Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? loop_ _publ_author_name 'Vivian Wing-Wah Yam' 'Ben Wai-Kin Chu' 'Chi-Chiu Ko' 'Nianyong Zhu' _publ_contact_author_name 'Vivian Wing-Wah Yam' _publ_contact_author_address ; Prof Vivian Wing-Wah Yam Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong CHINA ; _publ_contact_author_email WWYAM@HKU.HK _publ_section_title ; Synthesis, crystal structures, photophysics and cation-binding studies of luminescent functionalized ruthenium polypyridine complexes with orthometallated aminocarbene ligands ; data_mar831 _database_code_CSD 213863 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H35 Br F3 N5 O3 Ru S' _chemical_formula_sum 'C39 H35 Br F3 N5 O3 Ru S' _chemical_formula_weight 891.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.536(2) _cell_length_b 13.332(3) _cell_length_c 14.986(3) _cell_angle_alpha 69.68(3) _cell_angle_beta 82.28(3) _cell_angle_gamma 74.50(3) _cell_volume 1900.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mar300 _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8494 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4807 _reflns_number_gt 3416 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0746P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4807 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.68837(4) 0.29235(4) -0.18650(3) 0.03914(19) Uani 1 1 d . . . Br1 Br 1.05376(7) 0.23056(7) 0.11493(5) 0.0803(3) Uani 1 1 d . . . N1 N 0.8084(4) 0.1814(4) -0.2477(3) 0.0409(12) Uani 1 1 d . . . N2 N 0.5548(4) 0.2666(4) -0.2672(3) 0.0430(12) Uani 1 1 d . . . N3 N 0.5432(4) 0.3839(4) -0.1204(3) 0.0412(12) Uani 1 1 d . . . N4 N 0.6387(4) 0.1679(4) -0.0602(3) 0.0400(12) Uani 1 1 d . . . N5 N 0.8123(5) 0.4696(5) -0.2670(4) 0.0470(13) Uani 1 1 d . . . C1 C 0.8305(5) 0.3208(5) -0.1237(4) 0.0414(14) Uani 1 1 d . . . C2 C 0.8707(5) 0.4181(5) -0.1788(5) 0.0470(16) Uani 1 1 d . . . C3 C 0.9612(6) 0.4594(6) -0.1503(5) 0.0558(17) Uani 1 1 d . . . H3 H 0.9843 0.5240 -0.1889 0.067 Uiso 1 1 calc R . . C4 C 1.0154(6) 0.4004(6) -0.0623(5) 0.0592(19) Uani 1 1 d . . . H4 H 1.0760 0.4255 -0.0409 0.071 Uiso 1 1 calc R . . C5 C 0.9800(6) 0.3054(6) -0.0067(5) 0.0533(17) Uani 1 1 d . . . C6 C 0.8887(5) 0.2648(5) -0.0351(4) 0.0461(16) Uani 1 1 d . . . H6 H 0.8662 0.2004 0.0047 0.055 Uiso 1 1 calc R . . C7 C 0.7284(5) 0.4214(5) -0.2865(4) 0.0452(15) Uani 1 1 d . . . C8 C 0.6744(6) 0.4772(5) -0.3849(4) 0.0516(16) Uani 1 1 d . . . H8A H 0.5803 0.4828 -0.3805 0.062 Uiso 1 1 calc R . . H8B H 0.6882 0.5512 -0.4100 0.062 Uiso 1 1 calc R . . C9 C 0.7396(6) 0.4150(5) -0.4523(4) 0.0541(17) Uani 1 1 d . . . C10 C 0.8763(6) 0.3800(6) -0.4615(5) 0.073(2) Uani 1 1 d . . . H10 H 0.9284 0.3934 -0.4235 0.088 Uiso 1 1 calc R . . C11 C 0.9356(9) 0.3270(8) -0.5239(7) 0.107(3) Uani 1 1 d . . . H11 H 1.0272 0.3062 -0.5288 0.129 Uiso 1 1 calc R . . C12 C 0.8634(12) 0.3036(8) -0.5800(7) 0.111(3) Uani 1 1 d . . . H12 H 0.9048 0.2680 -0.6233 0.133 Uiso 1 1 calc R . . C14 C 0.7267(10) 0.3340(8) -0.5709(6) 0.097(3) Uani 1 1 d . . . H14 H 0.6756 0.3179 -0.6077 0.116 Uiso 1 1 calc R . . C15 C 0.6675(7) 0.3878(6) -0.5079(5) 0.069(2) Uani 1 1 d . . . H15 H 0.5759 0.4067 -0.5019 0.083 Uiso 1 1 calc R . . C16 C 0.9397(5) 0.1395(5) -0.2369(4) 0.0496(16) Uani 1 1 d . . . H16 H 0.9808 0.1642 -0.2002 0.060 Uiso 1 1 calc R . . C17 C 1.0169(6) 0.0628(5) -0.2763(5) 0.0589(18) Uani 1 1 d . . . C18 C 0.9536(7) 0.0276(6) -0.3306(5) 0.071(2) Uani 1 1 d . . . H18 H 1.0013 -0.0239 -0.3589 0.085 Uiso 1 1 calc R . . C19 C 0.8199(6) 0.0685(6) -0.3431(5) 0.0632(19) Uani 1 1 d . . . H19 H 0.7777 0.0439 -0.3793 0.076 Uiso 1 1 calc R . . C20 C 0.7494(6) 0.1448(5) -0.3024(4) 0.0446(15) Uani 1 1 d . . . C21 C 0.6099(6) 0.1933(5) -0.3127(4) 0.0458(15) Uani 1 1 d . . . C22 C 0.5326(6) 0.1701(6) -0.3688(5) 