani 1 1 d . . . H11A H -0.3820 -0.2479 -0.4798 0.046 Uiso 1 1 calc R . . H11B H -0.3041 -0.3132 -0.5201 0.046 Uiso 1 1 calc R . . C12 C -0.2383(4) -0.1322(3) -0.5287(2) 0.0587(8) Uani 1 1 d . . . H12A H -0.3033 -0.1586 -0.6094 0.088 Uiso 1 1 calc R . . H12B H -0.1453 -0.1157 -0.5214 0.088 Uiso 1 1 calc R . . H12C H -0.2331 -0.0564 -0.4896 0.088 Uiso 1 1 calc R . . C13 C -0.1009(2) -0.36502(19) -0.37130(18) 0.0307(5) Uani 1 1 d . . . H13A H -0.0067 -0.3580 -0.3315 0.037 Uiso 1 1 calc R . . H13B H -0.1157 -0.3604 -0.4493 0.037 Uiso 1 1 calc R . . C14 C -0.2105(3) -0.4902(2) -0.3777(2) 0.0481(6) Uani 1 1 d . . . H14A H -0.2026 -0.5572 -0.4177 0.072 Uiso 1 1 calc R . . H14B H -0.3041 -0.4984 -0.4188 0.072 Uiso 1 1 calc R . . H14C H -0.1955 -0.4955 -0.3006 0.072 Uiso 1 1 calc R . . C15 C 0.3080(2) -0.2718(2) 0.0519(2) 0.0319(5) Uani 1 1 d . . . H15A H 0.4113 -0.2264 0.0840 0.038 Uiso 1 1 calc R . . H15B H 0.2706 -0.2989 -0.0319 0.038 Uiso 1 1 calc R . . C16 C 0.2659(4) -0.3858(2) 0.0934(3) 0.0567(8) Uani 1 1 d . . . H16A H 0.3012 -0.4393 0.0690 0.085 Uiso 1 1 calc R . . H16B H 0.1637 -0.4318 0.0615 0.085 Uiso 1 1 calc R . . H16C H 0.3057 -0.3601 0.1766 0.085 Uiso 1 1 calc R . . C17 C 0.4167(2) -0.09565(19) 0.29910(18) 0.0291(4) Uani 1 1 d . . . H17A H 0.4788 -0.0059 0.3393 0.035 Uiso 1 1 calc R . . H17B H 0.4737 -0.1306 0.2818 0.035 Uiso 1 1 calc R . . C18 C 0.3632(3) -0.1589(2) 0.3783(2) 0.0411(6) Uani 1 1 d . . . H18A H 0.4425 -0.1482 0.4467 0.062 Uiso 1 1 calc R . . H18B H 0.3009 -0.2477 0.3393 0.062 Uiso 1 1 calc R . . H18C H 0.3116 -0.1213 0.4000 0.062 Uiso 1 1 calc R . . C19 C 0.3313(2) 0.28798(18) 0.06523(18) 0.0257(4) Uani 1 1 d . . . C20 C 0.4464(2) 0.3437(2) 0.0422(2) 0.0373(5) Uani 1 1 d . . . H20A H 0.4425 0.3099 -0.0282 0.045 Uiso 1 1 calc R . . C21 C 0.5669(2) 0.4485(2) 0.1215(2) 0.0448(6) Uani 1 1 d . . . H21A H 0.6454 0.4853 0.1057 0.054 Uiso 1 1 calc R . . C22 C 0.5727(3) 0.4990(2) 0.2230(2) 0.0456(6) Uani 1 1 d . . . H22A H 0.6550 0.5706 0.2771 0.055 Uiso 1 1 calc R . . C23 C 0.4588(3) 0.4455(2) 0.2462(2) 0.0426(6) Uani 1 1 d . . . H23A H 0.4629 0.4806 0.3162 0.051 Uiso 1 1 calc R . . C24 C 0.3388(2) 0.34106(19) 0.16772(19) 0.0327(5) Uani 1 1 d . . . H24A H 0.2606 0.3052 0.1841 0.039 Uiso 1 1 calc R . . C25 C 0.1079(2) 0.22360(18) -0.14623(18) 0.0259(4) Uani 1 1 d . . . C26 C 0.0749(2) 0.31475(19) -0.1127(2) 0.0320(5) Uani 1 1 d . . . H26A H 0.0798 0.3327 -0.0388 0.038 Uiso 1 1 calc R . . C27 C 0.0352(2) 0.3793(2) -0.1863(2) 0.0406(6) Uani 1 1 d . . . H27A H 0.0129 0.4415 -0.1628 0.049 Uiso 1 1 calc R . . C28 C 0.0279(3) 0.3532(2) -0.2941(2) 0.0436(6) Uani 1 1 d . . . H28A H 0.0039 0.3996 -0.3439 0.052 Uiso 1 1 calc R . . C29 C 0.0554(3) 0.2599(3) -0.3293(2) 0.0438(6) Uani 1 1 d . . . H29A H 0.0468 0.2399 -0.4044 0.053 Uiso 1 1 calc R . . C30 C 0.0956(2) 0.1953(2) -0.2560(2) 0.0355(5) Uani 1 1 d . . . H30A H 0.1148 0.1314 -0.2806 0.043 Uiso 1 1 calc R . . C31 C 0.2424(2) 0.07780(18) -0.10619(18) 0.0278(4) Uani 1 1 d . . . C32 C 0.2730(2) 0.01383(19) -0.15571(19) 0.0293(4) Uani 1 1 d . . . C33 C 0.2999(2) -0.06940(18) -0.21800(18) 0.0280(4) Uani 1 1 d . . . C34 C 0.4045(3) -0.1011(2) -0.1650(2) 0.0373(5) Uani 1 1 d . . . H34A H 0.4621 -0.0655 -0.0855 0.045 Uiso 1 1 calc R . . C35 C 0.4252(3) -0.1838(2) -0.2269(2) 0.0447(6) Uani 1 1 d . . . H35A H 0.4972 -0.2045 -0.1898 0.054 Uiso 1 1 calc R . . C36 C 0.3424(3) -0.2365(2) -0.3417(2) 0.0431(6) Uani 1 1 d . . . H36A H 0.3560 -0.2946 -0.3837 0.052 Uiso 1 1 calc R . . C37 C 0.2394(3) -0.2050(2) -0.3959(2) 0.0444(6) Uani 1 1 d . . . H37A H 0.1830 -0.2404 -0.4756 0.053 Uiso 1 1 calc R . . C38 C 0.2178(2) -0.1223(2) -0.3349(2) 0.0367(5) Uani 1 1 d . . . H38A H 0.1464 -0.1012 -0.3729 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 0.01877(11) 0.01547(11) 0.01940(12) 0.00354(8) 0.00802(9) 0.00824(8) P1 0.0220(2) 0.0190(2) 0.0239(3) 0.0050(2) 0.0104(2) 0.0095(2) N1 0.0218(8) 0.0162(7) 0.0201(8) 0.0041(6) 0.0094(6) 0.0090(6) N2 0.0208(7) 0.0171(7) 0.0216(8) 0.0038(6) 0.0090(6) 0.0100(6) C1 0.0253(9) 0.0189(9) 0.0201(10) 0.0034(7) 0.0086(8) 0.0095(8) C2 0.0318(11) 0.0237(10) 0.0218(10) 0.0032(8) 0.0105(9) 0.0129(8) C3 0.0286(10) 0.0198(9) 0.0243(10) 0.0034(8) 0.0129(8) 0.0102(8) C4 0.0232(9) 0.0178(8) 0.0215(9) 0.0042(7) 0.0116(8) 0.0085(7) C5 0.0260(10) 0.0181(9) 0.0278(10) 0.0061(8) 0.0149(8) 0.0110(8) C6 0.0227(9) 0.0174(8) 0.0256(10) 0.0069(7) 0.0123(8) 0.0104(7) C7 0.0241(9) 0.0219(9) 0.0302(11) 0.0103(8) 0.0138(8) 0.0132(8) C8 0.0219(9) 0.0212(9) 0.0297(11) 0.0085(8) 0.0110(8) 0.0111(8) C9 0.0195(9) 0.0194(9) 0.0247(10) 0.0065(7) 0.0086(8) 0.0092(7) C10 0.0221(9) 0.0231(9) 0.0216(10) 0.0046(8) 0.0064(8) 0.0098(8) C11 0.0481(14) 0.0402(13) 0.0229(11) 0.0005(9) 0.0059(10) 0.0269(11) C12 0.087(2) 0.081(2) 0.0361(15) 0.0269(15) 0.0313(15) 0.0586(19) C13 0.0400(12) 0.0287(10) 0.0245(11) 0.0023(8) 0.0132(9) 0.0194(9) C14 0.0553(16) 0.0259(11) 0.0567(17) 0.0013(11) 0.0229(14) 0.0173(11) C15 0.0361(11) 0.0339(11) 0.0342(12) 0.0107(9) 0.0141(10) 0.0250(10) C16 0.095(2) 0.0388(14) 0.0592(18) 0.0186(13) 0.0418(17) 0.0446(16) C17 0.0253(10) 0.0286(10) 0.0322(11) 0.0083(9) 0.0081(9) 0.0155(9) C18 0.0437(14) 0.0429(13) 0.0358(13) 0.0180(11) 0.0132(11) 0.0214(11) C19 0.0222(9) 0.0220(9) 0.0307(11) 0.0079(8) 0.0093(8) 0.0103(8) C20 0.0304(11) 0.0375(12) 0.0366(13) 0.0061(10) 0.0166(10) 0.0088(10) C21 0.0279(12) 0.0410(13) 0.0519(16) 0.0082(12) 0.0202(11) 0.0029(10) C22 0.0311(12) 0.0334(12) 0.0465(15) -0.0024(11) 0.0113(11) 0.0002(10) C23 0.0388(13) 0.0348(12) 0.0362(13) -0.0045(10) 0.0143(11) 0.0064(10) C24 0.0289(11) 0.0264(10) 0.0376(12) 0.0042(9) 0.0172(10) 0.0071(9) C25 0.0221(9) 0.0217(9) 0.0302(11) 0.0090(8) 0.0112(8) 0.0069(8) C26 0.0323(11) 0.0282(11) 0.0375(12) 0.0122(9) 0.0163(10) 0.0143(9) C27 0.0355(12) 0.0346(12) 0.0522(15) 0.0171(11) 0.0149(11) 0.0195(10) C28 0.0358(12) 0.0472(14) 0.0452(15) 0.0259(12) 0.0125(11) 0.0186(11) C29 0.0433(14) 0.0602(16) 0.0318(13) 0.0222(12) 0.0161(11) 0.0260(13) C30 0.0363(12) 0.0394(12) 0.0333(12) 0.0131(10) 0.0164(10) 0.0184(10) C31 0.0270(10) 0.0232(10) 0.0342(11) 0.0085(9) 0.0167(9) 0.0099(8) C32 0.0289(10) 0.0259(10) 0.0346(12) 0.0095(9) 0.0165(9) 0.0116(9) C33 0.0308(11) 0.0251(10) 0.0320(11) 0.0082(9) 0.0188(9) 0.0122(9) C34 0.0461(13) 0.0428(13) 0.0266(12) 0.0081(10) 0.0138(10) 0.0266(11) C35 0.0542(15) 0.0513(15) 0.0465(15) 0.0181(12) 0.0229(13) 0.0394(13) C36 0.0530(15) 0.0375(13) 0.0442(14) 0.0025(11) 0.0259(12) 0.0244(12) C37 0.0390(13) 0.0474(14) 0.0327(13) -0.0033(11) 0.0116(11) 0.0147(11) C38 0.0291(11) 0.0433(13) 0.0341(12) 0.0066(10) 0.0110(10) 0.0174(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.0561(15) 2 ? Ru1 N2 2.0561(15) . ? Ru1 N1 2.0589(15) 2 ? Ru1 N1 2.0589(15) . ? Ru1 P1 2.3777(5) . ? Ru1 P1 2.3777(5) 2 ? P1 C31 1.766(2) . ? P1 C25 1.836(2) . ? P1 C19 1.842(2) . ? N1 C1 1.370(2) . ? N1 C4 1.376(2) . ? N2 C9 1.369(2) . ? N2 C6 1.376(2) . ? C1 C10 1.393(3) 2 ? C1 C2 1.455(3) . ? C2 C3 1.363(3) . ? C2 C11 1.502(3) . ? C3 C4 1.451(3) . ? C3 C13 1.504(3) . ? C4 C5 1.395(3) . ? C5 C6 1.391(3) . ? C5 H5A 0.9500 . ? C6 C7 1.459(3) . ? C7 C8 1.361(3) . ? C7 C15 1.503(3) . ? C8 C9 1.452(3) . ? C8 C17 1.500(3) . ? C9 C10 1.390(3) . ? C10 C1 1.393(3) 2 ? C10 H10A 0.9500 . ? C11 C12 1.522(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.523(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.517(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.524(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.389(3) . ? C19 C20 1.395(3) . ? C20 C21 1.391(3) . ? C20 H20A 0.9500 . ? C21 C22 1.376(4) . ? C21 H21A 0.9500 . ? C22 C23 1.379(3) . ? C22 H22A 0.9500 . ? C23 C24 1.384(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.389(3) . ? C25 C26 1.393(3) . ? C26 C27 1.382(3) . ? C26 H26A 0.9500 . ? C27 C28 1.385(4) . ? C27 H27A 0.9500 . ? C28 C29 1.380(4) . ? C28 H28A 0.9500 . ? C29 C30 1.382(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.200(3) . ? C32 C33 1.436(3) . ? C33 C34 1.391(3) . ? C33 C38 1.394(3) . ? C34 C35 1.378(3) . ? C34 H34A 0.9500 . ? C35 C36 1.373(4) . ? C35 H35A 0.9500 . ? C36 C37 1.379(4) . ? C36 H36A 0.9500 . ? C37 C38 1.379(3) . ? C37 H37A 0.9500 . ? C38 H38A 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 N2 Ru1 N2 180.00(12) 2 . ? N2 Ru1 N1 89.59(6) 2 2 ? N2 Ru1 N1 90.41(6) . 2 ? N2 Ru1 N1 90.41(6) 2 . ? N2 Ru1 N1 89.59(6) . . ? N1 Ru1 N1 180.00(9) 2 . ? N2 Ru1 P1 90.10(4) 2 . ? N2 Ru1 P1 89.90(4) . . ? N1 Ru1 P1 94.54(4) 2 . ? N1 Ru1 P1 85.46(4) . . ? N2 Ru1 P1 89.90(4) 2 2 ? N2 Ru1 P1 90.10(4) . 2 ? N1 Ru1 P1 85.46(4) 2 2 ? N1 Ru1 P1 94.54(4) . 2 ? P1 Ru1 P1 180.00(3) . 2 ? C31 P1 C25 100.94(10) . . ? C31 P1 C19 101.06(10) . . ? C25 P1 C19 99.07(9) . . ? C31 P1 Ru1 110.37(7) . . ? C25 P1 Ru1 116.25(6) . . ? C19 P1 Ru1 125.60(7) . . ? C1 N1 C4 107.32(15) . . ? C1 N1 Ru1 125.82(12) . . ? C4 N1 Ru1 126.79(13) . . ? C9 N2 C6 106.93(15) . . ? C9 N2 Ru1 126.14(12) . . ? C6 N2 Ru1 126.93(13) . . ? N1 C1 C10 124.90(17) . 2 ? N1 C1 C2 109.41(17) . . ? C10 C1 C2 125.60(18) 2 . ? C3 C2 C1 106.85(17) . . ? C3 C2 C11 128.31(19) . . ? C1 C2 C11 124.84(19) . . ? C2 C3 C4 107.11(17) . . ? C2 C3 C13 127.65(19) . . ? C4 C3 C13 125.07(18) . . ? N1 C4 C5 124.37(17) . . ? N1 C4 C3 109.29(16) . . ? C5 C4 C3 126.34(17) . . ? C6 C5 C4 127.76(18) . . ? C6 C5 H5A 116.1 . . ? C4 C5 H5A 116.1 . . ? N2 C6 C5 124.41(17) . . ? N2 C6 C7 109.42(16) . . ? C5 C6 C7 126.18(17) . . ? C8 C7 C6 106.84(17) . . ? C8 C7 C15 127.04(18) . . ? C6 C7 C15 126.12(18) . . ? C7 C8 C9 106.89(17) . . ? C7 C8 C17 128.37(18) . . ? C9 C8 C17 124.73(18) . . ? N2 C9 C10 124.68(17) . . ? N2 C9 C8 109.91(17) . . ? C10 C9 C8 125.41(18) . . ? C9 C10 C1 128.00(18) . 2 ? C9 C10 H10A 116.0 . . ? C1 C10 H10A 116.0 2 . ? C2 C11 C12 113.2(2) . . ? C2 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C2 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 C14 111.99(19) . . ? C3 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? C3 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C15 C16 113.6(2) . . ? C7 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C7 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C8 C17 C18 114.36(18) . . ? C8 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? C8 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 118.53(19) . . ? C24 C19 P1 121.11(15) . . ? C20 C19 P1 120.34(17) . