# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_10 _database_code_depnum_ccdc_archive 'CCDC 892204' #TrackingRef '10.cif' # L1107 _audit_creation_method SHELXL-97 _audit_creation_date 3-Jun-2011 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C26 H24 Hg2 N16' _chemical_formula_sum 'C26 H24 Hg2 N16' _chemical_formula_weight 961.58 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 26 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 24 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Hg Hg 2 -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 16 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6753(2) _cell_length_b 10.3614(3) _cell_length_c 11.5961(4) _cell_angle_alpha 71.528(3) _cell_angle_beta 73.693(3) _cell_angle_gamma 78.321(3) _cell_volume 724.43(4) _cell_formula_units_Z 1 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 10757 _cell_measurement_theta_min 2.4011 _cell_measurement_theta_max 30.3993 _exptl_crystal_description tablet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 10.656 _exptl_absorpt_correction_T_min 0.280 _exptl_absorpt_correction_T_max 0.721 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. CrysAlisPro, Version 1.171.34.49 (Agilent Technologies, 2011) (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; Solvent used: MeCN Cooling Device: Oxford Instruments Cryojet XL Crystal mount: on a glass fibre Frames collected: 934 Seconds exposure per frame: 10.0 Degrees rotation per frame: 1.0 Crystal-detector distance (mm): 55.0 Client: Tushar Basu BAul Sample code: TSBB-309 (L1107) ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova, dual radiation diffractometer' _diffrn_detector_area_resol_mean 10.3801 _diffrn_detector 'Atlas CCD camera on \k goniostat' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 18011 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.47 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 4055 _reflns_number_gt 3767 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrysAlisPro, Version 1.171.34.49 (Agilent Technologies, 2011)' _computing_cell_refinement 'CrysAlisPro, Version 1.171.34.49 (Agilent Technologies, 2011)' _computing_data_reduction 'CrysAlisPro, Version 1.171.34.49 (Agilent Technologies, 2011)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.4840P] 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 4055 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0424 _refine_ls_wR_factor_gt 0.0408 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.015 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.125 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 0.272751(17) 0.393777(10) 0.016984(9) 0.02246(4) Uani 1 1 d . . . N1 N 0.2827(4) 0.3338(2) -0.1534(2) 0.0200(5) Uani 1 1 d . . . N2 N 0.2883(3) 0.1393(2) 0.0722(2) 0.0205(5) Uani 1 1 d . . . N3 N 0.3692(4) 0.4793(3) 0.1338(2) 0.0319(6) Uani 1 1 d . . . N4 N 0.2904(4) 0.4572(3) 0.2430(2) 0.0289(6) Uani 1 1 d . . . N5 N 0.2258(6) 0.4384(4) 0.3486(3) 0.0582(10) Uani 1 1 d . . . N6 N -0.1057(4) 0.3705(2) 0.0980(2) 0.0243(5) Uani 1 1 d . . . N7 N -0.1625(4) 0.2787(2) 0.0782(2) 0.0255(5) Uani 1 1 d . . . N8 N -0.2126(4) 0.1893(3) 0.0583(3) 0.0397(7) Uani 1 1 d . . . C1 C 0.2643(4) 0.2022(3) -0.1401(3) 0.0192(5) Uani 1 1 d . . . C2 C 0.2463(4) 0.1620(3) -0.2397(3) 0.0244(6) Uani 1 1 d . . . H2 H 0.2333 0.0692 -0.2295 0.029 Uiso 1 1 calc R . . C3 C 0.2474(5) 0.2580(3) -0.3535(3) 0.0277(6) Uani 1 1 d . . . H3 H 0.2337 0.2321 -0.4223 0.033 Uiso 1 1 calc R . . C4 C 0.2687(5) 0.3924(3) -0.3668(3) 0.0288(6) Uani 1 1 d . . . H4 H 0.2728 0.4599 -0.4450 0.035 Uiso 1 1 calc R . . C5 C 0.2839(5) 0.4263(3) -0.2636(3) 0.0262(6) Uani 1 1 d . . . H5 H 0.2957 0.5188 -0.2717 0.031 Uiso 1 1 calc R . . C6 C 0.2623(4) 0.1038(3) -0.0177(3) 0.0214(6) Uani 1 1 d . . . H6 H 0.2413 0.0118 -0.0049 0.026 Uiso 1 1 calc R . . C7 C 0.2782(4) 0.0486(3) 0.1938(3) 0.0225(6) Uani 1 1 d . . . C8 C 0.2313(5) -0.0867(3) 0.2294(3) 0.0310(7) Uani 1 1 d . . . H8 H 0.2083 -0.1240 0.1698 0.037 Uiso 1 1 calc R . . C9 C 0.2191(5) -0.1652(3) 0.3519(3) 0.0368(8) Uani 1 1 d . . . H9 H 0.1880 -0.2568 0.3751 0.044 Uiso 1 1 calc R . . C10 C 0.2505(5) -0.1146(3) 0.4419(3) 0.0346(7) Uani 1 1 d . . . C11 C 0.2992(6) 0.0192(3) 0.4049(3) 0.0363(8) Uani 1 1 d . . . H11 H 0.3233 0.0562 0.4643 0.044 Uiso 1 1 calc R . . C12 C 0.3130(5) 0.0990(3) 0.2827(3) 0.0296(7) Uani 1 1 d . . . H12 H 0.3470 0.1899 0.2595 0.036 Uiso 1 1 calc R . . C13 C 0.2376(6) -0.2024(4) 0.5749(4) 0.0507(11) Uani 1 1 d . . . H13A H 0.1330 -0.2657 0.5974 0.076 Uiso 1 1 calc R . . H13B H 0.1962 -0.1436 0.6315 0.076 Uiso 1 1 calc R . . H13C H 0.3753 -0.2550 0.5823 0.076 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 0.03623(7) 0.01755(6) 0.01901(6) -0.00587(4) -0.01001(5) -0.00893(4) N1 0.0261(12) 0.0183(11) 0.0191(11) -0.0075(9) -0.0066(10) -0.0048(9) N2 0.0204(11) 0.0157(10) 0.0243(12) -0.0041(9) -0.0061(10) -0.0008(8) N3 0.0456(16) 0.0384(15) 0.0220(13) -0.0129(11) -0.0074(12) -0.0208(13) N4 0.0344(14) 0.0308(14) 0.0286(15) -0.0136(11) -0.0142(12) -0.0014(11) N5 0.067(2) 0.087(3) 0.0285(17) -0.0240(18) -0.0090(16) -0.016(2) N6 0.0295(13) 0.0160(11) 0.0299(13) -0.0080(10) -0.0074(11) -0.0047(9) N7 0.0244(12) 0.0184(11) 0.0320(14) -0.0080(10) -0.0024(11) -0.0033(9) N8 0.0318(14) 0.0283(14) 0.065(2) -0.0198(14) -0.0069(14) -0.0125(12) C1 0.0176(12) 0.0164(12) 0.0271(14) -0.0110(11) -0.0065(11) 0.0003(10) C2 0.0237(14) 0.0229(14) 0.0322(16) -0.0166(12) -0.0059(12) -0.0018(11) C3 0.0298(15) 0.0370(17) 0.0244(15) -0.0184(13) -0.0089(12) -0.0025(13) C4 0.0368(17) 0.0307(16) 0.0205(15) -0.0085(12) -0.0093(13) -0.0018(13) C5 0.0406(17) 0.0185(13) 0.0209(14) -0.0047(11) -0.0083(13) -0.0062(12) C6 0.0237(13) 0.0146(12) 0.0271(15) -0.0071(11) -0.0058(12) -0.0027(10) C7 0.0199(13) 0.0191(13) 0.0250(15) -0.0036(11) -0.0041(11) -0.0007(10) C8 0.0296(16) 0.0256(15) 0.0390(18) -0.0018(13) -0.0148(14) -0.0078(12) C9 0.0280(16) 0.0283(16) 0.046(2) 0.0101(15) -0.0130(15) -0.0113(13) C10 0.0265(15) 0.0330(17) 0.0288(17) 0.0038(14) -0.0010(13) 0.0028(13) C11 0.050(2) 0.0290(16) 0.0235(16) -0.0075(13) -0.0084(15) 0.0082(14) C12 0.0418(18) 0.0195(14) 0.0235(15) -0.0045(12) -0.0074(13) 0.0024(12) C13 0.046(2) 0.049(2) 0.035(2) 0.0101(18) -0.0049(17) 0.0025(18) _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 N3 2.125(2) . ? Hg1 N1 2.232(2) . ? Hg1 N6 2.468(2) . ? Hg1 N2 2.496(2) . ? Hg1 N6 2.579(2) 2_565 ? Hg1 N3 2.823(3) 2_665 ? N1 C5 1.332(4) . ? N1 C1 1.350(3) . ? N2 C6 1.274(3) . ? N2 C7 1.417(4) . ? N3 N4 1.193(4) . ? N4 N5 1.144(4) . ? N6 N7 1.198(3) . ? N7 N8 1.152(3) . ? C1 C2 1.388(4) . ? C1 C6 1.461(4) . ? C2 C3 1.377(4) . ? C2 H2 0.9500 . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.383(4) . ? C7 C8 1.404(4) . ? C8 C9 1.385(5) . ? C8 H8 0.9500 . ? C9 C10 1.387(5) . ? C9 H9 0.9500 . ? C10 C11 1.393(5) . ? C10 C13 1.511(5) . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Hg1 N1 158.28(10) . . ? N3 Hg1 N6 108.70(9) . . ? N1 Hg1 N6 91.82(8) . . ? N3 Hg1 N2 118.41(9) . . ? N1 Hg1 N2 71.05(8) . . ? N6 Hg1 N2 80.13(7) . . ? N3 Hg1 N6 92.44(9) . 2_565 ? N1 Hg1 N6 84.57(8) . 2_565 ? N6 Hg1 N6 78.57(8) . 2_565 ? N2 Hg1 N6 146.88(8) . 2_565 ? N3 Hg1 N3 74.50(10) . 2_665 ? N1 Hg1 N3 83.85(7) . 2_665 ? N6 Hg1 N3 156.52(8) . 2_665 ? N2 Hg1 N3 119.61(8) . 2_665 ? N6 Hg1 N3 78.06(8) 2_565 2_665 ? C5 N1 C1 119.6(2) . . ? C5 N1 Hg1 121.81(18) . . ? C1 N1 Hg1 118.24(18) . . ? C6 N2 C7 122.8(2) . . ? C6 N2 Hg1 110.31(18) . . ? C7 N2 Hg1 125.40(18) . . ? N4 N3 Hg1 121.8(2) . . ? N4 N3 Hg1 132.2(2) . 2_665 ? Hg1 N3 Hg1 105.50(10) . 2_665 ? N5 N4 N3 175.7(3) . . ? N7 N6 Hg1 115.49(19) . . ? N7 N6 Hg1 111.42(19) . 2_565 ? Hg1 N6 Hg1 101.43(8) . 2_565 ? N8 N7 N6 178.5(3) . . ? N1 C1 C2 120.9(3) . . ? N1 C1 C6 118.1(2) . . ? C2 C1 C6 121.0(2) . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.4(3) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 122.3(3) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C1 121.1(2) . . ? N2 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C12 C7 C8 118.7(3) . . ? C12 C7 N2 117.2(3) . . ? C8 C7 N2 124.1(3) . . ? C9 C8 C7 119.4(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 122.2(3) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C9 C10 C11 117.7(3) . . ? C9 C10 C13 121.3(3) . . ? C11 C10 C13 121.0(3) . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C7 C12 C11 121.1(3) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 N3 Hg1 N1 C5 -58.9(4) . . . . ? N6 Hg1 N1 C5 102.3(2) . . . . ? N2 Hg1 N1 C5 -178.8(2) . . . . ? N6 Hg1 N1 C5 24.0(2) 2_565 . . . ? N3 Hg1 N1 C5 -54.5(2) 2_665 . . . ? N3 Hg1 N1 C1 128.2(3) . . . . ? N6 Hg1 N1 C1 -70.5(2) . . . . ? N2 Hg1 N1 C1 8.36(18) . . . . ? N6 Hg1 N1 C1 -148.9(2) 2_565 . . . ? N3 Hg1 N1 C1 132.6(2) 2_665 . . . ? N3 Hg1 N2 C6 -168.34(18) . . . . ? N1 Hg1 N2 C6 -9.74(18) . . . . ? N6 Hg1 N2 C6 85.65(19) . . . . ? N6 Hg1 N2 C6 35.1(3) 2_565 . . . ? N3 Hg1 N2 C6 -80.75(19) 2_665 . . . ? N3 Hg1 N2 C7 25.3(2) . . . . ? N1 Hg1 N2 C7 -176.1(2) . . . . ? N6 Hg1 N2 C7 -80.7(2) . . . . ? N6 Hg1 N2 C7 -131.3(2) 2_565 . . . ? N3 Hg1 N2 C7 112.9(2) 2_665 . . . ? N1 Hg1 N3 N4 -167.9(2) . . . . ? N6 Hg1 N3 N4 31.9(3) . . . . ? N2 Hg1 N3 N4 -56.8(3) . . . . ? N6 Hg1 N3 N4 110.7(3) 2_565 . . . ? N3 Hg1 N3 N4 -172.4(3) 2_665 . . . ? N1 Hg1 N3 Hg1 4.5(3) . . . 2_665 ? N6 Hg1 N3 Hg1 -155.65(9) . . . 2_665 ? N2 Hg1 N3 Hg1 115.65(9) . . . 2_665 ? N6 Hg1 N3 Hg1 -76.89(10) 2_565 . . 2_665 ? N3 Hg1 N3 Hg1 0.0 2_665 . . 2_665 ? N3 Hg1 N6 N7 -150.7(2) . . . . ? N1 Hg1 N6 N7 36.5(2) . . . . ? N2 Hg1 N6 N7 -33.9(2) . . . . ? N6 Hg1 N6 N7 120.6(3) 2_565 . . . ? N3 Hg1 N6 N7 115.2(2) 2_665 . . . ? N3 Hg1 N6 Hg1 88.71(11) . . . 2_565 ? N1 Hg1 N6 Hg1 -84.08(9) . . . 2_565 ? N2 Hg1 N6 Hg1 -154.48(9) . . . 2_565 ? N6 Hg1 N6 Hg1 0.0 2_565 . . 2_565 ? N3 Hg1 N6 Hg1 -5.4(2) 2_665 . . 2_565 ? C5 N1 C1 C2 -0.1(4) . . . . ? Hg1 N1 C1 C2 172.9(2) . . . . ? C5 N1 C1 C6 -179.7(3) . . . . ? Hg1 N1 C1 C6 -6.6(3) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? C6 C1 C2 C3 179.6(3) . . . . ? C1 C2 C3 C4 0.7(4) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? C1 N1 C5 C4 -0.6(4) . . . . ? Hg1 N1 C5 C4 -173.3(2) . . . . ? C3 C4 C5 N1 1.3(5) . . . . ? C7 N2 C6 C1 177.1(2) . . . . ? Hg1 N2 C6 C1 10.3(3) . . . . ? N1 C1 C6 N2 -3.6(4) . . . . ? C2 C1 C6 N2 176.8(3) . . . . ? C6 N2 C7 C12 178.8(3) . . . . ? Hg1 N2 C7 C12 -16.4(3) . . . . ? C6 N2 C7 C8 -2.4(4) . . . . ? Hg1 N2 C7 C8 162.3(2) . . . . ? C12 C7 C8 C9 0.7(4) . . . . ? N2 C7 C8 C9 -178.0(3) . . . . ? C7 C8 C9 C10 0.3(5) . . . . ? C8 C9 C10 C11 -1.1(5) . . . . ? C8 C9 C10 C13 -179.6(3) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C13 C10 C11 C12 179.3(3) . . . . ? C8 C7 C12 C11 -1.0(5) . . . . ? N2 C7 C12 C11 177.8(3) . . . . ? C10 C11 C12 C7 0.2(5) . . . . ? _iucr_refine_instructions_details ; TITL TSBB-309 (L1107) CELL 0.71073 6.67529 10.36136 11.59614 71.5275 73.6934 78.3208 ZERR 2 0.00021 0.00029 0.00041 0.0028 0.0029 0.0025 LATT 1 SFAC C H HG N UNIT 26 24 2 16 MERG 2 TEMP -113 L.S. 4 BOND $H CONF ACTA FMAP 2 BIND Hg1 N3_$1 BIND N3 HG1_$1 EQIV $1 1-x,1-y,-z PLAN 10 WGHT 0.016500 0.484000 FVAR 3.53728 HG1 3 0.272751 0.393777 0.016984 11.00000 0.03623 0.01755 = 0.01901 -0.00587 -0.01001 -0.00893 N1 4 0.282677 0.333846 -0.153409 11.00000 0.02611 0.01833 = 0.01906 -0.00754 -0.00661 -0.00476 N2 4 0.288331 0.139277 0.072211 11.00000 0.02038 0.01566 = 0.02428 -0.00412 -0.00612 -0.00084 N3 4 0.369191 0.479285 0.133776 11.00000 0.04557 0.03840 = 0.02197 -0.01295 -0.00742 -0.02080 N4 4 0.290365 0.457234 0.242961 11.00000 0.03438 0.03077 = 0.02856 -0.01359 -0.01425 -0.00143 N5 4 0.225784 0.438380 0.348560 11.00000 0.06686 0.08651 = 0.02854 -0.02398 -0.00899 -0.01565 N6 4 -0.105705 0.370548 0.098017 11.00000 0.02946 0.01603 = 0.02995 -0.00804 -0.00742 -0.00474 N7 4 -0.162462 0.278730 0.078192 11.00000 0.02439 0.01842 = 0.03203 -0.00804 -0.00238 -0.00328 N8 4 -0.212601 0.189326 0.058338 11.00000 0.03182 0.02826 = 0.06507 -0.01979 -0.00688 -0.01252 C1 1 0.264294 0.202238 -0.140119 11.00000 0.01760 0.01643 = 0.02706 -0.01104 -0.00651 0.00030 C2 1 0.246290 0.161998 -0.239728 11.00000 0.02371 0.02285 = 0.03217 -0.01660 -0.00586 -0.00175 AFIX 43 H2 2 0.233319 0.069166 -0.229517 11.00000 -1.20000 AFIX 0 C3 1 0.247418 0.257977 -0.353497 11.00000 0.02977 0.03699 = 0.02437 -0.01839 -0.00893 -0.00250 AFIX 43 H3 2 0.233701 0.232145 -0.422283 11.00000 -1.20000 AFIX 0 C4 1 0.268709 0.392445 -0.366824 11.00000 0.03680 0.03067 = 0.02051 -0.00846 -0.00931 -0.00183 AFIX 43 H4 2 0.272780 0.459855 -0.444969 11.00000 -1.20000 AFIX 0 C5 1 0.283916 0.426318 -0.263645 11.00000 0.04059 0.01851 = 0.02093 -0.00472 -0.00834 -0.00620 AFIX 43 H5 2 0.295654 0.518796 -0.271716 11.00000 -1.20000 AFIX 0 C6 1 0.262331 0.103788 -0.017684 11.00000 0.02373 0.01457 = 0.02706 -0.00707 -0.00584 -0.00267 AFIX 43 H6 2 0.241329 0.011824 -0.004901 11.00000 -1.20000 AFIX 0 C7 1 0.278167 0.048622 0.193841 11.00000 0.01992 0.01915 = 0.02497 -0.00361 -0.00413 -0.00067 C8 1 0.231346 -0.086672 0.229362 11.00000 0.02956 0.02562 = 0.03901 -0.00178 -0.01477 -0.00779 AFIX 43 H8 2 0.208304 -0.123996 0.169839 11.00000 -1.20000 AFIX 0 C9 1 0.219056 -0.165205 0.351920 11.00000 0.02801 0.02835 = 0.04562 0.01007 -0.01296 -0.01130 AFIX 43 H9 2 0.188046 -0.256804 0.375105 11.00000 -1.20000 AFIX 0 C10 1 0.250500 -0.114616 0.441945 11.00000 0.02648 0.03302 = 0.02877 0.00381 -0.00102 0.00280 C11 1 0.299229 0.019200 0.404858 11.00000 0.05045 0.02900 = 0.02348 -0.00748 -0.00840 0.00817 AFIX 43 H11 2 0.323334 0.056215 0.464280 11.00000 -1.20000 AFIX 0 C12 1 0.313031 0.098990 0.282714 11.00000 0.04179 0.01947 = 0.02350 -0.00448 -0.00736 0.00244 AFIX 43 H12 2 0.347018 0.189889 0.259485 11.00000 -1.20000 AFIX 0 C13 1 0.237599 -0.202437 0.574948 11.00000 0.04627 0.04855 = 0.03481 0.01013 -0.00491 0.00250 AFIX 137 H13A 2 0.132972 -0.265696 0.597356 11.00000 -1.50000 H13B 2 0.196174 -0.143614 0.631454 11.00000 -1.50000 H13C 2 0.375282 -0.254976 0.582317 11.00000 -1.50000 HKLF 4 REM TSBB-309 (L1107) REM R1 = 0.0204 for 3767 Fo > 4sig(Fo) and 0.0239 for all 4055 data REM 200 parameters refined using 0 restraints END WGHT 0.0165 0.4840 REM Highest difference peak 1.015, deepest hole -0.752, 1-sigma level 0.125 Q1 1 -0.3540 0.3925 0.0171 11.00000 0.05 1.01 Q2 1 -0.0363 0.3980 0.0161 11.00000 0.05 0.93 Q3 1 0.4321 0.4189 -0.0294 11.00000 0.05 0.88 Q4 1 0.4184 0.3870 0.0057 11.00000 0.05 0.83 Q5 1 0.1629 0.3925 0.0797 11.00000 0.05 0.82 Q6 1 0.1160 0.4508 0.0206 11.00000 0.05 0.71 Q7 1 0.1538 0.4968 -0.0015 11.00000 0.05 0.68 Q8 1 0.3364 0.4954 -0.0415 11.00000 0.05 0.65 Q9 1 0.1994 0.2958 0.0775 11.00000 0.05 0.65 Q10 1 0.0000 0.5000 0.0000 10.50000 0.05 0.64 ; data_2 _database_code_depnum_ccdc_archive 'CCDC 892205' #TrackingRef '2.cif' # L1021 _vrf_DIFMX01_2 ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 _refine_diff_density_max given = 9.547 Test value = 8.000 RESPONSE: The structure has a particularly heavy atom, Hg and large residuals are often encountered. In this particular circumstance, the residual electron density peaks of 9.55 and -1.36 e/A3 were located 1.08 and 0.59 A, respectively from the Hg atom, indicating ripples rather than real chemical species. The next largest residual electron denisty peak was 1.00 e/A3. The analytical absorption correction applied was based on the face-indexing of the crystal. Alternate absorption corrections, e.g. SADABS, were explored but the large residual remained. A refinement was attempted in P1 but, the ripple persisted. No evidence for twinning was found. The authors conclude that this feature of the structure is an artefact of the sample and that no chemical significance can be ascribed to it. ; _vrf_PLAT094_2 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 7.04 RESPONSE: See detailed response to "DIFMX01" ; _vrf_PLAT097_2 ; PROBLEM: Large Reported Max. (Positive) Residual Density 9.55 eA-3 RESPONSE: See detailed response to "DIFMX01" ; _vrf_DIFMX02_2 ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. RESPONSE: See detailed response to "DIFMX01" ; _audit_creation_method SHELXL-97 _audit_creation_date 22-Dec-2010 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C24 H20 Br4 Hg2 N4' _chemical_formula_sum 'C24 H20 Br4 Hg2 N4' _chemical_formula_weight 1085.06 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 24 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 20 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Br Br 4 -0.2901 2.4595 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Hg Hg 2 -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 4 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.03383(16) _cell_length_b 8.9441(2) _cell_length_c 10.0091(3) _cell_angle_alpha 106.595(3) _cell_angle_beta 100.732(2) _cell_angle_gamma 99.5612(19) _cell_volume 658.57(3) _cell_formula_units_Z 1 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 12264 _cell_measurement_theta_min 2.1868 _cell_measurement_theta_max 32.4787 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 17.694 _exptl_absorpt_correction_T_min 0.145 _exptl_absorpt_correction_T_max 0.358 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. CrysAlisPro, Version 1.171.34.40 (Agilent Technologies, 2010) (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; Solvent used: acetonitrile Cooling Device: Oxford Instruments Cryojet XL Crystal mount: on a glass fibre Frames collected: 1034 Seconds exposure per frame: 8.0 Degrees rotation per frame: 1.0 Crystal-detector distance (mm): 55.0 Client: Tushar Basu Baul Sample code: TSBB-297 (L1021) ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova, dual radiation diffractometer' _diffrn_detector_area_resol_mean 10.3801 _diffrn_detector 'Atlas CCD camera on \k goniostat' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 20442 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 32.55 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 4394 _reflns_number_gt 4057 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrysAlisPro, Version 1.171.34.40 (Agilent Technologies, 2010)' _computing_cell_refinement 'CrysAlisPro, Version 1.171.34.40 (Agilent Technologies, 2010)' _computing_data_reduction 'CrysAlisPro, Version 1.171.34.40 (Agilent Technologies, 2010)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2009)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+4.7432P] 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 4394 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 9.547 _refine_diff_density_min -1.356 _refine_diff_density_rms 0.232 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 0.21087(3) 0.19905(2) 0.08756(2) 0.02574(7) Uani 1 1 d . . . Br1 Br -0.10968(7) 0.14048(6) 0.11702(6) 0.02385(11) Uani 1 1 d . . . Br2 Br 0.43891(8) 0.18419(7) 0.29057(6) 0.02811(12) Uani 1 1 d . . . N1 N 0.2986(6) 0.2653(5) -0.1013(5) 0.0203(8) Uani 1 1 d . . . N2 N 0.2094(6) 0.4868(5) 0.1171(5) 0.0202(8) Uani 1 1 d . . . C1 C 0.2883(7) 0.4119(6) -0.1083(6) 0.0192(9) Uani 1 1 d . . . C2 C 0.3254(7) 0.4612(7) -0.2204(6) 0.0232(10) Uani 1 1 d . . . H2 H 0.3174 0.5654 -0.2224 0.028 Uiso 1 1 calc R . . C3 C 0.3740(8) 0.3583(8) -0.3289(7) 0.0302(12) Uani 1 1 d . . . H3 H 0.3967 0.3889 -0.4084 0.036 Uiso 1 1 calc R . . C4 C 0.3896(8) 0.2079(7) -0.3206(7) 0.0267(11) Uani 1 1 d . . . H4 H 0.4258 0.1354 -0.3929 0.032 Uiso 1 1 calc R . . C5 C 0.3507(8) 0.1663(7) -0.2040(7) 0.0271(11) Uani 1 1 d . . . H5 H 0.3617 0.0643 -0.1975 0.033 Uiso 1 1 calc R . . C6 C 0.2421(7) 0.5250(6) 0.0104(6) 0.0215(9) Uani 1 1 d . . . H6 H 0.2368 0.6291 0.0069 0.026 Uiso 1 1 calc R . . C7 C 0.1726(6) 0.5987(6) 0.2337(6) 0.0191(9) Uani 1 1 d . . . C8 C 0.1490(8) 0.7497(7) 0.2353(7) 0.0264(11) Uani 1 1 d . . . H8 H 0.1535 0.7823 0.1533 0.032 Uiso 1 1 calc R . . C9 C 0.1186(9) 0.8532(7) 0.3568(7) 0.0300(12) Uani 1 1 d . . . H9 H 0.1033 0.9566 0.3580 0.036 Uiso 1 1 calc R . . C10 C 0.1107(8) 0.8054(7) 0.4761(7) 0.0292(12) Uani 1 1 d . . . H10 H 0.0872 0.8752 0.5581 0.035 Uiso 1 1 calc R . . C11 C 0.1367(8) 0.6573(8) 0.4760(7) 0.0296(12) Uani 1 1 d . . . H11 H 0.1349 0.6268 0.5593 0.035 Uiso 1 1 calc R . . C12 C 0.1656(7) 0.5521(7) 0.3555(6) 0.0237(10) Uani 1 1 d . . . H12 H 0.1805 0.4489 0.3553 0.028 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 0.03171(12) 0.02406(11) 0.02573(12) 0.01325(8) 0.00811(8) 0.00778(8) Br1 0.0297(3) 0.0183(2) 0.0250(3) 0.00693(18) 0.0114(2) 0.00452(18) Br2 0.0309(3) 0.0282(3) 0.0263(3) 0.0125(2) 0.0033(2) 0.0077(2) N1 0.023(2) 0.0193(18) 0.020(2) 0.0079(15) 0.0068(16) 0.0056(15) N2 0.023(2) 0.0174(18) 0.022(2) 0.0067(15) 0.0087(17) 0.0057(15) C1 0.018(2) 0.018(2) 0.019(2) 0.0040(17) 0.0052(17) 0.0035(16) C2 0.025(2) 0.024(2) 0.024(3) 0.012(2) 0.009(2) 0.0056(19) C3 0.031(3) 0.036(3) 0.025(3) 0.010(2) 0.013(2) 0.003(2) C4 0.027(3) 0.026(2) 0.025(3) 0.003(2) 0.011(2) 0.004(2) C5 0.031(3) 0.018(2) 0.034(3) 0.006(2) 0.015(2) 0.008(2) C6 0.026(2) 0.018(2) 0.023(2) 0.0080(18) 0.0067(19) 0.0082(18) C7 0.017(2) 0.019(2) 0.019(2) 0.0042(17) 0.0034(17) 0.0036(16) C8 0.033(3) 0.027(2) 0.025(3) 0.011(2) 0.011(2) 0.013(2) C9 0.036(3) 0.023(2) 0.031(3) 0.006(2) 0.011(2) 0.008(2) C10 0.030(3) 0.029(3) 0.022(3) -0.001(2) 0.007(2) 0.004(2) C11 0.031(3) 0.030(3) 0.024(3) 0.008(2) 0.006(2) 0.000(2) C12 0.025(2) 0.022(2) 0.023(2) 0.0064(19) 0.005(2) 0.0043(19) _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 2.327(4) . ? Hg1 N2 2.507(4) . ? Hg1 Br2 2.5203(6) . ? Hg1 Br1 2.6299(6) . ? Hg1 Br1 3.0140(6) 2 ? N1 C5 1.334(7) . ? N1 C1 1.348(6) . ? N2 C6 1.268(7) . ? N2 C7 1.419(7) . ? C1 C2 1.381(7) . ? C1 C6 1.475(7) . ? C2 C3 1.374(8) . ? C2 H2 0.9500 . ? C3 C4 1.395(9) . ? C3 H3 0.9500 . ? C4 C5 1.394(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.391(7) . ? C7 C12 1.403(8) . ? C8 C9 1.392(8) . ? C8 H8 0.9500 . ? C9 C10 1.387(9) . ? C9 H9 0.9500 . ? C10 C11 1.375(9) . ? C10 H10 0.9500 . ? C11 C12 1.387(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? 