data_0 _publ_requested_journal ? _publ_section_title ; Ruthenium(II) Arene Complexes with N,O-Chelating Beta-Ketoamine Ligands: Synthesis, Structure and Antiproliferative Activity. ; _publ_contact_author_name 'Riccardo Pettinari' _publ_contact_author_address ;School of Pharmacy and School of Science and Technology Univeristy of Camerino Via S. Agostino 1, 62032 Camerino MC Italy ; _publ_contact_author_email riccardo.pettinari@unicam.it _publ_contact_author_phone '+39 0737402338' _publ_contact_author_fax ? loop_ _publ_author_name ; 'Pettinari, Riccardo' 'Marchetti, Fabio' 'Pettinari, Claudio' 'Petrini, Agnese' 'Scopelliti, Rosario' 'Clavel, Catherine M.' 'Dyson, Paul J.' ; data_HL_ph_naph _audit_update_record ; 2013-01-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H21 N3 O' _chemical_formula_sum 'C27 H21 N3 O' _chemical_formula_weight 403.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.924(5) _cell_length_b 18.158(6) _cell_length_c 11.927(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.92(2) _cell_angle_gamma 90.00 _cell_volume 2066.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 510 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 140(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 marmux _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8866 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.1252 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.67 _reflns_number_total 4717 _reflns_number_gt 3561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marmux - Micro-beam system, marresearch, 2010' _computing_cell_refinement 'automar, marresearch, 2010' _computing_data_reduction 'automar, marresearch, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.7082P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.056(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4717 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.69605(12) 0.49508(7) 0.39237(10) 0.0348(3) Uani 1 1 d . . . N1 N 0.65835(14) 0.39680(7) 0.50847(11) 0.0273(3) Uani 1 1 d . . . N2 N 0.54469(14) 0.35269(8) 0.51602(12) 0.0289(3) Uani 1 1 d . . . N3 N 0.45875(15) 0.52329(8) 0.22301(12) 0.0297(3) Uani 1 1 d . . . H3 H 0.548(3) 0.5345(13) 0.278(2) 0.056(6) Uiso 1 1 d . . . C1 C 0.62000(17) 0.44615(9) 0.41761(14) 0.0279(4) Uani 1 1 d . . . C2 C 0.43757(17) 0.37153(9) 0.42902(14) 0.0274(3) Uani 1 1 d . . . C3 C 0.47514(17) 0.42868(9) 0.35940(14) 0.0271(3) Uani 1 1 d . . . C4 C 0.79046(16) 0.38631(9) 0.59149(13) 0.0258(3) Uani 1 1 d . . . C5 C 0.90921(17) 0.42444(9) 0.58263(14) 0.0299(4) Uani 1 1 d . . . H5 H 0.9024 0.4589 0.5213 0.036 Uiso 1 1 calc R . . C6 C 1.03762(18) 0.41192(9) 0.66367(15) 0.0326(4) Uani 1 1 d . . . H6 H 1.1183 0.4378 0.6573 0.039 Uiso 1 1 calc R . . C7 C 1.04897(18) 0.36184(9) 0.75402(15) 0.0318(4) Uani 1 1 d . . . H7 H 1.1368 0.3534 0.8093 0.038 Uiso 1 1 calc R . . C8 C 0.93051(18) 0.32436(9) 0.76231(14) 0.0310(4) Uani 1 1 d . . . H8 H 0.9379 0.2900 0.8238 0.037 Uiso 1 1 calc R . . C9 C 0.80099(17) 0.33604(9) 0.68245(14) 0.0286(4) Uani 1 1 d . . . H9 H 0.7205 0.3102 0.6895 0.034 Uiso 1 1 calc R . . C10 C 0.29731(18) 0.33789(10) 0.42101(15) 0.0344(4) Uani 1 1 d . . . H10A H 0.3057 0.3034 0.4858 0.052 Uiso 1 1 calc R . . H10B H 0.2641 0.3115 0.3469 0.052 Uiso 1 1 calc R . . H10C H 0.2304 0.3768 0.4251 0.052 Uiso 1 1 calc R . . C11 C 0.40030(16) 0.46359(9) 0.25676(14) 0.0268(3) Uani 1 1 d . . . C12 C 0.26129(17) 0.43598(9) 0.18825(13) 0.0267(3) Uani 1 1 d . . . C13 C 0.24869(18) 0.36534(9) 0.13956(14) 0.0308(4) Uani 1 1 d . . . H13 H 0.3296 0.3355 0.1483 0.037 Uiso 1 1 calc R . . C14 C 0.11810(19) 0.33890(10) 0.07862(15) 0.0341(4) Uani 1 1 d . . . H14 H 0.1097 0.2912 0.0446 0.041 Uiso 1 1 calc R . . C15 C -0.00001(19) 0.38186(10) 0.06732(15) 0.0352(4) Uani 1 1 d . . . H15 H -0.0896 0.3634 0.0265 0.042 Uiso 1 1 calc R . . C16 C 0.01219(18) 0.45194(10) 0.11559(16) 0.0356(4) Uani 1 1 d . . . H16 H -0.0692 0.4812 0.1081 0.043 Uiso 1 1 calc R . . C17 C 0.14286(17) 0.47942(9) 0.17471(15) 0.0309(4) Uani 1 1 d . . . H17 H 0.1512 0.5279 0.2059 0.037 Uiso 1 1 calc R . . C18 C 0.42460(16) 0.56333(9) 0.11646(14) 0.0286(4) Uani 1 1 d . . . C19 C 0.35768(17) 0.53263(10) 0.01071(14) 0.0319(4) Uani 1 1 d . . . H19 H 0.3232 0.4836 0.0071 0.038 Uiso 1 1 calc R . . C20 C 0.34000(18) 0.57378(11) -0.09291(15) 0.0348(4) Uani 1 1 d . . . H20 H 0.2916 0.5526 -0.1656 0.042 Uiso 1 1 calc R . . C21 C 0.39173(18) 0.64363(11) -0.08970(15) 0.0353(4) Uani 1 1 d . . . H21 H 0.3809 0.6701 -0.1603 0.042 Uiso 1 1 calc R . . C22 C 0.46157(18) 0.67711(10) 0.01821(15) 0.0324(4) Uani 1 1 d . . . C23 C 0.5163(2) 0.74984(10) 0.02433(17) 0.0400(4) Uani 1 1 d . . . H23 H 0.5075 0.7768 -0.0456 0.048 Uiso 1 1 calc R . . C24 C 0.5812(2) 0.78150(11) 0.12868(18) 0.0444(5) Uani 1 1 d . . . H24 H 0.6179 0.8300 0.1310 0.053 Uiso 1 1 calc R . . C25 C 0.5938(2) 0.74274(10) 0.23256(17) 0.0410(4) Uani 1 1 d . . . H25 H 0.6381 0.7655 0.3050 0.049 Uiso 1 1 calc R . . C26 C 0.54292(18) 0.67244(10) 0.23111(15) 0.0337(4) Uani 1 1 d . . . H26 H 0.5521 0.6470 0.3024 0.040 Uiso 1 1 calc R . . C27 C 0.47667(17) 0.63736(9) 0.12391(14) 0.0291(4) 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 O1 0.0306(6) 0.0355(7) 0.0347(7) 0.0092(5) 0.0031(5) -0.0081(5) N1 0.0245(7) 0.0278(7) 0.0278(7) 0.0035(5) 0.0042(6) -0.0035(5) N2 0.0265(7) 0.0286(7) 0.0306(7) 0.0029(5) 0.0061(6) -0.0045(5) N3 0.0282(7) 0.0310(7) 0.0267(7) 0.0051(6) 0.0022(6) -0.0038(6) C1 0.0290(8) 0.0270(8) 0.0272(8) 0.0012(6) 0.0069(6) -0.0025(6) C2 0.0284(8) 0.0254(8) 0.0276(8) -0.0001(6) 0.0064(6) -0.0009(6) C3 0.0268(8) 0.0262(8) 0.0272(8) 0.0015(6) 0.0052(6) -0.0003(6) C4 0.0264(8) 0.0249(8) 0.0249(8) -0.0022(6) 0.0050(6) 0.0008(6) C5 0.0295(8) 0.0293(8) 0.0304(8) 0.0011(6) 0.0071(7) -0.0016(6) C6 0.0287(9) 0.0332(9) 0.0350(9) -0.0018(7) 0.0071(7) -0.0027(7) C7 0.0289(8) 0.0328(9) 0.0296(9) -0.0022(7) 0.0011(7) 0.0031(7) C8 0.0339(9) 0.0294(8) 0.0271(8) 0.0010(6) 0.0042(7) 0.0019(7) C9 0.0307(8) 0.0265(8) 0.0275(8) -0.0014(6) 0.0062(7) -0.0027(6) C10 0.0297(9) 0.0379(9) 0.0344(9) 0.0048(7) 0.0070(7) -0.0054(7) C11 0.0267(8) 0.0269(8) 0.0270(8) -0.0011(6) 0.0074(6) -0.0002(6) C12 0.0287(8) 0.0268(8) 0.0230(7) 0.0023(6) 0.0046(6) -0.0013(6) C13 0.0304(9) 0.0270(8) 0.0326(9) 0.0003(7) 0.0047(7) 0.0033(7) C14 0.0385(10) 0.0282(8) 0.0311(9) -0.0024(7) 0.0022(7) -0.0030(7) C15 0.0296(9) 0.0378(10) 0.0331(9) -0.0014(7) 0.0003(7) -0.0052(7) C16 0.0264(8) 0.0371(9) 0.0408(10) -0.0043(8) 0.0051(7) 0.0023(7) C17 0.0311(9) 0.0283(8) 0.0316(8) -0.0032(7) 0.0057(7) 0.0020(7) C18 0.0249(8) 0.0324(8) 0.0278(8) 0.0046(6) 0.0062(6) 0.0019(6) C19 0.0267(8) 0.0360(9) 0.0309(8) 0.0033(7) 0.0044(7) 0.0011(7) C20 0.0276(8) 0.0474(10) 0.0279(8) 0.0032(7) 0.0048(7) 0.0033(7) C21 0.0307(9) 0.0448(10) 0.0305(9) 0.0108(7) 0.0086(7) 0.0069(8) C22 0.0300(9) 0.0355(9) 0.0333(9) 0.0076(7) 0.0115(7) 0.0061(7) C23 0.0467(11) 0.0346(10) 0.0424(10) 0.0122(8) 0.0185(9) 0.0020(8) C24 0.0554(12) 0.0325(10) 0.0494(11) 0.0043(8) 0.0214(10) -0.0049(9) C25 0.0487(11) 0.0360(10) 0.0403(10) -0.0017(8) 0.0155(9) -0.0077(8) C26 0.0373(9) 0.0333(9) 0.0322(9) 0.0020(7) 0.0122(7) -0.0019(7) C27 0.0263(8) 0.0324(9) 0.0297(8) 0.0047(7) 0.0094(7) 0.0028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.255(2) . ? N1 C1 1.377(2) . ? N1 N2 1.4064(19) . ? N1 C4 1.422(2) . ? N2 C2 1.311(2) . ? N3 C11 1.342(2) . ? N3 C18 1.422(2) . ? N3 H3 0.97(2) . ? C1 C3 1.450(2) . ? C2 C3 1.441(2) . ? C2 C10 1.499(2) . ? C3 C11 1.398(2) . ? C4 C5 1.396(2) . ? C4 C9 1.400(2) . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 C7 1.391(2) . ? C6 H6 0.9500 . ? C7 C8 1.385(2) . ? C7 H7 0.9500 . ? C8 C9 1.390(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.485(2) . ? C12 C17 1.388(2) . ? C12 C13 1.399(2) . ? C13 C14 1.386(2) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.388(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.372(2) . ? C18 C27 1.434(2) . ? C19 C20 1.413(2) . ? C19 H19 0.9500 . ? C20 C21 1.365(3) . ? C20 H20 0.9500 . ? C21 C22 1.420(3) . ? C21 H21 0.9500 . ? C22 C23 1.422(3) . ? C22 C27 1.425(2) . ? C23 C24 1.362(3) . ? C23 H23 0.9500 . ? C24 C25 1.400(3) . ? C24 H24 0.9500 . ? C25 C26 1.371(3) . ? C25 H25 0.9500 . ? C26 C27 1.418(2) . ? C26 H26 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 C1 N1 N2 111.57(13) . . ? C1 N1 C4 129.64(13) . . ? N2 N1 C4 118.78(13) . . ? C2 N2 N1 106.93(13) . . ? C11 N3 C18 131.62(14) . . ? C11 N3 H3 110.9(14) . . ? C18 N3 H3 116.5(14) . . ? O1 C1 N1 126.52(15) . . ? O1 C1 C3 128.52(15) . . ? N1 C1 C3 104.97(13) . . ? N2 C2 C3 111.24(14) . . ? N2 C2 C10 118.77(15) . . ? C3 C2 C10 129.75(15) . . ? C11 C3 C2 132.24(15) . . ? C11 C3 C1 122.62(15) . . ? C2 C3 C1 105.13(13) . . ? C5 C4 C9 119.81(15) . . ? C5 C4 N1 121.14(14) . . ? C9 C4 N1 119.04(14) . . ? C6 C5 C4 119.88(16) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.63(16) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 119.12(16) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 121.29(16) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 119.27(15) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C3 117.36(14) . . ? N3 C11 C12 121.36(14) . . ? C3 C11 C12 121.28(14) . . ? C17 C12 C13 119.76(15) . . ? C17 C12 C11 120.11(15) . . ? C13 C12 C11 120.12(15) . . ? C14 C13 C12 119.95(16) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.07(16) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.08(16) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.22(16) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C12 C17 C16 119.89(16) . . ? C12 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 N3 123.40(16) . . ? C19 C18 C27 120.86(15) . . ? N3 C18 C27 115.49(14) . . ? C18 C19 C20 120.12(17) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 120.74(17) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.63(16) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 121.91(16) . . ? C21 C22 C27 119.45(16) . . ? C23 C22 C27 118.63(16) . . ? C24 C23 C22 121.13(17) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.11(18) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.90(18) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.50(16) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 118.71(16) . . ? C26 C27 C18 123.16(15) . . ? C22 C27 C18 118.13(15) . . ? 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 C1 N1 N2 C2 2.40(18) . . . . ? C4 N1 N2 C2 -178.36(13) . . . . ? N2 N1 C1 O1 176.18(16) . . . . ? C4 N1 C1 O1 -3.0(3) . . . . ? N2 N1 C1 C3 -3.94(17) . . . . ? C4 N1 C1 C3 176.93(15) . . . . ? N1 N2 C2 C3 0.28(18) . . . . ? N1 N2 C2 C10 -174.70(14) . . . . ? N2 C2 C3 C11 176.58(17) . . . . ? C10 C2 C3 C11 -9.1(3) . . . . ? N2 C2 C3 C1 -2.63(18) . . . . ? C10 C2 C3 C1 171.64(17) . . . . ? O1 C1 C3 C11 4.4(3) . . . . ? N1 C1 C3 C11 -175.45(15) . . . . ? O1 C1 C3 C2 -176.26(17) . . . . ? N1 C1 C3 C2 3.86(17) . . . . ? C1 N1 C4 C5 -6.0(2) . . . . ? N2 N1 C4 C5 174.91(14) . . . . ? C1 N1 C4 C9 174.86(16) . . . . ? N2 N1 C4 C9 -4.2(2) . . . . ? C9 C4 C5 C6 0.5(2) . . . . ? N1 C4 C5 C6 -178.65(14) . . . . ? C4 C5 C6 C7 -0.2(3) . . . . ? C5 C6 C7 C8 0.1(3) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C7 C8 C9 C4 0.4(2) . . . . ? C5 C4 C9 C8 -0.6(2) . . . . ? N1 C4 C9 C8 178.56(14) . . . . ? C18 N3 C11 C3 167.66(16) . . . . ? C18 N3 C11 C12 -12.7(3) . . . . ? C2 C3 C11 N3 169.83(17) . . . . ? C1 C3 C11 N3 -11.1(2) . . . . ? C2 C3 C11 C12 -9.8(3) . . . . ? C1 C3 C11 C12 169.30(15) . . . . ? N3 C11 C12 C17 -63.2(2) . . . . ? C3 C11 C12 C17 116.42(18) . . . . ? N3 C11 C12 C13 118.41(18) . . . . ? C3 C11 C12 C13 -62.0(2) . . . . ? C17 C12 C13 C14 -0.3(2) . . . . ? C11 C12 C13 C14 178.06(15) . . . . ? C12 C13 C14 C15 -0.9(3) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C13 C12 C17 C16 1.6(2) . . . . ? C11 C12 C17 C16 -176.76(15) . . . . ? C15 C16 C17 C12 -1.7(3) . . . . ? C11 N3 C18 C19 -26.6(3) . . . . ? C11 N3 C18 C27 159.14(17) . . . . ? N3 C18 C19 C20 -173.52(15) . . . . ? C27 C18 C19 C20 0.4(2) . . . . ? C18 C19 C20 C21 1.5(3) . . . . ? C19 C20 C21 C22 -1.5(3) . . . . ? C20 C21 C22 C23 -179.88(17) . . . . ? C20 C21 C22 C27 -0.4(3) . . . . ? C21 C22 C23 C24 179.01(18) . . . . ? C27 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C25 -0.6(3) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C25 C26 C27 C22 -1.2(3) . . . . ? C25 C26 C27 C18 178.35(17) . . . . ? C21 C22 C27 C26 -178.11(15) . . . . ? C23 C22 C27 C26 1.4(2) . . . . ? C21 C22 C27 C18 2.3(2) . . . . ? C23 C22 C27 C18 -178.25(16) . . . . ? C19 C18 C27 C26 178.12(16) . . . . ? N3 C18 C27 C26 -7.5(2) . . . . ? C19 C18 C27 C22 -2.3(2) . . . . ? N3 C18 C27 C22 172.11(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O1 0.97(2) 1.85(2) 2.698(2) 144(2) . _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.255 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.073 _iucr_refine_instructions_details ; TITL CC1 in P2(1)/n CELL 0.71073 9.9240 18.1580 11.9270 90.000 105.921 90.000 ZERR 4.00 0.0050 0.0060 0.0040 0.000 0.022 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 108 84 12 4 REM ------------------------------------------------------------------------- REM Data measured on the marmux REM Crystal colour: yellow; Crystal habit: prismatic REM ------------------------------------------------------------------------- L.S. 10 ACTA OMIT 3 3 2 OMIT 0 5 5 OMIT 0 10 0 OMIT 0 7 14 CONF HTAB N3 O1 WPDB -2 BOND $H SIZE 0.38 0.22 0.20 FMAP 2 PLAN 10 TEMP -133 WGHT 0.042000 0.708200 EXTI 0.055829 FVAR 0.36699 O1 4 0.696052 0.495077 0.392366 11.00000 0.03059 0.03548 = 0.03474 0.00925 0.00313 -0.00807 N1 3 0.658353 0.396801 0.508473 11.00000 0.02451 0.02785 = 0.02775 0.00348 0.00419 -0.00346 N2 3 0.544685 0.352687 0.516021 11.00000 0.02645 0.02858 = 0.03061 0.00286 0.00607 -0.00446 N3 3 0.458752 0.523291 0.223006 11.00000 0.02817 0.03101 = 0.02672 0.00512 0.00220 -0.00379 H3 2 0.547844 0.534508 0.277860 11.00000 0.05555 C1 1 0.619996 0.446151 0.417613 11.00000 0.02901 0.02701 = 0.02720 0.00121 0.00689 -0.00253 C2 1 0.437569 0.371526 0.429020 11.00000 0.02842 0.02539 = 0.02761 -0.00009 0.00644 -0.00091 C3 1 0.475137 0.428678 0.359397 11.00000 0.02677 0.02617 = 0.02722 0.00153 0.00525 -0.00035 C4 1 0.790461 0.386314 0.591489 11.00000 0.02642 0.02486 = 0.02488 -0.00219 0.00496 0.00076 C5 1 0.909215 0.424435 0.582627 11.00000 0.02948 0.02934 = 0.03037 0.00113 0.00714 -0.00156 AFIX 43 H5 2 0.902352 0.458871 0.521349 11.00000 -1.20000 AFIX 0 C6 1 1.037619 0.411918 0.663669 11.00000 0.02873 0.03316 = 0.03504 -0.00182 0.00708 -0.00275 AFIX 43 H6 2 1.118344 0.437822 0.657254 11.00000 -1.20000 AFIX 0 C7 1 1.048972 0.361839 0.754015 11.00000 0.02890 0.03282 = 0.02959 -0.00219 0.00110 0.00308 AFIX 43 H7 2 1.136802 0.353447 0.809308 11.00000 -1.20000 AFIX 0 C8 1 0.930511 0.324358 0.762309 11.00000 0.03392 0.02940 = 0.02714 0.00100 0.00423 0.00187 AFIX 43 H8 2 0.937922 0.289996 0.823771 11.00000 -1.20000 AFIX 0 C9 1 0.800993 0.336040 0.682454 11.00000 0.03072 0.02652 = 0.02752 -0.00143 0.00625 -0.00266 AFIX 43 H9 2 0.720514 0.310184 0.689545 11.00000 -1.20000 AFIX 0 C10 1 0.297313 0.337887 0.421010 11.00000 0.02975 0.03786 = 0.03441 0.00478 0.00697 -0.00540 AFIX 33 H10A 2 0.305715 0.303417 0.485794 11.00000 -1.50000 H10B 2 0.264141 0.311460 0.346894 11.00000 -1.50000 H10C 2 0.230380 0.376790 0.425103 11.00000 -1.50000 AFIX 0 C11 1 0.400302 0.463592 0.256760 11.00000 0.02669 0.02685 = 0.02702 -0.00110 0.00743 -0.00016 C12 1 0.261292 0.435982 0.188248 11.00000 0.02870 0.02681 = 0.02299 0.00231 0.00462 -0.00127 C13 1 0.248691 0.365342 0.139557 11.00000 0.03045 0.02700 = 0.03259 0.00025 0.00470 0.00329 AFIX 43 H13 2 0.329578 0.335528 0.148258 11.00000 -1.20000 AFIX 0 C14 1 0.118100 0.338902 0.078618 11.00000 0.03850 0.02825 = 0.03112 -0.00243 0.00219 -0.00298 AFIX 43 H14 2 0.109701 0.291231 0.044578 11.00000 -1.20000 AFIX 0 C15 1 -0.000014 0.381862 0.067319 11.00000 0.02960 0.03783 = 0.03309 -0.00144 0.00028 -0.00520 AFIX 43 H15 2 -0.089585 0.363380 0.026477 11.00000 -1.20000 AFIX 0 C16 1 0.012191 0.451941 0.115586 11.00000 0.02644 0.03705 = 0.04085 -0.00431 0.00509 0.00234 AFIX 43 H16 2 -0.069174 0.481187 0.108120 11.00000 -1.20000 AFIX 0 C17 1 0.142859 0.479421 0.174712 11.00000 0.03112 0.02835 = 0.03165 -0.00322 0.00571 0.00204 AFIX 43 H17 2 0.151207 0.527887 0.205864 11.00000 -1.20000 AFIX 0 C18 1 0.424596 0.563327 0.116457 11.00000 0.02494 0.03244 = 0.02777 0.00461 0.00623 0.00187 C19 1 0.357684 0.532635 0.010710 11.00000 0.02672 0.03604 = 0.03086 0.00332 0.00443 0.00112 AFIX 43 H19 2 0.323184 0.483640 0.007143 11.00000 -1.20000 AFIX 0 C20 1 0.340000 0.573779 -0.092908 11.00000 0.02760 0.04738 = 0.02787 0.00319 0.00476 0.00332 AFIX 43 H20 2 0.291560 0.552581 -0.165613 11.00000 -1.20000 AFIX 0 C21 1 0.391732 0.643626 -0.089699 11.00000 0.03067 0.04484 = 0.03050 0.01077 0.00861 0.00690 AFIX 43 H21 2 0.380920 0.670099 -0.160322 11.00000 -1.20000 AFIX 0 C22 1 0.461570 0.677112 0.018206 11.00000 0.03004 0.03555 = 0.03334 0.00764 0.01150 0.00609 C23 1 0.516339 0.749843 0.024325 11.00000 0.04673 0.03464 = 0.04241 0.01217 0.01847 0.00199 AFIX 43 H23 2 0.507537 0.776796 -0.045587 11.00000 -1.20000 AFIX 0 C24 1 0.581173 0.781498 0.128684 11.00000 0.05542 0.03253 = 0.04941 0.00433 0.02138 -0.00491 AFIX 43 H24 2 0.617926 0.829958 0.131022 11.00000 -1.20000 AFIX 0 C25 1 0.593763 0.742743 0.232561 11.00000 0.04865 0.03602 = 0.04029 -0.00165 0.01549 -0.00774 AFIX 43 H25 2 0.638140 0.765474 0.305027 11.00000 -1.20000 AFIX 0 C26 1 0.542920 0.672444 0.231108 11.00000 0.03730 0.03328 = 0.03215 0.00196 0.01222 -0.00191 AFIX 43 H26 2 0.552135 0.647036 0.302447 11.00000 -1.20000 AFIX 0 C27 1 0.476665 0.637358 0.123907 11.00000 0.02628 0.03238 = 0.02971 0.00469 0.00940 0.00283 HKLF 4 REM CC1 in P2(1)/n REM R1 = 0.0528 for 3561 Fo > 4sig(Fo) and 0.0739 for all 4717 data REM 285 parameters refined using 0 restraints END WGHT 0.0420 0.7081 REM Highest difference peak 0.255, deepest hole -0.293, 1-sigma level 0.073 Q1 1 0.2260 0.3621 0.0334 11.00000 0.05 0.26 Q2 1 0.4881 0.6310 0.3796 11.00000 0.05 0.25 Q3 1 0.3053 0.3847 0.0404 11.00000 0.05 0.25 Q4 1 0.4608 0.6550 0.2973 11.00000 0.05 0.24 Q5 1 0.2778 0.3195 0.5003 11.00000 0.05 0.24 Q6 1 0.5767 0.3223 0.5977 11.00000 0.05 0.24 Q7 1 0.8440 0.3456 0.7546 11.00000 0.05 0.23 Q8 1 0.5339 0.6707 0.3398 11.00000 0.05 0.23 Q9 1 0.7412 0.3437 0.7599 11.00000 0.05 0.23 Q10 1 0.5367 0.6734 0.4028 11.00000 0.05 0.22 ; data_1 _audit_update_record ; 2013-04-25 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H36 Cl N3 O Ru' _chemical_formula_sum 'C39 H36 Cl N3 O Ru' _chemical_formula_weight 699.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5770(4) _cell_length_b 21.8748(4) _cell_length_c 12.8619(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.999(4) _cell_angle_gamma 90.00 _cell_volume 3280.93(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4505 _cell_measurement_theta_min 3.7034 _cell_measurement_theta_max 72.8958 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 4.888 _exptl_absorpt_correction_T_min 0.50202 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.2665 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10551 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 73.04 _reflns_number_total 6266 _reflns_number_gt 4864 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+7.1707P] 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 6266 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1899 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.10292(4) 0.165677(19) 0.23547(3) 0.04057(17) Uani 1 1 d . . . Cl1 Cl 0.18555(19) 0.25093(8) 0.35813(15) 0.0682(5) Uani 1 1 d . . . O1 O -0.0404(4) 0.1817(2) 0.2737(3) 0.0502(10) Uani 1 1 d . . . N1 N -0.1318(4) 0.1926(2) 0.3971(4) 0.0478(11) Uani 1 1 d . . . N2 N -0.1212(5) 0.1728(3) 0.5039(5) 0.0520(12) Uani 1 1 d . . . N3 N 0.1687(4) 0.1128(2) 0.3852(4) 0.0451(10) Uani 1 1 d . . . C1 C -0.0448(5) 0.1712(3) 0.3689(5) 0.0424(12) Uani 1 1 d . . . C2 C -0.2220(5) 0.2331(3) 0.3372(6) 0.0503(14) Uani 1 1 d . . . C3 C -0.2189(6) 0.2669(4) 0.2472(7) 0.0618(17) Uani 1 1 d . . . H3 H -0.1567 0.2633 0.2251 0.074 Uiso 1 1 calc R . . C4 C -0.3093(8) 0.3062(4) 0.1897(7) 0.072(2) Uani 1 1 d . . . H4 H -0.3078 0.3280 0.1282 0.087 Uiso 1 1 calc R . . C5 C -0.3994(7) 0.3130(5) 0.2227(8) 0.079(2) Uani 1 1 d . . . H5 H -0.4593 0.3393 0.1843 0.095 Uiso 1 1 calc R . . C6 C -0.4011(7) 0.2805(5) 0.3132(8) 0.083(3) Uani 1 1 d . . . H6 H -0.4624 0.2856 0.3362 0.099 Uiso 1 1 calc R . . C7 C -0.3134(6) 0.2403(4) 0.3716(7) 0.070(2) Uani 1 1 d . . . H7 H -0.3161 0.2186 0.4327 0.084 Uiso 1 1 calc R . . C8 C -0.0275(6) 0.1397(3) 0.5405(5) 0.0495(13) Uani 1 1 d . . . C9 C 0.0099(7) 0.1153(4) 0.6575(6) 0.0628(17) Uani 1 1 d . . . H9A H 0.0731 0.1391 0.7062 0.094 Uiso 1 1 calc R . . H9B H 0.0333 0.0734 0.6586 0.094 Uiso 1 1 calc R . . H9C H -0.0527 0.1177 0.6829 0.094 Uiso 1 1 calc R . . C10 C 0.0271(5) 0.1361(3) 0.4612(5) 0.0447(12) Uani 1 1 d . . . C11 C 0.1298(5) 0.1065(3) 0.4645(4) 0.0423(12) Uani 1 1 d . . . C12 C 0.1949(5) 0.0670(3) 0.5630(5) 0.0447(12) Uani 1 1 d . . . C13 C 0.2840(6) 0.0902(3) 0.6538(5) 0.0549(15) Uani 1 1 d . . . H13 H 0.3004 0.1318 0.6568 0.066 Uiso 1 1 calc R . . C14 C 0.3494(6) 0.0527(3) 0.7406(5) 0.0542(15) Uani 1 1 d . . . H14 H 0.4081 0.0695 0.8018 0.065 Uiso 1 1 calc R . . C15 C 0.3290(5) -0.0096(3) 0.7377(5) 0.0451(12) Uani 1 1 d . . . C16 C 0.2384(6) -0.0330(3) 0.6470(5) 0.0543(15) Uani 1 1 d . . . H16 H 0.2223 -0.0746 0.6438 0.065 Uiso 1 1 calc R . . C17 C 0.1711(6) 0.0054(3) 0.5602(5) 0.0530(14) Uani 1 1 d . . . H17 H 0.1100 -0.0107 0.5004 0.064 Uiso 1 1 calc R . . C18 C 0.4049(5) -0.0519(3) 0.8260(5) 0.0477(13) Uani 1 1 d . . . C19 C 0.5201(6) -0.0363(4) 0.8872(6) 0.0619(17) Uani 1 1 d . . . H19 H 0.5488 0.0010 0.8751 0.074 Uiso 1 1 calc R . . C20 C 0.5909(7) -0.0770(5) 0.9658(6) 0.072(2) Uani 1 1 d . . . H20 H 0.6672 -0.0668 1.0054 0.086 Uiso 1 1 calc R . . C21 C 0.5500(8) -0.1320(4) 0.9857(6) 0.074(2) Uani 1 1 d . . . H21 H 0.5980 -0.1587 1.0390 0.089 Uiso 1 1 calc R . . C22 C 0.4372(9) -0.1475(4) 0.9261(7) 0.074(2) Uani 1 1 d . . . H22 H 0.4088 -0.1848 0.9391 0.089 Uiso 1 1 calc R . . C23 C 0.3662(7) -0.1076(4) 0.8469(6) 0.0616(17) Uani 1 1 d . . . H23 H 0.2904 -0.1187 0.8068 0.074 Uiso 1 1 calc R . . C24 C 0.2727(6) 0.0822(4) 0.3913(5) 0.0589(17) Uani 1 1 d . . . C25 C 0.3716(7) 0.1156(5) 0.4222(7) 0.074(2) Uani 1 1 d . . . H25 H 0.3741 0.1556 0.4471 0.089 Uiso 1 1 calc R . . C26 C 0.4689(8) 0.0879(7) 0.4153(8) 0.095(3) Uani 1 1 d . . . H26 H 0.5368 0.1100 0.4349 0.114 Uiso 1 1 calc R . . C27 C 0.4650(10) 0.0279(7) 0.3794(9) 0.102(4) Uani 1 1 d . . . H27 H 0.5297 0.0101 0.3740 0.123 Uiso 1 1 calc R . . C28 C 0.3649(10) -0.0053(5) 0.3519(8) 0.092(3) Uani 1 1 d . . . H28 H 0.3627 -0.0458 0.3295 0.110 Uiso 1 1 calc R . . C29 C 0.2686(8) 0.0215(4) 0.3577(6) 0.0674(19) Uani 1 1 d . . . H29 H 0.2010 -0.0008 0.3392 0.081 Uiso 1 1 calc R . . C30 C 0.2060(6) 0.1857(3) 0.1342(5) 0.0526(14) Uani 1 1 d . . . C31 C 0.2049(6) 0.1235(3) 0.1503(5) 0.0529(14) Uani 1 1 d . . . H31 H 0.2739 0.1023 0.1784 0.064 Uiso 1 1 calc R . . C32 C 0.1012(6) 0.0914(3) 0.1251(5) 0.0479(13) Uani 1 1 d . . . H32 H 0.1036 0.0496 0.1385 0.057 Uiso 1 1 calc R . . C33 C -0.0059(6) 0.1208(3) 0.0803(5) 0.0488(13) Uani 1 1 d . . . C34 C -0.0041(6) 0.1861(3) 0.0610(5) 0.0499(14) Uani 1 1 d . . . H34 H -0.0729 0.2073 0.0301 0.060 Uiso 1 1 calc R . . C35 C 0.0994(6) 0.2174(3) 0.0882(5) 0.0536(14) Uani 1 1 d . . . H35 H 0.0989 0.2593 0.0762 0.064 Uiso 1 1 calc R . . C36 C 0.3175(7) 0.2202(4) 0.1684(7) 0.0698(19) Uani 1 1 d . . . H36A H 0.3786 0.1950 0.2168 0.105 Uiso 1 1 calc R . . H36B H 0.3124 0.2568 0.2073 0.105 Uiso 1 1 calc R . . H36C H 0.3327 0.2306 0.1028 0.105 Uiso 1 1 calc R . . C37 C -0.1194(6) 0.0904(4) 0.0589(7) 0.0637(17) Uani 1 1 d . . . H37 H -0.1661 0.1191 0.0821 0.076 Uiso 1 1 calc R . . C38 C -0.1808(9) 0.0802(5) -0.0679(9) 0.097(3) Uani 1 1 d . . . H38A H -0.1909 0.1187 -0.1061 0.145 Uiso 1 1 calc R . . H38B H -0.2544 0.0618 -0.0825 0.145 Uiso 1 1 calc R . . H38C H -0.1355 0.0536 -0.0942 0.145 Uiso 1 1 calc R . . C39 C -0.1114(9) 0.0319(5) 0.1242(9) 0.089(3) Uani 1 1 d . . . H39A H -0.0738 0.0011 0.0973 0.134 Uiso 1 1 calc R . . H39B H -0.1871 0.0183 0.1145 0.134 Uiso 1 1 calc R . . H39C H -0.0681 0.0393 0.2023 0.134 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 0.0456(3) 0.0398(2) 0.0336(2) 0.00162(15) 0.01182(17) 0.00543(17) Cl1 0.0901(12) 0.0558(8) 0.0517(8) -0.0125(7) 0.0185(8) -0.0095(9) O1 0.050(2) 0.065(2) 0.038(2) 0.0038(18) 0.0201(18) 0.022(2) N1 0.046(3) 0.052(3) 0.046(3) -0.003(2) 0.018(2) 0.000(2) N2 0.052(3) 0.060(3) 0.046(3) -0.004(2) 0.022(2) -0.009(2) N3 0.048(3) 0.045(2) 0.040(2) 0.0069(19) 0.014(2) 0.005(2) C1 0.045(3) 0.041(3) 0.037(3) -0.006(2) 0.010(2) -0.003(2) C2 