Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_retiml2 _database_code_CSD 189597 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Santos, Isabel' 'Domingos, Angela' 'Garcia, Raquel' 'Paulo, Antonio' 'Xing, Yong-Heng' _publ_contact_author_name 'Prof Isabel Santos' _publ_contact_author_address ; Departamento de Quimica ITN Estrada Nacional 10 2686-953 Sacavem Codex PORTUGAL ; _publ_contact_author_email '?' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Rhenium (I) Tricarbonyl Complexes with Mercaptoimidazolyborate Ligands Bearing Piperazine Fragments ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Re{k3-Ph(u-H)B(timMe,pip)2}(CO)3].C4H8O.H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C39 H50 B N8 O9 Re S2' _chemical_formula_weight 1036.00 _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' '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' 'B' 'B' 0.0013 0.0007 '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 orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 18.068(3) _cell_length_b 27.733(4) _cell_length_c 9.1500(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4584.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.2 _cell_measurement_theta_max 14.9 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method ? _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 2.800 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.5841 _exptl_absorpt_correction_T_max 0.9998 _exptl_special_details ; Crystals were obtained by recrytallization from THF/n-hexane. ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 4585 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4125 _reflns_number_observed 2338 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 774 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^)+(0.0769P)^2^+26.8383P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3351 _refine_ls_number_parameters 281 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1600 _refine_ls_R_factor_obs 0.0700 _refine_ls_wR_factor_all 0.3496 _refine_ls_wR_factor_obs 0.1487 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_restrained_S_all 1.935 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max 0.005 _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 Re1 Re 0.17009(4) 0.2500 0.06404(9) 0.0527(3) Uani 1 d S . S1 S 0.1856(2) 0.31122(13) 0.2590(4) 0.0611(10) Uani 1 d . . O2 O 0.1565(8) 0.3286(5) -0.1654(15) 0.119(5) Uani 1 d . . N11 N 0.3308(5) 0.2956(3) 0.1908(10) 0.043(2) Uani 1 d . . N12 N 0.3116(5) 0.3552(3) 0.3455(10) 0.045(2) Uani 1 d . . C2 C 0.1610(7) 0.2988(6) -0.0804(18) 