0.0637(19) Uani 1 1 d . . . H22 H 0.5701 0.1194 -0.4003 0.076 Uiso 1 1 calc R . . C23 C 0.4006(7) 0.2228(7) -0.3771(5) 0.071(2) Uani 1 1 d . . . H23 H 0.3495 0.2077 -0.4146 0.085 Uiso 1 1 calc R . . C24 C 0.3439(6) 0.2977(6) -0.3300(5) 0.0553(17) Uani 1 1 d . . . C25 C 0.4262(5) 0.3164(5) -0.2759(4) 0.0512(16) Uani 1 1 d . . . H25 H 0.3902 0.3666 -0.2437 0.061 Uiso 1 1 calc R . . C26 C 1.1618(6) 0.0186(7) -0.2590(6) 0.095(3) Uani 1 1 d . . . H26A H 1.1739 -0.0419 -0.2004 0.143 Uiso 1 1 calc R . . H26B H 1.1980 0.0757 -0.2549 0.143 Uiso 1 1 calc R . . H26C H 1.2059 -0.0061 -0.3106 0.143 Uiso 1 1 calc R . . C27 C 0.1994(6) 0.3547(7) -0.3346(5) 0.078(2) Uani 1 1 d . . . H27A H 0.1499 0.3084 -0.2874 0.117 Uiso 1 1 calc R . . H27B H 0.1700 0.3690 -0.3967 0.117 Uiso 1 1 calc R . . H27C H 0.1862 0.4230 -0.3225 0.117 Uiso 1 1 calc R . . C28 C 0.4933(6) 0.4937(5) -0.1549(4) 0.0458(15) Uani 1 1 d . . . H28 H 0.5345 0.5329 -0.2098 0.055 Uiso 1 1 calc R . . C29 C 0.3878(6) 0.5520(5) -0.1161(4) 0.0488(16) Uani 1 1 d . . . C30 C 0.3298(6) 0.4923(6) -0.0318(5) 0.0564(18) Uani 1 1 d . . . H30 H 0.2580 0.5281 -0.0019 0.068 Uiso 1 1 calc R . . C31 C 0.3791(5) 0.3805(6) 0.0068(4) 0.0506(16) Uani 1 1 d . . . H31 H 0.3412 0.3409 0.0633 0.061 Uiso 1 1 calc R . . C32 C 0.4850(5) 0.3268(5) -0.0382(4) 0.0441(15) Uani 1 1 d . . . C33 C 0.5423(5) 0.2075(5) -0.0030(4) 0.0422(15) Uani 1 1 d . . . C34 C 0.5032(6) 0.1361(6) 0.0825(5) 0.0573(18) Uani 1 1 d . . . H34 H 0.4363 0.1632 0.1213 0.069 Uiso 1 1 calc R . . C35 C 0.5625(6) 0.0270(6) 0.1094(4) 0.0538(17) Uani 1 1 d . . . H35 H 0.5364 -0.0203 0.1667 0.065 Uiso 1 1 calc R . . C36 C 0.6615(6) -0.0139(5) 0.0521(5) 0.0495(16) Uani 1 1 d . . . C37 C 0.6960(5) 0.0597(5) -0.0317(4) 0.0447(15) Uani 1 1 d . . . H37 H 0.7628 0.0333 -0.0709 0.054 Uiso 1 1 calc R . . C38 C 0.3371(6) 0.6748(5) -0.1622(5) 0.067(2) Uani 1 1 d . . . H38A H 0.3971 0.7020 -0.2135 0.101 Uiso 1 1 calc R . . H38B H 0.3301 0.7109 -0.1157 0.101 Uiso 1 1 calc R . . H38C H 0.2519 0.6893 -0.1864 0.101 Uiso 1 1 calc R . . C39 C 0.7315(7) -0.1323(5) 0.0784(5) 0.0671(19) Uani 1 1 d . . . H39A H 0.6991 -0.1717 0.1401 0.101 Uiso 1 1 calc R . . H39B H 0.8244 -0.1393 0.0798 0.101 Uiso 1 1 calc R . . H39C H 0.7162 -0.1623 0.0322 0.101 Uiso 1 1 calc R . . C40 C 0.5796(10) -0.1411(8) -0.3827(7) 0.102(3) Uani 1 1 d . . . S1 S 0.7159(2) -0.2311(2) -0.3220(2) 0.0966(8) Uani 1 1 d . . . O1 O 0.7712(6) -0.2954(5) -0.3881(5) 0.118(2) Uani 1 1 d . . . O2 O 0.6535(7) -0.2938(5) -0.2338(4) 0.117(2) Uani 1 1 d . . . O3 O 0.7928(9) -0.1645(6) -0.3157(7) 0.204(5) Uani 1 1 d . . . F1 F 0.5088(7) -0.0770(5) -0.3334(5) 0.176(3) Uani 1 1 d . . . F2 F 0.4989(6) -0.1883(6) -0.4018(4) 0.145(2) Uani 1 1 d . . . F3 F 0.6268(8) -0.0714(5) -0.4673(4) 0.172(3) Uani 1 1 d . . . H5 H 0.829(5) 0.532(5) -0.309(4) 0.05(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0363(3) 0.0467(4) 0.0366(3) -0.0157(2) -0.0047(2) -0.0090(2) Br1 0.0666(5) 0.1132(7) 0.0661(5) -0.0387(5) -0.0291(4) -0.0039(4) N1 0.040(3) 0.046(3) 0.039(3) -0.015(3) 0.000(2) -0.013(2) N2 0.039(3) 0.054(3) 0.039(3) -0.013(3) -0.002(2) -0.018(2) N3 0.042(3) 0.048(4) 0.037(3) -0.016(3) -0.008(2) -0.011(2) N4 0.032(3) 0.050(4) 0.042(3) -0.020(3) -0.003(2) -0.008(2) N5 0.045(3) 0.047(4) 0.051(4) -0.012(3) -0.006(3) -0.017(3) C1 0.038(3) 0.046(4) 0.043(4) -0.023(3) 0.001(3) -0.005(3) C2 0.040(3) 0.053(4) 0.052(4) -0.026(4) 0.000(3) -0.006(3) C3 0.048(4) 0.060(5) 0.071(5) -0.030(4) -0.004(3) -0.020(3) C4 0.040(4) 0.079(6) 0.076(5) -0.047(5) -0.009(3) -0.010(4) C5 0.041(4) 0.070(5) 0.058(4) -0.035(4) -0.015(3) -0.003(3) C6 0.042(3) 0.052(4) 0.048(4) -0.025(3) -0.008(3) -0.003(3) C7 0.039(3) 0.051(4) 0.041(4) -0.016(3) -0.003(3) -0.001(3) C8 0.045(4) 0.060(5) 0.045(4) -0.010(3) -0.008(3) -0.012(3) C9 0.053(4) 0.066(5) 