# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1422 data_global # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Alfonso Casti\~neiras Departamento de Quimica Inorganica Universidad de Santiago de Compostela E-15706 Santiago de Compostela (Spain) ; _publ_contact_author_phone +34-981594636 _publ_contact_author_fax +34-981547163 _publ_contact_author_email qiac01@usc.es _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir, Please find enclosed the data of X-ray structure analyses of the compounds: [Ag(pyOS)(dppm)] (97il09) Compound No. 1 (with Z = 2) [HgCl2(pyOSBz)]2 (97il04) Compound No. 5 [PhHg(PyS)] (98il04) Compound No. 11 of the Dalton paper No. 9/00405J With thanks in advance, Yours sincerely, Alfonso Casti\~neiras ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reference No. 9/00405J The chemistry of pyridinethiols and related ligands-10. Heterocyclic-2- thione derivatives of silver(I) and mercury(II): The crystal structures of dimeric [(1-oxo-pyridine-2-thionato){bis(diphenylphosphino)methane}silver(I), {2-(benzylthio)pyridine-1-oxide}dichloromercury(II) and (pyridine-2- thionato) phenylmercury(II) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Tarlok S. Lobana' ;Guru Nanak Dev University Department of Chemistry Punjab Amritsar-143 005 India ; 'Seema Paul' ;Guru Nanak Dev University Department of Chemistry Punjab Amritsar-143 005 India ; 'Alfonso Castineiras' ; Universidad de Santiago de Compostela Departamento de Quimica Inorganica Facultad de Farmacia 15706 Santiago de Compostela Spain ; #======================================================================= data_97il09 #(Compound No. 1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Ag N O P2 S' _chemical_formula_weight 618.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 '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 'triclinic' _symmetry_space_group_name_H-M 'P 1 bar (No. 2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2139(4) _cell_length_b 12.2698(9) _cell_length_c 12.6138(11) _cell_angle_alpha 60.275(6) _cell_angle_beta 67.096(4) _cell_angle_gamma 88.802(5) _cell_volume 1355.86(16) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.491 _cell_measurement_theta_max 42.234 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 7.983 _exptl_absorpt_correction_type 'Psi-scan' _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.963 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Enraf Nonius ' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5823 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 74.29 _reflns_number_total 5526 _reflns_number_gt 4312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Enraf Nonius, 1994)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP Zsolnai, 1997)' _computing_publication_material 'SHELXL-97 (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 w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5526 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.54966(3) 0.67445(3) 0.44814(3) 0.04294(11) Uani 1 d . . . S1 S 0.54245(14) 0.82345(11) 0.21820(11) 0.0550(3) Uani 1 d . . . P1 P 0.30447(10) 0.60239(9) 0.58346(11) 0.0385(2) Uani 1 d . . . P2 P 0.74593(10) 0.60405(9) 0.47326(10) 0.0372(2) Uani 1 d . . . O1 O 0.5642(3) 0.8908(3) 0.4082(3) 0.0487(7) Uani 1 d . . . N1 N 0.5232(3) 0.9749(3) 0.3199(3) 0.0422(8) Uani 1 d . . . C1 C 0.5096(4) 0.9579(4) 0.2254(4) 0.0454(10) Uani 1 d . . . C2 C 0.4678(6) 1.0556(5) 0.1359(5) 0.0608(13) Uani 1 d . . . C3 C 0.4429(6) 1.1629(5) 0.1407(6) 0.0679(15) Uani 1 d . . . C4 C 0.4562(6) 1.1754(5) 0.2379(6) 0.0610(13) Uani 1 d . . . C5 C 0.4949(5) 1.0811(4) 0.3264(5) 0.0491(10) Uani 1 d . . . C10 C 0.2336(5) 0.5557(4) 0.4987(5) 0.0446(10) Uani 1 d . . . C11 C 0.2391(4) 0.7438(4) 0.5686(5) 0.0458(10) Uani 1 d . . . C12 C 0.1965(5) 0.8186(5) 0.4712(6) 0.0582(13) Uani 1 d . . . C13 C 0.1575(6) 0.9306(5) 0.4593(7) 0.0735(18) Uani 1 d . . . C14 C 0.1618(6) 0.9688(6) 0.5423(9) 0.085(2) Uani 1 d . . . C15 C 0.2064(6) 0.8973(6) 0.6382(8) 0.077(2) Uani 1 d . . . C16 C 0.2447(5) 0.7841(5) 0.6529(6) 0.0589(13) Uani 1 d . . . C21 C 0.2103(4) 0.4785(4) 0.7628(4) 0.0425(9) Uani 1 d . . . C22 C 0.2724(5) 0.3891(5) 0.8272(5) 0.0515(11) Uani 1 d . . . C23 C 0.2021(7) 0.2877(6) 0.9616(5) 0.0659(14) Uani 1 d . . . C24 C 0.0705(7) 0.2814(6) 1.0292(6) 0.0722(17) Uani 1 d . . . C25 C 0.0071(6) 0.3691(6) 0.9686(6) 0.0765(17) Uani 1 d . . . C26 C 0.0770(6) 0.4687(6) 0.8344(6) 0.0680(15) Uani 1 d . . . C31 C 0.9010(4) 0.7145(4) 0.3330(4) 0.0417(9) Uani 1 d . . . C32 C 0.8939(5) 0.8413(4) 0.2557(5) 0.0539(11) Uani 1 d . . . C33 C 1.0096(7) 0.9325(5) 0.1515(6) 0.0712(16) Uani 1 d . . . C34 C 1.1295(7) 0.8989(6) 0.1242(6) 0.0716(17) Uani 1 d . . . C35 C 1.1377(6) 0.7746(7) 0.1993(6) 0.0725(16) Uani 1 d . . . C36 C 1.0237(6) 0.6828(5) 0.3033(6) 0.0631(14) Uani 1 d . . . C41 C 0.7543(4) 0.5897(4) 0.6222(4) 0.0409(9) Uani 1 d . . . C42 C 0.8458(5) 0.6725(4) 0.6118(5) 0.0472(10) Uani 1 d . . . C43 C 0.8432(6) 0.6636(5) 0.7266(6) 0.0585(13) Uani 1 d . . . C44 C 0.7508(6) 0.5714(6) 0.8518(6) 0.0651(14) Uani 1 d . . . C45 C 0.6579(6) 0.4895(6) 0.8642(6) 0.0714(16) Uani 1 d . . . C46 C 0.6598(6) 0.4983(5) 0.7501(5) 0.0598(13) Uani 1 d . . . H2 H 0.455(5) 1.044(5) 0.068(5) 0.056(14) Uiso 1 d . . . H3 H 0.418(6) 1.235(6) 0.071(6) 0.080(18) Uiso 1 d . . . H4 H 0.434(5) 1.241(5) 0.257(5) 0.070(17) Uiso 1 d . . . H5 H 0.514(5) 1.082(5) 0.393(5) 0.057(14) Uiso 1 d . . . H12 H 0.195(5) 0.802(5) 0.417(5) 0.059(17) Uiso 1 d . . . H13 H 0.133(6) 0.980(6) 0.387(6) 0.072(18) Uiso 1 d . . . H14 H 0.153(6) 1.038(6) 0.534(6) 0.09(2) Uiso 1 d . . . H15 H 0.219(7) 0.937(7) 0.677(7) 0.11(3) Uiso 1 d . . . H16 H 0.276(5) 0.727(5) 0.720(5) 0.055(15) Uiso 1 d . . . H22 H 0.360(5) 0.391(5) 0.772(5) 0.053(14) Uiso 1 d . . . H23 H 0.245(6) 0.222(6) 1.001(6) 0.074(18) Uiso 1 d . . . H24 H 0.026(5) 0.219(5) 1.111(5) 0.059(15) Uiso 1 d . . . H25 H -0.097(6) 0.367(5) 1.017(6) 0.081(18) Uiso 1 d . . . H26 H 0.038(6) 0.521(6) 0.793(6) 0.08(2) Uiso 1 d . . . H32 H 0.811(5) 0.878(5) 0.271(5) 0.064(15) Uiso 1 d . . . H33 H 1.002(7) 1.013(7) 0.101(7) 0.12(3) Uiso 1 d . . . H34 H 1.200(7) 0.949(7) 0.061(7) 0.11(3) Uiso 1 d . . . H35 H 1.212(6) 0.755(6) 0.174(6) 0.072(18) Uiso 1 d . . . H36 H 1.035(5) 0.614(5) 0.340(5) 0.050(15) Uiso 1 d . . . H42 H 0.901(4) 0.730(4) 0.538(4) 0.036(12) Uiso 1 d . . . H43 H 0.909(6) 0.715(6) 0.719(6) 0.082(19) Uiso 1 d . . . H44 H 0.755(5) 0.570(5) 0.921(5) 0.061(15) Uiso 1 d . . . H45 H 0.598(6) 0.426(5) 0.941(6) 0.069(17) Uiso 1 d . . . H46 H 0.602(5) 0.446(5) 0.756(5) 0.052(14) Uiso 1 d . . . H101 H 0.153(5) 0.562(4) 0.523(4) 0.041(12) Uiso 1 d . . . H102 H 0.282(4) 0.619(4) 0.401(5) 0.042(12) 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 Ag 0.04302(17) 0.04344(18) 0.04865(18) -0.02680(14) -0.02270(14) 0.01527(12) S1 0.0799(8) 0.0493(6) 0.0444(6) -0.0288(5) -0.0299(6) 0.0211(6) P1 0.0379(5) 0.0340(5) 0.0452(6) -0.0235(4) -0.0163(4) 0.0098(4) P2 0.0383(5) 0.0322(5) 0.0429(5) -0.0202(4) -0.0188(4) 0.0092(4) O1 0.071(2) 0.0401(16) 0.0519(17) -0.0262(14) -0.0395(16) 0.0185(15) N1 0.0451(19) 0.0348(17) 0.0397(18) -0.0164(15) -0.0168(16) 0.0056(15) C1 0.047(2) 0.047(2) 0.036(2) -0.0205(19) -0.0132(18) 0.0064(19) C2 0.078(4) 0.060(3) 0.055(3) -0.029(3) -0.042(3) 0.024(3) C3 0.086(4) 0.049(3) 0.066(3) -0.021(3) -0.044(3) 0.026(3) C4 0.072(3) 0.041(2) 0.073(3) -0.028(2) -0.037(3) 0.019(2) C5 0.054(3) 0.042(2) 0.053(3) -0.025(2) -0.024(2) 0.008(2) C10 0.049(3) 0.035(2) 0.052(3) -0.022(2) -0.026(2) 0.0149(19) C11 0.038(2) 0.033(2) 0.057(3) -0.0251(19) -0.0103(19) 0.0029(17) C12 0.052(3) 0.041(2) 0.075(4) -0.028(3) -0.026(3) 0.015(2) C13 0.057(3) 0.037(3) 0.097(5) -0.023(3) -0.024(3) 0.013(2) C14 0.062(4) 0.042(3) 0.129(6) -0.046(4) -0.019(4) 0.017(3) C15 0.057(3) 0.059(3) 0.109(5) -0.062(4) -0.007(3) 0.001(3) C16 0.053(3) 0.048(3) 0.070(3) -0.038(3) -0.011(3) 0.006(2) C21 0.047(2) 0.037(2) 0.041(2) -0.0223(18) -0.0145(19) 0.0072(18) C22 0.064(3) 0.046(2) 0.048(3) -0.027(2) -0.024(2) 0.016(2) C23 0.083(4) 0.060(3) 0.049(3) -0.023(3) -0.033(3) 0.015(3) C24 0.100(5) 0.051(3) 0.041(3) -0.020(3) -0.014(3) 0.001(3) C25 0.068(4) 0.069(4) 0.059(3) -0.030(3) -0.002(3) 0.007(3) C26 0.057(3) 0.055(3) 0.061(3) -0.020(3) -0.013(3) 0.016(3) C31 0.047(2) 0.034(2) 0.042(2) -0.0187(17) -0.0194(18) 0.0054(17) C32 0.058(3) 0.037(2) 0.055(3) -0.019(2) -0.022(2) 0.007(2) C33 0.074(4) 0.041(3) 0.066(4) -0.011(3) -0.023(3) -0.005(3) C34 0.063(4) 0.063(4) 0.056(3) -0.021(3) -0.008(3) -0.012(3) C35 0.045(3) 0.082(4) 0.068(4) -0.036(3) -0.009(3) 0.004(3) C36 0.053(3) 0.048(3) 0.071(4) -0.023(3) -0.024(3) 0.013(2) C41 0.044(2) 0.040(2) 0.044(2) -0.0254(18) -0.0194(18) 0.0106(17) C42 0.049(3) 0.041(2) 0.050(3) -0.024(2) -0.021(2) 0.009(2) C43 0.065(3) 0.061(3) 0.072(3) -0.044(3) -0.038(3) 0.018(3) C44 0.086(4) 0.072(4) 0.063(3) -0.046(3) -0.042(3) 0.031(3) C45 0.078(4) 0.071(4) 0.041(3) -0.023(3) -0.011(3) -0.004(3) C46 0.060(3) 0.057(3) 0.051(3) -0.027(2) -0.016(2) -0.008(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 Ag P2 2.4254(10) . y Ag O1 2.440(3) . y Ag P1 2.4914(11) . y Ag S1 2.5844(12) . y Ag Ag 3.8457(7) 2_666 y S1 C1 1.721(5) . ? P1 C11 1.820(4) . y P1 C21 1.828(4) . y P1 C10 1.840(5) . y P2 C31 1.821(4) . y P2 C10 1.838(4) 2_666 y P2 C41 1.838(4) . y O1 N1 1.326(4) . y N1 C5 1.369(6) . ? N1 C1 1.370(5) . ? C1 C2 1.407(6) . ? C2 C3 1.366(8) . ? C2 H2 1.00(5) . ? C3 C4 1.370(8) . ? C3 H3 1.02(6) . ? C4 C5 1.360(7) . ? C4 H4 0.95(6) . ? C5 H5 0.95(5) . ? C10 P2 1.838(4) 2_666 ? C10 H101 0.86(5) . ? C10 H102 0.98(4) . ? C11 C12 1.378(7) . ? C11 C16 1.398(7) . ? C12 C13 1.387(7) . ? C12 H12 0.81(5) . ? C13 C14 