Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Neil Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol BRISTOL BS8 1TS UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_section_title ; Metal-metal charge transfer and solvatochromism in cyanomanganese carbonyl complexes of ruthenium and osmium ; loop_ _publ_author_name 'Neil Connelly' 'Chris Adams' 'Nicholas J. Goodwin' 'Owen D. Hayward' 'A. Orpen' 'Andrew J. Wood' data_8 _database_code_depnum_ccdc_archive 'CCDC 603279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H63 F18 Mn N7 O4.50 P4 Ru' _chemical_formula_weight 1299.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 9.972(2) _cell_length_b 13.579(2) _cell_length_c 20.985(5) _cell_angle_alpha 81.267(11) _cell_angle_beta 81.481(19) _cell_angle_gamma 76.760(11) _cell_volume 2715.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 117 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1322 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 27761 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12195 _reflns_number_gt 7056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0868P)^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 12195 _refine_ls_number_parameters 670 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1793 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.009 _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 0.75539(4) 0.40314(3) 0.16907(2) 0.02905(13) Uani 1 1 d . . . Mn1 Mn 0.36038(8) 0.52005(6) 0.34140(4) 0.0294(2) Uani 1 1 d . A . P1 P 0.39939(14) 0.68214(10) 0.31560(7) 0.0289(3) Uani 1 1 d . . . P2 P 0.23393(16) 0.47938(12) 0.06712(8) 0.0397(4) Uani 1 1 d . . . P3 P 0.7405(2) 0.09914(12) 0.06872(9) 0.0508(5) Uani 1 1 d . . . P4 P 0.0718(2) 0.71370(14) 0.60551(10) 0.0619(5) Uani 1 1 d D . . O1 O 0.1281(4) 0.5453(3) 0.2735(2) 0.0545(12) Uani 1 1 d . . . N1 N 0.6027(5) 0.4499(3) 0.2383(2) 0.0319(10) Uani 1 1 d . . . N2 N 0.7206(5) 0.5543(3) 0.1212(2) 0.0440(12) Uani 1 1 d . . . H2A H 0.7423 0.5530 0.0777 0.066 Uiso 1 1 calc R . . H2B H 0.7747 0.5899 0.1356 0.066 Uiso 1 1 calc R . . H2C H 0.6297 0.5849 0.1300 0.066 Uiso 1 1 calc R . . N3 N 0.9076(5) 0.4342(4) 0.2193(2) 0.0467(13) Uani 1 1 d . . . H3A H 0.9102 0.5015 0.2104 0.070 Uiso 1 1 calc R . . H3B H 0.9921 0.3960 0.2063 0.070 Uiso 1 1 calc R . . H3C H 0.8859 0.4185 0.2628 0.070 Uiso 1 1 calc R . . N4 N 0.9111(4) 0.3535(3) 0.0947(2) 0.0364(11) Uani 1 1 d . . . H4A H 0.9809 0.3065 0.1123 0.055 Uiso 1 1 calc R . . H4B H 0.9451 0.4076 0.0730 0.055 Uiso 1 1 calc R . . H4C H 0.8748 0.3248 0.0666 0.055 Uiso 1 1 calc R . . N5 N 0.7872(5) 0.2543(3) 0.2185(2) 0.0392(11) Uani 1 1 d . . . H5A H 0.8113 0.2550 0.2586 0.059 Uiso 1 1 calc R . . H5B H 0.8564 0.2129 0.1956 0.059 Uiso 1 1 calc R . . H5C H 0.7077 0.2306 0.2227 0.059 Uiso 1 1 calc R . . N6 N 0.6076(5) 0.3728(4) 0.1174(2) 0.0412(12) Uani 1 1 d . . . H6A H 0.6162 0.3042 0.1197 0.062 Uiso 1 1 calc R . . H6B H 0.6215 0.3997 0.0751 0.062 Uiso 1 1 calc R . . H6C H 0.5209 0.4013 0.1349 0.062 Uiso 1 1 calc R . . N7 N 0.2292(5) 0.5371(3) 0.2988(2) 0.0360(11) Uani 1 1 d . . . C1 C 0.5104(6) 0.4788(4) 0.2764(3) 0.0301(12) Uani 1 1 d . . . C2 C 0.4853(7) 0.4657(5) 0.4196(3) 0.0456(15) Uani 1 1 d . A . H2 H 0.5766 0.4766 0.4178 0.055 Uiso 1 1 calc R . . C3 C 0.3628(7) 0.5311(5) 0.4424(3) 0.0445(15) Uani 1 1 d . A . H3 H 0.3570 0.5936 0.4588 0.053 Uiso 1 1 calc R . . C4 C 0.2486(7) 0.4877(5) 0.4367(3) 0.0509(17) Uani 1 1 d . . . C5 C 0.3041(8) 0.3957(5) 0.4095(3) 0.0547(18) Uani 1 1 d . A . H5 H 0.2513 0.3513 0.3994 0.066 Uiso 1 1 calc R . . C6 C 0.4501(8) 0.3800(5) 0.3996(3) 0.0552(18) Uani 1 1 d . . . C7 C 0.5266(14) 0.2849(11) 0.3862(7) 0.060(4) Uani 0.50 1 d P A 1 H7A H 0.5247 0.2363 0.4257 0.090 Uiso 0.50 1 calc PR A 1 H7B H 0.6228 0.2896 0.3704 0.090 Uiso 0.50 1 calc PR A 1 H7C H 0.4864 0.2615 0.3528 0.090 Uiso 0.50 1 calc PR A 1 C7' C 0.1101(11) 0.5154(9) 0.4598(6) 0.041(3) Uani 0.50 1 d P B 2 H7'1 H 0.0821 0.5898 0.4561 0.061 Uiso 0.50 1 calc PR B 2 H7'2 H 0.0955 0.4870 0.5055 0.061 Uiso 0.50 1 calc PR B 2 H7'3 H 0.0544 0.4889 0.4344 0.061 Uiso 0.50 1 calc PR B 2 C8 C 0.4465(5) 0.7213(4) 0.2296(3) 0.0307(12) Uani 1 1 d . . . C9 C 0.3815(6) 0.6917(4) 0.1830(3) 0.0358(13) Uani 1 1 d . . . H9 H 0.3219 0.6449 0.1960 0.043 Uiso 1 1 calc R . . C10 C 0.4035(6) 0.7302(5) 0.1179(3) 0.0430(15) Uani 1 1 d . . . H10 H 0.3577 0.7105 0.0868 0.052 Uiso 1 1 calc R . . C11 C 0.4915(6) 0.7966(5) 0.0983(3) 0.0475(16) Uani 1 1 d . . . H11 H 0.5059 0.8229 0.0538 0.057 Uiso 1 1 calc R . . C12 C 0.5590(6) 0.8254(4) 0.1435(3) 0.0447(15) Uani 1 1 d . . . H12 H 0.6201 0.8709 0.1298 0.054 Uiso 1 1 calc R . . C13 C 0.5373(6) 0.7877(4) 0.2082(3) 0.0416(14) Uani 1 1 d . . . H13 H 0.5847 0.8072 0.2388 0.050 Uiso 1 1 calc R . . C14 C 0.5412(6) 0.6986(4) 0.3555(3) 0.0348(13) Uani 1 1 d . . . C15 C 0.6741(6) 0.6451(5) 0.3377(3) 0.0528(18) Uani 1 1 d . . . H15 H 0.6910 0.6060 0.3024 0.063 Uiso 1 1 calc R . . C16 C 0.7842(7) 0.6480(6) 0.3716(4) 0.061(2) Uani 1 1 d . . . H16 H 0.8744 0.6092 0.3602 0.073 Uiso 1 1 calc R . . C17 C 0.7604(7) 0.7079(5) 0.4214(4) 0.0576(18) Uani 1 1 d . . . H17 H 0.8344 0.7114 0.4441 0.069 Uiso 1 1 calc R . . C18 C 0.6303(8) 0.7616(6) 0.4377(4) 0.062(2) Uani 1 1 d . . . H18 H 0.6145 0.8027 0.4720 0.075 Uiso 1 1 calc R . . C19 C 0.5193(7) 0.7582(5) 0.4053(3) 0.0462(15) Uani 1 1 d . . . H19 H 0.4292 0.7965 0.4175 0.055 Uiso 1 1 calc R . . C20 C 0.2552(5) 0.7874(4) 0.3371(3) 0.0318(12) Uani 1 1 d . . . C21 C 0.2492(8) 0.8847(5) 0.3071(4) 0.081(3) Uani 1 1 d . . . H21 H 0.3201 0.8981 0.2735 0.097 Uiso 1 1 calc R . . C22 C 0.1417(8) 0.9645(5) 0.3247(4) 0.079(3) Uani 1 1 d . . . H22 H 0.1370 1.0309 0.3017 0.095 Uiso 1 1 calc R . . C23 C 0.0443(7) 0.9475(5) 0.3743(4) 0.061(2) Uani 1 1 d . . . H23 H -0.0283 1.0020 0.3873 0.073 Uiso 1 1 calc R . . C24 C 0.0512(8) 0.8525(5) 0.4055(4) 0.076(3) Uani 1 1 d . . . H24 H -0.0162 0.8405 0.4411 0.091 Uiso 1 1 calc R . . C25 C 0.1544(7) 0.7726(5) 0.3864(4) 0.070(2) Uani 1 1 d . . . H25 H 0.1550 0.7059 0.4081 0.083 Uiso 1 1 calc R . . C31 C 0.9692(11) 0.7915(6) 0.2134(6) 0.124(5) Uani 1 1 d . . . H31A H 1.0663 0.7972 0.2024 0.185 Uiso 1 1 calc R . . H31B H 0.9569 0.7542 0.2570 0.185 Uiso 1 1 calc R . . H31C H 0.9094 0.8598 0.2126 0.185 Uiso 1 1 calc R . . C32 C 0.9306(7) 0.7350(5) 0.1647(5) 0.069(2) Uani 1 1 d . . . C33 C 0.9614(9) 0.7681(6) 0.0959(5) 0.106(4) Uani 1 1 d . . . H33A H 1.0621 0.7552 0.0840 0.158 Uiso 1 1 calc R . . H33B H 0.9223 0.8411 0.0868 0.158 Uiso 1 1 calc R . . H33C H 0.9205 0.7301 0.0704 0.158 Uiso 1 1 calc R . . C34 C 0.1549(11) -0.0011(6) 0.1410(5) 0.109(4) Uani 1 1 d . . . H34A H 0.2434 -0.0400 0.1550 0.163 Uiso 1 1 calc R . . H34B H 0.1377 -0.0264 0.1023 0.163 Uiso 1 1 calc R . . H34C H 0.0798 -0.0091 0.1759 0.163 Uiso 1 1 calc R . . C35 C 0.1606(7) 0.1094(5) 0.1254(4) 0.0569(19) Uani 1 1 d . . . C36 C 0.2532(11) 0.1369(8) 0.0686(6) 0.137(5) Uani 1 1 d . . . H36A H 0.2494 0.0970 0.0340 0.205 Uiso 1 1 calc R . . H36B H 0.3482 0.1226 0.0799 0.205 Uiso 1 1 calc R . . H36C H 0.2244 0.2097 0.0536 0.205 Uiso 1 1 calc R . . C37 C 0.7233(19) 0.0092(9) 0.2978(7) 0.189(8) Uani 1 1 d . . . H37A H 0.7428 0.0515 0.3278 0.284 Uiso 1 1 calc R . . H37B H 0.7775 0.0210 0.2555 0.284 Uiso 1 1 calc R . . H37C H 0.7487 -0.0629 0.3152 0.284 Uiso 1 1 calc R . . C38 C 0.5860(19) 0.0340(14) 0.2907(13) 0.318(18) Uani 1 1 d . . . H38A H 0.5315 0.0140 0.3321 0.381 Uiso 1 1 calc R . . H38B H 0.5676 -0.0033 0.2570 0.381 Uiso 1 1 calc R . . C39 C 0.4083(14) 0.1536(10) 0.2656(8) 0.151(5) Uani 1 1 d . . . H39A H 0.3599 0.1314 0.3082 0.181 Uiso 1 1 calc R . . H39B H 0.4009 0.1073 0.2347 0.181 Uiso 1 1 calc R . . C40 C 0.3389(11) 0.2563(9) 0.2431(5) 0.113(4) Uani 1 1 d . . . H40A H 0.2428 0.2568 0.2375 0.170 Uiso 1 1 calc R . . H40B H 0.3875 0.2797 0.2014 0.170 Uiso 1 1 calc R . . H40C H 0.3393 0.3019 0.2750 0.170 Uiso 1 1 calc R . . C41 C 0.2707(18) -0.0101(14) 0.4944(9) 0.062(5) Uiso 0.50 1 d P C 1 H41A H 0.1990 0.0062 0.4648 0.093 Uiso 0.50 1 calc PR C 1 H41B H 0.2373 0.0263 0.5325 0.093 Uiso 0.50 1 calc PR C 1 H41C H 0.2914 -0.0836 0.5082 0.093 Uiso 0.50 1 calc PR C 1 C42 C 0.4069(17) 0.0238(13) 0.4581(8) 0.075(5) Uiso 0.50 1 d P C 1 H42A H 0.4416 -0.0124 0.4194 0.090 Uiso 0.50 1 calc PR C 1 H42B H 0.3874 0.0980 0.4439 0.090 Uiso 0.50 1 calc PR C 1 C42' C 0.363(2) -0.0160(16) 0.5239(11) 0.102(6) Uiso 0.50 1 d P C 2 H42C H 0.3272 0.0192 0.5630 0.123 Uiso 0.50 1 calc PR C 2 H42D H 0.3662 -0.0897 0.5364 0.123 Uiso 0.50 1 calc PR C 2 C41' C 0.270(2) 