0.035(4) -0.005(3) -0.006(3) -0.016(3) C10 0.055(4) 0.106(6) 0.052(5) -0.020(5) 0.002(3) -0.017(4) C11 0.079(6) 0.149(10) 0.074(7) -0.042(7) 0.025(5) -0.002(6) C12 0.152(10) 0.107(8) 0.065(7) -0.041(6) 0.021(6) -0.012(7) C14 0.121(8) 0.111(8) 0.068(6) -0.046(6) -0.006(5) -0.021(6) C15 0.064(4) 0.087(6) 0.056(5) -0.014(4) -0.014(4) -0.022(4) C16 0.041(4) 0.056(4) 0.054(4) -0.018(4) -0.005(3) -0.012(3) C17 0.051(4) 0.054(5) 0.071(5) -0.030(4) 0.001(3) -0.003(3) C18 0.065(5) 0.065(5) 0.092(6) -0.050(5) 0.000(4) 0.000(4) C19 0.060(4) 0.065(5) 0.083(5) -0.047(4) -0.005(4) -0.013(4) C20 0.046(4) 0.050(4) 0.047(4) -0.023(3) 0.001(3) -0.020(3) C21 0.046(4) 0.055(4) 0.044(4) -0.022(3) 0.000(3) -0.016(3) C22 0.057(4) 0.087(6) 0.068(5) -0.041(4) -0.010(3) -0.026(4) C23 0.066(5) 0.106(6) 0.060(5) -0.035(5) -0.006(4) -0.039(4) C24 0.049(4) 0.073(5) 0.043(4) -0.010(4) -0.004(3) -0.024(3) C25 0.041(4) 0.068(5) 0.043(4) -0.015(3) -0.005(3) -0.014(3) C26 0.057(5) 0.101(7) 0.137(8) -0.070(6) -0.010(5) 0.008(4) C27 0.044(4) 0.112(7) 0.075(5) -0.022(5) -0.019(3) -0.019(4) C28 0.051(4) 0.042(4) 0.045(4) -0.016(3) -0.006(3) -0.007(3) C29 0.045(4) 0.059(5) 0.047(4) -0.024(4) -0.009(3) -0.006(3) C30 0.038(3) 0.072(5) 0.066(5) -0.040(4) -0.005(3) 0.000(3) C31 0.042(4) 0.063(5) 0.047(4) -0.022(4) 0.004(3) -0.010(3) C32 0.037(3) 0.055(5) 0.043(4) -0.022(4) -0.006(3) -0.007(3) C33 0.039(3) 0.048(4) 0.041(4) -0.013(3) -0.007(3) -0.013(3) C34 0.056(4) 0.071(6) 0.043(4) -0.021(4) 0.003(3) -0.012(4) C35 0.053(4) 0.059(5) 0.041(4) -0.005(4) -0.001(3) -0.013(4) C36 0.054(4) 0.045(4) 0.049(4) -0.011(4) -0.008(3) -0.014(3) C37 0.044(3) 0.040(4) 0.051(4) -0.018(4) -0.008(3) -0.004(3) C38 0.065(4) 0.059(5) 0.074(5) -0.025(4) -0.012(4) -0.001(4) C39 0.076(5) 0.055(5) 0.065(5) -0.013(4) -0.006(4) -0.015(4) C40 0.119(8) 0.099(8) 0.102(8) -0.064(7) -0.023(6) 0.002(6) S1 0.0980(16) 0.0782(17) 0.122(2) -0.0347(16) -0.0292(15) -0.0199(13) O1 0.113(5) 0.078(4) 0.141(6) -0.040(4) 0.053(4) -0.011(3) O2 0.174(6) 0.096(5) 0.061(4) -0.010(3) 0.027(4) -0.036(4) O3 0.280(11) 0.125(6) 0.236(10) 0.010(6) -0.151(9) -0.118(7) F1 0.226(7) 0.113(5) 0.130(5) -0.044(4) 0.018(5) 0.047(5) F2 0.122(5) 0.197(7) 0.134(5) -0.061(5) -0.036(4) -0.042(4) F3 0.291(9) 0.111(5) 0.071(4) 0.006(4) -0.006(5) -0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C7 1.952(6) . ? Ru1 C1 2.050(5) . ? Ru1 N3 2.060(5) . ? Ru1 N1 2.064(4) . ? Ru1 N2 2.136(4) . ? Ru1 N4 2.151(5) . ? Br1 C5 1.904(6) . ? N1 C16 1.355(7) . ? N1 C20 1.369(7) . ? N2 C25 1.342(7) . ? N2 C21 1.345(7) . ? N3 C28 1.350(7) . ? N3 C32 1.367(7) . ? N4 C37 1.342(7) . ? N4 C33 1.356(7) . ? N5 C7 1.336(7) . ? N5 C2 1.400(8) . ? C1 C6 1.408(8) . ? C1 C2 1.414(8) . ? C2 C3 1.395(8) . ? C3 C4 1.389(9) . ? C4 C5 1.368(9) . ? C5 C6 1.396(8) . ? C7 C8 1.512(8) . ? C8 C9 1.506(8) . ? C9 C15 1.389(9) . ? C9 C10 1.394(9) . ? C10 C11 1.353(11) . ? C11 C12 1.365(12) . ? C12 C14 1.389(12) . ? C14 C15 1.367(10) . ? C16 C17 1.379(8) . ? C17 C18 1.380(9) . ? C17 C26 1.505(9) . ? C18 C19 1.381(9) . ? C19 C20 1.366(8) . ? C20 C21 1.444(8) . ? C21 C22 1.402(8) . ? C22 C23 1.380(9) . ? C23 C24 1.383(9) . ? C24 C25 1.384(8) . ? C24 C27 1.508(8) . ? C28 C29 1.362(8) . ? C29 C30 1.399(9) . ? C29 C38 1.513(9) . ? C30 C31 1.377(9) . ? C31 C32 1.385(8) . ? C32 C33 1.470(8) . ? C33 C34 1.393(8) . ? C34 C35 1.358(8) . ? C35 C36 1.380(8) . ? C36 C37 1.373(8) . ? C36 C39 1.488(9) . ? C40 F2 1.295(10) . ? C40 F1 1.335(9) . ? C40 F3 1.406(11) . ? C40 S1 1.733(10) . ? S1 O3 1.385(6) . ? S1 O2 1.474(6) . ? S1 O1 1.491(6) . ? 