Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_hgnbsb _database_code_CSD 156235 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Iacopino, Daniela' 'Menabue, Ledi' 'Saladini, Monica' _publ_contact_author_name 'Prof Monica Saladini' _publ_contact_author_address ; Prof Monica Saladini Department of Chemistry University of Modena and Reggio Emilia Via Campi 183 41100 Modena ITALY ; _publ_contact_author_email 'saladini@unimo.it' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H23 Hg N6 O6.50 S' _chemical_formula_weight 780.17 _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 'Hg' 'Hg' -2.3894 9.2266 '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' '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 ? _symmetry_space_group_name_H-M ? 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 20.459(3) _cell_length_b 18.653(3) _cell_length_c 17.972(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.97(2) _cell_angle_gamma 90.00 _cell_volume 6446.1(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method ? _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 4.889 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6633 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.1676 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5694 _reflns_number_observed 2666 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 53 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^)+(0.1279P)^2^+56.8955P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5641 _refine_ls_number_parameters 369 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.2017 _refine_ls_R_factor_obs 0.0860 _refine_ls_wR_factor_all 0.2822 _refine_ls_wR_factor_obs 0.1947 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.123 _refine_ls_restrained_S_all 1.098 _refine_ls_restrained_S_obs 1.117 _refine_ls_shift/esd_max 0.029 _refine_ls_shift/esd_mean 0.004 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 Hg Hg 0.18664(5) 0.06324(4) 0.45869(4) 0.0538(3) Uani 1 d . . N1 N 0.1765(10) 0.1359(8) 0.3437(8) 0.059(5) Uani 1 d D . C1 C 0.1518(13) 0.2027(10) 0.3447(11) 0.066(6) Uani 1 d D . C2 C 0.1385(15) 0.2466(10) 0.2786(12) 0.076(8) Uani 1 d D . C3 C 0.1539(16) 0.2221(11) 0.2133(12) 0.090(9) Uani 1 d D . C4 C 0.1829(12) 0.1516(10) 0.2174(11) 0.063(7) Uani 1 d D . C5 C 0.1922(11) 0.1094(9) 0.2834(11) 0.052(5) Uani 1 d D . N2 N 0.1971(11) -0.0088(8) 0.3339(10) 0.071(6) Uani 1 d D . C6 C 0.2143(11) 0.0379(10) 0.2854(10) 0.054(6) Uani 1 d D . C7 C 0.2554(14) 0.0143(13) 0.2423(14) 0.085(8) Uani 1 d D . C8 C 0.2746(14) -0.0572(16) 0.2460(14) 0.095(9) Uani 1 d D . C9 C 0.2515(16) -0.1039(12) 0.2943(15) 0.101(8) Uani 1 d DU . C10 C 0.2110(16) -0.0784(9) 0.3356(16) 0.092(8) Uani 1 d DU . N3 N 0.1377(11) 0.1506(10) 0.5244(10) 0.065(5) Uani 1 d D . C11 C 0.1756(12) 0.1984(11) 0.5775(14) 0.075(7) Uani 1 d D . C12 C 0.1471(16) 