# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jianzhuang Jiang' _publ_contact_author_email JZJIANG@SDU.EDU.CN _publ_section_title ; Heterobimetallic Porphyrin-basd Single-Chain Magnet Constructed from Manganese(III)-Porphyrin and trans-Dicyanobis(acetylacetonato)ruthenate(III) Containing Co-crystallized bulk anions and cations ; loop_ _publ_author_name 'Jianzhuang Jiang' 'Yuting Chen' 'Zhong-Hai Ni' 'Hailong Wang' 'Wolfgang Wernsdorfer' 'Daopeng Zhang' 'Li-Fang Zhang' # Attachment '1-3.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 758953' #TrackingRef '1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H38 N2 O5 P Ru' _chemical_formula_weight 722.73 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.969(2) _cell_length_b 12.312(2) _cell_length_c 14.000(2) _cell_angle_alpha 92.186(3) _cell_angle_beta 112.599(3) _cell_angle_gamma 111.187(3) _cell_volume 1738.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2073 _cell_measurement_theta_min 2.108 _cell_measurement_theta_max 22.231 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9137 _exptl_absorpt_correction_T_max 0.9529 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5671 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5331 _reflns_number_gt 3552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1997)' _computing_publication_material XP _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^)+(0.1117P)^2^+9.8055P] 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 5331 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.2280 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.5000 0.0000 0.5000 0.0531(5) Uani 1 2 d S . . Ru2 Ru 0.0000 0.5000 0.0000 0.0760(6) Uani 1 2 d S . . P1 P 0.9956(6) 0.1746(6) 0.3382(5) 0.173(3) Uani 1 1 d . . . O1 O 0.5361(7) 0.1697(6) 0.4885(6) 0.0639(19) Uani 1 1 d . . . O2 O 0.5564(6) 0.0413(7) 0.6568(5) 0.0643(19) Uani 1 1 d . . . O3 O 0.0401(9) 0.6701(7) -0.0092(6) 0.085(2) Uani 1 1 d . . . O4 O 0.0570(9) 0.5371(7) 0.1562(6) 0.088(2) Uani 1 1 d . . . O5 O 0.488(2) 0.5276(16) 0.9100(17) 0.302(12) Uani 1 1 d . . . H5A H 0.4775 0.4484 0.9209 0.363 Uiso 1 1 d R . . H5B H 0.5742 0.5827 0.9627 0.363 Uiso 1 1 d R . . N1 N 0.7936(10) 0.0395(8) 0.5339(8) 0.074(3) Uani 1 1 d . . . N2 N -0.2942(16) 0.4659(14) -0.0381(13) 0.137(5) Uani 1 1 d . . . C1 C 0.6892(11) 0.0265(9) 0.5227(7) 0.056(3) Uani 1 1 d . . . C2 C -0.1903(19) 0.4761(12) -0.0256(11) 0.096(4) Uani 1 1 d . . . C3 C 0.5489(15) 0.3617(11) 0.5221(12) 0.115(5) Uani 1 1 d . . . H3A H 0.5667 0.3651 0.4607 0.172 Uiso 1 1 calc R . . H3B H 0.6175 0.4275 0.5781 0.172 Uiso 1 1 calc R . . H3C H 0.4650 0.3658 0.5052 0.172 Uiso 1 1 calc R . . C4 C 0.5449(10) 0.2455(11) 0.5573(11) 0.073(3) Uani 1 1 d . . . C5 C 0.5534(12) 0.2319(11) 0.6566(11) 0.084(4) Uani 1 1 d . . . H5 H 0.5528 0.2935 0.6966 0.101 Uiso 1 1 calc R . . C6 C 0.5628(10) 0.1370(11) 0.7033(9) 0.070(3) Uani 1 1 d . . . C7 C 0.5804(14) 0.1363(13) 0.8141(10) 0.107(5) Uani 1 1 d . . . H7A H 0.6068 0.0736 0.8377 0.161 Uiso 1 1 calc R . . H7B H 0.4983 0.1236 0.8178 0.161 Uiso 1 1 calc R . . H7C H 0.6475 0.2114 0.8586 0.161 Uiso 1 1 calc R . . C8 C 0.0728(15) 0.8680(10) 0.0334(11) 0.105(5) Uani 1 1 d . . . H8A H 0.1159 0.8837 -0.0130 0.158 Uiso 1 1 calc R . . H8B H 0.1221 0.9306 0.0954 0.158 Uiso 1 1 calc R . . H8C H -0.0153 0.8642 -0.0023 0.158 Uiso 1 1 calc R . . C9 C 0.0661(12) 0.7506(10) 0.0652(11) 0.076(3) Uani 1 1 d . . . C10 C 0.0867(13) 0.7367(11) 0.1662(10) 0.088(4) Uani 1 1 d . . . H10 H 0.1078 0.8040 0.2134 0.105 Uiso 1 1 calc R . . C11 C 0.0800(11) 0.6352(11) 0.2067(9) 0.071(3) Uani 1 1 d . . . C12 C 0.1034(13) 0.6383(11) 0.3206(9) 0.090(4) Uani 1 1 d . . . H12A H 0.0258 0.6351 0.3280 0.134 Uiso 1 1 calc R . . H12B H 0.1775 0.7107 0.3638 0.134 Uiso 1 1 calc R . . H12C H 0.1217 0.5713 0.3425 0.134 Uiso 1 1 calc R . . C13 C 1.1102(14) 0.2651(14) 0.4927(11) 0.098(4) Uani 1 1 d . . . C14 C 1.0924(15) 0.3702(17) 0.5120(11) 0.107(5) Uani 1 1 d . . . H14 H 1.0209 0.3813 0.4628 0.129 Uiso 1 1 calc R . . C15 C 1.1732(19) 0.4501(16) 0.5961(17) 0.128(6) Uani 1 1 d . . . H15 H 1.1615 0.5200 0.6041 0.153 Uiso 1 1 calc R . . C16 C 1.273(2) 0.4372(18) 0.6723(16) 0.140(6) Uani 1 1 d . . . H16 H 1.3295 0.4960 0.7333 0.168 Uiso 1 1 calc R . . C17 C 1.2911(17) 0.3262(18) 0.6570(14) 0.138(6) Uani 1 1 d . . . H17 H 1.3513 0.3067 0.7109 0.166 Uiso 1 1 calc R . . C18 C 1.2134(16) 0.2531(13) 0.5578(12) 0.108(5) Uani 1 1 d . . . H18 H 1.2362 0.1942 0.5377 0.130 Uiso 1 1 calc R . . C19 C 0.8621(14) 0.2212(13) 0.2833(11) 0.099(5) Uani 1 1 d . . . C20 C 0.7745(15) 0.1983(14) 0.3294(13) 0.117(6) Uani 1 1 d . . . H20 H 0.7926 0.1686 0.3912 0.141 Uiso 1 1 calc R . . C21 C 0.6627(13) 0.2183(12) 0.2864(12) 0.093(4) Uani 1 1 d . . . H21 H 0.6050 0.2027 0.3185 0.112 Uiso 1 1 calc R . . C22 C 0.6360(12) 0.2616(11) 0.1956(11) 0.085(4) Uani 1 1 d . . . H22 H 0.5589 0.2745 0.1658 0.102 Uiso 1 1 calc R . . C23 C 0.7196(12) 0.2865(12) 0.1475(10) 0.085(4) Uani 1 1 d . . . H23 H 0.7022 0.3192 0.0875 0.102 Uiso 1 1 calc R . . C24 C 0.8316(13) 0.2617(11) 0.1901(10) 0.084(4) Uani 1 1 d . . . H24 H 0.8862 0.2727 0.1555 0.101 Uiso 1 1 calc R . . C25 C 1.1109(12) 0.2158(11) 0.2820(9) 0.077(3) Uani 1 1 d . . . C26 C 1.1518(13) 0.3241(11) 0.2578(9) 0.084(4) Uani 1 1 d . . . H26 H 1.1107 0.3742 0.2620 0.100 Uiso 1 1 calc R . . C27 C 1.2525(13) 0.3607(13) 0.2273(10) 0.091(4) Uani 1 1 d . . . H27 H 1.2796 0.4352 0.2103 0.109 Uiso 1 1 calc R . . C28 C 1.3129(13) 0.2884(16) 0.2220(10) 0.095(4) Uani 1 1 d . . . H28 H 1.3807 0.3130 0.2001 0.115 Uiso 1 1 calc R . . C29 C 1.2755(12) 0.1794(13) 0.2484(10) 0.089(4) Uani 1 1 d . . . H29 H 1.3191 0.1309 0.2463 0.107 Uiso 1 1 calc R . . C30 C 1.1737(12) 0.1423(11) 0.2779(11) 0.087(4) Uani 1 1 d . . . H30 H 1.1467 0.0679 0.2952 0.105 Uiso 1 1 calc R . . C31 C 0.9532(16) 0.0479(15) 0.3649(13) 0.125(5) Uani 1 1 d . . . H31A H 0.9011 0.0391 0.4051 0.150 Uiso 1 1 calc R . . H31B H 1.0294 0.0307 0.4038 0.150 Uiso 1 1 calc R . . C32 C 0.8660(16) -0.0346(16) 0.2488(14) 0.119(5) Uani 1 1 d . . . C33 C 0.8924(17) -0.1292(18) 0.2352(15) 0.138(6) Uani 1 1 d . . . H33 H 0.9671 -0.1336 0.2867 0.165 Uiso 1 1 calc R . . C34 C 0.8100(19) -0.2236(17) 0.1442(16) 0.144(7) Uani 1 1 d . . . H34 H 0.8288 -0.2899 0.1386 0.173 Uiso 1 1 calc R . . C35 C 0.7047(19) -0.2160(19) 0.0666(16) 0.140(6) Uani 1 1 d . . . H35 H 0.6533 -0.2741 0.0048 0.168 Uiso 1 1 calc R . . C36 C 0.6764(19) -0.124(2) 0.0804(18) 0.149(7) Uani 1 1 d . . . H36 H 0.6053 -0.1152 0.0278 0.178 Uiso 1 1 calc R . . C37 C 0.751(2) -0.0428(18) 0.1707(17) 0.146(7) Uani 1 1 d . . . H37 H 0.7210 0.0144 0.1812 0.175 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 0.0589(8) 0.0504(8) 0.0579(8) 0.0180(6) 0.0297(6) 0.0250(6) Ru2 0.1293(13) 0.0502(9) 0.0586(9) 0.0193(6) 0.0446(8) 0.0415(8) P1 0.214(5) 0.250(6) 0.285(7) 0.233(6) 0.219(6) 0.203(5) O1 0.069(5) 0.049(5) 0.075(5) 0.020(4) 0.032(4) 0.023(4) O2 0.067(4) 0.068(5) 0.055(5) 0.016(4) 0.027(4) 0.023(4) O3 0.135(7) 0.059(5) 0.072(5) 0.022(4) 0.048(5) 