Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Feliz, M.R.' 'Juliarena, P.' 'Piro, O.' 'Ruiz, G.' 'Tocho, J.' 'Torchia, G.' 'Wolcan, E.' _publ_requested_journal 'Dalton Transactions' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr M.R Feliz' _publ_contact_author_address ; Universidad Nacional de La Plata C.C 16, Suc. 4, La Plata 1900 ARGENTINA ; _publ_contact_author_phone '54 221 4257430' _publ_contact_author_fax '54 221 4254642' _publ_contact_author_email mfeliz@inifta.unlp.edu.ar _publ_requested_journal 'Dalton Transaction' _publ_requested_coeditor_name 'Malcolm H.Chisholm' _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Photoinduced charge Separation In R-CO2-Re(CO)3(2,2'-bipyridine) Complexes, Two Emitting Charge Transfer Excited States. ; #============================================================================== data_s93 _database_code_CSD 171630 _audit_creation_method SHELXL _chemical_name_systematic ; fac-Re(CO)3(2,2'-bipyridine)(anthracene-2-carboxylate) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H17 N2 O5 Re' _chemical_formula_weight 647.64 _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 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2~1~/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.951(1) _cell_length_b 15.089(2) _cell_length_c 18.253(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.53(1) _cell_angle_gamma 90.00 _cell_volume 2443.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.64 _cell_measurement_theta_max 20.42 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method ? _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 5.013 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.219 _exptl_absorpt_correction_T_max 0.363 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q-scan _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 1.6 _diffrn_reflns_number 5345 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.96 _reflns_number_total 5345 _reflns_number_observed 4281 _reflns_observed_criterion >2\s(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction 'SDP (Frenz, 1983)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _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^)+(0.0416P)^2^+2.5038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 5345 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_obs 0.0314 _refine_ls_wR_factor_all 0.0823 _refine_ls_wR_factor_obs 0.0731 _refine_ls_goodness_of_fit_all 1.085 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.24259(2) 0.143327(12) 0.104410(11) 0.03585(7) Uani 1 d . . C1 C 0.1771(6) 0.1565(3) 0.2004(3) 0.0452(12) Uani 1 d . . O1 O 0.1358(5) 0.1621(3) 0.2564(2) 