# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Nanhai Singh' _publ_contact_author_email NSINGH@BHU.AC.IN _publ_section_title ; Synthesis, crystal, molecular structure and properties of some new phenylmercury(II) dithiolate complexes ; loop_ _publ_author_name 'Nanhai Singh' 'Abhinav Kumar' 'Mary Mahon' 'Kieran Molloy' # Attachment 'CIF.txt' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 681258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H23 Hg N S2' _chemical_formula_sum 'C15 H23 Hg N S2' _chemical_formula_weight 482.05 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' 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 9.4107(5) _cell_length_b 12.8145(6) _cell_length_c 14.1706(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.681(2) _cell_angle_gamma 90.00 _cell_volume 1700.49(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37117 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 9.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1782 _exptl_absorpt_correction_T_max 0.3976 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'Nonius Kappa CCD' _diffrn_measurement_method '172 2.0 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23174 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.40 _reflns_number_total 3847 _reflns_number_gt 2678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0495P)^2^+0.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3847 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Hg Hg 0.63028(3) 0.13606(2) 0.49920(2) 0.03524(12) Uani 1 1 d . . . S1 S 0.4477(2) 0.18929(14) 0.59607(14) 0.0353(4) Uani 1 1 d . . . S2 S 0.58832(19) -0.01419(13) 0.65138(14) 0.0333(4) Uani 1 1 d . . . N N 0.4168(6) 0.0905(4) 0.7568(4) 0.0295(13) Uani 1 1 d . . . C1 C 0.8022(8) 0.1144(5) 0.4191(5) 0.0332(17) Uani 1 1 d . . . C2 C 0.8580(8) 0.1992(6) 0.3760(6) 0.0390(18) Uani 1 1 d . . . H2 H 0.8170 0.2663 0.3816 0.047 Uiso 1 1 calc R . . C3 C 0.9762(8) 0.1859(6) 0.3235(6) 0.0399(18) Uani 1 1 d . . . H3 H 1.0152 0.2444 0.2940 0.048 Uiso 1 1 calc R . . C4 C 1.0348(8) 0.0896(7) 0.3148(6) 0.0430(19) Uani 1 1 d . . . H4 H 1.1145 0.0809 0.2793 0.052 Uiso 1 1 calc R . . C5 C 0.9772(8) 0.0039(6) 0.3584(6) 0.043(2) Uani 1 1 d . . . H5 H 1.0173 -0.0635 0.3523 0.052 Uiso 1 1 calc R . . C6 C 0.8633(8) 0.0169(5) 0.4097(5) 0.0352(16) Uani 1 1 d . . . H6 H 0.8253 -0.0418 0.4395 0.042 Uiso 1 1 calc R . . C7 C 0.4788(7) 0.0864(5) 0.6771(5) 0.0282(15) Uani 1 1 d . . . C8 C 0.3204(7) 0.1763(5) 0.7782(5) 0.0307(15) Uani 1 1 d . . . H8A H 0.2467 0.1490 0.8170 0.037 Uiso 1 1 calc R . . H8B H 0.2714 0.2035 0.7183 0.037 Uiso 1 1 calc R . . C9 C 0.4012(7) 0.2647(5) 0.8316(5) 0.0342(17) Uani 1 1 d . . . H9A H 0.4777 0.2899 0.7941 0.041 Uiso 1 1 calc R . . H9B H 0.4466 0.2382 0.8929 0.041 Uiso 1 1 calc R . . C10 C 0.3017(8) 0.3558(5) 0.8499(6) 0.0378(17) Uani 1 1 d . . . H10A H 0.2621 0.3859 0.7885 0.045 Uiso 1 1 calc R . . H10B H 0.2210 0.3296 0.8830 0.045 Uiso 1 1 calc R . . C11 C 0.3804(9) 0.4407(6) 0.9098(6) 0.045(2) Uani 1 1 d . . . H11A H 0.4150 0.4121 0.9720 0.067 Uiso 1 1 calc R . . H11B H 0.3151 0.4988 0.9181 0.067 Uiso 1 1 calc R . . H11C H 0.4615 0.4658 0.8778 0.067 Uiso 1 1 calc R . . C12 C 