0.047(5) O4 0.146(8) 0.070(6) 0.071(6) 0.029(5) 0.057(5) 0.057(5) O5 0.24(2) 0.167(16) 0.37(3) 0.060(17) 0.046(19) 0.027(14) N1 0.070(6) 0.084(7) 0.096(7) 0.035(6) 0.048(6) 0.045(6) N2 0.147(13) 0.128(12) 0.158(13) 0.078(10) 0.069(12) 0.070(11) C1 0.063(7) 0.054(7) 0.055(7) 0.018(5) 0.026(6) 0.028(6) C2 0.156(15) 0.074(9) 0.083(10) 0.042(8) 0.063(11) 0.059(11) C3 0.141(13) 0.067(9) 0.125(12) 0.023(8) 0.033(10) 0.055(9) C4 0.057(7) 0.058(8) 0.079(9) 0.006(7) 0.009(6) 0.019(6) C5 0.094(9) 0.060(8) 0.083(10) -0.014(7) 0.023(7) 0.033(7) C6 0.067(7) 0.068(8) 0.067(8) -0.007(7) 0.033(6) 0.014(6) C7 0.115(11) 0.116(12) 0.079(10) 0.003(8) 0.051(8) 0.026(9) C8 0.155(13) 0.050(8) 0.111(11) 0.017(7) 0.054(10) 0.044(8) C9 0.104(9) 0.053(8) 0.086(10) 0.016(7) 0.049(8) 0.039(7) C10 0.133(11) 0.072(9) 0.083(10) 0.015(7) 0.059(8) 0.055(8) C11 0.085(8) 0.071(9) 0.058(8) 0.010(7) 0.028(6) 0.036(7) C12 0.116(10) 0.093(10) 0.062(8) 0.007(7) 0.042(7) 0.041(8) C13 0.095(10) 0.131(13) 0.088(11) 0.003(9) 0.052(9) 0.056(10) C14 0.105(11) 0.166(16) 0.061(9) 0.004(10) 0.021(8) 0.083(12) C15 0.120(14) 0.117(14) 0.128(16) -0.010(12) 0.033(12) 0.054(12) C16 0.123(14) 0.138(17) 0.123(15) -0.027(12) 0.027(12) 0.048(13) C17 0.119(13) 0.144(16) 0.116(15) -0.014(12) 0.018(11) 0.056(12) C18 0.119(12) 0.096(11) 0.092(11) -0.018(9) 0.012(9) 0.064(10) C19 0.135(11) 0.131(12) 0.129(12) 0.095(10) 0.105(10) 0.103(10) C20 0.150(13) 0.162(14) 0.164(14) 0.126(12) 0.128(12) 0.120(12) C21 0.098(10) 0.096(10) 0.140(13) 0.054(9) 0.082(9) 0.062(8) C22 0.077(8) 0.089(9) 0.099(10) 0.021(8) 0.038(8) 0.043(7) C23 0.081(8) 0.110(10) 0.078(8) 0.041(8) 0.039(7) 0.046(8) C24 0.100(9) 0.092(9) 0.104(10) 0.046(8) 0.072(8) 0.053(8) C25 0.096(9) 0.100(10) 0.095(9) 0.056(8) 0.069(8) 0.069(8) C26 0.108(10) 0.087(10) 0.086(9) 0.045(7) 0.051(8) 0.059(8) C27 0.079(9) 0.103(11) 0.083(9) 0.046(8) 0.034(8) 0.027(8) C28 0.067(8) 0.134(14) 0.088(10) 0.028(9) 0.048(7) 0.028(9) C29 0.083(9) 0.104(11) 0.096(10) 0.008(8) 0.046(8) 0.048(8) C30 0.086(9) 0.088(9) 0.128(11) 0.040(8) 0.073(9) 0.048(8) C31 0.105(11) 0.135(14) 0.128(14) 0.017(11) 0.044(10) 0.050(10) C32 0.097(12) 0.125(14) 0.134(15) -0.006(11) 0.038(11) 0.057(11) C33 0.108(13) 0.133(15) 0.140(16) -0.004(13) 0.025(11) 0.049(12) C34 0.117(14) 0.132(16) 0.150(17) -0.012(13) 0.024(13) 0.054(12) C35 0.112(14) 0.135(17) 0.141(17) -0.016(13) 0.028(13) 0.048(12) C36 0.118(15) 0.137(17) 0.145(18) -0.003(14) 0.018(13) 0.046(14) C37 0.116(15) 0.132(16) 0.147(17) -0.001(14) 0.022(13) 0.045(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.002(7) . ? Ru1 O1 2.002(7) 2_656 ? Ru1 O2 2.015(7) . ? Ru1 O2 2.015(7) 2_656 ? Ru1 C1 2.060(11) 2_656 ? Ru1 C1 2.060(11) . ? Ru2 O3 1.993(7) . ? Ru2 O3 1.993(7) 2_565 ? Ru2 O4 2.002(8) . ? Ru2 O4 2.002(8) 2_565 ? Ru2 C2 2.069(19) . ? Ru2 C2 2.069(19) 2_565 ? P1 C31 1.566(17) . ? P1 C25 1.773(11) . ? P1 C19 1.795(12) . ? P1 C13 2.057(15) . ? O1 C4 1.262(14) . ? O2 C6 1.287(13) . ? O3 C9 1.271(13) . ? O4 C11 1.257(13) . ? O5 H5A 0.9642 . ? O5 H5A 0.9642 . ? O5 H5B 0.9726 . ? N1 C1 1.146(12) . ? N2 C2 1.146(18) . ? C3 C4 1.522(16) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.374(17) . ? C5 C6 1.379(16) . ? C5 H5 0.9300 . ? C6 C7 1.484(16) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.513(15) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.366(16) . ? C10 C11 1.381(16) . ? C10 H10 0.9300 . ? C11 C12 1.506(15) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.287(18) . ? C13 C14 1.418(19) . ? C14 C15 1.279(19) . ? C14 H14 0.9300 . ? C15 C16 1.33(2) . ? C15 H15 0.9300 . ? C16 C17 1.48(2) . ? C16 H16 0.9300 . ? C17 C18 1.38(2) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.378(16) . ? C19 C20 1.385(16) . ? C20 C21 1.358(17) . ? C20 H20 0.9300 . ? C21 C22 1.366(17) . ? C21 H21 0.9300 . ? C22 C23 1.365(16) . ? C22 H22 0.9300 . ? C23 C24 1.392(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.349(15) . ? C25 C30 1.380(15) . ? C26 C27 1.363(17) . ? C26 H26 0.9300 . ? C27 C28 1.350(18) . ? C27 H27 0.9300 . ? C28 C29 1.367(18) . ? C28 H28 0.9300 . ? C29 C30 1.365(16) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.60(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.34(2) . ? C32 C37 1.35(2) . ? C33 C34 1.43(2) . ? C33 H33 0.9300 . ? C34 C35 1.35(2) . ? C34 H34 0.9300 . ? C35 C36 1.33(2) . ? C35 H35 0.9300 . ? C36 C37 1.33(2) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? 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 O1 180.000(1) . 2_656 ? O1 Ru1 O2 91.2(3) . . ? O1 Ru1 O2 88.8(3) 2_656 . ? O1 Ru1 O2 88.8(3) . 2_656 ? O1 Ru1 O2 91.2(3) 2_656 2_656 ? O2 Ru1 O2 180.000(1) . 2_656 ? O1 Ru1 C1 88.8(3) . 2_656 ? O1 Ru1 C1 91.2(3) 2_656 2_656 ? O2 Ru1 C1 88.2(3) . 2_656 ? O2 Ru1 C1 91.8(3) 2_656 2_656 ? O1 Ru1 C1 91.2(3) . . ? O1 Ru1 C1 88.8(3) 2_656 . ? O2 Ru1 C1 91.8(3) . . ? O2 Ru1 C1 88.2(3) 2_656 . ? C1 Ru1 C1 180.0(6) 2_656 . ? O3 Ru2 O3 180.0 . 2_565 ? O3 Ru2 O4 91.9(3) . . ? O3 Ru2 O4 88.1(3) 2_565 . ? O3 Ru2 O4 88.1(3) . 2_565 ? O3 Ru2 O4 91.9(3) 2_565 2_565 ? O4 Ru2 O4 180.0(5) . 2_565 ? O3 Ru2 C2 88.7(4) . . ? O3 Ru2 C2 91.3(4) 2_565 . ? O4 Ru2 C2 89.8(5) . . ? O4 Ru2 C2 90.2(5) 2_565 . ? O3 Ru2 C2 91.3(4) . 2_565 ? O3 Ru2 C2 88.7(4) 2_565 2_565 ? O4 Ru2 C2 90.2(5) . 2_565 ? O4 Ru2 C2 89.8(5) 2_565 2_565 ? C2 Ru2 C2 180.0(8) . 2_565 ? C31 P1 C25 118.4(8) . . ? C31 P1 C19 114.0(8) . . ? C25 P1 C19 115.0(5) . . ? C31 P1 C13 95.5(8) . . ? C25 P1 C13 102.5(7) . . ? C19 P1 C13 108.0(7) . . ? C4 O1 Ru1 123.4(7) . . ? C6 O2 Ru1 123.6(7) . . ? C9 O3 Ru2 124.3(7) . . ? C11 O4 Ru2 124.2(7) . . ? H5A O5 H5A 0.0 . . ? H5A O5 H5B 107.5 . . ? H5A O5 H5B 107.5 . . ? N1 C1 Ru1 178.8(10) . . ? N2 C2 Ru2 178.1(17) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C4 C5 126.4(11) . . ? O1 C4 C3 113.3(12) . . ? C5 C4 C3 120.3(13) . . ? C4 C5 C6 127.2(11) . . ? C4 C5 H5 116.4 . . ? C6 C5 H5 116.4 . . ? O2 C6 C5 124.5(11) . . ? O2 C6 C7 113.4(11) . . ? C5 C6 C7 122.1(12) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C10 125.1(10) . . ? O3 C9 C8 114.0(11) . . ? C10 C9 C8 120.9(11) . . ? C9 C10 C11 128.0(11) . . ? C9 C10 H10 116.0 . . ? C11 C10 H10 116.0 . . ? O4 C11 C10 125.2(11) . . ? O4 C11 C12 115.2(10) . . ? C10 C11 C12 119.5(11) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.3(14) . . ? C18 C13 P1 125.7(11) . . ? C14 C13 P1 112.1(11) . . ? C15 C14 C13 121.0(14) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 122.7(17) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C17 117.7(16) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C18 C17 C16 115.9(16) . . ? C18 C17 H17 122.0 . . ? C16 C17 H17 122.0 . . ? C13 C18 C17 121.2(14) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C24 C19 C20 118.5(11) . . ? C24 C19 P1 123.7(9) . . ? C20 C19 P1 117.2(9) . . ? C21 C20 C19 121.4(12) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.3(11) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 121.6(12) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 118.7(11) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C19 