0.0625(12) Uani 1 d . . C2 C 0.0574(6) 0.1944(4) 0.0633(4) 0.059(2) Uani 1 d . . O2 O -0.0536(5) 0.2245(4) 0.0357(3) 0.101(2) Uani 1 d . . C3 C 0.1462(6) 0.0304(4) 0.0958(3) 0.0490(13) Uani 1 d . . O3 O 0.0848(5) -0.0359(3) 0.0895(3) 0.0779(14) Uani 1 d . . O11 O 0.3653(4) 0.2644(2) 0.1038(2) 0.0445(8) Uani 1 d . . O12 O 0.3059(7) 0.3241(4) 0.2050(3) 0.101(2) Uani 1 d . . C4 C 0.3761(5) 0.3238(3) 0.1532(3) 0.0373(10) Uani 1 d . . C11 C 0.4790(5) 0.3992(3) 0.1398(3) 0.0353(10) Uani 1 d . . C12 C 0.6325(5) 0.3922(3) 0.1654(3) 0.0405(11) Uani 1 d . . C13 C 0.7320(6) 0.4638(4) 0.1524(3) 0.0464(12) Uani 1 d . . C14 C 0.6720(6) 0.5377(4) 0.1149(3) 0.0508(13) Uani 1 d . . C15 C 0.5196(6) 0.5453(3) 0.0897(3) 0.0455(12) Uani 1 d . . C16 C 0.4198(5) 0.4749(3) 0.1028(2) 0.0376(10) Uani 1 d . . C17 C 0.4592(8) 0.6216(4) 0.0501(4) 0.060(2) Uani 1 d . . H17 H 0.5235(8) 0.6672(4) 0.0400(4) 0.063(5) Uiso 1 calc R . C18 C 0.3111(9) 0.6284(4) 0.0272(4) 0.073(2) Uani 1 d . . H18 H 0.2734(9) 0.6792(4) 0.0024(4) 0.063(5) Uiso 1 calc R . C19 C 0.2124(8) 0.5596(5) 0.0403(3) 0.068(2) Uani 1 d . . H19 H 0.1101(8) 0.5655(5) 0.0240(3) 0.063(5) Uiso 1 calc R . C110 C 0.2629(6) 0.4851(4) 0.0762(3) 0.0518(13) Uani 1 d . . H110 H 0.1955(6) 0.4401(4) 0.0836(3) 0.063(5) Uiso 1 calc R . C111 C 0.6957(7) 0.3163(4) 0.2044(3) 0.0548(14) Uani 1 d . . H111 H 0.6334(7) 0.2698(4) 0.2144(3) 0.063(5) Uiso 1 calc R . C112 C 0.8456(8) 0.3114(5) 0.2269(4) 0.078(2) Uani 1 d . . H112 H 0.8847(8) 0.2620(5) 0.2532(4) 0.063(5) Uiso 1 calc R . C113 C 0.9432(8) 0.3796(6) 0.2114(5) 0.086(3) Uani 1 d . . H113 H 1.0464(8) 0.3737(6) 0.2252(5) 0.063(5) Uiso 1 calc R . C114 C 0.8885(6) 0.4532(5) 0.1768(4) 0.070(2) Uani 1 d . . H114 H 0.9545(6) 0.4986(5) 0.1686(4) 0.063(5) Uiso 1 calc R . N21 N 0.3437(5) 0.1344(3) 0.0032(2) 0.0393(9) Uani 1 d . . N22 N 0.4698(4) 0.0961(3) 0.1383(2) 0.0344(8) Uani 1 d . . C21 C 0.2732(8) 0.1535(4) -0.0638(3) 0.059(2) Uani 1 d . . H21 H 0.1698(8) 0.1634(4) -0.0692(3) 0.063(5) Uiso 1 calc R . C22 C 0.3455(10) 0.1592(4) -0.1249(3) 0.070(2) Uani 1 d . . H22 H 0.2925(10) 0.1723(4) -0.1709(3) 0.063(5) Uiso 1 calc R . C23 C 0.4961(9) 0.1453(4) -0.1172(3) 0.066(2) Uani 1 d . . H23 H 0.5477(9) 0.1501(4) -0.1580(3) 0.063(5) Uiso 1 calc R . C24 C 0.5734(7) 0.1241(4) -0.0492(3) 0.0545(14) Uani 1 d . . H24 H 0.6766(7) 0.1135(4) -0.0437(3) 0.063(5) Uiso 1 calc R . C25 C 0.4937(6) 0.1191(3) 0.0108(3) 0.0384(11) Uani 1 d . . C26 C 0.5644(5) 0.0969(3) 0.0861(3) 0.0362(10) Uani 1 d . . C27 C 0.7138(5) 0.0758(4) 0.1036(3) 0.0511(13) Uani 1 d . . H27 H 0.7766(5) 0.0751(4) 0.0668(3) 0.063(5) Uiso 1 calc R . C28 C 0.7709(6) 0.0558(4) 0.1752(4) 0.060(2) Uani 