# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2097 data_severi25 _publ_contact_author_name 'Dr. Kay Severin' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7768' _publ_author_name ; 'da Silva, Ana C.' 'Piotrowski, Holger' 'Polborn, Kurt' 'Mayer, Peter' ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Heterometallic bromo-bridged complexes with Re(CO)3 fragments ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C9 H6 BR3 O3 Re Ru 2 C6 H6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H18 Br3 O3 Re Ru' _chemical_formula_weight 845.35 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 11.896(3) _cell_length_b 11.297(3) _cell_length_c 18.236(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2450.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 18 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_method ? _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 10.461 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.2702 _exptl_absorpt_correction_T_max 0.9928 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Nonius_CAD4 _diffrn_measurement_method \o-scan _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% -5.5 _diffrn_reflns_number 4056 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 23.97 _reflns_number_total 2019 _reflns_number_observed 1428 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4(Nonius,_1977) _computing_cell_refinement CAD4(Nonius,_1977) _computing_data_reduction process_MOLEN(Fair,_1990) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ZORTEP(Zsolnai,Huttner,_1994) _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+3.0584P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2019 _refine_ls_number_parameters 140 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_obs 0.0405 _refine_ls_wR_factor_all 0.0840 _refine_ls_wR_factor_obs 0.0683 _refine_ls_goodness_of_fit_all 1.203 _refine_ls_goodness_of_fit_obs 1.180 _refine_ls_restrained_S_all 1.203 _refine_ls_restrained_S_obs 1.180 _refine_ls_shift/esd_max -0.111 _refine_ls_shift/esd_mean 0.013 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.90098(9) 0.2500 0.49693(6) 0.0506(3) Uani 1 d S . Re1 Re 0.99239(4) 0.2500 0.67483(3) 0.0470(2) Uani 1 d S . O1 O 0.8426(9) 0.2500 0.8100(7) 0.106(4) Uani 1 d S . O2 O 1.1376(7) 0.0636(7) 0.7471(5) 0.094(3) Uani 1 d . . Br1 Br 1.10193(12) 0.2500 0.54957(9) 0.0710(5) Uani 1 d S . Br2 Br 0.86774(9) 0.10105(10) 0.60030(6) 0.0704(3) Uani 1 d . . C1 C 0.8993(11) 0.2500 0.7555(7) 0.057(4) Uani 1 d S . C2 C 1.0823(9) 0.1323(10) 0.7200(6) 0.067(3) Uani 1 d . . C3 C 0.9489(12) 0.1902(14) 0.3906(6) 0.111(6) Uani 1 d . . H3 H 1.0129(12) 0.1495(14) 0.3757(6) 0.133 Uiso 1 calc R . C4 C 0.8559(16) 0.1284(13) 0.4122(7) 0.120(6) Uani 1 d . . H4 H 0.8557(16) 0.0461(13) 0.4128(7) 0.144 Uiso 1 calc R . C5 C 0.7627(11) 0.1918(13) 0.4329(6) 0.103(6) Uani 1 d . . H5 H 0.6982(11) 0.1515(13) 0.4472(6) 0.123 Uiso 1 calc R . C6 C 0.7181(10) 0.1908(11) 0.2262(7) 0.095(4) Uani 1 d D . H6 H 0.7740(10) 0.1493(11) 0.2016(7) 0.115 Uiso 1 calc R . C7 C 0.6379(10) 0.1332(11) 0.2615(7) 0.093(4) Uani 1 d D . H7 H 0.6395(10) 0.0509(11) 0.2619(7) 0.111 Uiso 1 calc R . C8 C 0.5556(10) 0.1882(12) 0.2964(7) 0.105(5) Uani 1 d D . H8 H 0.4993(10) 0.1457(12) 0.3202(7) 0.125 Uiso 1 calc R . C9 C 0.5821(29) -0.0742(35) 0.4967(40) 0.183(13) Uani 1 d D . H9 H 0.6422(29) -0.1263(35) 0.4920(40) 0.219 Uiso 1 calc R . C10 C 0.5755(47) -0.0048(52) 0.5537(28) 0.198(19) Uani 1 d D . H10 H 0.6258(47) -0.0087(52) 0.5926(28) 0.238 Uiso 1 calc R . C11 C 0.4925(67) 0.0705(28) 0.5516(21) 0.188(16) Uani 1 d D . H11 H 0.4885(67) 0.1262(28) 0.5891(21) 0.225 Uiso 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 0.0598(7) 0.0553(7) 0.0366(6) 0.000 -0.0006(5) 0.000 Re1 0.0486(3) 0.0503(3) 0.0421(3) 0.000 -0.0058(3) 0.000 O1 0.082(8) 0.177(14) 0.058(8) 0.000 -0.003(6) 0.000 O2 0.114(7) 0.068(5) 0.100(6) 0.014(5) -0.024(5) 0.024(5) Br1 0.0529(8) 0.1015(13) 0.0586(10) 0.000 0.0072(7) 0.000 Br2 0.0888(7) 0.0659(7) 0.0566(7) 0.0099(6) -0.0170(5) -0.0261(6) C1 0.058(8) 0.088(11) 0.025(7) 0.000 -0.011(7) 0.000 C2 0.076(7) 0.066(7) 0.058(7) -0.010(6) -0.006(6) 0.002(6) C3 0.126(10) 0.163(18) 0.042(7) -0.027(8) -0.006(7) 0.052(10) C4 0.232(21) 0.070(10) 0.059(10) -0.017(8) -0.038(12) -0.003(12) C5 0.106(9) 0.168(18) 0.035(6) 0.006(7) -0.023(6) -0.048(9) C6 0.067(7) 0.098(10) 0.122(12) -0.023(8) -0.004(7) 0.018(6) C7 0.103(10) 0.071(8) 0.104(12) -0.011(8) -0.050(9) 0.002(8) C8 0.065(7) 0.157(15) 0.092(9) 0.033(9) -0.016(7) -0.041(8) C9 0.128(20) 0.182(33) 0.238(36) 0.094(33) 0.048(21) 0.013(19) C10 0.222(30) 0.218(35) 0.154(26) 0.109(24) -0.131(24) -0.152(27) C11 0.369(55) 0.111(19) 0.083(17) -0.037(16) 0.056(21) -0.057(24) _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 C5 2.122(11) . ? Ru1 C5 2.122(11) 7_565 ? Ru1 C3 2.131(12) 7_565 ? Ru1 C3 2.131(12) . ? Ru1 C4 2.136(13) . ? Ru1 C4 2.136(13) 7_565 ? Ru1 Br2 2.558(2) 7_565 ? Ru1 Br2 2.558(2) . ? Ru1 Br1 2.576(2) . ? Re1 C1 1.840(14) . ? Re1 C2 1.895(12) 7_565 ? Re1 C2 1.895(11) . ? Re1 Br2 2.6224(12) . ? Re1 Br2 2.6224(12) 7_565 ? Re1 Br1 2.630(2) . ? O1 C1 1.20(2) . ? O2 C2 1.130(12) . ? C3 C3 1.35(3) 7_565 ? C3 C4 1.37(2) . ? C4 C5 1.37(2) . ? C5 C5 1.32(3) 7_565 ? C6 C7 1.321(11) . ? C6 C6 1.34(2) 7_565 ? C7 C8 1.322(11) . ? C8 C8 1.40(3) 7_565 ? C9 C11 1.25(3) 5_656 ? C9 C10 1.304(13) . ? C10 C11 1.304(13) . ? C11 C9 1.25(3) 5_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ru1 C5 36.1(8) . 7_565 ? C5 Ru1 C3 78.7(5) . 7_565 ? C5 Ru1 C3 66.9(5) 7_565 7_565 ? C5 Ru1 C3 66.9(5) . . ? C5 Ru1 C3 78.7(5) 7_565 . ? C3 Ru1 C3 37.0(9) 7_565 . ? C5 Ru1 C4 37.6(5) . . ? C5 Ru1 C4 66.8(6) 7_565 . ? C3 Ru1 C4 67.2(6) 7_565 . ? C3 Ru1 C4 37.3(5) . . ? C5 Ru1 C4 66.8(6) . 7_565 ? C5 Ru1 C4 37.6(5) 7_565 7_565 ? C3 Ru1 C4 37.3(5) 7_565 7_565 ? C3 Ru1 C4 67.2(6) . 7_565 ? C4 Ru1 C4 80.0(8) . 7_565 ? C5 Ru1 Br2 119.3(4) . 7_565 ? C5 Ru1 Br2 94.7(3) 7_565 7_565 ? C3 Ru1 Br2 120.2(4) 7_565 7_565 ? C3 Ru1 Br2 157.0(4) . 7_565 ? C4 Ru1 Br2 156.6(5) . 7_565 ? C4 Ru1 Br2 94.1(4) 7_565 7_565 ? C5 Ru1 Br2 94.7(3) . . ? C5 Ru1 Br2 119.3(4) 7_565 . ? C3 Ru1 Br2 157.0(4) 7_565 . ? C3 Ru1 Br2 120.2(4) . . ? C4 Ru1 Br2 94.1(4) . . ? C4 Ru1 Br2 156.6(5) 7_565 . ? Br2 Ru1 Br2 82.28(7) 7_565 . ? C5 Ru1 Br1 157.6(4) . . ? C5 Ru1 Br1 157.6(4) 7_565 . ? C3 Ru1 Br1 95.2(4) 7_565 . ? C3 Ru1 Br1 95.2(4) . . ? C4 Ru1 Br1 120.2(5) . . ? C4 Ru1 Br1 120.2(5) 7_565 . ? Br2 Ru1 Br1 82.46(5) 7_565 . ? Br2 Ru1 Br1 82.46(5) . . ? C1 Re1 C2 89.6(4) . 7_565 ? C1 Re1 C2 89.6(4) . . ? C2 Re1 C2 89.1(6) 7_565 . ? C1 Re1 Br2 94.2(3) . . ? C2 Re1 Br2 174.1(3) 7_565 . ? C2 Re1 Br2 95.4(3) . . ? C1 Re1 Br2 94.2(3) . 7_565 ? C2 Re1 Br2 95.4(3) 7_565 7_565 ? C2 Re1 Br2 174.1(3) . 7_565 ? Br2 Re1 Br2 79.83(6) . 7_565 ? C1 Re1 Br1 172.7(4) . . ? C2 Re1 Br1 95.6(3) 7_565 . ? C2 Re1 Br1 95.6(3) . . ? Br2 Re1 Br1 80.21(4) . . ? Br2 Re1 Br1 80.21(4) 7_565 . ? Ru1 Br1 Re1 82.18(5) . . ? Ru1 Br2 Re1 82.67(5) . . ? O1 C1 Re1 177.2(11) . . ? O2 C2 Re1 178.7(10) . . ? C3 C3 C4 120.7(9) 7_565 . ? C3 C3 Ru1 71.5(4) 7_565 . ? C4 C3 Ru1 71.5(8) . . ? C3 C4 C5 117.9(15) . . ? C3 C4 Ru1 71.1(8) . . ? C5 C4 Ru1 70.7(8) . . ? C5 C5 C4 121.4(9) 7_565 . ? C5 C5 Ru1 71.9(4) 7_565 . ? C4 C5 Ru1 71.8(8) . . ? C7 C6 C6 119.5(8) . 7_565 ? C6 C7 C8 122.6(13) . . ? C7 C8 C8 118.0(8) . 7_565 ? C11 C9 C10 119.9(20) 5_656 . ? C9 C10 C11 114.5(22) . . ? C9 C11 C10 125.4(19) 5_656 . ? 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 C5 Ru1 Br1 Re1 -125.6(9) . . . . ? C5 Ru1 Br1 Re1 125.6(9) 7_565 . . . ? C3 Ru1 Br1 Re1 161.4(4) 7_565 . . . ? C3 Ru1 Br1 Re1 -161.4(4) . . . . ? C4 Ru1 Br1 Re1 -131.9(5) . . . . ? C4 Ru1 Br1 Re1 131.9(5) 7_565 . . . ? Br2 Ru1 Br1 Re1 41.58(3) 7_565 . . . ? Br2 Ru1 Br1 Re1 -41.58(3) . . . . ? C1 Re1 Br1 Ru1 0.000(1) . . . . ? C2 Re1 Br1 Ru1 -135.2(3) 7_565 . . . ? C2 Re1 Br1 Ru1 135.2(3) . . . . ? Br2 Re1 Br1 Ru1 40.63(3) . . . . ? Br2 Re1 Br1 Ru1 -40.63(3) 7_565 . . . ? C5 Ru1 Br2 Re1 -160.7(4) . . . . ? C5 Ru1 Br2 Re1 -132.8(4) 7_565 . . . ? C3 Ru1 Br2 Re1 127.3(9) 7_565 . . . ? C3 Ru1 Br2 Re1 133.3(4) . . . . ? C4 Ru1 Br2 Re1 161.6(5) . . . . ? C4 Ru1 Br2 Re1 -124.2(10) 7_565 . . . ? Br2 Ru1 Br2 Re1 -41.69(5) 7_565 . . . ? Br1 Ru1 Br2 Re1 41.66(3) . . . . ? C1 Re1 Br2 Ru1 134.3(2) . . . . ? C2 Re1 Br2 Ru1 4.4(31) 7_565 . . . ? C2 Re1 Br2 Ru1 -135.7(3) . . . . ? Br2 Re1 Br2 Ru1 40.78(5) 7_565 . . . ? Br1 Re1 Br2 Ru1 -40.92(4) . . . . ? C2 Re1 C1 O1 -44.6(3) 7_565 . . . ? C2 Re1 C1 O1 44.6(3) . . . . ? Br2 Re1 C1 O1 139.95(8) . . . . ? Br2 Re1 C1 O1 -139.95(6) 7_565 . . . ? Br1 Re1 C1 O1 180.00(6) . . . . ? C1 Re1 C2 O2 -112.3(450) . . . . ? C2 Re1 C2 O2 -22.7(453) 7_565 . . . ? Br2 Re1 C2 O2 153.5(450) . . . . ? Br2 Re1 C2 O2 117.6(437) 7_565 . . . ? Br1 Re1 C2 O2 72.8(450) . . . . ? C5 Ru1 C3 C3 102.3(5) . . . 7_565 ? C5 Ru1 C3 C3 66.4(4) 7_565 . . 7_565 ? C3 Ru1 C3 C3 0.000(4) 7_565 . . 7_565 ? C4 Ru1 C3 C3 132.8(9) . . . 7_565 ? C4 Ru1 C3 C3 28.9(5) 7_565 . . 7_565 ? Br2 Ru1 C3 C3 -8.8(7) 7_565 . . 7_565 ? Br2 Ru1 C3 C3 -176.1(4) . . . 7_565 ? Br1 Ru1 C3 C3 -91.75(14) . . . 7_565 ? C5 Ru1 C3 C4 -30.5(9) . . . . ? C5 Ru1 C3 C4 -66.4(10) 7_565 . . . ? C3 Ru1 C3 C4 -132.8(9) 7_565 . . . ? C4 Ru1 C3 C4 0.0 . . . . ? C4 Ru1 C3 C4 -104.0(13) 7_565 . . . ? Br2 Ru1 C3 C4 -141.6(10) 7_565 . . . ? Br2 Ru1 C3 C4 51.1(10) . . . . ? Br1 Ru1 C3 C4 135.4(9) . . . . ? C3 C3 C4 C5 0.8(16) 7_565 . . . ? Ru1 C3 C4 C5 54.8(11) . . . . ? C3 C3 C4 Ru1 -54.0(6) 7_565 . . . ? Ru1 C3 C4 Ru1 0.0 . . . . ? C5 Ru1 C4 C3 130.0(14) . . . . ? C5 Ru1 C4 C3 102.2(10) 7_565 . . . ? C3 Ru1 C4 C3 28.6(9) 7_565 . . . ? C3 Ru1 C4 C3 0.0 . . . . ? C4 Ru1 C4 C3 65.3(11) 7_565 . . . ? Br2 Ru1 C4 C3 142.4(9) 7_565 . . . ? Br2 Ru1 C4 C3 -137.6(9) . . . . ? Br1 Ru1 C4 C3 -53.9(10) . . . . ? C5 Ru1 C4 C5 0.000(3) . . . . ? C5 Ru1 C4 C5 -27.9(8) 7_565 . . . ? C3 Ru1 C4 C5 -101.4(10) 7_565 . . . ? C3 Ru1 C4 C5 -130.0(14) . . . . ? C4 Ru1 C4 C5 -64.7(11) 7_565 . . . ? Br2 Ru1 C4 C5 12.4(17) 7_565 . . . ? Br2 Ru1 C4 C5 92.4(8) . . . . ? Br1 Ru1 C4 C5 176.0(7) . . . . ? C3 C4 C5 C5 -0.8(16) . . . 7_565 ? Ru1 C4 C5 C5 54.3(5) . . . 7_565 ? C3 C4 C5 Ru1 -55.0(12) . . . . ? Ru1 C4 C5 Ru1 0.000(2) . . . . ? C5 Ru1 C5 C5 0.000(2) 7_565 . . 7_565 ? C3 Ru1 C5 C5 -66.1(5) 7_565 . . 7_565 ? C3 Ru1 C5 C5 -102.9(5) . . . 7_565 ? C4 Ru1 C5 C5 -133.2(9) . . . 7_565 ? C4 Ru1 C5 C5 -28.9(5) 7_565 . . 7_565 ? Br2 Ru1 C5 C5 52.4(2) 7_565 . . 7_565 ? Br2 Ru1 C5 C5 136.15(15) . . . 7_565 ? Br1 Ru1 C5 C5 -142.2(9) . . . 7_565 ? C5 Ru1 C5 C4 133.2(9) 7_565 . . . ? C3 Ru1 C5 C4 67.1(10) 7_565 . . . ? C3 Ru1 C5 C4 30.3(9) . . . . ? C4 Ru1 C5 C4 0.000(3) . . . . ? C4 Ru1 C5 C4 104.3(13) 7_565 . . . ? Br2 Ru1 C5 C4 -174.4(8) 7_565 . . . ? Br2 Ru1 C5 C4 -90.6(9) . . . . ? Br1 Ru1 C5 C4 -9.0(15) . . . . ? C6 C6 C7 C8 1.1(16) 7_565 . . . ? C6 C7 C8 C8 -1.1(15) . . . 7_565 ? C11 C9 C10 C11 -5.0(49) 5_656 . . . ? C9 C10 C11 C9 5.4(52) . . . 5_656 ? _refine_diff_density_max 0.728 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.146 data_severi22 _publ_contact_author_name 'Dr. Kay Severin' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7768' _publ_author_name 'da Silva, Ana C.' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Heterometallic bromo-bridged complexes with Re(CO)3 fragments ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C20 H28 Br3 Ru2+ C6 Br3 O6 Re2-' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H28 Br6 O6 Re2 Ru2' _chemical_formula_weight 1490.48 _chemical_melting_point ? _chemical_compound_source ? 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' 'Re' 'Re' -1.0185 7.2310 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting anorthic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6067(13) _cell_length_b 12.8694(14) _cell_length_c 16.152(4) _cell_angle_alpha 77.44(2) _cell_angle_beta 78.986(15) _cell_angle_gamma 71.207(11) _cell_volume 1829.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 18 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.706 _exptl_crystal_density_method ? _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 13.993 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5335 _exptl_absorpt_correction_T_max 0.9989 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Nonius_MACH3 _diffrn_measurement_method \o-2\T-scan _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% -3.8 _diffrn_reflns_number 5940 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 23.97 _reflns_number_total 5702 _reflns_number_observed 4736 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4(Nonius,_1977) _computing_cell_refinement CAD4(Nonius,_1977) _computing_data_reduction process_MOLEN(Fair,_1990) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ZORTEP(Zsolnai,_1994) _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+10.8915P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5702 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_obs 0.0409 _refine_ls_wR_factor_all 0.1133 _refine_ls_wR_factor_obs 0.1037 _refine_ls_goodness_of_fit_all 1.131 _refine_ls_goodness_of_fit_obs 1.143 _refine_ls_restrained_S_all 1.131 _refine_ls_restrained_S_obs 1.143 _refine_ls_shift/esd_max 0.038 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.88596(5) 0.60510(4) 0.22146(3) 0.0468(2) Uani 1 d . . Re2 Re 1.22278(5) 0.66112(4) 0.19421(3) 0.0407(2) Uani 1 d . . Ru3 Ru 0.51349(9) 0.21949(6) 0.41984(5) 0.0337(2) Uani 1 d . . Ru4 Ru 0.59408(11) 0.16120(7) 0.21791(5) 0.0412(2) Uani 1 d . . Br5 Br 1.03443(14) 0.69565(13) 0.08447(7) 0.0615(4) Uani 1 d . . Br6 Br 0.97043(14) 0.73859(10) 0.29283(8) 0.0534(3) Uani 1 d . . Br7 Br 0.58078(14) 0.33309(8) 0.27679(7) 0.0456(3) Uani 1 d . . Br8 Br 0.71870(13) 0.06409(9) 0.35298(7) 0.0460(3) Uani 1 d . . Br9 Br 0.36051(13) 0.16921(9) 0.32822(7) 0.0472(3) Uani 1 d . . Br10 Br 1.15181(15) 0.47519(10) 0.24573(8) 0.0566(3) Uani 1 d . . O1 O 0.5858(12) 0.7739(10) 0.2027(9) 0.108(5) Uani 1 d . . O2 O 0.7518(12) 0.4851(8) 0.3845(6) 0.078(3) Uani 1 d . . O3 O 0.8314(13) 0.4501(10) 0.1204(7) 0.089(3) Uani 1 d . . O4 O 1.2906(12) 0.8827(8) 0.1286(8) 0.089(3) Uani 1 d . . O5 O 1.4130(11) 0.6101(7) 0.3361(6) 0.068(3) Uani 1 d . . O6 O 1.4962(11) 0.5492(10) 0.0809(6) 0.082(3) Uani 1 d . . C1 C 0.7006(15) 0.7077(13) 0.2085(10) 0.070(4) Uani 1 d . . C2 C 0.8010(15) 0.5301(11) 0.3234(9) 0.058(3) Uani 1 d . . C3 C 0.8479(14) 0.5100(12) 0.1599(9) 0.062(3) Uani 1 d . . C4 C 1.2620(14) 0.7992(12) 0.1532(9) 0.061(3) Uani 1 d . . C5 C 1.3411(13) 0.6288(9) 0.2840(7) 0.045(3) Uani 1 d . . C6 C 1.3930(14) 0.5928(11) 0.1232(8) 0.056(3) Uani 1 d . . C7 C 0.6225(12) 0.1874(8) 0.5339(6) 0.040(2) Uani 1 d . . C8 C 0.5882(14) 0.3011(9) 0.4985(7) 0.047(3) Uani 1 d . . H8 H 0.6621(14) 0.3365(9) 0.4856(7) 0.056 Uiso 1 calc R . C9 C 0.4410(14) 0.3625(9) 0.4821(7) 0.049(3) Uani 1 d . . H9 H 0.4212(14) 0.4375(9) 0.4583(7) 0.058 Uiso 1 calc R . C10 C 0.3257(13) 0.3145(10) 0.5004(6) 0.048(3) Uani 1 d . . C11 C 0.3625(13) 0.1984(10) 0.5358(7) 0.050(3) Uani 1 d . . H11 H 0.2885(13) 0.1632(10) 0.5486(7) 0.060 Uiso 1 calc R . C12 C 0.5042(13) 0.1375(9) 0.5514(6) 0.043(3) Uani 1 d . . H12 H 0.5238(13) 0.0620(9) 0.5739(6) 0.052 Uiso 1 calc R . C13 C 0.7764(14) 0.1158(11) 0.5509(9) 0.061(3) Uani 1 d . . H13 H 0.7939(14) 0.0453(11) 0.5311(9) 0.074 Uiso 1 calc R . C14 C 0.7863(17) 0.0890(12) 0.6460(9) 0.073(4) Uani 1 d . . H14A H 0.7703(100) 0.1565(15) 0.6673(14) 0.087 Uiso 1 calc R . H14B H 0.8827(37) 0.0397(60) 0.6561(10) 0.087 Uiso 1 calc R . H14C H 0.7120(66) 0.0538(67) 0.6749(11) 0.087 Uiso 1 calc R . C15 C 0.8982(16) 0.1682(15) 0.5015(12) 0.088(5) Uani 1 d . . H15A H 0.9939(16) 0.1175(38) 0.5114(54) 0.106 Uiso 1 calc R . H15B H 0.8861(70) 0.2363(46) 0.5209(47) 0.106 Uiso 1 calc R . H15C H 0.8903(73) 0.1834(80) 0.4414(13) 0.106 Uiso 1 calc R . C16 C 0.1734(15) 0.3790(12) 0.4782(8) 0.070(4) Uani 1 d . . H16A H 0.1034(20) 0.3807(65) 0.5294(11) 0.084 Uiso 1 calc R . H16B H 0.1471(42) 0.3440(43) 0.4392(46) 0.084 Uiso 1 calc R . H16C H 0.1722(29) 0.4537(24) 0.4519(52) 0.084 Uiso 1 calc R . C17 C 0.4903(17) 0.1615(13) 0.1073(8) 0.065(4) Uani 1 d . . C18 C 0.5698(24) 0.0514(13) 0.1415(9) 0.083(5) Uani 1 d . . H18 H 0.5213(24) -0.0033(13) 0.1569(9) 0.099 Uiso 1 calc R . C19 C 0.7138(22) 0.0242(13) 0.1523(9) 0.081(5) Uani 1 d . . H19 H 0.7619(22) -0.0482(13) 0.1761(9) 0.097 Uiso 1 calc R . C20 C 0.7944(18) 0.1055(15) 0.1274(8) 0.081(5) Uani 1 d . . C21 C 0.7137(17) 0.2154(11) 0.0979(7) 0.062(4) Uani 1 d . . H21 H 0.7609(17) 0.2708(11) 0.0851(7) 0.075 Uiso 1 calc R . C22 C 0.5617(17) 0.2443(11) 0.0870(7) 0.061(4) Uani 1 d . . H22 H 0.5105(17) 0.3174(11) 0.0667(7) 0.074 Uiso 1 calc R . C23 C 0.3356(24) 0.1823(21) 0.0952(11) 0.112(7) Uani 1 d . . H23 H 0.2904(24) 0.1405(21) 0.1453(11) 0.134 Uiso 1 calc R . C24 C 0.3392(26) 0.1294(21) 0.0171(13) 0.124(7) Uani 1 d . . H24A H 0.2404(32) 0.1315(107) 0.0120(54) 0.149 Uiso 1 calc R . H24B H 0.4008(126) 0.0536(40) 0.0247(43) 0.149 Uiso 1 calc R . H24C H 0.3786(145) 0.1705(72) -0.0339(17) 0.149 Uiso 1 calc R . C25 C 0.2509(26) 0.2893(30) 0.0887(20) 0.218(20) Uani 1 d . . H25A H 0.1588(119) 0.2963(48) 0.0700(161) 0.261 Uiso 1 calc R . H25B H 0.3021(123) 0.3355(40) 0.0481(122) 0.261 Uiso 1 calc R . H25C H 0.2314(240) 0.3124(71) 0.1435(40) 0.261 Uiso 1 calc R . C26 C 0.9566(18) 0.0832(25) 0.1452(12) 0.181(15) Uani 1 d . . H26A H 1.0245(23) 0.0635(173) 0.0952(48) 0.217 Uiso 1 calc R . H26B H 0.9782(80) 0.0232(116) 0.1924(88) 0.217 Uiso 1 calc R . H26C H 0.9669(64) 0.1491(58) 0.1588(129) 0.217 Uiso 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 Re1 0.0487(3) 0.0495(3) 0.0443(3) 0.0000(2) -0.0042(2) -0.0233(2) Re2 0.0431(3) 0.0434(3) 0.0344(3) -0.0007(2) -0.0073(2) -0.0137(2) Ru3 0.0463(5) 0.0264(4) 0.0283(4) -0.0011(3) -0.0041(3) -0.0131(3) Ru4 0.0621(6) 0.0340(5) 0.0294(4) -0.0042(3) -0.0076(4) -0.0162(4) Br5 0.0545(7) 0.0938(10) 0.0363(6) 0.0130(6) -0.0132(5) -0.0334(7) Br6 0.0593(7) 0.0501(7) 