C24 C23 120.5(10) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C30 119.7(10) . . ? C26 C25 P1 121.1(9) . . ? C30 C25 P1 118.5(9) . . ? C25 C26 C27 120.7(12) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 119.7(12) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.7(11) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 119.5(12) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C25 119.7(12) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? P1 C31 C32 101.1(12) . . ? P1 C31 H31A 111.6 . . ? C32 C31 H31A 111.6 . . ? P1 C31 H31B 111.6 . . ? C32 C31 H31B 111.6 . . ? H31A C31 H31B 109.4 . . ? C33 C32 C37 112.5(17) . . ? C33 C32 C31 114.3(16) . . ? C37 C32 C31 131.2(16) . . ? C32 C33 C34 122.3(17) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C35 C34 C33 119.6(18) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C36 C35 C34 118.4(19) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C37 119(2) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C36 C37 C32 127(2) . . ? C36 C37 H37 116.3 . . ? C32 C37 H37 116.3 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.233 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.095 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 758954' #TrackingRef '1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H94 F12 Mn N6 O6 P4 Ru' _chemical_formula_weight 2079.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.546(3) _cell_length_b 12.287(3) _cell_length_c 20.953(6) _cell_angle_alpha 86.763(5) _cell_angle_beta 80.229(5) _cell_angle_gamma 71.551(5) _cell_volume 2538.1(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1616 _cell_measurement_theta_min 2.249 _cell_measurement_theta_max 24.123 _exptl_crystal_description block _exptl_crystal_colour purple-black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 1.361 _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1069 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9404 _exptl_absorpt_correction_T_max 0.9558 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12618 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.1326 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8856 _reflns_number_gt 4573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0650P)^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 8856 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1750 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.0000 0.0000 0.0462(2) Uani 1 2 d S . . Mn1 Mn 1.0000 0.0000 0.0000 0.0448(3) Uani 1 2 d S . . P1 P 0.3811(3) 0.2231(2) 0.35439(11) 0.0989(8) Uani 1 1 d . . . P2 P 0.8027(2) 0.85677(16) 0.37813(9) 0.0783(6) Uani 1 1 d . . . O1 O 0.4516(4) 0.1658(3) 0.0224(2) 0.0609(11) Uani 1 1 d . . . O2 O 0.4482(3) -0.0386(3) 0.09146(19) 0.0588(11) Uani 1 1 d . . . O3 O 0.2740(6) 0.3405(5) 0.9467(3) 0.130(2) Uani 1 1 d . . . H3 H 0.3309 0.2889 0.9623 0.194 Uiso 1 1 calc R . . N1 N 0.7984(4) -0.0311(4) 0.0270(2) 0.0521(12) Uani 1 1 d . . . N2 N 1.0359(4) -0.0122(4) 0.0913(2) 0.0455(11) Uani 1 1 d . . . N3 N 0.9036(4) 0.1693(4) 0.0133(2) 0.0478(12) Uani 1 1 d . . . F1 F 0.5127(6) 0.1452(6) 0.3196(3) 0.196(3) Uani 1 1 d . . . F2 F 0.4270(11) 0.3148(9) 0.3716(6) 0.311(6) Uani 1 1 d . . . F3 F 0.2384(7) 0.2901(6) 0.3910(3) 0.209(3) Uani 1 1 d . . . F4 F 0.4056(11) 0.1585(9) 0.4160(3) 0.322(7) Uani 1 1 d . . . F5 F 0.3166(9) 0.1388(8) 0.3350(5) 0.279(5) Uani 1 1 d . . . F6 F 0.3508(9) 0.2861(7) 0.2936(3) 0.240(4) Uani 1 1 d . . . C1 C 0.6909(5) -0.0222(4) 0.0180(3) 0.0445(14) Uani 1 1 d . . . C2 C 1.1098(5) -0.1092(5) 0.1207(3) 0.0487(14) Uani 1 1 d . . . C3 C 1.1693(5) -0.2173(5) 0.0932(3) 0.0551(16) Uani 1 1 d . . . C4 C 1.2519(6) -0.3097(5) 0.1328(3) 0.0570(16) Uani 1 1 d . . . C5 C 1.1965(7) -0.3831(6) 0.1705(3) 0.082(2) Uani 1 1 d . . . H5 H 1.1062 -0.3774 0.1712 0.098 Uiso 1 1 calc R . . C6 C 1.2752(9) -0.4658(6) 0.2074(4) 0.088(2) Uani 1 1 d . . . H6 H 1.2376 -0.5162 0.2325 0.106 Uiso 1 1 calc R . . C7 C 1.4051(9) -0.4740(7) 0.2074(4) 0.090(2) Uani 1 1 d . . . H7 H 1.4565 -0.5293 0.2330 0.108 Uiso 1 1 calc R . . C8 C 1.4617(8) -0.4022(7) 0.1705(4) 0.093(2) Uani 1 1 d . . . H8 H 1.5520 -0.4087 0.1703 0.112 Uiso 1 1 calc R . . C9 C 1.3849(6) -0.3192(6) 0.1329(4) 0.083(2) Uani 1 1 d . . . H9 H 1.4237 -0.2697 0.1077 0.099 Uiso 1 1 calc R . . C10 C 1.1194(5) -0.0816(5) 0.1842(3) 0.0579(16) Uani 1 1 d . . . H10 H 1.1643 -0.1320 0.2138 0.069 Uiso 1 1 calc R . . C11 C 1.0519(6) 0.0306(5) 0.1937(3) 0.0607(16) Uani 1 1 d . . . H11 H 1.0396 0.0718 0.2313 0.073 Uiso 1 1 calc R . . C12 C 1.0031(5) 0.0740(5) 0.1356(3) 0.0478(14) Uani 1 1 d . . . C13 C 0.9310(6) 0.1889(5) 0.1256(3) 0.0547(15) Uani 1 1 d . . . C14 C 0.8998(7) 0.2696(5) 0.1814(3) 0.0667(18) Uani 1 1 d . . . C15 C 1.0036(10) 0.3073(8) 0.1962(4) 0.128(4) Uani 1 1 d . . . H15 H 1.0894 0.2853 0.1714 0.154 Uiso 1 1 calc R . . C16 C 0.9734(14) 0.3793(10) 0.2498(6) 0.156(5) Uani 1 1 d . . . H16 H 1.0404 0.4051 0.2612 0.187 Uiso 1 1 calc R . . C17 C 0.8479(15) 0.4118(8) 0.2852(6) 0.137(4) Uani 1 1 d . . . H17 H 0.8288 0.4634 0.3190 0.164 Uiso 1 1 calc R . . C18 C 0.7492(11) 0.3713(9) 0.2727(5) 0.131(4) Uani 1 1 d . . . H18 H 0.6652 0.3898 0.2992 0.157 Uiso 1 1 calc R . . C19 C 0.7776(8) 0.3012(7) 0.2192(4) 0.097(3) Uani 1 1 d . . . H19 H 0.7097 0.2751 0.2091 0.117 Uiso 1 1 calc R . . C20 C 0.8850(5) 0.2315(5) 0.0681(3) 0.0498(15) Uani 1 1 d . . . C21 C 0.8094(6) 0.3475(5) 0.0565(4) 0.0687(18) Uani 1 1 d . . . H21 H 0.7836 0.4076 0.0859 0.082 Uiso 1 1 calc R . . C22 C 0.7826(6) 0.3550(5) -0.0026(3) 0.0641(17) Uani 1 1 d . . . H22 H 0.7350 0.4212 -0.0226 0.077 Uiso 1 1 calc R . . C23 C 0.8394(5) 0.2438(5) -0.0307(3) 0.0523(15) Uani 1 1 d . . . C24 C 0.4453(9) 0.3238(6) 0.0819(4) 0.128(3) Uani 1 1 d . . . H24A H 0.5125 0.3372 0.0480 0.192 Uiso 1 1 calc R . . H24B H 0.4637 0.3399 0.1231 0.192 Uiso 1 1 calc R . . H24C H 0.3573 0.3731 0.0756 0.192 Uiso 1 1 calc R . . C25 C 0.4490(6) 0.1988(6) 0.0802(4) 0.076(2) Uani 1 1 d . . . C26 C 0.4497(7) 0.1321(8) 0.1351(4) 0.087(2) Uani 1 1 d . . . H26 H 0.4552 0.1646 0.1732 0.105 Uiso 1 1 calc R . . C27 C 0.4427(6) 0.0200(7) 0.1392(3) 0.0674(19) Uani 1 1 d . . . C28 C 0.4208(7) -0.0303(7) 0.2057(3) 0.099(3) Uani 1 1 d . . . H28A H 0.3327 0.0112 0.2281 0.148 Uiso 1 1 calc R . . H28B H 0.4887 -0.0249 0.2296 0.148 Uiso 1 1 calc R . . H28C H 0.4270 -0.1095 0.2021 0.148 Uiso 1 1 calc R . . C29 C 0.6386(7) 0.8745(6) 0.4267(3) 0.086(2) Uani 1 1 d . . . H29A H 0.6474 0.8718 0.4721 0.103 Uiso 1 1 calc R . . H29B H 0.5777 0.9494 0.4179 0.103 Uiso 1 1 calc R . . C30 C 0.5782(8) 0.7851(8) 0.4139(4) 0.084(2) Uani 1 1 d . . . C31 C 0.6138(8) 0.6787(9) 0.4429(4) 0.100(3) Uani 1 1 d . . . H31 H 0.6737 0.6633 0.4726 0.120 Uiso 1 1 calc R . . C32 C 0.4873(10) 0.8058(10) 0.3697(5) 0.122(3) Uani 1 1 d . . . H32 H 0.4597 0.8777 0.3505 0.146 Uiso 1 1 calc R . . C33 C 0.4376(12) 0.7196(17) 0.3544(6) 0.163(5) Uani 1 1 d . . . H33 H 0.3791 0.7327 0.3242 0.195 Uiso 1 1 calc R . . C34 C 0.4771(14) 0.6144(14) 0.3848(8) 0.151(5) Uani 1 1 d . . . H34 H 0.4447 0.5562 0.3751 0.181 Uiso 1 1 calc R . . C35 C 0.7923(6) 0.8425(6) 0.2958(3) 0.0674(18) Uani 1 1 d . . . C36 C 0.7871(7) 0.7396(6) 0.2730(4) 0.081(2) Uani 1 1 d . . . H36 H 0.7897 0.6778 0.3011 0.097 Uiso 1 1 calc R . . C37 C 0.7781(7) 0.7302(7) 0.2093(4) 0.085(2) Uani 1 1 d . . . H37 H 0.7764 0.6612 0.1940 0.103 Uiso 1 1 calc R . . C38 C 0.7717(7) 0.8218(8) 0.1678(4) 0.086(2) Uani 1 1 d . . . H38 H 0.7663 0.8145 0.1245 0.104 Uiso 1 1 calc R . . C39 C 0.7731(6) 0.9228(7) 0.1899(4) 0.080(2) Uani 1 1 d . . . H39 H 0.7668 0.9850 0.1618 0.096 Uiso 1 1 calc R . . C40 C 0.7839(6) 0.9343(6) 0.2533(4) 0.0730(19) Uani 1 1 d . . . H40 H 0.7856 1.0039 0.2679 0.088 Uiso 1 1 calc R . . C41 C 0.8607(13) 0.9759(8) 0.3883(5) 0.108(3) Uani 1 1 d . . . C42 C 0.9931(15) 0.9616(10) 0.3750(5) 0.160(5) Uani 1 1 d . . . H42 H 1.0522 0.8902 0.3611 0.191 Uiso 1 1 calc R . . C43 C 1.0477(18) 1.0545(15) 0.3815(6) 0.189(6) Uani 1 1 d . . . H43 H 1.1402 1.0443 0.3757 0.226 Uiso 1 1 calc R . . C44 C 0.954(3) 1.1554(15) 0.3964(11) 0.253(13) Uani 1 1 d . . . H44 H 0.9846 1.2181 0.3982 0.303 Uiso 1 1 calc R . . C45 C 0.821(2) 1.1747(16) 0.4091(14) 0.314(15) Uani 1 1 d . . . H45 H 0.7603 1.2470 0.4203 0.377 Uiso 1 1 calc R . . C46 C 0.9277(7) 0.7337(6) 0.4035(4) 0.0723(19) Uani 1 1 d . . . C47 C 1.0311(9) 0.6640(8) 0.3591(4) 0.095(2) Uani 1 1 d . . . H47 H 1.0303 0.6759 0.3149 0.114 Uiso 1 1 calc R . . C48 C 1.1343(9) 0.5776(8) 0.3805(5) 0.117(3) Uani 1 1 d . . . H48 H 1.2032 0.5310 0.3509 0.140 Uiso 1 1 calc R . . C49 C 1.0377(11) 0.6278(9) 0.4892(4) 0.110(3) Uani 1 1 d . . . H49 H 1.0418 0.6148 0.5331 0.132 Uiso 1 1 calc R . . C50 C 0.9310(8) 0.7162(6) 0.4690(4) 0.090(2) Uani 1 1 d . . . H50 H 0.8633 0.7626 0.4992 0.107 Uiso 1 1 calc R . . C51 C 1.1354(10) 0.5610(8) 0.4438(5) 0.114(3) Uani 1 1 d . . . H51 H 1.2053 0.5017 0.4575 0.137 Uiso 1 1 calc R . . C52 C 0.7766(15) 1.0767(11) 0.4043(7) 0.207(7) Uani 1 1 d . . . H52 H 0.6844 1.0858 0.4130 0.249 Uiso 1 1 calc R . . C53 C 0.5623(12) 0.5954(10) 0.4287(6) 0.134(4) Uani 1 1 d . . . H53 H 0.5863 0.5247 0.4496 0.160 Uiso 1 1 calc R . . C54 C 0.1444(9) 0.3539(8) 0.9836(6) 0.161(5) Uani 1 1 d . . . H54A H 0.1448 0.3720 1.0275 0.242 Uiso 1 1 calc R . . H54B H 0.1228 0.2838 0.9827 0.242 Uiso 1 1 calc R . . H54C H 0.0780 0.4149 0.9656 0.242 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 0.0327(4) 0.0479(5) 0.0587(5) -0.0092(3) -0.0074(3) -0.0120(3) Mn1 0.0302(6) 0.0417(7) 0.0626(9) 0.0006(6) -0.0094(6) -0.0105(6) P1 0.122(2) 0.0781(16) 0.0735(17) -0.0044(13) 0.0012(14) -0.0061(15) P2 0.0973(15) 0.0728(13) 0.0691(13) 0.0036(10) -0.0211(11) -0.0290(12) O1 0.052(2) 0.049(3) 0.084(3) -0.012(2) -0.020(2) -0.011(2) O2 0.042(2) 0.082(3) 0.057(3) -0.015(2) -0.0122(19) -0.020(2) O3 0.098(4) 0.109(5) 0.182(6) 0.015(4) -0.031(4) -0.029(4) N1 0.037(3) 0.058(3) 0.064(3) 0.004(2) -0.011(2) -0.017(2) N2 0.034(2) 0.041(3) 0.061(3) -0.001(2) -0.007(2) -0.011(2) N3 0.037(3) 0.046(3) 0.059(3) 0.001(3) -0.011(2) -0.011(2) F1 0.116(4) 0.245(7) 0.161(5) -0.082(5) -0.007(4) 0.042(5) F2 0.303(12) 0.282(11) 0.399(16) -0.173(11) -0.007(10) -0.161(10) F3 0.175(6) 0.186(6) 0.197(7) -0.042(5) 0.064(5) -0.001(5) F4 0.415(13) 0.285(10) 0.083(5) 0.034(6) -0.017(6) 0.129(10) F5 0.237(9) 0.235(9) 0.375(14) -0.128(9) 0.088(8) -0.137(8) F6 0.293(9) 0.206(7) 0.138(6) 0.071(5) -0.025(6) 0.021(7) C1 0.035(3) 0.046(3) 0.054(4) -0.006(3) -0.002(3) -0.016(3) C2 0.034(3) 0.051(4) 0.060(4) 0.003(3) -0.011(3) -0.011(3) C3 0.043(3) 0.044(4) 0.072(5) 0.011(3) -0.011(3) -0.006(3) C4 0.047(4) 0.052(4) 0.061(4) 0.002(3) -0.010(3) -0.001(3) C5 0.056(4) 0.083(5) 0.091(6) 0.022(4) -0.002(4) -0.009(4) C6 0.093(6) 0.066(5) 0.087(6) 0.021(4) -0.004(5) -0.008(5) C7 0.094(6) 0.064(5) 0.091(6) 0.000(4) -0.041(5) 0.017(5) C8 0.074(5) 0.076(6) 0.131(8) 0.010(5) -0.054(5) -0.007(5) C9 0.054(4) 0.070(5) 0.125(7) 0.020(4) -0.030(4) -0.015(4) C10 0.047(4) 0.056(4) 0.067(5) 0.006(3) -0.022(3) -0.005(3) C11 0.050(4) 0.063(5) 0.066(5) -0.007(3) -0.011(3) -0.011(3) C12 0.043(3) 0.045(4) 0.058(4) 0.008(3) -0.011(3) -0.017(3) C13 0.050(4) 0.057(4) 0.060(4) -0.003(3) -0.009(3) -0.021(3) C14 0.074(5) 0.059(4) 0.065(5) -0.003(3) -0.012(4) -0.016(4) C15 0.158(9) 0.135(8) 0.120(8) -0.048(6) 0.013(6) -0.096(7) C16 0.197(13) 0.168(11) 0.149(11) -0.044(8) -0.003(9) -0.128(10) C17 0.201(13) 0.072(6) 0.131(10) -0.037(6) -0.033(9) -0.026(8) C18 0.118(8) 0.132(9) 0.110(8) -0.045(7) -0.023(6) 0.017(7) C19 0.076(5) 0.116(7) 0.086(6) -0.041(5) -0.023(4) 0.001(5) C20 0.040(3) 0.045(4) 0.063(4) -0.001(3) -0.007(3) -0.012(3) C21 0.070(4) 0.046(4) 0.086(6) -0.007(4) -0.014(4) -0.010(3) C22 0.059(4) 0.040(4) 0.087(5) 0.011(3) -0.020(4) -0.005(3) C23 0.043(3) 0.040(4) 0.068(5) 0.004(3) -0.014(3) -0.004(3) C24 0.133(8) 0.085(6) 0.172(9) -0.056(6) -0.027(6) -0.032(6) C25 0.059(4) 0.073(5) 0.092(6) -0.046(5) -0.006(4) -0.011(4) C26 0.094(6) 0.113(7) 0.055(5) -0.029(5) -0.007(4) -0.030(5) C27 0.038(3) 0.102(6) 0.063(5) -0.001(4) -0.009(3) -0.023(4) C28 0.070(5) 0.156(8) 0.072(6) 0.003(5) -0.009(4) -0.040(5) C29 0.093(5) 0.074(5) 0.075(5) -0.003(4) -0.012(4) -0.004(4) C30 0.077(5) 0.093(7) 0.072(6) 0.003(5) 0.000(4) -0.020(5) C31 0.106(6) 0.110(7) 0.092(7) 0.016(6) -0.011(5) -0.049(6) C32 0.108(7) 0.149(10) 0.091(7) 0.011(6) -0.012(6) -0.020(7) C33 0.121(9) 0.262(18) 0.134(12) -0.034(12) -0.014(7) -0.097(13) C34 0.126(11) 0.178(14) 0.165(14) -0.041(11) 0.026(9) -0.091(11) C35 0.065(4) 0.075(5) 0.063(5) 0.008(4) -0.006(3) -0.027(4) C36 0.101(6) 0.075(5) 0.074(6) 0.010(4) -0.021(4) -0.036(4) C37 0.084(5) 0.098(6) 0.081(6) -0.001(5) -0.025(4) -0.033(5) C38 0.074(5) 0.123(7) 0.066(5) 0.010(5) -0.019(4) -0.034(5) C39 0.066(5) 0.107(7) 0.074(6) 0.022(5) -0.013(4) -0.039(5) C40 0.062(4) 0.086(5) 0.078(6) 0.006(4) -0.018(4) -0.031(4) C41 0.150(9) 0.082(7) 0.112(8) 0.008(5) -0.054(7) -0.048(7) C42 0.220(14) 0.152(10) 0.141(10) -0.029(7) 0.004(9) -0.118(11) C43 0.274(18) 0.203(14) 0.177(12) 0.036(11) -0.088(12) -0.178(16) C44 0.40(3) 0.098(12) 0.33(2) 0.041(13) -0.25(3) -0.087(19) C45 0.34(3) 0.106(12) 0.57(4) 0.019(15) -0.31(3) -0.056(17) C46 0.086(5) 0.079(5) 0.064(5) 0.009(4) -0.019(4) -0.041(4) C47 0.096(6) 0.114(7) 0.072(6) -0.003(5) -0.007(5) -0.032(6) C48 0.107(7) 0.118(8) 0.112(9) 0.010(6) -0.034(6) -0.010(6) C49 0.143(8) 0.117(8) 0.078(7) 0.016(6) -0.041(6) -0.042(7) C50 0.112(6) 0.081(6) 0.066(6) 0.003(4) -0.017(5) -0.015(5) C51 0.124(8) 0.104(7) 0.103(8) 0.016(6) -0.031(7) -0.017(6) C52 0.230(15) 0.087(8) 0.350(19) -0.013(10) -0.168(13) -0.048(10) C53 0.131(9) 0.138(10) 0.139(11) 0.018(8) -0.003(7) -0.066(8) C54 0.085(7) 0.110(8) 0.270(14) -0.027(8) 0.025(8) -0.026(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 O2 1.975(4) . ? Ru1 O2 1.975(4) 2_655 ? Ru1 O1 2.000(4) . ? Ru1 O1 2.000(4) 2_655 ? Ru1 C1 2.042(5) . ? Ru1 C1 2.042(5) 2_655 ? Mn1 N2 2.000(5) . ? Mn1 N2 2.000(5) 2_755 ? Mn1 N3 2.017(4) . ? Mn1 N3 2.017(4) 2_755 ? Mn1 N1 2.251(4) 2_755 ? Mn1 N1 2.251(4) . ? P1 F2 1.444(8) . ? P1 F6 1.482(6) . ? P1 F4 