0.0242(17) 0.4731(11) 0.091(7) Uiso 0.50 1 d P C 2 H41D H 0.1762 0.0138 0.4897 0.137 Uiso 0.50 1 calc PR C 2 H41E H 0.3045 -0.0117 0.4349 0.137 Uiso 0.50 1 calc PR C 2 H41F H 0.2667 0.0972 0.4610 0.137 Uiso 0.50 1 calc PR C 2 O11 O 0.8722(5) 0.6638(3) 0.1845(3) 0.0656(14) Uani 1 1 d . . . O12 O 0.0864(4) 0.1738(3) 0.1575(2) 0.0540(12) Uani 1 1 d . . . O13 O 0.5434(8) 0.1447(7) 0.2718(4) 0.135(3) Uani 1 1 d . . . O14 O 0.5000 0.0000 0.5000 0.072(2) Uiso 1 2 d S . . F1 F 0.2335(5) 0.5868(3) 0.0250(2) 0.0860(14) Uani 1 1 d . . . F2 F 0.0933(4) 0.5250(4) 0.1069(2) 0.0894(15) Uani 1 1 d . . . F3 F 0.1465(4) 0.4519(3) 0.01580(18) 0.0645(11) Uani 1 1 d . . . F4 F 0.2295(6) 0.3744(3) 0.1081(2) 0.1039(19) Uani 1 1 d . . . F5 F 0.3714(4) 0.4351(4) 0.0244(2) 0.1024(19) Uani 1 1 d . . . F6 F 0.3208(4) 0.5077(3) 0.11645(19) 0.0600(10) Uani 1 1 d . . . F7 F 0.6940(9) 0.1996(4) 0.0250(3) 0.157(3) Uani 1 1 d . . . F8 F 0.8459(9) 0.0550(5) 0.0168(4) 0.206(4) Uani 1 1 d . . . F9 F 0.6300(6) 0.0488(4) 0.0471(3) 0.125(2) Uani 1 1 d . . . F10 F 0.7781(7) 0.0002(4) 0.1165(3) 0.128(2) Uani 1 1 d . . . F11 F 0.6247(7) 0.1466(4) 0.1231(3) 0.136(2) Uani 1 1 d . . . F12 F 0.8368(6) 0.1535(4) 0.0947(4) 0.135(2) Uani 1 1 d . . . F17 F 0.1928(6) 0.6540(7) 0.6438(4) 0.204(5) Uani 1 1 d D . . F16 F -0.0015(11) 0.6280(7) 0.6388(4) 0.217(5) Uani 1 1 d D . . F15 F 0.0170(11) 0.7582(6) 0.6686(3) 0.200(4) Uani 1 1 d D . . F14 F -0.0475(8) 0.7522(9) 0.5683(5) 0.281(7) Uani 1 1 d D . . F13 F 0.1194(11) 0.8099(6) 0.5810(5) 0.215(4) Uani 1 1 d D . . F18 F 0.1701(11) 0.6773(8) 0.5487(3) 0.264(7) Uani 1 1 d 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 0.0291(2) 0.0276(2) 0.0292(2) -0.00788(18) 0.00015(18) -0.00295(17) Mn1 0.0301(4) 0.0335(4) 0.0242(4) -0.0052(3) -0.0013(3) -0.0059(3) P1 0.0276(7) 0.0321(7) 0.0273(7) -0.0098(6) 0.0000(6) -0.0051(6) P2 0.0347(8) 0.0473(9) 0.0359(9) -0.0063(7) -0.0026(7) -0.0063(7) P3 0.0728(13) 0.0348(9) 0.0475(11) -0.0119(8) -0.0109(9) -0.0101(8) P4 0.0782(14) 0.0505(11) 0.0522(12) -0.0071(9) -0.0002(10) -0.0084(10) O1 0.041(3) 0.069(3) 0.056(3) 0.002(2) -0.015(2) -0.017(2) N1 0.034(2) 0.031(2) 0.029(2) -0.009(2) -0.001(2) -0.0012(19) N2 0.059(3) 0.034(3) 0.037(3) -0.006(2) -0.002(2) -0.004(2) N3 0.045(3) 0.053(3) 0.045(3) -0.013(3) -0.004(2) -0.013(2) N4 0.032(3) 0.037(3) 0.038(3) -0.006(2) 0.003(2) -0.004(2) N5 0.044(3) 0.032(2) 0.037(3) -0.004(2) 0.003(2) -0.003(2) N6 0.031(3) 0.050(3) 0.045(3) -0.020(2) -0.003(2) -0.005(2) N7 0.031(3) 0.042(3) 0.034(3) -0.001(2) 0.001(2) -0.011(2) C1 0.036(3) 0.027(3) 0.028(3) -0.001(2) -0.011(2) -0.006(2) C2 0.046(4) 0.061(4) 0.030(3) -0.001(3) -0.010(3) -0.011(3) C3 0.056(4) 0.058(4) 0.022(3) -0.002(3) -0.006(3) -0.018(3) C4 0.053(4) 0.068(4) 0.028(3) 0.010(3) 0.002(3) -0.020(3) C5 0.077(5) 0.051(4) 0.039(4) 0.013(3) -0.014(4) -0.027(4) C6 0.068(5) 0.057(4) 0.035(4) 0.004(3) -0.018(3) 0.000(4) C7 0.053(8) 0.072(10) 0.042(8) -0.002(7) 0.006(7) 0.005(7) C7' 0.027(6) 0.051(7) 0.043(7) -0.009(6) 0.003(5) -0.006(5) C8 0.031(3) 0.033(3) 0.028(3) -0.008(2) 0.005(2) -0.006(2) C9 0.038(3) 0.037(3) 0.032(3) -0.005(3) -0.005(3) -0.008(2) C10 0.047(4) 0.051(4) 0.027(3) -0.001(3) -0.002(3) -0.004(3) C11 0.047(4) 0.051(4) 0.037(4) 0.009(3) 0.001(3) -0.008(3) C12 0.046(4) 0.037(3) 0.048(4) 0.000(3) 0.010(3) -0.016(3) C13 0.041(3) 0.038(3) 0.048(4) -0.010(3) 0.002(3) -0.013(3) C14 0.037(3) 0.038(3) 0.032(3) -0.011(2) -0.003(2) -0.010(2) C15 0.038(4) 0.063(4) 0.063(5) -0.035(4) -0.008(3) -0.002(3) C16 0.032(3) 0.074(5) 0.077(5) -0.021(4) -0.011(3) -0.005(3) C17 0.050(4) 0.064(4) 0.067(5) -0.008(4) -0.024(4) -0.019(4) C18 0.067(5) 0.073(5) 0.062(5) -0.033(4) -0.013(4) -0.027(4) C19 0.046(4) 0.052(4) 0.046(4) -0.019(3) -0.005(3) -0.012(3) C20 0.031(3) 0.030(3) 0.032(3) -0.008(2) 0.001(2) -0.002(2) C21 0.063(5) 0.059(5) 0.086(6) 0.010(4) 0.041(4) 0.011(4) C22 0.075(6) 0.047(4) 0.089(6) 0.005(4) 0.023(5) 0.011(4) C23 0.038(4) 0.055(4) 0.081(6) -0.018(4) 0.006(4) 0.006(3) C24 0.057(5) 0.048(4) 0.109(7) -0.015(4) 0.037(4) -0.007(4) C25 0.054(4) 0.039(4) 0.100(6) -0.004(4) 0.027(4) -0.005(3) C31 0.127(9) 0.057(5) 0.210(13) -0.010(7) -0.085(9) -0.029(6) C32 0.036(4) 0.036(4) 0.126(8) -0.008(4) -0.003(4) 0.006(3) C33 0.087(7) 0.044(5) 0.160(11) -0.010(5) 0.045(7) 0.000(4) C34 0.144(9) 0.046(5) 0.117(9) -0.003(5) 0.000(7) 0.005(5) C35 0.045(4) 0.048(4) 0.082(5) -0.023(4) -0.019(4) 0.000(3) C36 0.138(9) 0.109(8) 0.166(11) -0.086(8) 0.100(9) -0.061(7) C37 0.28(2) 0.072(8) 0.166(14) 0.018(8) -0.024(14) 0.040(10) C38 0.160(17) 0.175(17) 0.50(4) 0.18(2) -0.02(2) 0.038(13) C39 0.118(11) 0.131(11) 0.182(15) 0.017(10) 0.001(10) -0.015(9) C40 0.110(9) 0.142(10) 0.088(8) 0.011(7) -0.036(7) -0.028(7) O11 0.050(3) 0.050(3) 0.097(4) -0.020(3) 0.009(3) -0.015(2) O12 0.045(3) 0.047(3) 0.064(3) -0.016(2) -0.003(2) 0.006(2) O13 0.070(5) 0.176(8) 0.119(6) 0.045(5) 0.011(4) -0.001(5) F1 0.113(4) 0.084(3) 0.066(3) 0.026(2) -0.024(3) -0.046(3) F2 0.055(3) 0.120(4) 0.085(3) -0.034(3) 0.025(2) -0.007(3) F3 0.053(2) 0.104(3) 0.046(2) -0.007(2) -0.0099(19) -0.036(2) F4 0.186(6) 0.056(3) 0.086(4) 0.022(2) -0.075(4) -0.040(3) F5 0.039(2) 0.179(5) 0.098(4) -0.095(4) -0.007(2) 0.009(3) F6 0.069(3) 0.062(2) 0.057(2) -0.023(2) -0.016(2) -0.013(2) F7 0.298(9) 0.081(4) 0.080(4) 0.021(3) -0.062(5) -0.013(5) F8 0.248(9) 0.147(6) 0.225(8) -0.130(6) 0.165(7) -0.097(6) F9 0.135(5) 0.127(5) 0.140(6) -0.024(4) -0.050(4) -0.057(4) F10 0.160(6) 0.056(3) 0.165(6) 0.020(3) -0.073(5) -0.006(3) F11 0.156(6) 0.086(4) 0.141(6) -0.028(4) 0.054(5) -0.015(4) F12 0.131(5) 0.113(4) 0.198(7) -0.068(4) -0.054(5) -0.049(4) F17 0.069(4) 0.312(10) 0.140(6) 0.099(7) 0.017(4) 0.043(5) F16 0.300(11) 0.199(8) 0.204(9) 0.104(7) -0.137(8) -0.177(8) F15 0.321(11) 0.143(6) 0.101(5) -0.035(5) -0.043(6) 0.047(7) F14 0.163(7) 0.445(15) 0.243(10) 0.242(11) -0.149(8) -0.187(9) F13 0.298(11) 0.138(6) 0.228(10) -0.007(6) 0.039(9) -0.140(7) F18 0.331(12) 0.291(11) 0.066(4) -0.071(6) -0.020(6) 0.178(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.003(4) . ? Ru1 N6 2.099(4) . ? Ru1 N4 2.103(4) . ? Ru1 N5 2.105(4) . ? Ru1 N2 2.120(4) . ? Ru1 N3 2.121(5) . ? Mn1 N7 1.646(5) . ? Mn1 C1 1.913(6) . ? Mn1 C2 2.147(6) . ? Mn1 C3 2.152(6) . ? Mn1 C5 2.161(6) . ? Mn1 C4 2.175(6) . ? Mn1 C6 2.180(6) . ? Mn1 P1 2.2928(16) . ? P1 C14 1.817(6) . ? P1 C8 1.826(5) . ? P1 C20 1.838(5) . ? P2 F4 1.555(4) . ? P2 F2 1.569(4) . ? P2 F5 1.570(4) . ? P2 F6 1.584(4) . ? P2 F1 1.586(4) . ? P2 F3 1.615(4) . ? P3 F8 1.490(6) . ? P3 F12 1.538(5) . ? P3 F7 1.541(5) . ? P3 F10 1.557(5) . ? P3 F9 1.573(5) . ? P3 F11 1.594(6) . ? P4 F14 1.471(6) . ? P4 F13 1.484(6) . ? P4 F18 1.495(6) . ? P4 F15 1.514(6) . ? P4 F16 1.539(6) . ? P4 F17 1.550(6) . ? O1 N7 1.183(6) . ? N1 C1 1.162(7) . ? C2 C3 1.404(8) . ? C2 C6 1.425(9) . ? C3 C4 1.424(9) . ? C4 C7' 1.380(11) . ? C4 C5 1.413(9) . ? C5 C6 1.411(9) . ? C6 C7 1.388(14) . ? C8 C9 1.402(7) . ? C8 C13 1.402(8) . ? C9 C10 1.391(8) . ? C10 C11 1.377(8) . ? C11 C12 1.387(9) . ? C12 C13 1.382(8) . ? C14 C19 1.379(7) . ? C14 C15 1.385(8) . ? C15 C16 1.403(8) . ? C16 C17 1.381(9) . ? C17 C18 1.357(9) . ? C18 C19 1.395(9) . ? C20 C25 1.357(8) . ? C20 C21 1.367(9) . ? C21 C22 1.389(9) . ? C22 C23 1.346(10) . ? C23 C24 1.346(10) . ? C24 C25 1.377(9) . ? C31 C32 1.507(12) . ? C32 O11 1.229(8) . ? C32 C33 1.456(12) . ? C34 C35 1.498(10) . ? C35 O12 1.225(7) . ? C35 C36 1.453(11) . ? C37 C38 1.36(2) . ? C38 O13 1.475(16) . ? C39 O13 1.349(13) . ? C39 C40 1.450(14) . ? C41 C42 1.58(2) . ? C42 O14 1.325(17) . ? C42' O14 1.44(2) . ? C42' C41' 1.48(3) . ? O14 C42 1.325(17) 2_656 ? O14 C42' 1.44(2) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N6 89.06(18) . . ? N1 Ru1 N4 178.24(18) . . ? N6 Ru1 N4 89.18(18) . . ? N1 Ru1 N5 90.26(17) . . ? N6 Ru1 N5 91.52(19) . . ? N4 Ru1 N5 89.90(17) . . ? N1 Ru1 N2 88.46(18) . . ? N6 Ru1 N2 88.8(2) . . ? N4 Ru1 N2 91.39(18) . . ? N5 Ru1 N2 178.68(18) . . ? N1 Ru1 N3 92.09(18) . . ? N6 Ru1 N3 178.7(2) . . ? N4 Ru1 N3 89.66(19) . . ? N5 Ru1 N3 89.0(2) . . ? N2 Ru1 N3 90.7(2) . . ? N7 Mn1 C1 99.6(2) . . ? N7 Mn1 C2 159.3(2) . . ? C1 Mn1 C2 93.5(2) . . ? N7 Mn1 C3 130.4(2) . . ? C1 Mn1 C3 129.9(2) . . ? C2 Mn1 C3 38.1(2) . . ? N7 Mn1 C5 96.1(2) . . ? C1 Mn1 C5 114.1(3) . . ? C2 Mn1 C5 63.7(3) . . ? C3 Mn1 C5 63.8(3) . . ? N7 Mn1 C4 97.5(2) . . ? C1 Mn1 C4 149.1(2) . . ? C2 Mn1 C4 64.0(2) . . ? C3 Mn1 C4 38.4(2) . . ? C5 Mn1 C4 38.0(2) . . ? N7 Mn1 C6 126.6(3) . . ? C1 Mn1 C6 85.2(2) . . ? C2 Mn1 C6 38.5(2) . . ? C3 Mn1 C6 64.1(2) . . ? C5 Mn1 C6 