0.0525(7) -0.0145(5) 0.0063(6) -0.0222(6) Br7 0.0728(8) 0.0329(6) 0.0338(6) -0.0011(4) -0.0028(5) -0.0245(5) Br8 0.0559(7) 0.0373(6) 0.0386(6) -0.0051(5) -0.0083(5) -0.0046(5) Br9 0.0534(7) 0.0466(6) 0.0478(6) -0.0059(5) -0.0110(5) -0.0216(5) Br10 0.0681(8) 0.0434(6) 0.0576(7) -0.0029(5) -0.0166(6) -0.0142(6) O1 0.054(6) 0.082(8) 0.164(12) 0.035(8) -0.016(7) -0.022(6) O2 0.113(8) 0.073(7) 0.054(6) 0.001(5) 0.010(6) -0.057(6) O3 0.099(8) 0.116(9) 0.082(7) -0.032(7) -0.007(6) -0.062(7) O4 0.079(7) 0.056(6) 0.123(9) 0.017(6) -0.003(6) -0.035(5) O5 0.096(7) 0.058(5) 0.058(5) -0.001(4) -0.045(5) -0.021(5) O6 0.068(6) 0.100(8) 0.061(6) -0.011(6) 0.003(5) -0.010(6) C1 0.049(8) 0.069(9) 0.086(10) 0.010(8) -0.001(7) -0.028(7) C2 0.065(8) 0.064(8) 0.056(8) -0.019(7) -0.002(6) -0.030(7) C3 0.049(7) 0.077(9) 0.067(9) -0.011(7) -0.005(6) -0.031(7) C4 0.047(7) 0.069(9) 0.070(9) -0.002(7) -0.016(6) -0.022(7) C5 0.055(7) 0.040(6) 0.038(6) -0.008(5) -0.007(5) -0.009(5) C6 0.044(7) 0.074(9) 0.046(7) -0.010(6) 0.000(6) -0.014(6) C7 0.055(7) 0.034(6) 0.034(6) -0.009(4) -0.008(5) -0.013(5) C8 0.066(8) 0.039(6) 0.038(6) -0.005(5) -0.007(5) -0.021(6) C9 0.073(8) 0.037(6) 0.028(5) -0.006(5) 0.004(5) -0.012(6) C10 0.053(7) 0.053(7) 0.026(5) -0.011(5) 0.008(5) -0.004(5) C11 0.049(7) 0.058(7) 0.042(6) -0.001(5) -0.004(5) -0.020(6) C12 0.065(7) 0.033(6) 0.030(5) 0.003(4) -0.012(5) -0.013(5) C13 0.062(8) 0.056(8) 0.073(9) -0.020(7) -0.026(7) -0.010(6) C14 0.093(11) 0.063(9) 0.069(9) -0.015(7) -0.044(8) -0.010(8) C15 0.052(8) 0.110(13) 0.103(13) -0.012(10) -0.015(8) -0.025(9) C16 0.064(8) 0.075(9) 0.047(7) -0.009(7) -0.003(6) 0.011(7) C17 0.083(10) 0.086(10) 0.032(6) -0.008(6) -0.020(6) -0.027(8) C18 0.151(17) 0.063(10) 0.046(8) -0.016(7) -0.021(9) -0.039(11) C19 0.125(15) 0.054(9) 0.045(8) -0.018(7) -0.007(9) 0.002(9) C20 0.089(11) 0.096(12) 0.038(7) -0.015(8) 0.020(7) -0.012(9) C21 0.099(11) 0.060(8) 0.028(6) 0.000(6) 0.003(6) -0.034(8) C22 0.093(11) 0.058(8) 0.033(6) 0.008(6) -0.017(6) -0.025(7) C23 0.109(15) 0.160(20) 0.051(9) -0.026(11) -0.018(10) -0.011(14) C24 0.139(18) 0.160(21) 0.095(14) -0.045(14) -0.024(13) -0.053(16) C25 0.092(16) 0.331(46) 0.245(35) -0.214(35) -0.077(19) 0.057(22) C26 0.057(11) 0.302(35) 0.068(12) 0.014(16) 0.023(9) 0.058(16) _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 Re1 C1 1.861(15) . ? Re1 C3 1.891(15) . ? Re1 C2 1.900(14) . ? Re1 Br10 2.6112(14) . ? Re1 Br5 2.6519(13) . ? Re1 Br6 2.6561(13) . ? Re2 C4 1.887(14) . ? Re2 C6 1.886(13) . ? Re2 C5 1.906(12) . ? Re2 Br10 2.6175(14) . ? Re2 Br5 2.6417(13) . ? Re2 Br6 2.6582(13) . ? Ru3 C9 2.143(11) . ? Ru3 C8 2.155(11) . ? Ru3 C12 2.157(10) . ? Ru3 C11 2.163(11) . ? Ru3 C7 2.189(10) . ? Ru3 C10 2.194(10) . ? Ru3 Br7 2.5423(14) . ? Ru3 Br9 2.5747(14) . ? Ru3 Br8 2.5763(14) . ? Ru4 C19 2.144(14) . ? Ru4 C18 2.157(14) . ? Ru4 C21 2.154(12) . ? Ru4 C22 2.182(11) . ? Ru4 C20 2.201(13) . ? Ru4 C17 2.205(12) . ? Ru4 Br7 2.5496(14) . ? Ru4 Br8 2.5696(15) . ? Ru4 Br9 2.574(2) . ? O1 C1 1.16(2) . ? O2 C2 1.133(15) . ? O3 C3 1.17(2) . ? O4 C4 1.16(2) . ? O5 C5 1.127(13) . ? O6 C6 1.146(14) . ? C7 C8 1.406(15) . ? C7 C12 1.43(2) . ? C7 C13 1.51(2) . ? C8 C9 1.42(2) . ? C9 C10 1.39(2) . ? C10 C11 1.43(2) . ? C10 C16 1.50(2) . ? C11 C12 1.37(2) . ? C13 C14 1.51(2) . ? C13 C15 1.54(2) . ? C17 C22 1.40(2) . ? C17 C18 1.42(2) . ? C17 C23 1.47(2) . ? C18 C19 1.35(2) . ? C19 C20 1.44(2) . ? C20 C21 1.40(2) . ? C20 C26 1.56(3) . ? C21 C22 1.42(2) . ? C23 C25 1.35(3) . ? C23 C24 1.55(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C3 91.4(6) . . ? C1 Re1 C2 89.5(6) . . ? C3 Re1 C2 88.6(6) . . ? C1 Re1 Br10 174.5(5) . . ? C3 Re1 Br10 94.0(4) . . ? C2 Re1 Br10 91.4(4) . . ? C1 Re1 Br5 96.9(4) . . ? C3 Re1 Br5 92.6(4) . . ? C2 Re1 Br5 173.5(4) . . ? Br10 Re1 Br5 82.13(5) . . ? C1 Re1 Br6 92.7(5) . . ? C3 Re1 Br6 172.5(4) . . ? C2 Re1 Br6 97.7(4) . . ? Br10 Re1 Br6 81.88(4) . . ? Br5 Re1 Br6 80.69(4) . . ? C4 Re2 C6 89.4(6) . . ? C4 Re2 C5 91.4(5) . . ? C6 Re2 C5 89.2(5) . . ? C4 Re2 Br10 176.0(4) . . ? C6 Re2 Br10 92.2(4) . . ? C5 Re2 Br10 92.2(3) . . ? C4 Re2 Br5 94.0(4) . . ? C6 Re2 Br5 95.8(4) . . ? C5 Re2 Br5 172.7(3) . . ? Br10 Re2 Br5 82.20(5) . . ? C4 Re2 Br6 96.5(4) . . ? C6 Re2 Br6 173.3(4) . . ? C5 Re2 Br6 93.7(3) . . ? Br10 Re2 Br6 81.72(4) . . ? Br5 Re2 Br6 80.84(4) . . ? C9 Ru3 C8 38.7(5) . . ? C9 Ru3 C12 80.5(4) . . ? C8 Ru3 C12 68.3(4) . . ? C9 Ru3 C11 67.7(5) . . ? C8 Ru3 C11 80.6(5) . . ? C12 Ru3 C11 37.1(4) . . ? C9 Ru3 C7 69.0(4) . . ? C8 Ru3 C7 37.7(4) . . ? C12 Ru3 C7 38.5(4) . . ? C11 Ru3 C7 68.5(4) . . ? C9 Ru3 C10 37.4(5) . . ? C8 Ru3 C10 69.1(5) . . ? C12 Ru3 C10 68.6(4) . . ? C11 Ru3 C10 38.4(4) . . ? C7 Ru3 C10 82.2(4) . . ? C9 Ru3 Br7 92.1(3) . . ? C8 Ru3 Br7 96.9(3) . . ? C12 Ru3 Br7 163.8(3) . . ? C11 Ru3 Br7 150.7(3) . . ? C7 Ru3 Br7 125.3(3) . . ? C10 Ru3 Br7 113.5(3) . . ? C9 Ru3 Br9 125.5(3) . . ? C8 Ru3 Br9 164.1(3) . . ? C12 Ru3 Br9 115.0(3) . . ? C11 Ru3 Br9 93.4(3) . . ? C7 Ru3 Br9 151.7(3) . . ? C10 Ru3 Br9 97.1(3) . . ? Br7 Ru3 Br9 81.06(4) . . ? C9 Ru3 Br8 151.8(4) . . ? C8 Ru3 Br8 114.7(3) . . ? C12 Ru3 Br8 98.6(3) . . ? C11 Ru3 Br8 126.6(3) . . ? C7 Ru3 Br8 92.7(3) . . ? C10 Ru3 Br8 164.9(3) . . ? Br7 Ru3 Br8 81.08(4) . . ? Br9 Ru3 Br8 80.70(5) . . ? C19 Ru4 C18 36.6(6) . . ? C19 Ru4 C21 68.7(6) . . ? C18 Ru4 C21 80.2(6) . . ? C19 Ru4 C22 81.0(6) . . ? C18 Ru4 C22 68.0(5) . . ? C21 Ru4 C22 38.3(5) . . ? C19 Ru4 C20 38.7(7) . . ? C18 Ru4 C20 67.7(7) . . ? C21 Ru4 C20 37.6(5) . . ? C22 Ru4 C20 68.5(6) . . ? C19 Ru4 C17 67.6(6) . . ? C18 Ru4 C17 38.0(6) . . ? C21 Ru4 C17 67.7(6) . . ? C22 Ru4 C17 37.1(5) . . ? C20 Ru4 C17 80.3(6) . . ? C19 Ru4 Br7 151.5(6) . . ? C18 Ru4 Br7 163.6(5) . . ? C21 Ru4 Br7 92.0(4) . . ? C22 Ru4 Br7 96.9(4) . . ? C20 Ru4 Br7 114.0(5) . . ? C17 Ru4 Br7 125.6(4) . . ? C19 Ru4 Br8 91.9(4) . . ? C18 Ru4 Br8 115.3(4) . . ? C21 Ru4 Br8 123.1(4) . . ? C22 Ru4 Br8 161.4(4) . . ? C20 Ru4 Br8 95.2(4) . . ? C17 Ru4 Br8 152.6(4) . . ? Br7 Ru4 Br8 81.08(4) . . ? C19 Ru4 Br9 125.4(5) . . ? C18 Ru4 Br9 99.7(5) . . ? C21 Ru4 Br9 153.9(4) . . ? C22 Ru4 Br9 117.3(4) . . ? C20 Ru4 Br9 163.9(5) . . ? C17 Ru4 Br9 96.0(4) . . ? Br7 Ru4 Br9 80.95(5) . . ? Br8 Ru4 Br9 80.85(5) . . ? Re2 Br5 Re1 81.77(4) . . ? Re1 Br6 Re2 81.38(4) . . ? Ru3 Br7 Ru4 83.62(4) . . ? Ru4 Br8 Ru3 82.55(4) . . ? Ru4 Br9 Ru3 82.51(4) . . ? Re1 Br10 Re2 83.00(4) . . ? O1 C1 Re1 177.3(16) . . ? O2 C2 Re1 179.3(13) . . ? O3 C3 Re1 176.8(12) . . ? O4 C4 Re2 177.9(11) . . ? O5 C5 Re2 178.8(11) . . ? O6 C6 Re2 178.6(12) . . ? C8 C7 C12 117.1(10) . . ? C8 C7 C13 123.7(11) . . ? C12 C7 C13 119.2(10) . . ? C8 C7 Ru3 69.8(6) . . ? C12 C7 Ru3 69.6(6) . . ? C13 C7 Ru3 129.6(8) . . ? C7 C8 C9 120.4(11) . . ? C7 C8 Ru3 72.4(6) . . ? C9 C8 Ru3 70.2(7) . . ? C10 C9 C8 122.5(10) . . ? C10 C9 Ru3 73.3(7) . . ? C8 C9 Ru3 71.1(6) . . ? C9 C10 C11 116.5(11) . . ? C9 C10 C16 121.6(12) . . ? C11 C10 C16 121.7(12) . . ? C9 C10 Ru3 69.3(6) . . ? C11 C10 Ru3 69.7(6) . . ? C16 C10 Ru3 128.1(8) . . ? C12 C11 C10 121.9(11) . . ? C12 C11 Ru3 71.2(7) . . ? C10 C11 Ru3 72.0(6) . . ? C11 C12 C7 121.6(10) . . ? C11 C12 Ru3 71.7(6) . . ? C7 C12 Ru3 72.0(6) . . ? C7 C13 C14 110.4(11) . . ? C7 C13 C15 112.7(11) . . ? C14 C13 C15 111.2(12) . . ? C22 C17 C18 119.1(14) . . ? C22 C17 C23 123.1(16) . . ? C18 C17 C23 117.8(17) . . ? C22 C17 Ru4 70.6(7) . . ? C18 C17 Ru4 69.2(8) . . ? C23 C17 Ru4 132.5(11) . . ? C19 C18 C17 121.7(16) . . ? C19 C18 Ru4 71.2(9) . . ? C17 C18 Ru4 72.8(8) . . ? C18 C19 C20 121.1(15) . . ? C18 C19 Ru4 72.3(9) . . ? C20 C19 Ru4 72.8(8) . . ? C21 C20 C19 117.1(15) . . ? C21 C20 C26 118.2(19) . . ? C19 C20 C26 124.0(18) . . ? C21 C20 Ru4 69.4(8) . . ? C19 C20 Ru4 68.5(8) . . ? C26 C20 Ru4 124.8(11) . . ? C20 C21 C22 121.8(14) . . ? C20 C21 Ru4 73.0(7) . . ? C22 C21 Ru4 71.9(7) . . ? C17 C22 C21 119.1(13) . . ? C17 C22 Ru4 72.3(7) . . ? C21 C22 Ru4 69.8(7) . . ? C25 C23 C17 115.9(23) . . ? C25 C23 C24 112.7(19) . . ? C17 C23 C24 106.7(16) . . ? 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 C4 Re2 Br5 Re1 -138.8(4) . . . . ? C6 Re2 Br5 Re1 131.4(4) . . . . ? C5 Re2 Br5 Re1 -1.0(26) . . . . ? Br10 Re2 Br5 Re1 39.98(4) . . . . ? Br6 Re2 Br5 Re1 -42.84(4) . . . . ? C1 Re1 Br5 Re2 134.5(5) . . . . ? C3 Re1 Br5 Re2 -133.8(4) . . . . ? C2 Re1 Br5 Re2 -33.5(33) . . . . ? Br10 Re1 Br5 Re2 -40.10(4) . . . . ? Br6 Re1 Br5 Re2 42.90(4) . . . . ? C1 Re1 Br6 Re2 -139.2(4) . . . . ? C3 Re1 Br6 Re2 -16.2(33) . . . . ? C2 Re1 Br6 Re2 131.0(4) . . . . ? Br10 Re1 Br6 Re2 40.67(4) . . . . ? Br5 Re1 Br6 Re2 -42.62(4) . . . . ? C4 Re2 Br6 Re1 135.8(4) . . . . ? C6 Re2 Br6 Re1 -17.0(32) . . . . ? C5 Re2 Br6 Re1 -132.3(3) . . . . ? Br10 Re2 Br6 Re1 -40.57(4) . . . . ? Br5 Re2 Br6 Re1 42.81(4) . . . . ? C9 Ru3 Br7 Ru4 -166.6(3) . . . . ? C8 Ru3 Br7 Ru4 154.9(3) . . . . ? C12 Ru3 Br7 Ru4 131.0(11) . . . . ? C11 Ru3 Br7 Ru4 -121.9(7) . . . . ? C7 Ru3 Br7 Ru4 127.8(3) . . . . ? C10 Ru3 Br7 Ru4 -134.9(4) . . . . ? Br9 Ru3 Br7 Ru4 -41.03(4) . . . . ? Br8 Ru3 Br7 Ru4 40.86(4) . . . . ? C19 Ru4 Br7 Ru3 -118.4(8) . . . . ? C18 Ru4 Br7 Ru3 134.6(19) . . . . ? C21 Ru4 Br7 Ru3 -164.2(4) . . . . ? C22 Ru4 Br7 Ru3 157.7(4) . . . . ? C20 Ru4 Br7 Ru3 -132.8(5) . . . . ? C17 Ru4 Br7 Ru3 132.0(5) . . . . ? Br8 Ru4 Br7 Ru3 -41.00(4) . . . . ? Br9 Ru4 Br7 Ru3 41.07(4) . . . . ? C19 Ru4 Br8 Ru3 -167.3(6) . . . . ? C18 Ru4 Br8 Ru3 -138.2(6) . . . . ? C21 Ru4 Br8 Ru3 127.0(4) . . . . ? C22 Ru4 Br8 Ru3 125.7(11) . . . . ? C20 Ru4 Br8 Ru3 154.0(5) . . . . ? C17 Ru4 Br8 Ru3 -127.1(8) . . . . ? Br7 Ru4 Br8 Ru3 40.45(4) . . . . ? Br9 Ru4 Br8 Ru3 -41.73(4) . . . . ? C9 Ru3 Br8 Ru4 -118.2(6) . . . . ? C8 Ru3 Br8 Ru4 -134.2(3) . . . . ? C12 Ru3 Br8 Ru4 155.8(3) . . . . ? C11 Ru3 Br8 Ru4 129.0(4) . . . . ? C7 Ru3 Br8 Ru4 -166.0(3) . . . . ? C10 Ru3 Br8 Ru4 124.5(12) . . . . ? Br7 Ru3 Br8 Ru4 -40.59(4) . . . . ? Br9 Ru3 Br8 Ru4 41.73(4) . . . . ? C19 Ru4 Br9 Ru3 127.6(6) . . . . ? C18 Ru4 Br9 Ru3 156.1(5) . . . . ? C21 Ru4 Br9 Ru3 -116.4(8) . . . . ? C22 Ru4 Br9 Ru3 -133.7(4) . . . . ? C20 Ru4 Br9 Ru3 118.7(16) . . . . ? C17 Ru4 Br9 Ru3 -165.7(4) . . . . ? Br7 Ru4 Br9 Ru3 -40.56(4) . . . . ? Br8 Ru4 Br9 Ru3 41.77(4) . . . . ? C9 Ru3 Br9 Ru4 126.9(4) . . . . ? C8 Ru3 Br9 Ru4 124.6(11) . . . . ? C12 Ru3 Br9 Ru4 -136.9(3) . . . . ? C11 Ru3 Br9 Ru4 -168.2(3) . . . . ? C7 Ru3 Br9 Ru4 -119.9(6) . . . . ? C10 Ru3 Br9 Ru4 153.4(3) . . . . ? Br7 Ru3 Br9 Ru4 40.69(4) . . . . ? Br8 Ru3 Br9 Ru4 -41.66(4) . . . . ? C1 Re1 Br10 Re2 -39.4(44) . . . . ? C3 Re1 Br10 Re2 132.5(4) . . . . ? C2 Re1 Br10 Re2 -138.8(4) . . . . ? Br5 Re1 Br10 Re2 40.41(4) . . . . ? Br6 Re1 Br10 Re2 -41.24(4) . . . . ? C4 Re2 Br10 Re1 -23.0(64) . . . . ? C6 Re2 Br10 Re1 -136.1(4) . . . . ? C5 Re2 Br10 Re1 134.6(3) . . . . ? Br5 Re2 Br10 Re1 -40.59(4) . . . . ? Br6 Re2 Br10 Re1 41.22(4) . . . . ? C3 Re1 C1 O1 168.2(271) . . . . ? C2 Re1 C1 O1 79.6(271) . . . . ? Br10 Re1 C1 O1 -19.9(309) . . . . ? Br5 Re1 C1 O1 -99.0(271) . . . . ? Br6 Re1 C1 O1 -18.1(271) . . . . ? C1 Re1 C2 O2 -146.7(932) . . . . ? C3 Re1 C2 O2 121.8(932) . . . . ? Br10 Re1 C2 O2 27.9(932) . . . . ? Br5 Re1 C2 O2 21.4(961) . . . . ? Br6 Re1 C2 O2 -54.1(933) . . . . ? C1 Re1 C3 O3 144.5(233) . . . . ? C2 Re1 C3 O3 -126.1(233) . . . . ? Br10 Re1 C3 O3 -34.8(233) . . . . ? Br5 Re1 C3 O3 47.5(233) . . . . ? Br6 Re1 C3 O3 21.4(260) . . . . ? C6 Re2 C4 O4 -51.7(380) . . . . ? C5 Re2 C4 O4 37.5(380) . . . . ? Br10 Re2 C4 O4 -164.9(326) . . . . ? Br5 Re2 C4 O4 -147.4(380) . . . . ? Br6 Re2 C4 O4 131.3(380) . . . . ? C4 Re2 C5 O5 -49.2(495) . . . . ? C6 Re2 C5 O5 40.1(495) . . . . ? Br10 Re2 C5 O5 132.3(495) . . . . ? Br5 Re2 C5 O5 172.8(473) . . . . ? Br6 Re2 C5 O5 -145.9(495) . . . . ? C4 Re2 C6 O6 170.7(1000) . . . . ? C5 Re2 C6 O6 79.3(472) . . . . ? Br10 Re2 C6 O6 -12.9(472) . . . . ? Br5 Re2 C6 O6 -95.3(472) . . . . ? Br6 Re2 C6 O6 -36.2(495) . . . . ? C9 Ru3 C7 C8 -29.5(7) . . . . ? C8 Ru3 C7 C8 0.000(2) . . . . ? C12 Ru3 C7 C8 -130.9(10) . . . . ? C11 Ru3 C7 C8 -102.9(7) . . . . ? C10 Ru3 C7 C8 -65.7(7) . . . . ? Br7 Ru3 C7 C8 47.6(7) . . . . ? Br9 Ru3 C7 C8 -156.2(6) . . . . ? Br8 Ru3 C7 C8 128.6(6) . . . . ? C9 Ru3 C7 C12 101.5(7) . . . . ? C8 Ru3 C7 C12 130.9(10) . . . . ? C12 Ru3 C7 C12 0.0 . . . . ? C11 Ru3 C7 C12 28.1(6) . . . . ? C10 Ru3 C7 C12 65.3(7) . . . . ? Br7 Ru3 C7 C12 178.6(5) . . . . ? Br9 Ru3 C7 C12 -25.2(10) . . . . ? Br8 Ru3 C7 C12 -100.5(6) . . . . ? C9 Ru3 C7 C13 -147.0(12) . . . . ? C8 Ru3 C7 C13 -117.5(13) . . . . ? C12 Ru3 C7 C13 111.5(12) . . . . ? C11 Ru3 C7 C13 139.6(11) . . . . ? C10 Ru3 C7 C13 176.8(11) . . . . ? Br7 Ru3 C7 C13 -69.9(11) . . . . ? Br9 Ru3 C7 C13 86.3(12) . . . . ? Br8 Ru3 C7 C13 11.0(10) . . . . ? C12 C7 C8 C9 0.6(15) . . . . ? C13 C7 C8 C9 178.2(10) . . . . ? Ru3 C7 C8 C9 53.3(9) . . . . ? C12 C7 C8 Ru3 -52.7(8) . . . . ? C13 C7 C8 Ru3 124.9(11) . . . . ? Ru3 C7 C8 Ru3 0.000(1) . . . . ? C9 Ru3 C8 C7 132.7(10) . . . . ? C12 Ru3 C8 C7 30.4(6) . . . . ? C11 Ru3 C8 C7 66.8(7) . . . . ? C7 Ru3 C8 C7 0.000(2) . . . . ? C10 Ru3 C8 C7 104.8(7) . . . . ? Br7 Ru3 C8 C7 -142.6(6) . . . . ? Br9 Ru3 C8 C7 135.6(9) . . . . ? Br8 Ru3 C8 C7 -59.3(7) . . . . ? C9 Ru3 C8 C9 0.000(3) . . . . ? C12 Ru3 C8 C9 -102.3(7) . . . . ? C11 Ru3 C8 C9 -65.9(7) . . . . ? C7 Ru3 C8 C9 -132.7(10) . . . . ? C10 Ru3 C8 C9 -27.9(6) . . . . ? Br7 Ru3 C8 C9 84.7(6) . . . . ? Br9 Ru3 C8 C9 2.9(15) . . . . ? Br8 Ru3 C8 C9 168.0(5) . . . . ? C7 C8 C9 C10 0.4(16) . . . . ? Ru3 C8 C9 C10 54.7(9) . . . . ? C7 C8 C9 Ru3 -54.3(9) . . . . ? Ru3 C8 C9 Ru3 0.000(1) . . . . ? C8 Ru3 C9 C10 -134.0(10) . . . . ? C12 Ru3 C9 C10 -67.0(7) . . . . ? C11 Ru3 C9 C10 -30.7(6) . . . . ? C7 Ru3 C9 C10 -105.2(7) . . . . ? C10 Ru3 C9 C10 0.0 . . . . ? Br7 Ru3 C9 C10 127.5(6) . . . . ? Br9 Ru3 C9 C10 47.0(7) . . . . ? Br8 Ru3 C9 C10 -157.6(5) . . . . ? C8 Ru3 C9 C8 0.000(2) . . . . ? C12 Ru3 C9 C8 67.0(7) . . . . ? C11 Ru3 C9 C8 103.3(7) . . . . ? C7 Ru3 C9 C8 28.8(6) . . . . ? C10 Ru3 C9 C8 134.0(10) . . . . ? Br7 Ru3 C9 C8 -98.5(6) . . . . ? Br9 Ru3 C9 C8 -179.0(5) . . . . ? Br8 Ru3 C9 C8 -23.5(10) . . . . ? C8 C9 C10 C11 -0.9(15) . . . . ? Ru3 C9 C10 C11 52.9(9) . . . . ? C8 C9 C10 C16 -176.6(11) . . . . ? Ru3 C9 C10 C16 -122.9(10) . . . . ? C8 C9 C10 Ru3 -53.8(9) . . . . ? Ru3 C9 C10 Ru3 0.0 . . . . ? C9 Ru3 C10 C9 0.0 . . . . ? C8 Ru3 C10 C9 28.8(7) . . . . ? C12 Ru3 C10 C9 102.8(7) . . . . ? C11 Ru3 C10 C9 130.5(10) . . . . ? C7 Ru3 C10 C9 65.4(7) . . . . ? Br7 Ru3 C10 C9 -59.8(7) . . . . ? Br9 Ru3 C10 C9 -143.1(6) . . . . ? Br8 Ru3 C10 C9 136.3(11) . . . . ? C9 Ru3 C10 C11 -130.5(10) . . . . ? C8 Ru3 C10 C11 -101.7(7) . . . . ? C12 Ru3 C10 C11 -27.7(7) . . . . ? C11 Ru3 C10 C11 0.000(2) . . . . ? C7 Ru3 C10 C11 -65.0(7) . . . . ? Br7 Ru3 C10 C11 169.7(6) . . . . ? Br9 Ru3 C10 C11 86.4(7) . . . . ? Br8 Ru3 C10 C11 5.8(17) . . . . ? C9 Ru3 C10 C16 114.6(14) . . . . ? C8 Ru3 C10 C16 143.3(13) . . . . ? C12 Ru3 C10 C16 -142.6(13) . . . . ? C11 Ru3 C10 C16 -115.0(15) . . . . ? C7 Ru3 C10 C16 180.0(13) . . . . ? Br7 Ru3 C10 C16 54.8(13) . . . . ? Br9 Ru3 C10 C16 -28.6(12) . . . . ? Br8 Ru3 C10 C16 -109.2(14) . . . . ? C9 C10 C11 C12 0.3(16) . . . . ? C16 C10 C11 C12 176.1(11) . . . . ? Ru3 C10 C11 C12 53.0(10) . . . . ? C9 C10 C11 Ru3 -52.7(8) . . . . ? C16 C10 C11 Ru3 123.0(10) . . . . ? Ru3 C10 C11 Ru3 0.000(1) . . . . ? C9 Ru3 C11 C12 -104.3(8) . . . . ? C8 Ru3 C11 C12 -66.3(7) . . . . ? C12 Ru3 C11 C12 0.000(2) . . . . ? C7 Ru3 C11 C12 -29.0(7) . . . . ? C10 Ru3 C11 C12 -134.2(11) . . . . ? Br7 Ru3 C11 C12 -153.8(6) . . . . ? Br9 Ru3 C11 C12 128.6(7) . . . . ? Br8 Ru3 C11 C12 47.7(8) . . . . ? C9 Ru3 C11 C10 29.9(7) . . . . ? C8 Ru3 C11 C10 68.0(7) . . . . ? C12 Ru3 C11 C10 134.2(11) . . . . ? C7 Ru3 C11 C10 105.2(8) . . . . ? C10 Ru3 C11 C10 0.000(2) . . . . ? Br7 Ru3 C11 C10 -19.5(11) . . . . ? Br9 Ru3 C11 C10 -97.2(7) . . . . ? Br8 Ru3 C11 C10 -178.1(6) . . . . ? C10 C11 C12 C7 0.7(17) . . . . ? Ru3 C11 C12 C7 54.1(9) . . . . ? C10 C11 C12 Ru3 -53.4(10) . . . . ? Ru3 C11 C12 Ru3 0.000(1) . . . . ? C8 C7 C12 C11 -1.2(16) . . . . ? C13 C7 C12 C11 -178.8(11) . . . . ? Ru3 C7 C12 C11 -54.0(10) . . . . ? C8 C7 C12 Ru3 52.8(8) . . . . ? C13 C7 C12 Ru3 -124.8(10) . . . . ? Ru3 C7 C12 Ru3 0.0 . . . . ? C9 Ru3 C12 C11 65.4(8) . . . . ? C8 Ru3 C12 C11 103.6(8) . . . . ? C11 Ru3 C12 C11 0.000(2) . . . . ? C7 Ru3 C12 C11 133.4(10) . . . . ? C10 Ru3 C12 C11 28.5(7) . . . . ? Br7 Ru3 C12 C11 129.3(10) . . . . ? Br9 Ru3 C12 C11 -59.4(7) . . . . ? Br8 Ru3 C12 C11 -143.1(7) . . . . ? C9 Ru3 C12 C7 -68.1(7) . . . . ? C8 Ru3 C12 C7 -29.8(6) . . . . ? C11 Ru3 C12 C7 -133.4(10) . . . . ? C7 Ru3 C12 C7 0.0 . . . . ? C10 Ru3 C12 C7 -104.9(7) . . . . ? Br7 Ru3 C12 C7 -4.2(15) . . . . ? Br9 Ru3 C12 C7 167.1(5) . . . . ? Br8 Ru3 C12 C7 83.4(6) . . . . ? C8 C7 C13 C14 107.5(13) . . . . ? C12 C7 C13 C14 -75.0(13) . . . . ? Ru3 C7 C13 C14 -161.7(9) . . . . ? C8 C7 C13 C15 -17.5(17) . . . . ? C12 C7 C13 C15 160.0(12) . . . . ? Ru3 C7 C13 C15 73.3(14) . . . . ? C19 Ru4 C17 C22 -105.3(10) . . . . ? C18 Ru4 C17 C22 -133.3(14) . . . . ? C21 Ru4 C17 C22 -30.1(8) . . . . ? C22 Ru4 C17 C22 0.0 . . . . ? C20 Ru4 C17 C22 -67.1(9) . . . . ? Br7 Ru4 C17 C22 45.6(10) . . . . ? Br8 Ru4 C17 C22 -149.6(8) . . . . ? Br9 Ru4 C17 C22 128.7(8) . . . . ? C19 Ru4 C17 C18 27.9(10) . . . . ? C18 Ru4 C17 C18 0.0 . . . . ? C21 Ru4 C17 C18 103.1(11) . . . . ? C22 Ru4 C17 C18 133.3(14) . . . . ? C20 Ru4 C17 C18 66.1(11) . . . . ? Br7 Ru4 C17 C18 178.8(9) . . . . ? Br8 Ru4 C17 C18 -16.4(15) . . . . ? Br9 Ru4 C17 C18 -98.0(10) . . . . ? C19 Ru4 C17 C23 137.1(20) . . . . ? C18 Ru4 C17 C23 109.2(22) . . . . ? C21 Ru4 C17 C23 -147.7(20) . . . . ? C22 Ru4 C17 C23 -117.6(22) . . . . ? C20 Ru4 C17 C23 175.3(19) . . . . ? Br7 Ru4 C17 C23 -72.0(19) . . . . ? Br8 Ru4 C17 C23 92.8(20) . . . . ? Br9 Ru4 C17 C23 11.1(18) . . . . ? C22 C17 C18 C19 -2.2(20) . . . . ? C23 C17 C18 C19 178.0(14) . . . . ? Ru4 C17 C18 C19 -54.0(12) . . . . ? C22 C17 C18 Ru4 51.8(11) . . . . ? C23 