0.041(3) 0.053(3) 0.054(3) -0.018(3) 0.014(3) 0.001(3) C3 0.057(4) 0.065(4) 0.064(4) -0.001(3) 0.023(3) 0.017(3) C4 0.073(5) 0.073(5) 0.063(4) 0.002(4) 0.016(4) 0.017(4) C5 0.050(4) 0.095(6) 0.074(5) -0.011(5) 0.002(4) 0.019(4) C6 0.040(3) 0.115(7) 0.085(6) -0.020(5) 0.016(4) 0.008(4) C7 0.048(4) 0.090(5) 0.070(5) -0.008(4) 0.021(3) -0.004(4) C8 0.057(3) 0.050(3) 0.043(3) -0.009(2) 0.020(3) -0.011(3) C9 0.076(5) 0.072(4) 0.041(3) 0.004(3) 0.023(3) -0.005(4) C10 0.051(3) 0.040(3) 0.039(3) -0.002(2) 0.013(2) -0.005(2) C11 0.047(3) 0.040(3) 0.034(2) 0.005(2) 0.008(2) -0.005(2) C12 0.049(3) 0.044(3) 0.037(3) 0.005(2) 0.012(2) 0.000(2) C13 0.068(4) 0.042(3) 0.042(3) 0.000(2) 0.007(3) -0.005(3) C14 0.062(4) 0.052(3) 0.036(3) 0.001(2) 0.003(3) -0.007(3) C15 0.044(3) 0.051(3) 0.036(3) 0.001(2) 0.011(2) -0.004(2) C16 0.056(3) 0.046(3) 0.049(3) 0.008(3) 0.005(3) -0.007(3) C17 0.048(3) 0.051(3) 0.046(3) 0.003(3) 0.001(3) -0.007(3) C18 0.049(3) 0.054(3) 0.038(3) 0.004(2) 0.013(2) 0.001(3) C19 0.054(4) 0.075(4) 0.047(3) 0.004(3) 0.006(3) -0.004(3) C20 0.056(4) 0.103(6) 0.044(3) -0.005(4) 0.004(3) 0.014(4) C21 0.085(6) 0.077(5) 0.046(4) 0.007(3) 0.010(4) 0.027(4) C22 0.092(6) 0.059(4) 0.059(4) 0.011(3) 0.016(4) 0.008(4) C23 0.062(4) 0.064(4) 0.050(3) 0.007(3) 0.011(3) 0.003(3) C24 0.056(4) 0.079(4) 0.040(3) 0.012(3) 0.016(3) 0.018(3) C25 0.052(4) 0.109(6) 0.053(4) 0.015(4) 0.010(3) 0.005(4) C26 0.054(4) 0.155(11) 0.070(5) 0.033(6) 0.017(4) 0.015(6) C27 0.082(7) 0.158(12) 0.070(5) 0.033(7) 0.033(5) 0.057(8) C28 0.109(8) 0.105(7) 0.065(5) 0.020(5) 0.036(5) 0.057(7) C29 0.077(5) 0.066(4) 0.056(4) 0.013(3) 0.022(4) 0.026(4) C30 0.057(4) 0.058(3) 0.044(3) 0.007(3) 0.020(3) -0.002(3) C31 0.047(3) 0.065(4) 0.046(3) 0.008(3) 0.016(3) 0.010(3) C32 0.062(4) 0.042(3) 0.044(3) -0.006(2) 0.025(3) 0.006(3) C33 0.053(3) 0.053(3) 0.039(3) -0.005(2) 0.015(2) 0.004(3) C34 0.056(3) 0.057(3) 0.032(2) 0.006(2) 0.011(2) 0.014(3) C35 0.068(4) 0.050(3) 0.045(3) 0.008(3) 0.024(3) 0.006(3) C36 0.065(4) 0.079(5) 0.070(5) 0.007(4) 0.030(4) -0.014(4) C37 0.053(4) 0.067(4) 0.065(4) -0.009(3) 0.014(3) -0.002(3) C38 0.079(6) 0.094(6) 0.082(6) -0.023(5) -0.011(5) -0.013(5) C39 0.081(6) 0.091(6) 0.093(6) 0.008(5) 0.030(5) -0.031(5) _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 O1 2.068(4) . ? Ru1 N3 2.130(5) . ? Ru1 C32 2.152(6) . ? Ru1 C31 2.178(7) . ? Ru1 C33 2.184(6) . ? Ru1 C34 2.188(6) . ? Ru1 C35 2.193(6) . ? Ru1 C30 2.199(6) . ? Ru1 Cl1 2.4122(16) . ? O1 C1 1.268(7) . ? N1 C1 1.359(8) . ? N1 N2 1.399(8) . ? N1 C2 1.418(8) . ? N2 C8 1.311(9) . ? N3 C11 1.295(8) . ? N3 C24 1.444(9) . ? C1 C10 1.419(8) . ? C2 C3 1.385(11) . ? C2 C7 1.388(10) . ? C3 C4 1.396(11) . ? C3 H3 0.9300 . ? C4 C5 1.359(14) . ? C4 H4 0.9300 . ? C5 C6 1.370(15) . ? C5 H5 0.9300 . ? C6 C7 1.391(13) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.429(9) . ? C8 C9 1.497(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.431(9) . ? C11 C12 1.497(7) . ? C12 C13 1.377(9) . ? C12 C17 1.378(9) . ? C13 C14 1.382(9) . ? C13 H13 0.9300 . ? C14 C15 1.384(9) . ? C14 H14 0.9300 . ? C15 C16 1.387(9) . ? C15 C18 1.498(8) . ? C16 C17 1.400(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.376(10) . ? C18 C19 1.407(10) . ? C19 C20 1.390(11) . ? C19 H19 0.9300 . ? C20 C21 1.370(14) . ? C20 H20 0.9300 . ? C21 C22 1.378(14) . ? C21 H21 0.9300 . ? C22 C23 1.385(11) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.366(12) . ? C24 C29 1.393(12) . ? C25 C26 1.396(14) . ? C25 H25 0.9300 . ? C26 C27 1.386(19) . ? C26 H26 0.9300 . ? C27 C28 1.379(19) . ? C27 H27 0.9300 . ? C28 C29 1.372(13) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.376(10) . ? C30 C35 1.426(10) . ? C30 C36 1.506(10) . ? C31 C32 1.408(10) . ? C31 H31 0.9300 . ? C32 C33 1.406(9) . ? C32 H32 0.9300 . ? C33 C34 1.452(9) . ? C33 C37 1.504(10) . ? C34 C35 1.395(10) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C39 1.513(13) . ? C37 C38 1.537(12) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? 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 O1 Ru1 N3 87.45(18) . . ? O1 Ru1 C32 119.4(2) . . ? N3 Ru1 C32 95.2(2) . . ? O1 Ru1 C31 157.0(2) . . ? N3 Ru1 C31 97.0(2) . . ? C32 Ru1 C31 37.9(3) . . ? O1 Ru1 C33 89.4(2) . . ? N3 Ru1 C33 118.7(2) . . ? C32 Ru1 C33 37.8(2) . . ? C31 Ru1 C33 68.6(2) . . ? O1 Ru1 C34 87.3(2) . . ? N3 Ru1 C34 156.9(2) . . ? C32 Ru1 C34 68.1(2) . . ? C31 Ru1 C34 79.8(2) . . ? C33 Ru1 C34 38.8(3) . . ? O1 Ru1 C35 112.4(2) . . ? N3 Ru1 C35 159.5(2) . . ? C32 Ru1 C35 80.1(2) . . ? C31 Ru1 C35 67.0(2) . . ? C33 Ru1 C35 68.9(3) . . ? C34 Ru1 C35 37.1(3) . . ? O1 Ru1 C30 150.1(2) . . ? N3 Ru1 C30 121.9(2) . . ? C32 Ru1 C30 67.8(2) . . ? C31 Ru1 C30 36.6(3) . . ? C33 Ru1 C30 81.7(3) . . ? C34 Ru1 C30 67.9(3) . . ? C35 Ru1 C30 37.9(3) . . ? O1 Ru1 Cl1 85.05(15) . . ? N3 Ru1 Cl1 84.39(15) . . ? C32 Ru1 Cl1 155.56(19) . . ? C31 Ru1 Cl1 117.7(2) . . ? C33 Ru1 Cl1 156.05(18) . . ? C34 Ru1 Cl1 117.51(19) . . ? C35 Ru1 Cl1 91.75(19) . . ? C30 Ru1 Cl1 91.63(19) . . ? C1 O1 Ru1 123.8(4) . . ? C1 N1 N2 111.5(5) . . ? C1 N1 C2 129.1(5) . . ? N2 N1 C2 119.4(5) . . ? C8 N2 N1 105.4(5) . . ? C11 N3 C24 120.6(5) . . ? C11 N3 Ru1 129.6(4) . . ? C24 N3 Ru1 109.8(4) . . ? O1 C1 N1 121.8(5) . . ? O1 C1 C10 131.4(6) . . ? N1 C1 C10 106.7(5) . . ? C3 C2 C7 119.5(7) . . ? C3 C2 N1 121.3(6) . . ? C7 C2 N1 119.1(7) . . ? C2 C3 C4 119.9(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.7(9) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.3(8) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C7 121.7(8) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C2 C7 C6 118.9(9) . . ? C2 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? N2 C8 C10 112.5(6) . . ? N2 C8 C9 117.3(6) . . ? C10 C8 C9 130.1(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 C8 103.9(5) . . ? C1 C10 C11 123.8(5) . . ? C8 C10 C11 132.3(6) . . ? N3 C11 C10 122.1(5) . . ? N3 C11 C12 118.7(5) . . ? C10 C11 C12 119.2(5) . . ? C13 C12 C17 118.8(5) . . ? C13 C12 C11 121.2(5) . . ? C17 C12 C11 119.8(5) . . ? C12 C13 C14 121.0(6) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 118.1(6) . . ? C14 C15 C18 121.9(5) . . ? C16 C15 C18 120.0(6) . . ? C15 C16 C17 120.7(6) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C12 C17 C16 120.4(6) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C23 C18 C19 118.1(6) . . ? C23 C18 C15 121.5(6) . . ? C19 C18 C15 120.3(6) . . ? C20 C19 C18 119.8(7) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 121.0(8) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.5(7) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 120.0(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 121.6(8) . . ? C18 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C29 121.5(8) . . ? C25 C24 N3 118.4(8) . . ? C29 C24 N3 119.8(7) . . ? C24 C25 C26 118.3(10) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C27 C26 C25 120.5(11) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 119.9(9) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 120.1(11) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 119.5(10) . . ? C28 C29 H29 120.2 . . ? C24 C29 H29 120.2 . . ? C31 C30 C35 118.8(6) . . ? C31 C30 C36 120.8(7) . . ? C35 C30 C36 120.4(6) . . ? C31 C30 Ru1 70.9(4) . . ? C35 C30 Ru1 70.8(4) . . ? C36 C30 Ru1 128.2(5) . . ? C30 C31 C32 121.3(6) . . ? C30 C31 Ru1 72.5(4) . . ? C32 C31 Ru1 70.0(3) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? Ru1 C31 H31 131.0 . . ? C33 C32 C31 121.9(6) . . ? C33 C32 Ru1 72.4(3) . . ? C31 C32 Ru1 72.1(4) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? Ru1 C32 H32 129.0 . . ? C32 C33 C34 116.5(6) . . ? C32 C33 C37 124.8(6) . . ? C34 C33 C37 118.5(6) . . ? C32 C33 Ru1 69.8(3) . . ? C34 C33 Ru1 70.7(3) . . ? C37 C33 Ru1 126.4(5) . . ? C35 C34 C33 120.8(6) . . ? C35 C34 Ru1 71.6(4) . . ? C33 C34 Ru1 70.5(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? Ru1 C34 H34 131.1 . . ? C34 C35 C30 120.6(6) . . ? C34 C35 Ru1 71.2(3) . . ? C30 C35 Ru1 71.3(3) . . ? C34 C35 H35 119.7 . . ? C30 C35 H35 119.7 . . ? Ru1 C35 H35 130.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 C39 114.2(7) . . ? C33 C37 C38 108.9(7) . . ? C39 C37 C38 111.6(8) . . ? C33 C37 H37 107.2 . . ? C39 C37 H37 107.2 . . ? C38 C37 H37 107.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? 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 N3 Ru1 O1 C1 14.4(5) . . . . ? C32 Ru1 O1 C1 108.9(5) . . . . ? C31 Ru1 O1 C1 116.4(6) . . . . ? C33 Ru1 O1 C1 133.1(5) . . . . ? C34 Ru1 O1 C1 171.9(5) . . . . ? C35 Ru1 O1 C1 -160.1(5) . . . . ? C30 Ru1 O1 C1 -154.9(5) . . . . ? Cl1 Ru1 O1 C1 -70.2(5) . . . . ? C1 N1 N2 C8 0.3(7) . . . . ? C2 N1 N2 C8 -176.0(5) . . . . ? O1 Ru1 N3 C11 -8.3(5) . . . . ? C32 Ru1 N3 C11 -127.6(5) . . . . ? C31 Ru1 N3 C11 -165.7(6) . . . . ? C33 Ru1 N3 C11 -96.3(6) . . . . ? C34 Ru1 N3 C11 -85.4(8) . . . . ? C35 Ru1 N3 C11 156.9(6) . . . . ? C30 Ru1 N3 C11 165.4(5) . . . . ? Cl1 Ru1 N3 C11 76.9(5) . . . . ? O1 Ru1 N3 C24 172.7(5) . . . . ? C32 Ru1 N3 C24 53.4(5) . . . . ? C31 Ru1 N3 C24 15.3(5) . . . . ? C33 Ru1 N3 C24 84.7(5) . . . . ? C34 Ru1 N3 C24 95.7(7) . . . . ? C35 Ru1 N3 C24 -22.1(9) . . . . ? C30 Ru1 N3 C24 -13.6(5) . . . . ? Cl1 Ru1 N3 C24 -102.1(5) . . . . ? Ru1 O1 C1 N1 167.6(4) . . . . ? Ru1 O1 C1 C10 -15.6(9) . . . . ? N2 N1 C1 O1 177.1(5) . . . . ? C2 N1 C1 O1 -7.1(9) . . . . ? N2 N1 C1 C10 -0.4(6) . . . . ? C2 N1 C1 C10 175.5(6) . . . . ? C1 N1 C2 C3 -13.4(10) . . . . ? N2 N1 C2 C3 162.2(6) . . . . ? C1 N1 C2 C7 168.4(7) . . . . ? N2 N1 C2 C7 -16.0(9) . . . . ? C7 C2 C3 C4 -2.1(11) . . . . ? N1 C2 C3 C4 179.7(7) . . . . ? C2 C3 C4 C5 1.6(13) . . . . ? C3 C4 C5 C6 -0.3(14) . . . . ? C4 C5 C6 C7 -0.7(15) . . . . ? C3 C2 C7 C6 1.2(11) . . . . ? N1 C2 C7 C6 179.4(7) . . . . ? C5 C6 C7 C2 0.2(14) . . . . ? N1 N2 C8 C10 -0.1(7) . . . . ? N1 N2 C8 C9 176.3(6) . . . . ? O1 C1 C10 C8 -176.8(6) . . . . ? N1 C1 C10 C8 0.3(6) . . . . ? O1 C1 C10 C11 3.9(10) . . . . ? N1 C1 C10 C11 -179.0(5) . . . . ? N2 C8 C10 C1 -0.1(7) . . . . ? C9 C8 C10 C1 -175.9(7) . . . . ? N2 C8 C10 C11 179.1(6) . . . . ? C9 C8 C10 C11 3.2(11) . . . . ? C24 N3 C11 C10 -180.0(6) . . . . ? Ru1 N3 C11 C10 1.1(9) . . . . ? C24 N3 C11 C12 0.2(9) . . . . ? Ru1 N3 C11 C12 -178.7(4) . . . . ? C1 C10 C11 N3 4.3(9) . . . . ? C8 C10 C11 N3 -174.8(6) . . . . ? C1 C10 C11 C12 -175.9(5) . . . . ? C8 C10 C11 C12 5.0(9) . . . . ? N3 C11 C12 C13 86.4(8) . . . . ? C10 C11 C12 C13 -93.4(8) . . . . ? N3 C11 C12 C17 -89.1(8) . . . . ? C10 C11 C12 C17 91.1(7) . . . . ? C17 C12 C13 C14 0.5(11) . . . . ? C11 C12 C13 C14 -175.0(7) . . . . ? C12 C13 C14 C15 1.4(12) . . . . ? C13 C14 C15 C16 -2.1(11) . . . . ? C13 C14 C15 C18 174.8(7) . . . . ? C14 C15 C16 C17 1.0(11) . . . . ? C18 C15 C16 C17 -176.0(6) . . . . ? C13 C12 C17 C16 -1.7(11) . . . . ? C11 C12 C17 C16 174.0(6) . . . . ? C15 C16 C17 C12 0.9(11) . . . . ? C14 C15 C18 C23 157.0(7) . . . . ? C16 C15 C18 C23 -26.1(10) . . . . ? C14 C15 C18 C19 -25.5(10) . . . . ? C16 C15 C18 C19 151.3(7) . . . . ? C23 C18 C19 C20 0.1(11) . . . . ? C15 C18 C19 C20 -177.4(6) . . . . ? C18 C19 C20 C21 -0.7(12) . . . . ? C19 C20 C21 C22 0.7(13) . . . . ? C20 C21 C22 C23 -0.1(14) . . . . ? C19 C18 C23 C22 0.5(11) . . . . ? C15 C18 C23 C22 178.0(7) . . . . ? C21 C22 C23 C18 -0.5(13) . . . . ? C11 N3 C24 C25 -102.0(8) . . . . ? Ru1 N3 C24 C25 77.1(7) . . . . ? C11 N3 C24 C29 83.0(8) . . . . ? Ru1 N3 C24 C29 -97.9(6) . . . . ? C29 C24 C25 C26 2.4(11) . . . . ? N3 C24 C25 C26 -172.5(7) . . . . ? C24 C25 C26 C27 -0.9(13) . . . . ? C25 C26 C27 C28 -1.0(15) . . . . ? C26 C27 C28 C29 1.4(14) . . . . ? C27 C28 C29 C24 0.0(12) . . . . ? C25 C24 C29 C28 -2.0(11) . . . . ? N3 C24 C29 C28 172.8(7) . . . . ? O1 Ru1 C30 C31 -139.2(5) . . . . ? N3 Ru1 C30 C31 53.5(5) . . . . ? C32 Ru1 C30 C31 -28.6(4) . . . . ? C33 Ru1 C30 C31 -65.2(4) . . . . ? C34 Ru1 C30 C31 -103.0(4) . . . . ? C35 Ru1 C30 C31 -131.3(6) . . . . ? Cl1 Ru1 C30 C31 137.9(4) . . . . ? O1 Ru1 C30 C35 -7.9(7) . . . . ? N3 Ru1 C30 C35 -175.2(4) . . . . ? C32 Ru1 C30 C35 102.8(4) . . . . ? C31 Ru1 C30 C35 131.3(6) . . . . ? C33 Ru1 C30 C35 66.2(4) . . . . ? C34 Ru1 C30 C35 28.4(4) . . . . ? Cl1 Ru1 C30 C35 -90.8(4) . . . . ? O1 Ru1 C30 C36 106.2(7) . . . . ? N3 Ru1 C30 C36 -61.1(7) . . . . ? C32 Ru1 C30 C36 -143.2(7) . . . . ? C31 Ru1 C30 C36 -114.6(8) . . . . ? C33 Ru1 C30 C36 -179.8(7) . . . . ? C34 Ru1 C30 C36 142.4(7) . . . . ? C35 Ru1 C30 C36 114.0(8) . . . . ? Cl1 Ru1 C30 C36 23.3(7) . . . . ? C35 C30 C31 C32 -1.7(10) . . . . ? C36 C30 C31 C32 176.1(6) . . . . ? Ru1 C30 C31 C32 52.3(5) . . . . ? C35 C30 C31 Ru1 -54.0(5) . . . . ? C36 C30 C31 Ru1 123.7(6) . . . . ? O1 Ru1 C31 C30 123.4(6) . . . . ? N3 Ru1 C31 C30 -136.5(4) . . . . ? C32 Ru1 C31 C30 134.0(6) . . . . ? C33 Ru1 C31 C30 105.4(4) . . . . ? C34 Ru1 C31 C30 66.6(4) . . . . ? C35 Ru1 C31 C30 30.1(4) . . . . ? Cl1 Ru1 C31 C30 -49.2(4) . . . . ? O1 Ru1 C31 C32 -10.6(7) . . . . ? N3 Ru1 C31 C32 89.5(4) . . . . ? C33 Ru1 C31 C32 -28.6(4) . . . . ? C34 Ru1 C31 C32 -67.4(4) . . . . ? C35 Ru1 C31 C32 -103.9(4) . . . . ? C30 Ru1 C31 C32 -134.0(6) . . . . ? Cl1 Ru1 C31 C32 176.8(3) . . . . ? C30 C31 C32 C33 1.3(9) . . . . ? Ru1 C31 C32 C33 54.8(5) . . . . ? C30 C31 C32 Ru1 -53.4(6) . . . . ? O1 Ru1 C32 C33 41.9(4) . . . . ? N3 Ru1 C32 C33 131.9(4) . . . . ? C31 Ru1 C32 C33 -133.3(5) . . . . ? C34 Ru1 C32 C33 -31.5(4) . . . . ? C35 Ru1 C32 C33 -68.2(4) . . . . ? C30 Ru1 C32 C33 -105.7(4) . . . . ? Cl1 Ru1 C32 C33 -140.2(4) . . . . ? O1 Ru1 C32 C31 175.3(3) . . . . ? N3 Ru1 C32 C31 -94.7(4) . . . . ? C33 Ru1 C32 C31 133.3(5) . . . . ? C34 Ru1 C32 C31 101.8(4) . . . . ? C35 Ru1 C32 C31 65.1(4) . . . . ? C30 Ru1 C32 C31 27.6(4) . . . . ? Cl1 Ru1 C32 C31 -6.8(6) . . . . ? C31 C32 C33 C34 0.2(8) . . . . ? Ru1 C32 C33 C34 54.8(5) . . . . ? C31 C32 C33 C37 -175.5(6) . . . . ? Ru1 C32 C33 C37 -120.9(6) . . . . ? C31 C32 C33 Ru1 -54.6(5) . . . . ? O1 Ru1 C33 C32 -144.4(4) . . . . ? N3 Ru1 C33 C32 -57.6(4) . . . . ? C31 Ru1 C33 C32 28.7(4) . . . . ? C34 Ru1 C33 C32 129.2(6) . . . . ? C35 Ru1 C33 C32 101.3(4) . . . . ? C30 Ru1 C33 C32 64.3(4) . . . . ? Cl1 Ru1 C33 C32 139.2(4) . . . . ? O1 Ru1 C33 C34 86.4(4) . . . . ? N3 Ru1 C33 C34 173.2(3) . . . . ? C32 Ru1 C33 C34 -129.2(6) . . . . ? C31 Ru1 C33 C34 -100.5(4) . . . . ? C35 Ru1 C33 C34 -27.9(4) . . . . ? C30 Ru1 C33 C34 -65.0(4) . . . . ? Cl1 Ru1 C33 C34 10.0(7) . . . . ? O1 Ru1 C33 C37 -25.4(6) . . . . ? N3 Ru1 C33 C37 61.4(6) . . . . ? C32 Ru1 C33 C37 119.0(7) . . . . ? C31 Ru1 C33 C37 147.7(7) . . . . ? C34 Ru1 C33 C37 -111.8(7) . . . . ? C35 Ru1 C33 C37 -139.7(7) . . . . ? C30 Ru1 C33 C37 -176.7(6) . . . . ? Cl1 Ru1 C33 C37 -101.8(7) . . . . ? C32 C33 C34 C35 -1.3(8) . . . . ? C37 C33 C34 C35 174.7(6) . . . . ? Ru1 C33 C34 C35 53.1(5) . . . . ? C32 C33 C34 Ru1 -54.3(5) . . . . ? C37 C33 C34 Ru1 121.6(6) . . . . ? O1 Ru1 C34 C35 133.9(4) . . . . ? N3 Ru1 C34 C35 -149.1(5) . . . . ? C32 Ru1 C34 C35 -102.9(4) . . . . ? C31 Ru1 C34 C35 -65.2(4) . . . . ? C33 Ru1 C34 C35 -133.7(6) . . . . ? C30 Ru1 C34 C35 -28.9(4) . . . . ? Cl1 Ru1 C34 C35 50.9(4) . . . . ? O1 Ru1 C34 C33 -92.4(4) . . . . ? N3 Ru1 C34 C33 -15.4(8) . . . . ? C32 Ru1 C34 C33 30.8(4) . . . . ? C31 Ru1 C34 C33 68.5(4) . . . . ? C35 Ru1 C34 C33 133.7(6) . . . . ? C30 Ru1 C34 C33 104.7(4) . . . . ? Cl1 Ru1 C34 C33 -175.4(3) . . . . ? C33 C34 C35 C30 0.9(9) . . . . ? Ru1 C34 C35 C30 53.5(5) . . . . ? C33 C34 C35 Ru1 -52.6(5) . . . . ? C31 C30 C35 C34 0.6(9) . . . . ? C36 C30 C35 C34 -177.2(6) . . . . ? Ru1 C30 C35 C34 -53.4(5) . . . . ? C31 C30 C35 Ru1 54.0(5) . . . . ? C36 C30 C35 Ru1 -123.7(6) . . . . ? O1 Ru1 C35 C34 -51.1(4) . . . . ? N3 Ru1 C35 C34 144.9(6) . . . . ? C32 Ru1 C35 C34 66.7(4) . . . . ? C31 Ru1 C35 C34 104.0(4) . . . . ? C33 Ru1 C35 C34 29.1(4) . . . . ? C30 Ru1 C35 C34 133.1(6) . . . . ? Cl1 Ru1 C35 C34 -136.5(4) . . . . ? O1 Ru1 C35 C30 175.8(4) . . . . ? N3 Ru1 C35 C30 11.8(9) . . . . ? C32 Ru1 C35 C30 -66.4(4) . . . . ? C31 Ru1 C35 C30 -29.1(4) . . . . ? C33 Ru1 C35 C30 -104.1(4) . . . . ? C34 Ru1 C35 C30 -133.1(6) . . . . ? Cl1 Ru1 C35 C30 90.4(4) . . . . ? C32 C33 C37 C39 20.1(11) . . . . ? C34 C33 C37 C39 -155.5(7) . . . . ? Ru1 C33 C37 C39 -69.3(9) . . . . ? C32 C33 C37 C38 -105.5(8) . . . . ? C34 C33 C37 C38 78.9(8) . . . . ? Ru1 C33 C37 C38 165.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.886 _refine_diff_density_min -1.569 _refine_diff_density_rms 0.119 _iucr_refine_instructions_details ; TITL CC5 in P2(1)/c CELL 1.54178 12.576996 21.874847 12.861897 90.0000 111.9988 90.0000 ZERR 4.00 0.000427 0.000445 0.000350 0.0000 0.0036 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL RU UNIT 156 144 12 4 4 4 REM ------------------------------------------------------------------------- REM Data measured on the SUPERNOVA REM Crystal colour: orange; Crystal habit: prismatic REM ------------------------------------------------------------------------- L.S. 10 ACTA 134 OMIT -10 15 10 OMIT -10 16 9 OMIT -9 19 9 OMIT -9 20 8 OMIT -1 0 4 OMIT 6 0 2 OMIT -8 21 7 OMIT -9 15 10 OMIT -9 17 9 OMIT -8 17 11 OMIT -8 19 10 OMIT -9 18 9 OMIT -10 17 8 OMIT -8 21 8 OMIT -8 19 9 OMIT 1 0 6 FMAP 2 SIZE 0.1550 0.1227 0.0988 CONF BOND $H WPDB -2 PLAN 10 WGHT 0.090200 7.170700 FVAR 2.75277 RU1 6 0.102917 0.165677 0.235468 11.00000 0.04564 0.03984 = 0.03360 0.00162 0.01182 0.00543 CL1 5 0.185549 0.250929 0.358129 11.00000 0.09011 0.05575 = 0.05174 -0.01247 0.01853 -0.00955 O1 4 -0.040373 0.181715 0.273657 11.00000 0.05048 0.06512 = 0.03807 0.00379 0.02008 0.02232 N1 3 -0.131814 0.192617 0.397107 11.00000 0.04585 0.05241 = 0.04609 -0.00343 0.01846 -0.00007 N2 3 -0.121218 0.172784 0.503944 11.00000 0.05244 0.06021 = 0.04645 -0.00375 0.02199 -0.00912 N3 3 0.168717 0.112803 0.385154 11.00000 0.04813 0.04493 = 0.03969 0.00695 0.01366 0.00531 C1 1 -0.044782 0.171243 0.368906 11.00000 0.04488 0.04056 = 0.03713 -0.00581 0.00992 -0.00266 C2 1 -0.221991 0.233149 0.337155 11.00000 0.04066 0.05306 = 0.05374 -0.01814 0.01386 0.00146 C3 1 -0.218872 0.266878 0.247185 11.00000 0.05740 0.06462 = 0.06390 -0.00060 0.02330 0.01722 AFIX 43 H3 2 -0.156671 0.263345 0.225116 11.00000 -1.20000 AFIX 0 C4 1 -0.309277 0.306180 0.189711 11.00000 0.07318 0.07277 = 0.06305 0.00200 0.01615 0.01718 AFIX 43 H4 2 -0.307829 0.327958 0.128156 11.00000 -1.20000 AFIX 0 C5 1 -0.399411 0.312972 0.222727 11.00000 0.05009 0.09498 = 0.07439 -0.01118 0.00217 0.01880 AFIX 43 H5 2 -0.459269 0.339340 0.184312 11.00000 -1.20000 AFIX 0 C6 1 -0.401079 0.280547 0.313201 11.00000 0.04032 0.11532 = 0.08508 -0.01987 0.01568 0.00848 AFIX 43 H6 2 -0.462409 0.285572 0.336158 11.00000 -1.20000 AFIX 0 C7 1 -0.313446 0.240308 0.371620 11.00000 0.04774 0.08993 = 0.07022 -0.00803 0.02069 -0.00385 AFIX 43 H7 2 -0.316079 0.218564 0.432744 11.00000 -1.20000 AFIX 0 C8 1 -0.027497 0.139726 0.540493 11.00000 0.05663 0.04968 = 0.04344 -0.00875 0.02002 -0.01102 C9 1 0.009907 0.115295 0.657533 11.00000 0.07626 0.07224 = 0.04072 0.00426 0.02296 -0.00533 AFIX 33 H9A 2 0.073123 0.139080 0.706175 11.00000 -1.50000 H9B 2 0.033272 0.073448 0.658553 11.00000 -1.50000 H9C 2 -0.052696 0.117695 0.682900 11.00000 -1.50000 AFIX 0 C10 1 0.027084 0.136078 0.461162 11.00000 0.05146 0.03987 = 0.03897 -0.00213 0.01273 -0.00467 C11 1 0.129791 0.106483 0.464541 11.00000 0.04673 0.03988 = 0.03420 0.00523 0.00812 -0.00489 C12 1 0.194884 0.067025 0.562976 11.00000 0.04921 0.04425 = 0.03676 0.00505 0.01174 -0.00004 C13 1 0.283980 0.090203 0.653805 11.00000 0.06843 0.04183 = 0.04223 -0.00018 0.00672 -0.00489 AFIX 43 H13 2 0.300353 0.131774 0.656789 11.00000 -1.20000 AFIX 0 C14 1 0.349423 0.052654 0.740570 11.00000 0.06174 0.05200 = 0.03578 0.00079 0.00318 -0.00675 AFIX 43 H14 2 0.408084 0.069482 0.801812 11.00000 -1.20000 AFIX 0 C15 1 0.329014 -0.009622 0.737736 11.00000 0.04405 0.05107 = 0.03639 0.00141 0.01065 -0.00374 C16 1 0.238449 -0.032975 0.647027 11.00000 0.05556 0.04565 = 0.04873 0.00753 0.00450 -0.00671 AFIX 43 H16 2 0.222294 -0.074578 0.643820 11.00000 -1.20000 AFIX 0 C17 1 0.171081 0.005417 0.560228 11.00000 0.04819 0.05092 = 0.04589 0.00334 0.00149 -0.00691 AFIX 43 H17 2 0.109952 -0.010748 0.500409 11.00000 -1.20000 AFIX 0 C18 1 0.404916 -0.051879 0.826044 11.00000 0.04886 0.05357 = 0.03763 0.00384 0.01286 0.00050 C19 1 0.520122 -0.036334 0.887211 11.00000 0.05364 0.07470 = 0.04653 0.00370 0.00616 -0.00432 AFIX 43 H19 2 0.548814 0.001045 0.875135 11.00000 -1.20000 AFIX 0 C20 1 0.590890 -0.077048 0.965751 11.00000 0.05632 0.10269 = 0.04366 -0.00493 0.00363 0.01428 AFIX 43 H20 2 0.667203 -0.066787 1.005383 11.00000 -1.20000 AFIX 0 C21 1 0.549999 -0.132050 0.985698 11.00000 0.08537 0.07670 = 0.04647 0.00721 0.00955 0.02670 AFIX 43 H21 2 0.597954 -0.158728 1.039030 11.00000 -1.20000 AFIX 0 C22 1 0.437210 -0.147534 0.926087 11.00000 0.09233 0.05935 = 0.05901 0.01119 0.01596 0.00767 AFIX 43 H22 2 0.408819 -0.184808 0.939076 11.00000 -1.20000 AFIX 0 C23 1 0.366161 -0.107598 0.846861 11.00000 0.06235 0.06407 = 0.04957 0.00653 0.01075 0.00268 AFIX 43 H23 2 0.290402 -0.118717 0.806751 11.00000 -1.20000 AFIX 0 C24 1 0.272698 0.082234 0.391332 11.00000 0.05624 0.07852 = 0.04011 0.01218 0.01585 0.01822 C25 1 0.371610 0.115566 0.422172 11.00000 0.05226 0.10890 = 0.05313 0.01467 0.00961 0.00498 AFIX 43 H25 2 0.374111 0.155640 0.447126 11.00000 -1.20000 AFIX 0 C26 1 0.468857 0.087941 0.415276 11.00000 0.05423 0.15483 = 0.06971 0.03272 0.01681 0.01475 AFIX 43 H26 2 0.536795 0.109991 0.434887 11.00000 -1.20000 AFIX 0 C27 1 0.464953 0.027937 0.379450 11.00000 0.08179 0.15848 = 0.07019 0.03348 0.03313 0.05730 AFIX 43 H27 2 0.529742 0.010068 0.373957 11.00000 -1.20000 AFIX 0 C28 1 0.364904 -0.005254 0.351948 11.00000 0.10937 0.10514 = 0.06472 0.02009 0.03648 0.05727 AFIX 43 H28 2 0.362737 -0.045800 0.329494 11.00000 -1.20000 AFIX 0 C29 1 0.268592 0.021476 0.357681 11.00000 0.07703 0.06598 = 0.05639 0.01274 0.02170 0.02643 AFIX 43 H29 2 0.201035 -0.000812 0.339229 11.00000 -1.20000 AFIX 0 C30 1 0.206008 0.185677 0.134211 11.00000 0.05691 0.05825 = 0.04386 0.00685 0.02013 -0.00227 C31 1 0.204878 0.123545 0.150345 11.00000 0.04665 0.06508 = 0.04592 0.00764 0.01607 0.00983 AFIX 43 H31 2 0.273937 0.102346 0.178448 11.00000 -1.20000 AFIX 0 C32 1 0.101194 0.091432 0.125134 11.00000 0.06221 0.04184 = 0.04427 -0.00592 0.02537 0.00576 AFIX 43 H32 2 0.103607 0.049576 0.138508 11.00000 -1.20000 AFIX 0 C33 1 -0.005856 0.120781 0.080342 11.00000 0.05278 0.05265 = 0.03913 -0.00502 0.01521 0.00433 C34 1 -0.004140 0.186106 0.060981 11.00000 0.05609 0.05702 = 0.03160 0.00602 0.01061 0.01448 AFIX 43 H34 2 -0.072935 0.207347 0.030062 11.00000 -1.20000 AFIX 0 C35 1 0.099398 0.217389 0.088177 11.00000 0.06786 0.05004 = 0.04520 0.00839 0.02393 0.00575 AFIX 43 H35 2 0.098931 0.259331 0.076183 11.00000 -1.20000 AFIX 0 C36 1 0.317548 0.220171 0.168358 11.00000 0.06477 0.07871 = 0.07037 0.00749 0.03028 -0.01353 AFIX 33 H36A 2 0.378585 0.195038 0.216820 11.00000 -1.50000 H36B 2 0.312423 0.256824 0.207268 11.00000 -1.50000 H36C 2 0.332728 0.230637 0.102752 11.00000 -1.50000 AFIX 0 C37 1 -0.119413 0.090396 0.058907 11.00000 0.05284 0.06656 = 0.06500 -0.00894 0.01438 -0.00202 AFIX 13 H37 2 -0.166071 0.119143 0.082135 11.00000 -1.20000 AFIX 0 C38 1 -0.180816 0.080187 -0.067884 11.00000 0.07869 0.09389 = 0.08226 -0.02335 -0.01100 -0.01301 AFIX 33 H38A 2 -0.190943 0.118723 -0.106108 11.00000 -1.50000 H38B 2 -0.254361 0.061838 -0.082542 11.00000 -1.50000 H38C 2 -0.135497 0.053624 -0.094200 11.00000 -1.50000 AFIX 0 C39 1 -0.111362 0.031928 0.124217 11.00000 0.08134 0.09088 = 0.09335 0.00783 0.03033 -0.03096 AFIX 33 H39A 2 -0.073792 0.001081 0.097255 11.00000 -1.50000 H39B 2 -0.187055 0.018313 0.114520 11.00000 -1.50000 H39C 2 -0.068127 0.039283 0.202327 11.00000 -1.50000 HKLF 4 REM CC5 in P2(1)/c REM R1 = 0.0659 for 4864 Fo > 4sig(Fo) and 0.0913 for all 6266 data REM 406 parameters refined using 0 restraints END WGHT 0.0903 7.1553 REM Highest difference peak 1.886, deepest hole -1.569, 1-sigma level 0.119 Q1 1 0.0553 0.1355 0.2402 11.00000 0.05 1.89 Q2 1 0.1420 0.1987 0.2222 11.00000 0.05 1.71 Q3 1 0.1560 0.1379 0.2310 11.00000 0.05 1.67 Q4 1 0.0597 0.1951 0.2433 11.00000 0.05 1.57 Q5 1 0.1907 0.1556 0.2604 11.00000 0.05 1.02 Q6 1 0.1351 0.2083 0.3456 11.00000 0.05 0.87 Q7 1 0.0018 0.1653 0.2041 11.00000 0.05 0.85 Q8 1 0.0772 0.1226 0.1351 11.00000 0.05 0.81 Q9 1 0.0808 0.2069 0.1376 11.00000 0.05 0.74 Q10 1 0.1468 0.1294 0.3487 11.00000 0.05 0.67 ; data_4 _audit_update_record ; 2013-02-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H38 Cl N3 O Ru' _chemical_formula_sum 'C43 H38 Cl N3 O Ru' _chemical_formula_weight 749.