1 d . . H28 H 0.8727(6) 0.0431(4) 0.1878(4) 0.063(5) Uiso 1 calc R . C29 C 0.6749(6) 0.0549(4) 0.2275(3) 0.058(2) Uani 1 d . . H29 H 0.7104(6) 0.0406(4) 0.2763(3) 0.063(5) Uiso 1 calc R . C210 C 0.5265(6) 0.0751(4) 0.2077(3) 0.0488(12) Uani 1 d . . H210 H 0.4623(6) 0.0743(4) 0.2438(3) 0.063(5) 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 Re 0.03455(10) 0.03180(10) 0.04247(11) 0.00077(9) 0.00983(7) -0.00045(8) C1 0.042(3) 0.043(3) 0.052(3) 0.005(2) 0.013(2) 0.006(2) O1 0.072(3) 0.063(3) 0.060(3) 0.013(2) 0.035(2) 0.018(2) C2 0.047(3) 0.047(3) 0.082(4) 0.006(3) 0.008(3) 0.008(3) O2 0.058(3) 0.103(4) 0.137(5) 0.030(4) -0.003(3) 0.030(3) C3 0.037(2) 0.043(3) 0.069(4) 0.000(3) 0.015(2) 0.000(2) O3 0.068(3) 0.045(2) 0.125(4) -0.011(3) 0.029(3) -0.020(2) O11 0.055(2) 0.033(2) 0.049(2) -0.006(2) 0.024(2) -0.009(2) O12 0.144(5) 0.104(4) 0.067(3) -0.040(3) 0.061(3) -0.067(4) C4 0.043(3) 0.040(2) 0.030(2) -0.004(2) 0.010(2) -0.005(2) C11 0.039(2) 0.031(2) 0.037(2) -0.007(2) 0.010(2) -0.001(2) C12 0.037(2) 0.040(3) 0.044(3) -0.009(2) 0.007(2) 0.005(2) C13 0.038(2) 0.050(3) 0.052(3) -0.018(3) 0.008(2) -0.005(2) C14 0.057(3) 0.044(3) 0.054(3) -0.015(3) 0.014(3) -0.014(3) C15 0.060(3) 0.033(3) 0.045(3) -0.009(2) 0.012(2) -0.006(2) C16 0.044(2) 0.037(2) 0.032(2) -0.005(2) 0.005(2) 0.001(2) C17 0.080(5) 0.037(3) 0.065(4) 0.003(3) 0.014(3) 0.004(3) C18 0.097(6) 0.046(4) 0.075(5) 0.007(3) 0.007(4) 0.018(4) C19 0.065(4) 0.079(5) 0.057(4) -0.003(3) -0.009(3) 0.024(4) C110 0.050(3) 0.056(3) 0.049(3) 0.000(3) 0.001(2) 0.001(3) C111 0.057(3) 0.045(3) 0.062(4) -0.003(3) 0.005(3) 0.012(3) C112 0.066(4) 0.075(5) 0.088(5) -0.010(4) -0.010(4) 0.033(4) C113 0.043(3) 0.098(6) 0.113(7) -0.029(5) -0.008(4) 0.023(4) C114 0.040(3) 0.084(5) 0.086(5) -0.030(4) 0.005(3) -0.009(3) N21 0.050(2) 0.035(2) 0.032(2) -0.003(2) 0.006(2) -0.003(2) N22 0.040(2) 0.033(2) 0.033(2) 0.000(2) 0.013(2) 0.000(2) C21 0.070(4) 0.056(4) 0.047(3) 0.006(3) -0.006(3) -0.010(3) C22 0.108(6) 0.063(4) 0.035(3) 0.006(3) -0.001(3) -0.017(4) C23 0.105(6) 0.061(4) 0.039(3) -0.005(3) 0.031(3) -0.018(4) C24 0.074(4) 0.044(3) 0.053(3) -0.003(2) 0.032(3) -0.001(3) C25 0.050(3) 0.027(2) 0.041(3) -0.002(2) 0.018(2) -0.003(2) C26 0.041(2) 0.027(2) 0.044(3) -0.001(2) 0.016(2) -0.004(2) C27 0.041(3) 0.053(3) 0.063(3) 0.006(3) 0.019(3) -0.003(2) C28 0.038(3) 0.067(4) 0.075(4) 0.009(3) 0.005(3) 0.005(3) C29 0.052(3) 0.072(4) 0.051(3) 0.018(3) 0.004(3) 0.004(3) C210 0.050(3) 0.060(3) 0.037(3) 0.009(3) 0.009(2) -0.001(3) _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 Re C2 1.892(6) . ? Re C3 1.907(6) . ? Re C1 1.930(6) . ? Re O11 2.132(3) . ? Re N21 2.165(4) . ? Re N22 