0.2447(12) 0.6167(15) 0.088(9) Uani 1 d D . C13 C 0.0763(18) 0.2346(12) 0.6059(16) 0.107(11) Uani 1 d DU . C14 C 0.0353(13) 0.1876(13) 0.5513(16) 0.094(8) Uani 1 d DU . C15 C 0.0712(13) 0.1426(10) 0.5115(11) 0.063(7) Uani 1 d D . N4 N 0.0667(9) 0.0458(10) 0.4179(10) 0.064(5) Uani 1 d D . C16 C 0.0308(14) 0.0848(10) 0.4528(12) 0.071(8) Uani 1 d D . C17 C -0.0376(12) 0.0718(13) 0.4418(12) 0.066(6) Uani 1 d D . C18 C -0.0702(11) 0.0188(14) 0.3849(14) 0.072(7) Uani 1 d D . C19 C -0.0346(14) -0.0226(15) 0.3501(14) 0.090(9) Uani 1 d D . C20 C 0.0384(13) -0.0069(10) 0.3691(11) 0.066(7) Uani 1 d D . O1 O 0.1909(9) -0.0620(8) 0.5231(10) 0.074(5) Uani 1 d . . O2 O 0.2618(10) -0.1504(8) 0.5668(10) 0.094(6) Uani 1 d . . C21 C 0.2464(17) -0.0888(11) 0.5431(12) 0.066(7) Uani 1 d . . C22 C 0.3141(15) -0.0398(12) 0.5503(16) 0.084(8) Uani 1 d . . N5 N 0.2919(10) 0.0348(8) 0.5256(9) 0.060(5) Uani 1 d . . S S 0.3471(3) 0.0949(3) 0.5597(3) 0.0577(15) Uani 1 d . . O3 O 0.3894(9) 0.0822(8) 0.6398(8) 0.079(5) Uani 1 d . . O4 O 0.3102(9) 0.1626(7) 0.5398(9) 0.074(5) Uani 1 d . . C23 C 0.4072(8) 0.0914(8) 0.5069(7) 0.047(5) Uani 1 d G . C24 C 0.3880(7) 0.0585(8) 0.4373(8) 0.067(6) Uani 1 d G . C25 C 0.4319(10) 0.0507(8) 0.3951(7) 0.070(7) Uani 1 d G . C26 C 0.4896(9) 0.0787(9) 0.4172(10) 0.096(10) Uani 1 d G . C27 C 0.5199(7) 0.1126(9) 0.4941(11) 0.073(7) Uani 1 d G . C28 C 0.4729(8) 0.1145(8) 0.5358(7) 0.073(7) Uani 1 d G . N6 N 0.4975(15) 0.1569(14) 0.6103(13) 0.088(7) Uani 1 d . . O5 O 0.4702(12) 0.2107(12) 0.6180(12) 0.110(7) Uani 1 d . . O6 O 0.5511(13) 0.1332(12) 0.6572(13) 0.122(8) Uani 1 d . . OW1 O 0.5000 0.0004(16) 0.7500 0.120(10) Uiso 1 d S . H1 H 0.1459 0.2204 0.3916 0.084 Uiso 1 d . . H2 H 0.1165 0.2916 0.2789 0.121 Uiso 1 d . . H3 H 0.1453 0.2513 0.1673 0.135 Uiso 1 d . . H4 H 0.1993 0.1345 0.1760 0.081 Uiso 1 d . . H5 H 0.2723 0.0453 0.2098 0.091 Uiso 1 d . . H6 H 0.3018 -0.0771 0.2178 0.118 Uiso 1 d . . H7 H 0.2560 -0.1525 0.2932 0.150 Uiso 1 d . . H8 H 0.1953 -0.1104 0.3657 0.133 Uiso 1 d . . H9 H 0.2194 0.2003 0.5912 0.113 Uiso 1 d . . H10 H 0.1732 0.2821 0.6470 0.130 Uiso 1 d . . H11 H 0.0675 0.2621 0.6437 0.128 Uiso 1 d . . H12 H -0.0140 0.1866 0.5381 0.152 Uiso 1 d . . H13 H -0.0609 0.0973 0.4689 0.088 Uiso 1 d . . H14 H -0.1181 0.0080 0.3703 0.048 Uiso 1 d . . H15 H -0.0560 -0.0566 0.3148 0.064 Uiso 1 d . . H16 H 0.0651 -0.0343 0.3469 0.126 Uiso 1 d . . H17 H 0.3471 -0.0395 0.6038 0.113 Uiso 1 d . . H18 H 0.3383 -0.0586 0.5157 0.113 Uiso 1 d . . H19 H 0.3426 0.0417 0.4175 0.093 Uiso 1 d . . H20 H 0.4171 0.0236 0.3498 0.068 Uiso 1 d . . H21 H 0.5150 0.0770 0.3840 0.122 Uiso 1 d . . H22 H 0.5654 0.1299 0.5140 0.081 Uiso 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 Hg 0.0660(6) 0.0459(4) 0.0530(5) -0.0013(4) 0.0249(4) 0.0052(5) N1 0.077(14) 0.064(11) 0.035(8) -0.010(8) 0.018(9) 0.009(10) C1 0.070(17) 0.058(14) 