Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Joan Suades' 'Merce Font-Bardia' 'David Martin' 'Ulderico Mazzi' 'Carlos Piera' 'Raffaella Rossin' ; X.Solans ; _publ_contact_author_name 'Dr Joan Suades' _publ_contact_author_address ; Department of Chemistry Universitat Autonoma de Barcelona Edifici C, Campus UAB Bellaterra 08193 SPAIN ; _publ_contact_author_email JOAN.SUADES@UAB.ES _publ_section_title ; Rhenium and 99m-technetium complexes with coenzyme M (MESNA) ; data_suem13 _database_code_CSD 171988 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C6 H16 Na1 O6 Re1 S5' _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 Na O6 Re S5' _chemical_formula_weight 553.68 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' O O 0.0106 0.0060 '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' Na Na 0.0362 0.0249 '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 P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 7.7020(10) _cell_length_b 10.0090(10) _cell_length_c 20.6250(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.1240(10) _cell_angle_gamma 90.00 _cell_volume 1587.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4211 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description prismatic _exptl_crystal_colour browm _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 8.352 _exptl_absorpt_correction_type 'phi scan' _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.87 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type mar340 _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6276 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.027 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 33.04 _reflns_number_total 3321 _reflns_number_gt 1173 _reflns_threshold_expression >2sigma(I) _computing_data_collection marxds _computing_cell_refinement marxds _computing_data_reduction marxds _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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 w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+15.2188P] 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 3321 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.46501(6) 0.97837(9) 0.340737(18) 0.0258(5) Uani 1 d . . . Na Na -0.0852(6) 0.6709(9) 0.0220(2) 0.035(3) Uani 1 d . . . S1 S 0.5644(5) 1.0275(7) 0.24065(15) 0.036(2) Uani 1 d . . . S2 S 0.7127(4) 1.0988(7) 0.37960(14) 0.036(2) Uani 1 d . . . S3 S 0.5507(5) 0.8301(7) 0.42220(15) 0.039(2) Uani 1 d . . . S4 S 0.3336(4) 0.7918(6) 0.29565(13) 0.034(2) Uani 1 d . . . S5 S 0.0738(4) 0.9625(7) 0.11809(13) 0.027(2) Uani 1 d . . . O1 O 0.2957(12) 1.0751(17) 0.3633(4) 0.032(5) Uani 1 d . . . O2 O -0.0274(13) 1.0898(18) 0.1219(4) 0.044(6) Uani 1 d . . . O3 O 0.2318(13) 0.9735(14) 0.0829(4) 0.039(6) Uani 1 d . . . O4 O -0.0208(13) 0.8509(17) 0.0939(4) 0.042(6) Uani 1 d . . . O5 O 0.1120(15) 0.5077(13) 0.0716(4) 0.033(6) Uani 1 d . . . O6 O -0.3190(12) 