C17 C18 Ru4 -128.0(13) . . . . ? Ru4 C17 C18 Ru4 0.000(1) . . . . ? C19 Ru4 C18 C19 0.000(1) . . . . ? C21 Ru4 C18 C19 67.3(10) . . . . ? C22 Ru4 C18 C19 105.1(11) . . . . ? C20 Ru4 C18 C19 30.3(10) . . . . ? C17 Ru4 C18 C19 133.4(15) . . . . ? Br7 Ru4 C18 C19 130.0(17) . . . . ? Br8 Ru4 C18 C19 -54.9(11) . . . . ? Br9 Ru4 C18 C19 -139.3(9) . . . . ? C19 Ru4 C18 C17 -133.4(15) . . . . ? C21 Ru4 C18 C17 -66.1(10) . . . . ? C22 Ru4 C18 C17 -28.3(9) . . . . ? C20 Ru4 C18 C17 -103.1(10) . . . . ? C17 Ru4 C18 C17 0.000(1) . . . . ? Br7 Ru4 C18 C17 -3.4(26) . . . . ? Br8 Ru4 C18 C17 171.7(8) . . . . ? Br9 Ru4 C18 C17 87.4(9) . . . . ? C17 C18 C19 C20 -1.5(22) . . . . ? Ru4 C18 C19 C20 -56.3(12) . . . . ? C17 C18 C19 Ru4 54.8(12) . . . . ? Ru4 C18 C19 Ru4 0.000(1) . . . . ? C18 Ru4 C19 C18 0.000(1) . . . . ? C21 Ru4 C19 C18 -102.7(10) . . . . ? C22 Ru4 C19 C18 -65.0(10) . . . . ? C20 Ru4 C19 C18 -131.8(14) . . . . ? C17 Ru4 C19 C18 -29.0(9) . . . . ? Br7 Ru4 C19 C18 -153.0(8) . . . . ? Br8 Ru4 C19 C18 132.3(9) . . . . ? Br9 Ru4 C19 C18 52.1(11) . . . . ? C18 Ru4 C19 C20 131.8(14) . . . . ? C21 Ru4 C19 C20 29.1(9) . . . . ? C22 Ru4 C19 C20 66.7(9) . . . . ? C20 Ru4 C19 C20 0.0 . . . . ? C17 Ru4 C19 C20 102.8(10) . . . . ? Br7 Ru4 C19 C20 -21.2(15) . . . . ? Br8 Ru4 C19 C20 -95.9(9) . . . . ? Br9 Ru4 C19 C20 -176.1(7) . . . . ? C18 C19 C20 C21 4.7(20) . . . . ? Ru4 C19 C20 C21 -51.3(11) . . . . ? C18 C19 C20 C26 174.4(15) . . . . ? Ru4 C19 C20 C26 118.4(15) . . . . ? C18 C19 C20 Ru4 56.0(12) . . . . ? Ru4 C19 C20 Ru4 0.0 . . . . ? C19 Ru4 C20 C21 132.1(14) . . . . ? C18 Ru4 C20 C21 103.4(10) . . . . ? C21 Ru4 C20 C21 0.000(1) . . . . ? C22 Ru4 C20 C21 29.3(9) . . . . ? C17 Ru4 C20 C21 65.9(10) . . . . ? Br7 Ru4 C20 C21 -58.8(10) . . . . ? Br8 Ru4 C20 C21 -141.4(9) . . . . ? Br9 Ru4 C20 C21 143.6(13) . . . . ? C19 Ru4 C20 C19 0.0 . . . . ? C18 Ru4 C20 C19 -28.7(9) . . . . ? C21 Ru4 C20 C19 -132.1(14) . . . . ? C22 Ru4 C20 C19 -102.8(10) . . . . ? C17 Ru4 C20 C19 -66.1(10) . . . . ? Br7 Ru4 C20 C19 169.1(8) . . . . ? Br8 Ru4 C20 C19 86.6(9) . . . . ? Br9 Ru4 C20 C19 11.6(22) . . . . ? C19 Ru4 C20 C26 -117.2(22) . . . . ? C18 Ru4 C20 C26 -145.9(20) . . . . ? C21 Ru4 C20 C26 110.7(22) . . . . ? C22 Ru4 C20 C26 140.0(20) . . . . ? C17 Ru4 C20 C26 176.6(19) . . . . ? Br7 Ru4 C20 C26 51.9(19) . . . . ? Br8 Ru4 C20 C26 -30.7(18) . . . . ? Br9 Ru4 C20 C26 -105.6(23) . . . . ? C19 C20 C21 C22 -4.3(19) . . . . ? C26 C20 C21 C22 -174.6(13) . . . . ? Ru4 C20 C21 C22 -55.2(11) . . . . ? C19 C20 C21 Ru4 50.9(11) . . . . ? C26 C20 C21 Ru4 -119.4(13) . . . . ? Ru4 C20 C21 Ru4 0.000(1) . . . . ? C19 Ru4 C21 C20 -29.9(10) . . . . ? C18 Ru4 C21 C20 -66.0(11) . . . . ? C22 Ru4 C21 C20 -132.7(13) . . . . ? C20 Ru4 C21 C20 0.000(1) . . . . ? C17 Ru4 C21 C20 -103.5(11) . . . . ? Br7 Ru4 C21 C20 128.6(10) . . . . ? Br8 Ru4 C21 C20 47.9(11) . . . . ? Br9 Ru4 C21 C20 -158.1(9) . . . . ? C19 Ru4 C21 C22 102.8(10) . . . . ? C18 Ru4 C21 C22 66.7(9) . . . . ? C22 Ru4 C21 C22 0.0 . . . . ? C20 Ru4 C21 C22 132.7(13) . . . . ? C17 Ru4 C21 C22 29.3(8) . . . . ? Br7 Ru4 C21 C22 -98.7(8) . . . . ? Br8 Ru4 C21 C22 -179.3(6) . . . . ? Br9 Ru4 C21 C22 -25.4(13) . . . . ? C18 C17 C22 C21 2.6(18) . . . . ? C23 C17 C22 C21 -177.6(13) . . . . ? Ru4 C17 C22 C21 53.7(10) . . . . ? C18 C17 C22 Ru4 -51.1(11) . . . . ? C23 C17 C22 Ru4 128.7(14) . . . . ? Ru4 C17 C22 Ru4 0.0 . . . . ? C20 C21 C22 C17 0.8(18) . . . . ? Ru4 C21 C22 C17 -54.9(10) . . . . ? C20 C21 C22 Ru4 55.7(11) . . . . ? Ru4 C21 C22 Ru4 0.0 . . . . ? C19 Ru4 C22 C17 64.5(10) . . . . ? C18 Ru4 C22 C17 28.9(10) . . . . ? C21 Ru4 C22 C17 131.4(13) . . . . ? C20 Ru4 C22 C17 102.6(10) . . . . ? C17 Ru4 C22 C17 0.0 . . . . ? Br7 Ru4 C22 C17 -144.2(8) . . . . ? Br8 Ru4 C22 C17 133.2(11) . . . . ? Br9 Ru4 C22 C17 -60.8(9) . . . . ? C19 Ru4 C22 C21 -66.9(9) . . . . ? C18 Ru4 C22 C21 -102.5(10) . . . . ? C21 Ru4 C22 C21 0.0 . . . . ? C20 Ru4 C22 C21 -28.8(9) . . . . ? C17 Ru4 C22 C21 -131.4(13) . . . . ? Br7 Ru4 C22 C21 84.4(8) . . . . ? Br8 Ru4 C22 C21 1.8(17) . . . . ? Br9 Ru4 C22 C21 167.7(7) . . . . ? C22 C17 C23 C25 -19.7(26) . . . . ? C18 C17 C23 C25 160.1(20) . . . . ? Ru4 C17 C23 C25 73.6(26) . . . . ? C22 C17 C23 C24 106.7(20) . . . . ? C18 C17 C23 C24 -73.5(20) . . . . ? Ru4 C17 C23 C24 -159.9(14) . . . . ? _refine_diff_density_max 1.767 _refine_diff_density_min -1.586 _refine_diff_density_rms 0.191 data_e093 _publ_contact_author_name 'Dr. Kay Severin' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7768' _publ_author_name 'da Silva, Ana C.' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Heterometallic bromo-bridged complexes with Re(CO)3 fragments ; _audit_author_name 'Piotrowski, H.' _audit_block_code Re_Ru_Br_CO_C12H18_e093_Beck _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 15-Apr-00 _chemical_name_systematic ; ; _chemical_compound_source ; ; _chemical_name_common (CO)3Re(BR3)Ru(C12H18) _chemical_formula_moiety '3(C O), Re, Br3, Ru, C12 H18' _chemical_formula_sum 'C15 H18 Br3 O3 Re Ru' _chemical_formula_weight 773.29 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' 'O' 'O' 0.0106 0.0060 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9917(9) _cell_length_b 10.5637(11) _cell_length_c 10.9076(11) _cell_angle_alpha 111.142(11) _cell_angle_beta 91.800(12) _cell_angle_gamma 96.043(12) _cell_volume 958.26(17) _cell_formula_units_Z 2 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.9 _cell_special_details 'Triclinic P (as derived from metrics)' _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.6801(5) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 13.362 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1027 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' _exptl_special_details ; crystal embedded in oil and fixed with Lithelen ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0560 -1 0 0 0.0960 -2 1 -2 0.1890 0 1 0 0.0120 0 -1 0 0.0080 0 0 1 0.2000 0 0 -1 0.2600 -2 -2 3 0.1660 _diffrn_ambient_temperature 200(3) _diffrn_source_type 'Spellman DF4 Series' _diffrn_source_power 2.75_kW _diffrn_source_voltage 55_kV _diffrn_source_current 50_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 185.0 _kl_diffrn_detector_area_phi_incr 1.2 _kl_diffrn_detector_area_expos_time 2.00_min _kl_diffrn_detector_area_plate_dist 60.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.010 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 27 _diffrn_special_details ; no crystal decay in terms of mean intensity per image ; _diffrn_reflns_number 8528 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.85 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.956 _refine_diff_density_min -1.626 _refine_diff_density_rms 0.252 _reflns_number_total 4211 _reflns_number_gt 3564 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution ; SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79) ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4211 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ; details of H atom refinement: C-bonded H: riding with U(H)=1.2*U(C) for CH2 and CH, 1.5*U(C) for CH3 ; 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 Re Re 0.84466(2) 0.20795(2) 0.29598(3) 0.01778(8) Uani 1 1 d . . . Ru Ru 0.62093(5) -0.09724(5) 0.21835(5) 0.01408(11) Uani 1 1 d . . . Br1 Br 0.55246(6) 0.14698(7) 0.28331(8) 0.02681(16) Uani 1 1 d . . . Br2 Br 0.80411(7) -0.01285(7) 0.08047(7) 0.02746(15) Uani 1 1 d . . . Br3 Br 0.82963(7) 0.02127(7) 0.40173(7) 0.02687(15) Uani 1 1 d . . . C1 C 0.8416(7) 0.3399(7) 0.2132(7) 0.0242(14) Uani 1 1 d . . . O1 O 0.8398(6) 0.4192(6) 0.1676(6) 0.0378(13) Uani 1 1 d . . . C2 C 1.0581(7) 0.2238(7) 0.2951(7) 0.0226(13) Uani 1 1 d . . . O2 O 1.1845(5) 0.2322(6) 0.2950(6) 0.0381(13) Uani 1 1 d . . . C3 C 0.8598(7) 0.3517(7) 0.4640(7) 0.0236(14) Uani 1 1 d . . . O3 O 0.8688(7) 0.4357(6) 0.5651(6) 0.0438(14) Uani 1 1 d . . . C11 C 0.5898(6) -0.2637(6) 0.2919(7) 0.0179(12) Uani 1 1 d . . . C111 C 0.6711(7) -0.2796(7) 0.4063(7) 0.0251(14) Uani 1 1 d . . . H11A H 0.6662 -0.1983 0.4871 0.030 Uiso 1 1 calc R . . H11B H 0.7779 -0.2877 0.3895 0.030 Uiso 1 1 calc R . . C211 C 0.5974(8) -0.4089(8) 0.4251(9) 0.0329(17) Uani 1 1 d . . . H21A H 0.4893 -0.4051 0.4310 0.049 Uiso 1 1 calc R . . H21B H 0.6412 -0.4140 0.5063 0.049 Uiso 1 1 calc R . . H21C H 0.6146 -0.4900 0.3498 0.049 Uiso 1 1 calc R . . C21 C 0.4589(6) -0.1965(6) 0.3096(7) 0.0197(13) Uani 1 1 d . . . H21 H 0.4211 -0.1637 0.3943 0.024 Uiso 1 1 calc R . . C31 C 0.3841(6) -0.1781(6) 0.2025(7) 0.0186(12) Uani 1 1 d . . . C131 C 0.2446(7) -0.1059(7) 0.2223(8) 0.0263(15) Uani 1 1 d . . . H13A H 0.2382 -0.0570 0.1605 0.032 Uiso 1 1 calc R . . H13B H 0.2490 -0.0381 0.3135 0.032 Uiso 1 1 calc R . . C231 C 0.1074(7) -0.2126(9) 0.1973(10) 0.042(2) Uani 1 1 d . . . H23A H 0.1104 -0.2854 0.1111 0.063 Uiso 1 1 calc R . . H23B H 0.0161 -0.1692 0.1985 0.063 Uiso 1 1 calc R . . H23C H 0.1076 -0.2517 0.2662 0.063 Uiso 1 1 calc R . . C41 C 0.4415(6) -0.2250(6) 0.0767(7) 0.0203(13) Uani 1 1 d . . . H41 H 0.3941 -0.2087 0.0057 0.024 Uiso 1 1 calc R . . C51 C 0.5705(6) -0.2968(6) 0.0556(7) 0.0196(13) Uani 1 1 d . . . C151 C 0.6239(8) -0.3488(8) -0.0805(7) 0.0279(15) Uani 1 1 d . . . H15A H 0.6329 -0.2727 -0.1136 0.033 Uiso 1 1 calc R . . H15B H 0.5461 -0.4206 -0.1386 0.033 Uiso 1 1 calc R . . C251 C 0.7704(9) -0.4067(9) -0.0932(8) 0.0385(19) Uani 1 1 d . . . H25A H 0.8498 -0.3359 -0.0390 0.058 Uiso 1 1 calc R . . H25B H 0.7944 -0.4379 -0.1856 0.058 Uiso 1 1 calc R . . H25C H 0.7628 -0.4840 -0.0633 0.058 Uiso 1 1 calc R . . C61 C 0.6425(6) -0.3139(6) 0.1643(7) 0.0191(13) Uani 1 1 d . . . H61 H 0.7289 -0.3604 0.1515 0.023 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 Re 0.01952(12) 0.01581(13) 0.01961(16) 0.00807(11) 0.00293(9) 0.00300(8) Ru 0.0167(2) 0.0141(2) 0.0143(3) 0.0078(2) 0.00283(17) 0.00422(16) Br1 0.0221(3) 0.0222(3) 0.0395(5) 0.0135(3) 0.0060(3) 0.0082(2) Br2 0.0346(3) 0.0256(3) 0.0231(4) 0.0101(3) 0.0083(3) 0.0019(3) Br3 0.0301(3) 0.0280(3) 0.0262(4) 0.0152(3) -0.0015(3) 0.0018(3) C1 0.022(3) 0.019(3) 0.025(4) 0.001(3) 0.002(2) 0.001(2) O1 0.043(3) 0.033(3) 0.047(4) 0.025(3) 0.005(2) 0.005(2) C2 0.028(3) 0.023(3) 0.021(4) 0.012(3) 0.002(2) 0.007(2) O2 0.026(2) 0.047(3) 0.048(4) 0.023(3) 0.004(2) 0.007(2) C3 0.031(3) 0.015(3) 0.024(4) 0.006(3) 0.002(3) 0.000(2) O3 0.058(3) 0.030(3) 0.033(4) 0.001(3) 0.011(3) -0.001(3) C11 0.021(3) 0.020(3) 0.021(4) 0.017(3) 0.002(2) 0.003(2) C111 0.030(3) 0.027(3) 0.023(4) 0.016(3) 0.000(3) 0.005(3) C211 0.041(4) 0.030(4) 0.039(5) 0.026(4) 0.006(3) 0.008(3) C21 0.022(3) 0.020(3) 0.019(4) 0.008(3) 0.005(2) 0.004(2) C31 0.018(2) 0.013(3) 0.024(4) 0.006(3) 0.003(2) -0.001(2) C131 0.022(3) 0.028(3) 0.034(4) 0.016(3) 0.006(3) 0.011(3) C231 0.018(3) 0.045(5) 0.059(6) 0.014(5) 0.004(3) 0.006(3) C41 0.020(3) 0.021(3) 0.019(4) 0.008(3) -0.001(2) -0.003(2) C51 0.025(3) 0.016(3) 0.019(4) 0.008(3) 0.006(2) 0.002(2) C151 0.037(3) 0.028(4) 0.015(4) 0.004(3) 0.004(3) 0.002(3) C251 0.050(4) 0.040(4) 0.032(5) 0.015(4) 0.017(4) 0.025(4) C61 0.025(3) 0.010(3) 0.024(4) 0.008(3) 0.004(2) 0.003(2) 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 Re C3 1.902(7) . ? Re C2 1.909(6) . ? Re C1 1.917(7) . ? Re Br3 2.6139(7) . ? Re Br1 2.6256(7) . ? Re Br2 2.6289(9) . ? Ru C41 2.166(6) . ? Ru C21 2.177(6) . ? Ru C11 2.178(5) . ? Ru C61 2.179(6) . ? Ru C31 2.187(5) . ? Ru C51 2.203(7) . ? Ru Br3 2.5598(10) . ? Ru Br1 2.5652(8) . ? Ru Br2 2.5657(8) . ? C1 O1 1.118(8) . ? C2 O2 1.131(7) . ? C3 O3 1.132(9) . ? C11 C61 1.416(9) . ? C11 C21 1.421(8) . ? C11 C111 1.496(9) . ? C111 C211 1.539(9) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C21 C31 1.413(9) . ? C21 H21 0.9500 . ? C31 C41 1.415(9) . ? C31 C131 1.517(8) . ? C131 C231 1.527(10) . ? C131 H13A 0.9900 . ? C131 H13B 0.9900 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C41 C51 1.432(8) . ? C41 H41 0.9500 . ? C51 C61 1.410(9) . ? C51 C151 1.499(9) . ? C151 C251 1.499(10) . ? C151 H15A 0.9900 . ? C151 H15B 0.9900 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C61 H61 0.9500 . ? 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 C3 Re C2 90.4(3) . . ? C3 Re C1 89.7(3) . . ? C2 Re C1 89.7(3) . . ? C3 Re Br3 92.00(19) . . ? C2 Re Br3 93.97(18) . . ? C1 Re Br3 175.99(19) . . ? C3 Re Br1 95.81(18) . . ? C2 Re Br1 171.5(2) . . ? C1 Re Br1 96.08(18) . . ? Br3 Re Br1 80.14(2) . . ? C3 Re Br2 171.74(18) . . ? C2 Re Br2 93.6(2) . . ? C1 Re Br2 97.5(2) . . ? Br3 Re Br2 80.53(2) . . ? Br1 Re Br2 79.51(3) . . ? C41 Ru C21 68.6(2) . . ? C41 Ru C11 81.7(2) . . ? C21 Ru C11 38.1(2) . . ? C41 Ru C61 68.3(2) . . ? C21 Ru C61 68.1(2) . . ? C11 Ru C61 37.9(2) . . ? C41 Ru C31 37.9(2) . . ? C21 Ru C31 37.8(2) . . ? C11 Ru C31 68.7(2) . . ? C61 Ru C31 80.5(2) . . ? C41 Ru C51 38.3(2) . . ? C21 Ru C51 81.0(2) . . ? C11 Ru C51 68.7(2) . . ? C61 Ru C51 37.5(2) . . ? C31 Ru C51 68.6(2) . . ? C41 Ru Br3 170.22(17) . . ? C21 Ru Br3 103.68(18) . . ? C11 Ru Br3 88.56(17) . . ? C61 Ru Br3 103.63(18) . . ? C31 Ru Br3 137.45(18) . . ? C51 Ru Br3 136.79(16) . . ? C41 Ru Br1 105.07(17) . . ? C21 Ru Br1 104.33(16) . . ? C11 Ru Br1 137.36(17) . . ? C61 Ru Br1 171.19(15) . . ? C31 Ru Br1 90.70(15) . . ? C51 Ru Br1 139.03(17) . . ? Br3 Ru Br1 82.30(3) . . ? C41 Ru Br2 104.41(16) . . ? C21 Ru Br2 171.51(18) . . ? C11 Ru Br2 138.28(15) . . ? C61 Ru Br2 105.21(15) . . ? C31 Ru Br2 137.86(18) . . ? C51 Ru Br2 90.51(14) . . ? Br3 Ru Br2 82.77(3) . . ? Br1 Ru Br2 81.82(3) . . ? Ru Br1 Re 82.50(2) . . ? Ru Br2 Re 82.43(3) . . ? Ru Br3 Re 82.84(2) . . ? O1 C1 Re 178.4(6) . . ? O2 C2 Re 179.3(6) . . ? O3 C3 Re 178.8(6) . . ? C61 C11 C21 118.6(6) . . ? C61 C11 C111 120.8(5) . . ? C21 C11 C111 120.6(6) . . ? C61 C11 Ru 71.1(3) . . ? C21 C11 Ru 70.9(3) . . ? C111 C11 Ru 129.1(5) . . ? C11 C111 C211 108.8(6) . . ? C11 C111 H11A 109.9 . . ? C211 C111 H11A 109.9 . . ? C11 C111 H11B 109.9 . . ? C211 C111 H11B 109.9 . . ? H11A C111 H11B 108.3 . . ? C111 C211 H21A 109.5 . . ? C111 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C111 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C31 C21 C11 120.7(6) . . ? C31 C21 Ru 71.5(3) . . ? C11 C21 Ru 71.0(3) . . ? C31 C21 H21 119.6 . . ? C11 C21 H21 119.6 . . ? Ru C21 H21 130.5 . . ? C21 C31 C41 119.7(5) . . ? C21 C31 C131 120.3(6) . . ? C41 C31 C131 119.9(6) . . ? C21 C31 Ru 70.7(3) . . ? C41 C31 Ru 70.2(3) . . ? C131 C31 Ru 130.7(4) . . ? C31 C131 C231 108.6(6) . . ? C31 C131 H13A 110.0 . . ? C231 C131 H13A 110.0 . . ? C31 C131 H13B 110.0 . . ? C231 C131 H13B 110.0 . . ? H13A C131 H13B 108.3 . . ? C131 C231 H23A 109.5 . . ? C131 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C131 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C31 C41 C51 120.6(6) . . ? C31 C41 Ru 71.8(4) . . ? C51 C41 Ru 72.3(4) . . ? C31 C41 H41 119.7 . . ? C51 C41 H41 119.7 . . ? Ru C41 H41 128.5 . . ? C61 C51 C41 118.3(6) . . ? C61 C51 C151 123.1(6) . . ? C41 C51 C151 118.6(6) . . ? C61 C51 Ru 70.3(4) . . ? C41 C51 Ru 69.5(4) . . ? C151 C51 Ru 131.3(4) . . ? C51 C151 C251 116.1(6) . . ? C51 C151 H15A 108.3 . . ? C251 C151 H15A 108.3 . . ? C51 C151 H15B 108.3 . . ? C251 C151 H15B 108.3 . . ? H15A C151 H15B 107.4 . . ? C151 C251 H25A 109.5 . . ? C151 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C151 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C51 C61 C11 122.0(5) . . ? C51 C61 Ru 72.1(4) . . ? C11 C61 Ru 71.0(3) . . ? C51 C61 H61 119.0 . . ? C11 C61 H61 119.0 . . ? Ru C61 H61 130.7 . . ? 