0.059(13) -0.010(11) 0.009(12) 0.011(13) C2 0.117(24) 0.051(13) 0.056(13) 0.001(11) 0.022(15) 0.014(14) C3 0.142(28) 0.062(15) 0.052(13) 0.016(11) 0.013(16) -0.013(17) C4 0.074(18) 0.049(12) 0.050(12) -0.005(10) 0.003(12) -0.025(12) C5 0.041(14) 0.041(11) 0.063(13) -0.003(10) 0.003(11) 0.004(10) N2 0.093(17) 0.048(10) 0.073(12) -0.010(9) 0.031(12) 0.016(11) C6 0.056(16) 0.070(14) 0.033(9) -0.004(9) 0.012(10) 0.011(12) C7 0.081(22) 0.098(21) 0.076(16) -0.007(15) 0.029(16) 0.018(17) C8 0.086(21) 0.140(27) 0.066(15) 0.009(17) 0.036(15) 0.040(21) C9 0.148(25) 0.067(17) 0.079(17) -0.005(14) 0.025(19) 0.038(19) C10 0.161(26) 0.037(13) 0.117(20) -0.008(12) 0.098(20) 0.018(15) N3 0.076(16) 0.070(12) 0.062(11) -0.006(10) 0.040(12) 0.011(12) C11 0.081(20) 0.053(13) 0.083(16) -0.005(13) 0.021(15) 0.009(14) C12 0.129(29) 0.055(15) 0.094(19) -0.031(13) 0.056(21) -0.012(18) C13 0.202(39) 0.043(14) 0.109(20) -0.009(14) 0.095(23) 0.018(21) C14 0.132(26) 0.067(16) 0.116(20) -0.008(16) 0.086(19) 0.023(18) C15 0.098(22) 0.039(11) 0.066(14) 0.017(10) 0.048(15) 0.005(14) N4 0.050(12) 0.091(14) 0.054(10) -0.001(10) 0.023(10) -0.020(11) C16 0.116(25) 0.056(13) 0.066(14) 0.030(11) 0.063(17) 0.031(15) C17 0.065(17) 0.090(18) 0.052(12) 0.004(12) 0.032(13) -0.005(16) C18 0.037(15) 0.102(20) 0.070(15) 0.040(15) 0.009(13) 0.013(15) C19 0.072(22) 0.125(24) 0.065(16) -0.005(16) 0.013(16) 0.013(20) C20 0.109(24) 0.049(12) 0.037(11) 0.004(10) 0.020(13) 0.004(14) O1 0.060(11) 0.053(9) 0.123(14) 0.015(9) 0.050(10) 0.004(10) O2 0.133(17) 0.045(9) 0.117(13) 0.025(9) 0.058(13) 0.012(10) C21 0.115(25) 0.039(12) 0.055(13) -0.008(10) 0.041(15) 0.018(15) C22 0.081(20) 0.040(11) 0.124(22) 0.018(13) 0.024(17) 0.007(14) N5 0.070(14) 0.033(8) 0.055(10) 0.007(7) -0.004(10) 0.016(9) S 0.066(4) 0.057(3) 0.050(3) -0.008(2) 0.020(3) -0.007(3) O3 0.083(13) 0.100(12) 0.057(9) -0.016(8) 0.027(9) -0.020(10) O4 0.083(12) 0.046(8) 0.110(12) -0.015(8) 0.054(10) 0.013(9) C23 0.060(16) 0.049(11) 0.034(10) 0.002(8) 0.017(10) -0.002(11) C24 0.086(19) 0.055(12) 0.063(13) -0.006(11) 0.029(13) -0.001(14) C25 0.050(16) 0.090(19) 0.075(15) -0.010(13) 0.028(14) 0.020(15) C26 0.111(27) 0.110(24) 0.089(20) 0.013(17) 0.062(20) 0.028(21) C27 0.059(17) 0.072(16) 0.092(18) 0.008(14) 0.031(15) -0.004(14) C28 0.073(20) 0.087(17) 0.062(14) -0.009(13) 0.027(15) -0.014(16) N6 0.085(20) 0.083(16) 0.079(15) 0.006(14) 0.007(15) -0.016(16) O5 0.117(19) 0.099(15) 0.105(15) -0.022(12) 0.028(13) 0.011(14) O6 0.115(19) 0.115(17) 0.104(15) -0.014(13) -0.003(14) -0.024(15) _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 Hg N5 2.14(2) . ? Hg N4 2.33(2) . ? Hg N3 2.42(2) . ? Hg N1 2.420(15) . ? Hg O1 2.596(15) . ? Hg N2 2.68(2) . ? N1 C5 1.33(2) . ? N1 C1 1.35(2) . ? C1 C2 1.39(2) . ? C2 C3 1.39(3) . ? C3 C4 1.43(3) . ? C4 C5 1.38(2) . ? C5 C6 1.40(3) . ? N2 C10 1.33(2) . ? N2 C6 1.36(2) . ? C6 