Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_ax5 _database_code_CSD 180999 _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Kaim, Wolfgang' ; Institut fur Anorganische Chemie Universitat Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Knoedler, Axel' ; Institut fur Anorganische Chemie Universitat Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Wanner, Matthias' ; Institut fur Anorganische Chemie Universitat Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Fiedler, Jan' ; J. Heyrovsky Institute of Physical Chemistry Academy of Sciences of the Czech Republic Dolejskova 3 CZ-18223 Prague Czech Republic ; _publ_contact_author_name 'Prof W Kaim' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Stuttgart Pfaffenwaldring 55 Stuttgart D-70550 GERMANY ; _publ_contact_author_phone '049 711 685-4170' _publ_contact_author_fax '049 711 685-4165' _publ_contact_author_email 'kaim@iac.uni-stuttgart.de' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name 'Axel Knoedler, Matthias Wanner,Jan Fiedler' _publ_section_title ; Coordination ambivalence of the electroactive bis-chelate ligand bis(1-methyl-2-imidazolyl)glyoxal (BIG) in mononuclear and dinuclear complexes with re(CO)3CI ; #================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Re(CO)3Cl(big)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H10 Cl N4 O5 Re' _chemical_formula_weight 523.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.562(4) _cell_length_b 15.552(3) _cell_length_c 13.249(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.12(3) _cell_angle_gamma 90.00 _cell_volume 3214.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 7.759 _exptl_absorpt_correction_type Psi-Scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4864 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.01 _reflns_number_total 4677 _reflns_number_gt 4031 _reflns_threshold_expression >2sigma(I) computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4677 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 1.494 _refine_ls_restrained_S_all 1.494 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.128450(15) 0.307871(15) 0.70057(2) 0.01856(10) Uani 1 1 d . . . C3 C 0.0440(5) 0.2300(5) 0.5732(7) 0.0262(13) Uani 1 1 d . . . C2 C 0.0358(4) 0.3849(5) 0.6472(7) 0.0252(13) Uani 1 1 d . . . O3 O -0.0074(4) 0.1833(4) 0.4992(6) 0.0358(13) Uani 1 1 d . . . N2A N 0.2376(4) 0.2255(4) 0.7588(5) 0.0218(11) Uani 1 1 d . . . N1A N 0.3498(4) 0.1663(4) 0.7806(6) 0.0231(11) Uani 1 1 d . . . O2 O -0.0211(4) 0.4308(4) 0.6127(6) 0.0436(15) Uani 1 1 d . . . C1A C 0.3050(4) 0.2406(4) 0.7592(6) 0.0207(12) Uani 1 1 d . . . C3A C 0.2393(4) 0.1382(4) 0.7821(7) 0.0247(13) Uani 1 1 d . . . H3AA H 0.2001 0.1087 0.7873 0.030 Uiso 1 1 calc R . . C2A C 0.3081(5) 0.1032(5) 0.7962(7) 0.0306(15) Uani 1 1 d . . . H2AA H 0.3243 0.0457 0.8136 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.15880(11) 0.38204(11) 0.56608(15) 0.0245(3) Uani 1 1 d . . . N2B N 0.2263(3) 0.3937(4) 0.8480(5) 0.0207(10) Uani 1 1 d . . . C1B C 0.3012(4) 0.4212(4) 0.8757(5) 0.0182(11) Uani 1 1 d . . . C3B C 0.2144(5) 0.4354(5) 0.9276(7) 0.0274(14) Uani 1 1 d . . . H3BA H 0.1668 0.4302 0.9271 0.033 Uiso 1 1 calc R . . C1 C 0.1147(5) 0.2537(5) 0.8175(8) 0.0323(15) Uani 1 1 d . . . O11B O 0.3766(3) 0.4667(4) 0.8022(4) 0.0240(10) Uani 1 1 d . . . O11A O 0.3659(4) 0.3252(3) 0.6845(6) 0.0295(11) Uani 1 1 d . . . C11B C 0.3358(4) 0.4079(4) 0.8031(6) 0.0185(11) Uani 1 1 d . . . C11A C 0.3325(4) 0.3227(4) 0.7379(6) 0.0200(11) Uani 1 1 d . . . C2B C 0.2848(5) 0.4860(5) 1.0082(7) 0.0308(15) Uani 1 1 d . . . H2BA H 0.2943 0.5199 1.0734 0.037 Uiso 1 1 calc R . . O1 O 0.1060(5) 0.2208(5) 0.8865(7) 0.0482(17) Uani 1 1 d . . . C4A C 0.4256(5) 0.1531(5) 0.7833(8) 0.0337(16) Uani 1 1 d . . . H4AA H 0.4424 0.0938 0.8005 0.051 Uiso 1 1 calc R . . H4AB H 0.4719 0.1884 0.8484 0.051 Uiso 1 1 calc R . . H4AC H 0.4118 0.1687 0.7028 0.051 Uiso 1 1 calc R . . N1B N 0.3384(4) 0.4773(4) 0.9750(5) 0.0218(10) Uani 1 1 d . . . C4B C 0.4251(5) 0.5160(6) 1.0456(8) 0.039(2) Uani 1 1 d . . . H4BA H 0.4506 0.5012 1.0049 0.059 Uiso 1 1 calc R . . H4BB H 0.4601 0.4945 1.1308 0.059 Uiso 1 1 calc R . . H4BC H 0.4206 0.5774 1.0470 0.059 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 Re1 0.02368(15) 0.01576(15) 0.01804(14) -0.00085(8) 0.01354(11) -0.00192(8) C3 0.031(3) 0.025(3) 0.027(3) -0.002(3) 0.020(3) -0.001(3) C2 0.032(3) 0.021(3) 0.029(3) -0.003(3) 0.022(3) -0.003(2) O3 0.036(3) 0.027(3) 0.035(3) -0.010(2) 0.017(2) -0.010(2) N2A 0.029(3) 0.014(2) 0.023(2) 0.004(2) 0.016(2) 0.003(2) N1A 0.037(3) 0.010(2) 0.025(3) 0.000(2) 0.020(2) 0.002(2) O2 0.040(3) 0.044(4) 0.046(4) 0.009(3) 0.025(3) 0.011(3) C1A 0.031(3) 0.014(3) 0.021(3) -0.002(2) 0.017(2) -0.001(2) C3A 0.033(3) 0.014(3) 0.026(3) -0.002(2) 0.017(3) -0.005(2) C2A 0.043(4) 0.014(3) 0.030(3) 0.005(3) 0.020(3) 0.006(3) Cl1 0.0328(7) 0.0223(7) 0.0192(6) 0.0024(6) 0.0162(6) -0.0005(6) N2B 0.025(2) 0.021(3) 0.022(2) 0.002(2) 0.017(2) 0.003(2) C1B 0.028(3) 0.013(2) 0.013(2) -0.001(2) 0.013(2) -0.002(2) C3B 0.036(3) 0.031(4) 0.030(3) -0.007(3) 0.027(3) -0.006(3) C1 0.041(4) 0.030(4) 