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 N2 70.44(15) . . ? N1 Hg1 Br2 118.84(11) . . ? N2 Hg1 Br2 109.66(11) . . ? N1 Hg1 Br1 126.56(11) . . ? N2 Hg1 Br1 91.40(10) . . ? Br2 Hg1 Br1 114.59(2) . . ? N1 Hg1 Br1 84.90(11) . 2 ? N2 Hg1 Br1 146.02(11) . 2 ? Br2 Hg1 Br1 102.542(19) . 2 ? Br1 Hg1 Br1 84.768(17) . 2 ? Hg1 Br1 Hg1 95.232(17) . 2 ? C5 N1 C1 118.9(5) . . ? C5 N1 Hg1 124.4(4) . . ? C1 N1 Hg1 116.6(3) . . ? C6 N2 C7 121.3(5) . . ? C6 N2 Hg1 111.9(3) . . ? C7 N2 Hg1 126.8(3) . . ? N1 C1 C2 122.1(5) . . ? N1 C1 C6 118.8(5) . . ? C2 C1 C6 119.1(5) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 118.9(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.0(5) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? N2 C6 C1 121.7(5) . . ? N2 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? C8 C7 C12 119.4(5) . . ? C8 C7 N2 124.3(5) . . ? C12 C7 N2 116.3(5) . . ? C7 C8 C9 120.0(5) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.0(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.2(6) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.6(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 119.7(5) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? 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 N1 Hg1 Br1 Hg1 79.69(14) . . . 2 ? N2 Hg1 Br1 Hg1 146.18(11) . . . 2 ? Br2 Hg1 Br1 Hg1 -101.41(2) . . . 2 ? Br1 Hg1 Br1 Hg1 0.0 2 . . 2 ? N2 Hg1 N1 C5 176.5(5) . . . . ? Br2 Hg1 N1 C5 74.3(5) . . . . ? Br1 Hg1 N1 C5 -106.9(5) . . . . ? Br1 Hg1 N1 C5 -27.2(5) 2 . . . ? N2 Hg1 N1 C1 -6.3(4) . . . . ? Br2 Hg1 N1 C1 -108.5(4) . . . . ? Br1 Hg1 N1 C1 70.4(4) . . . . ? Br1 Hg1 N1 C1 150.0(4) 2 . . . ? N1 Hg1 N2 C6 5.5(4) . . . . ? Br2 Hg1 N2 C6 120.2(4) . . . . ? Br1 Hg1 N2 C6 -123.1(4) . . . . ? Br1 Hg1 N2 C6 -40.4(5) 2 . . . ? N1 Hg1 N2 C7 -176.2(5) . . . . ? Br2 Hg1 N2 C7 -61.6(4) . . . . ? Br1 Hg1 N2 C7 55.2(4) . . . . ? Br1 Hg1 N2 C7 137.9(3) 2 . . . ? C5 N1 C1 C2 1.8(8) . . . . ? Hg1 N1 C1 C2 -175.6(4) . . . . ? C5 N1 C1 C6 -175.9(5) . . . . ? Hg1 N1 C1 C6 6.7(6) . . . . ? N1 C1 C2 C3 0.2(8) . . . . ? C6 C1 C2 C3 177.9(5) . . . . ? C1 C2 C3 C4 -1.9(9) . . . . ? C2 C3 C4 C5 1.6(9) . . . . ? C1 N1 C5 C4 -2.0(9) . . . . ? Hg1 N1 C5 C4 175.1(4) . . . . ? C3 C4 C5 N1 0.4(9) . . . . ? C7 N2 C6 C1 177.2(5) . . . . ? Hg1 N2 C6 C1 -4.4(7) . . . . ? N1 C1 C6 N2 -1.2(8) . . . . ? C2 C1 C6 N2 -178.9(5) . . . . ? C6 N2 C7 C8 7.8(8) . . . . ? Hg1 N2 C7 C8 -170.3(4) . . . . ? C6 N2 C7 C12 -170.2(5) . . . . ? Hg1 N2 C7 C12 11.6(7) . . . . ? C12 C7 C8 C9 -0.0(9) . . . . ? N2 C7 C8 C9 -178.0(5) . . . . ? C7 C8 C9 C10 -0.5(10) . . . . ? C8 C9 C10 C11 1.5(10) . . . . ? C9 C10 C11 C12 -2.1(10) . . . . ? C10 C11 C12 C7 1.6(9) . . . . ? C8 C7 C12 C11 -0.5(8) . . . . ? N2 C7 C12 C11 177.6(5) . . . . ? _iucr_refine_instructions_details ; TITL L1021B_Mo in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 8.033833 8.944090 10.009078 106.5949 100.7318 99.5612 ZERR 1.00 0.000163 0.000233 0.000309 0.0025 0.0022 0.0019 LATT 1 SFAC C H BR HG N UNIT 24 20 4 2 4 MERG 2 TEMP -113 L.S. 4 BOND $H CONF ACTA FMAP 2 PLAN 10 BIND Hg1 Br1_$1 EQIV $1 -x,-y,-z WGHT 0.049700 4.743199 FVAR 4.38129 HG1 4 0.210871 0.199051 0.087561 11.00000 0.03171 0.02406 = 0.02573 0.01325 0.00811 0.00778 BR1 3 -0.109684 0.140478 0.117024 11.00000 0.02969 0.01826 = 0.02505 0.00693 0.01137 0.00452 BR2 3 0.438913 0.184188 0.290572 11.00000 0.03090 0.02821 = 0.02633 0.01254 0.00333 0.00769 N1 5 0.298624 0.265298 -0.101252 11.00000 0.02339 0.01930 = 0.02003 0.00793 0.00682 0.00561 N2 5 0.209374 0.486763 0.117063 11.00000 0.02328 0.01742 = 0.02181 0.00671 0.00865 0.00568 C1 1 0.288300 0.411857 -0.108286 11.00000 0.01832 0.01844 = 0.01944 0.00399 0.00515 0.00346 C2 1 0.325407 0.461248 -0.220355 11.00000 0.02481 0.02400 = 0.02440 0.01186 0.00854 0.00557 AFIX 43 H2 2 0.317405 0.565399 -0.222381 11.00000 -1.20000 AFIX 0 C3 1 0.374027 0.358254 -0.328931 11.00000 0.03050 0.03559 = 0.02530 0.01047 0.01255 0.00279 AFIX 43 H3 2 0.396698 0.388905 -0.408377 11.00000 -1.20000 AFIX 0 C4 1 0.389551 0.207917 -0.320580 11.00000 0.02749 0.02568 = 0.02498 0.00320 0.01144 0.00441 AFIX 43 H4 2 0.425828 0.135404 -0.392880 11.00000 -1.20000 AFIX 0 C5 1 0.350747 0.166302 -0.203999 11.00000 0.03103 0.01804 = 0.03386 0.00554 0.01489 0.00766 AFIX 43 H5 2 0.361743 0.064328 -0.197486 11.00000 -1.20000 AFIX 0 C6 1 0.242122 0.524972 0.010444 11.00000 0.02559 0.01827 = 0.02279 0.00795 0.00667 0.00818 AFIX 43 H6 2 0.236778 0.629142 0.006946 11.00000 -1.20000 AFIX 0 C7 1 0.172599 0.598694 0.233737 11.00000 0.01723 0.01927 = 0.01891 0.00419 0.00338 0.00364 C8 1 0.148952 0.749747 0.235261 11.00000 0.03338 0.02660 = 0.02491 0.01098 0.01097 0.01317 AFIX 43 H8 2 0.153525 0.782278 0.153327 11.00000 -1.20000 AFIX 0 C9 1 0.118591 0.853243 0.356806 11.00000 0.03635 0.02275 = 0.03054 0.00570 0.01143 0.00795 AFIX 43 H9 2 0.103289 0.956646 0.358021 11.00000 -1.20000 AFIX 0 C10 1 0.110679 0.805433 0.476112 11.00000 0.02997 0.02902 = 0.02206 -0.00074 0.00718 0.00434 AFIX 43 H10 2 0.087201 0.875202 0.558089 11.00000 -1.20000 AFIX 0 C11 1 0.136728 0.657326 0.476028 11.00000 0.03110 0.03047 = 0.02367 0.00808 0.00576 0.00031 AFIX 43 H11 2 0.134946 0.626795 0.559295 11.00000 -1.20000 AFIX 0 C12 1 0.165586 0.552075 0.355469 11.00000 0.02475 0.02217 = 0.02292 0.00639 0.00519 0.00425 AFIX 43 H12 2 0.180541 0.448872 0.355300 11.00000 -1.20000 HKLF 4 REM L1021B_Mo in P-1 REM R1 = 0.0384 for 4057 Fo > 4sig(Fo) and 0.0424 for all 4394 data REM 154 parameters refined using 0 restraints END WGHT 0.0497 4.7432 REM Highest difference peak 9.547, deepest hole -1.356, 1-sigma level 0.232 Q1 1 0.1960 0.2762 0.1877 11.00000 0.05 9.55 Q2 1 0.4499 0.1606 0.2275 11.00000 0.05 1.00 Q3 1 0.2727 0.2476 0.0166 11.00000 0.05 0.75 Q4 1 0.2653 0.4417 0.0324 11.00000 0.05 0.72 Q5 1 0.1825 0.5716 0.3040 11.00000 0.05 0.72 Q6 1 0.1396 0.2248 0.0524 11.00000 0.05 0.70 Q7 1 0.1575 0.1633 0.1589 11.00000 0.05 0.68 Q8 1 0.1271 0.5965 0.4089 11.00000 0.05 0.68 Q9 1 0.3865 0.2259 0.2851 11.00000 0.05 0.68 Q10 1 -0.1487 0.1715 0.1538 11.00000 0.05 0.68 ; data_3 _database_code_depnum_ccdc_archive 'CCDC 892206' #TrackingRef '3.cif' # L1017 _audit_creation_method SHELXL-97 _audit_creation_date 2010-Oct-28 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C12 H10 Hg I2 N2' _chemical_formula_sum 'C12 H10 Hg I2 N2' _chemical_formula_weight 636.53 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 48 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 40 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Hg Hg 4 -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; I I 8 -0.4742 1.8119 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 8 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 12.68311(19) _cell_length_b 7.13335(10) _cell_length_c 15.9101(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.8269(13) _cell_angle_gamma 90.00 _cell_volume 1439.28(4) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 13098 _cell_measurement_theta_min 2.0639 _cell_measurement_theta_max 32.3587 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 14.958 _exptl_absorpt_correction_T_min 0.168 _exptl_absorpt_correction_T_max 0.336 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; Solvent used: acetonitrile Cooling Device: Oxford Instruments Cryojet XL Crystal mount: on a glass fibre Frames collected: 553 Seconds exposure per frame: 8.0 Degrees rotation per frame: 1.0 Crystal-detector distance (mm): 55.0 Client: Tushar Basu Baul Sample code: TSBB-293 (L1017) ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova, dual radiation diffractometer' _diffrn_detector_area_resol_mean 10.3801 _diffrn_detector 'Atlas CCD camera on k goniostat' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 22859 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 32.43 _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 4851 _reflns_number_gt 4367 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 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 'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+3.6107P] 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 SHELXL97 _refine_ls_extinction_coef 0.00027(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4846 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 5.318 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.162 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 C1 C 0.6202(3) 0.7003(5) 0.0424(2) 0.0246(7) Uani 1 1 d . . . C2 C 0.6641(3) 0.7751(6) -0.0297(3) 0.0285(8) Uani 1 1 d . . . H2 H 0.6204 0.8292 -0.0722 0.034 Uiso 1 1 calc R . . C3 C 0.7728(3) 0.7697(6) -0.0387(3) 0.0300(8) Uani 1 1 d . . . H3 H 0.8049 0.8205 -0.0872 0.036 Uiso 1 1 calc R . . C4 C 0.8330(3) 0.6890(6) 0.0242(3) 0.0311(8) Uani 1 1 d . . . H4 H 0.9075 0.6823 0.0195 0.037 Uiso 1 1 calc R . . C5 C 0.7839(3) 0.6177(6) 0.0946(3) 0.0312(9) Uani 1 1 d . . . H5 H 0.8260 0.5633 0.1380 0.037 Uiso 1 1 calc R . . C6 C 0.5050(3) 0.7052(6) 0.0529(2) 0.0268(7) Uani 1 1 d . . . H6 H 0.4625 0.7662 0.0115 0.032 Uiso 1 1 calc R . . C7 C 0.3496(3) 0.6390(5) 0.1268(2) 0.0223(7) Uani 1 1 d . . . C8 C 0.2802(3) 0.7346(6) 0.0741(2) 0.0270(8) Uani 1 1 d . . . H8 H 0.3059 0.8003 0.0267 0.032 Uiso 1 1 calc R . . C9 C 0.1731(3) 0.7342(6) 0.0907(3) 0.0307(8) Uani 1 1 d . . . H9 H 0.1260 0.8007 0.0546 0.037 Uiso 1 1 calc R . . C10 C 0.1340(3) 0.6384(6) 0.1592(3) 0.0321(9) Uani 1 1 d . . . H10 H 0.0605 0.6385 0.1698 0.038 Uiso 1 1 calc R . . C11 C 0.2026(4) 0.5428(6) 0.2118(3) 0.0325(9) Uani 1 1 d . . . H11 H 0.1762 0.4766 0.2589 0.039 Uiso 1 1 calc R . . C12 C 0.3100(4) 0.5431(6) 0.1963(3) 0.0293(8) Uani 1 1 d . . . H12 H 0.3569 0.4779 0.2331 0.035 Uiso 1 1 calc R . . Hg1 Hg 0.588271(13) 0.48431(2) 0.215478(9) 0.02912(6) Uani 1 1 d . . . I1 I 0.55541(2) 0.64579(4) 0.362420(17) 0.03218(7) Uani 1 1 d . . . I2 I 0.60405(2) 0.11879(4) 0.174357(16) 0.03053(7) Uani 1 1 d . . . N1 N 0.6798(3) 0.6227(5) 0.1035(2) 0.0253(6) Uani 1 1 d . . . N2 N 0.4605(3) 0.6301(4) 0.1160(2) 0.0229(6) 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 C1 0.0269(17) 0.0212(17) 0.0257(18) -0.0042(14) 0.0062(14) -0.0022(14) C2 0.0311(19) 0.030(2) 0.0241(18) 0.0026(15) 0.0034(14) -0.0021(16) C3 0.034(2) 0.0276(19) 0.029(2) -0.0022(15) 0.0086(16) -0.0072(16) C4 0.0258(18) 0.036(2) 0.031(2) -0.0079(17) 0.0051(15) -0.0033(17) C5 0.031(2) 0.035(2) 0.028(2) -0.0043(16) -0.0018(15) 0.0018(17) C6 0.0268(17) 0.031(2) 0.0228(17) 0.0028(15) 0.0020(14) -0.0006(15) C7 0.0259(17) 0.0191(16) 0.0220(17) -0.0024(13) 0.0035(13) -0.0015(13) C8 0.0311(19) 0.0257(19) 0.0243(18) 0.0041(14) 0.0040(14) 0.0012(15) C9 0.0277(19) 0.034(2) 0.030(2) -0.0007(16) -0.0004(15) 0.0059(17) C10 0.0284(19) 0.037(2) 0.031(2) -0.0055(17) 0.0087(16) -0.0030(17) C11 0.037(2) 0.033(2) 0.028(2) 0.0027(16) 0.0090(17) -0.0041(18) C12 0.035(2) 0.0274(19) 0.0250(19) 0.0050(15) 0.0009(16) -0.0021(16) Hg1 0.03627(10) 0.03062(9) 0.02057(8) 0.00010(5) 0.00383(6) 0.00519(6) I1 0.03533(14) 0.03794(15) 0.02338(13) -0.00722(10) 0.00453(10) -0.00101(11) I2 0.04152(15) 0.02639(13) 0.02373(13) -0.00142(9) 0.00293(10) 0.00324(10) N1 0.0317(16) 0.0210(15) 0.0234(15) -0.0026(12) 0.0043(12) -0.0005(13) N2 0.0258(15) 0.0215(15) 0.0215(15) -0.0009(11) 0.0040(12) 0.0012(12) _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 C1 N1 1.342(5) . ? C1 C2 1.389(5) . ? C1 C6 1.474(5) . ? C2 C3 1.388(6) . ? C2 H2 0.9500 . ? C3 C4 1.376(6) . ? C3 H3 0.9500 . ? C4 C5 1.385(6) . ? C4 H4 0.9500 . ? C5 N1 1.330(5) . ? C5 H5 0.9500 . ? C6 N2 1.276(5) . ? C6 H6 0.9500 . ? C7 C8 1.387(5) . ? C7 C12 1.400(5) . ? C7 N2 1.421(5) . ? C8 C9 1.388(6) . ? C8 H8 0.9500 . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.379(7) . ? C10 H10 0.9500 . ? C11 C12 1.389(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Hg1 N1 2.357(3) . ? Hg1 N2 2.478(3) . ? Hg1 I1 2.6446(3) . ? Hg1 I2 2.6964(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.9(4) . . ? N1 C1 C6 118.4(3) . . ? C2 C1 C6 119.7(4) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 118.5(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 122.3(4) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C1 122.0(4) . . ? N2 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? C8 C7 C12 119.1(4) . . ? C8 C7 N2 124.7(3) . . ? C12 C7 N2 116.2(3) . . ? C7 C8 C9 119.9(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.4(4) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? N1 Hg1 N2 70.47(11) . . ? N1 Hg1 I1 124.84(8) . . ? N2 Hg1 I1 105.79(7) . . ? N1 Hg1 I2 100.53(8) . . ? N2 Hg1 I2 107.52(7) . . ? I1 Hg1 I2 130.455(11) . . ? C5 N1 C1 118.9(4) . . ? C5 N1 Hg1 124.7(3) . . ? C1 N1 Hg1 116.2(3) . . ? C6 N2 C7 121.8(3) . . ? C6 N2 Hg1 112.7(3) . . ? C7 N2 Hg1 125.5(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 N1 C1 C2 C3 -0.1(6) . . . . ? C6 C1 C2 C3 179.9(4) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 N1 0.5(7) . . . . ? N1 C1 C6 N2 -3.5(6) . . . . ? C2 C1 C6 N2 176.5(4) . . . . ? C12 C7 C8 C9 0.0(6) . . . . ? N2 C7 C8 C9 -179.9(4) . . . . ? C7 C8 C9 C10 -0.4(6) . . . . ? C8 C9 C10 C11 0.4(7) . . . . ? C9 C10 C11 C12 0.1(7) . . . . ? C10 C11 C12 C7 -0.5(7) . . . . ? C8 C7 C12 C11 0.5(6) . . . . ? N2 C7 C12 C11 -179.6(4) . . . . ? C4 C5 N1 C1 -0.3(6) . . . . ? C4 C5 N1 Hg1 175.0(3) . . . . ? C2 C1 N1 C5 0.0(6) . . . . ? C6 C1 N1 C5 -180.0(4) . . . . ? C2 C1 N1 Hg1 -175.6(3) . . . . ? C6 C1 N1 Hg1 4.4(4) . . . . ? N2 Hg1 N1 C5 -178.2(3) . . . . ? I1 Hg1 N1 C5 85.8(3) . . . . ? I2 Hg1 N1 C5 -73.2(3) . . . . ? N2 Hg1 N1 C1 -2.9(3) . . . . ? I1 Hg1 N1 C1 -98.9(3) . . . . ? I2 Hg1 N1 C1 102.1(3) . . . . ? C1 C6 N2 C7 178.5(3) . . . . ? C1 C6 N2 Hg1 0.7(5) . . . . ? C8 C7 N2 C6 -3.2(6) . . . . ? C12 C7 N2 C6 176.9(4) . . . . ? C8 C7 N2 Hg1 174.3(3) . . . . ? C12 C7 N2 Hg1 -5.6(5) . . . . ? N1 Hg1 N2 C6 1.1(3) . . . . ? I1 Hg1 N2 C6 123.1(3) . . . . ? I2 Hg1 N2 C6 -94.2(3) . . . . ? N1 Hg1 N2 C7 -176.6(3) . . . . ? I1 Hg1 N2 C7 -54.6(3) . . . . ? I2 Hg1 N2 C7 88.1(3) . . . . ? _iucr_refine_instructions_details ; TITL L1017A_Mo in P21/n #14 CELL 0.71073 12.68311 7.13335 15.91006 90 90.8269 90 ZERR 4 0.00019 0.0001 0.00022 0 0.0013 0 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H HG I N UNIT 48 40 4 8 8 MERG 2 TEMP -113 OMIT 0 0 2 OMIT -1 0 1 OMIT 3 0 1 OMIT 1 0 1 OMIT 0 1 2 L.S. 4 BOND $H CONF ACTA FMAP 2 PLAN 40 WGHT 0.027200 3.610700 EXTI 0.000270 FVAR 1.76453 C1 1 0.620207 0.700287 0.042401 11.00000 0.02693 0.02118 = 0.02574 -0.00419 0.00619 -0.00216 C2 1 0.664131 0.775111 -0.029665 11.00000 0.03113 0.03036 = 0.02409 0.00260 0.00336 -0.00208 AFIX 43 H2 2 0.620447 0.829230 -0.072170 11.00000 -1.20000 AFIX 0 C3 1 0.772797 0.769698 -0.038709 11.00000 0.03372 0.02756 = 0.02903 -0.00222 0.00857 -0.00719 AFIX 43 H3 2 0.804896 0.820513 -0.087245 11.00000 -1.20000 AFIX 0 C4 1 0.832971 0.689032 0.024243 11.00000 0.02575 0.03634 = 0.03144 -0.00786 0.00512 -0.00330 AFIX 43 H4 2 0.907458 0.682340 0.019509 11.00000 -1.20000 AFIX 0 C5 1 0.783855 0.617705 0.094566 11.00000 0.03102 0.03484 = 0.02760 -0.00434 -0.00178 0.00176 AFIX 43 H5 2 0.826003 0.563254 0.137954 11.00000 -1.20000 AFIX 0 C6 1 0.504978 0.705223 0.052931 11.00000 0.02684 0.03087 = 0.02282 0.00281 0.00201 -0.00057 AFIX 43 H6 2 0.462541 0.766173 0.011524 11.00000 -1.20000 AFIX 0 C7 1 0.349648 0.638983 0.126804 11.00000 0.02585 0.01912 = 0.02198 -0.00236 0.00349 -0.00150 C8 1 0.280210 0.734597 0.074107 11.00000 0.03106 0.02570 = 0.02427 0.00411 0.00398 0.00124 AFIX 43 H8 2 0.305931 0.800283 0.026678 11.00000 -1.20000 AFIX 0 C9 1 0.173091 0.734239 0.090723 11.00000 0.02771 0.03445 = 0.02992 -0.00067 -0.00040 0.00591 AFIX 43 H9 2 0.125954 0.800709 0.054606 11.00000 -1.20000 AFIX 0 C10 1 0.134010 0.638425 0.159153 11.00000 0.02844 0.03719 = 0.03081 -0.00553 0.00875 -0.00299 AFIX 43 H10 2 0.060496 0.638459 0.169783 11.00000 -1.20000 AFIX 0 C11 1 0.202576 0.542837 0.211834 11.00000 0.03701 0.03312 = 0.02774 0.00273 0.00903 -0.00409 AFIX 43 H11 2 0.176196 0.476600 0.258873 11.00000 -1.20000 AFIX 0 C12 1 0.310036 0.543123 0.196328 11.00000 0.03546 0.02741 = 0.02499 0.00500 0.00091 -0.00213 AFIX 43 H12 2 0.356931 0.477906 0.233104 11.00000 -1.20000 AFIX 0 HG1 3 0.588271 0.484314 0.215478 11.00000 0.03627 0.03062 = 0.02057 0.00010 0.00383 0.00519 I1 4 0.555407 0.645786 0.362420 11.00000 0.03533 0.03794 = 0.02338 -0.00722 0.00453 -0.00101 I2 4 0.604051 0.118792 0.174357 11.00000 0.04152 0.02639 = 0.02373 -0.00142 0.00293 0.00324 N1 5 0.679758 0.622739 0.103512 11.00000 0.03168 0.02099 = 0.02336 -0.00256 0.00432 -0.00054 N2 5 0.460515 0.630126 0.115962 11.00000 0.02584 0.02152 = 0.02155 -0.00087 0.00397 0.00120 HKLF 4 REM L1017A_Mo in P21/n #14 REM R1 = 0.0272 for 4367 Fo > 4sig(Fo) and 0.0321 for all 4846 data REM 155 parameters refined using 0 restraints END WGHT 0.0272 3.6107 REM Highest difference peak 5.318, deepest hole -1.494, 1-sigma level 0.162 Q1 1 0.5187 0.4514 0.2263 11.00000 0.05 5.32 Q2 1 0.6567 0.4846 0.2405 11.00000 0.05 0.88 Q3 1 0.5560 0.5845 0.2227 11.00000 0.05 0.80 Q4 1 0.6307 0.5721 0.2150 11.00000 0.05 0.78 Q5 1 0.5929 0.5687 0.3642 11.00000 0.05 0.73 Q6 1 0.5943 0.7127 0.3649 11.00000 0.05 0.72 Q7 1 0.5725 0.2077 0.1753 11.00000 0.05 0.71 Q8 1 0.5762 0.7351 0.0501 11.00000 0.05 0.64 Q9 1 0.5655 0.3587 0.2494 11.00000 0.05 0.62 Q10 1 0.6362 0.1919 0.1716 11.00000 0.05 0.59 ; data_4a _database_code_depnum_ccdc_archive 'CCDC 892207' #TrackingRef '4a.cif' # tu1dosm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl4 Hg2 N4' _chemical_formula_sum 'C26 H24 Cl4 Hg2 N4' _chemical_formula_weight 935.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2038(11) _cell_length_b 13.8179(19) _cell_length_c 14.4494(19) _cell_angle_alpha 115.149(2) _cell_angle_beta 99.505(2) _cell_angle_gamma 100.406(2) _cell_volume 1403.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3022 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 22.62 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 11.