1.359(10) . ? C13 H13 0.96(6) . ? C14 C15 1.372(11) . ? C14 H14 0.81(6) . ? C15 C16 1.389(7) . ? C15 H15 0.89(7) . ? C16 H16 0.99(5) . ? C21 C22 1.369(6) . ? C21 C26 1.383(7) . ? C22 C23 1.398(7) . ? C22 H22 0.95(5) . ? C23 C24 1.368(9) . ? C23 H23 0.95(6) . ? C24 C25 1.351(9) . ? C24 H24 0.86(5) . ? C25 C26 1.389(8) . ? C25 H25 1.08(6) . ? C26 H26 0.84(6) . ? C31 C36 1.380(7) . ? C31 C32 1.389(6) . ? C32 C33 1.392(7) . ? C32 H32 1.02(5) . ? C33 C34 1.361(9) . ? C33 H33 0.89(7) . ? C34 C35 1.364(9) . ? C34 H34 0.83(7) . ? C35 C36 1.383(8) . ? C35 H35 0.85(6) . ? C36 H36 0.77(5) . ? C41 C42 1.382(6) . ? C41 C46 1.382(6) . ? C42 C43 1.386(7) . ? C42 H42 0.81(4) . ? C43 C44 1.361(8) . ? C43 H43 0.93(6) . ? C44 C45 1.371(8) . ? C44 H44 0.89(5) . ? C45 C46 1.381(7) . ? C45 H45 0.87(6) . ? C46 H46 0.88(5) . ? 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 P2 Ag O1 107.22(8) . . y P2 Ag P1 137.92(4) . . y O1 Ag P1 96.58(8) . . y P2 Ag S1 124.55(4) . . y O1 Ag S1 72.85(7) . . y P1 Ag S1 95.16(4) . . y C1 S1 Ag 101.52(15) . . ? C11 P1 C21 103.61(19) . . y C11 P1 C10 102.6(2) . . y C21 P1 C10 103.2(2) . . y C11 P1 Ag 107.20(13) . . y C21 P1 Ag 128.20(15) . . y C10 P1 Ag 109.27(17) . . y C31 P2 C10 105.8(2) . 2_666 y C31 P2 C41 103.48(19) . . y C10 P2 C41 101.1(2) 2_666 . y C31 P2 Ag 113.99(14) . . y C10 P2 Ag 117.91(16) 2_666 . y C41 P2 Ag 112.85(14) . . y N1 O1 Ag 117.6(2) . . y O1 N1 C5 117.0(4) . . ? O1 N1 C1 122.1(3) . . ? C5 N1 C1 120.9(4) . . ? N1 C1 C2 116.4(4) . . ? N1 C1 S1 121.1(3) . . ? C2 C1 S1 122.4(4) . . ? C3 C2 C1 122.4(5) . . ? C3 C2 H2 120(3) . . ? C1 C2 H2 118(3) . . ? C2 C3 C4 119.3(5) . . ? C2 C3 H3 121(3) . . ? C4 C3 H3 119(3) . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4 113(3) . . ? C3 C4 H4 127(3) . . ? C4 C5 N1 121.9(5) . . ? C4 C5 H5 127(3) . . ? N1 C5 H5 111(3) . . ? P2 C10 P1 113.1(2) 2_666 . y P2 C10 H101 112(3) 2_666 . ? P1 C10 H101 109(3) . . ? P2 C10 H102 108(3) 2_666 . ? P1 C10 H102 106(3) . . ? H101 C10 H102 107(4) . . ? C12 C11 C16 118.9(5) . . ? C12 C11 P1 123.5(4) . . ? C16 C11 P1 117.3(4) . . ? C11 C12 C13 120.3(6) . . ? C11 C12 H12 123(4) . . ? C13 C12 H12 117(4) . . ? C14 C13 C12 120.6(7) . . ? C14 C13 H13 123(4) . . ? C12 C13 H13 116(4) . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 126(5) . . ? C15 C14 H14 113(5) . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 113(5) . . ? C16 C15 H15 126(5) . . ? C15 C16 C11 119.8(6) . . ? C15 C16 H16 125(3) . . ? C11 C16 H16 115(3) . . ? C22 C21 C26 118.8(4) . . ? C22 C21 P1 118.9(3) . . ? C26 C21 P1 122.3(4) . . ? C21 C22 C23 120.8(5) . . ? C21 C22 H22 117(3) . . ? C23 C22 H22 122(3) . . ? C24 C23 C22 118.7(6) . . ? C24 C23 H23 122(3) . . ? C22 C23 H23 119(4) . . ? C25 C24 C23 121.7(5) . . ? C25 C24 H24 119(4) . . ? C23 C24 H24 120(4) . . ? C24 C25 C26 119.4(6) . . ? C24 C25 H25 125(3) . . ? C26 C25 H25 116(3) . . ? C21 C26 C25 120.6(6) . . ? C21 C26 H26 118(4) . . ? C25 C26 H26 121(4) . . ? C36 C31 C32 118.5(4) . . ? C36 C31 P2 125.0(4) . . ? C32 C31 P2 116.4(4) . . ? C31 C32 C33 119.6(5) . . ? C31 C32 H32 126(3) . . ? C33 C32 H32 114(3) . . ? C34 C33 C32 120.9(6) . . ? C34 C33 H33 121(5) . . ? C32 C33 H33 118(5) . . ? C35 C34 C33 120.1(6) . . ? C35 C34 H34 116(5) . . ? C33 C34 H34 124(5) . . ? C34 C35 C36 119.7(6) . . ? C34 C35 H35 118(4) . . ? C36 C35 H35 122(4) . . ? C31 C36 C35 121.2(5) . . ? C31 C36 H36 124(4) . . ? C35 C36 H36 115(4) . . ? C42 C41 C46 118.2(4) . . ? C42 C41 P2 122.7(3) . . ? C46 C41 P2 119.0(4) . . ? C41 C42 C43 120.9(5) . . ? C41 C42 H42 121(3) . . ? C43 C42 H42 118(3) . . ? C44 C43 C42 120.0(5) . . ? C44 C43 H43 119(4) . . ? C42 C43 H43 120(4) . . ? C43 C44 C45 120.0(5) . . ? C43 C44 H44 115(3) . . ? C45 C44 H44 125(3) . . ? C44 C45 C46 120.2(5) . . ? C44 C45 H45 125(4) . . ? C46 C45 H45 115(4) . . ? C45 C46 C41 120.7(5) . . ? C45 C46 H46 121(3) . . ? C41 C46 H46 118(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Ag S1 C1 -114.54(16) . . . . ? O1 Ag S1 C1 -15.12(18) . . . . ? P1 Ag S1 C1 80.19(16) . . . . ? P2 Ag P1 C11 135.29(17) . . . . ? O1 Ag P1 C11 10.36(18) . . . . ? S1 Ag P1 C11 -62.92(17) . . . . ? P2 Ag P1 C21 11.44(18) . . . . ? O1 Ag P1 C21 -113.48(18) . . . . ? S1 Ag P1 C21 173.23(17) . . . . ? P2 Ag P1 C10 -114.16(15) . . . . ? O1 Ag P1 C10 120.91(16) . . . . ? S1 Ag P1 C10 47.63(15) . . . . ? O1 Ag P2 C31 -53.84(17) . . . . ? P1 Ag P2 C31 -175.33(15) . . . . ? S1 Ag P2 C31 26.87(16) . . . . ? O1 Ag P2 C10 -178.76(19) . . . 2_666 ? P1 Ag P2 C10 59.75(19) . . . 2_666 ? S1 Ag P2 C10 -98.05(19) . . . 