# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Martin Albrecht' _publ_contact_author_email MARTIN.ALBRECHT@UNIFR.CH _publ_section_title ; Probing the potential of N-heterocyclic carbenes in molecular electronics: Redox-active metal centers interlinked by a rigid ditopic carbene ligand ; loop_ _publ_author_name 'Martin Albrecht' 'Laszlo Mercs' 'Antonia Neels' # Attachment 'B809721F_compound2.CIF' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 680401' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H56 Cl8 Fe2 I2 N4 O2' _chemical_formula_weight 1273.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3269(10) _cell_length_b 12.2366(6) _cell_length_c 18.2520(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.195(7) _cell_angle_gamma 90.00 _cell_volume 2503.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20601 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 29.53 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max .45 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 2.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.384 _exptl_absorpt_correction_T_max 0.726 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27277 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29.28 _reflns_number_total 6768 _reflns_number_gt 5292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+3.0299P] 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 6768 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 C1 C 0.9370(3) 0.4029(3) 0.16029(17) 0.0191(6) Uani 1 1 d . . . C2 C 0.9172(3) 0.4810(3) 0.04603(17) 0.0206(6) Uani 1 1 d . . . C3 C 1.0382(3) 0.4546(3) 0.06715(17) 0.0199(6) Uani 1 1 d . . . C4 C 1.1559(3) 0.3555(3) 0.17356(18) 0.0229(6) Uani 1 1 d . . . H4A H 1.1938 0.3152 0.1361 0.027 Uiso 1 1 calc R . . H4B H 1.1355 0.3018 0.2103 0.027 Uiso 1 1 calc R . . C5 C 1.2454(3) 0.4367(3) 0.2124(2) 0.0267(7) Uani 1 1 d . . . H5A H 1.2035 0.4890 0.2411 0.032 Uiso 1 1 calc R . . H5B H 1.2819 0.4785 0.1750 0.032 Uiso 1 1 calc R . . C6 C 1.3432(3) 0.3787(4) 0.2644(2) 0.0357(9) Uani 1 1 d . . . H6A H 1.3061 0.3295 0.2977 0.043 Uiso 1 1 calc R . . H6B H 1.3914 0.3334 0.2349 0.043 Uiso 1 1 calc R . . C7 C 1.4243(4) 0.4595(5) 0.3107(3) 0.0507(12) Uani 1 1 d . . . H7A H 1.4547 0.5131 0.2781 0.076 Uiso 1 1 calc R . . H7B H 1.4914 0.4202 0.3388 0.076 Uiso 1 1 calc R . . H7C H 1.3792 0.4974 0.3451 0.076 Uiso 1 1 calc R . . C8 C 0.7282(3) 0.4484(3) 0.09917(19) 0.0254(7) Uani 1 1 d . . . H8A H 0.7057 0.4076 0.1419 0.031 Uiso 1 1 calc R . . H8B H 0.6949 0.4084 0.0538 0.031 Uiso 1 1 calc R . . C9 C 0.6709(3) 0.5598(3) 0.0972(2) 0.0307(8) Uani 1 1 d . . . H9A H 0.6777 0.5960 0.0495 0.037 Uiso 1 1 calc R . . H9B H 0.7125 0.6057 0.1376 0.037 Uiso 1 1 calc R . . C10 C 0.5395(4) 0.5483(4) 0.1065(2) 0.0362(9) Uani 1 1 d . . . H10A H 0.4987 0.5035 0.0653 0.043 Uiso 1 1 calc R . . H10B H 0.5338 0.5089 0.1532 0.043 Uiso 1 1 calc R . . C11 C 0.4759(5) 0.6556(4) 0.1077(4) 0.0553(13) Uani 1 1 d . . . H11A H 0.5059 0.6950 0.1533 0.083 Uiso 1 1 calc R . . H11B H 0.3901 0.6427 0.1057 0.083 Uiso 1 1 calc R . . H11C H 0.4900 0.6994 0.0648 0.083 Uiso 1 1 calc R . . C12 C 0.8751(3) 0.5273(3) -0.02206(18) 0.0211(6) Uani 1 1 d . . . H12 H 0.7935 0.5452 -0.0366 0.025 Uiso 1 1 calc R . . C14 C 0.7949(4) 0.2114(3) 0.1964(2) 0.0372(9) Uani 1 1 d . . . H14 H 0.7528 0.2156 0.1476 0.045 Uiso 1 1 calc R . . C15 C 0.7487(4) 0.2363(4) 0.2607(3) 0.0419(10) Uani 1 1 d . . . H15 H 0.6700 0.2613 0.2633 0.050 Uiso 1 1 calc R . . C16 C 0.8381(5) 0.2184(4) 0.3215(2) 0.0437(11) Uani 1 1 d . . . H16 H 0.8310 0.2292 0.3723 0.052 Uiso 1 1 calc R . . C17 C 0.9404(4) 0.1814(3) 0.2927(3) 0.0398(10) Uani 1 1 d . . . H17 H 1.0143 0.1616 0.3210 0.048 Uiso 1 1 calc R . . C18 C 0.9141(4) 0.1790(3) 0.2152(2) 0.0364(9) Uani 1 1 d . . . H18 H 0.9673 0.1591 0.1817 0.044 Uiso 1 1 calc R . . C19 C 0.8588(4) 0.0905(4) -0.0012(3) 0.0449(11) Uani 1 1 d . . . H19A H 0.8669 0.0374 0.0402 0.054 Uiso 1 1 calc R . . H19B H 0.8664 0.0498 -0.0472 0.054 Uiso 1 1 calc R . . C20 C 0.4092(5) 0.1325(5) 0.0620(3) 0.0511(12) Uani 1 1 d . . . H20A H 0.4730 0.0883 0.0446 0.061 Uiso 1 1 calc R . . H20B H 0.3767 0.0904 0.1009 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.71726(13) 0.15156(14) -0.00948(8) 0.0609(4) Uani 1 1 d . . . Cl2 Cl 0.97373(14) 0.18751(13) 0.01496(8) 0.0612(4) Uani 1 1 d . . . Cl3 Cl 0.46930(14) 0.25563(15) 0.09923(9) 0.0704(4) Uani 1 1 d . . . Cl4 Cl 0.29670(19) 0.15601(16) -0.01140(11) 0.0949(7) Uani 1 1 d . . . Fe1 Fe 0.89918(4) 0.33758(4) 0.25278(3) 0.02153(11) Uani 1 1 d . . . N1 N 1.0453(2) 0.4061(2) 0.13696(14) 0.0193(5) Uani 1 1 d . . . N2 N 0.8590(2) 0.4486(2) 0.10462(15) 0.0209(5) Uani 1 1 d . . . I1 I 0.78647(2) 0.51207(2) 0.293424(14) 0.03369(9) Uani 1 1 d . . . C13 C 1.0245(4) 0.3889(3) 0.31166(19) 0.0347(5) Uani 1 1 d . . . O1 O 1.0914(3) 0.4140(2) 0.35176(13) 0.0347(5) 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 C1 0.0228(15) 0.0211(15) 0.0137(13) 0.0003(11) 0.0031(11) -0.0015(12) C2 0.0212(14) 0.0250(16) 0.0160(13) 0.0020(12) 0.0038(11) 0.0005(12) C3 0.0213(15) 0.0229(15) 0.0156(13) 0.0028(11) 0.0031(11) 0.0003(12) C4 0.0239(15) 0.0249(16) 0.0189(14) 0.0037(12) -0.0001(12) 0.0043(13) C5 0.0235(16) 0.0300(18) 0.0258(16) 0.0043(14) 0.0008(13) -0.0008(14) C6 0.0274(18) 0.044(2) 0.0330(19) -0.0008(17) -0.0050(15) 0.0086(16) C7 0.035(2) 0.067(3) 0.045(3) -0.001(2) -0.0110(19) -0.004(2) C8 0.0213(15) 0.0351(19) 0.0202(15) 0.0057(14) 0.0039(12) -0.0004(14) C9 0.0263(17) 0.037(2) 0.0302(18) 0.0085(15) 0.0083(14) 0.0071(15) C10 0.0285(19) 0.044(2) 0.037(2) 0.0012(18) 0.0081(16) 0.0029(17) C11 0.041(2) 0.048(3) 0.081(4) 0.005(3) 0.023(3) 0.011(2) C12 0.0194(14) 0.0250(16) 0.0190(14) 0.0030(12) 0.0030(11) 0.0028(12) C14 0.049(2) 0.030(2) 0.0299(19) 0.0031(15) -0.0032(17) -0.0104(18) C15 0.035(2) 0.031(2) 0.063(3) 0.001(2) 0.018(2) -0.0127(17) C16 0.077(3) 0.034(2) 0.0240(18) 0.0039(16) 0.018(2) -0.020(2) C17 0.046(2) 0.0233(18) 0.046(2) 0.0146(17) -0.0060(19) -0.0031(17) C18 0.049(2) 0.0222(18) 0.042(2) -0.0031(16) 0.0179(18) -0.0060(16) C19 0.053(3) 0.036(2) 0.043(2) -0.0023(19) -0.002(2) 0.002(2) C20 0.047(3) 0.056(3) 0.049(3) 0.010(2) 0.001(2) -0.009(2) Cl1 0.0555(7) 0.0746(9) 0.0540(7) 0.0003(6) 0.0124(6) 0.0171(7) Cl2 0.0681(8) 0.0652(8) 0.0482(7) -0.0093(6) 0.0013(6) -0.0184(7) Cl3 0.0652(9) 0.0833(11) 0.0619(8) -0.0280(8) 0.0070(7) -0.0186(8) Cl4 0.1016(13) 0.0788(11) 0.0862(12) 0.0340(9) -0.0492(10) -0.0440(10) Fe1 0.0262(2) 0.0233(2) 0.0155(2) 0.00222(17) 0.00446(17) -0.00190(18) N1 0.0195(12) 0.0232(13) 0.0149(12) 0.0038(10) 0.0014(10) 0.0011(10) N2 0.0180(12) 0.0277(14) 0.0177(12) 0.0042(11) 0.0049(10) 0.0001(11) I1 0.03924(15) 0.03519(15) 0.02805(13) -0.00160(10) 0.00966(10) 0.00446(11) C13 0.0627(16) 0.0297(11) 0.0132(9) 0.0018(8) 0.0104(9) 0.0021(11) O1 0.0627(16) 0.0297(11) 0.0132(9) 0.0018(8) 0.0104(9) 0.0021(11) _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 C1 N1 1.356(4) . ? C1 N2 1.367(4) . ? C1 Fe1 1.969(3) . ? C2 C12 1.387(4) . ? C2 N2 1.391(4) . ? C2 C3 1.407(4) . ? C3 C12 1.386(4) 3_765 ? C3 N1 1.398(4) . ? C4 N1 1.470(4) . ? C4 C5 1.521(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.521(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N2 1.471(4) . ? C8 C9 1.508(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.500(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C3 1.386(4) 3_765 ? C12 H12 0.9500 . ? C14 C15 1.386(7) . ? C14 C18 1.402(6) . ? C14 Fe1 2.119(4) . ? C14 H14 0.9500 . ? C15 C16 1.410(7) . ? C15 Fe1 2.129(4) . ? C15 H15 0.9500 . ? C16 C17 1.413(7) . ? C16 Fe1 2.104(4) . ? C16 H16 0.9500 . ? C17 C18 1.404(6) . ? C17 Fe1 2.074(4) . ? C17 H17 0.9500 . ? C18 Fe1 2.072(4) . ? C18 H18 0.9500 . ? C19 Cl2 1.755(5) . ? C19 Cl1 1.756(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 Cl4 1.736(5) . ? C20 Cl3 1.751(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? Fe1 C13 1.769(5) . ? Fe1 I1 2.6475(6) . ? C13 O1 1.023(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 C1 N2 105.8(3) . . ? N1 C1 Fe1 126.7(2) . . ? N2 C1 Fe1 127.4(2) . . ? C12 C2 N2 131.7(3) . . ? C12 C2 C3 122.4(3) . . ? N2 C2 C3 105.9(3) . . ? C12 C3 N1 131.0(3) 3_765 . ? C12 C3 C2 123.1(3) 3_765 . ? N1 C3 C2 105.9(3) . . ? N1 C4 C5 113.9(3) . . ? N1 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 111.3(3) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 111.8(4) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 115.2(3) . . ? N2 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? N2 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 C9 C10 109.7(3) . