# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Kasper S. Pedersen' _publ_contact_author_address ; Department of Chemistry, University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; _publ_contact_author_email ksp@kiku.dk _publ_section_title ; A Linear Single-Molecule Magnet Based on [Ru(CN)~6~]^3-^ ; loop_ _publ_author_name _publ_author_address 'Kasper S. Pedersen' ; Department of Chemistry, University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; 'Magnus Schau-Magnussen' ; Department of Chemistry, University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; 'Jan Dreiser' ; Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI, Switzerland. ; 'Joscha Nehrkorn' ; Physikalisches Institut, Universitat Freiburg, D-79104 Freiburg, Germany ; 'Maren Gysler' ; Physikalisches Institut, Universitat Freiburg, D-79104 Freiburg, Germany ; ; A.Schnegg ; ; Institut fur Silizium-Photovoltaik, Helmholtz-Zentrum Berlin, D-12489 Berlin, Germany ; 'Karsten Holldack' ; Institut fur Methoden und Instrumente der Forschung mit Synchrotronstrahlung, Helmholtz-Zentrum Berlin, D-12489 Berlin, Germany ; 'Oliver Waldmann' ; Physikalisches Institut, Universitat Freiburg, D-79104 Freiburg, Germany ; 'H\/ogni Weihe' ; Department of Chemistry, University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; 'Stergios Piligkos' ; Department of Chemistry, University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; ; P.L.W.Tregenna-Piggott ; ; Deceased ; 'Jesper Bendix' ; Department of Chemistry, University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; loop_ _publ_section_references ; Coppens, P. (1970). Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall & C. P. Huber, pp 255-270. Copenhagen: Munksgaard. Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220--229. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Nonius (1999). COLLECT. Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; #------------------------------------------------------------------------- data_MnRuMn _database_code_depnum_ccdc_archive 'CCDC 806470' #TrackingRef '- KSP-MnRuMn.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraethylammonium {bis[(N,N'-Bis(5-bromosalicylidene)ethylenediamine)(methanol)manganese(iii)] \m-[hexacyanidoruthenate(iii)]} ; _chemical_name_common ; Tetraethylammonium (bis((N,N'-Bis(5- bromosalicylidene)ethylenediamine)(methanol)manganese(iii)) mu- (hexacyanidoruthenate(iii))) ; _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 Br4 Mn2 N10 O6 Ru, C8 H20 N' _chemical_formula_sum 'C48 H52 Br4 Mn2 N11 O6 Ru' _chemical_formula_weight 1409.60 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' Br Br -0.2901 2.4595 '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' 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' 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3004(16) _cell_length_b 15.5434(18) _cell_length_c 15.689(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.318(10) _cell_angle_gamma 90.00 _cell_volume 2711.