# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _publ_contact_author_name 'Biing-Chiau Tzeng' _publ_contact_author_address ; Chemistry and Biochemistry National Chung Cheng University 168, University Rd. Min-Hsiung Chia-Yi 621 TAIWAN ; _publ_section_title ; Anion...pi Interactions Existing in Re(I) and Pd(II) Complexes ; _publ_contact_author_email CHEBCT@CCU.EDU.TW loop_ _publ_author_name 'Biing-Chiau Tzeng' 'Gene-Hsiang Lee' 'Shie-Ming Peng' 'Ya-Ling Wu' # Attachment '1.CF3SO3.cif' data_ic11216 _database_code_depnum_ccdc_archive 'CCDC 622767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 F3 N2 O18 Re3 S4' _chemical_formula_weight 1276.04 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2003(4) _cell_length_b 16.5780(8) _cell_length_c 20.4180(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.307(1) _cell_angle_gamma 90.00 _cell_volume 3053.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 3168 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.90 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 12.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1499 _exptl_absorpt_correction_T_max 0.2612 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23266 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7002 _reflns_number_gt 5876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0174P)^2^+4.3156P] 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 7002 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.23853(3) 0.152771(17) -0.051973(14) 0.01644(8) Uani 1 1 d . . . Re2 Re -0.22715(3) 0.364777(17) 0.036150(14) 0.01650(8) Uani 1 1 d . . . Re3 Re 0.21218(3) 0.509924(17) 0.267220(14) 0.01656(8) Uani 1 1 d . . . S1 S 0.3392(2) 0.20665(11) 0.06275(9) 0.0204(4) Uani 1 1 d . . . S2 S 0.2668(2) 0.34478(11) 0.14493(9) 0.0186(4) Uani 1 1 d . . . S3 S 0.0323(2) 0.46988(11) 0.16390(10) 0.0237(4) Uani 1 1 d . . . O1 O 0.5588(6) 0.1788(4) -0.0793(3) 0.0341(14) Uani 1 1 d . . . O2 O 0.3319(7) -0.0174(3) 0.0064(3) 0.0417(16) Uani 1 1 d . . . O3 O 0.1219(7) 0.0848(4) -0.1931(3) 0.0382(15) Uani 1 1 d . . . O4 O -0.0850(6) 0.1253(3) -0.0293(3) 0.0313(14) Uani 1 1 d . . . O5 O 0.1506(6) 0.3276(3) -0.1058(3) 0.0328(14) Uani 1 1 d . . . O6 O 0.3033(7) 0.3355(3) 0.3166(3) 0.0370(15) Uani 1 1 d . . . O7 O 0.4376(7) 0.5242(4) 0.1698(3) 0.0417(16) Uani 1 1 d . . . O8 O 0.4363(7) 0.5631(4) 0.3920(3) 0.0454(17) Uani 1 1 d . . . O9 O 0.1121(7) 0.6911(3) 0.2427(3) 0.0339(14) Uani 1 1 d . . . O10 O -0.0443(7) 0.4948(4) 0.3469(3) 0.0431(17) Uani 1 1 d . . . O11 O -0.1661(6) 0.5439(3) 0.0041(3) 0.0330(14) Uani 1 1 d . . . O12 O -0.3210(7) 0.4034(4) 0.1730(3) 0.0449(17) Uani 1 1 d . . . O13 O -0.5549(6) 0.3886(4) -0.0292(3) 0.0515(19) Uani 1 1 d . . . O14 O -0.2714(6) 0.1808(3) 0.0656(3) 0.0325(14) Uani 1 1 d . . . O15 O -0.1649(6) 0.3175(4) -0.1036(3) 0.0370(15) Uani 1 1 d . . . N1 N 0.0056(6) 0.3474(3) 0.0777(3) 0.0159(13) Uani 1 1 d . . . N2 N 0.0761(6) 0.2849(3) 0.0500(3) 0.0143(12) Uani 1 1 d . . . C1 C 0.4440(8) 0.1698(5) -0.0712(4) 0.0218(17) Uani 1 1 d . . . C2 C 0.2972(8) 0.0435(5) -0.0151(4) 0.0236(17) Uani 1 1 d . . . C3 C 0.1679(8) 0.1094(5) -0.1414(4) 0.0218(17) Uani 1 1 d . . . C4 C 0.0330(9) 0.1369(5) -0.0336(4) 0.0237(17) Uani 1 1 d . . . C5 C 0.1815(8) 0.2655(5) -0.0865(4) 0.0250(18) Uani 1 1 d . . . C6 C 0.2686(9) 0.3960(5) 0.2953(4) 0.0231(17) Uani 1 1 d . . . C7 C 0.3618(9) 0.5190(4) 0.2069(4) 0.0239(17) Uani 1 1 d . . . C8 C 0.3519(9) 0.5464(5) 0.3462(4) 0.0251(18) Uani 1 1 d . . . C9 C 0.1495(9) 0.6258(5) 0.2486(4) 0.0231(17) Uani 1 1 d . . . C10 C 0.0481(9) 0.4994(5) 0.3181(4) 0.0249(18) Uani 1 1 d . . . C11 C -0.1884(8) 0.4797(5) 0.0174(4) 0.0224(17) Uani 1 1 d . . . C12 C -0.2796(8) 0.3907(5) 0.1257(4) 0.0256(18) Uani 1 1 d . . . C13 C -0.4342(9) 0.3788(5) -0.0048(4) 0.0292(19) Uani 1 1 d . . . C14 C -0.2555(8) 0.2464(5) 0.0555(4) 0.0226(17) Uani 1 1 d . . . C15 C -0.1852(8) 0.3349(5) -0.0525(4) 0.0232(17) Uani 1 1 d . . . C16 C 0.2108(8) 0.2763(4) 0.0799(3) 0.0155(15) Uani 1 1 d . . . C17 C 0.0913(8) 0.3862(4) 0.1269(3) 0.0166(15) Uani 1 1 d . . . S4 S 0.4234(2) 0.27165(12) -0.24570(10) 0.0282(5) Uani 1 1 d . . . O16 O 0.5535(7) 0.3111(4) -0.2130(4) 0.060(2) Uani 1 1 d . . . O17 O 0.4297(9) 0.2398(4) -0.3097(3) 0.062(2) Uani 1 1 d . . . O18 O 0.3522(9) 0.2218(5) -0.2051(3) 0.070(2) Uani 1 1 d . . . C18 C 0.2921(10) 0.3549(6) -0.2662(5) 0.042(2) Uani 1 1 d . . . F1 F 0.3387(6) 0.4092(3) -0.3053(3) 0.0542(15) Uani 1 1 d . . . F2 F 0.2678(7) 0.3942(4) -0.2136(3) 0.0713(19) Uani 1 1 d . . . F3 F 0.1602(6) 0.3293(4) -0.2992(3) 0.0686(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01567(16) 0.01820(15) 0.01595(15) -0.00328(11) 0.00433(12) -0.00036(12) Re2 0.01225(15) 0.01888(15) 0.01809(15) -0.00191(11) 0.00231(12) 0.00150(11) Re3 0.01860(16) 0.01477(14) 0.01625(15) -0.00287(11) 0.00326(12) -0.00111(12) S1 0.0178(10) 0.0236(10) 0.0188(9) -0.0048(8) 0.0009(8) 0.0062(8) S2 0.0158(9) 0.0185(9) 0.0186(9) -0.0061(7) -0.0036(7) 0.0034(7) S3 0.0230(11) 0.0194(10) 0.0255(10) -0.0093(8) -0.0030(8) 0.0069(8) O1 0.019(3) 0.048(4) 0.035(3) 0.007(3) 0.003(3) -0.003(3) O2 0.043(4) 0.020(3) 0.061(4) 0.005(3) 0.006(3) 0.002(3) O3 0.043(4) 0.051(4) 0.022(3) -0.016(3) 0.009(3) -0.018(3) O4 0.024(3) 0.039(4) 0.033(3) -0.004(3) 0.011(3) -0.009(3) O5 0.038(4) 0.021(3) 0.039(3) 0.003(3) 0.007(3) 0.004(3) O6 0.060(4) 0.023(3) 0.026(3) -0.001(3) 0.005(3) 0.008(3) O7 0.050(4) 0.032(4) 