37.9(3) . . ? C4 Mn1 C6 63.9(3) . . ? N7 Mn1 P1 96.37(16) . . ? C1 Mn1 P1 87.61(16) . . ? C2 Mn1 P1 100.11(18) . . ? C3 Mn1 P1 89.61(18) . . ? C5 Mn1 P1 152.56(19) . . ? C4 Mn1 P1 115.87(19) . . ? C6 Mn1 P1 137.0(2) . . ? C14 P1 C8 104.8(3) . . ? C14 P1 C20 104.5(2) . . ? C8 P1 C20 101.9(2) . . ? C14 P1 Mn1 111.37(19) . . ? C8 P1 Mn1 115.84(17) . . ? C20 P1 Mn1 117.10(18) . . ? F4 P2 F2 88.5(3) . . ? F4 P2 F5 92.8(3) . . ? F2 P2 F5 177.4(3) . . ? F4 P2 F6 91.3(2) . . ? F2 P2 F6 91.7(2) . . ? F5 P2 F6 90.5(2) . . ? F4 P2 F1 178.2(3) . . ? F2 P2 F1 90.3(3) . . ? F5 P2 F1 88.3(3) . . ? F6 P2 F1 90.1(2) . . ? F4 P2 F3 89.7(2) . . ? F2 P2 F3 88.7(2) . . ? F5 P2 F3 89.0(2) . . ? F6 P2 F3 179.0(2) . . ? F1 P2 F3 89.0(2) . . ? F8 P3 F12 95.5(4) . . ? F8 P3 F7 93.1(5) . . ? F12 P3 F7 87.0(4) . . ? F8 P3 F10 91.0(5) . . ? F12 P3 F10 93.4(4) . . ? F7 P3 F10 175.8(4) . . ? F8 P3 F9 90.2(4) . . ? F12 P3 F9 174.2(4) . . ? F7 P3 F9 92.3(4) . . ? F10 P3 F9 87.0(3) . . ? F8 P3 F11 178.6(5) . . ? F12 P3 F11 85.7(4) . . ? F7 P3 F11 86.2(4) . . ? F10 P3 F11 89.7(4) . . ? F9 P3 F11 88.6(4) . . ? F14 P4 F13 88.4(6) . . ? F14 P4 F18 94.7(6) . . ? F13 P4 F18 81.8(6) . . ? F14 P4 F15 101.2(7) . . ? F13 P4 F15 87.4(5) . . ? F18 P4 F15 160.5(7) . . ? F14 P4 F16 87.4(4) . . ? F13 P4 F16 168.3(6) . . ? F18 P4 F16 109.4(7) . . ? F15 P4 F16 82.7(6) . . ? F14 P4 F17 169.7(7) . . ? F13 P4 F17 101.0(6) . . ? F18 P4 F17 82.7(4) . . ? F15 P4 F17 83.5(5) . . ? F16 P4 F17 84.1(5) . . ? C1 N1 Ru1 177.0(4) . . ? O1 N7 Mn1 173.6(4) . . ? N1 C1 Mn1 177.2(5) . . ? C3 C2 C6 108.7(6) . . ? C3 C2 Mn1 71.1(3) . . ? C6 C2 Mn1 72.0(3) . . ? C2 C3 C4 108.2(6) . . ? C2 C3 Mn1 70.8(3) . . ? C4 C3 Mn1 71.7(3) . . ? C7' C4 C5 122.1(8) . . ? C7' C4 C3 130.4(8) . . ? C5 C4 C3 106.9(6) . . ? C7' C4 Mn1 131.3(7) . . ? C5 C4 Mn1 70.5(4) . . ? C3 C4 Mn1 69.9(3) . . ? C6 C5 C4 109.5(6) . . ? C6 C5 Mn1 71.7(4) . . ? C4 C5 Mn1 71.5(4) . . ? C7 C6 C5 118.8(9) . . ? C7 C6 C2 133.2(9) . . ? C5 C6 C2 106.7(6) . . ? C7 C6 Mn1 135.0(7) . . ? C5 C6 Mn1 70.3(4) . . ? C2 C6 Mn1 69.5(4) . . ? C9 C8 C13 118.1(5) . . ? C9 C8 P1 119.5(4) . . ? C13 C8 P1 122.2(4) . . ? C10 C9 C8 120.5(5) . . ? C11 C10 C9 120.2(6) . . ? C10 C11 C12 120.2(6) . . ? C13 C12 C11 120.0(6) . . ? C12 C13 C8 121.0(6) . . ? C19 C14 C15 119.1(5) . . ? C19 C14 P1 122.0(4) . . ? C15 C14 P1 118.8(4) . . ? C14 C15 C16 120.6(6) . . ? C17 C16 C15 119.5(6) . . ? C18 C17 C16 119.5(6) . . ? C17 C18 C19 121.7(6) . . ? C14 C19 C18 119.5(6) . . ? C25 C20 C21 117.2(5) . . ? C25 C20 P1 121.0(5) . . ? C21 C20 P1 121.7(5) . . ? C20 C21 C22 121.4(7) . . ? C23 C22 C21 119.9(7) . . ? C22 C23 C24 119.2(6) . . ? C23 C24 C25 121.0(7) . . ? C20 C25 C24 121.3(7) . . ? O11 C32 C33 122.4(9) . . ? O11 C32 C31 118.9(9) . . ? C33 C32 C31 118.7(8) . . ? O12 C35 C36 121.7(7) . . ? O12 C35 C34 121.5(8) . . ? C36 C35 C34 116.8(7) . . ? C37 C38 O13 109.8(16) . . ? O13 C39 C40 113.7(11) . . ? O14 C42 C41 107.0(13) . . ? O14 C42' C41' 109.6(16) . . ? C39 O13 C38 101.0(11) . . ? C42 O14 C42 180.0(10) 2_656 . ? C42 O14 C42' 117.0(11) 2_656 . ? C42 O14 C42' 63.0(11) . . ? C42 O14 C42' 63.0(11) 2_656 2_656 ? C42 O14 C42' 117.0(11) . 2_656 ? C42' O14 C42' 180.0(17) . 2_656 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.116 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.108 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 603280' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H89 F18 Mn N6 O6 P7 Ru' _chemical_formula_weight 1789.24 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 11.596(8) _cell_length_b 14.943(8) _cell_length_c 25.237(15) _cell_angle_alpha 104.96(2) _cell_angle_beta 100.72(4) _cell_angle_gamma 98.59(3) _cell_volume 4060(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Green-red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1834 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743183 _exptl_absorpt_correction_T_max 0.894391 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21254 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.2091 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13903 _reflns_number_gt 6360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0314P)^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 13903 _refine_ls_number_parameters 970 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1837 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 0.82084(6) 0.79855(4) 0.34155(3) 0.02470(18) Uani 1 1 d . . . Mn1 Mn 0.60594(9) 0.80263(7) 0.14646(4) 0.0209(3) Uani 1 1 d . . . P1 P 0.50886(17) 0.64633(13) 0.10820(8) 0.0249(5) Uani 1 1 d . . . P2 P 0.73271(17) 0.72632(14) 0.10119(8) 0.0255(5) Uani 1 1 d . . . P3 P 0.47625(17) 0.87977(13) 0.19023(8) 0.0234(5) Uani 1 1 d . . . P4 P 0.69745(17) 0.95986(14) 0.18240(8) 0.0248(5) Uani 1 1 d . . . N1 N 0.7336(5) 0.7902(4) 0.2637(2) 0.0223(15) Uani 1 1 d . . . N2 N 0.9789(5) 0.7788(4) 0.3131(2) 0.0341(17) Uani 1 1 d . . . H2A H 0.9974 0.7236 0.3173 0.051 Uiso 1 1 calc R . . H2B H 1.0405 0.8279 0.3338 0.051 Uiso 1 1 calc R . . H2C H 0.9665 0.7766 0.2761 0.051 Uiso 1 1 calc R . . N3 N 0.9122(5) 0.8094(4) 0.4241(2) 0.0310(16) Uani 1 1 d . . . H3A H 0.9816 0.7883 0.4230 0.047 Uiso 1 1 calc R . . H3B H 0.8651 0.7736 0.4393 0.047 Uiso 1 1 calc R . . H3C H 0.9293 0.8710 0.4456 0.047 Uiso 1 1 calc R . . N4 N 0.6626(5) 0.8204(4) 0.3686(2) 0.0317(16) Uani 1 1 d . . . H4A H 0.6823 0.8623 0.4038 0.048 Uiso 1 1 calc R . . H4B H 0.6207 0.7643 0.3694 0.048 Uiso 1 1 calc R . . H4C H 0.6168 0.8439 0.3443 0.048 Uiso 1 1 calc R . . N5 N 0.8755(5) 0.9457(4) 0.3573(2) 0.0336(17) Uani 1 1 d . . . H5A H 0.9425 0.9680 0.3860 0.050 Uiso 1 1 calc R . . H5B H 0.8158 0.9748 0.3671 0.050 Uiso 1 1 calc R . . H5C H 0.8919 0.9579 0.3257 0.050 Uiso 1 1 calc R . . N6 N 0.7684(5) 0.6514(4) 0.3282(2) 0.0372(17) Uani 1 1 d . . . H6A H 0.7662 0.6401 0.3618 0.056 Uiso 1 1 calc R . . H6B H 0.8220 0.6213 0.3126 0.056 Uiso 1 1 calc R . . H6C H 0.6942 0.6296 0.3045 0.056 Uiso 1 1 calc R . . C1 C 0.6849(6) 0.7918(4) 0.2186(3) 0.0207(17) Uani 1 1 d . . . C2 C 0.5433(6) 0.8217(5) 0.0809(3) 0.0247(18) Uani 1 1 d . . . O1 O 0.5051(4) 0.8326(4) 0.0379(2) 0.0377(14) Uani 1 1 d . . . C3 C 0.6189(6) 0.6160(5) 0.0657(3) 0.0286(19) Uani 1 1 d . . . H3D H 0.6485 0.5591 0.0704 0.034 Uiso 1 1 calc R . . H3E H 0.5875 0.6083 0.0252 0.034 Uiso 1 1 calc R . . C4 C 0.5882(6) 0.9915(5) 0.2243(3) 0.0280(19) Uani 1 1 d . . . H4D H 0.5574 1.0473 0.2184 0.034 Uiso 1 1 calc R . . H4E H 0.6198 1.0013 0.2650 0.034 Uiso 1 1 calc R . . C11 C 0.6981(7) 1.0364(5) 0.1365(3) 0.0277(19) Uani 1 1 d . . . C12 C 0.8051(7) 1.0740(5) 0.1242(3) 0.038(2) Uani 1 1 d . . . H12 H 0.8796 1.0656 0.1433 0.045 Uiso 1 1 calc R . . C13 C 0.8034(7) 1.1236(6) 0.0844(3) 0.044(2) Uani 1 1 d . . . H13 H 0.8761 1.1480 0.0760 0.053 Uiso 1 1 calc R . . C14 C 0.6948(7) 1.1368(5) 0.0571(3) 0.037(2) Uani 1 1 d . . . H14 H 0.6927 1.1709 0.0300 0.044 Uiso 1 1 calc R . . C15 C 0.5899(7) 1.1004(5) 0.0692(3) 0.042(2) Uani 1 1 d . . . H15 H 0.5157 1.1094 0.0501 0.050 Uiso 1 1 calc R . . C16 C 0.5905(7) 1.0514(5) 0.1085(3) 0.037(2) Uani 1 1 d . . . H16 H 0.5172 1.0276 0.1166 0.044 Uiso 1 1 calc R . . C21 C 0.8436(6) 1.0081(5) 0.2305(3) 0.0262(18) Uani 1 1 d . . . C22 C 0.9346(7) 0.9590(6) 0.2256(3) 0.038(2) Uani 1 1 d . . . H22 H 0.9182 0.8980 0.1991 0.045 Uiso 1 1 calc R . . C23 C 1.0517(7) 0.9979(7) 0.2594(4) 0.049(3) Uani 1 1 d . . . H23 H 1.1140 0.9641 0.2544 0.059 Uiso 1 1 calc R . . C24 C 1.0764(8) 1.0844(7) 0.2995(4) 0.057(3) Uani 1 1 d . . . H24 H 1.1551 1.1103 0.3226 0.069 Uiso 1 1 calc R . . C25 C 0.9849(8) 1.1336(6) 0.3058(4) 0.056(3) Uani 1 1 d . . . H25 H 1.0003 1.1932 0.3336 0.067 Uiso 1 1 calc R . . C26 C 0.8699(7) 1.0950(6) 0.2710(3) 0.042(2) Uani 1 1 d . . . H26 H 0.8082 1.1295 0.2753 0.051 Uiso 1 1 calc R . . C31 C 0.3464(6) 0.9111(5) 0.1512(3) 0.0247(18) Uani 1 1 d . . . C32 C 0.3087(7) 0.9948(6) 0.1728(3) 0.042(2) Uani 1 1 d . . . H32 H 0.3536 1.0384 0.2076 0.050 Uiso 1 1 calc R . . C33 C 0.2067(7) 1.0149(6) 0.1440(4) 0.048(2) Uani 1 1 d . . . H33 H 0.1835 1.0731 0.1585 0.058 Uiso 1 1 calc R . . C34 C 0.1383(7) 0.9502(6) 0.0940(4) 0.045(2) Uani 1 1 d . . . H34 H 0.0675 0.9634 0.0746 0.054 Uiso 1 1 calc R . . C35 C 0.1728(6) 0.8670(5) 0.0727(3) 0.034(2) Uani 1 1 d . . . H35 H 0.1259 0.8228 0.0384 0.041 Uiso 1 1 calc R . . C36 C 0.2764(6) 0.8469(5) 0.1010(3) 0.0298(19) Uani 1 1 d . . . H36 H 0.2994 0.7889 0.0860 0.036 Uiso 1 1 calc R . . C41 C 0.4200(6) 0.8519(5) 0.2475(3) 0.0279(19) Uani 1 1 d . . . C42 C 0.3901(6) 0.7580(5) 0.2473(3) 