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 57348 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 32.11 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.217 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.111 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398 _exptl_absorpt_coefficient_mu 3.738 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 130903 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 32.11 _reflns_number_total 9444 _reflns_number_gt 7878 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0152P)^2^+3.1455P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9444 _refine_ls_number_parameters 350 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 Ru Ru 0.0000 0.5000 0.0000 0.01310(4) Uani 1 2 d S . . C1 C -0.06412(15) 0.47625(12) 0.09836(12) 0.0164(3) Uani 1 1 d . . . N1 N -0.09576(14) 0.45858(11) 0.15571(11) 0.0203(3) Uani 1 1 d . . . C4 C 0.17219(17) 0.50260(13) 0.10634(13) 0.0216(3) Uani 1 1 d . . . N4 N 0.26930(16) 0.50370(14) 0.16600(13) 0.0326(4) Uani 1 1 d . . . C5 C -0.01346(19) 0.63067(13) 0.00986(13) 0.0227(4) Uani 1 1 d . . . N5 N -0.0207(2) 0.70425(12) 0.01235(14) 0.0372(5) Uani 1 1 d . . . Mn Mn -0.03319(2) 0.416691(16) 0.306602(18) 0.01230(5) Uani 1 1 d . . . O1 O 0.04774(14) 0.37159(9) 0.45646(9) 0.0239(3) Uani 1 1 d D . . H1 H 0.045(3) 0.3214(11) 0.467(2) 0.036 Uiso 1 1 d D . . C10 C 0.13773(18) 0.41021(14) 0.53862(13) 0.0249(4) Uani 1 1 d . . . H10A H 0.2171 0.4001 0.5399 0.030 Uiso 1 1 calc R . . H10B H 0.1351 0.3848 0.5949 0.030 Uiso 1 1 calc R . . H10C H 0.1230 0.4722 0.5376 0.030 Uiso 1 1 calc R . . N2 N 0.11791(12) 0.38497(9) 0.29645(10) 0.0142(3) Uani 1 1 d . . . O2 O 0.02586(11) 0.52749(8) 0.35160(9) 0.0168(2) Uani 1 1 d . . . N3 N -0.06845(13) 0.29156(9) 0.27674(10) 0.0146(3) Uani 1 1 d . . . O3 O -0.18458(11) 0.43481(8) 0.30710(9) 0.0176(2) Uani 1 1 d . . . C2 C 0.10789(15) 0.30302(11) 0.24666(13) 0.0170(3) Uani 1 1 d . . . H2A H 0.1887 0.2789 0.2625 0.020 Uiso 1 1 calc R . . H2B H 0.0665 0.3118 0.1776 0.020 Uiso 1 1 calc R . . C3 C 0.03576(15) 0.24249(11) 0.27873(13) 0.0177(3) Uani 1 1 d . . . H3A H 0.0079 0.1922 0.2360 0.021 Uiso 1 1 calc R . . H3B H 0.0860 0.2215 0.3434 0.021 Uiso 1 1 calc R . . C11 C 0.13810(15) 0.55474(11) 0.38640(12) 0.0156(3) Uani 1 1 d . . . C12 C 0.16844(17) 0.63012(12) 0.44192(13) 0.0198(3) Uani 1 1 d . . . H12 H 0.1084 0.6586 0.4544 0.024 Uiso 1 1 calc R . . C13 C 0.28335(17) 0.66328(12) 0.47835(14) 0.0218(3) Uani 1 1 d . . . H13 H 