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C23 C24 C19 120.8(2) . . ? C23 C24 H24A 119.6 . . ? C19 C24 H24A 119.6 . . ? C30 C25 C26 119.1(2) . . ? C30 C25 P1 123.08(17) . . ? C26 C25 P1 117.80(16) . . ? C27 C26 C25 120.5(2) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C26 C27 C28 119.8(2) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C29 C28 C27 119.9(2) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.4(2) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C29 C30 C25 120.2(2) . . ? C29 C30 H30A 119.9 . . ? C25 C30 H30A 119.9 . . ? C32 C31 P1 170.67(18) . . ? C31 C32 C33 176.1(2) . . ? C34 C33 C38 118.4(2) . . ? C34 C33 C32 122.0(2) . . ? C38 C33 C32 119.5(2) . . ? C35 C34 C33 120.6(2) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C36 C35 C34 120.4(2) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C37 119.8(2) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C36 C37 C38 120.3(2) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C37 C38 C33 120.5(2) . . ? C37 C38 H38A 119.8 . . ? C33 C38 H38A 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 P1 C31 -133.86(9) 2 . . . ? N2 Ru1 P1 C31 46.14(9) . . . . ? N1 Ru1 P1 C31 136.55(9) 2 . . . ? N1 Ru1 P1 C31 -43.45(9) . . . . ? N2 Ru1 P1 C25 -19.73(9) 2 . . . ? N2 Ru1 P1 C25 160.27(9) . . . . ? N1 Ru1 P1 C25 -109.32(9) 2 . . . ? N1 Ru1 P1 C25 70.68(9) . . . . ? N2 Ru1 P1 C19 104.97(9) 2 . . . ? N2 Ru1 P1 C19 -75.03(9) . . . . ? N1 Ru1 P1 C19 15.38(9) 2 . . . ? N1 Ru1 P1 C19 -164.62(9) . . . . ? N2 Ru1 N1 C1 -0.11(15) 2 . . . ? N2 Ru1 N1 C1 179.89(15) . . . . ? P1 Ru1 N1 C1 -90.18(14) . . . . ? P1 Ru1 N1 C1 89.82(14) 2 . . . ? N2 Ru1 N1 C4 -176.74(15) 2 . . . ? N2 Ru1 N1 C4 3.26(15) . . . . ? P1 Ru1 N1 C4 93.19(14) . . . . ? P1 Ru1 N1 C4 -86.81(14) 2 . . . ? N1 Ru1 N2 C9 -1.74(15) 2 . . . ? N1 Ru1 N2 C9 178.26(15) . . . . ? P1 Ru1 N2 C9 92.80(14) . . . . ? P1 Ru1 N2 C9 -87.20(14) 2 . . . ? N1 Ru1 N2 C6 179.02(15) 2 . . . ? N1 Ru1 N2 C6 -0.98(15) . . . . ? P1 Ru1 N2 C6 -86.44(14) . . . . ? P1 Ru1 N2 C6 93.56(14) 2 . . . ? C4 N1 C1 C10 175.77(18) . . . 2 ? Ru1 N1 C1 C10 -1.4(3) . . . 2 ? C4 N1 C1 C2 -0.9(2) . . . . ? Ru1 N1 C1 C2 -178.09(12) . . . . ? N1 C1 C2 C3 1.1(2) . . . . ? C10 C1 C2 C3 -175.53(19) 2 . . . ? N1 C1 C2 C11 -178.43(19) . . . . ? C10 C1 C2 C11 4.9(3) 2 . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? C11 C2 C3 C4 178.7(2) . . . . ? C1 C2 C3 C13 174.61(19) . . . . ? C11 C2 C3 C13 -5.9(4) . . . . ? C1 N1 C4 C5 -179.92(17) . . . . ? Ru1 N1 C4 C5 -2.8(3) . . . . ? C1 N1 C4 C3 0.4(2) . . . . ? Ru1 N1 C4 C3 177.53(12) . . . . ? C2 C3 C4 N1 0.3(2) . . . . ? C13 C3 C4 N1 -175.29(18) . . . . ? C2 C3 C4 C5 -179.38(18) . . . . ? C13 C3 C4 C5 5.0(3) . . . . ? N1 C4 C5 C6 -1.3(3) . . . . ? C3 C4 C5 C6 178.35(18) . . . . ? C9 N2 C6 C5 178.62(17) . . . . ? Ru1 N2 C6 C5 -2.0(3) . . . . ? C9 N2 C6 C7 -1.4(2) . . . . ? Ru1 N2 C6 C7 177.93(12) . . . . ? C4 C5 C6 N2 3.9(3) . . . . ? C4 C5 C6 C7 -176.10(18) . . . . ? N2 C6 C7 C8 1.1(2) . . . . ? C5 C6 C7 C8 -178.90(18) . . . . ? N2 C6 C7 C15 -177.86(18) . . . . ? C5 C6 C7 C15 2.1(3) . . . . ? C6 C7 C8 C9 -0.4(2) . . . . ? C15 C7 C8 C9 178.60(18) . . . . ? C6 C7 C8 C17 -179.24(18) . . . . ? C15 C7 C8 C17 -0.2(3) . . . . ? C6 N2 C9 C10 -178.59(17) . . . . ? Ru1 N2 C9 C10 2.1(3) . . . . ? C6 N2 C9 C8 1.2(2) . . . . ? Ru1 N2 C9 C8 -178.18(12) . . . . ? C7 C8 C9 N2 -0.5(2) . . . . ? C17 C8 C9 N2 178.42(17) . . . . ? C7 C8 C9 C10 179.29(18) . . . . ? C17 C8 C9 C10 -1.8(3) . . . . ? N2 C9 C10 C1 -0.2(3) . . . 2 ? C8 C9 C10 C1 -179.91(19) . . . 2 ? C3 C2 C11 C12 -107.5(3) . . . . ? C1 C2 C11 C12 72.0(3) . . . . ? C2 C3 C13 C14 -84.8(3) . . . . ? C4 C3 C13 C14 89.9(3) . . . . ? C8 C7 C15 C16 71.5(3) . . . . ? C6 C7 C15 C16 -109.7(2) . . . . ? C7 C8 C17 C18 -104.8(3) . . . . ? C9 C8 C17 C18 76.6(3) . . . . ? C31 P1 C19 C24 -150.06(18) . . . . ? C25 P1 C19 C24 106.82(18) . . . . ? Ru1 P1 C19 C24 -24.9(2) . . . . ? C31 P1 C19 C20 31.7(2) . . . . ? C25 P1 C19 C20 -71.39(19) . . . . ? Ru1 P1 C19 C20 156.92(15) . . . . ? C24 C19 C20 C21 1.4(3) . . . . ? P1 C19 C20 C21 179.68(19) . . . . ? C19 C20 C21 C22 -0.9(4) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C22 C23 C24 C19 0.5(4) . . . . ? C20 C19 C24 C23 -1.2(3) . . . . ? P1 C19 C24 C23 -179.47(19) . . . . ? C31 P1 C25 C30 13.33(19) . . . . ? C19 P1 C25 C30 116.56(18) . . . . ? Ru1 P1 C25 C30 -106.05(17) . . . . ? C31 P1 C25 C26 -164.69(16) . . . . ? C19 P1 C25 C26 -61.46(17) . . . . ? Ru1 P1 C25 C26 75.92(16) . . . . ? C30 C25 C26 C27 -2.3(3) . . . . ? P1 C25 C26 C27 175.85(17) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C29 2.3(4) . . . . ? C27 C28 C29 C30 -2.5(4) . . . . ? C28 C29 C30 C25 0.3(4) . . . . ? C26 C25 C30 C29 2.1(3) . . . . ? P1 C25 C30 C29 -175.92(18) . . . . ? C38 C33 C34 C35 -0.6(3) . . . . ? C32 C33 C34 C35 178.3(2) . . . . ? C33 C34 C35 C36 -0.3(4) . . . . ? C34 C35 C36 C37 1.1(4) . . . . ? C35 C36 C37 C38 -1.0(4) . . . . ? C36 C37 C38 C33 0.2(4) . . . . ? C34 C33 C38 C37 0.6(3) . . . . ? C32 C33 C38 C37 -178.3(2) . . . . ? #============================================================================= data_P2_Ru3 _database_code_depnum_ccdc_archive 'CCDC 834656' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H74 N4 P2 Ru, C H Cl3' _chemical_formula_sum 'C85 H75 Cl3 N4 P2 Ru' _chemical_formula_weight 1421.85 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0429(2) _cell_length_b 13.5072(2) _cell_length_c 13.9191(3) _cell_angle_alpha 62.832(1) _cell_angle_beta 80.910(1) _cell_angle_gamma 68.659(1) _cell_volume 1720.36(5) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13667 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; Chloroform molecule disordered over centre of inversion - one chloroform molecule per cell (i.e. one per porphyrin complex). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 19763 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 7847 _reflns_number_gt 6551 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _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^)+(0.0231P)^2^+1.6041P] 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 7847 _refine_ls_number_parameters 453 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.354 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.073 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 0.5000 0.5000 0.5000 0.01774(8) Uani 1 2 d S . . P1 P 0.29611(5) 0.64941(5) 0.44184(5) 0.02042(13) Uani 1 1 d . . . N1 N 0.41579(16) 0.39966(15) 0.63466(15) 0.0196(4) Uani 1 1 d . . . N2 N 0.46794(16) 0.41084(15) 0.42460(15) 0.0194(4) Uani 1 1 d . . . C1 C 0.4053(2) 0.4064(2) 0.73113(19) 0.0234(5) Uani 1 1 d . . . C2 C 0.3506(2) 0.3202(2) 0.81137(19) 0.0269(5) Uani 1 1 d . . . C3 C 0.3303(2) 0.2589(2) 0.76409(19) 0.0263(5) Uani 1 1 d . . . C4 C 0.3696(2) 0.31041(19) 0.65088(18) 0.0213(5) Uani 1 1 d . . . C5 C 0.3666(2) 0.27595(19) 0.57007(19) 0.0213(5) Uani 1 1 d . . . C6 C 0.4102(2) 0.32417(19) 0.46382(18) 0.0207(4) Uani 1 1 d . . . C7 C 0.4003(2) 0.2967(2) 0.37520(19) 0.0248(5) Uani 1 1 d . . . C8 C 0.4538(2) 0.3649(2) 0.28726(19) 0.0244(5) Uani 1 1 d . . . C9 C 0.4953(2) 0.43661(19) 0.31829(18) 0.0220(5) Uani 1 1 d . . . C10 C 0.5535(2) 0.51909(19) 0.24925(18) 0.0231(5) Uani 1 1 d . . . H10A H 0.5670 0.5254 0.1778 0.028 Uiso 1 1 calc R . . C11 C 0.2856(3) 0.1530(2) 0.8247(2) 0.0386(6) Uani 1 1 d . . . H11A H 0.2773 0.1354 0.9015 0.058 Uiso 1 1 calc R . . H11B H 0.3493 0.0849 0.8160 0.058 Uiso 1 1 calc R . . H11C H 0.2011 0.1702 0.7959 0.058 Uiso 1 1 calc R . . C12 C 0.3371(3) 0.2157(2) 0.3734(2) 0.0357(6) Uani 1 1 d . . . H12A H 0.3362 0.2252 0.2993 0.054 Uiso 1 1 calc R . . H12B H 0.2478 0.2354 0.3994 0.054 Uiso 1 1 calc R . . H12C H 0.3864 0.1337 0.4201 0.054 Uiso 1 1 calc R . . C13 C 0.3323(3) 0.2989(3) 0.9280(2) 0.0417(7) Uani 1 1 d . . . H13A H 0.2644 0.2614 0.9596 0.050 Uiso 1 1 calc R . . H13B H 0.3016 0.3756 0.9318 0.050 Uiso 1 1 calc R . . C14 C 0.4571(4) 0.2203(3) 0.9944(2) 0.0588(9) Uani 1 1 d . . . H14A H 0.4397 0.2064 1.0699 0.088 Uiso 1 1 calc R . . H14B H 0.5231 0.2592 0.9661 0.088 Uiso 1 1 calc R . . H14C H 0.4889 0.1448 0.9898 0.088 Uiso 1 1 calc R . . C15 C 0.4627(3) 0.3748(2) 0.1742(2) 0.0325(6) Uani 1 1 d . . . H15A H 0.4623 0.3002 0.1774 0.039 Uiso 1 1 calc R . . H15B H 0.5462 0.3859 0.1424 0.039 Uiso 1 1 calc R . . C16 C 0.3515(3) 0.4768(3) 0.1014(2) 0.0459(7) Uani 1 1 d . . . H16A H 0.3604 0.4780 0.0297 0.069 Uiso 1 1 calc R . . H16B H 0.3541 0.5514 0.0950 0.069 Uiso 1 1 calc R . . H16C H 0.2684 0.4666 0.1327 0.069 Uiso 1 1 calc R . . C17 C 0.3078(2) 0.1817(2) 0.59940(19) 0.0248(5) Uani 1 1 d . . . C18 C 0.3857(2) 0.0652(2) 0.6267(2) 0.0342(6) Uani 1 1 d . . . H18A H 0.4776 0.0444 0.6284 0.041 Uiso 1 1 calc R . . C19 C 0.3308(3) -0.0211(2) 0.6514(3) 0.0458(7) Uani 1 1 d . . . H19A H 0.3851 -0.1003 0.6698 0.055 Uiso 1 1 calc R . . C20 C 0.1974(3) 0.0081(3) 0.6493(3) 0.0475(8) Uani 1 1 d . . . H20A H 0.1599 -0.0509 0.6658 0.057 Uiso 1 1 calc R . . C21 C 0.1187(3) 0.1232(2) 0.6232(2) 0.0399(7) Uani 1 1 d . . . H21A H 0.0269 0.1435 0.6220 0.048 Uiso 1 1 calc R . . C22 C 0.1738(2) 0.2090(2) 0.5989(2) 0.0310(6) Uani 1 1 d . . . H22A H 0.1189 0.2879 0.5816 0.037 Uiso 1 1 calc R . . C23 C 0.1905(2) 0.63389(19) 0.36351(19) 0.0239(5) Uani 1 1 d . . . C24 C 0.1581(3) 0.7082(2) 0.2558(2) 0.0412(7) Uani 1 1 d . . . H24A H 0.1904 0.7724 0.2184 0.049 Uiso 1 1 calc R . . C25 C 0.0787(3) 0.6896(3) 0.2020(3) 0.0512(8) Uani 1 1 d . . . H25A H 0.0574 0.7409 0.1280 0.061 Uiso 1 1 calc R . . C26 C 0.0310(3) 0.5978(2) 0.2548(2) 0.0400(7) Uani 1 1 d . . . H26A H -0.0247 0.5865 0.2180 0.048 Uiso 1 1 calc R . . C27 C 0.0639(2) 0.5222(2) 0.3610(2) 0.0343(6) Uani 1 1 d . . . H27A H 0.0321 0.4577 0.3974 0.041 Uiso 1 1 calc R . . C28 C 0.1436(2) 0.5397(2) 0.4156(2) 0.0294(5) Uani 1 1 d . . . H28A H 0.1662 0.4868 0.4891 0.035 Uiso 1 1 calc R . . C29 C 0.2876(2) 0.80436(19) 0.3668(2) 0.0256(5) Uani 1 1 d . . . C30 C 0.3463(2) 0.8401(2) 0.2659(2) 0.0324(6) Uani 1 1 d . . . H30A H 0.3915 0.7841 0.2382 0.039 Uiso 1 1 calc R . . C31 C 0.3391(3) 0.9572(2) 0.2058(2) 0.0422(7) Uani 1 1 d . . . H31A H 0.3794 0.9809 0.1372 0.051 Uiso 1 1 calc R . . C32 C 0.2737(3) 1.0390(2) 0.2452(3) 0.0486(8) Uani 1 1 d . . . H32A H 0.2681 1.1191 0.2035 0.058 Uiso 1 1 calc R . . C33 C 0.2167(3) 1.0053(3) 0.3443(3) 0.0502(8) Uani 1 1 d . . . H33A H 0.1721 1.0621 0.3713 0.060 Uiso 1 1 calc R . . C34 C 0.2239(3) 0.8881(2) 0.4060(2) 0.0387(6) Uani 1 1 d . . . H34A H 0.1850 0.8652 0.4752 0.046 Uiso 1 1 calc R . . C35 C 0.1974(2) 0.6540(2) 0.5536(2) 0.0261(5) Uani 1 1 d . . . C36 C 0.1476(2) 0.6580(2) 0.6356(2) 0.0284(5) Uani 1 1 d . . . C37 C 0.0988(2) 0.6646(2) 0.7348(2) 0.0286(5) Uani 1 1 d . . . C38 C 0.1687(3) 0.6946(3) 0.7868(2) 0.0405(7) Uani 1 1 d . . . H38A H 0.2457 0.7117 0.7551 0.049 Uiso 1 1 calc R . . C39 C 0.1268(3) 0.6996(3) 0.8833(3) 0.0517(8) Uani 1 1 d . . . H39A H 0.1745 0.7205 0.9179 0.062 Uiso 1 1 calc R . . C40 C 0.0150(3) 0.6741(3) 0.9303(2) 0.0536(8) Uani 1 1 d . . . H40A H -0.0136 0.6769 0.9974 0.064 Uiso 1 1 calc R . . C41 C -0.0549(3) 0.6447(3) 0.8795(2) 0.0461(7) Uani 1 1 d . . . H41A H -0.1314 0.6270 0.9120 0.055 Uiso 1 1 calc R . . C42 C -0.0146(3) 0.6407(2) 0.7819(2) 0.0360(6) Uani 1 1 d . . . H42A H -0.0641 0.6218 0.7469 0.043 Uiso 1 1 calc R . . C100 C 0.9395(6) 0.0001(6) 1.0520(5) 0.0542(18) Uani 0.50 1 d PD A -1 H100 H 0.9304 -0.0740 1.1128 0.065 Uiso 0.50 1 calc PR A -1 Cl1 Cl 1.0535(2) 0.0385(2) 1.0912(2) 0.0660(6) Uani 0.50 1 d PD A -1 Cl2 Cl 0.78784(16) 0.11020(16) 1.02741(16) 0.0656(5) Uani 0.50 1 d PD A -1 Cl3 Cl 0.9931(4) -0.0273(2) 0.9393(2) 0.0941(9) Uani 0.50 1 d PD A -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 0.01912(13) 0.01939(13) 0.01730(14) -0.01003(11) 0.00116(9) -0.00685(10) P1 0.0205(3) 0.0216(3) 0.0201(3) -0.0103(2) 0.0007(2) -0.0065(2) N1 0.0198(9) 0.0204(9) 0.0202(10) -0.0103(8) 0.0020(7) -0.0072(7) N2 0.0205(9) 0.0203(9) 0.0200(10) -0.0114(8) 0.0002(7) -0.0061(7) C1 0.0211(11) 0.0280(12) 0.0233(12) -0.0137(10) 0.0037(9) -0.0085(9) C2 0.0256(12) 0.0353(13) 0.0223(13) -0.0136(11) 0.0061(9) -0.0136(10) C3 0.0238(11) 0.0306(12) 0.0248(13) -0.0110(10) 0.0031(9) -0.0121(10) C4 0.0185(10) 0.0217(11) 0.0229(12) -0.0100(9) 