0.4455(8) 0.0133(5) 0.8332(5) 0.0311(15) Uani 1 1 d . . . H12A H 0.4453 0.0492 0.8951 0.037 Uiso 1 1 calc R . . H12B H 0.5420 -0.0164 0.8297 0.037 Uiso 1 1 calc R . . C13 C 0.3370(8) -0.0759(5) 0.8288(5) 0.0334(16) Uani 1 1 d . . . H13A H 0.2402 -0.0471 0.8331 0.040 Uiso 1 1 calc R . . H13B H 0.3369 -0.1127 0.7674 0.040 Uiso 1 1 calc R . . C14 C 0.3729(9) -0.1521(6) 0.9089(6) 0.0416(19) Uani 1 1 d . . . H14A H 0.3701 -0.1149 0.9699 0.050 Uiso 1 1 calc R . . H14B H 0.4716 -0.1777 0.9058 0.050 Uiso 1 1 calc R . . C15 C 0.2728(11) -0.2449(6) 0.9070(7) 0.058(3) Uani 1 1 d . . . H15A H 0.1748 -0.2204 0.9105 0.086 Uiso 1 1 calc R . . H15B H 0.3009 -0.2904 0.9612 0.086 Uiso 1 1 calc R . . H15C H 0.2779 -0.2840 0.8480 0.086 Uiso 1 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 Hg 0.03601(18) 0.03786(17) 0.03282(17) -0.00240(13) 0.00825(12) -0.00300(13) S1 0.0430(11) 0.0298(9) 0.0341(10) 0.0029(8) 0.0081(8) 0.0045(8) S2 0.0347(10) 0.0270(9) 0.0386(10) -0.0035(8) 0.0061(8) 0.0046(7) N 0.028(3) 0.027(3) 0.033(3) -0.003(3) 0.000(3) 0.001(2) C1 0.032(4) 0.039(4) 0.027(4) -0.005(3) -0.005(3) 0.000(3) C2 0.043(5) 0.034(4) 0.037(4) -0.001(3) -0.008(4) -0.003(3) C3 0.032(4) 0.044(5) 0.045(5) -0.004(4) 0.010(4) -0.006(3) C4 0.032(4) 0.053(5) 0.044(5) -0.007(4) 0.002(4) 0.000(4) C5 0.044(5) 0.037(4) 0.047(5) -0.005(4) -0.006(4) 0.013(3) C6 0.037(4) 0.031(4) 0.038(4) 0.005(3) 0.007(3) 0.001(3) C7 0.031(4) 0.026(3) 0.027(4) -0.007(3) 0.003(3) -0.007(3) C8 0.031(4) 0.030(3) 0.033(4) -0.003(3) 0.010(3) 0.004(3) C9 0.034(4) 0.034(4) 0.035(4) -0.002(3) 0.001(3) 0.002(3) C10 0.038(4) 0.037(4) 0.038(4) 0.001(3) 0.004(3) 0.008(3) C11 0.049(5) 0.037(4) 0.048(5) -0.006(4) 0.001(4) -0.003(3) C12 0.033(4) 0.034(4) 0.027(4) 0.004(3) 0.002(3) 0.003(3) C13 0.033(4) 0.031(4) 0.035(4) 0.001(3) -0.001(3) 0.001(3) C14 0.045(5) 0.038(4) 0.042(5) 0.012(3) 0.004(4) 0.001(3) C15 0.090(7) 0.040(5) 0.044(6) 0.004(4) 0.011(5) -0.019(4) _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 C1 2.085(8) . ? Hg S1 2.402(2) . ? Hg S2 2.9465(19) . ? S1 C7 1.754(7) . ? S2 C7 1.712(7) . ? N C7 1.322(9) . ? N C12 1.472(8) . ? N C8 1.476(8) . ? C1 C2 1.376(10) . ? C1 C6 1.387(10) . ? C2 C3 1.408(11) . ? C2 H2 0.9500 . ? C3 C4 1.362(11) . ? C3 H3 0.9500 . ? C4 C5 1.396(11) . ? C4 H4 0.9500 . ? C5 C6 1.363(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.523(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.534(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.526(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.530(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.509(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.516(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 Hg S1 170.60(19) . . ? C1 Hg S2 118.6(2) . . ? S1 Hg S2 67.17(5) . . ? C7 S1 Hg 94.5(2) . . ? C7 S2 Hg 77.9(2) . . ? C7 N C12 122.5(6) . . ? C7 N C8 122.5(6) . . ? C12 N C8 114.9(6) . . ? C2 C1 C6 119.2(7) . . ? C2 C1 Hg 119.2(6) . . ? C6 C1 Hg 121.6(6) . . ? C1 C2 C3 119.7(7) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 120.4(7) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.5(7) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.0(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 