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 C7 Ru1 C1 79.6(2) . . ? C7 Ru1 N3 93.9(2) . . ? C1 Ru1 N3 90.39(19) . . ? C7 Ru1 N1 94.3(2) . . ? C1 Ru1 N1 98.46(19) . . ? N3 Ru1 N1 168.83(17) . . ? C7 Ru1 N2 95.3(2) . . ? C1 Ru1 N2 173.15(19) . . ? N3 Ru1 N2 94.59(17) . . ? N1 Ru1 N2 77.20(18) . . ? C7 Ru1 N4 169.8(2) . . ? C1 Ru1 N4 94.3(2) . . ? N3 Ru1 N4 77.87(19) . . ? N1 Ru1 N4 94.60(18) . . ? N2 Ru1 N4 91.38(16) . . ? C16 N1 C20 117.0(5) . . ? C16 N1 Ru1 126.0(4) . . ? C20 N1 Ru1 117.0(4) . . ? C25 N2 C21 119.5(5) . . ? C25 N2 Ru1 126.2(4) . . ? C21 N2 Ru1 114.3(3) . . ? C28 N3 C32 117.2(5) . . ? C28 N3 Ru1 125.9(4) . . ? C32 N3 Ru1 116.7(4) . . ? C37 N4 C33 118.7(5) . . ? C37 N4 Ru1 127.3(4) . . ? C33 N4 Ru1 114.0(4) . . ? C7 N5 C2 116.7(6) . . ? C6 C1 C2 115.5(5) . . ? C6 C1 Ru1 131.8(5) . . ? C2 C1 Ru1 112.6(4) . . ? C3 C2 N5 122.3(6) . . ? C3 C2 C1 124.3(6) . . ? N5 C2 C1 113.4(5) . . ? C4 C3 C2 117.5(6) . . ? C5 C4 C3 120.2(6) . . ? C4 C5 C6 122.1(6) . . ? C4 C5 Br1 118.3(4) . . ? C6 C5 Br1 119.6(5) . . ? C5 C6 C1 120.4(6) . . ? N5 C7 C8 114.2(5) . . ? N5 C7 Ru1 117.3(4) . . ? C8 C7 Ru1 128.5(5) . . ? C9 C8 C7 111.9(5) . . ? C15 C9 C10 116.0(7) . . ? C15 C9 C8 122.2(6) . . ? C10 C9 C8 121.7(6) . . ? C11 C10 C9 122.0(8) . . ? C10 C11 C12 121.1(8) . . ? C11 C12 C14 118.6(9) . . ? C15 C14 C12 119.9(8) . . ? C14 C15 C9 122.2(7) . . ? N1 C16 C17 124.8(6) . . ? C16 C17 C18 116.4(6) . . ? C16 C17 C26 121.4(6) . . ? C18 C17 C26 122.2(6) . . ? C17 C18 C19 120.4(6) . . ? C20 C19 C18 120.2(6) . . ? C19 C20 N1 121.2(5) . . ? C19 C20 C21 124.1(5) . . ? N1 C20 C21 114.7(5) . . ? N2 C21 C22 119.7(5) . . ? N2 C21 C20 116.8(5) . . ? C22 C21 C20 123.5(6) . . ? C23 C22 C21 119.8(6) . . ? C22 C23 C24 120.5(6) . . ? C23 C24 C25 116.5(6) . . ? C23 C24 C27 122.4(6) . . ? C25 C24 C27 121.1(6) . . ? N2 C25 C24 124.0(6) . . ? N3 C28 C29 125.6(6) . . ? C28 C29 C30 116.4(6) . . ? C28 C29 C38 121.4(6) . . ? C30 C29 C38 122.1(6) . . ? C31 C30 C29 119.9(6) . . ? C30 C31 C32 120.2(6) . . ? N3 C32 C31 120.8(6) . . ? N3 C32 C33 115.4(5) . . ? C31 C32 C33 123.8(6) . . ? N4 C33 C34 120.0(6) . . ? N4 C33 C32 115.7(5) . . ? C34 C33 C32 124.3(6) . . ? C35 C34 C33 120.1(6) . . ? C34 C35 C36 120.3(6) . . ? C37 C36 C35 117.3(6) . . ? C37 C36 C39 119.9(6) . . ? C35 C36 C39 122.8(6) . . ? N4 C37 C36 123.6(6) . . ? F2 C40 F1 106.3(9) . . ? F2 C40 F3 110.3(8) . . ? F1 C40 F3 106.9(8) . . ? F2 C40 S1 114.6(7) . . ? F1 C40 S1 111.3(7) . . ? F3 C40 S1 107.1(7) . . ? O3 S1 O2 118.5(5) . . ? O3 S1 O1 114.8(6) . . ? O2 S1 O1 113.3(4) . . ? O3 S1 C40 105.1(5) . . ? O2 S1 C40 101.5(5) . . ? O1 S1 C40 100.5(4) . . ? _diffrn_measured_fraction_theta_max 0.691 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.691 _refine_diff_density_max 1.171 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.092 data_mar158 _database_code_CSD 213864 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H51 Br F3 N5 O9 Ru S' _chemical_formula_sum 'C47 H51 Br F3 N5 O9 Ru S' _chemical_formula_weight 1099.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 14.063(3) _cell_length_b 17.027(3) _cell_length_c 20.484(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.50(3) _cell_angle_gamma 90.00 _cell_volume 4903.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 Mar300 _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13983 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.46 _reflns_number_total 6405 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6405 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.75694(3) 0.93965(3) 0.15953(2) 0.04268(18) Uani 1 1 d . . . Br2 Br 0.55933(6) 1.25046(4) 0.15375(4) 0.0765(3) Uani 1 1 d . . . O1 O 0.8175(3) 0.5803(2) 0.08867(19) 0.0630(12) Uani 1 1 d . . . O2 O 0.8748(4) 0.4213(3) 0.1094(2) 0.0856(15) Uani 1 1 d . . . O3 O 0.8302(5) 0.3731(4) -0.0569(4) 0.159(3) Uani 1 1 d . . . O4 O 0.6519(4) 0.4701(3) -0.0859(2) 0.0849(15) Uani 1 1 d . . . O5 O 0.6866(3) 0.5937(3) 0.0010(2) 0.0764(14) Uani 1 1 d . . . N1 N 0.8288(3) 0.9785(3) 0.2423(2) 0.0474(12) Uani 1 1 d . . . N2 