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 25.616(4) _cell_length_b 22.8086(14) _cell_length_c 12.793(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.701(10) _cell_angle_gamma 90.00 _cell_volume 6944.5(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 505 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6850 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS 2008, Bruker AXS, 2008' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49475 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10034 _reflns_number_gt 8147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+42.8967P] 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 10034 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.184377(9) 0.414674(10) 0.245344(18) 0.01332(6) Uani 1 1 d . . . Cl1 Cl 0.14987(3) 0.49555(3) 0.11554(6) 0.02143(15) Uani 1 1 d . . . O1 O 0.25631(8) 0.42490(9) 0.20900(16) 0.0145(4) Uani 1 1 d . . . N1 N 0.29527(10) 0.44063(10) 0.07479(19) 0.0123(4) Uani 1 1 d . . . N2 N 0.28904(10) 0.42158(11) -0.03331(19) 0.0139(5) Uani 1 1 d . . . N3 N 0.15291(10) 0.35740(12) 0.1022(2) 0.0170(5) Uani 1 1 d . . . C1 C 0.25498(11) 0.41708(12) 0.1089(2) 0.0119(5) Uani 1 1 d . . . C2 C 0.33753(11) 0.48206(12) 0.1327(2) 0.0119(5) Uani 1 1 d . . . C3 C 0.33079(12) 0.51869(13) 0.2142(2) 0.0149(5) Uani 1 1 d . . . H3 H 0.2979 0.5163 0.2317 0.018 Uiso 1 1 calc R . . C4 C 0.37329(12) 0.55894(13) 0.2698(3) 0.0178(6) Uani 1 1 d . . . H4 H 0.3695 0.5837 0.3262 0.021 Uiso 1 1 calc R . . C5 C 0.42124(12) 0.56292(14) 0.2428(3) 0.0184(6) Uani 1 1 d . . . H5 H 0.4499 0.5904 0.2807 0.022 Uiso 1 1 calc R . . C6 C 0.42686(13) 0.52691(15) 0.1610(3) 0.0223(6) Uani 1 1 d . . . H6 H 0.4594 0.5299 0.1424 0.027 Uiso 1 1 calc R . . C7 C 0.38507(12) 0.48601(14) 0.1050(3) 0.0182(6) Uani 1 1 d . . . H7 H 0.3891 0.4613 0.0487 0.022 Uiso 1 1 calc R . . C8 C 0.24428(12) 0.38705(12) -0.0663(2) 0.0135(5) Uani 1 1 d . . . C9 C 0.22563(14) 0.36142(15) -0.1827(2) 0.0213(6) Uani 1 1 d . . . H9A H 0.2533 0.3708 -0.2163 0.032 Uiso 1 1 calc R . . H9B H 0.1891 0.3780 -0.2291 0.032 Uiso 1 1 calc R . . H9C H 0.2223 0.3188 -0.1784 0.032 Uiso 1 1 calc R . . C10 C 0.21993(11) 0.38216(12) 0.0188(2) 0.0118(5) Uani 1 1 d . . . C11 C 0.17254(12) 0.35052(13) 0.0214(2) 0.0143(5) Uani 1 1 d . . . C12 C 0.14551(12) 0.30607(13) -0.0696(2) 0.0150(5) Uani 1 1 d . . . C13 C 0.09900(12) 0.32124(13) -0.1654(2) 0.0164(5) Uani 1 1 d . . . H13 H 0.0847 0.3601 -0.1743 0.020 Uiso 1 1 calc R . . C14 C 0.07358(12) 0.27915(13) -0.2480(2) 0.0154(5) Uani 1 1 d . . . H14 H 0.0426 0.2900 -0.3136 0.018 Uiso 1 1 calc R . . C15 C 0.09294(12) 0.22129(13) -0.2356(2) 0.0145(5) Uani 1 1 d . . . C16 C 0.14025(12) 0.20709(13) -0.1392(2) 0.0166(6) Uani 1 1 d . . . H16 H 0.1545 0.1682 -0.1295 0.020 Uiso 1 1 calc R . . C17 C 0.16636(12) 0.24927(14) -0.0584(2) 0.0174(6) Uani 1 1 d . . . H17 H 0.1987 0.2392 0.0051 0.021 Uiso 1 1 calc R . . C18 C 0.06300(12) 0.17462(13) -0.3177(2) 0.0140(5) Uani 1 1 d . . . C19 C 0.09133(12) 0.12480(13) -0.3317(2) 0.0170(6) Uani 1 1 d . . . H19 H 0.1308 0.1218 -0.2928 0.020 Uiso 1 1 calc R . . C20 C 0.06225(14) 0.07930(14) -0.4024(3) 0.0210(6) Uani 1 1 d . . . H20 H 0.0820 0.0457 -0.4117 0.025 Uiso 1 1 calc R . . C21 C 0.00409(13) 0.08310(14) -0.4595(2) 0.0192(6) Uani 1 1 d . . . H21 H -0.0158 0.0520 -0.5068 0.023 Uiso 1 1 calc R . . C22 C -0.02420(12) 0.13251(14) -0.4467(2) 0.0179(6) Uani 1 1 d . . . H22 H -0.0637 0.1353 -0.4854 0.021 Uiso 1 1 calc R . . C23 C 0.00486(12) 0.17848(13) -0.3771(2) 0.0154(5) Uani 1 1 d . . . H23 H -0.0149 0.2126 -0.3701 0.019 Uiso 1 1 calc R . . C24 C 0.10867(13) 0.31821(14) 0.1044(2) 0.0178(6) Uani 1 1 d . . . C25 C 0.05201(12) 0.33816(14) 0.0636(2) 0.0190(6) Uani 1 1 d . . . C26 C 0.03610(13) 0.39483(15) 0.0105(3) 0.0213(6) Uani 1 1 d . . . H26 H 0.0637 0.4202 0.0022 0.026 Uiso 1 1 calc R . . C27 C -0.01932(13) 0.41150(15) -0.0277(3) 0.0225(6) Uani 1 1 d . . . H27 H -0.0298 0.4486 -0.0628 0.027 Uiso 1 1 calc R . . C28 C -0.06126(15) 0.37426(18) -0.0157(3) 0.0294(8) Uani 1 1 d . . . H28 H -0.0994 0.3866 -0.0431 0.035 Uiso 1 1 calc R . . C29 C -0.04715(14) 0.32146(17) 0.0343(3) 0.0269(7) Uani 1 1 d . . . H29 H -0.0756 0.2970 0.0417 0.032 Uiso 1 1 calc R . . C30 C 0.00916(13) 0.30199(14) 0.0756(2) 0.0188(6) Uani 1 1 d . . . C31 C 0.02496(15) 0.24619(16) 0.1297(3) 0.0255(7) Uani 1 1 d . . . H31 H -0.0029 0.2219 0.1398 0.031 Uiso 1 1 calc R . . C32 C 0.07961(14) 0.22727(15) 0.1671(3) 0.0231(6) Uani 1 1 d . . . H32 H 0.0894 0.1900 0.2021 0.028 Uiso 1 1 calc R . . C33 C 0.12153(14) 0.26357(14) 0.1532(3) 0.0210(6) Uani 1 1 d . . . H33 H 0.1592 0.2500 0.1781 0.025 Uiso 1 1 calc R . . C34 C 0.13213(13) 0.44018(15) 0.3414(2) 0.0203(6) Uani 1 1 d . . . C35 C 0.13272(13) 0.37874(14) 0.3330(2) 0.0189(6) Uani 1 1 d . . . H35 H 0.0982 0.3579 0.3051 0.023 Uiso 1 1 calc R . . C36 C 0.18457(13) 0.34701(14) 0.3659(2) 0.0195(6) Uani 1 1 d . . . H36 H 0.1838 0.3054 0.3607 0.023 Uiso 1 1 calc R . . C37 C 0.23670(13) 0.37638(14) 0.4057(2) 0.0173(6) Uani 1 1 d . . . C38 C 0.23588(13) 0.43938(14) 0.4169(2) 0.0166(6) Uani 1 1 d . . . H38 H 0.2704 0.4603 0.4458 0.020 Uiso 1 1 calc R . . C39 C 0.18501(13) 0.47016(14) 0.3859(2) 0.0185(6) Uani 1 1 d . . . H39 H 0.1856 0.5116 0.3944 0.022 Uiso 1 1 calc R . . C40 C 0.07821(14) 0.47466(17) 0.3017(3) 0.0271(7) Uani 1 1 d . . . H40A H 0.0486 0.4518 0.2454 0.041 Uiso 1 1 calc R . . H40B H 0.0838 0.5116 0.2681 0.041 Uiso 1 1 calc R . . H40C H 0.0671 0.4830 0.3657 0.041 Uiso 1 1 calc R . . C41 C 0.29256(13) 0.34517(15) 0.4315(3) 0.0211(6) Uani 1 1 d . . . H41 H 0.3196 0.3744 0.4221 0.025 Uiso 1 1 calc R . . C42 C 0.31557(17) 0.32552(18) 0.5547(3) 0.0342(8) Uani 1 1 d . . . H42A H 0.3197 0.3597 0.6036 0.051 Uiso 1 1 calc R . . H42B H 0.3523 0.3068 0.5721 0.051 Uiso 1 1 calc R . . H42C H 0.2895 0.2975 0.5673 0.051 Uiso 1 1 calc R . . C43 C 0.28959(15) 0.29348(16) 0.3520(3) 0.0277(7) Uani 1 1 d . . . H43A H 0.2679 0.2614 0.3672 0.042 Uiso 1 1 calc R . . H43B H 0.3277 0.2798 0.3645 0.042 Uiso 1 1 calc R . . H43C H 0.2713 0.3063 0.2738 0.042 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 0.01438(10) 0.01583(11) 0.01024(10) -0.00251(8) 0.00512(7) -0.00426(9) Cl1 0.0236(4) 0.0227(4) 0.0179(3) 0.0045(3) 0.0076(3) 0.0037(3) O1 0.0144(9) 0.0193(11) 0.0097(9) -0.0014(7) 0.0046(7) -0.0048(8) N1 0.0130(10) 0.0124(11) 0.0115(10) -0.0010(8) 0.0045(8) -0.0019(9) N2 0.0167(11) 0.0146(12) 0.0116(10) -0.0018(9) 0.0066(9) -0.0001(9) N3 0.0163(11) 0.0196(13) 0.0152(11) -0.0047(9) 0.0058(9) -0.0055(10) C1 0.0125(11) 0.0111(12) 0.0121(11) 0.0011(10) 0.0046(9) -0.0001(10) C2 0.0097(11) 0.0119(12) 0.0124(12) 0.0011(10) 0.0022(9) -0.0007(10) C3 0.0143(12) 0.0134(13) 0.0187(13) 0.0001(10) 0.0082(10) 0.0005(10) C4 0.0186(14) 0.0155(14) 0.0187(14) -0.0033(11) 0.0061(11) -0.0020(11) C5 0.0140(13) 0.0181(14) 0.0204(14) 0.0005(11) 0.0032(11) -0.0038(11) C6 0.0141(13) 0.0304(18) 0.0234(15) -0.0019(13) 0.0080(12) -0.0063(12) C7 0.0151(13) 0.0228(15) 0.0176(13) -0.0035(11) 0.0072(11) -0.0031(11) C8 0.0140(12) 0.0137(13) 0.0122(12) 0.0000(10) 0.0043(10) 0.0011(10) C9 0.0256(15) 0.0273(17) 0.0138(13) -0.0062(12) 0.0105(12) -0.0057(13) C10 0.0131(12) 0.0113(12) 0.0115(11) -0.0015(9) 0.0052(10) -0.0004(10) C11 0.0148(12) 0.0150(13) 0.0124(12) -0.0027(10) 0.0041(10) -0.0024(10) C12 0.0161(13) 0.0180(14) 0.0114(12) -0.0052(10) 0.0057(10) -0.0057(11) C13 0.0191(13) 0.0128(13) 0.0177(13) -0.0029(10) 0.0074(11) -0.0029(11) C14 0.0172(13) 0.0160(14) 0.0115(12) -0.0008(10) 0.0037(10) -0.0022(11) C15 0.0154(12) 0.0172(14) 0.0110(12) -0.0024(10) 0.0048(10) -0.0029(11) C16 0.0175(13) 0.0150(14) 0.0165(13) -0.0026(10) 0.0052(11) -0.0005(11) C17 0.0152(12) 0.0198(15) 0.0141(13) -0.0011(11) 0.0019(10) -0.0004(11) C18 0.0168(13) 0.0150(13) 0.0107(12) -0.0018(10) 0.0058(10) -0.0039(10) C19 0.0170(13) 0.0182(14) 0.0136(13) 0.0005(11) 0.0032(10) 0.0002(11) C20 0.0263(15) 0.0162(15) 0.0190(14) -0.0029(11) 0.0067(12) 0.0022(12) C21 0.0232(14) 0.0166(14) 0.0143(13) -0.0035(11) 0.0028(11) -0.0041(12) C22 0.0163(13) 0.0181(15) 0.0152(13) -0.0022(11) 0.0012(10) -0.0035(11) C23 0.0174(13) 0.0145(13) 0.0142(12) -0.0021(10) 0.0055(10) -0.0005(11) C24 0.0187(13) 0.0207(15) 0.0147(13) -0.0042(11) 0.0070(11) -0.0052(11) C25 0.0179(14) 0.0250(16) 0.0149(13) -0.0078(11) 0.0070(11) -0.0053(12) C26 0.0216(15) 0.0247(16) 0.0169(14) -0.0025(12) 0.0061(11) 0.0020(12) C27 0.0230(15) 0.0223(16) 0.0202(14) -0.0024(12) 0.0056(12) 0.0020(13) C28 0.0244(16) 0.040(2) 0.0245(17) -0.0068(15) 0.0093(13) 0.0000(15) C29 0.0199(15) 0.040(2) 0.0235(16) -0.0080(14) 0.0107(13) -0.0045(14) C30 0.0197(14) 0.0249(16) 0.0136(13) -0.0068(11) 0.0083(11) -0.0076(12) C31 0.0296(17) 0.0253(17) 0.0231(16) -0.0038(13) 0.0114(13) -0.0098(14) C32 0.0284(16) 0.0175(15) 0.0204(15) -0.0008(12) 0.0055(12) -0.0023(13) C33 0.0269(15) 0.0165(15) 0.0190(14) -0.0018(11) 0.0078(12) -0.0014(12) C34 0.0204(14) 0.0290(17) 0.0137(13) -0.0027(12) 0.0089(11) -0.0017(12) C35 0.0218(14) 0.0246(16) 0.0144(13) -0.0040(11) 0.0114(11) -0.0086(12) C36 0.0241(15) 0.0200(15) 0.0166(13) -0.0011(11) 0.0101(12) -0.0072(12) C37 0.0221(14) 0.0188(14) 0.0119(12) 0.0004(10) 0.0074(11) -0.0028(11) C38 0.0199(14) 0.0195(14) 0.0106(12) -0.0042(10) 0.0060(10) -0.0064(11) C39 0.0242(15) 0.0194(15) 0.0128(13) -0.0046(11) 0.0078(11) -0.0040(12) C40 0.0215(15) 0.040(2) 0.0220(16) -0.0039(14) 0.0102(13) 0.0023(14) C41 0.0197(14) 0.0232(16) 0.0191(14) 0.0017(12) 0.0057(12) -0.0014(12) C42 0.041(2) 0.031(2) 0.0229(17) 0.0030(14) 0.0033(15) 0.0085(16) C43 0.0299(17) 0.0248(17) 0.0329(18) -0.0035(14) 0.0168(15) 0.0010(14) _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 O1 2.073(2) . ? Ru1 N3 2.148(2) . ? Ru1 C37 2.176(3) . ? Ru1 C38 2.176(3) . ? Ru1 C36 2.180(3) . ? Ru1 C35 2.186(3) . ? Ru1 C39 2.193(3) . ? Ru1 C34 2.203(3) . ? Ru1 Cl1 2.4200(8) . ? O1 C1 1.280(3) . ? N1 C1 1.370(3) . ? N1 N2 1.401(3) . ? N1 C2 1.421(3) . ? N2 C8 1.325(4) . ? N3 C11 1.316(4) . ? N3 C24 1.451(4) . ? C1 C10 1.416(4) . ? C2 C7 1.391(4) . ? C2 C3 1.396(4) . ? C3 C4 1.400(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(5) . ? C5 H5 0.9500 . ? C6 C7 1.401(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.445(4) . ? C8 C9 1.504(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.423(4) . ? C11 C12 1.506(4) . ? C12 C17 1.388(4) . ? C12 C13 1.400(4) . ? C13 C14 1.397(4) . ? C13 H13 0.9500 . ? C14 C15 1.398(4) . ? C14 H14 0.9500 . ? C15 C16 1.410(4) . ? C15 C18 1.493(4) . ? C16 C17 1.390(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.395(4) . ? C18 C23 1.402(4) . ? C19 C20 1.397(4) . ? C19 H19 0.9500 . ? C20 C21 1.399(4) . ? C20 H20 0.9500 . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.398(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C33 1.378(4) . ? C24 C25 1.423(4) . ? C25 C30 1.426(4) . ? C25 C26 1.447(5) . ? C26 C27 1.373(4) . ? C26 H26 0.9500 . ? C27 C28 1.422(5) . ? C27 H27 0.9500 . ? C28 C29 1.349(5) . ? C28 H28 0.9500 . ? C29 C30 1.412(5) . ? C29 H29 0.9500 . ? C30 C31 1.433(5) . ? C31 C32 1.371(5) . ? C31 H31 0.9500 . ? C32 C33 1.418(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.406(5) . ? C34 C39 1.434(4) . ? C34 C40 1.505(5) . ? C35 C36 1.432(5) . ? C35 H35 0.9500 . ? C36 C37 1.410(4) . ? C36 H36 0.9500 . ? C37 C38 1.445(4) . ? C37 C41 1.521(4) . ? C38 C39 1.402(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.531(5) . ? C41 C43 1.541(5) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N3 87.81(9) . . ? O1 Ru1 C37 88.16(10) . . ? N3 Ru1 C37 117.74(11) . . ? O1 Ru1 C38 86.53(9) . . ? N3 Ru1 C38 155.99(11) . . ? C37 Ru1 C38 38.79(11) . . ? O1 Ru1 C36 117.93(10) . . ? N3 Ru1 C36 94.26(11) . . ? C37 Ru1 C36 37.78(11) . . ? C38 Ru1 C36 68.16(11) . . ? O1 Ru1 C35 156.06(10) . . ? N3 Ru1 C35 95.83(10) . . ? C37 Ru1 C35 69.18(12) . . ? C38 Ru1 C35 80.55(11) . . ? C36 Ru1 C35 38.30(12) . . ? O1 Ru1 C39 112.39(10) . . ? N3 Ru1 C39 159.36(11) . . ? C37 Ru1 C39 69.13(12) . . ? C38 Ru1 C39 37.43(11) . . ? C36 Ru1 C39 80.30(12) . . ? C35 Ru1 C39 67.57(11) . . ? O1 Ru1 C34 150.31(10) . . ? N3 Ru1 C34 121.45(11) . . ? C37 Ru1 C34 82.52(12) . . ? C38 Ru1 C34 68.65(11) . . ? C36 Ru1 C34 68.63(12) . . ? C35 Ru1 C34 37.36(12) . . ? C39 Ru1 C34 38.07(11) . . ? O1 Ru1 Cl1 83.67(6) . . ? N3 Ru1 Cl1 87.25(8) . . ? C37 Ru1 Cl1 153.43(8) . . ? C38 Ru1 Cl1 115.23(9) . . ? C36 Ru1 Cl1 158.37(9) . . ? C35 Ru1 Cl1 120.07(9) . . ? C39 Ru1 Cl1 90.73(9) . . ? C34 Ru1 Cl1 92.19(9) . . ? C1 O1 Ru1 120.75(17) . . ? C1 N1 N2 111.6(2) . . ? C1 N1 C2 127.8(2) . . ? N2 N1 C2 120.5(2) . . ? C8 N2 N1 105.5(2) . . ? C11 N3 C24 118.0(2) . . ? C11 N3 Ru1 127.6(2) . . ? C24 N3 Ru1 114.09(18) . . ? O1 C1 N1 121.3(2) . . ? O1 C1 C10 131.8(3) . . ? N1 C1 C10 106.6(2) . . ? C7 C2 C3 120.9(3) . . ? C7 C2 N1 118.7(3) . . ? C3 C2 N1 120.4(2) . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 119.2(3) . . ? C2 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? N2 C8 C10 111.7(2) . . ? N2 C8 C9 117.8(2) . . ? C10 C8 C9 130.4(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 C11 123.8(2) . . ? C1 C10 C8 104.5(2) . . ? C11 C10 C8 131.8(2) . . ? N3 C11 C10 122.3(3) . . ? N3 C11 C12 119.2(2) . . ? C10 C11 C12 118.4(2) . . ? C17 C12 C13 119.4(3) . . ? C17 C12 C11 119.9(3) . . ? C13 C12 C11 120.6(3) . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 118.0(3) . . ? C14 C15 C18 121.7(3) . . ? C16 C15 C18 120.2(3) . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C12 C17 C16 120.5(3) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C23 118.7(3) . . ? C19 C18 C15 121.0(3) . . ? C23 C18 C15 120.2(3) . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 120.4(3) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? C33 C24 C25 119.7(3) . . ? C33 C24 N3 120.5(3) . . ? C25 C24 N3 119.6(3) . . ? C24 C25 C30 119.8(3) . . ? C24 C25 C26 122.0(3) . . ? C30 C25 C26 118.2(3) . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 121.3(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 120.3(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 121.1(3) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C25 119.9(3) . . ? C29 C30 C31 121.8(3) . . ? C25 C30 C31 118.3(3) . . ? C32 C31 C30 121.2(3) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 119.7(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C24 C33 C32 121.3(3) . . ? C24 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C39 118.1(3) . . ? C35 C34 C40 122.0(3) . . ? C39 C34 C40 119.9(3) . . ? C35 C34 Ru1 70.65(18) . . ? C39 C34 Ru1 70.60(17) . . ? C40 C34 Ru1 128.4(2) . . ? C34 C35 C36 121.1(3) . . ? C34 C35 Ru1 71.99(18) . . ? C36 C35 Ru1 70.64(17) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? Ru1 C35 H35 130.6 . . ? C37 C36 C35 121.2(3) . . ? C37 C36 Ru1 70.94(17) . . ? C35 C36 Ru1 71.06(17) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? Ru1 C36 H36 131.5 . . ? C36 C37 C38 117.5(3) . . ? C36 C37 C41 123.0(3) . . ? C38 C37 C41 119.4(3) . . ? C36 C37 Ru1 71.29(17) . . ? C38 C37 Ru1 70.61(17) . . ? C41 C37 Ru1 126.5(2) . . ? C39 C38 C37 121.1(3) . . ? C39 C38 Ru1 71.97(17) . . ? C37 C38 Ru1 70.60(16) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? Ru1 C38 H38 130.7 . . ? C38 C39 C34 121.1(3) . . ? C38 C39 Ru1 70.60(17) . . ? C34 C39 Ru1 71.33(17) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? Ru1 C39 H39 131.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C41 C42 109.5(3) . . ? C37 C41 C43 113.7(3) . . ? C42 C41 C43 111.2(3) . . ? C37 C41 H41 107.4 . . ? C42 C41 H41 107.4 . . ? C43 C41 H41 107.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 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 N3 Ru1 O1 C1 24.8(2) . . . . ? C37 Ru1 O1 C1 142.6(2) . . . . ? C38 Ru1 O1 C1 -178.6(2) . . . . ? C36 Ru1 O1 C1 118.4(2) . . . . ? C35 Ru1 O1 C1 124.2(3) . . . . ? C39 Ru1 O1 C1 -150.9(2) . . . . ? C34 Ru1 O1 C1 -146.0(2) . . . . ? Cl1 Ru1 O1 C1 -62.7(2) . . . . ? C1 N1 N2 C8 1.0(3) . . . . ? C2 N1 N2 C8 -175.7(2) . . . . ? O1 Ru1 N3 C11 -13.7(3) . . . . ? C37 Ru1 N3 C11 -100.5(3) . . . . ? C38 Ru1 N3 C11 -90.2(4) . . . . ? C36 Ru1 N3 C11 -131.6(3) . . . . ? C35 Ru1 N3 C11 -170.0(3) . . . . ? C39 Ru1 N3 C11 154.8(3) . . . . ? C34 Ru1 N3 C11 160.9(2) . . . . ? Cl1 Ru1 N3 C11 70.0(3) . . . . ? O1 Ru1 N3 C24 159.4(2) . . . . ? C37 Ru1 N3 C24 72.6(2) . . . . ? C38 Ru1 N3 C24 82.9(3) . . . . ? C36 Ru1 N3 C24 41.5(2) . . . . ? C35 Ru1 N3 C24 3.1(2) . . . . ? C39 Ru1 N3 C24 -32.1(4) . . . . ? C34 Ru1 N3 C24 -26.0(3) . . . . ? Cl1 Ru1 N3 C24 -116.9(2) . . . . ? Ru1 O1 C1 N1 159.2(2) . . . . ? Ru1 O1 C1 C10 -27.1(4) . . . . ? N2 N1 C1 O1 173.7(2) . . . . ? C2 N1 C1 O1 -9.9(4) . . . . ? N2 N1 C1 C10 -1.4(3) . . . . ? C2 N1 C1 C10 175.0(3) . . . . ? C1 N1 C2 C7 158.6(3) . . . . ? N2 N1 C2 C7 -25.2(4) . . . . ? C1 N1 C2 C3 -22.5(4) . . . . ? N2 N1 C2 C3 153.6(3) . . . . ? C7 C2 C3 C4 -1.3(4) . . . . ? N1 C2 C3 C4 179.9(3) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C4 C5 C6 C7 -0.4(5) . . . . ? C3 C2 C7 C6 0.8(4) . . . . ? N1 C2 C7 C6 179.6(3) . . . . ? C5 C6 C7 C2 0.1(5) . . . . ? N1 N2 C8 C10 -0.2(3) . . . . ? N1 N2 C8 C9 177.8(2) . . . . ? O1 C1 C10 C11 6.1(5) . . . . ? N1 C1 C10 C11 -179.5(3) . . . . ? O1 C1 C10 C8 -173.2(3) . . . . ? N1 C1 C10 C8 1.2(3) . . . . ? N2 C8 C10 C1 -0.6(3) . . . . ? C9 C8 C10 C1 -178.3(3) . . . . ? N2 C8 C10 C11 -179.9(3) . . . . ? C9 C8 C10 C11 2.5(5) . . . . ? C24 N3 C11 C10 -172.9(3) . . . . ? Ru1 N3 C11 C10 0.0(4) . . . . ? C24 N3 C11 C12 4.8(4) . . . . ? Ru1 N3 C11 C12 177.6(2) . . . . ? C1 C10 C11 N3 9.4(5) . . . . ? C8 C10 C11 N3 -171.5(3) . . . . ? C1 C10 C11 C12 -168.3(3) . . . . ? C8 C10 C11 C12 10.8(5) . . . . ? N3 C11 C12 C17 -92.3(4) . . . . ? C10 C11 C12 C17 85.4(4) . . . . ? N3 C11 C12 C13 87.0(4) . . . . ? C10 C11 C12 C13 -95.2(3) . . . . ? C17 C12 C13 C14 0.8(4) . . . . ? C11 C12 C13 C14 -178.5(3) . . . . ? C12 C13 C14 C15 1.6(4) . . . . ? C13 C14 C15 C16 -2.3(4) . . . . ? C13 C14 C15 C18 174.2(3) . . . . ? C14 C15 C16 C17 0.8(4) . . . . ? C18 C15 C16 C17 -175.8(3) . . . . ? C13 C12 C17 C16 -2.3(4) . . . . ? C11 C12 C17 C16 177.0(3) . . . . ? C15 C16 C17 C12 1.5(5) . . . . ? C14 C15 C18 C19 155.5(3) . . . . ? C16 C15 C18 C19 -28.1(4) . . . . ? C14 C15 C18 C23 -28.6(4) . . . . ? C16 C15 C18 C23 147.8(3) . . . . ? C23 C18 C19 C20 -0.8(4) . . . . ? C15 C18 C19 C20 175.2(3) . . . . ? C18 C19 C20 C21 -0.4(5) . . . . ? C19 C20 C21 C22 0.9(5) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C21 C22 C23 C18 -1.2(5) . . . . ? C19 C18 C23 C22 1.6(4) . . . . ? C15 C18 C23 C22 -174.4(3) . . . . ? C11 N3 C24 C33 83.5(4) . . . . ? Ru1 N3 C24 C33 -90.3(3) . . . . ? C11 N3 C24 C25 -101.5(3) . . . . ? Ru1 N3 C24 C25 84.7(3) . . . . ? C33 C24 C25 C30 1.2(4) . . . . ? N3 C24 C25 C30 -173.8(3) . . . . ? C33 C24 C25 C26 -179.3(3) . . . . ? N3 C24 C25 C26 5.6(4) . . . . ? C24 C25 C26 C27 179.6(3) . . . . ? C30 C25 C26 C27 -0.9(4) . . . . ? C25 C26 C27 C28 0.2(5) . . . . ? C26 C27 C28 C29 0.3(5) . . . . ? C27 C28 C29 C30 0.0(5) . . . . ? C28 C29 C30 C25 -0.7(5) . . . . ? C28 C29 C30 C31 179.6(3) . . . . ? C24 C25 C30 C29 -179.4(3) . . . . ? C26 C25 C30 C29 1.2(4) . . . . ? C24 C25 C30 C31 0.4(4) . . . . ? C26 C25 C30 C31 -179.1(3) . . . . ? C29 C30 C31 C32 178.4(3) . . . . ? C25 C30 C31 C32 -1.3(5) . . . . ? C30 C31 C32 C33 0.6(5) . . . . ? C25 C24 C33 C32 -2.0(5) . . . . ? N3 C24 C33 C32 173.0(3) . . . . ? C31 C32 C33 C24 1.1(5) . . . . ? O1 Ru1 C34 C35 -138.0(2) . . . . ? N3 Ru1 C34 C35 52.8(2) . . . . ? C37 Ru1 C34 C35 -65.24(19) . . . . ? C38 Ru1 C34 C35 -102.8(2) . . . . ? C36 Ru1 C34 C35 -28.82(18) . . . . ? C39 Ru1 C34 C35 -130.7(3) . . . . ? Cl1 Ru1 C34 C35 140.91(18) . . . . ? O1 Ru1 C34 C39 -7.3(3) . . . . ? N3 Ru1 C34 C39 -176.49(17) . . . . ? C37 Ru1 C34 C39 65.47(19) . . . . ? C38 Ru1 C34 C39 27.92(18) . . . . ? C36 Ru1 C34 C39 101.9(2) . . . . ? C35 Ru1 C34 C39 130.7(3) . . . . ? Cl1 Ru1 C34 C39 -88.38(18) . . . . ? O1 Ru1 C34 C40 106.0(3) . . . . ? N3 Ru1 C34 C40 -63.2(3) . . . . ? C37 Ru1 C34 C40 178.8(3) . . . . ? C38 Ru1 C34 C40 141.2(3) . . . . ? C36 Ru1 C34 C40 -144.8(3) . . . . ? C35 Ru1 C34 C40 -116.0(4) . . . . ? C39 Ru1 C34 C40 113.3(4) . . . . ? Cl1 Ru1 C34 C40 24.9(3) . . . . ? C39 C34 C35 C36 -1.2(4) . . . . ? C40 C34 C35 C36 176.7(3) . . . . ? Ru1 C34 C35 C36 52.9(3) . . . . ? C39 C34 C35 Ru1 -54.1(2) . . . . ? C40 C34 C35 Ru1 123.8(3) . . . . ? O1 Ru1 C35 C34 125.3(2) . . . . ? N3 Ru1 C35 C34 -136.92(19) . . . . ? C37 Ru1 C35 C34 105.6(2) . . . . ? C38 Ru1 C35 C34 67.03(19) . . . . ? C36 Ru1 C35 C34 133.6(3) . . . . ? C39 Ru1 C35 C34 30.37(18) . . . . ? Cl1 Ru1 C35 C34 -46.7(2) . . . . ? O1 Ru1 C35 C36 -8.3(3) . . . . ? N3 Ru1 C35 C36 89.49(18) . . . . ? C37 Ru1 C35 C36 -28.01(17) . . . . ? C38 Ru1 C35 C36 -66.56(18) . . . . ? C39 Ru1 C35 C36 -103.21(19) . . . . ? C34 Ru1 C35 C36 -133.6(3) . . . . ? Cl1 Ru1 C35 C36 179.68(14) . . . . ? C34 C35 C36 C37 -1.2(4) . . . . ? Ru1 C35 C36 C37 52.3(3) . . . . ? C34 C35 C36 Ru1 -53.5(3) . . . . ? O1 Ru1 C36 C37 42.0(2) . . . . ? N3 Ru1 C36 C37 131.75(18) . . . . ? C38 Ru1 C36 C37 -31.39(18) . . . . ? C35 Ru1 C36 C37 -134.2(3) . . . . ? C39 Ru1 C36 C37 -68.32(19) . . . . ? C34 Ru1 C36 C37 -106.1(2) . . . . ? Cl1 Ru1 C36 C37 -135.0(2) . . . . ? O1 Ru1 C36 C35 176.20(15) . . . . ? N3 Ru1 C36 C35 -94.02(18) . . . . ? C37 Ru1 C36 C35 134.2(3) . . . . ? C38 Ru1 C36 C35 102.84(19) . . . . ? C39 Ru1 C36 C35 65.91(18) . . . . ? C34 Ru1 C36 C35 28.16(17) . . . . ? Cl1 Ru1 C36 C35 -0.7(3) . . . . ? C35 C36 C37 C38 2.8(4) . . . . ? Ru1 C36 C37 C38 55.1(2) . . . . ? C35 C36 C37 C41 -174.3(3) . . . . ? Ru1 C36 C37 C41 -121.9(3) . . . . ? C35 C36 C37 Ru1 -52.4(3) . . . . ? O1 Ru1 C37 C36 -143.76(18) . . . . ? N3 Ru1 C37 C36 -57.2(2) . . . . ? C38 Ru1 C37 C36 129.5(3) . . . . ? C35 Ru1 C37 C36 28.37(18) . . . . ? C39 Ru1 C37 C36 101.4(2) . . . . ? C34 Ru1 C37 C36 64.50(19) . . . . ? Cl1 Ru1 C37 C36 144.35(17) . . . . ? O1 Ru1 C37 C38 86.75(17) . . . . ? N3 Ru1 C37 C38 173.31(16) . . . . ? C36 Ru1 C37 C38 -129.5(3) . . . . ? C35 Ru1 C37 C38 -101.12(19) . . . . ? C39 Ru1 C37 C38 -28.09(17) . . . . ? C34 Ru1 C37 C38 -64.99(18) . . . . ? Cl1 Ru1 C37 C38 14.9(3) . . . . ? O1 Ru1 C37 C41 -26.0(3) . . . . ? N3 Ru1 C37 C41 60.5(3) . . . . ? C38 Ru1 C37 C41 -112.8(3) . . . . ? C36 Ru1 C37 C41 117.8(3) . . . . ? C35 Ru1 C37 C41 146.1(3) . . . . ? C39 Ru1 C37 C41 -140.9(3) . . . . ? C34 Ru1 C37 C41 -177.8(3) . . . . ? Cl1 Ru1 C37 C41 -97.9(3) . . . . ? C36 C37 C38 C39 -2.0(4) . . . . ? C41 C37 C38 C39 175.2(3) . . . . ? Ru1 C37 C38 C39 53.5(2) . . . . ? C36 C37 C38 Ru1 -55.5(2) . . . . ? C41 C37 C38 Ru1 121.7(3) . . . . ? O1 Ru1 C38 C39 135.01(18) . . . . ? N3 Ru1 C38 C39 -148.3(2) . . . . ? C37 Ru1 C38 C39 -133.6(3) . . . . ? C36 Ru1 C38 C39 -103.0(2) . . . . ? C35 Ru1 C38 C39 -65.22(19) . . . . ? C34 Ru1 C38 C39 -28.36(18) . . . . ? Cl1 Ru1 C38 C39 53.67(19) . . . . ? O1 Ru1 C38 C37 -91.38(17) . . . . ? N3 Ru1 C38 C37 -14.7(3) . . . . ? C36 Ru1 C38 C37 30.62(17) . . . . ? C35 Ru1 C38 C37 68.40(18) . . . . ? C39 Ru1 C38 C37 133.6(3) . . . . ? C34 Ru1 C38 C37 105.26(19) . . . . ? Cl1 Ru1 C38 C37 -172.71(14) . . . . ? C37 C38 C39 C34 -0.3(4) . . . . ? Ru1 C38 C39 C34 52.5(2) . . . . ? C37 C38 C39 Ru1 -52.9(2) . . . . ? C35 C34 C39 C38 1.9(4) . . . . ? C40 C34 C39 C38 -176.0(3) . . . . ? Ru1 C34 C39 C38 -52.2(2) . . . . ? C35 C34 C39 Ru1 54.1(2) . . . . ? C40 C34 C39 Ru1 -123.8(3) . . . . ? O1 Ru1 C39 C38 -49.8(2) . . . . ? N3 Ru1 C39 C38 142.7(3) . . . . ? C37 Ru1 C39 C38 29.04(18) . . . . ? C36 Ru1 C39 C38 66.57(18) . . . . ? C35 Ru1 C39 C38 104.3(2) . . . . ? C34 Ru1 C39 C38 134.2(3) . . . . ? Cl1 Ru1 C39 C38 -133.21(17) . . . . ? O1 Ru1 C39 C34 176.09(17) . . . . ? N3 Ru1 C39 C34 8.5(4) . . . . ? C37 Ru1 C39 C34 -105.1(2) . . . . ? C38 Ru1 C39 C34 -134.2(3) . . . . ? C36 Ru1 C39 C34 -67.59(19) . . . . ? C35 Ru1 C39 C34 -29.84(19) . . . . ? Cl1 Ru1 C39 C34 92.63(18) . . . . ? C36 C37 C41 C42 -90.2(4) . . . . ? C38 C37 C41 C42 92.7(3) . . . . ? Ru1 C37 C41 C42 179.4(2) . . . . ? C36 C37 C41 C43 34.8(4) . . . . ? C38 C37 C41 C43 -142.2(3) . . . . ? Ru1 C37 C41 C43 -55.