0.0312(19) Uani 1 1 d . . . H42 H 0.3997 0.7095 0.2166 0.037 Uiso 1 1 calc R . . C43 C 0.3469(7) 0.7329(6) 0.2901(4) 0.041(2) Uani 1 1 d . . . H43 H 0.3300 0.6685 0.2896 0.050 Uiso 1 1 calc R . . C44 C 0.3289(7) 0.8031(7) 0.3336(4) 0.046(2) Uani 1 1 d . . . H44 H 0.2974 0.7865 0.3628 0.055 Uiso 1 1 calc R . . C45 C 0.3562(8) 0.8972(7) 0.3352(4) 0.056(3) Uani 1 1 d . . . H45 H 0.3446 0.9452 0.3656 0.067 Uiso 1 1 calc R . . C46 C 0.4005(7) 0.9209(6) 0.2922(3) 0.043(2) Uani 1 1 d . . . H46 H 0.4180 0.9855 0.2931 0.052 Uiso 1 1 calc R . . C51 C 0.7877(6) 0.7559(6) 0.0432(3) 0.033(2) Uani 1 1 d . . . C52 C 0.7858(6) 0.8434(6) 0.0355(3) 0.038(2) Uani 1 1 d . . . H52 H 0.7589 0.8894 0.0613 0.046 Uiso 1 1 calc R . . C53 C 0.8233(7) 0.8652(6) -0.0103(4) 0.051(2) Uani 1 1 d . . . H53 H 0.8217 0.9259 -0.0155 0.061 Uiso 1 1 calc R . . C54 C 0.8620(7) 0.7990(7) -0.0476(4) 0.055(3) Uani 1 1 d . . . H54 H 0.8877 0.8137 -0.0786 0.066 Uiso 1 1 calc R . . C55 C 0.8638(7) 0.7111(7) -0.0402(3) 0.049(2) Uani 1 1 d . . . H55 H 0.8903 0.6652 -0.0663 0.059 Uiso 1 1 calc R . . C56 C 0.8275(7) 0.6890(6) 0.0047(3) 0.042(2) Uani 1 1 d . . . H56 H 0.8295 0.6282 0.0096 0.051 Uiso 1 1 calc R . . C61 C 0.8620(6) 0.6906(5) 0.1371(3) 0.0291(19) Uani 1 1 d . . . C62 C 0.8479(7) 0.6176(5) 0.1619(3) 0.035(2) Uani 1 1 d . . . H62 H 0.7696 0.5840 0.1589 0.042 Uiso 1 1 calc R . . C63 C 0.9463(8) 0.5936(6) 0.1905(3) 0.043(2) Uani 1 1 d . . . H63 H 0.9356 0.5429 0.2066 0.052 Uiso 1 1 calc R . . C64 C 1.0597(7) 0.6432(6) 0.1958(3) 0.049(2) Uani 1 1 d . . . H64 H 1.1274 0.6271 0.2159 0.059 Uiso 1 1 calc R . . C65 C 1.0756(7) 0.7152(6) 0.1725(3) 0.045(2) Uani 1 1 d . . . H65 H 1.1544 0.7491 0.1765 0.054 Uiso 1 1 calc R . . C66 C 0.9787(7) 0.7395(5) 0.1432(3) 0.035(2) Uani 1 1 d . . . H66 H 0.9911 0.7898 0.1269 0.042 Uiso 1 1 calc R . . C71 C 0.3610(6) 0.6165(5) 0.0589(3) 0.0270(19) Uani 1 1 d . . . C72 C 0.3498(7) 0.6262(5) 0.0046(3) 0.037(2) Uani 1 1 d . . . H72 H 0.4193 0.6410 -0.0089 0.044 Uiso 1 1 calc R . . C73 C 0.2349(9) 0.6140(5) -0.0297(4) 0.053(3) Uani 1 1 d . . . H73 H 0.2262 0.6200 -0.0667 0.064 Uiso 1 1 calc R . . C74 C 0.1352(9) 0.5933(6) -0.0095(5) 0.067(3) Uani 1 1 d . . . H74 H 0.0576 0.5847 -0.0329 0.080 Uiso 1 1 calc R . . C75 C 0.1459(8) 0.5848(6) 0.0442(5) 0.069(3) Uani 1 1 d . . . H75 H 0.0763 0.5716 0.0580 0.082 Uiso 1 1 calc R . . C76 C 0.2584(7) 0.5956(5) 0.0778(4) 0.043(2) Uani 1 1 d . . . H76 H 0.2657 0.5886 0.1146 0.051 Uiso 1 1 calc R . . C81 C 0.4919(6) 0.5507(5) 0.1412(3) 0.0291(19) Uani 1 1 d . . . C86 C 0.5228(6) 0.5653(5) 0.1992(3) 0.036(2) Uani 1 1 d . . . H86 H 0.5549 0.6275 0.2239 0.043 Uiso 1 1 calc R . . C85 C 0.5070(7) 0.4894(6) 0.2212(4) 0.057(3) Uani 1 1 d . . . H85 H 0.5270 0.5001 0.2609 0.068 Uiso 1 1 calc R . . C84 C 0.4624(8) 0.3984(6) 0.1858(4) 0.065(3) Uani 1 1 d . . . H84 H 0.4502 0.3468 0.2010 0.078 Uiso 1 1 calc R . . C83 C 0.4357(8) 0.3830(6) 0.1282(4) 0.061(3) Uani 1 1 d . . . H83 H 0.4090 0.3202 0.1036 0.074 Uiso 1 1 calc R . . C82 C 0.4475(7) 0.4580(5) 0.1061(3) 0.048(2) Uani 1 1 d . . . H82 H 0.4250 0.4467 0.0664 0.058 Uiso 1 1 calc R . . C101 C 0.4562(8) 0.5152(6) 0.4028(4) 0.075(3) Uani 1 1 d . . . H10D H 0.3718 0.5050 0.4048 0.112 Uiso 1 1 calc R . . H10E H 0.5047 0.5018 0.4349 0.112 Uiso 1 1 calc R . . H10F H 0.4644 0.4729 0.3676 0.112 Uiso 1 1 calc R . . C102 C 0.4979(8) 0.6147(7) 0.4047(5) 0.054(3) Uani 1 1 d . . . C103 C 0.4995(9) 0.6890(7) 0.4568(4) 0.094(4) Uani 1 1 d . . . H10A H 0.5453 0.6755 0.4895 0.141 Uiso 1 1 calc R . . H10B H 0.4170 0.6898 0.4606 0.141 Uiso 1 1 calc R . . H10C H 0.5370 0.7508 0.4546 0.141 Uiso 1 1 calc R . . O11 O 0.5309(5) 0.6357(4) 0.3652(3) 0.0587(18) Uani 1 1 d . . . C111 C 0.8242(13) 0.3710(10) 0.3048(6) 0.170(7) Uani 1 1 d . . . H11D H 0.8968 0.3450 0.3039 0.254 Uiso 1 1 calc R . . H11E H 0.7618 0.3255 0.3110 0.254 Uiso 1 1 calc R . . H11F H 0.8424 0.4304 0.3355 0.254 Uiso 1 1 calc R . . C112 C 0.7808(11) 0.3895(9) 0.2500(7) 0.105(5) Uani 1 1 d . . . C113 C 0.7349(13) 0.3046(8) 0.1979(6) 0.158(6) Uani 1 1 d . . . H11A H 0.6727 0.2595 0.2045 0.237 Uiso 1 1 calc R . . H11B H 0.8013 0.2740 0.1898 0.237 Uiso 1 1 calc R . . H11C H 0.7010 0.3255 0.1657 0.237 Uiso 1 1 calc R . . O12 O 0.7793(6) 0.4704(5) 0.2451(3) 0.093(3) Uani 1 1 d . . . C121 C -0.1935(11) 0.5617(9) -0.2340(7) 0.165(7) Uani 1 1 d . . . H12D H -0.1654 0.5253 -0.2655 0.247 Uiso 1 1 calc R . . H12E H -0.2673 0.5808 -0.2487 0.247 Uiso 1 1 calc R . . H12F H -0.2096 0.5225 -0.2095 0.247 Uiso 1 1 calc R . . C122 C -0.1035(11) 0.6439(10) -0.2025(5) 0.082(4) Uani 1 1 d . . . C123 C -0.0978(12) 0.7226(10) -0.2219(7) 0.202(10) Uani 1 1 d . . . H12A H -0.1792 0.7297 -0.2366 0.304 Uiso 1 1 calc R . . H12B H -0.0544 0.7147 -0.2521 0.304 Uiso 1 1 calc R . . H12C H -0.0556 0.7792 -0.1908 0.304 Uiso 1 1 calc R . . O13 O -0.0431(9) 0.6417(8) -0.1583(4) 0.148(4) Uani 1 1 d . . . C131 C 0.5780(9) 1.1173(7) 0.4405(4) 0.085(4) Uani 1 1 d . . . H13D H 0.5320 1.1591 0.4257 0.127 Uiso 1 1 calc R . . H13E H 0.6105 1.1455 0.4812 0.127 Uiso 1 1 calc R . . H13F H 0.5253 1.0556 0.4333 0.127 Uiso 1 1 calc R . . C132 C 0.6784(9) 1.1047(7) 0.4119(4) 0.050(3) Uani 1 1 d . . . C133 C 0.7819(9) 1.1857(7) 0.4284(5) 0.096(4) Uani 1 1 d . . . H13A H 0.8195 1.2000 0.4685 0.144 Uiso 1 1 calc R . . H13B H 0.7540 1.2413 0.4213 0.144 Uiso 1 1 calc R . . H13C H 0.8406 1.1695 0.4060 0.144 Uiso 1 1 calc R . . O14 O 0.6762(5) 1.0313(4) 0.3778(3) 0.0622(19) Uani 1 1 d . . . C141 C 0.7839(10) 0.4994(8) 0.4618(5) 0.123(5) Uani 1 1 d . . . H14D H 0.7374 0.4737 0.4853 0.185 Uiso 1 1 calc R . . H14E H 0.8606 0.4788 0.4651 0.185 Uiso 1 1 calc R . . H14F H 0.7386 0.4763 0.4224 0.185 Uiso 1 1 calc R . . C142 C 0.8069(9) 0.6064(8) 0.4815(5) 0.072(3) Uani 1 1 d . . . C143 C 0.8644(14) 0.6538(9) 0.5400(5) 0.188(9) Uani 1 1 d . . . H14A H 0.9195 0.6169 0.5540 0.282 Uiso 1 1 calc R . . H14B H 0.8034 0.6598 0.5621 0.282 Uiso 1 1 calc R . . H14C H 0.9093 0.7169 0.5435 0.282 Uiso 1 1 calc R . . O15 O 0.7769(5) 0.6472(4) 0.4475(3) 0.0609(19) Uani 1 1 d . . . P5 P 1.2018(2) 1.03191(17) 0.45968(10) 0.0409(6) Uani 1 1 d . . . P6 P 0.4710(4) 1.2487(2) 0.31122(14) 0.1063(14) Uani 1 1 d . . . P7 P 1.1147(2) 0.6071(2) 0.39173(13) 0.0600(8) Uani 1 1 d . . . F1 F 1.1505(5) 0.9932(4) 0.5053(2) 0.096(2) Uani 1 1 d . . . F2 F 1.2685(4) 1.1269(4) 0.5080(2) 0.0773(17) Uani 1 1 d . . . F3 F 1.2495(5) 1.0733(4) 0.4149(2) 0.0712(16) Uani 1 1 d . . . F4 F 1.1317(4) 0.9382(3) 0.4107(2) 0.0781(17) Uani 1 1 d . . . F5 F 1.3144(4) 0.9868(4) 0.4692(2) 0.0703(16) Uani 1 1 d . . . F6 F 1.0861(4) 1.0770(4) 0.4499(2) 0.0750(17) Uani 1 1 d . . . F7 F 0.3589(8) 1.2919(5) 0.3136(5) 0.245(6) Uani 1 1 d . . . F8 F 0.4438(13) 1.2113(5) 0.2473(3) 0.304(8) Uani 1 1 d . . . F9 F 0.5896(10) 1.2061(6) 0.3113(4) 0.195(4) Uani 1 1 d . . . F10 F 0.4060(7) 1.1506(4) 0.3152(3) 0.144(3) Uani 1 1 d . . . F11 F 0.5387(8) 1.3459(4) 0.3061(3) 0.148(3) Uani 1 1 d . . . F12 F 0.5146(7) 1.2890(4) 0.3750(3) 0.128(3) Uani 1 1 d . . . F19 F 1.1983(6) 0.6210(5) 0.4502(3) 0.122(3) Uani 1 1 d . . . F20 F 1.0012(6) 0.6037(5) 0.4153(4) 0.156(4) Uani 1 1 d . . . F21 F 1.0997(5) 0.4968(4) 0.3776(3) 0.094(2) Uani 1 1 d . . . F22 F 1.0361(6) 0.5970(4) 0.3311(3) 0.120(3) Uani 1 1 d . . . F23 F 1.2276(5) 0.6144(4) 0.3665(3) 0.097(2) Uani 1 1 d . . . F24 F 1.1303(4) 0.7212(3) 0.4065(2) 0.0700(16) 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 0.0279(4) 0.0271(4) 0.0167(4) 0.0050(3) 0.0016(3) 0.0054(3) Mn1 0.0216(6) 0.0243(7) 0.0151(6) 0.0047(5) 0.0023(5) 0.0041(5) P1 0.0242(12) 0.0256(12) 0.0211(12) 0.0023(9) 0.0027(9) 0.0048(9) P2 0.0228(12) 0.0313(13) 0.0206(11) 0.0054(9) 0.0031(9) 0.0064(10) P3 0.0258(12) 0.0237(12) 0.0196(11) 0.0047(9) 0.0055(9) 0.0048(9) P4 0.0233(12) 0.0274(12) 0.0212(12) 0.0086(9) 0.0004(9) 0.0011(9) N1 0.023(4) 0.024(4) 0.019(4) 0.007(3) 0.004(3) 0.005(3) N2 0.041(4) 0.047(4) 0.016(4) 0.010(3) 0.008(3) 0.013(3) N3 0.040(4) 0.036(4) 0.022(4) 0.013(3) 0.011(3) 0.012(3) N4 0.030(4) 0.041(4) 0.022(4) 0.004(3) 0.006(3) 0.009(3) N5 0.037(4) 0.035(4) 0.028(4) 0.013(3) 0.003(3) 0.005(3) N6 0.049(4) 0.031(4) 0.029(4) 0.004(3) 0.003(3) 0.016(3) C1 0.024(4) 0.017(4) 0.020(4) 0.000(3) 0.010(4) 0.006(3) C2 0.028(5) 0.017(4) 0.025(5) 0.002(4) 0.005(4) 0.001(3) O1 0.036(3) 0.052(4) 0.021(3) 0.017(3) -0.006(3) 0.003(3) C3 0.027(5) 0.026(5) 0.024(5) -0.004(3) -0.002(4) 0.008(4) C4 0.027(5) 0.033(5) 0.023(4) 0.011(4) 0.002(4) 0.005(4) C11 0.032(5) 0.021(4) 0.027(5) 0.005(4) 0.008(4) -0.001(4) C12 0.030(5) 0.047(6) 0.035(5) 