# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Liang, Fupei' _publ_contact_author_email fliangoffice@yahoo.com _publ_section_title ; Structure and fluorescent properties of mercury(II) pyridine-2,3-dicarboxylate coordination polymers tuned by ancillary ligands and alkaline-earth metal ions ; loop_ _publ_author_name Z.Chen X.Wu S.Qin C.Lei F.Liang data_090119a _database_code_depnum_ccdc_archive 'CCDC 792170' #TrackingRef 'compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Hg2 N2 O8' _chemical_formula_sum 'C14 H6 Hg2 N2 O8' _chemical_formula_weight 731.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6509(11) _cell_length_b 8.9059(10) _cell_length_c 14.7490(15) _cell_angle_alpha 90.00 _cell_angle_beta 109.7900(10) _cell_angle_gamma 90.00 _cell_volume 1440.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3766 _cell_measurement_theta_min 2.718 _cell_measurement_theta_max 28.02 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 21.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2023 _exptl_absorpt_correction_T_max 0.4149 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method '\p and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 7353 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2543 _reflns_number_gt 2142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART ' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _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^)+(0.0316P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2543 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.32593(3) 0.31488(3) 0.28328(2) 0.03049(11) Uani 1 1 d . . . Hg2 Hg 0.59389(3) 0.00716(3) 0.33052(2) 0.02782(10) Uani 1 1 d . . . N1 N 0.3529(5) 0.3560(6) 0.4383(4) 0.0236(13) Uani 1 1 d . . . N2 N 0.7248(5) 0.3945(6) 0.0813(4) 0.0253(14) Uani 1 1 d . . . O1 O 0.4887(5) 0.1524(6) 0.3878(4) 0.0378(14) Uani 1 1 d . . . O2 O 0.6336(5) 0.1595(7) 0.5289(4) 0.0589(19) Uani 1 1 d . . . O3 O 0.6821(4) 0.3708(6) 0.7073(4) 0.0358(13) Uani 1 1 d . . . O4 O 0.5934(5) 0.1595(6) 0.7165(4) 0.0378(14) Uani 1 1 d . . . O5 O 0.6920(5) 0.2527(6) 0.2954(4) 0.0360(13) Uani 1 1 d . . . O6 O 0.8424(5) 0.3828(7) 0.2756(4) 0.0456(16) Uani 1 1 d . . . O7 O 0.4282(4) 0.3749(6) 0.1904(4) 0.0319(12) Uani 1 1 d . . . O8 O 0.4459(5) 0.1258(6) 0.1755(4) 0.0330(12) Uani 1 1 d . . . C1 C 0.5347(7) 0.1963(8) 0.4733(5) 0.0235(16) Uani 1 1 d . . . C2 C 0.5932(6) 0.2853(8) 0.6801(5) 0.0244(16) Uani 1 1 d . . . C3 C 0.4532(6) 0.3006(7) 0.5066(5) 0.0229(16) Uani 1 1 d . . . C4 C 0.4786(6) 0.3407(8) 0.6025(5) 0.0246(16) Uani 1 1 d . . . C5 C 0.3981(6) 0.4318(9) 0.6279(6) 0.0314(18) Uani 1 1 d . . . H5 H 0.4141 0.4595 0.6918 0.038 Uiso 1 1 calc R . . C6 C 0.2932(7) 0.4811(8) 0.5567(6) 0.0350(19) Uani 1 1 d . . . H6 H 0.2357 0.5378 0.5726 0.042 Uiso 1 1 calc R . . C7 C 0.2752(6) 0.4450(8) 0.4621(5) 0.0273(17) Uani 1 1 d . . . H7 H 0.2076 0.4833 0.4138 0.033 Uiso 1 1 calc R . . C8 C 0.7370(7) 0.3234(8) 0.2447(6) 0.0289(17) Uani 1 1 d . . . C9 C 0.4685(6) 0.2573(9) 0.1605(5) 0.0262(17) Uani 1 1 d . . . C10 C 0.6652(6) 0.3399(8) 0.1382(5) 0.0248(16) Uani 1 1 d . . . C11 C 0.5444(6) 0.2928(8) 0.0981(5) 0.0257(17) Uani 1 1 d . . . C12 C 0.4905(7) 0.2884(9) -0.0013(6) 0.035(2) Uani 1 1 d . . . H12 H 0.4113 0.2526 -0.0292 0.042 Uiso 1 1 calc R . . C13 C 0.5552(7) 0.3376(8) -0.0581(5) 0.0341(19) Uani 1 1 d . . . H13 H 0.5216 0.3324 -0.1249 0.041 Uiso 1 1 calc R . . C14 C 0.6715(7) 0.3951(8) -0.0141(5) 0.0274(17) Uani 1 1 d . . . H14 H 0.7133 0.4351 -0.0522 0.033 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 0.02160(17) 0.0438(2) 0.02454(17) -0.00058(13) 0.00587(12) -0.00290(14) Hg2 0.02444(17) 0.02884(17) 0.03131(18) -0.00155(12) 0.01090(13) 0.00400(12) N1 0.026(3) 0.024(3) 0.021(3) 0.001(3) 0.007(2) -0.002(3) N2 0.028(3) 0.022(3) 0.027(3) -0.001(3) 0.010(3) -0.005(3) O1 0.036(3) 0.049(4) 0.026(3) -0.012(3) 0.007(2) 0.012(3) O2 0.048(4) 0.088(5) 0.031(3) -0.008(3) 0.000(3) 0.045(4) O3 0.018(3) 0.043(3) 0.041(3) 0.010(3) 0.002(2) -0.004(3) O4 0.032(3) 0.032(3) 0.036(3) 0.010(2) -0.006(2) -0.005(3) O5 0.036(3) 0.037(3) 0.034(3) 0.004(3) 0.010(2) -0.012(3) O6 0.028(3) 0.065(4) 0.038(3) 0.008(3) 0.004(3) -0.018(3) O7 0.029(3) 0.039(3) 0.033(3) 0.006(2) 0.018(2) 0.000(3) O8 0.033(3) 0.032(3) 0.034(3) -0.001(2) 0.011(2) -0.011(3) C1 0.028(4) 0.024(4) 0.023(4) 0.004(3) 0.014(3) 0.000(3) C2 0.021(4) 0.036(4) 0.019(4) -0.003(3) 0.009(3) 0.005(3) C3 0.019(4) 0.019(4) 0.033(4) 0.003(3) 0.011(3) -0.002(3) C4 0.020(4) 0.031(4) 0.024(4) 0.002(3) 0.009(3) -0.005(3) C5 0.027(4) 0.037(4) 0.028(4) -0.010(4) 0.007(3) -0.002(4) C6 0.032(4) 0.033(5) 0.040(5) 0.003(4) 0.013(4) 0.008(4) C7 0.021(4) 0.030(4) 0.029(4) 0.003(3) 0.005(3) 0.006(3) C8 0.028(4) 0.023(4) 0.034(4) 0.001(3) 0.008(3) -0.006(3) C9 0.017(4) 0.036(4) 0.021(4) 0.000(3) 0.000(3) -0.002(3) C10 0.025(4) 0.025(4) 0.029(4) 0.004(3) 0.015(3) -0.001(3) C11 0.028(4) 0.025(4) 0.025(4) -0.005(3) 0.010(3) -0.002(3) C12 0.022(4) 0.037(5) 0.040(5) -0.002(4) 0.002(4) -0.006(3) C13 0.038(5) 0.042(5) 0.021(4) 0.000(3) 0.008(3) -0.002(4) C14 0.034(4) 0.024(4) 0.029(4) 0.005(3) 0.017(3) 0.002(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 Hg1 O7 2.164(5) . ? Hg1 N1 2.231(6) . ? Hg1 O3 2.351(5) 4_565 ? Hg1 O1 2.467(5) . ? Hg1 O4 2.560(5) 4_565 ? Hg1 O3 2.806(6) 3_666 ? Hg2 O1 2.143(5) . ? Hg2 O6 2.240(5) 2_645 ? Hg2 N2 2.302(5) 2_645 ? Hg2 O4 2.534(5) 3_656 ? Hg2 O8 2.578(5) . ? Hg2 O5 2.600(5) . ? N1 C7 1.337(9) . ? N1 C3 1.351(8) . ? N2 C14 1.331(9) . ? N2 C10 1.348(9) . ? N2 Hg2 2.302(5) 2_655 ? O1 C1 1.254(8) . ? O2 C1 1.212(8) . ? O3 C2 1.238(8) . ? O3 Hg1 2.351(5) 4_666 ? O3 Hg1 2.806(6) 3_666 ? O4 C2 1.242(9) . ? O4 Hg2 2.534(5) 3_656 ? O4 Hg1 2.560(5) 4_666 ? O5 C8 1.222(9) . ? O6 C8 1.271(9) . ? O6 Hg2 2.240(5) 2_655 ? O7 C9 1.286(9) . ? O8 C9 1.237(9) . ? C1 C3 1.524(10) . ? C2 C4 1.516(9) . ? C3 C4 1.390(10) . ? C4 C5 1.384(10) . ? C5 C6 1.385(10) . ? C5 H5 0.9300 . ? C6 C7 1.376(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.517(10) . ? C9 C11 1.509(10) . ? C10 C11 1.394(10) . ? C11 C12 1.387(10) . ? C12 C13 1.376(11) . ? C12 H12 0.9300 . ? C13 C14 1.387(10) . ? C13 H13 0.9300 . ? C14 H14 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 O7 Hg1 N1 133.7(2) . . ? O7 Hg1 O3 109.17(19) . 4_565 ? N1 Hg1 O3 115.7(2) . 4_565 ? O7 Hg1 O1 93.95(18) . . ? N1 Hg1 O1 69.14(19) . . ? O3 Hg1 O1 99.11(18) 4_565 . ? O7 Hg1 O4 118.17(18) . 4_565 ? N1 Hg1 O4 98.2(2) . 4_565 ? O3 Hg1 O4 52.31(16) 4_565 4_565 ? O1 Hg1 O4 141.43(18) . 4_565 ? O7 Hg1 O3 79.61(18) . 3_666 ? N1 Hg1 O3 77.36(18) . 3_666 ? O3 Hg1 O3 134.03(9) 4_565 3_666 ? O1 Hg1 O3 125.85(16) . 3_666 ? O4 Hg1 O3 83.20(15) 4_565 3_666 ? O1 Hg2 O6 160.65(19) . 2_645 ? O1 Hg2 N2 125.32(19) . 2_645 ? O6 Hg2 N2 73.84(19) 2_645 2_645 ? O1 Hg2 O4 84.7(2) . 3_656 ? O6 Hg2 O4 88.7(2) 2_645 3_656 ? N2 Hg2 O4 116.07(18) 2_645 3_656 ? O1 Hg2 O8 78.59(18) . . ? O6 Hg2 O8 82.14(17) 2_645 . ? N2 Hg2 O8 152.87(19) 2_645 . ? O4 Hg2 O8 75.04(16) 3_656 . ? O1 Hg2 O5 85.4(2) . . ? O6 Hg2 O5 90.3(2) 2_645 . ? N2 Hg2 O5 95.64(19) 2_645 . ? O4 Hg2 O5 146.53(16) 3_656 . ? O8 Hg2 O5 71.69(15) . . ? C7 N1 C3 120.8(6) . . ? C7 N1 Hg1 119.6(5) . . ? C3 N1 Hg1 119.4(5) . . ? C14 N2 C10 120.3(6) . . ? C14 N2 Hg2 127.3(5) . 2_655 ? C10 N2 Hg2 111.9(4) . 2_655 ? C1 O1 Hg2 118.6(5) . . ? C1 O1 Hg1 114.9(4) . . ? Hg2 O1 Hg1 121.9(2) . . ? C2 O3 Hg1 96.0(4) . 4_666 ? C2 O3 Hg1 126.3(4) . 3_666 ? Hg1 O3 Hg1 135.1(2) 4_666 3_666 ? C2 O4 Hg2 122.3(4) . 