N 0.8497(4) 1.0268(3) 0.1224(2) 0.0511(13) Uani 1 1 d . . . N3 N 0.7105(4) 0.9013(3) 0.0691(2) 0.0460(12) Uani 1 1 d . . . N4 N 0.8600(3) 0.8525(3) 0.1354(2) 0.0446(12) Uani 1 1 d . . . N5 N 0.5822(4) 0.9049(3) 0.2183(2) 0.0474(12) Uani 1 1 d . . . H5 H 0.5380 0.8781 0.2361 0.057 Uiso 1 1 calc R . . C1 C 0.8554(5) 1.0503(4) 0.0603(3) 0.070(2) Uani 1 1 d . . . H1 H 0.8215 1.0226 0.0282 0.084 Uiso 1 1 calc R . . C2 C 0.9090(7) 1.1134(5) 0.0417(4) 0.105(3) Uani 1 1 d . . . H2 H 0.9112 1.1283 -0.0019 0.126 Uiso 1 1 calc R . . C3 C 0.9595(7) 1.1541(5) 0.0895(5) 0.114(3) Uani 1 1 d . . . H3 H 0.9952 1.1979 0.0785 0.137 Uiso 1 1 calc R . . C4 C 0.9568(5) 1.1299(4) 0.1527(4) 0.083(2) Uani 1 1 d . . . H4 H 0.9912 1.1566 0.1851 0.100 Uiso 1 1 calc R . . C5 C 0.9023(5) 1.0655(4) 0.1682(3) 0.0578(17) Uani 1 1 d . . . C6 C 0.8949(4) 1.0354(3) 0.2347(3) 0.0485(16) Uani 1 1 d . . . C7 C 0.9510(5) 1.0616(4) 0.2867(4) 0.069(2) Uani 1 1 d . . . H7 H 0.9953 1.1013 0.2804 0.083 Uiso 1 1 calc R . . C8 C 0.9412(6) 1.0291(5) 0.3477(4) 0.077(2) Uani 1 1 d . . . H8 H 0.9798 1.0454 0.3827 0.093 Uiso 1 1 calc R . . C9 C 0.8733(6) 0.9721(4) 0.3561(3) 0.071(2) Uani 1 1 d . . . H9 H 0.8646 0.9498 0.3969 0.085 Uiso 1 1 calc R . . C10 C 0.8184(5) 0.9486(3) 0.3029(3) 0.0567(17) Uani 1 1 d . . . H10 H 0.7722 0.9104 0.3090 0.068 Uiso 1 1 calc R . . C11 C 0.6303(5) 0.9248(3) 0.0377(3) 0.0596(17) Uani 1 1 d . . . H11 H 0.5909 0.9603 0.0585 0.072 Uiso 1 1 calc R . . C12 C 0.6035(5) 0.8991(4) -0.0237(3) 0.073(2) Uani 1 1 d . . . H12 H 0.5474 0.9169 -0.0437 0.088 Uiso 1 1 calc R . . C13 C 0.6607(6) 0.8468(4) -0.0550(3) 0.074(2) Uani 1 1 d . . . H13 H 0.6447 0.8294 -0.0969 0.089 Uiso 1 1 calc R . . C14 C 0.7402(5) 0.8211(4) -0.0242(3) 0.0644(18) Uani 1 1 d . . . H14 H 0.7790 0.7849 -0.0446 0.077 Uiso 1 1 calc R . . C15 C 0.7651(5) 0.8480(3) 0.0382(3) 0.0504(16) Uani 1 1 d . . . C16 C 0.8495(4) 0.8206(3) 0.0751(3) 0.0471(15) Uani 1 1 d . . . C17 C 0.9142(5) 0.7676(3) 0.0515(3) 0.0585(18) Uani 1 1 d . . . H17 H 0.9061 0.7467 0.0098 0.070 Uiso 1 1 calc R . . C18 C 0.9889(6) 0.7465(4) 0.0895(4) 0.072(2) Uani 1 1 d . . . H18 H 1.0331 0.7109 0.0740 0.086 Uiso 1 1 calc R . . C19 C 1.0005(5) 0.7775(4) 0.1517(4) 0.0693(19) Uani 1 1 d . . . H19 H 1.0519 0.7630 0.1785 0.083 Uiso 1 1 calc R . . C20 C 0.9344(5) 0.8301(4) 0.1730(3) 0.0603(17) Uani 1 1 d . . . H20 H 0.9415 0.8508 0.2148 0.072 Uiso 1 1 calc R . . C21 C 0.6515(4) 1.0179(3) 0.1738(2) 0.0428(14) Uani 1 1 d . . . C22 C 0.5696(5) 0.9853(3) 0.2028(2) 0.0465(15) Uani 1 1 d . . . C23 C 0.4878(4) 1.0273(4) 0.2163(3) 0.0525(16) Uani 1 1 d . . . H23 H 0.4358 1.0026 0.2345 0.063 Uiso 1 1 calc R . . C24 C 0.4851(5) 1.1069(4) 0.2021(3) 0.0546(17) Uani 1 1 d . . . H24 H 0.4319 1.1369 0.2114 0.065 Uiso 1 1 calc R . . C25 C 0.5629(5) 1.1403(3) 0.1740(3) 0.0497(16) Uani 1 1 d . . . C26 C 0.6444(4) 1.0982(3) 0.1603(3) 0.0521(16) Uani 1 1 d . . . H26 H 0.6953 1.1239 0.1417 0.062 Uiso 1 1 calc R . . C27 C 0.6657(4) 0.8723(3) 0.2040(2) 0.0457(15) Uani 1 1 d . . . C28 C 0.6745(5) 0.7869(3) 0.2254(3) 0.0518(16) Uani 1 1 d . . . H28A H 0.7332 0.7798 0.2506 0.062 Uiso 1 1 calc R . . H28B H 0.6220 0.7736 0.2531 0.062 Uiso 1 1 calc R . . C29 C 0.6738(5) 0.7331(3) 0.1663(3) 0.0480(15) Uani 1 1 d . . . C30 C 0.7464(4) 0.6793(3) 0.1570(3) 0.0498(15) Uani 1 1 d . . . H30 H 0.7946 0.6741 0.1886 0.060 Uiso 1 1 calc R . . C31 C 0.7478(5) 0.6340(3) 0.1020(3) 0.0514(16) Uani 1 1 d . . . C32 C 0.6767(5) 0.6402(3) 0.0538(3) 0.0556(17) Uani 1 1 d . . . C33 C 0.6032(5) 0.6911(4) 0.0629(3) 0.0629(19) Uani 1 1 d . . . H33 H 0.5542 0.6947 0.0317 0.075 Uiso 1 1 calc R . . C34 C 0.6014(5) 0.7378(3) 0.1190(3) 0.0589(18) Uani 1 1 d . . . H34 H 0.5511 0.7724 0.1248 0.071 Uiso 1 1 calc R . . C35 C 0.8828(5) 0.5577(4) 0.1390(3) 0.0646(18) Uani 1 1 d . . . H35A