0.0007(9) -0.0058(9) C5 0.0180(10) 0.0196(11) 0.0268(12) -0.0107(10) -0.0018(9) -0.0049(8) C6 0.0198(10) 0.0212(11) 0.0231(12) -0.0124(9) -0.0015(9) -0.0049(9) C7 0.0265(12) 0.0252(12) 0.0268(13) -0.0147(10) -0.0019(10) -0.0077(9) C8 0.0284(12) 0.0253(11) 0.0239(12) -0.0153(10) -0.0024(9) -0.0068(9) C9 0.0247(11) 0.0226(11) 0.0225(12) -0.0133(10) -0.0003(9) -0.0071(9) C10 0.0267(11) 0.0261(12) 0.0189(12) -0.0125(10) 0.0010(9) -0.0078(9) C11 0.0503(16) 0.0459(16) 0.0291(15) -0.0130(13) 0.0087(12) -0.0339(14) C12 0.0437(15) 0.0402(15) 0.0392(16) -0.0253(13) 0.0029(12) -0.0217(12) C13 0.0580(18) 0.0552(18) 0.0291(15) -0.0241(14) 0.0203(13) -0.0377(15) C14 0.095(3) 0.068(2) 0.0239(16) -0.0126(15) -0.0023(16) -0.047(2) C15 0.0453(15) 0.0350(14) 0.0273(14) -0.0192(12) 0.0003(11) -0.0168(12) C16 0.0535(18) 0.0575(19) 0.0298(16) -0.0187(14) -0.0091(13) -0.0184(15) C17 0.0277(12) 0.0248(12) 0.0263(13) -0.0123(10) -0.0011(10) -0.0112(10) C18 0.0268(12) 0.0289(13) 0.0460(17) -0.0153(12) -0.0021(11) -0.0086(10) C19 0.0436(16) 0.0230(13) 0.069(2) -0.0172(14) -0.0031(15) -0.0115(12) C20 0.0492(17) 0.0387(16) 0.065(2) -0.0210(15) 0.0041(15) -0.0290(14) C21 0.0277(13) 0.0406(15) 0.0564(19) -0.0208(14) 0.0031(12) -0.0180(12) C22 0.0240(12) 0.0271(12) 0.0421(16) -0.0161(12) 0.0001(11) -0.0073(10) C23 0.0227(11) 0.0225(11) 0.0249(12) -0.0109(10) -0.0020(9) -0.0041(9) C24 0.0597(18) 0.0319(14) 0.0340(16) -0.0066(12) -0.0134(13) -0.0219(13) C25 0.078(2) 0.0380(16) 0.0370(17) -0.0047(13) -0.0283(16) -0.0220(15) C26 0.0440(15) 0.0362(15) 0.0481(18) -0.0219(14) -0.0161(13) -0.0108(12) C27 0.0309(13) 0.0350(14) 0.0448(17) -0.0226(13) 0.0013(12) -0.0128(11) C28 0.0270(12) 0.0306(13) 0.0301(14) -0.0128(11) 0.0020(10) -0.0102(10) C29 0.0216(11) 0.0215(11) 0.0331(14) -0.0098(10) -0.0054(10) -0.0069(9) C30 0.0250(12) 0.0296(13) 0.0358(15) -0.0081(11) -0.0025(11) -0.0085(10) C31 0.0350(14) 0.0366(15) 0.0412(17) -0.0017(13) -0.0023(12) -0.0160(12) C32 0.0494(17) 0.0274(14) 0.062(2) -0.0069(14) -0.0125(15) -0.0158(13) C33 0.0564(19) 0.0319(15) 0.070(2) -0.0275(16) -0.0029(17) -0.0143(14) C34 0.0436(15) 0.0307(14) 0.0461(17) -0.0205(13) 0.0012(13) -0.0124(12) C35 0.0231(11) 0.0267(12) 0.0293(13) -0.0144(11) 0.0004(10) -0.0063(9) C36 0.0258(12) 0.0281(12) 0.0316(14) -0.0145(11) 0.0016(10) -0.0079(10) C37 0.0298(12) 0.0248(12) 0.0263(13) -0.0124(10) 0.0017(10) -0.0027(10) C38 0.0331(14) 0.0487(17) 0.0453(17) -0.0291(15) 0.0025(12) -0.0089(12) C39 0.0470(18) 0.068(2) 0.050(2) -0.0400(18) -0.0075(15) -0.0080(15) C40 0.060(2) 0.068(2) 0.0316(16) -0.0301(16) 0.0048(14) -0.0097(17) C41 0.0472(17) 0.0496(17) 0.0401(17) -0.0224(15) 0.0174(14) -0.0178(14) C42 0.0369(14) 0.0372(14) 0.0397(16) -0.0223(13) 0.0091(12) -0.0147(12) C100 0.063(4) 0.055(4) 0.046(4) -0.011(3) -0.009(3) -0.031(4) Cl1 0.0527(10) 0.0565(11) 0.0842(18) -0.0167(12) -0.0171(10) -0.0241(9) Cl2 0.0506(9) 0.0621(10) 0.0713(12) -0.0109(9) -0.0087(8) -0.0250(8) Cl3 0.142(3) 0.0542(14) 0.0684(16) -0.0230(12) -0.0269(19) -0.0074(18) _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 2.0638(17) 2_666 ? Ru1 N2 2.0638(17) . ? Ru1 N1 2.0644(18) 2_666 ? Ru1 N1 2.0644(17) . ? Ru1 P1 2.3610(5) . ? Ru1 P1 2.3610(5) 2_666 ? P1 C35 1.765(2) . ? P1 C29 1.836(2) . ? P1 C23 1.839(2) . ? N1 C1 1.371(3) . ? N1 C4 1.388(3) . ? N2 C9 1.366(3) . ? N2 C6 1.387(3) . ? C1 C10 1.385(3) 2_666 ? C1 C2 1.442(3) . ? C2 C3 1.360(3) . ? C2 C13 1.507(3) . ? C3 C4 1.469(3) . ? C3 C11 1.510(3) . ? C4 C5 1.409(3) . ? C5 C6 1.403(3) . ? C5 C17 1.501(3) . ? C6 C7 1.470(3) . ? C7 C8 1.354(3) . ? C7 C12 1.508(3) . ? C8 C9 1.450(3) . ? C8 C15 1.507(3) . ? C9 C10 1.387(3) . ? C10 C1 1.385(3) 2_666 ? C10 H10A 0.9500 . ? 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 C14 1.524(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.523(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.389(3) . ? C17 C18 1.391(3) . ? C18 C19 1.387(3) . ? C18 H18A 0.9500 . ? C19 C20 1.381(4) . ? C19 H19A 0.9500 . ? C20 C21 1.380(4) . ? C20 H20A 0.9500 . ? C21 C22 1.384(3) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.385(3) . ? C23 C28 1.390(3) . ? C24 C25 1.391(4) . ? C24 H24A 0.9500 . ? C25 C26 1.369(4) . ? C25 H25A 0.9500 . ? C26 C27 1.372(4) . ? C26 H26A 0.9500 . ? C27 C28 1.390(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C34 1.391(3) . ? C29 C30 1.395(3) . ? C30 C31 1.388(4) . ? C30 H30A 0.9500 . ? C31 C32 1.375(4) . ? C31 H31A 0.9500 . ? C32 C33 1.366(5) . ? C32 H32A 0.9500 . ? C33 C34 1.392(4) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.201(3) . ? C36 C37 1.431(3) . ? C37 C42 1.394(3) . ? C37 C38 1.398(4) . ? C38 C39 1.373(4) . ? C38 H38A 0.9500 . ? C39 C40 1.385(4) . ? C39 H39A 0.9500 . ? C40 C41 1.380(4) . ? C40 H40A 0.9500 . ? C41 C42 1.380(4) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C100 Cl3 1.739(6) . ? C100 Cl2 1.742(6) . ? C100 Cl1 1.762(6) . ? C100 H100 1.0000 . ? 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 N2 179.999(2) 2_666 . ? N2 Ru1 N1 86.71(7) 2_666 2_666 ? N2 Ru1 N1 93.29(7) . 2_666 ? N2 Ru1 N1 93.29(7) 2_666 . ? N2 Ru1 N1 86.71(7) . . ? N1 Ru1 N1 179.999(2) 2_666 . ? N2 Ru1 P1 88.11(5) 2_666 . ? N2 Ru1 P1 91.89(5) . . ? N1 Ru1 P1 89.40(5) 2_666 . ? N1 Ru1 P1 90.60(5) . . ? N2 Ru1 P1 91.89(5) 2_666 2_666 ? N2 Ru1 P1 88.11(5) . 2_666 ? N1 Ru1 P1 90.60(5) 2_666 2_666 ? N1 Ru1 P1 89.40(5) . 2_666 ? P1 Ru1 P1 180.0 . 2_666 ? C35 P1 C29 100.90(11) . . ? C35 P1 C23 101.73(11) . . ? C29 P1 C23 103.78(11) . . ? C35 P1 Ru1 110.57(8) . . ? C29 P1 Ru1 119.65(7) . . ? C23 P1 Ru1 117.58(7) . . ? C1 N1 C4 106.99(18) . . ? C1 N1 Ru1 123.02(14) . . ? C4 N1 Ru1 129.82(14) . . ? C9 N2 C6 107.34(17) . . ? C9 N2 Ru1 122.83(14) . . ? C6 N2 Ru1 129.70(14) . . ? N1 C1 C10 125.3(2) . 2_666 ? N1 C1 C2 110.01(19) . . ? C10 C1 C2 124.6(2) 2_666 . ? C3 C2 C1 107.6(2) . . ? C3 C2 C13 128.1(2) . . ? C1 C2 C13 124.1(2) . . ? C2 C3 C4 106.7(2) . . ? C2 C3 C11 123.6(2) . . ? C4 C3 C11 129.5(2) . . ? N1 C4 C5 123.7(2) . . ? N1 C4 C3 108.68(19) . . ? C5 C4 C3 127.6(2) . . ? C6 C5 C4 125.8(2) . . ? C6 C5 C17 117.1(2) . . ? C4 C5 C17 117.0(2) . . ? N2 C6 C5 124.07(19) . . ? N2 C6 C7 108.43(19) . . ? C5 C6 C7 127.5(2) . . ? C8 C7 C6 106.98(19) . . ? C8 C7 C12 123.4(2) . . ? C6 C7 C12 129.5(2) . . ? C7 C8 C9 107.4(2) . . ? C7 C8 C15 128.3(2) . . ? C9 C8 C15 124.1(2) . . ? N2 C9 C10 125.7(2) . . ? N2 C9 C8 109.80(19) . . ? C10 C9 C8 124.5(2) . . ? C1 C10 C9 129.7(2) 2_666 . ? C1 C10 H10A 115.2 2_666 . ? C9 C10 H10A 115.2 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 C13 C14 112.4(2) . . ? C2 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C2 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C15 C16 112.7(2) . . ? C8 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C8 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 118.2(2) . . ? C22 C17 C5 120.7(2) . . ? C18 C17 C5 121.0(2) . . ? C19 C18 C17 120.7(2) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 119.8(2) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 119.9(2) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C21 C22 C17 121.2(2) . . ? C21 C22 H22A 119.4 . . ? C17 C22 H22A 119.4 . . ? C24 C23 C28 118.5(2) . . ? C24 C23 P1 124.00(19) . . ? C28 C23 P1 117.49(18) . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C23 C28 C27 120.5(2) . . ? C23 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C34 C29 C30 118.5(2) . . ? C34 C29 P1 122.7(2) . . ? C30 C29 P1 118.86(18) . . ? C31 C30 C29 120.4(2) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 120.3(3) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C29 C34 C33 120.4(3) . . ? C29 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C36 C35 P1 169.2(2) . . ? C35 C36 C37 174.6(3) . . ? C42 C37 C38 119.0(2) . . ? C42 C37 C36 122.4(2) . . ? C38 C37 C36 118.6(2) . . ? C39 C38 C37 120.5(3) . . ? C39 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C38 C39 C40 120.1(3) . . ? C38 C39 H39A 119.9 . . ? C40 C39 H39A 119.9 . . ? C41 C40 C39 119.8(3) . . ? C41 C40 H40A 120.1 . . ? C39 C40 H40A 120.1 . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41A 119.7 . . ? C40 C41 H41A 119.7 . . ? C41 C42 C37 119.9(3) . . ? C41 C42 H42A 120.0 . . ? C37 C42 H42A 120.0 . . ? Cl3 C100 Cl2 110.9(4) . . ? Cl3 C100 Cl1 110.7(4) . . ? Cl2 C100 Cl1 110.6(4) . . ? Cl3 C100 H100 108.1 . . ? Cl2 C100 H100 108.1 . . ? Cl1 C100 H100 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 P1 C35 -61.99(10) 2_666 . . . ? N2 Ru1 P1 C35 118.01(10) . . . . ? N1 Ru1 P1 C35 -148.72(10) 2_666 . . . ? N1 Ru1 P1 C35 31.28(10) . . . . ? N2 Ru1 P1 C29 54.50(11) 2_666 . . . ? N2 Ru1 P1 C29 -125.50(11) . . . . ? N1 Ru1 P1 C29 -32.23(10) 2_666 . . . ? N1 Ru1 P1 C29 147.77(10) . . . . ? N2 Ru1 P1 C23 -178.16(10) 2_666 . . . ? N2 Ru1 P1 C23 1.84(10) . . . . ? N1 Ru1 P1 C23 95.11(10) 2_666 . . . ? N1 Ru1 P1 C23 -84.89(10) . . . . ? N2 Ru1 N1 C1 -2.77(17) 2_666 . . . ? N2 Ru1 N1 C1 177.23(17) . . . . ? P1 Ru1 N1 C1 -90.92(16) . . . . ? P1 Ru1 N1 C1 89.08(16) 2_666 . . . ? N2 Ru1 N1 C4 -177.44(18) 2_666 . . . ? N2 Ru1 N1 C4 2.56(18) . . . . ? P1 Ru1 N1 C4 94.42(17) . . . . ? P1 Ru1 N1 C4 -85.58(17) 2_666 . . . ? N1 Ru1 N2 C9 -3.94(17) 2_666 . . . ? N1 Ru1 N2 C9 176.06(17) . . . . ? P1 Ru1 N2 C9 85.57(16) . . . . ? P1 Ru1 N2 C9 -94.43(16) 2_666 . . . ? N1 Ru1 N2 C6 -179.20(18) 2_666 . . . ? N1 Ru1 N2 C6 0.80(18) . . . . ? P1 Ru1 N2 C6 -89.69(17) . . . . ? P1 Ru1 N2 C6 90.31(17) 2_666 . . . ? C4 N1 C1 C10 176.9(2) . . . 2_666 ? Ru1 N1 C1 C10 1.2(3) . . . 2_666 ? C4 N1 C1 C2 -0.3(2) . . . . ? Ru1 N1 C1 C2 -176.04(14) . . . . ? N1 C1 C2 C3 1.3(3) . . . . ? C10 C1 C2 C3 -175.9(2) 2_666 . . . ? N1 C1 C2 C13 176.6(2) . . . . ? C10 C1 C2 C13 -0.7(4) 2_666 . . . ? C1 C2 C3 C4 -1.7(3) . . . . ? C13 C2 C3 C4 -176.7(2) . . . . ? C1 C2 C3 C11 174.1(2) . . . . ? C13 C2 C3 C11 -0.9(4) . . . . ? C1 N1 C4 C5 -179.0(2) . . . . ? Ru1 N1 C4 C5 -3.7(3) . . . . ? C1 N1 C4 C3 -0.7(2) . . . . ? Ru1 N1 C4 C3 174.58(14) . . . . ? C2 C3 C4 N1 1.6(2) . . . . ? C11 C3 C4 N1 -173.9(2) . . . . ? C2 C3 C4 C5 179.8(2) . . . . ? C11 C3 C4 C5 4.3(4) . . . . ? N1 C4 C5 C6 0.9(3) . . . . ? C3 C4 C5 C6 -177.1(2) . . . . ? N1 C4 C5 C17 -177.19(19) . . . . ? C3 C4 C5 C17 4.8(3) . . . . ? C9 N2 C6 C5 -179.1(2) . . . . ? Ru1 N2 C6 C5 -3.2(3) . . . . ? C9 N2 C6 C7 -0.8(2) . . . . ? Ru1 N2 C6 C7 175.02(14) . . . . ? C4 C5 C6 N2 2.7(3) . . . . ? C17 C5 C6 N2 -179.28(19) . . . . ? C4 C5 C6 C7 -175.3(2) . . . . ? C17 C5 C6 C7 2.8(3) . . . . ? N2 C6 C7 C8 1.2(2) . . . . ? C5 C6 C7 C8 179.3(2) . . . . ? N2 C6 C7 C12 -175.2(2) . . . . ? C5 C6 C7 C12 3.0(4) . . . . ? C6 C7 C8 C9 -1.0(2) . . . . ? C12 C7 C8 C9 175.7(2) . . . . ? C6 C7 C8 C15 -176.9(2) . . . . ? C12 C7 C8 C15 -0.3(4) . . . . ? C6 N2 C9 C10 179.9(2) . . . . ? Ru1 N2 C9 C10 3.7(3) . . . . ? C6 N2 C9 C8 0.2(2) . . . . ? Ru1 N2 C9 C8 -175.99(13) . . . . ? C7 C8 C9 N2 0.5(3) . . . . ? C15 C8 C9 N2 176.7(2) . . . . ? C7 C8 C9 C10 -179.2(2) . . . . ? C15 C8 C9 C10 -3.1(4) . . . . ? N2 C9 C10 C1 -1.0(4) . . . 2_666 ? C8 C9 C10 C1 178.7(2) . . . 