0.3026 0.7131 0.5171 0.026 Uiso 1 1 calc R . . C14 C 0.37156(16) 0.62355(12) 0.45815(13) 0.0205(3) Uani 1 1 d . . . C15 C 0.34674(16) 0.54934(12) 0.40576(13) 0.0192(3) Uani 1 1 d . . . H15 H 0.4076 0.5226 0.3930 0.023 Uiso 1 1 calc R . . C16 C 0.23060(15) 0.51285(11) 0.37085(12) 0.0156(3) Uani 1 1 d . . . C17 C 0.21337(15) 0.43140(11) 0.32264(12) 0.0157(3) Uani 1 1 d . . . H17 H 0.2770 0.4106 0.3093 0.019 Uiso 1 1 calc R . . Br1 Br 0.527964(17) 0.672441(13) 0.503130(16) 0.02750(5) Uani 1 1 d . . . C21 C -0.27330(15) 0.38067(12) 0.28977(12) 0.0157(3) Uani 1 1 d . . . C22 C -0.38129(16) 0.41297(12) 0.28902(13) 0.0193(3) Uani 1 1 d . . . H22 H -0.3862 0.4720 0.3026 0.023 Uiso 1 1 calc R . . C23 C -0.47980(16) 0.36033(14) 0.26892(13) 0.0219(4) Uani 1 1 d . . . H23 H -0.5524 0.3837 0.2666 0.026 Uiso 1 1 calc R . . C24 C -0.47247(16) 0.27310(14) 0.25208(14) 0.0234(4) Uani 1 1 d . . . C25 C -0.36862(17) 0.23820(13) 0.25357(14) 0.0232(4) Uani 1 1 d . . . H25 H -0.3645 0.1784 0.2428 0.028 Uiso 1 1 calc R . . C26 C -0.26831(15) 0.29156(12) 0.27120(12) 0.0174(3) Uani 1 1 d . . . C27 C -0.16412(15) 0.25158(12) 0.26799(12) 0.0174(3) Uani 1 1 d . . . H27 H -0.1665 0.1911 0.2587 0.021 Uiso 1 1 calc R . . Br2 Br -0.608692(19) 0.201490(17) 0.22362(2) 0.03870(6) Uani 1 1 d . . . N6 N 0.5000 0.0000 0.5000 0.0209(4) Uani 1 2 d S . . C30 C 0.5318(4) 0.0444(3) 0.4229(3) 0.0230(8) Uani 0.506(4) 1 d P A 1 H30A H 0.4589 0.0702 0.3728 0.028 Uiso 0.506(4) 1 calc PR A 1 H30B H 0.5652 0.0017 0.3938 0.028 Uiso 0.506(4) 1 calc PR A 1 C31 C 0.6289(3) 0.11711(16) 0.4757(3) 0.0535(9) Uani 1 1 d . A 1 H31A H 0.6526 0.1456 0.4305 0.080 Uiso 1 1 calc R A 1 H31B H 0.6998 0.0908 0.5259 0.080 Uiso 1 1 calc R A 1 H31C H 0.5941 0.1595 0.5031 0.080 Uiso 1 1 calc R A 1 C32 C 0.4052(3) -0.0649(2) 0.4451(3) 0.0201(8) Uani 0.494(4) 1 d P . 2 H32A H 0.4361 -0.1056 0.4122 0.024 Uiso 0.494(4) 1 calc PR A 2 H32B H 0.3331 -0.0358 0.3976 0.024 Uiso 0.494(4) 1 calc PR A 2 C40 C 0.6048(3) -0.0307(3) 0.5788(3) 0.0260(9) Uani 0.506(4) 1 d P A 3 H40A H 0.5816 -0.0529 0.6279 0.031 Uiso 0.506(4) 1 calc PR A 3 H40B H 0.6621 0.0173 0.6063 0.031 Uiso 0.506(4) 1 calc PR A 3 C41 C 0.6708(2) -0.10890(19) 0.5450(3) 0.0532(8) Uani 1 1 d . A 3 H41A H 0.7419 -0.1295 0.5996 0.080 Uiso 1 1 calc R A 3 H41B H 0.6951 -0.0866 0.4973 0.080 Uiso 1 1 calc R A 3 H41C H 0.6142 -0.1566 0.5181 0.080 Uiso 1 1 calc R A 3 C42 C 0.4410(4) 0.0725(3) 0.5363(3) 0.0235(9) Uani 0.494(4) 1 d P . 