2_666 ? O1 Ag P2 C41 63.83(16) . . . . ? P1 Ag P2 C41 -57.66(16) . . . . ? S1 Ag P2 C41 144.54(15) . . . . ? P2 Ag O1 N1 141.6(3) . . . . ? P1 Ag O1 N1 -73.5(3) . . . . ? S1 Ag O1 N1 19.9(3) . . . . ? Ag O1 N1 C5 161.4(3) . . . . ? Ag O1 N1 C1 -18.8(5) . . . . ? O1 N1 C1 C2 -178.7(4) . . . . ? C5 N1 C1 C2 1.0(6) . . . . ? O1 N1 C1 S1 1.2(6) . . . . ? C5 N1 C1 S1 -179.0(3) . . . . ? Ag S1 C1 N1 14.4(4) . . . . ? Ag S1 C1 C2 -165.7(4) . . . . ? N1 C1 C2 C3 0.6(8) . . . . ? S1 C1 C2 C3 -179.3(5) . . . . ? C1 C2 C3 C4 -1.5(9) . . . . ? C2 C3 C4 C5 0.6(9) . . . . ? C3 C4 C5 N1 1.1(8) . . . . ? O1 N1 C5 C4 177.8(4) . . . . ? C1 N1 C5 C4 -1.9(7) . . . . ? C11 P1 C10 P2 -168.3(3) . . . 2_666 ? C21 P1 C10 P2 -60.9(3) . . . 2_666 ? Ag P1 C10 P2 78.1(3) . . . 2_666 ? C21 P1 C11 C12 -129.8(4) . . . . ? C10 P1 C11 C12 -22.7(4) . . . . ? Ag P1 C11 C12 92.3(4) . . . . ? C21 P1 C11 C16 56.4(4) . . . . ? C10 P1 C11 C16 163.5(4) . . . . ? Ag P1 C11 C16 -81.4(4) . . . . ? C16 C11 C12 C13 -1.3(7) . . . . ? P1 C11 C12 C13 -175.0(4) . . . . ? C11 C12 C13 C14 0.7(9) . . . . ? C12 C13 C14 C15 0.7(10) . . . . ? C13 C14 C15 C16 -1.4(9) . . . . ? C14 C15 C16 C11 0.7(8) . . . . ? C12 C11 C16 C15 0.6(7) . . . . ? P1 C11 C16 C15 174.7(4) . . . . ? C11 P1 C21 C22 -144.3(4) . . . . ? C10 P1 C21 C22 108.9(4) . . . . ? Ag P1 C21 C22 -19.0(4) . . . . ? C11 P1 C21 C26 38.3(5) . . . . ? C10 P1 C21 C26 -68.4(5) . . . . ? Ag P1 C21 C26 163.6(4) . . . . ? C26 C21 C22 C23 1.7(7) . . . . ? P1 C21 C22 C23 -175.7(4) . . . . ? C21 C22 C23 C24 -1.9(8) . . . . ? C22 C23 C24 C25 1.1(9) . . . . ? C23 C24 C25 C26 -0.2(10) . . . . ? C22 C21 C26 C25 -0.8(9) . . . . ? P1 C21 C26 C25 176.6(5) . . . . ? C24 C25 C26 C21 0.0(10) . . . . ? C10 P2 C31 C36 -29.9(5) 2_666 . . . ? C41 P2 C31 C36 76.0(5) . . . . ? Ag P2 C31 C36 -161.1(4) . . . . ? C10 P2 C31 C32 153.6(4) 2_666 . . . ? C41 P2 C31 C32 -100.5(4) . . . . ? Ag P2 C31 C32 22.5(4) . . . . ? C36 C31 C32 C33 -0.2(8) . . . . ? P2 C31 C32 C33 176.5(4) . . . . ? C31 C32 C33 C34 0.2(9) . . . . ? C32 C33 C34 C35 -0.1(11) . . . . ? C33 C34 C35 C36 0.0(11) . . . . ? C32 C31 C36 C35 0.2(9) . . . . ? P2 C31 C36 C35 -176.2(5) . . . . ? C34 C35 C36 C31 -0.1(10) . . . . ? C31 P2 C41 C42 13.5(4) . . . . ? C10 P2 C41 C42 122.9(4) 2_666 . . . ? Ag P2 C41 C42 -110.1(4) . . . . ? C31 P2 C41 C46 -171.0(4) . . . . ? C10 P2 C41 C46 -61.6(4) 2_666 . . . ? Ag P2 C41 C46 65.3(4) . . . . ? C46 C41 C42 C43 0.3(7) . . . . ? P2 C41 C42 C43 175.7(4) . . . . ? C41 C42 C43 C44 0.9(8) . . . . ? C42 C43 C44 C45 -1.8(8) . . . . ? C43 C44 C45 C46 1.5(9) . . . . ? C44 C45 C46 C41 -0.4(9) . . . . ? C42 C41 C46 C45 -0.6(8) . . . . ? P2 C41 C46 C45 -176.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 74.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.787 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.084 #======================================================================= data_97il04 #(Compound No. 5) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H11 Cl2 Hg N O S' _chemical_formula_weight 488.77 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'triclinic' _symmetry_space_group_name_H-M ' P 1 bar (No. 2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4265(5) _cell_length_b 11.1825(11) _cell_length_c 11.7128(9) _cell_angle_alpha 112.297(6) _cell_angle_beta 99.680(6) _cell_angle_gamma 105.797(6) _cell_volume 713.70(10) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.372 _cell_measurement_theta_max 18.159 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 11.289 _exptl_absorpt_correction_type 'Psi-scan' _exptl_absorpt_correction_T_min 0.528 _exptl_absorpt_correction_T_max 0.972 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'MACH3 Enraf Nonius ' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3149 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.28 _reflns_number_total 2880 _reflns_number_gt 2368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Enraf Nonius, 1994)' _computing_data_reduction 'GENHKL (Kretschmar, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1997)' _computing_publication_material 'SHELXL-97 (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 w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2880 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _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 Hg Hg 0.25550(4) 0.03140(2) 0.90934(2) 0.04737(9) Uani 1 d . . . Cl1 Cl 0.2896(2) 0.03526(14) 1.11088(13) 0.0499(3) Uani 1 d . . . Cl2 Cl 0.1740(3) 0.01455(17) 0.70465(15) 0.0631(4) Uani 1 d . . . S1 S 0.9284(2) 0.31173(14) 1.21214(13) 0.0484(3) Uani 1 d . . . O1 O 0.5754(6) 0.2722(4) 1.0255(4) 0.0567(10) Uani 1 d . . . N1 N 0.7582(7) 0.2956(4) 0.9876(4) 0.0393(9) Uani 1 d . . . C1 C 0.7492(11) 0.2949(6) 0.8715(6) 0.0525(14) Uani 1 d . . . C2 C 0.9390(12) 0.3204(7) 0.8333(6) 0.0578(15) Uani 1 d . . . C3 C 1.1451(10) 0.3490(6) 0.9158(6) 0.0502(13) Uani 1 d . . . C4 C 1.1551(9) 0.3497(5) 1.0339(6) 0.0439(12) Uani 1 d . . . C5 C 0.9609(8) 0.3225(4) 1.0706(5) 0.0366(10) Uani 1 d . . . C6 C 1.2235(12) 0.3640(6) 1.3060(6) 0.0549(15) Uani 1 d . . . C7 C 1.3538(9) 0.5189(5) 