0.050(4) -0.015(3) 0.029(3) -0.010(3) O8 0.037(4) 0.065(5) 0.029(3) -0.021(3) -0.006(3) -0.001(3) O9 0.048(4) 0.020(3) 0.038(3) 0.002(3) 0.020(3) 0.002(3) O10 0.037(4) 0.045(4) 0.052(4) 0.019(3) 0.022(3) 0.003(3) O11 0.038(4) 0.025(3) 0.040(4) 0.004(3) 0.016(3) 0.005(3) O12 0.044(4) 0.065(5) 0.031(4) -0.002(3) 0.020(3) 0.010(3) O13 0.013(3) 0.071(5) 0.066(5) 0.000(4) -0.003(3) 0.007(3) O14 0.045(4) 0.025(3) 0.028(3) -0.007(3) 0.009(3) -0.008(3) O15 0.037(4) 0.057(4) 0.018(3) -0.010(3) 0.008(3) -0.004(3) N1 0.019(3) 0.016(3) 0.014(3) -0.005(2) 0.003(3) -0.002(2) N2 0.013(3) 0.017(3) 0.014(3) -0.003(2) 0.005(2) 0.004(2) C1 0.015(4) 0.025(4) 0.023(4) -0.002(3) -0.001(3) 0.003(3) C2 0.017(4) 0.028(5) 0.026(4) -0.002(3) 0.007(3) -0.003(3) C3 0.013(4) 0.026(4) 0.029(4) 0.000(3) 0.011(3) -0.006(3) C4 0.028(5) 0.024(4) 0.018(4) -0.002(3) 0.000(3) -0.002(4) C5 0.017(4) 0.030(5) 0.028(4) -0.004(4) 0.004(3) -0.002(3) C6 0.032(5) 0.021(4) 0.014(4) -0.004(3) 0.000(3) 0.001(4) C7 0.026(4) 0.018(4) 0.029(4) -0.003(3) 0.007(4) 0.000(3) C8 0.020(4) 0.034(5) 0.022(4) -0.012(3) 0.009(4) 0.004(4) C9 0.027(5) 0.025(4) 0.019(4) -0.003(3) 0.009(3) -0.004(3) C10 0.020(4) 0.026(4) 0.028(4) 0.009(3) 0.003(4) 0.002(3) C11 0.017(4) 0.028(4) 0.022(4) 0.001(3) 0.004(3) 0.007(3) C12 0.015(4) 0.025(4) 0.039(5) 0.005(4) 0.009(4) 0.005(3) C13 0.022(5) 0.031(5) 0.034(5) -0.006(4) 0.004(4) -0.001(4) C14 0.019(4) 0.024(4) 0.025(4) -0.007(3) 0.005(3) 0.000(3) C15 0.008(4) 0.029(4) 0.031(5) -0.004(3) -0.001(3) 0.003(3) C16 0.020(4) 0.011(3) 0.016(3) -0.006(3) 0.007(3) -0.002(3) C17 0.014(4) 0.018(4) 0.016(4) 0.000(3) -0.003(3) 0.001(3) S4 0.0326(12) 0.0237(10) 0.0271(11) -0.0019(9) 0.0032(9) -0.0072(9) O16 0.034(4) 0.032(4) 0.108(6) -0.006(4) -0.004(4) -0.003(3) O17 0.091(6) 0.045(4) 0.051(4) -0.009(4) 0.015(4) 0.022(4) O18 0.091(6) 0.069(5) 0.045(4) 0.018(4) -0.001(4) -0.020(5) C18 0.026(5) 0.059(7) 0.042(6) -0.006(5) 0.008(4) -0.012(5) F1 0.047(4) 0.041(3) 0.079(4) 0.010(3) 0.022(3) 0.007(3) F2 0.069(5) 0.081(5) 0.069(4) -0.021(4) 0.028(4) 0.008(4) F3 0.033(3) 0.105(6) 0.066(4) 0.000(4) 0.004(3) -0.012(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 Re1 C3 1.952(8) . ? Re1 C2 1.994(8) . ? Re1 C4 2.016(8) . ? Re1 C1 2.024(8) . ? Re1 C5 2.030(8) . ? Re1 S1 2.5083(18) . ? Re2 C13 1.939(8) . ? Re2 C15 1.986(8) . ? Re2 C11 1.989(8) . ? Re2 C12 2.027(9) . ? Re2 C14 2.029(8) . ? Re2 N1 2.162(6) . ? Re3 C8 1.951(8) . ? Re3 C10 2.000(8) . ? Re3 C6 2.012(8) . ? Re3 C9 2.021(8) . ? Re3 C7 2.024(8) . ? Re3 S3 2.5022(18) . ? S1 C16 1.736(7) . ? S2 C17 1.726(7) . ? S2 C16 1.747(7) . ? S3 C17 1.717(7) . ? O1 C1 1.111(8) . ? O2 C2 1.123(9) . ? O3 C3 1.133(9) . ? O4 C4 1.123(9) . ? O5 C5 1.118(9) . ? O6 C6 1.114(9) . ? O7 C7 1.129(9) . ? O8 C8 1.128(9) . ? O9 C9 1.134(9) . ? O10 C10 1.127(9) . ? O11 C11 1.127(9) . ? O12 C12 1.126(9) . ? O13 C13 1.136(9) . ? O14 C14 1.121(9) . ? O15 C15 1.132(9) . ? N1 C17 1.317(8) . ? N1 N2 1.400(7) . ? N2 C16 1.278(8) . ? S4 O16 1.411(6) . ? S4 O18 1.418(7) . ? S4 O17 1.421(7) . ? S4 C18 1.828(10) . ? C18 F2 1.314(11) . ? C18 F1 1.328(11) . ? C18 F3 1.337(10) . ? 