H 0.8492 0.5448 0.1783 0.077 Uiso 1 1 calc R . . H35B H 0.9267 0.6002 0.1488 0.077 Uiso 1 1 calc R . . C36 C 0.9363(5) 0.4865(5) 0.1151(3) 0.079(2) Uani 1 1 d . . . H36A H 0.9631 0.4979 0.0729 0.095 Uiso 1 1 calc R . . H36B H 0.9883 0.4743 0.1455 0.095 Uiso 1 1 calc R . . C37 C 0.8824(8) 0.3766(6) 0.0527(4) 0.134(4) Uani 1 1 d . . . H37A H 0.8603 0.3234 0.0602 0.160 Uiso 1 1 calc R . . H37B H 0.9481 0.3744 0.0395 0.160 Uiso 1 1 calc R . . C38 C 0.8188(9) 0.4176(7) -0.0016(5) 0.156(5) Uani 1 1 d . . . H38A H 0.7527 0.4184 0.0106 0.187 Uiso 1 1 calc R . . H38B H 0.8398 0.4712 -0.0087 0.187 Uiso 1 1 calc R . . C39 C 0.7944(10) 0.4133(8) -0.1180(5) 0.189(6) Uani 1 1 d . . . H39A H 0.8201 0.4661 -0.1185 0.227 Uiso 1 1 calc R . . H39B H 0.8193 0.3856 -0.1553 0.227 Uiso 1 1 calc R . . C40 C 0.6971(8) 0.4180(6) -0.1258(6) 0.144(4) Uani 1 1 d . . . H40A H 0.6823 0.4322 -0.1708 0.172 Uiso 1 1 calc R . . H40B H 0.6707 0.3661 -0.1187 0.172 Uiso 1 1 calc R . . C41 C 0.6563(6) 0.5499(4) -0.1045(3) 0.081(2) Uani 1 1 d . . . H41A H 0.6177 0.5584 -0.1439 0.097 Uiso 1 1 calc R . . H41B H 0.7214 0.5641 -0.1136 0.097 Uiso 1 1 calc R . . C42 C 0.6211(6) 0.5990(4) -0.0514(3) 0.077(2) Uani 1 1 d . . . H42A H 0.6150 0.6531 -0.0658 0.093 Uiso 1 1 calc R . . H42B H 0.5591 0.5806 -0.0383 0.093 Uiso 1 1 calc R . . S1 S 0.13101(15) 0.31525(12) 0.18845(10) 0.0774(6) Uani 1 1 d . . . O6 O 0.0518(4) 0.2857(4) 0.2243(3) 0.129(2) Uani 1 1 d . . . O7 O 0.1311(4) 0.2953(4) 0.1209(2) 0.119(2) Uani 1 1 d . . . O8 O 0.1553(4) 0.3946(3) 0.2043(3) 0.1022(17) Uani 1 1 d . . . C43 C 0.2278(8) 0.2587(6) 0.2203(5) 0.103(3) Uani 1 1 d . . . F1 F 0.2166(5) 0.1826(3) 0.2089(3) 0.163(3) Uani 1 1 d . . . F2 F 0.3102(4) 0.2795(4) 0.1932(3) 0.150(2) Uani 1 1 d . . . F3 F 0.2415(5) 0.2663(4) 0.2836(3) 0.159(2) Uani 1 1 d . . . O9 O 0.7488(6) 0.0833(6) 0.9135(4) 0.155(3) Uani 1 1 d . . . C44 C 0.7689(11) 0.0348(9) 0.8603(6) 0.178(6) Uani 1 1 d . . . H44A H 0.7286 -0.0112 0.8622 0.214 Uiso 1 1 calc R . . H44B H 0.7516 0.0629 0.8205 0.214 Uiso 1 1 calc R . . C45 C 0.8592(10) 0.0109(10) 0.8560(9) 0.236(9) Uani 1 1 d . . . H45A H 0.8652 -0.0219 0.8182 0.353 Uiso 1 1 calc R . . H45B H 0.8770 -0.0184 0.8945 0.353 Uiso 1 1 calc R . . H45C H 0.9000 0.0557 0.8523 0.353 Uiso 1 1 calc R . . C46 C 0.6635(11) 0.1254(11) 0.9195(8) 0.200(7) Uani 1 1 d . . . H46A H 0.6132 0.0872 0.9253 0.240 Uiso 1 1 calc R . . H46B H 0.6505 0.1513 0.8781 0.240 Uiso 1 1 calc R . . C47 C 0.6548(14) 0.1826(12) 0.9691(8) 0.266(11) Uani 1 1 d . . . H47A H 0.5921 0.2049 0.9667 0.398 Uiso 1 1 calc R . . H47B H 0.7011 0.2232 0.9632 0.398 Uiso 1 1 calc R . . H47C H 0.6652 0.1584 1.0110 0.398 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0442(3) 0.0386(3) 0.0454(3) -0.0011(2) 0.0041(2) 0.0006(2) Br2 0.0903(6) 0.0451(4) 0.0939(6) 0.0020(3) -0.0029(4) 0.0144(4) O1 0.065(3) 0.067(3) 0.056(3) -0.005(2) -0.009(2) 0.016(2) O2 0.109(5) 0.058(3) 0.090(4) -0.013(3) 0.008(3) 0.010(3) O3 0.154(7) 0.169(7) 0.152(6) -0.093(5) -0.051(5) 0.088(5) O4 0.084(4) 0.068(3) 0.102(4) -0.025(3) -0.007(3) 0.009(3) O5 0.091(4) 0.065(3) 0.071(3) -0.015(2) -0.026(3) 0.027(3) N1 0.048(3) 0.043(3) 0.052(3) -0.002(2) 0.000(2) 0.009(3) N2 0.049(4) 0.046(3) 0.058(3) 0.003(3) 0.006(3) -0.005(3) N3 0.048(3) 0.045(3) 0.045(3) 0.002(2) 0.002(2) 0.006(3) N4 0.042(3) 0.046(3) 0.046(3) 0.007(2) 0.003(2) -0.001(2) N5 0.050(4) 0.040(3) 0.053(3) 0.001(2) 0.010(2) -0.007(3) C1 0.062(5) 0.078(5) 0.071(5) 0.011(4) 0.002(4) -0.015(4) C2 0.100(7) 0.120(7) 0.094(6) 0.039(6) 0.009(5) -0.048(6) C3 0.098(8) 0.106(7) 0.139(9) 0.030(6) 0.011(6) -0.043(6) C4 0.075(6) 0.077(5) 0.098(6) 0.005(5) 0.002(5) -0.032(5) C5 0.045(4) 0.058(4) 0.071(5) -0.003(4) 0.008(3) -0.003(4) C6 0.036(4) 0.043(3) 0.067(4) -0.018(3) -0.001(3) 0.001(3) C7 0.051(5) 0.067(5) 