3_656 ? C2 O4 Hg1 86.2(4) . 4_666 ? Hg2 O4 Hg1 149.1(2) 3_656 4_666 ? C8 O5 Hg2 149.7(5) . . ? C8 O6 Hg2 117.6(5) . 2_655 ? C9 O7 Hg1 111.1(5) . . ? C9 O8 Hg2 115.4(4) . . ? O2 C1 O1 125.5(7) . . ? O2 C1 C3 120.0(6) . . ? O1 C1 C3 114.4(6) . . ? O3 C2 O4 122.4(6) . . ? O3 C2 C4 118.1(7) . . ? O4 C2 C4 119.5(7) . . ? N1 C3 C4 119.8(6) . . ? N1 C3 C1 117.2(6) . . ? C4 C3 C1 122.9(6) . . ? C5 C4 C3 119.7(6) . . ? C5 C4 C2 119.4(6) . . ? C3 C4 C2 120.9(6) . . ? C4 C5 C6 119.0(7) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 119.2(7) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? N1 C7 C6 121.3(7) . . ? N1 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? O5 C8 O6 123.9(7) . . ? O5 C8 C10 118.9(6) . . ? O6 C8 C10 117.2(7) . . ? O8 C9 O7 125.8(7) . . ? O8 C9 C11 120.8(7) . . ? O7 C9 C11 113.4(6) . . ? N2 C10 C11 120.2(6) . . ? N2 C10 C8 117.4(6) . . ? C11 C10 C8 122.2(6) . . ? C12 C11 C10 119.2(7) . . ? C12 C11 C9 119.2(6) . . ? C10 C11 C9 121.4(6) . . ? C13 C12 C11 119.3(7) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 118.8(7) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? N2 C14 C13 121.7(7) . . ? N2 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? 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 O7 Hg1 N1 C7 113.0(5) . . . . ? O3 Hg1 N1 C7 -82.0(5) 4_565 . . . ? O1 Hg1 N1 C7 -172.2(6) . . . . ? O4 Hg1 N1 C7 -30.0(5) 4_565 . . . ? O3 Hg1 N1 C7 51.0(5) 3_666 . . . ? O7 Hg1 N1 C3 -61.6(6) . . . . ? O3 Hg1 N1 C3 103.4(5) 4_565 . . . ? O1 Hg1 N1 C3 13.2(5) . . . . ? O4 Hg1 N1 C3 155.4(5) 4_565 . . . ? O3 Hg1 N1 C3 -123.5(5) 3_666 . . . ? O6 Hg2 O1 C1 -161.6(6) 2_645 . . . ? N2 Hg2 O1 C1 9.6(7) 2_645 . . . ? O4 Hg2 O1 C1 128.0(6) 3_656 . . . ? O8 Hg2 O1 C1 -156.3(6) . . . . ? O5 Hg2 O1 C1 -84.0(5) . . . . ? O6 Hg2 O1 Hg1 -6.8(8) 2_645 . . . ? N2 Hg2 O1 Hg1 164.4(2) 2_645 . . . ? O4 Hg2 O1 Hg1 -77.2(3) 3_656 . . . ? O8 Hg2 O1 Hg1 -1.5(2) . . . . ? O5 Hg2 O1 Hg1 70.8(3) . . . . ? O7 Hg1 O1 C1 115.6(5) . . . . ? N1 Hg1 O1 C1 -20.1(5) . . . . ? O3 Hg1 O1 C1 -134.3(5) 4_565 . . . ? O4 Hg1 O1 C1 -96.7(5) 4_565 . . . ? O3 Hg1 O1 C1 35.5(6) 3_666 . . . ? O7 Hg1 O1 Hg2 -40.1(3) . . . . ? N1 Hg1 O1 Hg2 -175.7(4) . . . . ? O3 Hg1 O1 Hg2 70.1(3) 4_565 . . . ? O4 Hg1 O1 Hg2 107.7(3) 4_565 . . . ? O3 Hg1 O1 Hg2 -120.1(3) 3_666 . . . ? O1 Hg2 O5 C8 -146.8(10) . . . . ? O6 Hg2 O5 C8 14.4(10) 2_645 . . . ? N2 Hg2 O5 C8 88.2(10) 2_645 . . . ? O4 Hg2 O5 C8 -73.7(11) 3_656 . . . ? O8 Hg2 O5 C8 -67.3(10) . . . . ? N1 Hg1 O7 C9 116.1(4) . . . . ? O3 Hg1 O7 C9 -49.6(4) 4_565 . . . ? O1 Hg1 O7 C9 51.4(4) . . . . ? O4 Hg1 O7 C9 -106.4(4) 4_565 . . . ? O3 Hg1 O7 C9 177.2(4) 3_666 . . . ? O1 Hg2 O8 C9 74.9(5) . . . . ? O6 Hg2 O8 C9 -106.9(5) 2_645 . . . ? N2 Hg2 O8 C9 -79.3(7) 2_645 . . . ? O4 Hg2 O8 C9 162.3(5) 3_656 . . . ? O5 Hg2 O8 C9 -14.0(5) . . . . ? Hg2 O1 C1 O2 -2.8(11) . . . . ? Hg1 O1 C1 O2 -159.3(7) . . . . ? Hg2 O1 C1 C3 179.3(4) . . . . ? Hg1 O1 C1 C3 22.8(8) . . . . ? Hg1 O3 C2 O4 19.1(8) 4_666 . . . ? Hg1 O3 C2 O4 -144.9(6) 3_666 . . . ? Hg1 O3 C2 C4 -163.7(5) 4_666 . . . ? Hg1 O3 C2 C4 32.3(9) 3_666 . . . ? Hg2 O4 C2 O3 175.3(5) 3_656 . . . ? Hg1 O4 C2 O3 -17.4(7) 4_666 . . . ? Hg2 O4 C2 C4 -1.8(9) 3_656 . . . ? Hg1 O4 C2 C4 165.5(6) 4_666 . . . ? C7 N1 C3 C4 -2.4(10) . . . . ? Hg1 N1 C3 C4 172.1(5) . . . . ? C7 N1 C3 C1 178.2(6) . . . . ? Hg1 N1 C3 C1 -7.3(8) . . . . ? O2 C1 C3 N1 170.1(7) . . . . ? O1 C1 C3 N1 -11.8(9) . . . . ? O2 C1 C3 C4 -9.2(11) . . . . ? O1 C1 C3 C4 168.8(7) . . . . ? N1 C3 C4 C5 2.9(10) . . . . ? C1 C3 C4 C5 -177.7(7) . . . . ? N1 C3 C4 C2 -177.5(6) . . . . ? C1 C3 C4 C2 1.9(10) . . . . ? O3 C2 C4 C5 -81.8(9) . . . . ? O4 C2 C4 C5 95.5(9) . . . . ? O3 C2 C4 C3 98.6(8) . . . . ? O4 C2 C4 C3 -84.2(9) . . . . ? C3 C4 C5 C6 0.1(11) . . . . ? C2 C4 C5 C6 -179.5(7) . . . . ? C4 C5 C6 C7 -3.5(11) . . . . ? C3 N1 C7 C6 -1.2(11) . . . . ? Hg1 N1 C7 C6 -175.7(6) . . . . ? C5 C6 C7 N1 4.2(12) . . . . ? Hg2 O5 C8 O6 -124.0(9) . . . . ? Hg2 O5 C8 C10 54.8(13) . . . . ? Hg2 O6 C8 O5 180.0(6) 2_655 . . . ? Hg2 O6 C8 C10 1.1(9) 2_655 . . . ? Hg2 O8 C9 O7 -89.2(7) . . . . ? Hg2 O8 C9 C11 93.9(6) . . . . ? Hg1 O7 C9 O8 5.0(8) . . . . ? Hg1 O7 C9 C11 -177.9(4) . . . . ? C14 N2 C10 C11 -4.2(10) . . . . ? Hg2 N2 C10 C11 168.1(5) 2_655 . . . ? C14 N2 C10 C8 172.0(6) . . . . ? Hg2 N2 C10 C8 -15.6(8) 2_655 . . . ? O5 C8 C10 N2 -168.5(7) . . . . ? O6 C8 C10 N2 10.4(10) . . . . ? O5 C8 C10 C11 7.7(11) . . . . ? O6 C8 C10 C11 -173.4(7) . . . . ? N2 C10 C11 C12 6.5(11) . . . . ? C8 C10 C11 C12 -169.6(7) . . . . ? N2 C10 C11 C9 -169.0(6) . . . . ? C8 C10 C11 C9 14.9(11) . . . . ? O8 C9 C11 C12 79.7(9) . . . . ? O7 C9 C11 C12 -97.6(8) . . . . ? O8 C9 C11 C10 -104.8(8) . . . . ? O7 C9 C11 C10 77.9(8) . . . . ? C10 C11 C12 C13 -3.2(12) . . . . ? C9 C11 C12 C13 172.4(7) . . . . ? C11 C12 C13 C14 -2.2(12) . . . . ? C10 N2 C14 C13 -1.3(11) . . . . ? Hg2 N2 C14 C13 -172.4(5) 2_655 . . . ? C12 C13 C14 N2 4.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.486 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.187 # Attachment 'compound 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 792171' #TrackingRef 'compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H11 Hg N3 O4, 2(H2 O)' _chemical_formula_sum 'C19 H15 Hg N3 O6' _chemical_formula_weight 581.93 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3973(17) _cell_length_b 20.078(4) _cell_length_c 13.076(4) _cell_angle_alpha 90.00 _cell_angle_beta 125.08(2) _cell_angle_gamma 90.00 _cell_volume 1804.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 8.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.192 _exptl_absorpt_correction_T_max 0.420 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _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 'CCD area detector' _diffrn_measurement_method '\p and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 15218 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3174 _reflns_number_gt 2886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART ' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL/PC (Sheldrick, 1999)' _computing_publication_material 'Bruker SHELXTL/PC and PLATON (Spek, 2003)' _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^)+(0.0797P)^2^+4.9219P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3174 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.18222(4) 0.333932(14) 0.19669(3) 0.02374(16) Uani 1 1 d . . . O1 O 0.0424(9) 0.2403(3) 0.0546(6) 0.0371(14) Uani 1 1 d . . . O2 O -0.1542(9) 0.1548(3) 0.0158(6) 0.0306(14) Uani 1 1 d . . . O1W O 0.2151(13) 0.0946(4) 0.0766(9) 0.074(3) Uani 1 1 d . . . H1WA H 0.2168 0.1368 0.0725 0.089 Uiso 1 1 d R . . H1WB H 0.1201 0.0827 0.0789 0.111 Uiso 1 1 d R . . O2W O 0.7250(15) 0.0367(4) 0.8419(8) 0.086(3) Uani 1 1 d . . . H2WA H 0.7720 0.0631 0.9037 0.128 Uiso 1 1 d R . . H2WB H 0.6305 0.0153 0.8331 0.128 Uiso 1 1 d R . . O3 O -0.5502(8) 0.2213(3) -0.1477(5) 0.0292(12) Uani 1 1 d . . . O4 O -0.6383(10) 0.1599(3) -0.0469(6) 0.0384(16) Uani 1 1 d . . . N1 N -0.0759(9) 0.2939(3) 0.1938(5) 0.0214(13) Uani 1 1 d . . . N2 N 0.1867(9) 0.3769(3) 0.0321(6) 0.0265(15) Uani 1 1 d . . . N3 N 0.2313(10) 0.4479(3) 0.2279(6) 0.0267(15) Uani 1 1 d . . . C1 C 0.1722(15) 0.3419(4) -0.0608(9) 0.039(2) Uani 1 1 d . . . H1 H 0.1501 0.2962 -0.0655 0.046 Uiso 1 1 calc R . . C2 C 0.1892(14) 0.3717(6) -0.1499(8) 0.043(2) Uani 1 1 d . . . H2 H 0.1780 0.3463 -0.2131 0.052 