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 113.5(4) . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 C12 C2 114.5(3) 3_765 . ? C3 C12 H12 122.7 3_765 . ? C2 C12 H12 122.7 . . ? C15 C14 C18 108.7(4) . . ? C15 C14 Fe1 71.3(2) . . ? C18 C14 Fe1 68.7(2) . . ? C15 C14 H14 125.6 . . ? C18 C14 H14 125.6 . . ? Fe1 C14 H14 125.9 . . ? C14 C15 C16 108.5(4) . . ? C14 C15 Fe1 70.6(2) . . ? C16 C15 Fe1 69.6(2) . . ? C14 C15 H15 125.8 . . ? C16 C15 H15 125.8 . . ? Fe1 C15 H15 125.6 . . ? C15 C16 C17 107.0(4) . . ? C15 C16 Fe1 71.5(2) . . ? C17 C16 Fe1 69.1(2) . . ? C15 C16 H16 126.5 . . ? C17 C16 H16 126.5 . . ? Fe1 C16 H16 124.5 . . ? C18 C17 C16 108.3(4) . . ? C18 C17 Fe1 70.1(2) . . ? C16 C17 Fe1 71.4(2) . . ? C18 C17 H17 125.8 . . ? C16 C17 H17 125.8 . . ? Fe1 C17 H17 124.3 . . ? C14 C18 C17 107.4(4) . . ? C14 C18 Fe1 72.3(2) . . ? C17 C18 Fe1 70.3(2) . . ? C14 C18 H18 126.3 . . ? C17 C18 H18 126.3 . . ? Fe1 C18 H18 122.8 . . ? Cl2 C19 Cl1 111.9(3) . . ? Cl2 C19 H19A 109.2 . . ? Cl1 C19 H19A 109.2 . . ? Cl2 C19 H19B 109.2 . . ? Cl1 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? Cl4 C20 Cl3 111.0(3) . . ? Cl4 C20 H20A 109.4 . . ? Cl3 C20 H20A 109.4 . . ? Cl4 C20 H20B 109.4 . . ? Cl3 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C13 Fe1 C1 97.07(15) . . ? C13 Fe1 C18 115.93(19) . . ? C1 Fe1 C18 93.36(15) . . ? C13 Fe1 C17 89.59(18) . . ? C1 Fe1 C17 127.57(17) . . ? C18 Fe1 C17 39.57(18) . . ? C13 Fe1 C16 100.80(18) . . ? C1 Fe1 C16 157.32(15) . . ? C18 Fe1 C16 66.27(17) . . ? C17 Fe1 C16 39.5(2) . . ? C13 Fe1 C14 153.80(18) . . ? C1 Fe1 C14 93.07(15) . . ? C18 Fe1 C14 39.07(18) . . ? C17 Fe1 C14 65.27(17) . . ? C16 Fe1 C14 64.97(17) . . ? C13 Fe1 C15 138.28(19) . . ? C1 Fe1 C15 124.63(17) . . ? C18 Fe1 C15 65.27(18) . . ? C17 Fe1 C15 65.32(19) . . ? C16 Fe1 C15 38.9(2) . . ? C14 Fe1 C15 38.07(18) . . ? C13 Fe1 I1 85.43(14) . . ? C1 Fe1 I1 94.89(10) . . ? C18 Fe1 I1 155.92(13) . . ? C17 Fe1 I1 137.53(14) . . ? C16 Fe1 I1 100.32(14) . . ? C14 Fe1 I1 117.77(13) . . ? C15 Fe1 I1 91.57(13) . . ? C1 N1 C3 111.2(3) . . ? C1 N1 C4 126.6(3) . . ? C3 N1 C4 121.9(3) . . ? C1 N2 C2 111.2(3) . . ? C1 N2 C8 126.0(3) . . ? C2 N2 C8 122.1(3) . . ? O1 C13 Fe1 171.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C2 C3 C12 0.1(6) . . . 3_765 ? N2 C2 C3 C12 178.6(3) . . . 3_765 ? C12 C2 C3 N1 -177.6(3) . . . . ? N2 C2 C3 N1 0.9(4) . . . . ? N1 C4 C5 C6 166.1(3) . . . . ? C4 C5 C6 C7 -172.9(4) . . . . ? N2 C8 C9 C10 -169.2(3) . . . . ? C8 C9 C10 C11 178.1(4) . . . . ? N2 C2 C12 C3 -178.2(3) . . . 3_765 ? C3 C2 C12 C3 -0.1(6) . . . 3_765 ? C18 C14 C15 C16 -0.8(5) . . . . ? Fe1 C14 C15 C16 -59.5(3) . . . . ? C18 C14 C15 Fe1 58.6(3) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? Fe1 C15 C16 C17 -60.3(3) . . . . ? C14 C15 C16 Fe1 60.1(3) . . . . ? C15 C16 C17 C18 1.2(5) . . . . ? Fe1 C16 C17 C18 -60.7(3) . . . . ? C15 C16 C17 Fe1 61.9(3) . . . . ? C15 C14 C18 C17 1.6(5) . . . . ? Fe1 C14 C18 C17 61.9(3) . . . . ? C15 C14 C18 Fe1 -60.3(3) . . . . ? C16 C17 C18 C14 -1.7(5) . . . . ? Fe1 C17 C18 C14 -63.2(3) . . . . ? C16 C17 C18 Fe1 61.5(3) . . . . ? N1 C1 Fe1 C13 43.5(3) . . . . ? N2 C1 Fe1 C13 -140.5(3) . . . . ? N1 C1 Fe1 C18 -73.1(3) . . . . ? N2 C1 Fe1 C18 102.8(3) . . . . ? N1 C1 Fe1 C17 -51.4(4) . . . . ? N2 C1 Fe1 C17 124.5(3) . . . . ? N1 C1 Fe1 C16 -98.3(5) . . . . ? N2 C1 Fe1 C16 77.6(6) . . . . ? N1 C1 Fe1 C14 -112.3(3) . . . . ? N2 C1 Fe1 C14 63.7(3) . . . . ? N1 C1 Fe1 C15 -135.2(3) . . . . ? N2 C1 Fe1 C15 40.8(4) . . . . ? N1 C1 Fe1 I1 129.5(3) . . . . ? N2 C1 Fe1 I1 -54.5(3) . . . . ? C14 C18 Fe1 C13 169.7(2) . . . . ? C17 C18 Fe1 C13 53.1(3) . . . . ? C14 C18 Fe1 C1 -90.7(3) . . . . ? C17 C18 Fe1 C1 152.6(3) . . . . ? C14 C18 Fe1 C17 116.7(4) . . . . ? C14 C18 Fe1 C16 78.9(3) . . . . ? C17 C18 Fe1 C16 -37.7(3) . . . . ? C17 C18 Fe1 C14 -116.7(4) . . . . ? C14 C18 Fe1 C15 36.1(3) . . . . ? C17 C18 Fe1 C15 -80.5(3) . . . . ? C14 C18 Fe1 I1 19.2(5) . . . . ? C17 C18 Fe1 I1 -97.5(4) . . . . ? C18 C17 Fe1 C13 -134.0(3) . . . . ? C16 C17 Fe1 C13 107.6(3) . . . . ? C18 C17 Fe1 C1 -35.4(3) . . . . ? C16 C17 Fe1 C1 -153.7(2) . . . . ? C16 C17 Fe1 C18 -118.3(4) . . . . ? C18 C17 Fe1 C16 118.3(4) . . . . ? C18 C17 Fe1 C14 38.3(3) . . . . ? C16 C17 Fe1 C14 -80.0(3) . . . . ? C18 C17 Fe1 C15 80.4(3) . . . . ? C16 C17 Fe1 C15 -37.9(3) . . . . ? C18 C17 Fe1 I1 143.2(2) . . . . ? C16 C17 Fe1 I1 24.9(3) . . . . ? C15 C16 Fe1 C13 166.8(3) . . . . ? C17 C16 Fe1 C13 -76.0(3) . . . . ? C15 C16 Fe1 C1 -51.8(6) . . . . ? C17 C16 Fe1 C1 65.4(6) . . . . ? C15 C16 Fe1 C18 -79.5(3) . . . . ? C17 C16 Fe1 C18 37.8(3) . . . . ? C15 C16 Fe1 C17 -117.2(4) . . . . ? C15 C16 Fe1 C14 -36.4(3) . . . . ? C17 C16 Fe1 C14 80.8(3) . . . . ? C17 C16 Fe1 C15 117.2(4) . . . . ? C15 C16 Fe1 I1 79.6(3) . . . . ? C17 C16 Fe1 I1 -163.2(2) . . . . ? C15 C14 Fe1 C13 98.5(5) . . . . ? C18 C14 Fe1 C13 -21.3(5) . . . . ? C15 C14 Fe1 C1 -148.7(3) . . . . ? C18 C14 Fe1 C1 91.6(3) . . . . ? C15 C14 Fe1 C18 119.7(4) . . . . ? C15 C14 Fe1 C17 80.9(3) . . . . ? C18 C14 Fe1 C17 -38.8(3) . . . . ? C15 C14 Fe1 C16 37.2(3) . . . . ? C18 C14 Fe1 C16 -82.6(3) . . . . ? C18 C14 Fe1 C15 -119.7(4) . . . . ? C15 C14 Fe1 I1 -51.5(3) . . . . ? C18 C14 Fe1 I1 -171.3(2) . . . . ? C14 C15 Fe1 C13 -139.0(3) . . . . ? C16 C15 Fe1 C13 -19.7(4) . . . . ? C14 C15 Fe1 C1 39.1(3) . . . . ? C16 C15 Fe1 C1 158.4(3) . . . . ? C14 C15 Fe1 C18 -37.1(3) . . . . ? C16 C15 Fe1 C18 82.3(3) . . . . ? C14 C15 Fe1 C17 -80.8(3) . . . . ? C16 C15 Fe1 C17 38.5(3) . . . . ? C14 C15 Fe1 C16 -119.3(4) . . . . ? C16 C15 Fe1 C14 119.3(4) . . . . ? C14 C15 Fe1 I1 136.1(3) . . . . ? C16 C15 Fe1 I1 -104.6(3) . . . . ? N2 C1 N1 C3 0.7(4) . . . . ? Fe1 C1 N1 C3 177.4(2) . . . . ? N2 C1 N1 C4 -172.6(3) . . . . ? Fe1 C1 N1 C4 4.1(5) . . . . ? C12 C3 N1 C1 -178.5(4) 3_765 . . . ? C2 C3 N1 C1 -1.1(4) . . . . ? C12 C3 N1 C4 -4.8(6) 3_765 . . . ? C2 C3 N1 C4 172.6(3) . . . . ? C5 C4 N1 C1 -106.1(4) . . . . ? C5 C4 N1 C3 81.2(4) . . . . ? N1 C1 N2 C2 -0.1(4) . . . . ? Fe1 C1 N2 C2 -176.7(2) . . . . ? N1 C1 N2 C8 170.1(3) . . . . ? Fe1 C1 N2 C8 -6.5(5) . . . . ? C12 C2 N2 C1 177.8(4) . . . . ? C3 C2 N2 C1 -0.5(4) . . . . ? C12 C2 N2 C8 7.1(6) . . . . ? C3 C2 N2 C8 -171.2(3) . . . . ? C9 C8 N2 C1 120.1(4) . . . . ? C9 C8 N2 C2 -70.7(4) . . . . ? C1 Fe1 C13 O1 174(3) . . . . ? C18 Fe1 C13 O1 -89(3) . . . . ? C17 Fe1 C13 O1 -58(3) . . . . ? C16 Fe1 C13 O1 -20(3) . . . . ? C14 Fe1 C13 O1 -74(3) . . . . ? C15 Fe1 C13 O1 -8(3) . . . . ? I1 Fe1 C13 O1 80(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.155 _refine_diff_density_min -1.691 _refine_diff_density_rms 0.129 # Attachment 'B809721F_compound3a.CIF' data_compound3a _database_code_depnum_ccdc_archive 'CCDC 680402' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Cl4 N4 Ru2' _chemical_formula_weight 1139.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6954(7) _cell_length_b 7.1268(3) _cell_length_c 34.419(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.422(5) _cell_angle_gamma 90.00 _cell_volume 2868.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34484 _cell_measurement_theta_min 1.18 _cell_measurement_theta_max 25.68 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.269 _exptl_absorpt_correction_T_max 0.720 _exptl_absorpt_process_details 'DELrefABS, (PLATON03, Speck, 2003)' _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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28304 _diffrn_reflns_av_R_equivalents 0.1066 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.15 _reflns_number_total 5106 _reflns_number_gt 4617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+2.7489P] 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 5106 _refine_ls_number_parameters 292 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.115 _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 C1 C 0.4655(3) 0.7484(5) 0.08055(11) 0.0489(9) Uani 1 1 d . . . C2 C 0.5363(3) 0.6394(5) 0.02394(12) 0.0485(9) Uani 1 1 d . . . C3 C 0.4375(3) 0.5379(5) 0.03162(11) 0.0466(8) Uani 1 1 d . . . C4 C 0.2930(3) 0.5302(6) 0.08425(12) 0.0509(9) Uani 1 1 d . . . H4A H 0.2881 0.5789 0.1111 0.061 Uiso 1 1 calc R . . H4B H 0.3018 0.3922 0.0859 0.061 Uiso 1 1 calc R . . C5 C 0.1827(3) 0.5748(6) 0.06234(12) 0.0543(9) Uani 1 1 d . . . H5A H 0.1872 0.5274 0.0354 0.065 Uiso 1 1 calc R . . H5B H 0.1724 0.7126 0.0612 0.065 Uiso 1 1 calc R . . C6 C 0.0808(4) 0.4870(8) 0.08164(16) 0.0724(13) Uani 1 1 d . . . H6A H 0.0838 0.5184 0.1097 0.087 Uiso 1 1 calc R . . H6B H 0.0858 0.3489 0.0792 