0.7623(16) -0.0367(4) 0.044(6) Uani 1 d . . . C1 C 0.7263(19) 1.151(3) 0.2529(6) 0.060(11) Uani 1 d . . . H1 H 0.7952 1.1557 0.2149 0.072 Uiso 1 calc R . . H1A H 0.6721 1.2370 0.2586 0.072 Uiso 1 calc R . . C2 C 0.8367(17) 1.120(2) 0.3088(6) 0.041(9) Uani 1 d . . . H2 H 0.9202 1.1917 0.3164 0.050 Uiso 1 calc R . . H2A H 0.9007 1.0387 0.3010 0.050 Uiso 1 calc R . . C3 C 0.8396(14) 0.9869(19) 0.4313(5) 0.046(9) Uani 1 d . . . H3 H 0.9001 0.9230 0.4053 0.044 Uiso 1 calc R . . H3A H 0.9251 1.0366 0.4578 0.044 Uiso 1 calc R . . C4 C 0.715(2) 0.915(3) 0.4743(6) 0.059(9) Uani 1 d . . . H4 H 0.6597 0.9784 0.5021 0.071 Uiso 1 calc R . . H4A H 0.7778 0.8502 0.5016 0.071 Uiso 1 calc R . . C5 C 0.2604(15) 0.821(2) 0.2087(5) 0.030(7) Uani 1 d . . . H5 H 0.3605 0.8434 0.1842 0.025 Uiso 1 calc R . . H5A H 0.2106 0.7390 0.1907 0.025 Uiso 1 calc R . . C6 C 0.1371(15) 0.924(2) 0.2013(5) 0.026(7) Uani 1 d . . . H6 H 0.1843 1.0034 0.2223 0.032 Uiso 1 calc R . . H6A H 0.0344 0.8980 0.2235 0.032 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 0.0273(3) 0.0259(14) 0.02425(19) -0.0004(3) 0.00111(12) 0.0005(3) Na 0.031(3) 0.036(11) 0.038(2) -0.001(4) 0.0014(16) 0.004(3) S1 0.042(2) 0.031(8) 0.0346(14) 0.000(2) 0.0022(10) -0.002(2) S2 0.0332(19) 0.036(8) 0.0378(14) 0.000(2) 0.0018(10) 0.000(2) S3 0.047(2) 0.033(8) 0.0374(14) 0.003(2) 0.0005(11) 0.000(2) S4 0.0317(18) 0.037(7) 0.0321(13) 0.002(2) -0.0004(9) -0.004(2) S5 0.0327(19) 0.021(8) 0.0257(11) 0.0013(19) 0.0001(8) 0.001(2) O1 0.045(6) 0.012(16) 0.038(4) 0.007(7) -0.003(3) 0.004(7) O2 0.046(7) 0.04(2) 0.046(5) -0.003(8) -0.004(4) 0.009(8) O3 0.040(6) 0.037(19) 0.039(4) 0.000(6) 0.007(3) -0.007(6) O4 0.047(6) 0.04(2) 0.041(5) -0.006(7) 0.000(4) -0.002(7) O5 0.039(7) 0.02(2) 0.035(4) 0.001(6) 0.003(4) -0.004(6) O6 0.045(6) 0.043(19) 0.044(5) -0.006(7) -0.001(4) 0.005(7) C1 0.050(10) 0.09(3) 0.039(6) 0.004(11) 0.001(5) -0.007(11) C2 0.027(8) 0.03(3) 0.063(8) 0.003(12) 0.005(5) -0.009(10) C3 0.036(6) 0.06(3) 0.042(6) -0.003(8) 0.011(3) 0.004(7) C4 0.045(9) 0.09(3) 0.042(6) 0.005(11) 0.004(5) 0.001(12) C5 0.035(7) 0.03(2) 0.026(4) -0.002(7) -0.002(3) -0.011(8) C6 0.025(6) 0.02(2) 0.029(5) -0.008(8) -0.001(3) 0.002(8) _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 O1 1.709(12) . ? Re S1 2.294(3) . ? Re S4 2.296(5) . ? Re S3 2.311(5) . ? Re S2 2.360(5) . ? Na O6 2.304(11) . ? Na O4 2.369(15) . ? Na O3 2.418(13) 4_575 ? Na O5 2.419(14) . ? Na O6 2.527(11) 4_675 ? Na O5 2.632(13) 3_565 ? Na Na 3.793(16) 3_565 ? Na Na 4.164(7) 4_675 ? Na Na 4.164(7) 4_575 ? S1 C1 1.76(2) . ? S2 C3 1.797(15) . ? S2 C2 1.800(13) . ? S3 C4 1.822(18) . ? S4 C5 1.874(10) . ? S5 O4 1.409(15) . ? S5 O3 1.454(10) . ? S5 O2 1.498(17) . ? S5 C6 1.802(11) . ? O3 Na 2.418(13) 4_675 ? O5 Na 2.632(13) 3_565 ? O6 Na 2.527(11) 4_575 ? C1 C2 1.429(19) . ? C1 H1 0.9700 . ? C1 H1A 0.9700 . ? C2 H2 0.9700 . ? C2 H2A 0.9700 . ? C3 C4 1.53(2) . ? C3 H3 0.9700 . ? C3 H3A 0.9700 . ? C4 H4 0.9700 . ? C4 H4A 0.9700 . ? C5 C6 1.40(2) . ? C5 H5 0.9700 . ? C5 H5A 0.9700 . ? C6 H6 0.9700 . ? C6 H6A 0.9700 . ? 