Uiso 1 1 calc R . . C3 C 0.2222(14) 0.4380(6) -0.1442(9) 0.050(3) Uani 1 1 d . . . H3 H 0.2331 0.4580 -0.2040 0.060 Uiso 1 1 calc R . . C4 C 0.2400(13) 0.4764(5) -0.0501(8) 0.039(2) Uani 1 1 d . . . C5 C 0.2268(11) 0.4428(4) 0.0428(7) 0.0281(18) Uani 1 1 d . . . C6 C 0.2477(10) 0.4803(4) 0.1428(7) 0.0257(17) Uani 1 1 d . . . C7 C 0.2806(15) 0.5471(5) -0.0338(10) 0.049(3) Uani 1 1 d . . . H7 H 0.2969 0.5692 -0.0897 0.059 Uiso 1 1 calc R . . C8 C 0.2953(15) 0.5815(5) 0.0578(12) 0.054(3) Uani 1 1 d . . . H8 H 0.3129 0.6274 0.0614 0.065 Uiso 1 1 calc R . . C9 C 0.2843(12) 0.5486(4) 0.1537(9) 0.037(2) Uani 1 1 d . . . C10 C 0.3030(14) 0.5830(5) 0.2515(11) 0.049(3) Uani 1 1 d . . . H10 H 0.3293 0.6285 0.2611 0.059 Uiso 1 1 calc R . . C11 C 0.2821(15) 0.5488(5) 0.3350(10) 0.050(3) Uani 1 1 d . . . H11 H 0.2879 0.5711 0.3994 0.059 Uiso 1 1 calc R . . C12 C 0.2524(13) 0.4807(4) 0.3204(9) 0.037(2) Uani 1 1 d . . . H12 H 0.2473 0.4573 0.3799 0.044 Uiso 1 1 calc R . . C13 C -0.0960(10) 0.2126(4) 0.0501(6) 0.0213(16) Uani 1 1 d . . . C14 C -0.1921(10) 0.2510(3) 0.1026(6) 0.0167(14) Uani 1 1 d . . . C15 C -0.3777(11) 0.2376(4) 0.0687(7) 0.0206(15) Uani 1 1 d . . . C16 C -0.4354(11) 0.2640(4) 0.1428(7) 0.0252(17) Uani 1 1 d . . . H16 H -0.5557 0.2532 0.1265 0.030 Uiso 1 1 calc R . . C17 C -0.3094(12) 0.3064(4) 0.2401(7) 0.0274(18) Uani 1 1 d . . . H17 H -0.3432 0.3241 0.2910 0.033 Uiso 1 1 calc R . . C18 C -0.1370(13) 0.3218(4) 0.2604(7) 0.0264(18) Uani 1 1 d . . . H18 H -0.0569 0.3526 0.3223 0.032 Uiso 1 1 calc R . . C19 C -0.5293(11) 0.2024(3) -0.0487(7) 0.0212(16) Uani 1 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 Hg1 0.0237(2) 0.0249(2) 0.0136(2) 0.00006(10) 0.00547(16) -0.00269(11) O1 0.033(3) 0.040(3) 0.049(4) -0.017(3) 0.031(3) -0.006(3) O2 0.041(4) 0.022(3) 0.025(3) -0.009(2) 0.016(3) -0.005(3) O1W 0.085(6) 0.061(5) 0.110(8) 0.035(5) 0.076(6) 0.034(5) O2W 0.120(8) 0.061(5) 0.058(6) -0.013(4) 0.040(6) -0.021(5) O3 0.029(3) 0.039(3) 0.014(3) -0.006(2) 0.010(2) -0.012(3) O4 0.037(4) 0.048(4) 0.021(3) -0.007(3) 0.011(3) -0.018(3) N1 0.022(3) 0.030(3) 0.009(3) -0.001(3) 0.007(3) 0.001(3) N2 0.024(4) 0.036(4) 0.012(3) 0.007(3) 0.006(3) 0.005(3) N3 0.024(3) 0.025(3) 0.017(3) 0.002(3) 0.003(3) 0.002(3) C1 0.045(6) 0.043(5) 0.022(5) -0.002(4) 0.016(5) 0.003(4) C2 0.037(5) 0.075(7) 0.015(4) 0.003(4) 0.014(4) 0.000(5) C3 0.033(5) 0.086(8) 0.021(5) 0.023(5) 0.009(4) -0.002(5) C4 0.023(4) 0.052(6) 0.031(5) 0.023(4) 0.010(4) 0.008(4) C5 0.019(4) 0.033(4) 0.025(4) 0.012(3) 0.009(4) 0.006(3) C6 0.008(3) 0.028(4) 0.025(4) 0.008(3) 0.000(3) 0.006(3) C7 0.040(6) 0.050(6) 0.051(7) 0.024(5) 0.023(5) 0.001(5) C8 0.037(6) 0.027(5) 0.078(8) 0.023(5) 0.021(6) -0.002(4) C9 0.020(4) 0.028(4) 0.052(6) 0.006(4) 0.015(4) -0.001(4) C10 0.041(6) 0.019(4) 0.063(7) -0.003(5) 0.016(5) 0.004(4) C11 0.043(6) 0.041(5) 0.046(6) -0.020(5) 0.014(5) 0.002(5) C12 0.033(5) 0.036(5) 0.032(5) -0.008(4) 0.014(4) -0.005(4) C13 0.016(4) 0.024(4) 0.009(3) 0.005(3) -0.002(3) 0.007(3) C14 0.019(4) 0.019(3) 0.008(3) 0.006(3) 0.006(3) 0.007(3) C15 0.019(4) 0.025(4) 0.012(4) 0.003(3) 0.006(3) 0.007(3) C16 0.023(4) 0.031(4) 0.021(4) 0.002(3) 0.012(3) 0.001(3) C17 0.042(5) 0.025(4) 0.021(4) -0.007(3) 0.022(4) -0.005(4) C18 0.031(5) 0.031(4) 0.012(4) -0.004(3) 0.009(4) 0.001(4) C19 0.028(4) 0.017(4) 0.013(4) -0.010(3) 0.009(3) -0.003(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 Hg1 O3 2.272(5) 4_666 ? Hg1 N1 2.291(6) . ? Hg1 N3 2.320(7) . ? Hg1 N2 2.338(6) . ? Hg1 O1 2.421(6) . ? Hg1 O4 2.779(6) 4_666 ? O1 C13 1.259(9) . ? O2 C13 1.239(9) . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3 C19 1.261(9) . ? O3 Hg1 2.272(5) 4_465 ? O4 C19 1.262(9) . ? O4 Hg1 2.779(6) 4_465 ? N1 C14 1.334(9) . ? N1 C18 1.359(10) . ? N2 C1 1.348(11) . ? N2 C5 1.354(10) . ? N3 C12 1.297(11) . ? N3 C6 1.362(10) . ? C1 C2 1.388(13) . ? C1 H1 0.9300 . ? C2 C3 1.352(15) . ? C2 H2 0.9300 . ? C3 C4 1.385(15) . ? C3 H3 0.9300 . ? C4 C5 1.447(12) . ? C4 C7 1.447(14) . ? C5 C6 1.429(12) . ? C6 C9 1.396(11) . ? C7 C8 1.326(16) . ? C7 H7 0.9300 . ? C8 C9 1.465(14) . ? C8 H8 0.9300 . ? C9 C10 1.381(14) . ? C10 C11 1.384(17) . ? C10 H10 0.9300 . ? C11 C12 1.384(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.534(10) . ? C14 C15 1.380(10) . ? C15 C16 1.413(10) . ? C15 C19 1.493(10) . ? C16 C17 1.384(11) . ? C16 H16 0.9300 . ? C17 C18 1.350(12) . ? C17 H17 0.9300 . ? C18 H18 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 O3 Hg1 N1 106.4(2) 4_666 . ? O3 Hg1 N3 109.9(2) 4_666 . ? N1 Hg1 N3 114.8(2) . . ? O3 Hg1 N2 118.2(2) 4_666 . ? N1 Hg1 N2 129.0(2) . . ? N3 Hg1 N2 72.7(2) . . ? O3 Hg1 O1 95.8(2) 4_666 . ? N1 Hg1 O1 71.2(2) . . ? N3 Hg1 O1 149.3(2) . . ? N2 Hg1 O1 80.6(2) . . ? O3 Hg1 O4 50.94(18) 4_666 4_666 ? N1 Hg1 O4 83.5(2) . 4_666 ? N3 Hg1 O4 80.0(2) . 4_666 ? N2 Hg1 O4 144.1(2) . 4_666 ? O1 Hg1 O4 130.4(2) . 4_666 ? C13 O1 Hg1 113.9(5) . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? C19 O3 Hg1 104.8(4) . 4_465 ? C19 O4 Hg1 81.0(4) . 4_465 ? C14 N1 C18 119.2(7) . . ? C14 N1 Hg1 116.1(4) . . ? C18 N1 Hg1 123.1(5) . . ? C1 N2 C5 119.4(7) . . ? C1 N2 Hg1 126.7(6) . . ? C5 N2 Hg1 113.6(5) . . ? C12 N3 C6 119.8(8) . . ? C12 N3 Hg1 125.4(6) . . ? C6 N3 Hg1 114.7(5) . . ? N2 C1 C2 122.1(9) . . ? N2 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.7(9) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.7(9) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 117.7(9) . . ? C3 C4 C7 125.0(9) . . ? C5 C4 C7 117.3(9) . . ? N2 C5 C6 120.0(7) . . ? N2 C5 C4 120.3(8) . . ? C6 C5 C4 119.7(8) . . ? N3 C6 C9 120.3(8) . . ? N3 C6 C5 118.7(7) . . ? C9 C6 C5 121.0(8) . . ? C8 C7 C4 122.4(9) . . ? C8 C7 H7 118.8 . . ? C4 C7 H7 118.8 . . ? C7 C8 C9 121.3(9) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C6 119.2(9) . . ? C10 C9 C8 122.5(9) . . ? C6 C9 C8 118.3(9) . . ? C11 C10 C9 118.9(9) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 118.5(10) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N3 C12 C11 123.2(10) . . ? N3 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? O2 C13 O1 126.3(7) . . ? O2 C13 C14 115.7(7) . . ? O1 C13 C14 117.8(6) . . ? N1 C14 C15 121.6(6) . . ? N1 C14 C13 115.0(6) . . ? C15 C14 C13 123.0(6) . . ? C14 C15 C16 118.4(7) . . ? C14 C15 C19 124.1(6) . . ? C16 C15 C19 117.2(7) . . ? C17 C16 C15 118.7(7) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C16 119.2(7) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 N1 122.5(7) . . ? C17 C18 H18 118.7 . . ? N1 C18 H18 118.7 . . ? O3 C19 O4 123.3(7) . . ? O3 C19 C15 116.5(6) . . ? O4 C19 C15 119.9(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O1 0.85 2.47 3.203(10) 144.3 . O1W H1WB O2 0.85 2.43 2.979(10) 123.1 . O2W H2WA O2 0.85 2.21 3.027(10) 161.8 1_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.446 _refine_diff_density_min -1.886 _refine_diff_density_rms 0.179 # Attachment 'compound 3.cif' data_090512a _database_code_depnum_ccdc_archive 'CCDC 792172' #TrackingRef 'compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H9 Ca Hg N3 O7 S2' _chemical_formula_sum 'C9 H9 Ca Hg N3 O7 S2' _chemical_formula_weight 575.98 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' 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' Ca Ca 0.2262 0.3064 '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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0665(19) _cell_length_b 6.8530(10) _cell_length_c 15.3784(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.6520(10) _cell_angle_gamma 90.00 _cell_volume 1607.