C7 1.39(2) . ? C7 C8 1.39(3) . ? C8 C9 1.42(3) . ? C9 C10 1.37(3) . ? N3 C11 1.34(2) . ? N3 C15 1.31(2) . ? C11 C12 1.37(3) . ? C12 C13 1.41(3) . ? C13 C14 1.37(3) . ? C14 C15 1.45(3) . ? C15 C16 1.54(3) . ? N4 C20 1.31(2) . ? N4 C16 1.33(2) . ? C16 C17 1.37(3) . ? C17 C18 1.42(3) . ? C18 C19 1.35(3) . ? C19 C20 1.44(3) . ? O1 C21 1.18(3) . ? O2 C21 1.23(2) . ? C21 C22 1.63(4) . ? C22 N5 1.48(3) . ? N5 S 1.56(2) . ? S O3 1.42(2) . ? S O4 1.451(15) . ? S C23 1.793(13) . ? C23 C24 1.33 . ? C23 C28 1.34 . ? C24 C25 1.37 . ? C25 C26 1.23 . ? C26 C27 1.45 . ? C27 C28 1.41 . ? C28 N6 1.49(3) . ? N6 O5 1.18(3) . ? N6 O6 1.22(3) . ? 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 N5 Hg N4 152.8(6) . . ? N5 Hg N3 113.4(6) . . ? N4 Hg N3 71.4(6) . . ? N5 Hg N1 113.3(7) . . ? N4 Hg N1 92.0(6) . . ? N3 Hg N1 96.4(6) . . ? N5 Hg O1 69.7(6) . . ? N4 Hg O1 83.4(6) . . ? N3 Hg O1 110.2(6) . . ? N1 Hg O1 149.8(5) . . ? N5 Hg N2 89.6(6) . . ? N4 Hg N2 92.5(6) . . ? N3 Hg N2 155.3(6) . . ? N1 Hg N2 64.8(5) . . ? O1 Hg N2 85.5(5) . . ? C5 N1 C1 123.5(15) . . ? C5 N1 Hg 121.0(12) . . ? C1 N1 Hg 115.4(12) . . ? N1 C1 C2 119.9(17) . . ? C1 C2 C3 119.5(17) . . ? C2 C3 C4 117.8(17) . . ? C5 C4 C3 119.9(17) . . ? N1 C5 C6 119.9(16) . . ? N1 C5 C4 119.3(16) . . ? C6 C5 C4 120.7(17) . . ? C10 N2 C6 122.7(16) . . ? C10 N2 Hg 123.2(14) . . ? C6 N2 Hg 109.1(11) . . ? C5 C6 C7 122.4(19) . . ? C5 C6 N2 118.2(17) . . ? C7 C6 N2 119.4(17) . . ? C6 C7 C8 119.5(19) . . ? C7 C8 C9 118.1(19) . . ? C10 C9 C8 120.4(18) . . ? C9 C10 N2 119.4(18) . . ? C11 N3 C15 120.9(17) . . ? C11 N3 Hg 124.0(15) . . ? C15 N3 Hg 114.5(14) . . ? C12 C11 N3 122.9(20) . . ? C11 C12 C13 116.4(19) . . ? C14 C13 C12 122.2(20) . . ? C13 C14 C15 115.8(21) . . ? C14 C15 N3 121.1(19) . . ? C14 C15 C16 120.0(20) . . ? N3 C15 C16 118.9(18) . . ? C20 N4 C16 122.4(18) . . ? C20 N4 Hg 119.4(15) . . ? C16 N4 Hg 117.7(15) . . ? N4 C16 C17 122.5(20) . . ? N4 C16 C15 116.9(21) . . ? C17 C16 C15 120.5(18) . . ? C16 C17 C18 115.8(18) . . ? C19 C18 C17 122.5(19) . . ? C18 C19 C20 116.9(21) . . ? N4 C20 C19 119.6(19) . . ? C21 O1 Hg 113.5(15) . . ? O1 C21 O2 127.4(29) . . ? O1 C21 C22 119.5(20) . . ? O2 C21 C22 112.8(25) . . ? N5 C22 C21 109.8(20) . . ? C22 N5 S 116.8(15) . . ? C22 N5 Hg 123.1(15) . . ? S N5 Hg 119.7(9) . . ? O3 S O4 118.7(10) . . ? O3 S N5 112.6(9) . . ? O4 S N5 106.5(9) . . ? O3 S C23 103.8(9) . . ? O4 S C23 107.1(8) . . ? N5 S C23 107.5(9) . . ? C24 C23 C28 116.7 . . ? C24 C23 S 118.7(10) . . ? C28 C23 S 124.3(10) . . ? C23 C24 C25 122.2 . . ? C26 C25 C24 121.1 . . ? C25 C26 C27 123.0 . . ? C28 C27 C26 111.7 . . ? C23 C28 C27 124.4 . . ? C23 C28 N6 120.5(16) . . ? C27 C28 N6 114.2(15) . . ? O5 N6 O6 125.5(27) . . ? O5 N6 C28 122.0(24) . . ? O6 N6 C28 112.2(25) . . ? _refine_diff_density_max 2.077 _refine_diff_density_min -1.750 _refine_diff_density_rms 0.206