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 O1 Re S1 114.9(4) . . ? O1 Re S4 104.2(5) . . ? S1 Re S4 88.33(16) . . ? O1 Re S3 111.0(4) . . ? S1 Re S3 134.10(17) . . ? S4 Re S3 82.79(17) . . ? O1 Re S2 103.5(5) . . ? S1 Re S2 83.86(14) . . ? S4 Re S2 152.03(17) . . ? S3 Re S2 83.54(18) . . ? O6 Na O4 99.1(5) . . ? O6 Na O3 92.8(4) . 4_575 ? O4 Na O3 103.8(4) . 4_575 ? O6 Na O5 160.9(6) . . ? O4 Na O5 98.3(4) . . ? O3 Na O5 75.3(4) 4_575 . ? O6 Na O6 105.9(4) . 4_675 ? O4 Na O6 87.2(4) . 4_675 ? O3 Na O6 156.6(6) 4_575 4_675 ? O5 Na O6 82.8(4) . 4_675 ? O6 Na O5 81.7(4) . 3_565 ? O4 Na O5 168.9(4) . 3_565 ? O3 Na O5 87.2(5) 4_575 3_565 ? O5 Na O5 82.7(4) . 3_565 ? O6 Na O5 82.0(4) 4_675 3_565 ? O6 Na Na 120.2(4) . 3_565 ? O4 Na Na 140.6(4) . 3_565 ? O3 Na Na 78.7(4) 4_575 3_565 ? O5 Na Na 43.5(3) . 3_565 ? O6 Na Na 79.8(4) 4_675 3_565 ? O5 Na Na 39.2(3) 3_565 3_565 ? O6 Na Na 123.1(5) . 4_675 ? O4 Na Na 63.2(3) . 4_675 ? O3 Na Na 142.4(3) 4_575 4_675 ? O5 Na Na 72.4(3) . 4_675 ? O6 Na Na 29.0(2) 4_675 4_675 ? O5 Na Na 107.1(3) 3_565 4_675 ? Na Na Na 90.62(18) 3_565 4_675 ? O6 Na Na 32.1(3) . 4_575 ? O4 Na Na 82.7(4) . 4_575 ? O3 Na Na 70.2(3) 4_575 4_575 ? O5 Na Na 144.7(4) . 4_575 ? O6 Na Na 132.4(5) 4_675 4_575 ? O5 Na Na 102.9(3) 3_565 4_575 ? Na Na Na 132.5(3) 3_565 4_575 ? Na Na Na 135.3(5) 4_675 4_575 ? C1 S1 Re 106.8(5) . . ? C3 S2 C2 105.0(7) . . ? C3 S2 Re 106.6(6) . . ? C2 S2 Re 103.9(5) . . ? C4 S3 Re 107.0(8) . . ? C5 S4 Re 111.4(7) . . ? O4 S5 O3 108.3(7) . . ? O4 S5 O2 115.6(8) . . ? O3 S5 O2 114.4(9) . . ? O4 S5 C6 105.9(9) . . ? O3 S5 C6 107.5(6) . . ? O2 S5 C6 104.4(7) . . ? S5 O3 Na 137.8(9) . 4_675 ? S5 O4 Na 155.6(6) . . ? Na O5 Na 97.3(4) . 3_565 ? Na O6 Na 119.0(4) . 4_575 ? C2 C1 S1 110.5(16) . . ? C2 C1 H1 109.5 . . ? S1 C1 H1 109.5 . . ? C2 C1 H1A 109.5 . . ? S1 C1 H1A 109.5 . . ? H1 C1 H1A 108.1 . . ? C1 C2 S2 111.2(10) . . ? C1 C2 H2 109.4 . . ? S2 C2 H2 109.4 . . ? C1 C2 H2A 109.4 . . ? S2 C2 H2A 109.4 . . ? H2 C2 H2A 108.0 . . ? C4 C3 S2 107.5(10) . . ? C4 C3 H3 110.2 . . ? S2 C3 H3 110.2 . . ? C4 C3 H3A 110.2 . . ? S2 C3 H3A 110.2 . . ? H3 C3 H3A 108.5 . . ? C3 C4 S3 108.4(9) . . ? C3 C4 H4 110.0 . . ? S3 C4 H4 110.0 . . ? C3 C4 H4A 110.0 . . ? S3 C4 H4A 110.0 . . ? H4 C4 H4A 108.4 . . ? C6 C5 S4 112.6(9) . . ? C6 C5 H5 109.1 . . ? S4 C5 H5 109.1 . . ? C6 C5 H5A 109.1 . . ? S4 C5 H5A 109.1 . . ? H5 C5 H5A 107.8 . . ? C5 C6 S5 114.1(9) . . ? C5 C6 H6 108.7 . . ? S5 C6 H6 108.7 . . ? C5 C6 H6A 108.7 . . ? S5 C6 H6A 108.7 . . ? H6 C6 H6A 107.6 . . ? _diffrn_measured_fraction_theta_max 0.226 _diffrn_reflns_theta_full 99.12 _diffrn_measured_fraction_theta_full 0.226 _refine_diff_density_max 0.784 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.127