1.494(7) . ? P1 F1 1.506(5) . ? P1 F5 1.512(8) . ? P1 F3 1.557(6) . ? P2 C35 1.770(7) . ? P2 C46 1.787(7) . ? P2 C41 1.791(9) . ? P2 C29 1.807(7) . ? O1 C25 1.292(8) . ? O2 C27 1.248(7) . ? O3 C54 1.416(9) . ? O3 H3 0.8200 . ? N1 C1 1.151(6) . ? N2 C12 1.368(7) . ? N2 C2 1.378(7) . ? N3 C20 1.367(7) . ? N3 C23 1.368(7) . ? C2 C3 1.388(7) . ? C2 C10 1.419(7) . ? C3 C23 1.391(8) 2_755 ? C3 C4 1.501(8) . ? C4 C5 1.369(8) . ? C4 C9 1.370(8) . ? C5 C6 1.384(9) . ? C5 H5 0.9300 . ? C6 C7 1.341(10) . ? C6 H6 0.9300 . ? C7 C8 1.354(10) . ? C7 H7 0.9300 . ? C8 C9 1.385(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.345(7) . ? C10 H10 0.9300 . ? C11 C12 1.413(8) . ? C11 H11 0.9300 . ? C12 C13 1.399(7) . ? C13 C20 1.390(8) . ? C13 C14 1.500(8) . ? C14 C19 1.346(9) . ? C14 C15 1.400(10) . ? C15 C16 1.399(12) . ? C15 H15 0.9300 . ? C16 C17 1.352(13) . ? C16 H16 0.9300 . ? C17 C18 1.355(13) . ? C17 H17 0.9300 . ? C18 C19 1.385(10) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.426(8) . ? C21 C22 1.307(8) . ? C21 H21 0.9300 . ? C22 C23 1.423(8) . ? C22 H22 0.9300 . ? C23 C3 1.391(8) 2_755 ? C24 C25 1.526(9) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.374(10) . ? C26 C27 1.400(9) . ? C26 H26 0.9300 . ? C27 C28 1.504(9) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.489(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.376(10) . ? C30 C32 1.400(11) . ? C31 C53 1.368(13) . ? C31 H31 0.9300 . ? C32 C33 1.395(15) . ? C32 H32 0.9300 . ? C33 C34 1.381(16) . ? C33 H33 0.9300 . ? C34 C53 1.354(15) . ? C34 H34 0.9300 . ? C35 C40 1.386(8) . ? C35 C36 1.396(9) . ? C36 C37 1.368(9) . ? C36 H36 0.9300 . ? C37 C38 1.375(9) . ? C37 H37 0.9300 . ? C38 C39 1.354(9) . ? C38 H38 0.9300 . ? C39 C40 1.372(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C52 1.297(13) . ? C41 C42 1.333(13) . ? C42 C43 1.453(14) . ? C42 H42 0.9300 . ? C43 C44 1.33(2) . ? C43 H43 0.9300 . ? C44 C45 1.33(3) . ? C44 H44 0.9300 . ? C45 C52 1.436(19) . ? C45 H45 0.9300 . ? C46 C50 1.381(9) . ? C46 C47 1.394(9) . ? C47 C48 1.376(10) . ? C47 H47 0.9300 . ? C48 C51 1.330(11) . ? C48 H48 0.9300 . ? C49 C51 1.365(11) . ? C49 C50 1.401(10) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 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 O2 Ru1 O2 180.0(3) . 2_655 ? O2 Ru1 O1 90.95(17) . . ? O2 Ru1 O1 89.05(17) 2_655 . ? O2 Ru1 O1 89.05(17) . 2_655 ? O2 Ru1 O1 90.95(17) 2_655 2_655 ? O1 Ru1 O1 180.0(2) . 2_655 ? O2 Ru1 C1 88.89(18) . . ? O2 Ru1 C1 91.11(18) 2_655 . ? O1 Ru1 C1 88.60(17) . . ? O1 Ru1 C1 91.40(17) 2_655 . ? O2 Ru1 C1 91.11(18) . 2_655 ? O2 Ru1 C1 88.89(18) 2_655 2_655 ? O1 Ru1 C1 91.40(17) . 2_655 ? O1 Ru1 C1 88.60(17) 2_655 2_655 ? C1 Ru1 C1 180.0(3) . 2_655 ? N2 Mn1 N2 180.0(4) . 2_755 ? N2 Mn1 N3 89.39(18) . . ? N2 Mn1 N3 90.61(18) 2_755 . ? N2 Mn1 N3 90.61(18) . 2_755 ? N2 Mn1 N3 89.39(18) 2_755 2_755 ? N3 Mn1 N3 180.0(4) . 2_755 ? N2 Mn1 N1 86.05(16) . 2_755 ? N2 Mn1 N1 93.95(16) 2_755 2_755 ? N3 Mn1 N1 91.40(16) . 2_755 ? N3 Mn1 N1 88.60(16) 2_755 2_755 ? N2 Mn1 N1 93.95(16) . . ? N2 Mn1 N1 86.05(16) 2_755 . ? N3 Mn1 N1 88.60(16) . . ? N3 Mn1 N1 91.40(16) 2_755 . ? N1 Mn1 N1 180.0(3) 2_755 . ? F2 P1 F6 88.1(6) . . ? F2 P1 F4 93.8(7) . . ? F6 P1 F4 177.4(7) . . ? F2 P1 F1 99.5(5) . . ? F6 P1 F1 91.1(4) . . ? F4 P1 F1 90.4(4) . . ? F2 P1 F5 172.7(7) . . ? F6 P1 F5 87.5(6) . . ? F4 P1 F5 90.4(7) . . ? F1 P1 F5 86.3(4) . . ? F2 P1 F3 87.4(5) . . ? F6 P1 F3 91.3(4) . . ? F4 P1 F3 87.0(4) . . ? F1 P1 F3 172.7(5) . . ? F5 P1 F3 86.9(5) . . ? C35 P2 C46 109.8(3) . . ? C35 P2 C41 110.3(4) . . ? C46 P2 C41 105.3(4) . . ? C35 P2 C29 109.3(3) . . ? C46 P2 C29 111.1(3) . . ? C41 P2 C29 110.9(5) . . ? C25 O1 Ru1 122.0(5) . . ? C27 O2 Ru1 125.5(5) . . ? C54 O3 H3 109.5 . . ? C1 N1 Mn1 152.3(4) . . ? C12 N2 C2 105.6(5) . . ? C12 N2 Mn1 127.9(4) . . ? C2 N2 Mn1 126.2(4) . . ? C20 N3 C23 106.4(5) . . ? C20 N3 Mn1 127.4(4) . . ? C23 N3 Mn1 126.2(4) . . ? N1 C1 Ru1 177.5(5) . . ? N2 C2 C3 126.4(6) . . ? N2 C2 C10 109.3(5) . . ? C3 C2 C10 124.2(5) . . ? C2 C3 C23 124.1(5) . 2_755 ? C2 C3 C4 117.5(6) . . ? C23 C3 C4 118.4(5) 2_755 . ? C5 C4 C9 119.0(6) . . ? C5 C4 C3 121.5(5) . . ? C9 C4 C3 119.5(6) . . ? C4 C5 C6 119.8(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.7(7) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 120.3(7) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 119.9(7) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C4 C9 C8 120.2(7) . . ? C4 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C2 107.6(5) . . ? C11 C10 H10 126.2 . . ? C2 C10 H10 126.2 . . ? C10 C11 C12 107.0(5) . . ? C10 C11 H11 126.5 . . ? C12 C11 H11 126.5 . . ? N2 C12 C13 125.4(6) . . ? N2 C12 C11 110.4(5) . . ? C13 C12 C11 124.2(6) . . ? C20 C13 C12 124.0(5) . . ? C20 C13 C14 118.6(6) . . ? C12 C13 C14 117.3(6) . . ? C19 C14 C15 119.7(7) . . ? C19 C14 C13 121.7(6) . . ? C15 C14 C13 118.6(6) . . ? C16 C15 C14 117.5(9) . . ? C16 C15 H15 121.2 . . ? C14 C15 H15 121.2 . . ? C17 C16 C15 120.8(10) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 121.6(10) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C19 117.9(10) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C14 C19 C18 122.4(8) . . ? C14 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? N3 C20 C13 125.8(5) . . ? N3 C20 C21 108.6(6) . . ? C13 C20 C21 125.6(6) . . ? C22 C21 C20 108.3(6) . . ? C22 C21 H21 125.9 . . ? C20 C21 H21 125.9 . . ? C21 C22 C23 107.8(6) . . ? C21 C22 H22 126.1 . . ? C23 C22 H22 126.1 . . ? N3 C23 C3 126.3(5) . 2_755 ? N3 C23 C22 109.0(5) . . ? C3 C23 C22 124.7(6) 2_755 . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 C26 125.7(7) . . ? O1 C25 C24 112.3(8) . . ? C26 C25 C24 122.1(7) . . ? C25 C26 C27 126.2(7) . . ? C25 C26 H26 116.9 . . ? C27 C26 H26 116.9 . . ? O2 C27 C26 124.1(7) . . ? O2 C27 C28 118.3(7) . . ? C26 C27 C28 117.5(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P2 113.0(5) . . ? C30 C29 H29A 109.0 . . ? P2 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? P2 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C32 118.2(9) . . ? C31 C30 C29 121.3(8) . . ? C32 C30 C29 120.4(9) . . ? C53 C31 C30 120.9(10) . . ? C53 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C30 120.6(11) . . ? C33 C32 H32 119.7 . . ? C30 C32 H32 119.7 . . ? C34 C33 C32 118.7(14) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C53 C34 C33 120.6(14) . . ? C53 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C40 C35 C36 118.9(7) . . ? C40 C35 P2 120.7(6) . . ? C36 C35 P2 120.3(6) . . ? C37 C36 C35 119.7(7) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.5(8) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 120.1(8) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.7(7) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C35 120.1(7) . . ? C39 C40 H40 119.9 . . ? C35 C40 H40 119.9 . . ? C52 C41 C42 119.6(11) . . ? C52 C41 P2 121.6(10) . . ? C42 C41 P2 118.7(9) . . ? C41 C42 C43 121.9(13) . . ? C41 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C44 C43 C42 