1.3673(5) 0.0440(12) Uani 1 d . . . C8 C 1.5588(11) 0.5711(7) 1.3473(6) 0.0561(15) Uani 1 d . . . C9 C 1.6806(12) 0.7144(7) 1.4081(6) 0.0647(17) Uani 1 d . . . C10 C 1.5989(13) 0.8023(7) 1.4855(7) 0.0688(19) Uani 1 d . . . C11 C 1.3987(14) 0.7531(7) 1.5074(7) 0.0680(18) Uani 1 d . . . C12 C 1.2750(11) 0.6099(6) 1.4472(6) 0.0537(14) Uani 1 d . . . H1 H 0.606(10) 0.265(6) 0.826(6) 0.049(16) Uiso 1 d . . . H2 H 0.939(11) 0.325(6) 0.751(6) 0.064(18) Uiso 1 d . . . H3 H 1.287(11) 0.358(7) 0.886(7) 0.07(2) Uiso 1 d . . . H4 H 1.270(8) 0.358(5) 1.082(5) 0.023(12) Uiso 1 d . . . H8 H 1.625(14) 0.499(9) 1.283(8) 0.12(3) Uiso 1 d . . . H9 H 1.860(18) 0.745(11) 1.407(10) 0.15(4) Uiso 1 d . . . H10 H 1.704(11) 0.891(7) 1.518(7) 0.068(19) Uiso 1 d . . . H11 H 1.340(11) 0.821(7) 1.559(6) 0.069(19) Uiso 1 d . . . H12 H 1.145(13) 0.589(8) 1.450(8) 0.09(3) Uiso 1 d . . . H61 H 1.301(10) 0.314(6) 1.247(6) 0.054(17) Uiso 1 d . . . H62 H 1.231(12) 0.331(7) 1.370(7) 0.08(2) 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 0.04320(13) 0.04892(13) 0.04647(13) 0.01815(9) 0.01167(9) 0.01777(9) Cl1 0.0492(7) 0.0504(7) 0.0478(7) 0.0187(6) 0.0137(6) 0.0203(6) Cl2 0.0687(10) 0.0662(9) 0.0484(8) 0.0232(7) 0.0112(7) 0.0239(8) S1 0.0520(8) 0.0440(7) 0.0429(7) 0.0182(6) 0.0132(6) 0.0110(6) O1 0.0293(19) 0.061(2) 0.062(3) 0.015(2) 0.0109(18) 0.0103(17) N1 0.030(2) 0.036(2) 0.044(2) 0.0129(18) 0.0042(18) 0.0130(17) C1 0.046(3) 0.055(3) 0.053(4) 0.024(3) 0.000(3) 0.022(3) C2 0.071(4) 0.065(4) 0.049(4) 0.032(3) 0.020(3) 0.032(3) C3 0.046(3) 0.059(3) 0.050(3) 0.026(3) 0.020(3) 0.020(3) C4 0.032(3) 0.048(3) 0.047(3) 0.017(2) 0.008(2) 0.017(2) C5 0.035(2) 0.030(2) 0.038(3) 0.0105(19) 0.007(2) 0.0117(19) C6 0.072(4) 0.048(3) 0.041(3) 0.019(3) 0.003(3) 0.027(3) C7 0.049(3) 0.051(3) 0.027(2) 0.015(2) 0.000(2) 0.022(2) C8 0.056(3) 0.073(4) 0.039(3) 0.023(3) 0.011(3) 0.029(3) C9 0.056(4) 0.071(4) 0.050(4) 0.025(3) 0.005(3) 0.008(3) C10 0.079(5) 0.048(3) 0.057(4) 0.020(3) -0.004(4) 0.010(3) C11 0.081(5) 0.060(4) 0.052(4) 0.014(3) 0.010(4) 0.033(4) C12 0.050(4) 0.055(4) 0.047(3) 0.015(3) 0.013(3) 0.019(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 Hg Cl2 2.2889(16) . y? Hg Cl1 2.3164(14) . y? Hg O1 2.568(4) . y? Hg Cl1 3.2317(14) 2_657 y? Hg S1 3.3116(14) 2_657 y? Hg Hg 3.8688(5) 2_657 y? Cl1 Cl1 4.081(3) 2_657 y? S1 C5 1.750(5) . ? S1 C6 1.831(7) . ? S1 O1 2.679(4) . ? O1 N1 1.320(5) . ? N1 C1 1.348(8) . ? N1 C5 1.368(6) . ? C1 C2 1.363(9) . ? C1 H1 0.88(6) . ? C2 C3 1.376(9) . ? C2 H2 0.99(6) . ? C3 C4 1.371(8) . ? C3 H3 1.02(7) . ? C4 C5 1.381(7) . ? C4 H4 0.81(5) . ? C6 C7 1.510(8) . ? C6 H61 1.00(6) . ? C6 H62 0.95(7) . ? C7 C12 1.373(8) . ? C7 C8 1.386(9) . ? C8 C9 1.397(10) . ? C8 H8 1.11(9) . ? C9 C10 1.352(10) . ? C9 H9 1.12(11) . ? C10 C11 1.362(11) . ? C10 H10 0.92(7) . ? C11 C12 1.398(9) . ? C11 H11 0.99(7) . ? C12 H12 0.81(8) . ? 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 Cl2 Hg Cl1 172.84(5) . . y? Cl2 Hg O1 98.43(11) . . y? Cl1 Hg O1 87.17(11) . . y? Cl2 Hg Cl1 92.46(5) . 2_657 y? Cl1 Hg Cl1 93.22(4) . 2_657 y? O1 Hg Cl1 76.09(9) . 2_657 y? Cl2 Hg S1 90.36(5) . 2_657 y? Cl1 Hg S1 86.71(4) . 2_657 y? O1 Hg S1 151.70(9) . 2_657 y? Cl1 Hg S1 76.71(4) 2_657 2_657 y? Cl2 Hg Hg 129.04(4) . 2_657 ? Cl1 Hg Hg 56.51(4) . 2_657 ? O1 Hg Hg 76.68(10) . 2_657 ? Cl1 Hg Hg 36.71(2) 2_657 2_657 ? S1 Hg Hg 76.91(3) 2_657 2_657 ? Hg Cl1 Cl1 52.25(3) . 2_657 ? C5 S1 C6 101.6(3) . . ? C5 S1 O1 58.28(19) . . ? C6 S1 O1 159.3(2) . . ? N1 O1 Hg 120.3(3) . . ? N1 O1 S1 71.8(3) . . ? Hg O1 S1 117.57(17) . . ? O1 N1 C1 121.8(4) . . ? O1 N1 C5 118.0(4) . . ? C1 N1 C5 120.2(5) . . ? N1 C1 C2 121.5(5) . . ? N1 C1 H1 109(4) . . ? C2 C1 H1 129(4) . . ? C1 C2 C3 119.3(6) . . ? C1 C2 H2 123(4) . . ? C3 C2 H2 117(4) . . ? C4 C3 C2 119.4(5) . . ? C4 C3 H3 119(4) . . ? C2 C3 H3 121(4) . . ? C3 C4 C5 120.6(5) . . ? C3 C4 H4 122(3) . . ? C5 C4 H4 117(3) . . ? N1 C5 C4 119.0(5) . . ? N1 C5 S1 111.8(4) . . ? C4 C5 S1 129.1(4) . . ? C7 C6 S1 113.4(4) . . ? C7 C6 H61 110(4) . . ? S1 C6 H61 108(3) . . ? C7 C6 H62 110(4) . . ? S1 C6 H62 111(4) . . ? H61 C6 H62 104(5) . . ? C12 C7 C8 118.9(6) . . ? C12 C7 C6 120.6(6) . . ? C8 C7 C6 120.4(5) . . ? C7 C8 C9 119.7(6) . . ? C7 C8 H8 120(5) . . ? C9 C8 H8 120(5) . . ? C10 C9 C8 120.4(7) . . ? C10 C9 H9 124(6) . . ? C8 C9 H9 114(5) . . ? C9 C10 C11 120.9(7) . . ? C9 C10 H10 107(4) . . ? C11 C10 H10 132(4) . . ? C10 C11 C12 119.4(7) . . ? C10 C11 H11 118(4) . . ? C12 C11 H11 122(4) . . ? C7 C12 C11 120.7(7) . . ? C7 C12 H12 124(6) . . ? C11 C12 H12 114(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Hg Cl1 Cl1 142.4(4) . . . 2_657 ? O1 Hg Cl1 Cl1 -75.88(9) . . . 2_657 ? S1 Hg Cl1 Cl1 76.47(4) 2_657 . . 2_657 ? Hg Hg Cl1 Cl1 0.0 2_657 . . 