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2956 _cell_measurement_theta_min 2.649 _cell_measurement_theta_max 27.725 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 10.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1626 _exptl_absorpt_correction_T_max 0.2925 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7491 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2823 _reflns_number_gt 2261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART ' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _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^)+(0.0299P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2823 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.129819(16) 0.47073(4) 0.281030(17) 0.02859(10) Uani 1 1 d . . . Ca1 Ca 0.43353(7) 0.32140(16) 0.18902(8) 0.0177(3) Uani 1 1 d . . . N1 N 0.1752(3) 0.5658(7) 0.4326(3) 0.0177(11) Uani 1 1 d . . . N2 N 0.2727(4) 0.3038(8) 0.1528(4) 0.0357(14) Uani 1 1 d . . . N3 N -0.1645(5) 0.5767(10) 0.1270(6) 0.071(2) Uani 1 1 d . . . O1 O 0.2893(3) 0.5280(7) 0.3536(3) 0.0339(11) Uani 1 1 d . . . O2 O 0.3949(3) 0.6679(7) 0.4841(3) 0.0343(11) Uani 1 1 d . . . O3 O 0.4290(3) 0.5191(5) 0.6796(3) 0.0227(10) Uani 1 1 d . . . O4 O 0.4210(2) 0.8385(5) 0.6870(3) 0.0228(10) Uani 1 1 d . . . O1W O 0.4258(3) 0.3023(6) 0.3479(3) 0.0302(10) Uani 1 1 d . . . H5A H 0.3879 0.3735 0.3542 0.045 Uiso 1 1 d R . . H5B H 0.4748 0.3176 0.3976 0.045 Uiso 1 1 d R . . O2W O 0.3474(3) 0.3479(8) 0.0132(3) 0.0480(14) Uani 1 1 d . . . H6A H 0.2940 0.3819 -0.0069 0.072 Uiso 1 1 d R . . H6B H 0.3488 0.2379 -0.0120 0.072 Uiso 1 1 d R . . O3W O 0.5310(3) 0.3808(7) 0.1146(3) 0.0410(12) Uani 1 1 d . . . H7A H 0.5452 0.2716 0.0989 0.061 Uiso 1 1 d R . . H7B H 0.5751 0.4475 0.1532 0.061 Uiso 1 1 d R . . S1 S 0.09837(10) 0.3446(3) 0.12356(12) 0.0345(4) Uani 1 1 d . . . S2 S -0.03994(10) 0.3343(2) 0.26752(12) 0.0303(4) Uani 1 1 d . . . C1 C 0.3200(4) 0.5993(9) 0.4377(4) 0.0228(14) Uani 1 1 d . . . C2 C 0.3872(4) 0.6769(8) 0.6525(4) 0.0171(13) Uani 1 1 d . . . C3 C 0.2608(3) 0.6062(8) 0.4880(4) 0.0160(12) Uani 1 1 d . . . C4 C 0.2913(3) 0.6627(8) 0.5839(4) 0.0150(12) Uani 1 1 d . . . C5 C 0.2315(4) 0.6889(9) 0.6218(4) 0.0236(14) Uani 1 1 d . . . H5 H 0.2507 0.7300 0.6858 0.028 Uiso 1 1 calc R . . C6 C 0.1442(4) 0.6535(9) 0.5638(5) 0.0290(16) Uani 1 1 d . . . H6 H 0.1035 0.6724 0.5878 0.035 Uiso 1 1 calc R . . C7 C 0.1173(4) 0.5895(9) 0.4696(4) 0.0268(15) Uani 1 1 d . . . H7 H 0.0583 0.5621 0.4309 0.032 Uiso 1 1 calc R . . C8 C 0.2030(4) 0.3200(9) 0.1419(4) 0.0258(15) Uani 1 1 d . . . C9 C -0.1141(5) 0.4769(10) 0.1844(6) 0.0369(17) Uani 1 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 Hg1 0.02506(16) 0.03427(17) 0.02331(15) -0.00727(12) 0.00807(11) -0.00292(12) Ca1 0.0159(6) 0.0111(6) 0.0225(7) -0.0003(5) 0.0056(5) 0.0001(5) N1 0.015(3) 0.018(3) 0.019(3) -0.002(2) 0.007(2) -0.002(2) N2 0.024(3) 0.043(4) 0.039(4) -0.007(3) 0.014(3) -0.002(3) N3 0.048(5) 0.039(4) 0.080(5) -0.002(4) -0.012(4) 0.005(3) O1 0.020(2) 0.057(3) 0.024(3) -0.015(2) 0.009(2) -0.006(2) O2 0.017(2) 0.056(3) 0.032(3) -0.006(2) 0.013(2) -0.013(2) O3 0.018(2) 0.010(2) 0.029(2) 0.0015(17) 0.0009(19) 0.0003(17) O4 0.022(2) 0.008(2) 0.029(2) -0.0033(17) 0.0035(19) -0.0031(17) O1W 0.022(2) 0.035(3) 0.033(3) -0.006(2) 0.012(2) 0.001(2) O2W 0.039(3) 0.058(4) 0.032(3) -0.002(2) 0.003(2) 0.006(3) O3W 0.046(3) 0.037(3) 0.051(3) -0.007(2) 0.032(3) -0.003(2) S1 0.0180(9) 0.0520(12) 0.0305(10) -0.0149(8) 0.0081(8) -0.0046(8) S2 0.0247(9) 0.0260(10) 0.0347(10) -0.0013(7) 0.0084(8) -0.0050(7) C1 0.019(4) 0.024(3) 0.026(4) 0.007(3) 0.011(3) 0.003(3) C2 0.019(3) 0.018(3) 0.016(3) -0.001(2) 0.009(3) -0.005(3) C3 0.008(3) 0.015(3) 0.024(3) 0.001(2) 0.007(3) 0.004(2) C4 0.009(3) 0.013(3) 0.019(3) -0.001(2) 0.003(2) 0.000(2) C5 0.021(4) 0.026(4) 0.020(3) -0.003(3) 0.005(3) 0.004(3) C6 0.021(4) 0.034(4) 0.040(4) -0.007(3) 0.021(3) -0.003(3) C7 0.012(3) 0.029(4) 0.033(4) -0.004(3) 0.005(3) -0.002(3) C8 0.033(4) 0.018(3) 0.026(4) -0.009(3) 0.013(3) -0.002(3) C9 0.027(4) 0.032(4) 0.041(4) -0.007(3) 0.006(3) -0.005(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 Hg1 N1 2.199(4) . ? Hg1 S1 2.3944(16) . ? Hg1 O1 2.467(4) . ? Hg1 S2 2.8442(17) 2 ? Hg1 S2 2.9616(17) . ? Hg1 N3 2.982(7) 2_545 ? Ca1 O3 2.337(4) 4_565 ? Ca1 O4 2.340(4) 4_575 ? Ca1 O2W 2.437(4) . ? Ca1 O3W 2.439(4) . ? Ca1 O1W 2.508(4) . ? Ca1 N2 2.546(6) . ? Ca1 O3 2.555(4) 3_666 ? Ca1 O4 2.599(4) 3_666 ? Ca1 C2 2.935(6) 3_666 ? Ca1 Ca1 4.0730(13) 2_655 ? Ca1 Ca1 4.0730(13) 2_645 ? N1 C3 1.349(7) . ? N1 C7 1.355(7) . ? N2 C8 1.131(7) . ? N3 C9 1.143(9) . ? N3 Hg1 2.982(7) 2 ? O1 C1 1.256(7) . ? O2 C1 1.243(7) . ? O3 C2 1.259(7) . ? O3 Ca1 2.337(4) 4_566 ? O3 Ca1 2.555(4) 3_666 ? O4 C2 1.251(7) . ? O4 Ca1 2.340(4) 4_576 ? O4 Ca1 2.599(4) 3_666 ? O1W H5A 0.8500 . ? O1W H5B 0.8500 . ? O2W H6A 0.8530 . ? O2W H6B 0.8525 . ? O3W H7A 0.8547 . ? O3W H7B 0.8526 . ? S1 C8 1.686(7) . ? S2 C9 1.655(8) . ? S2 Hg1 2.8442(16) 2_545 ? C1 C3 1.524(8) . ? C2 C4 1.500(7) . ? C2 Ca1 2.935(6) 3_666 ? C3 C4 1.381(7) . ? C4 C5 1.395(8) . ? C5 C6 1.373(8) . ? C5 H5 0.9300 . ? C6 C7 1.380(8) . ? C6 H6 0.9300 . ? C7 H7 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 N1 Hg1 S1 172.44(13) . . ? N1 Hg1 O1 71.37(15) . . ? S1 Hg1 O1 102.49(11) . . ? N1 Hg1 S2 84.88(12) . 2 ? S1 Hg1 S2 101.59(6) . 2 ? O1 Hg1 S2 109.58(11) . 2 ? N1 Hg1 S2 92.09(12) . . ? S1 Hg1 S2 92.67(5) . . ? O1 Hg1 S2 158.17(11) . . ? S2 Hg1 S2 82.11(3) 2 . ? N1 Hg1 N3 82.24(19) . 2_545 ? S1 Hg1 N3 93.41(17) . 2_545 ? O1 Hg1 N3 89.16(17) . 2_545 ? S2 Hg1 N3 152.46(17) 2 2_545 ? S2 Hg1 N3 74.17(15) . 2_545 ? O3 Ca1 O4 173.53(14) 4_565 4_575 ? O3 Ca1 O2W 91.09(16) 4_565 . ? O4 Ca1 O2W 84.54(15) 4_575 . ? O3 Ca1 O3W 98.50(16) 4_565 . ? O4 Ca1 O3W 84.55(15) 4_575 . ? O2W Ca1 O3W 70.49(16) . . ? O3 Ca1 O1W 89.64(15) 4_565 . ? O4 Ca1 O1W 91.17(14) 4_575 . ? O2W Ca1 O1W 144.61(16) . . ? O3W Ca1 O1W 144.16(15) . . ? O3 Ca1 N2 86.39(17) 4_565 . ? O4 Ca1 N2 87.76(16) 4_575 . ? O2W Ca1 N2 72.90(17) . . ? O3W Ca1 N2 143.12(17) . . ? O1W Ca1 N2 71.83(16) . . ? O3 Ca1 O3 117.98(11) 4_565 3_666 ? O4 Ca1 O3 68.32(12) 4_575 3_666 ? O2W Ca1 O3 136.77(16) . 3_666 ? O3W Ca1 O3 73.88(15) . 3_666 ? O1W Ca1 O3 71.51(14) . 3_666 ? N2 Ca1 O3 135.26(16) . 3_666 ? O3 Ca1 O4 67.58(13) 4_565 3_666 ? O4 Ca1 O4 118.78(11) 4_575 3_666 ? O2W Ca1 O4 138.41(16) . 3_666 ? O3W Ca1 O4 77.68(15) . 3_666 ? O1W Ca1 O4 73.38(13) . 3_666 ? N2 Ca1 O4 136.20(17) . 3_666 ? O3 Ca1 O4 50.51(11) 3_666 3_666 ? O3 Ca1 C2 92.78(15) 4_565 3_666 ? O4 Ca1 C2 93.57(15) 4_575 3_666 ? O2W Ca1 C2 143.77(17) . 3_666 ? O3W Ca1 C2 73.31(16) . 3_666 ? O1W Ca1 C2 71.47(14) . 3_666 ? N2 Ca1 C2 143.29(17) . 3_666 ? O3 Ca1 C2 25.33(13) 3_666 3_666 ? O4 Ca1 C2 25.21(14) 3_666 3_666 ? O3 Ca1 Ca1 149.83(11) 4_565 2_655 ? O4 Ca1 Ca1 36.57(9) 4_575 2_655 ? O2W Ca1 Ca1 112.49(13) . 2_655 ? O3W Ca1 Ca1 73.71(12) . 2_655 ? O1W Ca1 Ca1 81.79(10) . 2_655 ? N2 Ca1 Ca1 117.63(13) . 2_655 ? O3 Ca1 Ca1 31.97(9) 3_666 2_655 ? O4 Ca1 Ca1 82.25(9) 3_666 2_655 ? C2 Ca1 Ca1 57.06(12) 3_666 2_655 ? O3 Ca1 Ca1 35.37(9) 4_565 2_645 ? O4 Ca1 Ca1 150.82(10) 4_575 2_645 ? O2W Ca1 Ca1 120.52(13) . 2_645 ? O3W Ca1 Ca1 90.02(12) . 2_645 ? O1W Ca1 Ca1 76.68(10) . 2_645 ? N2 Ca1 Ca1 112.58(14) . 