0.023(4) -0.004(4) 0.000(4) C13 0.039(6) 0.056(6) 0.040(6) 0.022(5) 0.011(5) -0.002(5) C14 0.046(6) 0.041(5) 0.030(5) 0.025(4) 0.004(4) 0.008(5) C15 0.043(6) 0.038(5) 0.034(5) 0.015(4) -0.015(4) 0.000(4) C16 0.035(5) 0.038(5) 0.038(5) 0.019(4) 0.003(4) 0.004(4) C21 0.023(5) 0.026(5) 0.026(5) 0.009(4) 0.001(4) -0.003(4) C22 0.036(5) 0.045(6) 0.028(5) 0.013(4) 0.006(4) -0.005(4) C23 0.015(5) 0.082(8) 0.054(7) 0.036(6) 0.002(5) 0.002(5) C24 0.039(6) 0.076(8) 0.038(6) 0.025(6) -0.020(5) -0.024(6) C25 0.059(7) 0.045(6) 0.044(6) 0.019(5) -0.017(5) -0.023(5) C26 0.042(6) 0.042(6) 0.037(6) 0.017(5) -0.004(4) -0.001(5) C31 0.019(4) 0.034(5) 0.028(5) 0.014(4) 0.014(4) 0.006(4) C32 0.042(6) 0.044(6) 0.041(6) 0.008(4) 0.009(4) 0.022(5) C33 0.041(6) 0.040(6) 0.063(7) 0.013(5) 0.003(5) 0.020(5) C34 0.033(5) 0.054(6) 0.057(7) 0.030(5) 0.007(5) 0.014(5) C35 0.028(5) 0.036(5) 0.034(5) 0.010(4) 0.004(4) 0.000(4) C36 0.025(5) 0.035(5) 0.027(5) 0.005(4) 0.006(4) 0.008(4) C41 0.025(5) 0.036(5) 0.024(5) 0.009(4) 0.007(4) 0.006(4) C42 0.035(5) 0.033(5) 0.019(5) 0.002(4) 0.005(4) 0.000(4) C43 0.041(6) 0.042(6) 0.047(6) 0.018(5) 0.017(5) 0.008(4) C44 0.034(5) 0.066(7) 0.046(6) 0.023(5) 0.019(4) 0.007(5) C45 0.072(7) 0.067(7) 0.041(6) 0.013(5) 0.037(5) 0.024(6) C46 0.063(6) 0.040(6) 0.036(6) 0.013(4) 0.026(5) 0.019(5) C51 0.034(5) 0.044(6) 0.024(5) 0.010(4) 0.009(4) 0.011(4) C52 0.029(5) 0.048(6) 0.033(5) 0.006(4) 0.011(4) 0.001(4) C53 0.053(6) 0.065(7) 0.041(6) 0.023(5) 0.020(5) 0.011(5) C54 0.054(6) 0.095(8) 0.026(6) 0.025(6) 0.024(5) 0.017(6) C55 0.044(6) 0.077(8) 0.027(5) 0.007(5) 0.014(4) 0.022(5) C56 0.040(6) 0.057(6) 0.035(6) 0.013(5) 0.010(4) 0.024(5) C61 0.029(5) 0.033(5) 0.022(5) 0.002(4) 0.004(4) 0.009(4) C62 0.025(5) 0.030(5) 0.045(6) 0.009(4) 0.005(4) 0.004(4) C63 0.048(6) 0.047(6) 0.042(6) 0.024(5) 0.006(5) 0.017(5) C64 0.033(6) 0.068(7) 0.047(6) 0.020(5) -0.003(5) 0.017(5) C65 0.034(5) 0.058(6) 0.041(6) 0.014(5) 0.005(4) 0.009(5) C66 0.033(5) 0.047(6) 0.037(5) 0.026(4) 0.013(4) 0.013(4) C71 0.029(5) 0.020(4) 0.027(5) -0.001(4) 0.002(4) 0.008(4) C72 0.024(5) 0.033(5) 0.049(6) 0.011(4) -0.001(4) 0.008(4) C73 0.069(7) 0.032(6) 0.045(6) 0.002(4) -0.013(6) 0.018(5) C74 0.037(7) 0.041(6) 0.089(9) -0.010(6) -0.027(6) 0.008(5) C75 0.036(6) 0.040(6) 0.108(10) -0.004(6) 0.009(7) -0.004(5) C76 0.024(5) 0.024(5) 0.068(7) 0.001(4) 0.004(5) -0.003(4) C81 0.028(5) 0.025(5) 0.032(5) 0.009(4) 0.004(4) 0.000(4) C86 0.036(5) 0.029(5) 0.037(5) 0.009(4) 0.000(4) 0.001(4) C85 0.064(7) 0.056(7) 0.036(6) 0.019(5) -0.011(5) -0.010(5) C84 0.084(8) 0.036(6) 0.065(8) 0.024(6) -0.005(6) -0.008(6) C83 0.090(8) 0.024(5) 0.049(7) 0.003(5) -0.005(6) -0.011(5) C82 0.080(7) 0.024(5) 0.028(5) -0.003(4) 0.003(5) 0.004(5) C101 0.087(8) 0.053(7) 0.098(9) 0.024(6) 0.046(7) 0.022(6) C102 0.033(6) 0.055(7) 0.072(8) 0.019(6) 0.009(5) 0.010(5) C103 0.077(8) 0.078(8) 0.092(10) -0.030(7) 0.037(7) -0.013(6) O11 0.053(4) 0.057(4) 0.069(5) 0.025(4) 0.017(4) 0.006(3) C111 0.186(16) 0.136(14) 0.157(17) 0.061(13) -0.027(13) -0.005(12) C112 0.100(11) 0.045(9) 0.173(16) 0.020(10) 0.057(11) 0.017(8) C113 0.200(16) 0.090(11) 0.138(14) -0.044(9) 0.014(12) 0.058(10) O12 0.087(6) 0.065(5) 0.121(7) 0.006(5) 0.040(5) 0.015(5) C121 0.103(12) 0.075(10) 0.29(2) 0.022(12) 0.019(13) 0.019(9) C122 0.078(10) 0.110(11) 0.060(9) 0.015(8) 0.034(8) 0.019(9) C123 0.139(14) 0.148(15) 0.33(3) 0.165(18) 0.002(15) -0.030(12) O13 0.154(10) 0.206(11) 0.092(8) 0.038(8) 0.039(7) 0.059(8) C131 0.117(10) 0.080(8) 0.081(9) 0.030(7) 0.047(8) 0.052(7) C132 0.062(7) 0.050(7) 0.049(7) 0.022(5) 0.020(6) 0.028(6) C133 0.116(10) 0.054(8) 0.098(10) -0.006(7) 0.030(8) 0.003(7) O14 0.056(4) 0.052(4) 0.070(5) -0.003(4) 0.014(4) 0.027(4) C141 0.138(12) 0.078(10) 0.161(14) 0.076(10) 0.004(10) 0.008(9) C142 0.065(8) 0.080(9) 0.069(8) 0.039(7) 0.004(6) -0.007(6) C143 0.30(2) 0.116(12) 0.076(11) 0.046(9) -0.088(12) -0.040(13) O15 0.065(4) 0.077(5) 0.054(5) 0.041(4) 0.015(4) 0.015(4) P5 0.0289(14) 0.0578(17) 0.0284(14) 0.0028(12) 0.0049(11) 0.0058(12) P6 0.205(5) 0.0313(19) 0.060(2) 0.0071(16) -0.014(2) 0.023(2) P7 0.0470(17) 0.078(2) 0.079(2) 0.0513(18) 0.0195(16) 0.0279(15) F1 0.113(5) 0.123(5) 0.085(5) 0.056(4) 0.069(4) 0.031(4) F2 0.061(4) 0.086(4) 0.045(4) -0.029(3) 0.005(3) -0.011(3) F3 0.093(4) 0.087(4) 0.053(4) 0.033(3) 0.037(3) 0.030(3) F4 0.056(4) 0.057(4) 0.086(5) -0.030(3) 0.008(3) 0.002(3) F5 0.059(4) 0.103(4) 0.054(4) 0.022(3) 0.011(3) 0.035(3) F6 0.043(3) 0.090(4) 0.067(4) -0.017(3) -0.003(3) 0.026(3) F7 0.154(8) 0.072(6) 0.419(17) 0.027(8) -0.095(9) 0.035(6) F8 0.72(2) 0.037(5) 0.068(6) 0.007(4) -0.055(9) 0.010(8) F9 0.306(12) 0.117(7) 0.227(11) 0.062(7) 0.140(10) 0.125(8) F10 0.224(9) 0.046(4) 0.141(7) 0.019(4) 0.025(6) 0.000(5) F11 0.312(11) 0.052(4) 0.075(5) 0.013(4) 0.050(6) 0.026(5) F12 0.228(8) 0.074(5) 0.064(5) 0.016(4) -0.003(5) 0.030(5) F19 0.170(7) 0.130(6) 0.078(5) 0.057(5) -0.001(5) 0.059(5) F20 0.111(6) 0.120(6) 0.306(12) 0.090(7) 0.158(7) 0.047(5) F21 0.091(4) 0.067(4) 0.152(6) 0.072(4) 0.027(4) 0.030(4) F22 0.134(6) 0.097(5) 0.117(6) 0.048(4) -0.032(5) 0.034(4) F23 0.100(5) 0.094(5) 0.132(6) 0.050(4) 0.077(5) 0.036(4) F24 0.063(4) 0.064(4) 0.090(5) 0.030(3) 0.013(3) 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 N1 1.998(6) . ? Ru1 N5 2.106(5) . ? Ru1 N3 2.106(5) . ? Ru1 N6 2.112(5) . ? Ru1 N4 2.114(5) . ? Ru1 N2 2.122(6) . ? Mn1 C2 1.790(7) . ? Mn1 C1 1.937(7) . ? Mn1 P2 2.285(3) . ? Mn1 P4 2.295(3) . ? Mn1 P3 2.300(3) . ? Mn1 P1 2.302(3) . ? P1 C81 1.834(7) . ? P1 C71 1.838(7) . ? P1 C3 1.847(7) . ? P2 C61 1.826(7) . ? P2 C51 1.829(7) . ? P2 C3 1.846(7) . ? P3 C41 1.807(7) . ? P3 C31 1.831(7) . ? P3 C4 1.845(7) . ? P4 C21 1.812(7) . ? P4 C11 1.826(7) . ? P4 C4 1.834(7) . ? N1 C1 1.182(7) . ? C2 O1 1.156(7) . ? C11 C16 1.394(9) . ? C11 C12 1.406(9) . ? C12 C13 1.392(9) . ? C13 C14 1.388(9) . ? C14 C15 1.377(9) . ? C15 C16 1.377(9) . ? C21 C22 1.378(10) . ? C21 C26 1.379(10) . ? C22 C23 1.409(10) . ? C23 C24 1.372(12) . ? C24 C25 1.388(12) . ? C25 C26 1.398(10) . ? C31 C36 1.393(9) . ? C31 C32 1.398(9) . ? C32 C33 1.384(9) . ? C33 C34 1.387(11) . ? C34 C35 1.371(10) . ? C35 C36 1.393(9) . ? C41 C42 1.392(9) . ? C41 C46 1.396(10) . ? C42 C43 1.384(9) . ? C43 C44 1.380(11) . ? C44 C45 1.382(10) . ? C45 C46 1.387(10) . ? C51 C52 1.373(9) . ? C51 C56 1.399(10) . ? C52 C53 1.404(9) . ? C53 C54 1.370(11) . ? C54 C55 1.377(10) . ? C55 C56 1.379(10) . ? C61 C62 1.395(9) . ? C61 C66 1.399(9) . ? C62 C63 1.379(9) . ? C63 C64 1.375(10) . ? C64 C65 1.359(9) . ? C65 C66 1.376(9) . ? C71 C76 1.385(9) . ? C71 C72 1.399(9) . ? C72 C73 1.405(10) . ? C73 C74 1.373(12) . ? C74 C75 1.378(12) . ? C75 C76 1.380(11) . ? C81 C86 1.391(9) . ? C81 C82 1.397(10) . ? C86 C85 1.389(9) . ? C85 C84 1.380(11) . ? C84 C83 1.379(11) . ? C83 C82 1.376(9) . ? C101 C102 1.479(11) . ? C102 O11 1.228(10) . ? C102 C103 1.480(12) . ? C111 C112 1.492(16) . ? C112 O12 1.247(11) . ? C112 C113 1.516(16) . ? C121 C122 1.427(15) . ? C122 O13 1.213(12) . ? C122 C123 1.383(14) . ? C131 C132 1.489(11) . ? C132 O14 1.201(10) . ? C132 C133 1.483(11) . ? C141 C142 1.512(13) . ? C142 O15 1.205(10) . ? C142 C143 1.440(14) . ? P5 F5 1.564(5) . ? P5 F3 1.567(5) . ? P5 F1 1.585(5) . ? P5 F2 1.590(5) . ? P5 F4 1.595(5) . ? P5 F6 1.596(5) . ? P6 F8 1.519(8) . ? P6 F12 1.522(7) . ? P6 F7 1.538(9) . ? P6 F10 1.582(7) . ? P6 F11 1.592(7) . ? P6 F9 1.599(9) . ? P7 F20 1.541(6) . ? P7 F19 1.553(6) . ? P7 F23 1.560(5) . ? P7 F21 1.569(6) . ? P7 F22 1.587(6) . ? P7 F24 1.623(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N5 88.9(2) . . ? N1 Ru1 N3 179.1(2) . . ? N5 Ru1 N3 90.4(2) . . ? N1 Ru1 N6 92.8(2) . . ? N5 Ru1 N6 178.3(2) . . ? N3 Ru1 N6 88.0(2) . . ? N1 Ru1 N4 88.2(2) . . ? N5 Ru1 N4 89.6(2) . . ? N3 Ru1 N4 91.3(2) . . ? N6 Ru1 N4 90.3(2) . . ? N1 Ru1 N2 90.7(2) . . ? N5 Ru1 N2 89.5(2) . . ? N3 Ru1 N2 89.7(2) . . ? N6 Ru1 N2 90.6(2) . . ? N4 Ru1 N2 178.6(2) . . ? C2 Mn1 C1 174.9(3) . . ? C2 Mn1 P2 87.1(2) . . ? C1 Mn1 P2 92.2(2) . . ? C2 Mn1 P4 90.1(2) . . ? C1 Mn1 P4 85.3(2) . . ? P2 Mn1 P4 107.24(9) . . ? C2 Mn1 P3 91.7(2) . . ? C1 Mn1 P3 89.0(2) . . ? P2 Mn1 P3 178.78(8) . . ? P4 Mn1 P3 72.86(9) . . ? C2 Mn1 P1 88.0(2) . . ? C1 Mn1 P1 96.6(2) . . ? P2 Mn1 P1 73.61(9) . . ? P4 Mn1 P1 177.91(8) . . ? P3 Mn1 P1 106.25(9) . . ? C81 P1 C71 100.0(3) . . ? C81 P1 C3 103.2(3) . . ? C71 P1 C3 107.1(3) . . ? C81 P1 Mn1 130.3(3) . . ? C71 P1 Mn1 119.3(2) . . ? C3 P1 Mn1 93.6(2) . . ? C61 P2 C51 101.4(3) . . ? C61 P2 C3 105.7(3) . . ? C51 P2 C3 103.5(3) . . ? C61 P2 