Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Michael William George' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham Nottinghamshire NG7 2RD UNITED KINGDOM ; _publ_contact_author_email mike.george@nottingham.ac.uk _publ_section_title ; Using Picosecond and Nanosecond Time-resolved Infrared Spectroscopy for the Investigation of Excited States and Reaction Intermediates of Inorganic Systems ; loop_ _publ_author_name 'Marina K. Kuimova' 'Wassim Alsindi' 'Joanne Dyer' 'David C. Grills' 'Omar Jina' 'Pavel Matousek' 'Anthony W. Parker' 'Peter Portius' 'Xue Zhong Sun' 'Michael Towrie' 'Claire Wilson' 'Jixin Yang' 'Michael W. George' data_recocl _database_code_CSD 212244 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H12 Cl3 N4 O3.50 Re' _chemical_formula_weight 692.92 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 19.958(2) _cell_length_b 18.054(2) _cell_length_c 13.530(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.562(2) _cell_angle_gamma 90.00 _cell_volume 4360.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7240 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.5 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 5.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details 'Sadabs v2.03, Bruker 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13248 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4906 _reflns_number_gt 4176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _refine_special_details ; THF molecule included in lattice. Half occupied as symmetry generates a second site in the same region. ; _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^)+(0.0376P)^2^+14.1501P] 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 model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4906 _refine_ls_number_parameters 334 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _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 -0.341515(8) 0.658919(8) 0.580741(12) 0.02144(6) Uani 1 1 d . . . Cl1 Cl 0.25293(6) 0.39994(6) 1.06478(9) 0.0313(2) Uani 1 1 d . . . Cl2 Cl 0.16113(6) 0.25243(6) 1.01848(10) 0.0346(2) Uani 1 1 d . . . Cl3 Cl -0.30748(7) 0.60651(5) 0.44010(8) 0.0336(2) Uani 1 1 d . . . C1C C -0.3622(2) 0.7575(2) 0.5204(3) 0.0241(8) Uani 1 1 d . . . O1C O -0.37438(18) 0.81703(17) 0.4872(3) 0.0315(7) Uani 1 1 d . . . C2C C -0.4454(3) 0.6384(3) 0.4948(5) 0.0478(14) Uani 1 1 d . . . O2C O -0.5086(2) 0.6282(3) 0.4427(5) 0.093(2) Uani 1 1 d . . . O3C O -0.3790(3) 0.7197(3) 0.7603(4) 0.0836(18) Uani 1 1 d . . . C3C C -0.3636(3) 0.6955(3) 0.6961(4) 0.0441(13) Uani 1 1 d . . . C1 C -0.2358(2) 0.4105(2) 0.7250(3) 0.0253(8) Uani 1 1 d . . . H1A H -0.2138 0.3631 0.7485 