121.1(7) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? N C7 S2 122.5(5) . . ? N C7 S1 118.0(5) . . ? S2 C7 S1 119.4(4) . . ? N C8 C9 111.7(6) . . ? N C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 111.6(6) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.5(6) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N C12 C13 113.5(6) . . ? N C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C12 110.7(6) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 113.7(7) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.862 _refine_diff_density_min -2.030 _refine_diff_density_rms 0.192 #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 681259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H13 Hg N O S2' _chemical_formula_sum 'C11 H13 Hg N O S2' _chemical_formula_weight 439.93 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 9.43000(10) _cell_length_b 12.0310(2) _cell_length_c 21.6724(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2458.78(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24000 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 12.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.003 _exptl_absorpt_correction_T_max 0.011 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type 'Nonius Kappa CCD' _diffrn_measurement_method '363 1.6 degree images with \f and\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31979 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2817 _reflns_number_gt 2315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0516P)^2^+1.1094P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2817 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Hg Hg 0.61100(2) 0.155463(17) 0.475969(8) 0.03118(10) Uani 1 1 d . . . S1 S 0.42060(14) 0.21449(11) 0.54158(6) 0.0322(3) Uani 1 1 d . . . S2 S 0.58559(13) 0.02164(11) 0.59073(6) 0.0308(3) Uani 1 1 d . . . O O 0.1789(4) 0.1177(3) 0.74930(15) 0.0358(8) Uani 1 1 d . . . N N 0.3802(4) 0.1266(4) 0.65181(19) 0.0292(9) Uani 1 1 d . . . C1 C 0.7958(5) 0.1268(4) 0.4262(2) 0.0287(10) Uani 1 1 d . . . C2 C 0.8507(6) 0.2054(4) 0.3851(2) 0.0318(10) Uani 1 1 d . . . H2 H 0.7975 0.2704 0.3758 0.038 Uiso 1 1 calc R . . C3 C 0.9830(6) 0.1893(4) 0.3575(2) 0.0337(11) Uani 1 1 d . . . H3 H 1.0197 0.2434 0.3298 0.040 Uiso 1 1 calc R . . C4 C 1.0599(6) 0.0951(4) 0.3705(2) 0.0333(10) Uani 1 1 d . . . H4 H 1.1501 0.0842 0.3519 0.040 Uiso 1 1 calc R . . C5 C 1.0060(6) 0.0158(4) 0.4107(2) 0.0339(11) Uani 1 1 d . . . H5 H 1.0591 -0.0495 0.4193 0.041 Uiso 1 1 calc R . . C6 C 0.8741(5) 0.0317(4) 0.4384(2) 0.0319(11) Uani 1 1 d . . . H6 H 0.8376 -0.0229 0.4658 0.038 Uiso 1 1 calc R . . C7 C 0.4573(5) 0.1192(4) 0.6005(2) 0.0265(9) Uani 1 1 d . . . C8 C 0.2916(5) 0.2233(4) 0.6678(2) 0.0341(11) Uani 1 1 d . . . H8A H 0.2701 0.2663 0.6300 0.041 Uiso 1 1 calc R . . H8B H 0.3443 0.2724 0.6964 0.041 Uiso 1 1 calc R . . C9 C 0.1562(6) 0.1872(5) 0.6975(2) 0.0362(11) Uani 1 1 d . . . H9A H 0.1023 0.2537 0.7106 0.043 Uiso 1 1 calc R . . H9B H 0.0981 0.1467 0.6667 0.043 Uiso 1 1 calc R . . C10 C 0.2524(5) 0.0197(4) 0.7297(2) 0.0317(11) Uani 1 1 d . . . H10A H 0.1949 -0.0194 0.6982 0.038 Uiso 1 1 calc R . . H10B H 0.2643 -0.0310 0.7653 0.038 Uiso 1 1 calc R . . C11 C 0.3966(5) 0.0469(4) 0.7029(2) 0.0313(11) Uani 1 1 d . . . H11A H 0.4580 0.0793 0.7353 0.038 Uiso 1 1 calc R . . H11B H 0.4422 -0.0219 0.6876 0.038 Uiso 1 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 Hg 0.02917(14) 0.03659(14) 0.02777(14) -0.00206(7) 0.00388(7) -0.00062(8) S1 0.0350(7) 0.0329(6) 0.0288(6) 0.0048(5) 0.0039(5) 0.0062(5) S2 0.0279(6) 0.0318(6) 0.0327(6) -0.0004(5) 0.0016(4) 0.0055(5) O 0.038(2) 0.0380(19) 0.0315(19) 0.0003(15) 0.0096(14) 0.0008(17) N 0.026(2) 0.032(2) 0.029(2) 0.0010(17) 0.0042(15) 0.0029(17) C1 0.027(2) 0.036(3) 0.023(2) -0.0048(19) 0.0000(17) -0.0022(19) C2 0.032(3) 0.030(2) 0.034(3) -0.002(2) 0.000(2) 0.001(2) C3 0.041(3) 0.032(2) 0.028(2) -0.0009(19) 0.001(2) -0.005(2) C4 0.028(2) 0.039(3) 0.033(3) -0.009(2) -0.001(2) 0.000(2) C5 0.040(3) 0.029(3) 0.033(3) -0.005(2) -0.010(2) 0.004(2) C6 0.034(3) 0.033(3) 0.029(2) 0.000(2) -0.0032(18) -0.001(2) C7 0.024(2) 0.026(2) 0.029(2) 0.0010(18) -0.0015(18) -0.0029(19) C8 0.034(3) 0.033(3) 0.036(3) 0.003(2) 0.008(2) 0.006(2) C9 0.032(3) 0.042(3) 0.034(3) -0.004(2) 0.003(2) 0.006(2) C10 0.037(3) 0.030(2) 0.028(2) -0.0008(19) 0.0009(19) -0.002(2) C11 0.032(3) 0.035(3) 0.027(2) 0.006(2) -0.0007(18) 0.003(2) _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 C1 2.078(5) . ? Hg S1 2.3979(12) . ? Hg S2 2.9725(13) . ? S1 C7 1.750(5) . ? S2 C7 1.699(5) . ? O C9 1.416(7) . ? O C10 1.433(6) . ? N C7 1.332(6) . ? N C11 1.473(6) . ? N C8 1.474(6) . ? C1 C6 1.387(7) . ? C1 C2 1.400(7) . ? C2 C3 1.397(7) . ? C2 H2 0.9500 . ? C3 C4 1.375(8) . ? C3 H3 0.9500 . ? C4 C5 1.388(7) . ? C4 H4 0.9500 . ? C5 C6 1.395(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.494(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.515(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? 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 Hg S1 169.97(14) . . ? C1 Hg S2 114.32(14) . . ? S1 Hg S2 66.66(4) . . ? C7 S1 Hg 95.19(16) . . ? C7 S2 Hg 77.70(16) . . ? C9 O C10 108.9(3) . . ? C7 N C11 121.8(4) . . ? C7 N C8 123.9(4) . . ? C11 N C8 113.4(4) . . ? C6 C1 C2 118.8(5) . . ? C6 C1 Hg 119.0(4) . . ? C2 C1 Hg 121.9(4) . . ? C3 C2 C1 120.6(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.9(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.2(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.4(5) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N C7 S2 122.6(4) . . ? N C7 S1 117.2(4) . . ? S2 C7 S1 120.2(3) . . ? N C8 C9 110.8(4) . . ? N C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O C9 C8 112.6(4) . . ? O C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? O C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? O C10 C11 111.7(4) . . ? O C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? O C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? N C11 C10 109.6(4) . . ? N C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? N C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.968 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.176 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 681260' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H19 Hg N S2' _chemical_formula_sum 