0.087 Uiso 1 1 calc R . . C7 C -0.0335(4) 0.5524(9) 0.06417(19) 0.0871(16) Uani 1 1 d . . . H7A H -0.0401 0.6888 0.0670 0.131 Uiso 1 1 calc R . . H7B H -0.0960 0.4910 0.0777 0.131 Uiso 1 1 calc R . . H7C H -0.0378 0.5194 0.0365 0.131 Uiso 1 1 calc R . . C8 C 0.6514(3) 0.8864(5) 0.05710(12) 0.0496(9) Uani 1 1 d . . . H8A H 0.7202 0.8093 0.0525 0.059 Uiso 1 1 calc R . . H8B H 0.6584 0.9381 0.0837 0.059 Uiso 1 1 calc R . . C9 C 0.6481(4) 1.0486(6) 0.02811(13) 0.0552(9) Uani 1 1 d . . . H9A H 0.5802 1.1278 0.0327 0.066 Uiso 1 1 calc R . . H9B H 0.6412 0.9982 0.0014 0.066 Uiso 1 1 calc R . . C10 C 0.7563(4) 1.1679(7) 0.03213(16) 0.0700(13) Uani 1 1 d . . . H10A H 0.7448 1.2848 0.0170 0.084 Uiso 1 1 calc R . . H10B H 0.7675 1.2037 0.0598 0.084 Uiso 1 1 calc R . . C11 C 0.8631(6) 1.0731(10) 0.0187(3) 0.119(3) Uani 1 1 d . . . H11A H 0.8825 0.9689 0.0363 0.179 Uiso 1 1 calc R . . H11B H 0.9261 1.1637 0.0189 0.179 Uiso 1 1 calc R . . H11C H 0.8503 1.0249 -0.0077 0.179 Uiso 1 1 calc R . . C12 C 0.6032(4) 0.6068(5) -0.00788(11) 0.0494(9) Uani 1 1 d . . . H12A H 0.6704 0.6763 -0.0131 0.059 Uiso 1 1 calc R . . C13 C 0.4128(4) 0.8866(6) 0.19800(12) 0.0566(10) Uani 1 1 d . . . C14 C 0.5190(4) 0.9680(6) 0.19262(12) 0.0588(10) Uani 1 1 d . . . H14A H 0.5343 1.0888 0.2032 0.071 Uiso 1 1 calc R . . C15 C 0.6065(4) 0.8739(6) 0.17138(13) 0.0588(10) Uani 1 1 d . . . H15A H 0.6765 0.9367 0.1667 0.071 Uiso 1 1 calc R . . C16 C 0.5897(4) 0.6894(6) 0.15736(12) 0.0555(10) Uani 1 1 d . . . C17 C 0.4809(4) 0.6062(6) 0.16247(12) 0.0568(10) Uani 1 1 d . . . H17A H 0.4668 0.4829 0.1530 0.068 Uiso 1 1 calc R . . C18 C 0.3935(4) 0.7039(6) 0.18138(11) 0.0533(9) Uani 1 1 d . . . H18A H 0.3202 0.6477 0.1832 0.064 Uiso 1 1 calc R . . C19 C 0.3146(4) 0.9822(7) 0.21742(13) 0.0655(11) Uani 1 1 d . . . H19 H 0.2428 0.9495 0.2025 0.079 Uiso 1 1 calc R . . C20 C 0.3043(5) 0.9042(9) 0.25885(15) 0.0817(15) Uani 1 1 d . . . H20A H 0.2913 0.7684 0.2576 0.122 Uiso 1 1 calc R . . H20B H 0.2399 0.9647 0.2715 0.122 Uiso 1 1 calc R . . H20C H 0.3751 0.9298 0.2737 0.122 Uiso 1 1 calc R . . C21 C 0.3256(6) 1.1979(8) 0.21793(19) 0.0935(18) Uani 1 1 d . . . H21A H 0.3956 1.2336 0.2323 0.140 Uiso 1 1 calc R . . H21B H 0.2592 1.2525 0.2306 0.140 Uiso 1 1 calc R . . H21C H 0.3291 1.2446 0.1912 0.140 Uiso 1 1 calc R . . C22 C 0.6813(4) 0.5864(7) 0.13638(14) 0.0636(11) Uani 1 1 d . . . H22A H 0.7382 0.6761 0.1273 0.095 Uiso 1 1 calc R . . H22B H 0.6471 0.5198 0.1140 0.095 Uiso 1 1 calc R . . H22C H 0.7183 0.4959 0.1541 0.095 Uiso 1 1 calc R . . N1 N 0.3954(3) 0.6101(4) 0.06625(10) 0.0497(7) Uani 1 1 d . . . N2 N 0.5506(3) 0.7665(4) 0.05446(9) 0.0476(7) Uani 1 1 d . . . Cl1 Cl 0.26095(9) 0.97087(15) 0.11698(3) 0.0613(3) Uani 1 1 d . . . Cl2 Cl 0.50685(10) 1.17738(14) 0.10831(3) 0.0618(3) Uani 1 1 d . . . Ru1 Ru 0.45359(3) 0.87596(4) 0.134172(9) 0.04907(14) Uani 1 1 d . . . C23 C -0.102(3) 1.112(4) 0.1363(7) 0.136(4) Uani 0.40 1 d PD A 1 H23A H -0.0801 1.2430 0.1320 0.204 Uiso 0.40 1 calc PR A 1 H23B H -0.1856 1.1035 0.1377 0.204 Uiso 0.40 1 calc PR A 1 H23C H -0.0757 1.0345 0.1148 0.204 Uiso 0.40 1 calc PR A 1 C24 C -0.049(2) 1.044(3) 0.1740(8) 0.136(4) Uani 0.40 1 d PD A 1 H24A H 0.0263 1.1068 0.1779 0.163 Uiso 0.40 1 calc PR A 1 H24B H -0.0977 1.0826 0.1955 0.163 Uiso 0.40 1 calc PR A 1 C25 C -0.030(3) 0.837(3) 0.1765(8) 0.136(4) Uani 0.40 1 d PD A 1 H25A H -0.1028 0.7801 0.1667 0.163 Uiso 0.40 1 calc PR A 1 H25B H 0.0274 0.8079 0.1568 0.163 Uiso 0.40 1 calc PR A 1 C26 C 0.003(2) 0.725(3) 0.2108(7) 0.136(4) Uani 0.40 1 d PD A 1 H26A H -0.0637 0.7146 0.2276 0.163 Uiso 0.40 1 calc PR A 1 H26B H 0.0631 0.7953 0.2256 0.163 Uiso 0.40 1 calc PR A 1 C27 C 0.049(2) 0.525(3) 0.2037(8) 0.136(4) Uani 0.40 1 d PD A 1 H27A H 0.0578 0.4595 0.2285 0.204 Uiso 0.40 1 calc PR A 1 H27B H 0.1231 0.5330 0.1912 0.204 Uiso 0.40 1 calc PR A 1 H27C H -0.0053 0.4571 0.1867 0.204 Uiso 0.40 1 calc PR A 1 C28 C -0.1115(14) 1.193(2) 0.1510(5) 0.128(2) Uani 0.60 1 d PD B 2 H28A H -0.1289 1.2579 0.1264 0.192 Uiso 0.60 1 calc PR B 2 H28B H -0.0576 1.2682 0.1667 0.192 Uiso 0.60 1 calc PR B 2 H28C H -0.1821 1.1752 0.1652 0.192 Uiso 0.60 1 calc PR B 2 C29 C -0.0603(14) 1.009(2) 0.1428(5) 0.128(2) Uani 0.60 1 d PD B 2 H29A H 0.0112 1.0247 0.1283 0.154 Uiso 0.60 1 calc PR B 2 H29B H -0.1139 0.9311 0.1271 0.154 Uiso 0.60 1 calc PR B 2 C30 C -0.0349(16) 0.916(2) 0.1826(5) 0.128(2) Uani 0.60 1 d PD B 2 H30A H 0.0215 0.9915 0.1978 0.154 Uiso 0.60 1 calc PR B 2 H30B H -0.1059 0.9072 0.1976 0.154 Uiso 0.60 1 calc PR B 2 C31 C 0.0115(14) 0.725(2) 0.1753(4) 0.128(2) Uani 0.60 1 d PD B 2 H31A H 0.0808 0.7361 0.1595 0.154 Uiso 0.60 1 calc PR B 2 H31B H -0.0459 0.6516 0.1602 0.154 Uiso 0.60 1 calc PR B 2 C32 C 0.0408(15) 0.624(2) 0.2122(5) 0.128(2) Uani 0.60 1 d PD B 2 H32A H 0.0860 0.5121 0.2064 0.192 Uiso 0.60 1 calc PR B 2 H32B H -0.0297 0.5864 0.2249 0.192 Uiso 0.60 1 calc PR B 2 H32C H 0.0854 0.7068 0.2295 0.192 Uiso 0.60 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(2) 0.0407(19) 0.052(2) 0.0033(16) -0.0037(17) 0.0010(16) C2 0.053(2) 0.0441(19) 0.048(2) 0.0000(16) -0.0025(17) 0.0002(16) C3 0.046(2) 0.048(2) 0.046(2) 0.0012(16) 0.0013(15) 0.0036(16) C4 0.051(2) 0.049(2) 0.053(2) 0.0014(17) 0.0056(17) -0.0017(17) C5 0.051(2) 0.057(2) 0.055(2) -0.0012(18) 0.0035(18) -0.0024(18) C6 0.058(3) 0.082(3) 0.078(3) 0.007(3) 0.005(2) -0.006(2) C7 0.055(3) 0.106(4) 0.100(4) 0.003(3) 0.004(3) -0.001(3) C8 0.049(2) 0.048(2) 0.051(2) -0.0008(16) 0.0005(17) -0.0001(17) C9 0.058(2) 0.049(2) 0.059(2) 0.0039(18) -0.0021(19) -0.0017(18) C10 0.060(3) 0.062(3) 0.088(3) 0.020(2) -0.001(2) -0.008(2) C11 0.073(4) 0.092(4) 0.194(8) 0.054(5) 0.033(4) 0.008(3) C12 0.052(2) 0.048(2) 0.049(2) -0.0004(16) 0.0008(17) -0.0022(17) C13 0.064(3) 0.058(2) 0.048(2) -0.0024(18) -0.0015(18) 0.001(2) C14 0.070(3) 0.058(2) 0.048(2) -0.0064(18) -0.0076(19) -0.003(2) C15 0.057(2) 0.066(3) 0.054(2) -0.0006(19) -0.0059(19) -0.009(2) C16 0.060(2) 0.059(2) 0.047(2) 0.0053(18) -0.0007(18) 0.007(2) C17 0.067(3) 0.052(2) 0.051(2) 0.0007(17) -0.0040(19) 0.0082(19) C18 0.057(2) 0.057(2) 0.047(2) -0.0014(17) 0.0038(17) 0.0010(19) C19 0.072(3) 0.068(3) 0.057(2) -0.010(2) 0.006(2) 0.006(2) C20 0.077(3) 0.109(4) 0.059(3) -0.009(3) 0.011(2) 0.011(3) C21 0.103(4) 0.072(3) 0.107(4) -0.023(3) 0.029(3) 0.013(3) C22 0.064(3) 0.065(3) 0.062(3) 0.007(2) 0.005(2) 0.013(2) N1 0.0522(18) 0.0471(17) 0.0498(18) -0.0024(13) 0.0016(14) -0.0024(14) N2 0.0498(18) 0.0461(17) 0.0469(17) -0.0021(13) 0.0012(14) -0.0016(14) Cl1 0.0556(6) 0.0611(6) 0.0669(6) -0.0048(5) -0.0019(5) 0.0085(5) Cl2 0.0757(7) 0.0426(5) 0.0675(6) 0.0001(4) 0.0107(5) 0.0016(5) Ru1 0.0533(2) 0.0452(2) 0.0487(2) -0.00297(12) 0.00110(14) 0.00072(13) C23 0.146(10) 0.115(9) 0.145(10) -0.004(7) -0.017(7) -0.003(8) C24 0.146(10) 0.115(9) 0.145(10) -0.004(7) -0.017(7) -0.003(8) C25 0.146(10) 0.115(9) 0.145(10) -0.004(7) -0.017(7) -0.003(8) C26 0.146(10) 0.115(9) 0.145(10) -0.004(7) -0.017(7) -0.003(8) C27 0.146(10) 0.115(9) 0.145(10) -0.004(7) -0.017(7) -0.003(8) C28 0.118(5) 0.129(7) 0.137(6) -0.007(5) 0.004(4) -0.009(5) C29 0.118(5) 0.129(7) 0.137(6) -0.007(5) 0.004(4) -0.009(5) C30 0.118(5) 0.129(7) 0.137(6) -0.007(5) 0.004(4) -0.009(5) C31 0.118(5) 0.129(7) 0.137(6) -0.007(5) 0.004(4) -0.009(5) C32 0.118(5) 0.129(7) 0.137(6) -0.007(5) 0.004(4) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.363(5) . ? C1 N1 1.366(5) . ? C1 Ru1 2.065(4) . ? C2 C12 1.381(6) . ? C2 N2 1.394(5) . ? C2 C3 1.395(6) . ? C3 C12 1.392(5) 3_665 ? C3 N1 1.399(5) . ? C4 N1 1.476(5) . ? C4 C5 1.512(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.525(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N2 1.457(5) . ? C8 C9 1.526(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.503(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C3 1.392(5) 3_665 ? C12 H12A 0.9500 . ? C13 C14 1.388(6) . ? C13 C18 1.438(6) . ? C13 C19 1.506(6) . ? C13 Ru1 2.261(4) . ? C14 C15 1.438(6) . ? C14 Ru1 2.233(4) . ? C14 H14A 0.9500 . ? C15 C16 1.413(6) . ? C15 Ru1 2.173(4) . ? C15 H15A 0.9500 . ? C16 C17 1.419(6) . ? C16 C22 1.498(6) . ? C16 Ru1 2.208(4) . ? C17 C18 1.409(6) . ? C17 Ru1 2.175(4) . ? C17 H17A 0.9500 . ? C18 Ru1 2.167(4) . ? C18 H18A 0.9500 . ? C19 C20 1.538(7) . ? C19 C21 1.543(7) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Cl1 Ru1 2.4120(11) . ? Cl2 Ru1 2.4130(11) . ? C23 C24 1.507(18) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.493(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.471(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.538(17) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.470(15) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.544(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.487(15) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.494(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 105.8(3) . . ? N2 C1 Ru1 127.9(3) . . ? N1 C1 Ru1 125.9(3) . . ? C12 C2 N2 130.3(4) . . ? C12 C2 C3 123.4(4) . . ? N2 C2 C3 106.2(3) . . ? C12 C3 C2 123.1(4) 3_665 . ? C12 C3 N1 130.6(4) 3_665 . ? C2 C3 N1 106.3(3) . . ? N1 C4 C5 113.6(3) . . ? N1 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 111.5(4) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 113.1(4) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 113.3(3) . . ? N2 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 110.8(4) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 114.5(5) . . ? C11 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 C3 113.5(4) . 