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.28 _exptl_absorpt_process_details SADABS _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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13697 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4934 _reflns_number_gt 3716 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0585P)^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 4934 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.76696(5) 0.13482(4) 0.69235(3) 0.04575(17) Uani 1 1 d . . . Cl1 Cl 0.8780(3) 0.0859(2) 0.8318(2) 0.0442(6) Uani 1 1 d . . . Cl2 Cl 0.5507(3) 0.2291(2) 0.7412(2) 0.0500(7) Uani 1 1 d . . . N1 N 0.8470(10) 0.1007(7) 0.5419(6) 0.0343(18) Uani 1 1 d . . . N2 N 0.9797(10) 0.3069(7) 0.7205(6) 0.0367(19) Uani 1 1 d . . . C1 C 0.9377(12) 0.1888(9) 0.5373(7) 0.036(2) Uani 1 1 d . . . C2 C 0.9777(13) 0.1757(9) 0.4430(8) 0.046(3) Uani 1 1 d . . . H2 H 1.0387 0.2370 0.4392 0.055 Uiso 1 1 calc R . . C3 C 0.9262(13) 0.0713(10) 0.3554(8) 0.046(3) Uani 1 1 d . . . H3 H 0.9545 0.0620 0.2930 0.055 Uiso 1 1 calc R . . C4 C 0.8358(12) -0.0163(9) 0.3604(8) 0.042(2) Uani 1 1 d . . . H4 H 0.8011 -0.0868 0.3021 0.050 Uiso 1 1 calc R . . C5 C 0.7946(12) 0.0001(9) 0.4542(7) 0.039(2) Uani 1 1 d . . . H5 H 0.7285 -0.0604 0.4569 0.046 Uiso 1 1 calc R . . C6 C 0.9939(13) 0.2974(9) 0.6318(8) 0.041(2) Uani 1 1 d . . . H6 H 1.0411 0.3606 0.6264 0.050 Uiso 1 1 calc R . . C7 C 1.0349(14) 0.4175(8) 0.8096(8) 0.042(3) Uani 1 1 d . . . C8 C 0.9535(14) 0.4955(9) 0.8031(9) 0.048(3) Uani 1 1 d . . . H8 H 0.8682 0.4763 0.7423 0.057 Uiso 1 1 calc R . . C9 C 1.0005(18) 0.6018(10) 0.8880(10) 0.060(3) Uani 1 1 d . . . H9 H 0.9471 0.6550 0.8858 0.072 Uiso 1 1 calc R . . C10 C 1.1280(17) 0.6261(10) 0.9752(9) 0.060(3) Uani 1 1 d . . . H10 H 1.1622 0.6975 1.0323 0.073 Uiso 1 1 calc R . . C11 C 1.2062(14) 0.5494(9) 0.9811(8) 0.047(3) Uani 1 1 d . . . H11 H 1.2926 0.5693 1.0417 0.056 Uiso 1 1 calc R . . C12 C 1.1595(14) 0.4434(9) 0.8991(8) 0.043(3) Uani 1 1 d . . . C13 C 1.2398(14) 0.3584(10) 0.9064(10) 0.058(3) Uani 1 1 d . . . H13A H 1.3135 0.3880 0.9768 0.087 Uiso 1 1 calc R . . H13B H 1.3065 0.3385 0.8560 0.087 Uiso 1 1 calc R . . H13C H 1.1516 0.2935 0.8912 0.087 Uiso 1 1 calc R . . Hg21 Hg 0.61428(6) -0.13467(4) 0.73109(4) 0.04734(17) Uani 1 1 d . . . Cl21 Cl 0.5429(4) -0.1038(2) 0.5778(2) 0.0511(7) Uani 1 1 d . . . Cl22 Cl 0.8214(4) -0.2262(3) 0.7611(3) 0.0586(8) Uani 1 1 d . . . N21 N 0.4471(10) -0.0452(7) 0.8373(6) 0.040(2) Uani 1 1 d . . . N22 N 0.3817(11) -0.2712(7) 0.7412(7) 0.043(2) Uani 1 1 d . . . C21 C 0.3298(13) -0.1066(9) 0.8603(8) 0.042(3) Uani 1 1 d . . . C22 C 0.2344(14) -0.0587(11) 0.9268(9) 0.055(3) Uani 1 1 d . . . H22 H 0.1607 -0.1017 0.9462 0.066 Uiso 1 1 calc R . . C23 C 0.2469(15) 0.0514(11) 0.9648(9) 0.060(3) Uani 1 1 d . . . H23 H 0.1793 0.0838 1.0080 0.072 Uiso 1 1 calc R . . C24 C 0.3616(15) 0.1141(10) 0.9380(9) 0.054(3) Uani 1 1 d . . . H24 H 0.3720 0.1895 0.9625 0.064 Uiso 1 1 calc R . . C25 C 0.4597(14) 0.0640(9) 0.8753(9) 0.046(3) Uani 1 1 d . . . H25 H 0.5380 0.1068 0.8581 0.055 Uiso 1 1 calc R . . C26 C 0.3143(13) -0.2262(9) 0.8140(8) 0.045(3) Uani 1 1 d . . . H26 H 0.2537 -0.2690 0.8391 0.054 Uiso 1 1 calc R . . C27 C 0.3778(13) -0.3855(9) 0.7022(8) 0.042(3) Uani 1 1 d . . . C28 C 0.4386(17) -0.4244(11) 0.7711(11) 0.065(4) Uani 1 1 d . . . H28 H 0.4683 -0.3795 0.8442 0.078 Uiso 1 1 calc R . . C29 C 0.4537(16) -0.5302(12) 0.7288(12) 0.067(4) Uani 1 1 d . . . H29 H 0.4967 -0.5568 0.7742 0.081 Uiso 1 1 calc R . . C30 C 0.4069(16) -0.5987(10) 0.6207(13) 0.067(4) Uani 1 1 d . . . H30 H 0.4181 -0.6707 0.5941 0.081 Uiso 1 1 calc R . . C31 C 0.3433(16) -0.5609(10) 0.5514(10) 0.061(3) Uani 1 1 d . . . H31 H 0.3128 -0.6073 0.4785 0.074 Uiso 1 1 calc R . . C32 C 0.3252(14) -0.4545(10) 0.5906(10) 0.053(3) Uani 1 1 d . . . C33 C 0.2486(19) -0.4148(12) 0.5160(10) 0.079(4) Uani 1 1 d . . . H33A H 0.2233 -0.4722 0.4440 0.118 Uiso 1 1 calc R . . H33B H 0.3292 -0.3492 0.5257 0.118 Uiso 1 1 calc R . . H33C H 0.1444 -0.3976 0.5306 0.118 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 0.0585(3) 0.0429(3) 0.0450(3) 0.0229(2) 0.0255(2) 0.0185(2) Cl1 0.0547(16) 0.0374(15) 0.0388(14) 0.0172(12) 0.0092(12) 0.0144(13) Cl2 0.0512(16) 0.0397(16) 0.0564(17) 0.0174(13) 0.0138(13) 0.0204(13) N1 0.040(5) 0.030(5) 0.032(5) 0.014(4) 0.012(4) 0.007(4) N2 0.043(5) 0.030(5) 0.031(5) 0.011(4) 0.007(4) 0.006(4) C1 0.038(5) 0.042(6) 0.031(5) 0.017(5) 0.011(4) 0.016(5) C2 0.046(6) 0.038(7) 0.047(7) 0.017(6) 0.014(5) 0.004(5) C3 0.050(6) 0.058(8) 0.028(6) 0.018(6) 0.015(5) 0.014(6) C4 0.042(6) 0.048(7) 0.027(5) 0.010(5) 0.007(4) 0.014(5) C5 0.040(6) 0.040(6) 0.030(5) 0.015(5) 0.003(4) 0.006(5) C6 0.049(6) 0.034(6) 0.035(6) 0.014(5) 0.007(5) 0.005(5) C7 0.051(6) 0.032(6) 0.039(6) 0.013(5) 0.021(5) 0.002(5) C8 0.059(7) 0.051(7) 0.043(7) 0.026(6) 0.023(6) 0.020(6) C9 0.092(10) 0.043(7) 0.065(8) 0.029(7) 0.047(8) 0.029(7) C10 0.077(9) 0.034(7) 0.048(8) 0.005(6) 0.023(7) -0.003(6) C11 0.050(6) 0.035(7) 0.040(6) 0.009(5) 0.010(5) 0.003(5) C12 0.050(6) 0.044(7) 0.027(6) 0.008(5) 0.020(5) 0.012(5) C13 0.049(7) 0.061(8) 0.068(8) 0.031(7) 0.022(6) 0.018(6) Hg21 0.0533(3) 0.0461(3) 0.0568(3) 0.0315(2) 0.0235(2) 0.0197(2) Cl21 0.0583(17) 0.0513(18) 0.0478(16) 0.0281(14) 0.0130(13) 0.0134(14) Cl22 0.0565(17) 0.0536(19) 0.075(2) 0.0353(17) 0.0164(15) 0.0250(15) N21 0.044(5) 0.043(5) 0.033(5) 0.017(4) 0.009(4) 0.015(4) N22 0.053(5) 0.041(5) 0.040(5) 0.024(4) 0.012(4) 0.011(4) C21 0.040(6) 0.052(7) 0.041(6) 0.023(6) 0.015(5) 0.017(5) C22 0.043(6) 0.071(9) 0.051(7) 0.030(7) 0.013(6) 0.012(6) C23 0.060(8) 0.072(10) 0.040(7) 0.015(7) 0.016(6) 0.030(7) C24 0.064(8) 0.044(7) 0.054(7) 0.020(6) 0.017(6) 0.026(6) C25 0.050(6) 0.038(7) 0.056(7) 0.026(6) 0.016(5) 0.014(5) C26 0.049(6) 0.047(7) 0.044(7) 0.025(6) 0.015(5) 0.012(5) C27 0.046(6) 0.038(6) 0.046(7) 0.022(5) 0.022(5) 0.007(5) C28 0.082(9) 0.057(9) 0.069(9) 0.042(8) 0.027(7) 0.013(7) C29 0.061(8) 0.062(9) 0.095(11) 0.054(9) 0.014(8) 0.017(7) C30 0.069(9) 0.035(7) 0.110(12) 0.040(8) 0.038(9) 0.017(7) C31 0.072(8) 0.043(7) 0.062(8) 0.016(7) 0.035(7) 0.007(6) C32 0.043(6) 0.053(8) 0.072(9) 0.035(7) 0.025(6) 0.011(6) C33 0.104(11) 0.070(10) 0.060(9) 0.032(8) 0.023(8) 0.015(9) _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 2.256(7) . ? Hg1 Cl2 2.410(3) . ? Hg1 Cl1 2.474(3) . ? Hg1 N2 2.512(8) . ? Cl1 Hg21 2.982(3) . ? N1 C1 1.342(12) . ? N1 C5 1.353(12) . ? N2 C6 1.259(11) . ? N2 C7 1.444(12) . ? C1 C2 1.399(13) . ? C1 C6 1.459(14) . ? C2 C3 1.383(14) . ? C2 H2 0.9300 . ? C3 C4 1.338(14) . ? C3 H3 0.9300 . ? C4 C5 1.385(12) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.372(14) . ? C7 C8 1.393(15) . ? C8 C9 1.385(16) . ? C8 H8 0.9300 . ? C9 C10 1.368(17) . ? C9 H9 0.9300 . ? C10 C11 1.359(16) . ? C10 H10 0.9300 . ? C11 C12 1.367(14) . ? C11 H11 0.9300 . ? C12 C13 1.479(15) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Hg21 N21 2.337(8) . ? Hg21 Cl22 2.382(3) . ? Hg21 Cl21 2.428(3) . ? Hg21 N22 2.499(8) . ? N21 C21 1.343(13) . ? N21 C25 1.345(13) . ? N22 C26 1.248(12) . ? N22 C27 1.426(13) . ? C21 C22 1.367(14) . ? C21 C26 1.467(15) . ? C22 C23 1.357(17) . ? C22 H22 0.9300 . ? C23 C24 1.377(16) . ? C23 H23 0.9300 . ? C24 C25 1.363(14) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.383(15) . ? C27 C32 1.418(16) . ? C28 C29 1.363(17) . ? C28 H28 0.9300 . ? C29 C30 1.377(18) . ? C29 H29 0.9300 . ? C30 C31 1.385(18) . ? C30 H30 0.9300 . ? C31 C32 1.380(16) . ? C31 H31 0.9300 . ? C32 C33 1.504(17) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 Cl2 123.3(2) . . ? N1 Hg1 Cl1 127.7(2) . . ? Cl2 Hg1 Cl1 108.93(9) . . ? N1 Hg1 N2 70.8(3) . . ? Cl2 Hg1 N2 93.6(2) . . ? Cl1 Hg1 N2 108.17(19) . . ? Hg1 Cl1 Hg21 94.09(8) . . ? C1 N1 C5 119.0(8) . . ? C1 N1 Hg1 116.8(6) . . ? C5 N1 Hg1 123.9(6) . . ? C6 N2 C7 117.7(8) . . ? C6 N2 Hg1 109.2(6) . . ? C7 N2 Hg1 129.5(6) . . ? N1 C1 C2 120.0(9) . . ? N1 C1 C6 119.0(8) . . ? C2 C1 C6 121.0(9) . . ? C3 C2 C1 119.7(10) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 120.0(9) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.8(10) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.5(9) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C1 121.1(9) . . ? N2 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C12 C7 C8 121.3(10) . . ? C12 C7 N2 120.7(10) . . ? C8 C7 N2 117.9(10) . . ? C9 C8 C7 119.5(11) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 117.9(12) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C11 C10 C9 122.2(11) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 120.8(11) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 118.1(11) . . ? C11 C12 C13 121.2(11) . . ? C7 C12 C13 120.7(10) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N21 Hg21 Cl22 131.1(2) . . ? N21 Hg21 Cl21 103.3(2) . . ? Cl22 Hg21 Cl21 125.56(10) . . ? N21 Hg21 N22 68.5(3) . . ? Cl22 Hg21 N22 91.2(2) . . ? Cl21 Hg21 N22 114.8(2) . . ? N21 Hg21 Cl1 87.3(2) . . ? Cl22 Hg21 Cl1 92.66(9) . . ? Cl21 Hg21 Cl1 86.03(8) . . ? N22 Hg21 Cl1 150.6(2) . . ? C21 N21 C25 118.2(9) . . ? C21 N21 Hg21 118.2(7) . . ? C25 N21 Hg21 123.6(7) . . ? C26 N22 C27 120.5(9) . . ? C26 N22 Hg21 112.8(7) . . ? C27 N22 Hg21 121.7(6) . . ? N21 C21 C22 121.3(11) . . ? N21 C21 C26 116.8(9) . . ? C22 C21 C26 121.9(10) . . ? C23 C22 C21 120.3(11) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 118.7(11) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C25 C24 C23 119.1(11) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N21 C25 C24 122.3(10) . . ? N21 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N22 C26 C21 120.7(10) . . ? N22 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 121.5(11) . . ? C28 C27 N22 120.5(10) . . ? C32 C27 N22 117.7(9) . . ? C29 C28 C27 118.2(12) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 121.7(12) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 120.3(12) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 120.0(12) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 118.2(11) . . ? C31 C32 C33 120.3(12) . . ? C27 C32 C33 121.6(11) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 N1 Hg1 Cl1 Hg21 -90.8(3) . . . . ? Cl2 Hg1 Cl1 Hg21 89.28(9) . . . . ? N2 Hg1 Cl1 Hg21 -170.17(19) . . . . ? Cl2 Hg1 N1 C1 70.6(7) . . . . ? Cl1 Hg1 N1 C1 -109.3(6) . . . . ? N2 Hg1 N1 C1 -10.8(6) . . . . ? Cl2 Hg1 N1 C5 -102.5(7) . . . . ? Cl1 Hg1 N1 C5 77.6(8) . . . . ? N2 Hg1 N1 C5 176.1(8) . . . . ? N1 Hg1 N2 C6 15.2(7) . . . . ? Cl2 Hg1 N2 C6 -108.9(7) . . . . ? Cl1 Hg1 N2 C6 139.8(6) . . . . ? N1 Hg1 N2 C7 172.7(9) . . . . ? Cl2 Hg1 N2 C7 48.6(8) . . . . ? Cl1 Hg1 N2 C7 -62.7(8) . . . . ? C5 N1 C1 C2 -0.4(14) . . . . ? Hg1 N1 C1 C2 -173.9(7) . . . . ? C5 N1 C1 C6 179.9(9) . . . . ? Hg1 N1 C1 C6 6.4(11) . . . . ? N1 C1 C2 C3 -1.2(15) . . . . ? C6 C1 C2 C3 178.5(9) . . . . ? C1 C2 C3 C4 1.3(16) . . . . ? C2 C3 C4 C5 0.3(15) . . . . ? C1 N1 C5 C4 2.1(14) . . . . ? Hg1 N1 C5 C4 175.1(7) . . . . ? C3 C4 C5 N1 -2.1(15) . . . . ? C7 N2 C6 C1 -178.7(9) . . . . ? Hg1 N2 C6 C1 -18.1(11) . . . . ? N1 C1 C6 N2 9.8(15) . . . . ? C2 C1 C6 N2 -169.9(9) . . . . ? C6 N2 C7 C12 -122.2(10) . . . . ? Hg1 N2 C7 C12 81.9(11) . . . . ? C6 N2 C7 C8 60.1(13) . . . . ? Hg1 N2 C7 C8 -95.9(10) . . . . ? C12 C7 C8 C9 0.9(15) . . . . ? N2 C7 C8 C9 178.6(9) . . . . ? C7 C8 C9 C10 0.7(16) . . . . ? C8 C9 C10 C11 -1.0(18) . . . . ? C9 C10 C11 C12 -0.2(18) . . . . ? C10 C11 C12 C7 1.8(16) . . . . ? C10 C11 C12 C13 -177.9(10) . . . . ? C8 C7 C12 C11 -2.1(15) . . . . ? N2 C7 C12 C11 -179.8(9) . . . . ? C8 C7 C12 C13 177.5(10) . . . . ? N2 C7 C12 C13 -0.2(15) . . . . ? Hg1 Cl1 Hg21 N21 -92.6(2) . . . . ? Hg1 Cl1 Hg21 Cl22 136.37(10) . . . . ? Hg1 Cl1 Hg21 Cl21 10.89(9) . . . . ? Hg1 Cl1 Hg21 N22 -126.4(4) . . . . ? Cl22 Hg21 N21 C21 -64.2(8) . . . . ? Cl21 Hg21 N21 C21 119.4(7) . . . . ? N22 Hg21 N21 C21 7.6(7) . . . . ? Cl1 Hg21 N21 C21 -155.3(7) . . . . ? Cl22 Hg21 N21 C25 117.0(7) . . . . ? Cl21 Hg21 N21 C25 -59.4(8) . . . . ? N22 Hg21 N21 C25 -171.2(8) . . . . ? Cl1 Hg21 N21 C25 25.9(8) . . . . ? N21 Hg21 N22 C26 -14.3(7) . . . . ? Cl22 Hg21 N22 C26 119.9(7) . . . . ? Cl21 Hg21 N22 C26 -109.5(7) . . . . ? Cl1 Hg21 N22 C26 22.3(10) . . . . ? N21 Hg21 N22 C27 -169.3(8) . . . . ? Cl22 Hg21 N22 C27 -35.1(7) . . . . ? Cl21 Hg21 N22 C27 95.5(7) . . . . ? Cl1 Hg21 N22 C27 -132.7(7) . . . . ? C25 N21 C21 C22 -4.9(15) . . . . ? Hg21 N21 C21 C22 176.3(8) . . . . ? C25 N21 C21 C26 177.5(9) . . . . ? Hg21 N21 C21 C26 -1.4(11) . . . . ? N21 C21 C22 C23 5.2(17) . . . . ? C26 C21 C22 C23 -177.3(10) . . . . ? C21 C22 C23 C24 -2.3(17) . . . . ? C22 C23 C24 C25 -0.5(17) . . . . ? C21 N21 C25 C24 1.9(15) . . . . ? Hg21 N21 C25 C24 -179.3(8) . . . . ? C23 C24 C25 N21 0.8(17) . . . . ? C27 N22 C26 C21 175.1(9) . . . . ? Hg21 N22 C26 C21 19.7(12) . . . . ? N21 C21 C26 N22 -13.6(15) . . . . ? C22 C21 C26 N22 168.8(11) . . . . ? C26 N22 C27 C28 -54.0(14) . . . . ? Hg21 N22 C27 C28 99.2(10) . . . . ? C26 N22 C27 C32 131.8(11) . . . . ? Hg21 N22 C27 C32 -75.1(11) . . . . ? C32 C27 C28 C29 2.7(17) . . . . ? N22 C27 C28 C29 -171.4(10) . . . . ? C27 C28 C29 C30 -1.4(19) . . . . ? C28 C29 C30 C31 0(2) . . . . ? C29 C30 C31 C32 -0.5(18) . . . . ? C30 C31 C32 C27 1.8(17) . . . . ? C30 C31 C32 C33 -177.2(11) . . . . ? C28 C27 C32 C31 -2.9(16) . . . . ? N22 C27 C32 C31 171.3(10) . . . . ? C28 C27 C32 C33 176.0(11) . . . . ? N22 C27 C32 C33 -9.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.381 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.287 _iucr_refine_instructions_details ; TITL tu1dosm in P-1 CELL 0.71073 8.2038 13.8179 14.4494 115.149 99.505 100.406 ZERR 2.00 0.0011 0.0019 0.0019 0.002 0.002 0.002 LATT 1 SFAC C H N Cl Hg UNIT 52 48 8 8 4 OMIT -3.00 50.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 size 0.15 0.16 0.20 conf TEMP 20 WGHT 0.058500 FVAR 0.27989 HG1 5 0.766959 0.134823 0.692354 11.00000 0.05849 0.04289 = 0.04496 0.02293 0.02553 0.01852 CL1 4 0.878000 0.085856 0.831786 11.00000 0.05472 0.03744 = 0.03883 0.01724 0.00920 0.01436 CL2 4 0.550716 0.229125 0.741229 11.00000 0.05120 0.03969 = 0.05637 0.01737 0.01383 0.02042 N1 3 0.847005 0.100660 0.541899 11.00000 0.04004 0.02971 = 0.03226 0.01391 0.01229 0.00710 N2 3 0.979739 0.306883 0.720497 11.00000 0.04316 0.02963 = 0.03096 0.01125 0.00675 0.00639 C1 1 0.937699 0.188845 0.537318 11.00000 0.03819 0.04172 = 0.03142 0.01748 0.01052 0.01616 C2 1 0.977713 0.175743 0.442989 11.00000 0.04627 0.03796 = 0.04689 0.01738 0.01379 0.00416 AFIX 43 H2 2 1.038683 0.236989 0.439201 11.00000 -1.20000 AFIX 0 C3 1 0.926222 0.071334 0.355405 11.00000 0.05010 0.05844 = 0.02817 0.01815 0.01541 0.01426 AFIX 43 H3 2 0.954503 0.062028 0.292995 11.00000 -1.20000 AFIX 0 C4 1 0.835758 -0.016262 0.360435 11.00000 0.04199 0.04803 = 0.02657 0.01042 0.00745 0.01427 AFIX 43 H4 2 0.801119 -0.086844 0.302061 11.00000 -1.20000 AFIX 0 C5 1 0.794647 0.000093 0.454155 11.00000 0.03976 0.03982 = 0.03025 0.01542 0.00293 0.00605 AFIX 43 H5 2 0.728525 -0.060353 0.456890 11.00000 -1.20000 AFIX 0 C6 1 0.993935 0.297388 0.631785 11.00000 0.04876 0.03383 = 0.03489 0.01424 0.00732 0.00482 AFIX 43 H6 2 1.041063 0.360639 0.626411 11.00000 -1.20000 AFIX 0 C7 1 1.034939 0.417528 0.809619 11.00000 0.05100 0.03188 = 0.03884 0.01300 0.02133 0.00194 C8 1 0.953504 0.495520 0.803135 11.00000 0.05882 0.05126 = 0.04322 0.02614 0.02266 0.01999 AFIX 43 H8 2 0.868228 0.476344 0.742268 11.00000 -1.20000 AFIX 0 C9 1 1.000497 0.601775 0.887989 11.00000 0.09173 0.04253 = 0.06456 0.02885 0.04737 0.02922 AFIX 43 H9 2 0.947087 0.654970 0.885786 11.00000 -1.20000 AFIX 0 C10 1 1.127982 0.626082 0.975197 11.00000 0.07740 0.03361 = 0.04822 0.00454 0.02300 -0.00261 AFIX 43 H10 2 1.162220 0.697479 1.032341 11.00000 -1.20000 AFIX 0 C11 1 1.206222 0.549408 0.981103 11.00000 0.05046 0.03500 = 0.03995 0.00905 0.01029 0.00272 AFIX 43 H11 2 1.292638 0.569310 1.041707 11.00000 -1.20000 AFIX 0 C12 1 1.159540 0.443371 0.899096 11.00000 0.04961 0.04432 = 0.02700 0.00770 0.01982 0.01215 C13 1 1.239827 0.358367 0.906421 11.00000 0.04882 0.06126 = 0.06778 0.03051 0.02152 0.01842 AFIX 137 H13A 2 1.313536 0.387975 0.976823 11.00000 -1.50000 H13B 2 1.306478 0.338451 0.855972 11.00000 -1.50000 H13C 2 1.151588 0.293493 0.891225 11.00000 -1.50000 AFIX 0 HG21 5 0.614276 -0.134668 0.731092 11.00000 0.05328 0.04611 = 0.05682 0.03150 0.02346 0.01965 CL21 4 0.542937 -0.103837 0.577783 11.00000 0.05829 0.05125 = 0.04775 0.02812 0.01301 0.01339 CL22 4 0.821386 -0.226183 0.761097 11.00000 0.05646 0.05359 = 0.07504 0.03534 0.01643 0.02495 N21 3 0.447074 -0.045208 0.837345 11.00000 0.04365 0.04278 = 0.03334 0.01731 0.00862 0.01480 N22 3 0.381665 -0.271173 0.741220 11.00000 0.05269 0.04064 = 0.04028 0.02411 0.01231 0.01105 C21 1 0.329816 -0.106583 0.860294 11.00000 0.04001 0.05150 = 0.04132 0.02322 0.01540 0.01735 C22 1 0.234437 -0.058685 0.926839 11.00000 0.04288 0.07128 = 0.05087 0.03006 0.01308 0.01151 AFIX 43 H22 2 0.160701 -0.101747 0.946162 11.00000 -1.20000 AFIX 0 C23 1 0.246877 0.051363 0.964800 11.00000 0.06017 0.07239 = 0.04026 0.01461 0.01563 0.02951 AFIX 43 H23 2 0.179281 0.083817 1.008027 11.00000 -1.20000 AFIX 0 C24 1 0.361610 0.114053 0.938040 11.00000 0.06436 0.04390 = 0.05412 0.01992 0.01735 0.02566 AFIX 43 H24 2 0.372043 0.189546 0.962473 11.00000 -1.20000 AFIX 0 C25 1 0.459675 0.063966 0.875263 11.00000 0.04969 0.03773 = 0.05598 0.02634 0.01598 0.01418 AFIX 43 H25 2 0.538007 0.106755 0.858051 11.00000 -1.20000 AFIX 0 C26 1 0.314321 -0.226212 0.813990 11.00000 0.04947 0.04685 = 0.04383 0.02548 0.01528 0.01201 AFIX 43 H26 2 0.253674 -0.268993 0.839130 11.00000 -1.20000 AFIX 0 C27 1 0.377847 -0.385485 0.702207 11.00000 0.04619 0.03834 = 0.04556 0.02245 0.02222 0.00733 C28 1 0.438573 -0.424351 0.771076 11.00000 0.08203 0.05747 = 0.06907 0.04163 0.02683 0.01323 AFIX 43 H28 2 0.468310 -0.379465 0.844250 11.00000 -1.20000 AFIX 0 C29 1 0.453663 -0.530198 0.728823 11.00000 0.06140 0.06190 = 0.09522 0.05408 0.01396 0.01736 AFIX 43 H29 2 0.496666 -0.556830 0.774179 11.00000 -1.20000 AFIX 0 C30 1 0.406894 -0.598735 0.620724 11.00000 0.06892 0.03499 = 0.11048 0.03961 0.03832 0.01739 AFIX 43 H30 2 0.418064 -0.670710 0.594148 11.00000 -1.20000 AFIX 0 C31 1 0.343297 -0.560905 0.551439 11.00000 0.07155 0.04254 = 0.06248 0.01559 0.03503 0.00722 AFIX 43 H31 2 0.312780 -0.607253 0.478497 11.00000 -1.20000 AFIX 0 C32 1 0.325199 -0.454490 0.590586 11.00000 0.04275 0.05284 = 0.07205 0.03461 0.02501 0.01132 C33 1 0.248596 -0.414773 0.515969 11.00000 0.10374 0.07041 = 0.06001 0.03181 0.02326 0.01546 AFIX 137 H33A 2 0.223279 -0.472163 0.444003 11.00000 -1.50000 H33B 2 0.329191 -0.349238 0.525714 11.00000 -1.50000 H33C 2 0.144428 -0.397567 0.530564 11.00000 -1.50000 HKLF 4 REM tu1dosm in P-1 REM R1 = 0.0402 for 3716 Fo > 4sig(Fo) and 0.0608 for all 4934 data REM 327 parameters refined using 0 restraints END WGHT 0.0586 0.0000 REM Highest difference peak 1.381, deepest hole -1.078, 1-sigma level 0.287 Q1 1 0.7960 0.1830 0.7635 11.00000 0.05 1.38 Q2 1 0.6566 -0.0985 0.8044 11.00000 0.05 1.17 Q3 1 0.6984 0.1223 0.6295 11.00000 0.05 1.16 Q4 1 0.5984 -0.2056 0.7016 11.00000 0.05 0.93 Q5 1 0.5672 -0.1843 0.6482 11.00000 0.05 0.88 Q6 1 1.1263 0.4976 0.9438 11.00000 0.05 0.81 Q7 1 0.9521 0.4555 0.9109 11.00000 0.05 0.80 Q8 1 1.0174 0.6079 0.9406 11.00000 0.05 0.80 Q9 1 0.4967 -0.4083 0.7387 11.00000 0.05 0.78 Q10 1 1.1305 0.3803 0.8259 11.00000 0.05 0.77 Q11 1 0.2213 -0.4225 0.7952 11.00000 0.05 0.77 Q12 1 1.0728 0.4230 0.8714 11.00000 0.05 0.77 Q13 1 1.1039 0.5308 0.8258 11.00000 0.05 0.75 Q14 1 1.1418 0.4506 0.8303 11.00000 0.05 0.74 Q15 1 1.2056 0.4915 0.6951 11.00000 0.05 0.73 Q16 1 0.9162 0.5228 0.8487 11.00000 0.05 0.73 Q17 1 1.2534 0.4164 1.0608 11.00000 0.05 0.73 Q18 1 1.0432 0.4864 0.8168 11.00000 0.05 0.73 Q19 1 0.8207 0.4147 0.8388 11.00000 0.05 0.73 Q20 1 0.4207 -0.5567 0.8255 11.00000 0.05 0.73 ; data_4b _database_code_depnum_ccdc_archive 'CCDC 892208' #TrackingRef '4b.cif' # tu1einm _vrf_PLAT973_4b ; PROBLEM: Large Calcd. Positive Residual Density on Hg41 1.63 eA-3 RESPONSE: The structure has a particularly heavy atom, Hg and large residuals are often encountered. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl4 Hg2 N4' _chemical_formula_sum 'C26 H24 Cl4 Hg2 N4' _chemical_formula_weight 935.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0247(16) _cell_length_b 14.3877(19) _cell_length_c 17.542(2) _cell_angle_alpha 78.370(2) _cell_angle_beta 83.453(2) _cell_angle_gamma 78.383(2) _cell_volume 2903.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3040 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 21.88 _exptl_crystal_description 'rhombohedral prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 10.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.20 _exptl_absorpt_correction_T_max 0.29 _exptl_absorpt_process_details SADABS _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 '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 28274 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10210 _reflns_number_gt 5153 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0046P)^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 10210 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 0.99207(3) 0.77077(2) 0.69117(2) 0.05946(13) Uani 1 1 d . . . Cl1 Cl 0.94330(16) 0.83672(15) 0.55910(12) 0.0634(7) Uani 1 1 d . . . Cl2 Cl 1.11175(16) 0.62425(15) 0.74439(13) 0.0680(7) Uani 1 1 d . . . N1 N 0.8752(6) 0.8576(4) 0.7806(4) 0.0501(19) Uani 1 1 d . . . N2 N 1.1010(5) 0.8716(4) 0.7425(4) 0.0413(17) Uani 1 1 d . . . C1 C 0.9257(7) 0.9096(5) 0.8174(5) 0.049(2) Uani 1 1 d . . . C2 C 0.8638(7) 0.9574(6) 0.8739(5) 0.057(3) Uani 1 1 d . . . H2 H 0.9002 0.9910 0.9005 0.069 Uiso 1 1 calc R . . C3 C 0.7484(8) 0.9563(6) 0.8919(5) 0.070(3) Uani 1 1 d . . . H3 H 0.7069 0.9894 0.9294 0.084 Uiso 1 1 calc R . . C4 C 0.6989(7) 0.9060(6) 0.8534(5) 0.067(3) Uani 1 1 d . . . H4 H 0.6218 0.9039 0.8639 0.080 Uiso 1 1 calc R . . C5 C 0.7636(8) 0.8566(6) 0.7973(5) 0.062(3) Uani 1 1 d . . . H5 H 0.7282 0.8222 0.7709 0.075 Uiso 1 1 calc R . . C6 C 1.0467(7) 0.9102(5) 0.7991(5) 0.052(2) Uani 1 1 d . . . H6 H 1.0850 0.9387 0.8286 0.062 Uiso 1 1 calc R . . C7 C 1.2203(8) 0.8649(6) 0.7302(6) 0.049(2) Uani 1 1 d . . . C8 C 1.2854(8) 0.8359(6) 0.7937(6) 0.073(3) Uani 1 1 d . . . H8 H 1.2506 0.8262 0.8441 0.088 Uiso 1 1 calc R . . C9 C 1.4047(10) 0.8210(7) 0.7816(8) 0.100(4) Uani 1 1 d . . . H9 H 1.4495 0.8049 0.8238 0.120 Uiso 1 1 calc R . . C10 C 1.4539(10) 0.8306(7) 0.7068(9) 0.091(4) Uani 1 1 d . . . H10 H 1.5329 0.8181 0.6987 0.110 Uiso 1 1 calc R . . C11 C 1.3903(11) 0.8580(8) 0.6440(7) 0.097(4) Uani 1 1 d . . . H11 H 1.4261 0.8640 0.5938 0.116 Uiso 1 1 calc R . . C12 C 1.2729(10) 0.8770(6) 0.6545(6) 0.069(3) Uani 1 1 d . . . C13 C 1.2028(8) 0.9127(8) 0.5860(5) 0.121(4) Uani 1 1 d . . . H13A H 1.1618 0.8640 0.5805 0.181 Uiso 1 1 calc R . . H13B H 1.2516 0.9270 0.5397 0.181 Uiso 1 1 calc R . . H13C H 1.1498 0.9701 0.5940 0.181 Uiso 1 1 calc R . . Hg21 Hg 0.74904(3) 0.72810(3) 0.56069(2) 0.05997(12) Uani 1 1 d . . . Cl21 Cl 0.78628(16) 0.66367(15) 0.69511(12) 0.0630(7) Uani 1 1 d . . . Cl22 Cl 0.63557(15) 0.87361(14) 0.49831(12) 0.0604(6) Uani 1 1 d . . . N21 N 0.8741(6) 0.6437(5) 0.4753(4) 0.058(2) Uani 1 1 d . . . N22 N 0.6474(6) 0.6300(4) 0.4988(4) 0.0498(19) Uani 1 1 d . . . C21 C 0.8306(8) 0.6003(6) 0.4297(5) 0.058(3) Uani 1 1 d . . . C22 C 0.8965(9) 0.5513(6) 0.3740(5) 0.081(3) Uani 1 1 d . . . H22 H 0.8620 0.5224 0.3425 0.097 Uiso 1 1 calc R . . C23 C 1.0102(10) 0.5462(7) 0.3662(6) 0.089(4) Uani 1 1 d . . . H23 H 1.0552 0.5145 0.3290 0.107 Uiso 1 1 calc R . . C24 C 1.0569(8) 0.5877(7) 0.4130(6) 0.086(3) Uani 1 1 d . . . H24 H 1.1354 0.5833 0.4100 0.104 Uiso 1 1 calc R . . C25 C 0.9864(8) 0.6381(6) 0.4669(5) 0.068(3) Uani 1 1 d . . . H25 H 1.0197 0.6687 0.4977 0.081 Uiso 1 1 calc R . . C26 C 0.7090(9) 0.6012(5) 0.4409(5) 0.065(3) Uani 1 1 d . . . H26 H 0.6746 0.5798 0.4044 0.078 Uiso 1 1 calc R . . C27 C 0.5280(10) 0.6358(6) 0.5077(6) 0.066(3) Uani 1 1 d . . . C28 C 0.4605(10) 0.6711(6) 0.4428(6) 0.083(3) Uani 1 1 d . . . H28 H 0.4933 0.6869 0.3924 0.100 Uiso 1 1 calc R . . C29 C 0.3399(12) 0.6810(8) 0.4586(10) 0.125(5) Uani 1 1 d . . . H29 H 0.2939 0.7052 0.4173 0.150 Uiso 1 1 calc R . . C30 C 0.2886(14) 0.6563(12) 0.5328(12) 0.142(7) Uani 1 1 d . . . H30 H 0.2099 0.6629 0.5415 0.170 Uiso 1 1 calc R . . C31 C 