Mn1 123.9(2) . . ? C51 P2 Mn1 124.3(3) . . ? C3 P2 Mn1 94.3(2) . . ? C41 P3 C31 101.9(3) . . ? C41 P3 C4 104.4(3) . . ? C31 P3 C4 106.1(3) . . ? C41 P3 Mn1 124.3(3) . . ? C31 P3 Mn1 122.6(2) . . ? C4 P3 Mn1 94.2(2) . . ? C21 P4 C11 101.1(3) . . ? C21 P4 C4 105.7(3) . . ? C11 P4 C4 106.0(3) . . ? C21 P4 Mn1 126.2(2) . . ? C11 P4 Mn1 120.4(2) . . ? C4 P4 Mn1 94.7(2) . . ? C1 N1 Ru1 175.4(5) . . ? N1 C1 Mn1 176.6(6) . . ? O1 C2 Mn1 178.0(7) . . ? P2 C3 P1 96.2(3) . . ? P4 C4 P3 95.7(3) . . ? C16 C11 C12 118.3(6) . . ? C16 C11 P4 120.3(6) . . ? C12 C11 P4 121.1(5) . . ? C13 C12 C11 120.8(7) . . ? C14 C13 C12 119.4(7) . . ? C15 C14 C13 119.8(7) . . ? C16 C15 C14 121.2(7) . . ? C15 C16 C11 120.3(7) . . ? C22 C21 C26 117.8(7) . . ? C22 C21 P4 119.7(6) . . ? C26 C21 P4 122.5(6) . . ? C21 C22 C23 121.1(8) . . ? C24 C23 C22 120.4(9) . . ? C23 C24 C25 119.1(8) . . ? C24 C25 C26 119.7(9) . . ? C21 C26 C25 121.9(9) . . ? C36 C31 C32 118.3(7) . . ? C36 C31 P3 119.8(6) . . ? C32 C31 P3 121.7(6) . . ? C33 C32 C31 120.9(8) . . ? C32 C33 C34 120.0(8) . . ? C35 C34 C33 120.0(8) . . ? C34 C35 C36 120.4(8) . . ? C31 C36 C35 120.5(7) . . ? C42 C41 C46 117.1(7) . . ? C42 C41 P3 120.0(6) . . ? C46 C41 P3 122.8(6) . . ? C43 C42 C41 122.3(7) . . ? C44 C43 C42 118.9(8) . . ? C43 C44 C45 120.7(8) . . ? C44 C45 C46 119.4(8) . . ? C45 C46 C41 121.5(8) . . ? C52 C51 C56 119.0(7) . . ? C52 C51 P2 120.1(6) . . ? C56 C51 P2 120.8(6) . . ? C51 C52 C53 120.4(8) . . ? C54 C53 C52 119.9(8) . . ? C53 C54 C55 119.9(8) . . ? C54 C55 C56 120.6(8) . . ? C55 C56 C51 120.1(8) . . ? C62 C61 C66 117.9(7) . . ? C62 C61 P2 121.5(6) . . ? C66 C61 P2 120.6(5) . . ? C63 C62 C61 120.8(7) . . ? C64 C63 C62 119.9(7) . . ? C65 C64 C63 120.3(8) . . ? C64 C65 C66 120.7(8) . . ? C65 C66 C61 120.4(7) . . ? C76 C71 C72 119.2(7) . . ? C76 C71 P1 119.6(6) . . ? C72 C71 P1 120.7(6) . . ? C71 C72 C73 119.4(8) . . ? C74 C73 C72 119.8(9) . . ? C73 C74 C75 121.0(9) . . ? C74 C75 C76 119.5(10) . . ? C75 C76 C71 121.1(9) . . ? C86 C81 C82 118.2(7) . . ? C86 C81 P1 123.5(6) . . ? C82 C81 P1 118.2(6) . . ? C85 C86 C81 120.4(7) . . ? C84 C85 C86 120.5(8) . . ? C83 C84 C85 119.5(8) . . ? C82 C83 C84 120.4(8) . . ? C83 C82 C81 121.0(8) . . ? O11 C102 C101 122.0(10) . . ? O11 C102 C103 120.8(10) . . ? C101 C102 C103 117.2(9) . . ? O12 C112 C111 123.6(14) . . ? O12 C112 C113 119.0(15) . . ? C111 C112 C113 117.5(12) . . ? O13 C122 C123 124.7(15) . . ? O13 C122 C121 117.0(14) . . ? C123 C122 C121 118.1(13) . . ? O14 C132 C133 121.6(9) . . ? O14 C132 C131 121.2(10) . . ? C133 C132 C131 117.2(9) . . ? O15 C142 C143 123.7(11) . . ? O15 C142 C141 118.4(11) . . ? C143 C142 C141 118.0(10) . . ? F5 P5 F3 90.3(3) . . ? F5 P5 F1 91.7(3) . . ? F3 P5 F1 177.8(3) . . ? F5 P5 F2 91.4(3) . . ? F3 P5 F2 90.1(3) . . ? F1 P5 F2 89.0(3) . . ? F5 P5 F4 90.3(3) . . ? F3 P5 F4 89.6(3) . . ? F1 P5 F4 91.3(3) . . ? F2 P5 F4 178.3(3) . . ? F5 P5 F6 179.4(3) . . ? F3 P5 F6 90.0(3) . . ? F1 P5 F6 87.9(3) . . ? F2 P5 F6 89.1(3) . . ? F4 P5 F6 89.2(3) . . ? F8 P6 F12 172.9(8) . . ? F8 P6 F7 95.7(7) . . ? F12 P6 F7 90.0(6) . . ? F8 P6 F10 91.3(4) . . ? F12 P6 F10 92.7(4) . . ? F7 P6 F10 93.2(6) . . ? F8 P6 F11 87.7(4) . . ? F12 P6 F11 88.2(4) . . ? F7 P6 F11 88.3(5) . . ? F10 P6 F11 178.3(6) . . ? F8 P6 F9 86.5(7) . . ? F12 P6 F9 87.8(5) . . ? F7 P6 F9 177.7(6) . . ? F10 P6 F9 87.3(4) . . ? F11 P6 F9 91.3(6) . . ? F20 P7 F19 92.8(5) . . ? F20 P7 F23 177.1(4) . . ? F19 P7 F23 89.0(4) . . ? F20 P7 F21 91.0(3) . . ? F19 P7 F21 90.8(3) . . ? F23 P7 F21 91.2(3) . . ? F20 P7 F22 90.3(4) . . ? F19 P7 F22 176.3(4) . . ? F23 P7 F22 87.8(4) . . ? F21 P7 F22 91.2(4) . . ? F20 P7 F24 88.9(3) . . ? F19 P7 F24 89.1(4) . . ? F23 P7 F24 88.9(3) . . ? F21 P7 F24 179.9(4) . . ? F22 P7 F24 88.9(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.631 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.101 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 603281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H76 F18 Mn N6 O9 P6 Ru' _chemical_formula_weight 1540.96 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.091(4) _cell_length_b 31.216(5) _cell_length_c 16.167(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.48(3) _cell_angle_gamma 90.00 _cell_volume 7098(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 97 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3148 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.89 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 36451 _diffrn_reflns_av_R_equivalents 0.1689 _diffrn_reflns_av_sigmaI/netI 0.2412 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12454 _reflns_number_gt 4807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1004P)^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 12454 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2056 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.2327 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.867 _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 0.71315(6) 0.90453(2) 0.60735(6) 0.0391(3) Uani 1 1 d . . . Mn1 Mn 0.81284(9) 0.74937(4) 0.56975(10) 0.0290(4) Uani 1 1 d . . . N1 N 0.7516(5) 0.8442(2) 0.5931(5) 0.034(2) Uani 1 1 d . . . N2 N 0.6191(6) 0.8989(2) 0.5054(6) 0.062(3) Uani 1 1 d . . . H2A H 0.5625 0.8908 0.5216 0.093 Uiso 1 1 calc R . . H2B H 0.6405 0.8793 0.4710 0.093 Uiso 1 1 calc R . . H2C H 0.6135 0.9240 0.4796 0.093 Uiso 1 1 calc R . . N3 N 0.6081(5) 0.8876(2) 0.6878(5) 0.045(2) Uani 1 1 d . . . H3A H 0.5787 0.9111 0.7039 0.068 Uiso 1 1 calc R . . H3B H 0.6349 0.8743 0.7319 0.068 Uiso 1 1 calc R . . H3C H 0.5661 0.8702 0.6616 0.068 Uiso 1 1 calc R . . N4 N 0.8164(5) 0.9227(2) 0.5242(5) 0.045(2) Uani 1 1 d . . . H4C H 0.8457 0.8995 0.5066 0.067 Uiso 1 1 calc R . . H4D H 0.8589 0.9400 0.5499 0.067 Uiso 1 1 calc R . . H4E H 0.7882 0.9363 0.4810 0.067 Uiso 1 1 calc R . . N5 N 0.8060(6) 0.9091(2) 0.7083(6) 0.060(3) Uani 1 1 d . . . H5D H 0.7764 0.9024 0.7537 0.089 Uiso 1 1 calc R . . H5E H 0.8282 0.9357 0.7126 0.089 Uiso 1 1 calc R . . H5F H 0.8542 0.8910 0.7029 0.089 Uiso 1 1 calc R . . N6 N 0.6739(6) 0.9688(2) 0.6244(5) 0.048(2) Uani 1 1 d . . . H6C H 0.6278 0.9700 0.6596 0.072 Uiso 1 1 calc R . . H6D H 0.6531 0.9800 0.5760 0.072 Uiso 1 1 calc R . . H6E H 0.7240 0.9836 0.6448 0.072 Uiso 1 1 calc R . . C1 C 0.7745(6) 0.8075(3) 0.5846(7) 0.038(3) Uani 1 1 d . . . C2 C 0.8083(7) 0.7592(3) 0.4600(8) 0.039(3) Uani 1 1 d . . . O1 O 0.8068(5) 0.7642(2) 0.3874(5) 0.051(2) Uani 1 1 d . . . C3 C 0.8149(7) 0.7422(3) 0.6806(8) 0.038(3) Uani 1 1 d . . . O2 O 0.8134(5) 0.7361(2) 0.7528(5) 0.0460(19) Uani 1 1 d . . . P1 P 0.66459(17) 0.72595(8) 0.55739(18) 0.0335(7) Uani 1 1 d . . . O3 O 0.6025(4) 0.7367(2) 0.6338(5) 0.060(2) Uani 1 1 d . . . O4 O 0.5985(5) 0.7394(2) 0.4794(5) 0.051(2) Uani 1 1 d . . . O5 O 0.6578(4) 0.67599(18) 0.5470(4) 0.0449(19) Uani 1 1 d . . . C4 C 0.4985(10) 0.7379(7) 0.6293(11) 0.137(7) Uani 1 1 d . . . H4A H 0.4770 0.7642 0.6024 0.164 Uiso 1 1 calc R . . H4B H 0.4740 0.7141 0.5958 0.164 Uiso 1 1 calc R . . C5 C 0.4622(11) 0.7356(7) 0.7071(10) 0.159(9) Uani 1 1 d . . . H5A H 0.3940 0.7356 0.7013 0.239 Uiso 1 1 calc R . . H5B H 0.4836 0.7599 0.7395 0.239 Uiso 1 1 calc R . . H5C H 0.4839 0.7098 0.7343 0.239 Uiso 1 1 calc R . . C6 C 0.5752(9) 0.7811(4) 0.4583(8) 0.072(4) Uani 1 1 d . . . H6A H 0.6307 0.7954 0.4388 0.086 Uiso 1 1 calc R . . H6B H 0.5564 0.7962 0.5071 0.086 Uiso 1 1 calc R . . C7 C 0.4956(8) 0.7834(4) 0.3920(8) 0.081(5) Uani 1 1 d . . . H7A H 0.4813 0.8128 0.3793 0.122 Uiso 1 1 calc R . . H7B H 0.4401 0.7696 0.4113 0.122 Uiso 1 1 calc R . . H7C H 0.5145 0.7691 0.3430 0.122 Uiso 1 1 calc R . . C8 C 0.5732(9) 0.6496(4) 0.5305(10) 0.094(6) Uani 1 1 d . . . H8A H 0.5222 0.6623 0.5599 0.112 Uiso 1 1 calc R . . H8B H 0.5552 0.6517 0.4718 0.112 Uiso 1 1 calc R . . C9 C 0.5770(12) 0.6105(6) 0.5488(19) 0.28(2) Uani 1 1 d . . . H9A H 0.5165 0.5974 0.5347 0.420 Uiso 1 1 calc R . . H9B H 0.5922 0.6074 0.6072 0.420 Uiso 1 1 calc R . . H9C H 0.6251 0.5968 0.5186 0.420 Uiso 1 1 calc R . . P2 P 0.88756(17) 0.68423(7) 0.55522(18) 0.0320(7) Uani 1 1 d . . . C10 C 1.0093(6) 0.7063(3) 0.5710(7) 0.041(3) Uani 1 1 d . . . H10A H 1.0417 0.6964 0.6221 0.049 Uiso 1 1 calc R . . H10B H 1.0479 0.7006 0.5246 0.049 Uiso 1 1 calc R . . C11 C 0.8813(6) 0.6562(3) 0.4569(6) 0.034(2) Uani 1 1 d . . . C12 C 0.9258(7) 0.6724(3) 0.3875(7) 0.046(3) Uani 1 1 d . . . H12A H 0.9604 0.6977 0.3927 0.055 Uiso 1 1 calc R . . C13 C 0.9191(8) 0.6516(4) 0.3123(8) 0.062(4) Uani 1 1 d . . . H13A H 0.9509 0.6624 