0.033(4) 0.004(3) 0.026(3) 0.002(3) O11B 0.031(2) 0.020(2) 0.027(2) 0.0034(18) 0.021(2) -0.0018(17) O11A 0.046(3) 0.023(2) 0.037(3) 0.000(2) 0.034(3) -0.002(2) C11B 0.023(3) 0.017(3) 0.017(2) -0.001(2) 0.013(2) 0.000(2) C11A 0.026(3) 0.016(3) 0.022(3) -0.003(2) 0.017(2) -0.001(2) C2B 0.043(4) 0.030(4) 0.027(3) -0.008(3) 0.026(3) -0.006(3) O1 0.052(4) 0.052(4) 0.057(4) 0.020(3) 0.041(4) 0.002(3) C4A 0.037(4) 0.028(4) 0.039(4) -0.008(3) 0.024(3) 0.005(3) N1B 0.029(3) 0.021(3) 0.018(2) -0.002(2) 0.015(2) -0.003(2) C4B 0.034(4) 0.053(5) 0.029(4) -0.022(4) 0.019(3) -0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.917(7) . ? Re1 C3 1.918(7) . ? Re1 C1 1.919(8) . ? Re1 N2B 2.179(6) . ? Re1 N2A 2.192(6) . ? Re1 Cl1 2.4770(17) . ? C3 O3 1.145(9) . ? C2 O2 1.159(9) . ? N2A C1A 1.337(9) . ? N2A C3A 1.389(9) . ? N1A C2A 1.369(10) . ? N1A C1A 1.374(8) . ? N1A C4A 1.475(10) . ? C1A C11A 1.476(9) . ? C3A C2A 1.356(11) . ? N2B C1B 1.347(8) . ? N2B C3B 1.373(8) . ? C1B N1B 1.367(8) . ? C1B C11B 1.487(9) . ? C3B C2B 1.371(10) . ? C1 O1 1.147(10) . ? O11B C11B 1.218(8) . ? O11A C11A 1.219(8) . ? C11B C11A 1.563(9) . ? C2B N1B 1.367(9) . ? N1B C4B 1.482(9) . ? 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 C2 Re1 C3 87.1(3) . . ? C2 Re1 C1 90.6(3) . . ? C3 Re1 C1 88.1(3) . . ? C2 Re1 N2B 94.1(3) . . ? C3 Re1 N2B 178.6(3) . . ? C1 Re1 N2B 91.2(3) . . ? C2 Re1 N2A 176.7(3) . . ? C3 Re1 N2A 94.6(3) . . ? C1 Re1 N2A 92.3(3) . . ? N2B Re1 N2A 84.3(2) . . ? C2 Re1 Cl1 91.6(2) . . ? C3 Re1 Cl1 96.6(2) . . ? C1 Re1 Cl1 174.9(2) . . ? N2B Re1 Cl1 84.09(15) . . ? N2A Re1 Cl1 85.42(16) . . ? O3 C3 Re1 178.0(7) . . ? O2 C2 Re1 178.8(7) . . ? C1A N2A C3A 106.2(5) . . ? C1A N2A Re1 130.3(4) . . ? C3A N2A Re1 122.6(4) . . ? C2A N1A C1A 105.7(6) . . ? C2A N1A C4A 125.4(6) . . ? C1A N1A C4A 128.9(6) . . ? N2A C1A N1A 111.0(6) . . ? N2A C1A C11A 128.6(6) . . ? N1A C1A C11A 120.4(6) . . ? C2A C3A N2A 108.2(6) . . ? C3A C2A N1A 108.9(6) . . ? C1B N2B C3B 107.6(6) . . ? C1B N2B Re1 131.4(4) . . ? C3B N2B Re1 120.9(4) . . ? N2B C1B N1B 108.9(6) . . ? N2B C1B C11B 128.7(5) . . ? N1B C1B C11B 121.7(6) . . ? C2B C3B N2B 108.2(6) . . ? O1 C1 Re1 179.4(9) . . ? O11B C11B C1B 117.3(6) . . ? O11B C11B C11A 116.1(6) . . ? C1B C11B C11A 126.3(5) . . ? O11A C11A C1A 121.6(6) . . ? O11A C11A C11B 115.8(6) . . ? C1A C11A C11B 121.8(6) . . ? N1B C2B C3B 107.3(6) . . ? C1B N1B C2B 107.9(6) . . ? C1B N1B C4B 127.5(6) . . ? C2B N1B C4B 124.3(6) . . ? 