0.088(6) -0.031(4) -0.006(4) -0.001(4) C8 0.066(6) 0.086(6) 0.078(6) -0.032(4) -0.014(4) 0.016(5) C9 0.082(6) 0.078(5) 0.053(4) -0.009(4) -0.012(4) 0.021(5) C10 0.061(5) 0.054(4) 0.055(4) -0.006(3) 0.001(3) 0.007(3) C11 0.065(5) 0.055(4) 0.059(4) -0.001(3) 0.000(4) 0.006(4) C12 0.075(6) 0.080(5) 0.064(5) 0.001(4) -0.024(4) 0.012(4) C13 0.089(6) 0.081(5) 0.053(4) -0.014(4) -0.006(4) 0.002(5) C14 0.075(5) 0.063(4) 0.055(4) -0.014(3) 0.007(4) 0.007(4) C15 0.064(5) 0.046(4) 0.041(4) -0.003(3) 0.010(3) -0.006(3) C16 0.046(4) 0.045(3) 0.050(4) 0.004(3) 0.009(3) -0.002(3) C17 0.069(5) 0.046(4) 0.061(4) -0.002(3) 0.018(4) 0.012(4) C18 0.068(6) 0.066(5) 0.082(5) 0.004(4) 0.023(4) 0.026(4) C19 0.055(5) 0.068(5) 0.085(6) 0.008(4) -0.003(4) 0.011(4) C20 0.059(5) 0.065(4) 0.057(4) 0.000(3) 0.003(4) 0.007(4) C21 0.052(4) 0.037(3) 0.039(3) 0.000(3) -0.004(3) -0.007(3) C22 0.058(5) 0.042(4) 0.040(3) -0.003(3) -0.007(3) -0.005(3) C23 0.043(4) 0.057(4) 0.057(4) 0.005(3) 0.000(3) 0.008(3) C24 0.050(5) 0.059(4) 0.054(4) -0.004(3) -0.003(3) 0.017(4) C25 0.056(5) 0.043(3) 0.050(4) -0.005(3) -0.004(3) 0.007(3) C26 0.054(5) 0.050(4) 0.053(4) -0.002(3) 0.005(3) -0.003(3) C27 0.053(4) 0.044(3) 0.040(3) -0.008(3) 0.004(3) 0.007(3) C28 0.057(4) 0.042(3) 0.057(4) 0.004(3) 0.006(3) -0.001(3) C29 0.049(4) 0.038(3) 0.057(4) 0.006(3) 0.000(3) -0.007(3) C30 0.049(4) 0.044(3) 0.057(4) 0.002(3) 0.001(3) 0.003(3) C31 0.052(4) 0.040(3) 0.063(4) 0.004(3) 0.005(3) 0.003(3) C32 0.068(5) 0.036(3) 0.062(4) 0.001(3) -0.008(4) 0.004(3) C33 0.065(5) 0.052(4) 0.070(5) 0.003(4) -0.021(4) -0.001(4) C34 0.055(5) 0.047(4) 0.075(5) 0.005(3) -0.001(4) 0.006(3) C35 0.068(5) 0.065(4) 0.060(4) 0.002(3) -0.008(4) 0.010(4) C36 0.078(6) 0.104(6) 0.056(4) 0.007(4) 0.005(4) 0.042(5) C37 0.155(10) 0.129(8) 0.116(8) -0.045(7) -0.024(7) 0.065(7) C38 0.170(12) 0.188(11) 0.109(8) -0.057(8) -0.016(7) 0.082(9) C39 0.187(16) 0.259(16) 0.118(9) -0.062(9) -0.047(9) 0.097(12) C40 0.105(9) 0.144(9) 0.178(11) -0.058(8) -0.054(8) 0.039(8) C41 0.076(6) 0.088(6) 0.078(5) -0.013(4) -0.005(4) -0.008(5) C42 0.089(6) 0.064(4) 0.077(5) -0.010(4) -0.020(4) 0.011(4) S1 0.0611(14) 0.0851(14) 0.0864(15) -0.0269(11) 0.0071(11) 0.0067(11) O6 0.088(5) 0.146(5) 0.154(5) -0.051(4) 0.055(4) -0.033(4) O7 0.122(5) 0.155(5) 0.081(4) -0.056(4) -0.002(3) 0.037(4) O8 0.114(5) 0.070(3) 0.123(4) -0.026(3) 0.004(3) 0.010(3) C43 0.112(9) 0.091(7) 0.105(8) -0.021(6) 0.005(6) 0.019(6) F1 0.202(7) 0.082(4) 0.205(6) -0.007(4) 0.013(5) 0.045(4) F2 0.065(4) 0.174(6) 0.210(6) 0.006(5) 0.022(4) 0.025(4) F3 0.185(7) 0.175(6) 0.114(4) 0.000(4) -0.022(4) 0.059(5) O9 0.121(7) 0.221(9) 0.124(6) -0.001(6) -0.002(5) 0.031(6) C44 0.200(18) 0.215(16) 0.120(10) 0.004(10) -0.005(11) -0.050(13) C45 0.118(13) 0.212(16) 0.38(2) -0.092(15) 0.048(13) 0.033(12) C46 0.136(14) 0.237(19) 0.225(18) 0.100(14) -0.022(13) 0.020(13) C47 0.25(2) 0.34(3) 0.211(18) -0.047(16) 0.029(15) 0.125(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C27 1.963(6) . ? Ru1 C21 2.020(6) . ? Ru1 N3 2.055(4) . ? Ru1 N1 2.060(5) . ? Ru1 N2 2.129(5) . ? Ru1 N4 2.141(5) . ? Br2 C25 1.921(6) . ? O1 C31 1.373(7) . ? O1 C35 1.415(7) . ? O2 C37 1.395(8) . ? O2 C36 1.410(9) . ? O3 C38 1.375(9) . ? O3 C39 1.501(12) . ? O4 C40 1.373(10) . ? O4 C41 1.414(8) . ? O5 C32 1.352(7) . ? O5 C42 1.399(7) . ? N1 C10 1.354(7) . ? N1 C6 1.354(7) . ? N2 C1 1.338(7) . ? N2 C5 1.351(7) . ? N3 C11 1.346(7) . ? N3 C15 1.356(7) . ? N4 C20 1.337(7) . ? N4 C16 1.355(7) . ? N5 C27 1.338(7) . ? N5 C22 1.415(7) . ? C1 C2 1.371(9) . ? C2 C3 1.380(11) . ? C3 C4 1.361(10) . ? C4 C5 1.379(9) . ? C5 C6 1.463(8) . ? C6 C7 1.382(8) . ? C7 C8 1.379(9) . ? C8 C9 1.374(10) . ? C9 C10 1.377(8) . ? C11 C12 1.374(8) . ? C12 C13 1.370(9) . ? C13 C14 1.343(9) . ? C14 C15 1.393(8) . ? C15 C16 1.467(8) . ? C16 C17 1.378(8) . ? C17 C18 