0.2681 0.074 Uiso 1 1 calc R . . C14 C 0.8662(9) 0.6155(4) 0.3026(8) 0.066(4) Uani 1 1 d . . . H14A H 0.8603 0.6020 0.2513 0.079 Uiso 1 1 calc R . . C15 C 0.8208(9) 0.5986(4) 0.3689(8) 0.059(3) Uani 1 1 d . . . H15A H 0.7860 0.5734 0.3618 0.071 Uiso 1 1 calc R . . C16 C 0.8263(7) 0.6189(3) 0.4469(8) 0.051(3) Uani 1 1 d . . . H16A H 0.7942 0.6078 0.4907 0.061 Uiso 1 1 calc R . . C17 C 0.8876(7) 0.6401(3) 0.6300(6) 0.036(3) Uani 1 1 d . . . C18 C 0.8132(7) 0.6337(3) 0.6825(7) 0.044(3) Uani 1 1 d . . . H18A H 0.7614 0.6522 0.6799 0.052 Uiso 1 1 calc R . . C19 C 0.8167(8) 0.6002(4) 0.7377(7) 0.055(3) Uani 1 1 d . . . H19A H 0.7664 0.5956 0.7712 0.066 Uiso 1 1 calc R . . C20 C 0.8944(9) 0.5735(3) 0.7434(9) 0.068(4) Uani 1 1 d . . . H20A H 0.8968 0.5512 0.7816 0.081 Uiso 1 1 calc R . . C21 C 0.9706(8) 0.5798(3) 0.6917(9) 0.068(4) Uani 1 1 d . . . H21A H 1.0230 0.5616 0.6945 0.082 Uiso 1 1 calc R . . C22 C 0.9646(7) 0.6131(3) 0.6377(7) 0.052(3) Uani 1 1 d . . . H22A H 1.0151 0.6178 0.6043 0.062 Uiso 1 1 calc R . . P3 P 0.97272(17) 0.76230(7) 0.57642(17) 0.0313(6) Uani 1 1 d . . . C23 C 1.0364(6) 0.7830(3) 0.6659(6) 0.033(2) Uani 1 1 d . . . C24 C 0.9917(8) 0.8086(3) 0.7245(7) 0.045(3) Uani 1 1 d . . . H24A H 0.9276 0.8151 0.7146 0.054 Uiso 1 1 calc R . . C25 C 1.0371(8) 0.8240(3) 0.7934(7) 0.048(3) Uani 1 1 d . . . H25A H 1.0046 0.8408 0.8299 0.058 Uiso 1 1 calc R . . C26 C 1.1336(9) 0.8148(4) 0.8103(8) 0.062(4) Uani 1 1 d . . . H26A H 1.1653 0.8250 0.8584 0.075 Uiso 1 1 calc R . . C27 C 1.1813(8) 0.7903(4) 0.7546(8) 0.055(3) Uani 1 1 d . . . H27A H 1.2456 0.7845 0.7650 0.066 Uiso 1 1 calc R . . C28 C 1.1336(7) 0.7746(3) 0.6833(7) 0.044(3) Uani 1 1 d . . . H28A H 1.1665 0.7582 0.6465 0.052 Uiso 1 1 calc R . . C29 C 1.0249(6) 0.7900(3) 0.4922(6) 0.034(2) Uani 1 1 d . . . C30 C 0.9908(8) 0.8291(3) 0.4685(7) 0.057(3) Uani 1 1 d . . . H30A H 0.9410 0.8407 0.4965 0.069 Uiso 1 1 calc R . . C31 C 1.0259(9) 0.8521(4) 0.4060(8) 0.063(4) Uani 1 1 d . . . H31A H 0.9989 0.8784 0.3908 0.076 Uiso 1 1 calc R . . C32 C 1.1017(9) 0.8364(4) 0.3651(8) 0.066(4) Uani 1 1 d . . . H32A H 1.1259 0.8520 0.3221 0.080 Uiso 1 1 calc R . . C33 C 1.1414(8) 0.7976(4) 0.3878(7) 0.056(3) Uani 1 1 d . . . H33A H 1.1919 0.7868 0.3599 0.067 Uiso 1 1 calc R . . C34 C 1.1052(7) 0.7743(3) 0.4540(8) 0.057(3) Uani 1 1 d . . . H34A H 1.1340 0.7489 0.4720 0.068 Uiso 1 1 calc R . . P4 P 0.0888(2) 0.97056(9) 0.3100(2) 0.0584(10) Uani 1 1 d . . . P5 P 0.3936(2) 0.98883(9) 0.6257(2) 0.0563(9) Uani 1 1 d . . . P6 P 0.7688(3) 0.84763(17) 0.9690(6) 0.159(3) Uani 1 1 d . . . F1 F 0.0010(4) 0.9565(2) 0.3616(5) 0.086(3) Uani 1 1 d . . . F2 F 0.0692(5) 0.9333(2) 0.2477(5) 0.098(3) Uani 1 1 d . . . F3 F 0.0238(7) 1.0007(3) 0.2553(7) 0.156(4) Uani 1 1 d . . . F4 F 0.1781(5) 0.9853(2) 0.2606(5) 0.091(3) Uani 1 1 d . . . F5 F 0.1101(5) 1.0083(2) 0.3749(5) 0.097(3) Uani 1 1 d . . . F6 F 0.1560(5) 0.9406(2) 0.3660(5) 0.084(2) Uani 1 1 d . . . F7 F 0.3312(6) 0.9479(3) 0.6343(6) 0.127(4) Uani 1 1 d . . . F8 F 0.3284(6) 1.0022(3) 0.5512(6) 0.138(4) Uani 1 1 d . . . F9 F 0.4634(7) 0.9773(4) 0.7002(7) 0.154(5) Uani 1 1 d . . . F10 F 0.4576(7) 0.9622(3) 0.5725(10) 0.191(6) Uani 1 1 d . . . F11 F 0.4614(6) 1.0272(2) 0.6118(6) 0.123(4) Uani 1 1 d . . . F12 F 0.3348(8) 1.0104(5) 0.6842(10) 0.246(8) Uani 1 1 d . . . F13 F 0.7554(13) 0.8825(5) 0.9089(14) 0.331(13) Uani 1 1 d . . . F14 F 0.6805(8) 0.8329(5) 0.9467(12) 0.237(8) Uani 1 1 d . . . F15 F 0.7102(19) 0.8744(7) 1.0310(13) 0.343(14) Uani 1 1 d . . . F16 F 0.7680(17) 0.8129(7) 1.0412(18) 0.357(15) Uani 1 1 d . . . F17 F 0.8526(8) 0.8572(6) 1.020(2) 0.49(3) Uani 1 1 d . . . F18 F 0.8144(19) 0.8164(9) 0.9221(19) 0.409(18) Uani 1 1 d . . . C51 C 0.7089(13) 0.9976(6) 0.9210(11) 0.141(7) Uani 1 1 d . . . H51A H 0.7568 1.0067 0.8850 0.212 Uiso 1 1 calc R . . H51B H 0.7387 0.9836 0.9687 0.212 Uiso 1 1 calc R . . H51C H 0.6742 1.0221 0.9385 0.212 Uiso 1 1 calc R . . C52 C 0.6431(10) 0.9676(4) 0.8763(10) 0.066(4) Uani 1 1 d . . . C53 C 0.5623(10) 0.9502(5) 0.9246(10) 0.115(6) Uani 1 1 d . . . H53A H 0.5244 0.9309 0.8901 0.173 Uiso 1 1 calc R . . H53B H 0.5235 0.9735 0.9414 0.173 Uiso 1 1 calc R . . H53C H 0.5880 0.9352 0.9727 0.173 Uiso 1 1 calc R . . O11 O 0.6537(6) 0.9568(2) 0.8051(6) 0.072(3) Uani 1 1 d . . . C61 C 0.3434(8) 0.8837(4) 0.4564(8) 0.073(4) Uani 1 1 d . . . H61A H 0.4014 0.8941 0.4355 0.109 Uiso 1 1 calc R . . H61B H 0.3017 0.9073 0.4652 0.109 Uiso 1 1 calc R . . H61C H 0.3132 0.8643 0.4170 0.109 Uiso 1 1 calc R . . C62 C 0.3650(8) 0.8611(3) 0.5360(8) 0.047(3) Uani 1 1 d . . . O12 O 0.4460(5) 0.8566(2) 0.5675(5) 0.060(2) Uani 1 1 d . . . C63 C 0.2835(9) 0.8418(4) 0.5785(9) 0.088(5) Uani 1 1 d . . . H63A H 0.3070 0.8280 0.6287 0.132 Uiso 1 1 calc R . . H63B H 0.2519 0.8211 0.5426 0.132 Uiso 1 1 calc R . . H63C H 0.2395 0.8639 0.5914 0.132 Uiso 1 1 calc R . . C71 C 0.9046(8) 0.0503(4) 0.4379(8) 0.076(4) Uani 1 1 d . . . H71A H 0.9484 0.0545 0.4850 0.114 Uiso 1 1 calc R . . H71B H 0.9016 0.0205 0.4240 0.114 Uiso 1 1 calc R . . H71C H 0.8427 0.0602 0.4507 0.114 Uiso 1 1 calc R . . C72 C 0.9370(8) 0.0746(4) 0.3674(8) 0.054(3) Uani 1 1 d . . . C73 C 0.8776(8) 0.0731(4) 0.2857(9) 0.074(4) Uani 1 1 d . . . H73A H 0.9066 0.0907 0.2457 0.111 Uiso 1 1 calc R . . H73B H 0.8147 0.0834 0.2939 0.111 Uiso 1 1 calc R . . H73C H 0.8741 0.0440 0.2661 0.111 Uiso 1 1 calc R . . O13 O 1.0097(5) 0.0958(2) 0.3734(5) 0.065(2) Uani 1 1 d . . . C81 C 0.8157(13) 0.8996(8) 0.2529(12) 0.195(11) Uani 1 1 d . . . H81A H 0.8537 0.9173 0.2905 0.293 Uiso 1 1 calc R . . H81B H 0.7772 0.9175 0.2160 0.293 Uiso 1 1 calc R . . H81C H 0.8565 0.8822 0.2214 0.293 Uiso 1 1 calc R . . C82 C 0.7499(10) 0.8702(4) 0.3031(11) 0.074(4) Uani 1 1 d . . . C83 C 0.6926(13) 0.8419(5) 0.2467(11) 0.138(8) Uani 1 1 d . . . H83A H 0.6530 0.8240 0.2783 0.207 Uiso 1 1 calc R . . H83B H 0.7340 0.8244 0.2161 0.207 Uiso 1 1 calc R . . H83C H 0.6534 0.8590 0.2089 0.207 Uiso 1 1 calc R . . O14 O 0.7503(6) 0.8723(3) 0.3771(6) 0.072(3) 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 0.0294(5) 0.0207(4) 0.0685(7) 0.0001(4) 0.0141(4) 0.0026(4) Mn1 0.0255(8) 0.0188(7) 0.0437(10) -0.0001(7) 0.0100(7) -0.0003(6) N1 0.034(5) 0.022(4) 0.046(6) 0.004(4) 0.011(4) 0.000(3) N2 0.058(6) 0.025(5) 0.108(9) 0.010(5) 0.047(6) -0.001(4) N3 0.035(5) 0.040(5) 0.062(7) 0.008(4) 0.011(5) 0.006(4) N4 0.035(5) 0.022(4) 0.080(7) -0.004(4) 0.017(5) -0.005(4) N5 0.062(6) 0.025(5) 0.097(8) 0.006(5) 0.051(6) 0.008(4) N6 0.048(6) 0.039(5) 0.058(7) -0.003(4) 0.012(5) 0.006(4) C1 0.026(5) 0.032(6) 0.056(8) 0.007(5) 0.004(5) -0.003(4) C2 0.025(6) 0.023(6) 0.066(9) -0.009(5) -0.020(6) 0.004(4) O1 0.050(5) 0.052(5) 0.053(6) -0.001(4) 0.003(5) 0.001(3) C3 0.034(6) 0.028(6) 0.052(8) -0.005(5) -0.006(6) 0.005(4) O2 0.037(4) 0.050(5) 0.052(6) 0.004(4) 0.018(4) -0.002(3) P1 0.0270(14) 0.0322(15) 0.0422(18) -0.0029(13) 0.0085(14) -0.0002(11) O3 0.021(4) 0.096(6) 0.064(6) -0.027(4) 0.021(4) -0.018(4) O4 0.038(4) 0.040(5) 0.076(6) -0.006(4) 0.012(4) 0.001(3) O5 0.040(4) 0.026(4) 0.069(6) 0.003(3) 0.004(4) -0.012(3) C4 0.051(10) 0.24(2) 0.121(17) -0.024(15) 0.027(11) -0.007(11) C5 0.071(11) 0.33(3) 0.085(14) -0.028(16) 0.072(10) 0.013(14) C6 0.069(9) 0.059(9) 0.090(11) -0.014(8) 0.033(8) -0.004(7) C7 0.058(8) 0.081(10) 0.101(12) -0.035(8) -0.033(9) 0.016(7) C8 0.069(9) 0.059(9) 0.147(15) 0.039(9) -0.039(9) -0.057(7) C9 0.080(13) 0.097(15) 0.65(6) 0.16(2) -0.13(2) -0.052(11) P2 0.0290(14) 0.0179(13) 0.0501(19) 0.0032(12) 0.0104(13) 0.0004(10) C10 0.019(5) 0.022(5) 0.083(9) 0.009(5) 0.002(5) 0.003(4) C11 0.031(6) 0.027(5) 0.044(7) -0.002(5) 0.006(5) 0.003(4) C12 0.050(7) 0.037(6) 0.054(8) -0.002(6) 0.020(6) 0.004(5) C13 0.053(8) 0.065(9) 0.070(10) -0.028(7) 0.027(7) 0.021(6) C14 0.082(10) 0.058(9) 0.054(9) -0.047(7) -0.014(8) 0.026(7) C15 0.066(8) 0.042(7) 0.069(10) -0.035(7) -0.008(8) 0.004(6) C16 0.045(7) 0.018(6) 0.090(10) -0.005(6) -0.004(7) 0.007(5) C17 0.036(6) 0.024(5) 0.048(7) -0.002(5) 0.004(6) 0.003(4) C18 0.037(6) 0.031(6) 0.064(8) 0.006(5) 0.015(6) -0.003(5) C19 0.051(7) 0.060(8) 0.055(8) 0.016(7) 0.009(6) -0.004(6) C20 0.064(8) 0.023(6) 0.116(12) 0.025(7) 0.005(8) -0.011(6) C21 0.039(7) 0.047(7) 0.119(12) 0.034(8) 0.002(8) 0.003(5) C22 0.035(6) 0.045(7) 0.078(9) 0.027(6) 0.018(6) 0.008(5) P3 0.0250(13) 0.0224(13) 0.0475(18) 0.0006(12) 0.0098(13) -0.0006(10) C23 0.030(6) 0.029(6) 0.042(7) 0.014(5) 0.009(5) -0.001(4) C24 0.045(7) 0.037(6) 0.052(8) 0.001(6) -0.004(6) -0.017(5) C25 0.055(8) 0.035(6) 0.055(9) 0.002(6) 0.007(7) -0.006(5) C26 