2_666 ? C3 C2 C13 C14 93.2(3) . . . . ? C1 C2 C13 C14 -81.0(3) . . . . ? C7 C8 C15 C16 94.6(3) . . . . ? C9 C8 C15 C16 -80.7(3) . . . . ? C6 C5 C17 C22 -97.7(3) . . . . ? C4 C5 C17 C22 80.5(3) . . . . ? C6 C5 C17 C18 81.6(3) . . . . ? C4 C5 C17 C18 -100.2(3) . . . . ? C22 C17 C18 C19 0.8(4) . . . . ? C5 C17 C18 C19 -178.6(3) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 -0.4(5) . . . . ? C19 C20 C21 C22 0.2(5) . . . . ? C20 C21 C22 C17 0.5(4) . . . . ? C18 C17 C22 C21 -1.0(4) . . . . ? C5 C17 C22 C21 178.4(2) . . . . ? C35 P1 C23 C24 126.1(2) . . . . ? C29 P1 C23 C24 21.6(2) . . . . ? Ru1 P1 C23 C24 -113.0(2) . . . . ? C35 P1 C23 C28 -55.67(19) . . . . ? C29 P1 C23 C28 -160.13(17) . . . . ? Ru1 P1 C23 C28 65.22(19) . . . . ? C28 C23 C24 C25 1.1(4) . . . . ? P1 C23 C24 C25 179.3(2) . . . . ? C23 C24 C25 C26 0.2(5) . . . . ? C24 C25 C26 C27 -1.3(5) . . . . ? C25 C26 C27 C28 1.1(4) . . . . ? C24 C23 C28 C27 -1.3(3) . . . . ? P1 C23 C28 C27 -179.60(18) . . . . ? C26 C27 C28 C23 0.2(4) . . . . ? C35 P1 C29 C34 4.6(2) . . . . ? C23 P1 C29 C34 109.6(2) . . . . ? Ru1 P1 C29 C34 -116.9(2) . . . . ? C35 P1 C29 C30 -174.86(19) . . . . ? C23 P1 C29 C30 -69.8(2) . . . . ? Ru1 P1 C29 C30 63.7(2) . . . . ? C34 C29 C30 C31 -1.0(4) . . . . ? P1 C29 C30 C31 178.43(19) . . . . ? C29 C30 C31 C32 -0.1(4) . . . . ? C30 C31 C32 C33 0.7(4) . . . . ? C31 C32 C33 C34 -0.3(5) . . . . ? C30 C29 C34 C33 1.4(4) . . . . ? P1 C29 C34 C33 -178.0(2) . . . . ? C32 C33 C34 C29 -0.8(5) . . . . ? C29 P1 C35 C36 -75.7(12) . . . . ? C23 P1 C35 C36 177.6(12) . . . . ? Ru1 P1 C35 C36 51.9(12) . . . . ? C42 C37 C38 C39 0.5(4) . . . . ? C36 C37 C38 C39 -178.6(3) . . . . ? C37 C38 C39 C40 0.4(5) . . . . ? C38 C39 C40 C41 -0.5(5) . . . . ? C39 C40 C41 C42 -0.2(5) . . . . ? C40 C41 C42 C37 1.1(4) . . . . ? C38 C37 C42 C41 -1.3(4) . . . . ? C36 C37 C42 C41 177.9(2) . . . . ? #============================================================================= data_P2-Ru4 _database_code_depnum_ccdc_archive 'CCDC 834657' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H58 N4 P2 Ru' _chemical_formula_sum 'C84 H58 N4 P2 Ru' _chemical_formula_weight 1286.35 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' 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 23.5610(2) _cell_length_b 13.1750(1) _cell_length_c 61.8138(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.249(1) _cell_angle_gamma 90.00 _cell_volume 18938.5(3) _cell_formula_units_Z 12 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 72794 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7968 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; One and a half independent molecules in the asymmetric unit - One molecule on general position and one on centre of symmetry. Overall Z = 12. ; _diffrn_ambient_temperature 180(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 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 37279 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -73 _diffrn_reflns_limit_l_max 73 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 25.02 _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.857 _reflns_number_total 14306 _reflns_number_gt 10783 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _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^)+(0.0580P)^2^+20.8783P] 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 14306 _refine_ls_number_parameters 1217 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.447 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.117 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 0.037243(11) 0.19374(2) 0.161805(5) 0.02583(10) Uani 1 1 d . . . P1 P -0.01508(4) 0.26495(7) 0.187573(17) 0.0272(2) Uani 1 1 d . . . P2 P 0.09367(4) 0.12227(7) 0.137016(17) 0.0306(2) Uani 1 1 d . . . N1 N 0.08677(10) 0.1184(2) 0.18710(5) 0.0268(7) Uani 1 1 d . . . N2 N 0.09159(11) 0.3158(2) 0.16677(5) 0.0277(7) Uani 1 1 d . . . N3 N -0.01365(11) 0.2711(2) 0.13696(5) 0.0270(7) Uani 1 1 d . . . N4 N -0.01689(11) 0.0703(2) 0.15668(5) 0.0286(7) Uani 1 1 d . . . C1 C 0.07596(13) 0.0234(3) 0.19499(6) 0.0265(8) Uani 1 1 d . . . C2 C 0.12057(14) 0.0002(3) 0.21305(6) 0.0314(9) Uani 1 1 d . . . H2A H 0.1229 -0.0594 0.2218 0.038 Uiso 1 1 calc R . . C3 C 0.15829(14) 0.0772(3) 0.21545(6) 0.0309(9) Uani 1 1 d . . . H3A H 0.1923 0.0813 0.2260 0.037 Uiso 1 1 calc R . . C4 C 0.13795(13) 0.1525(3) 0.19911(6) 0.0273(9) Uani 1 1 d . . . C5 C 0.16576(13) 0.2430(3) 0.19532(6) 0.0277(9) Uani 1 1 d . . . C6 C 0.14383(14) 0.3189(3) 0.18054(6) 0.0301(9) Uani 1 1 d . . . C7 C 0.16981(15) 0.4162(3) 0.17797(7) 0.0341(9) Uani 1 1 d . . . H7A H 0.2064 0.4380 0.1852 0.041 Uiso 1 1 calc R . . C8 C 0.13334(15) 0.4707(3) 0.16357(7) 0.0366(10) Uani 1 1 d . . . H8A H 0.1389 0.5385 0.1591 0.044 Uiso 1 1 calc R . . C9 C 0.08430(14) 0.4076(3) 0.15607(6) 0.0301(9) Uani 1 1 d . . . C10 C 0.03899(14) 0.4335(3) 0.13950(6) 0.0285(9) Uani 1 1 d . . . C11 C -0.00590(14) 0.3692(3) 0.13051(6) 0.0292(9) Uani 1 1 d . . . C12 C -0.05304(14) 0.3956(3) 0.11338(6) 0.0338(9) Uani 1 1 d . . . H12A H -0.0582 0.4588 0.1059 0.041 Uiso 1 1 calc R . . C13 C -0.08804(15) 0.3152(3) 0.10994(6) 0.0349(10) Uani 1 1 d . . . H13A H -0.1224 0.3109 0.0995 0.042 Uiso 1 1 calc R . . C14 C -0.06428(14) 0.2361(3) 0.12486(6) 0.0306(9) Uani 1 1 d . . . C15 C -0.08904(14) 0.1409(3) 0.12708(6) 0.0297(9) Uani 1 1 d . . . C16 C -0.06642(14) 0.0635(3) 0.14120(6) 0.0314(9) Uani 1 1 d . . . C17 C -0.09143(15) -0.0348(3) 0.14307(7) 0.0393(10) Uani 1 1 d . . . H17A H -0.1258 -0.0595 0.1345 0.047 Uiso 1 1 calc R . . C18 C -0.05772(15) -0.0859(3) 0.15909(7) 0.0371(10) Uani 1 1 d . . . H18A H -0.0635 -0.1535 0.1636 0.044 Uiso 1 1 calc R . . C19 C -0.01129(14) -0.0196(3) 0.16810(6) 0.0294(9) Uani 1 1 d . . . C20 C 0.03107(14) -0.0413(3) 0.18610(6) 0.0301(9) Uani 1 1 d . . . C21 C 0.22484(14) 0.2614(3) 0.20833(7) 0.0330(10) Uani 1 1 d . . . C22 C 0.23339(15) 0.2754(3) 0.23068(7) 0.0386(10) Uani 1 1 d . . . H22A H 0.2016 0.2718 0.2383 0.046 Uiso 1 1 calc R . . C23 C 0.28843(17) 0.2948(3) 0.24226(8) 0.0477(12) Uani 1 1 d . . . H23A H 0.2939 0.3042 0.2577 0.057 Uiso 1 1 calc R . . C24 C 0.33478(17) 0.3001(3) 0.23110(9) 0.0542(13) Uani 1 1 d . . . H24A H 0.3722 0.3137 0.2388 0.065 Uiso 1 1 calc R . . C25 C 0.32664(16) 0.2857(3) 0.20886(9) 0.0520(13) Uani 1 1 d . . . H25A H 0.3586 0.2886 0.2013 0.062 Uiso 1 1 calc R . . C26 C 0.27215(15) 0.2668(3) 0.19732(7) 0.0407(10) Uani 1 1 d . . . H26A H 0.2670 0.2576 0.1819 0.049 Uiso 1 1 calc R . . C27 C 0.04380(14) 0.5369(3) 0.12969(7) 0.0327(9) Uani 1 1 d . . . C28 C 0.03456(17) 0.6243(3) 0.14123(8) 0.0450(11) Uani 1 1 d . . . H28A H 0.0203 0.6189 0.1547 0.054 Uiso 1 1 calc R . . C29 C 0.04587(19) 0.7188(3) 0.13325(8) 0.0546(13) Uani 1 1 d . . . H29A H 0.0389 0.7781 0.1412 0.066 Uiso 1 1 calc R . . C30 C 0.06719(17) 0.7273(4) 0.11389(9) 0.0520(13) Uani 1 1 d . . . H30A H 0.0759 0.7923 0.1086 0.062 Uiso 1 1 calc R . . C31 C 0.07578(16) 0.6423(4) 0.10224(8) 0.0476(11) Uani 1 1 d . . . H31A H 0.0903 0.6480 0.0888 0.057 Uiso 1 1 calc R . . C32 C 0.06320(15) 0.5474(3) 0.11003(7) 0.0402(10) Uani 1 1 d . . . H32A H 0.0681 0.4887 0.1016 0.048 Uiso 1 1 calc R . . C33 C -0.14780(14) 0.1231(3) 0.11386(6) 0.0328(9) Uani 1 1 d . . . C34 C -0.15588(17) 0.0748(4) 0.09401(8) 0.0688(16) Uani 1 1 d . . . H34A H -0.1236 0.0504 0.0881 0.083 Uiso 1 1 calc R . . C35 C -0.21089(18) 0.0610(5) 0.08237(9) 0.0811(19) Uani 1 1 d . . . H35A H -0.2156 0.0280 0.0685 0.097 Uiso 1 1 calc R . . C36 C -0.25787(16) 0.0937(3) 0.09040(8) 0.0464(11) Uani 1 1 d . . . H36A H -0.2953 0.0840 0.0823 0.056 Uiso 1 1 calc R . . C37 C -0.25080(17) 0.1398(4) 0.10996(8) 0.0601(14) Uani 1 1 d . . . H37A H -0.2834 0.1635 0.1158 0.072 Uiso 1 1 calc R . . C38 C -0.19566(16) 0.1532(4) 0.12186(8) 0.0610(14) Uani 1 1 d . . . H38A H -0.1915 0.1842 0.1359 0.073 Uiso 1 1 calc R . . C39 C 0.02900(14) -0.1429(3) 0.19687(6) 0.0331(9) Uani 1 1 d . . . C40 C -0.01058(16) -0.1638(3) 0.21044(8) 0.0506(12) Uani 1 1 d . . . H40A H -0.0372 -0.1129 0.2131 0.061 Uiso 1 1 calc R . . C41 C -0.01200(19) -0.2580(4) 0.22031(9) 0.0625(15) Uani 1 1 d . . . H41A H -0.0399 -0.2711 0.2295 0.075 Uiso 1 1 calc R . . C42 C 0.02602(18) -0.3319(3) 0.21707(8) 0.0539(13) Uani 1 1 d . . . H42A H 0.0250 -0.3961 0.2240 0.065 Uiso 1 1 calc R . . C43 C 0.0661(2) -0.3124(3) 0.20368(8) 0.0571(13) Uani 1 1 d . . . H43A H 0.0931 -0.3632 0.2014 0.069 Uiso 1 1 calc R . . C44 C 0.06710(17) -0.2190(3) 0.19353(8) 0.0483(12) Uani 1 1 d . . . H44A H 0.0945 -0.2069 0.1841 0.058 Uiso 1 1 calc R . . C45 C -0.05718(14) 0.1829(3) 0.20308(7) 0.0315(9) Uani 1 1 d . . . C46 C -0.09535(14) 0.1119(3) 0.19233(7) 0.0377(10) Uani 1 1 d . . . H46A H -0.1002 0.1061 0.1768 0.045 Uiso 1 1 calc R . . C47 C -0.12628(16) 0.0497(3) 0.20423(8) 0.0453(11) Uani 1 1 d . . . H47A H -0.1517 0.0006 0.1968 0.054 Uiso 1 1 calc R . . C48 C -0.12089(18) 0.0578(3) 0.22646(8) 0.0529(12) Uani 1 1 d . . . H48A H -0.1429 0.0156 0.2344 0.064 Uiso 1 1 calc R . . C49 C -0.0834(2) 0.1274(4) 0.23716(9) 0.0686(15) Uani 1 1 d . . . H49A H -0.0792 0.1334 0.2527 0.082 Uiso 1 1 calc R . . C50 C -0.05144(19) 0.1893(3) 0.22549(8) 0.0540(12) Uani 1 1 d . . . H50A H -0.0252 0.2368 0.2331 0.065 Uiso 1 1 calc R . . C51 C -0.06491(14) 0.3677(3) 0.17764(6) 0.0303(9) Uani 1 1 d . . . C52 C -0.04777(16) 0.4684(3) 0.17897(7) 0.0450(11) Uani 1 1 d . . . H52A H -0.0098 0.4850 0.1858 0.054 Uiso 1 1 calc R . . C53 C -0.0853(2) 0.5456(4) 0.17050(8) 0.0599(13) Uani 1 1 d . . . H53A H -0.0732 0.6145 0.1716 0.072 Uiso 1 1 calc R . . C54 C -0.13996(18) 0.5206(4) 0.16050(8) 0.0580(14) Uani 1 1 d . . . H54A H -0.1658 0.5727 0.1546 0.070 Uiso 1 1 calc R . . C55 C -0.15748(17) 0.4216(4) 0.15900(7) 0.0531(13) Uani 1 1 d . . . H55A H -0.1955 0.4053 0.1522 0.064 Uiso 1 1 calc R . . C56 C -0.12034(15) 0.3455(3) 0.16724(7) 0.0410(10) Uani 1 1 d . . . H56A H -0.1327 0.2768 0.1658 0.049 Uiso 1 1 calc R . . C57 C 0.03046(15) 0.3276(3) 0.20882(7) 0.0333(9) Uani 1 1 d . . . C58 C 0.06227(15) 0.3736(3) 0.22242(7) 0.0343(10) Uani 1 1 d . . . C59 C 0.10044(14) 0.4313(3) 0.23842(7) 0.0343(10) Uani 1 1 d . . . C60 C 0.09028(18) 0.4434(4) 0.25955(8) 0.0561(13) Uani 1 1 d . . . H60A H 0.0571 0.4135 0.2638 0.067 Uiso 1 1 calc R . . C61 C 0.12799(19) 0.4988(4) 0.27470(8) 0.0645(14) Uani 1 1 d . . . H61A H 0.1207 0.5067 0.2893 0.077 Uiso 1 1 calc R . . C62 C 0.17594(17) 0.5420(3) 0.26848(8) 0.0530(12) Uani 1 1 d . . . H62A H 0.2020 0.5793 0.2788 0.064 Uiso 1 1 calc R . . C63 C 0.18634(17) 0.5317(3) 0.24751(8) 0.0481(12) Uani 1 1 d . . . H63A H 0.2194 0.5622 0.2433 0.058 Uiso 1 1 calc R . . C64 C 0.14864(15) 0.4767(3) 0.23245(7) 0.0401(10) Uani 1 1 d . . . H64A H 0.1559 0.4701 0.2178 0.048 Uiso 1 1 calc R . . C65 C 0.05385(15) 0.0727(3) 0.11130(7) 0.0333(9) Uani 1 1 d . . . C66 C 0.05016(18) 0.1213(3) 0.09146(8) 0.0499(12) Uani 1 1 d . . . H66A H 0.0701 0.1833 0.0905 0.060 Uiso 1 1 calc R . . C67 C 0.0174(2) 0.0802(4) 0.07286(8) 0.0645(14) Uani 1 1 d . . . H67A H 0.0153 0.1149 0.0593 0.077 Uiso 1 1 calc R . . C68 C -0.01188(18) -0.0090(4) 0.07364(8) 0.0568(13) Uani 1 1 d . . . H68A H -0.0338 -0.0366 0.0607 0.068 Uiso 1 1 calc R . . C69 C -0.00912(17) -0.0579(3) 0.09332(9) 0.0524(12) Uani 1 1 d . . . H69A H -0.0292 -0.1200 0.0941 0.063 Uiso 1 1 calc R . . C70 C 0.02320(16) -0.0167(3) 0.11218(8) 0.0445(11) Uani 1 1 d . . . H70A H 0.0242 -0.0504 0.1258 0.053 Uiso 1 1 calc R . . C71 C 0.15171(14) 0.2000(3) 0.12929(6) 0.0319(9) Uani 1 1 d . . . C72 C 0.13866(16) 0.2954(3) 0.12045(7) 0.0367(10) Uani 1 1 d . . . H72A H 0.0996 0.3165 0.1174 0.044 Uiso 1 1 calc R . . C73 C 0.18121(16) 