'C21 H19 Hg N S2' _chemical_formula_weight 550.08 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' S S 0.1246 0.1234 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8490(3) _cell_length_b 11.6810(5) _cell_length_c 18.5340(7) _cell_angle_alpha 80.935(2) _cell_angle_beta 85.358(2) _cell_angle_gamma 90.025(2) _cell_volume 1885.47(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32748 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 8.388 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23996 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1070 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.25 _diffrn_reflns_theta_max 27.41 _reflns_number_total 23996 _reflns_number_gt 17531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0998P)^2^+8.1740P] 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 SHELXL _refine_ls_extinction_coef 0.0058(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 23996 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.2017 _refine_ls_wR_factor_gt 0.1836 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Hg1 Hg 0.89035(4) 0.65477(3) 0.02930(2) 0.03356(13) Uani 1 1 d . . . Hg2 Hg 0.38962(4) 0.83143(3) 0.02949(2) 0.03381(13) Uani 1 1 d . . . S1 S 0.8651(3) 0.4786(2) 0.15927(15) 0.0349(5) Uani 1 1 d . . . S2 S 1.0774(3) 0.6779(2) 0.11254(14) 0.0322(5) Uani 1 1 d . . . S3 S 0.5768(3) 0.7660(2) 0.11227(14) 0.0321(5) Uani 1 1 d . . . S4 S 0.3631(3) 0.9413(2) 0.16116(15) 0.0343(5) Uani 1 1 d . . . N1 N 1.0655(9) 0.5481(7) 0.2446(5) 0.0282(17) Uani 1 1 d . . . N2 N 0.5643(10) 0.8288(7) 0.2441(5) 0.0299(17) Uani 1 1 d . . . C1 C 0.7313(11) 0.6461(9) -0.0464(5) 0.0281(18) Uani 1 1 d . . . C2 C 0.6744(14) 0.5461(10) -0.0584(6) 0.038(2) Uani 1 1 d . . . H2 H 0.7125 0.4760 -0.0336 0.046 Uiso 1 1 calc R . . C3 C 0.5617(14) 0.5400(10) -0.1055(6) 0.042(3) Uani 1 1 d . . . H3 H 0.5204 0.4680 -0.1128 0.051 Uiso 1 1 calc R . . C4 C 0.5131(15) 0.6441(11) -0.1411(7) 0.043(3) Uani 1 1 d . . . H4 H 0.4390 0.6425 -0.1753 0.051 Uiso 1 1 calc R . . C5 C 0.5635(11) 0.7464(9) -0.1304(6) 0.033(2) Uani 1 1 d . . . H5 H 0.5259 0.8169 -0.1549 0.040 Uiso 1 1 calc R . . C6 C 0.6723(12) 0.7448(9) -0.0821(4) 0.032(2) Uani 1 1 d . . . H6 H 0.7092 0.8171 -0.0729 0.038 Uiso 1 1 calc R . . C7 C 1.0044(10) 0.5636(7) 0.1765(7) 0.026(2) Uani 1 1 d . . . C8 C 0.9981(11) 0.4664(9) 0.3071(6) 0.0300(19) Uani 1 1 d . . . H8A H 0.9013 0.4361 0.2938 0.036 Uiso 1 1 calc R . . H8B H 0.9744 0.5087 0.3489 0.036 Uiso 1 1 calc R . . C9 C 1.0995(15) 0.3645(11) 0.3315(7) 0.024(3) Uani 1 1 d . . . C10 C 1.1661(14) 0.3011(9) 0.2807(6) 0.034(2) Uani 1 1 d . . . H10 H 1.1556 0.3250 0.2299 0.041 Uiso 1 1 calc R . . C11 C 1.2493(17) 0.2010(11) 0.3039(6) 0.045(3) Uani 1 1 d . . . H11 H 1.2894 0.1544 0.2695 0.054 Uiso 1 1 calc R . . C12 C 1.2721(19) 0.1711(14) 0.3776(10) 0.055(4) Uani 1 1 d . . . H12 H 1.3328 0.1061 0.3929 0.066 Uiso 1 1 calc R . . C13 C 1.206(2) 0.2362(17) 0.4312(9) 0.041(4) Uani 1 1 d . . . H13 H 1.2181 0.2169 0.4821 0.049 Uiso 1 1 calc R . . C14 C 1.121(2) 0.3314(15) 0.4012(9) 0.044(4) Uani 1 1 d . . . H14 H 1.0750 0.3769 0.4348 0.053 Uiso 1 1 calc R . . C15 C 1.1992(10) 0.6118(8) 0.2603(5) 0.0281(19) Uani 1 1 d . . . H15A H 1.2471 0.6549 0.2137 0.034 Uiso 1 1 calc R . . H15B H 1.2737 0.5556 0.2813 0.034 Uiso 1 1 calc R . . C16 C 1.1610(12) 0.6964(9) 0.3130(5) 0.0274(19) Uani 1 1 d . . . C17 C 1.2027(18) 0.6695(15) 0.3833(10) 0.049(4) Uani 1 1 d . . . H17 H 1.2551 0.5995 0.3972 0.059 Uiso 1 1 calc R . . C18 C 1.169(2) 0.7445(19) 0.4359(8) 0.048(5) Uani 1 1 d . . . H18 H 1.1982 0.7283 0.4847 0.057 Uiso 1 1 calc R . . C19 C 1.088(2) 0.8460(18) 0.4092(12) 0.057(5) Uani 1 1 d . . . H19 H 1.0600 0.8979 0.4424 0.069 Uiso 1 1 calc R . . C20 C 1.0497(19) 0.8723(15) 0.3416(10) 0.040(4) Uani 1 1 d . . . H20 H 0.9986 0.9425 0.3267 0.048 Uiso 1 1 calc R . . C21 C 1.0833(14) 0.7992(10) 0.2941(6) 0.035(2) Uani 1 1 d . . . H21 H 1.0532 0.8181 0.2456 0.042 Uiso 1 1 calc R . . C22 C 0.2250(11) 0.8712(9) -0.0457(5) 0.032(2) Uani 1 1 d . . . C23 C 0.1753(11) 0.7899(7) -0.0824(6) 0.0295(19) Uani 1 1 d . . . H23 H 0.2136 0.7133 -0.0748 0.035 Uiso 1 1 calc R . . C24 C 0.0646(13) 0.8214(10) -0.1325(5) 0.039(2) Uani 1 1 d . . . H24 H 0.0268 0.7637 -0.1574 0.047 Uiso 1 1 calc R . . C25 C 0.0092(12) 0.9324(10) -0.1469(7) 0.035(3) Uani 1 1 d . . . H25 H -0.0627 0.9525 -0.1821 0.042 Uiso 1 1 calc R . . C26 C 0.0643(16) 1.0143(10) -0.1070(8) 0.050(3) Uani 1 1 d . . . H26 H 0.0297 1.0918 -0.1162 0.060 Uiso 1 1 calc R . . C27 C 0.1667(14) 0.9861(8) -0.0550(6) 0.040(3) Uani 1 1 d . . . H27 H 0.1975 1.0413 -0.0264 0.048 Uiso 1 1 calc R . . C28 C 0.5067(12) 0.8481(8) 0.1813(6) 0.028(2) Uani 1 1 d . . . C29 C 0.6983(10) 0.7588(9) 0.2597(5) 0.0277(19) Uani 1 1 d . . . H29A H 0.7731 0.8056 0.2797 0.033 Uiso 1 1 calc R . . H29B H 0.7452 0.7378 0.2133 0.033 Uiso 1 1 calc R . . C30 C 0.6605(13) 0.6461(10) 0.3151(6) 0.037(2) Uani 1 1 d . . . C31 C 0.5871(13) 0.5562(10) 0.2914(6) 0.031(2) Uani 1 1 d . . . H31 H 0.5613 0.5632 0.2422 0.038 Uiso 1 1 calc R . . C32 C 0.5506(16) 0.4528(14) 0.3418(10) 0.040(4) Uani 1 1 d . . . H32 H 0.4964 0.3912 0.3272 0.048 Uiso 1 1 calc R . . C33 C 0.597(2) 0.4434(14) 0.4142(7) 0.038(4) Uani 1 1 d . . . H33 H 0.5772 0.3744 0.4484 0.046 Uiso 1 1 calc R . . C34 C 0.671(2) 0.5367(19) 0.4335(12) 0.052(5) Uani 1 1 d . . . H34 H 0.6971 0.5320 0.4825 0.063 Uiso 1 1 calc R . . C35 C 0.7069(15) 0.6349(13) 0.3854(7) 0.036(3) Uani 1 1 d . . . H35 H 0.7636 0.6953 0.3999 0.043 Uiso 1 1 calc R . . C36 C 0.4979(12) 0.8803(9) 0.3065(6) 0.033(2) Uani 1 1 d . . . H36A H 0.4719 0.8172 0.3480 0.040 Uiso 1 1 calc R . . H36B H 0.4023 0.9185 0.2927 0.040 Uiso 1 1 calc R . . C37 C 0.5974(16) 0.9669(14) 0.3320(9) 0.033(3) Uani 1 1 d . . . C38 C 0.6144(19) 0.9592(14) 0.4096(7) 0.031(3) Uani 1 1 d . . . H38 H 0.5722 0.8975 0.4452 0.037 Uiso 1 1 calc R . . C39 C 0.698(3) 1.0501(17) 0.4276(11) 0.046(5) Uani 1 1 d . . . H39 H 0.7084 1.0500 0.4782 0.056 Uiso 1 1 calc R . . C40 C 0.7635(18) 1.1355(14) 0.3816(8) 0.043(4) Uani 1 1 d . . . H40 H 0.8188 1.1938 0.3991 0.052 Uiso 1 1 calc R . . C41 C 0.7516(17) 1.1402(10) 0.3078(7) 0.045(3) Uani 1 1 d . . . H41 H 0.8027 1.1999 0.2738 0.054 Uiso 1 1 calc R . . C42 C 0.6652(15) 1.0581(10) 0.2828(6) 0.034(2) Uani 1 1 d . . . H42 H 0.6523 1.0640 0.2320 0.041 Uiso 1 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 Hg1 0.0295(2) 0.0403(3) 