2_645 ? O3 Ca1 Ca1 82.62(9) 3_666 2_645 ? O4 Ca1 Ca1 32.43(9) 3_666 2_645 ? C2 Ca1 Ca1 57.52(12) 3_666 2_645 ? Ca1 Ca1 Ca1 114.55(5) 2_655 2_645 ? C3 N1 C7 119.9(5) . . ? C3 N1 Hg1 119.8(4) . . ? C7 N1 Hg1 120.3(4) . . ? C8 N2 Ca1 170.9(5) . . ? C9 N3 Hg1 104.8(6) . 2 ? C1 O1 Hg1 113.2(4) . . ? C2 O3 Ca1 151.1(4) . 4_566 ? C2 O3 Ca1 94.5(3) . 3_666 ? Ca1 O3 Ca1 112.66(15) 4_566 3_666 ? C2 O4 Ca1 155.4(4) . 4_576 ? C2 O4 Ca1 92.6(3) . 3_666 ? Ca1 O4 Ca1 111.01(14) 4_576 3_666 ? Ca1 O1W H5A 117.2 . . ? Ca1 O1W H5B 114.2 . . ? H5A O1W H5B 108.6 . . ? Ca1 O2W H6A 115.9 . . ? Ca1 O2W H6B 108.1 . . ? H6A O2W H6B 108.7 . . ? Ca1 O3W H7A 109.1 . . ? Ca1 O3W H7B 109.7 . . ? H7A O3W H7B 113.1 . . ? C8 S1 Hg1 97.3(2) . . ? C9 S2 Hg1 100.3(2) . 2_545 ? C9 S2 Hg1 104.6(3) . . ? Hg1 S2 Hg1 133.67(6) 2_545 . ? O2 C1 O1 125.8(6) . . ? O2 C1 C3 116.2(5) . . ? O1 C1 C3 118.0(5) . . ? O4 C2 O3 122.3(5) . . ? O4 C2 C4 120.3(5) . . ? O3 C2 C4 117.1(5) . . ? O4 C2 Ca1 62.2(3) . 3_666 ? O3 C2 Ca1 60.2(3) . 3_666 ? C4 C2 Ca1 170.4(4) . 3_666 ? N1 C3 C4 120.9(5) . . ? N1 C3 C1 116.7(5) . . ? C4 C3 C1 122.2(5) . . ? C3 C4 C5 119.1(5) . . ? C3 C4 C2 122.6(5) . . ? C5 C4 C2 118.0(5) . . ? C6 C5 C4 119.4(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 119.4(6) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? N1 C7 C6 121.2(5) . . ? N1 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? N2 C8 S1 179.0(6) . . ? N3 C9 S2 179.2(8) . . ? 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 O1 Hg1 N1 C3 -0.1(4) . . . . ? S2 Hg1 N1 C3 -112.7(4) 2 . . . ? S2 Hg1 N1 C3 165.4(4) . . . . ? N3 Hg1 N1 C3 91.7(4) 2_545 . . . ? O1 Hg1 N1 C7 178.0(5) . . . . ? S2 Hg1 N1 C7 65.3(4) 2 . . . ? S2 Hg1 N1 C7 -16.6(4) . . . . ? N3 Hg1 N1 C7 -90.3(5) 2_545 . . . ? N1 Hg1 O1 C1 -5.9(4) . . . . ? S1 Hg1 O1 C1 178.7(4) . . . . ? S2 Hg1 O1 C1 71.4(4) 2 . . . ? S2 Hg1 O1 C1 -48.3(6) . . . . ? N3 Hg1 O1 C1 -88.0(5) 2_545 . . . ? O1 Hg1 S1 C8 8.5(3) . . . . ? S2 Hg1 S1 C8 121.8(2) 2 . . . ? S2 Hg1 S1 C8 -155.7(2) . . . . ? N3 Hg1 S1 C8 -81.4(3) 2_545 . . . ? N1 Hg1 S2 C9 115.6(3) . . . . ? S1 Hg1 S2 C9 -70.3(3) . . . . ? O1 Hg1 S2 C9 155.4(4) . . . . ? S2 Hg1 S2 C9 31.1(3) 2 . . . ? N3 Hg1 S2 C9 -163.1(3) 2_545 . . . ? N1 Hg1 S2 Hg1 -124.04(14) . . . 2_545 ? S1 Hg1 S2 Hg1 50.08(9) . . . 2_545 ? O1 Hg1 S2 Hg1 -84.2(3) . . . 2_545 ? S2 Hg1 S2 Hg1 151.42(11) 2 . . 2_545 ? N3 Hg1 S2 Hg1 -42.71(18) 2_545 . . 2_545 ? Hg1 O1 C1 O2 -168.8(5) . . . . ? Hg1 O1 C1 C3 10.3(7) . . . . ? Ca1 O4 C2 O3 159.8(6) 4_576 . . . ? Ca1 O4 C2 O3 -4.1(6) 3_666 . . . ? Ca1 O4 C2 C4 -26.6(12) 4_576 . . . ? Ca1 O4 C2 C4 169.4(4) 3_666 . . . ? Ca1 O4 C2 Ca1 163.9(9) 4_576 . . 3_666 ? Ca1 O3 C2 O4 164.5(5) 4_566 . . . ? Ca1 O3 C2 O4 4.2(6) 3_666 . . . ? Ca1 O3 C2 C4 -9.2(11) 4_566 . . . ? Ca1 O3 C2 C4 -169.6(4) 3_666 . . . ? Ca1 O3 C2 Ca1 160.3(8) 4_566 . . 3_666 ? C7 N1 C3 C4 3.1(8) . . . . ? Hg1 N1 C3 C4 -178.8(4) . . . . ? C7 N1 C3 C1 -173.0(5) . . . . ? Hg1 N1 C3 C1 5.1(7) . . . . ? O2 C1 C3 N1 168.3(5) . . . . ? O1 C1 C3 N1 -10.9(8) . . . . ? O2 C1 C3 C4 -7.7(9) . . . . ? O1 C1 C3 C4 173.1(5) . . . . ? N1 C3 C4 C5 -3.7(8) . . . . ? C1 C3 C4 C5 172.2(5) . . . . ? N1 C3 C4 C2 169.6(5) . . . . ? C1 C3 C4 C2 -14.5(8) . . . . ? O4 C2 C4 C3 115.2(6) . . . . ? O3 C2 C4 C3 -70.9(7) . . . . ? O4 C2 C4 C5 -71.3(7) . . . . ? O3 C2 C4 C5 102.6(6) . . . . ? C3 C4 C5 C6 1.6(9) . . . . ? C2 C4 C5 C6 -172.1(5) . . . . ? C4 C5 C6 C7 1.1(9) . . . . ? C3 N1 C7 C6 -0.4(9) . . . . ? Hg1 N1 C7 C6 -178.4(5) . . . . ? C5 C6 C7 N1 -1.7(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H5A O1 0.85 1.98 2.829(6) 173.1 . O1W H5B O2 0.85 2.15 2.999(6) 173.3 3_666 O2W H6A N3 0.85 2.17 2.935(8) 149.1 3_565 O2W H6B O1 0.85 2.60 3.385(7) 154.3 4_565 O3W H7A O2 0.85 2.08 2.785(6) 138.7 2_645 O3W H7B O1W 0.85 2.43 2.973(6) 122.0 2_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.253 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.150 # Attachment 'compound 4.cif' data_090426c _database_code_depnum_ccdc_archive 'CCDC 792173' #TrackingRef 'compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H9 Hg N3 O7 S2 Sr' _chemical_formula_sum 'C9 H9 Hg N3 O7 S2 Sr' _chemical_formula_weight 623.52 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' 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' Sr Sr -1.5307 3.2498 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 30.740(3) _cell_length_b 6.8408(5) _cell_length_c 15.7361(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.679(2) _cell_angle_gamma 90.00 _cell_volume 3251.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3608 _cell_measurement_theta_min 3.952 _cell_measurement_theta_max 27.874 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 13.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1118 _exptl_absorpt_correction_T_max 0.2827 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7768 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2858 _reflns_number_gt 2327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART ' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _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^)+(0.0725P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00099(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2858 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 0.424486(11) 0.52160(6) 0.62534(2) 0.0360(2) Uani 1 1 d . . . Sr1 Sr 0.27761(2) 0.23803(11) 0.32698(4) 0.0179(2) Uani 1 1 d . . . N1 N 0.4088(2) 0.6708(11) 0.4883(4) 0.0263(16) Uani 1 1 d . . . N2 N 0.3593(2) 0.1843(12) 0.4373(5) 0.0378(19) Uani 1 1 d . . . N3 N 0.4958(3) 0.6280(17) 0.8639(6) 0.060(3) Uani 1 1 d . . . O1 O 0.34176(19) 0.5532(9) 0.5680(3) 0.0271(13) Uani 1 1 d . . . O2 O 0.29485(18) 0.5403(9) 0.4424(4) 0.0270(13) Uani 1 1 d . . . O3 O 0.29820(18) 0.5632(8) 0.2608(3) 0.0209(12) Uani 1 1 d . . . O4 O 0.28887(17) 0.8740(8) 0.2947(3) 0.0225(12) Uani 1 1 d . . . O5 O 0.2669(2) -0.0113(8) 0.4523(4) 0.0293(14) Uani 1 1 d . . . H5A H 0.2725 -0.1296 0.4409 0.044 Uiso 1 1 d R . . H5B H 0.2421 -0.0044 0.4683 0.044 Uiso 1 1 d R . . O6 O 0.3082(2) 0.1873(9) 0.1881(4) 0.0389(16) Uani 1 1 d . . . H6A H 0.3111 0.2911 0.1603 0.058 Uiso 1 1 d R . . H6B H 0.2966 0.0960 0.1553 0.058 Uiso 1 1 d R . . O7 O 0.20088(19) 0.3140(9) 0.3933(4) 0.0323(14) Uani 1 1 d . . . H7A H 0.1864 0.2101 0.3978 0.048 Uiso 1 1 d R . . H7B H 0.2066 0.3732 0.4417 0.048 Uiso 1 1 d R . . S1 S 0.43041(9) 0.1764(5) 0.58106(19) 0.0524(7) Uani 1 1 d . . . S2 S 0.41416(8) 0.7002(4) 0.75448(17) 0.0471(7) Uani 1 1 d . . . C1 C 0.3326(3) 0.5778(11) 0.4886(5) 0.0199(17) Uani 1 1 d . . . C2 C 0.3109(3) 0.7190(12) 0.3006(4) 0.0186(17) Uani 1 1 d . . . C3 C 0.3676(2) 0.6601(12) 0.4421(5) 0.0184(16) Uani 1 1 d . . . C4 C 0.3571(2) 0.7227(11) 0.3569(5) 0.0186(16) Uani 1 1 d . . . C5 C 0.3912(3) 0.8084(13) 0.3202(5) 0.0273(19) Uani 1 1 d . . . H5 H 0.3850 0.8581 0.2642 0.033 Uiso 1 1 calc R . . C6 C 0.4334(3) 0.8181(15) 0.3675(6) 0.034(2) Uani 1 1 d . . . H6 H 0.4564 0.8717 0.3440 0.041 Uiso 1 1 calc R . . C7 C 0.4409(3) 0.7456(13) 0.4511(6) 0.031(2) Uani 1 1 d . . . H7 H 0.4696 0.7491 0.4830 0.038 Uiso 1 1 calc R . . C8 C 0.3888(3) 0.1808(13) 0.4974(6) 0.032(2) Uani 1 1 d . . . C9 C 0.4628(3) 0.6576(15) 0.8171(6) 0.039(2) Uani 1 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 Hg1 0.0293(3) 0.0491(3) 0.0247(3) -0.00385(15) -0.00784(15) 0.00043(16) Sr1 0.0186(4) 0.0188(4) 0.0153(4) -0.0003(3) 0.0003(3) -0.0010(3) N1 0.019(3) 0.038(4) 0.022(3) -0.006(3) 0.002(3) 0.002(3) N2 0.033(4) 0.034(5) 0.044(5) -0.011(4) 0.000(4) -0.007(4) N3 