0.3604(3) 0.11601(7) 0.0436(11) Uani 1 1 d . . . H73A H 0.1714 0.4260 0.1102 0.052 Uiso 1 1 calc R . . C74 C 0.23786(16) 0.3305(4) 0.11997(7) 0.0489(12) Uani 1 1 d . . . H74A H 0.2673 0.3754 0.1170 0.059 Uiso 1 1 calc R . . C75 C 0.25155(17) 0.2353(4) 0.12819(8) 0.0583(14) Uani 1 1 d . . . H75A H 0.2906 0.2139 0.1306 0.070 Uiso 1 1 calc R . . C76 C 0.20909(16) 0.1698(3) 0.13300(7) 0.0486(12) Uani 1 1 d . . . H76A H 0.2192 0.1044 0.1388 0.058 Uiso 1 1 calc R . . C77 C 0.13158(15) 0.0133(3) 0.14781(7) 0.0366(10) Uani 1 1 d . . . C78 C 0.15907(15) -0.0543(3) 0.15687(7) 0.0399(10) Uani 1 1 d . . . C79 C 0.19414(15) -0.1337(3) 0.16850(7) 0.0399(10) Uani 1 1 d . . . C80 C 0.22741(17) -0.1108(4) 0.18850(8) 0.0570(13) Uani 1 1 d . . . H80A H 0.2278 -0.0436 0.1941 0.068 Uiso 1 1 calc R . . C81 C 0.2601(2) -0.1856(5) 0.20037(9) 0.0732(16) Uani 1 1 d . . . H81A H 0.2828 -0.1701 0.2141 0.088 Uiso 1 1 calc R . . C82 C 0.2593(2) -0.2818(5) 0.19210(12) 0.0781(19) Uani 1 1 d . . . H82A H 0.2808 -0.3336 0.2004 0.094 Uiso 1 1 calc R . . C83 C 0.22785(19) -0.3055(4) 0.17190(11) 0.0717(17) Uani 1 1 d . . . H83A H 0.2289 -0.3721 0.1661 0.086 Uiso 1 1 calc R . . C84 C 0.19463(17) -0.2305(3) 0.16008(9) 0.0526(13) Uani 1 1 d . . . H84A H 0.1724 -0.2460 0.1463 0.063 Uiso 1 1 calc R . . Ru1A Ru 0.2500 0.2500 0.0000 0.02666(12) Uani 1 2 d S . . P1A P 0.15500(4) 0.20245(8) -0.015198(17) 0.0304(2) Uani 1 1 d . . . N1A N 0.27976(11) 0.2185(2) -0.02876(5) 0.0279(7) Uani 1 1 d . . . N2A N 0.26863(11) 0.1042(2) 0.01011(5) 0.0268(7) Uani 1 1 d . . . C1A C 0.28248(14) 0.2863(3) -0.04558(6) 0.0307(9) Uani 1 1 d . . . C2A C 0.30422(14) 0.2344(3) -0.06304(7) 0.0352(10) Uani 1 1 d . . . H2AA H 0.3102 0.2632 -0.0766 0.042 Uiso 1 1 calc R A . C3A C 0.31445(14) 0.1378(3) -0.05670(6) 0.0327(9) Uani 1 1 d . A . H3AA H 0.3288 0.0858 -0.0650 0.039 Uiso 1 1 calc R . . C4A C 0.29990(13) 0.1268(3) -0.03509(6) 0.0282(9) Uani 1 1 d . A . C5A C 0.30575(13) 0.0377(3) -0.02229(6) 0.0302(9) Uani 1 1 d . . . C6A C 0.29126(13) 0.0283(3) -0.00136(6) 0.0302(9) Uani 1 1 d . A . C7A C 0.29731(14) -0.0633(3) 0.01199(7) 0.0358(10) Uani 1 1 d . . . H7AA H 0.3119 -0.1268 0.0081 0.043 Uiso 1 1 calc R A . C8A C 0.27837(14) -0.0414(3) 0.03079(7) 0.0357(10) Uani 1 1 d . A . H8AA H 0.2773 -0.0868 0.0427 0.043 Uiso 1 1 calc R . . C9A C 0.25992(14) 0.0627(3) 0.02987(6) 0.0304(9) Uani 1 1 d . A . C10A C 0.23558(14) 0.1128(3) 0.04606(6) 0.0324(9) Uani 1 1 d . . . C11A C 0.33046(15) -0.0550(3) -0.03167(6) 0.0330(9) Uani 1 1 d . A . C12A C 0.38559(15) -0.0535(3) -0.03696(6) 0.0350(10) Uani 1 1 d . . . H12B H 0.4070 0.0079 -0.0353 0.042 Uiso 1 1 calc R A . C13A C 0.41001(17) -0.1395(3) -0.04454(7) 0.0435(11) Uani 1 1 d . A . H13B H 0.4479 -0.1367 -0.0480 0.052 Uiso 1 1 calc R . . C14A C 0.3797(2) -0.2284(4) -0.04710(8) 0.0572(13) Uani 1 1 d . . . H14A H 0.3964 -0.2873 -0.0523 0.069 Uiso 1 1 calc R A . C15A C 0.3247(2) -0.2323(4) -0.04211(9) 0.0634(14) Uani 1 1 d . A . H15A H 0.3034 -0.2938 -0.0440 0.076 Uiso 1 1 calc R . . C16A C 0.30058(18) -0.1457(3) -0.03434(7) 0.0493(12) Uani 1 1 d . . . H16A H 0.2629 -0.1491 -0.0308 0.059 Uiso 1 1 calc R A . C17A C 0.22846(16) 0.0509(3) 0.06582(7) 0.0377(10) Uani 1 1 d . A . C18A C 0.27582(18) 0.0227(3) 0.08105(7) 0.0506(12) Uani 1 1 d . . . H18B H 0.3131 0.0450 0.0792 0.061 Uiso 1 1 calc R A . C19A C 0.2695(2) -0.0370(4) 0.09880(8) 0.0659(15) Uani 1 1 d . A . H19A H 0.3024 -0.0560 0.1090 0.079 Uiso 1 1 calc R . . C20A C 0.2157(3) -0.0692(4) 0.10173(9) 0.0700(16) Uani 1 1 d . . . H20A H 0.2115 -0.1105 0.1140 0.084 Uiso 1 1 calc R A . C21A C 0.1683(2) -0.0422(4) 0.08710(9) 0.0608(14) Uani 1 1 d . A . H21A H 0.1311 -0.0641 0.0892 0.073 Uiso 1 1 calc R . . C22A C 0.17492(17) 0.0179(3) 0.06914(7) 0.0477(11) Uani 1 1 d . . . H22B H 0.1419 0.0365 0.0590 0.057 Uiso 1 1 calc R A . C23A C 0.12914(14) 0.2419(3) -0.04353(6) 0.0323(9) Uani 1 1 d . A . C24A C 0.15607(16) 0.2061(3) -0.06029(7) 0.0443(11) Uani 1 1 d . . . H24B H 0.1876 0.1608 -0.0570 0.053 Uiso 1 1 calc R A . C25A C 0.13784(18) 0.2351(4) -0.08195(8) 0.0534(12) Uani 1 1 d . A . H25B H 0.1563 0.2089 -0.0933 0.064 Uiso 1 1 calc R . . C26A C 0.09277(18) 0.3022(3) -0.08674(8) 0.0518(12) Uani 1 1 d . . . H26B H 0.0798 0.3220 -0.1015 0.062 Uiso 1 1 calc R A . C27A C 0.06679(18) 0.3400(3) -0.07032(8) 0.0520(12) Uani 1 1 d . A . H27A H 0.0362 0.3873 -0.0737 0.062 Uiso 1 1 calc R . . C28A C 0.08419(16) 0.3108(3) -0.04888(7) 0.0431(11) Uani 1 1 d . . . H28B H 0.0654 0.3378 -0.0377 0.052 Uiso 1 1 calc R A . C29A C 0.13459(14) 0.0676(3) -0.01504(6) 0.0390(10) Uiso 0.50 1 d PD A 1 C30A C 0.1407(2) 0.0059(7) -0.03238(17) 0.051(2) Uiso 0.50 1 d PD A 1 H30B H 0.1545 0.0345 -0.0446 0.061 Uiso 0.50 1 calc PR A 1 C31A C 0.1276(3) -0.0952(8) -0.03270(18) 0.053(3) Uiso 0.50 1 d PD A 1 H31B H 0.1339 -0.1371 -0.0446 0.063 Uiso 0.50 1 calc PR A 1 C32A C 0.1042(2) -0.1358(5) -0.01465(9) 0.0890(18) Uiso 0.50 1 d PD A 1 H32B H 0.0903 -0.2036 -0.0150 0.107 Uiso 0.50 1 calc PR A 1 C33A C 0.1019(4) -0.0701(10) 0.0046(2) 0.091(4) Uiso 0.50 1 d PD A 1 H33A H 0.0907 -0.0971 0.0176 0.109 Uiso 0.50 1 calc PR A 1 C34A C 0.1168(3) 0.0349(8) 0.00346(18) 0.069(3) Uiso 0.50 1 d PD A 1 H34B H 0.1143 0.0800 0.0153 0.083 Uiso 0.50 1 calc PR A 1 C29' C 0.13459(14) 0.0676(3) -0.01504(6) 0.0390(10) Uiso 0.50 1 d PD A 2 C30' C 0.1587(3) -0.0067(6) -0.02420(11) 0.0342(19) Uiso 0.50 1 d PD A 2 H30' H 0.1902 0.0099 -0.0314 0.041 Uiso 0.50 1 calc PR A 2 C31' C 0.1421(3) -0.1083(7) -0.02430(13) 0.040(2) Uiso 0.50 1 d PD A 2 H31' H 0.1610 -0.1567 -0.0321 0.048 Uiso 0.50 1 calc PR A 2 C32' C 0.1042(2) -0.1358(5) -0.01465(9) 0.0890(18) Uiso 0.50 1 d PD A 2 H32' H 0.0981 -0.2068 -0.0136 0.107 Uiso 0.50 1 calc PR A 2 C33' C 0.0675(5) -0.0697(9) -0.00461(16) 0.080(3) Uiso 0.50 1 d PD A 2 H33' H 0.0351 -0.0938 0.0012 0.095 Uiso 0.50 1 calc PR A 2 C34' C 0.0837(4) 0.0357(8) -0.00401(14) 0.064(3) Uiso 0.50 1 d PD A 2 H34' H 0.0633 0.0844 0.0031 0.077 Uiso 0.50 1 calc PR A 2 C35A C 0.10358(14) 0.2574(3) -0.00085(7) 0.0333(9) Uani 1 1 d . A . C36A C 0.06987(15) 0.2896(3) 0.00989(7) 0.0332(9) Uani 1 1 d . . . C37A C 0.02916(14) 0.3288(3) 0.02286(7) 0.0309(9) Uani 1 1 d . A . C38A C 0.03461(16) 0.3105(3) 0.04500(7) 0.0418(11) Uani 1 1 d . . . H38B H 0.0659 0.2709 0.0521 0.050 Uiso 1 1 calc R A . C39A C -0.00501(18) 0.3493(4) 0.05695(8) 0.0524(12) Uani 1 1 d . A . H39A H -0.0011 0.3359 0.0722 0.063 Uiso 1 1 calc R . . C40A C -0.05010(18) 0.4072(3) 0.04692(9) 0.0559(13) Uani 1 1 d . . . H40B H -0.0775 0.4333 0.0552 0.067 Uiso 1 1 calc R A . C41A C -0.05545(16) 0.4274(3) 0.02500(9) 0.0515(12) Uani 1 1 d . A . H41B H -0.0862 0.4689 0.0182 0.062 Uiso 1 1 calc R . . C42A C -0.01681(15) 0.3882(3) 0.01269(7) 0.0388(10) Uani 1 1 d . . . H42B H -0.0213 0.4013 -0.0026 0.047 Uiso 1 1 calc R A . 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 0.02552(15) 0.02555(19) 0.0256(2) 0.00156(13) 0.00165(12) 0.00127(12) P1 0.0260(4) 0.0270(6) 0.0274(6) -0.0003(4) 0.0011(4) -0.0004(4) P2 0.0324(5) 0.0281(6) 0.0315(7) 0.0031(5) 0.0056(4) 0.0040(4) N1 0.0234(14) 0.0293(19) 0.027(2) -0.0016(14) 0.0019(13) 0.0009(12) N2 0.0288(15) 0.0257(18) 0.027(2) -0.0002(14) 0.0006(13) 0.0014(12) N3 0.0295(15) 0.0329(19) 0.0174(19) -0.0007(14) -0.0002(13) 0.0028(13) N4 0.0299(15) 0.0287(19) 0.027(2) 0.0011(14) 0.0030(14) -0.0012(13) C1 0.0304(18) 0.023(2) 0.026(2) 0.0013(16) 0.0058(16) 0.0007(15) C2 0.0332(19) 0.032(2) 0.029(3) 0.0061(18) 0.0049(17) 0.0071(17) C3 0.0279(18) 0.037(2) 0.027(3) -0.0007(18) 0.0010(16) 0.0028(16) C4 0.0249(17) 0.033(2) 0.024(2) 0.0015(17) 0.0027(15) 0.0059(15) C5 0.0234(17) 0.029(2) 0.030(3) -0.0009(18) 0.0024(16) -0.0002(15) C6 0.0253(18) 0.036(2) 0.029(3) -0.0023(18) 0.0054(16) -0.0030(16) C7 0.0322(19) 0.033(2) 0.036(3) 0.0003(19) 0.0028(17) -0.0074(17) C8 0.042(2) 0.030(2) 0.037(3) 0.0032(19) 0.0061(19) -0.0041(17) C9 0.0345(19) 0.025(2) 0.031(3) 0.0034(17) 0.0053(17) 0.0019(15) C10 0.0332(19) 0.027(2) 0.026(2) 0.0021(17) 0.0091(17) 0.0022(16) C11 0.0343(19) 0.029(2) 0.025(2) 0.0040(17) 0.0073(16) 0.0053(16) C12 0.039(2) 0.036(2) 0.026(3) 0.0077(18) 0.0021(17) 0.0094(18) C13 0.0313(19) 0.044(3) 0.027(3) 0.0030(19) -0.0013(17) 0.0046(17) C14 0.0285(18) 0.036(2) 0.027(3) -0.0017(18) 0.0009(16) 0.0047(16) C15 0.0314(18) 0.033(2) 0.023(2) -0.0045(18) -0.0008(16) 0.0047(16) C16 0.0302(18) 0.033(2) 0.029(3) -0.0026(18) -0.0013(17) -0.0037(16) C17 0.035(2) 0.040(3) 0.038(3) 0.000(2) -0.0063(18) -0.0054(18) C18 0.039(2) 0.029(2) 0.041(3) 0.0025(19) 0.0018(19) -0.0043(17) C19 0.0322(18) 0.024(2) 0.032(3) 0.0012(17) 0.0044(17) -0.0021(15) C20 0.0320(18) 0.030(2) 0.029(3) 0.0012(17) 0.0077(17) 0.0030(16) C21 0.0302(19) 0.028(2) 0.040(3) 0.0007(18) 0.0027(18) -0.0002(16) C22 0.035(2) 0.033(2) 0.047(3) -0.003(2) 0.0019(19) 0.0053(17) C23 0.049(2) 0.045(3) 0.044(3) -0.011(2) -0.010(2) 0.003(2) C24 0.033(2) 0.047(3) 0.077(4) -0.007(3) -0.009(2) -0.0067(19) C25 0.030(2) 0.050(3) 0.077(4) 0.000(3) 0.009(2) -0.0022(18) C26 0.038(2) 0.037(3) 0.045(3) 0.000(2) 0.003(2) -0.0011(17) C27 0.0345(19) 0.031(2) 0.031(3) 0.0062(19) 0.0016(17) 0.0001(16) C28 0.055(2) 0.034(3) 0.048(3) 0.003(2) 0.017(2) 0.0031(19) C29 0.072(3) 0.027(3) 0.066(4) 0.006(2) 0.015(3) 0.004(2) C30 0.051(3) 0.039(3) 0.066(4) 0.024(3) 0.007(2) -0.004(2) C31 0.051(2) 0.054(3) 0.040(3) 0.016(2) 0.010(2) 0.002(2) C32 0.043(2) 0.042(3) 0.035(3) 0.007(2) 0.0054(19) 0.0026(18) C33 0.0339(19) 0.033(2) 0.029(3) 0.0006(18) -0.0025(17) 0.0010(16) C34 0.036(2) 0.116(5) 0.052(4) -0.041(3) 0.000(2) 0.011(2) C35 0.040(2) 0.143(5) 0.055(4) -0.054(4) -0.008(2) 0.005(3) C36 0.035(2) 0.052(3) 0.048(3) -0.005(2) -0.006(2) -0.0033(19) C37 0.035(2) 0.080(4) 0.064(4) -0.029(3) 0.004(2) 0.003(2) C38 0.038(2) 0.095(4) 0.049(3) -0.038(3) 0.001(2) 0.001(2) C39 0.0336(19) 0.030(2) 0.035(3) 0.0063(18) 0.0006(17) -0.0018(16) C40 0.039(2) 0.046(3) 0.071(4) 0.020(2) 0.022(2) 0.0087(19) C41 0.054(3) 0.056(3) 0.081(4) 0.036(3) 0.023(3) 0.006(2) C42 0.061(3) 0.034(3) 0.066(4) 0.023(2) 0.007(2) 0.004(2) C43 0.075(3) 0.036(3) 0.064(4) 0.012(2) 0.022(3) 0.020(2) C44 0.055(3) 0.037(3) 0.058(3) 0.008(2) 0.023(2) 0.007(2) C45 0.0349(19) 0.030(2) 0.029(3) 0.0038(18) 0.0040(17) 0.0044(16) C46 0.036(2) 0.037(3) 0.040(3) -0.001(2) 0.0075(18) -0.0047(17) C47 0.040(2) 0.033(3) 0.064(4) 0.000(2) 0.011(2) -0.0045(18) C48 0.058(3) 0.049(3) 0.054(4) 0.014(2) 0.019(2) -0.009(2) C49 0.092(4) 0.075(4) 0.040(3) 0.006(3) 0.014(3) -0.029(3) C50 0.070(3) 0.053(3) 0.038(3) 0.008(2) 0.008(2) -0.020(2) C51 0.0322(19) 0.032(2) 0.028(3) 0.0037(18) 0.0105(16) 0.0072(16) C52 0.041(2) 0.042(3) 0.051(3) 0.008(2) 0.007(2) 0.0082(19) C53 0.070(3) 0.041(3) 0.072(4) 0.016(3) 0.021(3) 0.011(2) C54 0.051(3) 0.070(4) 0.054(4) 0.030(3) 0.012(2) 0.026(2) C55 0.041(2) 0.072(4) 0.046(3) 0.018(3) 0.006(2) 0.012(2) C56 0.038(2) 0.048(3) 0.036(3) 0.006(2) 0.0031(19) 0.0051(19) C57 0.0313(19) 0.032(2) 0.037(3) 0.0009(19) 0.0072(18) 0.0013(16) C58 0.0302(19) 0.032(2) 0.040(3) 0.000(2) 0.0030(18) 0.0029(17) C59 0.0301(19) 0.035(2) 0.036(3) -0.0060(19) -0.0004(18) 0.0025(16) C60 0.050(3) 0.073(4) 0.046(3) -0.011(3) 0.008(2) -0.025(2) C61 0.068(3) 0.085(4) 0.040(3) -0.018(3) 0.008(2) -0.024(3) C62 0.046(2) 0.058(3) 0.051(4) -0.014(2) -0.002(2) -0.015(2) C63 0.041(2) 0.047(3) 0.055(4) -0.006(2) 0.006(2) -0.0146(19) C64 