0.3552(12) 0.6233(9) 0.5903(9) 0.116(5) Uani 1 1 d . . . H31 H 0.3209 0.6076 0.6403 0.140 Uiso 1 1 calc R . . C32 C 0.4743(10) 0.6099(7) 0.5815(6) 0.073(3) Uani 1 1 d . . . C33 C 0.5427(8) 0.5654(8) 0.6516(6) 0.123(4) Uani 1 1 d . . . H33A H 0.6224 0.5612 0.6359 0.184 Uiso 1 1 calc R . . H33B H 0.5270 0.5020 0.6724 0.184 Uiso 1 1 calc R . . H33C H 0.5220 0.6050 0.6908 0.184 Uiso 1 1 calc R . . Hg41 Hg 0.53509(3) 0.77447(3) 0.18645(2) 0.06002(12) Uani 1 1 d . . . Cl41 Cl 0.48105(17) 0.84986(16) 0.05672(12) 0.0714(7) Uani 1 1 d . . . Cl42 Cl 0.64342(16) 0.62106(15) 0.23483(13) 0.0710(7) Uani 1 1 d . . . N41 N 0.4157(6) 0.8674(4) 0.2695(4) 0.0516(19) Uani 1 1 d . . . N42 N 0.6484(5) 0.8666(4) 0.2462(4) 0.0471(19) Uani 1 1 d . . . C41 C 0.4632(7) 0.9180(6) 0.3095(5) 0.044(2) Uani 1 1 d . . . C42 C 0.3996(7) 0.9702(6) 0.3629(5) 0.062(3) Uani 1 1 d . . . H42 H 0.4348 1.0026 0.3912 0.074 Uiso 1 1 calc R . . C43 C 0.2836(7) 0.9736(5) 0.3736(5) 0.056(2) Uani 1 1 d . . . H43 H 0.2401 1.0087 0.4092 0.067 Uiso 1 1 calc R . . C44 C 0.2318(7) 0.9246(6) 0.3315(5) 0.066(3) Uani 1 1 d . . . H44 H 0.1535 0.9265 0.3368 0.079 Uiso 1 1 calc R . . C45 C 0.3034(7) 0.8727(6) 0.2810(5) 0.057(3) Uani 1 1 d . . . H45 H 0.2703 0.8388 0.2527 0.068 Uiso 1 1 calc R . . C46 C 0.5872(7) 0.9132(5) 0.2959(5) 0.054(2) Uani 1 1 d . . . H46 H 0.6224 0.9452 0.3245 0.064 Uiso 1 1 calc R . . C47 C 0.7705(7) 0.8567(6) 0.2418(6) 0.054(2) Uani 1 1 d . . . C48 C 0.8263(8) 0.8447(6) 0.3091(6) 0.071(3) Uani 1 1 d . . . H48 H 0.7844 0.8478 0.3568 0.085 Uiso 1 1 calc R . . C49 C 0.9433(8) 0.8282(6) 0.3054(7) 0.083(3) Uani 1 1 d . . . H49 H 0.9812 0.8193 0.3505 0.100 Uiso 1 1 calc R . . C50 C 1.0041(9) 0.8252(7) 0.2334(9) 0.096(4) Uani 1 1 d . . . H50 H 1.0833 0.8147 0.2302 0.116 Uiso 1 1 calc R . . C51 C 0.9495(10) 0.8373(8) 0.1684(7) 0.093(4) Uani 1 1 d . . . H51 H 0.9918 0.8338 0.1209 0.112 Uiso 1 1 calc R . . C52 C 0.8320(9) 0.8546(6) 0.1704(6) 0.063(3) Uani 1 1 d . . . C53 C 0.7752(7) 0.8745(7) 0.0962(5) 0.099(3) Uani 1 1 d . . . H53A H 0.7341 0.8240 0.0958 0.148 Uiso 1 1 calc R . . H53B H 0.8316 0.8773 0.0529 0.148 Uiso 1 1 calc R . . H53C H 0.7233 0.9351 0.0923 0.148 Uiso 1 1 calc R . . Hg61 Hg 0.28285(3) 0.73533(3) 0.05784(2) 0.06337(12) Uani 1 1 d . . . Cl61 Cl 0.32340(17) 0.67264(15) 0.19084(12) 0.0664(7) Uani 1 1 d . . . Cl62 Cl 0.16245(17) 0.87552(15) -0.00530(13) 0.0727(7) Uani 1 1 d . . . N61 N 0.4101(6) 0.6531(5) -0.0303(4) 0.0488(19) Uani 1 1 d . . . N62 N 0.1882(6) 0.6285(4) 0.0004(4) 0.055(2) Uani 1 1 d . . . C61 C 0.3688(8) 0.6026(6) -0.0722(5) 0.054(2) Uani 1 1 d . . . C62 C 0.4366(8) 0.5557(6) -0.1274(5) 0.065(3) Uani 1 1 d . . . H62 H 0.4048 0.5224 -0.1570 0.078 Uiso 1 1 calc R . . C63 C 0.5519(8) 0.5586(7) -0.1384(5) 0.081(3) Uani 1 1 d . . . H63 H 0.5985 0.5283 -0.1757 0.097 Uiso 1 1 calc R . . C64 C 0.5944(7) 0.6071(6) -0.0930(5) 0.069(3) Uani 1 1 d . . . H64 H 0.6718 0.6091 -0.0974 0.083 Uiso 1 1 calc R . . C65 C 0.5201(8) 0.6540(6) -0.0396(5) 0.077(3) Uani 1 1 d . . . H65 H 0.5498 0.6877 -0.0092 0.092 Uiso 1 1 calc R . . C66 C 0.2475(8) 0.5985(5) -0.0579(5) 0.059(3) Uani 1 1 d . . . H66 H 0.2129 0.5734 -0.0920 0.071 Uiso 1 1 calc R . . C67 C 0.0678(9) 0.6284(6) 0.0108(6) 0.058(3) Uani 1 1 d . . . C68 C 0.0017(9) 0.6633(6) -0.0535(6) 0.073(3) Uani 1 1 d . . . H68 H 0.0365 0.6828 -0.1027 0.088 Uiso 1 1 calc R . . C69 C -0.1124(10) 0.6688(7) -0.0440(7) 0.090(4) Uani 1 1 d . . . H69 H -0.1559 0.6922 -0.0867 0.108 Uiso 1 1 calc R . . C70 C -0.1658(8) 0.6391(7) 0.0302(8) 0.080(3) Uani 1 1 d . . . H70 H -0.2443 0.6431 0.0370 0.096 Uiso 1 1 calc R . . C71 C -0.0990(9) 0.6040(6) 0.0927(6) 0.074(3) Uani 1 1 d . . . H71 H -0.1333 0.5841 0.1420 0.088 Uiso 1 1 calc R . . C72 C 0.0190(8) 0.5980(6) 0.0831(6) 0.053(2) Uani 1 1 d . . . C73 C 0.0857(7) 0.5571(7) 0.1533(5) 0.091(3) Uani 1 1 d . . . H73A H 0.1583 0.5772 0.1444 0.136 Uiso 1 1 calc R . . H73B H 0.0970 0.4879 0.1623 0.136 Uiso 1 1 calc R . . H73C H 0.0446 0.5801 0.1981 0.136 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 0.0678(3) 0.0605(3) 0.0534(3) -0.0224(2) -0.0062(2) -0.0069(2) Cl1 0.0674(15) 0.0729(17) 0.0524(16) -0.0169(14) -0.0072(11) -0.0123(12) Cl2 0.0757(16) 0.0545(16) 0.0739(18) -0.0202(14) -0.0090(12) -0.0015(12) N1 0.046(5) 0.055(5) 0.054(5) -0.026(4) -0.004(4) -0.004(4) N2 0.042(5) 0.043(4) 0.040(5) -0.008(4) 0.003(3) -0.015(3) C1 0.056(6) 0.042(6) 0.055(6) -0.030(5) -0.009(5) -0.001(5) C2 0.057(6) 0.069(7) 0.053(6) -0.026(5) -0.010(5) -0.009(5) C3 0.083(8) 0.070(7) 0.057(7) -0.034(6) -0.005(6) 0.009(6) C4 0.062(7) 0.061(7) 0.070(8) -0.022(6) -0.004(5) 0.014(5) C5 0.074(7) 0.056(7) 0.065(7) -0.019(5) -0.026(6) -0.012(5) C6 0.043(6) 0.054(6) 0.062(7) -0.025(5) -0.009(5) 0.001(4) C7 0.054(7) 0.041(6) 0.049(7) -0.008(5) 0.009(6) -0.008(5) C8 0.056(7) 0.072(7) 0.074(8) 0.019(6) 0.010(6) -0.010(6) C9 0.076(10) 0.085(9) 0.134(13) 0.020(8) -0.028(8) -0.031(7) C10 0.083(10) 0.039(7) 0.148(15) -0.008(8) 0.021(10) -0.027(6) C11 0.084(10) 0.104(10) 0.111(12) -0.043(9) 0.041(8) -0.039(8) C12 0.092(9) 0.061(7) 0.068(9) -0.031(6) 0.014(7) -0.042(6) C13 0.119(9) 0.217(13) 0.055(8) -0.033(8) 0.019(7) -0.105(9) Hg21 0.0683(3) 0.0642(3) 0.0511(3) -0.0229(2) -0.00616(19) -0.0074(2) Cl21 0.0724(16) 0.0742(17) 0.0444(15) -0.0127(13) -0.0062(11) -0.0151(12) Cl22 0.0627(14) 0.0599(16) 0.0580(16) -0.0196(13) -0.0066(11) 0.0003(11) N21 0.060(5) 0.068(5) 0.053(5) -0.027(4) -0.011(4) -0.008(4) N22 0.056(5) 0.051(5) 0.048(5) -0.015(4) 0.000(4) -0.020(4) C21 0.050(6) 0.068(7) 0.052(7) -0.022(6) -0.006(5) 0.008(5) C22 0.125(9) 0.059(7) 0.056(7) -0.032(6) -0.012(7) 0.012(7) C23 0.090(9) 0.077(8) 0.082(9) -0.033(7) 0.015(7) 0.036(7) C24 0.081(8) 0.095(9) 0.084(9) -0.037(7) 0.003(6) 0.000(6) C25 0.078(8) 0.057(7) 0.065(8) -0.016(6) -0.013(6) 0.002(6) C26 0.115(9) 0.048(6) 0.041(7) -0.023(5) -0.022(6) -0.010(6) C27 0.100(9) 0.047(6) 0.053(8) -0.001(6) -0.003(7) -0.030(6) C28 0.080(9) 0.091(8) 0.073(9) 0.008(7) -0.002(7) -0.028(6) C29 0.076(11) 0.086(9) 0.217(18) -0.006(11) -0.052(10) -0.025(8) C30 0.093(14) 0.143(14) 0.21(2) -0.053(15) 0.021(13) -0.062(11) C31 0.097(12) 0.135(13) 0.150(15) -0.078(12) 0.038(9) -0.073(10) C32 0.082(9) 0.091(8) 0.061(9) -0.026(7) 0.012(7) -0.051(7) C33 0.153(10) 0.179(12) 0.072(9) -0.037(9) 0.007(8) -0.109(9) Hg41 0.0682(3) 0.0589(3) 0.0568(3) -0.0251(2) -0.00685(18) -0.00487(19) Cl41 0.0823(17) 0.0781(18) 0.0528(16) -0.0171(14) -0.0112(12) -0.0039(13) Cl42 0.0677(15) 0.0618(16) 0.0855(19) -0.0203(14) -0.0162(12) -0.0038(12) N41 0.055(5) 0.056(5) 0.046(5) -0.021(4) -0.002(4) -0.005(4) N42 0.054(5) 0.037(5) 0.053(5) -0.018(4) 0.002(4) -0.010(4) C41 0.045(6) 0.049(6) 0.042(6) -0.013(5) -0.004(4) -0.014(5) C42 0.070(7) 0.067(7) 0.053(6) -0.037(5) -0.004(5) 0.003(5) C43 0.057(7) 0.045(6) 0.055(6) -0.012(5) 0.006(5) 0.010(5) C44 0.063(7) 0.056(7) 0.079(8) -0.025(6) -0.002(5) -0.001(5) C45 0.049(6) 0.059(7) 0.068(7) -0.022(5) -0.008(5) -0.010(5) C46 0.059(6) 0.057(6) 0.052(6) -0.023(5) -0.008(5) -0.012(5) C47 0.040(6) 0.052(6) 0.075(8) -0.028(6) 0.001(6) -0.009(4) C48 0.060(7) 0.072(7) 0.091(9) -0.031(6) -0.003(6) -0.020(5) C49 0.044(7) 0.083(8) 0.125(11) -0.016(7) -0.028(6) -0.009(6) C50 0.052(8) 0.083(8) 0.157(14) -0.045(9) 0.031(8) -0.018(6) C51 0.075(9) 0.113(10) 0.105(11) -0.050(8) 0.039(7) -0.044(7) C52 0.075(8) 0.063(7) 0.056(7) -0.026(6) 0.015(6) -0.020(5) C53 0.112(8) 0.127(10) 0.072(8) -0.047(7) 0.024(6) -0.046(7) Hg61 0.0694(3) 0.0709(3) 0.0543(3) -0.0271(2) -0.00563(19) -0.0071(2) Cl61 0.0812(16) 0.0665(17) 0.0589(17) -0.0231(14) -0.0158(12) -0.0133(12) Cl62 0.0840(17) 0.0653(17) 0.0683(18) -0.0255(14) -0.0112(13) 0.0036(13) N61 0.052(5) 0.056(5) 0.043(5) -0.020(4) -0.005(4) -0.009(4) N62 0.071(6) 0.047(5) 0.057(6) -0.017(4) -0.007(4) -0.024(4) C61 0.076(7) 0.045(6) 0.045(6) -0.013(5) -0.007(5) -0.014(5) C62 0.097(8) 0.056(7) 0.049(7) -0.027(5) 0.008(6) -0.020(6) C63 0.080(8) 0.080(8) 0.076(8) -0.035(6) 0.010(6) 0.012(6) C64 0.072(7) 0.074(7) 0.067(7) -0.034(6) 0.005(5) -0.008(5) C65 0.078(7) 0.101(8) 0.062(7) -0.052(6) -0.009(6) 0.000(6) C66 0.104(8) 0.047(6) 0.034(6) -0.013(5) -0.004(5) -0.026(6) C67 0.086(8) 0.046(6) 0.049(8) -0.014(6) -0.019(7) -0.017(6) C68 0.092(8) 0.088(8) 0.049(7) -0.006(6) -0.005(6) -0.042(7) C69 0.105(10) 0.085(8) 0.087(10) 0.008(7) -0.039(8) -0.041(7) C70 0.055(7) 0.057(7) 0.131(12) -0.007(7) -0.022(8) -0.018(5) C71 0.076(8) 0.066(7) 0.075(8) -0.014(6) 0.015(6) -0.016(6) C72 0.055(7) 0.050(6) 0.059(8) -0.015(5) 0.007(6) -0.020(5) C73 0.087(7) 0.134(10) 0.056(7) -0.019(7) -0.014(6) -0.025(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 2.362(6) . ? Hg1 Cl2 2.383(2) . ? Hg1 Cl1 2.411(2) . ? Hg1 N2 2.489(6) . ? N1 C5 1.343(8) . ? N1 C1 1.347(8) . ? N2 C6 1.284(8) . ? N2 C7 1.413(8) . ? C1 C2 1.382(9) . ? C1 C6 1.455(9) . ? C2 C3 1.390(9) . ? C2 H2 0.9300 . ? C3 C4 1.340(10) . ? C3 H3 0.9300 . ? C4 C5 1.401(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.381(10) . ? C7 C12 1.398(11) . ? C8 C9 1.405(11) . ? C8 H8 0.9300 . ? C9 C10 1.368(13) . ? C9 H9 0.9300 . ? C10 C11 1.360(13) . ? C10 H10 0.9300 . ? C11 C12 1.382(12) . ? C11 H11 0.9300 . ? C12 C13 1.491(11) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Hg21 N21 2.338(6) . ? Hg21 Cl22 2.389(2) . ? Hg21 Cl21 2.411(2) . ? Hg21 N22 2.507(6) . ? N21 C21 1.315(9) . ? N21 C25 1.329(9) . ? N22 C26 1.275(8) . ? N22 C27 1.414(10) . ? C21 C22 1.398(10) . ? C21 C26 1.451(10) . ? C22 C23 1.347(11) . ? C22 H22 0.9300 . ? C23 C24 1.334(11) . ? C23 H23 0.9300 . ? C24 C25 1.409(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.394(11) . ? C27 C28 1.423(11) . ? C28 C29 1.428(12) . ? C28 H28 0.9300 . ? C29 C30 1.386(17) . ? C29 H29 0.9300 . ? C30 C31 1.311(17) . ? C30 H30 0.9300 . ? C31 C32 1.401(13) . ? C31 H31 0.9300 . ? C32 C33 1.516(12) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? Hg41 N41 2.347(6) . ? Hg41 Cl42 2.372(2) . ? Hg41 Cl41 2.416(2) . ? Hg41 N42 2.516(6) . ? N41 C45 1.330(8) . ? N41 C41 1.346(8) . ? N42 C46 1.281(8) . ? N42 C47 1.441(8) . ? C41 C42 1.383(9) . ? C41 C46 1.473(9) . ? C42 C43 1.379(9) . ? C42 H42 0.9300 . ? C43 C44 1.387(9) . ? C43 H43 0.9300 . ? C44 C45 1.385(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C52 1.383(10) . ? C47 C48 1.387(11) . ? C48 C49 1.376(10) . ? C48 H48 0.9300 . ? C49 C50 1.390(13) . ? C49 H49 0.9300 . ? C50 C51 1.345(13) . ? C50 H50 0.9300 . ? C51 C52 1.382(11) . ? C51 H51 0.9300 . ? C52 C53 1.489(11) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? Hg61 N61 2.366(6) . ? Hg61 Cl62 2.383(2) . ? Hg61 Cl61 2.393(2) . ? Hg61 N62 2.503(6) . ? N61 C65 1.317(8) . ? N61 C61 1.325(8) . ? N62 C66 1.277(8) . ? N62 C67 1.438(9) . ? C61 C62 1.386(10) . ? C61 C66 1.464(10) . ? C62 C63 1.385(10) . ? C62 H62 0.9300 . ? C63 C64 1.358(10) . ? C63 H63 0.9300 . ? C64 C65 1.397(9) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C72 1.363(11) . ? C67 C68 1.404(11) . ? C68 C69 1.352(11) . ? C68 H68 0.9300 . ? C69 C70 1.408(12) . ? C69 H69 0.9300 . ? C70 C71 1.386(11) . ? C70 H70 0.9300 . ? C71 C72 1.396(10) . ? C71 H71 0.9300 . ? C72 C73 1.500(10) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? 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 Cl2 117.00(16) . . ? N1 Hg1 Cl1 111.21(16) . . ? Cl2 Hg1 Cl1 130.93(7) . . ? N1 Hg1 N2 69.3(2) . . ? Cl2 Hg1 N2 92.82(15) . . ? Cl1 Hg1 N2 112.65(15) . . ? C5 N1 C1 119.0(7) . . ? C5 N1 Hg1 124.1(5) . . ? C1 N1 Hg1 116.9(5) . . ? C6 N2 C7 119.6(7) . . ? C6 N2 Hg1 113.4(5) . . ? C7 N2 Hg1 124.1(5) . . ? N1 C1 C2 119.9(8) . . ? N1 C1 C6 118.6(7) . . ? C2 C1 C6 121.4(8) . . ? C1 C2 C3 121.4(7) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 117.9(8) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 119.8(9) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 122.0(8) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? N2 C6 C1 120.5(7) . . ? N2 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 120.2(9) . . ? C8 C7 N2 119.0(9) . . ? C12 C7 N2 120.4(9) . . ? C7 C8 C9 119.4(9) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 119.1(11) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 121.7(13) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.3(12) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.2(10) . . ? C11 C12 C13 120.5(11) . . ? C7 C12 C13 120.2(10) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N21 Hg21 Cl22 114.40(17) . . ? N21 Hg21 Cl21 111.80(18) . . ? Cl22 Hg21 Cl21 132.77(7) . . ? N21 Hg21 N22 69.1(2) . . ? Cl22 Hg21 N22 90.50(15) . . ? Cl21 Hg21 N22 114.97(16) . . ? C21 N21 C25 116.6(7) . . ? C21 N21 Hg21 118.0(6) . . ? C25 N21 Hg21 125.4(6) . . ? C26 N22 C27 122.8(8) . . ? C26 N22 Hg21 110.2(6) . . ? C27 N22 Hg21 123.3(5) . . ? N21 C21 C22 123.1(9) . . ? N21 C21 C26 117.4(8) . . ? C22 C21 C26 119.5(9) . . ? C23 C22 C21 119.7(9) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 118.5(9) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 119.6(10) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N21 C25 C24 122.6(9) . . ? N21 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? N22 C26 C21 122.6(8) . . ? N22 C26 H26 118.7 . . ? C21 C26 H26 118.7 . . ? C32 C27 N22 119.9(10) . . ? C32 C27 C28 119.0(11) . . ? N22 C27 C28 121.0(10) . . ? C27 C28 C29 116.9(11) . . ? C27 C28 H28 121.5 . . ? C29 C28 H28 121.5 . . ? C30 C29 C28 122.8(15) . . ? C30 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C31 C30 C29 117.5(19) . . ? C31 C30 H30 121.2 . . ? C29 C30 H30 121.2 . . ? C30 C31 C32 124.5(17) . . ? C30 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C27 C32 C31 119.1(11) . . ? C27 C32 C33 121.1(11) . . ? C31 C32 C33 119.8(12) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N41 Hg41 Cl42 121.84(16) . . ? N41 Hg41 Cl41 104.84(16) . . ? Cl42 Hg41 Cl41 131.56(7) . . ? N41 Hg41 N42 69.6(2) . . ? Cl42 Hg41 N42 94.54(14) . . ? Cl41 Hg41 N42 114.50(15) . . ? C45 N41 C41 117.2(7) . . ? C45 N41 Hg41 124.5(5) . . ? C41 N41 Hg41 118.4(5) . . ? C46 N42 C47 119.5(7) . . ? C46 N42 Hg41 112.0(5) . . ? C47 N42 Hg41 127.3(4) . . ? N41 C41 C42 121.9(7) . . ? N41 C41 C46 117.1(7) . . ? C42 C41 C46 120.9(8) . . ? C43 C42 C41 119.3(7) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 120.0(7) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 116.0(8) . . ? C45 C44 H44 122.0 . . ? C43 C44 H44 122.0 . . ? N41 C45 C44 125.5(8) . . ? N41 C45 H45 117.3 . . ? C44 C45 H45 117.3 . . ? N42 C46 C41 122.6(7) . . ? N42 C46 H46 118.7 . . ? C41 C46 H46 118.7 . . ? C52 C47 C48 120.3(9) . . ? C52 C47 N42 119.4(9) . . ? C48 C47 N42 120.3(8) . . ? C49 C48 C47 120.1(9) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C48 C49 C50 119.0(10) . . ? C48 C49 H49 120.5 . . ? C50 C49 H49 120.5 . . ? C51 C50 C49 120.6(11) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 121.6(11) . . ? C50 C51 H51 119.2 . . ? C52 C51 H51 119.2 . . ? C51 C52 C47 118.4(9) . . ? C51 C52 C53 119.7(9) . . ? C47 C52 C53 121.9(9) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N61 Hg61 Cl62 113.25(16) . . ? N61 Hg61 Cl61 112.21(16) . . ? Cl62 Hg61 Cl61 133.76(7) . . ? N61 Hg61 N62 68.4(2) . . ? Cl62 Hg61 N62 91.02(16) . . ? Cl61 Hg61 N62 113.23(16) . . ? C65 N61 C61 118.0(7) . . ? C65 N61 Hg61 123.6(5) . . ? C61 N61 Hg61 118.4(6) . . ? C66 N62 C67 120.2(7) . . ? C66 N62 Hg61 112.4(6) . . ? C67 N62 Hg61 123.8(5) . . ? N61 C61 C62 122.1(9) . . ? N61 C61 C66 117.1(8) . . ? C62 C61 C66 120.9(8) . . ? C63 C62 C61 119.8(8) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C64 C63 C62 117.8(8) . . ? C64 C63 H63 121.1 . . ? C62 C63 H63 121.1 . . ? C63 C64 C65 118.9(9) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? N61 C65 C64 123.3(8) . . ? N61 C65 H65 118.3 . . ? C64 C65 H65 118.3 . . ? N62 C66 C61 121.3(8) . . ? N62 C66 H66 119.3 . . ? C61 C66 H66 119.3 . . ? C72 C67 C68 121.0(10) . . ? C72 C67 N62 119.7(9) . . ? C68 C67 N62 119.2(9) . . ? C69 C68 C67 120.1(10) . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C68 C69 C70 120.4(10) . . ? C68 C69 H69 119.8 . . ? C70 C69 H69 119.8 . . ? C71 C70 C69 118.7(10) . . ? C71 C70 H70 120.6 . . ? C69 C70 H70 120.6 . . ? C70 C71 C72 121.1(9) . . ? C70 C71 H71 119.4 . . ? C72 C71 H71 119.4 . . ? C67 C72 C71 118.8(9) . . ? C67 C72 C73 123.3(9) . . ? C71 C72 C73 118.0(9) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? 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 Hg1 N1 C5 -101.5(6) . . . . ? Cl1 Hg1 N1 C5 69.0(6) . . . . ? N2 Hg1 N1 C5 176.2(6) . . . . ? Cl2 Hg1 N1 C1 77.4(6) . . . . ? Cl1 Hg1 N1 C1 -112.0(5) . . . . ? N2 Hg1 N1 C1 -4.9(5) . . . . ? N1 Hg1 N2 C6 9.0(5) . . . . ? Cl2 Hg1 N2 C6 -108.9(5) . . . . ? Cl1 Hg1 N2 C6 114.1(5) . . . . ? N1 Hg1 N2 C7 169.9(6) . . . . ? Cl2 Hg1 N2 C7 52.0(6) . . . . ? Cl1 Hg1 N2 C7 -85.0(6) . . . . ? C5 N1 C1 C2 2.9(12) . . . . ? Hg1 N1 C1 C2 -176.1(6) . . . . ? C5 N1 C1 C6 179.9(7) . . . . ? Hg1 N1 C1 C6 0.9(9) . . . . ? N1 C1 C2 C3 -2.6(12) . . . . ? C6 C1 C2 C3 -179.5(7) . . . . ? C1 C2 C3 C4 1.0(13) . . . . ? C2 C3 C4 C5 0.2(13) . . . . ? C1 N1 C5 C4 -1.8(12) . . . . ? Hg1 N1 C5 C4 177.1(6) . . . . ? C3 C4 C5 N1 0.2(13) . . . . ? C7 N2 C6 C1 -174.1(7) . . . . ? Hg1 N2 C6 C1 -12.3(9) . . . . ? N1 C1 C6 N2 8.3(11) . . . . ? C2 C1 C6 N2 -174.7(8) . . . . ? C6 N2 C7 C8 43.5(11) . . . . ? Hg1 N2 C7 C8 -116.3(7) . . . . ? C6 N2 C7 C12 -143.6(8) . . . . ? Hg1 N2 C7 C12 56.6(9) . . . . ? C12 C7 C8 C9 1.7(13) . . . . ? N2 C7 C8 C9 174.6(7) . . . . ? C7 C8 C9 C10 -3.6(14) . . . . ? C8 C9 C10 C11 2.8(17) . . . . ? C9 C10 C11 C12 -0.1(17) . . . . ? C10 C11 C12 C7 -1.8(15) . . . . ? C10 C11 C12 C13 176.3(10) . . . . ? C8 C7 C12 C11 1.0(13) . . . . ? N2 C7 C12 C11 -171.8(7) . . . . ? C8 C7 C12 C13 -177.2(8) . . . . ? N2 C7 C12 C13 10.0(12) . . . . ? Cl22 Hg21 N21 C21 -70.7(7) . . . . ? Cl21 Hg21 N21 C21 119.4(6) . . . . ? N22 Hg21 N21 C21 9.9(6) . . . . ? Cl22 Hg21 N21 C25 106.9(6) . . . . ? Cl21 Hg21 N21 C25 -62.9(7) . . . . ? N22 Hg21 N21 C25 -172.4(7) . . . . ? N21 Hg21 N22 C26 -13.8(6) . . . . ? Cl22 Hg21 N22 C26 102.2(6) . . . . ? Cl21 Hg21 N22 C26 -119.0(5) . . . . ? N21 Hg21 N22 C27 -172.7(7) . . . . ? Cl22 Hg21 N22 C27 -56.6(6) . . . . ? Cl21 Hg21 N22 C27 82.2(6) . . . . ? C25 N21 C21 C22 -0.7(13) . . . . ? Hg21 N21 C21 C22 177.1(7) . . . . ? C25 N21 C21 C26 176.8(7) . . . . ? Hg21 N21 C21 C26 -5.4(10) . . . . ? N21 C21 C22 C23 0.8(14) . . . . ? C26 C21 C22 C23 -176.6(8) . . . . ? C21 C22 C23 C24 0.7(15) . . . . ? C22 C23 C24 C25 -2.2(16) . . . . ? C21 N21 C25 C24 -0.9(13) . . . . ? Hg21 N21 C25 C24 -178.6(7) . . . . ? C23 C24 C25 N21 2.4(15) . . . . ? C27 N22 C26 C21 176.5(7) . . . . ? Hg21 N22 C26 C21 17.6(10) . . . . ? N21 C21 C26 N22 -9.7(12) . . . . ? C22 C21 C26 N22 167.9(9) . . . . ? C26 N22 C27 C32 141.1(9) . . . . ? Hg21 N22 C27 C32 -62.7(10) . . . . ? C26 N22 C27 C28 -41.2(12) . . . . ? Hg21 N22 C27 C28 115.0(8) . . . . ? C32 C27 C28 C29 2.3(13) . . . . ? N22 C27 C28 C29 -175.5(8) . . . . ? C27 C28 C29 C30 -1.2(17) . . . . ? C28 C29 C30 C31 1(2) . . . . ? C29 C30 C31 C32 -1(2) . . . . ? N22 C27 C32 C31 175.0(8) . . . . ? C28 C27 C32 C31 -2.7(13) . . . . ? N22 C27 C32 C33 -6.5(13) . . . . ? C28 C27 C32 C33 175.7(8) . . . . ? C30 C31 C32 C27 2.2(19) . . . . ? C30 C31 C32 C33 -176.3(14) . . . . ? Cl42 Hg41 N41 C45 -99.7(6) . . . . ? Cl41 Hg41 N41 C45 66.8(6) . . . . ? N42 Hg41 N41 C45 177.9(6) . . . . ? Cl42 Hg41 N41 C41 79.3(6) . . . . ? Cl41 Hg41 N41 C41 -114.2(5) . . . . ? N42 Hg41 N41 C41 -3.1(5) . . . . ? N41 Hg41 N42 C46 4.3(5) . . . . ? Cl42 Hg41 N42 C46 -118.0(5) . . . . ? Cl41 Hg41 N42 C46 101.8(5) . . . . ? N41 Hg41 N42 C47 171.4(7) . . . . ? Cl42 Hg41 N42 C47 49.1(6) . . . . ? Cl41 Hg41 N42 C47 -91.1(6) . . . . ? C45 N41 C41 C42 2.8(11) . . . . ? Hg41 N41 C41 C42 -176.3(6) . . . . ? C45 N41 C41 C46 -179.1(7) . . . . ? Hg41 N41 C41 C46 1.8(9) . . . . ? N41 C41 C42 C43 -2.4(12) . . . . ? C46 C41 C42 C43 179.6(7) . . . . ? C41 C42 C43 C44 0.3(12) . . . . ? C42 C43 C44 C45 1.1(12) . . . . ? C41 N41 C45 C44 -1.2(12) . . . . ? Hg41 N41 C45 C44 177.8(6) . . . . ? C43 C44 C45 N41 -0.8(13) . . . . ? C47 N42 C46 C41 -173.6(7) . . . . ? Hg41 N42 C46 C41 -5.3(9) . . . . ? N41 C41 C46 N42 2.8(11) . . . . ? C42 C41 C46 N42 -179.1(8) . . . . ? C46 N42 C47 C52 -146.5(8) . . . . ? Hg41 N42 C47 C52 47.3(10) . . . . ? C46 N42 C47 C48 36.6(11) . . . . ? Hg41 N42 C47 C48 -129.7(7) . . . . ? C52 C47 C48 C49 -1.6(13) . . . . ? N42 C47 C48 C49 175.3(7) . . . . ? C47 C48 C49 C50 0.9(14) . . . . ? C48 C49 C50 C51 -0.6(16) . . . . ? C49 C50 C51 C52 1.1(18) . . . . ? C50 C51 C52 C47 -1.9(15) . . . . ? C50 C51 C52 C53 175.6(10) . . . . ? C48 C47 C52 C51 2.1(13) . . . . ? N42 C47 C52 C51 -174.9(7) . . . . ? C48 C47 C52 C53 -175.3(8) . . . . ? N42 C47 C52 C53 7.7(13) . . . . ? Cl62 Hg61 N61 C65 106.8(6) . . . . ? Cl61 Hg61 N61 C65 -64.5(7) . . . . ? N62 Hg61 N61 C65 -171.7(7) . . . . ? Cl62 Hg61 N61 C61 -73.6(6) . . . . ? Cl61 Hg61 N61 C61 115.1(6) . . . . ? N62 Hg61 N61 C61 7.8(6) . . . . ? N61 Hg61 N62 C66 -12.9(6) . . . . ? Cl62 Hg61 N62 C66 101.8(6) . . . . ? Cl61 Hg61 N62 C66 -118.7(6) . . . . ? N61 Hg61 N62 C67 -171.4(7) . . . . ? Cl62 Hg61 N62 C67 -56.7(6) . . . . ? Cl61 Hg61 N62 C67 82.8(6) . . . . ? C65 N61 C61 C62 -3.2(12) . . . . ? Hg61 N61 C61 C62 177.3(6) . . . . ? C65 N61 C61 C66 176.9(7) . . . . ? Hg61 N61 C61 C66 -2.7(9) . . . . ? N61 C61 C62 C63 1.8(13) . . . . ? C66 C61 C62 C63 -178.3(8) . . . . ? C61 C62 C63 C64 0.9(13) . . . . ? C62 C63 C64 C65 -2.1(14) . . . . ? C61 N61 C65 C64 1.9(13) . . . . ? Hg61 N61 C65 C64 -178.5(7) . . . . ? C63 C64 C65 N61 0.7(15) . . . . ? C67 N62 C66 C61 176.7(7) . . . . ? Hg61 N62 C66 C61 17.3(9) . . . . ? N61 C61 C66 N62 -10.9(12) . . . . ? C62 C61 C66 N62 169.2(8) . . . . ? C66 N62 C67 C72 137.0(8) . . . . ? Hg61 N62 C67 C72 -66.1(9) . . . . ? C66 N62 C67 C68 -45.6(11) . . . . ? Hg61 N62 C67 C68 111.4(7) . . . . ? C72 C67 C68 C69 1.1(13) . . . . ? N62 C67 C68 C69 -176.4(8) . . . . ? C67 C68 C69 C70 -0.2(14) . . . . ? C68 C69 C70 C71 -0.4(14) . . . . ? C69 C70 C71 C72 0.1(13) . . . . ? C68 C67 C72 C71 -1.3(12) . . . . ? N62 C67 C72 C71 176.1(6) . . . . ? C68 C67 C72 C73 178.0(8) . . . . ? N62 C67 C72 C73 -4.6(12) . . . . ? C70 C71 C72 C67 0.7(12) . . . . ? C70 C71 C72 C73 -178.