0.030 Uiso 1 1 calc R . . C2 C -0.3125(2) 0.4185(2) 0.6721(4) 0.0299(9) Uani 1 1 d . . . H2A H -0.3440 0.3767 0.6602 0.036 Uiso 1 1 calc R . . C3 C -0.3435(2) 0.4883(2) 0.6362(4) 0.0275(9) Uani 1 1 d . . . H3A H -0.3965 0.4930 0.5994 0.033 Uiso 1 1 calc R . . N4 N -0.30155(18) 0.54912(17) 0.6516(3) 0.0205(6) Uani 1 1 d . . . C4A C -0.2257(2) 0.5414(2) 0.7054(3) 0.0192(7) Uani 1 1 d . . . C4B C -0.1824(2) 0.60899(19) 0.7221(3) 0.0167(7) Uani 1 1 d . . . N5 N -0.22153(19) 0.67190(17) 0.6787(3) 0.0182(6) Uani 1 1 d . . . C6 C -0.1834(2) 0.7356(2) 0.6945(3) 0.0225(8) Uani 1 1 d . . . H6A H -0.2103 0.7797 0.6628 0.027 Uiso 1 1 calc R . . C7 C -0.1062(2) 0.7393(2) 0.7556(3) 0.0235(8) Uani 1 1 d . . . H7A H -0.0812 0.7856 0.7669 0.028 Uiso 1 1 calc R . . C8B C -0.0666(2) 0.5377(2) 0.8213(3) 0.0171(7) Uani 1 1 d . . . C8 C -0.0658(2) 0.6756(2) 0.7997(3) 0.0208(8) Uani 1 1 d . . . H8A H -0.0129 0.6773 0.8412 0.025 Uiso 1 1 calc R . . C8A C -0.1045(2) 0.6081(2) 0.7821(3) 0.0174(7) Uani 1 1 d . . . N9 N 0.00774(18) 0.53832(17) 0.8751(2) 0.0192(6) Uani 1 1 d . . . C9A C 0.0419(2) 0.4716(2) 0.9068(3) 0.0191(7) Uani 1 1 d . . . C10 C 0.1216(2) 0.4694(2) 0.9644(3) 0.0219(8) Uani 1 1 d . . . H10A H 0.1499 0.5140 0.9802 0.026 Uiso 1 1 calc R . . C11 C 0.1569(2) 0.4028(2) 0.9963(3) 0.0228(8) Uani 1 1 d . . . C12 C 0.1149(2) 0.3355(2) 0.9737(3) 0.0228(8) Uani 1 1 d . . . C13 C 0.0383(2) 0.3364(2) 0.9184(3) 0.0240(8) Uani 1 1 d . . . H13A H 0.0110 0.2913 0.9029 0.029 Uiso 1 1 calc R . . C13A C 0.0002(2) 0.4044(2) 0.8843(3) 0.0194(7) Uani 1 1 d . . . N14 N -0.07562(18) 0.40472(17) 0.8310(3) 0.0207(7) Uani 1 1 d . . . C14B C -0.1907(2) 0.4737(2) 0.7437(3) 0.0192(7) Uani 1 1 d . . . C14A C -0.1087(2) 0.4705(2) 0.8003(3) 0.0182(7) Uani 1 1 d . . . O1S O -0.4979(5) 0.4807(4) 0.3751(6) 0.054(2) Uani 0.50 1 d PD A -1 C2S C -0.5204(7) 0.5216(6) 0.2742(8) 0.054(3) Uani 0.50 1 d PD A -1 H2SA H -0.4794 0.5543 0.2787 0.065 Uiso 0.50 1 calc PR A -1 H2SB H -0.5649 0.5524 0.2597 0.065 Uiso 0.50 1 calc PR A -1 C3S C -0.5394(7) 0.4632(6) 0.1806(11) 0.073(5) Uani 0.50 1 d PD A -1 H3SA H -0.5898 0.4413 0.1565 0.087 Uiso 0.50 1 calc PR A -1 H3SB H -0.5347 0.4836 0.1161 0.087 Uiso 0.50 1 calc PR A -1 C4S C -0.4765(7) 0.4083(7) 0.2470(9) 0.062(3) Uani 0.50 1 d PD A -1 H4SA H -0.4331 0.4161 0.2312 0.075 Uiso 0.50 1 calc PR A -1 H4SB H -0.4943 0.3567 0.2271 0.075 Uiso 0.50 1 calc PR A -1 C5S C -0.4538(5) 0.4228(5) 0.3706(7) 0.037(2) Uani 0.50 1 d PD A -1 H5SB H -0.4624 0.3779 0.4055 0.044 Uiso 0.50 1 calc PR A -1 H5SA H -0.4001 0.4362 0.4101 0.044 Uiso 0.50 1 calc PR A -1 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 0.01385(9) 0.02261(9) 0.02257(9) 0.00675(6) 