2_657 ? Cl2 Hg O1 N1 -58.1(4) . . . . ? Cl1 Hg O1 N1 126.4(4) . . . . ? Cl1 Hg O1 N1 32.3(3) 2_657 . . . ? S1 Hg O1 N1 48.7(5) 2_657 . . . ? Hg Hg O1 N1 70.1(3) 2_657 . . . ? Cl2 Hg O1 S1 -142.28(15) . . . . ? Cl1 Hg O1 S1 42.21(15) . . . . ? Cl1 Hg O1 S1 -51.82(14) 2_657 . . . ? S1 Hg O1 S1 -35.5(3) 2_657 . . . ? Hg Hg O1 S1 -14.01(13) 2_657 . . . ? C5 S1 O1 N1 1.4(3) . . . . ? C6 S1 O1 N1 16.2(7) . . . . ? C5 S1 O1 Hg 116.8(2) . . . . ? C6 S1 O1 Hg 131.5(6) . . . . ? Hg O1 N1 C1 67.1(5) . . . . ? S1 O1 N1 C1 178.9(5) . . . . ? Hg O1 N1 C5 -113.6(4) . . . . ? S1 O1 N1 C5 -1.7(3) . . . . ? O1 N1 C1 C2 179.4(5) . . . . ? C5 N1 C1 C2 0.1(8) . . . . ? N1 C1 C2 C3 -0.7(9) . . . . ? C1 C2 C3 C4 0.8(9) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? O1 N1 C5 C4 -178.9(4) . . . . ? C1 N1 C5 C4 0.5(7) . . . . ? O1 N1 C5 S1 2.7(5) . . . . ? C1 N1 C5 S1 -177.9(4) . . . . ? C3 C4 C5 N1 -0.4(7) . . . . ? C3 C4 C5 S1 177.7(4) . . . . ? C6 S1 C5 N1 -176.1(3) . . . . ? O1 S1 C5 N1 -1.4(3) . . . . ? C6 S1 C5 C4 5.7(5) . . . . ? O1 S1 C5 C4 -179.6(5) . . . . ? C5 S1 C6 C7 76.8(5) . . . . ? O1 S1 C6 C7 64.1(9) . . . . ? S1 C6 C7 C12 55.5(7) . . . . ? S1 C6 C7 C8 -126.7(5) . . . . ? C12 C7 C8 C9 -0.1(9) . . . . ? C6 C7 C8 C9 -178.0(5) . . . . ? C7 C8 C9 C10 -0.5(10) . . . . ? C8 C9 C10 C11 1.0(11) . . . . ? C9 C10 C11 C12 -1.0(11) . . . . ? C8 C7 C12 C11 0.2(9) . . . . ? C6 C7 C12 C11 178.0(6) . . . . ? C10 C11 C12 C7 0.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.467 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.142 #======================================================================= data_98il04 #(Compound No. 11) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H9 Hg N S' _chemical_formula_weight 387.84 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' '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 'monoclinic' _symmetry_space_group_name_H-M 'C2/c (No. 15)' 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 30.135(3) _cell_length_b 6.7304(11) _cell_length_c 23.061(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.371(9) _cell_angle_gamma 90.00 _cell_volume 4355.7(10) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25? _cell_measurement_theta_min 9.318 _cell_measurement_theta_max 20.811 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 14.283 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.985 _exptl_special_details ; ? ; _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_type 'MACH3 Enraf Nonius ' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5367 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.1632 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.98 _reflns_number_total 5234 _reflns_number_gt 2319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Nonius, 1994)' _computing_data_reduction 'GENHKL (Kretschmar, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1997)' _computing_publication_material 'SHELXL-97 (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 w=1/[\s^2^(Fo^2^)+(0.0288P)^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 5234 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1953 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.000 _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 Hg1 Hg 0.100173(16) 0.78066(7) 0.188457(19) 0.04972(15) Uani 1 d . . . S1 S 0.07601(11) 0.7717(5) 0.27564(13) 0.0513(8) Uani 1 d . . . N1 N 0.1683(4) 0.7157(13) 0.3073(4) 0.051(2) Uani 1 d . . . C11 C 0.1151(4) 0.7888(18) 0.1081(4) 0.045(3) Uani 1 d . . . C12 C 0.1123(4) 0.616(2) 0.0727(6) 0.058(4) Uani 1 d . . . H12 H 0.1053 0.4956 0.0872 0.070 Uiso 1 calc R . . C13 C 0.1197(4) 0.619(2) 0.0180(6) 0.068(4) Uani 1 d . . . H13 H 0.1169 0.5018 -0.0045 0.082 Uiso 1 calc R . . C14 C 0.1310(5) 0.791(3) -0.0046(5) 0.083(5) Uani 1 d . . . H14 H 0.1362 0.7930 -0.0420 0.099 Uiso 1 calc R . . C15 C 0.1344(5) 0.962(2) 0.0303(7) 0.080(5) Uani 1 d . . . H15 H 0.1427 1.0805 0.0163 0.096 Uiso 1 calc R . . C16 C 0.1259(5) 0.9598(18) 0.0848(6) 0.061(4) Uani 1 d . . . H16 H 0.1275 1.0782 0.1063 0.073 Uiso 1 calc R . . C17 C 0.1340(4) 0.7247(15) 0.3296(5) 0.046(3) Uani 1 d . . . C18 C 0.1412(5) 0.6954(16) 0.3916(5) 0.056(3) Uani 1 d . . . H18 H 0.1158 0.7015 0.4054 0.068 Uiso 1 calc R . . C19 C 0.1866(5) 0.657(2) 0.4324(6) 0.074(4) Uani 1 d . . . H19 H 0.1923 0.6406 0.4745 0.089 Uiso 1 calc R . . C110 C 0.2231(5) 0.6423(19) 0.4116(6) 0.068(4) Uani 1 d . . . H110 H 0.2540 0.6123 0.4382 0.082 Uiso 1 calc R . . C111 C 0.2117(5) 0.6757(18) 0.3467(7) 0.064(4) Uani 1 d . . . H111 H 0.2362 0.6688 0.3313 0.076 Uiso 1 calc R . . Hg2 Hg 0.068634(14) 1.26131(7) 0.283042(18) 0.04348(14) Uani 1 d . . . S2 S 0.11143(10) 1.2733(5) 0.21439(13) 0.0476(7) Uani 1 d . . . N2 N 0.1702(3) 1.2015(12) 0.3306(4) 0.044(2) Uani 1 d . . . C21 C 0.0326(3) 1.2644(17) 0.3434(4) 0.042(3) Uani 1 d . . . C22 C 0.0238(4) 1.0860(18) 0.3681(5) 0.049(3) Uani 1 d . . . H22 H 0.0327 0.9665 0.3552 