4 H42A H 0.4184 0.0484 0.5850 0.028 Uiso 0.494(4) 1 calc PR A 4 H42B H 0.4999 0.1192 0.5656 0.028 Uiso 0.494(4) 1 calc PR A 4 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 Ru 0.01666(8) 0.01254(8) 0.01208(8) 0.00086(6) 0.00803(6) 0.00251(6) C1 0.0151(7) 0.0181(7) 0.0151(7) 0.0011(6) 0.0057(6) 0.0047(6) N1 0.0174(7) 0.0272(8) 0.0170(7) 0.0043(6) 0.0080(6) 0.0040(6) C4 0.0225(8) 0.0271(9) 0.0184(8) 0.0038(7) 0.0119(7) 0.0013(7) N4 0.0228(8) 0.0519(12) 0.0235(8) 0.0082(8) 0.0103(7) 0.0002(8) C5 0.0342(10) 0.0200(9) 0.0177(8) 0.0005(7) 0.0146(8) 0.0029(7) N5 0.0667(14) 0.0190(8) 0.0294(10) -0.0009(7) 0.0239(10) 0.0061(9) Mn 0.01193(10) 0.01280(11) 0.01384(11) -0.00047(9) 0.00710(9) -0.00001(8) O1 0.0380(8) 0.0147(6) 0.0144(6) 0.0010(5) 0.0069(5) -0.0039(6) C10 0.0243(9) 0.0326(10) 0.0151(8) 0.0004(7) 0.0058(7) -0.0048(8) N2 0.0140(6) 0.0150(6) 0.0145(6) 0.0009(5) 0.0069(5) 0.0017(5) O2 0.0151(5) 0.0142(5) 0.0234(6) -0.0017(5) 0.0103(5) -0.0016(4) N3 0.0140(6) 0.0157(7) 0.0152(6) -0.0020(5) 0.0071(5) 0.0002(5) O3 0.0156(5) 0.0179(6) 0.0234(6) -0.0025(5) 0.0123(5) -0.0010(4) C2 0.0164(7) 0.0181(8) 0.0192(8) -0.0038(6) 0.0101(6) 0.0002(6) C3 0.0158(7) 0.0161(8) 0.0227(8) -0.0041(6) 0.0095(6) 0.0002(6) C11 0.0166(7) 0.0149(7) 0.0164(7) 0.0026(6) 0.0081(6) -0.0012(6) C12 0.0211(8) 0.0163(8) 0.0234(9) -0.0019(7) 0.0111(7) -0.0015(6) C13 0.0245(9) 0.0159(8) 0.0242(9) -0.0018(7) 0.0098(7) -0.0040(7) C14 0.0165(7) 0.0190(8) 0.0230(9) 0.0032(7) 0.0054(6) -0.0050(6) C15 0.0162(7) 0.0191(8) 0.0219(8) 0.0032(7) 0.0078(6) -0.0008(6) C16 0.0152(7) 0.0157(8) 0.0164(7) 0.0018(6) 0.0073(6) -0.0010(6) C17 0.0147(7) 0.0184(8) 0.0156(7) 0.0022(6) 0.0081(6) 0.0013(6) Br1 0.01727(8) 0.02242(9) 0.03659(11) 0.00025(8) 0.00558(8) -0.00608(7) C21 0.0155(7) 0.0207(8) 0.0127(7) 0.0006(6) 0.0076(6) 0.0001(6) C22 0.0183(8) 0.0221(8) 0.0204(8) 0.0021(7) 0.0111(7) 0.0024(6) C23 0.0153(8) 0.0326(10) 0.0203(8) 0.0030(7) 0.0100(7) 0.0029(7) C24 0.0143(8) 0.0328(10) 0.0239(9) -0.0051(8) 0.0090(7) -0.0068(7) C25 0.0178(8) 0.0257(9) 0.0277(9) -0.0081(7) 0.0113(7) -0.0063(7) C26 0.0146(7) 0.0212(8) 0.0176(8) -0.0037(6) 0.0081(6) -0.0024(6) C27 0.0176(7) 0.0168(8) 0.0182(8) -0.0044(6) 0.0081(6) -0.0020(6) Br2 0.01983(10) 0.04573(14) 0.05529(15) -0.01827(11) 0.02062(10) -0.01488(9) N6 0.0187(10) 0.0231(11) 0.0244(11) -0.0075(9) 0.0126(8) -0.0072(8) C30 0.0277(19) 0.0233(18) 0.0231(18) -0.0010(14) 0.0157(15) -0.0039(14) C31 0.0453(15) 0.0203(10) 0.120(3) -0.0076(14) 0.0589(18) -0.0100(10) C32 0.0186(16) 0.0181(17) 0.0241(18) -0.0076(13) 0.0094(14) -0.0065(13) C40 0.0181(17) 0.0262(19) 0.029(2) 0.0048(15) 0.0056(14) -0.0026(14) C41 0.0216(11) 0.0467(16) 0.086(2) 0.0229(15) 0.0175(13) 0.0035(10) C42 0.0222(18) 0.0216(18) 0.032(2) -0.0095(15) 0.0160(16) -0.0056(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C1 2.0447(17) . ? Ru C1 2.0448(18) 3_565 ? Ru C5 2.049(2) . ? Ru C5 2.049(2) 3_565 ? Ru C4 2.0613(19) . ? Ru C4 2.0613(19) 3_565 ? C1 N1 1.156(2) . ? N1 Mn 2.2499(16) . ? C4 N4 1.161(3) . ? C5 N5 1.149(3) . ? Mn O2 