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 Re1 C2 92.0(3) . . ? C3 Re1 C4 88.5(3) . . ? C2 Re1 C4 90.3(3) . . ? C3 Re1 C1 91.3(3) . . ? C2 Re1 C1 90.3(3) . . ? C4 Re1 C1 179.4(3) . . ? C3 Re1 C5 89.9(3) . . ? C2 Re1 C5 178.1(3) . . ? C4 Re1 C5 89.8(3) . . ? C1 Re1 C5 89.6(3) . . ? C3 Re1 S1 177.8(2) . . ? C2 Re1 S1 87.0(2) . . ? C4 Re1 S1 93.4(2) . . ? C1 Re1 S1 86.8(2) . . ? C5 Re1 S1 91.1(2) . . ? C13 Re2 C15 89.2(3) . . ? C13 Re2 C11 90.0(3) . . ? C15 Re2 C11 89.4(3) . . ? C13 Re2 C12 88.6(3) . . ? C15 Re2 C12 176.7(3) . . ? C11 Re2 C12 93.1(3) . . ? C13 Re2 C14 92.7(3) . . ? C15 Re2 C14 89.6(3) . . ? C11 Re2 C14 177.1(3) . . ? C12 Re2 C14 88.1(3) . . ? C13 Re2 N1 177.5(3) . . ? C15 Re2 N1 88.3(2) . . ? C11 Re2 N1 90.1(3) . . ? C12 Re2 N1 93.8(3) . . ? C14 Re2 N1 87.1(3) . . ? C8 Re3 C10 92.3(3) . . ? C8 Re3 C6 87.9(3) . . ? C10 Re3 C6 87.1(3) . . ? C8 Re3 C9 88.8(3) . . ? C10 Re3 C9 87.9(3) . . ? C6 Re3 C9 173.8(3) . . ? C8 Re3 C7 93.6(3) . . ? C10 Re3 C7 174.0(3) . . ? C6 Re3 C7 94.3(3) . . ? C9 Re3 C7 91.1(3) . . ? C8 Re3 S3 177.3(2) . . ? C10 Re3 S3 88.4(2) . . ? C6 Re3 S3 94.7(2) . . ? C9 Re3 S3 88.7(2) . . ? C7 Re3 S3 85.6(2) . . ? C16 S1 Re1 106.5(2) . . ? C17 S2 C16 88.4(3) . . ? C17 S3 Re3 111.8(2) . . ? C17 N1 N2 114.5(6) . . ? C17 N1 Re2 129.3(5) . . ? N2 N1 Re2 116.2(4) . . ? C16 N2 N1 111.8(5) . . ? O1 C1 Re1 177.5(7) . . ? O2 C2 Re1 178.9(8) . . ? O3 C3 Re1 177.6(7) . . ? O4 C4 Re1 173.4(7) . . ? O5 C5 Re1 179.5(7) . . ? O6 C6 Re3 173.8(6) . . ? O7 C7 Re3 175.5(7) . . ? O8 C8 Re3 176.0(7) . . ? O9 C9 Re3 175.1(7) . . ? O10 C10 Re3 178.9(7) . . ? O11 C11 Re2 177.1(7) . . ? O12 C12 Re2 174.0(7) . . ? O13 C13 Re2 178.5(8) . . ? O14 C14 Re2 179.4(7) . . ? O15 C15 Re2 178.3(7) . . ? N2 C16 S1 127.8(5) . . ? N2 C16 S2 113.9(5) . . ? S1 C16 S2 118.3(4) . . ? N1 C17 S3 122.4(5) . . ? N1 C17 S2 111.3(5) . . ? S3 C17 S2 126.2(4) . . ? O16 S4 O18 116.1(5) . . ? O16 S4 O17 115.1(5) . . ? O18 S4 O17 115.3(5) . . ? O16 S4 C18 102.7(4) . . ? O18 S4 C18 102.3(5) . . ? O17 S4 C18 102.4(4) . . ? F2 C18 F1 106.4(8) . . ? F2 C18 F3 106.7(8) . . ? F1 C18 F3 106.3(8) . . ? F2 C18 S4 113.4(7) . . ? F1 C18 S4 111.9(6) . . ? F3 C18 S4 111.7(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.479 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.229