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.994 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.110 _iucr_refine_instructions_details ; TITL CC4 in C2/c CELL 0.71073 25.6157 22.8086 12.7928 90.0000 111.7013 90.0000 ZERR 8.00 0.0040 0.0014 0.0027 0.0000 0.0100 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O CL RU UNIT 344 304 24 8 8 8 REM ---------------------------------------------------------- REM Data collection: Bruker Nonius APEX II CCD REM Absorption correction: SADABS REM Crystal habit: prismatic; Crystal colour: red REM ---------------------------------------------------------- L.S. 10 OMIT 4 6 2 OMIT -7 5 3 OMIT -1 3 1 OMIT -2 0 2 ACTA CONF SIZE 0.302 0.277 0.233 BOND $H WPDB -2 FMAP 2 PLAN 10 TEMP -173 WGHT 0.026600 42.896702 FVAR 0.19236 RU1 6 0.184377 0.414674 0.245344 11.00000 0.01438 0.01583 = 0.01024 -0.00251 0.00512 -0.00426 CL1 5 0.149868 0.495550 0.115539 11.00000 0.02358 0.02275 = 0.01790 0.00454 0.00762 0.00367 O1 4 0.256309 0.424897 0.208996 11.00000 0.01445 0.01929 = 0.00974 -0.00136 0.00462 -0.00477 N1 3 0.295271 0.440634 0.074790 11.00000 0.01296 0.01243 = 0.01148 -0.00098 0.00454 -0.00187 N2 3 0.289041 0.421576 -0.033309 11.00000 0.01671 0.01459 = 0.01159 -0.00177 0.00662 -0.00012 N3 3 0.152907 0.357405 0.102245 11.00000 0.01625 0.01963 = 0.01519 -0.00471 0.00576 -0.00547 C1 1 0.254981 0.417084 0.108933 11.00000 0.01249 0.01108 = 0.01206 0.00106 0.00462 -0.00009 C2 1 0.337532 0.482059 0.132656 11.00000 0.00969 0.01190 = 0.01235 0.00114 0.00220 -0.00067 C3 1 0.330793 0.518692 0.214226 11.00000 0.01428 0.01341 = 0.01874 0.00012 0.00818 0.00048 AFIX 43 H3 2 0.297902 0.516346 0.231737 11.00000 -1.20000 AFIX 0 C4 1 0.373287 0.558935 0.269792 11.00000 0.01858 0.01551 = 0.01866 -0.00334 0.00610 -0.00200 AFIX 43 H4 2 0.369471 0.583701 0.326250 11.00000 -1.20000 AFIX 0 C5 1 0.421236 0.562919 0.242793 11.00000 0.01397 0.01807 = 0.02036 0.00047 0.00319 -0.00384 AFIX 43 H5 2 0.449904 0.590355 0.280672 11.00000 -1.20000 AFIX 0 C6 1 0.426860 0.526911 0.160982 11.00000 0.01411 0.03044 = 0.02337 -0.00191 0.00804 -0.00626 AFIX 43 H6 2 0.459411 0.529878 0.142427 11.00000 -1.20000 AFIX 0 C7 1 0.385073 0.486010 0.104959 11.00000 0.01514 0.02283 = 0.01762 -0.00350 0.00716 -0.00308 AFIX 43 H7 2 0.389148 0.461264 0.048725 11.00000 -1.20000 AFIX 0 C8 1 0.244279 0.387053 -0.066269 11.00000 0.01404 0.01373 = 0.01217 0.00005 0.00426 0.00112 C9 1 0.225626 0.361415 -0.182667 11.00000 0.02556 0.02729 = 0.01381 -0.00618 0.01051 -0.00568 AFIX 33 H9A 2 0.253313 0.370827 -0.216329 11.00000 -1.50000 H9B 2 0.189083 0.377958 -0.229127 11.00000 -1.50000 H9C 2 0.222325 0.318753 -0.178400 11.00000 -1.50000 AFIX 0 C10 1 0.219927 0.382157 0.018770 11.00000 0.01306 0.01129 = 0.01149 -0.00153 0.00516 -0.00042 C11 1 0.172538 0.350523 0.021369 11.00000 0.01484 0.01496 = 0.01240 -0.00272 0.00414 -0.00242 C12 1 0.145510 0.306072 -0.069642 11.00000 0.01613 0.01804 = 0.01137 -0.00516 0.00571 -0.00570 C13 1 0.099002 0.321242 -0.165410 11.00000 0.01913 0.01279 = 0.01770 -0.00286 0.00741 -0.00285 AFIX 43 H13 2 0.084740 0.360131 -0.174260 11.00000 -1.20000 AFIX 0 C14 1 0.073579 0.279147 -0.247959 11.00000 0.01725 0.01602 = 0.01150 -0.00076 0.00368 -0.00225 AFIX 43 H14 2 0.042627 0.290025 -0.313565 11.00000 -1.20000 AFIX 0 C15 1 0.092935 0.221293 -0.235606 11.00000 0.01541 0.01716 = 0.01097 -0.00243 0.00485 -0.00289 C16 1 0.140246 0.207085 -0.139250 11.00000 0.01748 0.01498 = 0.01651 -0.00261 0.00518 -0.00047 AFIX 43 H16 2 0.154453 0.168164 -0.129466 11.00000 -1.20000 AFIX 0 C17 1 0.166360 0.249272 -0.058413 11.00000 0.01523 0.01983 = 0.01414 -0.00112 0.00190 -0.00044 AFIX 43 H17 2 0.198745 0.239162 0.005055 11.00000 -1.20000 AFIX 0 C18 1 0.062999 0.174615 -0.317742 11.00000 0.01679 0.01499 = 0.01072 -0.00182 0.00579 -0.00388 C19 1 0.091335 0.124797 -0.331733 11.00000 0.01700 0.01818 = 0.01357 0.00054 0.00319 0.00024 AFIX 43 H19 2 0.130803 0.121785 -0.292814 11.00000 -1.20000 AFIX 0 C20 1 0.062249 0.079298 -0.402401 11.00000 0.02631 0.01618 = 0.01895 -0.00288 0.00670 0.00216 AFIX 43 H20 2 0.082019 0.045695 -0.411689 11.00000 -1.20000 AFIX 0 C21 1 0.004085 0.083103 -0.459515 11.00000 0.02315 0.01656 = 0.01433 -0.00349 0.00285 -0.00414 AFIX 43 H21 2 -0.015830 0.051959 -0.506797 11.00000 -1.20000 AFIX 0 C22 1 -0.024203 0.132515 -0.446653 11.00000 0.01628 0.01810 = 0.01521 -0.00217 0.00118 -0.00354 AFIX 43 H22 2 -0.063706 0.135264 -0.485361 11.00000 -1.20000 AFIX 0 C23 1 0.004859 0.178485 -0.377124 11.00000 0.01735 0.01447 = 0.01417 -0.00211 0.00550 -0.00046 AFIX 43 H23 2 -0.014912 0.212560 -0.370070 11.00000 -1.20000 AFIX 0 C24 1 0.108672 0.318212 0.104358 11.00000 0.01873 0.02067 = 0.01467 -0.00420 0.00695 -0.00518 C25 1 0.052006 0.338160 0.063607 11.00000 0.01789 0.02498 = 0.01486 -0.00776 0.00700 -0.00531 C26 1 0.036104 0.394834 0.010516 11.00000 0.02159 0.02465 = 0.01686 -0.00253 0.00608 0.00199 AFIX 43 H26 2 0.063702 0.420235 0.002184 11.00000 -1.20000 AFIX 0 C27 1 -0.019318 0.411501 -0.027695 11.00000 0.02295 0.02235 = 0.02018 -0.00239 0.00557 0.00198 AFIX 43 H27 2 -0.029835 0.448644 -0.062799 11.00000 -1.20000 AFIX 0 C28 1 -0.061261 0.374256 -0.015744 11.00000 0.02441 0.03951 = 0.02448 -0.00685 0.00927 0.00002 AFIX 43 H28 2 -0.099379 0.386602 -0.043080 11.00000 -1.20000 AFIX 0 C29 1 -0.047145 0.321458 0.034254 11.00000 0.01985 0.03967 = 0.02348 -0.00801 0.01072 -0.00452 AFIX 43 H29 2 -0.075558 0.296968 0.041746 11.00000 -1.20000 AFIX 0 C30 1 0.009164 0.301992 0.075640 11.00000 0.01970 0.02486 = 0.01360 -0.00679 0.00829 -0.00765 C31 1 0.024959 0.246189 0.129687 11.00000 0.02965 0.02531 = 0.02311 -0.00377 0.01141 -0.00978 AFIX 43 H31 2 -0.002935 0.221888 0.139763 11.00000 -1.20000 AFIX 0 C32 1 0.079612 0.227269 0.167096 11.00000 0.02840 0.01746 = 0.02041 -0.00084 0.00552 -0.00233 AFIX 43 H32 2 0.089354 0.190016 0.202142 11.00000 -1.20000 AFIX 0 C33 1 0.121530 0.263574 0.153224 11.00000 0.02687 0.01646 = 0.01904 -0.00183 0.00776 -0.00142 AFIX 43 H33 2 0.159221 0.249969 0.178104 11.00000 -1.20000 AFIX 0 C34 1 0.132134 0.440175 0.341363 11.00000 0.02040 0.02895 = 0.01366 -0.00273 0.00891 -0.00173 C35 1 0.132720 0.378740 0.332997 11.00000 0.02176 0.02455 = 0.01444 -0.00403 0.01141 -0.00860 AFIX 43 H35 2 0.098165 0.357931 0.305097 11.00000 -1.20000 AFIX 0 C36 1 0.184569 0.347014 0.365857 11.00000 0.02414 0.02003 = 0.01657 -0.00109 0.01009 -0.00720 AFIX 43 H36 2 0.183823 0.305449 0.360736 11.00000 -1.20000 AFIX 0 C37 1 0.236700 0.376378 0.405672 11.00000 0.02209 0.01878 = 0.01193 0.00041 0.00745 -0.00275 C38 1 0.235878 0.439376 0.416904 11.00000 0.01989 0.01954 = 0.01063 -0.00423 0.00596 -0.00642 AFIX 43 H38 2 0.270360 0.460273 0.445792 11.00000 -1.20000 AFIX 0 C39 1 0.185013 0.470157 0.385855 11.00000 0.02419 0.01940 = 0.01283 -0.00464 0.00776 -0.00405 AFIX 43 H39 2 0.185589 0.511552 0.394431 11.00000 -1.20000 AFIX 0 C40 1 0.078210 0.474664 0.301684 11.00000 0.02154 0.03955 = 0.02196 -0.00389 0.01016 0.00230 AFIX 33 H40A 2 0.048647 0.451817 0.245385 11.00000 -1.50000 H40B 2 0.083770 0.511620 0.268118 11.00000 -1.50000 H40C 2 0.067109 0.483007 0.365718 11.00000 -1.50000 AFIX 0 C41 1 0.292559 0.345168 0.431528 11.00000 0.01975 0.02316 = 0.01912 0.00166 0.00568 -0.00136 AFIX 13 H41 2 0.319574 0.374423 0.422140 11.00000 -1.20000 AFIX 0 C42 1 0.315573 0.325520 0.554722 11.00000 0.04083 0.03147 = 0.02294 0.00303 0.00326 0.00847 AFIX 33 H42A 2 0.319707 0.359691 0.603580 11.00000 -1.50000 H42B 2 0.352258 0.306791 0.572131 11.00000 -1.50000 H42C 2 0.289480 0.297504 0.567292 11.00000 -1.50000 AFIX 0 C43 1 0.289590 0.293479 0.352006 11.00000 0.02993 0.02481 = 0.03286 -0.00355 0.01678 0.00103 AFIX 33 H43A 2 0.267905 0.261427 0.367174 11.00000 -1.50000 H43B 2 0.327691 0.279788 0.364478 11.00000 -1.50000 H43C 2 0.271284 0.306344 0.273780 11.00000 -1.50000 HKLF 4 REM CC4 in C2/c REM R1 = 0.0502 for 8147 Fo > 4sig(Fo) and 0.0683 for all 10034 data REM 442 parameters refined using 0 restraints END WGHT 0.0266 42.8574 REM Highest difference peak 2.994, deepest hole -1.184, 1-sigma level 0.110 Q1 1 0.2149 0.3751 0.2953 11.00000 0.05 2.99 Q2 1 0.1685 0.4425 0.2315 11.00000 0.05 1.29 Q3 1 0.0814 0.3699 0.0564 11.00000 0.05 1.02 Q4 1 0.1520 0.5268 0.1266 11.00000 0.05 1.02 Q5 1 -0.0207 0.2607 0.0982 11.00000 0.05 0.89 Q6 1 0.0893 0.2658 0.1307 11.00000 0.05 0.74 Q7 1 -0.0313 0.3583 0.0166 11.00000 0.05 0.71 Q8 1 0.0636 0.3074 0.0943 11.00000 0.05 0.66 Q9 1 0.1345 0.3837 0.0774 11.00000 0.05 0.63 Q10 1 0.2209 0.4190 0.2745 11.00000 0.05 0.61 ; data_5 _audit_update_record ; 2013-01-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H34 Cl N3 O Ru, C H2 Cl2' _chemical_formula_sum 'C38 H36 Cl3 N3 O Ru' _chemical_formula_weight 758.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.586(5) _cell_length_b 9.776(3) _cell_length_c 23.383(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.560(17) _cell_angle_gamma 90.00 _cell_volume 3330.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 488 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 140(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 marmux _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14715 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.74 _reflns_number_total 7713 _reflns_number_gt 5100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marmux - Micro-beam system, marresearch, 2010' _computing_cell_refinement 'automar, marresearch, 2010' _computing_data_reduction 'automar, marresearch, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7713 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.44477(2) 0.63525(3) 0.273784(15) 0.02468(12) Uani 1 1 d . . . Cl1 Cl 0.41868(9) 0.40443(11) 0.23605(5) 0.0362(3) Uani 1 1 d . . . O1 O 0.3475(2) 0.5819(3) 0.33242(13) 0.0307(7) Uani 1 1 d . . . N1 N 0.2939(2) 0.4383(4) 0.40251(16) 0.0275(8) Uani 1 1 d . . . N2 N 0.3277(3) 0.3410(4) 0.44201(16) 0.0312(8) Uani 1 1 d . . . N3 N 0.5463(2) 0.5383(4) 0.32725(15) 0.0274(8) Uani 1 1 d . . . C1 C 0.3621(3) 0.4901(4) 0.37070(18) 0.0263(9) Uani 1 1 d . . . C2 C 0.1978(3) 0.4654(4) 0.39943(19) 0.0273(9) Uani 1 1 d . . . C3 C 0.1572(3) 0.5477(4) 0.3572(2) 0.0306(10) Uani 1 1 d . . . H3 H 0.1941 0.5906 0.3300 0.037 Uiso 1 1 calc R . . C4 C 0.0638(3) 0.5675(5) 0.3545(2) 0.0356(11) Uani 1 1 d . . . H4 H 0.0367 0.6235 0.3252 0.043 Uiso 1 1 calc R . . C5 C 0.0086(3) 0.5068(5) 0.3942(2) 0.0383(11) Uani 1 1 d . . . H5 H -0.0560 0.5204 0.3920 0.046 Uiso 1 1 calc R . . C6 C 0.0492(3) 0.4257(5) 0.4373(2) 0.0369(11) Uani 1 1 d . . . H6 H 0.0121 0.3846 0.4648 0.044 Uiso 1 1 calc R . . C7 C 0.1429(3) 0.4045(5) 0.4403(2) 0.0342(10) Uani 1 1 d . . . H7 H 0.1701 0.3492 0.4699 0.041 Uiso 1 1 calc R . . C8 C 0.4168(3) 0.3347(4) 0.43480(19) 0.0299(10) Uani 1 1 d . . . C9 C 0.4734(3) 0.2392(5) 0.4726(2) 0.0412(12) Uani 1 1 d . . . H9A H 0.5135 0.2927 0.4989 0.062 Uiso 1 1 calc R . . H9B H 0.5109 0.1809 0.4488 0.062 Uiso 1 1 calc R . . H9C H 0.4326 0.1820 0.4947 0.062 Uiso 1 1 calc R . . C10 C 0.4445(3) 0.4270(4) 0.39054(18) 0.0263(9) Uani 1 1 d . . . C11 C 0.5324(3) 0.4538(4) 0.36979(18) 0.0258(9) Uani 1 1 d . . . C12 C 0.6131(3) 0.3750(4) 0.39531(18) 0.0265(9) Uani 1 1 d . . . C13 C 0.6382(3) 0.2565(5) 0.3676(2) 0.0340(10) Uani 1 1 d . . . H13 H 0.6047 0.2272 0.3341 0.041 Uiso 1 1 calc R . . C14 C 0.7124(4) 0.1807(5) 0.3890(2) 0.0423(12) Uani 1 1 d . . . H14 H 0.7293 0.0992 0.3700 0.051 Uiso 1 1 calc R . . C15 C 0.7622(4) 0.2226(5) 0.4378(2) 0.0431(12) Uani 1 1 d . . . H15 H 0.8131 0.1705 0.4523 0.052 Uiso 1 1 calc R . . C16 C 0.7370(4) 0.3404(5) 0.4650(2) 0.0404(12) Uani 1 1 d . . . H16 H 0.7705 0.3699 0.4985 0.048 Uiso 1 1 calc R . . C17 C 0.6625(3) 0.4171(5) 0.4437(2) 0.0365(11) Uani 1 1 d . . . H17 H 0.6456 0.4986 0.4627 0.044 Uiso 1 1 calc R . . C18 C 0.6399(3) 0.5586(4) 0.31128(19) 0.0289(9) Uani 1 1 d . . . C19 C 0.6729(3) 0.4860(5) 0.26589(19) 0.0337(10) Uani 1 1 d . . . H19 H 0.6344 0.4223 0.2457 0.040 Uiso 1 1 calc R . . C20 C 0.7634(3) 0.5062(5) 0.2497(2) 0.0335(10) Uani 1 1 d . . . H20 H 0.7857 0.4552 0.2186 0.040 Uiso 1 1 calc R . . C21 C 0.8198(3) 0.5974(5) 0.2775(2) 0.0345(10) Uani 1 1 d . . . H21 H 0.8807 0.6100 0.2656 0.041 Uiso 1 1 calc R . . C22 C 0.7877(3) 0.6747(4) 0.32477(19) 0.0292(9) Uani 1 1 d . . . C23 C 0.8445(3) 0.7671(5) 0.3559(2) 0.0352(11) Uani 1 1 d . . . H23 H 0.9059 0.7804 0.3451 0.042 Uiso 1 1 calc R . . C24 C 0.8134(3) 0.8374(5) 0.4011(2) 0.0361(11) Uani 1 1 d . . . H24 H 0.8532 0.8986 0.4217 0.043 Uiso 1 1 calc R . . C25 C 0.7214(3) 0.8201(5) 0.4178(2) 0.0330(10) Uani 1 1 d . . . H25 H 0.6999 0.8706 0.4492 0.040 Uiso 1 1 calc R . . C26 C 0.6640(3) 0.7313(4) 0.3888(2) 0.0320(10) Uani 1 1 d . . . H26 H 0.6027 0.7204 0.4002 0.038 Uiso 1 1 calc R . . C27 C 0.6956(3) 0.6545(4) 0.3412(2) 0.0313(10) Uani 1 1 d . . . C28 C 0.4856(3) 0.7097(4) 0.18929(18) 0.0284(9) Uani 1 1 d . . . C29 C 0.5420(3) 0.7703(4) 0.23247(18) 0.0278(9) Uani 1 1 d . . . H29 H 0.6068 0.7648 0.2302 0.033 Uiso 1 1 calc R . . C30 C 0.5043(3) 0.8400(4) 0.27984(19) 0.0279(9) Uani 1 1 d . . . H30 H 0.5441 0.8787 0.3087 0.034 Uiso 1 1 calc R . . C31 C 0.4081(3) 0.8519(4) 0.28402(19) 0.0269(9) Uani 1 1 d . . . C32 C 0.3500(3) 0.7927(4) 0.23867(18) 0.0265(9) Uani 1 1 d . . . H32 H 0.2853 0.8024 0.2396 0.032 Uiso 1 1 calc R . . C33 C 0.3880(3) 0.7216(4) 0.19360(19) 0.0293(9) Uani 1 1 d . . . H33 H 0.3484 0.6803 0.1652 0.035 Uiso 1 1 calc R . . C34 C 0.5271(3) 0.6278(5) 0.1429(2) 0.0347(10) Uani 1 1 d . . . H34A H 0.5939 0.6245 0.1496 0.052 Uiso 1 1 calc R . . H34B H 0.5122 0.6706 0.1058 0.052 Uiso 1 1 calc R . . H34C H 0.5023 0.5346 0.1431 0.052 Uiso 1 1 calc R . . C35 C 0.3654(3) 0.9230(5) 0.3333(2) 0.0322(10) Uani 1 1 d . . . H35 H 0.3019 0.8860 0.3364 0.039 Uiso 1 1 calc R . . C36 C 0.3572(4) 1.0743(5) 0.3187(2) 0.0448(13) Uani 1 1 d . . . H36A H 0.4177 1.1102 0.3098 0.067 Uiso 1 1 calc R . . H36B H 0.3341 1.1239 0.3515 0.067 Uiso 1 1 calc R . . H36C H 0.3146 1.0862 0.2855 0.067 Uiso 1 1 calc R . . C37 C 0.4170(4) 0.8996(6) 0.3904(2) 0.0475(13) Uani 1 1 d . . . H37A H 0.4235 0.8011 0.3973 0.071 Uiso 1 1 calc R . . H37B H 0.3827 0.9409 0.4211 0.071 Uiso 1 1 calc R . . H37C H 0.4779 0.9417 0.3896 0.071 Uiso 1 1 calc R . . C38 C 0.1478(4) -0.1202(5) 0.4208(2) 0.0403(12) Uani 1 1 d . . . H38A H 0.1319 -0.1194 0.3792 0.048 Uiso 1 1 calc R . . H38B H 0.1937 -0.1933 0.4284 0.048 Uiso 1 1 calc R . . Cl2 Cl 0.19593(9) 0.03960(12) 0.44123(5) 0.0412(3) Uani 1 1 d . . . Cl3 Cl 0.04866(10) -0.15591(15) 0.45850(6) 0.0517(4) 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 Ru1 0.02274(18) 0.02559(19) 0.02552(19) 0.00332(14) -0.00104(13) -0.00058(14) Cl1 0.0463(7) 0.0286(5) 0.0333(6) 0.0008(4) -0.0032(5) -0.0037(5) O1 0.0250(16) 0.0335(16) 0.0339(17) 0.0139(14) 0.0052(13) 0.0018(13) N1 0.0248(19) 0.0301(19) 0.0277(19) 0.0052(15) 0.0033(15) -0.0005(15) N2 0.033(2) 0.033(2) 0.0271(19) 0.0070(16) 0.0012(16) 0.0002(16) N3 0.0213(18) 0.0311(19) 0.0294(19) 0.0069(16) -0.0038(15) 0.0029(15) C1 0.028(2) 0.027(2) 0.024(2) 0.0008(17) -0.0010(18) -0.0005(18) C2 0.024(2) 0.031(2) 0.027(2) -0.0031(18) 0.0004(17) -0.0039(18) C3 0.030(2) 0.028(2) 0.034(2) -0.0040(19) 0.0017(19) -0.0010(18) C4 0.031(2) 0.034(3) 0.042(3) 0.005(2) 0.006(2) 0.004(2) C5 0.031(3) 0.036(3) 0.049(3) -0.004(2) 0.007(2) -0.001(2) C6 0.037(3) 0.031(2) 0.044(3) 0.000(2) 0.010(2) -0.009(2) C7 0.042(3) 0.028(2) 0.032(2) -0.0004(19) 0.004(2) -0.007(2) C8 0.034(2) 0.029(2) 0.027(2) -0.0033(17) 0.0037(19) 0.0023(19) C9 0.038(3) 0.050(3) 0.035(3) 0.017(2) 0.001(2) 0.004(2) C10 0.025(2) 0.030(2) 0.024(2) -0.0002(17) 0.0013(17) -0.0001(18) C11 0.030(2) 0.022(2) 0.025(2) 0.0018(16) -0.0013(18) 0.0004(17) C12 0.026(2) 0.027(2) 0.027(2) 0.0026(18) -0.0014(17) 0.0027(18) C13 0.041(3) 0.036(2) 0.024(2) 0.0002(19) -0.007(2) 0.006(2) C14 0.048(3) 0.047(3) 0.031(3) -0.002(2) -0.003(2) 0.022(2) C15 0.041(3) 0.048(3) 0.039(3) 0.007(2) -0.008(2) 0.016(2) C16 0.046(3) 0.041(3) 0.033(3) 0.002(2) -0.015(2) 0.002(2) C17 0.039(3) 0.033(2) 0.036(3) 0.004(2) -0.007(2) -0.001(2) C18 0.021(2) 0.034(2) 0.031(2) 0.0036(19) -0.0054(18) 0.0012(18) C19 0.037(3) 0.034(2) 0.030(2) 0.0014(19) 0.002(2) 0.005(2) C20 0.037(3) 0.034(2) 0.030(2) 0.003(2) 0.003(2) 0.006(2) C21 0.029(2) 0.043(3) 0.031(2) 0.003(2) 0.0053(19) 0.009(2) C22 0.028(2) 0.029(2) 0.031(2) 0.0037(18) -0.0022(19) 0.0025(18) C23 0.028(2) 0.041(3) 0.036(3) 0.006(2) -0.004(2) -0.003(2) C24 0.033(3) 0.036(3) 0.039(3) 0.002(2) -0.006(2) -0.002(2) C25 0.032(2) 0.034(2) 0.032(2) 0.000(2) -0.002(2) 0.002(2) C26 0.031(2) 0.031(2) 0.034(2) -0.0008(19) 0.001(2) 0.0008(19) C27 0.032(2) 0.031(2) 0.030(2) 0.0084(19) -0.0022(19) 0.0000(19) C28 0.035(2) 0.027(2) 0.023(2) 0.0072(17) 0.0034(19) 0.0033(19) C29 0.023(2) 0.028(2) 0.032(2) 0.0055(18) 0.0014(18) -0.0012(17) C30 0.032(2) 0.021(2) 0.031(2) 0.0033(17) 0.0001(19) -0.0057(17) C31 0.031(2) 0.0196(19) 0.030(2) 0.0013(17) 0.0001(18) 0.0029(17) C32 0.026(2) 0.023(2) 0.030(2) 0.0082(17) -0.0049(18) 0.0065(17) C33 0.034(2) 0.026(2) 0.027(2) 0.0058(18) -0.0056(19) -0.0002(19) C34 0.036(3) 0.038(3) 0.031(2) -0.001(2) 0.002(2) 0.003(2) C35 0.032(2) 0.033(2) 0.031(2) 0.0013(19) -0.002(2) 0.000(2) C36 0.057(3) 0.036(3) 0.043(3) 0.003(2) 0.011(3) 0.014(2) C37 0.052(3) 0.062(3) 0.028(3) -0.009(2) -0.006(2) 0.020(3) C38 0.051(3) 0.038(3) 0.032(3) 0.002(2) -0.003(2) 0.000(2) Cl2 0.0452(7) 0.0399(6) 0.0379(7) 0.0004(5) -0.0053(5) -0.0037(5) Cl3 0.0454(8) 0.0601(9) 0.0487(8) 0.0132(6) -0.0078(6) -0.0122(6) _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 O1 2.083(3) . ? Ru1 N3 2.118(3) . ? Ru1 C30 2.184(4) . ? Ru1 C33 2.185(4) . ? Ru1 C29 2.193(4) . ? Ru1 C31 2.200(4) . ? Ru1 C32 2.203(4) . ? Ru1 C28 2.212(4) . ? Ru1 Cl1 2.4465(13) . ? O1 C1 1.278(5) . ? N1 C1 1.367(5) . ? N1 N2 1.401(5) . ? N1 C2 1.424(5) . ? N2 C8 1.319(6) . ? N3 C11 1.315(5) . ? N3 C18 1.445(5) . ? C1 C10 1.411(6) . ? C2 C3 1.386(6) . ? C2 C7 1.407(6) . ? C3 C4 1.375(6) . ? C3 H3 0.9500 . ? C4 C5 1.388(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(7) . ? C5 H5 0.9500 . ? C6 C7 1.381(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.444(6) . ? C8 C9 1.506(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.416(6) . ? C11 C12 1.507(6) . ? C12 C17 1.378(6) . ? C12 C13 1.385(6) . ? C13 C14 1.386(6) . ? C13 H13 0.9500 . ? C14 C15 1.388(7) . ? C14 H14 0.9500 . ? C15 C16 1.373(7) . ? C15 H15 0.9500 . ? C16 C17 1.393(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.382(6) . ? C18 C27 1.407(6) . ? C19 C20 1.404(7) . ? C19 H19 0.9500 . ? C20 C21 1.359(7) . ? C20 H20 0.9500 . ? C21 C22 1.435(6) . ? C21 H21 0.9500 . ? C22 C23 1.407(6) . ? C22 C27 1.427(6) . ? C23 C24 1.355(7) . ? C23 H23 0.9500 . ? C24 C25 1.424(6) . ? C24 H24 0.9500 . ? C25 C26 1.364(6) . ? C25 H25 0.9500 . ? C26 C27 1.436(6) . ? C26 H26 0.9500 . ? C28 C29 1.405(6) . ? C28 C33 1.437(6) . ? C28 C34 1.497(6) . ? C29 C30 1.432(6) . ? C29 H29 0.9500 . ? C30 C31 1.415(6) . ? C30 H30 0.9500 . ? C31 C32 1.448(6) . ? C31 C35 1.503(6) . ? C32 C33 1.397(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.520(7) . ? C35 C36 1.521(6) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Cl3 1.761(5) . ? C38 Cl2 1.770(5) . ? C38 H38A 0.9900 . ? C38 H38B 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 O1 Ru1 N3 88.74(13) . . ? O1 Ru1 C30 117.85(15) . . ? N3 Ru1 C30 96.12(16) . . ? O1 Ru1 C33 114.74(15) . . ? N3 Ru1 C33 155.14(15) . . ? C30 Ru1 C33 80.55(17) . . ? O1 Ru1 C29 156.00(15) . . ? N3 Ru1 C29 94.62(15) . . ? C30 Ru1 C29 38.18(16) . . ? C33 Ru1 C29 67.50(16) . . ? O1 Ru1 C31 89.61(14) . . ? N3 Ru1 C31 122.24(16) . . ? C30 Ru1 C31 37.67(16) . . ? C33 Ru1 C31 68.70(16) . . ? C29 Ru1 C31 68.52(16) . . ? O1 Ru1 C32 89.20(14) . . ? N3 Ru1 C32 160.54(15) . . ? C30 Ru1 C32 67.94(16) . . ? C33 Ru1 C32 37.13(16) . . ? C29 Ru1 C32 79.77(16) . . ? C31 Ru1 C32 38.39(16) . . ? O1 Ru1 C28 152.74(15) . . ? N3 Ru1 C28 117.73(15) . . ? C30 Ru1 C28 68.55(16) . . ? C33 Ru1 C28 38.13(16) . . ? C29 Ru1 C28 37.18(16) . . ? C31 Ru1 C28 81.77(16) . . ? C32 Ru1 C28 68.07(16) . . ? O1 Ru1 Cl1 84.66(9) . . ? N3 Ru1 Cl1 83.89(10) . . ? C30 Ru1 Cl1 157.50(12) . . ? C33 Ru1 Cl1 90.00(12) . . ? C29 Ru1 Cl1 119.31(12) . . ? C31 Ru1 Cl1 153.18(12) . . ? C32 Ru1 Cl1 115.17(12) . . ? C28 Ru1 Cl1 91.44(12) . . ? C1 O1 Ru1 122.7(3) . . ? C1 N1 N2 111.5(3) . . ? C1 N1 C2 130.0(4) . . ? N2 N1 C2 118.5(3) . . ? C8 N2 N1 105.5(3) . . ? C11 N3 C18 117.4(4) . . ? C11 N3 Ru1 126.9(3) . . ? C18 N3 Ru1 115.4(3) . . ? O1 C1 N1 122.6(4) . . ? O1 C1 C10 130.5(4) . . ? N1 C1 C10 106.8(4) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 N1 122.2(4) . . ? C7 C2 N1 118.4(4) . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.8(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.0(5) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 120.7(5) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 119.6(5) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? N2 C8 C10 111.8(4) . . ? N2 C8 C9 118.1(4) . . ? C10 C8 C9 130.1(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 C11 125.3(4) . . ? C1 C10 C8 104.3(4) . . ? C11 C10 C8 130.4(4) . . ? N3 C11 C10 123.2(4) . . ? N3 C11 C12 118.5(4) . . ? C10 C11 C12 118.2(4) . . ? C17 C12 C13 119.7(4) . . ? C17 C12 C11 122.9(4) . . ? C13 C12 C11 117.4(4) . . ? C12 C13 C14 119.8(4) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 120.7(5) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C12 C17 C16 120.2(5) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C27 120.7(4) . . ? C19 C18 N3 119.6(4) . . ? C27 C18 N3 119.6(4) . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 121.3(4) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C27 119.3(4) . . ? C23 C22 C21 122.1(4) . . ? C27 C22 C21 118.6(4) . . ? C24 C23 C22 121.3(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.3(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 120.3(4) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.4(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C18 C27 C22 119.2(4) . . ? C18 C27 C26 122.4(4) . . ? C22 C27 C26 118.4(4) . . ? C29 C28 C33 117.8(4) . . ? C29 C28 C34 120.2(4) . . ? C33 C28 C34 121.9(4) . . ? C29 C28 Ru1 70.7(2) . . ? C33 C28 Ru1 69.9(2) . . ? C34 C28 Ru1 127.2(3) . . ? C28 C29 C30 121.6(4) . . ? C28 C29 Ru1 72.1(2) . . ? C30 C29 Ru1 70.6(2) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? Ru1 C29 H29 130.9 . . ? C31 C30 C29 120.6(4) . . ? C31 C30 Ru1 71.8(2) . . ? C29 C30 Ru1 71.3(2) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? Ru1 C30 H30 129.8 . . ? C30 C31 C32 117.8(4) . . ? C30 C31 C35 122.4(4) . . ? C32 C31 C35 119.8(4) . . ? C30 C31 Ru1 70.5(2) . . ? C32 C31 Ru1 70.9(2) . . ? C35 C31 Ru1 129.8(3) . . ? C33 C32 C31 120.9(4) . . ? C33 C32 Ru1 70.8(2) . . ? C31 C32 Ru1 70.7(2) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? Ru1 C32 H32 132.0 . . ? C32 C33 C28 121.4(4) . . ? C32 C33 Ru1 72.1(2) . . ? C28 C33 Ru1 71.9(2) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? Ru1 C33 H33 129.1 . . ? C28 C34 H34A 109.5 . . ? C28 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 C37 113.4(4) . . ? C31 C35 C36 108.0(4) . . ? C37 C35 C36 111.9(4) . . ? C31 C35 H35 107.7 . . ? C37 C35 H35 107.7 . . ? C36 C35 H35 107.7 . . ? 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 . . ? Cl3 C38 Cl2 111.4(3) . . ? Cl3 C38 H38A 109.3 . . ? Cl2 C38 H38A 109.3 . . ? Cl3 C38 H38B 109.3 . . ? Cl2 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? 