0.059 Uiso 1 calc R . . C23 C 0.0014(4) 1.0846(19) 0.4125(5) 0.055(4) Uani 1 d . . . H23 H -0.0049 0.9650 0.4282 0.066 Uiso 1 calc R . . C24 C -0.0109(4) 1.263(2) 0.4323(5) 0.050(3) Uani 1 d . . . H24 H -0.0249 1.2642 0.4621 0.060 Uiso 1 calc R . . C25 C -0.0025(4) 1.438(2) 0.4081(6) 0.062(4) Uani 1 d . . . H25 H -0.0108 1.5578 0.4215 0.074 Uiso 1 calc R . . C26 C 0.0188(4) 1.4362(17) 0.3631(5) 0.046(3) Uani 1 d . . . H26 H 0.0236 1.5561 0.3462 0.056 Uiso 1 calc R . . C27 C 0.1677(3) 1.2315(15) 0.2723(5) 0.040(2) Uani 1 d . . . C28 C 0.2072(4) 1.2294(19) 0.2555(6) 0.067(4) Uani 1 d . . . H28 H 0.2046 1.2494 0.2145 0.080 Uiso 1 calc R . . C29 C 0.2515(4) 1.196(2) 0.3033(7) 0.077(4) Uani 1 d . . . H29 H 0.2790 1.1909 0.2940 0.092 Uiso 1 calc R . . C210 C 0.2543(5) 1.171(2) 0.3620(8) 0.078(4) Uani 1 d . . . H210 H 0.2836 1.1552 0.3943 0.093 Uiso 1 calc R . . C211 C 0.2127(5) 1.1688(18) 0.3729(6) 0.067(4) Uani 1 d . . . H211 H 0.2146 1.1423 0.4133 0.080 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 Hg1 0.0564(3) 0.0601(3) 0.0398(2) -0.0037(3) 0.0261(2) -0.0010(3) S1 0.068(2) 0.0480(19) 0.0511(17) -0.0015(17) 0.0375(16) 0.0031(18) N1 0.065(7) 0.047(6) 0.056(6) -0.010(5) 0.041(5) -0.014(6) C11 0.043(6) 0.062(8) 0.035(6) 0.017(6) 0.021(5) 0.016(6) C12 0.047(8) 0.075(9) 0.056(9) -0.023(7) 0.023(7) -0.011(7) C13 0.045(8) 0.122(13) 0.039(8) -0.025(8) 0.015(7) 0.005(9) C14 0.061(9) 0.158(16) 0.033(7) 0.003(10) 0.022(6) 0.017(11) C15 0.075(11) 0.118(14) 0.061(10) 0.032(10) 0.043(9) 0.016(10) C16 0.077(11) 0.063(9) 0.049(8) 0.017(7) 0.031(8) 0.021(8) C17 0.068(7) 0.037(7) 0.041(6) -0.013(6) 0.030(6) -0.015(6) C18 0.083(10) 0.048(8) 0.053(7) -0.003(6) 0.042(7) -0.011(7) C19 0.074(11) 0.105(12) 0.047(8) -0.008(8) 0.027(8) -0.014(10) C110 0.073(10) 0.065(9) 0.070(10) -0.016(8) 0.029(8) -0.008(8) C111 0.060(9) 0.055(9) 0.090(10) -0.027(8) 0.045(9) -0.031(7) Hg2 0.0384(2) 0.0526(3) 0.0428(2) -0.0027(2) 0.01883(19) -0.0003(3) S2 0.0464(16) 0.0541(19) 0.0478(15) -0.0027(16) 0.0239(13) 0.0002(17) N2 0.041(5) 0.038(6) 0.051(6) -0.012(5) 0.013(5) -0.010(5) C21 0.038(6) 0.045(7) 0.045(6) -0.010(6) 0.017(5) -0.016(6) C22 0.045(9) 0.061(9) 0.044(8) -0.013(6) 0.019(7) 0.006(7) C23 0.048(9) 0.066(9) 0.050(9) 0.004(7) 0.016(7) -0.012(7) C24 0.042(6) 0.072(9) 0.044(6) 0.008(8) 0.025(5) 0.006(8) C25 0.067(11) 0.066(9) 0.074(11) -0.015(7) 0.050(9) -0.003(7) C26 0.041(8) 0.050(8) 0.048(8) -0.001(6) 0.017(7) 0.002(6) C27 0.039(5) 0.028(6) 0.052(6) 0.000(6) 0.014(5) 0.003(6) C28 0.050(7) 0.086(10) 0.072(8) -0.023(9) 0.032(7) -0.021(9) C29 0.037(7) 0.092(12) 0.106(12) -0.018(10) 0.031(8) -0.018(8) C210 0.039(8) 0.065(10) 0.110(13) -0.005(9) 0.003(9) 0.010(7) C211 0.068(10) 0.049(8) 0.070(9) 0.001(7) 0.010(8) 0.000(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 Hg1 C11 2.062(9) . y? Hg1 S1 2.376(3) . y? Hg1 N1 2.795(10) . y? Hg1 S2 3.365(3) . y? S1 C17 1.766(12) . ? S1 Hg2 3.312(3) . y? N1 C17 1.313(12) . ? N1 C111 1.319(15) . ? C11 C16 1.359(14) . ? C11 C12 1.406(15) . ? C12 C13 1.358(15) . ? C12 H12 0.9300 . ? C13 C14 1.360(19) . ? C13 H13 0.9300 . ? C14 C15 1.386(18) . ? C14 H14 0.9300 . ? C15 C16 1.373(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.380(13) . ? C18 C19 1.373(17) . ? C18 H18 0.9300 . ? C19 C110 1.356(16) . ? C19 H19 0.9300 . ? C110 C111 1.425(16) . ? C110 H110 0.9300 . ? C111 H111 0.9300 . ? Hg2 C21 2.054(9) . y? Hg2 S2 2.380(3) . y? Hg2 N2 2.879(9) . y? S2 C27 1.757(10) . ? N2 C211 1.315(14) . ? N2 C27 1.335(12) . ? C21 C26 1.361(13) . ? C21 C22 1.395(14) . ? C22 C23 1.416(13) . ? C22 H22 0.9300 . ? C23 C24 1.384(15) . ? C23 H23 0.9300 . ? C24 C25 1.363(15) . ? C24 H24 0.9300 . ? C25 C26 1.406(13) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.378(13) . ? C28 C29 1.406(17) . ? C28 H28 0.9300 . ? C29 C210 1.335(17) . ? C29 H29 0.9300 . ? C210 C211 1.365(16) . ? C210 H210 0.9300 . ? C211 H211 0.9300 . ? 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 C11 Hg1 S1 175.2(3) . . y? C11 Hg1 N1 124.2(3) . . y? S1 Hg1 N1 60.57(18) . . y? C11 Hg1 S2 95.3(3) . . y? S1 Hg1 S2 85.23(9) . . y? N1 Hg1 S2 89.39(19) . . y? C17 S1 Hg1 94.1(3) . . ? C17 S1 Hg2 102.1(4) . . ? Hg1 S1 Hg2 93.74(9) . . y? C17 N1 C111 117.5(10) . . ? C17 N1 Hg1 88.6(7) . . ? C111 N1 Hg1 153.8(8) . . ? C16 C11 C12 116.4(10) . . ? C16 C11 Hg1 122.7(9) . . ? C12 C11 Hg1 120.9(9) . . ? C13 C12 C11 122.1(13) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 121.2(13) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 117.3(11) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? C16 C15 C14 121.7(14) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C11 C16 C15 121.4(13) . . ? C11 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? N1 C17 C18 123.5(11) . . ? N1 C17 S1 116.8(8) . . ? C18 C17 S1 119.8(9) . . ? C19 C18 C17 