0.071(4) Uani 1 d . . C11 C 0.2789(6) 0.3198(4) 0.2667(13) 0.042(3) Uani 1 d . . O4 O 0.6579(5) 0.4615(3) -0.0817(9) 0.066(2) Uani 1 d . . N2 N 0.5960(5) 0.4678(3) 0.1839(10) 0.041(2) Uani 1 d . . C13 C 0.3982(6) 0.3179(4) 0.2204(12) 0.040(3) Uani 1 d . . H13 H 0.4436(6) 0.3088(4) 0.1812(12) 0.048 Uiso 1 calc R . N1 N 0.5031(5) 0.3982(4) 0.3188(10) 0.051(3) Uani 1 d . . C5 C 0.5810(7) 0.4707(5) 0.3417(13) 0.059(4) Uani 1 d . . H5A H 0.5391(7) 0.4918(5) 0.3594(13) 0.070 Uiso 1 calc R . H5B H 0.6237(7) 0.4839(5) 0.3921(13) 0.070 Uiso 1 calc R . O3 O 0.4314(5) 0.3941(4) 0.5195(11) 0.081(3) Uani 1 d . . C3 C 0.4418(7) 0.3849(5) 0.3929(14) 0.053(3) Uani 1 d . . C12 C 0.3879(6) 0.3537(4) 0.3122(13) 0.042(3) Uani 1 d . . C9 C 0.6617(6) 0.5055(4) -0.0148(14) 0.045(3) Uani 1 d . . B1 B 0.3236(12) 0.2500 0.0960(23) 0.055(5) Uani 1 d SD . H1A H 0.2739(12) 0.2500 0.0452(23) 0.067 Uiso 1 calc SRD . H1B H 0.3635(12) 0.2500 0.0186(23) 0.067 Uiso 1 calc SRD . C14 C 0.2715(7) 0.3892(4) 0.4340(15) 0.063(4) Uani 1 d . . H14A H 0.3057(7) 0.4110(4) 0.4798(15) 0.095 Uiso 1 calc R . H14B H 0.2441(7) 0.3722(4) 0.5077(15) 0.095 Uiso 1 calc R . H14C H 0.2379(7) 0.4071(4) 0.3735(15) 0.095 Uiso 1 calc R . C16 C 0.6651(9) 0.5922(5) 0.1258(19) 0.082(5) Uani 1 d . . H16 H 0.6651(9) 0.6217(5) 0.1743(19) 0.098 Uiso 1 calc R . C10 C 0.6972(7) 0.5443(6) -0.0787(15) 0.066(4) Uani 1 d . . H10 H 0.7191(7) 0.5412(6) -0.1702(15) 0.079 Uiso 1 calc R . C8 C 0.6271(6) 0.5094(4) 0.1223(13) 0.042(3) Uani 1 d . . C6 C 0.5312(6) 0.4488(4) 0.1071(12) 0.044(3) Uani 1 d . . H6A H 0.5407(6) 0.4483(4) 0.0028(12) 0.053 Uiso 1 calc R . H6B H 0.4890(6) 0.4697(4) 0.1247(12) 0.053 Uiso 1 calc R . C4 C 0.5641(7) 0.4197(5) 0.3992(13) 0.062(4) Uani 1 d . . H4A H 0.6078(7) 0.3996(5) 0.3891(13) 0.074 Uiso 1 calc R . H4B H 0.5516(7) 0.4213(5) 0.5021(13) 0.074 Uiso 1 calc R . C40 C 0.6692(9) 0.4582(7) -0.2376(16) 0.096(5) Uani 1 d . . H40A H 0.6650(9) 0.4251(7) -0.2678(16) 0.144 Uiso 1 calc R . H40B H 0.7176(9) 0.4700(7) -0.2617(16) 0.144 Uiso 1 calc R . H40C H 0.6325(9) 0.4772(7) -0.2871(16) 0.144 Uiso 1 calc R . C7 C 0.5136(7) 0.3985(5) 0.1592(12) 0.057(4) Uani 1 d . . H7A H 0.4690(7) 0.3871(5) 0.1116(12) 0.068 Uiso 1 calc R . H7B H 0.5538(7) 0.3770(5) 0.1332(12) 0.068 Uiso 1 calc R . C15 C 0.6997(9) 0.5869(6) -0.0055(21) 0.082(5) Uani 1 d . . H15 H 0.7254(9) 0.6128(6) -0.0456(21) 0.098 Uiso 1 calc R . C17 C 0.6295(7) 0.5520(5) 0.1852(16) 0.063(4) Uani 1 d . . H17 H 0.6061(7) 0.5556(5) 0.2750(16) 0.075 Uiso 1 calc R . O1 O 0.0032(8) 0.2500 0.1000(18) 0.089(5) Uani 1 d S . C1 C 