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 C41 Ru Br1 Re -145.20(16) . . . . ? C21 Ru Br1 Re 143.58(18) . . . . ? C11 Ru Br1 Re 120.8(2) . . . . ? C61 Ru Br1 Re 174.2(12) . . . . ? C31 Ru Br1 Re 179.25(18) . . . . ? C51 Ru Br1 Re -123.7(2) . . . . ? Br3 Ru Br1 Re 41.36(2) . . . . ? Br2 Ru Br1 Re -42.39(2) . . . . ? C3 Re Br1 Ru -131.6(2) . . . . ? C2 Re Br1 Ru 5.7(14) . . . . ? C1 Re Br1 Ru 138.1(2) . . . . ? Br3 Re Br1 Ru -40.61(2) . . . . ? Br2 Re Br1 Ru 41.48(2) . . . . ? C41 Ru Br2 Re 145.88(17) . . . . ? C21 Ru Br2 Re 179.3(11) . . . . ? C11 Ru Br2 Re -120.5(3) . . . . ? C61 Ru Br2 Re -143.10(18) . . . . ? C31 Ru Br2 Re 124.3(2) . . . . ? C51 Ru Br2 Re -178.07(16) . . . . ? Br3 Ru Br2 Re -40.88(2) . . . . ? Br1 Ru Br2 Re 42.33(2) . . . . ? C3 Re Br2 Ru 14.6(14) . . . . ? C2 Re Br2 Ru 133.57(19) . . . . ? C1 Re Br2 Ru -136.30(18) . . . . ? Br3 Re Br2 Ru 40.14(2) . . . . ? Br1 Re Br2 Ru -41.48(2) . . . . ? C41 Ru Br3 Re 178.9(9) . . . . ? C21 Ru Br3 Re -144.50(16) . . . . ? C11 Ru Br3 Re -179.78(15) . . . . ? C61 Ru Br3 Re 145.09(16) . . . . ? C31 Ru Br3 Re -124.1(2) . . . . ? C51 Ru Br3 Re 124.1(2) . . . . ? Br1 Ru Br3 Re -41.55(2) . . . . ? Br2 Ru Br3 Re 41.12(2) . . . . ? C3 Re Br3 Ru 136.23(19) . . . . ? C2 Re Br3 Ru -133.2(2) . . . . ? C1 Re Br3 Ru 21(3) . . . . ? Br1 Re Br3 Ru 40.68(2) . . . . ? Br2 Re Br3 Ru -40.21(2) . . . . ? C3 Re C1 O1 -6(20) . . . . ? C2 Re C1 O1 -96(20) . . . . ? Br3 Re C1 O1 109(20) . . . . ? Br1 Re C1 O1 90(20) . . . . ? Br2 Re C1 O1 170(20) . . . . ? C3 Re C2 O2 95(71) . . . . ? C1 Re C2 O2 -176(100) . . . . ? Br3 Re C2 O2 3(71) . . . . ? Br1 Re C2 O2 -43(72) . . . . ? Br2 Re C2 O2 -78(71) . . . . ? C2 Re C3 O3 -91(28) . . . . ? C1 Re C3 O3 180(100) . . . . ? Br3 Re C3 O3 3(28) . . . . ? Br1 Re C3 O3 84(28) . . . . ? Br2 Re C3 O3 29(29) . . . . ? C41 Ru C11 C61 65.2(4) . . . . ? C21 Ru C11 C61 130.9(6) . . . . ? C31 Ru C11 C61 102.3(4) . . . . ? C51 Ru C11 C61 27.9(4) . . . . ? Br3 Ru C11 C61 -114.6(3) . . . . ? Br1 Ru C11 C61 168.4(3) . . . . ? Br2 Ru C11 C61 -37.1(5) . . . . ? C41 Ru C11 C21 -65.7(4) . . . . ? C61 Ru C11 C21 -130.9(6) . . . . ? C31 Ru C11 C21 -28.6(4) . . . . ? C51 Ru C11 C21 -103.0(4) . . . . ? Br3 Ru C11 C21 114.5(4) . . . . ? Br1 Ru C11 C21 37.5(5) . . . . ? Br2 Ru C11 C21 -168.0(3) . . . . ? C41 Ru C11 C111 -180.0(6) . . . . ? C21 Ru C11 C111 -114.3(7) . . . . ? C61 Ru C11 C111 114.8(7) . . . . ? C31 Ru C11 C111 -143.0(6) . . . . ? C51 Ru C11 C111 142.6(6) . . . . ? Br3 Ru C11 C111 0.2(5) . . . . ? Br1 Ru C11 C111 -76.8(6) . . . . ? Br2 Ru C11 C111 77.7(6) . . . . ? C61 C11 C111 C211 -95.3(7) . . . . ? C21 C11 C111 C211 85.4(7) . . . . ? Ru C11 C111 C211 174.8(4) . . . . ? C61 C11 C21 C31 -1.1(9) . . . . ? C111 C11 C21 C31 178.3(6) . . . . ? Ru C11 C21 C31 53.5(5) . . . . ? C61 C11 C21 Ru -54.5(5) . . . . ? C111 C11 C21 Ru 124.8(6) . . . . ? C41 Ru C21 C31 -28.8(4) . . . . ? C11 Ru C21 C31 -133.2(6) . . . . ? C61 Ru C21 C31 -103.2(4) . . . . ? C51 Ru C21 C31 -66.5(4) . . . . ? Br3 Ru C21 C31 157.4(3) . . . . ? Br1 Ru C21 C31 72.0(4) . . . . ? Br2 Ru C21 C31 -63.8(12) . . . . ? C41 Ru C21 C11 104.4(4) . . . . ? C61 Ru C21 C11 30.0(4) . . . . ? C31 Ru C21 C11 133.2(6) . . . . ? C51 Ru C21 C11 66.8(4) . . . . ? Br3 Ru C21 C11 -69.4(4) . . . . ? Br1 Ru C21 C11 -154.8(3) . . . . ? Br2 Ru C21 C11 69.4(12) . . . . ? C11 C21 C31 C41 -1.0(9) . . . . ? Ru C21 C31 C41 52.3(5) . . . . ? C11 C21 C31 C131 -179.8(5) . . . . ? Ru C21 C31 C131 -126.6(5) . . . . ? C11 C21 C31 Ru -53.3(5) . . . . ? C41 Ru C31 C21 133.1(5) . . . . ? C11 Ru C31 C21 28.8(4) . . . . ? C61 Ru C31 C21 66.4(4) . . . . ? C51 Ru C31 C21 103.4(4) . . . . ? Br3 Ru C31 C21 -33.5(5) . . . . ? Br1 Ru C31 C21 -112.8(3) . . . . ? Br2 Ru C31 C21 168.6(3) . . . . ? C21 Ru C31 C41 -133.1(5) . . . . ? C11 Ru C31 C41 -104.3(4) . . . . ? C61 Ru C31 C41 -66.7(4) . . . . ? C51 Ru C31 C41 -29.7(4) . . . . ? Br3 Ru C31 C41 -166.6(3) . . . . ? Br1 Ru C31 C41 114.0(3) . . . . ? Br2 Ru C31 C41 35.5(4) . . . . ? C41 Ru C31 C131 -113.0(8) . . . . ? C21 Ru C31 C131 113.9(8) . . . . ? C11 Ru C31 C131 142.7(7) . . . . ? C61 Ru C31 C131 -179.7(7) . . . . ? C51 Ru C31 C131 -142.7(7) . . . . ? Br3 Ru C31 C131 80.4(7) . . . . ? Br1 Ru C31 C131 1.0(6) . . . . ? Br2 Ru C31 C131 -77.5(7) . . . . ? C21 C31 C131 C231 -90.6(8) . . . . ? C41 C31 C131 C231 90.6(7) . . . . ? Ru C31 C131 C231 179.5(5) . . . . ? C21 C31 C41 C51 3.0(9) . . . . ? C131 C31 C41 C51 -178.2(5) . . . . ? Ru C31 C41 C51 55.5(5) . . . . ? C21 C31 C41 Ru -52.5(5) . . . . ? C131 C31 C41 Ru 126.3(5) . . . . ? C21 Ru C41 C31 28.7(3) . . . . ? C11 Ru C41 C31 65.9(4) . . . . ? C61 Ru C41 C31 102.8(4) . . . . ? C51 Ru C41 C31 131.8(5) . . . . ? Br3 Ru C41 C31 67.2(11) . . . . ? Br1 Ru C41 C31 -71.0(4) . . . . ? Br2 Ru C41 C31 -156.3(3) . . . . ? C21 Ru C41 C51 -103.1(4) . . . . ? C11 Ru C41 C51 -66.0(4) . . . . ? C61 Ru C41 C51 -29.0(3) . . . . ? C31 Ru C41 C51 -131.8(5) . . . . ? Br3 Ru C41 C51 -64.7(10) . . . . ? Br1 Ru C41 C51 157.1(3) . . . . ? Br2 Ru C41 C51 71.9(3) . . . . ? C31 C41 C51 C61 -2.9(9) . . . . ? Ru C41 C51 C61 52.4(5) . . . . ? C31 C41 C51 C151 177.9(6) . . . . ? Ru C41 C51 C151 -126.8(6) . . . . ? C31 C41 C51 Ru -55.3(5) . . . . ? C41 Ru C51 C61 -132.2(5) . . . . ? C21 Ru C51 C61 -65.6(3) . . . . ? C11 Ru C51 C61 -28.1(3) . . . . ? C31 Ru C51 C61 -102.7(4) . . . . ? Br3 Ru C51 C61 34.8(4) . . . . ? Br1 Ru C51 C61 -167.2(2) . . . . ? Br2 Ru C51 C61 114.8(3) . . . . ? C21 Ru C51 C41 66.6(4) . . . . ? C11 Ru C51 C41 104.1(4) . . . . ? C61 Ru C51 C41 132.2(5) . . . . ? C31 Ru C51 C41 29.5(3) . . . . ? Br3 Ru C51 C41 167.0(3) . . . . ? Br1 Ru C51 C41 -34.9(4) . . . . ? Br2 Ru C51 C41 -113.0(3) . . . . ? C41 Ru C51 C151 110.5(7) . . . . ? C21 Ru C51 C151 177.1(6) . . . . ? C11 Ru C51 C151 -145.4(7) . . . . ? C61 Ru C51 C151 -117.2(7) . . . . ? C31 Ru C51 C151 140.0(7) . . . . ? Br3 Ru C51 C151 -82.4(7) . . . . ? Br1 Ru C51 C151 75.6(6) . . . . ? Br2 Ru C51 C151 -2.5(6) . . . . ? C61 C51 C151 C251 -7.0(10) . . . . ? C41 C51 C151 C251 172.2(6) . . . . ? Ru C51 C151 C251 85.2(8) . . . . ? C41 C51 C61 C11 0.8(9) . . . . ? C151 C51 C61 C11 180.0(6) . . . . ? Ru C51 C61 C11 52.8(5) . . . . ? C41 C51 C61 Ru -52.0(5) . . . . ? C151 C51 C61 Ru 127.2(6) . . . . ? C21 C11 C61 C51 1.2(9) . . . . ? C111 C11 C61 C51 -178.1(6) . . . . ? Ru C11 C61 C51 -53.3(5) . . . . ? C21 C11 C61 Ru 54.5(5) . . . . ? C111 C11 C61 Ru -124.8(6) . . . . ? C41 Ru C61 C51 29.6(3) . . . . ? C21 Ru C61 C51 104.2(4) . . . . ? C11 Ru C61 C51 134.4(5) . . . . ? C31 Ru C61 C51 67.0(3) . . . . ? Br3 Ru C61 C51 -156.3(3) . . . . ? Br1 Ru C61 C51 72.1(13) . . . . ? Br2 Ru C61 C51 -70.2(3) . . . . ? C41 Ru C61 C11 -104.8(4) . . . . ? C21 Ru C61 C11 -30.2(3) . . . . ? C31 Ru C61 C11 -67.4(4) . . . . ? C51 Ru C61 C11 -134.4(5) . . . . ? Br3 Ru C61 C11 69.3(3) . . . . ? Br1 Ru C61 C11 -62.3(13) . . . . ? Br2 Ru C61 C11 155.4(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Re Ru 3.4229 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? _kl_archive_SHELXL_comment 'release 97-2' _kl_archive_SHELXL_res ; TITL e093 in P -1 CELL 0.71073 8.9917 10.5637 10.9076 111.142 91.800 96.043 ZERR 2.0 0.0009 0.0011 0.0011 0.011 0.012 0.012 LATT 1 SFAC C H O BR RU RE UNIT 30 36 6 6 2 2 L.S. 14 FMAP 2 PLAN -25 TEMP -73 ACTA BOND $H CONF WGHT 0.048200 FVAR 0.31039 RE 6 0.844660 0.207954 0.295975 11.00000 0.01952 0.01581 = 0.01961 0.00807 0.00293 0.00300 RU 5 0.620930 -0.097244 0.218347 11.00000 0.01674 0.01407 = 0.01426 0.00779 0.00283 0.00422 BR1 4 0.552465 0.146983 0.283313 11.00000 0.02209 0.02221 = 0.03951 0.01353 0.00598 0.00823 BR2 4 0.804113 -0.012853 0.080472 11.00000 0.03463 0.02560 = 0.02313 0.01010 0.00832 0.00192 BR3 4 0.829626 0.021272 0.401727 11.00000 0.03010 0.02804 = 0.02621 0.01521 -0.00153 0.00180 C1 1 0.841624 0.339926 0.213163 11.00000 0.02218 0.01897 = 0.02507 0.00095 0.00196 0.00124 O1 3 0.839760 0.419200 0.167612 11.00000 0.04273 0.03312 = 0.04666 0.02535 0.00456 0.00530 C2 1 1.058064 0.223782 0.295098 11.00000 0.02799 0.02277 = 0.02121 0.01178 0.00199 0.00709 O2 3 1.184501 0.232187 0.295050 11.00000 0.02550 0.04673 = 0.04788 0.02331 0.00439 0.00713 C3 1 0.859783 0.351707 0.464033 11.00000 0.03053 0.01504 = 0.02374 0.00589 0.00235 0.00045 O3 3 0.868813 0.435663 0.565072 11.00000 0.05802 0.03040 = 0.03293 0.00080 0.01122 -0.00108 C11 1 0.589826 -0.263729 0.291930 11.00000 0.02096 0.01980 = 0.02058 0.01658 0.00184 0.00272 C111 1 0.671145 -0.279576 0.406324 11.00000 0.03046 0.02734 = 0.02335 0.01593 0.00030 0.00476 AFIX 23 H11A 2 0.666174 -0.198340 0.487121 11.00000 -1.20000 H11B 2 0.777933 -0.287691 0.389494 11.00000 -1.20000 AFIX 0 C211 1 0.597385 -0.408896 0.425081 11.00000 0.04132 0.03025 = 0.03890 0.02557 0.00646 0.00774 AFIX 137 H21A 2 0.489316 -0.405091 0.431044 11.00000 -1.50000 H21B 2 0.641232 -0.413978 0.506321 11.00000 -1.50000 H21C 2 0.614625 -0.489988 0.349822 11.00000 -1.50000 AFIX 0 C21 1 0.458850 -0.196543 0.309602 11.00000 0.02236 0.01960 = 0.01856 0.00797 0.00525 0.00417 AFIX 43 H21 2 0.421128 -0.163694 0.394318 11.00000 -1.20000 AFIX 0 C31 1 0.384103 -0.178070 0.202483 11.00000 0.01750 0.01324 = 0.02364 0.00576 0.00271 -0.00061 C131 1 0.244627 -0.105887 0.222348 11.00000 0.02245 0.02781 = 0.03422 0.01551 0.00576 0.01096 AFIX 23 H13A 2 0.238153 -0.056972 0.160538 11.00000 -1.20000 H13B 2 0.249024 -0.038105 0.313455 11.00000 -1.20000 AFIX 0 C231 1 0.107400 -0.212600 0.197311 11.00000 0.01835 0.04516 = 0.05910 0.01362 0.00412 0.00552 AFIX 137 H23A 2 0.110429 -0.285364 0.111104 11.00000 -1.50000 H23B 2 0.016074 -0.169188 0.198525 11.00000 -1.50000 H23C 2 0.107628 -0.251732 0.266238 11.00000 -1.50000 AFIX 0 C41 1 0.441537 -0.224987 0.076733 11.00000 0.02037 0.02070 = 0.01890 0.00785 -0.00106 -0.00343 AFIX 43 H41 2 0.394112 -0.208677 0.005720 11.00000 -1.20000 AFIX 0 C51 1 0.570537 -0.296846 0.055565 11.00000 0.02509 0.01598 = 0.01905 0.00760 0.00639 0.00201 C151 1 0.623885 -0.348819 -0.080525 11.00000 0.03739 0.02807 = 0.01505 0.00441 0.00396 0.00229 AFIX 23 H15A 2 0.632867 -0.272721 -0.113589 11.00000 -1.20000 H15B 2 0.546064 -0.420590 -0.138649 11.00000 -1.20000 AFIX 0 C251 1 0.770396 -0.406653 -0.093229 11.00000 0.05027 0.03972 = 0.03213 0.01472 0.01705 0.02452 AFIX 137 H25A 2 0.849760 -0.335856 -0.039008 11.00000 -1.50000 H25B 2 0.794429 -0.437902 -0.185642 11.00000 -1.50000 H25C 2 0.762766 -0.484003 -0.063342 11.00000 -1.50000 AFIX 0 C61 1 0.642501 -0.313864 0.164275 11.00000 0.02510 0.01038 = 0.02365 0.00809 0.00420 0.00305 AFIX 43 H61 2 0.728934 -0.360360 0.151527 11.00000 -1.20000 HKLF 4 END ; _kl_archive_SCHAKAL_comment 'release 99 for Win32 systems' _kl_archive_SCHAKAL_dat ? _kl_archive_ORTEP_comment ? _kl_archive_ORTEP_ins ? _kl_archive_rtf_text ? data_e094 _publ_contact_author_name 'Dr. Kay Severin' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7768' _publ_author_name 'da Silva, Ana C.' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Heterometallic bromo-bridged complexes with Re(CO)3 fragments ; _audit_author_name 'Piotrowski, H.' _audit_block_code Re2_Ru2_Br_CO_(C12H18)_e094_Beck _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 16-Apr-00 _chemical_name_systematic ; ; _chemical_compound_source ; ; _chemical_name_common Re2Br3(CO)6+Ru2Br3(C12H18)2 _chemical_formula_moiety 'Re2, Br3, 6(C O), Ru2, Br3, 2(C12 H18)' _chemical_formula_sum 'C30 H36 Br6 O6 Re2 Ru2' _chemical_formula_weight 1546.58 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' 'O' 'O' 0.0106 0.0060 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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' _symmetry_Int_Tables_number 14 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 15.3340(11) _cell_length_b 15.1881(9) _cell_length_c 17.0439(10) _cell_angle_alpha 90 _cell_angle_beta 91.680(8) _cell_angle_gamma 90 _cell_volume 3967.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.0 _cell_special_details 'Monoclinic P (as derived from metrics)' _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.5891(3) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 12.908 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1950 _exptl_absorpt_correction_T_max 0.3495 _exptl_absorpt_process_details 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' _exptl_special_details ; crystal embedded in oil and fixed with Lithelen ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 0 0.0500 -1 -1 0 0.0460 -1 1 0 0.0570 1 -1 0 0.0510 0 1 -1 0.1010 0 1 1 0.1250 2 -1 2 0.1230 0 -1 -1 0.1040 -1 0 2 0.1140 -1 0 -1 0.0860 0 0 -1 0.1430 _diffrn_ambient_temperature 200(3) _diffrn_source_type 'Spellman DF4 Series' _diffrn_source_power 2.75_kW _diffrn_source_voltage 55_kV _diffrn_source_current 50_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 194.0 _kl_diffrn_detector_area_phi_incr 1.0 _kl_diffrn_detector_area_expos_time 2.00_min _kl_diffrn_detector_area_plate_dist 60.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.006 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 9 _kl_diffrn_detector_area_profile_max 21 _diffrn_special_details ; no crystal decay in terms of mean intensity per image ; _diffrn_reflns_number 36602 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.97 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.723 _refine_diff_density_min -1.541 _refine_diff_density_rms 0.162 _reflns_number_total 9483 _reflns_number_gt 6927 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution ; SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79) ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 9483 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_special_details ; details of H atom refinement: C-bonded H: riding with U(H)=1.2*U(C) for CH2 and CH, 1.5*U(C) for CH3 ; 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 C111 C 0.9453(4) 0.1772(4) 0.8070(4) 0.0314(13) Uani 1 1 d . . . O111 O 0.9985(3) 0.1905(3) 0.7623(3) 0.0490(12) Uani 1 1 d . . . C211 C 0.9349(4) 0.1821(4) 0.9641(4) 0.0316(13) Uani 1 1 d . . . O211 O 0.9822(3) 0.2001(3) 1.0155(3) 0.0445(11) Uani 1 1 d . . . C311 C 0.8955(3) 0.0346(4) 0.8852(3) 0.0290(12) Uani 1 1 d . . . O311 O 0.9188(3) -0.0376(3) 0.8895(3) 0.0409(10) Uani 1 1 d . . . Re1 Re 0.857340(13) 0.152478(13) 0.879467(12) 0.02108(5) Uani 1 1 d . . . Br11 Br 0.78439(4) 0.31018(3) 0.87159(3) 0.02925(12) Uani 1 1 d . . . Br21 Br 0.72508(4) 0.12079(4) 0.97050(3) 0.03077(12) Uani 1 1 d . . . Br31 Br 0.73805(4) 0.12006(4) 0.76959(3) 0.03066(12) Uani 1 1 d . . . Re2 Re 0.640134(13) 0.213705(13) 0.862550(13) 0.02292(5) Uani 1 1 d . . . C121 C 0.5868(4) 0.2782(4) 0.7787(4) 0.0315(12) Uani 1 1 d . . . O121 O 0.5521(3) 0.3139(3) 0.7279(3) 0.0497(12) Uani 1 1 d . . . C221 C 0.5420(4) 0.1371(4) 0.8563(4) 0.0363(14) Uani 1 1 d . . . O221 O 0.4808(3) 0.0948(3) 0.8513(4) 0.0596(15) Uani 1 1 d . . . C321 C 0.5807(4) 0.2810(4) 0.9375(4) 0.0329(13) Uani 1 1 d . . . O321 O 0.5440(3) 0.3191(3) 0.9852(3) 0.0541(13) Uani 1 1 d . . . C112 C 0.7622(3) 0.2418(3) 0.5695(3) 0.0198(10) Uani 1 1 d . . . C11A C 0.7753(4) 0.3390(3) 0.5695(3) 0.0271(12) Uani 1 1 d . . . H11A H 0.7233 0.3682 0.5455 0.032 Uiso 1 1 calc R . . H11B H 0.8263 0.3540 0.5378 0.032 Uiso 1 1 calc R . . C11B C 0.7902(4) 0.3719(4) 0.6534(4) 0.0349(14) Uani 1 1 d . . . H11C H 0.7407 0.3548 0.6851 0.052 Uiso 1 1 calc R . . H11D H 0.7957 0.4362 0.6532 0.052 Uiso 1 1 calc R . . H11E H 0.8439 0.3458 0.6758 0.052 Uiso 1 1 calc R . . C212 C 0.8357(3) 0.1834(3) 0.5706(3) 0.0191(10) Uani 1 1 d . . . H212 H 0.8931 0.2072 0.5725 0.023 Uiso 1 1 calc R . . C312 C 0.8243(3) 0.0916(3) 0.5689(3) 0.0232(11) Uani 1 1 d . . . C31A C 0.9018(4) 0.0302(4) 0.5686(4) 0.0329(13) Uani 1 1 d . . . H31A H 0.9529 0.0615 0.5481 0.040 Uiso 1 1 calc R . . H31B H 0.8887 -0.0205 0.5337 0.040 Uiso 1 1 calc R . . C31B C 0.9229(4) -0.0027(4) 0.6509(4) 0.0411(15) Uani 1 1 d . . . H31C H 0.9392 0.0472 0.6847 0.062 Uiso 1 1 calc R . . H31D H 0.9715 -0.0445 0.6495 0.062 Uiso 1 1 calc R . . H31E H 0.8716 -0.0321 0.6717 0.062 Uiso 1 1 calc R . . C412 C 0.7385(3) 0.0567(3) 0.5667(3) 0.0246(11) Uani 1 1 d . . . H412 H 0.7307 -0.0053 0.5656 0.030 Uiso 1 1 calc R . . C512 C 0.6649(3) 0.1117(3) 0.5661(3) 0.0232(11) Uani 1 1 d . . . C51A C 0.5750(3) 0.0730(4) 0.5640(3) 0.0349(14) Uani 1 1 d . . . H51A H 0.5753 0.0165 0.5351 0.042 Uiso 1 1 calc R . . H51B H 0.5344 0.1136 0.5358 0.042 Uiso 1 1 calc R . . C51B C 0.5438(4) 0.0577(6) 0.6461(4) 0.053(2) Uani 1 1 d . . . H51C H 0.5855 0.0198 0.6748 0.079 Uiso 1 1 calc R . . H51D H 0.4865 0.0291 0.6435 0.079 Uiso 1 1 calc R . . H51E H 0.5392 0.1143 0.6734 0.079 Uiso 1 1 calc R . . C612 C 0.6775(3) 0.2046(3) 0.5680(3) 0.0225(10) Uani 1 1 d . . . H612 H 0.6280 0.2423 0.5683 0.027 Uiso 1 1 calc R . . Ru1 Ru 0.74922(2) 0.15005(3) 0.47128(2) 0.01800(8) Uani 1 1 d . . . Br12 Br 0.62368(4) 0.13486(5) 0.37056(3) 0.03846(15) Uani 1 1 d . . . Br22 Br 0.79594(5) 0.26638(4) 0.37167(4) 0.04474(17) Uani 1 1 d . . . Br32 Br 0.82518(4) 0.05150(4) 0.37279(4) 0.03984(15) Uani 1 1 d . . . Ru2 Ru 0.74513(2) 0.14902(3) 0.27190(2) 0.01933(8) Uani 1 1 d . . . C122 C 0.7748(3) 0.2350(3) 0.1742(3) 0.0244(11) Uani 1 1 d . . . C12A C 0.8079(4) 0.3279(4) 0.1736(3) 0.0327(13) Uani 1 1 d . . . H12A H 0.8653 0.3310 0.2016 0.039 Uiso 1 1 calc R . . H12B H 0.7669 0.3668 0.2010 0.039 Uiso 1 1 calc R . . C12B C 0.8171(5) 0.3594(4) 0.0888(4) 0.0434(16) Uani 1 1 d . . . H12C H 0.8605 0.3231 0.0628 0.065 Uiso 1 1 calc R . . H12D H 0.8358 0.4210 0.0888 0.065 Uiso 1 1 calc R . . H12E H 0.7607 0.3540 0.0606 0.065 Uiso 1 1 calc R . . C222 C 0.6835(3) 0.2184(3) 0.1733(3) 0.0232(10) Uani 1 1 d . . . H222 H 0.6438 0.2665 0.1722 0.028 Uiso 1 1 calc R . . C322 C 0.6509(3) 0.1307(3) 0.1743(3) 0.0229(11) Uani 1 1 d . . . C32A C 0.5545(3) 0.1136(4) 0.1731(3) 0.0296(12) Uani 1 1 d . . . H32A H 0.5240 0.1640 0.1969 0.036 Uiso 1 1 calc R . . H32B H 0.5423 0.0603 0.2044 0.036 Uiso 1 1 calc R . . C32B C 0.5213(4) 0.1006(5) 0.0891(4) 0.0413(15) Uani 1 1 d . . . H32C H 0.5213 0.1572 0.0615 0.062 Uiso 1 1 calc R . . H32D H 0.4617 0.0771 0.0892 0.062 Uiso 1 1 calc R . . H32E H 0.5593 0.0591 0.0624 0.062 Uiso 1 1 calc R . . C422 C 0.7108(3) 0.0596(3) 0.1762(3) 0.0224(11) Uani 1 1 d . . . H422 H 0.6896 0.0008 0.1774 0.027 Uiso 1 1 calc R . . C522 C 0.8026(3) 0.0752(3) 0.1763(3) 0.0232(10) Uani 1 1 d . . . C52A C 0.8633(4) -0.0017(4) 0.1781(3) 0.0322(13) Uani 1 1 d . . . H52A H 0.8398 -0.0487 0.2118 0.039 Uiso 1 1 calc R . . H52B H 0.9209 0.0164 0.2003 0.039 Uiso 1 1 calc R . . C52B C 0.8735(4) -0.0364(4) 0.0953(4) 0.0418(16) Uani 1 1 d . . . H52C H 0.8161 -0.0523 0.0728 0.063 Uiso 1 1 calc R . . H52D H 0.9112 -0.0885 0.0967 0.063 Uiso 1 1 calc R . . H52E H 0.8997 0.0092 0.0629 0.063 Uiso 1 1 calc R . . C622 C 0.8329(3) 0.1629(4) 0.1746(3) 0.0253(11) Uani 1 1 d . . . H622 H 0.8939 0.1737 0.1736 0.030 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 C111 0.041(3) 0.022(3) 0.031(3) -0.002(2) 0.000(3) -0.002(2) O111 0.051(3) 0.047(3) 0.050(3) 0.003(2) 0.027(2) -0.015(2) C211 0.030(3) 0.026(3) 0.039(4) -0.003(2) 0.002(3) 0.001(2) O211 0.035(2) 0.054(3) 0.044(3) -0.014(2) -0.015(2) -0.001(2) C311 0.024(3) 0.034(3) 0.029(3) -0.004(2) 0.003(2) 0.000(2) O311 0.040(2) 0.031(2) 0.052(3) -0.002(2) 0.006(2) 0.0083(18) Re1 0.02199(10) 0.02206(10) 0.01923(11) -0.00123(8) 0.00102(7) -0.00031(8) Br11 0.0350(3) 0.0229(2) 0.0297(3) -0.0006(2) -0.0018(2) -0.0012(2) Br21 0.0341(3) 0.0356(3) 0.0228(3) 0.0064(2) 0.0056(2) 0.0060(2) Br31 0.0349(3) 0.0336(3) 0.0233(3) -0.0041(2) -0.0014(2) -0.0004(2) Re2 0.02404(10) 0.02074(10) 0.02398(11) 0.00231(9) 0.00081(8) 0.00208(8) C121 0.030(3) 0.033(3) 0.032(3) 0.000(3) -0.003(2) -0.004(2) O121 0.047(3) 0.054(3) 0.047(3) 0.021(2) -0.019(2) 0.003(2) C221 0.041(3) 0.025(3) 0.044(4) 0.003(3) 0.004(3) 0.005(3) O221 0.040(3) 0.035(2) 0.104(5) -0.004(3) 0.002(3) -0.014(2) C321 0.040(3) 0.026(3) 0.034(3) 0.006(3) 0.006(3) -0.001(2) O321 0.070(3) 0.035(2) 0.059(3) -0.006(2) 0.034(3) 0.012(2) C112 0.020(2) 0.025(2) 0.014(3) -0.002(2) 0.0007(18) 0.0001(19) C11A 0.030(3) 0.022(3) 0.028(3) -0.002(2) -0.002(2) 0.003(2) C11B 0.046(3) 0.028(3) 0.031(4) -0.012(2) 0.004(3) -0.005(2) C212 0.017(2) 0.024(2) 0.015(3) -0.002(2) -0.0029(18) -0.0007(19) C312 0.031(3) 0.022(2) 0.017(3) 0.003(2) 0.002(2) 0.002(2) C31A 0.030(3) 0.029(3) 0.040(4) 0.004(3) 0.007(3) 0.010(2) C31B 0.043(3) 0.038(3) 0.041(4) -0.003(3) -0.012(3) 0.016(3) C412 0.035(3) 0.021(2) 0.018(3) 