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 N3 Ru1 O1 C1 -16.9(3) . . . . ? C30 Ru1 O1 C1 -113.1(3) . . . . ? C33 Ru1 O1 C1 154.6(3) . . . . ? C29 Ru1 O1 C1 -115.4(4) . . . . ? C31 Ru1 O1 C1 -139.1(3) . . . . ? C32 Ru1 O1 C1 -177.5(3) . . . . ? C28 Ru1 O1 C1 149.8(4) . . . . ? Cl1 Ru1 O1 C1 67.1(3) . . . . ? C1 N1 N2 C8 0.8(5) . . . . ? C2 N1 N2 C8 178.7(4) . . . . ? O1 Ru1 N3 C11 14.6(4) . . . . ? C30 Ru1 N3 C11 132.4(4) . . . . ? C33 Ru1 N3 C11 -146.9(4) . . . . ? C29 Ru1 N3 C11 170.8(4) . . . . ? C31 Ru1 N3 C11 103.3(4) . . . . ? C32 Ru1 N3 C11 98.6(5) . . . . ? C28 Ru1 N3 C11 -158.6(3) . . . . ? Cl1 Ru1 N3 C11 -70.2(4) . . . . ? O1 Ru1 N3 C18 -171.5(3) . . . . ? C30 Ru1 N3 C18 -53.7(3) . . . . ? C33 Ru1 N3 C18 27.1(5) . . . . ? C29 Ru1 N3 C18 -15.3(3) . . . . ? C31 Ru1 N3 C18 -82.8(3) . . . . ? C32 Ru1 N3 C18 -87.5(5) . . . . ? C28 Ru1 N3 C18 15.3(4) . . . . ? Cl1 Ru1 N3 C18 103.7(3) . . . . ? Ru1 O1 C1 N1 -168.3(3) . . . . ? Ru1 O1 C1 C10 14.3(6) . . . . ? N2 N1 C1 O1 -179.1(4) . . . . ? C2 N1 C1 O1 3.3(7) . . . . ? N2 N1 C1 C10 -1.2(5) . . . . ? C2 N1 C1 C10 -178.8(4) . . . . ? C1 N1 C2 C3 5.3(7) . . . . ? N2 N1 C2 C3 -172.2(4) . . . . ? C1 N1 C2 C7 -175.7(4) . . . . ? N2 N1 C2 C7 6.9(6) . . . . ? C7 C2 C3 C4 -1.3(7) . . . . ? N1 C2 C3 C4 177.7(4) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C4 C5 C6 C7 -0.7(7) . . . . ? C5 C6 C7 C2 -0.1(7) . . . . ? C3 C2 C7 C6 1.1(7) . . . . ? N1 C2 C7 C6 -178.0(4) . . . . ? N1 N2 C8 C10 -0.1(5) . . . . ? N1 N2 C8 C9 178.9(4) . . . . ? O1 C1 C10 C11 -1.1(8) . . . . ? N1 C1 C10 C11 -178.7(4) . . . . ? O1 C1 C10 C8 178.7(4) . . . . ? N1 C1 C10 C8 1.1(5) . . . . ? N2 C8 C10 C1 -0.6(5) . . . . ? C9 C8 C10 C1 -179.4(5) . . . . ? N2 C8 C10 C11 179.1(4) . . . . ? C9 C8 C10 C11 0.3(8) . . . . ? C18 N3 C11 C10 178.6(4) . . . . ? Ru1 N3 C11 C10 -7.6(6) . . . . ? C18 N3 C11 C12 -5.3(6) . . . . ? Ru1 N3 C11 C12 168.5(3) . . . . ? C1 C10 C11 N3 -2.9(7) . . . . ? C8 C10 C11 N3 177.4(4) . . . . ? C1 C10 C11 C12 -179.0(4) . . . . ? C8 C10 C11 C12 1.3(7) . . . . ? N3 C11 C12 C17 96.5(5) . . . . ? C10 C11 C12 C17 -87.3(5) . . . . ? N3 C11 C12 C13 -82.6(5) . . . . ? C10 C11 C12 C13 93.7(5) . . . . ? C17 C12 C13 C14 0.4(7) . . . . ? C11 C12 C13 C14 179.4(4) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C16 0.1(8) . . . . ? C14 C15 C16 C17 -0.1(8) . . . . ? C13 C12 C17 C16 -0.4(7) . . . . ? C11 C12 C17 C16 -179.4(4) . . . . ? C15 C16 C17 C12 0.3(8) . . . . ? C11 N3 C18 C19 97.5(5) . . . . ? Ru1 N3 C18 C19 -77.0(4) . . . . ? C11 N3 C18 C27 -84.0(5) . . . . ? Ru1 N3 C18 C27 101.5(4) . . . . ? C27 C18 C19 C20 0.8(7) . . . . ? N3 C18 C19 C20 179.3(4) . . . . ? C18 C19 C20 C21 -0.6(7) . . . . ? C19 C20 C21 C22 0.4(7) . . . . ? C20 C21 C22 C23 178.0(4) . . . . ? C20 C21 C22 C27 -0.6(7) . . . . ? C27 C22 C23 C24 -0.3(7) . . . . ? C21 C22 C23 C24 -178.8(4) . . . . ? C22 C23 C24 C25 -0.6(7) . . . . ? C23 C24 C25 C26 0.7(7) . . . . ? C24 C25 C26 C27 0.0(7) . . . . ? C19 C18 C27 C22 -0.9(6) . . . . ? N3 C18 C27 C22 -179.4(4) . . . . ? C19 C18 C27 C26 -179.6(4) . . . . ? N3 C18 C27 C26 1.9(6) . . . . ? C23 C22 C27 C18 -177.8(4) . . . . ? C21 C22 C27 C18 0.8(6) . . . . ? C23 C22 C27 C26 0.9(6) . . . . ? C21 C22 C27 C26 179.5(4) . . . . ? C25 C26 C27 C18 177.9(4) . . . . ? C25 C26 C27 C22 -0.8(6) . . . . ? O1 Ru1 C28 C29 137.9(3) . . . . ? N3 Ru1 C28 C29 -57.1(3) . . . . ? C30 Ru1 C28 C29 28.4(3) . . . . ? C33 Ru1 C28 C29 130.8(4) . . . . ? C31 Ru1 C28 C29 65.1(3) . . . . ? C32 Ru1 C28 C29 102.4(3) . . . . ? Cl1 Ru1 C28 C29 -141.0(2) . . . . ? O1 Ru1 C28 C33 7.0(4) . . . . ? N3 Ru1 C28 C33 172.0(2) . . . . ? C30 Ru1 C28 C33 -102.4(3) . . . . ? C29 Ru1 C28 C33 -130.8(4) . . . . ? C31 Ru1 C28 C33 -65.8(3) . . . . ? C32 Ru1 C28 C33 -28.5(2) . . . . ? Cl1 Ru1 C28 C33 88.2(2) . . . . ? O1 Ru1 C28 C34 -108.3(4) . . . . ? N3 Ru1 C28 C34 56.7(4) . . . . ? C30 Ru1 C28 C34 142.2(4) . . . . ? C33 Ru1 C28 C34 -115.3(5) . . . . ? C29 Ru1 C28 C34 113.8(5) . . . . ? C31 Ru1 C28 C34 178.9(4) . . . . ? C32 Ru1 C28 C34 -143.8(4) . . . . ? Cl1 Ru1 C28 C34 -27.2(4) . . . . ? C33 C28 C29 C30 0.9(6) . . . . ? C34 C28 C29 C30 -175.0(4) . . . . ? Ru1 C28 C29 C30 -52.5(4) . . . . ? C33 C28 C29 Ru1 53.4(3) . . . . ? C34 C28 C29 Ru1 -122.5(4) . . . . ? O1 Ru1 C29 C28 -130.9(3) . . . . ? N3 Ru1 C29 C28 131.8(3) . . . . ? C30 Ru1 C29 C28 -134.2(4) . . . . ? C33 Ru1 C29 C28 -30.4(2) . . . . ? C31 Ru1 C29 C28 -105.3(3) . . . . ? C32 Ru1 C29 C28 -67.0(3) . . . . ? Cl1 Ru1 C29 C28 46.2(3) . . . . ? O1 Ru1 C29 C30 3.3(5) . . . . ? N3 Ru1 C29 C30 -94.0(3) . . . . ? C33 Ru1 C29 C30 103.8(3) . . . . ? C31 Ru1 C29 C30 28.9(3) . . . . ? C32 Ru1 C29 C30 67.2(3) . . . . ? C28 Ru1 C29 C30 134.2(4) . . . . ? Cl1 Ru1 C29 C30 -179.6(2) . . . . ? C28 C29 C30 C31 -1.0(6) . . . . ? Ru1 C29 C30 C31 -54.3(3) . . . . ? C28 C29 C30 Ru1 53.2(4) . . . . ? O1 Ru1 C30 C31 -45.8(3) . . . . ? N3 Ru1 C30 C31 -137.6(3) . . . . ? C33 Ru1 C30 C31 67.2(3) . . . . ? C29 Ru1 C30 C31 132.7(4) . . . . ? C32 Ru1 C30 C31 30.8(3) . . . . ? C28 Ru1 C30 C31 104.9(3) . . . . ? Cl1 Ru1 C30 C31 133.5(3) . . . . ? O1 Ru1 C30 C29 -178.5(2) . . . . ? N3 Ru1 C30 C29 89.7(3) . . . . ? C33 Ru1 C30 C29 -65.4(3) . . . . ? C31 Ru1 C30 C29 -132.7(4) . . . . ? C32 Ru1 C30 C29 -101.9(3) . . . . ? C28 Ru1 C30 C29 -27.7(2) . . . . ? Cl1 Ru1 C30 C29 0.9(5) . . . . ? C29 C30 C31 C32 -0.7(6) . . . . ? Ru1 C30 C31 C32 -54.7(3) . . . . ? C29 C30 C31 C35 179.4(4) . . . . ? Ru1 C30 C31 C35 125.4(4) . . . . ? C29 C30 C31 Ru1 54.0(3) . . . . ? O1 Ru1 C31 C30 140.6(3) . . . . ? N3 Ru1 C31 C30 52.4(3) . . . . ? C33 Ru1 C31 C30 -102.5(3) . . . . ? C29 Ru1 C31 C30 -29.2(3) . . . . ? C32 Ru1 C31 C30 -130.2(4) . . . . ? C28 Ru1 C31 C30 -65.3(3) . . . . ? Cl1 Ru1 C31 C30 -142.1(3) . . . . ? O1 Ru1 C31 C32 -89.2(2) . . . . ? N3 Ru1 C31 C32 -177.5(2) . . . . ? C30 Ru1 C31 C32 130.2(4) . . . . ? C33 Ru1 C31 C32 27.7(2) . . . . ? C29 Ru1 C31 C32 100.9(3) . . . . ? C28 Ru1 C31 C32 64.8(3) . . . . ? Cl1 Ru1 C31 C32 -11.9(4) . . . . ? O1 Ru1 C31 C35 24.2(4) . . . . ? N3 Ru1 C31 C35 -64.1(5) . . . . ? C30 Ru1 C31 C35 -116.5(5) . . . . ? C33 Ru1 C31 C35 141.0(5) . . . . ? C29 Ru1 C31 C35 -145.7(5) . . . . ? C32 Ru1 C31 C35 113.4(5) . . . . ? C28 Ru1 C31 C35 178.2(4) . . . . ? Cl1 Ru1 C31 C35 101.5(4) . . . . ? C30 C31 C32 C33 2.5(6) . . . . ? C35 C31 C32 C33 -177.5(4) . . . . ? Ru1 C31 C32 C33 -52.0(3) . . . . ? C30 C31 C32 Ru1 54.5(3) . . . . ? C35 C31 C32 Ru1 -125.6(4) . . . . ? O1 Ru1 C32 C33 -135.4(3) . . . . ? N3 Ru1 C32 C33 140.7(4) . . . . ? C30 Ru1 C32 C33 104.0(3) . . . . ? C29 Ru1 C32 C33 66.1(3) . . . . ? C31 Ru1 C32 C33 134.2(4) . . . . ? C28 Ru1 C32 C33 29.2(3) . . . . ? Cl1 Ru1 C32 C33 -51.6(3) . . . . ? O1 Ru1 C32 C31 90.4(3) . . . . ? N3 Ru1 C32 C31 6.4(6) . . . . ? C30 Ru1 C32 C31 -30.3(2) . . . . ? C33 Ru1 C32 C31 -134.2(4) . . . . ? C29 Ru1 C32 C31 -68.2(3) . . . . ? C28 Ru1 C32 C31 -105.1(3) . . . . ? Cl1 Ru1 C32 C31 174.1(2) . . . . ? C31 C32 C33 C28 -2.7(6) . . . . ? Ru1 C32 C33 C28 -54.7(4) . . . . ? C31 C32 C33 Ru1 52.0(3) . . . . ? C29 C28 C33 C32 1.0(6) . . . . ? C34 C28 C33 C32 176.8(4) . . . . ? Ru1 C28 C33 C32 54.8(4) . . . . ? C29 C28 C33 Ru1 -53.8(3) . . . . ? C34 C28 C33 Ru1 122.0(4) . . . . ? O1 Ru1 C33 C32 50.7(3) . . . . ? N3 Ru1 C33 C32 -149.9(3) . . . . ? C30 Ru1 C33 C32 -65.7(3) . . . . ? C29 Ru1 C33 C32 -103.2(3) . . . . ? C31 Ru1 C33 C32 -28.5(3) . . . . ? C28 Ru1 C33 C32 -132.9(4) . . . . ? Cl1 Ru1 C33 C32 134.8(2) . . . . ? O1 Ru1 C33 C28 -176.5(2) . . . . ? N3 Ru1 C33 C28 -17.0(5) . . . . ? C30 Ru1 C33 C28 67.1(3) . . . . ? C29 Ru1 C33 C28 29.7(2) . . . . ? C31 Ru1 C33 C28 104.4(3) . . . . ? C32 Ru1 C33 C28 132.9(4) . . . . ? Cl1 Ru1 C33 C28 -92.3(2) . . . . ? C30 C31 C35 C37 -37.1(6) . . . . ? C32 C31 C35 C37 143.0(4) . . . . ? Ru1 C31 C35 C37 53.8(6) . . . . ? C30 C31 C35 C36 87.6(5) . . . . ? C32 C31 C35 C36 -92.3(5) . . . . ? Ru1 C31 C35 C36 178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.74 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.045 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.137 _iucr_refine_instructions_details ; TITL CC2 in P2(1)/n CELL 0.71073 14.5860 9.7760 23.3830 90.000 92.560 90.000 ZERR 4.00 0.0050 0.0030 0.0060 0.000 0.017 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O CL RU UNIT 152 144 12 4 12 4 REM ------------------------------------------------------------------------- REM Data measured on the marmux REM Crystal colour: yellow; Crystal habit: prismatic REM ------------------------------------------------------------------------- L.S. 10 OMIT -1 4 9 OMIT 4 3 1 OMIT 5 0 5 OMIT 1 2 15 OMIT -1 1 16 ACTA CONF SIZE 0.46 0.28 0.19 WPDB -2 BOND $H FMAP 2 PLAN 10 TEMP -133 WGHT 0.082500 FVAR 0.22543 MOLE 1 RU1 6 0.444774 0.635253 0.273784 11.00000 0.02274 0.02559 = 0.02552 0.00332 -0.00104 -0.00058 CL1 5 0.418675 0.404428 0.236054 11.00000 0.04633 0.02862 = 0.03327 0.00083 -0.00315 -0.00371 O1 4 0.347528 0.581913 0.332425 11.00000 0.02499 0.03349 = 0.03391 0.01395 0.00519 0.00181 N1 3 0.293855 0.438313 0.402507 11.00000 0.02482 0.03013 = 0.02771 0.00520 0.00330 -0.00051 N2 3 0.327727 0.340957 0.442013 11.00000 0.03312 0.03326 = 0.02710 0.00703 0.00124 0.00020 N3 3 0.546270 0.538307 0.327253 11.00000 0.02131 0.03114 = 0.02937 0.00685 -0.00379 0.00292 C1 1 0.362118 0.490149 0.370697 11.00000 0.02817 0.02680 = 0.02385 0.00081 -0.00103 -0.00054 C2 1 0.197816 0.465424 0.399428 11.00000 0.02383 0.03128 = 0.02682 -0.00315 0.00042 -0.00388 C3 1 0.157206 0.547679 0.357203 11.00000 0.02954 0.02812 = 0.03429 -0.00398 0.00171 -0.00099 AFIX 43 H3 2 0.194117 0.590590 0.329952 11.00000 -1.20000 AFIX 0 C4 1 0.063802 0.567544 0.354520 11.00000 0.03064 0.03437 = 0.04203 0.00508 0.00572 0.00375 AFIX 43 H4 2 0.036712 0.623519 0.325165 11.00000 -1.20000 AFIX 0 C5 1 0.008571 0.506833 0.394168 11.00000 0.03073 0.03555 = 0.04912 -0.00403 0.00661 -0.00147 AFIX 43 H5 2 -0.055986 0.520372 0.391952 11.00000 -1.20000 AFIX 0 C6 1 0.049215 0.425745 0.437262 11.00000 0.03655 0.03086 = 0.04394 0.00010 0.00986 -0.00926 AFIX 43 H6 2 0.012050 0.384589 0.464831 11.00000 -1.20000 AFIX 0 C7 1 0.142890 0.404547 0.440342 11.00000 0.04229 0.02825 = 0.03237 -0.00036 0.00437 -0.00679 AFIX 43 H7 2 0.170078 0.349230 0.469887 11.00000 -1.20000 AFIX 0 C8 1 0.416832 0.334712 0.434803 11.00000 0.03420 0.02909 = 0.02658 -0.00333 0.00371 0.00232 C9 1 0.473394 0.239216 0.472600 11.00000 0.03820 0.05020 = 0.03502 0.01718 0.00071 0.00388 AFIX 33 H9A 2 0.513466 0.292663 0.498889 11.00000 -1.50000 H9B 2 0.510910 0.180869 0.448848 11.00000 -1.50000 H9C 2 0.432612 0.181976 0.494658 11.00000 -1.50000 AFIX 0 C10 1 0.444508 0.427030 0.390541 11.00000 0.02507 0.02969 = 0.02417 -0.00019 0.00128 -0.00005 C11 1 0.532450 0.453805 0.369794 11.00000 0.03020 0.02233 = 0.02473 0.00179 -0.00128 0.00043 C12 1 0.613088 0.375027 0.395306 11.00000 0.02592 0.02655 = 0.02676 0.00258 -0.00144 0.00270 C13 1 0.638201 0.256462 0.367601 11.00000 0.04086 0.03635 = 0.02398 0.00023 -0.00726 0.00640 AFIX 43 H13 2 0.604666 0.227159 0.334051 11.00000 -1.20000 AFIX 0 C14 1 0.712407 0.180679 0.388968 11.00000 0.04802 0.04747 = 0.03091 -0.00249 -0.00276 0.02231 AFIX 43 H14 2 0.729349 0.099201 0.369978 11.00000 -1.20000 AFIX 0 C15 1 0.762223 0.222629 0.437836 11.00000 0.04119 0.04777 = 0.03940 0.00700 -0.00800 0.01574 AFIX 43 H15 2 0.813116 0.170522 0.452301 11.00000 -1.20000 AFIX 0 C16 1 0.736964 0.340446 0.464992 11.00000 0.04564 0.04069 = 0.03338 0.00152 -0.01474 0.00209 AFIX 43 H16 2 0.770541 0.369886 0.498505 11.00000 -1.20000 AFIX 0 C17 1 0.662459 0.417096 0.443748 11.00000 0.03943 0.03271 = 0.03649 0.00448 -0.00744 -0.00081 AFIX 43 H17 2 0.645645 0.498647 0.462730 11.00000 -1.20000 AFIX 0 C18 1 0.639875 0.558612 0.311277 11.00000 0.02109 0.03363 = 0.03143 0.00362 -0.00540 0.00117 C19 1 0.672925 0.485967 0.265887 11.00000 0.03712 0.03448 = 0.02968 0.00138 0.00190 0.00538 AFIX 43 H19 2 0.634413 0.422322 0.245666 11.00000 -1.20000 AFIX 0 C20 1 0.763446 0.506230 0.249653 11.00000 0.03696 0.03391 = 0.02962 0.00324 0.00251 0.00553 AFIX 43 H20 2 0.785714 0.455211 0.218602 11.00000 -1.20000 AFIX 0 C21 1 0.819833 0.597426 0.277501 11.00000 0.02948 0.04317 = 0.03107 0.00317 0.00526 0.00914 AFIX 43 H21 2 0.880710 0.610026 0.265644 11.00000 -1.20000 AFIX 0 C22 1 0.787652 0.674722 0.324765 11.00000 0.02775 0.02866 = 0.03083 0.00367 -0.00224 0.00248 C23 1 0.844492 0.767081 0.355942 11.00000 0.02849 0.04101 = 0.03554 0.00556 -0.00385 -0.00289 AFIX 43 H23 2 0.905865 0.780371 0.345120 11.00000 -1.20000 AFIX 0 C24 1 0.813418 0.837422 0.401086 11.00000 0.03269 0.03560 = 0.03920 0.00202 -0.00624 -0.00229 AFIX 43 H24 2 0.853197 0.898620 0.421726 11.00000 -1.20000 AFIX 0 C25 1 0.721428 0.820084 0.417753 11.00000 0.03173 0.03448 = 0.03234 -0.00040 -0.00220 0.00151 AFIX 43 H25 2 0.699939 0.870561 0.449185 11.00000 -1.20000 AFIX 0 C26 1 0.663984 0.731349 0.388814 11.00000 0.03073 0.03114 = 0.03413 -0.00084 0.00079 0.00084 AFIX 43 H26 2 0.602716 0.720363 0.400214 11.00000 -1.20000 AFIX 0 C27 1 0.695624 0.654475 0.341221 11.00000 0.03195 0.03141 = 0.03009 0.00841 -0.00222 0.00001 C28 1 0.485618 0.709712 0.189289 11.00000 0.03531 0.02672 = 0.02336 0.00719 0.00338 0.00327 C29 1 0.542022 0.770281 0.232468 11.00000 0.02325 0.02842 = 0.03171 0.00548 0.00144 -0.00123 AFIX 43 H29 2 0.606784 0.764837 0.230185 11.00000 -1.20000 AFIX 0 C30 1 0.504265 0.840032 0.279844 11.00000 0.03221 0.02067 = 0.03076 0.00328 0.00011 -0.00568 AFIX 43 H30 2 0.544132 0.878699 0.308741 11.00000 -1.20000 AFIX 0 C31 1 0.408077 0.851903 0.284018 11.00000 0.03144 0.01957 = 0.02961 0.00135 0.00015 0.00294 C32 1 0.350043 0.792724 0.238667 11.00000 0.02571 0.02318 = 0.03017 0.00815 -0.00489 0.00653 AFIX 43 H32 2 0.285313 0.802361 0.239559 11.00000 -1.20000 AFIX 0 C33 1 0.387995 0.721615 0.193600 11.00000 0.03422 0.02602 = 0.02702 0.00580 -0.00563 -0.00019 AFIX 43 H33 2 0.348427 0.680282 0.165222 11.00000 -1.20000 AFIX 0 C34 1 0.527078 0.627762 0.142922 11.00000 0.03576 0.03759 = 0.03082 -0.00121 0.00158 0.00281 AFIX 33 H34A 2 0.593855 0.624461 0.149578 11.00000 -1.50000 H34B 2 0.512249 0.670576 0.105756 11.00000 -1.50000 H34C 2 0.502270 0.534608 0.143081 11.00000 -1.50000 AFIX 0 C35 1 0.365425 0.923010 0.333256 11.00000 0.03216 0.03290 = 0.03114 0.00133 -0.00188 0.00038 AFIX 13 H35 2 0.301940 0.885962 0.336375 11.00000 -1.20000 AFIX 0 C36 1 0.357225 1.074291 0.318740 11.00000 0.05651 0.03623 = 0.04255 0.00288 0.01139 0.01363 AFIX 33 H36A 2 0.417660 1.110192 0.309800 11.00000 -1.50000 H36B 2 0.334140 1.123945 0.351543 11.00000 -1.50000 H36C 2 0.314591 1.086214 0.285524 11.00000 -1.50000 AFIX 0 C37 1 0.416961 0.899607 0.390363 11.00000 0.05155 0.06217 = 0.02812 -0.00939 -0.00626 0.01997 AFIX 33 H37A 2 0.423530 0.801143 0.397263 11.00000 -1.50000 H37B 2 0.382702 0.940906 0.421073 11.00000 -1.50000 H37C 2 0.477873 0.941684 0.389569 11.00000 -1.50000 AFIX 0 MOLE 2 C38 1 0.147767 -0.120190 0.420835 11.00000 0.05089 0.03806 = 0.03164 0.00165 -0.00256 -0.00044 AFIX 23 H38A 2 0.131856 -0.119450 0.379231 11.00000 -1.20000 H38B 2 0.193702 -0.193258 0.428434 11.00000 -1.20000 AFIX 0 CL2 5 0.195926 0.039599 0.441234 11.00000 0.04522 0.03986 = 0.03789 0.00044 -0.00535 -0.00368 CL3 5 0.048658 -0.155914 0.458499 11.00000 0.04538 0.06012 = 0.04867 0.01324 -0.00780 -0.01219 MOLE 0 HKLF 4 REM CC2 in P2(1)/n REM R1 = 0.0592 for 5100 Fo > 4sig(Fo) and 0.0952 for all 7713 data REM 415 parameters refined using 0 restraints END WGHT 0.0825 0.0000 REM Highest difference peak 1.045, deepest hole -1.046, 1-sigma level 0.137 Q1 1 0.5030 0.6459 0.3209 11.00000 0.05 1.05 Q2 1 0.3850 0.6346 0.2313 11.00000 0.05 1.01 Q3 1 0.4436 0.5035 0.2707 11.00000 0.05 0.93 Q4 1 0.4235 0.5216 0.2510 11.00000 0.05 0.87 Q5 1 0.5363 0.6366 0.2719 11.00000 0.05 0.85 Q6 1 0.4841 0.5188 0.2877 11.00000 0.05 0.82 Q7 1 0.4454 0.7196 0.3182 11.00000 0.05 0.81 Q8 1 0.5225 0.7082 0.2927 11.00000 0.05 0.77 Q9 1 0.3550 0.6358 0.2769 11.00000 0.05 0.74 Q10 1 0.3607 0.5819 0.2674 11.00000 0.05 0.73 ; data_8 _audit_update_record ; 2013-05-08 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H42 Cl N3 O Ru' _chemical_formula_sum 'C37 H42 Cl N3 O Ru' _chemical_formula_weight 681.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.337(2) _cell_length_b 20.592(4) _cell_length_c 14.3231(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.579(12) _cell_angle_gamma 90.00 _cell_volume 3340.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 159 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5591 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2008, Bruker AXS, 2008' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56695 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7635 _reflns_number_gt 5112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+9.1375P] 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 7635 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.44335(4) 0.157656(19) 0.13505(2) 0.03840(12) Uani 1 1 d . . . Cl1 Cl 0.55510(12) 0.25164(6) 0.19024(9) 0.0488(3) Uani 1 1 d . . . O1 O 0.3100(3) 0.19510(16) 0.2132(2) 0.0396(8) Uani 1 1 d . B . N1 N 0.2003(3) 0.20204(19) 0.3447(2) 0.0336(9) Uani 1 1 d . B . N2 N 0.2064(4) 0.1818(2) 0.4377(3) 0.0467(11) Uani 1 1 d . B . N3 N 0.5161(3) 0.11230(18) 0.2581(3) 0.0363(9) Uani 1 1 d . B . C1 C 0.2981(4) 0.1815(2) 0.2993(3) 0.0294(9) Uani 1 1 d . . . C2 C 0.0958(4) 0.2328(2) 0.3086(3) 0.0365(10) Uani 1 1 d . . . C3 C 0.0923(5) 0.2645(3) 0.2229(4) 0.0491(13) Uani 1 1 d . B . H3 H 0.1611 0.2673 0.1876 0.059 Uiso 1 1 calc R . . C4 C -0.0133(6) 0.2923(4) 0.1893(5) 0.080(2) Uani 1 1 d . . . H4 H -0.0167 0.3138 0.1305 0.096 Uiso 1 1 calc R B . C5 C -0.1132(6) 0.2888(4) 0.2408(6) 0.091(2) Uani 1 1 d . B . H5 H -0.1844 0.3086 0.2180 0.110 Uiso 1 1 calc R . . C6 C -0.1098(6) 0.2567(3) 0.3250(6) 0.077(2) Uani 1 1 d . . . H6 H -0.1792 0.2537 0.3595 0.092 Uiso 1 1 calc R B . C7 C -0.0055(5) 0.2287(3) 0.3601(4) 0.0541(14) Uani 1 1 d . B . H7 H -0.0032 0.2069 0.4186 0.065 Uiso 1 1 calc R . . C8 C 0.3064(4) 0.1497(3) 0.4489(3) 0.0462(13) Uani 1 1 d . . . C9 C 0.3349(6) 0.1235(4) 0.5458(4) 0.080(2) Uani 1 1 d . B . H9A H 0.2747 0.1380 0.5881 0.120 Uiso 1 1 calc R . . H9B H 0.4125 0.1395 0.5682 0.120 Uiso 1 1 calc R . . H9C H 0.3361 0.0759 0.5438 0.120 Uiso 1 1 calc R . . C10 C 0.3710(4) 0.1467(2) 0.3646(3) 0.0335(10) Uani 1 1 d . B . C11 C 0.4788(4) 0.1140(2) 0.3437(3) 0.0325(10) Uani 1 1 d . . . C12 C 0.5515(5) 0.0835(2) 0.4233(3) 0.0448(12) Uani 1 1 d . A . H12A H 0.5979 0.0469 0.3993 0.054 Uiso 1 1 calc R . . H12B H 0.4983 0.0661 0.4702 0.054 Uiso 1 1 calc R . . C13 C 0.6361(5) 0.1343(3) 0.4701(4) 0.0670(19) Uani 1 1 d . . . H13A H 0.6546 0.1672 0.4225 0.080 Uiso 0.401(10) 1 calc PR A 1 H13B H 0.5932 0.1568 0.5194 0.080 Uiso 0.401(10) 1 calc PR A 1 H13C H 0.5914 0.1725 0.4910 0.080 Uiso 0.599(10) 1 d PR A 2 H13D H 0.6952 0.1489 0.4259 0.080 Uiso 0.599(10) 1 d PR A 2 C14A C 0.7483(14) 0.1099(9) 0.5123(13) 0.054(5) Uani 0.401(10) 1 d P A 1 H14A H 0.8012 0.1467 0.5294 0.065 Uiso 0.401(10) 1 calc PR A 1 H14B H 0.7883 0.0820 0.4672 0.065 Uiso 0.401(10) 1 calc PR A 1 C15A C 0.7214(17) 0.0724(10) 0.5962(15) 0.066(6) Uani 0.401(10) 1 d P A 1 H15A H 0.6615 0.0392 0.5782 0.079 Uiso 0.401(10) 1 calc PR A 1 H15B H 0.6856 0.1021 0.6413 0.079 Uiso 0.401(10) 1 calc PR A 1 C16A C 0.8270(16) 0.0383(11) 0.6456(15) 0.077(6) Uani 0.401(10) 1 d P A 1 H16A H 0.8561 0.0042 0.6036 0.092 Uiso 0.401(10) 1 calc PR A 1 H16B H 0.8913 0.0703 0.6560 0.092 Uiso 0.401(10) 1 calc PR A 1 C17A C 0.8016(18) 0.0078(12) 0.7370(17) 0.127(10) Uani 0.401(10) 1 d P A 1 H17A H 0.7814 0.0417 0.7816 0.190 Uiso 0.401(10) 1 calc PR A 1 H17B H 0.8715 -0.0159 0.7611 0.190 Uiso 0.401(10) 1 calc PR A 1 H17C H 0.7352 -0.0224 0.7283 0.190 Uiso 0.401(10) 1 calc PR A 1 C14B C 0.7019(15) 0.0969(9) 0.5597(10) 0.080(6) Uani 0.599(10) 1 d P A 2 H14C H 0.7324 0.1294 0.6056 0.096 Uiso 0.599(10) 1 calc PR A 2 H14D H 0.6440 0.0692 0.5908 0.096 Uiso 0.599(10) 1 calc PR A 2 C15B C 0.8019(9) 0.0557(6) 0.5286(7) 0.068(4) Uani 0.599(10) 1 d P A 2 H15C H 0.8605 0.0847 0.5008 0.082 Uiso 0.599(10) 1 calc PR A 2 H15D H 0.7707 0.0266 0.4783 0.082 Uiso 0.599(10) 1 calc PR A 2 C16B C 0.8674(13) 0.0132(9) 0.6041(9) 0.096(6) Uani 0.599(10) 1 d P A 2 H16C H 0.9037 0.0432 0.6513 0.115 Uiso 0.599(10) 1 calc PR A 2 H16D H 0.8067 -0.0121 0.6359 0.115 Uiso 0.599(10) 1 calc PR A 2 C17B C 0.9531(18) -0.0294(8) 0.5797(13) 0.171(10) Uani 0.599(10) 1 d P A 2 H17D H 0.9272 -0.0522 0.5223 0.257 Uiso 0.599(10) 1 calc PR A 2 H17E H 0.9673 -0.0610 0.6301 0.257 Uiso 0.599(10) 1 calc PR A 2 H17F H 1.0261 -0.0056 0.5691 0.257 Uiso 0.599(10) 1 calc PR A 2 C18 C 0.6268(5) 0.0792(2) 0.2438(4) 0.0476(13) Uani 1 1 d . . . C19 C 0.7292(5) 0.1141(3) 0.2375(5) 0.0630(17) Uani 1 1 d . B . H19 H 0.7278 0.1601 0.2436 0.076 Uiso 1 1 calc R . . C20 C 0.8367(6) 0.0820(3) 0.2222(6) 0.082(2) Uani 1 1 d . . . H20 H 0.9072 0.1065 0.2179 0.098 Uiso 1 1 calc R B . C21 C 0.8403(6) 0.0159(3) 0.2134(5) 0.077(2) Uani 1 1 d . B . H21 H 0.9135 -0.0049 0.2037 0.092 Uiso 1 1 calc R . . C22 C 0.7367(5) -0.0216(3) 0.2186(4) 0.0543(15) Uani 1 1 d . . . C23 C 0.7366(6) -0.0904(3) 0.2113(4) 0.0599(16) Uani 1 1 d . B . H23 H 0.8087 -0.1124 0.2017 0.072 Uiso 1 1 calc R . . C24 C 0.6358(6) -0.1254(3) 0.2176(3) 0.0586(17) Uani 1 1 d . . . H24 H 0.6385 -0.1714 0.2130 0.070 Uiso 1 1 calc R B . C25 C 0.5288(6) -0.0946(2) 0.2308(3) 0.0482(14) Uani 1 1 d . B . H25 H 0.4589 -0.1198 0.2341 0.058 Uiso 1 1 calc R . . C26 C 0.5229(5) -0.0281(2) 0.2389(3) 0.0419(12) Uani 1 1 d . . . H26 H 0.4491 -0.0077 0.2483 0.050 Uiso 1 1 calc R B . C27 C 0.6267(5) 0.0103(2) 0.2334(3) 0.0442(12) Uani 1 1 d . B . C28A C 0.5215(7) 0.1491(6) 0.0003(8) 0.052(4) Uani 0.621(12) 1 d PG B 1 C29A C 0.4298(9) 0.1935(5) -0.0122(8) 0.041(3) Uani 0.621(12) 1 d PG B 1 H29A H 0.4450 0.2357 -0.0357 0.049 Uiso 0.621(12) 1 calc PR B 1 C30A C 0.3159(8) 0.1762(5) 0.0099(7) 0.039(3) Uani 0.621(12) 1 d PG B 1 H30A H 0.2531 0.2065 0.0014 0.047 Uiso 0.621(12) 1 calc PR B 1 C31A C 0.2937(8) 0.1145(5) 0.0444(7) 0.038(3) Uani 0.621(12) 1 d PG B 1 C32A C 0.3854(11) 0.0701(5) 0.0568(8) 0.030(2) Uani 0.621(12) 1 d PG B 1 H32A H 0.3703 0.0280 0.0804 0.036 Uiso 0.621(12) 1 calc PR B 1 C33A C 0.4994(10) 0.0874(6) 0.0348(9) 0.038(3) Uani 0.621(12) 1 d PG B 1 H33A H 0.5621 0.0571 0.0433 0.045 Uiso 0.621(12) 1 calc PR B 1 C34A C 0.6528(11) 0.1720(6) -0.0191(8) 0.058(3) Uani 0.621(12) 1 d P B 1 H34A H 0.6638 0.1722 -0.0865 0.086 Uiso 0.621(12) 1 calc PR B 1 H34B H 0.7094 0.1419 0.0115 0.086 Uiso 0.621(12) 1 calc PR B 1 H34C H 0.6658 0.2158 0.0060 0.086 Uiso 0.621(12) 1 calc PR B 1 C35A C 0.1700(11) 0.1001(8) 0.0808(10) 0.046(3) Uani 0.621(12) 1 d P B 1 H35A H 0.1456 0.1406 0.1134 0.055 Uiso 0.621(12) 1 calc PR B 1 C36A C 0.0801(9) 0.0912(8) -0.0021(7) 0.075(4) Uani 0.621(12) 1 d P B 1 H36A H 0.0999 0.0522 -0.0371 0.112 Uiso 0.621(12) 1 calc PR B 1 H36B H 0.0824 0.1292 -0.0432 0.112 Uiso 0.621(12) 1 calc PR B 1 H36C H 0.0006 0.0866 0.0215 0.112 Uiso 0.621(12) 1 calc PR B 1 C37A C 0.1674(9) 0.0472(6) 0.1526(8) 0.079(4) Uani 0.621(12) 1 d P B 1 H37A H 0.1894 0.0058 0.1242 0.118 Uiso 0.621(12) 1 calc PR B 1 H37B H 0.0877 0.0437 0.1759 0.118 Uiso 0.621(12) 1 calc PR B 1 H37C H 0.2235 0.0573 0.2046 0.118 Uiso 0.621(12) 1 calc PR B 1 C28B C 0.5677(13) 0.1456(9) 0.0172(12) 0.032(4) Uani 0.379(12) 1 d PG B 2 C29B C 0.4806(17) 0.1919(7) -0.0016(13) 0.056(8) Uani 0.379(12) 1 d PG B 2 H29B H 0.5017 0.2339 -0.0227 0.067 Uiso 0.379(12) 1 calc PR B 2 C30B C 0.3628(15) 0.1767(8) 0.0103(14) 0.041(6) Uani 0.379(12) 1 d PG B 2 H30B H 0.3033 0.2083 -0.0026 0.049 Uiso 0.379(12) 1 calc PR B 2 C31B C 0.3321(13) 0.1152(10) 0.0411(16) 0.083(11) Uani 0.379(12) 1 d PG B 2 C32B C 0.4191(18) 0.0689(8) 0.0599(17) 0.065(10) Uani 0.379(12) 1 d PG B 2 H32B H 0.3981 0.0269 0.0810 0.078 Uiso 0.379(12) 1 calc PR B 2 C33B C 0.5370(16) 0.0841(8) 0.0480(14) 0.037(5) Uani 0.379(12) 1 d PG B 2 H33B H 0.5965 0.0525 0.0609 0.045 Uiso 0.379(12) 1 calc PR B 2 C34B C 0.705(3) 0.1590(19) 0.0131(18) 0.134(14) Uani 0.379(12) 1 d P B 2 H34D H 0.7301 0.1527 -0.0510 0.201 Uiso 0.379(12) 1 calc PR B 2 H34E H 0.7488 0.1288 0.0550 0.201 Uiso 0.379(12) 1 calc PR B 2 H34F H 0.7224 0.2037 0.0329 0.201 Uiso 0.379(12) 1 calc PR B 2 C35B C 0.212(5) 0.101(3) 0.056(3) 0.16(3) Uani 0.379(12) 1 d P B 2 H35B H 0.2122 0.1007 0.1261 0.195 Uiso 0.379(12) 1 calc PR B 2 C36B C 0.160(3) 0.0280(19) 0.030(3) 0.19(2) Uani 0.379(12) 1 d P B 2 H36D H 0.2084 -0.0049 0.0630 0.281 Uiso 0.379(12) 1 calc PR B 2 H36E H 0.1622 0.0210 -0.0375 0.281 Uiso 0.379(12) 1 calc PR B 2 H36F H 0.0782 0.0247 0.0492 0.281 Uiso 0.379(12) 1 calc PR B 2 C37B C 0.122(4) 0.138(3) 0.036(3) 0.20(3) Uani 0.379(12) 1 d P B 2 H37D H 0.0532 0.1214 0.0682 0.301 Uiso 0.379(12) 1 calc PR B 2 H37E H 0.1041 0.1362 -0.0320 0.301 Uiso 0.379(12) 1 calc PR B 2 H37F H 0.1385 0.1823 0.0549 0.301 Uiso 0.379(12) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0554(3) 0.0342(2) 0.02652(18) -0.00594(17) 0.01213(15) -0.0107(2) Cl1 0.0493(8) 0.0334(6) 0.0640(8) -0.0114(6) 0.0070(6) -0.0050(6) O1 0.0393(19) 0.055(2) 0.0243(15) 0.0048(14) 0.0049(13) 0.0028(16) N1 0.030(2) 0.044(2) 0.0258(18) -0.0011(16) -0.0009(15) -0.0018(17) N2 0.044(3) 0.073(3) 0.0234(19) 0.0022(19) 0.0050(17) 0.005(2) N3 0.039(2) 0.032(2) 0.037(2) -0.0105(17) 0.0027(17) -0.0038(17) C1 0.031(2) 0.034(2) 0.024(2) -0.0039(17) 0.0020(17) -0.0077(18) C2 0.029(3) 0.032(2) 0.047(3) -0.008(2) -0.002(2) -0.0019(19) C3 0.033(3) 0.057(3) 0.057(3) 0.010(3) -0.003(2) 0.001(2) C4 0.066(5) 0.082(5) 0.090(5) 0.027(4) -0.008(4) 0.013(4) C5 0.050(4) 0.088(6) 0.135(7) 0.022(5) -0.005(4) 0.028(4) C6 0.044(4) 0.069(4) 0.119(6) 0.004(4) 0.017(4) 0.010(3) C7 0.045(3) 0.050(3) 0.068(4) -0.003(3) 0.011(3) 0.005(3) C8 0.044(3) 0.071(4) 0.023(2) 0.001(2) 0.000(2) 0.010(3) C9 0.086(5) 0.127(6) 0.028(3) 0.017(3) 0.013(3) 0.045(4) C10 0.041(3) 0.038(3) 0.0208(19) -0.0027(18) -0.0007(18) -0.003(2) C11 0.035(3) 0.033(2) 0.029(2) -0.0082(18) -0.0052(18) -0.0029(19) C12 0.053(3) 0.048(3) 0.033(2) -0.013(2) -0.009(2) 0.009(2) C13 0.058(4) 0.062(4) 0.078(4) -0.034(3) -0.036(3) 0.020(3) C14A 0.037(9) 0.067(11) 0.059(11) -0.010(9) 0.002(7) -0.003(8) C15A 0.032(10) 0.082(13) 0.081(15) 0.013(10) -0.023(9) -0.006(9) C16A 0.044(10) 0.093(15) 0.091(15) 0.056(12) -0.019(9) 0.002(9) C17A 0.078(15) 0.14(2) 0.16(2) 0.053(18) -0.056(14) -0.031(14) C14B 0.063(10) 0.112(14) 0.061(11) -0.056(10) -0.031(8) 0.042(10) C15B 0.061(7) 0.093(9) 0.048(6) -0.016(5) -0.015(5) 0.033(6) C16B 0.067(9) 0.166(16) 0.053(7) -0.009(8) -0.017(6) 0.054(9) C17B 0.21(2) 0.100(13) 0.187(19) -0.035(12) -0.128(17) 0.065(14) C18 0.056(3) 0.038(3) 0.050(3) -0.008(2) 0.015(3) 0.001(2) C19 0.050(4) 0.039(3) 0.102(5) -0.011(3) 0.028(3) -0.007(3) C20 0.054(4) 0.057(4) 0.138(7) -0.010(4) 0.043(4) -0.007(3) C21 0.072(5) 0.053(4) 0.109(6) -0.004(4) 0.043(4) 0.009(3) C22 0.073(4) 0.043(3) 0.049(3) -0.001(2) 0.024(3) 0.007(3) C23 0.097(5) 0.047(3) 0.038(3) -0.002(2) 0.021(3) 0.013(3) C24 0.118(6) 0.035(3) 0.023(2) 0.001(2) 0.003(3) -0.001(3) C25 0.082(4) 0.035(3) 0.026(2) 0.004(2) -0.015(2) -0.008(3) C26 0.064(3) 0.038(3) 0.023(2) -0.0009(19) -0.004(2) -0.007(2) C27 0.058(3) 0.038(3) 0.037(3) -0.009(2) 0.009(2) -0.010(2) C28A 0.045(8) 0.079(10) 0.031(5) -0.022(6) 0.004(6) -0.040(9) C29A 0.053(10) 0.047(6) 0.024(5) 0.004(4) 0.001(5) -0.028(5) C30A 0.029(7) 0.072(8) 0.015(4) 0.004(4) -0.009(4) -0.012(5) C31A 0.035(7) 0.061(7) 0.019(5) 0.000(4) 0.003(4) -0.025(5) C32A 0.036(6) 0.039(6) 0.017(5) -0.013(4) 0.010(4) -0.010(4) C33A 0.026(7) 0.052(7) 0.036(6) -0.022(5) 0.004(5) -0.009(5) C34A 0.054(8) 0.079(8) 0.041(6) -0.021(5) 0.022(5) -0.026(6) C35A 0.034(6) 0.066(7) 0.038(8) -0.002(5) -0.001(5) -0.021(5) C36A 0.039(6) 0.126(12) 0.059(6) -0.011(7) 0.001(5) -0.018(6) C37A 0.059(7) 0.104(10) 0.074(7) 0.030(7) 0.014(5) -0.022(6) C28B 0.023(9) 0.040(8) 0.033(9) -0.019(6) 0.017(7) -0.022(7) C29B 0.11(2) 0.036(11) 0.024(9) -0.011(7) 0.011(11) -0.049(13) C30B 0.053(18) 0.020(8) 0.046(10) -0.015(6) -0.017(10) -0.004(8) C31B 0.047(17) 0.12(2) 0.080(17) -0.047(18) -0.001(13) -0.044(17) C32B 0.09(2) 0.064(16) 0.042(12) 0.002(11) -0.007(13) -0.044(13) C33B 0.047(13) 0.041(9) 0.024(8) -0.015(6) 0.004(8) 0.003(8) C34B 0.09(2) 0.25(4) 0.058(16) 0.044(19) 0.043(14) 0.02(2) C35B 0.30(9) 0.16(4) 0.033(18) -0.020(18) -0.02(4) -0.01(5) C36B 0.13(3) 0.22(4) 0.21(4) -0.12(3) 0.05(3) -0.06(3) C37B 0.20(5) 0.32(7) 0.09(3) -0.07(3) 0.03(3) -0.16(5) _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 C31B 2.004(19) . ? Ru1 C30B 2.008(18) . ? Ru1 O1 2.070(3) . ? Ru1 N3 2.128(4) . ? Ru1 C32B 2.13(2) . ? Ru1 C29B 2.140(18) . ? Ru1 C33A 2.154(11) . ? Ru1 C28A 2.167(11) . ? Ru1 C32A 2.207(11) . ? Ru1 C29A 2.233(10) . ? Ru1 C33B 2.257(18) . ? Ru1 C28B 2.261(16) . ? O1 C1 1.277(5) . ? N1 C1 1.376(5) . ? N1 N2 1.394(5) . ? N1 C2 1.420(6) . ? N2 C8 1.316(6) . ? N3 C11 1.316(5) . ? N3 C18 1.452(6) . ? C1 C10 1.416(6) . ? C2 C3 1.390(7) . ? C2 C7 1.395(7) . ? C3 C4 1.393(8) . ? C3 H3 0.9500 . ? C4 C5 1.380(9) . ? C4 H4 0.9500 . ? C5 C6 1.374(10) . ? C5 H5 0.9500 . ? C6 C7 1.390(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.441(6) . ? C8 C9 1.510(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.438(6) . ? C11 C12 1.512(6) . ? C12 C13 1.550(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14A 1.471(18) . ? C13 C14B 1.646(16) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 H13C 0.9901 . ? C13 H13D 0.9900 . ? C14A C15A 1.47(3) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A C16A 1.53(2) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.49(3) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C14B C15B 1.499(18) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B C16B 1.555(16) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B C17B 1.366(19) . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18 C19 1.372(7) . ? C18 C27 1.426(7) . ? C19 C20 1.412(8) . ? C19 H19 0.9500 . ? C20 C21 1.367(8) . ? C20 H20 0.9500 . ? C21 C22 1.411(8) . ? C21 H21 0.9500 . ? C22 C23 1.421(7) . ? C22 C27 1.433(7) . ? C23 C24 1.358(8) . ? C23 H23 0.9500 . ? C24 C25 1.389(8) . ? C24 H24 0.9500 . ? C25 C26 1.378(7) . ? C25 H25 0.9500 . ? C26 C27 1.423(7) . ? C26 H26 0.9500 . ? C28A C29A 1.3900 . ? C28A C33A 1.3900 . ? C28A C34A 1.597(13) . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A C31A 1.3900 . ? C30A H30A 0.9500 . ? C31A C32A 1.3900 . ? C31A C35A 1.546(13) . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A H33A 0.9500 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A C37A 1.501(18) . ? C35A C36A 1.540(18) . ? C35A H35A 1.0000 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C28B C29B 1.3900 . ? C28B C33B 1.3900 . ? C28B C34B 1.59(3) . ? C29B C30B 1.3900 . ? C29B H29B 0.9500 . ? C30B C31B 1.3900 . ? C30B H30B 0.9500 . ? C31B C32B 1.3900 . ? C31B C35B 1.41(6) . ? C32B C33B 1.3900 . ? C32B H32B 0.9500 . ? C33B H33B 0.9500 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B C37B 1.29(7) . ? C35B C36B 1.66(6) . ? C35B H35B 1.0000 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31B Ru1 C30B 40.5(3) . . ? C31B Ru1 O1 94.2(5) . . ? C30B Ru1 O1 95.4(5) . . ? C31B Ru1 N3 125.0(6) . . ? C30B Ru1 N3 165.1(5) . . ? O1 Ru1 N3 88.89(13) . . ? C31B Ru1 C32B 39.1(4) . . ? C30B Ru1 C32B 71.0(5) . . ? O1 Ru1 C32B 120.8(6) . . ? N3 Ru1 C32B 94.5(6) . . ? C31B Ru1 C29B 70.9(5) . . ? C30B Ru1 C29B 39.0(3) . . ? O1 Ru1 C29B 123.5(5) . . ? N3 Ru1 C29B 144.8(5) . . ? C32B Ru1 C29B 81.2(4) . . ? C31B Ru1 C33A 57.0(6) . . ? C30B Ru1 C33A 71.0(5) . . ? O1 Ru1 C33A 148.8(3) . . ? N3 Ru1 C33A 98.2(3) . . ? C32B Ru1 C33A 28.7(8) . . ? C29B Ru1 C33A 62.3(7) . . ? C31B Ru1 C28A 68.7(6) . . ? C30B Ru1 C28A 53.9(5) . . ? O1 Ru1 C28A 148.2(3) . . ? N3 Ru1 C28A 122.9(3) . . ? C32B Ru1 C28A 61.9(7) . . ? C29B Ru1 C28A 26.7(7) . . ? C33A Ru1 C28A 37.53(18) . . ? C31B Ru1 C32A 30.5(8) . . ? C30B Ru1 C32A 66.1(6) . . ? O1 Ru1 C32A 111.8(3) . . ? N3 Ru1 C32A 99.1(3) . . ? C32B Ru1 C32A 10.0(8) . . ? C29B Ru1 C32A 82.6(6) . . ? C33A Ru1 C32A 37.16(18) . . ? C28A Ru1 C32A 66.8(3) . . ? C31B Ru1 C29A 59.7(7) . . ? C30B Ru1 C29A 23.9(6) . . ? O1 Ru1 C29A 111.5(3) . . ? N3 Ru1 C29A 159.2(3) . . ? C32B Ru1 C29A 78.7(7) . . ? C29B Ru1 C29A 15.3(5) . . ? C33A Ru1 C29A 66.6(2) . . ? C28A Ru1 C29A 36.80(17) . . ? C32A Ru1 C29A 77.5(2) . . ? C31B Ru1 C33B 68.5(5) . . ? C30B Ru1 C33B 81.1(5) . . ? O1 Ru1 C33B 157.2(5) . . ? N3 Ru1 C33B 89.3(4) . . ? C32B Ru1 C33B 36.8(3) . . ? C29B Ru1 C33B 66.3(4) . . ? C33A Ru1 C33B 11.8(6) . . ? C28A Ru1 C33B 39.8(7) . . ? C32A Ru1 C33B 46.2(7) . . ? C29A Ru1 C33B 73.4(6) . . ? C31B Ru1 C28B 81.1(5) . . ? C30B Ru1 C28B 68.4(4) . . ? O1 Ru1 C28B 160.0(5) . . ? N3 Ru1 C28B 109.8(5) . . ? C32B Ru1 C28B 66.4(4) . . ? C29B Ru1 C28B 36.7(3) . . ? C33A Ru1 C28B 38.4(7) . . ? C28A Ru1 C28B 14.6(4) . . ? C32A Ru1 C28B 73.3(6) . . ? C29A Ru1 C28B 49.5(5) . . ? C33B Ru1 C28B 35.8(2) . . ? C1 O1 Ru1 123.5(3) . . ? C1 N1 N2 110.7(4) . . ? C1 N1 C2 129.9(4) . . ? N2 N1 C2 119.1(4) . . ? C8 N2 N1 105.8(4) . . ? C11 N3 C18 117.4(4) . . ? C11 N3 Ru1 129.2(3) . . ? C18 N3 Ru1 113.3(3) . . ? O1 C1 N1 120.8(4) . . ? O1 C1 C10 131.7(4) . . ? N1 C1 C10 107.6(3) . . ? C3 C2 C7 120.3(5) . . ? C3 C2 N1 121.5(4) . . ? C7 C2 N1 118.2(5) . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 120.2(6) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.5(6) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 119.4(6) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? N2 C8 C10 112.8(4) . . ? N2 C8 C9 116.1(4) . . ? C10 C8 C9 131.1(5) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 C11 125.2(4) . . ? C1 C10 C8 103.1(4) . . ? C11 C10 C8 131.6(4) . . ? N3 C11 C10 121.2(4) . . ? N3 C11 C12 120.3(4) . . ? C10 C11 C12 118.4(4) . . ? C11 C12 C13 110.6(4) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14A C13 C12 117.1(8) . . ? C12 C13 C14B 105.8(8) . . ? C14A C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C14B C13 H13A 138.9 . . ? C14A C13 H13B 108.0 . . ? C12 C13 H13B 108.0 . . ? C14B C13 H13B 83.2 . . ? H13A C13 H13B 107.3 . . ? C14A C13 H13C 126.3 . . ? C12 C13 H13C 110.6 . . ? C14B C13 H13C 110.9 . . ? H13A C13 H13C 77.9 . . ? C14A C13 H13D 76.6 . . ? C12 C13 H13D 110.6 . . ? C14B C13 H13D 110.2 . . ? H13B C13 H13D 133.0 . . ? H13C C13 H13D 108.8 . . ? C13 C14A C15A 107.9(13) . . ? C15A C14A H13D 145.5 . . ? C13 C14A H14A 110.1 . . ? C15A C14A H14A 110.1 . . ? H13D C14A H14A 90.6 . . ? C13 C14A H14B 110.1 . . ? C15A C14A H14B 110.1 . . ? H13D C14A H14B 87.4 . . ? H14A C14A H14B 108.4 . . ? C14A C15A C16A 115.5(16) . . ? C14A C15A H15A 108.4 . . ? C16A C15A H15A 108.4 . . ? C14A C15A H15B 108.4 . . ? C16A C15A H15B 108.4 . . ? H15A C15A H15B 107.5 . . ? C17A C16A C15A 114.9(18) . . ? C17A C16A H16A 108.6 . . ? C15A C16A H16A 108.6 . . ? C17A C16A H16B 108.6 . . ? C15A C16A H16B 108.6 . . ? H16A C16A H16B 107.5 . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C15B C14B C13 110.8(11) . . ? C15B C14B H14C 109.5 . . ? C13 C14B H14C 109.5 . . ? C15B C14B H14D 109.5 . . ? C13 C14B H14D 109.5 . . ? H14C C14B H14D 108.1 . . ? C14B C15B C16B 117.1(11) . . ? C14B C15B H15C 108.0 . . ? C16B C15B H15C 108.0 . . ? C14B C15B H15D 108.0 . . ? C16B C15B H15D 108.0 . . ? H15C C15B H15D 107.3 . . ? C17B C16B C15B 120.4(12) . . ? C17B C16B H16C 107.2 . . ? C15B C16B H16C 107.2 . . ? C17B C16B H16D 107.2 . . ? C15B C16B H16D 107.2 . . ? H16C C16B H16D 106.9 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C19 C18 C27 120.8(5) . . ? C19 C18 N3 120.1(5) . . ? C27 C18 N3 119.0(5) . . ? C18 C19 C20 120.1(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 120.7(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.7(6) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 122.7(6) . . ? C21 C22 C27 119.3(5) . . ? C23 C22 C27 118.0(6) . . ? C24 C23 C22 121.5(6) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 120.6(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 120.8(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.3(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C18 122.9(5) . . ? C26 C27 C22 118.8(5) . . ? C18 C27 C22 118.3(5) . . ? C29A C28A C33A 120.0 . . ? C29A C28A C34A 118.8(9) . . ? C33A C28A C34A 121.0(9) . . ? C29A C28A Ru1 74.2(3) . . ? C33A C28A Ru1 70.7(4) . . ? C34A C28A Ru1 123.5(7) . . ? C28A C29A C30A 120.0 . . ? C28A C29A Ru1 69.0(4) . . ? C30A C29A Ru1 74.1(4) . . ? C28A C29A H29A 120.0 . . ? C30A C29A H29A 120.0 . . ? Ru1 C29A H29A 129.2 . . ? C31A C30A C29A 120.0 . . ? C31A C30A Ru1 71.7(4) . . ? C29A C30A Ru1 70.1(4) . . ? C31A C30A H30A 120.0 . . ? C29A C30A H30A 120.0 . . ? Ru1 C30A H30A 130.9 . . ? C30A C31A C32A 120.0 . . ? C30A C31A C35A 118.4(10) . . ? C32A C31A C35A 121.0(10) . . ? C30A C31A Ru1 72.7(4) . . ? C32A C31A Ru1 69.4(4) . . ? C35A C31A Ru1 123.2(8) . . ? C33A C32A C31A 120.0 . . ? C33A C32A Ru1 69.4(4) . . ? C31A C32A Ru1 74.5(3) . . ? C33A C32A H32A 120.0 . . ? C31A C32A H32A 120.0 . . ? Ru1 C32A H32A 128.4 . . ? C32A C33A C28A 120.0 . . ? C32A C33A Ru1 73.5(4) . . ? C28A C33A Ru1 71.8(4) . . ? C32A C33A H33A 120.0 . . ? C28A C33A H33A 120.0 . . ? Ru1 C33A H33A 126.7 . . ? C28A C34A H34A 109.5 . . ? C28A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C28A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C37A C35A C36A 114.1(10) . . ? C37A C35A C31A 114.6(12) . . ? C36A C35A C31A 110.0(10) . . ? C37A C35A H35A 105.8 . . ? C36A C35A H35A 105.8 . . ? C31A C35A H35A 105.8 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C35A C37A H37A 109.5 . . ? C35A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C35A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C29B C28B C33B 120.0 . . ? C29B C28B C34B 124.3(17) . . ? C33B C28B C34B 115.5(17) . . ? C29B C28B Ru1 66.9(6) . . ? C33B C28B Ru1 71.9(7) . . ? C34B C28B Ru1 130.9(13) . . ? C30B C29B C28B 120.0 . . ? C30B C29B Ru1 65.4(6) . . ? C28B C29B Ru1 76.4(6) . . ? C30B C29B H29B 120.0 . . ? C28B C29B H29B 120.0 . . ? Ru1 C29B H29B 130.7 . . ? C29B C30B C31B 120.0 . . ? C29B C30B Ru1 75.7(6) . . ? C31B C30B Ru1 69.6(7) . . ? C29B C30B H30B 120.0 . . ? C31B C30B H30B 120.0 . . ? Ru1 C30B H30B 126.7 . . ? C32B C31B C30B 120.0 . . ? C32B C31B C35B 121(3) . . ? C30B C31B C35B 119(3) . . ? C32B C31B Ru1 75.4(7) . . ? C30B C31B Ru1 69.9(7) . . ? C35B C31B Ru1 124(2) . . ? C33B C32B C31B 120.0 . . ? C33B C32B Ru1 76.5(6) . . ? C31B C32B Ru1 65.4(6) . . ? C33B C32B H32B 120.0 . . ? C31B C32B H32B 120.0 . . ? Ru1 C32B H32B 130.5 . . ? C32B C33B C28B 120.0 . . ? C32B C33B Ru1 66.7(6) . . ? C28B C33B Ru1 72.2(6) . . ? C32B C33B H33B 120.0 . . ? C28B C33B H33B 120.0 . . ? Ru1 C33B H33B 134.5 . . ? C28B C34B H34D 109.5 . . ? C28B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C28B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C37B C35B C31B 127(5) . . ? C37B C35B C36B 102(5) . . ? C31B C35B C36B 119(4) . . ? C37B C35B H35B 101.5 . . ? C31B C35B H35B 101.5 . . ? C36B C35B H35B 101.5 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C35B C37B H37D 109.5 . . ? C35B C37B H37E 109.5 . . ? H37D C37B H37E 108.0 . . ? C35B C37B H37F 111.0 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 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 C31B Ru1 O1 C1 120.5(7) . . . . ? C30B Ru1 O1 C1 161.2(6) . . . . ? N3 Ru1 O1 C1 -4.5(3) . . . . ? C32B Ru1 O1 C1 90.0(7) . . . . ? C29B Ru1 O1 C1 -169.6(6) . . . . ? C33A Ru1 O1 C1 99.5(7) . . . . ? C28A Ru1 O1 C1 175.5(6) . . . . ? C32A Ru1 O1 C1 94.8(4) . . . . ? C29A Ru1 O1 C1 179.5(4) . . . . ? C33B Ru1 O1 C1 81.1(12) . . . . ? C28B Ru1 O1 C1 -164.1(12) . . . . ? C1 N1 N2 C8 0.2(5) . . . . ? C2 N1 N2 C8 173.8(4) . . . . ? C31B Ru1 N3 C11 -95.1(7) . . . . ? C30B Ru1 N3 C11 -108(2) . . . . ? O1 Ru1 N3 C11 -0.8(4) . . . . ? C32B Ru1 N3 C11 -121.6(7) . . . . ? C29B Ru1 N3 C11 157.4(8) . . . . ? C33A Ru1 N3 C11 -150.2(5) . . . . ? C28A Ru1 N3 C11 179.2(5) . . . . ? C32A Ru1 N3 C11 -112.7(5) . . . . ? C29A Ru1 N3 C11 168.6(7) . . . . ? C33B Ru1 N3 C11 -158.0(6) . . . . ? C28B Ru1 N3 C11 171.9(6) . . . . ? C31B Ru1 N3 C18 89.7(7) . . . . ? C30B Ru1 N3 C18 77(2) . . . . ? O1 Ru1 N3 C18 -176.0(3) . . . . ? C32B Ru1 N3 C18 63.2(6) . . . . ? C29B Ru1 N3 C18 -17.8(8) . . . . ? C33A Ru1 N3 C18 34.6(5) . . . . ? C28A Ru1 N3 C18 4.0(5) . . . . ? C32A Ru1 N3 C18 72.1(5) . . . . ? C29A Ru1 N3 C18 -6.6(9) . . . . ? C33B Ru1 N3 C18 26.8(6) . . . . ? C28B Ru1 N3 C18 -3.3(6) . . . . ? Ru1 O1 C1 N1 -172.6(3) . . . . ? Ru1 O1 C1 C10 7.6(7) . . . . ? N2 N1 C1 O1 -179.9(4) . . . . ? C2 N1 C1 O1 7.4(7) . . . . ? N2 N1 C1 C10 0.0(5) . . . . ? C2 N1 C1 C10 -172.8(4) . . . . ? C1 N1 C2 C3 -19.9(7) . . . . ? N2 N1 C2 C3 167.9(4) . . . . ? C1 N1 C2 C7 158.1(5) . . . . ? N2 N1 C2 C7 -14.2(6) . . . . ? C7 C2 C3 C4 0.3(8) . . . . ? N1 C2 C3 C4 178.1(5) . . . . ? C2 C3 C4 C5 0.5(10) . . . . ? C3 C4 C5 C6 -1.3(13) . . . . ? C4 C5 C6 C7 1.3(12) . . . . ? C5 C6 C7 C2 -0.6(10) . . . . ? C3 C2 C7 C6 -0.2(8) . . . . ? N1 C2 C7 C6 -178.1(5) . . . . ? N1 N2 C8 C10 -0.3(6) . . . . ? N1 N2 C8 C9 178.9(5) . . . . ? O1 C1 C10 C11 -3.8(8) . . . . ? N1 C1 C10 C11 176.4(4) . . . . ? O1 C1 C10 C8 179.7(5) . . . . ? N1 C1 C10 C8 -0.1(5) . . . . ? N2 C8 C10 C1 0.3(6) . . . . ? C9 C8 C10 C1 -178.8(6) . . . . ? N2 C8 C10 C11 -175.9(5) . . . . ? C9 C8 C10 C11 5.1(10) . . . . ? C18 N3 C11 C10 179.0(4) . . . . ? Ru1 N3 C11 C10 4.0(6) . . . . ? C18 N3 C11 C12 1.3(6) . . . . ? Ru1 N3 C11 C12 -173.7(3) . . . . ? C1 C10 C11 N3 -2.6(7) . . . . ? C8 C10 C11 N3 172.8(5) . . . . ? C1 C10 C11 C12 175.1(4) . . . . ? C8 C10 C11 C12 -9.5(8) . . . . ? N3 C11 C12 C13 91.8(5) . . . . ? C10 C11 C12 C13 -86.0(5) . . . . ? C11 C12 C13 C14A -150.0(9) . . . . ? C11 C12 C13 C14B 175.8(7) . . . . ? C12 C13 C14A C15A -70.2(17) . . . . ? C14B C13 C14A C15A 7.3(16) . . . . ? C13 C14A C15A C16A 175.2(17) . . . . ? C14A C15A C16A C17A 172(2) . . . . ? C14A C13 C14B C15B -34.6(14) . . . . ? C12 C13 C14B C15B 80.8(14) . . . . ? C13 C14B C15B C16B -175.7(12) . . . . ? C14B C15B C16B C17B 174.7(17) . . . . ? C11 N3 C18 C19 -99.3(6) . . . . ? Ru1 N3 C18 C19 76.6(6) . . . . ? C11 N3 C18 C27 82.7(6) . . . . ? Ru1 N3 C18 C27 -101.5(5) . . . . ? C27 C18 C19 C20 -1.0(10) . . . . ? N3 C18 C19 C20 -179.0(6) . . . . ? C18 C19 C20 C21 0.0(11) . . . . ? C19 C20 C21 C22 0.6(12) . . . . ? C20 C21 C22 C23 -179.0(7) . . . . ? C20 C21 C22 C27 -0.1(10) . . . . ? C21 C22 C23 C24 179.2(6) . . . . ? C27 C22 C23 C24 0.3(8) . . . . ? C22 C23 C24 C25 0.6(8) . . . . ? C23 C24 C25 C26 -0.9(7) . . . . ? C24 C25 C26 C27 0.4(7) . . . . ? C25 C26 C27 C18 -178.3(5) . . . . ? C25 C26 C27 C22 0.4(7) . . . . ? C19 C18 C27 C26 -179.8(5) . . . . ? N3 C18 C27 C26 -1.8(7) . . . . ? C19 C18 C27 C22 1.5(8) . . . . ? N3 C18 C27 C22 179.5(4) . . . . ? C21 C22 C27 C26 -179.7(5) . . . . ? C23 C22 C27 C26 -0.8(7) . . . . ? C21 C22 C27 C18 -0.9(8) . . . . ? C23 C22 C27 C18 178.0(5) . . . . ? C31B Ru1 C28A C29A 67.5(8) . . . . ? C30B Ru1 C28A C29A 23.9(8) . . . . ? O1 Ru1 C28A C29A 6.2(7) . . . . ? N3 Ru1 C28A C29A -173.8(3) . . . . ? C32B Ru1 C28A C29A 110.1(8) . . . . ? C29B Ru1 C28A C29A -22.3(10) . . . . ? C33A Ru1 C28A C29A 130.53(19) . . . . ? C32A Ru1 C28A C29A 100.5(2) . . . . ? C33B Ru1 C28A C29A 149.0(10) . . . . ? C28B Ru1 C28A C29A -146(3) . . . . ? C31B Ru1 C28A C33A -63.1(8) . . . . ? C30B Ru1 C28A C33A -106.6(8) . . . . ? O1 Ru1 C28A C33A -124.3(7) . . . . ? N3 Ru1 C28A C33A 55.7(3) . . . . ? C32B Ru1 C28A C33A -20.4(8) . . . . ? C29B Ru1 C28A C33A -152.8(11) . . . . ? C32A Ru1 C28A C33A -30.08(14) . . . . ? C29A Ru1 C28A C33A -130.53(19) . . . . ? C33B Ru1 C28A C33A 18.5(10) . . . . ? C28B Ru1 C28A C33A 84(3) . . . . ? C31B Ru1 C28A C34A -178.1(13) . . . . ? C30B Ru1 C28A C34A 138.4(14) . . . . ? O1 Ru1 C28A C34A 120.6(7) . . . . ? N3 Ru1 C28A C34A -59.4(11) . . . . ? C32B Ru1 C28A C34A -135.5(12) . . . . ? C29B Ru1 C28A C34A 92.1(16) . . . . ? C33A Ru1 C28A C34A -115.1(11) . . . . ? C32A Ru1 C28A C34A -145.1(11) . . . . ? C29A Ru1 C28A C34A 114.4(11) . . . . ? C33B Ru1 C28A C34A -96.5(10) . . . . ? C28B Ru1 C28A C34A -31(2) . . . . ? C33A C28A C29A C30A 0.0 . . . . ? C34A C28A C29A C30A -175.9(9) . . . . ? Ru1 C28A C29A C30A -55.9(4) . . . . ? C33A C28A C29A Ru1 55.9(4) . . . . ? C34A C28A C29A Ru1 -120.0(8) . . . . ? C31B Ru1 C29A C28A -94.5(8) . . . . ? C30B Ru1 C29A C28A -126.1(15) . . . . ? O1 Ru1 C29A C28A -176.5(4) . . . . ? N3 Ru1 C29A C28A 14.9(8) . . . . ? C32B Ru1 C29A C28A -57.7(8) . . . . ? C29B Ru1 C29A C28A 40(3) . . . . ? C33A Ru1 C29A C28A -30.31(15) . . . . ? C32A Ru1 C29A C28A -67.8(3) . . . . ? C33B Ru1 C29A C28A -20.1(8) . . . . ? C28B Ru1 C29A C28A 10.8(9) . . . . ? C31B Ru1 C29A C30A 37.2(8) . . . . ? C30B Ru1 C29A C30A 5.7(15) . . . . ? O1 Ru1 C29A C30A -44.7(4) . . . . ? N3 Ru1 C29A C30A 146.6(8) . . . . ? C32B Ru1 C29A C30A 74.1(7) . . . . ? C29B Ru1 C29A C30A 172(3) . . . . ? C33A Ru1 C29A C30A 101.4(3) . . . . ? C28A Ru1 C29A C30A 131.8(2) . . . . ? C32A Ru1 C29A C30A 64.0(3) . . . . ? C33B Ru1 C29A C30A 111.6(7) . . . . ? C28B Ru1 C29A C30A 142.6(9) . . . . ? C28A C29A C30A C31A 0.0 . . . . ? Ru1 C29A C30A C31A -53.5(3) . . . . ? C28A C29A C30A Ru1 53.5(3) . . . . ? C31B Ru1 C30A C31A 16.2(12) . . . . ? C30B Ru1 C30A C31A 122(3) . . . . ? O1 Ru1 C30A C31A -88.3(4) . . . . ? N3 Ru1 C30A C31A -14.7(8) . . . . ? C32B Ru1 C30A C31A 36.5(9) . . . . ? C29B Ru1 C30A C31A 130.1(9) . . . . ? C33A Ru1 C30A C31A 65.8(3) . . . . ? C28A Ru1 C30A C31A 103.4(3) . . . . ? C32A Ru1 C30A C31A 28.69(16) . . . . ? C29A Ru1 C30A C31A 132.8(2) . . . . ? C33B Ru1 C30A C31A 69.8(8) . . . . ? C28B Ru1 C30A C31A 104.8(7) . . . . ? C31B Ru1 C30A C29A -116.7(11) . . . . ? C30B Ru1 C30A C29A -11(3) . . . . ? O1 Ru1 C30A C29A 138.9(4) . . . . ? N3 Ru1 C30A C29A -147.6(8) . . . . ? C32B Ru1 C30A C29A -96.3(8) . . . . ? C29B Ru1 C30A C29A -2.8(9) . . . . ? C33A Ru1 C30A C29A -67.1(3) . . . . ? C28A Ru1 C30A C29A -29.43(16) . . . . ? C32A Ru1 C30A C29A -104.1(3) . . . . ? C33B Ru1 C30A C29A -63.0(7) . . . . ? C28B Ru1 C30A C29A -28.0(7) . . . . ? C29A C30A C31A C32A 0.0 . . . . ? Ru1 C30A C31A C32A -52.8(3) . . . . ? C29A C30A C31A C35A 171.7(11) . . . . ? Ru1 C30A C31A C35A 118.9(10) . . . . ? C29A C30A C31A Ru1 52.8(3) . . . . ? C31B Ru1 C31A C30A -85(5) . . . . ? C30B Ru1 C31A C30A -15.2(9) . . . . ? O1 Ru1 C31A C30A 88.4(4) . . . . ? N3 Ru1 C31A C30A 173.6(4) . . . . ? C32B Ru1 C31A C30A -127.7(11) . . . . ? C29B Ru1 C31A C30A -37.6(7) . . . . ? C33A Ru1 C31A C30A -102.7(3) . . . . ? C28A Ru1 C31A C30A -65.0(3) . . . . ? C32A Ru1 C31A C30A -132.5(2) . . . . ? C29A Ru1 C31A C30A -28.37(14) . . . . ? C33B Ru1 C31A C30A -105.8(7) . . . . ? C28B Ru1 C31A C30A -72.2(7) . . . . ? C31B Ru1 C31A C32A 48(5) . . . . ? C30B Ru1 C31A C32A 117.3(9) . . . . ? O1 Ru1 C31A C32A -139.1(4) . . . . ? N3 Ru1 C31A C32A -53.8(4) . . . . ? C32B Ru1 C31A C32A 4.8(11) . . . . ? C29B Ru1 C31A C32A 94.9(7) . . . . ? C33A Ru1 C31A C32A 29.84(15) . . . . ? C28A Ru1 C31A C32A 67.6(3) . . . . ? C29A Ru1 C31A C32A 104.2(3) . . . . ? C33B Ru1 C31A C32A 26.7(8) . . . . ? C28B Ru1 C31A C32A 60.4(7) . . . . ? C31B Ru1 C31A C35A 162(6) . . . . ? C30B Ru1 C31A C35A -128.3(15) . . . . ? O1 Ru1 C31A C35A -24.7(10) . . . . ? N3 Ru1 C31A C35A 60.5(12) . . . . ? C32B Ru1 C31A C35A 119.2(15) . . . . ? C29B Ru1 C31A C35A -150.7(12) . . . . ? C33A Ru1 C31A C35A 144.2(12) . . . . ? C28A Ru1 C31A C35A -178.1(12) . . . . ? C32A Ru1 C31A C35A 114.4(12) . . . . ? C29A Ru1 C31A C35A -141.5(12) . . . . ? C33B Ru1 C31A C35A 141.1(12) . . . . ? C28B Ru1 C31A C35A 174.7(12) . . . . ? C30A C31A C32A C33A 0.0 . . . . ? C35A C31A C32A C33A -171.5(11) . . . . ? Ru1 C31A C32A C33A -54.3(4) . . . . ? C30A C31A C32A Ru1 54.3(4) . . . . ? C35A C31A C32A Ru1 -117.2(10) . . . . ? C31B Ru1 C32A C33A 117.5(13) . . . . ? C30B Ru1 C32A C33A 89.7(6) . . . . ? O1 Ru1 C32A C33A 175.9(4) . . . . ? N3 Ru1 C32A C33A -91.7(3) . . . . ? C32B Ru1 C32A C33A -28(5) . . . . ? C29B Ru1 C32A C33A 52.8(6) . . . . ? C28A Ru1 C32A C33A 30.37(15) . . . . ? C29A Ru1 C32A C33A 67.5(3) . . . . ? C33B Ru1 C32A C33A -11.4(10) . . . . ? C28B Ru1 C32A C33A 16.4(6) . . . . ? C31B Ru1 C32A C31A -13.8(14) . . . . ? C30B Ru1 C32A C31A -41.6(7) . . . . ? O1 Ru1 C32A C31A 44.7(4) . . . . ? N3 Ru1 C32A C31A 137.1(3) . . . . ? C32B Ru1 C32A C31A -160(5) . . . . ? C29B Ru1 C32A C31A -78.5(6) . . . . ? C33A Ru1 C32A C31A -131.25(18) . . . . ? C28A Ru1 C32A C31A -100.9(2) . . . . ? C29A Ru1 C32A C31A -63.8(3) . . . . ? C33B Ru1 C32A C31A -142.6(10) . . . . ? C28B Ru1 C32A C31A -114.8(6) . . . . ? C31A C32A C33A C28A 0.0 . . . . ? Ru1 C32A C33A C28A -56.8(3) . . . . ? C31A C32A C33A Ru1 56.8(3) . . . . ? C29A C28A C33A C32A 0.0 . . . . ? C34A C28A C33A C32A 175.8(10) . . . . ? Ru1 C28A C33A C32A 57.6(3) . . . . ? C29A C28A C33A Ru1 -57.6(3) . . . . ? C34A C28A C33A Ru1 118.2(8) . . . . ? C31B Ru1 C33A C32A -32.5(9) . . . . ? C30B Ru1 C33A C32A -75.3(7) . . . . ? O1 Ru1 C33A C32A -7.3(7) . . . . ? N3 Ru1 C33A C32A 94.2(3) . . . . ? C32B Ru1 C33A C32A 9.8(15) . . . . ? C29B Ru1 C33A C32A -116.9(6) . . . . ? C28A Ru1 C33A C32A -130.30(17) . . . . ? C29A Ru1 C33A C32A -100.5(2) . . . . ? C33B Ru1 C33A C32A 136(4) . . . . ? C28B Ru1 C33A C32A -154.2(8) . . . . ? C31B Ru1 C33A C28A 97.8(9) . . . . ? C30B Ru1 C33A C28A 55.0(6) . . . . ? O1 Ru1 C33A C28A 123.0(7) . . . . ? N3 Ru1 C33A C28A -135.5(3) . . . . ? C32B Ru1 C33A C28A 140.1(15) . . . . ? C29B Ru1 C33A C28A 13.4(5) . . . . ? C32A Ru1 C33A C28A 130.30(17) . . . . ? C29A Ru1 C33A C28A 29.75(15) . . . . ? C33B Ru1 C33A C28A -94(4) . . . . ? C28B Ru1 C33A C28A -23.9(8) . . . . ? C30A C31A C35A C37A -154.1(10) . . . . ? C32A C31A C35A C37A 17.5(15) . . . . ? Ru1 C31A C35A C37A -66.9(15) . . . . ? C30A C31A C35A C36A 75.7(13) . . . . ? C32A C31A C35A C36A -112.6(12) . . . . ? Ru1 C31A C35A C36A 162.9(9) . . . . ? C31B Ru1 C28B C29B 69.9(5) . . . . ? C30B Ru1 C28B C29B 29.9(3) . . . . ? O1 Ru1 C28B C29B -7.7(13) . . . . ? N3 Ru1 C28B C29B -166.0(5) . . . . ? C32B Ru1 C28B C29B 107.9(5) . . . . ? C33A Ru1 C28B C29B 116.2(8) . . . . ? C28A Ru1 C28B C29B 39(3) . . . . ? C32A Ru1 C28B C29B 100.2(7) . . . . ? C29A Ru1 C28B C29B 12.5(8) . . . . ? C33B Ru1 C28B C29B 135.3(4) . . . . ? C31B Ru1 C28B C33B -65.4(6) . . . . ? C30B Ru1 C28B C33B -105.4(6) . . . . ? O1 Ru1 C28B C33B -143.0(13) . . . . ? N3 Ru1 C28B C33B 58.8(6) . . . . ? C32B Ru1 C28B C33B -27.4(3) . . . . ? C29B Ru1 C28B C33B -135.3(4) . . . . ? C33A Ru1 C28B C33B -19.1(9) . . . . ? C28A Ru1 C28B C33B -96(3) . . . . ? C32A Ru1 C28B C33B -35.1(8) . . . . ? C29A Ru1 C28B C33B -122.8(8) . . . . ? C31B Ru1 C28B C34B -174(2) . . . . ? C30B Ru1 C28B C34B 146(2) . . . . ? O1 Ru1 C28B C34B 109(2) . . . . ? N3 Ru1 C28B C34B -50(2) . . . . ? C32B Ru1 C28B C34B -136(2) . . . . ? C29B Ru1 C28B C34B 116(2) . . . . ? C33A Ru1 C28B C34B -128(2) . . . . ? C28A Ru1 C28B C34B 155(4) . . . . ? C32A Ru1 C28B C34B -144(2) . . . . ? C29A Ru1 C28B C34B 129(2) . . . . ? C33B Ru1 C28B C34B -108(2) . . . . ? C33B C28B C29B C30B 0.0 . . . . ? C34B C28B C29B C30B -175.4(18) . . . . ? Ru1 C28B C29B C30B -50.6(6) . . . . ? C33B C28B C29B Ru1 50.6(6) . . . . ? C34B C28B C29B Ru1 -124.8(16) . . . . ? C31B Ru1 C29B C30B 31.7(3) . . . . ? O1 Ru1 C29B C30B -50.5(6) . . . . ? N3 Ru1 C29B C30B 155.9(8) . . . . ? C32B Ru1 C29B C30B 70.7(5) . . . . ? C33A Ru1 C29B C30B 93.6(7) . . . . ? C28A Ru1 C29B C30B 112.0(10) . . . . ? C32A Ru1 C29B C30B 60.7(7) . . . . ? C29A Ru1 C29B C30B -9(2) . . . . ? C33B Ru1 C29B C30B 105.9(5) . . . . ? C28B Ru1 C29B C30B 132.6(4) . . . . ? C31B Ru1 C29B C28B -101.0(5) . . . . ? C30B Ru1 C29B C28B -132.6(4) . . . . ? O1 Ru1 C29B C28B 176.8(5) . . . . ? N3 Ru1 C29B C28B 23.3(8) . . . . ? C32B Ru1 C29B C28B -62.0(5) . . . . ? C33A Ru1 C29B C28B -39.0(7) . . . . ? C28A Ru1 C29B C28B -20.7(10) . . . . ? C32A Ru1 C29B C28B -71.9(7) . . . . ? C29A Ru1 C29B C28B -142(2) . . . . ? C33B Ru1 C29B C28B -26.7(2) . . . . ? C28B C29B C30B C31B 0.0 . . . . ? Ru1 C29B C30B C31B -55.7(7) . . . . ? C28B C29B C30B Ru1 55.7(7) . . . . ? C31B Ru1 C30B C29B -130.3(3) . . . . ? O1 