0.0662(10) 0.2500 0.0854(23) 0.061(5) Uani 1 d S . O1S O 0.4848(23) 0.2500 0.7817(46) 0.280(17) Uani 1 d SU . C1S C 0.4368(15) 0.2918(10) 0.7204(31) 0.177(11) Uani 1 d U . H1S1 H 0.4650(15) 0.3081(10) 0.6450(31) 0.212 Uiso 1 calc R . H1S2 H 0.4285(15) 0.3148(10) 0.7985(31) 0.212 Uiso 1 calc R . C2S C 0.3587(16) 0.2774(9) 0.6538(30) 0.186(12) Uani 1 d U . H2S1 H 0.3187(16) 0.2898(9) 0.7136(30) 0.224 Uiso 1 calc R . H2S2 H 0.3533(16) 0.2898(9) 0.5553(30) 0.224 Uiso 1 calc R . O2S O 0.0398(12) 0.2500 0.4663(31) 0.180(10) Uani 1 d S . 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 0.0439(4) 0.0487(4) 0.0655(5) 0.000 -0.0002(4) 0.000 S1 0.043(2) 0.060(2) 0.081(2) -0.016(2) 0.013(2) 0.0024(14) O2 0.150(12) 0.097(9) 0.109(10) 0.051(9) -0.007(9) -0.001(8) N11 0.045(5) 0.031(5) 0.053(6) 0.009(4) 0.013(5) 0.007(5) N12 0.050(6) 0.035(5) 0.049(6) -0.002(5) 0.009(5) 0.000(4) C2 0.057(8) 0.077(10) 0.079(10) 0.001(10) -0.003(8) -0.008(7) C11 0.046(6) 0.034(7) 0.047(7) -0.010(6) 0.006(5) -0.002(5) O4 0.070(6) 0.072(6) 0.055(6) 0.007(5) 0.015(5) 0.001(5) N2 0.041(5) 0.038(6) 0.044(6) 0.001(5) -0.016(4) -0.009(4) C13 0.039(6) 0.028(6) 0.052(7) 0.000(6) 0.002(5) -0.006(5) N1 0.051(6) 0.061(7) 0.040(6) 0.015(5) -0.006(5) -0.017(5) C5 0.054(8) 0.075(11) 0.047(8) -0.008(8) -0.003(6) -0.010(7) O3 0.073(6) 0.110(9) 0.060(6) -0.029(6) 0.013(5) -0.025(6) C3 0.061(8) 0.052(8) 0.046(8) -0.008(7) 0.009(6) -0.005(6) C12 0.061(7) 0.023(6) 0.042(7) 0.003(6) 0.006(6) 0.004(5) C9 0.045(6) 0.034(6) 0.054(7) 0.008(6) -0.006(6) 0.007(6) B1 0.052(11) 0.054(12) 0.060(14) 0.000 -0.007(11) 0.000 C14 0.079(9) 0.048(8) 0.062(8) -0.012(8) 0.005(8) 0.017(7) C16 0.121(13) 0.034(8) 0.090(11) -0.002(8) -0.038(12) 0.008(9) C10 0.051(7) 0.095(12) 0.051(8) 0.023(9) -0.007(7) -0.011(7) C8 0.040(6) 0.033(7) 0.051(7) -0.005(6) -0.003(6) 0.001(5) C6 0.043(6) 0.043(7) 0.046(7) 0.002(6) -0.001(5) -0.003(5) C4 0.054(7) 0.079(11) 0.052(9) 0.014(8) -0.009(6) -0.010(7) C40 0.113(13) 0.107(13) 0.068(10) -0.010(10) 0.017(10) 0.022(12) C7 0.055(7) 0.075(10) 0.040(7) -0.004(7) -0.010(6) -0.021(7) C15 0.105(12) 0.060(11) 0.081(11) 0.025(10) -0.041(10) -0.030(9) C17 0.073(9) 0.044(8) 0.071(9) 0.004(8) -0.008(8) -0.007(7) O1 0.064(9) 0.090(12) 0.113(13) 0.000 -0.003(9) 0.000 C1 0.042(10) 0.053(12) 0.089(16) 0.000 0.002(11) 0.000 O1S 0.277(19) 0.284(19) 0.278(19) 0.000 0.009(10) 0.000 C1S 0.187(13) 0.170(13) 0.174(14) 0.006(9) 0.026(9) 0.010(9) C2S 0.202(14) 0.181(15) 0.176(14) 0.016(9) 0.011(9) 0.019(9) O2S 0.109(15) 0.191(26) 0.240(28) 0.000 0.034(18) 0.000 _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 