0.000(2) 0.004(2) -0.005(2) C512 0.025(3) 0.032(3) 0.013(3) -0.003(2) 0.0041(19) -0.005(2) C51A 0.023(3) 0.052(4) 0.030(3) -0.002(3) 0.001(2) -0.013(3) C51B 0.030(3) 0.088(6) 0.040(4) 0.007(4) 0.005(3) -0.030(3) C612 0.022(2) 0.028(3) 0.018(3) -0.005(2) 0.0011(19) 0.001(2) Ru1 0.02027(18) 0.01905(18) 0.0148(2) -0.00135(16) 0.00206(14) -0.00171(15) Br12 0.0245(3) 0.0699(4) 0.0210(3) 0.0016(3) 0.0011(2) -0.0027(3) Br22 0.0838(5) 0.0316(3) 0.0190(3) -0.0028(2) 0.0059(3) -0.0276(3) Br32 0.0471(4) 0.0493(4) 0.0231(3) -0.0048(3) 0.0009(3) 0.0195(3) Ru2 0.02201(19) 0.02120(19) 0.0149(2) -0.00204(16) 0.00214(15) -0.00225(16) C122 0.031(3) 0.026(3) 0.016(3) 0.000(2) 0.001(2) -0.005(2) C12A 0.042(3) 0.031(3) 0.025(3) 0.000(2) 0.001(2) -0.010(2) C12B 0.065(4) 0.033(3) 0.033(4) 0.009(3) 0.011(3) -0.009(3) C222 0.027(3) 0.023(2) 0.020(3) -0.001(2) -0.001(2) 0.002(2) C322 0.024(2) 0.028(3) 0.016(3) -0.005(2) -0.002(2) -0.002(2) C32A 0.023(3) 0.033(3) 0.033(3) -0.005(2) 0.004(2) 0.001(2) C32B 0.027(3) 0.055(4) 0.042(4) 0.011(3) -0.010(3) -0.006(3) C422 0.026(3) 0.021(2) 0.020(3) -0.006(2) 0.001(2) -0.002(2) C522 0.028(3) 0.031(3) 0.011(2) -0.003(2) 0.0021(19) 0.000(2) C52A 0.031(3) 0.040(3) 0.026(3) -0.005(3) 0.003(2) 0.009(2) C52B 0.040(3) 0.051(4) 0.034(4) -0.019(3) -0.003(3) 0.019(3) C622 0.022(2) 0.040(3) 0.014(3) -0.002(2) 0.0053(19) -0.005(2) 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 C111 O111 1.151(7) . ? C111 Re1 1.892(6) . ? C211 O211 1.154(7) . ? C211 Re1 1.896(6) . ? C311 O311 1.155(7) . ? C311 Re1 1.886(6) . ? Re1 Br31 2.6258(6) . ? Re1 Br21 2.6337(6) . ? Re1 Br11 2.6452(6) . ? Br11 Re2 2.6540(6) . ? Br21 Re2 2.6330(6) . ? Br31 Re2 2.6319(6) . ? Re2 C321 1.891(6) . ? Re2 C121 1.898(6) . ? Re2 C221 1.903(6) . ? C121 O121 1.141(7) . ? C221 O221 1.138(7) . ? C321 O321 1.158(7) . ? C112 C612 1.417(7) . ? C112 C212 1.434(7) . ? C112 C11A 1.489(7) . ? C112 Ru1 2.183(5) . ? C11A C11B 1.525(8) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C11B H11C 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C212 C312 1.406(7) . ? C212 Ru1 2.179(5) . ? C212 H212 0.9500 . ? C312 C412 1.417(7) . ? C312 C31A 1.512(7) . ? C312 Ru1 2.184(5) . ? C31A C31B 1.514(9) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C31B H31C 0.9800 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C412 C512 1.403(7) . ? C412 Ru1 2.167(5) . ? C412 H412 0.9500 . ? C512 C612 1.424(7) . ? C512 C51A 1.499(7) . ? C512 Ru1 2.178(5) . ? C51A C51B 1.511(9) . ? C51A H51A 0.9900 . ? C51A H51B 0.9900 . ? C51B H51C 0.9800 . ? C51B H51D 0.9800 . ? C51B H51E 0.9800 . ? C612 Ru1 2.173(5) . ? C612 H612 0.9500 . ? Ru1 Br12 2.5520(7) . ? Ru1 Br32 2.5553(7) . ? Ru1 Br22 2.5667(7) . ? Br12 Ru2 2.5544(7) . ? Br22 Ru2 2.5687(7) . ? Br32 Ru2 2.5561(8) . ? Ru2 C122 2.174(5) . ? Ru2 C222 2.176(5) . ? Ru2 C422 2.176(5) . ? Ru2 C622 2.177(5) . ? Ru2 C522 2.184(5) . ? Ru2 C322 2.190(5) . ? C122 C622 1.412(7) . ? C122 C222 1.422(7) . ? C122 C12A 1.501(7) . ? C12A C12B 1.532(8) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C12B H12C 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C222 C322 1.423(7) . ? C222 H222 0.9500 . ? C322 C422 1.419(7) . ? C322 C32A 1.500(7) . ? C32A C32B 1.518(8) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C32B H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C422 C522 1.428(7) . ? C422 H422 0.9500 . ? C522 C622 1.411(7) . ? C522 C52A 1.493(7) . ? C52A C52B 1.518(8) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C52B H52C 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C622 H622 0.9500 . ? 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 O111 C111 Re1 178.5(5) . . ? O211 C211 Re1 179.8(6) . . ? O311 C311 Re1 179.3(5) . . ? C311 Re1 C111 89.8(2) . . ? C311 Re1 C211 90.0(2) . . ? C111 Re1 C211 90.4(3) . . ? C311 Re1 Br31 93.86(17) . . ? C111 Re1 Br31 93.81(18) . . ? C211 Re1 Br31 174.33(17) . . ? C311 Re1 Br21 92.26(17) . . ? C111 Re1 Br21 175.07(18) . . ? C211 Re1 Br21 94.10(18) . . ? Br31 Re1 Br21 81.57(2) . . ? C311 Re1 Br11 173.07(16) . . ? C111 Re1 Br11 95.48(17) . . ? C211 Re1 Br11 94.52(17) . . ? Br31 Re1 Br11 81.309(19) . . ? Br21 Re1 Br11 82.162(19) . . ? Re1 Br11 Re2 81.579(16) . . ? Re2 Br21 Re1 82.190(18) . . ? Re1 Br31 Re2 82.363(18) . . ? C321 Re2 C121 91.3(3) . . ? C321 Re2 C221 88.4(3) . . ? C121 Re2 C221 87.2(2) . . ? C321 Re2 Br31 173.52(19) . . ? C121 Re2 Br31 93.84(18) . . ? C221 Re2 Br31 95.72(19) . . ? C321 Re2 Br21 93.24(18) . . ? C121 Re2 Br21 175.03(18) . . ? C221 Re2 Br21 94.90(18) . . ? Br31 Re2 Br21 81.472(19) . . ? C321 Re2 Br11 94.58(18) . . ? C121 Re2 Br11 95.68(17) . . ? C221 Re2 Br11 175.79(17) . . ? Br31 Re2 Br11 81.030(19) . . ? Br21 Re2 Br11 82.007(19) . . ? O121 C121 Re2 176.9(5) . . ? O221 C221 Re2 176.5(5) . . ? O321 C321 Re2 177.2(5) . . ? C612 C112 C212 118.2(4) . . ? C612 C112 C11A 121.3(4) . . ? C212 C112 C11A 120.5(4) . . ? C612 C112 Ru1 70.6(3) . . ? C212 C112 Ru1 70.6(3) . . ? C11A C112 Ru1 129.9(4) . . ? C112 C11A C11B 109.9(5) . . ? C112 C11A H11A 109.7 . . ? C11B C11A H11A 109.7 . . ? C112 C11A H11B 109.7 . . ? C11B C11A H11B 109.7 . . ? H11A C11A H11B 108.2 . . ? C11A C11B H11C 109.5 . . ? C11A C11B H11D 109.5 . . ? H11C C11B H11D 109.5 . . ? C11A C11B H11E 109.5 . . ? H11C C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C312 C212 C112 121.1(4) . . ? C312 C212 Ru1 71.4(3) . . ? C112 C212 Ru1 71.0(3) . . ? C312 C212 H212 119.5 . . ? C112 C212 H212 119.5 . . ? Ru1 C212 H212 131.0 . . ? C212 C312 C412 119.1(5) . . ? C212 C312 C31A 121.0(5) . . ? C412 C312 C31A 119.9(5) . . ? C212 C312 Ru1 71.0(3) . . ? C412 C312 Ru1 70.4(3) . . ? C31A C312 Ru1 130.2(4) . . ? C312 C31A C31B 110.3(5) . . ? C312 C31A H31A 109.6 . . ? C31B C31A H31A 109.6 . . ? C312 C31A H31B 109.6 . . ? C31B C31A H31B 109.6 . . ? H31A C31A H31B 108.1 . . ? C31A C31B H31C 109.5 . . ? C31A C31B H31D 109.5 . . ? H31C C31B H31D 109.5 . . ? C31A C31B H31E 109.5 . . ? H31C C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C512 C412 C312 121.5(5) . . ? C512 C412 Ru1 71.6(3) . . ? C312 C412 Ru1 71.6(3) . . ? C512 C412 H412 119.2 . . ? C312 C412 H412 119.2 . . ? Ru1 C412 H412 130.2 . . ? C412 C512 C612 118.8(4) . . ? C412 C512 C51A 120.5(5) . . ? C612 C512 C51A 120.8(5) . . ? C412 C512 Ru1 70.7(3) . . ? C612 C512 Ru1 70.7(3) . . ? C51A C512 Ru1 130.7(4) . . ? C512 C51A C51B 110.7(5) . . ? C512 C51A H51A 109.5 . . ? C51B C51A H51A 109.5 . . ? C512 C51A H51B 109.5 . . ? C51B C51A H51B 109.5 . . ? H51A C51A H51B 108.1 . . ? C51A C51B H51C 109.5 . . ? C51A C51B H51D 109.5 . . ? H51C C51B H51D 109.5 . . ? C51A C51B H51E 109.5 . . ? H51C C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? C112 C612 C512 121.3(5) . . ? C112 C612 Ru1 71.4(3) . . ? C512 C612 Ru1 71.1(3) . . ? C112 C612 H612 119.4 . . ? C512 C612 H612 119.4 . . ? Ru1 C612 H612 130.9 . . ? C412 Ru1 C612 68.2(2) . . ? C412 Ru1 C512 37.7(2) . . ? C612 Ru1 C512 38.21(19) . . ? C412 Ru1 C212 68.10(19) . . ? C612 Ru1 C212 68.42(18) . . ? C512 Ru1 C212 81.18(19) . . ? C412 Ru1 C112 81.34(19) . . ? C612 Ru1 C112 37.96(18) . . ? C512 Ru1 C112 69.18(18) . . ? C212 Ru1 C112 38.38(18) . . ? C412 Ru1 C312 38.00(19) . . ? C612 Ru1 C312 81.03(19) . . ? C512 Ru1 C312 68.69(19) . . ? C212 Ru1 C312 37.60(19) . . ? C112 Ru1 C312 68.97(19) . . ? C412 Ru1 Br12 111.93(14) . . ? C612 Ru1 Br12 98.98(13) . . ? C512 Ru1 Br12 91.31(13) . . ? C212 Ru1 Br12 166.76(13) . . ? C112 Ru1 Br12 128.58(13) . . ? C312 Ru1 Br12 147.79(14) . . ? C412 Ru1 Br32 98.97(14) . . ? C612 Ru1 Br32 166.52(14) . . ? C512 Ru1 Br32 128.50(14) . . ? C212 Ru1 Br32 111.58(13) . . ? C112 Ru1 Br32 147.64(13) . . ? C312 Ru1 Br32 91.28(14) . . ? Br12 Ru1 Br32 81.63(2) . . ? C412 Ru1 Br22 167.24(14) . . ? C612 Ru1 Br22 113.39(14) . . ? C512 Ru1 Br22 149.11(14) . . ? C212 Ru1 Br22 100.27(13) . . ? C112 Ru1 Br22 92.68(13) . . ? C312 Ru1 Br22 129.26(14) . . ? Br12 Ru1 Br22 80.61(2) . . ? Br32 Ru1 Br22 80.05(2) . . ? Ru1 Br12 Ru2 83.40(2) . . ? Ru1 Br22 Ru2 82.83(2) . . ? Ru1 Br32 Ru2 83.30(2) . . ? C122 Ru2 C222 38.16(19) . . ? C122 Ru2 C422 81.48(19) . . ? C222 Ru2 C422 68.51(19) . . ? C122 Ru2 C622 37.9(2) . . ? C222 Ru2 C622 68.3(2) . . ? C422 Ru2 C622 68.30(19) . . ? C122 Ru2 C522 68.8(2) . . ? C222 Ru2 C522 81.31(19) . . ? C422 Ru2 C522 38.22(18) . . ? C622 Ru2 C522 37.7(2) . . ? C122 Ru2 C322 69.02(19) . . ? C222 Ru2 C322 38.03(19) . . ? C422 Ru2 C322 37.94(19) . . ? C622 Ru2 C322 80.93(19) . . ? C522 Ru2 C322 68.91(19) . . ? C122 Ru2 Br12 136.67(14) . . ? C222 Ru2 Br12 103.90(14) . . ? C422 Ru2 Br12 106.03(13) . . ? C622 Ru2 Br12 171.41(14) . . ? C522 Ru2 Br12 139.96(14) . . ? C322 Ru2 Br12 90.68(14) . . ? C122 Ru2 Br32 139.12(14) . . ? C222 Ru2 Br32 171.64(14) . . ? C422 Ru2 Br32 104.08(14) . . ? C622 Ru2 Br32 105.84(15) . . ? C522 Ru2 Br32 90.44(14) . . ? C322 Ru2 Br32 136.98(14) . . ? Br12 Ru2 Br32 81.57(2) . . ? C122 Ru2 Br22 91.40(14) . . ? C222 Ru2 Br22 106.95(14) . . ? C422 Ru2 Br22 172.61(14) . . ? C622 Ru2 Br22 104.78(14) . . ? C522 Ru2 Br22 136.76(14) . . ? C322 Ru2 Br22 140.52(14) . . ? Br12 Ru2 Br22 80.53(2) . . ? Br32 Ru2 Br22 80.00(2) . . ? C622 C122 C222 119.0(5) . . ? C622 C122 C12A 121.0(5) . . ? C222 C122 C12A 120.0(5) . . ? C622 C122 Ru2 71.2(3) . . ? C222 C122 Ru2 71.0(3) . . ? C12A C122 Ru2 130.4(4) . . ? C122 C12A C12B 109.9(5) . . ? C122 C12A H12A 109.7 . . ? C12B C12A H12A 109.7 . . ? C122 C12A H12B 109.7 . . ? C12B C12A H12B 109.7 . . ? H12A C12A H12B 108.2 . . ? C12A C12B H12C 109.5 . . ? C12A C12B H12D 109.5 . . ? H12C C12B H12D 109.5 . . ? C12A C12B H12E 109.5 . . ? H12C C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C122 C222 C322 120.8(5) . . ? C122 C222 Ru2 70.9(3) . . ? C322 C222 Ru2 71.5(3) . . ? C122 C222 H222 119.6 . . ? C322 C222 H222 119.6 . . ? Ru2 C222 H222 130.7 . . ? C422 C322 C222 119.1(4) . . ? C422 C322 C32A 120.4(5) . . ? C222 C322 C32A 120.6(5) . . ? C422 C322 Ru2 70.5(3) . . ? C222 C322 Ru2 70.4(3) . . ? C32A C322 Ru2 131.3(4) . . ? C322 C32A C32B 109.8(5) . . ? C322 C32A H32A 109.7 . . ? C32B C32A H32A 109.7 . . ? C322 C32A H32B 109.7 . . ? C32B C32A H32B 109.7 . . ? H32A C32A H32B 108.2 . . ? C32A C32B H32C 109.5 . . ? C32A C32B H32D 109.5 . . ? H32C C32B H32D 109.5 . . ? C32A C32B H32E 109.5 . . ? H32C C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C322 C422 C522 120.8(5) . . ? C322 C422 Ru2 71.6(3) . . ? C522 C422 Ru2 71.2(3) . . ? C322 C422 H422 119.6 . . ? C522 C422 H422 119.6 . . ? Ru2 C422 H422 130.2 . . ? C622 C522 C422 118.8(5) . . ? C622 C522 C52A 122.2(5) . . ? C422 C522 C52A 118.9(5) . . ? C622 C522 Ru2 70.8(3) . . ? C422 C522 Ru2 70.6(3) . . ? C52A C522 Ru2 130.7(4) . . ? C522 C52A C52B 109.5(5) . . ? C522 C52A H52A 109.8 . . ? C52B C52A H52A 109.8 . . ? C522 C52A H52B 109.8 . . ? C52B C52A H52B 109.8 . . ? H52A C52A H52B 108.2 . . ? C52A C52B H52C 109.5 . . ? C52A C52B H52D 109.5 . . ? H52C C52B H52D 109.5 . . ? C52A C52B H52E 109.5 . . ? H52C C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C522 C622 C122 121.6(5) . . ? C522 C622 Ru2 71.4(3) . . ? C122 C622 Ru2 71.0(3) . . ? C522 C622 H622 119.2 . . ? C122 C622 H622 119.2 . . ? Ru2 C622 H622 131.4 . . ? 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 O311 C311 Re1 C111 136(38) . . . . ? O311 C311 Re1 C211 46(38) . . . . ? O311 C311 Re1 Br31 -130(38) . . . . ? O311 C311 Re1 Br21 -48(38) . . . . ? O311 C311 Re1 Br11 -85(39) . . . . ? O111 C111 Re1 C311 35(23) . . . . ? O111 C111 Re1 C211 125(23) . . . . ? O111 C111 Re1 Br31 -59(23) . . . . ? O111 C111 Re1 Br21 -79(24) . . . . ? O111 C111 Re1 Br11 -141(23) . . . . ? O211 C211 Re1 C311 83(100) . . . . ? O211 C211 Re1 C111 -7(100) . . . . ? O211 C211 Re1 Br31 -145(100) . . . . ? O211 C211 Re1 Br21 175(100) . . . . ? O211 C211 Re1 Br11 -103(100) . . . . ? C311 Re1 Br11 Re2 -4.3(15) . . . . ? C111 Re1 Br11 Re2 134.82(18) . . . . ? C211 Re1 Br11 Re2 -134.35(18) . . . . ? Br31 Re1 Br11 Re2 41.789(18) . . . . ? Br21 Re1 Br11 Re2 -40.823(18) . . . . ? C311 Re1 Br21 Re2 -134.73(18) . . . . ? C111 Re1 Br21 Re2 -20.5(19) . . . . ? C211 Re1 Br21 Re2 135.15(17) . . . . ? Br31 Re1 Br21 Re2 -41.168(17) . . . . ? Br11 Re1 Br21 Re2 41.142(17) . . . . ? C311 Re1 Br31 Re2 132.89(17) . . . . ? C111 Re1 Br31 Re2 -137.09(17) . . . . ? C211 Re1 Br31 Re2 0.7(18) . . . . ? Br21 Re1 Br31 Re2 41.169(17) . . . . ? Br11 Re1 Br31 Re2 -42.122(17) . . . . ? Re1 Br31 Re2 C321 -5.7(15) . . . . ? Re1 Br31 Re2 C121 137.14(17) . . . . ? Re1 Br31 Re2 C221 -135.31(19) . . . . ? Re1 Br31 Re2 Br21 -41.195(18) . . . . ? Re1 Br31 Re2 Br11 41.988(17) . . . . ? Re1 Br21 Re2 C321 -135.17(17) . . . . ? Re1 Br21 Re2 C121 22(2) . . . . ? Re1 Br21 Re2 C221 136.14(19) . . . . ? Re1 Br21 Re2 Br31 41.065(17) . . . . ? Re1 Br21 Re2 Br11 -40.994(17) . . . . ? Re1 Br11 Re2 C321 133.49(18) . . . . ? Re1 Br11 Re2 C121 -134.72(18) . . . . ? Re1 Br11 Re2 C221 -2(3) . . . . ? Re1 Br11 Re2 Br31 -41.709(17) . . . . ? Re1 Br11 Re2 Br21 40.854(17) . . . . ? C321 Re2 C121 O121 -101(11) . . . . ? C221 Re2 C121 O121 -12(11) . . . . ? Br31 Re2 C121 O121 83(11) . . . . ? Br21 Re2 C121 O121 103(10) . . . . ? Br11 Re2 C121 O121 165(11) . . . . ? C321 Re2 C221 O221 60(10) . . . . ? C121 Re2 C221 O221 -31(10) . . . . ? Br31 Re2 C221 O221 -125(10) . . . . ? Br21 Re2 C221 O221 153(10) . . . . ? Br11 Re2 C221 O221 -164(8) . . . . ? C121 Re2 C321 O321 144(12) . . . . ? C221 Re2 C321 O321 57(12) . . . . ? Br31 Re2 C321 O321 -73(12) . . . . ? Br21 Re2 C321 O321 -38(12) . . . . ? Br11 Re2 C321 O321 -120(12) . . . . ? C612 C112 C11A C11B 95.9(6) . . . . ? C212 C112 C11A C11B -84.5(6) . . . . ? Ru1 C112 C11A C11B -173.9(4) . . . . ? C612 C112 C212 C312 1.0(7) . . . . ? C11A C112 C212 C312 -178.6(5) . . . . ? Ru1 C112 C212 C312 -53.0(4) . . . . ? C612 C112 C212 Ru1 54.0(4) . . . . ? C11A C112 C212 Ru1 -125.6(5) . . . . ? C112 C212 C312 C412 -0.5(8) . . . . ? Ru1 C212 C312 C412 -53.3(4) . . . . ? C112 C212 C312 C31A 178.9(5) . . . . ? Ru1 C212 C312 C31A 126.1(5) . . . . ? C112 C212 C312 Ru1 52.8(4) . . . . ? C212 C312 C31A C31B 97.6(6) . . . . ? C412 C312 C31A C31B -83.0(6) . . . . ? Ru1 C312 C31A C31B -171.8(4) . . . . ? C212 C312 C412 C512 0.0(8) . . . . ? C31A C312 C412 C512 -179.4(5) . . . . ? Ru1 C312 C412 C512 -53.5(5) . . . . ? C212 C312 C412 Ru1 53.6(4) . . . . ? C31A C312 C412 Ru1 -125.8(5) . . . . ? C312 C412 C512 C612 -0.2(8) . . . . ? Ru1 C412 C512 C612 -53.7(4) . . . . ? C312 C412 C512 C51A -179.9(5) . . . . ? Ru1 C412 C512 C51A 126.6(5) . . . . ? C312 C412 C512 Ru1 53.6(5) . . . . ? C412 C512 C51A C51B 89.9(7) . . . . ? C612 C512 C51A C51B -89.8(7) . . . . ? Ru1 C512 C51A C51B 180.0(5) . . . . ? C212 C112 C612 C512 -1.1(7) . . . . ? C11A C112 C612 C512 178.5(5) . . . . ? Ru1 C112 C612 C512 52.9(4) . . . . ? C212 C112 C612 Ru1 -54.0(4) . . . . ? C11A C112 C612 Ru1 125.6(5) . . . . ? C412 C512 C612 C112 0.7(7) . . . . ? C51A C512 C612 C112 -179.6(5) . . . . ? Ru1 C512 C612 C112 -53.0(4) . . . . ? C412 C512 C612 Ru1 53.7(4) . . . . ? C51A C512 C612 Ru1 -126.6(5) . . . . ? C512 C412 Ru1 C612 29.9(3) . . . . ? C312 C412 Ru1 C612 -103.8(3) . . . . ? C312 C412 Ru1 C512 -133.7(4) . . . . ? C512 C412 Ru1 C212 104.5(3) . . . . ? C312 C412 Ru1 C212 -29.3(3) . . . . ? C512 C412 Ru1 C112 67.0(3) . . . . ? C312 C412 Ru1 C112 -66.8(3) . . . . ? C512 C412 Ru1 C312 133.7(4) . . . . ? C512 C412 Ru1 Br12 -61.2(3) . . . . ? C312 C412 Ru1 Br12 165.0(3) . . . . ? C512 C412 Ru1 Br32 -145.8(3) . . . . ? C312 C412 Ru1 Br32 80.5(3) . . . . ? C512 C412 Ru1 Br22 129.7(6) . . . . ? C312 C412 Ru1 Br22 -4.1(8) . . . . ? C112 C612 Ru1 C412 104.4(3) . . . . ? C512 C612 Ru1 C412 -29.5(3) . . . . ? C112 C612 Ru1 C512 133.9(4) . . . . ? C112 C612 Ru1 C212 30.3(3) . . . . ? C512 C612 Ru1 C212 -103.6(3) . . . . ? C512 C612 Ru1 C112 -133.9(4) . . . . ? C112 C612 Ru1 C312 67.2(3) . . . . ? C512 C612 Ru1 C312 -66.8(3) . . . . ? C112 C612 Ru1 Br12 -145.5(3) . . . . ? C512 C612 Ru1 Br12 80.6(3) . . . . ? C112 C612 Ru1 Br32 123.0(5) . . . . ? C512 C612 Ru1 Br32 -11.0(7) . . . . ? C112 C612 Ru1 Br22 -61.9(3) . . . . ? C512 C612 Ru1 Br22 164.2(2) . . . . ? C612 C512 Ru1 C412 131.5(4) . . . . ? C51A C512 Ru1 C412 -114.1(6) . . . . ? C412 C512 Ru1 C612 -131.5(4) . . . . ? C51A C512 Ru1 C612 114.4(6) . . . . ? C412 C512 Ru1 C212 -65.4(3) . . . . ? C612 C512 Ru1 C212 66.1(3) . . . . ? C51A C512 Ru1 C212 -179.4(5) . . . . ? C412 C512 Ru1 C112 -103.2(3) . . . . ? C612 C512 Ru1 C112 28.3(3) . . . . ? C51A C512 Ru1 C112 142.7(6) . . . . ? C412 C512 Ru1 C312 -28.5(3) . . . . ? C612 C512 Ru1 C312 103.0(3) . . . . ? C51A C512 Ru1 C312 -142.6(6) . . . . ? C412 C512 Ru1 Br12 125.6(3) . . . . ? C612 C512 Ru1 Br12 -102.9(3) . . . . ? C51A C512 Ru1 Br12 11.5(5) . . . . ? C412 C512 Ru1 Br32 45.2(3) . . . . ? C612 C512 Ru1 Br32 176.7(2) . . . . ? C51A C512 Ru1 Br32 -68.8(6) . . . . ? C412 C512 Ru1 Br22 -160.7(2) . . . . ? C612 C512 Ru1 Br22 -29.1(4) . . . . ? C51A C512 Ru1 Br22 85.3(6) . . . . ? C312 C212 Ru1 C412 29.6(3) . . . . ? C112 C212 Ru1 C412 -104.2(3) . . . . ? C312 C212 Ru1 C612 103.8(3) . . . . ? C112 C212 Ru1 C612 -30.0(3) . . . . ? C312 C212 Ru1 C512 66.3(3) . . . . ? C112 C212 Ru1 C512 -67.5(3) . . . . ? C312 C212 Ru1 C112 133.8(4) . . . . ? C112 C212 Ru1 C312 -133.8(4) . . . . ? C312 C212 Ru1 Br12 122.4(5) . . . . ? C112 C212 Ru1 Br12 -11.4(8) . . . . ? C312 C212 Ru1 Br32 -61.7(3) . . . . ? C112 C212 Ru1 Br32 164.5(2) . . . . ? C312 C212 Ru1 Br22 -145.0(3) . . . . ? C112 C212 Ru1 Br22 81.2(3) . . . . ? C612 C112 Ru1 C412 -65.5(3) . . . . ? C212 C112 Ru1 C412 65.5(3) . . . . ? C11A C112 Ru1 C412 179.5(5) . . . . ? C212 C112 Ru1 C612 130.9(4) . . . . ? C11A C112 Ru1 C612 -115.1(6) . . . . ? C612 C112 Ru1 C512 -28.5(3) . . . . ? C212 C112 Ru1 C512 102.5(3) . . . . ? C11A C112 Ru1 C512 -143.5(5) . . . . ? C612 C112 Ru1 C212 -130.9(4) . . . . ? C11A C112 Ru1 C212 114.0(6) . . . . ? C612 C112 Ru1 C312 -102.8(3) . . . . ? C212 C112 Ru1 C312 28.1(3) . . . . ? C11A C112 Ru1 C312 142.2(5) . . . . ? C612 C112 Ru1 Br12 