0.039(5) 0.100(9) 0.035(5) -0.013(5) -0.010(4) 0.013(5) O1 0.029(3) 0.037(4) 0.015(3) 0.001(2) 0.003(2) 0.002(3) O2 0.015(3) 0.044(4) 0.021(3) 0.002(3) 0.002(2) -0.002(3) O3 0.025(3) 0.014(3) 0.021(3) 0.001(2) -0.001(2) -0.001(2) O4 0.021(3) 0.021(3) 0.022(3) -0.004(2) -0.006(2) 0.008(2) O5 0.032(3) 0.031(4) 0.028(3) 0.000(2) 0.014(3) 0.004(3) O6 0.060(4) 0.019(3) 0.044(4) -0.004(3) 0.027(3) -0.010(3) O7 0.044(4) 0.030(4) 0.024(3) 0.000(3) 0.009(3) -0.001(3) S1 0.0484(16) 0.0460(16) 0.0518(16) -0.0080(13) -0.0194(13) 0.0169(13) S2 0.0372(14) 0.0592(18) 0.0391(13) -0.0134(13) -0.0079(11) 0.0184(13) C1 0.022(4) 0.013(4) 0.023(4) 0.002(3) 0.002(3) 0.002(3) C2 0.026(4) 0.023(4) 0.011(3) -0.002(3) 0.012(3) -0.003(4) C3 0.014(4) 0.022(4) 0.017(4) -0.003(3) -0.001(3) 0.003(3) C4 0.012(4) 0.021(4) 0.021(4) -0.003(3) -0.001(3) 0.003(3) C5 0.029(5) 0.028(5) 0.026(4) 0.007(4) 0.008(4) -0.001(4) C6 0.021(4) 0.045(6) 0.036(5) 0.003(4) 0.006(4) -0.005(4) C7 0.014(4) 0.034(5) 0.044(5) -0.001(4) 0.003(4) -0.005(4) C8 0.038(5) 0.023(5) 0.036(5) -0.007(4) 0.008(4) 0.002(4) C9 0.034(5) 0.050(6) 0.031(5) -0.005(4) 0.003(4) -0.007(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 N1 2.354(7) . ? Hg1 S2 2.442(3) . ? Hg1 S1 2.478(3) . ? Hg1 N3 2.530(9) 2_656 ? Hg1 O1 2.545(6) . ? Sr1 O6 2.558(6) . ? Sr1 O4 2.578(5) 1_545 ? Sr1 O3 2.584(5) . ? Sr1 O5 2.674(6) . ? Sr1 O4 2.694(5) 4_545 ? Sr1 O2 2.738(6) . ? Sr1 O3 2.753(5) 4_545 ? Sr1 O7 2.799(6) . ? Sr1 N2 2.801(8) . ? Sr1 C2 3.071(8) 4_545 ? N1 C7 1.339(11) . ? N1 C3 1.340(9) . ? N2 C8 1.182(11) . ? N3 C9 1.157(12) . ? N3 Hg1 2.530(9) 2_656 ? O1 C1 1.240(10) . ? O2 C1 1.276(9) . ? O3 C2 1.261(9) . ? O3 Sr1 2.753(5) 4 ? O4 C2 1.253(9) . ? O4 Sr1 2.578(5) 1_565 ? O4 Sr1 2.694(5) 4 ? O5 H5A 0.8529 . ? O5 H5B 0.8471 . ? O6 H6A 0.8476 . ? O6 H6B 0.8446 . ? O7 H7A 0.8487 . ? O7 H7B 0.8511 . ? S1 C8 1.657(10) . ? S2 C9 1.656(10) . ? C1 C3 1.518(11) . ? C2 C4 1.528(10) . ? C2 Sr1 3.071(8) 4 ? C3 C4 1.387(11) . ? C4 C5 1.414(11) . ? C5 C6 1.374(11) . ? C5 H5 0.9300 . ? C6 C7 1.385(13) . ? C6 H6 0.9300 . ? C7 H7 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 N1 Hg1 S2 120.62(18) . . ? N1 Hg1 S1 99.72(18) . . ? S2 Hg1 S1 137.60(11) . . ? N1 Hg1 N3 88.2(3) . 2_656 ? S2 Hg1 N3 94.2(2) . 2_656 ? S1 Hg1 N3 99.9(3) . 2_656 ? N1 Hg1 O1 67.4(2) . . ? S2 Hg1 O1 88.70(14) . . ? S1 Hg1 O1 95.85(15) . . ? N3 Hg1 O1 152.9(3) 2_656 . ? O6 Sr1 O4 67.43(19) . 1_545 ? O6 Sr1 O3 67.45(18) . . ? O4 Sr1 O3 134.45(17) 1_545 . ? O6 Sr1 O5 131.20(19) . . ? O4 Sr1 O5 64.44(17) 1_545 . ? O3 Sr1 O5 156.82(18) . . ? O6 Sr1 O4 77.87(19) . 4_545 ? O4 Sr1 O4 107.79(13) 1_545 4_545 ? O3 Sr1 O4 68.08(16) . 4_545 ? O5 Sr1 O4 124.31(18) . 4_545 ? O6 Sr1 O2 127.80(18) . . ? O4 Sr1 O2 147.53(17) 1_545 . ? O3 Sr1 O2 65.51(17) . . ? O5 Sr1 O2 91.58(17) . . ? O4 Sr1 O2 103.81(17) 4_545 . ? O6 Sr1 O3 85.57(18) . 4_545 ? O4 Sr1 O3 67.26(16) 1_545 4_545 ? O3 Sr1 O3 114.81(11) . 4_545 ? O5 Sr1 O3 83.37(18) . 4_545 ? O4 Sr1 O3 48.17(16) 4_545 4_545 ? O2 Sr1 O3 134.66(16) . 4_545 ? O6 Sr1 O7 144.3(2) . . ? O4 Sr1 O7 113.96(18) 1_545 . ? O3 Sr1 O7 106.07(18) . . ? O5 Sr1 O7 67.41(18) . . ? O4 Sr1 O7 67.69(17) 4_545 . ? O2 Sr1 O7 71.66(17) . . ? O3 Sr1 O7 64.82(17) 4_545 . ? O6 Sr1 N2 94.8(2) . . ? O4 Sr1 N2 81.8(2) 1_545 . ? O3 Sr1 N2 96.0(2) . . ? O5 Sr1 N2 71.2(2) . . ? O4 Sr1 N2 164.0(2) 4_545 . ? O2 Sr1 N2 69.3(2) . . ? O3 Sr1 N2 146.4(2) 4_545 . ? O7 Sr1 N2 120.9(2) . . ? O6 Sr1 C2 81.76(19) . 4_545 ? O4 Sr1 C2 88.01(18) 1_545 4_545 ? O3 Sr1 C2 91.53(18) . 4_545 ? O5 Sr1 C2 103.88(19) . 4_545 ? O4 Sr1 C2 23.97(18) 4_545 4_545 ? O2 Sr1 C2 120.33(18) . 4_545 ? O3 Sr1 C2 24.23(18) 4_545 4_545 ? O7 Sr1 C2 63.00(17) . 4_545 ? N2 Sr1 C2 169.8(2) . 4_545 ? O6 Sr1 Sr1 65.45(14) . 4_545 ? O4 Sr1 Sr1 35.26(11) 1_545 4_545 ? O3 Sr1 Sr1 123.50(12) . 4_545 ? O5 Sr1 Sr1 79.65(13) . 4_545 ? O4 Sr1 Sr1 73.11(12) 4_545 4_545 ? O2 Sr1 Sr1 166.08(12) . 4_545 ? O3 Sr1 Sr1 34.12(11) 4_545 4_545 ? O7 Sr1 Sr1 94.87(13) . 4_545 ? N2 Sr1 Sr1 117.05(16) . 4_545 ? C2 Sr1 Sr1 52.81(15) 4_545 4_545 ? O6 Sr1 Sr1 78.35(15) . 4 ? O4 Sr1 Sr1 134.63(11) 1_545 4 ? O3 Sr1 Sr1 36.70(12) . 4 ? O5 Sr1 Sr1 145.46(13) . 4 ? O4 Sr1 Sr1 33.53(12) 4_545 4 ? O2 Sr1 Sr1 77.49(12) . 4 ? O3 Sr1 Sr1 81.69(11) 4_545 4 ? O7 Sr1 Sr1 78.06(12) . 4 ? N2 Sr1 Sr1 131.37(17) . 4 ? C2 Sr1 Sr1 57.46(15) 4_545 4 ? Sr1 Sr1 Sr1 103.67(3) 4_545 4 ? C7 N1 C3 118.9(7) . . ? C7 N1 Hg1 121.6(6) . . ? C3 N1 Hg1 119.1(5) . . ? C8 N2 Sr1 164.8(7) . . ? C9 N3 Hg1 144.9(8) . 2_656 ? C1 O1 Hg1 113.3(5) . . ? C1 O2 Sr1 125.0(5) . . ? C2 O3 Sr1 127.2(4) . . ? C2 O3 Sr1 92.2(5) . 4 ? Sr1 O3 Sr1 109.17(19) . 4 ? C2 O4 Sr1 153.3(5) . 1_565 ? C2 O4 Sr1 95.1(4) . 4 ? Sr1 O4 Sr1 111.21(18) 1_565 4 ? Sr1 O5 H5A 113.1 . . ? Sr1 O5 H5B 115.1 . . ? H5A O5 H5B 110.1 . . ? Sr1 O6 H6A 114.7 . . ? Sr1 O6 H6B 116.2 . . ? H6A O6 H6B 112.2 . . ? Sr1 O7 H7A 111.6 . . ? Sr1 O7 H7B 112.0 . . ? H7A O7 H7B 110.4 . . ? C8 S1 Hg1 96.9(3) . . ? C9 S2 Hg1 99.5(3) . . ? O1 C1 O2 124.1(7) . . ? O1 C1 C3 119.1(7) . . ? O2 C1 C3 116.8(7) . . ? O4 C2 O3 124.4(7) . . ? O4 C2 C4 117.5(7) . . ? O3 C2 C4 118.1(7) . . ? O4 C2 Sr1 60.9(4) . 4 ? O3 C2 Sr1 63.6(4) . 4 ? C4 C2 Sr1 173.7(5) . 4 ? N1 C3 C4 122.3(7) . . ? N1 C3 C1 116.2(7) . . ? C4 C3 C1 121.5(7) . . ? C3 C4 C5 117.8(7) . . ? C3 C4 C2 125.4(7) . . ? C5 C4 C2 116.7(7) . . ? C6 C5 C4 119.8(7) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 118.1(8) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? N1 C7 C6 123.1(8) . . ? N1 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? N2 C8 S1 179.6(9) . . ? N3 C9 S2 177.0(9) . . ? 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 S2 Hg1 N1 C7 99.9(6) . . . . ? S1 Hg1 N1 C7 -93.7(6) . . . . ? N3 Hg1 N1 C7 6.0(7) 2_656 . . . ? O1 Hg1 N1 C7 173.9(7) . . . . ? S2 Hg1 N1 C3 -88.2(6) . . . . ? S1 Hg1 N1 C3 78.2(6) . . . . ? N3 Hg1 N1 C3 178.0(6) 2_656 . . . ? O1 Hg1 N1 C3 -14.1(5) . . . . ? O6 Sr1 N2 C8 164(3) . . . . ? O4 Sr1 N2 C8 -129(3) 1_545 . . . ? O3 Sr1 N2 C8 97(3) . . . . ? O5 Sr1 N2 C8 -63(3) . . . . ? O4 Sr1 N2 C8 103(3) 4_545 . . . ? O2 Sr1 N2 C8 36(3) . . . . ? O3 Sr1 N2 C8 -106(3) 4_545 . . . ? O7 Sr1 N2 C8 -16(3) . . . . ? C2 Sr1 N2 C8 -126(3) 4_545 . . . ? Sr1 Sr1 N2 C8 -131(3) 4_545 . . . ? Sr1 Sr1 N2 C8 86(3) 4 . . . ? N1 Hg1 O1 C1 19.4(5) . . . . ? S2 Hg1 O1 C1 143.5(5) . . . . ? S1 Hg1 O1 C1 -78.7(6) . . . . ? N3 Hg1 O1 C1 46.8(9) 2_656 . . . ? O6 Sr1 O2 C1 -64.7(7) . . . . ? O4 Sr1 O2 C1 43.6(7) 1_545 . . . ? O3 Sr1 O2 C1 -92.3(6) . . . . ? O5 Sr1 O2 C1 84.1(6) . . . . ? O4 Sr1 O2 C1 -150.0(6) 4_545 . . . ? O3 Sr1 O2 C1 166.3(5) 4_545 . . . ? O7 Sr1 O2 C1 149.6(6) . . . . ? N2 Sr1 O2 C1 14.9(6) . . . . ? C2 Sr1 O2 C1 -168.8(6) 4_545 . . . ? Sr1 Sr1 O2 C1 134.6(6) 4_545 . . . ? Sr1 Sr1 O2 C1 -129.0(6) 4 . . . ? O6 Sr1 O3 C2 -150.7(6) . . . . ? O4 Sr1 O3 C2 -142.4(6) 1_545 . . . ? O5 Sr1 O3 C2 -3.3(9) . . . . ? O4 Sr1 O3 C2 123.8(6) 4_545 . . . ? O2 Sr1 O3 C2 6.0(6) . . . . ? O3 Sr1 O3 C2 135.8(6) 4_545 . . . ? O7 Sr1 O3 C2 66.6(6) . . . . ? N2 Sr1 O3 C2 -58.0(6) . . . . ? C2 Sr1 O3 C2 128.9(6) 4_545 . . . ? Sr1 Sr1 O3 C2 173.9(5) 4_545 . . . ? Sr1 Sr1 O3 C2 108.3(6) 4 . . . ? O6 Sr1 O3 Sr1 101.0(2) . . . 4 ? O4 Sr1 O3 Sr1 109.3(2) 1_545 . . 4 ? O5 Sr1 O3 Sr1 -111.6(4) . . . 4 ? O4 Sr1 O3 Sr1 15.49(17) 4_545 . . 4 ? O2 Sr1 O3 Sr1 -102.3(2) . . . 4 ? O3 Sr1 O3 Sr1 27.53(19) 4_545 . . 4 ? O7 Sr1 O3 Sr1 -41.7(2) . . . 4 ? N2 Sr1 O3 Sr1 -166.3(2) . . . 