114.2(17) . . ? C44 C43 H43 122.9 . . ? C42 C43 H43 122.9 . . ? C45 C44 C43 126(2) . . ? C45 C44 H44 116.9 . . ? C43 C44 H44 116.9 . . ? C44 C45 C52 116(2) . . ? C44 C45 H45 122.2 . . ? C52 C45 H45 122.2 . . ? C50 C46 C47 119.4(7) . . ? C50 C46 P2 118.6(6) . . ? C47 C46 P2 121.5(6) . . ? C48 C47 C46 120.1(8) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C51 C48 C47 119.9(9) . . ? C51 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C51 C49 C50 119.2(9) . . ? C51 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? C46 C50 C49 119.1(7) . . ? C46 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C48 C51 C49 122.4(9) . . ? C48 C51 H51 118.8 . . ? C49 C51 H51 118.8 . . ? C41 C52 C45 122.4(16) . . ? C41 C52 H52 118.8 . . ? C45 C52 H52 118.8 . . ? C34 C53 C31 120.9(12) . . ? C34 C53 H53 119.5 . . ? C31 C53 H53 119.5 . . ? O3 C54 H54A 109.5 . . ? O3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.580 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.071 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 758955' #TrackingRef '1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H94 Cl2 Mn N6 O14 P2 Ru' _chemical_formula_weight 1988.74 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' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5763(11) _cell_length_b 12.3936(12) _cell_length_c 20.440(2) _cell_angle_alpha 85.583(2) _cell_angle_beta 77.824(2) _cell_angle_gamma 69.901(2) _cell_volume 2459.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3969 _cell_measurement_theta_min 2.618 _cell_measurement_theta_max 25.759 _exptl_crystal_description block _exptl_crystal_colour purple-black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.343 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1029 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9141 _exptl_absorpt_correction_T_max 0.9257 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12190 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8594 _reflns_number_gt 6376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0807P)^2^+0.3747P] 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 8594 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.0000 0.0000 0.0000 0.03889(13) Uani 1 2 d S . . Mn1 Mn 0.5000 0.0000 0.0000 0.03856(18) Uani 1 2 d S . . Cl1 Cl 0.88044(15) 0.24066(11) 0.35110(6) 0.0911(4) Uani 1 1 d . . . P1 P 0.28852(13) 0.86466(9) 0.38796(5) 0.0683(3) Uani 1 1 d . . . O1 O -0.0508(2) 0.16850(19) 0.01478(12) 0.0520(6) Uani 1 1 d . . . O2 O -0.0658(2) -0.0251(2) 0.09771(11) 0.0510(6) Uani 1 1 d . . . O3 O 0.8874(6) 0.1440(4) 0.3909(2) 0.170(2) Uani 1 1 d . . . O4 O 0.8984(6) 0.3258(4) 0.3853(2) 0.173(2) Uani 1 1 d . . . O5 O 0.9777(6) 0.2146(5) 0.2936(2) 0.162(2) Uani 1 1 d . . . O6 O 0.7513(6) 0.2825(5) 0.3352(3) 0.188(2) Uani 1 1 d . . . O7 O 0.7777(4) 0.3410(3) 0.93455(19) 0.1030(11) Uani 1 1 d . . . H7 H 0.8343 0.2871 0.9497 0.154 Uiso 1 1 d R . . N1 N 0.2953(3) -0.0265(2) 0.02793(14) 0.0468(7) Uani 1 1 d . . . N2 N 0.4025(3) 0.1706(2) 0.01207(14) 0.0441(6) Uani 1 1 d . . . N3 N 0.5308(3) -0.0126(2) 0.09471(13) 0.0431(6) Uani 1 1 d . . . C1 C 0.1901(3) -0.0193(3) 0.01822(15) 0.0396(7) Uani 1 1 d . . . C2 C -0.0586(6) 0.3327(4) 0.0680(3) 0.1009(17) Uani 1 1 d . . . H2A H -0.0365 0.3542 0.0220 0.151 Uiso 1 1 calc R . . H2B H 0.0079 0.3393 0.0915 0.151 Uiso 1 1 calc R . . H2C H -0.1483 0.3825 0.0880 0.151 Uiso 1 1 calc R . . C3 C -0.0567(4) 0.2098(3) 0.0718(2) 0.0625(10) Uani 1 1 d . . . C4 C -0.0656(4) 0.1539(4) 0.1319(2) 0.0699(12) Uani 1 1 d . . . H4 H -0.0640 0.1922 0.1689 0.084 Uiso 1 1 calc R . . C5 C -0.0771(4) 0.0444(4) 0.14301(18) 0.0596(10) Uani 1 1 d . . . C6 C -0.1073(5) 0.0026(5) 0.21388(18) 0.0826(14) Uani 1 1 d . . . H6A H -0.2011 0.0429 0.2339 0.124 Uiso 1 1 calc R . . H6B H -0.0476 0.0166 0.2392 0.124 Uiso 1 1 calc R . . H6C H -0.0923 -0.0783 0.2137 0.124 Uiso 1 1 calc R . . C7 C 0.3415(3) 0.2463(3) -0.03424(18) 0.0482(8) Uani 1 1 d . . . C8 C 0.2820(4) 0.3591(3) -0.0058(2) 0.0622(10) Uani 1 1 d . . . H8 H 0.2347 0.4254 -0.0269 0.075 Uiso 1 1 calc R . . C9 C 0.3066(4) 0.3522(3) 0.0566(2) 0.0639(10) Uani 1 1 d . . . H9 H 0.2806 0.4126 0.0864 0.077 Uiso 1 1 calc R . . C10 C 0.3807(3) 0.2339(3) 0.06832(18) 0.0485(8) Uani 1 1 d . . . C11 C 0.4234(3) 0.1910(3) 0.12774(18) 0.0506(8) Uani 1 1 d . . . C12 C 0.3913(4) 0.2740(3) 0.18415(19) 0.0604(10) Uani 1 1 d . . . C13 C 0.2639(5) 0.3096(4) 0.2245(2) 0.0853(14) Uani 1 1 d . . . H13 H 0.1964 0.2831 0.2163 0.102 Uiso 1 1 calc R . . C14 C 0.2329(6) 0.3837(5) 0.2770(3) 0.110(2) Uani 1 1 d . . . H14 H 0.1455 0.4067 0.3038 0.132 Uiso 1 1 calc R . . C15 C 0.3293(9) 0.4226(5) 0.2893(3) 0.114(2) Uani 1 1 d . . . H15 H 0.3077 0.4747 0.3237 0.137 Uiso 1 1 calc R . . C16 C 0.4593(9) 0.3859(6) 0.2515(3) 0.133(3) Uani 1 1 d . . . H16 H 0.5265 0.4107 0.2616 0.160 Uiso 1 1 calc R . . C17 C 0.4922(6) 0.3110(5) 0.1976(3) 0.1068(19) Uani 1 1 d . . . H17 H 0.5802 0.2867 0.1715 0.128 Uiso 1 1 calc R . . C18 C 0.4931(3) 0.0764(3) 0.13918(17) 0.0478(8) Uani 1 1 d . . . C19 C 0.5396(4) 0.0318(3) 0.19995(19) 0.0565(9) Uani 1 1 d . . . H19 H 0.5265 0.0737 0.2381 0.068 Uiso 1 1 calc R . . C20 C 0.6056(4) -0.0817(3) 0.19154(18) 0.0568(9) Uani 1 1 d . . . H20 H 0.6464 -0.1328 0.2229 0.068 Uiso 1 1 calc R . . C21 C 0.6016(3) -0.1096(3) 0.12578(17) 0.0465(8) Uani 1 1 d . . . C22 C 0.6632(3) -0.2190(3) 0.09827(18) 0.0496(8) Uani 1 1 d . . . C23 C 0.7428(4) -0.3123(3) 0.13970(17) 0.0525(9) Uani 1 1 d . . . C24 C 0.6878(4) -0.3908(3) 0.1744(2) 0.0682(11) Uani 1 1 d . . . H24 H 0.5993 -0.3867 0.1723 0.082 Uiso 1 1 calc R . . C25 C 0.7639(5) -0.4759(4) 0.2124(2) 0.0798(13) Uani 1 1 d . . . H25 H 0.7265 -0.5290 0.2356 0.096 Uiso 1 1 calc R . . C26 C 0.8942(5) -0.4820(4) 0.2160(2) 0.0789(13) Uani 1 1 d . . . H26 H 0.9447 -0.5386 0.2420 0.095 Uiso 1 1 calc R . . C27 C 0.9498(5) -0.4056(4) 0.1815(2) 0.0832(13) Uani 1 1 d . . . H27 H 1.0384 -0.4103 0.1838 0.100 Uiso 1 1 calc R . . C28 C 0.8749(4) -0.3204(4) 0.1430(2) 0.0709(11) Uani 1 1 d . . . H28 H 0.9136 -0.2686 0.1194 0.085 Uiso 1 1 calc R . . C29 C 0.2798(4) 0.8512(3) 0.30268(18) 0.0598(10) Uani 1 1 d . . . C30 C 0.2799(4) 0.7477(4) 0.2809(2) 0.0698(11) Uani 1 1 d . . . H30 H 0.2879 0.6850 0.3098 0.084 Uiso 1 1 calc R . . C31 C 0.2680(5) 0.7394(4) 0.2157(2) 0.0758(12) Uani 1 1 d . . . H31 H 0.2696 0.6703 0.2002 0.091 Uiso 1 1 calc R . . C32 C 0.2538(5) 0.8329(4) 0.1735(2) 0.0752(12) Uani 1 1 d . . . H32 H 0.2454 0.8267 0.1297 0.090 Uiso 1 1 calc R . . C33 C 0.2520(4) 0.9355(4) 0.1956(2) 0.0704(11) Uani 1 1 d . . . H33 H 0.2425 0.9982 0.1667 0.084 Uiso 1 1 calc R . . C34 C 0.2641(4) 0.9459(4) 0.26061(19) 0.0620(10) Uani 1 1 d . . . H34 H 0.2617 1.0155 0.2759 0.074 Uiso 1 1 calc R . . C35 C 0.3409(7) 0.9849(4) 0.3968(3) 0.0967(17) Uani 1 1 d . . . C36 C 0.2426(10) 1.0940(5) 0.4073(4) 0.165(4) Uani 1 1 d . . . H36 H 0.1491 1.1068 0.4126 0.198 Uiso 1 1 calc R . . C37 C 0.2958(19) 1.1848(8) 0.4094(7) 0.251(9) Uani 1 1 d . . . H37 H 0.2353 1.2599 0.4147 0.302 Uiso 1 1 calc R . . C38 C 0.429(2) 