0.069(9) 0.055(8) 0.061(10) 0.005(7) -0.005(8) -0.029(7) C27 0.040(7) 0.072(9) 0.052(9) 0.023(7) -0.003(7) -0.032(6) C28 0.027(6) 0.048(7) 0.057(8) -0.005(6) 0.012(6) -0.007(5) C29 0.026(5) 0.048(7) 0.029(6) -0.009(5) 0.010(5) -0.008(4) C30 0.062(8) 0.029(6) 0.085(10) 0.029(6) 0.045(7) 0.001(5) C31 0.075(9) 0.047(7) 0.070(10) 0.013(7) 0.023(8) -0.014(6) C32 0.080(10) 0.054(8) 0.068(10) 0.000(7) 0.033(8) -0.032(7) C33 0.059(8) 0.069(9) 0.044(8) -0.004(6) 0.040(6) -0.020(6) C34 0.038(6) 0.045(7) 0.091(10) -0.013(6) 0.035(7) -0.012(5) P4 0.049(2) 0.0322(17) 0.094(3) -0.0071(18) 0.009(2) 0.0001(14) P5 0.0420(18) 0.0420(19) 0.086(3) 0.0168(18) 0.010(2) 0.0018(14) P6 0.058(3) 0.068(3) 0.355(11) 0.016(5) 0.041(5) 0.006(2) F1 0.043(4) 0.062(5) 0.155(8) -0.025(4) 0.032(5) -0.015(3) F2 0.090(6) 0.080(5) 0.127(8) -0.038(5) 0.021(5) -0.019(4) F3 0.127(8) 0.152(9) 0.189(11) 0.076(8) 0.006(8) 0.068(7) F4 0.089(5) 0.051(4) 0.140(7) 0.005(4) 0.066(5) -0.013(4) F5 0.083(5) 0.068(5) 0.144(8) -0.051(5) 0.048(5) -0.026(4) F6 0.067(5) 0.103(6) 0.085(6) 0.011(4) 0.031(4) 0.032(4) F7 0.090(6) 0.100(6) 0.189(10) 0.076(7) 0.004(6) -0.036(5) F8 0.127(8) 0.108(7) 0.169(10) 0.092(7) -0.071(7) -0.055(6) F9 0.095(7) 0.206(11) 0.155(10) 0.111(9) -0.028(7) -0.048(7) F10 0.113(8) 0.129(8) 0.342(19) -0.109(10) 0.117(10) -0.033(6) F11 0.103(6) 0.073(5) 0.190(10) 0.055(6) -0.030(7) -0.039(5) F12 0.134(10) 0.359(19) 0.251(17) -0.193(15) 0.066(11) 0.045(11) F13 0.36(2) 0.158(12) 0.51(3) 0.225(17) 0.31(2) 0.100(13) F14 0.096(9) 0.226(15) 0.39(2) 0.101(16) 0.037(12) -0.082(9) F15 0.43(3) 0.30(2) 0.29(2) -0.04(2) -0.10(2) 0.21(2) F16 0.34(3) 0.210(19) 0.50(4) -0.01(2) -0.16(3) 0.137(19) F17 0.035(7) 0.211(17) 1.23(8) 0.03(3) -0.002(18) -0.028(8) F18 0.38(3) 0.38(3) 0.48(4) -0.23(3) 0.17(3) 0.13(3) C51 0.157(17) 0.151(17) 0.119(16) -0.053(13) 0.044(14) -0.058(14) C52 0.077(10) 0.053(8) 0.065(10) -0.003(7) -0.014(9) -0.004(7) C53 0.097(12) 0.119(13) 0.139(16) -0.045(11) 0.076(12) -0.031(10) O11 0.094(7) 0.059(6) 0.066(7) -0.005(5) 0.017(6) -0.001(5) C61 0.040(7) 0.098(10) 0.082(11) 0.008(8) 0.018(7) -0.001(7) C62 0.038(7) 0.044(7) 0.062(9) -0.026(6) 0.010(7) -0.004(5) O12 0.046(5) 0.042(5) 0.091(7) -0.001(4) 0.005(5) -0.007(4) C63 0.051(8) 0.099(11) 0.117(13) -0.001(9) 0.033(9) -0.016(7) C71 0.046(8) 0.123(12) 0.063(10) 0.020(8) 0.027(7) 0.000(7) C72 0.038(7) 0.051(7) 0.073(10) -0.001(7) 0.006(7) 0.013(6) C73 0.056(8) 0.055(8) 0.112(13) 0.029(8) 0.016(9) 0.005(6) O13 0.037(5) 0.051(5) 0.109(8) -0.006(5) 0.024(5) 0.006(4) C81 0.124(17) 0.35(3) 0.118(18) -0.054(19) 0.039(14) -0.139(19) C82 0.056(9) 0.079(10) 0.087(12) -0.016(10) 0.003(10) 0.006(7) C83 0.19(2) 0.066(11) 0.150(18) -0.013(11) -0.055(16) -0.037(11) O14 0.078(7) 0.064(6) 0.075(7) -0.017(5) -0.005(6) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.978(8) . ? Ru1 N5 2.034(9) . ? Ru1 N2 2.059(9) . ? Ru1 N3 2.096(8) . ? Ru1 N6 2.104(7) . ? Ru1 N4 2.118(8) . ? Mn1 C2 1.797(13) . ? Mn1 C3 1.805(12) . ? Mn1 C1 1.914(10) . ? Mn1 P1 2.211(3) . ? Mn1 P3 2.285(3) . ? Mn1 P2 2.308(3) . ? N1 C1 1.198(10) . ? C2 O1 1.184(12) . ? C3 O2 1.184(11) . ? P1 O5 1.571(6) . ? P1 O4 1.579(8) . ? P1 O3 1.592(7) . ? O3 C4 1.464(15) . ? O4 C6 1.381(12) . ? O5 C8 1.460(11) . ? C4 C5 1.39(2) . ? C6 C7 1.505(15) . ? C8 C9 1.255(17) . ? P2 C11 1.812(10) . ? P2 C17 1.832(10) . ? P2 C10 1.851(9) . ? C10 P3 1.827(8) . ? C11 C16 1.403(12) . ? C11 C12 1.413(13) . ? C12 C13 1.376(14) . ? C13 C14 1.355(16) . ? C14 C15 1.385(17) . ? C15 C16 1.408(15) . ? C17 C22 1.375(12) . ? C17 C18 1.402(13) . ? C18 C19 1.373(13) . ? C19 C20 1.373(15) . ? C20 C21 1.414(16) . ? C21 C22 1.357(14) . ? P3 C23 1.776(10) . ? P3 C29 1.808(10) . ? C23 C28 1.406(12) . ? C23 C24 1.418(14) . ? C24 C25 1.339(14) . ? C25 C26 1.400(15) . ? C26 C27 1.385(16) . ? C27 C28 1.389(14) . ? C29 C30 1.358(12) . ? C29 C34 1.410(13) . ? C30 C31 1.358(14) . ? C31 C32 1.381(16) . ? C32 C33 1.374(15) . ? C33 C34 1.415(14) . ? P4 F3 1.551(8) . ? P4 F2 1.552(7) . ? P4 F6 1.577(7) . ? P4 F5 1.594(7) . ? P4 F1 1.595(7) . ? P4 F4 1.598(7) . ? P5 F12 1.459(10) . ? P5 F8 1.527(8) . ? P5 F10 1.529(10) . ? P5 F9 1.550(9) . ? P5 F11 1.557(7) . ? P5 F7 1.562(7) . ? P6 F14 1.356(12) . ? P6 F18 1.414(15) . ? P6 F17 1.43(2) . ? P6 F13 1.464(14) . ? P6 F15 1.58(2) . ? P6 F16 1.59(3) . ? C51 C52 1.478(17) . ? C52 O11 1.216(15) . ? C52 C53 1.518(18) . ? C61 C62 1.483(15) . ? C62 O12 1.229(11) . ? C62 C63 1.500(15) . ? C71 C72 1.464(16) . ? C72 O13 1.218(12) . ? C72 C73 1.520(16) . ? C81 C82 1.57(2) . ? C82 O14 1.198(15) . ? C82 C83 1.474(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N5 89.6(3) . . ? N1 Ru1 N2 89.6(3) . . ? N5 Ru1 N2 179.0(3) . . ? N1 Ru1 N3 92.3(3) . . ? N5 Ru1 N3 87.9(3) . . ? N2 Ru1 N3 91.7(3) . . ? N1 Ru1 N6 179.0(3) . . ? N5 Ru1 N6 89.4(3) . . ? N2 Ru1 N6 91.4(3) . . ? N3 Ru1 N6 87.6(3) . . ? N1 Ru1 N4 88.7(3) . . ? N5 Ru1 N4 93.3(3) . . ? N2 Ru1 N4 87.1(3) . . ? N3 Ru1 N4 178.4(3) . . ? N6 Ru1 N4 91.4(3) . . ? C2 Mn1 C3 177.1(4) . . ? C2 Mn1 C1 88.2(4) . . ? C3 Mn1 C1 88.9(4) . . ? C2 Mn1 P1 89.5(3) . . ? C3 Mn1 P1 90.4(3) . . ? C1 Mn1 P1 93.0(3) . . ? C2 Mn1 P3 89.6(3) . . ? C3 Mn1 P3 91.1(3) . . ? C1 Mn1 P3 96.4(3) . . ? P1 Mn1 P3 170.49(11) . . ? C2 Mn1 P2 92.2(3) . . ? C3 Mn1 P2 90.7(3) . . ? C1 Mn1 P2 169.3(3) . . ? P1 Mn1 P2 97.69(10) . . ? P3 Mn1 P2 72.90(9) . . ? C1 N1 Ru1 179.7(8) . . ? N1 C1 Mn1 179.0(9) . . ? O1 C2 Mn1 177.5(9) . . ? O2 C3 Mn1 177.2(9) . . ? O5 P1 O4 98.6(4) . . ? O5 P1 O3 105.1(4) . . ? O4 P1 O3 103.8(4) . . ? O5 P1 Mn1 112.9(3) . . ? O4 P1 Mn1 119.5(3) . . ? O3 P1 Mn1 114.9(3) . . ? C4 O3 P1 124.3(9) . . ? C6 O4 P1 124.6(7) . . ? C8 O5 P1 128.5(7) . . ? C5 C4 O3 112.2(14) . . ? O4 C6 C7 112.1(10) . . ? C9 C8 O5 118.9(12) . . ? C11 P2 C17 102.3(4) . . ? C11 P2 C10 107.2(5) . . ? C17 P2 C10 103.0(4) . . ? C11 P2 Mn1 121.1(3) . . ? C17 P2 Mn1 125.2(3) . . ? C10 P2 Mn1 94.8(3) . . ? P3 C10 P2 95.8(4) . . ? C16 C11 C12 118.3(10) . . ? C16 C11 P2 120.0(9) . . ? C12 C11 P2 121.5(7) . . ? C13 C12 C11 121.5(10) . . ? C14 C13 C12 120.2(12) . . ? C13 C14 C15 120.2(11) . . ? C14 C15 C16 121.2(11) . . ? C11 C16 C15 118.5(12) . . ? C22 C17 C18 118.2(9) . . ? C22 C17 P2 119.3(8) . . ? C18 C17 P2 122.4(7) . . ? C19 C18 C17 120.2(10) . . ? C18 C19 C20 120.2(11) . . ? C19 C20 C21 120.4(11) . . ? C22 C21 C20 117.8(10) . . ? C21 C22 C17 123.1(11) . . ? C23 P3 C29 103.4(4) . . ? C23 P3 C10 104.9(4) . . ? C29 P3 C10 107.1(5) . . ? C23 P3 Mn1 123.4(3) . . ? C29 P3 Mn1 119.6(3) . . ? C10 P3 Mn1 96.2(3) . . ? C28 C23 C24 116.0(10) . . ? C28 C23 P3 122.3(8) . . ? C24 C23 P3 121.7(7) . . ? C25 C24 C23 123.3(10) . . ? C24 C25 C26 119.9(12) . . ? C27 C26 C25 119.4(12) . . ? C26 C27 C28 120.3(11) . . ? C27 C28 C23 121.1(11) . . ? C30 C29 C34 118.0(10) . . ? C30 C29 P3 119.3(7) . . ? C34 C29 P3 122.5(8) . . ? C29 C30 C31 123.1(11) . . ? C30 C31 C32 119.7(12) . . ? C33 C32 C31 120.0(11) . . ? C32 C33 C34 119.8(11) . . ? C29 C34 C33 119.2(11) . . ? F3 P4 F2 90.5(6) . . ? F3 P4 F6 178.9(6) . . ? F2 P4 F6 90.4(4) . . ? F3 P4 F5 90.5(6) . . ? F2 P4 F5 179.0(5) . . ? F6 P4 F5 88.7(5) . . ? F3 P4 F1 90.9(5) . . ? F2 P4 F1 91.2(4) . . ? F6 P4 F1 89.7(4) . . ? F5 P4 F1 88.9(4) . . ? F3 P4 F4 89.7(5) . . ? F2 P4 F4 90.3(4) . . ? F6 P4 F4 89.6(4) . . ? F5 P4 F4 89.6(4) . . ? F1 P4 F4 178.4(5) . . ? F12 P5 F8 92.7(8) . . ? F12 P5 F10 173.2(10) . . ? F8 P5 F10 93.0(8) . . ? F12 P5 F9 87.9(8) . . ? F8 P5 F9 176.9(5) . . ? F10 P5 F9 86.7(7) . . ? F12 P5 F11 96.6(8) . . ? F8 P5 F11 91.2(4) . . ? F10 P5 F11 87.0(6) . . ? F9 P5 F11 85.7(5) . . ? F12 P5 F7 88.6(8) . . ? F8 P5 F7 88.8(4) . . ? F10 P5 F7 87.8(6) . . ? F9 P5 F7 94.3(5) . . ? F11 P5 F7 174.8(6) . . ? F14 P6 F18 93.6(15) . . ? F14 P6 F17 159.6(16) . . ? F18 P6 F17 93.8(15) . . ? F14 P6 F13 89.8(11) . . ? F18 P6 F13 101.7(19) . . ? F17 P6 F13 107.3(13) . . ? F14 P6 F15 80.9(11) . . ? F18 P6 F15 168(2) . . ? F17 P6 F15 88.2(15) . . ? F13 P6 F15 88.7(9) . . ? F14 P6 F16 85.2(10) . . ? F18 P6 F16 86.9(15) . . ? F17 P6 F16 76.2(13) . . ? F13 P6 F16 170.4(12) . . ? F15 P6 F16 82.4(14) . . ? O11 C52 C51 121.9(15) . . ? O11 C52 C53 121.8(12) . . ? C51 C52 C53 116.3(14) . . ? O12 C62 C61 123.4(11) . . ? O12 C62 C63 118.8(12) . . ? C61 C62 C63 117.8(11) . . ? O13 C72 C71 121.3(12) . . ? O13 C72 C73 120.2(12) . . ? C71 C72 C73 118.5(11) . . ? O14 C82 C83 128.2(16) . . ? O14 C82 C81 121.3(14) . . ? C83 C82 C81 110.5(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.074 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.122 #===END