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 C2 Re1 C3 O3 -66(21) . . . . ? C1 Re1 C3 O3 25(21) . . . . ? N2B Re1 C3 O3 83(24) . . . . ? N2A Re1 C3 O3 117(21) . . . . ? Cl1 Re1 C3 O3 -157(21) . . . . ? C3 Re1 C2 O2 -25(33) . . . . ? C1 Re1 C2 O2 -113(33) . . . . ? N2B Re1 C2 O2 155(33) . . . . ? N2A Re1 C2 O2 95(33) . . . . ? Cl1 Re1 C2 O2 71(33) . . . . ? C2 Re1 N2A C1A 1(5) . . . . ? C3 Re1 N2A C1A 120.6(6) . . . . ? C1 Re1 N2A C1A -151.1(6) . . . . ? N2B Re1 N2A C1A -60.1(6) . . . . ? Cl1 Re1 N2A C1A 24.4(6) . . . . ? C2 Re1 N2A C3A -167(4) . . . . ? C3 Re1 N2A C3A -47.1(6) . . . . ? C1 Re1 N2A C3A 41.2(6) . . . . ? N2B Re1 N2A C3A 132.2(5) . . . . ? Cl1 Re1 N2A C3A -143.3(5) . . . . ? C3A N2A C1A N1A 0.6(7) . . . . ? Re1 N2A C1A N1A -168.6(4) . . . . ? C3A N2A C1A C11A 179.3(6) . . . . ? Re1 N2A C1A C11A 10.1(10) . . . . ? C2A N1A C1A N2A -1.1(8) . . . . ? C4A N1A C1A N2A 177.2(7) . . . . ? C2A N1A C1A C11A -179.9(6) . . . . ? C4A N1A C1A C11A -1.6(11) . . . . ? C1A N2A C3A C2A 0.1(8) . . . . ? Re1 N2A C3A C2A 170.4(5) . . . . ? N2A C3A C2A N1A -0.8(8) . . . . ? C1A N1A C2A C3A 1.1(8) . . . . ? C4A N1A C2A C3A -177.2(7) . . . . ? C2 Re1 N2B C1B -130.5(6) . . . . ? C3 Re1 N2B C1B 80(11) . . . . ? C1 Re1 N2B C1B 138.8(6) . . . . ? N2A Re1 N2B C1B 46.6(6) . . . . ? Cl1 Re1 N2B C1B -39.3(6) . . . . ? C2 Re1 N2B C3B 44.6(6) . . . . ? C3 Re1 N2B C3B -105(11) . . . . ? C1 Re1 N2B C3B -46.1(6) . . . . ? N2A Re1 N2B C3B -138.3(6) . . . . ? Cl1 Re1 N2B C3B 135.8(5) . . . . ? C3B N2B C1B N1B 2.2(7) . . . . ? Re1 N2B C1B N1B 177.8(4) . . . . ? C3B N2B C1B C11B -168.2(7) . . . . ? Re1 N2B C1B C11B 7.4(10) . . . . ? C1B N2B C3B C2B -2.6(8) . . . . ? Re1 N2B C3B C2B -178.7(5) . . . . ? C2 Re1 C1 O1 79(90) . . . . ? C3 Re1 C1 O1 -8(90) . . . . ? N2B Re1 C1 O1 173(100) . . . . ? N2A Re1 C1 O1 -102(90) . . . . ? Cl1 Re1 C1 O1 -165(100) . . . . ? N2B C1B C11B O11B 143.8(7) . . . . ? N1B C1B C11B O11B -25.5(9) . . . . ? N2B C1B C11B C11A -42.3(10) . . . . ? N1B C1B C11B C11A 148.4(6) . . . . ? N2A C1A C11A O11A -145.7(7) . . . . ? N1A C1A C11A O11A 33.0(10) . . . . ? N2A C1A C11A C11B 45.6(10) . . . . ? N1A C1A C11A C11B -135.8(6) . . . . ? O11B C11B C11A O11A -5.1(9) . . . . ? C1B C11B C11A O11A -179.0(6) . . . . ? O11B C11B C11A C1A 164.3(6) . . . . ? C1B C11B C11A C1A -9.7(10) . . . . ? N2B C3B C2B N1B 1.9(9) . . . . ? N2B C1B N1B C2B -1.0(7) . . . . ? C11B C1B N1B C2B 170.2(6) . . . . ? N2B C1B N1B C4B 172.9(7) . . . . ? C11B C1B N1B C4B -15.9(10) . . . . ? C3B C2B N1B C1B -0.6(8) . . . . ? C3B C2B N1B C4B -174.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.650 _refine_diff_density_min -3.723 _refine_diff_density_rms 0.303