1.1653(12) 0.4040(8) 0.261(10) Uani 1 1 d . . . H38 H 0.4560 1.2271 0.4102 0.313 Uiso 1 1 calc R . . C39 C 0.5325(13) 1.0579(10) 0.3895(4) 0.189(5) Uani 1 1 d . . . H39 H 0.6254 1.0492 0.3803 0.227 Uiso 1 1 calc R . . C40 C 0.4852(9) 0.9640(6) 0.3897(3) 0.135(3) Uani 1 1 d . . . H40 H 0.5471 0.8893 0.3853 0.162 Uiso 1 1 calc R . . C41 C 0.4156(5) 0.7406(4) 0.4140(2) 0.0675(11) Uani 1 1 d . . . C42 C 0.5232(5) 0.6735(4) 0.3675(3) 0.0840(13) Uani 1 1 d . . . H42 H 0.5254 0.6870 0.3219 0.101 Uiso 1 1 calc R . . C43 C 0.6283(6) 0.5856(5) 0.3895(3) 0.0999(16) Uani 1 1 d . . . H43 H 0.7006 0.5392 0.3586 0.120 Uiso 1 1 calc R . . C44 C 0.6260(6) 0.5671(5) 0.4553(4) 0.1020(18) Uani 1 1 d . . . H44 H 0.6980 0.5087 0.4692 0.122 Uiso 1 1 calc R . . C45 C 0.5211(7) 0.6317(5) 0.5020(3) 0.0989(17) Uani 1 1 d . . . H45 H 0.5214 0.6165 0.5473 0.119 Uiso 1 1 calc R . . C46 C 0.4124(5) 0.7213(4) 0.4823(2) 0.0807(13) Uani 1 1 d . . . H46 H 0.3404 0.7665 0.5139 0.097 Uiso 1 1 calc R . . C47 C 0.0583(5) 0.7988(5) 0.4238(2) 0.0872(15) Uani 1 1 d . . . C48 C 0.0943(6) 0.6891(6) 0.4504(3) 0.1067(18) Uani 1 1 d . . . H48 H 0.1532 0.6693 0.4807 0.128 Uiso 1 1 calc R . . C49 C 0.0445(9) 0.6083(7) 0.4330(4) 0.136(2) Uani 1 1 d . . . H49 H 0.0695 0.5348 0.4515 0.163 Uiso 1 1 calc R . . C50 C -0.0423(9) 0.6368(10) 0.3881(5) 0.151(3) Uani 1 1 d . . . H50 H -0.0748 0.5821 0.3757 0.182 Uiso 1 1 calc R . . C51 C -0.0814(8) 0.7462(11) 0.3615(4) 0.158(3) Uani 1 1 d . . . H51 H -0.1419 0.7655 0.3320 0.189 Uiso 1 1 calc R . . C52 C -0.0313(6) 0.8277(7) 0.3784(3) 0.120(2) Uani 1 1 d . . . H52 H -0.0567 0.9010 0.3598 0.144 Uiso 1 1 calc R . . C53 C 0.1204(5) 0.8836(4) 0.4393(2) 0.0826(14) Uani 1 1 d . . . H53A H 0.1279 0.8759 0.4860 0.099 Uiso 1 1 calc R . . H53B H 0.0596 0.9608 0.4325 0.099 Uiso 1 1 calc R . . C54 C 0.6453(6) 0.3559(5) 0.9730(4) 0.127(2) Uani 1 1 d . . . H54A H 0.6321 0.3981 1.0128 0.190 Uiso 1 1 calc R . . H54B H 0.6364 0.2821 0.9852 0.190 Uiso 1 1 calc R . . H54C H 0.5775 0.3975 0.9473 0.190 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 0.0296(2) 0.0446(2) 0.0436(2) -0.00345(16) -0.00972(15) -0.01182(16) Mn1 0.0271(3) 0.0370(4) 0.0516(4) 0.0035(3) -0.0122(3) -0.0091(3) Cl1 0.1163(11) 0.0794(8) 0.0564(7) -0.0012(6) -0.0224(7) -0.0029(7) P1 0.0859(8) 0.0588(6) 0.0551(6) -0.0013(5) -0.0194(5) -0.0142(6) O1 0.0462(14) 0.0493(14) 0.0615(15) -0.0059(12) -0.0146(11) -0.0139(11) O2 0.0414(13) 0.0702(16) 0.0463(13) -0.0014(12) -0.0098(10) -0.0241(12) O3 0.227(6) 0.117(4) 0.121(4) 0.047(3) -0.028(4) -0.014(4) O4 0.230(6) 0.140(4) 0.137(4) -0.057(3) -0.067(4) -0.016(4) O5 0.206(5) 0.197(5) 0.089(3) -0.043(3) 0.026(3) -0.098(4) O6 0.156(5) 0.169(5) 0.237(6) 0.049(4) -0.094(5) -0.028(4) O7 0.081(2) 0.099(3) 0.130(3) 0.013(2) -0.029(2) -0.030(2) N1 0.0329(15) 0.0534(17) 0.0563(17) 0.0060(13) -0.0132(12) -0.0160(13) N2 0.0351(14) 0.0393(15) 0.0572(17) 0.0026(13) -0.0145(12) -0.0090(12) N3 0.0321(14) 0.0433(15) 0.0522(16) 0.0051(13) -0.0110(12) -0.0102(12) C1 0.0377(18) 0.0403(18) 0.0399(17) 0.0009(14) -0.0063(13) -0.0132(14) C2 0.122(5) 0.068(3) 0.120(4) -0.028(3) -0.032(3) -0.030(3) C3 0.052(2) 0.058(2) 0.077(3) -0.020(2) -0.0109(19) -0.0151(18) C4 0.069(3) 0.084(3) 0.059(3) -0.027(2) -0.009(2) -0.025(2) C5 0.0378(19) 0.093(3) 0.048(2) -0.009(2) -0.0055(15) -0.0219(19) C6 0.073(3) 0.135(4) 0.045(2) -0.004(2) -0.0054(19) -0.044(3) C7 0.0420(19) 0.0387(18) 0.062(2) 0.0052(16) -0.0159(16) -0.0091(15) C8 0.060(2) 0.043(2) 0.076(3) 0.0054(19) -0.020(2) -0.0054(18) C9 0.065(3) 0.047(2) 0.077(3) -0.0017(19) -0.020(2) -0.0110(19) C10 0.0388(18) 0.0420(19) 0.064(2) -0.0015(16) -0.0099(16) -0.0118(15) C11 0.0417(19) 0.051(2) 0.060(2) -0.0040(17) -0.0108(16) -0.0162(16) C12 0.069(3) 0.050(2) 0.064(2) 0.0003(18) -0.023(2) -0.0168(19) C13 0.063(3) 0.098(4) 0.084(3) -0.028(3) -0.021(2) -0.004(2) C14 0.091(4) 0.120(5) 0.091(4) -0.034(3) -0.024(3) 0.010(4) C15 0.156(7) 0.073(4) 0.104(5) -0.021(3) -0.023(5) -0.025(4) C16 0.184(8) 0.140(6) 0.127(5) -0.025(5) -0.035(5) -0.111(6) C17 0.118(5) 0.122(5) 0.110(4) -0.028(3) -0.011(3) -0.078(4) C18 0.0385(18) 0.051(2) 0.056(2) 0.0022(16) -0.0118(15) -0.0158(16) C19 0.053(2) 0.053(2) 0.063(2) -0.0022(18) -0.0207(18) -0.0107(18) C20 0.049(2) 0.062(2) 0.060(2) 0.0086(18) -0.0207(17) -0.0157(18) C21 0.0337(17) 0.049(2) 0.055(2) 0.0111(16) -0.0158(14) -0.0108(15) C22 0.0359(18) 0.047(2) 0.064(2) 0.0090(17) -0.0158(15) -0.0095(15) C23 0.045(2) 0.049(2) 0.056(2) 0.0071(17) -0.0145(16) -0.0057(16) C24 0.056(2) 0.069(3) 0.074(3) 0.016(2) -0.015(2) -0.017(2) C25 0.083(3) 0.063(3) 0.080(3) 0.026(2) -0.018(2) -0.013(2) C26 0.084(3) 0.064(3) 0.073(3) 0.010(2) -0.034(2) 0.004(2) C27 0.058(3) 0.088(3) 0.099(3) 0.014(3) -0.036(2) -0.009(2) C28 0.056(2) 0.073(3) 0.085(3) 0.016(2) -0.029(2) -0.019(2) C29 0.061(2) 0.063(2) 0.053(2) -0.0012(19) -0.0088(18) -0.0198(19) C30 0.081(3) 0.069(3) 0.061(3) 0.001(2) -0.013(2) -0.028(2) C31 0.081(3) 0.083(3) 0.069(3) -0.009(2) -0.017(2) -0.031(2) C32 0.074(3) 0.099(4) 0.056(2) 0.002(2) -0.016(2) -0.032(3) C33 0.068(3) 0.084(3) 0.066(3) 0.019(2) -0.020(2) -0.035(2) C34 0.054(2) 0.070(3) 0.063(2) 0.007(2) -0.0146(18) -0.023(2) C35 0.150(5) 0.066(3) 0.083(3) 0.002(3) -0.053(4) -0.031(3) C36 0.291(11) 0.065(4) 0.144(6) -0.002(4) -0.099(7) -0.033(5) C37 0.46(3) 0.072(5) 0.274(13) 0.015(6) -0.242(17) -0.059(10) C38 0.50(3) 0.136(10) 0.271(14) 0.029(9) -0.261(19) -0.157(16) C39 0.313(14) 0.172(8) 0.179(8) 0.040(7) -0.131(9) -0.163(10) C40 0.199(8) 0.117(5) 0.134(6) 0.013(4) -0.072(6) -0.088(6) C41 0.075(3) 0.063(3) 0.068(3) 0.004(2) -0.025(2) -0.023(2) C42 0.072(3) 0.083(3) 0.092(3) 0.001(3) -0.019(3) -0.018(3) C43 0.081(4) 0.091(4) 0.119(5) 0.001(3) -0.031(3) -0.012(3) C44 0.091(4) 0.076(4) 0.142(6) 0.015(4) -0.052(4) -0.019(3) C45 0.129(5) 0.084(4) 0.102(4) 0.026(3) -0.063(4) -0.040(4) C46 0.099(4) 0.074(3) 0.076(3) 0.004(2) -0.035(3) -0.029(3) C47 0.060(3) 0.125(4) 0.055(3) 0.009(3) 0.000(2) -0.014(3) C48 0.103(4) 0.138(5) 0.079(3) 0.026(4) -0.011(3) -0.048(4) C49 0.118(6) 0.163(7) 0.136(6) 0.024(5) -0.007(5) -0.074(5) C50 0.110(6) 0.212(10) 0.148(8) -0.023(7) 0.005(5) -0.087(7) C51 0.096(5) 0.262(12) 0.135(7) -0.001(7) -0.030(5) -0.081(7) C52 0.079(4) 0.179(7) 0.083(4) 0.014(4) -0.017(3) -0.023(4) C53 0.081(3) 0.086(3) 0.054(2) -0.004(2) -0.007(2) 0.003(3) C54 0.077(4) 0.095(4) 0.195(7) -0.021(4) 0.003(4) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.000(2) . ? Ru1 O1 2.000(2) 2 ? Ru1 O2 2.009(2) 2 ? Ru1 O2 2.009(2) . ? Ru1 C1 2.052(3) . ? Ru1 C1 2.052(3) 2 ? Mn1 N3 2.016(3) 2_655 ? Mn1 N3 2.016(3) . ? Mn1 N2 2.017(3) 2_655 ? Mn1 N2 2.017(3) . ? Mn1 N1 2.250(3) 2_655 ? Mn1 N1 2.250(3) . ? Cl1 O5 1.366(4) . ? Cl1 O6 1.384(6) . ? Cl1 O3 1.385(4) . ? Cl1 O4 1.395(5) . ? P1 C29 1.788(4) . ? P1 C41 1.792(4) . ? P1 C35 1.792(6) . ? P1 C53 1.812(5) . ? O1 C3 1.290(4) . ? O2 C5 1.272(4) . ? O7 C54 1.412(6) . ? O7 H7 0.8200 . ? N1 C1 1.143(4) . ? N2 C10 1.376(4) . ? N2 C7 1.377(4) . ? N3 C21 1.369(4) . ? N3 C18 1.379(4) . ? C2 C3 