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.192 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.112 _iucr_refine_instructions_details ; TITL tu1einm in P-1 CELL 0.71073 12.0247 14.3877 17.5422 78.370 83.453 78.383 ZERR 2.00 0.0016 0.0019 0.0023 0.002 0.002 0.002 LATT 1 SFAC C H N Cl Hg UNIT 104 96 16 16 8 OMIT -3.00 50.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 30 conf size 0.15 0.21 0.22 TEMP 20 WGHT 0.004600 FVAR 0.14502 HG1 5 0.992069 0.770766 0.691171 11.00000 0.06784 0.06054 = 0.05340 -0.02240 -0.00620 -0.00687 CL1 4 0.943298 0.836723 0.559101 11.00000 0.06742 0.07292 = 0.05243 -0.01690 -0.00716 -0.01229 CL2 4 1.111749 0.624249 0.744390 11.00000 0.07565 0.05451 = 0.07386 -0.02016 -0.00900 -0.00151 N1 3 0.875207 0.857557 0.780635 11.00000 0.04647 0.05482 = 0.05370 -0.02611 -0.00407 -0.00423 N2 3 1.100985 0.871644 0.742510 11.00000 0.04202 0.04313 = 0.04004 -0.00781 0.00326 -0.01451 C1 1 0.925684 0.909617 0.817437 11.00000 0.05621 0.04215 = 0.05483 -0.03045 -0.00934 -0.00146 C2 1 0.863845 0.957400 0.873935 11.00000 0.05660 0.06855 = 0.05316 -0.02578 -0.01017 -0.00942 AFIX 43 H2 2 0.900182 0.991022 0.900516 11.00000 -1.20000 AFIX 0 C3 1 0.748412 0.956274 0.891889 11.00000 0.08260 0.07009 = 0.05732 -0.03442 -0.00495 0.00919 AFIX 43 H3 2 0.706897 0.989377 0.929407 11.00000 -1.20000 AFIX 0 C4 1 0.698873 0.905980 0.853422 11.00000 0.06233 0.06123 = 0.07005 -0.02160 -0.00351 0.01372 AFIX 43 H4 2 0.621759 0.903857 0.863928 11.00000 -1.20000 AFIX 0 C5 1 0.763591 0.856611 0.797335 11.00000 0.07412 0.05595 = 0.06498 -0.01936 -0.02564 -0.01191 AFIX 43 H5 2 0.728202 0.822158 0.770880 11.00000 -1.20000 AFIX 0 C6 1 1.046657 0.910186 0.799106 11.00000 0.04266 0.05408 = 0.06231 -0.02497 -0.00925 0.00118 AFIX 43 H6 2 1.084951 0.938708 0.828633 11.00000 -1.20000 AFIX 0 C7 1 1.220295 0.864928 0.730218 11.00000 0.05407 0.04124 = 0.04911 -0.00806 0.00909 -0.00836 C8 1 1.285380 0.835855 0.793712 11.00000 0.05585 0.07217 = 0.07389 0.01898 0.01017 -0.00951 AFIX 43 H8 2 1.250548 0.826176 0.844076 11.00000 -1.20000 AFIX 0 C9 1 1.404653 0.821030 0.781563 11.00000 0.07598 0.08502 = 0.13361 0.02003 -0.02750 -0.03077 AFIX 43 H9 2 1.449544 0.804908 0.823772 11.00000 -1.20000 AFIX 0 C10 1 1.453919 0.830622 0.706805 11.00000 0.08261 0.03884 = 0.14831 -0.00839 0.02085 -0.02672 AFIX 43 H10 2 1.532888 0.818088 0.698743 11.00000 -1.20000 AFIX 0 C11 1 1.390346 0.858013 0.644017 11.00000 0.08352 0.10393 = 0.11096 -0.04306 0.04133 -0.03869 AFIX 43 H11 2 1.426062 0.864023 0.593835 11.00000 -1.20000 AFIX 0 C12 1 1.272861 0.876957 0.654478 11.00000 0.09218 0.06104 = 0.06756 -0.03061 0.01384 -0.04198 C13 1 1.202762 0.912675 0.586043 11.00000 0.11920 0.21697 = 0.05487 -0.03301 0.01914 -0.10470 AFIX 137 H13A 2 1.161779 0.863957 0.580457 11.00000 -1.50000 H13B 2 1.251603 0.926981 0.539657 11.00000 -1.50000 H13C 2 1.149773 0.970084 0.593956 11.00000 -1.50000 AFIX 0 HG21 5 0.749036 0.728100 0.560686 11.00000 0.06829 0.06421 = 0.05107 -0.02289 -0.00617 -0.00744 CL21 4 0.786278 0.663670 0.695114 11.00000 0.07244 0.07424 = 0.04437 -0.01268 -0.00616 -0.01514 CL22 4 0.635568 0.873614 0.498314 11.00000 0.06274 0.05988 = 0.05797 -0.01958 -0.00660 0.00031 N21 3 0.874110 0.643664 0.475283 11.00000 0.06006 0.06772 = 0.05282 -0.02689 -0.01133 -0.00818 N22 3 0.647378 0.629957 0.498756 11.00000 0.05645 0.05132 = 0.04758 -0.01512 -0.00005 -0.01982 C21 1 0.830606 0.600338 0.429670 11.00000 0.04991 0.06774 = 0.05213 -0.02164 -0.00567 0.00796 C22 1 0.896502 0.551326 0.373986 11.00000 0.12545 0.05878 = 0.05624 -0.03178 -0.01221 0.01216 AFIX 43 H22 2 0.862001 0.522399 0.342499 11.00000 -1.20000 AFIX 0 C23 1 1.010226 0.546225 0.366186 11.00000 0.09030 0.07699 = 0.08193 -0.03342 0.01540 0.03607 AFIX 43 H23 2 1.055190 0.514542 0.329040 11.00000 -1.20000 AFIX 0 C24 1 1.056876 0.587651 0.412954 11.00000 0.08081 0.09483 = 0.08366 -0.03728 0.00253 -0.00011 AFIX 43 H24 2 1.135424 0.583255 0.410007 11.00000 -1.20000 AFIX 0 C25 1 0.986360 0.638120 0.466858 11.00000 0.07846 0.05699 = 0.06475 -0.01583 -0.01285 0.00245 AFIX 43 H25 2 1.019687 0.668739 0.497736 11.00000 -1.20000 AFIX 0 C26 1 0.708971 0.601154 0.440872 11.00000 0.11501 0.04826 = 0.04074 -0.02349 -0.02218 -0.00971 AFIX 43 H26 2 0.674600 0.579828 0.404397 11.00000 -1.20000 AFIX 0 C27 1 0.527993 0.635773 0.507736 11.00000 0.10022 0.04718 = 0.05339 -0.00099 -0.00339 -0.03004 C28 1 0.460478 0.671085 0.442823 11.00000 0.08013 0.09091 = 0.07266 0.00811 -0.00216 -0.02784 AFIX 43 H28 2 0.493351 0.686942 0.392436 11.00000 -1.20000 AFIX 0 C29 1 0.339938 0.681047 0.458619 11.00000 0.07607 0.08643 = 0.21698 -0.00570 -0.05180 -0.02491 AFIX 43 H29 2 0.293877 0.705176 0.417317 11.00000 -1.20000 AFIX 0 C30 1 0.288620 0.656322 0.532816 11.00000 0.09327 0.14303 = 0.20829 -0.05337 0.02098 -0.06178 AFIX 43 H30 2 0.209909 0.662922 0.541546 11.00000 -1.20000 AFIX 0 C31 1 0.355158 0.623276 0.590253 11.00000 0.09680 0.13529 = 0.14986 -0.07784 0.03826 -0.07306 AFIX 43 H31 2 0.320911 0.607641 0.640253 11.00000 -1.20000 AFIX 0 C32 1 0.474265 0.609884 0.581535 11.00000 0.08234 0.09074 = 0.06070 -0.02569 0.01246 -0.05070 C33 1 0.542715 0.565440 0.651610 11.00000 0.15274 0.17929 = 0.07171 -0.03749 0.00731 -0.10940 AFIX 137 H33A 2 0.622445 0.561175 0.635921 11.00000 -1.50000 H33B 2 0.527038 0.501987 0.672438 11.00000 -1.50000 H33C 2 0.522000 0.605020 0.690836 11.00000 -1.50000 AFIX 0 HG41 5 0.535093 0.774474 0.186446 11.00000 0.06819 0.05892 = 0.05678 -0.02511 -0.00685 -0.00487 CL41 4 0.481048 0.849860 0.056725 11.00000 0.08229 0.07811 = 0.05276 -0.01711 -0.01117 -0.00395 CL42 4 0.643417 0.621065 0.234831 11.00000 0.06774 0.06179 = 0.08546 -0.02026 -0.01622 -0.00384 N41 3 0.415669 0.867401 0.269532 11.00000 0.05484 0.05637 = 0.04624 -0.02145 -0.00205 -0.00533 N42 3 0.648375 0.866639 0.246248 11.00000 0.05442 0.03729 = 0.05274 -0.01822 0.00243 -0.00962 C41 1 0.463159 0.918005 0.309486 11.00000 0.04495 0.04903 = 0.04231 -0.01325 -0.00446 -0.01384 C42 1 0.399629 0.970155 0.362857 11.00000 0.07001 0.06712 = 0.05304 -0.03668 -0.00364 0.00288 AFIX 43 H42 2 0.434821 1.002596 0.391185 11.00000 -1.20000 AFIX 0 C43 1 0.283599 0.973571 0.373649 11.00000 0.05748 0.04501 = 0.05514 -0.01190 0.00650 0.01015 AFIX 43 H43 2 0.240074 1.008725 0.409205 11.00000 -1.20000 AFIX 0 C44 1 0.231757 0.924600 0.331501 11.00000 0.06333 0.05601 = 0.07890 -0.02532 -0.00221 -0.00059 AFIX 43 H44 2 0.153537 0.926474 0.336843 11.00000 -1.20000 AFIX 0 C45 1 0.303439 0.872735 0.280975 11.00000 0.04876 0.05941 = 0.06815 -0.02202 -0.00847 -0.01022 AFIX 43 H45 2 0.270327 0.838785 0.252669 11.00000 -1.20000 AFIX 0 C46 1 0.587160 0.913200 0.295919 11.00000 0.05909 0.05670 = 0.05226 -0.02316 -0.00774 -0.01182 AFIX 43 H46 2 0.622404 0.945240 0.324549 11.00000 -1.20000 AFIX 0 C47 1 0.770528 0.856674 0.241848 11.00000 0.04043 0.05192 = 0.07465 -0.02808 0.00086 -0.00865 C48 1 0.826263 0.844673 0.309126 11.00000 0.05984 0.07237 = 0.09057 -0.03073 -0.00307 -0.02035 AFIX 43 H48 2 0.784432 0.847756 0.356816 11.00000 -1.20000 AFIX 0 C49 1 0.943328 0.828215 0.305441 11.00000 0.04447 0.08320 = 0.12478 -0.01564 -0.02820 -0.00931 AFIX 43 H49 2 0.981190 0.819253 0.350461 11.00000 -1.20000 AFIX 0 C50 1 1.004134 0.825187 0.233426 11.00000 0.05208 0.08328 = 0.15691 -0.04480 0.03122 -0.01808 AFIX 43 H50 2 1.083273 0.814728 0.230187 11.00000 -1.20000 AFIX 0 C51 1 0.949523 0.837250 0.168379 11.00000 0.07475 0.11295 = 0.10512 -0.05041 0.03860 -0.04409 AFIX 43 H51 2 0.991830 0.833814 0.120896 11.00000 -1.20000 AFIX 0 C52 1 0.832031 0.854630 0.170421 11.00000 0.07528 0.06300 = 0.05641 -0.02647 0.01467 -0.02013 C53 1 0.775195 0.874508 0.096241 11.00000 0.11232 0.12722 = 0.07160 -0.04694 0.02445 -0.04593 AFIX 137 H53A 2 0.734090 0.823951 0.095774 11.00000 -1.50000 H53B 2 0.831583 0.877263 0.052853 11.00000 -1.50000 H53C 2 0.723261 0.935128 0.092260 11.00000 -1.50000 AFIX 0 HG61 5 0.282846 0.735334 0.057841 11.00000 0.06940 0.07091 = 0.05428 -0.02713 -0.00563 -0.00713 CL61 4 0.323401 0.672638 0.190840 11.00000 0.08116 0.06650 = 0.05894 -0.02313 -0.01578 -0.01335 CL62 4 0.162450 0.875522 -0.005300 11.00000 0.08402 0.06528 = 0.06831 -0.02553 -0.01121 0.00365 N61 3 0.410064 0.653051 -0.030258 11.00000 0.05208 0.05609 = 0.04275 -0.01998 -0.00541 -0.00858 N62 3 0.188175 0.628515 0.000403 11.00000 0.07103 0.04735 = 0.05728 -0.01679 -0.00688 -0.02449 C61 1 0.368842 0.602648 -0.072191 11.00000 0.07618 0.04522 = 0.04451 -0.01273 -0.00679 -0.01421 C62 1 0.436578 0.555709 -0.127399 11.00000 0.09670 0.05623 = 0.04929 -0.02699 0.00800 -0.01964 AFIX 43 H62 2 0.404761 0.522368 -0.156962 11.00000 -1.20000 AFIX 0 C63 1 0.551852 0.558597 -0.138423 11.00000 0.08005 0.08002 = 0.07630 -0.03538 0.00957 0.01181 AFIX 43 H63 2 0.598543 0.528311 -0.175681 11.00000 -1.20000 AFIX 0 C64 1 0.594418 0.607107 -0.093034 11.00000 0.07196 0.07391 = 0.06665 -0.03382 0.00514 -0.00799 AFIX 43 H64 2 0.671757 0.609059 -0.097407 11.00000 -1.20000 AFIX 0 C65 1 0.520108 0.654049 -0.039644 11.00000 0.07797 0.10063 = 0.06227 -0.05249 -0.00872 0.00026 AFIX 43 H65 2 0.549848 0.687692 -0.009200 11.00000 -1.20000 AFIX 0 C66 1 0.247483 0.598463 -0.057908 11.00000 0.10408 0.04708 = 0.03399 -0.01262 -0.00412 -0.02561 AFIX 43 H66 2 0.212875 0.573406 -0.091999 11.00000 -1.20000 AFIX 0 C67 1 0.067843 0.628377 0.010781 11.00000 0.08615 0.04577 = 0.04866 -0.01397 -0.01909 -0.01701 C68 1 0.001731 0.663348 -0.053513 11.00000 0.09174 0.08770 = 0.04873 -0.00590 -0.00459 -0.04227 AFIX 43 H68 2 0.036513 0.682819 -0.102683 11.00000 -1.20000 AFIX 0 C69 1 -0.112421 0.668751 -0.044034 11.00000 0.10526 0.08485 = 0.08715 0.00760 -0.03943 -0.04107 AFIX 43 H69 2 -0.155930 0.692156 -0.086734 11.00000 -1.20000 AFIX 0 C70 1 -0.165784 0.639128 0.030150 11.00000 0.05535 0.05692 = 0.13076 -0.00702 -0.02233 -0.01831 AFIX 43 H70 2 -0.244324 0.643060 0.037002 11.00000 -1.20000 AFIX 0 C71 1 -0.098971 0.603999 0.092748 11.00000 0.07630 0.06610 = 0.07534 -0.01392 0.01471 -0.01594 AFIX 43 H71 2 -0.133271 0.584093 0.141990 11.00000 -1.20000 AFIX 0 C72 1 0.018977 0.597995 0.083119 11.00000 0.05483 0.05008 = 0.05904 -0.01475 0.00681 -0.02022 C73 1 0.085746 0.557131 0.153309 11.00000 0.08698 0.13432 = 0.05584 -0.01943 -0.01439 -0.02522 AFIX 137 H73A 2 0.158321 0.577202 0.144388 11.00000 -1.50000 H73B 2 0.097009 0.487935 0.162350 11.00000 -1.50000 H73C 2 0.044643 0.580102 0.198113 11.00000 -1.50000 HKLF 4 REM tu1einm in P-1 REM R1 = 0.0382 for 5153 Fo > 4sig(Fo) and 0.0973 for all 10210 data REM 653 parameters refined using 0 restraints END WGHT 0.0276 0.0000 REM Highest difference peak 1.193, deepest hole -0.809, 1-sigma level 0.112 Q1 1 0.2215 0.7509 0.0151 11.00000 0.05 1.01 Q2 1 0.9512 0.6991 0.7248 11.00000 0.05 0.88 Q3 1 0.4632 0.7972 0.1466 11.00000 0.05 0.83 Q4 1 0.6963 0.7342 0.5123 11.00000 0.05 0.82 Q5 1 1.0270 0.8421 0.6583 11.00000 0.05 0.77 Q6 1 1.0352 0.7548 0.7387 11.00000 0.05 0.76 Q7 1 0.6985 0.6610 0.5925 11.00000 0.05 0.75 Q8 1 0.2337 0.6707 0.0927 11.00000 0.05 0.74 Q9 1 0.4975 0.7211 0.2236 11.00000 0.05 0.73 Q10 1 0.7721 0.7939 0.5288 11.00000 0.05 0.67 Q11 1 0.9535 0.7529 0.6378 11.00000 0.05 0.66 Q12 1 0.7154 0.7545 0.5020 11.00000 0.05 0.64 Q13 1 0.9183 0.8151 0.6831 11.00000 0.05 0.62 Q14 1 0.3036 0.8197 0.0186 11.00000 0.05 0.56 Q15 1 0.5804 0.7651 0.2409 11.00000 0.05 0.54 Q16 1 0.3412 0.7237 0.1149 11.00000 0.05 0.53 Q17 1 0.8032 0.7071 0.6165 11.00000 0.05 0.53 Q18 1 0.8348 0.7149 0.5820 11.00000 0.05 0.52 Q19 1 0.9051 0.7968 0.6640 11.00000 0.05 0.50 Q20 1 0.7674 0.6984 0.6276 11.00000 0.05 0.47 Q21 1 0.5523 0.8565 0.1413 11.00000 0.05 0.47 Q22 1 0.6094 0.8235 0.1572 11.00000 0.05 0.46 Q23 1 0.5440 0.8247 0.2395 11.00000 0.05 0.45 Q24 1 0.9924 0.8135 0.7412 11.00000 0.05 0.41 Q25 1 -0.1991 0.7225 -0.0703 11.00000 0.05 0.40 Q26 1 0.0462 0.6419 -0.0114 11.00000 0.05 0.40 Q27 1 0.6615 0.7778 0.5572 11.00000 0.05 0.38 Q28 1 0.3666 0.6804 0.0685 11.00000 0.05 0.38 Q29 1 0.8159 0.6744 0.5656 11.00000 0.05 0.37 Q30 1 1.0598 0.8455 0.4593 11.00000 0.05 0.37 ; data_5 _database_code_depnum_ccdc_archive 'CCDC 892209' #TrackingRef '5.cif' # tu1secm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl4 Hg2 N4' _chemical_formula_sum 'C26 H24 Cl4 Hg2 N4' _chemical_formula_weight 935.47 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' Cl Cl 0.1484 0.1585 '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/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 7.7944(9) _cell_length_b 8.4673(10) _cell_length_c 21.336(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.221(2) _cell_angle_gamma 90.00 _cell_volume 1402.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5329 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.72 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 11.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.18 _exptl_absorpt_process_details SADABS _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 '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 12935 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2465 _reflns_number_gt 2096 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0338P)^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 2465 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.18187(2) 0.34843(2) 0.041888(10) 0.04664(10) Uani 1 1 d . . . Cl1 Cl 0.05977(18) 0.59641(17) 0.07268(8) 0.0585(4) Uani 1 1 d . . . Cl2 Cl 0.03199(17) 0.13062(15) 0.08798(7) 0.0528(4) Uani 1 1 d . . . N1 N 0.3480(5) 0.2371(5) -0.02857(19) 0.0385(10) Uani 1 1 d . . . N2 N 0.4908(5) 0.3665(4) 0.0844(2) 0.0385(10) Uani 1 1 d . . . C1 C 0.5173(6) 0.2251(5) -0.0115(2) 0.0346(11) Uani 1 1 d . . . C2 C 0.6246(7) 0.1404(5) -0.0456(3) 0.0438(13) Uani 1 1 d . . . H2 H 0.7415 0.1328 -0.0326 0.053 Uiso 1 1 calc R . . C3 C 0.5563(7) 0.0656(6) -0.1003(3) 0.0497(13) Uani 1 1 d . . . H3 H 0.6268 0.0068 -0.1244 0.060 Uiso 1 1 calc R . . C4 C 0.3842(7) 0.0797(6) -0.1182(3) 0.0527(14) Uani 1 1 d . . . H4 H 0.3360 0.0322 -0.1550 0.063 Uiso 1 1 calc R . . C5 C 0.2834(7) 0.1654(5) -0.0808(3) 0.0472(14) Uani 1 1 d . . . H5 H 0.1659 0.1733 -0.0926 0.057 Uiso 1 1 calc R . . C6 C 0.5875(6) 0.3031(5) 0.0471(2) 0.0405(12) Uani 1 1 d . . . H6 H 0.7062 0.3059 0.0568 0.049 Uiso 1 1 calc R . . C7 C 0.5635(6) 0.4394(5) 0.1412(2) 0.0366(11) Uani 1 1 d . . . C8 C 0.7302(7) 0.4126(6) 0.1672(3) 0.0489(13) Uani 1 1 d . . . H8 H 0.7996 0.3415 0.1479 0.059 Uiso 1 1 calc R . . C9 C 0.7952(7) 0.4896(7) 0.2211(3) 0.0542(15) Uani 1 1 d . . . C10 C 0.6895(7) 0.5937(7) 0.2497(3) 0.0532(14) Uani 1 1 d . . . H10 H 0.7319 0.6479 0.2857 0.064 Uiso 1 1 calc R . . C11 C 0.5245(8) 0.6172(6) 0.2254(3) 0.0574(15) Uani 1 1 d . . . H11 H 0.4548 0.6867 0.2453 0.069 Uiso 1 1 calc R . . C12 C 0.4588(7) 0.5400(6) 0.1718(2) 0.0499(13) Uani 1 1 d . . . H12 H 0.3446 0.5553 0.1562 0.060 Uiso 1 1 calc R . . C13 C 0.9782(8) 0.4585(10) 0.2480(4) 0.097(3) Uani 1 1 d . . . H13A H 0.9775 0.3910 0.2841 0.146 Uiso 1 1 calc R . . H13B H 1.0331 0.5567 0.2601 0.146 Uiso 1 1 calc R . . H13C H 1.0404 0.4080 0.2167 0.146 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 0.03578(14) 0.05047(15) 0.05425(18) 0.00395(10) 0.00726(11) 0.00652(9) Cl1 0.0514(8) 0.0563(8) 0.0656(10) -0.0054(7) -0.0075(7) 0.0191(6) Cl2 0.0428(7) 0.0541(8) 0.0624(10) 0.0131(6) 0.0101(7) 0.0037(6) N1 0.034(2) 0.039(2) 0.042(3) -0.0004(19) 0.001(2) 0.0036(17) N2 0.037(2) 0.040(2) 0.038(3) 0.0019(18) 0.003(2) 0.0027(17) C1 0.028(2) 0.036(2) 0.040(3) 0.005(2) 0.003(2) 0.002(2) C2 0.033(3) 0.051(3) 0.048(4) 0.007(3) 0.005(3) 0.009(2) C3 0.049(3) 0.056(3) 0.046(4) -0.003(3) 0.011(3) 0.007(3) C4 0.054(3) 0.055(3) 0.048(4) -0.011(3) -0.001(3) 0.007(3) C5 0.041(3) 0.052(3) 0.046(4) 0.000(3) -0.005(3) 0.002(2) C6 0.029(3) 0.051(3) 0.042(3) 0.004(2) 0.004(2) 0.000(2) C7 0.036(3) 0.039(3) 0.035(3) 0.005(2) 0.003(2) 0.000(2) C8 0.043(3) 0.060(3) 0.044(4) -0.007(3) 0.004(3) 0.009(3) C9 0.049(3) 0.078(4) 0.036(3) -0.003(3) 0.006(3) -0.003(3) C10 0.058(4) 0.062(3) 0.039(3) -0.002(3) 0.001(3) -0.005(3) C11 0.063(4) 0.065(4) 0.044(4) -0.008(3) 0.006(3) 0.014(3) C12 0.045(3) 0.063(3) 0.041(3) -0.002(3) -0.003(3) 0.009(3) C13 0.059(4) 0.151(7) 0.076(5) -0.041(5) -0.024(4) 0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.276(4) . ? Hg1 Cl1 2.4207(14) . ? Hg1 Cl2 2.4376(13) . ? Hg1 N2 2.500(4) . ? Hg1 Cl1 2.9836(15) 3_565 ? Cl1 Hg1 2.9837(15) 3_565 ? N1 C5 1.328(7) . ? N1 C1 1.340(5) . ? N2 C6 1.265(6) . ? N2 C7 1.429(6) . ? C1 C2 1.363(7) . ? C1 C6 1.473(7) . ? C2 C3 1.391(7) . ? C2 H2 0.9300 . ? C3 C4 1.366(7) . ? C3 H3 0.9300 . ? C4 C5 1.376(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.384(7) . ? C7 C8 1.384(7) . ? C8 C9 1.378(7) . ? C8 H8 0.9300 . ? C9 C10 1.385(8) . ? C9 C13 1.511(8) . ? C10 C11 1.356(8) . ? C10 H10 0.9300 . ? C11 C12 1.376(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 Cl1 143.12(11) . . ? N1 Hg1 Cl2 105.99(11) . . ? Cl1 Hg1 Cl2 109.40(5) . . ? N1 Hg1 N2 71.22(14) . . ? Cl1 Hg1 N2 103.76(9) . . ? Cl2 Hg1 N2 112.40(9) . . ? N1 Hg1 Cl1 83.02(10) . 3_565 ? Cl1 Hg1 Cl1 81.49(5) . 3_565 ? Cl2 Hg1 Cl1 99.15(5) . 3_565 ? N2 Hg1 Cl1 143.45(10) . 3_565 ? Hg1 Cl1 Hg1 98.51(5) . 3_565 ? C5 N1 C1 118.8(4) . . ? C5 N1 Hg1 123.3(3) . . ? C1 N1 Hg1 117.2(3) . . ? C6 N2 C7 120.3(4) . . ? C6 N2 Hg1 110.7(3) . . ? C7 N2 Hg1 128.9(3) . . ? N1 C1 C2 122.1(5) . . ? N1 C1 C6 118.5(4) . . ? C2 C1 C6 119.4(4) . . ? C1 C2 C3 118.8(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.1(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.8(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.4(5) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C1 121.9(5) . . ? N2 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? C12 C7 C8 119.0(5) . . ? C12 C7 N2 117.4(4) . . ? C8 C7 N2 123.6(4) . . ? C9 C8 C7 121.1(5) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 118.7(5) . . ? C8 C9 C13 119.7(5) . . ? C10 C9 C13 121.6(5) . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 121.1(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 119.6(5) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 N1 Hg1 Cl1 Hg1 66.16(17) . . . 3_565 ? Cl2 Hg1 Cl1 Hg1 -96.76(6) . . . 3_565 ? N2 Hg1 Cl1 Hg1 143.10(10) . . . 3_565 ? Cl1 Hg1 Cl1 Hg1 0.0 3_565 . . 3_565 ? Cl1 Hg1 N1 C5 -96.5(4) . . . . ? Cl2 Hg1 N1 C5 66.7(4) . . . . ? N2 Hg1 N1 C5 175.5(4) . . . . ? Cl1 Hg1 N1 C5 -30.8(4) 3_565 . . . ? Cl1 Hg1 N1 C1 93.0(4) . . . . ? Cl2 Hg1 N1 C1 -103.7(3) . . . . ? N2 Hg1 N1 C1 5.0(3) . . . . ? Cl1 Hg1 N1 C1 158.7(3) 3_565 . . . ? N1 Hg1 N2 C6 -1.2(3) . . . . ? Cl1 Hg1 N2 C6 -143.1(3) . . . . ? Cl2 Hg1 N2 C6 98.9(3) . . . . ? Cl1 Hg1 N2 C6 -48.8(4) 3_565 . . . ? N1 Hg1 N2 C7 176.9(4) . . . . ? Cl1 Hg1 N2 C7 35.0(4) . . . . ? Cl2 Hg1 N2 C7 -83.1(4) . . . . ? Cl1 Hg1 N2 C7 129.3(3) 3_565 . . . ? C5 N1 C1 C2 -0.6(7) . . . . ? Hg1 N1 C1 C2 170.2(4) . . . . ? C5 N1 C1 C6 -179.1(4) . . . . ? Hg1 N1 C1 C6 -8.3(6) . . . . ? N1 C1 C2 C3 0.7(7) . . . . ? C6 C1 C2 C3 179.2(4) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? C2 C3 C4 C5 -1.1(8) . . . . ? C1 N1 C5 C4 -0.3(8) . . . . ? Hg1 N1 C5 C4 -170.6(4) . . . . ? C3 C4 C5 N1 1.2(8) . . . . ? C7 N2 C6 C1 179.2(4) . . . . ? Hg1 N2 C6 C1 -2.5(6) . . . . ? N1 C1 C6 N2 7.4(7) . . . . ? C2 C1 C6 N2 -171.2(5) . . . . ? C6 N2 C7 C12 164.0(5) . . . . ? Hg1 N2 C7 C12 -13.9(6) . . . . ? C6 N2 C7 C8 -17.1(7) . . . . ? Hg1 N2 C7 C8 165.0(4) . . . . ? C12 C7 C8 C9 -2.9(8) . . . . ? N2 C7 C8 C9 178.2(5) . . . . ? C7 C8 C9 C10 0.8(8) . . . . ? C7 C8 C9 C13 -179.5(6) . . . . ? C8 C9 C10 C11 1.0(9) . . . . ? C13 C9 C10 C11 -178.7(6) . . . . ? C9 C10 C11 C12 -0.7(9) . . . . ? C10 C11 C12 C7 -1.5(9) . . . . ? C8 C7 C12 C11 3.3(8) . . . . ? N2 C7 C12 C11 -177.