45.7(3) . . . . ? C212 C112 Ru1 Br12 176.7(2) . . . . ? C11A C112 Ru1 Br12 -69.3(5) . . . . ? C612 C112 Ru1 Br32 -158.6(2) . . . . ? C212 C112 Ru1 Br32 -27.6(4) . . . . ? C11A C112 Ru1 Br32 86.4(5) . . . . ? C612 C112 Ru1 Br22 125.9(3) . . . . ? C212 C112 Ru1 Br22 -103.2(3) . . . . ? C11A C112 Ru1 Br22 10.8(4) . . . . ? C212 C312 Ru1 C412 -132.0(4) . . . . ? C31A C312 Ru1 C412 113.0(6) . . . . ? C212 C312 Ru1 C612 -66.1(3) . . . . ? C412 C312 Ru1 C612 65.9(3) . . . . ? C31A C312 Ru1 C612 178.9(5) . . . . ? C212 C312 Ru1 C512 -103.7(3) . . . . ? C412 C312 Ru1 C512 28.3(3) . . . . ? C31A C312 Ru1 C512 141.3(5) . . . . ? C412 C312 Ru1 C212 132.0(4) . . . . ? C31A C312 Ru1 C212 -115.0(6) . . . . ? C212 C312 Ru1 C112 -28.7(3) . . . . ? C412 C312 Ru1 C112 103.3(3) . . . . ? C31A C312 Ru1 C112 -143.7(5) . . . . ? C212 C312 Ru1 Br12 -158.7(2) . . . . ? C412 C312 Ru1 Br12 -26.7(4) . . . . ? C31A C312 Ru1 Br12 86.3(5) . . . . ? C212 C312 Ru1 Br32 125.0(3) . . . . ? C412 C312 Ru1 Br32 -103.0(3) . . . . ? C31A C312 Ru1 Br32 10.1(5) . . . . ? C212 C312 Ru1 Br22 46.9(3) . . . . ? C412 C312 Ru1 Br22 178.8(2) . . . . ? C31A C312 Ru1 Br22 -68.1(5) . . . . ? C412 Ru1 Br12 Ru2 -136.16(15) . . . . ? C612 Ru1 Br12 Ru2 153.82(14) . . . . ? C512 Ru1 Br12 Ru2 -168.57(14) . . . . ? C212 Ru1 Br12 Ru2 136.4(6) . . . . ? C112 Ru1 Br12 Ru2 127.32(17) . . . . ? C312 Ru1 Br12 Ru2 -118.8(3) . . . . ? Br32 Ru1 Br12 Ru2 -39.81(2) . . . . ? Br22 Ru1 Br12 Ru2 41.41(2) . . . . ? C412 Ru1 Br22 Ru2 128.6(6) . . . . ? C612 Ru1 Br22 Ru2 -136.98(14) . . . . ? C512 Ru1 Br22 Ru2 -117.8(3) . . . . ? C212 Ru1 Br22 Ru2 152.22(13) . . . . ? C112 Ru1 Br22 Ru2 -169.88(13) . . . . ? C312 Ru1 Br22 Ru2 125.32(18) . . . . ? Br12 Ru1 Br22 Ru2 -41.19(2) . . . . ? Br32 Ru1 Br22 Ru2 41.87(2) . . . . ? C412 Ru1 Br32 Ru2 150.83(14) . . . . ? C612 Ru1 Br32 Ru2 133.4(6) . . . . ? C512 Ru1 Br32 Ru2 124.77(17) . . . . ? C212 Ru1 Br32 Ru2 -139.28(14) . . . . ? C112 Ru1 Br32 Ru2 -121.2(2) . . . . ? C312 Ru1 Br32 Ru2 -171.77(14) . . . . ? Br12 Ru1 Br32 Ru2 39.79(2) . . . . ? Br22 Ru1 Br32 Ru2 -42.07(2) . . . . ? Ru1 Br12 Ru2 C122 -123.3(2) . . . . ? Ru1 Br12 Ru2 C222 -146.64(14) . . . . ? Ru1 Br12 Ru2 C422 142.11(14) . . . . ? Ru1 Br12 Ru2 C622 -170.2(10) . . . . ? Ru1 Br12 Ru2 C522 120.3(2) . . . . ? Ru1 Br12 Ru2 C322 177.31(14) . . . . ? Ru1 Br12 Ru2 Br32 39.80(2) . . . . ? Ru1 Br12 Ru2 Br22 -41.38(2) . . . . ? Ru1 Br32 Ru2 C122 122.5(2) . . . . ? Ru1 Br32 Ru2 C222 -171.2(9) . . . . ? Ru1 Br32 Ru2 C422 -144.26(14) . . . . ? Ru1 Br32 Ru2 C622 144.70(15) . . . . ? Ru1 Br32 Ru2 C522 179.64(14) . . . . ? Ru1 Br32 Ru2 C322 -121.6(2) . . . . ? Ru1 Br32 Ru2 Br12 -39.75(2) . . . . ? Ru1 Br32 Ru2 Br22 42.04(2) . . . . ? Ru1 Br22 Ru2 C122 178.35(14) . . . . ? Ru1 Br22 Ru2 C222 142.91(14) . . . . ? Ru1 Br22 Ru2 C422 -166.0(10) . . . . ? Ru1 Br22 Ru2 C622 -145.76(15) . . . . ? Ru1 Br22 Ru2 C522 -121.7(2) . . . . ? Ru1 Br22 Ru2 C322 120.6(2) . . . . ? Ru1 Br22 Ru2 Br12 41.15(2) . . . . ? Ru1 Br22 Ru2 Br32 -41.86(2) . . . . ? C222 Ru2 C122 C622 -131.3(4) . . . . ? C422 Ru2 C122 C622 -65.4(3) . . . . ? C522 Ru2 C122 C622 -27.9(3) . . . . ? C322 Ru2 C122 C622 -102.6(3) . . . . ? Br12 Ru2 C122 C622 -169.8(2) . . . . ? Br32 Ru2 C122 C622 36.3(4) . . . . ? Br22 Ru2 C122 C622 112.6(3) . . . . ? C422 Ru2 C122 C222 65.9(3) . . . . ? C622 Ru2 C122 C222 131.3(4) . . . . ? C522 Ru2 C122 C222 103.3(3) . . . . ? C322 Ru2 C122 C222 28.7(3) . . . . ? Br12 Ru2 C122 C222 -38.5(4) . . . . ? Br32 Ru2 C122 C222 167.6(2) . . . . ? Br22 Ru2 C122 C222 -116.2(3) . . . . ? C222 Ru2 C122 C12A 113.6(6) . . . . ? C422 Ru2 C122 C12A 179.5(5) . . . . ? C622 Ru2 C122 C12A -115.1(6) . . . . ? C522 Ru2 C122 C12A -143.0(5) . . . . ? C322 Ru2 C122 C12A 142.3(5) . . . . ? Br12 Ru2 C122 C12A 75.1(5) . . . . ? Br32 Ru2 C122 C12A -78.8(5) . . . . ? Br22 Ru2 C122 C12A -2.5(5) . . . . ? C622 C122 C12A C12B 89.7(6) . . . . ? C222 C122 C12A C12B -89.5(6) . . . . ? Ru2 C122 C12A C12B -179.3(4) . . . . ? C622 C122 C222 C322 1.1(8) . . . . ? C12A C122 C222 C322 -179.7(5) . . . . ? Ru2 C122 C222 C322 -53.4(4) . . . . ? C622 C122 C222 Ru2 54.4(4) . . . . ? C12A C122 C222 Ru2 -126.4(5) . . . . ? C422 Ru2 C222 C122 -104.1(3) . . . . ? C622 Ru2 C222 C122 -29.8(3) . . . . ? C522 Ru2 C222 C122 -66.6(3) . . . . ? C322 Ru2 C222 C122 -133.4(4) . . . . ? Br12 Ru2 C222 C122 153.9(3) . . . . ? Br32 Ru2 C222 C122 -75.9(10) . . . . ? Br22 Ru2 C222 C122 69.7(3) . . . . ? C122 Ru2 C222 C322 133.4(4) . . . . ? C422 Ru2 C222 C322 29.3(3) . . . . ? C622 Ru2 C222 C322 103.6(3) . . . . ? C522 Ru2 C222 C322 66.7(3) . . . . ? Br12 Ru2 C222 C322 -72.8(3) . . . . ? Br32 Ru2 C222 C322 57.4(10) . . . . ? Br22 Ru2 C222 C322 -156.9(3) . . . . ? C122 C222 C322 C422 0.1(8) . . . . ? Ru2 C222 C322 C422 -52.9(4) . . . . ? C122 C222 C322 C32A -179.8(5) . . . . ? Ru2 C222 C322 C32A 127.1(5) . . . . ? C122 C222 C322 Ru2 53.1(4) . . . . ? C122 Ru2 C322 C422 103.5(3) . . . . ? C222 Ru2 C322 C422 132.3(4) . . . . ? C622 Ru2 C322 C422 66.2(3) . . . . ? C522 Ru2 C322 C422 29.0(3) . . . . ? Br12 Ru2 C322 C422 -115.7(3) . . . . ? Br32 Ru2 C322 C422 -37.4(4) . . . . ? Br22 Ru2 C322 C422 168.4(2) . . . . ? C122 Ru2 C322 C222 -28.8(3) . . . . ? C422 Ru2 C322 C222 -132.3(4) . . . . ? C622 Ru2 C322 C222 -66.1(3) . . . . ? C522 Ru2 C322 C222 -103.3(3) . . . . ? Br12 Ru2 C322 C222 112.0(3) . . . . ? Br32 Ru2 C322 C222 -169.7(2) . . . . ? Br22 Ru2 C322 C222 36.1(4) . . . . ? C122 Ru2 C322 C32A -142.7(5) . . . . ? C222 Ru2 C322 C32A -114.0(6) . . . . ? C422 Ru2 C322 C32A 113.8(6) . . . . ? C622 Ru2 C322 C32A 179.9(5) . . . . ? C522 Ru2 C322 C32A 142.7(5) . . . . ? Br12 Ru2 C322 C32A -2.0(5) . . . . ? Br32 Ru2 C322 C32A 76.4(5) . . . . ? Br22 Ru2 C322 C32A -77.8(5) . . . . ? C422 C322 C32A C32B -86.5(6) . . . . ? C222 C322 C32A C32B 93.4(6) . . . . ? Ru2 C322 C32A C32B -176.5(4) . . . . ? C222 C322 C422 C522 -0.7(8) . . . . ? C32A C322 C422 C522 179.2(5) . . . . ? Ru2 C322 C422 C522 -53.6(4) . . . . ? C222 C322 C422 Ru2 52.9(4) . . . . ? C32A C322 C422 Ru2 -127.2(5) . . . . ? C122 Ru2 C422 C322 -66.6(3) . . . . ? C222 Ru2 C422 C322 -29.3(3) . . . . ? C622 Ru2 C422 C322 -103.6(3) . . . . ? C522 Ru2 C422 C322 -133.1(5) . . . . ? Br12 Ru2 C422 C322 69.6(3) . . . . ? Br32 Ru2 C422 C322 154.7(3) . . . . ? Br22 Ru2 C422 C322 -82.5(11) . . . . ? C122 Ru2 C422 C522 66.4(3) . . . . ? C222 Ru2 C422 C522 103.7(3) . . . . ? C622 Ru2 C422 C522 29.5(3) . . . . ? C322 Ru2 C422 C522 133.1(5) . . . . ? Br12 Ru2 C422 C522 -157.3(3) . . . . ? Br32 Ru2 C422 C522 -72.2(3) . . . . ? Br22 Ru2 C422 C522 50.6(12) . . . . ? C322 C422 C522 C622 0.0(7) . . . . ? Ru2 C422 C522 C622 -53.7(4) . . . . ? C322 C422 C522 C52A -179.7(5) . . . . ? Ru2 C422 C522 C52A 126.5(5) . . . . ? C322 C422 C522 Ru2 53.8(4) . . . . ? C122 Ru2 C522 C622 28.0(3) . . . . ? C222 Ru2 C522 C622 65.5(3) . . . . ? C422 Ru2 C522 C622 131.6(5) . . . . ? C322 Ru2 C522 C622 102.8(3) . . . . ? Br12 Ru2 C522 C622 166.8(2) . . . . ? Br32 Ru2 C522 C622 -115.8(3) . . . . ? Br22 Ru2 C522 C622 -40.0(4) . . . . ? C122 Ru2 C522 C422 -103.6(3) . . . . ? C222 Ru2 C522 C422 -66.1(3) . . . . ? C622 Ru2 C522 C422 -131.6(5) . . . . ? C322 Ru2 C522 C422 -28.8(3) . . . . ? Br12 Ru2 C522 C422 35.2(4) . . . . ? Br32 Ru2 C522 C422 112.5(3) . . . . ? Br22 Ru2 C522 C422 -171.7(2) . . . . ? C122 Ru2 C522 C52A 144.5(5) . . . . ? C222 Ru2 C522 C52A -178.0(5) . . . . ? C422 Ru2 C522 C52A -111.9(6) . . . . ? C622 Ru2 C522 C52A 116.5(6) . . . . ? C322 Ru2 C522 C52A -140.7(5) . . . . ? Br12 Ru2 C522 C52A -76.7(5) . . . . ? Br32 Ru2 C522 C52A 0.7(5) . . . . ? Br22 Ru2 C522 C52A 76.5(5) . . . . ? C622 C522 C52A C52B -96.2(6) . . . . ? C422 C522 C52A C52B 83.5(6) . . . . ? Ru2 C522 C52A C52B 172.0(4) . . . . ? C422 C522 C622 C122 1.2(8) . . . . ? C52A C522 C622 C122 -179.0(5) . . . . ? Ru2 C522 C622 C122 -52.4(5) . . . . ? C422 C522 C622 Ru2 53.6(4) . . . . ? C52A C522 C622 Ru2 -126.6(5) . . . . ? C222 C122 C622 C522 -1.8(8) . . . . ? C12A C122 C622 C522 179.0(5) . . . . ? Ru2 C122 C622 C522 52.6(5) . . . . ? C222 C122 C622 Ru2 -54.3(4) . . . . ? C12A C122 C622 Ru2 126.5(5) . . . . ? C122 Ru2 C622 C522 -134.5(5) . . . . ? C222 Ru2 C622 C522 -104.4(3) . . . . ? C422 Ru2 C622 C522 -29.9(3) . . . . ? C322 Ru2 C622 C522 -67.1(3) . . . . ? Br12 Ru2 C622 C522 -79.8(11) . . . . ? Br32 Ru2 C622 C522 69.3(3) . . . . ? Br22 Ru2 C622 C522 152.9(3) . . . . ? C222 Ru2 C622 C122 30.0(3) . . . . ? C422 Ru2 C622 C122 104.6(3) . . . . ? C522 Ru2 C622 C122 134.5(5) . . . . ? C322 Ru2 C622 C122 67.3(3) . . . . ? Br12 Ru2 C622 C122 54.7(11) . . . . ? Br32 Ru2 C622 C122 -156.2(3) . . . . ? Br22 Ru2 C622 C122 -72.7(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Re1 Re2 3.4619 . . ? Ru1 Ru2 3.3970 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? _kl_archive_SHELXL_comment 'release 97-2' _kl_archive_SHELXL_res ; TITL e094 in P 21/n CELL 0.71073 15.3340 15.1881 17.0439 90.000 91.680 90.000 ZERR 4 0.0011 0.0009 0.0010 0.000 0.008 0.000 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC C H O BR RU RE UNIT 120 144 24 24 8 8 L.S. 14 TEMP -73 ACTA BOND $H CONF FMAP 2 PLAN -25 WGHT 0.030000 FVAR 0.10396 C111 1 0.945258 0.177201 0.807003 11.00000 0.04086 0.02221 = 0.03116 -0.00160 0.00032 -0.00204 O111 3 0.998526 0.190459 0.762254 11.00000 0.05124 0.04728 = 0.05011 0.00252 0.02704 -0.01483 C211 1 0.934860 0.182059 0.964107 11.00000 0.03015 0.02563 = 0.03921 -0.00271 0.00178 0.00128 O211 3 0.982248 0.200091 1.015492 11.00000 0.03541 0.05359 = 0.04355 -0.01389 -0.01493 -0.00091 C311 1 0.895516 0.034575 0.885150 11.00000 0.02445 0.03377 = 0.02888 -0.00351 0.00333 0.00023 O311 3 0.918822 -0.037597 0.889476 11.00000 0.03977 0.03071 = 0.05236 -0.00222 0.00628 0.00832 REM ------------------------------------------------------------------------ RE1 6 0.857340 0.152478 0.879467 11.00000 0.02199 0.02206 = 0.01923 -0.00123 0.00102 -0.00031 REM ------------------------------------------------------------------------ BR11 4 0.784395 0.310176 0.871588 11.00000 0.03504 0.02289 = 0.02966 -0.00061 -0.00183 -0.00120 BR21 4 0.725080 0.120785 0.970497 11.00000 0.03414 0.03561 = 0.02282 0.00639 0.00558 0.00597 BR31 4 0.738045 0.120056 0.769595 11.00000 0.03489 0.03360 = 0.02334 -0.00411 -0.00137 -0.00037 REM ------------------------------------------------------------------------ RE2 6 0.640134 0.213705 0.862550 11.00000 0.02404 0.02074 = 0.02398 0.00231 0.00081 0.00208 REM ------------------------------------------------------------------------ C121 1 0.586762 0.278221 0.778748 11.00000 0.03010 0.03263 = 0.03151 -0.00014 -0.00256 -0.00421 O121 3 0.552071 0.313913 0.727858 11.00000 0.04658 0.05424 = 0.04716 0.02079 -0.01943 0.00276 C221 1 0.542015 0.137066 0.856293 11.00000 0.04052 0.02505 = 0.04352 0.00294 0.00380 0.00488 O221 3 0.480824 0.094786 0.851332 11.00000 0.04003 0.03462 = 0.10409 -0.00426 0.00226 -0.01431 C321 1 0.580681 0.281021 0.937454 11.00000 0.03978 0.02574 = 0.03359 0.00600 0.00625 -0.00126 O321 3 0.543990 0.319139 0.985211 11.00000 0.07015 0.03530 = 0.05890 -0.00606 0.03435 0.01157 REM ------------------------------------------------------------------------ REM ------------------------------------------------------------------------ C112 1 0.762213 0.241848 0.569523 11.00000 0.01997 0.02491 = 0.01439 -0.00233 0.00073 0.00005 C11A 1 0.775315 0.339015 0.569498 11.00000 0.03017 0.02241 = 0.02845 -0.00165 -0.00150 0.00316 AFIX 23 H11A 2 0.723306 0.368206 0.545549 11.00000 -1.20000 H11B 2 0.826330 0.354008 0.537818 11.00000 -1.20000 AFIX 0 C11B 1 0.790234 0.371878 0.653395 11.00000 0.04551 0.02814 = 0.03106 -0.01175 0.00352 -0.00544 AFIX 137 H11C 2 0.740699 0.354826 0.685117 11.00000 -1.50000 H11D 2 0.795734 0.436162 0.653199 11.00000 -1.50000 H11E 2 0.843852 0.345757 0.675768 11.00000 -1.50000 AFIX 0 C212 1 0.835706 0.183424 0.570586 11.00000 0.01745 0.02418 = 0.01544 -0.00232 -0.00294 -0.00065 AFIX 43 H212 2 0.893051 0.207155 0.572458 11.00000 -1.20000 AFIX 0 C312 1 0.824262 0.091600 0.568903 11.00000 0.03065 0.02203 = 0.01691 0.00315 0.00250 0.00166 C31A 1 0.901805 0.030150 0.568604 11.00000 0.03049 0.02872 = 0.03992 0.00412 0.00686 0.00989 AFIX 23 H31A 2 0.952949 0.061521 0.548111 11.00000 -1.20000 H31B 2 0.888656 -0.020494 0.533654 11.00000 -1.20000 AFIX 0 C31B 1 0.922897 -0.002700 0.650879 11.00000 0.04348 0.03786 = 0.04111 -0.00347 -0.01234 0.01556 AFIX 137 H31C 2 0.939226 0.047202 0.684670 11.00000 -1.50000 H31D 2 0.971529 -0.044485 0.649511 11.00000 -1.50000 H31E 2 0.871587 -0.032077 0.671697 11.00000 -1.50000 AFIX 0 C412 1 0.738533 0.056723 0.566706 11.00000 0.03457 0.02112 = 0.01833 0.00010 0.00397 -0.00520 AFIX 43 H412 2 0.730681 -0.005314 0.565596 11.00000 -1.20000 AFIX 0 C512 1 0.664945 0.111671 0.566132 11.00000 0.02454 0.03165 = 0.01350 -0.00267 0.00405 -0.00528 C51A 1 0.574965 0.073046 0.563976 11.00000 0.02301 0.05208 = 0.02972 -0.00214 0.00051 -0.01269 AFIX 23 H51A 2 0.575272 0.016511 0.535075 11.00000 -1.20000 H51B 2 0.534359 0.113594 0.535796 11.00000 -1.20000 AFIX 0 C51B 1 0.543790 0.057728 0.646146 11.00000 0.02996 0.08759 = 0.04025 0.00744 0.00473 -0.02987 AFIX 137 H51C 2 0.585468 0.019829 0.674826 11.00000 -1.50000 H51D 2 0.486486 0.029136 0.643510 11.00000 -1.50000 H51E 2 0.539197 0.114284 0.673394 11.00000 -1.50000 AFIX 0 C612 1 0.677470 0.204565 0.568011 11.00000 0.02202 0.02804 = 0.01754 -0.00479 0.00111 0.00114 AFIX 43 H612 2 0.628048 0.242272 0.568255 11.00000 -1.20000 AFIX 0 REM ------------------------------------------------------------------------ RU1 5 0.749224 0.150051 0.471282 11.00000 0.02027 0.01905 = 0.01477 -0.00135 0.00206 -0.00171 REM ------------------------------------------------------------------------ BR12 4 0.623681 0.134859 0.370557 11.00000 0.02448 0.06989 = 0.02104 0.00164 0.00107 -0.00269 BR22 4 0.795937 0.266378 0.371673 11.00000 0.08381 0.03164 = 0.01903 -0.00281 0.00593 -0.02760 BR32 4 0.825179 0.051502 0.372792 11.00000 0.04706 0.04932 = 0.02315 -0.00483 0.00087 0.01949 REM ------------------------------------------------------------------------ RU2 5 0.745126 0.149020 0.271902 11.00000 0.02201 0.02120 = 0.01487 -0.00204 0.00214 -0.00225 REM ------------------------------------------------------------------------ C122 1 0.774751 0.234953 0.174178 11.00000 0.03072 0.02618 = 0.01641 -0.00046 0.00096 -0.00491 C12A 1 0.807945 0.327939 0.173562 11.00000 0.04245 0.03057 = 0.02503 -0.00008 0.00113 -0.01016 AFIX 23 H12A 2 0.865308 0.330965 0.201637 11.00000 -1.20000 H12B 2 0.766906 0.366780 0.201008 11.00000 -1.20000 AFIX 0 C12B 1 0.817075 0.359364 0.088801 11.00000 0.06514 0.03265 = 0.03309 0.00863 0.01144 -0.00937 AFIX 137 H12C 2 0.860526 0.323118 0.062817 11.00000 -1.50000 H12D 2 0.835831 0.421047 0.088769 11.00000 -1.50000 H12E 2 0.760711 0.354032 0.060588 11.00000 -1.50000 AFIX 0 C222 1 0.683457 0.218409 0.173347 11.00000 0.02658 0.02332 = 0.01966 -0.00090 -0.00131 0.00250 AFIX 43 H222 2 0.643773 0.266456 0.172171 11.00000 -1.20000 AFIX 0 C322 1 0.650868 0.130734 0.174256 11.00000 0.02421 0.02824 = 0.01624 -0.00520 -0.00192 -0.00208 C32A 1 0.554526 0.113610 0.173083 11.00000 0.02323 0.03309 = 0.03263 -0.00537 0.00377 0.00130 AFIX 23 H32A 2 0.524045 0.164020 0.196868 11.00000 -1.20000 H32B 2 0.542264 0.060336 0.204359 11.00000 -1.20000 AFIX 0 C32B 1 0.521258 0.100583 0.089134 11.00000 0.02703 0.05474 = 0.04163 0.01061 -0.01017 -0.00568 AFIX 137 H32C 2 0.521256 0.157191 0.061538 11.00000 -1.50000 H32D 2 0.461740 0.077082 0.089220 11.00000 -1.50000 H32E 2 0.559297 0.059066 0.062440 11.00000 -1.50000 AFIX 0 C422 1 0.710835 0.059551 0.176191 11.00000 0.02644 0.02058 = 0.02003 -0.00614 0.00067 -0.00166 AFIX 43 H422 2 0.689639 0.000806 0.177397 11.00000 -1.20000 AFIX 0 C522 1 0.802637 0.075187 0.176346 11.00000 0.02792 0.03092 = 0.01093 -0.00260 0.00208 0.00001 C52A 1 0.863293 -0.001727 0.178065 11.00000 0.03059 0.03983 = 0.02642 -0.00547 0.00252 0.00869 AFIX 23 H52A 2 0.839833 -0.048675 0.211776 11.00000 -1.20000 H52B 2 0.920882 0.016393 0.200346 11.00000 -1.20000 AFIX 0 C52B 1 0.873462 -0.036432 0.095288 11.00000 0.04039 0.05126 = 0.03351 -0.01879 -0.00310 0.01945 AFIX 137 H52C 2 0.816050 -0.052335 0.072806 11.00000 -1.50000 H52D 2 0.911161 -0.088544 0.096749 11.00000 -1.50000 H52E 2 0.899737 0.009184 0.062884 11.00000 -1.50000 AFIX 0 C622 1 0.832941 0.162865 0.174568 11.00000 0.02222 0.03995 = 0.01406 -0.00167 0.00531 -0.00474 AFIX 43 H622 2 0.893925 0.173660 0.173610 11.00000 -1.20000 HKLF 4 END ; _kl_archive_SCHAKAL_comment 'release 99 for Win32 systems' _kl_archive_SCHAKAL_dat ? _kl_archive_ORTEP_comment ? _kl_archive_ORTEP_ins ? _kl_archive_rtf_text ? data_e117 _publ_contact_author_name 'Dr. Kay Severin' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7768' _publ_author_name 'da Silva, Ana C.' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Heterometallic bromo-bridged complexes with Re(CO)3 fragments ; _audit_author_name 'Piotrowski, H.' _audit_block_code Re_Rh_(CO)3_C10H15_Br3_e117_beck _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 16-May-00 _chemical_name_systematic ; ; _chemical_compound_source ; ; _chemical_name_common cp(Me)5-Rh-Br3-Re-(CO)3 _chemical_formula_moiety 'Re1, Rh1, Br3, (C O)3, (C10 H15)' _chemical_formula_sum 'C13 H15 Br3 O3 Re Rh' _chemical_formula_weight 748.081 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' 'O' 'O' 0.0106 0.0060 '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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' _symmetry_Int_Tables_number 14 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 9.6576(8) _cell_length_b 14.8986(17) _cell_length_c 12.3070(10) _cell_angle_alpha 90 _cell_angle_beta 90.434(10) _cell_angle_gamma 90 _cell_volume 1770.