3_665 ? C2 C12 H12A 123.3 . . ? C3 C12 H12A 123.3 3_665 . ? C14 C13 C18 117.2(4) . . ? C14 C13 C19 124.4(4) . . ? C18 C13 C19 118.2(4) . . ? C14 C13 Ru1 70.9(2) . . ? C18 C13 Ru1 67.5(2) . . ? C19 C13 Ru1 128.9(3) . . ? C13 C14 C15 121.6(4) . . ? C13 C14 Ru1 73.1(2) . . ? C15 C14 Ru1 68.7(2) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? Ru1 C14 H14A 132.0 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 Ru1 72.5(2) . . ? C14 C15 Ru1 73.2(2) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? Ru1 C15 H15A 126.7 . . ? C15 C16 C17 117.6(4) . . ? C15 C16 C22 121.7(4) . . ? C17 C16 C22 120.6(4) . . ? C15 C16 Ru1 69.9(2) . . ? C17 C16 Ru1 69.9(2) . . ? C22 C16 Ru1 129.7(3) . . ? C18 C17 C16 120.9(4) . . ? C18 C17 Ru1 70.7(2) . . ? C16 C17 Ru1 72.4(2) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? Ru1 C17 H17A 129.9 . . ? C17 C18 C13 121.5(4) . . ? C17 C18 Ru1 71.4(2) . . ? C13 C18 Ru1 74.6(2) . . ? C17 C18 H18A 119.2 . . ? C13 C18 H18A 119.2 . . ? Ru1 C18 H18A 126.7 . . ? C13 C19 C20 109.0(4) . . ? C13 C19 C21 113.0(4) . . ? C20 C19 C21 111.0(4) . . ? C13 C19 H19 107.9 . . ? C20 C19 H19 107.9 . . ? C21 C19 H19 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 N1 C3 110.6(3) . . ? C1 N1 C4 127.8(3) . . ? C3 N1 C4 121.4(3) . . ? C1 N2 C2 111.0(3) . . ? C1 N2 C8 128.1(3) . . ? C2 N2 C8 120.7(3) . . ? C1 Ru1 C18 116.83(15) . . ? C1 Ru1 C15 116.80(17) . . ? C18 Ru1 C15 80.31(16) . . ? C1 Ru1 C17 89.93(15) . . ? C18 Ru1 C17 37.87(16) . . ? C15 Ru1 C17 67.71(17) . . ? C1 Ru1 C16 89.65(15) . . ? C18 Ru1 C16 68.43(16) . . ? C15 Ru1 C16 37.61(16) . . ? C17 Ru1 C16 37.76(17) . . ? C1 Ru1 C14 154.85(16) . . ? C18 Ru1 C14 66.48(16) . . ? C15 Ru1 C14 38.05(17) . . ? C17 Ru1 C14 79.22(16) . . ? C16 Ru1 C14 67.88(16) . . ? C1 Ru1 C13 154.64(15) . . ? C18 Ru1 C13 37.82(15) . . ? C15 Ru1 C13 67.55(17) . . ? C17 Ru1 C13 68.08(15) . . ? C16 Ru1 C13 80.60(16) . . ? C14 Ru1 C13 35.98(16) . . ? C1 Ru1 Cl1 89.29(11) . . ? C18 Ru1 Cl1 91.40(12) . . ? C15 Ru1 Cl1 153.66(13) . . ? C17 Ru1 Cl1 118.92(13) . . ? C16 Ru1 Cl1 156.67(12) . . ? C14 Ru1 Cl1 115.84(12) . . ? C13 Ru1 Cl1 90.60(12) . . ? C1 Ru1 Cl2 92.20(11) . . ? C18 Ru1 Cl2 150.69(11) . . ? C15 Ru1 Cl2 90.41(12) . . ? C17 Ru1 Cl2 156.30(13) . . ? C16 Ru1 Cl2 118.62(12) . . ? C14 Ru1 Cl2 89.13(12) . . ? C13 Ru1 Cl2 113.03(11) . . ? Cl1 Ru1 Cl2 84.72(4) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C23 115(2) . . ? C25 C24 H24A 108.5 . . ? C23 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C26 C25 C24 128(2) . . ? C26 C25 H25A 105.3 . . ? C24 C25 H25A 105.3 . . ? C26 C25 H25B 105.3 . . ? C24 C25 H25B 105.3 . . ? H25A C25 H25B 106.0 . . ? C25 C26 C27 117(2) . . ? C25 C26 H26A 108.0 . . ? C27 C26 H26A 108.0 . . ? C25 C26 H26B 108.0 . . ? C27 C26 H26B 108.0 . . ? H26A C26 H26B 107.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C28 C29 C30 106.5(13) . . ? C28 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? C28 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C31 C30 C29 107.8(13) . . ? C31 C30 H30A 110.2 . . ? C29 C30 H30A 110.2 . . ? C31 C30 H30B 110.2 . . ? C29 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? C30 C31 C32 112.0(14) . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C2 C3 C12 0.1(7) . . . 3_665 ? N2 C2 C3 C12 -178.3(3) . . . 3_665 ? C12 C2 C3 N1 179.2(4) . . . . ? N2 C2 C3 N1 0.8(4) . . . . ? N1 C4 C5 C6 179.1(4) . . . . ? C4 C5 C6 C7 171.3(4) . . . . ? N2 C8 C9 C10 -179.6(4) . . . . ? C8 C9 C10 C11 69.7(6) . . . . ? N2 C2 C12 C3 177.9(4) . . . 3_665 ? C3 C2 C12 C3 -0.1(6) . . . 3_665 ? C18 C13 C14 C15 -0.1(6) . . . . ? C19 C13 C14 C15 -175.5(4) . . . . ? Ru1 C13 C14 C15 -50.8(4) . . . . ? C18 C13 C14 Ru1 50.8(3) . . . . ? C19 C13 C14 Ru1 -124.7(4) . . . . ? C13 C14 C15 C16 -4.2(6) . . . . ? Ru1 C14 C15 C16 -56.9(4) . . . . ? C13 C14 C15 Ru1 52.8(4) . . . . ? C14 C15 C16 C17 4.6(6) . . . . ? Ru1 C15 C16 C17 -52.7(3) . . . . ? C14 C15 C16 C22 -177.8(4) . . . . ? Ru1 C15 C16 C22 124.9(4) . . . . ? C14 C15 C16 Ru1 57.3(4) . . . . ? C15 C16 C17 C18 -0.9(6) . . . . ? C22 C16 C17 C18 -178.5(4) . . . . ? Ru1 C16 C17 C18 -53.6(4) . . . . ? C15 C16 C17 Ru1 52.7(3) . . . . ? C22 C16 C17 Ru1 -124.9(4) . . . . ? C16 C17 C18 C13 -3.4(6) . . . . ? Ru1 C17 C18 C13 -57.7(4) . . . . ? C16 C17 C18 Ru1 54.3(4) . . . . ? C14 C13 C18 C17 3.8(6) . . . . ? C19 C13 C18 C17 179.5(4) . . . . ? Ru1 C13 C18 C17 56.2(4) . . . . ? C14 C13 C18 Ru1 -52.4(4) . . . . ? C19 C13 C18 Ru1 123.3(4) . . . . ? C14 C13 C19 C20 -103.5(5) . . . . ? C18 C13 C19 C20 81.2(5) . . . . ? Ru1 C13 C19 C20 164.0(4) . . . . ? C14 C13 C19 C21 20.5(7) . . . . ? C18 C13 C19 C21 -154.9(4) . . . . ? Ru1 C13 C19 C21 -72.0(6) . . . . ? N2 C1 N1 C3 1.3(4) . . . . ? Ru1 C1 N1 C3 -171.6(3) . . . . ? N2 C1 N1 C4 177.1(3) . . . . ? Ru1 C1 N1 C4 4.2(5) . . . . ? C12 C3 N1 C1 177.6(4) 3_665 . . . ? C2 C3 N1 C1 -1.4(4) . . . . ? C12 C3 N1 C4 1.5(6) 3_665 . . . ? C2 C3 N1 C4 -177.5(3) . . . . ? C5 C4 N1 C1 112.7(4) . . . . ? C5 C4 N1 C3 -71.9(5) . . . . ? N1 C1 N2 C2 -0.8(4) . . . . ? Ru1 C1 N2 C2 171.9(3) . . . . ? N1 C1 N2 C8 -175.8(3) . . . . ? Ru1 C1 N2 C8 -3.0(6) . . . . ? C12 C2 N2 C1 -178.3(4) . . . . ? C3 C2 N2 C1 0.0(4) . . . . ? C12 C2 N2 C8 -2.9(6) . . . . ? C3 C2 N2 C8 175.4(3) . . . . ? C9 C8 N2 C1 -110.3(4) . . . . ? C9 C8 N2 C2 75.1(4) . . . . ? N2 C1 Ru1 C18 -138.3(3) . . . . ? N1 C1 Ru1 C18 33.1(4) . . . . ? N2 C1 Ru1 C15 -45.8(4) . . . . ? N1 C1 Ru1 C15 125.6(3) . . . . ? N2 C1 Ru1 C17 -110.6(3) . . . . ? N1 C1 Ru1 C17 60.8(3) . . . . ? N2 C1 Ru1 C16 -72.9(3) . . . . ? N1 C1 Ru1 C16 98.5(3) . . . . ? N2 C1 Ru1 C14 -46.9(6) . . . . ? N1 C1 Ru1 C14 124.5(4) . . . . ? N2 C1 Ru1 C13 -139.6(4) . . . . ? N1 C1 Ru1 C13 31.7(6) . . . . ? N2 C1 Ru1 Cl1 130.5(3) . . . . ? N1 C1 Ru1 Cl1 -58.2(3) . . . . ? N2 C1 Ru1 Cl2 45.8(3) . . . . ? N1 C1 Ru1 Cl2 -142.8(3) . . . . ? C17 C18 Ru1 C1 49.2(3) . . . . ? C13 C18 Ru1 C1 -179.1(2) . . . . ? C17 C18 Ru1 C15 -66.0(3) . . . . ? C13 C18 Ru1 C15 65.7(3) . . . . ? C13 C18 Ru1 C17 131.7(4) . . . . ? C17 C18 Ru1 C16 -28.8(3) . . . . ? C13 C18 Ru1 C16 102.9(3) . . . . ? C17 C18 Ru1 C14 -103.1(3) . . . . ? C13 C18 Ru1 C14 28.5(3) . . . . ? C17 C18 Ru1 C13 -131.7(4) . . . . ? C17 C18 Ru1 Cl1 139.2(2) . . . . ? C13 C18 Ru1 Cl1 -89.2(2) . . . . ? C17 C18 Ru1 Cl2 -139.1(2) . . . . ? C13 C18 Ru1 Cl2 -7.5(4) . . . . ? C16 C15 Ru1 C1 -48.2(3) . . . . ? C14 C15 Ru1 C1 -179.2(2) . . . . ? C16 C15 Ru1 C18 67.1(3) . . . . ? C14 C15 Ru1 C18 -64.0(3) . . . . ? C16 C15 Ru1 C17 29.8(3) . . . . ? C14 C15 Ru1 C17 -101.3(3) . . . . ? C14 C15 Ru1 C16 -131.1(4) . . . . ? C16 C15 Ru1 C14 131.1(4) . . . . ? C16 C15 Ru1 C13 104.3(3) . . . . ? C14 C15 Ru1 C13 -26.8(2) . . . . ? C16 C15 Ru1 Cl1 140.3(2) . . . . ? C14 C15 Ru1 Cl1 9.2(4) . . . . ? C16 C15 Ru1 Cl2 -140.9(2) . . . . ? C14 C15 Ru1 Cl2 88.1(2) . . . . ? C18 C17 Ru1 C1 -137.5(3) . . . . ? C16 C17 Ru1 C1 89.5(3) . . . . ? C16 C17 Ru1 C18 -133.0(4) . . . . ? C18 C17 Ru1 C15 103.3(3) . . . . ? C16 C17 Ru1 C15 -29.7(3) . . . . ? C18 C17 Ru1 C16 133.0(4) . . . . ? C18 C17 Ru1 C14 65.4(3) . . . . ? C16 C17 Ru1 C14 -67.6(3) . . . . ? C18 C17 Ru1 C13 29.6(2) . . . . ? C16 C17 Ru1 C13 -103.4(3) . . . . ? C18 C17 Ru1 Cl1 -48.3(3) . . . . ? C16 C17 Ru1 Cl1 178.7(2) . . . . ? C18 C17 Ru1 Cl2 127.2(3) . . . . ? C16 C17 Ru1 Cl2 -5.8(5) . . . . ? C15 C16 Ru1 C1 138.3(3) . . . . ? C17 C16 Ru1 C1 -90.3(3) . . . . ? C22 C16 Ru1 C1 23.2(4) . . . . ? C15 C16 Ru1 C18 -102.5(3) . . . . ? C17 C16 Ru1 C18 28.9(2) . . . . ? C22 C16 Ru1 C18 142.4(5) . . . . ? C17 C16 Ru1 C15 131.4(4) . . . . ? C22 C16 Ru1 C15 -115.1(5) . . . . ? C15 C16 Ru1 C17 -131.4(4) . . . . ? C22 