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.073 _refine_diff_density_min -1.149 _refine_diff_density_rms 0.119 _iucr_refine_instructions_details ; TITL tu1secm in P2(1)/c CELL 0.71073 7.7944 8.4673 21.3359 90.000 95.221 90.000 ZERR 2.00 0.0009 0.0010 0.0024 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Cl Hg UNIT 52 48 8 8 4 OMIT -3.00 50.00 L.S. 10 ACTA BOND FMAP 2 PLAN 20 size 0.23 0.34 0.46 conf TEMP 20 WGHT 0.033800 FVAR 0.31648 MOLE 1 HG1 5 0.181866 0.348430 0.041888 11.00000 0.03578 0.05047 = 0.05425 0.00395 0.00726 0.00652 CL1 4 0.059770 0.596405 0.072681 11.00000 0.05136 0.05629 = 0.06561 -0.00536 -0.00747 0.01907 CL2 4 0.031989 0.130622 0.087977 11.00000 0.04281 0.05407 = 0.06240 0.01308 0.01014 0.00372 N1 3 0.347985 0.237102 -0.028565 11.00000 0.03393 0.03864 = 0.04242 -0.00043 0.00144 0.00357 N2 3 0.490848 0.366526 0.084441 11.00000 0.03687 0.04010 = 0.03833 0.00187 0.00258 0.00275 C1 1 0.517266 0.225062 -0.011460 11.00000 0.02757 0.03592 = 0.04035 0.00455 0.00347 0.00193 C2 1 0.624636 0.140404 -0.045634 11.00000 0.03292 0.05062 = 0.04808 0.00699 0.00478 0.00948 AFIX 43 H2 2 0.741494 0.132797 -0.032613 11.00000 -1.20000 AFIX 0 C3 1 0.556282 0.065573 -0.100346 11.00000 0.04867 0.05597 = 0.04576 -0.00329 0.01122 0.00708 AFIX 43 H3 2 0.626753 0.006760 -0.124422 11.00000 -1.20000 AFIX 0 C4 1 0.384174 0.079693 -0.118214 11.00000 0.05380 0.05541 = 0.04770 -0.01137 -0.00142 0.00718 AFIX 43 H4 2 0.335955 0.032247 -0.154998 11.00000 -1.20000 AFIX 0 C5 1 0.283407 0.165376 -0.080815 11.00000 0.04142 0.05248 = 0.04607 -0.00039 -0.00475 0.00171 AFIX 43 H5 2 0.165867 0.173322 -0.092562 11.00000 -1.20000 AFIX 0 C6 1 0.587498 0.303126 0.047055 11.00000 0.02915 0.05093 = 0.04162 0.00388 0.00375 -0.00017 AFIX 43 H6 2 0.706213 0.305884 0.056788 11.00000 -1.20000 AFIX 0 C7 1 0.563524 0.439417 0.141179 11.00000 0.03607 0.03857 = 0.03514 0.00476 0.00336 0.00038 C8 1 0.730241 0.412640 0.167185 11.00000 0.04255 0.06047 = 0.04377 -0.00710 0.00375 0.00884 AFIX 43 H8 2 0.799629 0.341478 0.147924 11.00000 -1.20000 AFIX 0 C9 1 0.795159 0.489639 0.221136 11.00000 0.04918 0.07785 = 0.03606 -0.00327 0.00575 -0.00320 C10 1 0.689456 0.593727 0.249675 11.00000 0.05802 0.06200 = 0.03910 -0.00222 0.00120 -0.00500 AFIX 43 H10 2 0.731857 0.647878 0.285728 11.00000 -1.20000 AFIX 0 C11 1 0.524546 0.617231 0.225409 11.00000 0.06302 0.06503 = 0.04432 -0.00772 0.00603 0.01354 AFIX 43 H11 2 0.454759 0.686699 0.245345 11.00000 -1.20000 AFIX 0 C12 1 0.458776 0.540016 0.171790 11.00000 0.04450 0.06274 = 0.04129 -0.00210 -0.00298 0.00869 AFIX 43 H12 2 0.344642 0.555311 0.156205 11.00000 -1.20000 AFIX 0 C13 1 0.978215 0.458499 0.247956 11.00000 0.05907 0.15141 = 0.07625 -0.04121 -0.02437 0.02315 AFIX 137 H13A 2 0.977464 0.390995 0.284080 11.00000 -1.50000 H13B 2 1.033074 0.556700 0.260143 11.00000 -1.50000 H13C 2 1.040381 0.408023 0.216680 11.00000 -1.50000 HKLF 4 REM tu1secm in P2(1)/c REM R1 = 0.0289 for 2096 Fo > 4sig(Fo) and 0.0347 for all 2465 data REM 164 parameters refined using 0 restraints END WGHT 0.0338 0.0000 REM Highest difference peak 1.073, deepest hole -1.149, 1-sigma level 0.119 Q1 1 0.0632 0.3601 0.0522 11.00000 0.05 1.07 Q2 1 0.1633 0.3494 0.0893 11.00000 0.05 1.02 Q3 1 0.3058 0.3762 0.0386 11.00000 0.05 0.74 Q4 1 0.1788 0.2540 0.0414 11.00000 0.05 0.71 Q5 1 0.1929 0.3505 -0.0107 11.00000 0.05 0.55 Q6 1 0.1798 0.4738 0.0425 11.00000 0.05 0.52 Q7 1 0.9268 0.2989 0.0449 11.00000 0.05 0.46 Q8 1 0.0706 0.3455 0.0077 11.00000 0.05 0.43 Q9 1 0.3227 0.2831 0.1201 11.00000 0.05 0.33 Q10 1 0.6869 0.4744 0.1404 11.00000 0.05 0.33 Q11 1 0.3947 -0.1907 -0.1484 11.00000 0.05 0.32 Q12 1 0.8099 0.3316 0.3395 11.00000 0.05 0.32 Q13 1 0.1296 0.5683 0.1021 11.00000 0.05 0.32 Q14 1 0.8533 0.3543 0.0327 11.00000 0.05 0.31 Q15 1 -0.0047 0.5381 0.0299 11.00000 0.05 0.31 Q16 1 0.5536 0.3546 -0.0585 11.00000 0.05 0.30 Q17 1 0.7262 0.2110 -0.1212 11.00000 0.05 0.30 Q18 1 0.5508 0.2624 0.0285 11.00000 0.05 0.30 Q19 1 -0.0120 0.5391 0.0735 11.00000 0.05 0.29 Q20 1 0.0508 0.6513 0.0190 11.00000 0.05 0.29 ; data_6 _database_code_depnum_ccdc_archive 'CCDC 892210' #TrackingRef '6.cif' # t1tusham _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl4 Hg2 N4' _chemical_formula_sum 'C26 H24 Cl4 Hg2 N4' _chemical_formula_weight 935.47 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' 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' _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 7.5731(19) _cell_length_b 15.346(4) _cell_length_c 12.503(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.653(4) _cell_angle_gamma 90.00 _cell_volume 1440.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2758 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 22.64 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 11.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1172 _exptl_absorpt_correction_T_max 0.1545 _exptl_absorpt_process_details SADABS _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 '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 13356 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2528 _reflns_number_gt 1885 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0267P)^2^+1.0774P] 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 2528 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.68283(4) 0.05924(2) 0.60594(3) 0.05642(15) Uani 1 1 d . . . Cl1 Cl 0.5653(3) 0.09482(14) 0.42137(18) 0.0654(6) Uani 1 1 d . . . Cl2 Cl 0.9087(3) -0.02893(16) 0.6976(3) 0.1043(11) Uani 1 1 d . . . N1 N 0.4907(8) 0.1202(4) 0.7190(5) 0.0440(16) Uani 1 1 d . . . N2 N 0.7762(8) 0.2115(4) 0.6533(5) 0.0461(16) Uani 1 1 d . . . C1 C 0.5212(10) 0.2041(5) 0.7487(6) 0.0450(19) Uani 1 1 d . . . C2 C 0.4097(10) 0.2485(5) 0.8072(6) 0.049(2) Uani 1 1 d . . . H2 H 0.4315 0.3068 0.8246 0.059 Uiso 1 1 calc R . . C3 C 0.2650(11) 0.2067(6) 0.8405(7) 0.056(2) Uani 1 1 d . . . H3 H 0.1878 0.2357 0.8802 0.067 Uiso 1 1 calc R . . C4 C 0.2395(11) 0.1199(5) 0.8123(7) 0.056(2) Uani 1 1 d . . . H4 H 0.1468 0.0884 0.8356 0.067 Uiso 1 1 calc R . . C5 C 0.3530(11) 0.0808(5) 0.7494(7) 0.051(2) Uani 1 1 d . . . H5 H 0.3303 0.0235 0.7274 0.061 Uiso 1 1 calc R . . C6 C 0.6765(10) 0.2480(5) 0.7125(6) 0.046(2) Uani 1 1 d . . . H6 H 0.7016 0.3051 0.7345 0.055 Uiso 1 1 calc R . . C7 C 0.9213(10) 0.2559(5) 0.6167(6) 0.0419(19) Uani 1 1 d . . . C8 C 0.9448(12) 0.3453(6) 0.6181(7) 0.060(2) Uani 1 1 d . . . H8 H 0.8629 0.3810 0.6460 0.072 Uiso 1 1 calc R . . C9 C 1.0895(14) 0.3817(6) 0.5782(8) 0.076(3) Uani 1 1 d . . . H9 H 1.1037 0.4419 0.5803 0.091 Uiso 1 1 calc R . . C10 C 1.2135(12) 0.3313(7) 0.5353(7) 0.064(2) Uani 1 1 d . . . C11 C 1.1910(11) 0.2429(6) 0.5323(6) 0.057(2) Uani 1 1 d . . . H11 H 1.2731 0.2078 0.5036 0.069 Uiso 1 1 calc R . . C12 C 1.0468(11) 0.2056(5) 0.5716(7) 0.055(2) Uani 1 1 d . . . H12 H 1.0326 0.1454 0.5679 0.066 Uiso 1 1 calc R . . C13 C 1.3664(12) 0.3754(8) 0.4898(8) 0.097(4) Uani 1 1 d . . . H13A H 1.4568 0.3913 0.5478 0.146 Uiso 1 1 calc R . . H13B H 1.3236 0.4268 0.4509 0.146 Uiso 1 1 calc R . . H13C H 1.4157 0.3361 0.4419 0.146 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 0.0628(2) 0.03804(19) 0.0691(3) -0.0068(2) 0.01136(16) 0.00382(18) Cl1 0.0916(17) 0.0496(13) 0.0571(14) -0.0073(11) 0.0177(12) -0.0240(12) Cl2 0.0662(16) 0.0410(14) 0.196(3) 0.0150(17) -0.0168(18) -0.0007(12) N1 0.050(4) 0.039(4) 0.045(4) -0.007(3) 0.009(3) 0.001(3) N2 0.057(4) 0.031(4) 0.049(4) -0.004(3) 0.005(3) 0.004(3) C1 0.054(5) 0.035(5) 0.044(5) 0.003(4) 0.002(4) 0.007(4) C2 0.058(5) 0.040(5) 0.050(5) -0.006(4) 0.009(4) 0.005(4) C3 0.057(5) 0.054(6) 0.059(6) -0.007(5) 0.014(4) 0.006(4) C4 0.050(5) 0.049(5) 0.071(6) -0.016(5) 0.021(5) -0.010(4) C5 0.052(5) 0.040(5) 0.059(6) -0.006(4) 0.004(4) -0.004(4) C6 0.054(5) 0.035(4) 0.047(5) -0.007(4) 0.004(4) -0.003(4) C7 0.042(5) 0.042(5) 0.042(5) -0.003(4) 0.004(4) -0.005(4) C8 0.077(6) 0.047(5) 0.059(6) -0.006(4) 0.021(5) -0.003(5) C9 0.100(8) 0.053(6) 0.081(7) -0.004(5) 0.036(6) -0.028(6) C10 0.062(6) 0.081(8) 0.052(6) -0.004(5) 0.015(5) -0.018(5) C11 0.059(6) 0.065(6) 0.048(6) 0.002(5) 0.010(4) 0.008(5) C12 0.061(5) 0.043(5) 0.060(6) 0.006(4) 0.005(5) 0.012(4) C13 0.071(7) 0.129(10) 0.095(9) 0.010(7) 0.027(6) -0.035(7) _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(6) . ? Hg1 Cl2 2.355(3) . ? Hg1 Cl1 2.423(2) . ? Hg1 N2 2.490(6) . ? N1 C5 1.305(9) . ? N1 C1 1.352(9) . ? N2 C6 1.258(9) . ? N2 C7 1.420(9) . ? C1 C2 1.370(10) . ? C1 C6 1.477(10) . ? C2 C3 1.380(10) . ? C2 H2 0.9300 . ? C3 C4 1.385(11) . ? C3 H3 0.9300 . ? C4 C5 1.378(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.383(10) . ? C7 C12 1.401(10) . ? C8 C9 1.381(11) . ? C8 H8 0.9300 . ? C9 C10 1.378(12) . ? C9 H9 0.9300 . ? C10 C11 1.368(12) . ? C10 C13 1.515(11) . ? C11 C12 1.380(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 Cl2 113.76(17) . . ? N1 Hg1 Cl1 107.73(16) . . ? Cl2 Hg1 Cl1 138.07(11) . . ? N1 Hg1 N2 70.3(2) . . ? Cl2 Hg1 N2 104.98(15) . . ? Cl1 Hg1 N2 94.10(15) . . ? C5 N1 C1 118.4(7) . . ? C5 N1 Hg1 124.9(5) . . ? C1 N1 Hg1 116.5(5) . . ? C6 N2 C7 121.8(6) . . ? C6 N2 Hg1 112.6(5) . . ? C7 N2 Hg1 125.6(5) . . ? N1 C1 C2 121.6(7) . . ? N1 C1 C6 117.7(7) . . ? C2 C1 C6 120.6(7) . . ? C1 C2 C3 120.1(8) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 117.4(8) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C5 C4 C3 119.2(8) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.2(7) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C1 122.8(7) . . ? N2 C6 H6 118.6 . . ? C1 C6 H6 118.6 . . ? C8 C7 C12 117.3(7) . . ? C8 C7 N2 125.2(7) . . ? C12 C7 N2 117.4(7) . . ? C9 C8 C7 120.2(8) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 121.9(9) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C11 C10 C9 118.5(8) . . ? C11 C10 C13 122.1(9) . . ? C9 C10 C13 119.4(9) . . ? C10 C11 C12 120.2(8) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 121.8(8) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 Hg1 N1 C5 -83.8(6) . . . . ? Cl1 Hg1 N1 C5 90.0(6) . . . . ? N2 Hg1 N1 C5 178.1(7) . . . . ? Cl2 Hg1 N1 C1 100.3(5) . . . . ? Cl1 Hg1 N1 C1 -85.9(5) . . . . ? N2 Hg1 N1 C1 2.2(5) . . . . ? N1 Hg1 N2 C6 -1.0(5) . . . . ? Cl2 Hg1 N2 C6 -111.3(5) . . . . ? Cl1 Hg1 N2 C6 106.4(5) . . . . ? N1 Hg1 N2 C7 -179.1(6) . . . . ? Cl2 Hg1 N2 C7 70.6(6) . . . . ? Cl1 Hg1 N2 C7 -71.7(6) . . . . ? C5 N1 C1 C2 -1.4(11) . . . . ? Hg1 N1 C1 C2 174.8(6) . . . . ? C5 N1 C1 C6 -179.3(7) . . . . ? Hg1 N1 C1 C6 -3.1(8) . . . . ? N1 C1 C2 C3 2.2(12) . . . . ? C6 C1 C2 C3 180.0(7) . . . . ? C1 C2 C3 C4 0.0(12) . . . . ? C2 C3 C4 C5 -2.8(13) . . . . ? C1 N1 C5 C4 -1.6(12) . . . . ? Hg1 N1 C5 C4 -177.4(6) . . . . ? C3 C4 C5 N1 3.7(13) . . . . ? C7 N2 C6 C1 177.9(7) . . . . ? Hg1 N2 C6 C1 -0.3(9) . . . . ? N1 C1 C6 N2 2.3(11) . . . . ? C2 C1 C6 N2 -175.6(7) . . . . ? C6 N2 C7 C8 -16.4(12) . . . . ? Hg1 N2 C7 C8 161.6(6) . . . . ? C6 N2 C7 C12 166.4(7) . . . . ? Hg1 N2 C7 C12 -15.6(9) . . . . ? C12 C7 C8 C9 -1.4(12) . . . . ? N2 C7 C8 C9 -178.6(8) . . . . ? C7 C8 C9 C10 0.5(14) . . . . ? C8 C9 C10 C11 0.2(14) . . . . ? C8 C9 C10 C13 178.2(9) . . . . ? C9 C10 C11 C12 0.0(13) . . . . ? C13 C10 C11 C12 -178.0(8) . . . . ? C10 C11 C12 C7 -0.9(13) . . . . ? C8 C7 C12 C11 1.6(12) . . . . ? N2 C7 C12 C11 179.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.718 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.120 _iucr_refine_instructions_details ; TITL t1tusham in P2(1)/n CELL 0.71073 7.5731 15.3463 12.5034 90.000 97.653 90.000 ZERR 2.00 0.0019 0.0039 0.0032 0.000 0.004 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N Hg Cl UNIT 52 48 8 4 8 OMIT -3.00 50.00 L.S. 10 BOND $H ACTA FMAP 2 PLAN 20 size 0.27 0.29 0.34 conf TEMP 20 WGHT 0.026700 1.077400 FVAR 0.31787 MOLE 1 HG1 4 0.682826 0.059236 0.605937 11.00000 0.06283 0.03804 = 0.06908 -0.00676 0.01136 0.00382 CL1 5 0.565324 0.094825 0.421365 11.00000 0.09158 0.04957 = 0.05714 -0.00734 0.01774 -0.02395 CL2 5 0.908691 -0.028925 0.697619 11.00000 0.06616 0.04103 = 0.19642 0.01504 -0.01678 -0.00068 N1 3 0.490675 0.120205 0.719028 11.00000 0.04953 0.03861 = 0.04475 -0.00699 0.00942 0.00076 N2 3 0.776211 0.211512 0.653275 11.00000 0.05711 0.03132 = 0.04917 -0.00378 0.00471 0.00419 C1 1 0.521231 0.204125 0.748708 11.00000 0.05446 0.03534 = 0.04392 0.00254 0.00238 0.00719 C2 1 0.409680 0.248463 0.807230 11.00000 0.05803 0.04013 = 0.05014 -0.00560 0.00892 0.00517 AFIX 43 H2 2 0.431454 0.306754 0.824570 11.00000 -1.20000 AFIX 0 C3 1 0.265023 0.206720 0.840480 11.00000 0.05674 0.05398 = 0.05945 -0.00722 0.01406 0.00572 AFIX 43 H3 2 0.187772 0.235734 0.880225 11.00000 -1.20000 AFIX 0 C4 1 0.239456 0.119906 0.812315 11.00000 0.05045 0.04893 = 0.07099 -0.01562 0.02143 -0.00991 AFIX 43 H4 2 0.146839 0.088401 0.835604 11.00000 -1.20000 AFIX 0 C5 1 0.352958 0.080789 0.749353 11.00000 0.05176 0.04006 = 0.05892 -0.00615 0.00397 -0.00442 AFIX 43 H5 2 0.330298 0.023509 0.727409 11.00000 -1.20000 AFIX 0 C6 1 0.676515 0.248002 0.712541 11.00000 0.05413 0.03538 = 0.04733 -0.00666 0.00364 -0.00328 AFIX 43 H6 2 0.701631 0.305068 0.734546 11.00000 -1.20000 AFIX 0 C7 1 0.921317 0.255939 0.616723 11.00000 0.04182 0.04180 = 0.04161 -0.00274 0.00367 -0.00515 C8 1 0.944847 0.345288 0.618102 11.00000 0.07726 0.04652 = 0.05885 -0.00587 0.02115 -0.00288 AFIX 43 H8 2 0.862934 0.381024 0.646003 11.00000 -1.20000 AFIX 0 C9 1 1.089533 0.381657 0.578202 11.00000 0.09963 0.05291 = 0.08055 -0.00417 0.03608 -0.02825 AFIX 43 H9 2 1.103733 0.441853 0.580341 11.00000 -1.20000 AFIX 0 C10 1 1.213540 0.331347 0.535293 11.00000 0.06195 0.08115 = 0.05178 -0.00445 0.01455 -0.01812 C11 1 1.190953 0.242888 0.532277 11.00000 0.05891 0.06513 = 0.04850 0.00197 0.01004 0.00800 AFIX 43 H11 2 1.273081 0.207761 0.503645 11.00000 -1.20000 AFIX 0 C12 1 1.046797 0.205609 0.571554 11.00000 0.06117 0.04267 = 0.06003 0.00555 0.00514 0.01165 AFIX 43 H12 2 1.032555 0.145443 0.567942 11.00000 -1.20000 AFIX 0 C13 1 1.366426 0.375391 0.489828 11.00000 0.07150 0.12923 = 0.09525 0.00952 0.02669 -0.03526 AFIX 137 H13A 2 1.456816 0.391257 0.547831 11.00000 -1.50000 H13B 2 1.323628 0.426769 0.450900 11.00000 -1.50000 H13C 2 1.415699 0.336053 0.441947 11.00000 -1.50000 HKLF 4 REM t1tusham in P2(1)/n REM R1 = 0.0413 for 1885 Fo > 4sig(Fo) and 0.0648 for all 2528 data REM 164 parameters refined using 0 restraints END WGHT 0.0232 1.3578 REM Highest difference peak 0.718, deepest hole -1.043, 1-sigma level 0.120 Q1 1 0.5386 0.0606 0.6154 11.00000 0.05 0.72 Q2 1 0.8282 0.0581 0.5966 11.00000 0.05 0.60 Q3 1 1.0110 -0.1011 0.8017 11.00000 0.05 0.58 Q4 1 0.7555 0.0724 0.6747 11.00000 0.05 0.56 Q5 1 0.6488 0.0349 0.4679 11.00000 0.05 0.55 Q6 1 0.7510 0.0929 0.6557 11.00000 0.05 0.55 Q7 1 0.7187 0.3131 0.8561 11.00000 0.05 0.51 Q8 1 0.8066 0.3662 0.8599 11.00000 0.05 0.45 Q9 1 0.9366 -0.0094 0.6230 11.00000 0.05 0.44 Q10 1 0.9346 -0.0579 0.8184 11.00000 0.05 0.44 Q11 1 0.5537 0.1112 0.2779 11.00000 0.05 0.44 Q12 1 0.8436 -0.0178 0.7178 11.00000 0.05 0.44 Q13 1 0.7726 0.0071 0.6397 11.00000 0.05 0.42 Q14 1 0.9848 -0.0414 0.7592 11.00000 0.05 0.42 Q15 1 0.7134 0.0221 0.5438 11.00000 0.05 0.41 Q16 1 0.8679 -0.0598 0.6463 11.00000 0.05 0.41 Q17 1 0.5228 0.0221 0.3846 11.00000 0.05 0.39 Q18 1 0.6166 0.1022 0.5558 11.00000 0.05 0.39 Q19 1 1.0043 -0.0164 0.8236 11.00000 0.05 0.37 Q20 1 1.3146 0.2161 0.4343 11.00000 0.05 0.37 ; data_7 _database_code_depnum_ccdc_archive 'CCDC 892211' #TrackingRef '7.cif' # L1022 _audit_creation_method SHELXL-97 _audit_creation_date 10-12-20 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C26 H24 Br4 Hg2 N4' _chemical_formula_sum 'C26 H24 Br4 Hg2 N4' _chemical_formula_weight 1113.32 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 52 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 48 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Br Br 8 -0.2901 2.4595 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Hg Hg 4 -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 8 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.2201(1) _cell_length_b 17.5934(3) _cell_length_c 10.0430(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.6895(9) _cell_angle_gamma 90.00 _cell_volume 1404.94(4) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 33060 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 16.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 0.213 _exptl_special_details ; Solvent used: MeCN / MeOH Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.506(1) Frames collected: 438 Seconds exposure per frame: 54 Degrees rotation per frame: 1.8 Crystal-Detector distance (mm): 30.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 41875 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.99 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 8003 _reflns_number_gt 7309 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF94 (Beurskens et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2006)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+2.3344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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_abs_structure_details 'Flack & Bernardinelli (2000), 3798 Friedel pairs' _refine_ls_abs_structure_Flack 0.259(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 8003 _refine_ls_number_parameters 328 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.359 _refine_diff_density_min -2.002 _refine_diff_density_rms 0.249 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 0.82158(3) 0.497219(14) 0.93857(2) 0.02669(6) Uani 1 1 d . . . Hg21 Hg 0.39573(3) 0.564968(14) 0.54611(2) 0.02772(6) Uani 1 1 d . . . Br1 Br 0.53934(8) 0.43897(4) 0.83919(7) 0.03179(15) Uani 1 1 d . . . Br2 Br 1.07440(9) 0.42380(4) 0.89472(7) 0.03288(16) Uani 1 1 d . . . Br21 Br 0.67589(9) 0.61996(4) 0.66301(7) 0.03063(15) Uani 1 1 d . . . Br22 Br 0.14572(9) 0.64349(4) 0.58394(7) 0.03110(15) Uani 1 1 d . . . N1 N 0.9614(7) 0.6090(3) 1.0039(5) 0.0230(11) Uani 1 1 d . . . N2 N 0.8521(6) 0.5166(3) 1.1873(5) 0.0218(11) Uani 1 1 d . . . N21 N 0.2655(7) 0.4510(3) 0.4776(5) 0.0236(11) Uani 1 1 d . . . N22 N 0.3871(7) 0.5443(3) 0.3015(5) 0.0229(11) Uani 1 1 d . . . C1 C 0.9856(8) 0.6305(4) 1.1362(6) 0.0230(12) Uani 1 1 d . . . C2 C 1.0741(9) 0.6957(4) 1.1861(7) 0.0274(14) Uani 1 1 d . . . H2 H 1.0878 0.7102 1.2794 0.033 Uiso 1 1 calc R . . C3 C 1.1430(8) 0.7401(4) 1.0999(7) 0.0289(14) Uani 1 1 d . . . H3 H 1.2031 0.7854 1.1322 0.035 Uiso 1 1 calc R . . C4 C 1.1210(8) 0.7160(4) 0.9657(7) 0.0262(13) Uani 1 1 d . . . H4 H 1.1694 0.7441 0.9047 0.031 Uiso 1 1 calc R . . C5 C 1.0284(8) 0.6508(4) 0.9193(7) 0.0267(13) Uani 1 1 d . . . H5 H 1.0123 0.6355 0.8261 0.032 Uiso 1 1 calc R . . C6 C 0.9174(8) 0.5812(4) 1.2280(6) 0.0240(13) Uani 1 1 d . . . H6 H 0.9221 0.5977 1.3190 0.029 Uiso 1 1 calc R . . C7 C 0.7903(8) 0.4677(4) 1.2775(6) 0.0217(12) Uani 1 1 d . . . C8 C 0.7979(8) 0.4861(4) 1.4156(6) 0.0267(14) Uani 1 1 d . . . H8 H 0.8438 0.5332 1.4537 0.032 Uiso 1 1 calc R . . C9 C 0.7366(9) 0.4337(4) 1.4952(6) 0.0253(13) Uani 1 1 d . . . H9 H 0.7402 0.4462 1.5879 0.030 Uiso 1 1 calc R . . C10 C 0.6712(8) 0.3648(4) 1.4438(6) 0.0238(13) Uani 1 1 d . . . C11 C 0.6660(9) 0.3468(4) 1.3060(7) 0.0268(14) Uani 1 1 d . . . H11 H 0.6229 0.2991 1.2689 0.032 Uiso 1 1 calc R . . C12 C 0.7241(9) 0.3988(4) 1.2240(7) 0.0278(14) Uani 1 1 d . . . H12 H 0.7180 0.3868 1.1306 0.033 Uiso 1 1 calc R . . C13 C 0.6051(10) 0.3085(4) 1.5316(8) 0.0324(15) Uani 1 1 d . . . H13A H 0.6112 0.3309 1.6221 0.049 Uiso 1 1 calc R . . H13B H 0.6733 0.2621 1.5431 0.049 Uiso 1 1 calc R . . H13C H 0.4879 0.2959 1.4865 0.049 Uiso 1 1 calc R . . C21 C 0.2579(8) 0.4285(4) 0.3472(6) 0.0203(11) Uani 1 1 d . . . C22 C 0.1816(9) 0.3607(4) 0.2965(7) 0.0290(14) Uani 1 1 d . . . H22 H 0.1786 0.3451 0.2053 0.035 Uiso 1 1 calc R . . C23 C 0.1093(9) 0.3156(4) 0.3796(8) 0.0316(15) Uani 1 1 d . . . H23 H 0.0559 0.2690 0.3463 0.038 Uiso 1 1 calc R . . C24 C 0.1169(8) 0.3402(4) 0.5126(8) 0.0314(15) Uani 1 1 d . . . H24 H 0.0692 0.3104 0.5719 0.038 Uiso 1 1 calc R . . C25 C 0.1951(8) 0.4090(4) 0.5580(6) 0.0264(14) Uani 1 1 d . . . H25 H 0.1982 0.4264 0.6482 0.032 Uiso 1 1 calc R . . C26 C 0.3287(8) 0.4783(4) 0.2610(6) 0.0230(13) Uani 1 1 d . . . H26 H 0.3320 0.4614 0.1719 0.028 Uiso 1 1 calc R . . C27 C 0.4512(8) 0.5934(4) 0.2150(6) 0.0212(12) Uani 1 1 d . . . C28 C 0.4340(8) 0.5821(4) 0.0759(7) 0.0266(14) Uani 1 1 d . . . H28 H 0.3773 0.5382 0.0323 0.032 Uiso 1 1 calc R . . C29 C 0.4991(9) 0.6344(4) -0.0010(7) 0.0263(13) Uani 1 1 d . . . H29 H 0.4871 0.6251 -0.0962 0.032 Uiso 1 1 calc R . . C30 C 0.5818(8) 0.7003(4) 0.0582(7) 0.0234(12) Uani 1 1 d . . . C31 C 0.5971(9) 0.7104(4) 0.1999(7) 0.0261(14) Uani 1 1 d . . . H31 H 0.6540 0.7540 0.2446 0.031 Uiso 1 1 calc R . . C32 C 0.5323(9) 0.6591(4) 0.2753(7) 0.0295(15) Uani 1 1 d . . . H32 H 0.5428 0.6685 0.3702 0.035 Uiso 1 1 calc R . . C33 C 0.6475(9) 0.7573(5) -0.0244(7) 0.0314(15) Uani 1 1 d . . . H33A H 0.7661 0.7676 0.0198 0.047 Uiso 1 1 calc R . . H33B H 0.5826 0.8044 -0.0301 0.047 Uiso 1 1 calc R . . H33C H 0.6372 0.7373 -0.1172 0.047 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 0.02541(11) 0.03142(13) 0.02421(11) -0.00611(10) 0.00806(9) -0.00523(10) Hg21 0.02617(12) 0.03292(14) 0.02537(11) -0.00840(10) 0.00893(9) -0.00541(10) Br1 0.0279(3) 0.0391(4) 0.0274(3) -0.0059(3) 0.0052(3) -0.0091(3) Br2 0.0307(3) 0.0366(4) 0.0335(4) -0.0034(3) 0.0121(3) 0.0041(3) Br21 0.0291(3) 0.0366(4) 0.0246(3) -0.0041(3) 0.0038(2) -0.0066(3) Br22 0.0307(3) 0.0353(4) 0.0297(3) -0.0057(3) 0.0120(3) 0.0016(3) N1 0.022(3) 0.030(3) 0.018(2) 0.004(2) 0.006(2) 0.002(2) N2 0.018(2) 0.027(3) 0.020(2) -0.003(2) 0.0053(19) 0.0011(19) N21 0.023(3) 0.029(3) 0.019(2) 0.000(2) 0.004(2) -0.005(2) N22 0.021(2) 0.024(3) 0.022(2) 0.001(2) 0.004(2) -0.0011(19) C1 0.021(3) 0.026(3) 0.022(3) -0.000(2) 0.004(2) 0.001(2) C2 0.031(3) 0.026(3) 0.025(3) -0.004(3) 0.006(3) -0.001(3) C3 0.024(3) 0.029(4) 0.031(3) 0.001(3) 0.004(3) -0.003(3) C4 0.022(3) 0.027(3) 0.031(3) 0.004(3) 0.009(3) -0.001(2) C5 0.022(3) 0.033(4) 0.024(3) 0.003(3) 0.004(2) -0.003(3) C6 0.027(3) 0.029(4) 0.016(2) 0.002(2) 0.007(2) 0.004(2) C7 0.018(3) 0.030(3) 0.016(2) 0.001(2) 0.004(2) 0.002(2) C8 0.032(3) 0.028(4) 0.022(3) -0.004(3) 0.011(2) -0.001(3) C9 0.032(3) 0.030(3) 0.016(3) 0.002(2) 0.011(2) 0.005(3) C10 0.020(3) 0.030(3) 0.022(3) 0.004(3) 0.007(2) 0.004(2) C11 0.034(3) 0.020(3) 0.028(3) -0.001(2) 0.009(3) -0.004(3) C12 0.027(3) 0.032(4) 0.024(3) -0.008(3) 0.005(2) -0.002(3) C13 0.035(4) 0.029(4) 0.034(3) 0.007(3) 0.009(3) 0.002(3) C21 0.021(3) 0.018(3) 