118.5(11) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C110 C19 C18 120.5(12) . . ? C110 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C110 C111 116.2(13) . . ? C19 C110 H110 121.9 . . ? C111 C110 H110 121.9 . . ? N1 C111 C110 123.8(11) . . ? N1 C111 H111 118.1 . . ? C110 C111 H111 118.1 . . ? C21 Hg2 S2 177.3(3) . . y? C21 Hg2 N2 119.6(3) . . y? S2 Hg2 N2 59.97(19) . . y? C21 Hg2 S1 96.1(3) . . y? S2 Hg2 S1 86.38(9) . . y? N2 Hg2 S1 78.38(17) . . y? C27 S2 Hg2 95.5(3) . . ? C27 S2 Hg1 89.1(3) . . ? Hg2 S2 Hg1 92.34(9) . . y? C211 N2 C27 117.1(10) . . ? C211 N2 Hg2 156.8(8) . . ? C27 N2 Hg2 86.1(6) . . ? C26 C21 C22 117.9(9) . . ? C26 C21 Hg2 122.4(8) . . ? C22 C21 Hg2 119.6(8) . . ? C21 C22 C23 120.8(10) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.2(11) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 120.2(9) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.8(11) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 122.0(11) . . ? C21 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? N2 C27 C28 122.9(10) . . ? N2 C27 S2 118.3(8) . . ? C28 C27 S2 118.8(9) . . ? C27 C28 C29 116.8(12) . . ? C27 C28 H28 121.6 . . ? C29 C28 H28 121.6 . . ? C210 C29 C28 120.5(12) . . ? C210 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C210 C211 117.7(13) . . ? C29 C210 H210 121.1 . . ? C211 C210 H210 121.1 . . ? N2 C211 C210 124.9(13) . . ? N2 C211 H211 117.6 . . ? C210 C211 H211 117.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Hg1 S1 C17 171(4) . . . . ? N1 Hg1 S1 C17 -0.7(4) . . . . ? S2 Hg1 S1 C17 -92.7(4) . . . . ? C11 Hg1 S1 Hg2 -87(4) . . . . ? N1 Hg1 S1 Hg2 101.7(2) . . . . ? S2 Hg1 S1 Hg2 9.70(7) . . . . ? C11 Hg1 N1 C17 -178.1(7) . . . . ? S1 Hg1 N1 C17 1.0(5) . . . . ? S2 Hg1 N1 C17 85.8(6) . . . . ? C11 Hg1 N1 C111 -4(2) . . . . ? S1 Hg1 N1 C111 175.0(19) . . . . ? S2 Hg1 N1 C111 -100.2(18) . . . . ? S1 Hg1 C11 C16 98(4) . . . . ? N1 Hg1 C11 C16 -91.7(10) . . . . ? S2 Hg1 C11 C16 1.2(10) . . . . ? S1 Hg1 C11 C12 -79(4) . . . . ? N1 Hg1 C11 C12 91.5(9) . . . . ? S2 Hg1 C11 C12 -175.6(9) . . . . ? C16 C11 C12 C13 -0.4(17) . . . . ? Hg1 C11 C12 C13 176.6(9) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C12 C11 C16 C15 -1.2(18) . . . . ? Hg1 C11 C16 C15 -178.2(10) . . . . ? C14 C15 C16 C11 2(2) . . . . ? C111 N1 C17 C18 0.3(16) . . . . ? Hg1 N1 C17 C18 177.3(10) . . . . ? C111 N1 C17 S1 -178.3(9) . . . . ? Hg1 N1 C17 S1 -1.3(7) . . . . ? Hg1 S1 C17 N1 1.5(8) . . . . ? Hg2 S1 C17 N1 -93.2(8) . . . . ? Hg1 S1 C17 C18 -177.1(8) . . . . ? Hg2 S1 C17 C18 88.2(9) . . . . ? N1 C17 C18 C19 0.8(17) . . . . ? S1 C17 C18 C19 179.3(10) . . . . ? C17 C18 C19 C110 -2(2) . . . . ? C18 C19 C110 C111 2(2) . . . . ? C17 N1 C111 C110 -0.1(18) . . . . ? Hg1 N1 C111 C110 -173.4(11) . . . . ? C19 C110 C111 N1 -1.0(19) . . . . ? C17 S1 Hg2 C21 -97.9(4) . . . . ? Hg1 S1 Hg2 C21 167.1(3) . . . . ? C17 S1 Hg2 S2 81.2(3) . . . . ? Hg1 S1 Hg2 S2 -13.77(10) . . . . ? C17 S1 Hg2 N2 21.1(4) . . . . ? Hg1 S1 Hg2 N2 -73.84(19) . . . . ? C21 Hg2 S2 C27 81(6) . . . . ? N2 Hg2 S2 C27 -1.0(4) . . . . ? S1 Hg2 S2 C27 -79.6(3) . . . . ? C21 Hg2 S2 Hg1 170(6) . . . . ? N2 Hg2 S2 Hg1 88.3(2) . . . . ? S1 Hg2 S2 Hg1 9.66(7) . . . . ? C11 Hg1 S2 C27 -102.9(4) . . . . ? S1 Hg1 S2 C27 81.9(3) . . . . ? N1 Hg1 S2 C27 21.4(4) . . . . ? C11 Hg1 S2 Hg2 161.6(3) . . . . ? S1 Hg1 S2 Hg2 -13.55(10) . . . . ? N1 Hg1 S2 Hg2 -74.06(18) . . . . ? C21 Hg2 N2 C211 2(2) . . . . ? S2 Hg2 N2 C211 179(2) . . . . ? S1 Hg2 N2 C211 -88.7(19) . . . . ? C21 Hg2 N2 C27 -175.7(6) . . . . ? S2 Hg2 N2 C27 1.3(5) . . . . ? S1 Hg2 N2 C27 93.8(6) . . . . ? S2 Hg2 C21 C26 21(7) . . . . ? N2 Hg2 C21 C26 100.9(9) . . . . ? S1 Hg2 C21 C26 -179.0(9) . . . . ? S2 Hg2 C21 C22 -156(6) . . . . ? N2 Hg2 C21 C22 -75.8(9) . . . . ? S1 Hg2 C21 C22 4.3(9) . . . . ? C26 C21 C22 C23 -0.5(16) . . . . ? Hg2 C21 C22 C23 176.4(8) . . . . ? C21 C22 C23 C24 -1.2(18) . . . . ? C22 C23 C24 C25 1.4(17) . . . . ? C23 C24 C25 C26 0.0(18) . . . . ? C22 C21 C26 C25 1.9(17) . . . . ? Hg2 C21 C26 C25 -174.9(9) . . . . ? C24 C25 C26 C21 -2(2) . . . . ? C211 N2 C27 C28 -0.1(16) . . . . ? Hg2 N2 C27 C28 178.8(10) . . . . ? C211 N2 C27 S2 179.4(8) . . . . ? Hg2 N2 C27 S2 -1.7(7) . . . . ? Hg2 S2 C27 N2 2.1(8) . . . . ? Hg1 S2 C27 N2 -90.2(8) . . . . ? Hg2 S2 C27 C28 -178.4(9) . . . . ? Hg1 S2 C27 C28 89.3(9) . . . . ? N2 C27 C28 C29 -0.6(18) . . . . ? S2 C27 C28 C29 179.9(10) . . . . ? C27 C28 C29 C210 -1(2) . . . . ? C28 C29 C210 C211 3(2) . . . . ? C27 N2 C211 C210 2.6(18) . . . . ? Hg2 N2 C211 C210 -174.6(13) . . . . ? C29 C210 C211 N2 -4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.460 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.460 _refine_diff_density_max 0.920 _refine_diff_density_min -2.138 _refine_diff_density_rms 0.234 #=======================================================================