C16 Ru1 C17 113.6(5) . . . . ? C15 C16 Ru1 C14 -30.1(3) . . . . ? C17 C16 Ru1 C14 101.3(3) . . . . ? C22 C16 Ru1 C14 -145.2(5) . . . . ? C15 C16 Ru1 C13 -65.2(3) . . . . ? C17 C16 Ru1 C13 66.2(3) . . . . ? C22 C16 Ru1 C13 179.7(4) . . . . ? C15 C16 Ru1 Cl1 -134.3(3) . . . . ? C17 C16 Ru1 Cl1 -2.9(4) . . . . ? C22 C16 Ru1 Cl1 110.6(4) . . . . ? C15 C16 Ru1 Cl2 46.0(3) . . . . ? C17 C16 Ru1 Cl2 177.3(2) . . . . ? C22 C16 Ru1 Cl2 -69.1(4) . . . . ? C13 C14 Ru1 C1 -133.3(4) . . . . ? C15 C14 Ru1 C1 1.6(5) . . . . ? C13 C14 Ru1 C18 -29.9(3) . . . . ? C15 C14 Ru1 C18 105.0(3) . . . . ? C13 C14 Ru1 C15 -134.8(4) . . . . ? C13 C14 Ru1 C17 -67.4(3) . . . . ? C15 C14 Ru1 C17 67.5(3) . . . . ? C13 C14 Ru1 C16 -105.1(3) . . . . ? C15 C14 Ru1 C16 29.8(2) . . . . ? C15 C14 Ru1 C13 134.8(4) . . . . ? C13 C14 Ru1 Cl1 49.7(3) . . . . ? C15 C14 Ru1 Cl1 -175.5(2) . . . . ? C13 C14 Ru1 Cl2 133.4(2) . . . . ? C15 C14 Ru1 Cl2 -91.8(2) . . . . ? C14 C13 Ru1 C1 133.7(4) . . . . ? C18 C13 Ru1 C1 1.9(5) . . . . ? C19 C13 Ru1 C1 -107.0(5) . . . . ? C14 C13 Ru1 C18 131.8(4) . . . . ? C19 C13 Ru1 C18 -108.9(5) . . . . ? C14 C13 Ru1 C15 28.2(3) . . . . ? C18 C13 Ru1 C15 -103.6(3) . . . . ? C19 C13 Ru1 C15 147.5(4) . . . . ? C14 C13 Ru1 C17 102.2(3) . . . . ? C18 C13 Ru1 C17 -29.6(3) . . . . ? C19 C13 Ru1 C17 -138.5(4) . . . . ? C14 C13 Ru1 C16 65.1(3) . . . . ? C18 C13 Ru1 C16 -66.8(3) . . . . ? C19 C13 Ru1 C16 -175.7(4) . . . . ? C18 C13 Ru1 C14 -131.8(4) . . . . ? C19 C13 Ru1 C14 119.3(5) . . . . ? C14 C13 Ru1 Cl1 -136.7(3) . . . . ? C18 C13 Ru1 Cl1 91.5(2) . . . . ? C19 C13 Ru1 Cl1 -17.4(4) . . . . ? C14 C13 Ru1 Cl2 -52.2(3) . . . . ? C18 C13 Ru1 Cl2 176.0(2) . . . . ? C19 C13 Ru1 Cl2 67.1(4) . . . . ? C23 C24 C25 C26 -170(3) . . . . ? C24 C25 C26 C27 -163(3) . . . . ? C28 C29 C30 C31 177.1(13) . . . . ? C29 C30 C31 C32 179.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.625 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.074 # Attachment 'B809721F_compound6b.CIF' data_compound6b _database_code_depnum_ccdc_archive 'CCDC 690656' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H34 Br2 N2 Ru' _chemical_formula_weight 575.39 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' Ru Ru -1.2594 0.8363 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 17.9231(8) _cell_length_b 12.3593(4) _cell_length_c 20.8012(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.923(4) _cell_angle_gamma 90.00 _cell_volume 4605.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35621 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 25.60 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 4.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_T_max 0.374 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46581 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.16 _reflns_number_total 8198 _reflns_number_gt 6279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^] 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 8198 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0535 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 C1 C 0.17301(15) 1.0189(2) 0.24103(13) 0.0211(6) Uani 1 1 d . . . C2 C 0.06746(17) 1.0695(3) 0.28929(15) 0.0328(7) Uani 1 1 d . . . H3 H 0.0186 1.0968 0.2951 0.039 Uiso 1 1 calc R . . C3 C 0.11344(17) 1.0291(3) 0.33456(15) 0.0321(7) Uani 1 1 d . . . H2 H 0.1038 1.0228 0.3790 0.039 Uiso 1 1 calc R . . C4 C 0.23993(17) 0.9475(3) 0.34230(15) 0.0290(7) Uani 1 1 d . . . H4A H 0.2775 0.9209 0.3123 0.035 Uiso 1 1 calc R . . H4B H 0.2211 0.8846 0.3664 0.035 Uiso 1 1 calc R . . C5 C 0.27645(18) 1.0270(3) 0.38911(15) 0.0321(7) Uani 1 1 d . . . H5A H 0.2949 1.0901 0.3651 0.039 Uiso 1 1 calc R . . H5B H 0.2389 1.0531 0.4193 0.039 Uiso 1 1 calc R . . C6 C 0.3403(2) 0.9762(3) 0.42656(19) 0.0503(10) Uani 1 1 d . . . H6A H 0.3758 0.9451 0.3961 0.060 Uiso 1 1 calc R . . H6B H 0.3211 0.9162 0.4528 0.060 Uiso 1 1 calc R . . C7 C 0.3814(2) 1.0553(4) 0.4702(2) 0.0592(12) Uani 1 1 d . . . H7A H 0.4036 1.1123 0.4442 0.089 Uiso 1 1 calc R . . H7B H 0.4209 1.0173 0.4948 0.089 Uiso 1 1 calc R . . H7C H 0.3464 1.0877 0.4998 0.089 Uiso 1 1 calc R . . C8 C 0.06729(16) 1.1005(2) 0.17202(15) 0.0275(7) Uani 1 1 d . . . H8A H 0.0184 1.0638 0.1666 0.033 Uiso 1 1 calc R . . H8B H 0.0981 1.0800 0.1353 0.033 Uiso 1 1 calc R . . C9 C 0.05558(17) 1.2219(2) 0.17176(15) 0.0299(7) Uani 1 1 d . . . H9A H 0.1046 1.2582 0.1778 0.036 Uiso 1 1 calc R . . H9B H 0.0247 1.2420 0.2085 0.036 Uiso 1 1 calc R . . C10 C 0.01779(18) 1.2622(3) 0.10987(16) 0.0363(8) Uani 1 1 d . . . H10A H 0.0161 1.3423 0.1109 0.044 Uiso 1 1 calc R . . H10B H 0.0482 1.2406 0.0732 0.044 Uiso 1 1 calc R . . C11 C -0.0605(2) 1.2195(3) 0.0990(2) 0.0569(11) Uani 1 1 d . . . H11A H -0.0590 1.1406 0.0949 0.085 Uiso 1 1 calc R . . H11B H -0.0825 1.2510 0.0594 0.085 Uiso 1 1 calc R . . H11C H -0.0909 1.2394 0.1355 0.085 Uiso 1 1 calc R . . C12 C 0.31342(16) 0.8551(2) 0.10896(14) 0.0242(6) Uani 1 1 d . . . C13 C 0.24735(16) 0.8852(2) 0.07472(14) 0.0259(6) Uani 1 1 d . . . H13A H 0.2506 0.9157 0.0330 0.031 Uiso 1 1 calc R . . C14 C 0.17586(16) 0.8706(2) 0.10149(14) 0.0278(7) Uani 1 1 d . . . H14A H 0.1325 0.8935 0.0777 0.033 Uiso 1 1 calc R . . C15 C 0.16816(16) 0.8232(2) 0.16209(14) 0.0247(6) Uani 1 1 d . . . C16 C 0.23433(16) 0.7922(2) 0.19792(14) 0.0248(6) Uani 1 1 d . . . H16A H 0.2310 0.7593 0.2390 0.030 Uiso 1 1 calc R . . C17 C 0.30482(16) 0.8111(2) 0.17134(14) 0.0248(6) Uani 1 1 d . . . H17A H 0.3484 0.7936 0.1964 0.030 Uiso 1 1 calc R . . C18 C 0.39048(17) 0.8756(3) 0.08407(15) 0.0316(7) Uani 1 1 d . . . H18A H 0.4225 0.9016 0.1212 0.038 Uiso 1 1 calc R . . C19 C 0.3919(2) 0.9626(3) 0.03230(19) 0.0444(9) Uani 1 1 d . . . H19A H 0.3672 0.9355 -0.0072 0.067 Uiso 1 1 calc R . . H19B H 0.4438 0.9813 0.0237 0.067 Uiso 1 1 calc R . . H19C H 0.3657 1.0272 0.0471 0.067 Uiso 1 1 calc R . . C20 C 0.4246(2) 0.7704(3) 0.06039(18) 0.0425(9) Uani 1 1 d . . . H20A H 0.4268 0.7176 0.0955 0.064 Uiso 1 1 calc R . . H20B H 0.4751 0.7844 0.0459 0.064 Uiso 1 1 calc R . . H20C H 0.3937 0.7416 0.0246 0.064 Uiso 1 1 calc R . . C21 C 0.09336(17) 0.8060(3) 0.19023(17) 0.0344(8) Uani 1 1 d . . . H21A H 0.0576 0.8579 0.1714 0.052 Uiso 1 1 calc R . . H21B H 0.0973 0.8166 0.2369 0.052 Uiso 1 1 calc R . . H21C H 0.0762 0.7322 0.1809 0.052 Uiso 1 1 calc R . . C22 C -0.32346(16) 0.9744(2) 0.24357(14) 0.0223(6) Uani 1 1 d . . . C23 C -0.38507(18) 0.9799(3) 0.33672(15) 0.0343(8) Uani 1 1 d . . . H23A H -0.3953 0.9724 0.3810 0.041 Uiso 1 1 calc R . . C24 C -0.43153(18) 1.0178(3) 0.29095(15) 0.0339(8) Uani 1 1 d . . . H24A H -0.4812 1.0422 0.2963 0.041 Uiso 1 1 calc R . . C25 C -0.25608(17) 0.9079(3) 0.34508(15) 0.0301(7) Uani 1 1 d . . . H25A H -0.2183 0.8809 0.3154 0.036 Uiso 1 1 calc R . . H25B H -0.2736 0.8459 0.3706 0.036 Uiso 1 1 calc R . . C26 C -0.22037(19) 0.9915(3) 0.39004(15) 0.0350(8) Uani 1 1 d . . . H26A H -0.2008 1.0520 0.3644 0.042 Uiso 1 1 calc R . . H26B H -0.2586 1.0209 0.4185 0.042 Uiso 1 1 calc R . . C27 C -0.1576(2) 0.9427(4) 0.4305(2) 0.0556(11) Uani 1 1 d . . . H27A H -0.1219 0.9072 0.4019 0.067 Uiso 1 1 calc R . . H27B H -0.1781 0.8865 0.4588 0.067 Uiso 1 1 calc R . . C28 C -0.1162(3) 1.0262(4) 0.4716(2) 0.0688(14) Uani 1 1 d . . . H28A H -0.0912 1.0777 0.4438 0.103 Uiso 1 1 calc R . . H28B H -0.0790 0.9899 0.4997 0.103 Uiso 1 1 calc R . . H28C H -0.1518 1.0650 0.4980 0.103 Uiso 1 1 calc R . . C29 C -0.43129(17) 1.0477(3) 0.17363(15) 0.0294(7) Uani 1 1 d . . . H29A H -0.4760 1.0019 0.1659 0.035 Uiso 1 1 calc R . . H29B H -0.3972 1.0353 0.1379 0.035 Uiso 1 1 calc R . . C30 C -0.45452(18) 1.1645(3) 0.17356(16) 0.0353(8) Uani 1 1 d . . . H30A H -0.4098 1.2111 0.1792 0.042 Uiso 1 1 calc R . . H30B H -0.4874 1.1782 0.2100 0.042 Uiso 1 1 calc R . . C31 C -0.4953(3) 1.1926(4) 0.11118(19) 0.0645(13) Uani 1 1 d . . . H31A H -0.4592 1.1922 0.0762 0.077 Uiso 1 1 calc R . . H31B H -0.5329 1.1357 0.1014 0.077 Uiso 1 1 calc R . . C32 C -0.5339(3) 1.3000(4) 0.1114(2) 0.0738(15) Uani 1 1 d . . . H32A H -0.5729 1.2992 0.1433 0.111 Uiso 1 1 calc R . . H32B H -0.5565 1.3142 0.0687 0.111 Uiso 1 1 calc R . . H32C H -0.4975 1.3568 0.1224 0.111 Uiso 1 1 calc R . . C33 C -0.17822(16) 0.8192(2) 0.11252(14) 0.0239(6) Uani 1 1 d . . . C34 C -0.24208(16) 0.8499(2) 0.07650(14) 0.0256(7) Uani 1 1 d . . . H34A H -0.2368 0.8817 0.0353 0.031 Uiso 1 1 calc R . . C35 C -0.31476(16) 0.8344(2) 0.10042(14) 0.0251(6) Uani 1 1 d . . . H35A H -0.3571 0.8584 0.0757 0.030 Uiso 1 1 calc R . . C36 C -0.32501(16) 0.7840(2) 0.16016(15) 0.0272(7) Uani 1 1 d . . . C37 C -0.26090(16) 