0.0316(2) -0.00524(14) -0.00734(16) 0.00524(15) Hg2 0.0298(2) 0.0396(2) 0.0324(2) -0.00421(14) -0.00752(16) -0.00342(15) S1 0.0301(12) 0.0329(13) 0.0424(14) -0.0037(10) -0.0120(11) -0.0041(9) S2 0.0302(12) 0.0302(13) 0.0350(12) 0.0007(9) -0.0077(10) -0.0024(9) S3 0.0267(11) 0.0364(13) 0.0361(12) -0.0110(9) -0.0095(10) 0.0042(9) S4 0.0328(13) 0.0335(13) 0.0386(13) -0.0086(10) -0.0087(11) 0.0102(10) N1 0.018(3) 0.034(4) 0.034(4) -0.006(3) -0.004(3) -0.004(3) N2 0.030(4) 0.029(4) 0.031(4) -0.007(3) -0.001(3) 0.000(3) C1 0.030(5) 0.035(5) 0.018(4) -0.008(3) 0.011(3) 0.004(4) C2 0.046(6) 0.039(6) 0.030(5) -0.010(4) 0.007(4) -0.003(5) C3 0.046(7) 0.044(6) 0.039(6) -0.009(5) -0.007(5) -0.006(5) C4 0.042(7) 0.061(8) 0.025(5) -0.006(5) -0.001(5) -0.004(5) C5 0.026(5) 0.033(5) 0.041(5) -0.005(4) 0.003(4) 0.000(4) C6 0.038(5) 0.046(6) 0.013(3) -0.006(3) -0.007(4) 0.015(4) C7 0.010(4) 0.013(4) 0.054(6) 0.000(4) -0.005(4) 0.002(3) C8 0.023(4) 0.032(5) 0.036(5) -0.006(4) -0.002(4) -0.001(4) C9 0.027(7) 0.025(5) 0.018(5) 0.002(4) 0.000(5) 0.003(5) C10 0.031(6) 0.030(5) 0.041(6) -0.002(4) -0.002(5) -0.003(5) C11 0.060(8) 0.042(6) 0.031(5) -0.001(4) 0.004(5) 0.016(6) C12 0.056(10) 0.038(7) 0.068(10) -0.002(6) -0.005(8) 0.024(7) C13 0.046(9) 0.057(9) 0.019(6) 0.003(5) -0.008(5) 0.002(6) C14 0.040(8) 0.045(8) 0.051(9) -0.025(6) 0.007(6) -0.002(6) C15 0.020(4) 0.031(5) 0.032(5) 0.001(4) -0.006(4) -0.002(4) C16 0.023(5) 0.033(5) 0.026(4) -0.001(4) -0.004(4) -0.006(4) C17 0.052(9) 0.044(7) 0.053(8) -0.011(6) -0.015(7) -0.004(7) C18 0.063(11) 0.073(11) 0.012(5) -0.022(6) 0.003(5) -0.014(8) C19 0.043(9) 0.054(10) 0.082(12) -0.029(8) -0.015(8) -0.013(7) C20 0.040(9) 0.034(7) 0.048(8) -0.008(5) -0.006(7) -0.005(6) C21 0.026(5) 0.042(6) 0.035(6) -0.003(4) -0.005(5) -0.006(5) C22 0.023(5) 0.041(5) 0.031(5) 0.003(4) -0.004(4) -0.007(4) C23 0.029(4) 0.012(4) 0.046(5) 0.001(3) -0.001(4) 0.005(3) C24 0.043(6) 0.047(6) 0.025(5) 0.000(4) -0.006(4) 0.001(5) C25 0.020(4) 0.047(6) 0.033(5) 0.004(5) -0.002(4) 0.017(4) C26 0.064(8) 0.025(6) 0.059(8) -0.006(5) -0.003(6) 0.009(5) C27 0.056(7) 0.022(5) 0.046(6) -0.004(4) -0.027(5) -0.002(4) C28 0.031(5) 0.028(5) 0.025(5) -0.003(4) -0.008(4) -0.009(4) C29 0.020(4) 0.041(5) 0.023(4) -0.008(4) -0.001(3) 0.004(4) C30 0.027(5) 0.040(6) 0.043(6) -0.010(4) 0.000(5) 0.006(5) C31 0.019(5) 0.040(6) 0.035(5) -0.007(4) -0.002(4) 0.006(4) C32 0.021(7) 0.038(7) 0.060(9) -0.002(6) -0.005(6) -0.002(5) C33 0.045(7) 0.043(8) 0.021(5) 0.007(5) 0.009(5) 0.001(6) C34 0.049(10) 0.064(10) 0.050(9) -0.020(7) -0.018(7) 0.007(8) C35 0.041(7) 0.047(7) 0.023(5) -0.019(5) -0.004(5) 0.004(6) C36 0.032(5) 0.034(5) 0.036(5) -0.011(4) -0.003(4) 0.003(4) C37 0.024(7) 0.039(7) 0.036(7) -0.005(5) -0.008(6) 0.004(5) C38 0.036(6) 0.047(7) 0.013(4) -0.007(4) -0.010(4) -0.003(5) C39 0.050(8) 0.050(9) 0.045(9) -0.027(7) -0.005(7) -0.012(6) C40 0.060(9) 0.043(7) 0.032(6) -0.016(5) -0.013(6) -0.006(7) C41 0.050(7) 0.033(6) 0.053(7) -0.011(5) 0.004(6) -0.008(5) C42 0.038(6) 0.045(6) 0.021(5) -0.008(4) -0.003(5) -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 Hg1 C1 2.079(10) . ? Hg1 S2 2.395(2) . ? Hg1 S1 2.905(3) . ? Hg2 C22 2.098(9) . ? Hg2 S3 