0.044(2) 0.040(3) 0.036(3) -0.009(2) 0.0081(19) -0.0040(19) C65 0.039(2) 0.027(2) 0.035(3) -0.0003(19) 0.0077(18) 0.0028(16) C66 0.061(3) 0.046(3) 0.040(3) 0.003(2) -0.002(2) -0.008(2) C67 0.079(3) 0.065(4) 0.045(4) 0.005(3) -0.005(3) -0.015(3) C68 0.059(3) 0.065(4) 0.042(3) -0.007(3) -0.006(2) -0.004(2) C69 0.050(2) 0.038(3) 0.068(4) -0.013(3) 0.006(2) -0.008(2) C70 0.055(2) 0.036(3) 0.043(3) -0.003(2) 0.010(2) 0.000(2) C71 0.036(2) 0.035(2) 0.026(3) -0.0019(18) 0.0073(17) 0.0015(17) C72 0.037(2) 0.037(3) 0.037(3) -0.002(2) 0.0095(18) 0.0032(18) C73 0.050(2) 0.042(3) 0.041(3) 0.000(2) 0.014(2) -0.004(2) C74 0.039(2) 0.063(3) 0.046(3) 0.001(2) 0.011(2) -0.013(2) C75 0.035(2) 0.067(4) 0.073(4) 0.021(3) 0.009(2) 0.005(2) C76 0.038(2) 0.051(3) 0.056(3) 0.012(2) 0.008(2) 0.0041(19) C77 0.038(2) 0.038(3) 0.035(3) 0.002(2) 0.0079(18) 0.0035(18) C78 0.036(2) 0.040(3) 0.045(3) 0.001(2) 0.0106(19) 0.0070(19) C79 0.035(2) 0.043(3) 0.043(3) 0.010(2) 0.011(2) 0.0088(18) C80 0.050(3) 0.068(4) 0.054(4) 0.006(3) 0.010(2) 0.022(2) C81 0.059(3) 0.097(5) 0.065(4) 0.016(3) 0.015(3) 0.031(3) C82 0.050(3) 0.078(4) 0.107(6) 0.048(4) 0.016(3) 0.023(3) C83 0.046(3) 0.039(3) 0.132(6) 0.013(3) 0.020(3) 0.008(2) C84 0.042(2) 0.039(3) 0.079(4) 0.006(3) 0.015(2) 0.005(2) Ru1A 0.0235(2) 0.0340(3) 0.0226(3) 0.00173(19) 0.00414(17) 0.00406(17) P1A 0.0271(5) 0.0353(6) 0.0284(7) 0.0000(5) 0.0037(4) 0.0041(4) N1A 0.0264(15) 0.037(2) 0.020(2) 0.0017(14) 0.0034(13) 0.0018(13) N2A 0.0252(14) 0.0330(19) 0.022(2) 0.0005(14) 0.0049(13) 0.0028(12) C1A 0.0269(18) 0.043(3) 0.022(3) 0.0028(18) 0.0026(16) 0.0062(16) C2A 0.0326(19) 0.051(3) 0.023(3) 0.0032(19) 0.0057(17) 0.0073(18) C3A 0.0332(19) 0.040(3) 0.025(3) -0.0058(19) 0.0055(17) 0.0040(17) C4A 0.0253(17) 0.040(3) 0.020(2) 0.0001(18) 0.0031(15) 0.0027(16) C5A 0.0248(17) 0.037(2) 0.030(3) -0.0025(18) 0.0057(16) -0.0024(15) C6A 0.0271(18) 0.029(2) 0.036(3) -0.0019(18) 0.0073(17) -0.0009(15) C7A 0.039(2) 0.035(3) 0.036(3) 0.0009(19) 0.0140(18) 0.0022(17) C8A 0.039(2) 0.036(3) 0.034(3) 0.0083(19) 0.0095(18) 0.0007(17) C9A 0.0290(18) 0.037(2) 0.024(3) 0.0064(18) 0.0021(16) 0.0053(16) C10A 0.0282(18) 0.043(3) 0.026(3) 0.0050(19) 0.0040(16) 0.0044(16) C11A 0.039(2) 0.035(2) 0.025(3) -0.0035(18) 0.0057(17) -0.0021(17) C12A 0.039(2) 0.038(3) 0.029(3) -0.0018(19) 0.0069(18) -0.0003(17) C13A 0.049(2) 0.052(3) 0.031(3) -0.003(2) 0.0076(19) 0.013(2) C14A 0.085(3) 0.041(3) 0.050(4) -0.006(2) 0.025(3) 0.009(3) C15A 0.091(4) 0.035(3) 0.069(4) -0.011(3) 0.028(3) -0.015(3) C16A 0.058(3) 0.044(3) 0.050(3) -0.009(2) 0.021(2) -0.011(2) C17A 0.045(2) 0.039(3) 0.030(3) 0.0016(19) 0.0126(19) 0.0125(18) C18A 0.054(3) 0.061(3) 0.039(3) 0.014(2) 0.013(2) 0.017(2) C19A 0.090(4) 0.075(4) 0.034(3) 0.021(3) 0.014(3) 0.036(3) C20A 0.117(4) 0.052(3) 0.051(4) 0.025(3) 0.044(3) 0.030(3) C21A 0.083(3) 0.047(3) 0.063(4) 0.010(3) 0.044(3) 0.005(3) C22A 0.050(2) 0.054(3) 0.041(3) 0.010(2) 0.015(2) 0.010(2) C23A 0.0263(18) 0.040(3) 0.029(3) 0.0004(18) -0.0012(16) -0.0042(16) C24A 0.037(2) 0.061(3) 0.033(3) -0.003(2) 0.0012(19) 0.0074(19) C25A 0.049(3) 0.079(4) 0.032(3) -0.004(2) 0.008(2) -0.004(2) C26A 0.053(3) 0.064(3) 0.033(3) 0.011(2) -0.012(2) -0.008(2) C27A 0.052(3) 0.050(3) 0.048(4) 0.013(2) -0.010(2) 0.005(2) C28A 0.040(2) 0.044(3) 0.044(3) 0.003(2) 0.002(2) 0.0080(19) C35A 0.0252(18) 0.037(2) 0.037(3) 0.0001(19) 0.0019(17) -0.0001(16) C36A 0.0299(19) 0.033(2) 0.035(3) 0.0027(18) 0.0002(18) -0.0010(16) C37A 0.0297(19) 0.029(2) 0.035(3) -0.0023(18) 0.0072(17) -0.0052(15) C38A 0.041(2) 0.045(3) 0.040(3) 0.005(2) 0.011(2) 0.0048(18) C39A 0.058(3) 0.067(3) 0.036(3) -0.003(2) 0.019(2) -0.001(2) C40A 0.048(3) 0.057(3) 0.069(4) -0.011(3) 0.028(2) 0.007(2) C41A 0.037(2) 0.049(3) 0.070(4) 0.002(3) 0.013(2) 0.0136(19) C42A 0.035(2) 0.038(3) 0.042(3) 0.003(2) 0.0029(19) -0.0005(17) _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 2.048(3) . ? Ru1 N1 2.051(3) . ? Ru1 N4 2.059(3) . ? Ru1 N3 2.060(3) . ? Ru1 P1 2.3597(10) . ? Ru1 P2 2.3784(10) . ? P1 C57 1.762(4) . ? P1 C51 1.832(4) . ? P1 C45 1.838(4) . ? P2 C77 1.764(4) . ? P2 C65 1.831(4) . ? P2 C71 1.832(4) . ? N1 C1 1.381(4) . ? N1 C4 1.386(4) . ? N2 C9 1.376(4) . ? N2 C6 1.380(4) . ? N3 C11 1.373(4) . ? N3 C14 1.382(4) . ? N4 C19 1.375(4) . ? N4 C16 1.388(4) . ? C1 C20 1.401(5) . ? C1 C2 1.438(5) . ? C2 C3 1.341(5) . ? C2 H2A 0.9500 . ? C3 C4 1.441(5) . ? C3 H3A 0.9500 . ? C4 C5 1.399(5) . ? C5 C6 1.396(5) . ? C5 C21 1.511(5) . ? C6 C7 1.440(5) . ? C7 C8 1.342(5) . ? C7 H7A 0.9500 . ? C8 C9 1.439(5) . ? C8 H8A 0.9500 . ? C9 C10 1.398(5) . ? C10 C11 1.399(5) . ? C10 C27 1.503(5) . ? C11 C12 1.449(5) . ? C12 C13 1.338(5) . ? C12 H12A 0.9500 . ? C13 C14 1.444(5) . ? C13 H13A 0.9500 . ? C14 C15 1.399(5) . ? C15 C16 1.391(5) . ? C15 C33 1.509(5) . ? C16 C17 1.435(5) . ? C17 C18 1.346(5) . ? C17 H17A 0.9500 . ? C18 C19 1.440(5) . ? C18 H18A 0.9500 . ? C19 C20 1.399(5) . ? C20 C39 1.498(5) . ? C21 C22 1.376(5) . ? C21 C26 1.398(5) . ? C22 C23 1.400(5) . ? C22 H22A 0.9500 . ? C23 C24 1.384(6) . ? C23 H23A 0.9500 . ? C24 C25 1.370(6) . ? C24 H24A 0.9500 . ? C25 C26 1.387(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.373(5) . ? C27 C28 1.389(5) . ? C28 C29 1.381(6) . ? C28 H28A 0.9500 . ? C29 C30 1.375(6) . ? C29 H29A 0.9500 . ? C30 C31 1.364(6) . ? C30 H30A 0.9500 . ? C31 C32 1.389(6) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.361(5) . ? C33 C34 1.368(5) . ? C34 C35 1.390(6) . ? C34 H34A 0.9500 . ? C35 C36 1.354(6) . ? C35 H35A 0.9500 . ? C36 C37 1.340(6) . ? C36 H36A 0.9500 . ? C37 C38 1.397(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.379(5) . ? C39 C44 1.383(5) . ? C40 C41 1.387(6) . ? C40 H40A 0.9500 . ? C41 C42 1.359(6) . ? C41 H41A 0.9500 . ? C42 C43 1.376(6) . ? C42 H42A 0.9500 . ? C43 C44 1.383(6) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.373(6) . ? C45 C46 1.390(5) . ? C46 C47 1.384(5) . ? C46 H46A 0.9500 . ? C47 C48 1.364(6) . ? C47 H47A 0.9500 . ? C48 C49 1.368(6) . ? C48 H48A 0.9500 . ? C49 C50 1.388(6) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.385(5) . ? C51 C56 1.391(5) . ? C52 C53 1.393(5) . ? C52 H52A 0.9500 . ? C53 C54 1.377(6) . ? C53 H53A 0.9500 . ? C54 C55 1.367(6) . ? C54 H54A 0.9500 . ? C55 C56 1.373(5) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C58 1.198(5) . ? C58 C59 1.441(5) . ? C59 C60 1.375(6) . ? C59 C64 1.385(5) . ? C60 C61 1.390(6) . ? C60 H60A 0.9500 . ? C61 C62 1.374(6) . ? C61 H61A 0.9500 . ? C62 C63 1.364(6) . ? C62 H62A 0.9500 . ? C63 C64 1.383(5) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 C66 1.373(6) . ? C65 C70 1.388(5) . ? C66 C67 1.387(6) . ? C66 H66A 0.9500 . ? C67 C68 1.369(6) . ? C67 H67A 0.9500 . ? C68 C69 1.369(6) . ? C68 H68A 0.9500 . ? C69 C70 1.396(6) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C71 C72 1.386(5) . ? C71 C76 1.392(5) . ? C72 C73 1.379(5) . ? C72 H72A 0.9500 . ? C73 C74 1.375(5) . ? C73 H73A 0.9500 . ? C74 C75 1.373(6) . ? C74 H74A 0.9500 . ? C75 C76 1.389(6) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 C78 1.188(5) . ? C78 C79 1.450(5) . ? C79 C84 1.378(6) . ? C79 C80 1.387(6) . ? C80 C81 1.386(6) . ? C80 H80A 0.9500 . ? C81 C82 1.366(8) . ? C81 H81A 0.9500 . ? C82 C83 1.381(8) . ? C82 H82A 0.9500 . ? C83 C84 1.392(6) . ? C83 H83A 0.9500 . ? C84 H84A 0.9500 . ? Ru1A N2A 2.046(3) . ? Ru1A N2A 2.046(3) 7 ? Ru1A N1A 2.056(3) 7 ? Ru1A N1A 2.056(3) . ? Ru1A P1A 2.3684(9) 7 ? Ru1A P1A 2.3684(9) . ? P1A C35A 1.767(4) . ? P1A C23A 1.835(4) . ? P1A C29A 1.842(4) . ? N1A C4A 1.377(4) . ? N1A C1A 1.380(5) . ? N2A C6A 1.381(4) . ? N2A C9A 1.383(4) . ? C1A C10A 1.395(5) 7 ? C1A C2A 1.440(5) . ? C2A C3A 1.342(5) . ? C2A H2AA 0.9500 . ? C3A C4A 1.439(5) . ? C3A H3AA 0.9500 . ? C4A C5A 1.411(5) . ? C5A C6A 1.396(5) . ? C5A C11A 1.508(5) . ? C6A C7A 1.457(5) . ? C7A C8A 1.342(5) . ? C7A H7AA 0.9500 . ? C8A C9A 1.438(5) . ? C8A H8AA 0.9500 . ? C9A C10A 1.396(5) . ? C10A C1A 1.395(5) 7 ? C10A C17A 1.500(5) . ? C11A C16A 1.384(5) . ? C11A C12A 1.389(5) . ? C12A C13A 1.386(5) . ? C12A H12B 0.9500 . ? C13A C14A 1.369(6) . ? C13A H13B 0.9500 . ? C14A C15A 1.379(6) . ? C14A H14A 0.9500 . ? C15A C16A 1.394(6) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C17A C22A 1.380(5) . ? C17A C18A 1.390(5) . ? C18A C19A 1.378(6) . ? C18A H18B 0.9500 . ? C19A C20A 1.377(7) . ? C19A H19A 0.9500 . ? C20A C21A 1.367(7) . ? C20A H20A 0.9500 . ? C21A C22A 1.392(6) . ? C21A H21A 0.9500 . ? C22A H22B 0.9500 . ? C23A C24A 1.382(5) . ? C23A C28A 1.394(5) . ? C24A C25A 1.392(6) . ? C24A H24B 0.9500 . ? C25A C26A 1.376(6) . ? C25A H25B 0.9500 . ? C26A C27A 1.362(6) . ? C26A H26B 0.9500 . ? C27A C28A 1.378(6) . ? C27A H27A 0.9500 . ? C28A H28B 0.9500 . ? C29A C34A 1.350(11) . ? C29A C30A 1.371(10) . ? C30A C31A 1.366(13) . ? C30A H30B 0.9500 . ? C31A C32A 1.426(12) . ? C31A H31B 0.9500 . ? C32A C33A 1.481(13) . ? C32A H32B 0.9500 . ? C33A C34A 1.432(15) . ? C33A H33A 0.9500 . ? C34A H34B 0.9500 . ? C30' C31' 1.395(11) . ? C30' H30' 0.9500 . ? C31' H31' 0.9500 . ? C33' C34' 1.440(14) . ? C33' H33' 0.9500 . ? C34' H34' 0.9500 . ? C35A C36A 1.192(5) . ? C36A C37A 1.441(5) . ? C37A C38A 1.375(5) . ? C37A C42A 1.400(5) . ? C38A C39A 1.378(6) . ? C38A H38B 0.9500 . ? C39A C40A 1.372(6) . ? C39A H39A 0.9500 . ? C40A C41A 1.366(6) . ? C40A H40B 0.9500 . ? C41A C42A 1.377(6) . ? C41A H41B 0.9500 . ? C42A H42B 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 N2 Ru1 N1 90.02(11) . . ? N2 Ru1 N4 179.50(12) . . ? N1 Ru1 N4 89.85(11) . . ? N2 Ru1 N3 89.92(11) . . ? N1 Ru1 N3 178.55(11) . . ? N4 Ru1 N3 90.22(11) . . ? N2 Ru1 P1 88.20(8) . . ? N1 Ru1 P1 88.44(8) . . ? N4 Ru1 P1 92.29(8) . . ? N3 Ru1 P1 90.11(8) . . ? N2 Ru1 P2 90.38(8) . . ? N1 Ru1 P2 89.49(8) . . ? N4 Ru1 P2 89.13(8) . . ? N3 Ru1 P2 91.96(8) . . ? P1 Ru1 P2 177.49(3) . . ? C57 P1 C51 100.64(17) . . ? C57 P1 C45 101.64(18) . . ? C51 P1 C45 103.82(16) . . ? C57 P1 Ru1 111.58(12) . . ? C51 P1 Ru1 116.35(12) . . ? C45 P1 Ru1 120.16(13) . . ? C77 P2 C65 101.30(18) . . ? C77 P2 C71 101.50(17) . . ? C65 P2 C71 105.82(18) . . ? C77 P2 Ru1 112.34(14) . . ? C65 P2 Ru1 116.03(12) . . ? C71 P2 Ru1 117.69(13) . . ? C1 N1 C4 107.4(3) . . ? C1 N1 Ru1 126.4(2) . . ? C4 N1 Ru1 126.2(2) . . ? C9 N2 C6 107.5(3) . . ? C9 N2 Ru1 126.3(2) . . ? C6 N2 Ru1 126.2(2) . . ? C11 N3 C14 107.5(3) . . ? C11 N3 Ru1 126.4(2) . . ? C14 N3 Ru1 126.0(2) . . ? C19 N4 C16 107.4(3) . . ? C19 N4 Ru1 126.6(2) . . ? C16 N4 Ru1 126.1(2) . . ? N1 C1 C20 125.7(3) . . ? N1 C1 C2 108.3(3) . . ? C20 C1 C2 125.9(3) . . ? C3 C2 C1 108.3(3) . . ? C3 C2 H2A 125.9 . . ? C1 C2 H2A 125.9 . . ? C2 C3 C4 107.7(3) . . ? C2 C3 H3A 126.2 . . ? C4 C3 H3A 126.2 . . ? N1 C4 C5 125.3(3) . . ? N1 C4 C3 108.3(3) . . ? C5 C4 C3 126.3(3) . . ? C6 C5 C4 125.9(3) . . ? C6 C5 C21 116.5(3) . . ? C4 C5 C21 117.6(3) . . ? N2 C6 C5 125.6(3) . . ? N2 C6 C7 108.1(3) . . ? C5 C6 C7 126.2(3) . . ? C8 C7 C6 108.1(3) . . ? C8 C7 H7A 125.9 . . ? C6 C7 H7A 125.9 . . ? C7 C8 C9 107.5(3) . . ? C7 C8 H8A 126.3 . . ? C9 C8 H8A 126.3 . . ? N2 C9 C10 126.1(3) . . ? N2 C9 C8 108.7(3) . . ? C10 C9 C8 125.1(3) . . ? C9 C10 C11 125.6(3) . . ? C9 C10 C27 114.7(3) . . ? C11 C10 C27 119.4(3) . . ? N3 C11 C10 125.6(3) . . ? N3 C11 C12 108.5(3) . . ? C10 C11 C12 125.9(3) . . ? C13 C12 C11 107.8(3) . . ? C13 C12 H12A 126.1 . . ? C11 C12 H12A 126.1 . . ? C12 C13 C14 107.7(3) . . ? C12 C13 H13A 126.1 . . ? C14 C13 H13A 126.1 . . ? N3 C14 C15 125.7(3) . . ? N3 C14 C13 108.5(3) . . ? C15 C14 C13 125.8(3) . . ? C16 C15 C14 126.5(3) . . ? C16 C15 C33 116.8(3) . . ? C14 C15 C33 116.5(3) . . ? N4 C16 C15 125.4(3) . . ? N4 C16 C17 108.3(3) . . ? C15 C16 C17 126.2(3) . . ? C18 C17 C16 108.0(3) . . ? C18 C17 H17A 126.0 . . ? C16 C17 H17A 126.0 . . ? C17 C18 C19 107.6(3) . . ? C17 C18 H18A 126.2 . . ? C19 C18 H18A 126.2 . . ? N4 C19 C20 125.5(3) . . ? N4 C19 C18 108.7(3) . . ? C20 C19 C18 125.7(3) . . ? C19 C20 C1 125.8(3) . . ? C19 C20 C39 117.7(3) . . ? C1 C20 C39 116.5(3) . . ? C22 C21 C26 118.8(3) . . ? C22 C21 C5 122.0(3) . . ? C26 C21 C5 119.2(4) . . ? C21 C22 C23 120.8(4) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.2(4) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C32 C27 C28 118.2(4) . . ? C32 C27 C10 120.4(4) . . ? C28 C27 C10 121.1(4) . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 119.9(4) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C27 C32 C31 121.2(4) . . ? C27 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C38 C33 C34 117.2(3) . . ? C38 C33 C15 120.0(4) . . ? C34 C33 C15 122.8(3) . . ? C33 C34 C35 120.6(4) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 121.2(4) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C37 C36 C35 119.0(4) . . ? C37 C36 H36A 120.5 . . ? C35 C36 H36A 120.5 . . ? C36 C37 C38 120.2(4) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C33 C38 C37 121.7(4) . . ? C33 C38 H38A 119.1 . . ? C37 C38 H38A 119.1 . . ? C40 C39 C44 117.7(4) . . ? C40 C39 C20 121.5(3) . . ? C44 C39 C20 120.8(3) . . ? C39 C40 C41 120.9(4) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C42 C41 C40 120.9(4) . . ? C42 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C41 C42 C43 119.2(4) . . ? C41 C42 H42A 120.4 . . ? C43 C42 H42A 120.4 . . ? C42 C43 C44 120.2(4) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C39 C44 C43 121.2(4) . . ? C39 C44 H44A 119.4 . . ? C43 C44 H44A 119.4 . . ? C50 C45 C46 118.3(4) . . ? C50 C45 P1 121.1(3) . . ? C46 C45 P1 120.6(3) . . ? C47 C46 C45 120.0(4) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C48 C47 C46 121.2(4) . . ? C48 C47 H47A 119.4 . . ? C46 C47 H47A 119.4 . . ? C47 C48 C49 119.2(4) . . ? C47 C48 H48A 120.4 . . ? C49 C48 H48A 120.4 . . ? C48 C49 C50 120.3(5) . . ? C48 C49 H49A 119.8 . . ? C50 C49 H49A 119.8 . . ? C45 C50 C49 121.0(4) . . ? C45 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C52 C51 C56 118.2(3) . . ? C52 C51 P1 121.5(3) . . ? C56 C51 P1 120.2(3) . . ? C51 C52 C53 121.1(4) . . ? C51 C52 H52A 119.5 . . ? C53 C52 H52A 119.5 . . ? C54 C53 C52 119.0(4) . . ? C54 C53 H53A 120.5 . . ? C52 C53 H53A 120.5 . . ? C55 C54 C53 120.6(4) . . ? C55 C54 H54A 119.7 . . ? C53 C54 H54A 119.7 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55A 119.9 . . ? C56 C55 H55A 119.9 . . ? C55 C56 C51 120.9(4) . . ? C55 C56 H56A 119.6 . . ? C51 C56 H56A 119.6 . . ? C58 C57 P1 176.4(4) . . ? C57 C58 C59 178.5(5) . . ? C60 C59 C64 118.6(4) . . ? C60 C59 C58 121.9(4) . . ? C64 C59 C58 119.6(4) . . ? C59 C60 C61 120.7(4) . . ? C59 C60 H60A 119.6 . . ? C61 C60 H60A 119.6 . . ? C62 C61 C60 119.6(5) . . ? C62 C61 H61A 120.2 . . ? C60 C61 H61A 120.2 . . ? C63 C62 C61 120.4(4) . . ? C63 C62 H62A 119.8 . . ? C61 C62 H62A 119.8 . . ? C62 C63 C64 119.8(4) . . ? C62 C63 H63A 120.1 . . ? C64 C63 H63A 120.1 . . ? C63 C64 C59 120.8(4) . . ? C63 C64 H64A 119.6 . . ? C59 C64 H64A 119.6 . . ? C66 C65 C70 118.1(4) . . ? C66 C65 P2 124.0(3) . . ? C70 C65 P2 117.8(3) . . ? C65 C66 C67 120.4(4) . . ? C65 C66 H66A 119.8 . . ? C67 C66 H66A 119.8 . . ? C68 C67 C66 121.4(5) . . ? C68 C67 H67A 119.3 . . ? C66 C67 H67A 119.3 . . ? C69 C68 C67 119.0(4) . . ? C69 C68 H68A 120.5 . . ? C67 C68 H68A 120.5 . . ? C68 C69 C70 120.0(4) . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C65 C70 C69 121.0(4) . . ? C65 C70 H70A 119.5 . . ? C69 C70 H70A 119.5 . . ? C72 C71 C76 118.2(4) . . ? C72 C71 P2 118.8(3) . . ? C76 C71 P2 122.9(3) . . ? C73 C72 C71 121.3(4) . . ? C73 C72 H72A 119.4 . . ? C71 C72 H72A 119.4 . . ? C74 C73 C72 120.2(4) . . ? C74 C73 H73A 119.9 . . ? C72 C73 H73A 119.9 . . ? C75 C74 C73 119.4(4) . . ? C75 C74 H74A 120.3 . . ? C73 C74 H74A 120.3 . . ? C74 C75 C76 120.8(4) . . ? C74 C75 H75A 119.6 . . ? C76 C75 H75A 119.6 . . ? C75 C76 C71 120.1(4) . . ? C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? C78 C77 P2 173.4(4) . . ? C77 C78 C79 177.6(5) . . ? C84 C79 C80 120.0(4) . . ? C84 C79 C78 121.3(4) . . ? C80 C79 C78 118.7(4) . . ? C81 C80 C79 120.3(5) . . ? C81 C80 H80A 119.9 . . ? C79 C80 H80A 119.9 . . ? C82 C81 C80 119.2(5) . . ? C82 C81 H81A 120.4 . . ? C80 C81 H81A 120.4 . . ? C81 C82 C83 121.4(5) . . ? C81 C82 H82A 119.3 . . ? C83 C82 H82A 119.3 . . ? C82 C83 C84 119.3(5) . . ? C82 C83 H83A 120.4 . . ? C84 C83 H83A 120.4 . . ? C79 C84 C83 119.8(5) . . ? C79 C84 H84A 120.1 . . ? C83 C84 H84A 120.1 . . ? N2A Ru1A N2A 180.0(2) . 7 ? N2A Ru1A N1A 90.67(12) . 7 ? N2A Ru1A N1A 89.33(12) 7 7 ? N2A Ru1A N1A 89.33(12) . . ? N2A Ru1A N1A 90.67(12) 7 . ? N1A Ru1A N1A 180.00(13) 7 . ? N2A Ru1A P1A 89.11(8) . 7 ? N2A Ru1A P1A 90.89(8) 7 7 ? N1A Ru1A P1A 92.03(8) 7 7 ? N1A Ru1A P1A 87.97(8) . 7 ? N2A Ru1A P1A 90.89(8) . . ? N2A Ru1A P1A 89.11(8) 7 . ? N1A Ru1A P1A 87.97(8) 7 . ? N1A Ru1A P1A 92.03(8) . . ? P1A Ru1A P1A 180.00(7) 7 . ? C35A P1A C23A 102.35(18) . . ? C35A P1A C29A 101.06(17) . . ? C23A P1A C29A 103.40(17) . . ? C35A P1A Ru1A 111.90(12) . . ? C23A P1A Ru1A 116.83(11) . . ? C29A P1A Ru1A 118.95(11) . . ? C4A N1A C1A 107.1(3) . . ? C4A N1A Ru1A 127.2(2) . . ? C1A N1A Ru1A 125.8(2) . . ? C6A N2A C9A 107.0(3) . . ? C6A N2A Ru1A 127.2(3) . . ? C9A N2A Ru1A 125.9(2) . . ? N1A C1A C10A 125.6(3) . 7 ? N1A C1A C2A 108.8(3) . . ? C10A C1A C2A 125.5(4) 7 . ? C3A C2A C1A 107.5(4) . . ? C3A C2A H2AA 126.3 . . ? C1A C2A H2AA 126.3 . . ? C2A C3A C4A 107.9(3) . . ? C2A C3A H3AA 126.0 . . ? C4A C3A H3AA 126.0 . . ? N1A C4A C5A 125.3(3) . . ? N1A C4A C3A 108.7(3) . . ? C5A C4A C3A 126.0(3) . . ? C6A C5A C4A 125.2(3) . . ? C6A C5A C11A 116.9(3) . . ? C4A C5A C11A 117.9(3) . . ? N2A C6A C5A 125.8(3) . . ? N2A C6A C7A 108.7(3) . . ? C5A C6A C7A 125.6(3) . . ? C8A C7A C6A 107.2(3) . . ? C8A C7A H7AA 126.4 . . ? C6A C7A H7AA 126.4 . . ? C7A C8A C9A 108.2(3) . . ? C7A C8A H8AA 125.9 . . ? C9A C8A H8AA 125.9 . . ? N2A C9A C10A 125.7(3) . . ? N2A C9A C8A 109.0(3) . . ? C10A C9A C8A 125.4(3) . . ? C1A C10A C9A 126.4(3) 7 . ? C1A C10A C17A 117.5(3) 7 . ? C9A C10A C17A 116.1(3) . . ? C16A C11A C12A 117.5(4) . . ? C16A C11A C5A 121.7(3) . . ? C12A C11A C5A 120.8(3) . . ? C13A C12A C11A 121.5(4) . . ? C13A C12A H12B 119.3 . . ? C11A C12A H12B 119.3 . . ? C14A C13A C12A 120.1(4) . . ? C14A C13A H13B 119.9 . . ? C12A C13A H13B 119.9 . . ? C13A C14A C15A 119.8(4) . . ? C13A C14A H14A 120.1 . . ? C15A C14A H14A 120.1 . . ? C14A C15A C16A 119.7(4) . . ? C14A C15A H15A 120.1 . . ? C16A C15A H15A 120.1 . . ? C11A C16A C15A 121.4(4) . . ? C11A C16A H16A 119.3 . . ? C15A C16A H16A 119.3 . . ? C22A C17A C18A 117.9(4) . . ? C22A C17A C10A 121.1(3) . . ? C18A C17A C10A 120.9(3) . . ? C19A C18A C17A 121.0(4) . . ? C19A C18A H18B 119.5 . . ? C17A C18A H18B 119.5 . . ? C20A C19A C18A 120.0(5) . . ? C20A C19A H19A 120.0 . . ? C18A C19A H19A 120.0 . . ? C21A C20A C19A 120.3(5) . . ? C21A C20A H20A 119.8 . . ? C19A C20A H20A 119.8 . . ? C20A C21A C22A 119.4(4) . . ? C20A C21A H21A 120.3 . . ? C22A C21A H21A 120.3 . . ? C17A C22A C21A 121.3(4) . . ? C17A C22A H22B 119.3 . . ? C21A C22A H22B 119.3 . . ? C24A C23A C28A 117.9(4) . . ? C24A C23A P1A 119.8(3) . . ? C28A C23A P1A 122.3(3) . . ? C23A C24A C25A 121.3(4) . . ? C23A C24A H24B 119.4 . . ? C25A C24A H24B 119.4 . . ? C26A C25A C24A 119.4(4) . . ? C26A C25A H25B 120.3 . . ? C24A C25A H25B 120.3 . . ? C27A C26A C25A 119.9(4) . . ? C27A C26A H26B 120.0 . . ? C25A C26A H26B 120.0 . . ? C26A C27A C28A 121.0(4) . . ? C26A C27A H27A 119.5 . . ? C28A C27A H27A 119.5 . . ? C27A C28A C23A 120.5(4) . . ? C27A C28A H28B 119.8 . . ? C23A C28A H28B 119.8 . . ? C34A C29A C30A 124.0(7) . . ? C34A C29A P1A 115.4(6) . . ? C30A C29A P1A 120.5(5) . . ? C31A C30A C29A 122.5(9) . . ? C31A C30A H30B 118.7 . . ? C29A C30A H30B 118.7 . . ? C30A C31A C32A 118.0(10) . . ? C30A C31A H31B 121.0 . . ? C32A C31A H31B 121.0 . . ? C31A C32A C33A 118.6(8) . . ? C31A C32A H32B 120.7 . . ? C33A C32A H32B 120.7 . . ? C34A C33A C32A 118.9(11) . . ? C34A C33A H33A 120.6 . . ? C32A C33A H33A 120.6 . . ? C29A C34A C33A 117.6(10) . . ? C29A C34A H34B 121.2 . . ? C33A C34A H34B 121.2 . . ? C31' C30' H30' 117.3 . . ? C30' C31' H31' 119.5 . . ? C34' C33' H33' 122.5 . . ? C33' C34' H34' 120.8 . . ? C36A C35A P1A 175.6(4) . . ? C35A C36A C37A 179.9(5) . . ? C38A C37A C42A 119.1(4) . . ? C38A C37A C36A 121.8(3) . . ? C42A C37A C36A 119.1(4) . . ? C37A C38A C39A 120.3(4) . . ? C37A C38A H38B 119.8 . . ? C39A C38A H38B 119.8 . . ? C40A C39A C38A 120.4(4) . . ? C40A C39A H39A 119.8 . . ? C38A C39A H39A 119.8 . . ? C41A C40A C39A 119.8(4) . . ? C41A C40A H40B 120.1 . . ? C39A C40A H40B 120.1 . . ? C40A C41A C42A 120.7(4) . . ? C40A C41A H41B 119.6 . . ? C42A C41A H41B 119.6 . . ? C41A C42A C37A 119.6(4) . . ? C41A C42A H42B 120.2 . . ? C37A C42A H42B 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 P1 C57 -35.24(16) . . . . ? N1 Ru1 P1 C57 54.83(16) . . . . ? N4 Ru1 P1 C57 144.62(16) . . . . ? N3 Ru1 P1 C57 -125.15(16) . . . . ? N2 Ru1 P1 C51 79.43(16) . . . . ? N1 Ru1 P1 C51 169.50(15) . . . . ? N4 Ru1 P1 C51 -100.71(16) . . . . ? N3 Ru1 P1 C51 -10.49(16) . . . . ? N2 Ru1 P1 C45 -153.98(16) . . . . ? N1 Ru1 P1 C45 -63.90(16) . . . . ? N4 Ru1 P1 C45 25.88(16) . . . . ? N3 Ru1 P1 C45 116.11(16) . . . . ? N2 Ru1 P2 C77 109.80(16) . . . . ? N1 Ru1 P2 C77 19.78(16) . . . . ? N4 Ru1 P2 C77 -70.08(16) . . . . ? N3 Ru1 P2 C77 -160.27(16) . . . . ? N2 Ru1 P2 C65 -134.33(16) . . . . ? N1 Ru1 P2 C65 135.65(16) . . . . ? N4 Ru1 P2 C65 45.79(16) . . . . ? N3 Ru1 P2 C65 -44.40(16) . . . . ? N2 Ru1 P2 C71 -7.53(16) . . . . ? N1 Ru1 P2 C71 -97.55(16) . . . . ? N4 Ru1 P2 C71 172.59(16) . . . . ? N3 Ru1 P2 C71 82.40(16) . . . . ? N2 Ru1 N1 C1 177.6(3) . . . . ? N4 Ru1 N1 C1 -2.9(3) . . . . ? P1 Ru1 N1 C1 89.4(3) . . . . ? N2 Ru1 N1 C4 -3.9(3) . . . . ? N4 Ru1 N1 C4 175.6(3) . . . . ? P1 Ru1 N1 C4 -92.1(3) . . . . ? P2 Ru1 N1 C4 86.5(3) . . . . ? N1 Ru1 N2 C9 -175.3(3) . . . . ? N3 Ru1 N2 C9 3.3(3) . . . . ? P1 Ru1 N2 C9 -86.8(3) . . . . ? P2 Ru1 N2 C9 95.2(3) . . . . ? N1 Ru1 N2 C6 8.8(3) . . . . ? N3 Ru1 N2 C6 -172.7(3) . . . . ? P1 Ru1 N2 C6 97.2(3) . . . . ? P2 Ru1 N2 C6 -80.7(3) . . . . ? N2 Ru1 N3 C11 -3.3(3) . . . . ? N4 Ru1 N3 C11 177.2(3) . . . . ? P1 Ru1 N3 C11 84.9(3) . . . . ? P2 Ru1 N3 C11 -93.6(3) . . . . ? N2 Ru1 N3 C14 -178.0(3) . . . . ? N4 Ru1 N3 C14 2.4(3) . . . . ? P1 Ru1 N3 C14 -89.9(3) . . . . ? P2 Ru1 N3 C14 91.6(3) . . . . ? N1 Ru1 N4 C19 -0.8(3) . . . . ? N3 Ru1 N4 C19 -179.4(3) . . . . ? P1 Ru1 N4 C19 -89.3(3) . . . . ? P2 Ru1 N4 C19 88.7(3) . . . . ? N1 Ru1 N4 C16 178.1(3) . . . . ? N3 Ru1 N4 C16 -0.5(3) . . . . ? P1 Ru1 N4 C16 89.6(3) . . . . ? P2 Ru1 N4 C16 -92.4(3) . . . . ? C4 N1 C1 C20 -174.1(3) . . . . ? Ru1 N1 C1 C20 4.6(5) . . . . ? C4 N1 C1 C2 2.6(4) . . . . ? Ru1 N1 C1 C2 -178.7(2) . . . . ? N1 C1 C2 C3 -2.2(4) . . . . ? C20 C1 C2 C3 174.5(3) . . . . ? C1 C2 C3 C4 1.0(4) . . . . ? C1 N1 C4 C5 175.8(3) . . . . ? Ru1 N1 C4 C5 -2.9(5) . . . . ? C1 N1 C4 C3 -2.0(4) . . . . ? Ru1 N1 C4 C3 179.3(2) . . . . ? C2 C3 C4 N1 0.6(4) . . . . ? C2 C3 C4 C5 -177.2(3) . . . . ? N1 C4 C5 C6 7.5(6) . . . . ? C3 C4 C5 C6 -175.1(4) . . . . ? N1 C4 C5 C21 -172.7(3) . . . . ? C3 C4 C5 C21 4.7(5) . . . . ? C9 N2 C6 C5 175.8(4) . . . . ? Ru1 N2 C6 C5 -7.6(5) . . . . ? C9 N2 C6 C7 -0.6(4) . . . . ? Ru1 N2 C6 C7 176.0(2) . . . . ? C4 C5 C6 N2 -1.9(6) . . . . ? C21 C5 C6 N2 178.3(3) . . . . ? C4 C5 C6 C7 173.9(4) . . . . ? C21 C5 C6 C7 -5.9(6) . . . . ? N2 C6 C7 C8 1.8(4) . . . . ? C5 C6 C7 C8 -174.6(4) . . . . ? C6 C7 C8 C9 -2.1(4) . . . . ? C6 N2 C9 C10 175.1(4) . . . . ? Ru1 N2 C9 C10 -1.4(5) . . . . ? C6 N2 C9 C8 -0.7(4) . . . . ? Ru1 N2 C9 C8 -177.2(2) . . . . ? C7 C8 C9 N2 1.8(4) . . . . ? C7 C8 C9 C10 -174.1(4) . . . . ? N2 C9 C10 C11 -2.0(6) . . . . ? C8 C9 C10 C11 173.1(4) . . . . ? N2 C9 C10 C27 -176.3(3) . . . . ? C8 C9 C10 C27 -1.2(5) . . . . ? C14 N3 C11 C10 177.0(3) . . . . ? Ru1 N3 C11 C10 1.4(5) . . . . ? C14 N3 C11 C12 -1.2(4) . . . . ? Ru1 N3 C11 C12 -176.8(2) . . . . ? C9 C10 C11 N3 2.0(6) . . . . ? C27 C10 C11 N3 176.1(3) . . . . ? C9 C10 C11 C12 179.9(4) . . . . ? C27 C10 C11 C12 -6.1(6) . . . . ? N3 C11 C12 C13 0.5(4) . . . . ? C10 C11 C12 C13 -177.6(4) . . . . ? C11 C12 C13 C14 0.4(4) . . . . ? C11 N3 C14 C15 -177.1(3) . . . . ? Ru1 N3 C14 C15 -1.5(5) . . . . ? C11 N3 C14 C13 1.4(4) . . . . ? Ru1 N3 C14 C13 177.0(2) . . . . ? C12 C13 C14 N3 -1.1(4) . . . . ? C12 C13 C14 C15 177.4(4) . . . . ? N3 C14 C15 C16 -2.4(6) . . . . ? C13 C14 C15 C16 179.3(4) . . . . ? N3 C14 C15 C33 173.5(3) . . . . ? C13 C14 C15 C33 -4.8(5) . . . . ? C19 N4 C16 C15 176.4(4) . . . . ? Ru1 N4 C16 C15 -2.7(5) . . . . ? C19 N4 C16 C17 -0.9(4) . . . . ? Ru1 N4 C16 C17 -179.9(2) . . . . ? C14 C15 C16 N4 4.7(6) . . . . ? C33 C15 C16 N4 -171.2(3) . . . . ? C14 C15 C16 C17 -178.5(4) . . . . ? C33 C15 C16 C17 5.6(6) . . . . ? N4 C16 C17 C18 -0.4(4) . . . . ? C15 C16 C17 C18 -177.7(4) . . . . ? C16 C17 C18 C19 1.5(5) . . . . ? C16 N4 C19 C20 -175.7(3) . . . . ? Ru1 N4 C19 C20 3.4(5) . . . . ? C16 N4 C19 C18 1.8(4) . . . . ? Ru1 N4 C19 C18 -179.2(2) . . . . ? C17 C18 C19 N4 -2.0(4) . . . . ? C17 C18 C19 C20 175.4(4) . . . . ? N4 C19 C20 C1 -2.4(6) . . . . ? C18 C19 C20 C1 -179.4(4) . . . . ? N4 C19 C20 C39 178.1(3) . . . . ? C18 C19 C20 C39 1.0(6) . . . . ? N1 C1 C20 C19 -1.8(6) . . . . ? C2 C1 C20 C19 -178.0(4) . . . . ? N1 C1 C20 C39 177.7(3) . . . . ? C2 C1 C20 C39 1.5(5) . . . . ? C6 C5 C21 C22 113.6(4) . . . . ? C4 C5 C21 C22 -66.2(5) . . . . ? C6 C5 C21 C26 -64.9(5) . . . . ? C4 C5 C21 C26 115.3(4) . . . . ? C26 C21 C22 C23 0.1(6) . . . . ? C5 C21 C22 C23 -178.5(4) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C26 0.7(7) . . . . ? C24 C25 C26 C21 -0.5(6) . . . . ? C22 C21 C26 C25 0.2(6) . . . . ? C5 C21 C26 C25 178.7(4) . . . . ? C9 C10 C27 C32 100.1(4) . . . . ? C11 C10 C27 C32 -74.5(4) . . . . ? C9 C10 C27 C28 -73.1(4) . . . . ? C11 C10 C27 C28 112.2(4) . . . . ? C32 C27 C28 C29 -1.4(6) . . . . ? C10 C27 C28 C29 172.1(4) . . . . ? C27 C28 C29 C30 -0.9(6) . . . . ? C28 C29 C30 C31 1.7(7) . . . . ? C29 C30 C31 C32 -0.3(6) . . . . ? C28 C27 C32 C31 2.8(5) . . . . ? C10 C27 C32 C31 -170.7(3) . . . . ? C30 C31 C32 C27 -2.0(6) . . . . ? C16 C15 C33 C38 91.2(5) . . . . ? C14 C15 C33 C38 -85.1(5) . . . . ? C16 C15 C33 C34 -87.0(5) . . . . ? C14 C15 C33 C34 96.7(5) . . . . ? C38 C33 C34 C35 2.3(8) . . . . ? C15 C33 C34 C35 -179.4(5) . . . . ? C33 C34 C35 C36 -0.8(9) . . . . ? C34 C35 C36 C37 -0.2(9) . . . . ? C35 C36 C37 C38 -0.4(8) . . . . ? C34 C33 C38 C37 -2.9(8) . . . . ? C15 C33 C38 C37 178.8(4) . . . . ? C36 C37 C38 C33 2.0(8) . . . . ? C19 C20 C39 C40 -75.9(5) . . . . ? C1 C20 C39 C40 104.6(4) . . . . ? C19 C20 C39 C44 104.3(4) . . . . ? C1 C20 C39 C44 -75.2(5) . . . . ? C44 C39 C40 C41 -0.1(7) . . . . ? C20 C39 C40 C41 -179.9(4) . . . . ? C39 C40 C41 C42 0.7(8) . . . . ? C40 C41 C42 C43 -0.4(8) . . . . ? C41 C42 C43 C44 -0.6(7) . . . . ? C40 C39 C44 C43 -0.9(6) . . . . ? C20 C39 C44 C43 179.0(4) . . . . ? C42 C43 C44 C39 1.2(7) . . . . ? C57 P1 C45 C50 5.6(4) . . . . ? C51 P1 C45 C50 -98.5(3) . . . . ? Ru1 P1 C45 C50 129.3(3) . . . . ? C57 P1 C45 C46 -173.7(3) . . . . ? C51 P1 C45 C46 82.1(3) . . . . ? Ru1 P1 C45 C46 -50.1(3) . . . . ? C50 C45 C46 C47 -0.2(5) . . . . ? P1 C45 C46 C47 179.2(3) . . . . ? C45 C46 C47 C48 1.2(6) . . . . ? C46 C47 C48 C49 -1.2(7) . . . . ? C47 C48 C49 C50 0.3(7) . . . . ? C46 C45 C50 C49 -0.8(6) . . . . ? P1 C45 C50 C49 179.8(4) . . . . ? C48 C49 C50 C45 0.7(8) . . . . ? C57 P1 C51 C52 30.0(4) . . . . ? C45 P1 C51 C52 134.9(3) . . . . ? Ru1 P1 C51 C52 -90.7(3) . . . . ? C57 P1 C51 C56 -154.2(3) . . . . ? C45 P1 C51 C56 -49.2(3) . . . . ? Ru1 P1 C51 C56 85.1(3) . . . . ? C56 C51 C52 C53 1.2(6) . . . . ? P1 C51 C52 C53 177.1(3) . . . . ? C51 C52 C53 C54 -0.6(7) . . . . ? C52 C53 C54 C55 0.4(7) . . . . ? C53 C54 C55 C56 -0.8(7) . . . . ? C54 C55 C56 C51 1.4(7) . . . . ? C52 C51 C56 C55 -1.6(6) . . . . ? P1 C51 C56 C55 -177.6(3) . . . . ? C64 C59 C60 C61 -0.9(7) . . . . ? C58 C59 C60 C61 179.5(4) . . . . ? C59 C60 C61 C62 0.0(8) . . . . ? C60 C61 C62 C63 0.7(8) . . . . ? C61 C62 C63 C64 -0.5(7) . . . . ? C62 C63 C64 C59 -0.4(6) . . . . ? C60 C59 C64 C63 1.1(6) . . . . ? C58 C59 C64 C63 -179.3(4) . . . . ? C77 P2 C65 C66 -133.8(3) . . . . ? C71 P2 C65 C66 -28.2(4) . . . . ? Ru1 P2 C65 C66 104.3(3) . . . . ? C77 P2 C65 C70 49.6(3) . . . . ? C71 P2 C65 C70 155.2(3) . . . . ? Ru1 P2 C65 C70 -72.3(3) . . . . ? C70 C65 C66 C67 -1.2(6) . . . . ? P2 C65 C66 C67 -177.8(3) . . . . ? C65 C66 C67 C68 -0.1(7) . . . . ? C66 C67 C68 C69 0.6(7) . . . . ? C67 C68 C69 C70 0.0(7) . . . . ? C66 C65 C70 C69 1.9(6) . . . . ? P2 C65 C70 C69 178.7(3) . . . . ? C68 C69 C70 C65 -1.3(6) . . . . ? C77 P2 C71 C72 -178.4(3) . . . . ? C65 P2 C71 C72 76.2(3) . . . . ? Ru1 P2 C71 C72 -55.4(4) . . . . ? C77 P2 C71 C76 -2.0(4) . . . . ? C65 P2 C71 C76 -107.4(4) . . . . ? Ru1 P2 C71 C76 121.0(3) . . . . ? C76 C71 C72 C73 -1.9(6) . . . . ? P2 C71 C72 C73 174.6(3) . . . . ? C71 C72 C73 C74 1.2(6) . . . . ? C72 C73 C74 C75 0.5(7) . . . . ? C73 C74 C75 C76 -1.4(7) . . . . ? C74 C75 C76 C71 0.6(7) . . . . ? C72 C71 C76 C75 1.0(6) . . . . ? P2 C71 C76 C75 -175.4(4) . . . . ? C84 C79 C80 C81 -1.7(6) . . . . ? C78 C79 C80 C81 178.1(4) . . . . ? C79 C80 C81 C82 0.2(7) . . . . ? C80 C81 C82 C83 1.9(8) . . . . ? C81 C82 C83 C84 -2.4(8) . . . . ? C80 C79 C84 C83 1.1(6) . . . . ? C78 C79 C84 C83 -178.6(4) . . . . ? C82 C83 C84 C79 0.9(7) . . . . ? N2A Ru1A P1A C35A 112.57(17) . . . . ? N2A Ru1A P1A C35A -67.43(17) 7 . . . ? N1A Ru1A P1A C35A 21.93(17) 7 . . . ? N1A Ru1A P1A C35A -158.07(17) . . . . ? N2A Ru1A P1A C23A -129.94(17) . . . . ? N2A Ru1A P1A C23A 50.06(17) 7 . . . ? N1A Ru1A P1A C23A 139.42(17) 7 . . . ? N1A Ru1A P1A C23A -40.58(17) . . . . ? N2A Ru1A P1A C29A -4.74(17) . . . . ? N2A Ru1A P1A C29A 175.26(17) 7 . . . ? N1A Ru1A P1A C29A -95.37(17) 7 . . . ? N1A Ru1A P1A C29A 84.63(17) . . . . ? N2A Ru1A N1A C4A 2.2(3) . . . . ? N2A Ru1A N1A C4A -177.8(3) 7 . . . ? P1A Ru1A N1A C4A 91.4(3) 7 . . . ? P1A Ru1A N1A C4A -88.6(3) . . . . ? N2A Ru1A N1A C1A -178.6(3) . . . . ? N2A Ru1A N1A C1A 1.4(3) 7 . . . ? P1A Ru1A N1A C1A -89.5(3) 7 . . . ? P1A Ru1A N1A C1A 90.5(3) . . . . ? N1A Ru1A N2A C6A 179.0(3) 7 . . . ? N1A Ru1A N2A C6A -1.0(3) . . . . ? P1A Ru1A N2A C6A -89.0(3) 7 . . . ? P1A Ru1A N2A C6A 91.0(3) . . . . ? N1A Ru1A N2A C9A 0.0(3) 7 . . . ? N1A Ru1A N2A C9A 180.0(3) . . . . ? P1A Ru1A N2A C9A 92.0(3) 7 . . . ? P1A Ru1A N2A C9A -88.0(3) . . . . ? C4A N1A C1A C10A 177.9(3) . . . 7 ? Ru1A N1A C1A C10A -1.3(5) . . . 7 ? C4A N1A C1A C2A 0.9(4) . . . . ? Ru1A N1A C1A C2A -178.4(2) . . . . ? N1A C1A C2A C3A -0.3(4) . . . . ? C10A C1A C2A C3A -177.3(3) 7 . . . ? C1A C2A C3A C4A -0.5(4) . . . . ? C1A N1A C4A C5A 178.2(3) . . . . ? Ru1A N1A C4A C5A -2.6(5) . . . . ? C1A N1A C4A C3A -1.2(4) . . . . ? Ru1A N1A C4A C3A 178.1(2) . . . . ? C2A C3A C4A N1A 1.0(4) . . . . ? C2A C3A C4A C5A -178.3(3) . . . . ? N1A C4A C5A C6A 1.0(5) . . . . ? C3A C4A C5A C6A -179.8(3) . . . . ? N1A C4A C5A C11A -178.1(3) . . . . ? C3A C4A C5A C11A 1.2(5) . . . . ? C9A N2A C6A C5A 179.2(3) . . . . ? Ru1A N2A C6A C5A 0.0(5) . . . . ? C9A N2A C6A C7A -0.6(4) . . . . ? Ru1A N2A C6A C7A -179.8(2) . . . . ? C4A C5A C6A N2A 0.4(5) . . . . ? C11A C5A C6A N2A 179.4(3) . . . . ? C4A C5A C6A C7A -179.8(3) . . . . ? C11A C5A C6A C7A -0.8(5) . . . . ? N2A C6A C7A C8A 0.2(4) . . . . ? C5A C6A C7A C8A -179.5(3) . . . . ? C6A C7A C8A C9A 0.2(4) . . . . ? C6A N2A C9A C10A -177.5(3) . . . . ? Ru1A N2A C9A C10A 1.7(5) . . . . ? C6A N2A C9A C8A 0.8(4) . . . . ? Ru1A N2A C9A C8A 179.9(2) . . . . ? C7A C8A C9A N2A -0.6(4) . . . . ? C7A C8A C9A C10A 177.6(3) . . . . ? N2A C9A C10A C1A -2.2(6) . . . 7 ? C8A C9A C10A C1A 179.8(3) . . . 7 ? N2A C9A C10A C17A 177.8(3) . . . . ? C8A C9A C10A C17A -0.2(5) . . . . ? C6A C5A C11A C16A 58.3(5) . . . . ? C4A C5A C11A C16A -122.6(4) . . . . ? C6A C5A C11A C12A -118.5(4) . . . . ? C4A C5A C11A C12A 60.6(5) . . . . ? C16A C11A C12A C13A -0.3(6) . . . . ? C5A C11A C12A C13A 176.6(4) . . . . ? C11A C12A C13A C14A 0.4(6) . . . . ? C12A C13A C14A C15A -0.1(7) . . . . ? C13A C14A C15A C16A -0.4(8) . . . . ? C12A C11A C16A C15A -0.2(6) . . . . ? C5A C11A C16A C15A -177.1(4) . . . . ? C14A C15A C16A C11A 0.6(8) . . . . ? C1A C10A C17A C22A 73.3(5) 7 . . . ? C9A C10A C17A C22A -106.7(4) . . . . ? C1A C10A C17A C18A -108.4(4) 7 . . . ? C9A C10A C17A C18A 71.6(5) . . . . ? C22A C17A C18A C19A 0.6(7) . . . . ? C10A C17A C18A C19A -177.8(4) . . . . ? C17A C18A C19A C20A -0.4(8) . . . . ? C18A C19A C20A C21A 0.0(8) . . . . ? C19A C20A C21A C22A 0.3(8) . . . . ? C18A C17A C22A C21A -0.3(7) . . . . ? C10A C17A C22A C21A 178.0(4) . . . . ? C20A C21A C22A C17A -0.1(7) . . . . ? C35A P1A C23A C24A -174.7(3) . . . . ? C29A P1A C23A C24A -70.0(3) . . . . ? Ru1A P1A C23A C24A 62.7(3) . . . . ? C35A P1A C23A C28A 7.9(4) . . . . ? C29A P1A C23A C28A 112.7(3) . . . . ? Ru1A P1A C23A C28A -114.6(3) . . . . ? C28A C23A C24A C25A -2.0(6) . . . . ? P1A C23A C24A C25A -179.5(3) . . . . ? C23A C24A C25A C26A 1.1(6) . . . . ? C24A C25A C26A C27A 0.5(6) . . . . ? C25A C26A C27A C28A -1.2(7) . . . . ? C26A C27A C28A C23A 0.3(6) . . . . ? C24A C23A C28A C27A 1.3(6) . . . . ? P1A C23A C28A C27A 178.7(3) . . . . ? C35A P1A C29A C34A -37.0(4) . . . . ? C23A P1A C29A C34A -142.7(4) . . . . ? Ru1A P1A C29A C34A 85.9(4) . . . . ? C35A P1A C29A C30A 146.3(3) . . . . ? C23A P1A C29A C30A 40.7(3) . . . . ? Ru1A P1A C29A C30A -90.8(3) . . . . ? C34A C29A C30A C31A 1.8(3) . . . . ? P1A C29A C30A C31A 178.1(3) . . . . ? C29A C30A C31A C32A 3.1(3) . . . . ? C30A C31A C32A C33A -7.4(5) . . . . ? C31A C32A C33A C34A 7.3(7) . . . . ? C30A C29A C34A C33A -1.9(6) . . . . ? P1A C29A C34A C33A -178.4(4) . . . . ? C32A C33A C34A C29A -2.7(8) . . . . ? C42A C37A C38A C39A 0.6(6) . . . . ? C36A C37A C38A C39A 179.8(4) . . . . ? C37A C38A C39A C40A -0.5(6) . . . . ? C38A C39A C40A C41A -0.6(7) . . . . ? C39A C40A C41A C42A 1.5(7) . . . . ? C40A C41A C42A C37A -1.4(6) . . . . ? C38A C37A C42A C41A 0.3(6) . . . . ? C36A C37A C42A C41A -179.0(4) . . . . ?