4 ? C2 Sr1 O3 Sr1 20.6(2) 4_545 . . 4 ? Sr1 Sr1 O3 Sr1 65.6(2) 4_545 . . 4 ? N1 Hg1 S1 C8 -39.7(4) . . . . ? S2 Hg1 S1 C8 122.9(3) . . . . ? N3 Hg1 S1 C8 -129.5(4) 2_656 . . . ? O1 Hg1 S1 C8 28.4(4) . . . . ? N1 Hg1 S2 C9 -130.1(4) . . . . ? S1 Hg1 S2 C9 70.0(4) . . . . ? N3 Hg1 S2 C9 -39.7(5) 2_656 . . . ? O1 Hg1 S2 C9 167.2(4) . . . . ? Hg1 O1 C1 O2 158.3(6) . . . . ? Hg1 O1 C1 C3 -22.5(9) . . . . ? Sr1 O2 C1 O1 -109.3(8) . . . . ? Sr1 O2 C1 C3 71.5(8) . . . . ? Sr1 O4 C2 O3 -175.4(7) 1_565 . . . ? Sr1 O4 C2 O3 -4.1(8) 4 . . . ? Sr1 O4 C2 C4 1.8(15) 1_565 . . . ? Sr1 O4 C2 C4 173.1(5) 4 . . . ? Sr1 O4 C2 Sr1 -171.3(11) 1_565 . . 4 ? Sr1 O3 C2 O4 -112.2(7) . . . . ? Sr1 O3 C2 O4 4.0(7) 4 . . . ? Sr1 O3 C2 C4 70.6(8) . . . . ? Sr1 O3 C2 C4 -173.2(5) 4 . . . ? Sr1 O3 C2 Sr1 -116.2(5) . . . 4 ? C7 N1 C3 C4 0.4(12) . . . . ? Hg1 N1 C3 C4 -171.8(6) . . . . ? C7 N1 C3 C1 -178.7(7) . . . . ? Hg1 N1 C3 C1 9.1(9) . . . . ? O1 C1 C3 N1 10.6(11) . . . . ? O2 C1 C3 N1 -170.1(7) . . . . ? O1 C1 C3 C4 -168.5(7) . . . . ? O2 C1 C3 C4 10.8(11) . . . . ? N1 C3 C4 C5 -2.9(12) . . . . ? C1 C3 C4 C5 176.2(7) . . . . ? N1 C3 C4 C2 -178.7(7) . . . . ? C1 C3 C4 C2 0.3(12) . . . . ? O4 C2 C4 C3 97.3(9) . . . . ? O3 C2 C4 C3 -85.3(9) . . . . ? O4 C2 C4 C5 -78.5(9) . . . . ? O3 C2 C4 C5 98.8(9) . . . . ? C3 C4 C5 C6 3.3(12) . . . . ? C2 C4 C5 C6 179.5(8) . . . . ? C4 C5 C6 C7 -1.2(14) . . . . ? C3 N1 C7 C6 1.9(13) . . . . ? Hg1 N1 C7 C6 173.8(7) . . . . ? C5 C6 C7 N1 -1.4(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O2 0.85 2.36 3.197(8) 167.2 1_545 O5 H5B O2 0.85 1.98 2.748(8) 150.5 7_556 O5 H5B O1 0.85 2.56 3.308(9) 148.4 7_556 O6 H6A O1 0.85 2.15 2.918(8) 149.7 6_565 O6 H6B O7 0.84 2.08 2.847(9) 150.3 4_545 O7 H7A O1 0.85 2.11 2.948(9) 169.1 7_556 O7 H7B O5 0.85 1.96 2.795(8) 167.2 7_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.634 _refine_diff_density_min -2.017 _refine_diff_density_rms 0.239 # Attachment 'compound 5.cif' data_090512g _database_code_depnum_ccdc_archive 'CCDC 792174' #TrackingRef 'compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H9 Ba Hg N3 O7 S2' _chemical_formula_sum 'C9 H9 Ba Hg N3 O7 S2' _chemical_formula_weight 673.24 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' 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' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 30.645(3) _cell_length_b 7.0037(9) _cell_length_c 15.9747(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.309(2) _cell_angle_gamma 90.00 _cell_volume 3373.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1583 _cell_measurement_theta_min 2.986 _cell_measurement_theta_max 25.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 11.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4547 _exptl_absorpt_correction_T_max 0.7205 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8308 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2977 _reflns_number_gt 1957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART ' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _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^)+(0.0107P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000081(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2977 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _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 0.425778(14) 0.53732(6) 0.62516(3) 0.04437(15) Uani 1 1 d . . . Ba1 Ba 0.278935(17) 0.24019(7) 0.32957(3) 0.02386(15) Uani 1 1 d . . . N1 N 0.4117(2) 0.6774(10) 0.4901(4) 0.0315(19) Uani 1 1 d . . . N2 N 0.3647(3) 0.1856(11) 0.4479(5) 0.045(2) Uani 1 1 d . . . N3 N 0.4940(3) 0.6403(14) 0.8631(5) 0.064(3) Uani 1 1 d . . . O1 O 0.34386(17) 0.5599(8) 0.5682(3) 0.0323(15) Uani 1 1 d . . . O2 O 0.29766(17) 0.5543(7) 0.4434(3) 0.0278(14) Uani 1 1 d . . . O3 O 0.30376(17) 0.5685(7) 0.2617(3) 0.0256(14) Uani 1 1 d . . . O4 O 0.29278(18) 0.8689(7) 0.2979(4) 0.0301(15) Uani 1 1 d . . . O5 O 0.26821(18) -0.0247(7) 0.4568(4) 0.0364(16) Uani 1 1 d . . . H5A H 0.2738 -0.1430 0.4454 0.055 Uiso 1 1 d R . . H5B H 0.2434 -0.0178 0.4728 0.055 Uiso 1 1 d R . . O6 O 0.3073(2) 0.1816(8) 0.1787(4) 0.0486(19) Uani 1 1 d . . . H6A H 0.3102 0.2854 0.1509 0.073 Uiso 1 1 d R . . H6B H 0.2957 0.0904 0.1459 0.073 Uiso 1 1 d R . . O7 O 0.19820(19) 0.3078(7) 0.3972(4) 0.0388(16) Uani 1 1 d . . . H7A H 0.1837 0.2040 0.4017 0.058 Uiso 1 1 d R . . H7B H 0.2039 0.3671 0.4456 0.058 Uiso 1 1 d R . . S1 S 0.43437(9) 0.1958(4) 0.58880(18) 0.0554(8) Uani 1 1 d . . . S2 S 0.41319(9) 0.7047(4) 0.75251(18) 0.0573(8) Uani 1 1 d . . . C1 C 0.3346(3) 0.5868(10) 0.4888(6) 0.021(2) Uani 1 1 d . . . C2 C 0.3149(3) 0.7194(12) 0.3030(5) 0.020(2) Uani 1 1 d . . . C3 C 0.3701(3) 0.6677(11) 0.4422(5) 0.020(2) Uani 1 1 d . . . C4 C 0.3601(3) 0.7252(11) 0.3578(5) 0.022(2) Uani 1 1 d . . . C5 C 0.3951(3) 0.8045(11) 0.3231(6) 0.031(2) Uani 1 1 d . . . H5 H 0.3898 0.8490 0.2674 0.038 Uiso 1 1 calc R . . C6 C 0.4370(3) 0.8169(13) 0.3707(6) 0.040(3) Uani 1 1 d . . . H6 H 0.4602 0.8680 0.3473 0.048 Uiso 1 1 calc R . . C7 C 0.4444(3) 0.7519(12) 0.4544(6) 0.041(3) Uani 1 1 d . . . H7 H 0.4728 0.7603 0.4865 0.049 Uiso 1 1 calc R . . C8 C 0.3925(3) 0.1917(13) 0.5049(6) 0.036(2) Uani 1 1 d . . . C9 C 0.4614(3) 0.6660(14) 0.8161(6) 0.041(3) Uani 1 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 Hg1 0.0376(3) 0.0597(3) 0.0302(2) -0.0036(2) -0.00912(17) -0.0008(2) Ba1 0.0277(3) 0.0218(3) 0.0202(3) -0.0006(3) -0.0006(2) -0.0015(3) N1 0.034(5) 0.039(5) 0.017(4) -0.003(4) -0.007(4) -0.007(4) N2 0.050(6) 0.040(5) 0.041(6) -0.011(4) -0.003(4) -0.001(5) N3 0.041(6) 0.110(8) 0.033(6) -0.016(6) -0.014(4) 0.006(6) O1 0.025(4) 0.053(4) 0.018(4) 0.001(3) 0.003(3) 0.001(3) O2 0.021(3) 0.034(3) 0.026(4) 0.000(3) 0.000(3) -0.009(3) O3 0.032(4) 0.015(3) 0.027(4) -0.003(3) -0.004(3) -0.002(3) O4 0.033(4) 0.020(3) 0.034(4) -0.001(3) -0.005(3) 0.015(3) O5 0.034(4) 0.034(3) 0.044(4) 0.005(3) 0.016(3) -0.002(3) O6 0.074(5) 0.036(4) 0.040(4) -0.007(3) 0.020(4) -0.015(4) O7 0.055(4) 0.032(3) 0.030(4) 0.000(3) 0.011(3) -0.006(3) S1 0.0529(19) 0.0481(18) 0.055(2) -0.0028(15) -0.0180(14) 0.0100(15) S2 0.0463(18) 0.074(2) 0.0445(18) -0.0159(16) -0.0116(13) 0.0221(16) C1 0.029(6) 0.008(4) 0.027(6) -0.005(4) 0.005(4) 0.000(4) C2 0.018(5) 0.034(6) 0.009(5) 0.004(4) 0.011(4) -0.004(4) C3 0.020(5) 0.020(4) 0.017(5) -0.010(4) -0.002(4) -0.005(4) C4 0.023(5) 0.018(5) 0.024(5) -0.011(4) -0.002(4) -0.005(4) C5 0.033(6) 0.027(5) 0.037(6) 0.003(4) 0.012(5) 0.000(5) C6 0.025(6) 0.053(7) 0.043(7) 0.003(5) 0.008(5) -0.012(5) C7 0.019(5) 0.046(6) 0.055(8) -0.003(6) 0.003(5) 0.001(5) C8 0.033(6) 0.034(6) 0.041(7) -0.007(5) 0.008(5) 0.000(5) C9 0.047(7) 0.053(6) 0.026(6) -0.012(5) 0.009(5) 0.000(6) _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 N1 2.339(7) . ? Hg1 S2 2.438(3) . ? Hg1 S1 2.486(3) . ? Hg1 O1 2.518(5) . ? Hg1 N3 2.536(9) 2_656 ? Ba1 O4 2.697(5) 1_545 ? Ba1 O3 2.709(5) . ? Ba1 O6 2.736(6) . ? Ba1 O5 2.815(5) . ? Ba1 O2 2.847(5) . ? Ba1 O4 2.862(5) 4_545 ? Ba1 O7 2.911(6) . ? Ba1 O3 2.944(5) 4_545 ? Ba1 N2 2.973(8) . ? Ba1 C2 3.256(8) 4_545 ? N1 C7 1.344(10) . ? N1 C3 1.366(10) . ? N2 C8 1.132(11) . ? N3 C9 1.153(12) . ? N3 Hg1 2.536(9) 2_656 ? O1 C1 1.264(9) . ? O2 C1 1.251(9) . ? O3 C2 1.260(8) . ? O3 Ba1 2.944(5) 4 ? O4 C2 1.243(8) . ? O4 Ba1 2.697(5) 1_565 ? O4 Ba1 2.862(5) 4 ? O5 H5A 0.8715 . ? O5 H5B 0.8452 . ? O6 H6A 0.8650 . ? O6 H6B 0.8608 . ? O7 H7A 0.8621 . ? O7 H7B 0.8666 . ? S1 C8 1.682(10) . ? S2 C9 1.658(11) . ? C1 C3 1.532(11) . ? C2 C4 1.499(11) . ? C2 Ba1 3.256(8) 4 ? C3 C4 1.388(11) . ? C4 C5 1.408(10) . ? C5 C6 1.373(12) . ? C5 H5 0.9300 . ? C6 C7 1.392(12) . ? C6 H6 0.9300 . ? C7 H7 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 N1 Hg1 S2 122.52(18) . . ? N1 Hg1 S1 101.41(18) . . ? S2 Hg1 S1 134.16(10) . . ? N1 Hg1 O1 68.5(2) . . ? S2 Hg1 O1 88.56(14) . . ? S1 Hg1 O1 96.69(14) . . ? N1 Hg1 N3 88.0(3) . 