0.021(3) -0.003(2) 0.004(2) 0.001(2) C22 0.035(4) 0.028(3) 0.026(3) -0.006(3) 0.010(3) -0.006(3) C23 0.029(3) 0.027(4) 0.037(4) -0.001(3) 0.004(3) -0.005(3) C24 0.021(3) 0.036(4) 0.036(4) 0.012(3) 0.006(3) 0.001(3) C25 0.021(3) 0.039(4) 0.019(3) 0.006(3) 0.005(2) -0.001(3) C26 0.022(3) 0.024(4) 0.022(3) -0.004(2) 0.005(2) -0.000(2) C27 0.019(3) 0.022(3) 0.022(3) -0.004(2) 0.003(2) 0.004(2) C28 0.023(3) 0.033(4) 0.025(3) -0.009(3) 0.008(2) -0.008(2) C29 0.027(3) 0.030(4) 0.024(3) 0.002(3) 0.008(2) 0.005(3) C30 0.021(3) 0.023(3) 0.026(3) 0.001(2) 0.008(2) 0.001(2) C31 0.026(3) 0.025(3) 0.028(3) -0.002(3) 0.008(3) -0.001(2) C32 0.038(4) 0.027(3) 0.024(3) -0.003(3) 0.007(3) 0.004(3) C33 0.034(4) 0.033(4) 0.028(3) 0.005(3) 0.008(3) -0.001(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 2.288(6) . ? Hg1 N2 2.471(5) . ? Hg1 Br1 2.5010(7) . ? Hg1 Br2 2.5779(8) . ? Hg1 Br21 3.4749(8) . ? Hg21 N21 2.295(6) . ? Hg21 N22 2.467(5) . ? Hg21 Br21 2.4993(7) . ? Hg21 Br22 2.5831(7) . ? Hg21 Br1 3.6344(8) . ? N1 C5 1.343(8) . ? N1 C1 1.348(8) . ? N2 C6 1.278(9) . ? N2 C7 1.434(8) . ? N21 C25 1.330(8) . ? N21 C21 1.355(8) . ? N22 C26 1.283(8) . ? N22 C27 1.418(8) . ? C1 C2 1.383(10) . ? C1 C6 1.477(9) . ? C2 C3 1.388(10) . ? C2 H2 0.9500 . ? C3 C4 1.381(10) . ? C3 H3 0.9500 . ? C4 C5 1.390(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.380(10) . ? C7 C8 1.410(8) . ? C8 C9 1.395(9) . ? C8 H8 0.9500 . ? C9 C10 1.373(10) . ? C9 H9 0.9500 . ? C10 C11 1.410(9) . ? C10 C13 1.516(10) . ? C11 C12 1.393(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.383(9) . ? C21 C26 1.453(9) . ? C22 C23 1.390(10) . ? C22 H22 0.9500 . ? C23 C24 1.391(11) . ? C23 H23 0.9500 . ? C24 C25 1.392(11) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.383(9) . ? C27 C32 1.394(10) . ? C28 C29 1.393(9) . ? C28 H28 0.9500 . ? C29 C30 1.398(10) . ? C29 H29 0.9500 . ? C30 C31 1.408(9) . ? C30 C33 1.487(9) . ? C31 C32 1.369(10) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N2 71.13(18) . . ? N1 Hg1 Br1 144.52(13) . . ? N2 Hg1 Br1 107.83(12) . . ? N1 Hg1 Br2 96.39(13) . . ? N2 Hg1 Br2 111.26(12) . . ? Br1 Hg1 Br2 115.66(3) . . ? N1 Hg1 Br21 74.98(13) . . ? N2 Hg1 Br21 130.20(13) . . ? Br1 Hg1 Br21 80.75(2) . . ? Br2 Hg1 Br21 107.78(2) . . ? N21 Hg21 N22 71.30(18) . . ? N21 Hg21 Br21 141.55(14) . . ? N22 Hg21 Br21 108.38(12) . . ? N21 Hg21 Br22 100.57(14) . . ? N22 Hg21 Br22 113.72(12) . . ? Br21 Hg21 Br22 113.36(3) . . ? N21 Hg21 Br1 74.97(13) . . ? N22 Hg21 Br1 129.66(12) . . ? Br21 Hg21 Br1 77.54(2) . . ? Br22 Hg21 Br1 108.31(2) . . ? Hg1 Br1 Hg21 98.70(2) . . ? Hg21 Br21 Hg1 102.94(2) . . ? C5 N1 C1 119.2(6) . . ? C5 N1 Hg1 123.1(4) . . ? C1 N1 Hg1 117.5(4) . . ? C6 N2 C7 121.3(5) . . ? C6 N2 Hg1 111.9(4) . . ? C7 N2 Hg1 126.5(4) . . ? C25 N21 C21 120.3(6) . . ? C25 N21 Hg21 123.0(5) . . ? C21 N21 Hg21 116.6(4) . . ? C26 N22 C27 121.7(5) . . ? C26 N22 Hg21 111.3(4) . . ? C27 N22 Hg21 126.8(4) . . ? N1 C1 C2 121.5(6) . . ? N1 C1 C6 117.8(6) . . ? C2 C1 C6 120.6(6) . . ? C1 C2 C3 120.1(6) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 117.6(7) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 120.4(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 121.1(6) . . ? N1 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? N2 C6 C1 121.2(6) . . ? N2 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C12 C7 C8 120.0(6) . . ? C12 C7 N2 116.7(5) . . ? C8 C7 N2 123.3(6) . . ? C9 C8 C7 118.6(6) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C10 C9 C8 122.2(6) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 118.5(6) . . ? C9 C10 C13 121.5(6) . . ? C11 C10 C13 119.9(6) . . ? C12 C11 C10 120.3(6) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C7 C12 C11 120.4(6) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N21 C21 C22 120.9(6) . . ? N21 C21 C26 118.2(6) . . ? C22 C21 C26 120.9(6) . . ? C21 C22 C23 119.6(6) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 118.5(7) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 C25 119.3(6) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N21 C25 C24 121.3(6) . . ? N21 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? N22 C26 C21 122.1(6) . . ? N22 C26 H26 118.9 . . ? C21 C26 H26 118.9 . . ? C28 C27 C32 118.2(6) . . ? C28 C27 N22 124.9(6) . . ? C32 C27 N22 116.8(6) . . ? C27 C28 C29 120.7(6) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C30 121.7(6) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 116.3(6) . . ? C29 C30 C33 121.9(6) . . ? C31 C30 C33 121.8(6) . . ? C32 C31 C30 121.9(7) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C27 121.1(6) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 N1 Hg1 Br1 Hg21 48.7(2) . . . . ? N2 Hg1 Br1 Hg21 130.98(13) . . . . ? Br2 Hg1 Br1 Hg21 -103.78(3) . . . . ? Br21 Hg1 Br1 Hg21 1.589(19) . . . . ? N21 Hg21 Br1 Hg1 150.61(14) . . . . ? N22 Hg21 Br1 Hg1 101.44(16) . . . . ? Br21 Hg21 Br1 Hg1 -2.23(3) . . . . ? Br22 Hg21 Br1 Hg1 -113.01(3) . . . . ? N21 Hg21 Br21 Hg1 -43.5(2) . . . . ? N22 Hg21 Br21 Hg1 -126.34(13) . . . . ? Br22 Hg21 Br21 Hg1 106.41(3) . . . . ? Br1 Hg21 Br21 Hg1 1.63(2) . . . . ? N1 Hg1 Br21 Hg21 -156.23(14) . . . . ? N2 Hg1 Br21 Hg21 -107.93(16) . . . . ? Br1 Hg1 Br21 Hg21 -2.34(3) . . . . ? Br2 Hg1 Br21 Hg21 111.76(3) . . . . ? N2 Hg1 N1 C5 173.8(5) . . . . ? Br1 Hg1 N1 C5 -91.8(5) . . . . ? Br2 Hg1 N1 C5 63.4(5) . . . . ? Br21 Hg1 N1 C5 -43.3(5) . . . . ? N2 Hg1 N1 C1 -2.0(4) . . . . ? Br1 Hg1 N1 C1 92.5(5) . . . . ? Br2 Hg1 N1 C1 -112.3(4) . . . . ? Br21 Hg1 N1 C1 141.0(5) . . . . ? N1 Hg1 N2 C6 5.2(4) . . . . ? Br1 Hg1 N2 C6 -137.3(4) . . . . ? Br2 Hg1 N2 C6 94.8(4) . . . . ? Br21 Hg1 N2 C6 -44.4(5) . . . . ? N1 Hg1 N2 C7 178.8(5) . . . . ? Br1 Hg1 N2 C7 36.2(5) . . . . ? Br2 Hg1 N2 C7 -91.6(5) . . . . ? Br21 Hg1 N2 C7 129.1(4) . . . . ? N22 Hg21 N21 C25 -174.4(6) . . . . ? Br21 Hg21 N21 C25 89.4(5) . . . . ? Br22 Hg21 N21 C25 -62.7(5) . . . . ? Br1 Hg21 N21 C25 43.6(5) . . . . ? N22 Hg21 N21 C21 3.4(4) . . . . ? Br21 Hg21 N21 C21 -92.8(5) . . . . ? Br22 Hg21 N21 C21 115.1(4) . . . . ? Br1 Hg21 N21 C21 -138.6(5) . . . . ? N21 Hg21 N22 C26 -5.7(4) . . . . ? Br21 Hg21 N22 C26 133.7(4) . . . . ? Br22 Hg21 N22 C26 -99.3(4) . . . . ? Br1 Hg21 N22 C26 44.8(5) . . . . ? N21 Hg21 N22 C27 -179.8(5) . . . . ? Br21 Hg21 N22 C27 -40.4(5) . . . . ? Br22 Hg21 N22 C27 86.6(5) . . . . ? Br1 Hg21 N22 C27 -129.3(4) . . . . ? C5 N1 C1 C2 1.7(9) . . . . ? Hg1 N1 C1 C2 177.6(5) . . . . ? C5 N1 C1 C6 -177.0(6) . . . . ? Hg1 N1 C1 C6 -1.1(7) . . . . ? N1 C1 C2 C3 -1.1(10) . . . . ? C6 C1 C2 C3 177.6(6) . . . . ? C1 C2 C3 C4 -0.7(10) . . . . ? C2 C3 C4 C5 1.9(10) . . . . ? C1 N1 C5 C4 -0.5(9) . . . . ? Hg1 N1 C5 C4 -176.1(5) . . . . ? C3 C4 C5 N1 -1.4(10) . . . . ? C7 N2 C6 C1 178.1(6) . . . . ? Hg1 N2 C6 C1 -8.0(7) . . . . ? N1 C1 C6 N2 6.7(9) . . . . ? C2 C1 C6 N2 -172.1(6) . . . . ? C6 N2 C7 C12 -179.2(6) . . . . ? Hg1 N2 C7 C12 7.8(8) . . . . ? C6 N2 C7 C8 -0.6(9) . . . . ? Hg1 N2 C7 C8 -173.5(5) . . . . ? C12 C7 C8 C9 -0.4(10) . . . . ? N2 C7 C8 C9 -178.9(6) . . . . ? C7 C8 C9 C10 0.8(10) . . . . ? C8 C9 C10 C11 -0.1(10) . . . . ? C8 C9 C10 C13 180.0(6) . . . . ? C9 C10 C11 C12 -0.9(10) . . . . ? C13 C10 C11 C12 179.0(6) . . . . ? C8 C7 C12 C11 -0.7(10) . . . . ? N2 C7 C12 C11 178.0(6) . . . . ? C10 C11 C12 C7 1.4(11) . . . . ? C25 N21 C21 C22 -2.0(10) . . . . ? Hg21 N21 C21 C22 -179.9(5) . . . . ? C25 N21 C21 C26 176.7(6) . . . . ? Hg21 N21 C21 C26 -1.2(7) . . . . ? N21 C21 C22 C23 1.1(10) . . . . ? C26 C21 C22 C23 -177.6(6) . . . . ? C21 C22 C23 C24 -0.3(11) . . . . ? C22 C23 C24 C25 0.4(10) . . . . ? C21 N21 C25 C24 2.1(10) . . . . ? Hg21 N21 C25 C24 179.9(5) . . . . ? C23 C24 C25 N21 -1.3(10) . . . . ? C27 N22 C26 C21 -178.0(5) . . . . ? Hg21 N22 C26 C21 7.5(7) . . . . ? N21 C21 C26 N22 -4.8(9) . . . . ? C22 C21 C26 N22 173.9(7) . . . . ? C26 N22 C27 C28 10.9(10) . . . . ? Hg21 N22 C27 C28 -175.6(5) . . . . ? C26 N22 C27 C32 -171.4(6) . . . . ? Hg21 N22 C27 C32 2.1(8) . . . . ? C32 C27 C28 C29 1.2(10) . . . . ? N22 C27 C28 C29 178.9(6) . . . . ? C27 C28 C29 C30 -0.8(10) . . . . ? C28 C29 C30 C31 0.7(10) . . . . ? C28 C29 C30 C33 -178.4(6) . . . . ? C29 C30 C31 C32 -1.0(10) . . . . ? C33 C30 C31 C32 178.0(7) . . . . ? C30 C31 C32 C27 1.5(11) . . . . ? C28 C27 C32 C31 -1.6(10) . . . . ? N22 C27 C32 C31 -179.4(6) . . . . ? _iucr_refine_instructions_details ; TITL TSBB-298 (L1022) CELL 0.71073 8.2201 17.5934 10.0430 90.0000 104.6895 90.0000 ZERR 2 0.0001 0.0003 0.0002 0.0000 0.0009 0.0000 LATT -1 SYMM -X, .50+Y, -Z SFAC C H BR HG N UNIT 52 48 8 4 8 MERG 2 TEMP -113 L.S. 4 BOND $H CONF ACTA FMAP 2 TWIN PLAN 10 BIND Hg1 Br21 BIND Hg21 Br1 WGHT 0.038800 2.334400 BASF 0.25930 FVAR 0.33190 HG1 4 0.821584 0.497219 0.938569 11.00000 0.02541 0.03142 = 0.02421 -0.00611 0.00806 -0.00523 HG21 4 0.395728 0.564968 0.546107 11.00000 0.02617 0.03292 = 0.02537 -0.00840 0.00893 -0.00541 BR1 3 0.539338 0.438968 0.839185 11.00000 0.02787 0.03912 = 0.02741 -0.00590 0.00522 -0.00911 BR2 3 1.074402 0.423799 0.894724 11.00000 0.03071 0.03660 = 0.03348 -0.00337 0.01209 0.00406 BR21 3 0.675885 0.619957 0.663009 11.00000 0.02906 0.03658 = 0.02464 -0.00413 0.00382 -0.00662 BR22 3 0.145724 0.643492 0.583940 11.00000 0.03065 0.03526 = 0.02975 -0.00565 0.01200 0.00160 N1 5 0.961446 0.608972 1.003851 11.00000 0.02183 0.02985 = 0.01768 0.00375 0.00584 0.00175 N2 5 0.852084 0.516644 1.187347 11.00000 0.01843 0.02668 = 0.02042 -0.00256 0.00529 0.00111 N21 5 0.265513 0.450966 0.477635 11.00000 0.02271 0.02906 = 0.01851 0.00018 0.00441 -0.00488 N22 5 0.387058 0.544309 0.301457 11.00000 0.02125 0.02440 = 0.02239 0.00053 0.00436 -0.00114 C1 1 0.985646 0.630493 1.136218 11.00000 0.02089 0.02567 = 0.02159 -0.00001 0.00394 0.00116 C2 1 1.074145 0.695725 1.186097 11.00000 0.03075 0.02574 = 0.02500 -0.00362 0.00572 -0.00085 AFIX 43 H2 2 1.087821 0.710191 1.279426 11.00000 -1.20000 AFIX 0 C3 1 1.143010 0.740082 1.099943 11.00000 0.02449 0.02929 = 0.03125 0.00108 0.00403 -0.00279 AFIX 43 H3 2 1.203099 0.785373 1.132152 11.00000 -1.20000 AFIX 0 C4 1 1.120969 0.715962 0.965693 11.00000 0.02228 0.02663 = 0.03106 0.00401 0.00910 -0.00135 AFIX 43 H4 2 1.169369 0.744108 0.904686 11.00000 -1.20000 AFIX 0 C5 1 1.028431 0.650774 0.919257 11.00000 0.02201 0.03285 = 0.02434 0.00291 0.00406 -0.00265 AFIX 43 H5 2 1.012291 0.635527 0.826067 11.00000 -1.20000 AFIX 0 C6 1 0.917402 0.581177 1.228049 11.00000 0.02670 0.02928 = 0.01644 0.00155 0.00651 0.00402 AFIX 43 H6 2 0.922139 0.597716 1.319000 11.00000 -1.20000 AFIX 0 C7 1 0.790279 0.467651 1.277544 11.00000 0.01847 0.02993 = 0.01617 0.00094 0.00368 0.00226 C8 1 0.797878 0.486088 1.415614 11.00000 0.03223 0.02841 = 0.02167 -0.00449 0.01099 -0.00143 AFIX 43 H8 2 0.843801 0.533204 1.453666 11.00000 -1.20000 AFIX 0 C9 1 0.736568 0.433715 1.495180 11.00000 0.03234 0.03003 = 0.01599 0.00210 0.01091 0.00457 AFIX 43 H9 2 0.740172 0.446156 1.587932 11.00000 -1.20000 AFIX 0 C10 1 0.671175 0.364766 1.443850 11.00000 0.02039 0.02986 = 0.02216 0.00438 0.00703 0.00396 C11 1 0.666049 0.346832 1.305984 11.00000 0.03378 0.01997 = 0.02761 -0.00053 0.00939 -0.00369 AFIX 43 H11 2 0.622870 0.299117 1.268872 11.00000 -1.20000 AFIX 0 C12 1 0.724075 0.398830 1.223983 11.00000 0.02740 0.03178 = 0.02367 -0.00788 0.00548 -0.00221 AFIX 43 H12 2 0.718004 0.386813 1.130628 11.00000 -1.20000 AFIX 0 C13 1 0.605064 0.308454 1.531637 11.00000 0.03518 0.02860 = 0.03350 0.00668 0.00913 0.00155 AFIX 137 H13A 2 0.611206 0.330938 1.622057 11.00000 -1.50000 H13B 2 0.673338 0.262104 1.543131 11.00000 -1.50000 H13C 2 0.487901 0.295908 1.486486 11.00000 -1.50000 AFIX 0 C21 1 0.257884 0.428506 0.347152 11.00000 0.02109 0.01787 = 0.02106 -0.00261 0.00389 0.00110 C22 1 0.181595 0.360729 0.296474 11.00000 0.03463 0.02798 = 0.02600 -0.00571 0.01048 -0.00559 AFIX 43 H22 2 0.178614 0.345099 0.205342 11.00000 -1.20000 AFIX 0 C23 1 0.109289 0.315588 0.379597 11.00000 0.02850 0.02651 = 0.03744 -0.00053 0.00408 -0.00477 AFIX 43 H23 2 0.055910 0.268977 0.346283 11.00000 -1.20000 AFIX 0 C24 1 0.116859 0.340207 0.512638 11.00000 0.02110 0.03625 = 0.03587 0.01167 0.00570 0.00071 AFIX 43 H24 2 0.069155 0.310370 0.571943 11.00000 -1.20000 AFIX 0 C25 1 0.195067 0.409026 0.557996 11.00000 0.02109 0.03888 = 0.01913 0.00565 0.00504 -0.00136 AFIX 43 H25 2 0.198168 0.426374 0.648185 11.00000 -1.20000 AFIX 0 C26 1 0.328724 0.478287 0.261012 11.00000 0.02250 0.02401 = 0.02193 -0.00403 0.00482 -0.00005 AFIX 43 H26 2 0.331955 0.461405 0.171867 11.00000 -1.20000 AFIX 0 C27 1 0.451175 0.593400 0.215015 11.00000 0.01872 0.02196 = 0.02183 -0.00381 0.00335 0.00368 C28 1 0.434045 0.582077 0.075901 11.00000 0.02294 0.03275 = 0.02519 -0.00889 0.00826 -0.00817 AFIX 43 H28 2 0.377319 0.538157 0.032329 11.00000 -1.20000 AFIX 0 C29 1 0.499136 0.634428 -0.001021 11.00000 0.02655 0.02957 = 0.02351 0.00170 0.00765 0.00544 AFIX 43 H29 2 0.487055 0.625096 -0.096206 11.00000 -1.20000 AFIX 0 C30 1 0.581773 0.700340 0.058194 11.00000 0.02142 0.02335 = 0.02640 0.00127 0.00795 0.00106 C31 1 0.597096 0.710418 0.199944 11.00000 0.02621 0.02469 = 0.02798 -0.00159 0.00812 -0.00060 AFIX 43 H31 2 0.654022 0.754040 0.244579 11.00000 -1.20000 AFIX 0 C32 1 0.532277 0.659130 0.275263 11.00000 0.03769 0.02665 = 0.02367 -0.00320 0.00704 0.00362 AFIX 43 H32 2 0.542754 0.668501 0.370225 11.00000 -1.20000 AFIX 0 C33 1 0.647516 0.757284 -0.024351 11.00000 0.03365 0.03260 = 0.02833 0.00506 0.00835 -0.00150 AFIX 137 H33A 2 0.766070 0.767642 0.019809 11.00000 -1.50000 H33B 2 0.582597 0.804425 -0.030052 11.00000 -1.50000 H33C 2 0.637218 0.737322 -0.117222 11.00000 -1.50000 HKLF 4 REM TSBB-298 (L1022) REM R1 = 0.0318 for 7309 Fo > 4sig(Fo) and 0.0383 for all 8003 data REM 328 parameters refined using 1 restraints END WGHT 0.0388 2.3420 REM Highest difference peak 2.359, deepest hole -2.002, 1-sigma level 0.249 Q1 1 0.3687 0.4976 -0.0366 11.00000 0.05 2.36 Q2 1 0.9521 0.5647 1.5731 11.00000 0.05 2.29 Q3 1 0.2514 0.5688 0.3344 11.00000 0.05 0.85 Q4 1 0.3990 0.4296 0.5448 11.00000 0.05 0.85 Q5 1 -0.0320 0.4252 0.5855 11.00000 0.05 0.79 Q6 1 -0.1475 0.2932 0.4773 11.00000 0.05 0.74 Q7 1 0.1394 0.4854 0.5882 11.00000 0.05 0.70 Q8 1 0.3827 0.6328 -0.0228 11.00000 0.05 0.67 Q9 1 0.6266 0.8300 0.1771 11.00000 0.05 0.67 Q10 1 -0.0551 0.3074 0.4550 11.00000 0.05 0.66 ; data_8 _database_code_depnum_ccdc_archive 'CCDC 892212' #TrackingRef '8.cif' # L1018 _audit_creation_method SHELXL-97 _audit_creation_date 10-09-09 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C13 H12 Hg I2 N2' _chemical_formula_sum 'C13 H12 Hg I2 N2' _chemical_formula_weight 650.56 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 26 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 24 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Hg Hg 2 -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; I I 4 -0.4742 1.8119 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 4 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7545(1) _cell_length_b 9.9076(2) _cell_length_c 10.9202(2) _cell_angle_alpha 76.8887(10) _cell_angle_beta 83.9298(10) _cell_angle_gamma 76.6521(10) _cell_volume 793.78(2) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 21886 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 13.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.033 _exptl_absorpt_correction_T_max 0.072 _exptl_special_details ; Solvent used: MeCN Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.457(1) Frames collected: 737 Seconds exposure per frame: 16 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 35.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 17262 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.990 _reflns_number_total 3607 _reflns_number_gt 3330 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF94 (Beurskens et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2006)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+1.7003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 3607 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.231 _refine_diff_density_min -4.185 _refine_diff_density_rms 0.366 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 C1 C 0.8288(8) -0.0846(7) 1.0517(6) 0.0313(12) Uani 1 1 d . . . C2 C 0.8474(9) -0.0681(7) 1.1728(6) 0.0337(13) Uani 1 1 d . . . H2 H 0.7847 0.0149 1.2006 0.040 Uiso 1 1 calc R . . C3 C 0.9584(10) -0.1742(8) 1.2522(7) 0.0418(16) Uani 1 1 d . . . H3 H 0.9737 -0.1648 1.3348 0.050 Uiso 1 1 calc R . . C4 C 1.0457(10) -0.2932(8) 1.2091(7) 0.0425(16) Uani 1 1 d . . . H4 H 1.1214 -0.3677 1.2621 0.051 Uiso 1 1 calc R . . C5 C 1.0229(9) -0.3038(8) 1.0883(7) 0.0406(15) Uani 1 1 d . . . H5 H 1.0841 -0.3864 1.0592 0.049 Uiso 1 1 calc R . . C6 C 0.7148(8) 0.0288(7) 0.9657(6) 0.0308(12) Uani 1 1 d . . . H6 H 0.6544 0.1124 0.9935 0.037 Uiso 1 1 calc R . . C7 C 0.5890(7) 0.1248(6) 0.7698(6) 0.0276(11) Uani 1 1 d . . . C8 C 0.5019(8) 0.2578(7) 0.7925(6) 0.0341(13) Uani 1 1 d . . . H8 H 0.5125 0.2806 0.8709 0.041 Uiso 1 1 calc R . . C9 C 0.4022(9) 0.3552(7) 0.7040(7) 0.0366(14) Uani 1 1 d . . . H9 H 0.3462 0.4452 0.7216 0.044 Uiso 1 1 calc R . . C10 C 0.3799(8) 0.3262(7) 0.5878(6) 0.0327(13) Uani 1 1 d . . . C11 C 0.4676(9) 0.1962(7) 0.5626(6) 0.0376(14) Uani 1 1 d . . . H11 H 0.4567 0.1747 0.4836 0.045 Uiso 1 1 calc R . . C12 C 0.5719(8) 0.0963(7) 0.6522(6) 0.0331(13) Uani 1 1 d . . . H12 H 0.6321 0.0078 0.6331 0.040 Uiso 1 1 calc R . . C13 C 0.2668(10) 0.4328(7) 0.4922(7) 0.0418(15) Uani 1 1 d . . . H13A H 0.3363 0.4499 0.4121 0.050 Uiso 1 1 calc R . . H13B H 0.2262 0.5218 0.5218 0.050 Uiso 1 1 calc R . . H13C H 0.1639 0.3965 0.4803 0.050 Uiso 1 1 calc R . . Hg1 Hg 0.83718(3) -0.21352(2) 0.80704(2) 0.03561(11) Uani 1 1 d . . . I1 I 0.56962(6) -0.34929(5) 0.85700(4) 0.04147(14) Uani 1 1 d . . . I2 I 1.09800(6) -0.20679(5) 0.63161(4) 0.04291(14) Uani 1 1 d . . . N1 N 0.9163(7) -0.2004(6) 1.0104(5) 0.0338(11) Uani 1 1 d . . . N2 N 0.6962(7) 0.0166(5) 0.8554(5) 0.0287(10) 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 C1 0.027(3) 0.033(3) 0.035(3) -0.007(2) 0.001(2) -0.010(2) C2 0.034(3) 0.037(3) 0.033(3) -0.010(3) 0.001(2) -0.013(3) C3 0.042(4) 0.054(4) 0.033(3) -0.007(3) -0.001(3) -0.021(3) C4 0.039(3) 0.041(4) 0.044(4) 0.004(3) -0.011(3) -0.010(3) C5 0.038(3) 0.037(3) 0.044(4) -0.006(3) -0.007(3) -0.002(3) C6 0.028(3) 0.029(3) 0.035(3) -0.010(2) 0.002(2) -0.005(2) C7 0.023(3) 0.028(3) 0.030(3) -0.006(2) -0.001(2) -0.003(2) C8 0.034(3) 0.032(3) 0.037(3) -0.011(3) -0.003(2) -0.002(2) C9 0.039(3) 0.032(3) 0.041(4) -0.014(3) -0.004(3) -0.004(3) C10 0.030(3) 0.036(3) 0.030(3) -0.006(2) -0.002(2) -0.003(2) C11 0.042(4) 0.039(3) 0.030(3) -0.012(3) 0.000(3) -0.002(3) C12 0.037(3) 0.030(3) 0.032(3) -0.012(2) -0.001(2) 0.000(2) C13 0.045(4) 0.035(3) 0.040(4) -0.004(3) -0.011(3) 0.004(3) Hg1 0.03760(16) 0.03217(15) 0.03529(17) -0.00931(11) -0.00194(10) -0.00172(10) I1 0.0460(3) 0.0394(3) 0.0433(3) -0.01681(19) 0.00511(19) -0.01307(19) I2 0.0400(2) 0.0484(3) 0.0422(3) -0.0203(2) 0.00475(19) -0.0058(2) N1 0.037(3) 0.031(3) 0.032(3) -0.004(2) -0.007(2) -0.005(2) N2 0.032(2) 0.029(2) 0.026(2) -0.0056(19) -0.0004(19) -0.007(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 C1 N1 1.338(8) . ? C1 C2 1.395(9) . ? C1 C6 1.471(9) . ? C2 C3 1.387(10) . ? C2 H2 0.9500 . ? C3 C4 1.373(12) . ? C3 H3 0.9500 . ? C4 C5 1.379(11) . ? C4 H4 0.9500 . ? C5 N1 1.350(9) . ? C5 H5 0.9500 . ? C6 N2 1.264(8) . ? C6 H6 0.9500 . ? C7 C8 1.399(9) . ? C7 C12 1.402(9) . ? C7 N2 1.418(7) . ? C8 C9 1.361(9) . ? C8 H8 0.9500 . ? C9 C10 1.399(9) . ? C9 H9 0.9500 . ? C10 C11 1.384(9) . ? C10 C13 1.496(9) . ? C11 C12 1.396(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Hg1 N1 2.404(5) . ? Hg1 N2 2.438(5) . ? Hg1 I2 2.6363(5) . ? Hg1 I1 2.6698(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 N1 C1 C2 121.3(6) . . ? N1 C1 C6 118.9(6) . . ? C2 C1 C6 119.7(6) . . ? C3 C2 C1 119.3(6) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 118.7(7) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.6(7) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.9(7) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? N2 C6 C1 120.9(6) . . ? N2 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 117.6(6) . . ? C8 C7 N2 125.4(6) . . ? C12 C7 N2 117.0(5) . . ? C9 C8 C7 121.1(6) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 121.8(6) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 118.0(6) . . ? C11 C10 C13 120.6(6) . . ? C9 C10 C13 121.4(6) . . ? C10 C11 C12 120.6(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.9(6) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 Hg1 N2 69.73(18) . . ? N1 Hg1 I2 114.29(14) . . ? N2 Hg1 I2 114.55(12) . . ? N1 Hg1 I1 104.46(13) . . ? N2 Hg1 I1 101.71(12) . . ? I2 Hg1 I1 133.685(17) . . ? C1 N1 C5 119.1(6) . . ? C1 N1 Hg1 114.6(4) . . ? C5 N1 Hg1 125.9(5) . . ? C6 N2 C7 122.3(5) . . ? C6 N2 Hg1 115.1(4) . . ? C7 N2 Hg1 122.5(4) . . ? 