1.8850(13) . ? Mn O3 1.8866(12) . ? Mn N2 1.9940(14) . ? Mn N3 2.0041(15) . ? Mn O1 2.2380(14) . ? O1 C10 1.424(2) . ? O1 H1 0.799(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N2 C17 1.287(2) . ? N2 C2 1.472(2) . ? O2 C11 1.319(2) . ? N3 C27 1.285(2) . ? N3 C3 1.480(2) . ? O3 C21 1.311(2) . ? C2 C3 1.519(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C11 C12 1.412(2) . ? C11 C16 1.420(2) . ? C12 C13 1.378(3) . ? C12 H12 0.9500 . ? C13 C14 1.398(3) . ? C13 H13 0.9500 . ? C14 C15 1.373(3) . ? C14 Br1 1.9014(18) . ? C15 C16 1.412(2) . ? C15 H15 0.9500 . ? C16 C17 1.443(2) . ? C17 H17 0.9500 . ? C21 C22 1.415(2) . ? C21 C26 1.422(3) . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 C25 1.379(3) . ? C24 Br2 1.8989(19) . ? C25 C26 1.412(2) . ? C25 H25 0.9500 . ? C26 C27 1.444(2) . ? C27 H27 0.9500 . ? N6 C40 1.433(4) 3_656 ? N6 C40 1.433(4) . ? N6 C32 1.504(3) . ? N6 C32 1.504(4) 3_656 ? N6 C42 1.573(4) 3_656 ? N6 C42 1.573(4) . ? N6 C30 1.580(4) 3_656 ? N6 C30 1.580(4) . ? C30 C31 1.595(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C31 1.681(5) 3_656 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C40 C41 1.669(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C41 1.529(5) 3_656 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru C1 180.00(4) . 3_565 ? C1 Ru C5 93.00(7) . . ? C1 Ru C5 87.00(7) 3_565 . ? C1 Ru C5 87.00(7) . 3_565 ? C1 Ru C5 93.00(7) 3_565 3_565 ? C5 Ru C5 180.0 . 3_565 ? C1 Ru C4 89.26(7) . . ? C1 Ru C4 90.74(7) 3_565 . ? C5 Ru C4 90.44(8) . . ? C5 Ru C4 89.56(8) 3_565 . ? C1 Ru C4 90.74(7) . 3_565 ? C1 Ru C4 89.26(7) 3_565 3_565 ? C5 Ru C4 89.56(8) . 3_565 ? C5 Ru C4 90.44(8) 3_565 3_565 ? C4 Ru C4 180.0 . 3_565 ? N1 C1 Ru 175.86(16) . . ? C1 N1 Mn 144.12(14) . . ? N4 C4 Ru 179.6(2) . . ? N5 C5 Ru 177.55(17) . . ? O2 Mn O3 94.88(5) . . ? O2 Mn N2 91.88(6) . . ? O3 Mn N2 173.02(6) . . ? O2 Mn N3 169.86(6) . . ? O3 Mn N3 91.75(6) . . ? N2 Mn N3 81.79(6) . . ? O2 Mn O1 88.03(5) . . ? O3 Mn O1 92.23(6) . . ? N2 Mn O1 89.74(6) . . ? N3 Mn O1 84.04(6) . . ? O2 Mn N1 91.91(6) . . ? O3 Mn N1 93.84(6) . . ? N2 Mn N1 84.18(6) . . ? N3 Mn N1 95.30(6) . . ? O1 Mn N1 173.91(6) . . ? C10 O1 Mn 130.05(12) . . ? C10 O1 H1 108(2) . . ? Mn O1 H1 119(2) . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C17 N2 C2 120.85(14) . . ? C17 N2 Mn 126.18(12) . . ? C2 N2 Mn 112.78(10) . . ? C11 O2 Mn 128.03(11) . . ? C27 N3 C3 119.87(15) . . ? C27 N3 Mn 126.22(12) . . ? C3 N3 Mn 113.35(11) . . ? C21 O3 Mn 129.71(11) . . ? N2 C2 C3 106.77(14) . . ? N2 C2 H2A 110.4 . . ? C3 C2 H2A 110.4 . . ? N2 C2 H2B 110.4 . . ? C3 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N3 C3 C2 107.28(14) . . ? N3 C3 H3A 110.3 . . ? C2 C3 H3A 110.3 . . ? N3 C3 H3B 110.3 . . ? C2 C3 H3B 110.3 . . ? H3A C3 H3B 108.5 . . ? O2 C11 C12 118.41(16) . . ? O2 C11 C16 123.76(16) . . ? C12 C11 C16 117.83(16) . . ? C13 C12 C11 121.33(17) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 119.91(17) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.77(17) . . ? C15 C14 Br1 119.25(14) . . ? C13 C14 Br1 119.98(14) . . ? C14 C15 C16 119.92(17) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.10(16) . . ? C15 C16 C17 116.95(15) . . ? C11 C16 C17 122.92(15) . . ? N2 C17 C16 124.67(15) . . ? N2 C17 H17 117.7 . . ? C16 C17 H17 117.7 . . ? O3 C21 C22 117.97(16) . . ? O3 C21 C26 124.22(15) . . ? C22 C21 C26 117.80(16) . . ? C23 C22 C21 121.33(18) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 119.89(17) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.99(17) . . ? C25 C24 Br2 119.43(16) . . ? C23 C24 Br2 119.57(14) . . ? C24 C25 C26 119.86(18) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.08(16) . . ? C25 C26 C27 117.03(17) . . ? C21 C26 C27 122.88(16) . . ? N3 C27 C26 125.01(17) . . ? N3 C27 H27 117.5 . . ? C26 C27 H27 117.5 . . ? C40 N6 C40 179.999(1) 3_656 . ? C40 N6 C32 62.5(2) 3_656 . ? C40 N6 C32 117.5(2) . . ? C40 N6 C32 117.5(2) 3_656 3_656 ? C40 N6 C32 62.5(2) . 3_656 ? C32 N6 C32 180.0 . 3_656 ? C40 N6 C42 108.1(2) 3_656 3_656 ? C40 N6 C42 71.9(2) . 3_656 ? C32 N6 C42 71.2(2) . 3_656 ? C32 N6 C42 108.8(2) 3_656 3_656 ? C40 N6 C42 71.9(2) 3_656 . ? C40 N6 C42 108.1(2) . . ? C32 N6 C42 108.8(2) . . ? C32 N6 C42 71.2(2) 3_656 . ? C42 N6 C42 179.999(2) 3_656 . ? C40 N6 C30 112.3(2) 3_656 3_656 ? C40 N6 C30 67.7(2) . 3_656 ? C32 N6 C30 76.1(2) . 3_656 ? C32 N6 C30 103.9(2) 3_656 3_656 ? C42 N6 C30 105.5(2) 3_656 3_656 ? C42 N6 C30 74.5(2) . 3_656 ? C40 N6 C30 67.7(2) 3_656 . ? C40 N6 C30 112.3(2) . . ? C32 N6 C30 103.9(2) . . ? C32 N6 C30 76.1(2) 3_656 . ? C42 N6 C30 74.5(2) 3_656 . ? C42 N6 C30 105.5(2) . . ? C30 N6 C30 180.00(15) 3_656 . ? N6 C30 C31 106.8(3) . . ? N6 C30 H30A 110.4 . . ? C31 C30 H30A 110.4 . . ? N6 C30 H30B 110.4 . . ? C31 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 C31 106.1(2) . 3_656 ? N6 C32 H32A 110.5 . . ? C31 C32 H32A 110.5 3_656 . ? N6 C32 H32B 110.5 . . ? C31 C32 H32B 110.5 3_656 . ? H32A C32 H32B 108.7 . . ? N6 C40 C41 110.4(3) . . ? N6 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? N6 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 C42 N6 110.7(3) 3_656 . ? C41 C42 H42A 109.5 3_656 . ? N6 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 3_656 . ? N6 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N5 0.799(17) 1.898(17) 2.693(2) 173(3) 2_545 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 32.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.073 _refine_diff_density_min -1.464 _refine_diff_density_rms 0.089