0.7526(2) 0.19778(15) 0.0255(6) Uani 1 1 d . . . H37A H -0.2662 0.7181 0.2382 0.031 Uiso 1 1 calc R . . C38 C -0.18921(16) 0.7733(2) 0.17440(14) 0.0258(7) Uani 1 1 d . . . H38A H -0.1467 0.7561 0.2009 0.031 Uiso 1 1 calc R . . C39 C -0.09981(17) 0.8390(3) 0.09042(16) 0.0317(7) Uani 1 1 d . . . H39A H -0.0695 0.8659 0.1284 0.038 Uiso 1 1 calc R . . C40 C -0.0961(2) 0.9250(3) 0.0378(2) 0.0462(9) Uani 1 1 d . . . H40A H -0.1222 0.8987 -0.0013 0.069 Uiso 1 1 calc R . . H40B H -0.0438 0.9398 0.0287 0.069 Uiso 1 1 calc R . . H40C H -0.1200 0.9915 0.0523 0.069 Uiso 1 1 calc R . . C41 C -0.0650(2) 0.7334(3) 0.06906(18) 0.0440(9) Uani 1 1 d . . . H41A H -0.0625 0.6827 0.1053 0.066 Uiso 1 1 calc R . . H41B H -0.0146 0.7473 0.0543 0.066 Uiso 1 1 calc R . . H41C H -0.0956 0.7022 0.0338 0.066 Uiso 1 1 calc R . . C42 C -0.40176(17) 0.7636(3) 0.18433(18) 0.0357(8) Uani 1 1 d . . . H42A H -0.4371 0.8146 0.1639 0.054 Uiso 1 1 calc R . . H42B H -0.4013 0.7737 0.2311 0.054 Uiso 1 1 calc R . . H42C H -0.4170 0.6894 0.1738 0.054 Uiso 1 1 calc R . . N1 N 0.17766(14) 0.9979(2) 0.30527(11) 0.0255(5) Uani 1 1 d . . . N2 N 0.10428(13) 1.0641(2) 0.23201(12) 0.0246(5) Uani 1 1 d . . . N3 N -0.31897(14) 0.9534(2) 0.30778(12) 0.0263(6) Uani 1 1 d . . . N4 N -0.39390(13) 1.0149(2) 0.23422(12) 0.0264(6) Uani 1 1 d . . . Ru1 Ru 0.244140(12) 0.963072(18) 0.171093(11) 0.01943(6) Uani 1 1 d . . . Ru2 Ru -0.250856(12) 0.924475(18) 0.173518(11) 0.01955(6) Uani 1 1 d . . . Br1 Br 0.359263(17) 1.04114(3) 0.231105(16) 0.03635(9) Uani 1 1 d . . . Br2 Br 0.239203(19) 1.14646(3) 0.114355(16) 0.03532(8) Uani 1 1 d . . . Br3 Br -0.136215(17) 1.00352(3) 0.233841(16) 0.03560(9) Uani 1 1 d . . . Br4 Br -0.260108(18) 1.10967(3) 0.119551(16) 0.03476(8) 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 C1 0.0203(14) 0.0214(17) 0.0216(14) -0.0005(11) -0.0010(11) -0.0009(11) C2 0.0278(16) 0.040(2) 0.0309(18) 0.0000(14) 0.0096(13) 0.0082(14) C3 0.0341(17) 0.039(2) 0.0239(16) 0.0009(14) 0.0101(13) 0.0057(14) C4 0.0340(17) 0.0259(19) 0.0268(17) 0.0023(13) -0.0035(13) 0.0045(13) C5 0.0373(18) 0.031(2) 0.0272(17) -0.0028(13) -0.0041(14) -0.0012(14) C6 0.051(2) 0.049(3) 0.049(2) -0.0015(18) -0.0241(18) 0.0054(18) C7 0.059(3) 0.077(3) 0.040(2) 0.006(2) -0.0205(19) -0.020(2) C8 0.0213(15) 0.0315(19) 0.0294(17) 0.0011(13) -0.0017(12) 0.0032(12) C9 0.0265(16) 0.0277(18) 0.0356(18) -0.0005(14) 0.0018(13) 0.0015(13) C10 0.0368(18) 0.035(2) 0.0374(19) 0.0086(15) 0.0054(14) 0.0074(15) C11 0.055(2) 0.041(2) 0.072(3) 0.012(2) -0.031(2) -0.0005(18) C12 0.0282(15) 0.0227(17) 0.0217(15) -0.0071(12) 0.0026(12) 0.0018(12) C13 0.0335(16) 0.0250(18) 0.0190(15) -0.0045(12) -0.0005(12) -0.0031(13) C14 0.0279(16) 0.0254(18) 0.0293(17) -0.0038(13) -0.0090(13) -0.0051(13) C15 0.0263(15) 0.0175(16) 0.0301(17) -0.0030(12) -0.0002(12) -0.0048(12) C16 0.0315(16) 0.0200(17) 0.0231(15) 0.0005(12) 0.0019(12) -0.0006(12) C17 0.0281(15) 0.0214(17) 0.0247(16) -0.0043(12) -0.0023(12) 0.0035(12) C18 0.0262(16) 0.042(2) 0.0272(17) -0.0077(14) 0.0049(13) -0.0020(14) C19 0.042(2) 0.041(2) 0.052(2) -0.0001(17) 0.0220(17) -0.0057(16) C20 0.046(2) 0.044(2) 0.039(2) -0.0012(16) 0.0135(16) 0.0113(17) C21 0.0255(16) 0.032(2) 0.046(2) -0.0023(15) 0.0062(14) -0.0099(13) C22 0.0245(15) 0.0181(17) 0.0244(15) -0.0002(11) -0.0010(12) -0.0040(11) C23 0.0390(18) 0.041(2) 0.0236(16) 0.0004(14) 0.0092(14) 0.0029(15) C24 0.0273(16) 0.045(2) 0.0303(18) -0.0004(14) 0.0089(13) 0.0031(14) C25 0.0348(17) 0.0284(19) 0.0266(17) 0.0035(13) -0.0055(13) 0.0009(13) C26 0.0431(19) 0.037(2) 0.0249(17) 0.0020(14) -0.0034(14) -0.0004(15) C27 0.057(2) 0.061(3) 0.047(2) -0.0003(19) -0.0236(19) 0.003(2) C28 0.072(3) 0.091(4) 0.042(2) 0.003(2) -0.024(2) -0.026(3) C29 0.0258(16) 0.035(2) 0.0276(17) -0.0014(13) -0.0037(13) 0.0042(13) C30 0.0339(18) 0.041(2) 0.0309(18) 0.0023(15) 0.0036(14) 0.0070(15) C31 0.091(3) 0.071(3) 0.031(2) 0.0068(19) -0.001(2) 0.045(3) C32 0.077(3) 0.081(4) 0.063(3) 0.025(3) 0.007(2) 0.042(3) C33 0.0250(15) 0.0219(17) 0.0248(16) -0.0077(12) 0.0018(12) 0.0004(12) C34 0.0329(16) 0.0256(18) 0.0183(15) -0.0068(12) 0.0003(12) -0.0034(13) C35 0.0237(15) 0.0251(18) 0.0262(16) -0.0029(12) -0.0047(12) -0.0019(12) C36 0.0297(16) 0.0175(17) 0.0347(18) -0.0038(12) 0.0043(13) -0.0059(12) C37 0.0324(16) 0.0176(17) 0.0266(16) 0.0012(12) 0.0025(12) -0.0007(12) C38 0.0289(16) 0.0224(17) 0.0260(17) -0.0040(12) -0.0014(12) 0.0053(12) C39 0.0257(16) 0.038(2) 0.0313(18) -0.0081(14) 0.0045(13) -0.0012(13) C40 0.039(2) 0.037(2) 0.064(3) 0.0038(18) 0.0217(18) -0.0051(16) C41 0.045(2) 0.045(2) 0.043(2) 0.0055(17) 0.0156(16) 0.0112(17) C42 0.0284(17) 0.0278(19) 0.051(2) 0.0006(15) 0.0064(15) -0.0079(13) N1 0.0272(13) 0.0257(15) 0.0235(13) -0.0019(10) 0.0007(10) 0.0031(11) N2 0.0231(12) 0.0270(15) 0.0238(13) 0.0004(10) 0.0010(10) 0.0028(10) N3 0.0290(13) 0.0296(15) 0.0205(13) -0.0019(10) 0.0021(10) 0.0010(11) N4 0.0254(13) 0.0301(15) 0.0239(13) -0.0006(11) 0.0020(10) 0.0025(11) Ru1 0.01886(11) 0.01941(13) 0.02002(12) -0.00214(9) 0.00074(8) -0.00069(9) Ru2 0.01977(11) 0.01911(13) 0.01981(12) -0.00121(9) 0.00110(9) -0.00230(9) Br1 0.02514(16) 0.0440(2) 0.03989(19) -0.01564(15) 0.00093(13) -0.00600(13) Br2 0.04162(19) 0.02543(19) 0.03948(19) 0.00536(13) 0.00972(14) 0.00012(13) Br3 0.02815(16) 0.0412(2) 0.03737(19) -0.01120(15) 0.00030(13) -0.00919(14) Br4 0.04036(18) 0.02404(19) 0.04022(19) 0.00508(13) 0.00634(14) -0.00189(13) _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 C1 N2 1.360(4) . ? C1 N1 1.361(4) . ? C1 Ru1 2.084(3) . ? C2 C3 1.328(4) . ? C2 N2 1.383(4) . ? C2 H3 0.9500 . ? C3 N1 1.375(4) . ? C3 H2 0.9500 . ? C4 N1 1.473(4) . ? C4 C5 1.516(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.501(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.509(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N2 1.464(4) . ? C8 C9 1.515(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.519(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.510(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.411(4) . ? C12 C17 1.420(4) . ? C12 C18 1.513(4) . ? C12 Ru1 2.258(3) . ? C13 C14 1.426(4) . ? C13 Ru1 2.226(3) . ? C13 H13A 0.9500 . ? C14 C15 1.401(4) . ? C14 Ru1 2.187(3) . ? C14 H14A 0.9500 . ? C15 C16 1.432(4) . ? C15 C21 1.496(4) . ? C15 Ru1 2.205(3) . ? C16 C17 1.416(4) . ? C16 Ru1 2.193(3) . ? C16 H16A 0.9500 . ? C17 Ru1 2.170(3) . ? C17 H17A 0.9500 . ? C18 C19 1.523(5) . ? C18 C20 1.526(5) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.360(4) . ? C22 N4 1.366(4) . ? C22 Ru2 2.080(3) . ? C23 C24 1.329(5) . ? C23 N3 1.386(4) . ? C23 H23A 0.9500 . ? C24 N4 1.379(4) . ? C24 H24A 0.9500 . ? C25 N3 1.459(4) . ? C25 C26 1.520(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.508(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.518(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N4 1.465(4) . ? C29 C30 1.502(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.509(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.496(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.399(4) . ? C33 C38 1.426(4) . ? C33 C39 1.513(4) . ? C33 Ru2 2.260(3) . ? C34 C35 1.423(4) . ? C34 Ru2 2.229(3) . ? C34 H34A 0.9500 . ? C35 C36 1.408(4) . ? C35 Ru2 2.179(3) . ? C35 H35A 0.9500 . ? C36 C37 1.422(4) . ? C36 C42 1.502(4) . ? C36 Ru2 2.199(3) . ? C37 C38 1.412(4) . ? C37 Ru2 2.192(3) . ? C37 H37A 0.9500 . ? C38 Ru2 2.170(3) . ? C38 H38A 0.9500 . ? C39 C41 1.519(5) . ? C39 C40 1.528(5) . ? C39 H39A 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? Ru1 Br2 2.5556(4) . ? Ru1 Br1 2.5639(4) . ? Ru2 Br4 2.5523(4) . ? Ru2 Br3 2.5647(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 103.8(2) . . ? N2 C1 Ru1 127.8(2) . . ? N1 C1 Ru1 127.1(2) . . ? C3 C2 N2 106.9(3) . . ? C3 C2 H3 126.6 . . ? N2 C2 H3 126.6 . . ? C2 C3 N1 107.4(3) . . ? C2 C3 H2 126.3 . . ? N1 C3 H2 126.3 . . ? N1 C4 C5 111.4(3) . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 111.6(3) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 112.9(3) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 111.5(2) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 112.7(3) . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 113.5(3) . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 116.6(3) . . ? C13 C12 C18 122.9(3) . . ? C17 C12 C18 120.3(3) . . ? C13 C12 Ru1 70.45(16) . . ? C17 C12 Ru1 67.96(16) . . ? C18 C12 Ru1 128.5(2) . . ? C12 C13 C14 121.3(3) . . ? C12 C13 Ru1 72.88(16) . . ? C14 C13 Ru1 69.65(16) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? Ru1 C13 H13A 130.9 . . ? C15 C14 C13 121.4(3) . . ? C15 C14 Ru1 72.09(16) . . ? C13 C14 Ru1 72.67(16) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? Ru1 C14 H14A 128.2 . . ? C14 C15 C16 118.4(3) . . ? C14 C15 C21 121.9(3) . . ? C16 C15 C21 119.7(3) . . ? C14 C15 Ru1 70.70(16) . . ? C16 C15 Ru1 70.56(16) . . ? C21 C15 Ru1 129.6(2) . . ? C17 C16 C15 119.1(3) . . ? C17 C16 Ru1 70.18(17) . . ? C15 C16 Ru1 71.45(17) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? Ru1 C16 H16A 130.5 . . ? C16 C17 C12 123.1(3) . . ? C16 C17 Ru1 71.95(17) . . ? C12 C17 Ru1 74.70(17) . . ? C16 C17 H17A 118.5 . . ? C12 C17 H17A 118.5 . . ? Ru1 C17 H17A 127.0 . . ? C12 C18 C19 113.4(3) . . ? C12 C18 C20 110.4(3) . . ? C19 C18 C20 110.9(3) . . ? C12 C18 H18A 107.3 . . ? C19 C18 H18A 107.3 . . ? C20 C18 H18A 107.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 N4 103.5(2) . . ? N3 C22 Ru2 127.8(2) . . ? N4 C22 Ru2 127.3(2) . . ? C24 C23 N3 107.2(3) . . ? C24 C23 H23A 126.4 . . ? N3 C23 H23A 126.4 . . ? C23 C24 N4 106.9(3) . . ? C23 C24 H24A 126.5 . . ? N4 C24 H24A 126.5 . . ? N3 C25 C26 111.5(3) . . ? N3 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N3 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.3(3) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 112.6(4) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 C30 112.7(3) . . ? N4 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? N4 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C29 C30 C31 110.4(3) . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 114.3(4) . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 117.1(3) . . ? C34 C33 C39 123.0(3) . . ? C38 C33 C39 119.8(3) . . ? C34 C33 Ru2 70.62(16) . . ? C38 C33 Ru2 67.82(16) . . ? C39 C33 Ru2 129.4(2) . . ? C33 C34 C35 121.2(3) . . ? C33 C34 Ru2 73.06(16) . . ? C35 C34 Ru2 69.26(16) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? Ru2 C34 H34A 131.1 . . ? C36 C35 C34 121.1(3) . . ? C36 C35 Ru2 72.01(16) . . ? C34 C35 Ru2 73.09(16) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? Ru2 C35 H35A 127.6 . . ? C35 C36 C37 118.7(3) . . ? C35 C36 C42 121.2(3) . . ? C37 C36 C42 120.2(3) . . ? C35 C36 Ru2 70.48(16) . . ? C37 C36 Ru2 70.84(16) . . ? C42 C36 Ru2 130.3(2) . . ? C38 C37 C36 119.2(3) . . ? C38 C37 Ru2 70.27(17) . . ? C36 C37 Ru2 71.36(17) . . ? C38 C37 H37A 120.4 . . ? C36 C37 H37A 120.4 . . ? Ru2 C37 H37A 130.5 . . ? C37 C38 C33 122.5(3) . . ? C37 C38 Ru2 71.95(17) . . ? C33 C38 Ru2 74.70(17) . . ? C37 C38 H38A 118.7 . . ? C33 C38 H38A 118.7 . . ? Ru2 C38 H38A 126.6 . . ? C33 C39 C41 110.1(3) . . ? C33 C39 C40 113.2(3) . . ? C41 C39 C40 111.1(3) . . ? C33 C39 H39A 107.4 . . ? C41 C39 H39A 107.4 . . ? C40 C39 H39A 107.4 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C1 N1 C3 110.9(2) . . ? C1 N1 C4 127.9(2) . . ? C3 N1 C4 121.2(2) . . ? C1 N2 C2 110.9(2) . . ? C1 N2 C8 128.8(2) . . ? C2 N2 C8 120.3(2) . . ? C22 N3 C23 111.0(2) . . ? C22 N3 C25 127.9(3) . . ? C23 N3 C25 121.1(3) . . ? C22 N4 C24 111.3(2) . . ? C22 N4 C29 128.2(2) . . ? C24 N4 C29 120.4(2) . . ? C1 Ru1 C17 127.10(11) . . ? C1 Ru1 C14 107.07(11) . . ? C17 Ru1 C14 79.54(11) . . ? C1 Ru1 C16 94.88(11) . . ? C17 Ru1 C16 37.86(11) . . ? C14 Ru1 C16 67.49(11) . . ? C1 Ru1 C15 85.88(11) . . ? C17 Ru1 C15 68.28(11) . . ? C14 Ru1 C15 37.21(11) . . ? C16 Ru1 C15 38.00(11) . . ? C1 Ru1 C13 143.77(10) . . ? C17 Ru1 C13 66.41(11) . . ? C14 Ru1 C13 37.68(11) . . ? C16 Ru1 C13 79.48(11) . . ? C15 Ru1 C13 67.61(11) . . ? C1 Ru1 C12 162.98(11) . . ? C17 Ru1 C12 37.34(11) . . ? C14 Ru1 C12 67.57(11) . . ? C16 Ru1 C12 68.11(11) . . ? C15 Ru1 C12 80.69(11) . . ? C13 Ru1 C12 36.67(10) . . ? C1 Ru1 Br2 90.93(8) . . ? C17 Ru1 Br2 141.09(8) . . ? C14 Ru1 Br2 98.51(8) . . ? C16 Ru1 Br2 165.89(8) . . ? C15 Ru1 Br2 130.12(8) . . ? C13 Ru1 Br2 88.24(8) . . ? C12 Ru1 Br2 105.71(8) . . ? C1 Ru1 Br1 92.10(7) . . ? C17 Ru1 Br1 85.95(8) . . ? C14 Ru1 Br1 160.46(8) . . ? C16 Ru1 Br1 107.97(8) . . ? C15 Ru1 Br1 145.20(8) . . ? C13 Ru1 Br1 123.81(8) . . ? C12 Ru1 Br1 92.98(7) . . ? Br2 Ru1 Br1 84.603(14) . . ? C22 Ru2 C38 125.45(11) . . ? C22 Ru2 C35 108.30(11) . . ? C38 Ru2 C35 79.72(11) . . ? C22 Ru2 C37 93.91(11) . . ? C38 Ru2 C37 37.78(11) . . ? C35 Ru2 C37 67.67(11) . . ? C22 Ru2 C36 86.18(11) . . ? C38 Ru2 C36 68.07(11) . . ? C35 Ru2 C36 37.51(11) . . ? C37 Ru2 C36 37.80(11) . . ? C22 Ru2 C34 145.28(11) . . ? C38 Ru2 C34 66.44(11) . . ? C35 Ru2 C34 37.64(11) . . ? C37 Ru2 C34 79.43(11) . . ? C36 Ru2 C34 67.64(11) . . ? C22 Ru2 C33 161.79(11) . . ? C38 Ru2 C33 37.48(11) . . ? C35 Ru2 C33 67.24(11) . . ? C37 Ru2 C33 67.95(11) . . ? C36 Ru2 C33 80.29(11) . . ? C34 Ru2 C33 36.31(10) . . ? C22 Ru2 Br4 90.51(8) . . ? C38 Ru2 Br4 143.25(8) . . ? C35 Ru2 Br4 97.27(8) . . ? C37 Ru2 Br4 164.94(8) . . ? C36 Ru2 Br4 128.51(8) . . ? C34 Ru2 Br4 88.75(8) . . ? C33 Ru2 Br4 107.44(8) . . ? C22 Ru2 Br3 93.10(8) . . ? C38 Ru2 Br3 85.67(8) . . ? C35 Ru2 Br3 158.42(8) . . ? C37 Ru2 Br3 109.09(8) . . ? C36 Ru2 Br3 146.47(8) . . ? C34 Ru2 Br3 121.39(8) . . ? C33 Ru2 Br3 91.54(7) . . ? Br4 Ru2 Br3 84.995(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N1 -0.7(4) . . . . ? N1 C4 C5 C6 -179.5(3) . . . . ? C4 C5 C6 C7 175.9(3) . . . . ? N2 C8 C9 C10 179.6(2) . . . . ? C8 C9 C10 C11 64.0(4) . . . . ? C17 C12 C13 C14 -0.7(4) . . . . ? C18 C12 C13 C14 -176.1(3) . . . . ? Ru1 C12 C13 C14 -52.2(3) . . . . ? C17 C12 C13 Ru1 51.5(2) . . . . ? C18 C12 C13 Ru1 -123.9(3) . . . . ? C12 C13 C14 C15 -1.7(4) . . . . ? Ru1 C13 C14 C15 -55.4(3) . . . . ? C12 C13 C14 Ru1 53.6(3) . . . . ? C13 C14 C15 C16 1.8(4) . . . . ? Ru1 C14 C15 C16 -53.8(2) . . . . ? C13 C14 C15 C21 -179.1(3) . . . . ? Ru1 C14 C15 C21 125.3(3) . . . . ? C13 C14 C15 Ru1 55.6(3) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C21 C15 C16 C17 -178.6(3) . . . . ? Ru1 C15 C16 C17 -53.4(2) . . . . ? C14 C15 C16 Ru1 53.9(2) . . . . ? C21 C15 C16 Ru1 -125.2(3) . . . . ? C15 C16 C17 C12 -3.1(4) . . . . ? Ru1 C16 C17 C12 -57.1(3) . . . . ? C15 C16 C17 Ru1 54.0(2) . . . . ? C13 C12 C17 C16 3.1(4) . . . . ? C18 C12 C17 C16 178.7(3) . . . . ? Ru1 C12 C17 C16 55.8(3) . . . . ? C13 C12 C17 Ru1 -52.7(2) . . . . ? C18 C12 C17 Ru1 122.8(3) . . . . ? C13 C12 C18 C19 19.7(4) . . . . ? C17 C12 C18 C19 -155.5(3) . . . . ? Ru1 C12 C18 C19 -70.7(4) . . . . ? C13 C12 C18 C20 -105.5(3) . . . . ? C17 C12 C18 C20 79.3(3) . . . . ? Ru1 C12 C18 C20 164.1(2) . . . . ? N3 C23 C24 N4 -0.3(4) . . . . ? N3 C25 C26 C27 177.5(3) . . . . ? C25 C26 C27 C28 174.9(3) . . . . ? N4 C29 C30 C31 -177.8(3) . . . . ? C29 C30 C31 C32 168.4(4) . . . . ? C38 C33 C34 C35 -0.9(4) . . . . ? C39 C33 C34 C35 -177.0(3) . . . . ? Ru2 C33 C34 C35 -51.9(3) . . . . ? C38 C33 C34 Ru2 51.0(2) . . . . ? C39 C33 C34 Ru2 -125.1(3) . . . . ? C33 C34 C35 C36 -2.4(4) . . . . ? Ru2 C34 C35 C36 -55.9(3) . . . . ? C33 C34 C35 Ru2 53.6(3) . . . . ? C34 C35 C36 C37 2.6(4) . . . . ? Ru2 C35 C36 C37 -53.8(2) . . . . ? C34 C35 C36 C42 -177.6(3) . . . . ? Ru2 C35 C36 C42 126.0(3) . . . . ? C34 C35 C36 Ru2 56.4(3) . . . . ? C35 C36 C37 C38 0.3(4) . . . . ? C42 C36 C37 C38 -179.5(3) . . . . ? Ru2 C36 C37 C38 -53.3(2) . . . . ? C35 C36 C37 Ru2 53.6(2) . . . . ? C42 C36 C37 Ru2 -126.1(3) . . . . ? C36 C37 C38 C33 -3.7(4) . . . . ? Ru2 C37 C38 C33 -57.5(3) . . . . ? C36 C37 C38 Ru2 53.8(2) . . . . ? C34 C33 C38 C37 3.9(4) . . . . ? C39 C33 C38 C37 -179.9(3) . . . . ? Ru2 C33 C38 C37 56.3(3) . . . . ? C34 C33 C38 Ru2 -52.3(2) . . . . ? C39 C33 C38 Ru2 123.9(3) . . . . ? C34 C33 C39 C41 -106.6(3) . . . . ? C38 C33 C39 C41 77.4(4) . . . . ? Ru2 C33 C39 C41 162.1(2) . . . . ? C34 C33 C39 C40 18.3(4) . . . . ? C38 C33 C39 C40 -157.6(3) . . . . ? Ru2 C33 C39 C40 -72.9(4) . . . . ? N2 C1 N1 C3 0.3(3) . . . . ? Ru1 C1 N1 C3 -167.6(2) . . . . ? N2 C1 N1 C4 179.2(3) . . . . ? Ru1 C1 N1 C4 11.4(4) . . . . ? C2 C3 N1 C1 0.3(4) . . . . ? C2 C3 N1 C4 -178.8(3) . . . . ? C5 C4 N1 C1 113.6(3) . . . . ? C5 C4 N1 C3 -67.5(4) . . . . ? N1 C1 N2 C2 -0.7(3) . . . . ? Ru1 C1 N2 C2 167.0(2) . . . . ? N1 C1 N2 C8 -178.1(3) . . . . ? Ru1 C1 N2 C8 -10.3(4) . . . . ? C3 C2 N2 C1 0.9(4) . . . . ? C3 C2 N2 C8 178.5(3) . . . . ? C9 C8 N2 C1 -114.7(3) . . . . ? C9 C8 N2 C2 68.2(3) . . . . ? N4 C22 N3 C23 0.3(3) . . . . ? Ru2 C22 N3 C23 -167.1(2) . . . . ? N4 C22 N3 C25 179.5(3) . . . . ? Ru2 C22 N3 C25 12.0(4) . . . . ? C24 C23 N3 C22 0.0(4) . . . . ? C24 C23 N3 C25 -179.3(3) . . . . ? C26 C25 N3 C22 110.6(3) . . . . ? C26 C25 N3 C23 -70.3(4) . . . . ? N3 C22 N4 C24 -0.5(3) . . . . ? Ru2 C22 N4 C24 167.0(2) . . . . ? N3 C22 N4 C29 -177.3(3) . . . . ? Ru2 C22 N4 C29 -9.7(4) . . . . ? C23 