2_656 ? S2 Hg1 N3 95.6(2) . 2_656 ? S1 Hg1 N3 98.6(2) . 2_656 ? O1 Hg1 N3 154.1(2) . 2_656 ? O4 Ba1 O3 132.74(17) 1_545 . ? O4 Ba1 O6 66.72(17) 1_545 . ? O3 Ba1 O6 67.57(16) . . ? O4 Ba1 O5 62.77(16) 1_545 . ? O3 Ba1 O5 157.85(16) . . ? O6 Ba1 O5 129.35(16) . . ? O4 Ba1 O2 147.60(16) 1_545 . ? O3 Ba1 O2 63.95(15) . . ? O6 Ba1 O2 128.27(15) . . ? O5 Ba1 O2 94.83(15) . . ? O4 Ba1 O4 107.28(13) 1_545 4_545 ? O3 Ba1 O4 71.49(15) . 4_545 ? O6 Ba1 O4 75.22(18) . 4_545 ? O5 Ba1 O4 123.21(16) . 4_545 ? O2 Ba1 O4 104.63(15) . 4_545 ? O4 Ba1 O7 113.53(16) 1_545 . ? O3 Ba1 O7 109.19(15) . . ? O6 Ba1 O7 140.97(18) . . ? O5 Ba1 O7 67.80(15) . . ? O2 Ba1 O7 74.01(15) . . ? O4 Ba1 O7 67.51(16) 4_545 . ? O4 Ba1 O3 70.36(15) 1_545 4_545 ? O3 Ba1 O3 115.27(10) . 4_545 ? O6 Ba1 O3 83.32(17) . 4_545 ? O5 Ba1 O3 83.51(15) . 4_545 ? O2 Ba1 O3 133.55(14) . 4_545 ? O4 Ba1 O3 45.01(14) 4_545 4_545 ? O7 Ba1 O3 62.40(15) . 4_545 ? O4 Ba1 N2 81.05(19) 1_545 . ? O3 Ba1 N2 94.83(19) . . ? O6 Ba1 N2 99.0(2) . . ? O5 Ba1 N2 70.1(2) . . ? O2 Ba1 N2 68.84(18) . . ? O4 Ba1 N2 166.28(19) 4_545 . ? O7 Ba1 N2 119.9(2) . . ? O3 Ba1 N2 147.82(18) 4_545 . ? O4 Ba1 C2 89.16(18) 1_545 4_545 ? O3 Ba1 C2 93.22(18) . 4_545 ? O6 Ba1 C2 78.64(18) . 4_545 ? O5 Ba1 C2 103.69(19) . 4_545 ? O2 Ba1 C2 120.26(17) . 4_545 ? O4 Ba1 C2 22.26(16) 4_545 4_545 ? O7 Ba1 C2 62.49(17) . 4_545 ? O3 Ba1 C2 22.75(15) 4_545 4_545 ? N2 Ba1 C2 170.0(2) . 4_545 ? O4 Ba1 Ba1 37.19(12) 1_545 4_545 ? O3 Ba1 Ba1 123.02(11) . 4_545 ? O6 Ba1 Ba1 62.67(12) . 4_545 ? O5 Ba1 Ba1 79.04(11) . 4_545 ? O2 Ba1 Ba1 167.47(11) . 4_545 ? O4 Ba1 Ba1 70.63(10) 4_545 4_545 ? O7 Ba1 Ba1 93.50(11) . 4_545 ? O3 Ba1 Ba1 35.46(10) 4_545 4_545 ? N2 Ba1 Ba1 118.23(15) . 4_545 ? C2 Ba1 Ba1 52.03(14) 4_545 4_545 ? O4 Ba1 Ba1 134.72(12) 1_545 4 ? O3 Ba1 Ba1 39.09(11) . 4 ? O6 Ba1 Ba1 76.96(12) . 4 ? O5 Ba1 Ba1 146.69(11) . 4 ? O2 Ba1 Ba1 76.91(11) . 4 ? O4 Ba1 Ba1 34.72(10) 4_545 4 ? O7 Ba1 Ba1 78.92(10) . 4 ? O3 Ba1 Ba1 79.68(10) 4_545 4 ? N2 Ba1 Ba1 132.30(15) . 4 ? C2 Ba1 Ba1 56.94(15) 4_545 4 ? Ba1 Ba1 Ba1 102.17(2) 4_545 4 ? C7 N1 C3 118.3(8) . . ? C7 N1 Hg1 121.7(6) . . ? C3 N1 Hg1 119.7(6) . . ? C8 N2 Ba1 163.7(8) . . ? C9 N3 Hg1 144.0(8) . 2_656 ? C1 O1 Hg1 113.7(5) . . ? C1 O2 Ba1 124.7(5) . . ? C2 O3 Ba1 124.8(5) . . ? C2 O3 Ba1 92.7(4) . 4 ? Ba1 O3 Ba1 105.45(17) . 4 ? C2 O4 Ba1 154.5(5) . 1_565 ? C2 O4 Ba1 97.0(5) . 4 ? Ba1 O4 Ba1 108.09(18) 1_565 4 ? Ba1 O5 H5A 115.0 . . ? Ba1 O5 H5B 114.1 . . ? H5A O5 H5B 109.8 . . ? Ba1 O6 H6A 113.9 . . ? Ba1 O6 H6B 119.0 . . ? H6A O6 H6B 112.4 . . ? Ba1 O7 H7A 112.3 . . ? Ba1 O7 H7B 111.1 . . ? H7A O7 H7B 110.8 . . ? C8 S1 Hg1 96.0(3) . . ? C9 S2 Hg1 100.1(3) . . ? O2 C1 O1 124.9(8) . . ? O2 C1 C3 115.7(8) . . ? O1 C1 C3 119.4(7) . . ? O4 C2 O3 125.3(8) . . ? O4 C2 C4 116.8(7) . . ? O3 C2 C4 117.7(7) . . ? O4 C2 Ba1 60.7(4) . 4 ? O3 C2 Ba1 64.6(4) . 4 ? C4 C2 Ba1 173.7(5) . 4 ? N1 C3 C4 123.5(8) . . ? N1 C3 C1 114.8(7) . . ? C4 C3 C1 121.7(7) . . ? C3 C4 C5 116.4(8) . . ? C3 C4 C2 125.5(7) . . ? C5 C4 C2 118.0(8) . . ? C6 C5 C4 120.8(9) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.0(9) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? N1 C7 C6 122.0(9) . . ? N1 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? N2 C8 S1 178.6(10) . . ? N3 C9 S2 177.2(10) . . ? 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 S2 Hg1 N1 C7 100.1(6) . . . . ? S1 Hg1 N1 C7 -93.6(6) . . . . ? O1 Hg1 N1 C7 173.7(7) . . . . ? N3 Hg1 N1 C7 4.8(7) 2_656 . . . ? S2 Hg1 N1 C3 -86.4(6) . . . . ? S1 Hg1 N1 C3 79.9(6) . . . . ? O1 Hg1 N1 C3 -12.9(6) . . . . ? N3 Hg1 N1 C3 178.2(6) 2_656 . . . ? O4 Ba1 N2 C8 -141(3) 1_545 . . . ? O3 Ba1 N2 C8 87(3) . . . . ? O6 Ba1 N2 C8 155(3) . . . . ? O5 Ba1 N2 C8 -76(3) . . . . ? O2 Ba1 N2 C8 27(3) . . . . ? O4 Ba1 N2 C8 91(3) 4_545 . . . ? O7 Ba1 N2 C8 -29(3) . . . . ? O3 Ba1 N2 C8 -113(3) 4_545 . . . ? Ba1 Ba1 N2 C8 -141(3) 4_545 . . . ? Ba1 Ba1 N2 C8 74(3) 4 . . . ? N1 Hg1 O1 C1 17.5(5) . . . . ? S2 Hg1 O1 C1 143.5(5) . . . . ? S1 Hg1 O1 C1 -82.2(5) . . . . ? N3 Hg1 O1 C1 43.6(8) 2_656 . . . ? O4 Ba1 O2 C1 36.9(8) 1_545 . . . ? O3 Ba1 O2 C1 -92.9(6) . . . . ? O6 Ba1 O2 C1 -70.8(7) . . . . ? O5 Ba1 O2 C1 80.5(6) . . . . ? O4 Ba1 O2 C1 -153.3(6) 4_545 . . . ? O7 Ba1 O2 C1 145.7(7) . . . . ? O3 Ba1 O2 C1 166.1(6) 4_545 . . . ? N2 Ba1 O2 C1 14.0(6) . . . . ? C2 Ba1 O2 C1 -170.6(6) 4_545 . . . ? Ba1 Ba1 O2 C1 140.6(6) 4_545 . . . ? Ba1 Ba1 O2 C1 -132.2(6) 4 . . . ? O4 Ba1 O3 C2 -143.0(6) 1_545 . . . ? O6 Ba1 O3 C2 -158.5(6) . . . . ? O5 Ba1 O3 C2 -14.9(8) . . . . ? O2 Ba1 O3 C2 2.9(6) . . . . ? O4 Ba1 O3 C2 120.3(6) 4_545 . . . ? O7 Ba1 O3 C2 63.2(6) . . . . ? O3 Ba1 O3 C2 131.0(6) 4_545 . . . ? N2 Ba1 O3 C2 -60.7(6) . . . . ? C2 Ba1 O3 C2 125.2(6) 4_545 . . . ? Ba1 Ba1 O3 C2 170.9(5) 4_545 . . . ? Ba1 Ba1 O3 C2 104.5(6) 4 . . . ? O4 Ba1 O3 Ba1 112.5(2) 1_545 . . 4 ? O6 Ba1 O3 Ba1 96.9(2) . . . 4 ? O5 Ba1 O3 Ba1 -119.4(4) . . . 4 ? O2 Ba1 O3 Ba1 -101.66(19) . . . 4 ? O4 Ba1 O3 Ba1 15.74(15) 4_545 . . 4 ? O7 Ba1 O3 Ba1 -41.3(2) . . . 4 ? O3 Ba1 O3 Ba1 26.47(17) 4_545 . . 4 ? N2 Ba1 O3 Ba1 -165.3(2) . . . 4 ? C2 Ba1 O3 Ba1 20.6(2) 4_545 . . 4 ? Ba1 Ba1 O3 Ba1 66.35(18) 4_545 . . 4 ? N1 Hg1 S1 C8 -40.9(4) . . . . ? S2 Hg1 S1 C8 122.9(3) . . . . ? O1 Hg1 S1 C8 28.4(4) . . . . ? N3 Hg1 S1 C8 -130.6(4) 2_656 . . . ? N1 Hg1 S2 C9 -130.2(4) . . . . ? S1 Hg1 S2 C9 68.7(4) . . . . ? O1 Hg1 S2 C9 166.6(4) . . . . ? N3 Hg1 S2 C9 -39.0(5) 2_656 . . . ? Ba1 O2 C1 O1 -105.9(8) . . . . ? Ba1 O2 C1 C3 75.0(8) . . . . ? Hg1 O1 C1 O2 160.6(6) . . . . ? Hg1 O1 C1 C3 -20.3(8) . . . . ? Ba1 O4 C2 O3 -171.6(7) 1_565 . . . ? Ba1 O4 C2 O3 -1.6(8) 4 . . . ? Ba1 O4 C2 C4 3.4(16) 1_565 . . . ? Ba1 O4 C2 C4 173.4(6) 4 . . . ? Ba1 O4 C2 Ba1 -170.0(12) 1_565 . . 4 ? Ba1 O3 C2 O4 -109.4(7) . . . . ? Ba1 O3 C2 O4 1.5(8) 4 . . . ? Ba1 O3 C2 C4 75.7(8) . . . . ? Ba1 O3 C2 C4 -173.4(6) 4 . . . ? Ba1 O3 C2 Ba1 -110.9(4) . . . 4 ? C7 N1 C3 C4 2.1(13) . . . . ? Hg1 N1 C3 C4 -171.6(6) . . . . ? C7 N1 C3 C1 -178.1(7) . . . . ? Hg1 N1 C3 C1 8.2(9) . . . . ? O2 C1 C3 N1 -171.3(7) . . . . ? O1 C1 C3 N1 9.4(11) . . . . ? O2 C1 C3 C4 8.5(11) . . . . ? O1 C1 C3 C4 -170.7(7) . . . . ? N1 C3 C4 C5 -2.8(12) . . . . ? C1 C3 C4 C5 177.4(7) . . . . ? N1 C3 C4 C2 -179.3(8) . . . . ? C1 C3 C4 C2 0.9(12) . . . . ? O4 C2 C4 C3 95.5(10) . . . . ? O3 C2 C4 C3 -89.1(10) . . . . ? O4 C2 C4 C5 -80.9(9) . . . . ? O3 C2 C4 C5 94.5(9) . . . . ? C3 C4 C5 C6 2.1(12) . . . . ? C2 C4 C5 C6 178.8(8) . . . . ? C4 C5 C6 C7 -0.8(14) . . . . ? C3 N1 C7 C6 -0.6(13) . . . . ? Hg1 N1 C7 C6 173.0(7) . . . . ? C5 C6 C7 N1 0.0(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O2 0.87 2.25 3.102(7) 167.7 1_545 O5 H5B O2 0.85 2.01 2.794(7) 153.8 7_556 O5 H5B O1 0.85 2.65 3.394(8) 147.1 7_556 O6 H6A O1 0.87 2.11 2.891(8) 149.2 6_565 O6 H6B O7 0.86 2.11 2.877(7) 147.3 4_545 O7 H7A O1 0.86 2.12 2.976(8) 170.2 7_556 O7 H7B O5 0.87 1.98 2.819(8) 163.8 7_556 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.984 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.180