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.0 _cell_special_details ; Monoclinic P (as derived from metrics), pseudo-orthorhombic ; _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.8062(5) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 14.535 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1416 _exptl_absorpt_correction_T_max 0.5046 _exptl_absorpt_process_details 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' _exptl_special_details ; crystal embedded in oil and fixed with Lithelen ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -2 1 0.0250 0 2 1 0.0310 0 -2 -1 0.0290 0 2 -1 0.0430 3 -2 3 0.0780 -3 2 -3 0.1040 _diffrn_ambient_temperature 200(3) _diffrn_source_type 'Spellman DF4 Series' _diffrn_source_power 2.75_kW _diffrn_source_voltage 55_kV _diffrn_source_current 50_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 200.2 _kl_diffrn_detector_area_phi_incr 1.4 _kl_diffrn_detector_area_expos_time 4.00_min _kl_diffrn_detector_area_plate_dist 60.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.008 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 21 _diffrn_special_details ; no crystal decay in terms of mean intensity per image ; _diffrn_reflns_number 16749 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.07 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.788 _refine_diff_density_min -2.038 _refine_diff_density_rms 0.262 _reflns_number_total 4233 _reflns_number_gt 3398 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution ; SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79) ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4233 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ; details of H atom refinement: riding with U(H)=1.5*U(C) for CH3 ; 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 Rh Rh 0.36359(3) 0.18159(2) 0.24854(3) 0.01256(8) Uani 1 1 d . . . Re Re 0.620793(19) 0.027393(13) 0.240005(16) 0.01696(6) Uani 1 1 d . . . Br1 Br 0.62718(5) 0.20356(3) 0.26776(4) 0.02128(11) Uani 1 1 d . . . Br2 Br 0.42932(5) 0.07384(4) 0.09744(4) 0.02618(12) Uani 1 1 d . . . Br3 Br 0.41038(6) 0.04652(4) 0.37318(5) 0.03214(14) Uani 1 1 d . . . O1 O 0.8545(4) 0.0220(3) 0.0757(3) 0.0317(9) Uani 1 1 d . . . C1 C 0.7648(5) 0.0251(4) 0.1365(4) 0.0208(10) Uani 1 1 d . . . O2 O 0.8359(4) -0.0265(3) 0.4101(3) 0.0341(10) Uani 1 1 d . . . C2 C 0.7521(5) -0.0043(4) 0.3483(4) 0.0236(11) Uani 1 1 d . . . O3 O 0.5755(5) -0.1709(3) 0.1954(6) 0.0618(17) Uani 1 1 d . . . C3 C 0.5915(6) -0.0967(4) 0.2126(6) 0.0335(14) Uani 1 1 d . . . C4 C 0.3049(5) 0.3182(3) 0.2827(4) 0.0164(9) Uani 1 1 d . . . C5 C 0.2257(5) 0.2572(3) 0.3482(4) 0.0151(9) Uani 1 1 d . . . C6 C 0.1489(5) 0.1999(3) 0.2774(4) 0.0171(10) Uani 1 1 d . . . C7 C 0.2775(5) 0.2962(3) 0.1701(4) 0.0172(10) Uani 1 1 d . . . C8 C 0.1778(5) 0.2248(3) 0.1679(4) 0.0193(10) Uani 1 1 d . . . C9 C 0.3952(6) 0.3925(3) 0.3216(5) 0.0249(11) Uani 1 1 d . . . H9A H 0.4374 0.4225 0.2592 0.037 Uiso 1 1 calc R . . H9B H 0.4681 0.3682 0.3690 0.037 Uiso 1 1 calc R . . H9C H 0.3396 0.4358 0.3623 0.037 Uiso 1 1 calc R . . C10 C 0.2179(6) 0.2586(4) 0.4696(4) 0.0267(12) Uani 1 1 d . . . H10A H 0.1563 0.2106 0.4942 0.040 Uiso 1 1 calc R . . H10B H 0.1817 0.3168 0.4935 0.040 Uiso 1 1 calc R . . H10C H 0.3106 0.2495 0.5005 0.040 Uiso 1 1 calc R . . C11 C 0.0487(5) 0.1291(3) 0.3117(5) 0.0253(12) Uani 1 1 d . . . H11A H 0.0129 0.0978 0.2473 0.038 Uiso 1 1 calc R . . H11B H -0.0283 0.1571 0.3505 0.038 Uiso 1 1 calc R . . H11C H 0.0957 0.0861 0.3596 0.038 Uiso 1 1 calc R . . C12 C 0.1139(6) 0.1865(4) 0.0673(5) 0.0309(12) Uani 1 1 d . . . H12A H 0.0477 0.1396 0.0871 0.046 Uiso 1 1 calc R . . H12B H 0.1864 0.1608 0.0215 0.046 Uiso 1 1 calc R . . H12C H 0.0656 0.2341 0.0272 0.046 Uiso 1 1 calc R . . C13 C 0.3358(7) 0.3436(4) 0.0734(4) 0.0326(14) Uani 1 1 d . . . H13A H 0.4031 0.3887 0.0977 0.049 Uiso 1 1 calc R . . H13B H 0.2607 0.3731 0.0330 0.049 Uiso 1 1 calc R . . H13C H 0.3817 0.2999 0.0262 0.049 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 Rh 0.01132(16) 0.01220(17) 0.01418(16) -0.00043(12) 0.00175(13) 0.00082(13) Re 0.01212(9) 0.01378(9) 0.02501(10) 0.00112(8) 0.00271(7) 0.00094(8) Br1 0.0155(2) 0.0181(2) 0.0302(3) -0.00491(19) -0.0017(2) -0.00179(19) Br2 0.0213(2) 0.0296(3) 0.0276(3) -0.0140(2) -0.0042(2) 0.0069(2) Br3 0.0247(3) 0.0339(3) 0.0380(3) 0.0219(2) 0.0155(2) 0.0113(2) O1 0.027(2) 0.038(2) 0.030(2) -0.0022(18) 0.0091(17) 0.0049(18) C1 0.015(2) 0.020(3) 0.027(2) -0.003(2) 0.001(2) 0.002(2) O2 0.031(2) 0.041(3) 0.030(2) 0.0088(19) -0.0010(18) 0.010(2) C2 0.021(3) 0.023(3) 0.027(3) 0.004(2) 0.008(2) 0.002(2) O3 0.029(2) 0.018(2) 0.138(5) -0.006(3) -0.007(3) -0.0063(19) C3 0.016(2) 0.026(3) 0.059(4) -0.001(3) -0.002(3) 0.001(2) C4 0.016(2) 0.011(2) 0.022(2) -0.0019(18) 0.0015(19) 0.0004(18) C5 0.013(2) 0.016(2) 0.016(2) -0.0006(18) 0.0033(18) 0.0047(18) C6 0.011(2) 0.016(2) 0.024(2) -0.0020(18) 0.0016(19) 0.0037(18) C7 0.018(2) 0.012(2) 0.021(2) 0.0025(18) 0.0031(19) 0.0066(18) C8 0.015(2) 0.021(2) 0.022(2) -0.0039(19) -0.0019(19) 0.0071(19) C9 0.025(3) 0.017(3) 0.032(3) -0.005(2) 0.002(2) -0.005(2) C10 0.028(3) 0.034(3) 0.019(2) -0.005(2) 0.006(2) 0.002(2) C11 0.019(2) 0.015(2) 0.043(3) 0.001(2) 0.007(2) 0.000(2) C12 0.028(3) 0.035(3) 0.029(3) -0.008(2) -0.012(2) 0.004(3) C13 0.042(3) 0.029(3) 0.027(3) 0.012(2) 0.009(3) 0.009(3) 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 Rh C6 2.124(4) . ? Rh C7 2.128(5) . ? Rh C5 2.139(4) . ? Rh C8 2.143(5) . ? Rh C4 2.154(5) . ? Rh Br2 2.5408(6) . ? Rh Br3 2.5684(7) . ? Rh Br1 2.5757(6) . ? Re C2 1.892(6) . ? Re C1 1.893(4) . ? Re C3 1.900(6) . ? Re Br2 2.6321(7) . ? Re Br3 2.6358(6) . ? Re Br1 2.6474(6) . ? O1 C1 1.150(6) . ? O2 C2 1.155(7) . ? O3 C3 1.136(7) . ? C4 C5 1.439(6) . ? C4 C7 1.447(7) . ? C4 C9 1.486(7) . ? C5 C6 1.425(7) . ? C5 C10 1.496(6) . ? C6 C8 1.427(7) . ? C6 C11 1.494(7) . ? C7 C8 1.435(7) . ? C7 C13 1.496(6) . ? C8 C12 1.493(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 C6 Rh C7 66.05(18) . . ? C6 Rh C5 39.06(19) . . ? C7 Rh C5 66.09(17) . . ? C6 Rh C8 39.08(18) . . ? C7 Rh C8 39.25(19) . . ? C5 Rh C8 65.45(18) . . ? C6 Rh C4 65.65(18) . . ? C7 Rh C4 39.48(18) . . ? C5 Rh C4 39.16(17) . . ? C8 Rh C4 65.54(19) . . ? C6 Rh Br2 116.93(14) . . ? C7 Rh Br2 105.90(13) . . ? C5 Rh Br2 155.91(14) . . ? C8 Rh Br2 93.66(13) . . ? C4 Rh Br2 143.81(13) . . ? C6 Rh Br3 99.69(13) . . ? C7 Rh Br3 165.06(11) . . ? C5 Rh Br3 100.23(12) . . ? C8 Rh Br3 130.93(14) . . ? C4 Rh Br3 131.97(13) . . ? Br2 Rh Br3 84.16(2) . . ? C6 Rh Br1 159.04(14) . . ? C7 Rh Br1 108.80(13) . . ? C5 Rh Br1 119.98(14) . . ? C8 Rh Br1 145.87(14) . . ? C4 Rh Br1 97.08(13) . . ? Br2 Rh Br1 83.99(2) . . ? Br3 Rh Br1 82.84(2) . . ? C2 Re C1 88.7(2) . . ? C2 Re C3 88.9(3) . . ? C1 Re C3 88.4(2) . . ? C2 Re Br2 177.02(14) . . ? C1 Re Br2 94.14(16) . . ? C3 Re Br2 92.0(2) . . ? C2 Re Br3 95.99(14) . . ? C1 Re Br3 173.73(16) . . ? C3 Re Br3 95.81(17) . . ? Br2 Re Br3 81.084(19) . . ? C2 Re Br1 98.12(17) . . ? C1 Re Br1 95.08(16) . . ? C3 Re Br1 172.24(18) . . ? Br2 Re Br1 80.846(18) . . ? Br3 Re Br1 80.208(17) . . ? Rh Br1 Re 80.802(16) . . ? Rh Br2 Re 81.743(19) . . ? Rh Br3 Re 81.157(16) . . ? O1 C1 Re 177.9(5) . . ? O2 C2 Re 176.1(5) . . ? O3 C3 Re 179.1(6) . . ? C5 C4 C7 107.5(4) . . ? C5 C4 C9 127.1(4) . . ? C7 C4 C9 125.4(4) . . ? C5 C4 Rh 69.8(3) . . ? C7 C4 Rh 69.3(3) . . ? C9 C4 Rh 127.7(4) . . ? C6 C5 C4 108.2(4) . . ? C6 C5 C10 126.1(4) . . ? C4 C5 C10 125.6(5) . . ? C6 C5 Rh 69.9(2) . . ? C4 C5 Rh 71.0(2) . . ? C10 C5 Rh 128.1(4) . . ? C5 C6 C8 108.5(4) . . ? C5 C6 C11 125.8(4) . . ? C8 C6 C11 125.6(5) . . ? C5 C6 Rh 71.0(2) . . ? C8 C6 Rh 71.2(3) . . ? C11 C6 Rh 126.3(3) . . ? C8 C7 C4 107.7(4) . . ? C8 C7 C13 126.2(5) . . ? C4 C7 C13 126.0(5) . . ? C8 C7 Rh 70.9(3) . . ? C4 C7 Rh 71.2(3) . . ? C13 C7 Rh 126.2(3) . . ? C6 C8 C7 108.2(4) . . ? C6 C8 C12 126.9(5) . . ? C7 C8 C12 124.9(5) . . ? C6 C8 Rh 69.7(3) . . ? C7 C8 Rh 69.8(3) . . ? C12 C8 Rh 127.5(4) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 C6 Rh Br1 Re 141.5(4) . . . . ? C7 Rh Br1 Re -146.58(13) . . . . ? C5 Rh Br1 Re 140.75(14) . . . . ? C8 Rh Br1 Re -129.5(2) . . . . ? C4 Rh Br1 Re 174.62(13) . . . . ? Br2 Rh Br1 Re -41.801(18) . . . . ? Br3 Rh Br1 Re 43.043(18) . . . . ? C2 Re Br1 Rh -136.77(14) . . . . ? C1 Re Br1 Rh 133.79(16) . . . . ? C3 Re Br1 Rh 17.6(14) . . . . ? Br2 Re Br1 Rh 40.403(17) . . . . ? Br3 Re Br1 Rh -42.041(19) . . . . ? C6 Rh Br2 Re -139.35(15) . . . . ? C7 Rh Br2 Re 149.84(14) . . . . ? C5 Rh Br2 Re -143.5(3) . . . . ? C8 Rh Br2 Re -172.21(14) . . . . ? C4 Rh Br2 Re 135.8(2) . . . . ? Br3 Rh Br2 Re -41.418(19) . . . . ? Br1 Rh Br2 Re 41.969(17) . . . . ? C2 Re Br2 Rh 29(3) . . . . ? C1 Re Br2 Rh -135.44(16) . . . . ? C3 Re Br2 Rh 136.05(17) . . . . ? Br3 Re Br2 Rh 40.476(19) . . . . ? Br1 Re Br2 Rh -40.949(17) . . . . ? C6 Rh Br3 Re 157.81(14) . . . . ? C7 Rh Br3 Re 174.6(6) . . . . ? C5 Rh Br3 Re -162.51(14) . . . . ? C8 Rh Br3 Re 131.21(16) . . . . ? C4 Rh Br3 Re -136.33(17) . . . . ? Br2 Rh Br3 Re 41.424(19) . . . . ? Br1 Rh Br3 Re -43.225(18) . . . . ? C2 Re Br3 Rh 139.38(17) . . . . ? C1 Re Br3 Rh 0.6(15) . . . . ? C3 Re Br3 Rh -131.1(2) . . . . ? Br2 Re Br3 Rh -40.03(2) . . . . ? Br1 Re Br3 Rh 42.137(19) . . . . ? C2 Re C1 O1 21(14) . . . . ? C3 Re C1 O1 -68(14) . . . . ? Br2 Re C1 O1 -160(14) . . . . ? Br3 Re C1 O1 160(12) . . . . ? Br1 Re C1 O1 119(14) . . . . ? C1 Re C2 O2 -35(7) . . . . ? C3 Re C2 O2 54(7) . . . . ? Br2 Re C2 O2 161(5) . . . . ? Br3 Re C2 O2 150(7) . . . . ? Br1 Re C2 O2 -129(7) . . . . ? C2 Re C3 O3 -83(49) . . . . ? C1 Re C3 O3 6(49) . . . . ? Br2 Re C3 O3 100(49) . . . . ? Br3 Re C3 O3 -179(100) . . . . ? Br1 Re C3 O3 123(48) . . . . ? C6 Rh C4 C5 37.5(3) . . . . ? C7 Rh C4 C5 118.8(4) . . . . ? C8 Rh C4 C5 80.5(3) . . . . ? Br2 Rh C4 C5 140.4(2) . . . . ? Br3 Rh C4 C5 -43.4(3) . . . . ? Br1 Rh C4 C5 -130.2(3) . . . . ? C6 Rh C4 C7 -81.3(3) . . . . ? C5 Rh C4 C7 -118.8(4) . . . . ? C8 Rh C4 C7 -38.2(3) . . . . ? Br2 Rh C4 C7 21.6(4) . . . . ? Br3 Rh C4 C7 -162.2(2) . . . . ? Br1 Rh C4 C7 111.1(2) . . . . ? C6 Rh C4 C9 159.3(5) . . . . ? C7 Rh C4 C9 -119.4(5) . . . . ? C5 Rh C4 C9 121.8(6) . . . . ? C8 Rh C4 C9 -157.6(5) . . . . ? Br2 Rh C4 C9 -97.8(5) . . . . ? Br3 Rh C4 C9 78.4(4) . . . . ? Br1 Rh C4 C9 -8.3(4) . . . . ? C7 C4 C5 C6 -1.0(5) . . . . ? C9 C4 C5 C6 177.0(5) . . . . ? Rh C4 C5 C6 -60.3(3) . . . . ? C7 C4 C5 C10 -177.0(4) . . . . ? C9 C4 C5 C10 1.1(8) . . . . ? Rh C4 C5 C10 123.8(5) . . . . ? C7 C4 C5 Rh 59.3(3) . . . . ? C9 C4 C5 Rh -122.7(5) . . . . ? C7 Rh C5 C6 80.9(3) . . . . ? C8 Rh C5 C6 37.7(3) . . . . ? C4 Rh C5 C6 118.5(4) . . . . ? Br2 Rh C5 C6 5.8(5) . . . . ? Br3 Rh C5 C6 -92.8(3) . . . . ? Br1 Rh C5 C6 179.6(2) . . . . ? C6 Rh C5 C4 -118.5(4) . . . . ? C7 Rh C5 C4 -37.6(3) . . . . ? C8 Rh C5 C4 -80.8(3) . . . . ? Br2 Rh C5 C4 -112.6(3) . . . . ? Br3 Rh C5 C4 148.7(3) . . . . ? Br1 Rh C5 C4 61.1(3) . . . . ? C6 Rh C5 C10 120.7(6) . . . . ? C7 Rh C5 C10 -158.4(5) . . . . ? C8 Rh C5 C10 158.4(5) . . . . ? C4 Rh C5 C10 -120.8(6) . . . . ? Br2 Rh C5 C10 126.6(4) . . . . ? Br3 Rh C5 C10 27.9(5) . . . . ? Br1 Rh C5 C10 -59.7(5) . . . . ? C4 C5 C6 C8 -0.6(5) . . . . ? C10 C5 C6 C8 175.2(5) . . . . ? Rh C5 C6 C8 -61.7(3) . . . . ? C4 C5 C6 C11 -177.4(4) . . . . ? C10 C5 C6 C11 -1.5(8) . . . . ? Rh C5 C6 C11 121.6(5) . . . . ? C4 C5 C6 Rh 61.0(3) . . . . ? C10 C5 C6 Rh -123.1(5) . . . . ? C7 Rh C6 C5 -81.0(3) . . . . ? C8 Rh C6 C5 -118.1(4) . . . . ? C4 Rh C6 C5 -37.5(3) . . . . ? Br2 Rh C6 C5 -177.3(2) . . . . ? Br3 Rh C6 C5 94.3(3) . . . . ? Br1 Rh C6 C5 -1.0(6) . . . . ? C7 Rh C6 C8 37.1(3) . . . . ? C5 Rh C6 C8 118.1(4) . . . . ? C4 Rh C6 C8 80.6(3) . . . . ? Br2 Rh C6 C8 -59.2(3) . . . . ? Br3 Rh C6 C8 -147.6(3) . . . . ? Br1 Rh C6 C8 117.1(4) . . . . ? C7 Rh C6 C11 158.0(5) . . . . ? C5 Rh C6 C11 -121.0(6) . . . . ? C8 Rh C6 C11 120.9(6) . . . . ? C4 Rh C6 C11 -158.5(5) . . . . ? Br2 Rh C6 C11 61.7(5) . . . . ? Br3 Rh C6 C11 -26.7(5) . . . . ? Br1 Rh C6 C11 -122.0(4) . . . . ? C5 C4 C7 C8 2.3(5) . . . . ? C9 C4 C7 C8 -175.8(5) . . . . ? Rh C4 C7 C8 61.9(3) . . . . ? C5 C4 C7 C13 178.7(5) . . . . ? C9 C4 C7 C13 0.7(8) . . . . ? Rh C4 C7 C13 -121.6(5) . . . . ? C5 C4 C7 Rh -59.6(3) . . . . ? C9 C4 C7 Rh 122.3(5) . . . . ? C6 Rh C7 C8 -37.0(3) . . . . ? C5 Rh C7 C8 -79.9(3) . . . . ? C4 Rh C7 C8 -117.2(4) . . . . ? Br2 Rh C7 C8 75.9(2) . . . . ? Br3 Rh C7 C8 -55.2(7) . . . . ? Br1 Rh C7 C8 164.9(2) . . . . ? C6 Rh C7 C4 80.2(3) . . . . ? C5 Rh C7 C4 37.3(3) . . . . ? C8 Rh C7 C4 117.2(4) . . . . ? Br2 Rh C7 C4 -166.9(2) . . . . ? Br3 Rh C7 C4 62.0(7) . . . . ? Br1 Rh C7 C4 -78.0(2) . . . . ? C6 Rh C7 C13 -158.4(5) . . . . ? C5 Rh C7 C13 158.7(5) . . . . ? C8 Rh C7 C13 -121.4(6) . . . . ? C4 Rh C7 C13 121.4(6) . . . . ? Br2 Rh C7 C13 -45.5(5) . . . . ? Br3 Rh C7 C13 -176.6(4) . . . . ? Br1 Rh C7 C13 43.4(5) . . . . ? C5 C6 C8 C7 2.1(5) . . . . ? C11 C6 C8 C7 178.9(4) . . . . ? Rh C6 C8 C7 -59.5(3) . . . . ? C5 C6 C8 C12 -176.1(5) . . . . ? C11 C6 C8 C12 0.6(8) . . . . ? Rh C6 C8 C12 122.3(5) . . . . ? C5 C6 C8 Rh 61.6(3) . . . . ? C11 C6 C8 Rh -121.7(5) . . . . ? C4 C7 C8 C6 -2.7(5) . . . . ? C13 C7 C8 C6 -179.1(5) . . . . ? Rh C7 C8 C6 59.4(3) . . . . ? C4 C7 C8 C12 175.5(5) . . . . ? C13 C7 C8 C12 -0.9(8) . . . . ? Rh C7 C8 C12 -122.3(5) . . . . ? C4 C7 C8 Rh -62.1(3) . . . . ? C13 C7 C8 Rh 121.4(5) . . . . ? C7 Rh C8 C6 -119.3(4) . . . . ? C5 Rh C8 C6 -37.7(3) . . . . ? C4 Rh C8 C6 -80.9(3) . . . . ? Br2 Rh C8 C6 129.9(3) . . . . ? Br3 Rh C8 C6 44.4(3) . . . . ? Br1 Rh C8 C6 -145.4(2) . . . . ? C6 Rh C8 C7 119.3(4) . . . . ? C5 Rh C8 C7 81.6(3) . . . . ? C4 Rh C8 C7 38.4(3) . . . . ? Br2 Rh C8 C7 -110.8(2) . . . . ? Br3 Rh C8 C7 163.7(2) . . . . ? Br1 Rh C8 C7 -26.1(4) . . . . ? C6 Rh C8 C12 -121.6(6) . . . . ? C7 Rh C8 C12 119.1(6) . . . . ? C5 Rh C8 C12 -159.2(5) . . . . ? C4 Rh C8 C12 157.5(5) . . . . ? Br2 Rh C8 C12 8.3(5) . . . . ? Br3 Rh C8 C12 -77.2(5) . . . . ? Br1 Rh C8 C12 93.0(5) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Re Rh 3.386 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? _kl_archive_SHELXL_comment 'release 97-2' _kl_archive_SHELXL_res ; TITL e117 in P21/n CELL 0.71073 9.6576 14.8986 12.3070 90.000 90.434 90.000 ZERR 4 0.0008 0.0017 0.0010 0.000 0.010 0.000 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC C H O BR RE RH UNIT 52 60 12 12 4 4 L.S. 12 FMAP 2 PLAN -25 TEMP -73 BOND $H CONF ACTA WGHT 0.027300 FVAR 0.19723 RH 6 0.363593 0.181593 0.248537 11.00000 0.01132 0.01220 = 0.01418 -0.00043 0.00175 0.00082 RE 5 0.620793 0.027393 0.240005 11.00000 0.01212 0.01378 = 0.02501 0.00112 0.00271 0.00094 BR1 4 0.627181 0.203557 0.267758 11.00000 0.01546 0.01812 = 0.03023 -0.00491 -0.00172 -0.00179 BR2 4 0.429317 0.073841 0.097440 11.00000 0.02131 0.02958 = 0.02757 -0.01401 -0.00419 0.00691 BR3 4 0.410377 0.046517 0.373182 11.00000 0.02472 0.03391 = 0.03803 0.02186 0.01554 0.01132 O1 3 0.854509 0.022002 0.075725 11.00000 0.02687 0.03789 = 0.03039 -0.00219 0.00915 0.00488 C1 1 0.764765 0.025058 0.136487 11.00000 0.01501 0.02039 = 0.02696 -0.00332 0.00149 0.00164 O2 3 0.835944 -0.026454 0.410065 11.00000 0.03106 0.04121 = 0.02998 0.00881 -0.00103 0.00969 C2 1 0.752058 -0.004254 0.348323 11.00000 0.02108 0.02284 = 0.02712 0.00445 0.00793 0.00166 O3 3 0.575494 -0.170894 0.195402 11.00000 0.02926 0.01790 = 0.13802 -0.00622 -0.00693 -0.00632 C3 1 0.591538 -0.096687 0.212609 11.00000 0.01553 0.02617 = 0.05864 -0.00126 -0.00170 0.00132 C4 1 0.304917 0.318163 0.282700 11.00000 0.01618 0.01110 = 0.02188 -0.00188 0.00150 0.00045 C5 1 0.225690 0.257210 0.348241 11.00000 0.01282 0.01610 = 0.01639 -0.00057 0.00330 0.00469 C6 1 0.148900 0.199890 0.277350 11.00000 0.01101 0.01578 = 0.02443 -0.00201 0.00161 0.00367 C7 1 0.277481 0.296241 0.170062 11.00000 0.01795 0.01238 = 0.02144 0.00254 0.00314 0.00664 C8 1 0.177832 0.224839 0.167886 11.00000 0.01497 0.02101 = 0.02176 -0.00394 -0.00190 0.00713 C9 1 0.395171 0.392499 0.321636 11.00000 0.02535 0.01711 = 0.03223 -0.00544 0.00242 -0.00501 AFIX 33 H9A 2 0.437406 0.422469 0.259228 11.00000 -1.50000 H9B 2 0.468057 0.368197 0.369019 11.00000 -1.50000 H9C 2 0.339551 0.435840 0.362332 11.00000 -1.50000 AFIX 0 C10 1 0.217890 0.258644 0.469563 11.00000 0.02752 0.03393 = 0.01883 -0.00535 0.00576 0.00164 AFIX 33 H10A 2 0.156274 0.210623 0.494169 11.00000 -1.50000 H10B 2 0.181680 0.316766 0.493488 11.00000 -1.50000 H10C 2 0.310607 0.249482 0.500521 11.00000 -1.50000 AFIX 0 C11 1 0.048705 0.129136 0.311655 11.00000 0.01896 0.01452 = 0.04254 0.00084 0.00684 -0.00005 AFIX 33 H11A 2 0.012950 0.097757 0.247328 11.00000 -1.50000 H11B 2 -0.028259 0.157097 0.350538 11.00000 -1.50000 H11C 2 0.095700 0.086143 0.359600 11.00000 -1.50000 AFIX 0 C12 1 0.113876 0.186540 0.067287 11.00000 0.02819 0.03518 = 0.02918 -0.00769 -0.01241 0.00362 AFIX 33 H12A 2 0.047686 0.139555 0.087092 11.00000 -1.50000 H12B 2 0.186365 0.160781 0.021535 11.00000 -1.50000 H12C 2 0.065590 0.234140 0.027191 11.00000 -1.50000 AFIX 0 C13 1 0.335759 0.343551 0.073390 11.00000 0.04208 0.02881 = 0.02698 0.01188 0.00902 0.00852 AFIX 33 H13A 2 0.403061 0.388661 0.097656 11.00000 -1.50000 H13B 2 0.260695 0.373054 0.032998 11.00000 -1.50000 H13C 2 0.381687 0.299920 0.026206 11.00000 -1.50000 HKLF 4 REM e117 in P21/n REM R1 = 0.0257 for 3398 Fo > 4sig(Fo) and 0.0374 for all 4233 data REM 190 parameters refined using 0 restraints END ; _kl_archive_SCHAKAL_comment ? _kl_archive_SCHAKAL_dat ? _kl_archive_ORTEP_comment ? _kl_archive_ORTEP_ins ? _kl_archive_rtf_text ? data_e105 _publ_contact_author_name 'Dr. Kay Severin' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7768' _publ_author_name 'da Silva, Ana C.' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Heterometallic bromo-bridged complexes with Re(CO)3 fragments ; _audit_author_name 'Mayer, P.' _audit_block_code Re_Ir_(CO)3_C10H15_Br3_e105_beck _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 30-Apr-00 _chemical_name_systematic ; ; _chemical_compound_source ; ; _chemical_name_common ? _chemical_formula_moiety 'Re1 Ir1 Br3 O3 C13 H15' _chemical_formula_sum 'C13 H15 Br3 Ir O3 Re' _chemical_formula_weight 837.392 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' 'O' 'O' 0.0106 0.0060 '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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 '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' _symmetry_Int_Tables_number 14 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 9.7123(7) _cell_length_b 14.9342(10) _cell_length_c 12.2606(10) _cell_angle_alpha 90 _cell_angle_beta 90.574(10) _cell_angle_gamma 90 _cell_volume 1778.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.9 _cell_special_details 'Monoclinic P (as derived from metrics)' _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.1278(4) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 21.022 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2626 _exptl_absorpt_correction_T_max 0.4960 _exptl_absorpt_process_details 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 3 -1 0.0210 0 -2 -1 0.0330 0 2 1 0.0160 -3 -1 0 0.2030 0 -1 1 0.0130 3 -1 3 0.1030 _diffrn_ambient_temperature 200(3) _diffrn_source_type 'Spellman DF4 Series' _diffrn_source_power 2.75_kW _diffrn_source_voltage 55_kV _diffrn_source_current 50_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 170.0 _kl_diffrn_detector_area_phi_incr 1.0 _kl_diffrn_detector_area_expos_time 4.00_min _kl_diffrn_detector_area_plate_dist 70.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.007 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 21 _diffrn_special_details ? _diffrn_reflns_number 11649 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.92 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.152 _refine_diff_density_min -2.678 _refine_diff_density_rms 0.262 _reflns_number_total 3421 _reflns_number_gt 2939 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3421 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ; refinement of H atoms riding with U(H)=1.5*U(C) for CH3 ; 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 Ir Ir 0.36233(3) 0.181001(16) 0.248349(17) 0.01249(9) Uani 1 1 d . . . Re Re 0.62276(3) 0.025408(18) 0.240424(19) 0.01714(9) Uani 1 1 d . . . Br1 Br 0.62455(8) 0.20129(5) 0.26753(5) 0.02120(16) Uani 1 1 d . . . Br2 Br 0.43095(8) 0.07220(5) 0.09912(5) 0.02700(18) Uani 1 1 d . . . Br3 Br 0.41243(9) 0.04621(5) 0.37255(6) 0.03121(19) Uani 1 1 d . . . O1 O 0.8549(6) 0.0216(4) 0.0761(4) 0.0337(13) Uani 1 1 d . . . C1 C 0.7665(8) 0.0232(5) 0.1373(5) 0.0198(15) Uani 1 1 d . . . O2 O 0.8375(6) -0.0282(4) 0.4113(4) 0.0334(14) Uani 1 1 d . . . C2 C 0.7529(8) -0.0053(5) 0.3485(5) 0.0230(16) Uani 1 1 d . . . O3 O 0.5801(8) -0.1733(4) 0.1986(8) 0.062(2) Uani 1 1 d . . . C3 C 0.5969(9) -0.0984(5) 0.2142(7) 0.0329(18) Uani 1 1 d . . . C4 C 0.3041(8) 0.3169(4) 0.2829(5) 0.0164(14) Uani 1 1 d . . . C5 C 0.2252(8) 0.2577(4) 0.3474(5) 0.0177(14) Uani 1 1 d . . . C6 C 0.1484(7) 0.1985(4) 0.2779(5) 0.0156(13) Uani 1 1 d . . . C7 C 0.2743(8) 0.2958(4) 0.1688(5) 0.0177(14) Uani 1 1 d . . . C8 C 0.1778(8) 0.2242(4) 0.1660(5) 0.0172(14) Uani 1 1 d . . . C9 C 0.3933(9) 0.3910(5) 0.3206(6) 0.0264(17) Uani 1 1 d . . . H9A H 0.4348 0.4204 0.2575 0.040 Uiso 1 1 calc R . . H9B H 0.4661 0.3673 0.3684 0.040 Uiso 1 1 calc R . . H9C H 0.3381 0.4346 0.3610 0.040 Uiso 1 1 calc R . . C10 C 0.2155(8) 0.2593(5) 0.4708(5) 0.0252(17) Uani 1 1 d . . . H10A H 0.1540 0.2113 0.4948 0.038 Uiso 1 1 calc R . . H10B H 0.1790 0.3172 0.4943 0.038 Uiso 1 1 calc R . . H10C H 0.3073 0.2502 0.5029 0.038 Uiso 1 1 calc R . . C11 C 0.0479(8) 0.1286(5) 0.3121(6) 0.0242(15) Uani 1 1 d . . . H11A H 0.0123 0.0973 0.2475 0.036 Uiso 1 1 calc R . . H11B H -0.0285 0.1569 0.3506 0.036 Uiso 1 1 calc R . . H11C H 0.0940 0.0856 0.3606 0.036 Uiso 1 1 calc R . . C12 C 0.1157(8) 0.1842(6) 0.0671(6) 0.0286(18) Uani 1 1 d . . . H12A H 0.0502 0.1376 0.0881 0.043 Uiso 1 1 calc R . . H12B H 0.1882 0.1578 0.0224 0.043 Uiso 1 1 calc R . . H12C H 0.0675 0.2307 0.0252 0.043 Uiso 1 1 calc R . . C13 C 0.3314(9) 0.3425(5) 0.0710(6) 0.0300(18) Uani 1 1 d . . . H13A H 0.3987 0.3876 0.0947 0.045 Uiso 1 1 calc R . . H13B H 0.2564 0.3717 0.0306 0.045 Uiso 1 1 calc R . . H13C H 0.3765 0.2987 0.0238 0.045 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 Ir 0.01279(17) 0.01343(14) 0.01124(12) -0.00037(8) -0.00035(9) 0.00062(9) Re 0.01378(18) 0.01509(15) 0.02258(14) 0.00089(9) 0.00078(10) 0.00107(10) Br1 0.0167(4) 0.0200(3) 0.0269(3) -0.0042(3) -0.0030(3) -0.0021(3) Br2 0.0235(4) 0.0314(4) 0.0259(3) -0.0135(3) -0.0057(3) 0.0068(3) Br3 0.0253(5) 0.0340(4) 0.0345(4) 0.0202(3) 0.0132(3) 0.0105(3) O1 0.027(4) 0.045(3) 0.029(3) -0.002(3) 0.005(2) 0.002(3) C1 0.021(4) 0.019(3) 0.020(3) -0.001(3) -0.004(3) -0.001(3) O2 0.020(3) 0.053(4) 0.027(2) 0.016(3) -0.004(2) 0.013(3) C2 0.021(4) 0.019(4) 0.028(3) 0.000(3) 0.011(3) -0.006(3) O3 0.031(4) 0.021(3) 0.132(7) -0.009(4) -0.005(4) -0.005(3) C3 0.014(5) 0.021(4) 0.063(5) 0.005(4) -0.001(4) -0.002(3) C4 0.021(4) 0.013(3) 0.015(3) 0.001(2) -0.001(3) 0.004(3) C5 0.022(4) 0.018(3) 0.014(3) -0.003(2) 0.004(2) 0.002(3) C6 0.009(4) 0.018(3) 0.020(3) 0.003(3) 0.000(2) -0.001(3) C7 0.024(4) 0.014(3) 0.014(3) 0.002(3) -0.002(3) 0.008(3) C8 0.019(4) 0.016(3) 0.017(3) 0.000(2) -0.002(2) 0.005(3) C9 0.035(5) 0.015(3) 0.029(3) -0.005(3) -0.004(3) -0.003(3) C10 0.035(5) 0.031(4) 0.010(3) -0.005(3) 0.003(3) -0.003(3) C11 0.019(4) 0.019(3) 0.035(3) -0.005(3) 0.007(3) -0.002(3) C12 0.017(4) 0.043(5) 0.026(3) -0.005(3) -0.016(3) -0.003(4) C13 0.039(5) 0.028(4) 0.023(3) 0.004(3) 0.003(3) 0.006(4) 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 Ir C6 2.129(7) . ? Ir C5 2.144(6) . ? Ir C7 2.146(6) . ? Ir C8 2.147(7) . ? Ir C4 2.150(6) . ? Ir Br2 2.5410(7) . ? Ir Br3 2.5677(7) . ? Ir Br1 2.5731(8) . ? Re C2 1.879(8) . ? Re C3 1.893(8) . ? Re C1 1.894(7) . ? Re Br2 2.6260(8) . ? Re Br3 2.6382(8) . ? Re Br1 2.6476(8) . ? O1 C1 1.145(9) . ? O2 C2 1.172(9) . ? O3 C3 1.146(10) . ? C4 C5 1.416(9) . ? C4 C7 1.460(8) . ? C4 C9 1.477(10) . ? C5 C6 1.433(9) . ? C5 C10 1.517(8) . ? C6 C8 1.455(9) . ? C6 C11 1.492(10) . ? C7 C8 1.422(10) . ? C7 C13 1.498(9) . ? C8 C12 1.475(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 C6 Ir C5 39.2(3) . . ? C6 Ir C7 66.1(3) . . ? C5 Ir C7 65.4(2) . . ? C6 Ir C8 39.8(2) . . ? C5 Ir C8 65.5(2) . . ? C7 Ir C8 38.7(3) . . ? C6 Ir C4 65.9(3) . . ? C5 Ir C4 38.5(3) . . ? C7 Ir C4 39.7(2) . . ? C8 Ir C4 65.7(3) . . ? C6 Ir Br2 117.67(18) . . ? C5 Ir Br2 156.75(19) . . ? C7 Ir Br2 106.84(16) . . ? C8 Ir Br2 94.44(16) . . ? C4 Ir Br2 144.79(16) . . ? C6 Ir Br3 100.08(17) . . ? C5 Ir Br3 101.44(17) . . ? C7 Ir Br3 165.52(19) . . ? C8 Ir Br3 131.82(19) . . ? C4 Ir Br3 132.20(16) . . ? Br2 Ir Br3 82.89(3) . . ? C6 Ir Br1 159.53(18) . . ? C5 Ir Br1 120.35(19) . . ? C7 Ir Br1 109.7(2) . . ? C8 Ir Br1 145.90(19) . . ? C4 Ir Br1 97.6(2) . . ? Br2 Ir Br1 82.80(3) . . ? Br3 Ir Br1 81.76(3) . . ? C2 Re C3 88.2(3) . . ? C2 Re C1 88.3(3) . . ? C3 Re C1 88.1(3) . . ? C2 Re Br2 176.4(2) . . ? C3 Re Br2 93.2(3) . . ? C1 Re Br2 95.0(2) . . ? C2 Re Br3 96.6(2) . . ? C3 Re Br3 96.7(3) . . ? C1 Re Br3 173.2(2) . . ? Br2 Re Br3 79.93(3) . . ? C2 Re Br1 98.6(2) . . ? C3 Re Br1 172.3(3) . . ? C1 Re Br1 95.6(2) . . ? Br2 Re Br1 79.78(2) . . ? Br3 Re Br1 79.06(2) . . ? Ir Br1 Re 82.33(2) . . ? Ir Br2 Re 83.37(2) . . ? Ir Br3 Re 82.61(2) . . ? O1 C1 Re 179.0(6) . . ? O2 C2 Re 175.8(6) . . ? O3 C3 Re 179.4(9) . . ? C5 C4 C7 107.3(6) . . ? C5 C4 C9 127.7(6) . . ? C7 C4 C9 124.8(6) . . ? C5 C4 Ir 70.5(4) . . ? C7 C4 Ir 70.0(4) . . ? C9 C4 Ir 127.9(5) . . ? C4 C5 C6 109.5(5) . . ? C4 C5 C10 125.9(6) . . ? C6 C5 C10 124.4(6) . . ? C4 C5 Ir 71.0(4) . . ? C6 C5 Ir 69.8(4) . . ? C10 C5 Ir 128.2(5) . . ? C5 C6 C8 107.0(6) . . ? C5 C6 C11 127.1(6) . . ? C8 C6 C11 125.8(6) . . ? C5 C6 Ir 71.0(4) . . ? C8 C6 Ir 70.8(4) . . ? C11 C6 Ir 127.1(5) . . ? C8 C7 C4 108.0(6) . . ? C8 C7 C13 125.4(6) . . ? C4 C7 C13 126.6(7) . . ? C8 C7 Ir 70.7(4) . . ? C4 C7 Ir 70.3(3) . . ? C13 C7 Ir 125.9(5) . . ? C7 C8 C6 108.1(5) . . ? C7 C8 C12 126.0(6) . . ? C6 C8 C12 125.8(6) . . ? C7 C8 Ir 70.6(4) . . ? C6 C8 Ir 69.4(4) . . ? C12 C8 Ir 126.6(5) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 C6 Ir Br1 Re 139.4(5) . . . . ? C5 Ir Br1 Re 141.1(2) . . . . ? C7 Ir Br1 Re -146.54(17) . . . . ? C8 Ir Br1 Re -128.4(3) . . . . ? C4 Ir Br1 Re 174.35(16) . . . . ? Br2 Ir Br1 Re -41.17(2) . . . . ? Br3 Ir Br1 Re 42.64(2) . . . . ? C2 Re Br1 Ir -136.8(2) . . . . ? C3 Re Br1 Ir 16(2) . . . . ? C1 Re Br1 Ir 134.0(2) . . . . ? Br2 Re Br1 Ir 39.95(2) . . . . ? Br3 Re Br1 Ir -41.65(2) . . . . ? C6 Ir Br2 Re -138.75(19) . . . . ? C5 Ir Br2 Re -143.5(4) . . . . ? C7 Ir Br2 Re 149.9(2) . . . . ? C8 Ir Br2 Re -172.70(19) . . . . ? C4 Ir Br2 Re 134.5(3) . . . . ? Br3 Ir Br2 Re -41.07(3) . . . . ? Br1 Ir Br2 Re 41.47(2) . . . . ? C2 Re Br2 Ir 23(4) . . . . ? C3 Re Br2 Ir 136.4(3) . . . . ? C1 Re Br2 Ir -135.3(2) . . . . ? Br3 Re Br2 Ir 40.12(2) . . . . ? Br1 Re Br2 Ir -40.45(2) . . . . ? C6 Ir Br3 Re 157.86(18) . . . . ? C5 Ir Br3 Re -162.2(2) . . . . ? C7 Ir Br3 Re 174.1(7) . . . . ? C8 Ir Br3 Re 130.5(2) . . . . ? C4 Ir Br3 Re -135.7(3) . . . . ? Br2 Ir Br3 Re 40.92(3) . . . . ? Br1 Ir Br3 Re -42.79(2) . . . . ? C2 Re Br3 Ir 139.3(2) . . . . ? C3 Re Br3 Ir -131.8(3) . . . . ? C1 Re Br3 Ir 2.8(17) . . . . ? Br2 Re Br3 Ir -39.69(2) . . . . ? Br1 Re Br3 Ir 41.72(2) . . . . ? C2 Re C1 O1 -7(37) . . . . ? C3 Re C1 O1 -95(37) . . . . ? Br2 Re C1 O1 172(100) . . . . ? Br3 Re C1 O1 130(36) . . . . ? Br1 Re C1 O1 91(37) . . . . ? C3 Re C2 O2 45(9) . . . . ? C1 Re C2 O2 -43(9) . . . . ? Br2 Re C2 O2 159(6) . . . . ? Br3 Re C2 O2 142(9) . . . . ? Br1 Re C2 O2 -138(9) . . . . ? C2 Re C3 O3 113(97) . . . . ? C1 Re C3 O3 -158(97) . . . . ? Br2 Re C3 O3 -64(97) . . . . ? Br3 Re C3 O3 17(97) . . . . ? Br1 Re C3 O3 -40(99) . . . . ? C6 Ir C4 C5 36.8(4) . . . . ? C7 Ir C4 C5 117.7(6) . . . . ? C8 Ir C4 C5 80.6(4) . . . . ? Br2 Ir C4 C5 141.1(3) . . . . ? Br3 Ir C4 C5 -44.8(5) . . . . ? Br1 Ir C4 C5 -130.6(4) . . . . ? C6 Ir C4 C7 -81.0(4) . . . . ? C5 Ir C4 C7 -117.7(6) . . . . ? C8 Ir C4 C7 -37.2(4) . . . . ? Br2 Ir C4 C7 23.4(6) . . . . ? Br3 Ir C4 C7 -162.5(3) . . . . ? Br1 Ir C4 C7 111.7(4) . . . . ? C6 Ir C4 C9 159.9(6) . . . . ? C5 Ir C4 C9 123.2(7) . . . . ? C7 Ir C4 C9 -119.1(8) . . . . ? C8 Ir C4 C9 -156.3(6) . . . . ? Br2 Ir C4 C9 -95.7(6) . . . . ? Br3 Ir C4 C9 78.4(6) . . . . ? Br1 Ir C4 C9 -7.4(6) . . . . ? C7 C4 C5 C6 1.2(8) . . . . ? C9 C4 C5 C6 177.2(7) . . . . ? Ir C4 C5 C6 -59.4(5) . . . . ? C7 C4 C5 C10 -175.5(7) . . . . ? C9 C4 C5 C10 0.5(12) . . . . ? Ir C4 C5 C10 123.9(7) . . . . ? C7 C4 C5 Ir 60.6(5) . . . . ? C9 C4 C5 Ir -123.4(7) . . . . ? C6 Ir C5 C4 -120.2(5) . . . . ? C7 Ir C5 C4 -38.5(4) . . . . ? C8 Ir C5 C4 -81.2(4) . . . . ? Br2 Ir C5 C4 -113.5(5) . . . . ? Br3 Ir C5 C4 147.8(3) . . . . ? Br1 Ir C5 C4 60.8(4) . . . . ? C7 Ir C5 C6 81.7(4) . . . . ? C8 Ir C5 C6 39.0(4) . . . . ? C4 Ir C5 C6 120.2(5) . . . . ? Br2 Ir C5 C6 6.7(7) . . . . ? Br3 Ir C5 C6 -92.0(3) . . . . ? Br1 Ir C5 C6 -179.0(3) . . . . ? C6 Ir C5 C10 118.5(8) . . . . ? C7 Ir C5 C10 -159.8(7) . . . . ? C8 Ir C5 C10 157.5(7) . . . . ? C4 Ir C5 C10 -121.3(8) . . . . ? Br2 Ir C5 C10 125.3(6) . . . . ? Br3 Ir C5 C10 26.6(7) . . . . ? Br1 Ir C5 C10 -60.5(7) . . . . ? C4 C5 C6 C8 -1.9(8) . . . . ? C10 C5 C6 C8 174.8(7) . . . . ? Ir C5 C6 C8 -62.0(5) . . . . ? C4 C5 C6 C11 -177.2(7) . . . . ? C10 C5 C6 C11 -0.5(12) . . . . ? Ir C5 C6 C11 122.7(7) . . . . ? C4 C5 C6 Ir 60.1(5) . . . . ? C10 C5 C6 Ir -123.1(7) . . . . ? C7 Ir C6 C5 -79.8(4) . . . . ? C8 Ir C6 C5 -116.6(5) . . . . ? C4 Ir C6 C5 -36.1(3) . . . . ? Br2 Ir C6 C5 -177.0(3) . . . . ? Br3 Ir C6 C5 95.8(3) . . . . ? Br1 Ir C6 C5 2.4(7) . . . . ? C5 Ir C6 C8 116.6(5) . . . . ? C7 Ir C6 C8 36.7(4) . . . . ? C4 Ir C6 C8 80.4(4) . . . . ? Br2 Ir C6 C8 -60.5(4) . . . . ? Br3 Ir C6 C8 -147.7(3) . . . . ? Br1 Ir C6 C8 118.9(5) . . . . ? C5 Ir C6 C11 -122.6(7) . . . . ? C7 Ir C6 C11 157.6(6) . . . . ? C8 Ir C6 C11 120.9(7) . . . . ? C4 Ir C6 C11 -158.7(6) . . . . ? Br2 Ir C6 C11 60.4(6) . . . . ? Br3 Ir C6 C11 -26.8(6) . . . . ? Br1 Ir C6 C11 -120.2(6) . . . . ? C5 C4 C7 C8 0.0(8) . . . . ? C9 C4 C7 C8 -176.2(7) . . . . ? Ir C4 C7 C8 61.0(5) . . . . ? C5 C4 C7 C13 178.4(7) . . . . ? C9 C4 C7 C13 2.2(12) . . . . ? Ir C4 C7 C13 -120.7(7) . . . . ? C5 C4 C7 Ir -60.9(5) . . . . ? C9 C4 C7 Ir 122.9(7) . . . . ? C6 Ir C7 C8 -37.8(4) . . . . ? C5 Ir C7 C8 -80.9(4) . . . . ? C4 Ir C7 C8 -118.2(6) . . . . ? Br2 Ir C7 C8 75.6(4) . . . . ? Br3 Ir C7 C8 -55.3(9) . . . . ? Br1 Ir C7 C8 163.8(3) . . . . ? C6 Ir C7 C4 80.5(4) . . . . ? C5 Ir C7 C4 37.3(4) . . . . ? C8 Ir C7 C4 118.2(6) . . . . ? Br2 Ir C7 C4 -166.2(4) . . . . ? Br3 Ir C7 C4 62.9(9) . . . . ? Br1 Ir C7 C4 -77.9(4) . . . . ? C6 Ir C7 C13 -158.1(7) . . . . ? C5 Ir C7 C13 158.7(7) . . . . ? C8 Ir C7 C13 -120.3(7) . . . . ? C4 Ir C7 C13 121.4(8) . . . . ? Br2 Ir C7 C13 -44.7(6) . . . . ? Br3 Ir C7 C13 -175.6(5) . . . . ? Br1 Ir C7 C13 43.5(6) . . . . ? C4 C7 C8 C6 -1.2(8) . . . . ? C13 C7 C8 C6 -179.6(7) . . . . ? Ir C7 C8 C6 59.5(5) . . . . ? C4 C7 C8 C12 177.5(7) . . . . ? C13 C7 C8 C12 -0.8(12) . . . . ? Ir C7 C8 C12 -121.8(7) . . . . ? C4 C7 C8 Ir -60.7(5) . . . . ? C13 C7 C8 Ir 120.9(7) . . . . ? C5 C6 C8 C7 1.9(8) . . . . ? C11 C6 C8 C7 177.3(7) . . . . ? Ir C6 C8 C7 -60.2(5) . . . . ? C5 C6 C8 C12 -176.8(7) . . . . ? C11 C6 C8 C12 -1.5(12) . . . . ? Ir C6 C8 C12 121.0(7) . . . . ? C5 C6 C8 Ir 62.1(5) . . . . ? C11 C6 C8 Ir -122.5(7) . . . . ? C6 Ir C8 C7 119.0(5) . . . . ? C5 Ir C8 C7 80.6(4) . . . . ? C4 Ir C8 C7 38.2(4) . . . . ? Br2 Ir C8 C7 -111.6(3) . . . . ? Br3 Ir C8 C7 164.0(3) . . . . ? Br1 Ir C8 C7 -27.9(5) . . . . ? C5 Ir C8 C6 -38.4(4) . . . . ? C7 Ir C8 C6 -119.0(5) . . . . ? C4 Ir C8 C6 -80.8(4) . . . . ? Br2 Ir C8 C6 129.4(4) . . . . ? Br3 Ir C8 C6 45.0(4) . . . . ? Br1 Ir C8 C6 -146.9(3) . . . . ? C6 Ir C8 C12 -120.0(8) . . . . ? C5 Ir C8 C12 -158.4(7) . . . . ? C7 Ir C8 C12 121.0(8) . . . . ? C4 Ir C8 C12 159.2(7) . . . . ? Br2 Ir C8 C12 9.4(6) . . . . ? Br3 Ir C8 C12 -75.0(7) . . . . ? Br1 Ir C8 C12 93.1(7) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? _kl_archive_SHELXL_comment 'release 97-2' _kl_archive_SHELXL_res ; TITL e105 in P21/n (14), sir97 CELL 0.71073 9.7123 14.9342 12.2606 90.000 90.574 90.000 ZERR 4 0.0007 0.0010 0.0010 0.000 0.010 0.000 LATT 1 SYMM .50000-X, .50000+Y, .50000-Z SFAC C H O BR RE IR UNIT 52 60 12 12 4 4 L.S. 8 FMAP 2 PLAN -25 TEMP -73 BOND $H CONF ACTA WGHT 0.031000 FVAR 0.16754 IR 6 0.362330 0.181001 0.248349 11.00000 0.01279 0.01343 = 0.01124 -0.00037 -0.00035 0.00062 RE 5 0.622762 0.025408 0.240424 11.00000 0.01378 0.01509 = 0.02258 0.00089 0.00078 0.00107 BR1 4 0.624546 0.201290 0.267532 11.00000 0.01670 0.01998 = 0.02686 -0.00415 -0.00305 -0.00209 BR2 4 0.430946 0.072196 0.099121 11.00000 0.02355 0.03143 = 0.02590 -0.01346 -0.00575 0.00678 BR3 4 0.412433 0.046210 0.372551 11.00000 0.02534 0.03404 = 0.03452 0.02019 0.01319 0.01053 O1 3 0.854863 0.021634 0.076118 11.00000 0.02660 0.04534 = 0.02939 -0.00215 0.00547 0.00197 C1 1 0.766549 0.023160 0.137256 11.00000 0.02064 0.01892 = 0.01979 -0.00134 -0.00367 -0.00149 O2 3 0.837544 -0.028192 0.411334 11.00000 0.02029 0.05262 = 0.02726 0.01553 -0.00418 0.01255 C2 1 0.752944 -0.005265 0.348492 11.00000 0.02130 0.01949 = 0.02846 -0.00029 0.01070 -0.00573 O3 3 0.580097 -0.173278 0.198645 11.00000 0.03127 0.02091 = 0.13228 -0.00926 -0.00505 -0.00543 C3 1 0.596900 -0.098411 0.214182 11.00000 0.01408 0.02124 = 0.06349 0.00546 -0.00078 -0.00223 C4 1 0.304066 0.316891 0.282936 11.00000 0.02081 0.01306 = 0.01527 0.00058 -0.00101 0.00440 C5 1 0.225183 0.257747 0.347404 11.00000 0.02153 0.01822 = 0.01355 -0.00319 0.00444 0.00230 C6 1 0.148402 0.198510 0.277861 11.00000 0.00904 0.01766 = 0.01999 0.00257 -0.00026 -0.00070 C7 1 0.274348 0.295816 0.168789 11.00000 0.02434 0.01441 = 0.01433 0.00235 -0.00204 0.00805 C8 1 0.177817 0.224231 0.165996 11.00000 0.01918 0.01583 = 0.01650 -0.00044 -0.00206 0.00501 C9 1 0.393304 0.391008 0.320615 11.00000 0.03535 0.01485 = 0.02900 -0.00462 -0.00420 -0.00345 AFIX 33 H9A 2 0.434848 0.420377 0.257492 11.00000 -1.50000 H9B 2 0.466126 0.367260 0.368362 11.00000 -1.50000 H9C 2 0.338147 0.434560 0.360991 11.00000 -1.50000 AFIX 0 C10 1 0.215508 0.259265 0.470769 11.00000 0.03470 0.03088 = 0.00994 -0.00463 0.00287 -0.00326 AFIX 33 H10A 2 0.153998 0.211307 0.494829 11.00000 -1.50000 H10B 2 0.178999 0.317224 0.494324 11.00000 -1.50000 H10C 2 0.307274 0.250245 0.502873 11.00000 -1.50000 AFIX 0 C11 1 0.047933 0.128568 0.312075 11.00000 0.01939 0.01852 = 0.03493 -0.00462 0.00659 -0.00211 AFIX 33 H11A 2 0.012304 0.097256 0.247466 11.00000 -1.50000 H11B 2 -0.028454 0.156933 0.350637 11.00000 -1.50000 H11C 2 0.093975 0.085589 0.360587 11.00000 -1.50000 AFIX 0 C12 1 0.115727 0.184197 0.067109 11.00000 0.01716 0.04254 = 0.02564 -0.00481 -0.01636 -0.00251 AFIX 33 H12A 2 0.050164 0.137553 0.088123 11.00000 -1.50000 H12B 2 0.188224 0.157770 0.022351 11.00000 -1.50000 H12C 2 0.067549 0.230675 0.025163 11.00000 -1.50000 AFIX 0 C13 1 0.331437 0.342476 0.071004 11.00000 0.03879 0.02771 = 0.02348 0.00450 0.00279 0.00551 AFIX 33 H13A 2 0.398686 0.387557 0.094692 11.00000 -1.50000 H13B 2 0.256437 0.371747 0.030554 11.00000 -1.50000 H13C 2 0.376538 0.298652 0.023789 11.00000 -1.50000 HKLF 4 REM e105 in P21/n (14), sir97 REM R1 = 0.0286 for 2939 Fo > 4sig(Fo) and 0.0341 for all 3421 data REM 190 parameters refined using 0 restraints END WGHT 0.0310 0.0000 REM Highest difference peak 1.152, deepest hole -2.678, 1-sigma level 0.262 Q1 1 0.6249 0.0847 0.2399 11.00000 0.05 1.15 Q2 1 0.4248 0.2362 0.1939 11.00000 0.05 1.05 Q3 1 0.6251 -0.0332 0.2439 11.00000 0.05 1.04 Q4 1 0.2846 0.1401 0.2953 11.00000 0.05 1.03 Q5 1 0.2879 0.2283 0.3006 11.00000 0.05 1.02 Q6 1 0.3669 0.1189 0.2800 11.00000 0.05 1.02 ; _kl_archive_SCHAKAL_comment ? _kl_archive_SCHAKAL_dat ? _kl_archive_ORTEP_comment ? _kl_archive_ORTEP_ins ? _kl_archive_rtf_text ?