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 N1 C1 C2 C3 -0.3(9) . . . . ? C6 C1 C2 C3 -178.5(6) . . . . ? C1 C2 C3 C4 -0.5(10) . . . . ? C2 C3 C4 C5 0.7(10) . . . . ? C3 C4 C5 N1 -0.2(11) . . . . ? N1 C1 C6 N2 1.5(9) . . . . ? C2 C1 C6 N2 179.8(6) . . . . ? C12 C7 C8 C9 0.9(10) . . . . ? N2 C7 C8 C9 179.7(6) . . . . ? C7 C8 C9 C10 1.0(10) . . . . ? C8 C9 C10 C11 -2.1(10) . . . . ? C8 C9 C10 C13 178.6(7) . . . . ? C9 C10 C11 C12 1.3(10) . . . . ? C13 C10 C11 C12 -179.4(6) . . . . ? C10 C11 C12 C7 0.6(10) . . . . ? C8 C7 C12 C11 -1.7(9) . . . . ? N2 C7 C12 C11 179.4(6) . . . . ? C2 C1 N1 C5 0.8(9) . . . . ? C6 C1 N1 C5 179.1(6) . . . . ? C2 C1 N1 Hg1 173.8(5) . . . . ? C6 C1 N1 Hg1 -7.9(7) . . . . ? C4 C5 N1 C1 -0.6(10) . . . . ? C4 C5 N1 Hg1 -172.7(5) . . . . ? N2 Hg1 N1 C1 7.5(4) . . . . ? I2 Hg1 N1 C1 116.2(4) . . . . ? I1 Hg1 N1 C1 -89.8(4) . . . . ? N2 Hg1 N1 C5 180.0(6) . . . . ? I2 Hg1 N1 C5 -71.4(6) . . . . ? I1 Hg1 N1 C5 82.6(6) . . . . ? C1 C6 N2 C7 -179.2(5) . . . . ? C1 C6 N2 Hg1 5.7(7) . . . . ? C8 C7 N2 C6 4.1(9) . . . . ? C12 C7 N2 C6 -177.1(6) . . . . ? C8 C7 N2 Hg1 178.8(5) . . . . ? C12 C7 N2 Hg1 -2.4(7) . . . . ? N1 Hg1 N2 C6 -6.9(4) . . . . ? I2 Hg1 N2 C6 -115.2(4) . . . . ? I1 Hg1 N2 C6 94.3(4) . . . . ? N1 Hg1 N2 C7 178.0(5) . . . . ? I2 Hg1 N2 C7 69.8(4) . . . . ? I1 Hg1 N2 C7 -80.7(4) . . . . ? _iucr_refine_instructions_details ; TITL TSBB-294 (L1018) CELL 0.71073 7.7545 9.9076 10.9202 76.8887 83.9298 76.6521 ZERR 2 0.0001 0.0002 0.0002 0.0010 0.0010 0.0010 LATT 1 SFAC C H HG I N UNIT 26 24 2 4 4 MERG 2 TEMP -113 L.S. 4 BOND $H CONF ACTA FMAP 2 PLAN 40 WGHT 0.066200 1.700300 FVAR 1.26034 C1 1 0.828754 -0.084600 1.051675 11.00000 0.02679 0.03325 = 0.03494 -0.00705 0.00142 -0.01036 C2 1 0.847411 -0.068135 1.172776 11.00000 0.03368 0.03738 = 0.03338 -0.00983 0.00063 -0.01301 AFIX 43 H2 2 0.784746 0.014893 1.200575 11.00000 -1.20000 AFIX 0 C3 1 0.958396 -0.174225 1.252218 11.00000 0.04233 0.05372 = 0.03349 -0.00688 -0.00149 -0.02125 AFIX 43 H3 2 0.973664 -0.164759 1.334817 11.00000 -1.20000 AFIX 0 C4 1 1.045743 -0.293186 1.209086 11.00000 0.03862 0.04086 = 0.04410 0.00446 -0.01128 -0.00969 AFIX 43 H4 2 1.121417 -0.367708 1.262099 11.00000 -1.20000 AFIX 0 C5 1 1.022944 -0.303818 1.088350 11.00000 0.03829 0.03662 = 0.04433 -0.00644 -0.00716 -0.00247 AFIX 43 H5 2 1.084115 -0.386383 1.059202 11.00000 -1.20000 AFIX 0 C6 1 0.714822 0.028812 0.965700 11.00000 0.02796 0.02931 = 0.03540 -0.00965 0.00184 -0.00527 AFIX 43 H6 2 0.654367 0.112418 0.993472 11.00000 -1.20000 AFIX 0 C7 1 0.589011 0.124770 0.769791 11.00000 0.02331 0.02776 = 0.03032 -0.00584 -0.00142 -0.00294 C8 1 0.501886 0.257794 0.792474 11.00000 0.03362 0.03168 = 0.03661 -0.01124 -0.00253 -0.00201 AFIX 43 H8 2 0.512457 0.280553 0.870923 11.00000 -1.20000 AFIX 0 C9 1 0.402209 0.355161 0.703994 11.00000 0.03854 0.03240 = 0.04075 -0.01383 -0.00386 -0.00443 AFIX 43 H9 2 0.346247 0.445182 0.721640 11.00000 -1.20000 AFIX 0 C10 1 0.379947 0.326243 0.587759 11.00000 0.02952 0.03559 = 0.03045 -0.00554 -0.00172 -0.00323 C11 1 0.467621 0.196184 0.562554 11.00000 0.04214 0.03865 = 0.03035 -0.01167 0.00031 -0.00188 AFIX 43 H11 2 0.456749 0.174696 0.483613 11.00000 -1.20000 AFIX 0 C12 1 0.571917 0.096279 0.652150 11.00000 0.03660 0.02995 = 0.03166 -0.01205 -0.00120 0.00002 AFIX 43 H12 2 0.632108 0.007804 0.633137 11.00000 -1.20000 AFIX 0 C13 1 0.266830 0.432813 0.492237 11.00000 0.04457 0.03463 = 0.04012 -0.00420 -0.01138 0.00407 AFIX 137 H13A 2 0.336297 0.449947 0.412073 11.00000 -1.20000 H13B 2 0.226241 0.521826 0.521784 11.00000 -1.20000 H13C 2 0.163859 0.396467 0.480286 11.00000 -1.20000 AFIX 0 HG1 3 0.837181 -0.213520 0.807040 11.00000 0.03760 0.03217 = 0.03529 -0.00931 -0.00194 -0.00172 I1 4 0.569620 -0.349287 0.856996 11.00000 0.04596 0.03937 = 0.04335 -0.01681 0.00511 -0.01307 I2 4 1.098004 -0.206788 0.631609 11.00000 0.04002 0.04837 = 0.04223 -0.02032 0.00475 -0.00576 N1 5 0.916265 -0.200352 1.010384 11.00000 0.03686 0.03119 = 0.03239 -0.00431 -0.00682 -0.00521 N2 5 0.696204 0.016612 0.855369 11.00000 0.03158 0.02885 = 0.02582 -0.00556 -0.00043 -0.00737 HKLF 4 REM TSBB-294 (L1018) REM R1 = 0.0397 for 3330 Fo > 4sig(Fo) and 0.0443 for all 3607 data REM 164 parameters refined using 0 restraints END WGHT 0.0662 1.7003 REM Highest difference peak 1.231, deepest hole -4.185, 1-sigma level 0.366 Q1 1 0.7740 -0.1599 0.7217 11.00000 0.05 1.23 Q2 1 0.9953 -0.0767 1.4720 11.00000 0.05 0.85 Q3 1 0.4222 0.2240 1.0179 11.00000 0.05 0.83 Q4 1 1.1182 -0.2342 0.7074 11.00000 0.05 0.81 Q5 1 0.5327 0.4759 0.8151 11.00000 0.05 0.80 Q6 1 1.1044 -0.2429 0.5391 11.00000 0.05 0.80 Q7 1 0.5909 -0.3689 0.9376 11.00000 0.05 0.78 Q8 1 0.9036 -0.1658 0.8170 11.00000 0.05 0.75 Q9 1 0.8314 -0.1803 0.8963 11.00000 0.05 0.74 Q10 1 0.9126 -0.0443 1.4118 11.00000 0.05 0.74 Q11 1 0.9360 -0.1217 1.3359 11.00000 0.05 0.74 Q12 1 0.6298 0.0607 0.4136 11.00000 0.05 0.72 Q13 1 0.8450 -0.0211 0.4743 11.00000 0.05 0.72 Q14 1 0.5846 -0.4720 0.9370 11.00000 0.05 0.72 Q15 1 0.9954 -0.1371 1.3171 11.00000 0.05 0.70 Q16 1 0.5550 -0.4371 0.7996 11.00000 0.05 0.70 Q17 1 1.1320 -0.0969 0.5386 11.00000 0.05 0.69 Q18 1 0.5247 -0.3210 0.9553 11.00000 0.05 0.68 Q19 1 0.5505 0.4118 0.7618 11.00000 0.05 0.68 Q20 1 0.8826 -0.1408 1.4378 11.00000 0.05 0.68 ; data_9 _database_code_depnum_ccdc_archive 'CCDC 892213' #TrackingRef '9.cif' # L1008 _vrf_PLAT241_9 ; PROBLEM: Check High Ueq as Compared to Neighbors for O5 RESPONSE: The nitrate-O5 atom is less strongly bound to the Hg atom and suffers from marginally greater thermal motion compared to its neighbours. No evidence for multiple sites was found. ; _audit_creation_method SHELXL-97 _audit_creation_date 10-03-09 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C13 H12 Hg N4 O6' _chemical_formula_sum 'C13 H12 Hg N4 O6' _chemical_formula_weight 520.76 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 52 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 48 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Hg Hg 4 -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 16 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 24 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 10.6101(2) _cell_length_b 14.2146(2) _cell_length_c 10.3608(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.2161(11) _cell_angle_gamma 90.00 _cell_volume 1550.22(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 93796 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 9.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.145 _exptl_absorpt_correction_T_max 0.388 _exptl_special_details ; Solvent used: MeCN Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.963(1) Frames collected: 741 Seconds exposure per frame: 30 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 30.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 42486 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.01 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 4503 _reflns_number_gt 3755 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF94 (Beurskens et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2006)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+4.0441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00101(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4501 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.037 _refine_diff_density_min -1.600 _refine_diff_density_rms 0.146 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 0.226343(14) 0.242984(10) 0.163102(15) 0.02756(7) Uani 1 1 d . . . O1 O 0.0250(3) 0.2473(2) 0.0032(3) 0.0353(7) Uani 1 1 d . . . O2 O 0.1904(3) 0.2920(3) -0.0825(3) 0.0400(7) Uani 1 1 d . . . O3 O 0.0060(3) 0.2864(2) -0.1998(3) 0.0376(7) Uani 1 1 d . . . O4 O 0.1635(3) 0.3788(2) 0.2275(3) 0.0383(7) Uani 1 1 d . . . O5 O 0.3646(4) 0.3860(3) 0.2889(5) 0.0699(13) Uani 1 1 d . . . O6 O 0.2423(5) 0.4994(3) 0.3356(4) 0.0620(11) Uani 1 1 d . . . N1 N 0.2162(3) 0.0872(2) 0.1535(3) 0.0292(7) Uani 1 1 d . . . N2 N 0.4253(3) 0.1898(2) 0.1150(3) 0.0303(7) Uani 1 1 d . . . N3 N 0.0716(3) 0.2759(2) -0.0943(3) 0.0291(7) Uani 1 1 d . . . N4 N 0.2601(4) 0.4230(3) 0.2860(4) 0.0394(9) Uani 1 1 d . . . C1 C 0.3252(4) 0.0413(3) 0.1396(4) 0.0277(8) Uani 1 1 d . . . C2 C 0.3298(4) -0.0557(3) 0.1328(4) 0.0339(9) Uani 1 1 d . . . H2 H 0.4081 -0.0869 0.1273 0.041 Uiso 1 1 calc R . . C3 C 0.2191(4) -0.1068(3) 0.1341(4) 0.0350(9) Uani 1 1 d . . . H3 H 0.2198 -0.1734 0.1264 0.042 Uiso 1 1 calc R . . C4 C 0.1082(5) -0.0601(3) 0.1468(5) 0.0379(10) Uani 1 1 d . . . H4 H 0.0313 -0.0941 0.1485 0.045 Uiso 1 1 calc R . . C5 C 0.1094(4) 0.0375(3) 0.1570(5) 0.0357(9) Uani 1 1 d . . . H5 H 0.0327 0.0697 0.1668 0.043 Uiso 1 1 calc R . . C6 C 0.4359(4) 0.1005(3) 0.1231(4) 0.0304(8) Uani 1 1 d . . . H6 H 0.5161 0.0720 0.1184 0.036 Uiso 1 1 calc R . . C7 C 0.5291(4) 0.2485(3) 0.0880(4) 0.0273(8) Uani 1 1 d . . . C8 C 0.6554(4) 0.2270(3) 0.1279(4) 0.0299(8) Uani 1 1 d . . . H8 H 0.6770 0.1713 0.1764 0.036 Uiso 1 1 calc R . . C9 C 0.7494(4) 0.2867(3) 0.0972(4) 0.0319(9) Uani 1 1 d . . . H9 H 0.8356 0.2714 0.1256 0.038 Uiso 1 1 calc R . . C10 C 0.7221(4) 0.3688(3) 0.0256(4) 0.0325(9) Uani 1 1 d . . . C11 C 0.5946(4) 0.3887(3) -0.0142(5) 0.0384(10) Uani 1 1 d . . . H11 H 0.5732 0.4439 -0.0638 0.046 Uiso 1 1 calc R . . C12 C 0.4978(4) 0.3303(3) 0.0162(5) 0.0366(10) Uani 1 1 d . . . H12 H 0.4115 0.3457 -0.0114 0.044 Uiso 1 1 calc R . . C13 C 0.8257(5) 0.4336(3) -0.0063(5) 0.0416(11) Uani 1 1 d . . . H131 H 0.8422 0.4226 -0.0960 0.062 Uiso 1 1 calc R . . H132 H 0.9032 0.4216 0.0534 0.062 Uiso 1 1 calc R . . H133 H 0.7991 0.4991 0.0031 0.062 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 0.02707(10) 0.02608(10) 0.02995(10) -0.00168(6) 0.00523(6) 0.00048(5) O1 0.0326(16) 0.0445(19) 0.0304(16) 0.0027(12) 0.0105(13) -0.0011(12) O2 0.0318(16) 0.056(2) 0.0324(16) 0.0068(15) 0.0039(13) -0.0085(15) O3 0.0364(17) 0.0454(18) 0.0291(15) 0.0019(14) -0.0030(13) -0.0017(14) O4 0.0401(18) 0.0303(15) 0.0441(18) -0.0095(13) 0.0036(14) -0.0020(13) O5 0.038(2) 0.080(3) 0.090(3) -0.026(3) 0.003(2) -0.015(2) O6 0.104(3) 0.0343(19) 0.046(2) -0.0146(16) 0.006(2) -0.015(2) N1 0.0296(18) 0.0293(17) 0.0297(18) -0.0008(14) 0.0077(14) -0.0024(13) N2 0.0283(17) 0.0302(17) 0.0331(18) 0.0022(14) 0.0060(14) -0.0037(13) N3 0.0311(18) 0.0273(16) 0.0291(17) -0.0017(14) 0.0039(14) -0.0015(14) N4 0.048(2) 0.036(2) 0.034(2) -0.0019(17) 0.0068(18) -0.0139(17) C1 0.031(2) 0.0253(18) 0.0267(19) -0.0002(15) 0.0034(16) -0.0011(15) C2 0.041(2) 0.031(2) 0.031(2) 0.0002(17) 0.0076(18) 0.0035(17) C3 0.046(3) 0.0241(19) 0.035(2) 0.0004(16) 0.006(2) -0.0027(17) C4 0.043(3) 0.028(2) 0.044(3) -0.0045(19) 0.011(2) -0.0110(18) C5 0.032(2) 0.034(2) 0.042(2) -0.0041(19) 0.0095(19) -0.0039(17) C6 0.030(2) 0.031(2) 0.031(2) -0.0004(16) 0.0033(17) 0.0020(16) C7 0.0275(19) 0.0265(19) 0.029(2) -0.0035(15) 0.0094(16) -0.0013(14) C8 0.028(2) 0.0278(18) 0.034(2) 0.0035(17) 0.0047(17) 0.0043(15) C9 0.029(2) 0.032(2) 0.035(2) -0.0004(18) 0.0072(17) 0.0011(17) C10 0.033(2) 0.032(2) 0.034(2) -0.0009(17) 0.0081(18) 0.0004(16) C11 0.036(2) 0.033(2) 0.047(3) 0.010(2) 0.006(2) 0.0006(17) C12 0.029(2) 0.032(2) 0.048(3) 0.0098(19) 0.0034(19) 0.0044(16) C13 0.038(2) 0.037(2) 0.052(3) 0.006(2) 0.011(2) -0.0038(19) _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 O4 2.174(3) . ? Hg1 N1 2.218(4) . ? Hg1 N2 2.353(3) . ? Hg1 O1 2.534(3) . ? Hg1 O2 2.620(3) . ? Hg1 O5 2.739(4) . ? Hg1 O2 2.755(3) 4_566 ? Hg1 O3 2.913(3) 4_566 ? O1 N3 1.248(5) . ? O2 N3 1.272(5) . ? O3 N3 1.230(5) . ? O4 N4 1.287(5) . ? O5 N4 1.224(6) . ? O6 N4 1.227(5) . ? N1 C5 1.340(5) . ? N1 C1 1.351(5) . ? N2 C6 1.276(5) . ? N2 C7 1.438(5) . ? C1 C2 1.381(6) . ? C1 C6 1.473(6) . ? C2 C3 1.383(6) . ? C2 H2 0.9500 . ? C3 C4 1.371(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.386(6) . ? C7 C12 1.398(6) . ? C8 C9 1.377(6) . ? C8 H8 0.9500 . ? C9 C10 1.393(6) . ? C9 H9 0.9500 . ? C10 C11 1.394(6) . ? C10 C13 1.502(6) . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H131 0.9800 . ? C13 H132 0.9800 . ? C13 H133 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Hg1 N1 152.22(12) . . ? O4 Hg1 N2 131.90(12) . . ? N1 Hg1 N2 73.13(12) . . ? O4 Hg1 O1 85.03(11) . . ? N1 Hg1 O1 87.86(11) . . ? N2 Hg1 O1 125.05(11) . . ? O4 Hg1 O2 92.82(12) . . ? N1 Hg1 O2 102.81(12) . . ? N2 Hg1 O2 84.53(11) . . ? O1 Hg1 O2 49.52(10) . . ? O4 Hg1 O5 50.35(12) . . ? N1 Hg1 O5 141.44(14) . . ? N2 Hg1 O5 84.14(12) . . ? O1 Hg1 O5 130.57(13) . . ? O2 Hg1 O5 105.59(13) . . ? O4 Hg1 O2 77.41(12) . 4_566 ? N1 Hg1 O2 81.42(11) . 4_566 ? N2 Hg1 O2 112.33(11) . 4_566 ? O1 Hg1 O2 115.03(10) . 4_566 ? O2 Hg1 O2 163.04(13) . 4_566 ? O5 Hg1 O2 78.99(13) . 4_566 ? O4 Hg1 O3 71.46(11) . 4_566 ? N1 Hg1 O3 80.87(11) . 4_566 ? N2 Hg1 O3 148.52(11) . 4_566 ? O1 Hg1 O3 70.12(9) . 4_566 ? O2 Hg1 O3 118.94(9) . 4_566 ? O5 Hg1 O3 106.81(11) . 4_566 ? O2 Hg1 O3 44.93(9) 4_566 4_566 ? N3 O1 Hg1 98.6(2) . . ? N3 O2 Hg1 93.8(2) . . ? N3 O2 Hg1 97.5(2) . 4_565 ? Hg1 O2 Hg1 149.38(16) . 4_565 ? N3 O3 Hg1 91.0(2) . 4_565 ? N4 O4 Hg1 108.7(3) . . ? N4 O5 Hg1 83.0(3) . . ? C5 N1 C1 119.1(4) . . ? C5 N1 Hg1 124.2(3) . . ? C1 N1 Hg1 116.7(3) . . ? C6 N2 C7 121.8(4) . . ? C6 N2 Hg1 112.3(3) . . ? C7 N2 Hg1 125.8(3) . . ? O3 N3 O1 121.5(4) . . ? O3 N3 O2 120.4(3) . . ? O1 N3 O2 118.1(4) . . ? O5 N4 O6 123.9(4) . . ? O5 N4 O4 117.8(4) . . ? O6 N4 O4 118.3(4) . . ? N1 C1 C2 121.6(4) . . ? N1 C1 C6 116.2(3) . . ? C2 C1 C6 122.1(4) . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.6(4) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N2 C6 C1 120.7(4) . . ? N2 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C8 C7 C12 119.9(4) . . ? C8 C7 N2 123.3(4) . . ? C12 C7 N2 116.7(4) . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 122.1(4) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C9 C10 C11 117.2(4) . . ? C9 C10 C13 121.5(4) . . ? C11 C10 C13 121.3(4) . . ? C12 C11 C10 122.0(4) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C7 119.0(4) . . ? C11 C12 H12 120.5 . . ? C7 C12 H12 120.5 . . ? C10 C13 H131 109.5 . . ? C10 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? C10 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? 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 O4 Hg1 O1 N3 98.2(2) . . . . ? N1 Hg1 O1 N3 -108.7(2) . . . . ? N2 Hg1 O1 N3 -41.1(3) . . . . ? O2 Hg1 O1 N3 0.2(2) . . . . ? O5 Hg1 O1 N3 74.8(3) . . . . ? O2 Hg1 O1 N3 171.8(2) 4_566 . . . ? O3 Hg1 O1 N3 170.3(2) 4_566 . . . ? O4 Hg1 O2 N3 -81.2(3) . . . . ? N1 Hg1 O2 N3 75.7(3) . . . . ? N2 Hg1 O2 N3 147.0(3) . . . . ? O1 Hg1 O2 N3 -0.2(2) . . . . ? O5 Hg1 O2 N3 -130.7(2) . . . . ? O2 Hg1 O2 N3 -27.1(3) 4_566 . . . ? O3 Hg1 O2 N3 -10.9(3) 4_566 . . . ? O4 Hg1 O2 Hg1 167.1(3) . . . 4_565 ? N1 Hg1 O2 Hg1 -36.0(3) . . . 4_565 ? N2 Hg1 O2 Hg1 35.3(3) . . . 4_565 ? O1 Hg1 O2 Hg1 -111.9(3) . . . 4_565 ? O5 Hg1 O2 Hg1 117.6(3) . . . 4_565 ? O2 Hg1 O2 Hg1 -138.77(18) 4_566 . . 4_565 ? O3 Hg1 O2 Hg1 -122.5(2) 4_566 . . 4_565 ? N1 Hg1 O4 N4 125.4(3) . . . . ? N2 Hg1 O4 N4 -24.7(3) . . . . ? O1 Hg1 O4 N4 -158.9(3) . . . . ? O2 Hg1 O4 N4 -109.9(3) . . . . ? O5 Hg1 O4 N4 -1.9(3) . . . . ? O2 Hg1 O4 N4 84.1(3) 4_566 . . . ? O3 Hg1 O4 N4 130.5(3) 4_566 . . . ? O4 Hg1 O5 N4 1.9(3) . . . . ? N1 Hg1 O5 N4 -141.6(3) . . . . ? N2 Hg1 O5 N4 165.1(3) . . . . ? O1 Hg1 O5 N4 32.9(4) . . . . ? O2 Hg1 O5 N4 82.5(3) . . . . ? O2 Hg1 O5 N4 -80.8(3) 4_566 . . . ? O3 Hg1 O5 N4 -45.1(3) 4_566 . . . ? O4 Hg1 N1 C5 31.1(5) . . . . ? N2 Hg1 N1 C5 -171.7(4) . . . . ? O1 Hg1 N1 C5 -44.0(3) . . . . ? O2 Hg1 N1 C5 -91.6(3) . . . . ? O5 Hg1 N1 C5 131.8(3) . . . . ? O2 Hg1 N1 C5 71.7(3) 4_566 . . . ? O3 Hg1 N1 C5 26.2(3) 4_566 . . . ? O4 Hg1 N1 C1 -150.8(3) . . . . ? N2 Hg1 N1 C1 6.4(3) . . . . ? O1 Hg1 N1 C1 134.1(3) . . . . ? O2 Hg1 N1 C1 86.5(3) . . . . ? O5 Hg1 N1 C1 -50.1(4) . . . . ? O2 Hg1 N1 C1 -110.2(3) 4_566 . . . ? O3 Hg1 N1 C1 -155.7(3) 4_566 . . . ? O4 Hg1 N2 C6 157.7(3) . . . . ? N1 Hg1 N2 C6 -8.2(3) . . . . ? O1 Hg1 N2 C6 -83.1(3) . . . . ? O2 Hg1 N2 C6 -113.4(3) . . . . ? O5 Hg1 N2 C6 140.3(3) . . . . ? O2 Hg1 N2 C6 64.8(3) 4_566 . . . ? O3 Hg1 N2 C6 27.4(4) 4_566 . . . ? O4 Hg1 N2 C7 -18.2(4) . . . . ? N1 Hg1 N2 C7 175.9(4) . . . . ? O1 Hg1 N2 C7 101.0(3) . . . . ? O2 Hg1 N2 C7 70.7(3) . . . . ? O5 Hg1 N2 C7 -35.6(3) . . . . ? O2 Hg1 N2 C7 -111.1(3) 4_566 . . . ? O3 Hg1 N2 C7 -148.5(3) 4_566 . . . ? Hg1 O3 N3 O1 -153.5(3) 4_565 . . . ? Hg1 O3 N3 O2 24.9(4) 4_565 . . . ? Hg1 O1 N3 O3 178.1(3) . . . . ? Hg1 O1 N3 O2 -0.3(4) . . . . ? Hg1 O2 N3 O3 -178.1(3) . . . . ? Hg1 O2 N3 O3 -26.6(4) 4_565 . . . ? Hg1 O2 N3 O1 0.3(4) . . . . ? Hg1 O2 N3 O1 151.8(3) 4_565 . . . ? Hg1 O5 N4 O6 177.1(4) . . . . ? Hg1 O5 N4 O4 -2.9(4) . . . . ? Hg1 O4 N4 O5 3.8(5) . . . . ? Hg1 O4 N4 O6 -176.2(3) . . . . ? C5 N1 C1 C2 -1.9(6) . . . . ? Hg1 N1 C1 C2 179.9(3) . . . . ? C5 N1 C1 C6 174.0(4) . . . . ? Hg1 N1 C1 C6 -4.2(5) . . . . ? N1 C1 C2 C3 3.1(6) . . . . ? C6 C1 C2 C3 -172.6(4) . . . . ? C1 C2 C3 C4 -2.3(7) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C1 N1 C5 C4 0.0(6) . . . . ? Hg1 N1 C5 C4 178.1(3) . . . . ? C3 C4 C5 N1 0.7(7) . . . . ? C7 N2 C6 C1 -174.7(4) . . . . ? Hg1 N2 C6 C1 9.2(5) . . . . ? N1 C1 C6 N2 -4.0(6) . . . . ? C2 C1 C6 N2 172.0(4) . . . . ? C6 N2 C7 C8 -32.0(6) . . . . ? Hg1 N2 C7 C8 143.6(3) . . . . ? C6 N2 C7 C12 147.3(4) . . . . ? Hg1 N2 C7 C12 -37.2(5) . . . . ? C12 C7 C8 C9 0.3(6) . . . . ? N2 C7 C8 C9 179.5(4) . . . . ? C7 C8 C9 C10 -0.4(7) . . . . ? C8 C9 C10 C11 0.1(7) . . . . ? C8 C9 C10 C13 179.5(4) . . . . ? C9 C10 C11 C12 0.5(7) . . . . ? C13 C10 C11 C12 -178.9(4) . . . . ? C10 C11 C12 C7 -0.6(7) . . . . ? C8 C7 C12 C11 0.2(7) . . . . ? N2 C7 C12 C11 -179.1(4) . . . . ? _iucr_refine_instructions_details ; TITL TSBB-289 (L1008) CELL 0.71073 10.6101 14.2146 10.3608 89.9999 97.2161 89.9999 ZERR 4 0.0002 0.0002 0.0002 0.0000 0.0011 0.0000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H HG N O UNIT 52 48 4 16 24 MERG 2 OMIT 0 2 0 OMIT 1 1 0 TEMP -113 L.S. 4 BOND $H CONF ACTA BIND HG1 O5 BIND HG1 O2_$1 BIND HG1 O3_$1 BIND O5 HG1 BIND O2 HG1_$2 BIND O3 HG1_$2 EQIV $1 X,1/2-Y, 1/2+Z EQIV $2 X,1/2-Y,-1/2+Z FMAP 2 PLAN 20 WGHT 0.030000 4.044100 EXTI 0.001015 FVAR 0.35389 HG1 3 0.226343 0.242984 0.163102 11.00000 0.02707 0.02608 = 0.02995 -0.00168 0.00523 0.00048 O1 5 0.025022 0.247272 0.003242 11.00000 0.03256 0.04452 = 0.03037 0.00267 0.01054 -0.00109 O2 5 0.190426 0.291995 -0.082537 11.00000 0.03176 0.05567 = 0.03244 0.00684 0.00391 -0.00849 O3 5 0.006046 0.286418 -0.199838 11.00000 0.03638 0.04541 = 0.02914 0.00193 -0.00300 -0.00172 O4 5 0.163493 0.378766 0.227501 11.00000 0.04012 0.03026 = 0.04415 -0.00954 0.00358 -0.00205 O5 5 0.364626 0.385954 0.288880 11.00000 0.03758 0.08048 = 0.09036 -0.02647 0.00296 -0.01508 O6 5 0.242279 0.499422 0.335640 11.00000 0.10446 0.03428 = 0.04646 -0.01463 0.00577 -0.01472 N1 4 0.216206 0.087220 0.153525 11.00000 0.02956 0.02929 = 0.02971 -0.00084 0.00766 -0.00237 N2 4 0.425275 0.189816 0.115036 11.00000 0.02831 0.03016 = 0.03309 0.00225 0.00605 -0.00373 N3 4 0.071646 0.275868 -0.094272 11.00000 0.03108 0.02726 = 0.02910 -0.00170 0.00389 -0.00153 N4 4 0.260107 0.422968 0.286049 11.00000 0.04813 0.03640 = 0.03396 -0.00186 0.00676 -0.01387 C1 1 0.325192 0.041289 0.139612 11.00000 0.03121 0.02528 = 0.02666 -0.00023 0.00336 -0.00112 C2 1 0.329826 -0.055674 0.132831 11.00000 0.04114 0.03056 = 0.03078 0.00023 0.00760 0.00350 AFIX 43 H2 2 0.408146 -0.086887 0.127336 11.00000 -1.20000 AFIX 0 C3 1 0.219060 -0.106771 0.134138 11.00000 0.04608 0.02409 = 0.03513 0.00043 0.00626 -0.00274 AFIX 43 H3 2 0.219808 -0.173355 0.126382 11.00000 -1.20000 AFIX 0 C4 1 0.108154 -0.060124 0.146770 11.00000 0.04285 0.02844 = 0.04380 -0.00448 0.01129 -0.01104 AFIX 43 H4 2 0.031267 -0.094084 0.148488 11.00000 -1.20000 AFIX 0 C5 1 0.109424 0.037496 0.157046 11.00000 0.03196 0.03405 = 0.04247 -0.00412 0.00953 -0.00388 AFIX 43 H5 2 0.032704 0.069661 0.166794 11.00000 -1.20000 AFIX 0 C6 1 0.435907 0.100549 0.123115 11.00000 0.02967 0.03058 = 0.03085 -0.00041 0.00331 0.00202 AFIX 43 H6 2 0.516147 0.071974 0.118437 11.00000 -1.20000 AFIX 0 C7 1 0.529147 0.248517 0.087967 11.00000 0.02746 0.02652 = 0.02936 -0.00349 0.00941 -0.00133 C8 1 0.655393 0.226991 0.127950 11.00000 0.02815 0.02775 = 0.03395 0.00351 0.00468 0.00430 AFIX 43 H8 2 0.676995 0.171287 0.176394 11.00000 -1.20000 AFIX 0 C9 1 0.749446 0.286683 0.097172 11.00000 0.02890 0.03223 = 0.03549 -0.00039 0.00721 0.00113 AFIX 43 H9 2 0.835627 0.271407 0.125641 11.00000 -1.20000 AFIX 0 C10 1 0.722142 0.368750 0.025604 11.00000 0.03324 0.03156 = 0.03373 -0.00087 0.00810 0.00035 C11 1 0.594573 0.388669 -0.014233 11.00000 0.03593 0.03270 = 0.04686 0.00981 0.00609 0.00057 AFIX 43 H11 2 0.573238 0.443938 -0.063751 11.00000 -1.20000 AFIX 0 C12 1 0.497848 0.330307 0.016180 11.00000 0.02883 0.03245 = 0.04803 0.00979 0.00338 0.00440 AFIX 43 H12 2 0.411527 0.345693 -0.011382 11.00000 -1.20000 AFIX 0 C13 1 0.825657 0.433639 -0.006255 11.00000 0.03791 0.03666 = 0.05187 0.00601 0.01147 -0.00376 AFIX 137 H131 2 0.842225 0.422609 -0.095963 11.00000 -1.50000 H132 2 0.903217 0.421582 0.053362 11.00000 -1.50000 H133 2 0.799052 0.499052 0.003054 11.00000 -1.50000 HKLF 4 1 0 0 1 0 -1 0 1 0 0 REM TSBB-289 (L1008) REM R1 = 0.0305 for 3755 Fo > 4sig(Fo) and 0.0418 for all 4501 data REM 219 parameters refined using 0 restraints END WGHT 0.0300 4.0443 REM Highest difference peak 2.037, deepest hole -1.600, 1-sigma level 0.146 Q1 1 0.3242 0.2532 0.0177 11.00000 0.05 2.04 Q2 1 0.2989 0.2352 0.1478 11.00000 0.05 1.46 Q3 1 0.2986 0.2450 0.2226 11.00000 0.05 1.06 Q4 1 0.2235 0.2812 0.1599 11.00000 0.05 1.06 Q5 1 0.1345 0.2419 0.0795 11.00000 0.05 0.99 Q6 1 0.2351 0.2394 0.0862 11.00000 0.05 0.73 Q7 1 0.2315 0.2419 0.2367 11.00000 0.05 0.68 Q8 1 0.2010 0.1605 0.1746 11.00000 0.05 0.64 Q9 1 0.4304 0.2226 0.0286 11.00000 0.05 0.62 Q10 1 0.3493 0.2164 0.3190 11.00000 0.05 0.60 ; # End of CIF ============================================================