1.89(2) . ? Re1 C2 1.90(2) 7_565 ? Re1 C2 1.90(2) . ? Re1 S1 2.478(4) 7_565 ? Re1 S1 2.478(4) . ? Re1 B1 2.79(2) . ? S1 C11 1.704(11) . ? O2 C2 1.14(2) . ? N11 C11 1.346(13) . ? N11 C13 1.392(12) . ? N11 B1 1.539(14) . ? N12 C11 1.353(13) . ? N12 C12 1.412(14) . ? N12 C14 1.439(14) . ? O4 C9 1.368(14) . ? O4 C40 1.44(2) . ? N2 C8 1.401(14) . ? N2 C6 1.464(13) . ? N2 C5 1.471(15) . ? C13 C12 1.315(14) . ? N1 C3 1.349(14) . ? N1 C4 1.452(14) . ? N1 C7 1.473(14) . ? C5 C4 1.54(2) . ? O3 C3 1.201(14) . ? C3 C12 1.50(2) . ? C9 C10 1.38(2) . ? C9 C8 1.41(2) . ? B1 N11 1.539(14) 7_565 ? C16 C15 1.36(2) . ? C16 C17 1.40(2) . ? C10 C15 1.36(2) . ? C8 C17 1.31(2) . ? C6 C7 1.51(2) . ? O1 C1 1.15(2) . ? O1S C1S 1.55(3) 7_565 ? O1S C1S 1.55(3) . ? C1S C2S 1.59(3) . ? C2S C2S 1.52(5) 7_565 ? 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 C2 89.2(6) . 7_565 ? C1 Re1 C2 89.2(6) . . ? C2 Re1 C2 90.9(9) 7_565 . ? C1 Re1 S1 92.2(5) . 7_565 ? C2 Re1 S1 91.3(5) 7_565 7_565 ? C2 Re1 S1 177.4(4) . 7_565 ? C1 Re1 S1 92.2(5) . . ? C2 Re1 S1 177.4(4) 7_565 . ? C2 Re1 S1 91.3(5) . . ? S1 Re1 S1 86.5(2) 7_565 . ? C1 Re1 B1 168.0(8) . . ? C2 Re1 B1 99.2(5) 7_565 . ? C2 Re1 B1 99.2(5) . . ? S1 Re1 B1 79.2(3) 7_565 . ? S1 Re1 B1 79.2(3) . . ? C11 S1 Re1 103.7(4) . . ? C11 N11 C13 106.7(9) . . ? C11 N11 B1 129.9(12) . . ? C13 N11 B1 123.3(11) . . ? C11 N12 C12 106.9(9) . . ? C11 N12 C14 123.7(10) . . ? C12 N12 C14 129.2(10) . . ? O2 C2 Re1 178.6(13) . . ? N11 C11 N12 109.4(9) . . ? N11 C11 S1 126.7(9) . . ? N12 C11 S1 123.7(8) . . ? C9 O4 C40 119.4(11) . . ? C8 N2 C6 115.1(9) . . ? C8 N2 C5 115.1(10) . . ? C6 N2 C5 110.0(9) . . ? C12 C13 N11 109.7(10) . . ? C3 N1 C4 118.7(10) . . ? C3 N1 C7 127.3(10) . . ? C4 N1 C7 113.7(9) . . ? N2 C5 C4 108.8(11) . . ? O3 C3 N1 123.7(12) . . ? O3 C3 C12 119.7(12) . . ? N1 C3 C12 116.4(10) . . ? C13 C12 N12 107.3(10) . . ? C13 C12 C3 131.3(11) . . ? N12 C12 C3 120.8(10) . . ? O4 C9 C10 121.9(12) . . ? O4 C9 C8 116.5(10) . . ? C10 C9 C8 121.6(12) . . ? N11 B1 N11 110.4(14) 7_565 . ? N11 B1 Re1 98.3(9) 7_565 . ? N11 B1 Re1 98.3(9) . . ? C15 C16 C17 117.9(15) . . ? C15 C10 C9 118.9(14) . . ? C17 C8 N2 125.3(12) . . ? C17 C8 C9 116.4(12) . . ? N2 C8 C9 118.2(10) . . ? N2 C6 C7 110.5(9) . . ? N1 C4 C5 110.7(10) . . ? N1 C7 C6 110.2(11) . . ? C10 C15 C16 120.9(15) . . ? C8 C17 C16 124.2(15) . . ? O1 C1 Re1 179.2(20) . . ? C1S O1S C1S 96.5(33) 7_565 . ? O1S C1S C2S 116.6(25) . . ? C2S C2S C1S 104.6(14) 7_565 . ? _refine_diff_density_max 1.194 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.151 #===END