0.00340(7) 0.00157(6) Cl1 0.0165(5) 0.0380(6) 0.0321(5) 0.0031(4) 0.0044(4) 0.0065(4) Cl2 0.0279(6) 0.0278(5) 0.0433(6) 0.0055(4) 0.0116(5) 0.0112(4) Cl3 0.0500(7) 0.0220(5) 0.0243(5) 0.0011(4) 0.0126(5) 0.0003(5) C1C 0.018(2) 0.028(2) 0.0220(19) 0.0027(16) 0.0047(16) 0.0017(16) O1C 0.0316(18) 0.0247(14) 0.0329(16) 0.0053(13) 0.0097(14) 0.0056(13) C2C 0.023(3) 0.037(3) 0.060(3) 0.026(2) -0.002(2) -0.004(2) O2C 0.017(2) 0.064(3) 0.138(5) 0.054(3) -0.019(2) -0.0100(19) O3C 0.102(4) 0.115(4) 0.057(3) 0.047(3) 0.057(3) 0.077(3) C3C 0.040(3) 0.057(3) 0.041(3) 0.028(2) 0.023(2) 0.029(3) C1 0.021(2) 0.0221(19) 0.026(2) 0.0071(15) 0.0045(17) -0.0020(16) C2 0.021(2) 0.028(2) 0.031(2) 0.0098(17) 0.0031(18) -0.0066(17) C3 0.0160(19) 0.030(2) 0.031(2) 0.0071(17) 0.0060(17) -0.0043(17) N4 0.0146(16) 0.0211(15) 0.0219(15) 0.0058(12) 0.0047(13) -0.0020(13) C4A 0.0164(18) 0.0228(18) 0.0159(16) 0.0027(14) 0.0051(15) -0.0023(15) C4B 0.0190(18) 0.0150(16) 0.0160(16) 0.0020(13) 0.0079(15) 0.0006(14) N5 0.0169(16) 0.0183(15) 0.0170(15) 0.0001(12) 0.0055(13) 0.0020(12) C6 0.024(2) 0.0161(17) 0.0253(19) -0.0017(14) 0.0092(17) 0.0019(15) C7 0.021(2) 0.0182(17) 0.0268(19) -0.0022(15) 0.0072(17) -0.0037(15) C8B 0.0160(18) 0.0190(17) 0.0145(16) 0.0002(13) 0.0052(14) -0.0021(14) C8 0.0168(19) 0.0213(18) 0.0199(18) -0.0033(14) 0.0043(16) -0.0035(15) C8A 0.0155(18) 0.0187(17) 0.0177(17) 0.0002(14) 0.0071(15) -0.0011(14) N9 0.0150(15) 0.0221(15) 0.0171(14) 0.0030(12) 0.0040(13) 0.0016(12) C9A 0.0177(19) 0.0224(17) 0.0169(17) 0.0021(14) 0.0074(15) 0.0002(15) C10 0.0161(18) 0.0250(18) 0.0216(18) 0.0019(15) 0.0057(15) -0.0002(15) C11 0.0153(19) 0.033(2) 0.0174(17) 0.0018(15) 0.0049(15) 0.0032(16) C12 0.023(2) 0.0249(19) 0.0193(18) 0.0032(15) 0.0086(17) 0.0085(16) C13 0.024(2) 0.0212(19) 0.0243(19) 0.0008(15) 0.0089(18) 0.0015(16) C13A 0.0185(19) 0.0207(17) 0.0155(16) 0.0013(14) 0.0045(15) 0.0025(15) N14 0.0182(16) 0.0216(15) 0.0189(15) 0.0025(12) 0.0052(13) 0.0011(13) C14B 0.0142(18) 0.0224(18) 0.0172(17) 0.0029(14) 0.0038(15) -0.0017(15) C14A 0.0144(18) 0.0213(17) 0.0155(16) 0.0011(14) 0.0035(14) -0.0004(15) O1S 0.051(5) 0.073(5) 0.036(4) 0.017(4) 0.015(4) 0.002(4) C2S 0.056(8) 0.055(7) 0.054(7) 0.018(6) 0.027(6) 0.008(6) C3S 0.046(7) 0.069(9) 0.076(10) 0.050(8) 0.003(7) -0.013(7) C4S 0.066(10) 0.064(7) 0.071(8) 0.011(7) 0.043(8) 0.008(7) C5S 0.033(5) 0.054(6) 0.018(4) 0.017(4) 0.007(4) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2C 1.906(5) . ? Re1 C3C 1.919(5) . ? Re1 C1C 1.924(4) . ? Re1 N5 2.170(3) . ? Re1 N4 2.191(3) . ? Re1 Cl3 2.4766(11) . ? Cl1 C11 1.717(4) . ? Cl2 C12 1.723(4) . ? C1C O1C 1.148(5) . ? C2C O2C 1.151(6) . ? O3C C3C 