Ru1 C30B C29B 139.7(6) . . . . ? N3 Ru1 C30B C29B -114(2) . . . . ? C32B Ru1 C30B C29B -99.6(4) . . . . ? C33A Ru1 C30B C29B -69.2(8) . . . . ? C28A Ru1 C30B C29B -31.0(8) . . . . ? C32A Ru1 C30B C29B -108.9(8) . . . . ? C29A Ru1 C30B C29B 5.8(16) . . . . ? C33B Ru1 C30B C29B -63.1(4) . . . . ? C28B Ru1 C30B C29B -28.2(3) . . . . ? O1 Ru1 C30B C31B -90.1(7) . . . . ? N3 Ru1 C30B C31B 16(2) . . . . ? C32B Ru1 C30B C31B 30.6(3) . . . . ? C29B Ru1 C30B C31B 130.3(3) . . . . ? C33A Ru1 C30B C31B 61.1(9) . . . . ? C28A Ru1 C30B C31B 99.2(9) . . . . ? C32A Ru1 C30B C31B 21.4(9) . . . . ? C29A Ru1 C30B C31B 136.0(16) . . . . ? C33B Ru1 C30B C31B 67.2(5) . . . . ? C28B Ru1 C30B C31B 102.0(5) . . . . ? C29B C30B C31B C32B 0.0 . . . . ? Ru1 C30B C31B C32B -58.6(6) . . . . ? C29B C30B C31B C35B 178(3) . . . . ? Ru1 C30B C31B C35B 119(3) . . . . ? C29B C30B C31B Ru1 58.6(6) . . . . ? C30B Ru1 C31B C32B 130.2(3) . . . . ? O1 Ru1 C31B C32B -136.3(6) . . . . ? N3 Ru1 C31B C32B -44.8(6) . . . . ? C29B Ru1 C31B C32B 99.7(4) . . . . ? C33A Ru1 C31B C32B 30.9(9) . . . . ? C28A Ru1 C31B C32B 71.3(8) . . . . ? C32A Ru1 C31B C32B -8.8(16) . . . . ? C29A Ru1 C31B C32B 111.1(7) . . . . ? C33B Ru1 C31B C32B 28.4(3) . . . . ? C28B Ru1 C31B C32B 63.2(5) . . . . ? O1 Ru1 C31B C30B 93.5(6) . . . . ? N3 Ru1 C31B C30B -174.9(7) . . . . ? C32B Ru1 C31B C30B -130.2(3) . . . . ? C29B Ru1 C31B C30B -30.5(3) . . . . ? C33A Ru1 C31B C30B -99.3(9) . . . . ? C28A Ru1 C31B C30B -58.9(7) . . . . ? C32A Ru1 C31B C30B -139.0(15) . . . . ? C29A Ru1 C31B C30B -19.1(8) . . . . ? C33B Ru1 C31B C30B -101.8(4) . . . . ? C28B Ru1 C31B C30B -66.9(5) . . . . ? C30B Ru1 C31B C35B -112(3) . . . . ? O1 Ru1 C31B C35B -19(3) . . . . ? N3 Ru1 C31B C35B 73(3) . . . . ? C32B Ru1 C31B C35B 117(3) . . . . ? C29B Ru1 C31B C35B -143(3) . . . . ? C33A Ru1 C31B C35B 148(3) . . . . ? C28A Ru1 C31B C35B -171(3) . . . . ? C32A Ru1 C31B C35B 109(3) . . . . ? C29A Ru1 C31B C35B -131(3) . . . . ? C33B Ru1 C31B C35B 146(3) . . . . ? C28B Ru1 C31B C35B -179(3) . . . . ? C30B C31B C32B C33B 0.0 . . . . ? C35B C31B C32B C33B -178(3) . . . . ? Ru1 C31B C32B C33B -55.9(6) . . . . ? C30B C31B C32B Ru1 55.9(6) . . . . ? C35B C31B C32B Ru1 -122(3) . . . . ? C31B Ru1 C32B C33B 132.5(3) . . . . ? C30B Ru1 C32B C33B 100.8(5) . . . . ? O1 Ru1 C32B C33B -174.3(6) . . . . ? N3 Ru1 C32B C33B -82.9(6) . . . . ? C29B Ru1 C32B C33B 61.9(4) . . . . ? C33A Ru1 C32B C33B 16.0(12) . . . . ? C28A Ru1 C32B C33B 42.3(6) . . . . ? C32A Ru1 C32B C33B 159(5) . . . . ? C29A Ru1 C32B C33B 77.3(6) . . . . ? C28B Ru1 C32B C33B 26.8(2) . . . . ? C30B Ru1 C32B C31B -31.7(3) . . . . ? O1 Ru1 C32B C31B 53.3(6) . . . . ? N3 Ru1 C32B C31B 144.7(7) . . . . ? C29B Ru1 C32B C31B -70.6(5) . . . . ? C33A Ru1 C32B C31B -116.4(13) . . . . ? C28A Ru1 C32B C31B -90.2(6) . . . . ? C32A Ru1 C32B C31B 27(5) . . . . ? C29A Ru1 C32B C31B -55.2(7) . . . . ? C33B Ru1 C32B C31B -132.5(3) . . . . ? C28B Ru1 C32B C31B -105.7(5) . . . . ? C31B C32B C33B C28B 0.0 . . . . ? Ru1 C32B C33B C28B -50.8(6) . . . . ? C31B C32B C33B Ru1 50.8(6) . . . . ? C29B C28B C33B C32B 0.0 . . . . ? C34B C28B C33B C32B 175.8(17) . . . . ? Ru1 C28B C33B C32B 48.4(5) . . . . ? C29B C28B C33B Ru1 -48.4(5) . . . . ? C34B C28B C33B Ru1 127.4(15) . . . . ? C31B Ru1 C33B C32B -30.0(3) . . . . ? C30B Ru1 C33B C32B -70.1(6) . . . . ? O1 Ru1 C33B C32B 12.8(12) . . . . ? N3 Ru1 C33B C32B 98.4(7) . . . . ? C29B Ru1 C33B C32B -107.9(5) . . . . ? C33A Ru1 C33B C32B -41(4) . . . . ? C28A Ru1 C33B C32B -112.1(7) . . . . ? C32A Ru1 C33B C32B -4.9(11) . . . . ? C29A Ru1 C33B C32B -93.4(7) . . . . ? C28B Ru1 C33B C32B -135.2(3) . . . . ? C31B Ru1 C33B C28B 105.2(5) . . . . ? C30B Ru1 C33B C28B 65.1(6) . . . . ? O1 Ru1 C33B C28B 148.0(12) . . . . ? N3 Ru1 C33B C28B -126.4(6) . . . . ? C32B Ru1 C33B C28B 135.2(3) . . . . ? C29B Ru1 C33B C28B 27.3(3) . . . . ? C33A Ru1 C33B C28B 95(4) . . . . ? C28A Ru1 C33B C28B 23.1(7) . . . . ? C32A Ru1 C33B C28B 130.3(10) . . . . ? C29A Ru1 C33B C28B 41.8(6) . . . . ? C32B C31B C35B C37B -174(4) . . . . ? C30B C31B C35B C37B 8(6) . . . . ? Ru1 C31B C35B C37B 93(5) . . . . ? C32B C31B C35B C36B -39(4) . . . . ? C30B C31B C35B C36B 143(3) . . . . ? Ru1 C31B C35B C36B -132(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.929 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.092 _iucr_refine_instructions_details ; TITL CC7 in P2(1)/c CELL 0.71073 11.3370 20.5920 14.3231 90.0000 92.5794 90.0000 ZERR 4.00 0.0024 0.0038 0.0013 0.0000 0.0120 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL RU UNIT 148 168 12 4 4 4 REM ---------------------------------------------------------- REM Data collection: Bruker Nonius APEX II CCD REM Absorption correction: SADABS REM Crystal habit: prismatic; Crystal colour: orange REM ---------------------------------------------------------- L.S. 10 OMIT 0 1 2 ACTA CONF WPDB -2 SIZE 0.489 0.443 0.118 BOND $H FMAP 2 PLAN 10 TEMP -173 EQIV $1 1-X, -Y, 1-Z FREE C17A C37A_$1 FREE C37A C17A_$1 WGHT 0.023900 9.137500 FVAR 0.35639 0.40137 0.62078 RU1 6 0.443351 0.157656 0.135046 11.00000 0.05543 0.03419 = 0.02652 -0.00594 0.01213 -0.01066 CL1 5 0.555096 0.251640 0.190239 11.00000 0.04930 0.03343 = 0.06397 -0.01144 0.00702 -0.00497 O1 4 0.310013 0.195097 0.213235 11.00000 0.03934 0.05546 = 0.02432 0.00485 0.00485 0.00281 N1 3 0.200330 0.202042 0.344724 11.00000 0.03042 0.04432 = 0.02583 -0.00109 -0.00087 -0.00177 N2 3 0.206442 0.181830 0.437680 11.00000 0.04410 0.07286 = 0.02336 0.00218 0.00497 0.00501 N3 3 0.516099 0.112301 0.258080 11.00000 0.03923 0.03228 = 0.03742 -0.01046 0.00273 -0.00384 C1 1 0.298085 0.181531 0.299303 11.00000 0.03080 0.03386 = 0.02370 -0.00395 0.00197 -0.00768 C2 1 0.095827 0.232813 0.308610 11.00000 0.02934 0.03236 = 0.04735 -0.00775 -0.00246 -0.00185 C3 1 0.092277 0.264535 0.222896 11.00000 0.03320 0.05666 = 0.05691 0.01038 -0.00281 0.00083 AFIX 43 H3 2 0.161090 0.267253 0.187620 11.00000 -1.20000 AFIX 0 C4 1 -0.013341 0.292305 0.189293 11.00000 0.06581 0.08212 = 0.09017 0.02704 -0.00794 0.01261 AFIX 43 H4 2 -0.016694 0.313797 0.130544 11.00000 -1.20000 AFIX 0 C5 1 -0.113155 0.288796 0.240805 11.00000 0.04975 0.08844 = 0.13546 0.02155 -0.00503 0.02766 AFIX 43 H5 2 -0.184417 0.308613 0.217961 11.00000 -1.20000 AFIX 0 C6 1 -0.109784 0.256728 0.325035 11.00000 0.04407 0.06885 = 0.11891 0.00360 0.01735 0.01027 AFIX 43 H6 2 -0.179231 0.253727 0.359509 11.00000 -1.20000 AFIX 0 C7 1 -0.005482 0.228659 0.360123 11.00000 0.04492 0.05012 = 0.06812 -0.00338 0.01076 0.00538 AFIX 43 H7 2 -0.003177 0.206851 0.418625 11.00000 -1.20000 AFIX 0 C8 1 0.306383 0.149702 0.448880 11.00000 0.04423 0.07067 = 0.02339 0.00124 -0.00020 0.01008 C9 1 0.334929 0.123482 0.545755 11.00000 0.08631 0.12730 = 0.02780 0.01724 0.01344 0.04471 AFIX 33 H9A 2 0.274730 0.137994 0.588112 11.00000 -1.50000 H9B 2 0.412486 0.139523 0.568236 11.00000 -1.50000 H9C 2 0.336094 0.075916 0.543777 11.00000 -1.50000 AFIX 0 C10 1 0.371024 0.146654 0.364649 11.00000 0.04129 0.03817 = 0.02081 -0.00271 -0.00067 -0.00271 C11 1 0.478839 0.113993 0.343735 11.00000 0.03450 0.03331 = 0.02923 -0.00818 -0.00515 -0.00292 C12 1 0.551451 0.083538 0.423291 11.00000 0.05262 0.04786 = 0.03279 -0.01276 -0.00922 0.00930 AFIX 23 H12A 2 0.597946 0.046950 0.399278 11.00000 -1.20000 H12B 2 0.498267 0.066137 0.470213 11.00000 -1.20000 AFIX 0 C13 1 0.636083 0.134274 0.470104 11.00000 0.05794 0.06173 = 0.07789 -0.03404 -0.03574 0.02028 AFIX 23 PART 1 H13A 2 0.654573 0.167176 0.422532 21.00000 -1.20000 H13B 2 0.593221 0.156760 0.519407 21.00000 -1.20000 PART 2 H13C 2 0.591353 0.172524 0.490954 -21.00000 -1.20000 H13D 2 0.695243 0.148914 0.425884 -21.00000 -1.20000 AFIX 0 PART 1 C14A 1 0.748300 0.109939 0.512267 21.00000 0.03666 0.06691 = 0.05932 -0.00962 0.00168 -0.00319 AFIX 23 H14A 2 0.801185 0.146712 0.529438 21.00000 -1.20000 H14B 2 0.788350 0.081966 0.467247 21.00000 -1.20000 AFIX 0 C15A 1 0.721378 0.072413 0.596154 21.00000 0.03186 0.08242 = 0.08069 0.01338 -0.02338 -0.00565 AFIX 23 H15A 2 0.661468 0.039184 0.578174 21.00000 -1.20000 H15B 2 0.685580 0.102085 0.641316 21.00000 -1.20000 AFIX 0 C16A 1 0.827022 0.038267 0.645624 21.00000 0.04365 0.09333 = 0.09082 0.05574 -0.01856 0.00229 AFIX 23 H16A 2 0.856075 0.004208 0.603623 21.00000 -1.20000 H16B 2 0.891326 0.070337 0.656050 21.00000 -1.20000 AFIX 0 C17A 1 0.801630 0.007820 0.736984 21.00000 0.07778 0.14039 = 0.15607 0.05321 -0.05576 -0.03133 AFIX 33 H17A 2 0.781448 0.041682 0.781616 21.00000 -1.50000 H17B 2 0.871533 -0.015868 0.761072 21.00000 -1.50000 H17C 2 0.735215 -0.022371 0.728324 21.00000 -1.50000 AFIX 0 PART 2 C14B 1 0.701869 0.096883 0.559707 -21.00000 0.06254 0.11225 = 0.06095 -0.05618 -0.03082 0.04215 AFIX 23 H14C 2 0.732405 0.129417 0.605591 -21.00000 -1.20000 H14D 2 0.643980 0.069205 0.590794 -21.00000 -1.20000 AFIX 0 C15B 1 0.801854 0.055713 0.528568 -21.00000 0.06124 0.09330 = 0.04823 -0.01629 -0.01451 0.03306 AFIX 23 H15C 2 0.860550 0.084677 0.500835 -21.00000 -1.20000 H15D 2 0.770740 0.026598 0.478265 -21.00000 -1.20000 AFIX 0 C16B 1 0.867393 0.013238 0.604149 -21.00000 0.06724 0.16587 = 0.05276 -0.00939 -0.01664 0.05385 AFIX 23 H16C 2 0.903689 0.043150 0.651316 -21.00000 -1.20000 H16D 2 0.806718 -0.012073 0.635921 -21.00000 -1.20000 AFIX 0 C17B 1 0.953056 -0.029388 0.579712 -21.00000 0.21434 0.10032 = 0.18709 -0.03460 -0.12786 0.06519 AFIX 33 H17D 2 0.927184 -0.052192 0.522327 -21.00000 -1.50000 H17E 2 0.967332 -0.060976 0.630137 -21.00000 -1.50000 H17F 2 1.026096 -0.005571 0.569144 -21.00000 -1.50000 AFIX 0 PART 0 C18 1 0.626849 0.079160 0.243753 11.00000 0.05589 0.03802 = 0.05002 -0.00821 0.01537 0.00068 C19 1 0.729242 0.114139 0.237546 11.00000 0.05018 0.03909 = 0.10192 -0.01149 0.02821 -0.00744 AFIX 43 H19 2 0.727840 0.160072 0.243589 11.00000 -1.20000 AFIX 0 C20 1 0.836677 0.081993 0.222194 11.00000 0.05363 0.05729 = 0.13843 -0.01021 0.04337 -0.00666 AFIX 43 H20 2 0.907174 0.106546 0.217935 11.00000 -1.20000 AFIX 0 C21 1 0.840344 0.015946 0.213396 11.00000 0.07159 0.05330 = 0.10896 -0.00416 0.04301 0.00943 AFIX 43 H21 2 0.913495 -0.004945 0.203699 11.00000 -1.20000 AFIX 0 C22 1 0.736682 -0.021551 0.218557 11.00000 0.07295 0.04267 = 0.04911 -0.00132 0.02427 0.00658 C23 1 0.736611 -0.090382 0.211272 11.00000 0.09674 0.04690 = 0.03778 -0.00248 0.02075 0.01325 AFIX 43 H23 2 0.808736 -0.112381 0.201739 11.00000 -1.20000 AFIX 0 C24 1 0.635813 -0.125435 0.217622 11.00000 0.11812 0.03524 = 0.02259 0.00140 0.00322 -0.00052 AFIX 43 H24 2 0.638514 -0.171430 0.213046 11.00000 -1.20000 AFIX 0 C25 1 0.528791 -0.094644 0.230750 11.00000 0.08194 0.03527 = 0.02572 0.00406 -0.01499 -0.00825 AFIX 43 H25 2 0.458862 -0.119794 0.234125 11.00000 -1.20000 AFIX 0 C26 1 0.522852 -0.028076 0.238933 11.00000 0.06434 0.03788 = 0.02283 -0.00085 -0.00440 -0.00692 AFIX 43 H26 2 0.449136 -0.007711 0.248324 11.00000 -1.20000 AFIX 0 C27 1 0.626688 0.010304 0.233375 11.00000 0.05757 0.03845 = 0.03733 -0.00906 0.00922 -0.00951 AFIX 66 PART 1 C28A 1 0.521548 0.149125 0.000301 31.00000 0.04505 0.07942 = 0.03104 -0.02213 0.00359 -0.03981 C29A 1 0.429791 0.193495 -0.012155 31.00000 0.05316 0.04653 = 0.02396 0.00358 0.00146 -0.02845 AFIX 43 H29A 2 0.444951 0.235655 -0.035732 31.00000 -1.20000 AFIX 65 C30A 1 0.315850 0.176180 0.009885 31.00000 0.02931 0.07238 = 0.01467 0.00357 -0.00907 -0.01154 AFIX 43 H30A 2 0.253138 0.206506 0.001372 31.00000 -1.20000 AFIX 65 C31A 1 0.293667 0.114494 0.044382 31.00000 0.03546 0.06054 = 0.01929 0.00037 0.00308 -0.02548 C32A 1 0.385423 0.070123 0.056839 31.00000 0.03570 0.03876 = 0.01739 -0.01326 0.00975 -0.01009 AFIX 43 H32A 2 0.370261 0.027963 0.080416 31.00000 -1.20000 AFIX 65 C33A 1 0.499364 0.087437 0.034799 31.00000 0.02584 0.05172 = 0.03636 -0.02203 0.00389 -0.00873 AFIX 43 H33A 2 0.562076 0.057111 0.043312 31.00000 -1.20000 AFIX 0 C34A 1 0.652845 0.171965 -0.019051 31.00000 0.05418 0.07944 = 0.04103 -0.02122 0.02185 -0.02565 AFIX 33 H34A 2 0.663840 0.172174 -0.086525 31.00000 -1.50000 H34B 2 0.709447 0.141935 0.011502 31.00000 -1.50000 H34C 2 0.665811 0.215802 0.005996 31.00000 -1.50000 AFIX 0 C35A 1 0.169973 0.100129 0.080775 31.00000 0.03390 0.06586 = 0.03847 -0.00220 -0.00087 -0.02147 AFIX 13 H35A 2 0.145608 0.140595 0.113355 31.00000 -1.20000 AFIX 0 C36A 1 0.080057 0.091218 -0.002055 31.00000 0.03871 0.12634 = 0.05895 -0.01093 0.00139 -0.01816 AFIX 33 H36A 2 0.099945 0.052165 -0.037149 31.00000 -1.50000 H36B 2 0.082374 0.129186 -0.043185 31.00000 -1.50000 H36C 2 0.000633 0.086632 0.021456 31.00000 -1.50000 AFIX 0 C37A 1 0.167430 0.047155 0.152592 31.00000 0.05899 0.10448 = 0.07361 0.02983 0.01443 -0.02161 AFIX 33 H37A 2 0.189351 0.005838 0.124173 31.00000 -1.50000 H37B 2 0.087735 0.043685 0.175935 31.00000 -1.50000 H37C 2 0.223543 0.057343 0.204573 31.00000 -1.50000 AFIX 66 PART 2 C28B 1 0.567725 0.145581 0.017223 -31.00000 0.02329 0.03990 = 0.03292 -0.01876 0.01733 -0.02167 C29B 1 0.480643 0.191870 -0.001625 -31.00000 0.10877 0.03609 = 0.02434 -0.01118 0.01054 -0.04901 AFIX 43 H29B 2 0.501662 0.233884 -0.022658 -31.00000 -1.20000 AFIX 65 C30B 1 0.362809 0.176686 0.010303 -31.00000 0.05318 0.02029 = 0.04629 -0.01461 -0.01742 -0.00384 AFIX 43 H30B 2 0.303293 0.208322 -0.002578 -31.00000 -1.20000 AFIX 65 C31B 1 0.332056 0.115212 0.041078 -31.00000 0.04689 0.12124 = 0.08035 -0.04725 -0.00075 -0.04368 C32B 1 0.419136 0.068923 0.059926 -31.00000 0.08736 0.06429 = 0.04228 0.00159 -0.00661 -0.04370 AFIX 43 H32B 2 0.398117 0.026909 0.080959 -31.00000 -1.20000 AFIX 65 C33B 1 0.536971 0.084107 0.047998 -31.00000 0.04747 0.04072 = 0.02443 -0.01498 0.00376 0.00274 AFIX 43 H33B 2 0.596486 0.052470 0.060880 -31.00000 -1.20000 AFIX 0 C34B 1 0.705448 0.158994 0.013138 -31.00000 0.09279 0.25479 = 0.05813 0.04376 0.04338 0.02243 AFIX 33 H34D 2 0.730066 0.152742 -0.050960 -31.00000 -1.50000 H34E 2 0.748766 0.128793 0.054966 -31.00000 -1.50000 H34F 2 0.722436 0.203719 0.032889 -31.00000 -1.50000 AFIX 0 C35B 1 0.212238 0.101288 0.056295 -31.00000 0.29694 0.15565 = 0.03272 -0.01993 -0.01654 -0.00991 AFIX 13 H35B 2 0.212212 0.100723 0.126107 -31.00000 -1.20000 AFIX 0 C36B 1 0.159932 0.028006 0.030045 -31.00000 0.13248 0.22337 = 0.20987 -0.12297 0.05033 -0.05547 AFIX 33 H36D 2 0.208409 -0.004914 0.062951 -31.00000 -1.50000 H36E 2 0.162231 0.020967 -0.037517 -31.00000 -1.50000 H36F 2 0.078246 0.024659 0.049188 -31.00000 -1.50000 AFIX 0 C37B 1 0.121509 0.137513 0.035584 -31.00000 0.19564 0.32205 = 0.08720 -0.07246 0.02787 -0.16314 AFIX 33 H37D 2 0.053171 0.121441 0.068189 -31.00000 -1.50000 H37E 2 0.104103 0.136209 -0.032032 -31.00000 -1.50000 H37F 2 0.138549 0.182318 0.054914 -31.00000 -1.50000 PART 0 HKLF 4 REM CC7 in P2(1)/c REM R1 = 0.0649 for 5112 Fo > 4sig(Fo) and 0.1104 for all 7635 data REM 492 parameters refined using 0 restraints END WGHT 0.0238 9.1437 REM Highest difference peak 0.929, deepest hole -1.091, 1-sigma level 0.092 Q1 1 0.4036 0.1280 0.1389 11.00000 0.05 0.93 Q2 1 0.7378 0.1186 -0.0929 11.00000 0.05 0.73 Q3 1 0.7757 0.2007 0.0392 11.00000 0.05 0.64 Q4 1 0.5335 0.2300 0.2388 11.00000 0.05 0.59 Q5 1 0.5007 0.1505 0.1546 11.00000 0.05 0.57 Q6 1 0.5838 0.2475 0.2440 11.00000 0.05 0.48 Q7 1 0.4625 0.1044 0.1098 11.00000 0.05 0.44 Q8 1 0.4219 0.1879 0.1367 11.00000 0.05 0.41 Q9 1 0.7765 -0.0228 0.2616 11.00000 0.05 0.40 Q10 1 0.4578 0.0815 0.2643 11.00000 0.05 0.36 ; data_9 _audit_update_record ; 2013-05-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H46 Cl N3 O Ru, C H2 Cl2' _chemical_formula_sum 'C40 H48 Cl3 N3 O Ru' _chemical_formula_weight 794.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 33.517(5) _cell_length_b 33.517(5) _cell_length_c 19.157(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 18638(5) _cell_formula_units_Z 18 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 1493 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7416 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 140(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 marmux _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14977 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.1628 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7524 _reflns_number_gt 5277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marmux - Micro-beam system, marresearch, 2010' _computing_cell_refinement 'automar, marresearch, 2010' _computing_data_reduction 'automar, marresearch, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1702P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7524 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.3012 _refine_ls_wR_factor_gt 0.2690 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.39660(2) 0.43139(2) 0.86590(3) 0.0574(3) Uani 1 1 d . . . Cl1 Cl 0.47370(6) 0.49863(6) 0.87659(9) 0.0645(5) Uani 1 1 d . . . O1 O 0.40744(17) 0.44285(18) 0.7589(2) 0.0648(12) Uani 1 1 d . . . N1 N 0.4461(2) 0.4474(2) 0.6549(3) 0.0602(14) Uani 1 1 d . . . N2 N 0.4776(2) 0.4354(2) 0.6284(3) 0.0614(14) Uani 1 1 d . . . N3 N 0.4357(2) 0.39603(19) 0.8642(3) 0.0577(13) Uani 1 1 d . . . C1 C 0.4362(2) 0.4343(2) 0.7237(3) 0.0592(16) Uani 1 1 d . . . C2 C 0.4361(3) 0.4771(3) 0.6145(3) 0.0628(17) Uani 1 1 d . . . C3 C 0.3947(3) 0.4771(3) 0.6236(4) 0.073(2) Uani 1 1 d . . . H3 H 0.3723 0.4564 0.6556 0.088 Uiso 1 1 calc R . . C4 C 0.3864(3) 0.5081(3) 0.5850(4) 0.081(2) Uani 1 1 d . . . H4 H 0.3588 0.5090 0.5920 0.097 Uiso 1 1 calc R . . C5 C 0.4194(4) 0.5375(3) 0.5361(4) 0.084(3) Uani 1 1 d . . . H5 H 0.4137 0.5580 0.5093 0.100 Uiso 1 1 calc R . . C6 C 0.4605(3) 0.5370(3) 0.5268(4) 0.081(2) Uani 1 1 d . . . H6 H 0.4826 0.5568 0.4936 0.097 Uiso 1 1 calc R . . C7 C 0.4684(3) 0.5074(3) 0.5663(3) 0.0702(19) Uani 1 1 d . . . H7 H 0.4966 0.5075 0.5607 0.084 Uiso 1 1 calc R . . C8 C 0.4874(2) 0.4157(3) 0.6808(3) 0.0626(17) Uani 1 1 d . . . C9 C 0.5213(3) 0.3991(3) 0.6667(4) 0.0686(19) Uani 1 1 d . . . H9A H 0.5316 0.4057 0.6181 0.103 Uiso 1 1 calc R . . H9B H 0.5062 0.3659 0.6751 0.103 Uiso 1 1 calc R . . H9C H 0.5479 0.4152 0.6979 0.103 Uiso 1 1 calc R . . C10 C 0.4623(2) 0.4141(2) 0.7439(3) 0.0594(16) Uani 1 1 d . . . C11 C 0.4629(2) 0.3963(2) 0.8113(3) 0.0577(16) Uani 1 1 d . . . C12 C 0.4976(2) 0.3813(2) 0.8265(4) 0.0618(17) Uani 1 1 d . . . H12A H 0.5012 0.3661 0.7846 0.074 Uiso 1 1 calc R . . H12B H 0.4859 0.3585 0.8649 0.074 Uiso 1 1 calc R . . C13 C 0.5445(3) 0.4215(3) 0.8470(4) 0.075(2) Uani 1 1 d . . . H13A H 0.5563 0.4440 0.8081 0.090 Uiso 1 1 calc R . . H13B H 0.5405 0.4372 0.8880 0.090 Uiso 1 1 calc R . . C14 C 0.5800(4) 0.4079(4) 0.8645(6) 0.109(3) Uani 1 1 d . . . H14A H 0.6099 0.4363 0.8724 0.131 Uiso 1 1 calc R . . H14B H 0.5836 0.3920 0.8235 0.131 Uiso 1 1 calc R . . C15 C 0.5691(5) 0.3769(5) 0.9278(8) 0.140(5) Uani 1 1 d . . . H15A H 0.5617 0.3912 0.9670 0.168 Uiso 1 1 calc R . . H15B H 0.5410 0.3472 0.9173 0.168 Uiso 1 1 calc R . . C16 C 0.6055(7) 0.3664(7) 0.9523(12) 0.211(10) Uani 1 1 d . . . H16A H 0.6332 0.3952 0.9675 0.254 Uiso 1 1 calc R . . H16B H 0.6146 0.3531 0.9135 0.254 Uiso 1 1 calc R . . C17 C 0.5860(8) 0.3305(8) 1.0167(14) 0.287(16) Uani 1 1 d . . . H17A H 0.5530 0.3194 1.0228 0.430 Uiso 1 1 calc R . . H17B H 0.6025 0.3458 1.0595 0.430 Uiso 1 1 calc R . . H17C H 0.5904 0.3043 1.0067 0.430 Uiso 1 1 calc R . . C18 C 0.4382(2) 0.3767(2) 0.9304(3) 0.0580(16) Uani 1 1 d . . . C19 C 0.4149(2) 0.3273(2) 0.9375(3) 0.0590(16) Uani 1 1 d . . . C20 C 0.3903(3) 0.2966(3) 0.8822(3) 0.0649(18) Uani 1 1 d . . . H20 H 0.3888 0.3086 0.8379 0.078 Uiso 1 1 calc R . . C21 C 0.3686(3) 0.2501(3) 0.8917(4) 0.073(2) Uani 1 1 d . . . H21 H 0.3525 0.2302 0.8538 0.087 Uiso 1 1 calc R . . C22 C 0.3695(3) 0.2308(3) 0.9567(4) 0.072(2) Uani 1 1 d . . . H22 H 0.3537 0.1983 0.9627 0.087 Uiso 1 1 calc R . . C23 C 0.3934(3) 0.2594(3) 1.0116(4) 0.075(2) Uani 1 1 d . . . H23 H 0.3942 0.2463 1.0551 0.090 Uiso 1 1 calc R . . C24 C 0.4171(3) 0.3086(2) 1.0046(4) 0.0650(17) Uani 1 1 d . . . C25 C 0.4422(3) 0.3386(3) 1.0600(4) 0.0697(19) Uani 1 1 d . . . H25 H 0.4431 0.3266 1.1045 0.084 Uiso 1 1 calc R . . C26 C 0.4656(3) 0.3859(3) 1.0486(3) 0.0684(19) Uani 1 1 d . . . H26 H 0.4840 0.4059 1.0851 0.082 Uiso 1 1 calc R . . C27 C 0.4629(2) 0.4047(2) 0.9859(3) 0.0583(16) Uani 1 1 d . . . H27 H 0.4781 0.4373 0.9807 0.070 Uiso 1 1 calc R . . C28 C 0.3746(3) 0.4459(3) 0.9675(4) 0.071(2) Uani 1 1 d . . . C29 C 0.3678(3) 0.4713(3) 0.9125(4) 0.0652(18) Uani 1 1 d . . . C30 C 0.3413(3) 0.4498(3) 0.8520(4) 0.071(2) Uani 1 1 d . . . C31 C 0.3223(3) 0.4004(3) 0.8437(4) 0.0705(19) Uani 1 1 d . . . C32 C 0.3276(3) 0.3743(3) 0.8985(4) 0.071(2) Uani 1 1 d . . . C33 C 0.3525(3) 0.3966(3) 0.9604(4) 0.072(2) Uani 1 1 d . . . C34 C 0.4055(3) 0.4716(4) 1.0283(4) 0.093(3) Uani 1 1 d . . . H34A H 0.3877 0.4769 1.0639 0.139 Uiso 1 1 calc R . . H34B H 0.4308 0.5013 1.0120 0.139 Uiso 1 1 calc R . . H34C H 0.4182 0.4534 1.0483 0.139 Uiso 1 1 calc R . . C35 C 0.3890(3) 0.5240(3) 0.9205(5) 0.096(3) Uani 1 1 d . . . H35A H 0.4226 0.5390 0.9159 0.144 Uiso 1 1 calc R . . H35B H 0.3813 0.5308 0.9666 0.144 Uiso 1 1 calc R . . H35C H 0.3768 0.5354 0.8842 0.144 Uiso 1 1 calc R . . C36 C 0.3362(3) 0.4775(3) 0.7949(5) 0.086(2) Uani 1 1 d . . . H36A H 0.3369 0.5047 0.8150 0.130 Uiso 1 1 calc R . . H36B H 0.3069 0.4586 0.7708 0.130 Uiso 1 1 calc R . . H36C H 0.3617 0.4873 0.7616 0.130 Uiso 1 1 calc R . . C37 C 0.2963(3) 0.3769(3) 0.7786(4) 0.086(3) Uani 1 1 d . . . H37A H 0.2874 0.3442 0.7804 0.129 Uiso 1 1 calc R . . H37B H 0.3160 0.3913 0.7378 0.129 Uiso 1 1 calc R . . H37C H 0.2687 0.3797 0.7752 0.129 Uiso 1 1 calc R . . C38 C 0.3056(3) 0.3213(3) 0.8901(6) 0.107(4) Uani 1 1 d . . . H38A H 0.2725 0.3064 0.8991 0.161 Uiso 1 1 calc R . . H38B H 0.3198 0.3099 0.9235 0.161 Uiso 1 1 calc R . . H38C H 0.3108 0.3142 0.8425 0.161 Uiso 1 1 calc R . . C39 C 0.3524(4) 0.3671(4) 1.0203(4) 0.093(3) Uani 1 1 d . . . H39A H 0.3816 0.3836 1.0458 0.139 Uiso 1 1 calc R . . H39B H 0.3488 0.3382 1.0019 0.139 Uiso 1 1 calc R . . H39C H 0.3268 0.3604 1.0518 0.139 Uiso 1 1 calc R . . Cl2 Cl 0.25277(13) 0.19436(14) 0.9247(2) 0.1414(12) Uani 1 1 d . . . Cl3 Cl 0.17197(17) 0.10354(16) 0.9182(4) 0.207(2) Uani 1 1 d . . . C40 C 0.2325(4) 0.1356(4) 0.9291(6) 0.110(3) Uani 1 1 d . . . H40A H 0.2408 0.1280 0.9749 0.132 Uiso 1 1 calc R . . H40B H 0.2474 0.1268 0.8923 0.132 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 0.0576(4) 0.0546(4) 0.0570(4) 0.0037(2) 0.0058(2) 0.0258(3) Cl1 0.0606(10) 0.0544(10) 0.0698(10) 0.0028(7) 0.0053(7) 0.0221(8) O1 0.062(3) 0.073(3) 0.064(3) 0.005(2) 0.003(2) 0.038(3) N1 0.069(4) 0.059(3) 0.052(3) 0.002(2) 0.000(2) 0.032(3) N2 0.062(4) 0.064(4) 0.055(3) -0.001(3) 0.005(2) 0.029(3) N3 0.060(3) 0.053(3) 0.058(3) 0.002(2) 0.003(2) 0.027(3) C1 0.064(4) 0.059(4) 0.051(3) 0.005(3) 0.006(3) 0.027(3) C2 0.067(4) 0.067(4) 0.054(3) -0.009(3) -0.012(3) 0.034(4) C3 0.087(6) 0.073(5) 0.060(4) 0.005(3) 0.002(4) 0.040(4) C4 0.093(6) 0.094(6) 0.069(5) -0.004(4) -0.004(4) 0.057(5) C5 0.125(8) 0.076(5) 0.053(4) -0.001(3) -0.008(4) 0.053(6) C6 0.105(7) 0.080(6) 0.064(4) 0.003(4) 0.002(4) 0.051(5) C7 0.082(5) 0.070(5) 0.053(4) 0.007(3) -0.002(3) 0.033(4) C8 0.058(4) 0.074(5) 0.050(3) -0.001(3) 0.003(3) 0.028(4) C9 0.062(4) 0.080(5) 0.066(4) 0.001(3) 0.012(3) 0.037(4) C10 0.056(4) 0.067(4) 0.056(3) 0.002(3) 0.006(3) 0.032(3) C11 0.058(4) 0.056(4) 0.056(3) -0.001(3) -0.002(3) 0.027(3) C12 0.067(4) 0.059(4) 0.058(4) 0.001(3) 0.002(3) 0.031(4) C13 0.067(5) 0.086(6) 0.075(5) 0.002(4) 0.006(4) 0.041(4) C14 0.082(7) 0.130(9) 0.133(8) -0.015(7) -0.023(6) 0.067(7) C15 0.146(12) 0.128(11) 0.182(13) -0.022(9) -0.057(10) 0.094(10) C16 0.192(18) 0.197(19) 0.30(2) -0.062(17) -0.143(17) 0.140(16) C17 0.28(3) 0.23(3) 0.36(3) 0.06(2) -0.16(3) 0.13(2) C18 0.063(4) 0.052(4) 0.058(4) 0.004(3) 0.011(3) 0.028(3) C19 0.065(4) 0.049(4) 0.056(4) 0.004(3) 0.011(3) 0.023(3) C20 0.080(5) 0.062(4) 0.051(3) 0.003(3) 0.007(3) 0.035(4) C21 0.088(6) 0.058(4) 0.068(4) -0.007(3) 0.004(4) 0.033(4) C22 0.086(5) 0.047(4) 0.072(4) 0.007(3) 0.006(4) 0.025(4) C23 0.094(6) 0.067(5) 0.067(4) 0.020(4) 0.014(4) 0.044(5) C24 0.070(5) 0.055(4) 0.065(4) 0.005(3) 0.005(3) 0.028(4) C25 0.081(5) 0.073(5) 0.061(4) 0.008(3) 0.004(3) 0.043(4) C26 0.071(5) 0.069(5) 0.057(4) -0.005(3) 0.000(3) 0.028(4) C27 0.064(4) 0.053(4) 0.056(3) -0.003(3) -0.002(3) 0.028(3) C28 0.067(5) 0.081(5) 0.064(4) 0.002(4) 0.017(3) 0.036(4) C29 0.066(4) 0.063(4) 0.067(4) 0.004(3) 0.013(3) 0.033(4) C30 0.063(5) 0.081(5) 0.075(5) 0.013(4) 0.009(4) 0.040(4) C31 0.057(4) 0.073(5) 0.074(4) -0.008(4) 0.005(3) 0.027(4) C32 0.061(4) 0.054(4) 0.093(5) 0.006(4) 0.027(4) 0.025(4) C33 0.073(5) 0.072(5) 0.071(4) 0.012(4) 0.029(4) 0.035(4) C34 0.103(7) 0.127(8) 0.057(4) -0.028(5) -0.005(4) 0.064(6) C35 0.096(7) 0.056(5) 0.129(7) -0.006(5) 0.018(6) 0.033(5) C36 0.086(6) 0.103(7) 0.090(5) 0.016(5) -0.003(4) 0.062(6) C37 0.052(4) 0.108(7) 0.086(5) -0.022(5) -0.009(4) 0.032(5) C38 0.073(6) 0.061(5) 0.175(11) 0.000(6) 0.035(6) 0.024(5) C39 0.113(7) 0.112(7) 0.078(5) 0.037(5) 0.040(5) 0.074(6) Cl2 0.121(3) 0.146(3) 0.167(3) -0.033(2) -0.001(2) 0.074(2) Cl3 0.143(4) 0.126(3) 0.361(7) -0.037(4) 0.039(4) 0.074(3) C40 0.116(9) 0.122(9) 0.117(8) 0.017(7) 0.004(6) 0.078(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.084(5) . ? Ru1 N3 2.164(6) . ? Ru1 C29 2.195(7) . ? Ru1 C31 2.208(8) . ? Ru1 C28 2.219(7) . ? Ru1 C32 2.230(7) . ? Ru1 C30 2.242(8) . ? Ru1 C33 2.257(7) . ? Ru1 Cl1 2.4443(19) . ? O1 C1 1.320(8) . ? N1 C1 1.376(8) . ? N1 N2 1.399(8) . ? N1 C2 1.426(9) . ? N2 C8 1.329(9) . ? N3 C11 1.360(8) . ? N3 C18 1.444(8) . ? C1 C10 1.401(10) . ? C2 C3 1.397(11) . ? C2 C7 1.398(10) . ? C3 C4 1.410(11) . ? C3 H3 0.9500 . ? C4 C5 1.408(12) . ? C4 H4 0.9500 . ? C5 C6 1.397(13) . ? C5 H5 0.9500 . ? C6 C7 1.375(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.459(9) . ? C8 C9 1.516(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.428(9) . ? C11 C12 1.506(10) . ? C12 C13 1.524(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.510(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.518(17) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.503(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.62(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C27 1.385(9) . ? C18 C19 1.443(9) . ? C19 C20 1.419(9) . ? C19 C24 1.446(9) . ? C20 C21 1.364(11) . ? C20 H20 0.9500 . ? C21 C22 1.410(10) . ? C21 H21 0.9500 . ? C22 C23 1.377(11) . ? C22 H22 0.9500 . ? C23 C24 1.435(10) . ? C23 H23 0.9500 . ? C24 C25 1.415(10) . ? C25 C26 1.390(11) . ? C25 H25 0.9500 . ? C26 C27 1.381(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.439(11) . ? C28 C29 1.443(11) . ? C28 C34 1.511(11) . ? C29 C30 1.419(11) . ? C29 C35 1.544(10) . ? C30 C31 1.453(12) . ? C30 C36 1.498(11) . ? C31 C32 1.434(11) . ? C31 C37 1.499(10) . ? C32 C33 1.427(12) . ? C32 C38 1.554(11) . ? C33 C39 1.513(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Cl2 C40 1.736(12) . ? Cl3 C40 1.771(13) . ? C40 H40A 0.9900 . ? C40 H40B 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 O1 Ru1 N3 89.37(19) . . ? O1 Ru1 C29 112.2(2) . . ? N3 Ru1 C29 155.8(2) . . ? O1 Ru1 C31 87.0(2) . . ? N3 Ru1 C31 126.2(3) . . ? C29 Ru1 C31 68.2(3) . . ? O1 Ru1 C28 150.3(3) . . ? N3 Ru1 C28 119.5(3) . . ? C29 Ru1 C28 38.2(3) . . ? C31 Ru1 C28 81.5(3) . . ? O1 Ru1 C32 116.4(3) . . ? N3 Ru1 C32 100.8(3) . . ? C29 Ru1 C32 79.9(3) . . ? C31 Ru1 C32 37.7(3) . . ? C28 Ru1 C32 68.0(3) . . ? O1 Ru1 C30 85.7(2) . . ? N3 Ru1 C30 163.7(3) . . ? C29 Ru1 C30 37.3(3) . . ? C31 Ru1 C30 38.1(3) . . ? C28 Ru1 C30 68.5(3) . . ? C32 Ru1 C30 67.9(3) . . ? O1 Ru1 C33 153.2(3) . . ? N3 Ru1 C33 98.5(3) . . ? C29 Ru1 C33 67.4(3) . . ? C31 Ru1 C33 67.6(3) . . ? C28 Ru1 C33 37.5(3) . . ? C32 Ru1 C33 37.1(3) . . ? C30 Ru1 C33 79.6(3) . . ? O1 Ru1 Cl1 84.61(15) . . ? N3 Ru1 Cl1 81.67(16) . . ? C29 Ru1 Cl1 89.3(2) . . ? C31 Ru1 Cl1 150.9(2) . . ? C28 Ru1 Cl1 92.2(2) . . ? C32 Ru1 Cl1 158.8(2) . . ? C30 Ru1 Cl1 113.3(2) . . ? C33 Ru1 Cl1 121.8(2) . . ? C1 O1 Ru1 122.8(4) . . ? C1 N1 N2 110.5(5) . . ? C1 N1 C2 129.7(6) . . ? N2 N1 C2 118.7(5) . . ? C8 N2 N1 106.3(5) . . ? C11 N3 C18 118.0(6) . . ? C11 N3 Ru1 126.5(4) . . ? C18 N3 Ru1 114.7(4) . . ? O1 C1 N1 120.3(6) . . ? O1 C1 C10 131.5(6) . . ? N1 C1 C10 108.1(6) . . ? C3 C2 C7 119.4(7) . . ? C3 C2 N1 120.8(7) . . ? C7 C2 N1 119.8(7) . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.3(9) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 120.6(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 119.1(8) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C2 121.9(8) . . ? C6 C7 H7 119.1 . . ? C2 C7 H7 119.1 . . ? N2 C8 C10 111.2(6) . . ? N2 C8 C9 117.7(6) . . ? C10 C8 C9 131.2(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 C11 126.6(6) . . ? C1 C10 C8 104.0(6) . . ? C11 C10 C8 129.4(7) . . ? N3 C11 C10 121.8(6) . . ? N3 C11 C12 118.7(6) . . ? C10 C11 C12 119.3(6) . . ? C11 C12 C13 112.4(6) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 114.2(8) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 C15 115.4(9) . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14B 108.4 . . ? C15 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C16 C15 C14 117.7(15) . . ? C16 C15 H15A 107.9 . . ? C14 C15 H15A 107.9 . . ? C16 C15 H15B 107.9 . . ? C14 C15 H15B 107.9 . . ? H15A C15 H15B 107.2 . . ? C15 C16 C17 109.8(18) . . ? C15 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C27 C18 C19 120.2(6) . . ? C27 C18 N3 121.3(6) . . ? C19 C18 N3 118.6(6) . . ? C20 C19 C18 123.1(6) . . ? C20 C19 C24 119.2(6) . . ? C18 C19 C24 117.7(6) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 121.4(7) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 119.6(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 121.5(6) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 122.4(7) . . ? C25 C24 C19 120.0(6) . . ? C23 C24 C19 117.5(6) . . ? C26 C25 C24 119.2(7) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C27 C26 C25 121.9(7) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C18 120.8(7) . . ? C26 C27 H27 119.6 . . ? C18 C27 H27 119.6 . . ? C33 C28 C29 117.9(7) . . ? C33 C28 C34 122.7(8) . . ? C29 C28 C34 119.3(8) . . ? C33 C28 Ru1 72.7(4) . . ? C29 C28 Ru1 70.0(4) . . ? C34 C28 Ru1 126.3(6) . . ? C30 C29 C28 122.6(7) . . ? C30 C29 C35 118.5(7) . . ? C28 C29 C35 119.0(7) . . ? C30 C29 Ru1 73.2(4) . . ? C28 C29 Ru1 71.8(4) . . ? C35 C29 Ru1 130.1(6) . . ? C29 C30 C31 118.4(7) . . ? C29 C30 C36 121.1(8) . . ? C31 C30 C36 120.3(8) . . ? C29 C30 Ru1 69.6(4) . . ? C31 C30 Ru1 69.7(4) . . ? C36 C30 Ru1 128.5(5) . . ? C32 C31 C30 119.8(7) . . ? C32 C31 C37 120.2(8) . . ? C30 C31 C37 120.0(8) . . ? C32 C31 Ru1 72.0(4) . . ? C30 C31 Ru1 72.2(4) . . ? C37 C31 Ru1 129.0(5) . . ? C33 C32 C31 120.6(7) . . ? C33 C32 C38 120.1(8) . . ? C31 C32 C38 119.3(8) . . ? C33 C32 Ru1 72.5(4) . . ? C31 C32 Ru1 70.3(4) . . ? C38 C32 Ru1 130.3(5) . . ? C32 C33 C28 120.6(7) . . ? C32 C33 C39 118.6(8) . . ? C28 C33 C39 120.7(8) . . ? C32 C33 Ru1 70.4(4) . . ? C28 C33 Ru1 69.8(4) . . ? C39 C33 Ru1 137.1(6) . . ? C28 C34 H34A 109.5 . . ? C28 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Cl2 C40 Cl3 111.2(6) . . ? Cl2 C40 H40A 109.4 . . ? Cl3 C40 H40A 109.4 . . ? Cl2 C40 H40B 109.4 . . ? Cl3 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? 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 N3 Ru1 O1 C1 -9.6(5) . . . . ? C29 Ru1 O1 C1 159.2(5) . . . . ? C31 Ru1 O1 C1 -135.8(6) . . . . ? C28 Ru1 O1 C1 157.2(6) . . . . ? C32 Ru1 O1 C1 -111.3(6) . . . . ? C30 Ru1 O1 C1 -174.0(6) . . . . ? C33 Ru1 O1 C1 -117.4(7) . . . . ? Cl1 Ru1 O1 C1 72.1(5) . . . . ? C1 N1 N2 C8 -0.9(8) . . . . ? C2 N1 N2 C8 168.1(6) . . . . ? O1 Ru1 N3 C11 13.2(6) . . . . ? C29 Ru1 N3 C11 -140.6(6) . . . . ? C31 Ru1 N3 C11 99.1(6) . . . . ? C28 Ru1 N3 C11 -159.3(5) . . . . ? C32 Ru1 N3 C11 130.0(6) . . . . ? C30 Ru1 N3 C11 85.4(10) . . . . ? C33 Ru1 N3 C11 167.5(6) . . . . ? Cl1 Ru1 N3 C11 -71.4(5) . . . . ? O1 Ru1 N3 C18 -177.1(5) . . . . ? C29 Ru1 N3 C18 29.0(8) . . . . ? C31 Ru1 N3 C18 -91.2(5) . . . . ? C28 Ru1 N3 C18 10.4(6) . . . . ? C32 Ru1 N3 C18 -60.4(5) . . . . ? C30 Ru1 N3 C18 -105.0(9) . . . . ? C33 Ru1 N3 C18 -22.8(5) . . . . ? Cl1 Ru1 N3 C18 98.3(4) . . . . ? Ru1 O1 C1 N1 -172.4(5) . . . . ? Ru1 O1 C1 C10 5.1(11) . . . . ? N2 N1 C1 O1 179.4(6) . . . . ? C2 N1 C1 O1 12.0(11) . . . . ? N2 N1 C1 C10 1.3(8) . . . . ? C2 N1 C1 C10 -166.1(7) . . . . ? C1 N1 C2 C3 -37.1(11) . . . . ? N2 N1 C2 C3 156.4(6) . . . . ? C1 N1 C2 C7 141.4(8) . . . . ? N2 N1 C2 C7 -25.1(9) . . . . ? C7 C2 C3 C4 -1.0(11) . . . . ? N1 C2 C3 C4 177.5(7) . . . . ? C2 C3 C4 C5 2.1(12) . . . . ? C3 C4 C5 C6 -1.4(12) . . . . ? C4 C5 C6 C7 -0.3(13) . . . . ? C5 C6 C7 C2 1.4(12) . . . . ? C3 C2 C7 C6 -0.7(11) . . . . ? N1 C2 C7 C6 -179.3(7) . . . . ? N1 N2 C8 C10 0.1(8) . . . . ? N1 N2 C8 C9 -179.8(6) . . . . ? O1 C1 C10 C11 1.3(13) . . . . ? N1 C1 C10 C11 179.1(7) . . . . ? O1 C1 C10 C8 -179.0(7) . . . . ? N1 C1 C10 C8 -1.2(8) . . . . ? N2 C8 C10 C1 0.7(8) . . . . ? C9 C8 C10 C1 -179.4(8) . . . . ? N2 C8 C10 C11 -179.6(7) . . . . ? C9 C8 C10 C11 0.3(13) . . . . ? C18 N3 C11 C10 179.1(6) . . . . ? Ru1 N3 C11 C10 -11.5(9) . . . . ? C18 N3 C11 C12 -6.5(9) . . . . ? Ru1 N3 C11 C12 162.9(5) . . . . ? C1 C10 C11 N3 2.2(12) . . . . ? C8 C10 C11 N3 -177.4(7) . . . . ? C1 C10 C11 C12 -172.2(7) . . . . ? C8 C10 C11 C12 8.2(11) . . . . ? N3 C11 C12 C13 -91.6(8) . . . . ? C10 C11 C12 C13 83.0(8) . . . . ? C11 C12 C13 C14 178.6(7) . . . . ? C12 C13 C14 C15 -63.9(12) . . . . ? C13 C14 C15 C16 -173.4(12) . . . . ? C14 C15 C16 C17 -176.3(16) . . . . ? C11 N3 C18 C27 101.7(8) . . . . ? Ru1 N3 C18 C27 -68.9(7) . . . . ? C11 N3 C18 C19 -77.3(8) . . . . ? Ru1 N3 C18 C19 112.1(6) . . . . ? C27 C18 C19 C20 -177.9(7) . . . . ? N3 C18 C19 C20 1.0(10) . . . . ? C27 C18 C19 C24 2.2(10) . . . . ? N3 C18 C19 C24 -178.9(6) . . . . ? C18 C19 C20 C21 -179.6(7) . . . . ? C24 C19 C20 C21 0.3(11) . . . . ? C19 C20 C21 C22 0.6(13) . . . . ? C20 C21 C22 C23 -1.2(13) . . . . ? C21 C22 C23 C24 0.8(13) . . . . ? C22 C23 C24 C25 -179.3(8) . . . . ? C22 C23 C24 C19 0.0(12) . . . . ? C20 C19 C24 C25 178.8(7) . . . . ? C18 C19 C24 C25 -1.3(11) . . . . ? C20 C19 C24 C23 -0.6(10) . . . . ? C18 C19 C24 C23 179.3(7) . . . . ? C23 C24 C25 C26 177.8(8) . . . . ? C19 C24 C25 C26 -1.5(11) . . . . ? C24 C25 C26 C27 3.8(12) . . . . ? C25 C26 C27 C18 -3.0(12) . . . . ? C19 C18 C27 C26 -0.1(11) . . . . ? N3 C18 C27 C26 -179.0(6) . . . . ? O1 Ru1 C28 C33 132.5(6) . . . . ? N3 Ru1 C28 C33 -62.8(5) . . . . ? C29 Ru1 C28 C33 129.4(7) . . . . ? C31 Ru1 C28 C33 64.1(5) . . . . ? C32 Ru1 C28 C33 27.4(5) . . . . ? C30 Ru1 C28 C33 101.3(5) . . . . ? Cl1 Ru1 C28 C33 -144.5(5) . . . . ? O1 Ru1 C28 C29 3.1(8) . . . . ? N3 Ru1 C28 C29 167.8(4) . . . . ? C31 Ru1 C28 C29 -65.3(5) . . . . ? C32 Ru1 C28 C29 -102.0(5) . . . . ? C30 Ru1 C28 C29 -28.1(5) . . . . ? C33 Ru1 C28 C29 -129.4(7) . . . . ? Cl1 Ru1 C28 C29 86.1(4) . . . . ? O1 Ru1 C28 C34 -109.3(8) . . . . ? N3 Ru1 C28 C34 55.5(8) . . . . ? C29 Ru1 C28 C34 -112.3(9) . . . . ? C31 Ru1 C28 C34 -177.6(8) . . . . ? C32 Ru1 C28 C34 145.7(9) . . . . ? C30 Ru1 C28 C34 -140.4(9) . . . . ? C33 Ru1 C28 C34 118.3(10) . . . . ? Cl1 Ru1 C28 C34 -26.2(8) . . . . ? C33 C28 C29 C30 -1.4(11) . . . . ? C34 C28 C29 C30 176.4(7) . . . . ? Ru1 C28 C29 C30 55.2(6) . . . . ? C33 C28 C29 C35 177.0(7) . . . . ? C34 C28 C29 C35 -5.1(11) . . . . ? Ru1 C28 C29 C35 -126.4(7) . . . . ? C33 C28 C29 Ru1 -56.6(6) . . . . ? C34 C28 C29 Ru1 121.3(7) . . . . ? O1 Ru1 C29 C30 47.9(5) . . . . ? N3 Ru1 C29 C30 -160.5(5) . . . . ? C31 Ru1 C29 C30 -29.2(5) . . . . ? C28 Ru1 C29 C30 -133.7(7) . . . . ? C32 Ru1 C29 C30 -66.6(5) . . . . ? C33 Ru1 C29 C30 -103.1(5) . . . . ? Cl1 Ru1 C29 C30 131.8(4) . . . . ? O1 Ru1 C29 C28 -178.4(4) . . . . ? N3 Ru1 C29 C28 -26.8(8) . . . . ? C31 Ru1 C29 C28 104.5(5) . . . . ? C32 Ru1 C29 C28 67.1(5) . . . . ? C30 Ru1 C29 C28 133.7(7) . . . . ? C33 Ru1 C29 C28 30.6(5) . . . . ? Cl1 Ru1 C29 C28 -94.5(4) . . . . ? O1 Ru1 C29 C35 -65.4(8) . . . . ? N3 Ru1 C29 C35 86.2(9) . . . . ? C31 Ru1 C29 C35 -142.5(8) . . . . ? C28 Ru1 C29 C35 112.9(9) . . . . ? C32 Ru1 C29 C35 -179.9(8) . . . . ? C30 Ru1 C29 C35 -113.4(9) . . . . ? C33 Ru1 C29 C35 143.6(8) . . . . ? Cl1 Ru1 C29 C35 18.5(7) . . . . ? C28 C29 C30 C31 -3.1(11) . . . . ? C35 C29 C30 C31 178.4(7) . . . . ? Ru1 C29 C30 C31 51.5(6) . . . . ? C28 C29 C30 C36 -178.0(7) . . . . ? C35 C29 C30 C36 3.5(11) . . . . ? Ru1 C29 C30 C36 -123.4(7) . . . . ? C28 C29 C30 Ru1 -54.6(6) . . . . ? C35 C29 C30 Ru1 127.0(7) . . . . ? O1 Ru1 C30 C29 -136.4(4) . . . . ? N3 Ru1 C30 C29 150.9(7) . . . . ? C31 Ru1 C30 C29 132.8(6) . . . . ? C28 Ru1 C30 C29 28.7(4) . . . . ? C32 Ru1 C30 C29 102.8(5) . . . . ? C33 Ru1 C30 C29 66.0(5) . . . . ? Cl1 Ru1 C30 C29 -54.2(4) . . . . ? O1 Ru1 C30 C31 90.7(4) . . . . ? N3 Ru1 C30 C31 18.1(10) . . . . ? C29 Ru1 C30 C31 -132.8(6) . . . . ? C28 Ru1 C30 C31 -104.1(5) . . . . ? C32 Ru1 C30 C31 -30.0(4) . . . . ? C33 Ru1 C30 C31 -66.8(4) . . . . ? Cl1 Ru1 C30 C31 173.0(4) . . . . ? O1 Ru1 C30 C36 -22.4(8) . . . . ? N3 Ru1 C30 C36 -95.0(11) . . . . ? C29 Ru1 C30 C36 114.1(10) . . . . ? C31 Ru1 C30 C36 -113.1(10) . . . . ? C28 Ru1 C30 C36 142.8(9) . . . . ? C32 Ru1 C30 C36 -143.1(9) . . . . ? C33 Ru1 C30 C36 -179.9(9) . . . . ? Cl1 Ru1 C30 C36 59.9(9) . . . . ? C29 C30 C31 C32 4.7(11) . . . . ? C36 C30 C31 C32 179.6(7) . . . . ? Ru1 C30 C31 C32 56.1(6) . . . . ? C29 C30 C31 C37 -176.7(7) . . . . ? C36 C30 C31 C37 -1.7(11) . . . . ? Ru1 C30 C31 C37 -125.3(7) . . . . ? C29 C30 C31 Ru1 -51.4(6) . . . . ? C36 C30 C31 Ru1 123.5(7) . . . . ? O1 Ru1 C31 C32 142.5(4) . . . . ? N3 Ru1 C31 C32 55.5(5) . . . . ? C29 Ru1 C31 C32 -102.1(5) . . . . ? C28 Ru1 C31 C32 -64.9(5) . . . . ? C30 Ru1 C31 C32 -130.7(6) . . . . ? C33 Ru1 C31 C32 -28.6(4) . . . . ? Cl1 Ru1 C31 C32 -144.1(4) . . . . ? O1 Ru1 C31 C30 -86.7(4) . . . . ? N3 Ru1 C31 C30 -173.8(4) . . . . ? C29 Ru1 C31 C30 28.6(4) . . . . ? C28 Ru1 C31 C30 65.8(5) . . . . ? C32 Ru1 C31 C30 130.7(6) . . . . ? C33 Ru1 C31 C30 102.1(5) . . . . ? Cl1 Ru1 C31 C30 -13.3(7) . . . . ? O1 Ru1 C31 C37 27.8(8) . . . . ? N3 Ru1 C31 C37 -59.2(9) . . . . ? C29 Ru1 C31 C37 143.2(9) . . . . ? C28 Ru1 C31 C37 -179.6(9) . . . . ? C32 Ru1 C31 C37 -114.7(10) . . . . ? C30 Ru1 C31 C37 114.6(10) . . . . ? C33 Ru1 C31 C37 -143.3(9) . . . . ? Cl1 Ru1 C31 C37 101.2(8) . . . . ? C30 C31 C32 C33 -1.8(11) . . . . ? C37 C31 C32 C33 179.6(7) . . . . ? Ru1 C31 C32 C33 54.4(6) . . . . ? C30 C31 C32 C38 177.8(7) . . . . ? C37 C31 C32 C38 -0.8(11) . . . . ? Ru1 C31 C32 C38 -126.0(7) . . . . ? C30 C31 C32 Ru1 -56.2(6) . . . . ? C37 C31 C32 Ru1 125.2(7) . . . . ? O1 Ru1 C32 C33 -175.4(4) . . . . ? N3 Ru1 C32 C33 89.9(5) . . . . ? C29 Ru1 C32 C33 -65.6(5) . . . . ? C31 Ru1 C32 C33 -132.7(7) . . . . ? C28 Ru1 C32 C33 -27.7(5) . . . . ? C30 Ru1 C32 C33 -102.4(5) . . . . ? Cl1 Ru1 C32 C33 -4.9(9) . . . . ? O1 Ru1 C32 C31 -42.7(5) . . . . ? N3 Ru1 C32 C31 -137.4(4) . . . . ? C29 Ru1 C32 C31 67.2(5) . . . . ? C28 Ru1 C32 C31 105.0(5) . . . . ? C30 Ru1 C32 C31 30.3(4) . . . . ? C33 Ru1 C32 C31 132.7(7) . . . . ? Cl1 Ru1 C32 C31 127.9(6) . . . . ? O1 Ru1 C32 C38 69.5(9) . . . . ? N3 Ru1 C32 C38 -25.2(9) . . . . ? C29 Ru1 C32 C38 179.4(9) . . . . ? C31 Ru1 C32 C38 112.2(10) . . . . ? C28 Ru1 C32 C38 -142.8(10) . . . . ? C30 Ru1 C32 C38 142.5(10) . . . . ? C33 Ru1 C32 C38 -115.0(11) . . . . ? Cl1 Ru1 C32 C38 -119.9(8) . . . . ? C31 C32 C33 C28 -2.9(11) . . . . ? C38 C32 C33 C28 177.5(7) . . . . ? Ru1 C32 C33 C28 50.5(6) . . . . ? C31 C32 C33 C39 172.8(7) . . . . ? C38 C32 C33 C39 -6.8(11) . . . . ? Ru1 C32 C33 C39 -133.8(7) . . . . ? C31 C32 C33 Ru1 -53.4(6) . . . . ? C38 C32 C33 Ru1 127.0(7) . . . . ? C29 C28 C33 C32 4.4(10) . . . . ? C34 C28 C33 C32 -173.3(7) . . . . ? Ru1 C28 C33 C32 -50.8(6) . . . . ? C29 C28 C33 C39 -171.2(7) . . . . ? C34 C28 C33 C39 11.1(11) . . . . ? Ru1 C28 C33 C39 133.6(7) . . . . ? C29 C28 C33 Ru1 55.2(6) . . . . ? C34 C28 C33 Ru1 -122.5(7) . . . . ? O1 Ru1 C33 C32 9.1(8) . . . . ? N3 Ru1 C33 C32 -96.7(5) . . . . ? C29 Ru1 C33 C32 103.7(5) . . . . ? C31 Ru1 C33 C32 29.1(5) . . . . ? C28 Ru1 C33 C32 134.9(7) . . . . ? C30 Ru1 C33 C32 66.9(5) . . . . ? Cl1 Ru1 C33 C32 177.9(4) . . . . ? O1 Ru1 C33 C28 -125.8(6) . . . . ? N3 Ru1 C33 C28 128.5(5) . . . . ? C29 Ru1 C33 C28 -31.1(5) . . . . ? C31 Ru1 C33 C28 -105.8(5) . . . . ? C32 Ru1 C33 C28 -134.9(7) . . . . ? C30 Ru1 C33 C28 -68.0(5) . . . . ? Cl1 Ru1 C33 C28 43.0(5) . . . . ? O1 Ru1 C33 C39 120.4(10) . . . . ? N3 Ru1 C33 C39 14.7(10) . . . . ? C29 Ru1 C33 C39 -144.9(11) . . . . ? C31 Ru1 C33 C39 140.4(11) . . . . ? C28 Ru1 C33 C39 -113.8(12) . . . . ? C32 Ru1 C33 C39 111.3(11) . . . . ? C30 Ru1 C33 C39 178.2(10) . . . . ? Cl1 Ru1 C33 C39 -70.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.732 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.142 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 604 59 ' ' 2 0.000 0.000 0.500 14 0 ' ' 3 0.333 0.667 0.667 604 59 ' ' 4 0.333 0.667 0.167 14 0 ' ' 5 0.667 0.333 0.333 604 59 ' ' 6 0.667 0.333 0.833 14 0 ' ' _platon_squeeze_details ? _iucr_refine_instructions_details ; TITL CC8 in R-3 CELL 0.71073 33.5170 33.5170 19.1570 90.000 90.000 120.000 ZERR 18.00 0.0047 0.0047 0.0038 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O CL RU UNIT 720 864 54 18 54 18 REM ------------------------------------------------------------------------- REM Data measured on the marmux REM Crystal colour: red; Crystal habit: prismatic REM ------------------------------------------------------------------------- L.S. 10 ACTA CONF BOND $H SIZE 0.32 0.22 0.19 WPDB -2 FMAP 2 PLAN 10 TEMP -133 WGHT 0.170200 FVAR 0.71496 RU1 6 0.396602 0.431394 0.865898 11.00000 0.05761 0.05458 = 0.05703 0.00365 0.00581 0.02585 CL1 5 0.473704 0.498627 0.876588 11.00000 0.06065 0.05438 = 0.06978 0.00280 0.00526 0.02213 O1 4 0.407444 0.442854 0.758873 11.00000 0.06185 0.07338 = 0.06435 0.00521 0.00342 0.03775 N1 3 0.446113 0.447449 0.654865 11.00000 0.06883 0.05949 = 0.05170 0.00213 -0.00040 0.03174 N2 3 0.477586 0.435398 0.628447 11.00000 0.06245 0.06352 = 0.05507 -0.00050 0.00503 0.02922 N3 3 0.435748 0.396032 0.864243 11.00000 0.06035 0.05329 = 0.05811 0.00226 0.00280 0.02730 C1 1 0.436228 0.434324 0.723654 11.00000 0.06384 0.05863 = 0.05073 0.00527 0.00608 0.02735 C2 1 0.436081 0.477108 0.614485 11.00000 0.06740 0.06700 = 0.05440 -0.00872 -0.01228 0.03386 C3 1 0.394740 0.477113 0.623589 11.00000 0.08653 0.07346 = 0.06041 0.00467 0.00178 0.04007 AFIX 43 H3 2 0.372319 0.456355 0.655620 11.00000 -1.20000 AFIX 0 C4 1 0.386420 0.508065 0.585031 11.00000 0.09266 0.09447 = 0.06853 -0.00409 -0.00378 0.05694 AFIX 43 H4 2 0.358849 0.509028 0.591966 11.00000 -1.20000 AFIX 0 C5 1 0.419416 0.537533 0.536132 11.00000 0.12484 0.07630 = 0.05311 -0.00050 -0.00794 0.05291 AFIX 43 H5 2 0.413705 0.557979 0.509255 11.00000 -1.20000 AFIX 0 C6 1 0.460462 0.536963 0.526803 11.00000 0.10483 0.08045 = 0.06430 0.00346 0.00249 0.05124 AFIX 43 H6 2 0.482599 0.556751 0.493615 11.00000 -1.20000 AFIX 0 C7 1 0.468389 0.507369 0.566312 11.00000 0.08169 0.06953 = 0.05307 0.00688 -0.00218 0.03313 AFIX 43 H7 2 0.496612 0.507490 0.560717 11.00000 -1.20000 AFIX 0 C8 1 0.487396 0.415692 0.680789 11.00000 0.05755 0.07360 = 0.05017 -0.00146 0.00292 0.02791 C9 1 0.521270 0.399147 0.666720 11.00000 0.06160 0.08032 = 0.06585 0.00090 0.01181 0.03689 AFIX 33 H9A 2 0.531608 0.405669 0.618079 11.00000 -1.50000 H9B 2 0.506230 0.365893 0.675124 11.00000 -1.50000 H9C 2 0.547866 0.415183 0.697865 11.00000 -1.50000 AFIX 0 C10 1 0.462288 0.414142 0.743891 11.00000 0.05604 0.06722 = 0.05598 0.00222 0.00627 0.03164 C11 1 0.462938 0.396312 0.811338 11.00000 0.05840 0.05616 = 0.05619 -0.00148 -0.00164 0.02677 C12 1 0.497598 0.381343 0.826513 11.00000 0.06676 0.05940 = 0.05815 0.00145 0.00237 0.03072 AFIX 23 H12A 2 0.501183 0.366133 0.784607 11.00000 -1.20000 H12B 2 0.485880 0.358482 0.864861 11.00000 -1.20000 AFIX 0 C13 1 0.544476 0.421530 0.847035 11.00000 0.06718 0.08645 = 0.07508 0.00245 0.00578 0.04102 AFIX 23 H13A 2 0.556271 0.443963 0.808122 11.00000 -1.20000 H13B 2 0.540501 0.437201 0.888021 11.00000 -1.20000 AFIX 0 C14 1 0.579959 0.407871 0.864464 11.00000 0.08188 0.13021 = 0.13277 -0.01470 -0.02251 0.06675 AFIX 23 H14A 2 0.609897 0.436252 0.872358 11.00000 -1.20000 H14B 2 0.583594 0.391952 0.823509 11.00000 -1.20000 AFIX 0 C15 1 0.569144 0.376885 0.927761 11.00000 0.14572 0.12778 = 0.18186 -0.02210 -0.05731 0.09408 AFIX 23 H15A 2 0.561670 0.391222 0.967035 11.00000 -1.20000 H15B 2 0.540992 0.347241 0.917310 11.00000 -1.20000 AFIX 0 C16 1 0.605533 0.366441 0.952331 11.00000 0.19230 0.19716 = 0.30183 -0.06229 -0.14303 0.14023 AFIX 23 H16A 2 0.633174 0.395249 0.967465 11.00000 -1.20000 H16B 2 0.614566 0.353093 0.913517 11.00000 -1.20000 AFIX 0 C17 1 0.585959 0.330451 1.016675 11.00000 0.27770 0.22767 = 0.35956 0.06093 -0.15632 0.12941 AFIX 33 H17A 2 0.553037 0.319433 1.022831 11.00000 -1.50000 H17B 2 0.602549 0.345838 1.059467 11.00000 -1.50000 H17C 2 0.590425 0.304265 1.006733 11.00000 -1.50000 AFIX 0 C18 1 0.438197 0.376743 0.930408 11.00000 0.06288 0.05246 = 0.05809 0.00408 0.01062 0.02843 C19 1 0.414912 0.327292 0.937502 11.00000 0.06456 0.04902 = 0.05583 0.00382 0.01107 0.02280 C20 1 0.390264 0.296623 0.882153 11.00000 0.08010 0.06239 = 0.05079 0.00345 0.00712 0.03450 AFIX 43 H20 2 0.388845 0.308647 0.837901 11.00000 -1.20000 AFIX 0 C21 1 0.368585 0.250084 0.891726 11.00000 0.08774 0.05789 = 0.06773 -0.00675 0.00382 0.03263 AFIX 43 H21 2 0.352536 0.230229 0.853786 11.00000 -1.20000 AFIX 0 C22 1 0.369495 0.230830 0.956740 11.00000 0.08650 0.04682 = 0.07184 0.00662 0.00616 0.02492 AFIX 43 H22 2 0.353717 0.198340 0.962659 11.00000 -1.20000 AFIX 0 C23 1 0.393395 0.259411 1.011610 11.00000 0.09388 0.06727 = 0.06743 0.02037 0.01354 0.04384 AFIX 43 H23 2 0.394242 0.246252 1.055116 11.00000 -1.20000 AFIX 0 C24 1 0.417051 0.308628 1.004551 11.00000 0.06985 0.05505 = 0.06515 0.00519 0.00514 0.02762 C25 1 0.442211 0.338628 1.060018 11.00000 0.08101 0.07333 = 0.06062 0.00759 0.00359 0.04305 AFIX 43 H25 2 0.443113 0.326582 1.104507 11.00000 -1.20000 AFIX 0 C26 1 0.465588 0.385928 1.048635 11.00000 0.07086 0.06858 = 0.05685 -0.00460 -0.00030 0.02819 AFIX 43 H26 2 0.483965 0.405898 1.085077 11.00000 -1.20000 AFIX 0 C27 1 0.462876 0.404734 0.985896 11.00000 0.06405 0.05285 = 0.05639 -0.00313 -0.00151 0.02797 AFIX 43 H27 2 0.478124 0.437264 0.980738 11.00000 -1.20000 AFIX 0 C28 1 0.374565 0.445856 0.967468 11.00000 0.06678 0.08097 = 0.06352 0.00181 0.01690 0.03625 C29 1 0.367770 0.471331 0.912542 11.00000 0.06626 0.06347 = 0.06688 0.00411 0.01261 0.03319 C30 1 0.341308 0.449766 0.851986 11.00000 0.06329 0.08131 = 0.07517 0.01287 0.00949 0.04027 C31 1 0.322305 0.400449 0.843657 11.00000 0.05714 0.07272 = 0.07426 -0.00800 0.00476 0.02696 C32 1 0.327623 0.374341 0.898490 11.00000 0.06075 0.05430 = 0.09256 0.00583 0.02739 0.02468 C33 1 0.352539 0.396585 0.960373 11.00000 0.07261 0.07209 = 0.07121 0.01175 0.02875 0.03517 C34 1 0.405506 0.471630 1.028270 11.00000 0.10269 0.12670 = 0.05695 -0.02779 -0.00477 0.06384 AFIX 33 H34A 2 0.387653 0.476903 1.063880 11.00000 -1.50000 H34B 2 0.430762 0.501302 1.012041 11.00000 -1.50000 H34C 2 0.418173 0.453405 1.048329 11.00000 -1.50000 AFIX 0 C35 1 0.389046 0.523950 0.920531 11.00000 0.09561 0.05611 = 0.12860 -0.00604 0.01824 0.03277 AFIX 33 H35A 2 0.422608 0.538958 0.915903 11.00000 -1.50000 H35B 2 0.381251 0.530849 0.966581 11.00000 -1.50000 H35C 2 0.376782 0.535436 0.884178 11.00000 -1.50000 AFIX 0 C36 1 0.336243 0.477481 0.794920 11.00000 0.08557 0.10349 = 0.08951 0.01577 -0.00283 0.06158 AFIX 33 H36A 2 0.336894 0.504685 0.815031 11.00000 -1.50000 H36B 2 0.306869 0.458626 0.770776 11.00000 -1.50000 H36C 2 0.361652 0.487259 0.761626 11.00000 -1.50000 AFIX 0 C37 1 0.296340 0.376870 0.778618 11.00000 0.05244 0.10816 = 0.08623 -0.02222 -0.00896 0.03198 AFIX 33 H37A 2 0.287382 0.344217 0.780367 11.00000 -1.50000 H37B 2 0.315988 0.391295 0.737802 11.00000 -1.50000 H37C 2 0.268675 0.379680 0.775159 11.00000 -1.50000 AFIX 0 C38 1 0.305637 0.321342 0.890104 11.00000 0.07277 0.06065 = 0.17511 0.00009 0.03464 0.02356 AFIX 33 H38A 2 0.272455 0.306433 0.899080 11.00000 -1.50000 H38B 2 0.319770 0.309927 0.923462 11.00000 -1.50000 H38C 2 0.310822 0.314247 0.842480 11.00000 -1.50000 AFIX 0 C39 1 0.352438 0.367097 1.020262 11.00000 0.11297 0.11206 = 0.07782 0.03691 0.04020 0.07432 AFIX 33 H39A 2 0.381609 0.383627 1.045792 11.00000 -1.50000 H39B 2 0.348808 0.338165 1.001937 11.00000 -1.50000 H39C 2 0.326831 0.360402 1.051843 11.00000 -1.50000 AFIX 0 CL2 5 0.252767 0.194362 0.924657 11.00000 0.12083 0.14621 = 0.16746 -0.03333 -0.00050 0.07443 CL3 5 0.171966 0.103543 0.918161 11.00000 0.14274 0.12612 = 0.36074 -0.03698 0.03902 0.07392 C40 1 0.232507 0.135561 0.929117 11.00000 0.11566 0.12204 = 0.11700 0.01657 0.00360 0.07752 AFIX 23 H40A 2 0.240757 0.128042 0.974936 11.00000 -1.20000 H40B 2 0.247445 0.126825 0.892314 11.00000 -1.20000 HKLF 4 REM CC8 in R-3 REM R1 = 0.0966 for 5277 Fo > 4sig(Fo) and 0.1263 for all 7524 data REM 433 parameters refined using 0 restraints END WGHT 0.1701 0.0000 REM Highest difference peak 0.732, deepest hole -1.344, 1-sigma level 0.142 Q1 1 0.3973 0.2422 1.1265 11.00000 0.05 0.54 Q2 1 0.3301 0.2172 0.9397 11.00000 0.05 0.47 Q3 1 0.4220 0.2908 0.9319 11.00000 0.05 0.46 Q4 1 0.3964 0.4293 0.9436 11.00000 0.05 0.46 Q5 1 0.3942 0.3347 1.0008 11.00000 0.05 0.45 Q6 1 0.4351 0.4667 0.8219 11.00000 0.05 0.44 Q7 1 0.4940 0.4359 1.0604 11.00000 0.05 0.43 Q8 1 0.4955 0.3280 1.0846 11.00000 0.05 0.42 Q9 1 0.4061 0.2873 0.9981 11.00000 0.05 0.42 Q10 1 0.4242 0.4778 0.9063 11.00000 0.05 0.41 ;