2.392(2) . ? Hg2 S4 2.924(3) . ? S1 C7 1.665(9) . ? S2 C7 1.726(10) . ? S3 C28 1.789(12) . ? S4 C28 1.699(11) . ? N1 C7 1.399(14) . ? N1 C8 1.466(12) . ? N1 C15 1.469(11) . ? N2 C28 1.296(13) . ? N2 C29 1.463(12) . ? N2 C36 1.467(13) . ? C1 C2 1.329(15) . ? C1 C6 1.363(13) . ? C2 C3 1.387(16) . ? C3 C4 1.375(17) . ? C4 C5 1.324(16) . ? C5 C6 1.364(14) . ? C8 C9 1.525(15) . ? C9 C14 1.32(2) . ? C9 C10 1.384(18) . ? C10 C11 1.410(16) . ? C11 C12 1.39(2) . ? C12 C13 1.43(3) . ? C13 C14 1.41(3) . ? C15 C16 1.516(14) . ? C16 C17 1.37(2) . ? C16 C21 1.395(16) . ? C17 C18 1.43(2) . ? C18 C19 1.43(3) . ? C19 C20 1.31(3) . ? C20 C21 1.34(2) . ? C22 C23 1.345(14) . ? C22 C27 1.428(15) . ? C23 C24 1.414(14) . ? C24 C25 1.380(15) . ? C25 C26 1.408(18) . ? C26 C27 1.378(16) . ? C29 C30 1.555(15) . ? C30 C31 1.381(16) . ? C30 C35 1.385(17) . ? C31 C32 1.42(2) . ? C32 C33 1.42(2) . ? C33 C34 1.38(3) . ? C34 C35 1.36(3) . ? C36 C37 1.496(18) . ? C37 C42 1.39(2) . ? C37 C38 1.45(2) . ? C38 C39 1.39(2) . ? C39 C40 1.31(3) . ? C40 C41 1.37(2) . ? C41 C42 1.384(16) . ? 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 Hg1 S2 176.1(3) . . ? C1 Hg1 S1 116.5(3) . . ? S2 Hg1 S1 67.26(7) . . ? C22 Hg2 S3 174.0(3) . . ? C22 Hg2 S4 117.4(3) . . ? S3 Hg2 S4 67.40(8) . . ? C7 S1 Hg1 77.6(4) . . ? C7 S2 Hg1 92.9(4) . . ? C28 S3 Hg2 95.0(3) . . ? C28 S4 Hg2 79.8(4) . . ? C7 N1 C8 121.8(7) . . ? C7 N1 C15 123.8(8) . . ? C8 N1 C15 114.4(7) . . ? C28 N2 C29 125.0(9) . . ? C28 N2 C36 120.7(9) . . ? C29 N2 C36 114.2(8) . . ? C2 C1 C6 116.9(10) . . ? C2 C1 Hg1 122.4(8) . . ? C6 C1 Hg1 120.5(8) . . ? C1 C2 C3 122.7(11) . . ? C4 C3 C2 116.2(11) . . ? C5 C4 C3 123.8(12) . . ? C4 C5 C6 116.3(10) . . ? C1 C6 C5 124.1(10) . . ? N1 C7 S1 121.5(7) . . ? N1 C7 S2 116.5(7) . . ? S1 C7 S2 122.0(7) . . ? N1 C8 C9 113.8(9) . . ? C14 C9 C10 118.2(12) . . ? C14 C9 C8 121.5(13) . . ? C10 C9 C8 120.2(11) . . ? C9 C10 C11 120.2(11) . . ? C12 C11 C10 119.3(12) . . ? C11 C12 C13 121.4(13) . . ? C14 C13 C12 113.6(14) . . ? C9 C14 C13 127.2(15) . . ? N1 C15 C16 112.8(8) . . ? C17 C16 C21 118.4(12) . . ? C17 C16 C15 118.3(11) . . ? C21 C16 C15 123.3(9) . . ? C16 C17 C18 121.3(16) . . ? C17 C18 C19 114.3(15) . . ? C20 C19 C18 124.3(18) . . ? C19 C20 C21 119.3(17) . . ? C20 C21 C16 122.4(12) . . ? C23 C22 C27 121.8(9) . . ? C23 C22 Hg2 120.6(8) . . ? C27 C22 Hg2 117.6(7) . . ? C22 C23 C24 118.3(9) . . ? C25 C24 C23 122.9(10) . . ? C24 C25 C26 116.8(10) . . ? C27 C26 C25 122.3(10) . . ? C26 C27 C22 117.8(9) . . ? N2 C28 S4 124.6(9) . . ? N2 C28 S3 117.8(8) . . ? S4 C28 S3 117.5(6) . . ? N2 C29 C30 112.6(8) . . ? C31 C30 C35 121.2(11) . . ? C31 C30 C29 118.6(10) . . ? C35 C30 C29 120.1(11) . . ? C30 C31 C32 119.2(12) . . ? C33 C32 C31 118.9(14) . . ? C34 C33 C32 118.5(15) . . ? C35 C34 C33 122.8(17) . . ? C34 C35 C30 119.3(14) . . ? N2 C36 C37 115.0(10) . . ? C42 C37 C38 119.9(13) . . ? C42 C37 C36 120.9(13) . . ? C38 C37 C36 119.1(13) . . ? C39 C38 C37 114.1(14) . . ? C40 C39 C38 126.3(16) . . ? C39 C40 C41 119.3(14) . . ? C40 C41 C42 120.1(12) . . ? C41 C42 C37 120.1(11) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 3.594 _refine_diff_density_min -3.044 _refine_diff_density_rms 0.299