1.131(6) . ? C1 C2 1.377(6) . ? C1 C14B 1.405(5) . ? C2 C3 1.393(6) . ? C3 N4 1.340(5) . ? N4 C4A 1.362(5) . ? C4A C14B 1.388(5) . ? C4A C4B 1.453(5) . ? C4B N5 1.354(5) . ? C4B C8A 1.395(5) . ? N5 C6 1.342(5) . ? C6 C7 1.387(6) . ? C7 C8 1.377(5) . ? C8B N9 1.329(5) . ? C8B C14A 1.430(5) . ? C8B C8A 1.453(5) . ? C8 C8A 1.405(5) . ? N9 C9A 1.355(5) . ? C9A C13A 1.426(5) . ? C9A C10 1.426(5) . ? C10 C11 1.363(6) . ? C11 C12 1.429(6) . ? C12 C13 1.369(6) . ? C13 C13A 1.408(5) . ? C13A N14 1.354(5) . ? N14 C14A 1.332(5) . ? C14B C14A 1.465(5) . ? O1S C5S 1.386(7) . ? O1S C2S 1.436(7) . ? C2S C3S 1.558(14) . ? C3S C4S 1.535(12) . ? C4S C5S 1.548(12) . ? 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 C2C Re1 C3C 88.9(3) . . ? C2C Re1 C1C 87.29(19) . . ? C3C Re1 C1C 86.76(19) . . ? C2C Re1 N5 174.96(18) . . ? C3C Re1 N5 93.33(19) . . ? C1C Re1 N5 97.34(15) . . ? C2C Re1 N4 100.07(17) . . ? C3C Re1 N4 97.29(17) . . ? C1C Re1 N4 171.63(15) . . ? N5 Re1 N4 75.17(12) . . ? C2C Re1 Cl3 93.1(2) . . ? C3C Re1 Cl3 176.53(14) . . ? C1C Re1 Cl3 96.17(12) . . ? N5 Re1 Cl3 84.46(9) . . ? N4 Re1 Cl3 79.57(9) . . ? O1C C1C Re1 178.0(4) . . ? O2C C2C Re1 178.0(5) . . ? O3C C3C Re1 176.4(4) . . ? C2 C1 C14B 118.8(4) . . ? C1 C2 C3 119.7(4) . . ? N4 C3 C2 122.5(4) . . ? C3 N4 C4A 117.9(3) . . ? C3 N4 Re1 126.4(3) . . ? C4A N4 Re1 115.2(2) . . ? N4 C4A C14B 122.9(3) . . ? N4 C4A C4B 116.0(3) . . ? C14B C4A C4B 121.1(3) . . ? N5 C4B C8A 122.6(3) . . ? N5 C4B C4A 116.7(3) . . ? C8A C4B C4A 120.7(3) . . ? C6 N5 C4B 118.2(3) . . ? C6 N5 Re1 125.6(3) . . ? C4B N5 Re1 116.0(2) . . ? N5 C6 C7 122.5(4) . . ? C8 C7 C6 119.7(4) . . ? N9 C8B C14A 122.0(3) . . ? N9 C8B C8A 117.6(3) . . ? C14A C8B C8A 120.4(3) . . ? C7 C8 C8A 118.7(4) . . ? C4B C8A C8 118.2(3) . . ? C4B C8A C8B 119.0(3) . . ? C8 C8A C8B 122.7(3) . . ? C8B N9 C9A 116.5(3) . . ? N9 C9A C13A 121.7(3) . . ? N9 C9A C10 118.5(3) . . ? C13A C9A C10 119.7(3) . . ? C11 C10 C9A 119.3(4) . . ? C10 C11 C12 120.8(4) . . ? C10 C11 Cl1 119.4(3) . . ? C12 C11 Cl1 119.7(3) . . ? C13 C12 C11 120.8(4) . . ? C13 C12 Cl2 119.6(3) . . ? C11 C12 Cl2 119.6(3) . . ? C12 C13 C13A 119.8(4) . . ? N14 C13A C13 119.3(3) . . ? N14 C13A C9A 121.1(3) . . ? C13 C13A C9A 119.6(4) . . ? C14A N14 C13A 116.8(3) . . ? C4A C14B C1 118.3(4) . . ? C4A C14B C14A 119.2(3) . . ? C1 C14B C14A 122.5(3) . . ? N14 C14A C8B 121.9(3) . . ? N14 C14A C14B 118.8(3) . . ? C8B C14A C14B 119.3(3) . . ? C5S O1S C2S 106.3(8) . . ? O1S C2S C3S 106.5(8) . . ? C4S C3S C2S 97.1(9) . . ? C3S C4S C5S 106.9(9) . . ? O1S C5S C4S 106.9(7) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.087 _refine_diff_density_min -1.574 _refine_diff_density_rms 0.132