C24 N4 C22 0.5(4) . . . . ? C23 C24 N4 C29 177.5(3) . . . . ? C30 C29 N4 C22 -120.6(3) . . . . ? C30 C29 N4 C24 62.9(4) . . . . ? N2 C1 Ru1 C17 -134.0(2) . . . . ? N1 C1 Ru1 C17 30.9(3) . . . . ? N2 C1 Ru1 C14 -44.4(3) . . . . ? N1 C1 Ru1 C14 120.6(2) . . . . ? N2 C1 Ru1 C16 -112.3(3) . . . . ? N1 C1 Ru1 C16 52.7(3) . . . . ? N2 C1 Ru1 C15 -75.3(3) . . . . ? N1 C1 Ru1 C15 89.6(3) . . . . ? N2 C1 Ru1 C13 -33.5(4) . . . . ? N1 C1 Ru1 C13 131.5(2) . . . . ? N2 C1 Ru1 C12 -113.2(4) . . . . ? N1 C1 Ru1 C12 51.7(5) . . . . ? N2 C1 Ru1 Br2 54.8(2) . . . . ? N1 C1 Ru1 Br2 -140.2(2) . . . . ? N2 C1 Ru1 Br1 139.5(2) . . . . ? N1 C1 Ru1 Br1 -55.6(2) . . . . ? C16 C17 Ru1 C1 36.9(2) . . . . ? C12 C17 Ru1 C1 170.13(16) . . . . ? C16 C17 Ru1 C14 -66.62(18) . . . . ? C12 C17 Ru1 C14 66.57(17) . . . . ? C12 C17 Ru1 C16 133.2(3) . . . . ? C16 C17 Ru1 C15 -29.59(17) . . . . ? C12 C17 Ru1 C15 103.60(18) . . . . ? C16 C17 Ru1 C13 -103.71(19) . . . . ? C12 C17 Ru1 C13 29.47(16) . . . . ? C16 C17 Ru1 C12 -133.2(3) . . . . ? C16 C17 Ru1 Br2 -157.24(13) . . . . ? C12 C17 Ru1 Br2 -24.1(2) . . . . ? C16 C17 Ru1 Br1 126.52(16) . . . . ? C12 C17 Ru1 Br1 -100.29(16) . . . . ? C15 C14 Ru1 C1 -58.10(19) . . . . ? C13 C14 Ru1 C1 169.46(18) . . . . ? C15 C14 Ru1 C17 67.71(18) . . . . ? C13 C14 Ru1 C17 -64.74(18) . . . . ? C15 C14 Ru1 C16 30.13(17) . . . . ? C13 C14 Ru1 C16 -102.3(2) . . . . ? C13 C14 Ru1 C15 -132.4(3) . . . . ? C15 C14 Ru1 C13 132.4(3) . . . . ? C15 C14 Ru1 C12 104.7(2) . . . . ? C13 C14 Ru1 C12 -27.72(17) . . . . ? C15 C14 Ru1 Br2 -151.71(16) . . . . ? C13 C14 Ru1 Br2 75.84(17) . . . . ? C15 C14 Ru1 Br1 110.4(3) . . . . ? C13 C14 Ru1 Br1 -22.0(4) . . . . ? C17 C16 Ru1 C1 -151.24(17) . . . . ? C15 C16 Ru1 C1 76.92(18) . . . . ? C15 C16 Ru1 C17 -131.8(3) . . . . ? C17 C16 Ru1 C14 102.29(19) . . . . ? C15 C16 Ru1 C14 -29.54(17) . . . . ? C17 C16 Ru1 C15 131.8(3) . . . . ? C17 C16 Ru1 C13 64.90(17) . . . . ? C15 C16 Ru1 C13 -66.94(18) . . . . ? C17 C16 Ru1 C12 28.47(16) . . . . ? C15 C16 Ru1 C12 -103.37(19) . . . . ? C17 C16 Ru1 Br2 94.8(3) . . . . ? C15 C16 Ru1 Br2 -37.1(4) . . . . ? C17 C16 Ru1 Br1 -57.43(17) . . . . ? C15 C16 Ru1 Br1 170.73(15) . . . . ? C14 C15 Ru1 C1 125.55(19) . . . . ? C16 C15 Ru1 C1 -103.33(18) . . . . ? C21 C15 Ru1 C1 9.7(3) . . . . ? C14 C15 Ru1 C17 -101.64(19) . . . . ? C16 C15 Ru1 C17 29.49(17) . . . . ? C21 C15 Ru1 C17 142.5(3) . . . . ? C16 C15 Ru1 C14 131.1(3) . . . . ? C21 C15 Ru1 C14 -115.9(4) . . . . ? C14 C15 Ru1 C16 -131.1(3) . . . . ? C21 C15 Ru1 C16 113.0(3) . . . . ? C14 C15 Ru1 C13 -29.20(18) . . . . ? C16 C15 Ru1 C13 101.93(19) . . . . ? C21 C15 Ru1 C13 -145.1(3) . . . . ? C14 C15 Ru1 C12 -64.95(18) . . . . ? C16 C15 Ru1 C12 66.17(18) . . . . ? C21 C15 Ru1 C12 179.2(3) . . . . ? C14 C15 Ru1 Br2 37.8(2) . . . . ? C16 C15 Ru1 Br2 168.92(13) . . . . ? C21 C15 Ru1 Br2 -78.1(3) . . . . ? C14 C15 Ru1 Br1 -146.69(15) . . . . ? C16 C15 Ru1 Br1 -15.6(2) . . . . ? C21 C15 Ru1 Br1 97.4(3) . . . . ? C12 C13 Ru1 C1 -151.16(19) . . . . ? C14 C13 Ru1 C1 -17.2(3) . . . . ? C12 C13 Ru1 C17 -29.98(17) . . . . ? C14 C13 Ru1 C17 104.0(2) . . . . ? C12 C13 Ru1 C14 -134.0(3) . . . . ? C12 C13 Ru1 C16 -67.32(18) . . . . ? C14 C13 Ru1 C16 66.64(18) . . . . ? C12 C13 Ru1 C15 -105.1(2) . . . . ? C14 C13 Ru1 C15 28.86(18) . . . . ? C14 C13 Ru1 C12 134.0(3) . . . . ? C12 C13 Ru1 Br2 119.67(17) . . . . ? C14 C13 Ru1 Br2 -106.38(17) . . . . ? C12 C13 Ru1 Br1 37.4(2) . . . . ? C14 C13 Ru1 Br1 171.31(15) . . . . ? C13 C12 Ru1 C1 103.1(4) . . . . ? C17 C12 Ru1 C1 -27.8(4) . . . . ? C18 C12 Ru1 C1 -139.8(3) . . . . ? C13 C12 Ru1 C17 131.0(3) . . . . ? C18 C12 Ru1 C17 -112.0(3) . . . . ? C13 C12 Ru1 C14 28.43(18) . . . . ? C17 C12 Ru1 C14 -102.55(19) . . . . ? C18 C12 Ru1 C14 145.5(3) . . . . ? C13 C12 Ru1 C16 102.14(19) . . . . ? C17 C12 Ru1 C16 -28.84(17) . . . . ? C18 C12 Ru1 C16 -140.8(3) . . . . ? C13 C12 Ru1 C15 64.77(18) . . . . ? C17 C12 Ru1 C15 -66.20(18) . . . . ? C18 C12 Ru1 C15 -178.2(3) . . . . ? C17 C12 Ru1 C13 -131.0(3) . . . . ? C18 C12 Ru1 C13 117.1(3) . . . . ? C13 C12 Ru1 Br2 -64.45(17) . . . . ? C17 C12 Ru1 Br2 164.58(15) . . . . ? C18 C12 Ru1 Br2 52.6(3) . . . . ? C13 C12 Ru1 Br1 -149.68(17) . . . . ? C17 C12 Ru1 Br1 79.35(16) . . . . ? C18 C12 Ru1 Br1 -32.6(3) . . . . ? N3 C22 Ru2 C38 32.6(3) . . . . ? N4 C22 Ru2 C38 -131.9(2) . . . . ? N3 C22 Ru2 C35 122.9(2) . . . . ? N4 C22 Ru2 C35 -41.7(3) . . . . ? N3 C22 Ru2 C37 55.2(3) . . . . ? N4 C22 Ru2 C37 -109.4(3) . . . . ? N3 C22 Ru2 C36 92.2(3) . . . . ? N4 C22 Ru2 C36 -72.4(3) . . . . ? N3 C22 Ru2 C34 132.2(2) . . . . ? N4 C22 Ru2 C34 -32.4(4) . . . . ? N3 C22 Ru2 C33 50.3(5) . . . . ? N4 C22 Ru2 C33 -114.3(4) . . . . ? N3 C22 Ru2 Br4 -139.3(2) . . . . ? N4 C22 Ru2 Br4 56.2(2) . . . . ? N3 C22 Ru2 Br3 -54.2(2) . . . . ? N4 C22 Ru2 Br3 141.2(2) . . . . ? C37 C38 Ru2 C22 38.6(2) . . . . ? C33 C38 Ru2 C22 171.05(16) . . . . ? C37 C38 Ru2 C35 -66.66(18) . . . . ? C33 C38 Ru2 C35 65.83(17) . . . . ? C33 C38 Ru2 C37 132.5(3) . . . . ? C37 C38 Ru2 C36 -29.42(18) . . . . ? C33 C38 Ru2 C36 103.07(18) . . . . ? C37 C38 Ru2 C34 -103.64(19) . . . . ? C33 C38 Ru2 C34 28.85(16) . . . . ? C37 C38 Ru2 C33 -132.5(3) . . . . ? C37 C38 Ru2 Br4 -155.06(14) . . . . ? C33 C38 Ru2 Br4 -22.6(2) . . . . ? C37 C38 Ru2 Br3 129.28(17) . . . . ? C33 C38 Ru2 Br3 -98.23(16) . . . . ? C36 C35 Ru2 C22 -56.9(2) . . . . ? C34 C35 Ru2 C22 171.35(17) . . . . ? C36 C35 Ru2 C38 67.23(18) . . . . ? C34 C35 Ru2 C38 -64.53(18) . . . . ? C36 C35 Ru2 C37 29.78(17) . . . . ? C34 C35 Ru2 C37 -102.0(2) . . . . ? C34 C35 Ru2 C36 -131.8(3) . . . . ? C36 C35 Ru2 C34 131.8(3) . . . . ? C36 C35 Ru2 C33 104.25(19) . . . . ? C34 C35 Ru2 C33 -27.52(18) . . . . ? C36 C35 Ru2 Br4 -149.85(16) . . . . ? C34 C35 Ru2 Br4 78.39(17) . . . . ? C36 C35 Ru2 Br3 115.4(2) . . . . ? C34 C35 Ru2 Br3 -16.4(3) . . . . ? C38 C37 Ru2 C22 -149.40(18) . . . . ? C36 C37 Ru2 C22 78.62(18) . . . . ? C36 C37 Ru2 C38 -132.0(3) . . . . ? C38 C37 Ru2 C35 102.40(19) . . . . ? C36 C37 Ru2 C35 -29.57(17) . . . . ? C38 C37 Ru2 C36 132.0(3) . . . . ? C38 C37 Ru2 C34 64.98(18) . . . . ? C36 C37 Ru2 C34 -67.00(18) . . . . ? C38 C37 Ru2 C33 28.95(17) . . . . ? C36 C37 Ru2 C33 -103.02(19) . . . . ? C38 C37 Ru2 Br4 103.8(3) . . . . ? C36 C37 Ru2 Br4 -28.1(4) . . . . ? C38 C37 Ru2 Br3 -54.76(18) . . . . ? C36 C37 Ru2 Br3 173.27(15) . . . . ? C35 C36 Ru2 C22 127.16(19) . . . . ? C37 C36 Ru2 C22 -101.41(18) . . . . ? C42 C36 Ru2 C22 12.3(3) . . . . ? C35 C36 Ru2 C38 -102.03(19) . . . . ? C37 C36 Ru2 C38 29.40(18) . . . . ? C42 C36 Ru2 C38 143.2(3) . . . . ? C37 C36 Ru2 C35 131.4(3) . . . . ? C42 C36 Ru2 C35 -114.8(4) . . . . ? C35 C36 Ru2 C37 -131.4(3) . . . . ? C42 C36 Ru2 C37 113.7(4) . . . . ? C35 C36 Ru2 C34 -29.51(17) . . . . ? C37 C36 Ru2 C34 101.93(19) . . . . ? C42 C36 Ru2 C34 -144.3(3) . . . . ? C35 C36 Ru2 C33 -65.06(18) . . . . ? C37 C36 Ru2 C33 66.37(18) . . . . ? C42 C36 Ru2 C33 -179.9(3) . . . . ? C35 C36 Ru2 Br4 39.6(2) . . . . ? C37 C36 Ru2 Br4 170.99(14) . . . . ? C42 C36 Ru2 Br4 -75.3(3) . . . . ? C35 C36 Ru2 Br3 -143.01(15) . . . . ? C37 C36 Ru2 Br3 -11.6(3) . . . . ? C42 C36 Ru2 Br3 102.2(3) . . . . ? C33 C34 Ru2 C22 -148.5(2) . . . . ? C35 C34 Ru2 C22 -14.5(3) . . . . ? C33 C34 Ru2 C38 -29.72(18) . . . . ? C35 C34 Ru2 C38 104.3(2) . . . . ? C33 C34 Ru2 C35 -134.0(3) . . . . ? C33 C34 Ru2 C37 -66.99(18) . . . . ? C35 C34 Ru2 C37 67.00(18) . . . . ? C33 C34 Ru2 C36 -104.6(2) . . . . ? C35 C34 Ru2 C36 29.41(18) . . . . ? C35 C34 Ru2 C33 134.0(3) . . . . ? C33 C34 Ru2 Br4 122.39(17) . . . . ? C35 C34 Ru2 Br4 -103.62(17) . . . . ? C33 C34 Ru2 Br3 39.0(2) . . . . ? C35 C34 Ru2 Br3 173.02(14) . . . . ? C34 C33 Ru2 C22 107.8(4) . . . . ? C38 C33 Ru2 C22 -23.9(4) . . . . ? C39 C33 Ru2 C22 -135.0(3) . . . . ? C34 C33 Ru2 C38 131.7(3) . . . . ? C39 C33 Ru2 C38 -111.0(3) . . . . ? C34 C33 Ru2 C35 28.46(18) . . . . ? C38 C33 Ru2 C35 -103.24(19) . . . . ? C39 C33 Ru2 C35 145.7(3) . . . . ? C34 C33 Ru2 C37 102.52(19) . . . . ? C38 C33 Ru2 C37 -29.17(17) . . . . ? C39 C33 Ru2 C37 -140.2(3) . . . . ? C34 C33 Ru2 C36 65.24(19) . . . . ? C38 C33 Ru2 C36 -66.46(18) . . . . ? C39 C33 Ru2 C36 -177.5(3) . . . . ? C38 C33 Ru2 C34 -131.7(3) . . . . ? C39 C33 Ru2 C34 117.3(4) . . . . ? C34 C33 Ru2 Br4 -62.23(17) . . . . ? C38 C33 Ru2 Br4 166.07(15) . . . . ? C39 C33 Ru2 Br4 55.0(3) . . . . ? C34 C33 Ru2 Br3 -147.47(17) . . . . ? C38 C33 Ru2 Br3 80.84(16) . . . . ? C39 C33 Ru2 Br3 -30.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.288 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.073