2.167(4) . ? C1 O1 1.134(6) . ? C2 O2 1.147(7) . ? C3 O3 1.140(6) . ? O11 C4 1.267(6) . ? O12 C4 1.201(6) . ? C4 C11 1.504(7) . ? C11 C12 1.396(6) . ? C11 C16 1.395(7) . ? C12 C111 1.426(8) . ? C12 C13 1.440(7) . ? C13 C14 1.380(8) . ? C13 C114 1.422(7) . ? C14 C15 1.386(8) . ? C15 C17 1.428(8) . ? C15 C16 1.428(7) . ? C16 C110 1.433(7) . ? C17 C18 1.340(10) . ? C18 C19 1.404(10) . ? C19 C110 1.348(8) . ? C111 C112 1.353(8) . ? C112 C113 1.403(11) . ? C113 C114 1.337(10) . ? N21 C21 1.332(7) . ? N21 C25 1.352(6) . ? N22 C210 1.339(6) . ? N22 C26 1.355(6) . ? C21 C22 1.364(10) . ? C22 C23 1.353(10) . ? C23 C24 1.377(9) . ? C24 C25 1.385(7) . ? C25 C26 1.475(7) . ? C26 C27 1.371(7) . ? C27 C28 1.374(8) . ? C28 C29 1.366(8) . ? C29 C210 1.364(7) . ? 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 Re C3 88.2(2) . . ? C2 Re C1 87.9(3) . . ? C3 Re C1 88.8(2) . . ? C2 Re O11 94.2(2) . . ? C3 Re O11 173.1(2) . . ? C1 Re O11 97.7(2) . . ? C2 Re N21 97.4(2) . . ? C3 Re N21 96.3(2) . . ? C1 Re N21 172.7(2) . . ? O11 Re N21 77.01(14) . . ? C2 Re N22 171.1(2) . . ? C3 Re N22 97.3(2) . . ? C1 Re N22 99.2(2) . . ? O11 Re N22 79.55(14) . . ? N21 Re N22 75.06(15) . . ? O1 C1 Re 177.9(5) . . ? O2 C2 Re 177.3(6) . . ? O3 C3 Re 177.9(5) . . ? C4 O11 Re 126.4(3) . . ? O12 C4 O11 124.3(5) . . ? O12 C4 C11 121.4(5) . . ? O11 C4 C11 114.2(4) . . ? C12 C11 C16 121.2(4) . . ? C12 C11 C4 119.0(4) . . ? C16 C11 C4 119.8(4) . . ? C11 C12 C111 122.5(5) . . ? C11 C12 C13 119.4(5) . . ? C111 C12 C13 118.1(5) . . ? C14 C13 C114 123.4(6) . . ? C14 C13 C12 118.7(5) . . ? C114 C13 C12 118.0(6) . . ? C13 C14 C15 122.2(5) . . ? C14 C15 C17 121.7(5) . . ? C14 C15 C16 119.5(5) . . ? C17 C15 C16 118.8(5) . . ? C11 C16 C15 118.9(4) . . ? C11 C16 C110 123.0(5) . . ? C15 C16 C110 118.0(5) . . ? C18 C17 C15 120.8(6) . . ? C17 C18 C19 120.6(6) . . ? C110 C19 C18 121.4(6) . . ? C19 C110 C16 120.4(6) . . ? C112 C111 C12 120.6(6) . . ? C111 C112 C113 121.1(7) . . ? C114 C113 C112 120.4(6) . . ? C113 C114 C13 121.8(7) . . ? C21 N21 C25 118.4(5) . . ? C21 N21 Re 124.7(4) . . ? C25 N21 Re 116.3(3) . . ? C210 N22 C26 118.2(4) . . ? C210 N22 Re 125.0(3) . . ? C26 N22 Re 116.4(3) . . ? N21 C21 C22 123.1(6) . . ? C23 C22 C21 118.5(6) . . ? C22 C23 C24 120.4(6) . . ? C23 C24 C25 118.4(6) . . ? N21 C25 C24 121.1(5) . . ? N21 C25 C26 115.7(4) . . ? C24 C25 C26 123.2(5) . . ? N22 C26 C27 121.0(5) . . ? N22 C26 C25 115.2(4) . . ? C27 C26 C25 123.7(4) . . ? C26 C27 C28 120.1(5) . . ? C29 C28 C27 118.6(5) . . ? C210 C29 C28 119.5(5) . . ? N22 C210 C29 122.6(5) . . ? _refine_diff_density_max 1.676 _refine_diff_density_min -1.582 _refine_diff_density_rms 0.115 #===END