1.339(9) . ? C18 C19 1.386(9) . ? C19 C20 1.368(9) . ? C21 C26 1.398(7) . ? C21 C22 1.423(8) . ? C22 C23 1.389(8) . ? C23 C24 1.385(8) . ? C24 C25 1.373(8) . ? C25 C26 1.387(8) . ? C27 C28 1.521(7) . ? C28 C29 1.518(7) . ? C29 C30 1.387(8) . ? C29 C34 1.390(8) . ? C30 C31 1.367(8) . ? C31 C32 1.391(8) . ? C32 C33 1.364(9) . ? C33 C34 1.398(8) . ? C35 C36 1.515(9) . ? C37 C38 1.573(12) . ? C39 C40 1.376(14) . ? C41 C42 1.467(9) . ? S1 O7 1.426(5) . ? S1 O8 1.429(5) . ? S1 O6 1.441(6) . ? S1 C43 1.778(10) . ? C43 F3 1.312(9) . ? C43 F1 1.324(9) . ? C43 F2 1.345(11) . ? O9 C44 1.402(14) . ? O9 C46 1.406(16) . ? C44 C45 1.338(17) . ? C46 C47 1.415(19) . ? 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 C27 Ru1 C21 80.1(2) . . ? C27 Ru1 N3 92.1(2) . . ? C21 Ru1 N3 97.0(2) . . ? C27 Ru1 N1 96.8(2) . . ? C21 Ru1 N1 90.89(19) . . ? N3 Ru1 N1 169.0(2) . . ? C27 Ru1 N2 170.8(2) . . ? C21 Ru1 N2 92.9(2) . . ? N3 Ru1 N2 94.75(19) . . ? N1 Ru1 N2 77.2(2) . . ? C27 Ru1 N4 99.0(2) . . ? C21 Ru1 N4 173.85(19) . . ? N3 Ru1 N4 76.88(18) . . ? N1 Ru1 N4 95.26(18) . . ? N2 Ru1 N4 88.60(18) . . ? C31 O1 C35 119.3(5) . . ? C37 O2 C36 116.0(7) . . ? C38 O3 C39 113.0(8) . . ? C40 O4 C41 115.9(8) . . ? C32 O5 C42 119.8(5) . . ? C10 N1 C6 117.7(5) . . ? C10 N1 Ru1 124.9(4) . . ? C6 N1 Ru1 117.3(4) . . ? C1 N2 C5 117.9(5) . . ? C1 N2 Ru1 126.9(4) . . ? C5 N2 Ru1 114.9(4) . . ? C11 N3 C15 117.0(5) . . ? C11 N3 Ru1 125.4(4) . . ? C15 N3 Ru1 117.6(4) . . ? C20 N4 C16 118.4(5) . . ? C20 N4 Ru1 126.1(4) . . ? C16 N4 Ru1 115.5(4) . . ? C27 N5 C22 117.3(5) . . ? N2 C1 C2 123.1(7) . . ? C1 C2 C3 118.2(7) . . ? C4 C3 C2 119.8(7) . . ? C3 C4 C5 119.2(7) . . ? N2 C5 C4 121.7(6) . . ? N2 C5 C6 115.1(5) . . ? C4 C5 C6 123.1(6) . . ? N1 C6 C7 121.5(6) . . ? N1 C6 C5 115.1(5) . . ? C7 C6 C5 123.4(6) . . ? C8 C7 C6 120.0(7) . . ? C9 C8 C7 118.9(6) . . ? C8 C9 C10 118.9(7) . . ? N1 C10 C9 123.0(7) . . ? N3 C11 C12 123.3(6) . . ? C13 C12 C11 119.0(6) . . ? C14 C13 C12 118.9(6) . . ? C13 C14 C15 120.7(6) . . ? N3 C15 C14 121.1(6) . . ? N3 C15 C16 115.7(5) . . ? C14 C15 C16 123.3(6) . . ? N4 C16 C17 121.7(5) . . ? N4 C16 C15 114.2(5) . . ? C17 C16 C15 124.1(6) . . ? C18 C17 C16 119.1(6) . . ? C17 C18 C19 120.3(6) . . ? C20 C19 C18 118.5(6) . . ? N4 C20 C19 122.1(6) . . ? C26 C21 C22 114.2(5) . . ? C26 C21 Ru1 131.8(5) . . ? C22 C21 Ru1 114.1(4) . . ? C23 C22 N5 123.6(6) . . ? C23 C22 C21 124.4(5) . . ? N5 C22 C21 111.9(5) . . ? C24 C23 C22 118.7(6) . . ? C25 C24 C23 118.4(6) . . ? C24 C25 C26 122.8(5) . . ? C24 C25 Br2 118.6(5) . . ? C26 C25 Br2 118.5(5) . . ? C25 C26 C21 121.4(6) . . ? N5 C27 C28 113.5(5) . . ? N5 C27 Ru1 116.5(4) . . ? C28 C27 Ru1 130.0(4) . . ? C29 C28 C27 110.4(4) . . ? C30 C29 C34 118.1(6) . . ? C30 C29 C28 121.2(5) . . ? C34 C29 C28 120.7(6) . . ? C31 C30 C29 120.9(6) . . ? C30 C31 O1 124.5(5) . . ? C30 C31 C32 121.0(6) . . ? O1 C31 C32 114.5(5) . . ? O5 C32 C33 125.1(6) . . ? O5 C32 C31 115.9(6) . . ? C33 C32 C31 119.0(6) . . ? C32 C33 C34 120.2(6) . . ? C29 C34 C33 120.8(6) . . ? O1 C35 C36 107.5(5) . . ? O2 C36 C35 110.3(6) . . ? O2 C37 C38 107.0(7) . . ? O3 C38 C37 105.2(8) . . ? C40 C39 O3 115.7(13) . . ? O4 C40 C39 116.2(9) . . ? O4 C41 C42 109.3(6) . . ? O5 C42 C41 107.7(6) . . ? O7 S1 O8 116.0(4) . . ? O7 S1 O6 115.6(4) . . ? O8 S1 O6 113.5(3) . . ? O7 S1 C43 101.9(4) . . ? O8 S1 C43 104.7(4) . . ? O6 S1 C43 102.6(5) . . ? F3 C43 F1 106.5(9) . . ? F3 C43 F2 106.0(9) . . ? F1 C43 F2 106.6(8) . . ? F3 C43 S1 113.6(7) . . ? F1 C43 S1 112.3(7) . . ? F2 C43 S1 111.5(7) . . ? C44 O9 C46 123.9(12) . . ? C45 C44 O9 116.1(13) . . ? O9 C46 C47 120.3(15) . . ? _diffrn_measured_fraction_theta_max 0.704 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.704 _refine_diff_density_max 0.535 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.072