1.512(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.364(6) . ? C4 C5 1.401(6) . ? C4 H4 0.9300 . ? C5 C6 1.507(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C22 1.392(5) 2_655 ? C7 C8 1.433(5) . ? C8 C9 1.346(5) . ? C8 H8 0.9300 . ? C9 C10 1.435(5) . ? C9 H9 0.9300 . ? C10 C11 1.389(5) . ? C11 C18 1.384(5) . ? C11 C12 1.510(5) . ? C12 C13 1.367(6) . ? C12 C17 1.379(6) . ? C13 C14 1.380(6) . ? C13 H13 0.9300 . ? C14 C15 1.341(9) . ? C14 H14 0.9300 . ? C15 C16 1.368(9) . ? C15 H15 0.9300 . ? C16 C17 1.404(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.433(5) . ? C19 C20 1.345(5) . ? C19 H19 0.9300 . ? C20 C21 1.426(5) . ? C20 H20 0.9300 . ? C21 C22 1.390(5) . ? C22 C7 1.392(5) 2_655 ? C22 C23 1.498(5) . ? C23 C24 1.377(5) . ? C23 C28 1.381(5) . ? C24 C25 1.384(6) . ? C24 H24 0.9300 . ? C25 C26 1.372(6) . ? C25 H25 0.9300 . ? C26 C27 1.357(6) . ? C26 H26 0.9300 . ? C27 C28 1.386(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.384(5) . ? C29 C30 1.389(5) . ? C30 C31 1.381(5) . ? C30 H30 0.9300 . ? C31 C32 1.374(6) . ? C31 H31 0.9300 . ? C32 C33 1.374(6) . ? C32 H32 0.9300 . ? C33 C34 1.381(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.393(8) . ? C35 C40 1.434(9) . ? C36 C37 1.427(14) . ? C36 H36 0.9300 . ? C37 C38 1.33(2) . ? C37 H37 0.9300 . ? C38 C39 1.407(17) . ? C38 H38 0.9300 . ? C39 C40 1.416(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.381(6) . ? C41 C46 1.393(6) . ? C42 C43 1.388(7) . ? C42 H42 0.9300 . ? C43 C44 1.343(7) . ? C43 H43 0.9300 . ? C44 C45 1.358(8) . ? C44 H44 0.9300 . ? C45 C46 1.403(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.380(8) . ? C47 C52 1.405(7) . ? C47 C53 1.500(7) . ? C48 C49 1.380(9) . ? C48 H48 0.9300 . ? C49 C50 1.375(10) . ? C49 H49 0.9300 . ? C50 C51 1.379(11) . ? C50 H50 0.9300 . ? C51 C52 1.384(11) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 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 O1 180.0(2) . 2 ? O1 Ru1 O2 89.00(10) . 2 ? O1 Ru1 O2 91.00(10) 2 2 ? O1 Ru1 O2 91.00(10) . . ? O1 Ru1 O2 89.00(10) 2 . ? O2 Ru1 O2 180.00(17) 2 . ? O1 Ru1 C1 87.75(11) . . ? O1 Ru1 C1 92.25(11) 2 . ? O2 Ru1 C1 90.10(10) 2 . ? O2 Ru1 C1 89.90(10) . . ? O1 Ru1 C1 92.25(11) . 2 ? O1 Ru1 C1 87.75(11) 2 2 ? O2 Ru1 C1 89.90(10) 2 2 ? O2 Ru1 C1 90.10(10) . 2 ? C1 Ru1 C1 180.0(2) . 2 ? N3 Mn1 N3 180.00(2) 2_655 . ? N3 Mn1 N2 89.83(11) 2_655 2_655 ? N3 Mn1 N2 90.17(11) . 2_655 ? N3 Mn1 N2 90.17(11) 2_655 . ? N3 Mn1 N2 89.83(11) . . ? N2 Mn1 N2 180.0 2_655 . ? N3 Mn1 N1 94.70(10) 2_655 2_655 ? N3 Mn1 N1 85.30(10) . 2_655 ? N2 Mn1 N1 89.10(10) 2_655 2_655 ? N2 Mn1 N1 90.90(10) . 2_655 ? N3 Mn1 N1 85.30(10) 2_655 . ? N3 Mn1 N1 94.70(10) . . ? N2 Mn1 N1 90.90(10) 2_655 . ? N2 Mn1 N1 89.10(10) . . ? N1 Mn1 N1 180.00(13) 2_655 . ? O5 Cl1 O6 109.4(4) . . ? O5 Cl1 O3 111.0(3) . . ? O6 Cl1 O3 107.8(4) . . ? O5 Cl1 O4 109.1(4) . . ? O6 Cl1 O4 108.6(4) . . ? O3 Cl1 O4 110.9(3) . . ? C29 P1 C41 110.62(19) . . ? C29 P1 C35 110.1(2) . . ? C41 P1 C35 106.3(2) . . ? C29 P1 C53 108.4(2) . . ? C41 P1 C53 111.0(2) . . ? C35 P1 C53 110.4(3) . . ? C3 O1 Ru1 122.3(2) . . ? C5 O2 Ru1 123.1(2) . . ? C54 O7 H7 109.5 . . ? C1 N1 Mn1 153.0(2) . . ? C10 N2 C7 106.5(3) . . ? C10 N2 Mn1 127.1(2) . . ? C7 N2 Mn1 126.4(2) . . ? C21 N3 C18 106.6(3) . . ? C21 N3 Mn1 126.7(2) . . ? C18 N3 Mn1 126.6(2) . . ? N1 C1 Ru1 177.9(3) . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 125.7(4) . . ? O1 C3 C2 113.7(4) . . ? C4 C3 C2 120.6(4) . . ? C3 C4 C5 126.2(4) . . ? C3 C4 H4 116.9 . . ? C5 C4 H4 116.9 . . ? O2 C5 C4 125.5(3) . . ? O2 C5 C6 115.3(4) . . ? C4 C5 C6 119.2(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C22 126.1(3) . 2_655 ? N2 C7 C8 109.0(3) . . ? C22 C7 C8 124.9(3) 2_655 . ? C9 C8 C7 108.0(3) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? C8 C9 C10 106.8(3) . . ? C8 C9 H9 126.6 . . ? C10 C9 H9 126.6 . . ? N2 C10 C11 125.7(3) . . ? N2 C10 C9 109.7(3) . . ? C11 C10 C9 124.6(3) . . ? C18 C11 C10 124.4(3) . . ? C18 C11 C12 117.3(3) . . ? C10 C11 C12 118.3(3) . . ? C13 C12 C17 119.0(4) . . ? C13 C12 C11 120.6(4) . . ? C17 C12 C11 120.3(4) . . ? C12 C13 C14 121.6(5) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 119.7(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 120.6(6) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 118.6(5) . . ? C12 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? N3 C18 C11 126.3(3) . . ? N3 C18 C19 109.0(3) . . ? C11 C18 C19 124.7(3) . . ? C20 C19 C18 107.3(3) . . ? C20 C19 H19 126.3 . . ? C18 C19 H19 126.3 . . ? C19 C20 C21 107.6(3) . . ? C19 C20 H20 126.2 . . ? C21 C20 H20 126.2 . . ? N3 C21 C22 126.3(3) . . ? N3 C21 C20 109.5(3) . . ? C22 C21 C20 124.2(3) . . ? C21 C22 C7 124.2(3) . 2_655 ? C21 C22 C23 117.7(3) . . ? C7 C22 C23 118.1(3) 2_655 . ? C24 C23 C28 119.0(3) . . ? C24 C23 C22 121.6(3) . . ? C28 C23 C22 119.4(3) . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.3(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 120.2(4) . . ? C23 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C34 C29 C30 121.0(4) . . ? C34 C29 P1 119.6(3) . . ? C30 C29 P1 119.3(3) . . ? C31 C30 C29 118.9(4) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C32 C31 C30 120.3(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 120.4(4) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 118.9(4) . . ? C33 C34 H34 120.5 . . ? C29 C34 H34 120.5 . . ? C36 C35 C40 122.9(6) . . ? C36 C35 P1 119.6(6) . . ? C40 C35 P1 117.4(4) . . ? C35 C36 C37 115.1(10) . . ? C35 C36 H36 122.4 . . ? C37 C36 H36 122.4 . . ? C38 C37 C36 122.0(12) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C39 124.7(12) . . ? C37 C38 H38 117.6 . . ? C39 C38 H38 117.6 . . ? C38 C39 C40 115.3(12) . . ? C38 C39 H39 122.4 . . ? C40 C39 H39 122.4 . . ? C39 C40 C35 119.4(9) . . ? C39 C40 H40 120.3 . . ? C35 C40 H40 120.3 . . ? C42 C41 C46 120.7(4) . . ? C42 C41 P1 120.5(3) . . ? C46 C41 P1 118.4(4) . . ? C41 C42 C43 119.2(5) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 120.4(5) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 121.5(5) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C44 C45 C46 120.3(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 118.0(5) . . ? C41 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? C48 C47 C52 118.8(6) . . ? C48 C47 C53 121.0(5) . . ? C52 C47 C53 120.1(6) . . ? C47 C48 C49 121.3(7) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C50 C49 C48 119.7(8) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 120.2(9) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C52 120.5(8) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C47 119.6(8) . . ? C51 C52 H52 120.2 . . ? C47 C52 H52 120.2 . . ? C47 C53 P1 113.0(3) . . ? C47 C53 H53A 109.0 . . ? P1 C53 H53A 109.0 . . ? C47 C53 H53B 109.0 . . ? P1 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? O7 C54 H54A 109.5 . . ? O7 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O7 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.404 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.060