Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_address ; Chemistry Chung Yuan Christian University Chung Li 320 TAIWAN ; _publ_contact_author_email JDCHEN@CYCU.EDU.TW _publ_section_title ; Crystal Structures and Solution Behaviors of Dinuclear d10-Metal Complexes Containing Anions of N,N-Bis(pyrimidine-2-yl)formamidine ; loop_ _publ_author_name 'Jhy-Der Chen.' 'Zhi-Kai Chan.' 'Tsun-Ren Chen.' 'Chen W. Liu' data_1a _database_code_depnum_ccdc_archive 'CCDC 640642' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H21 I3 N18 Zn2' _chemical_formula_weight 1109.06 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.688(2) _cell_length_b 11.6319(7) _cell_length_c 25.9213(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.3440(10) _cell_angle_gamma 90.00 _cell_volume 9039.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 3.150 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2423 _exptl_absorpt_correction_T_max 0.3319 _exptl_absorpt_process_details ? _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_decay_% ? _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _diffrn_reflns_number 48772 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.38 _reflns_number_total 8277 _reflns_number_gt 4859 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0100P)^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 8277 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Zn1 Zn 0.539968(12) 0.88631(4) 0.118727(16) 0.06301(12) Uani 1 1 d . . . Zn2 Zn 0.432448(13) 0.77828(3) 0.146658(16) 0.06131(12) Uani 1 1 d . . . I1 I 0.231302(8) 0.65937(2) 0.170407(11) 0.08276(10) Uani 1 1 d . . . I2 I 0.238357(11) 0.48979(3) 0.089585(13) 0.11693(13) Uani 1 1 d . . . I3 I 0.220821(9) 0.82634(3) 0.249681(13) 0.10564(12) Uani 1 1 d . . . N1 N 0.38558(9) 0.8555(2) 0.20071(10) 0.0591(7) Uani 1 1 d . . . N2 N 0.40286(9) 1.0498(2) 0.22523(10) 0.0601(7) Uani 1 1 d . . . N3 N 0.44733(8) 0.9322(2) 0.18174(10) 0.0513(7) Uani 1 1 d . . . N4 N 0.51121(8) 1.0025(2) 0.16039(10) 0.0521(7) Uani 1 1 d . . . N5 N 0.53175(9) 1.1993(3) 0.17539(11) 0.0642(8) Uani 1 1 d . . . N6 N 0.57038(9) 1.0659(2) 0.13165(10) 0.0603(7) Uani 1 1 d . . . N7 N 0.38031(9) 0.7601(2) 0.08449(11) 0.0562(7) Uani 1 1 d . . . N8 N 0.37876(10) 0.7817(3) -0.00770(12) 0.0749(9) Uani 1 1 d . . . N9 N 0.44329(8) 0.8148(2) 0.06150(10) 0.0509(7) Uani 1 1 d . . . N10 N 0.51158(8) 0.8585(2) 0.04425(10) 0.0532(7) Uani 1 1 d . . . N11 N 0.52499(9) 0.8261(3) -0.04112(12) 0.0676(8) Uani 1 1 d . . . N12 N 0.57934(10) 0.9074(3) 0.02924(11) 0.0718(8) Uani 1 1 d . . . N13 N 0.39786(11) 0.5659(3) 0.17477(12) 0.0725(8) Uani 1 1 d . . . N14 N 0.46201(10) 0.4437(3) 0.19210(12) 0.0784(9) Uani 1 1 d . . . N15 N 0.46610(9) 0.6393(2) 0.17068(10) 0.0576(7) Uani 1 1 d . . . N16 N 0.53311(10) 0.7147(2) 0.16213(11) 0.0624(8) Uani 1 1 d . . . N17 N 0.59993(12) 0.6053(3) 0.18744(14) 0.0911(11) Uani 1 1 d . . . N18 N 0.59587(9) 0.7894(3) 0.14702(11) 0.0658(8) Uani 1 1 d . . . C1 C 0.34886(12) 0.8626(3) 0.21934(14) 0.0710(10) Uani 1 1 d . . . H1A H 0.3302 0.7990 0.2168 0.085 Uiso 1 1 calc R . . C2 C 0.33751(12) 0.9604(4) 0.24217(14) 0.0752(11) Uani 1 1 d . . . H2B H 0.3119 0.9643 0.2558 0.090 Uiso 1 1 calc R . . C3 C 0.36563(12) 1.0530(3) 0.24411(13) 0.0702(10) Uani 1 1 d . . . H3A H 0.3584 1.1210 0.2592 0.084 Uiso 1 1 calc R . . C4 C 0.41077(11) 0.9497(3) 0.20448(12) 0.0517(8) Uani 1 1 d . . . C5 C 0.47680(11) 1.0134(3) 0.18247(12) 0.0520(8) Uani 1 1 d . . . H5B H 0.4732 1.0821 0.1994 0.062 Uiso 1 1 calc R . . C6 C 0.53840(11) 1.0959(3) 0.15691(13) 0.0543(9) Uani 1 1 d . . . C7 C 0.56080(14) 1.2795(3) 0.16623(15) 0.0788(11) Uani 1 1 d . . . H7A H 0.5580 1.3539 0.1782 0.095 Uiso 1 1 calc R . . C8 C 0.59464(14) 1.2567(4) 0.13982(17) 0.0841(12) Uani 1 1 d . . . H8B H 0.6142 1.3140 0.1341 0.101 Uiso 1 1 calc R . . C9 C 0.59816(12) 1.1483(4) 0.12284(14) 0.0749(11) Uani 1 1 d . . . H9A H 0.6203 1.1306 0.1047 0.090 Uiso 1 1 calc R . . C10 C 0.33886(13) 0.7239(3) 0.07377(16) 0.0734(11) Uani 1 1 d . . . H10A H 0.3253 0.7043 0.1014 0.088 Uiso 1 1 calc R . . C11 C 0.31517(13) 0.7144(4) 0.02275(19) 0.0907(13) Uani 1 1 d . . . H11B H 0.2858 0.6886 0.0151 0.109 Uiso 1 1 calc R . . C12 C 0.33678(13) 0.7449(4) -0.01656(16) 0.0884(13) Uani 1 1 d . . . H12B H 0.3211 0.7395 -0.0514 0.106 Uiso 1 1 calc R . . C13 C 0.39924(11) 0.7856(3) 0.04329(15) 0.0559(9) Uani 1 1 d . . . C14 C 0.46944(11) 0.8296(3) 0.02757(13) 0.0539(8) Uani 1 1 d . . . H14B H 0.4580 0.8195 -0.0084 0.065 Uiso 1 1 calc R . . C15 C 0.53931(11) 0.8650(3) 0.00798(15) 0.0570(9) Uani 1 1 d . . . C16 C 0.55487(14) 0.8316(3) -0.07151(15) 0.0798(11) Uani 1 1 d . . . H16A H 0.5471 0.8041 -0.1059 0.096 Uiso 1 1 calc R . . C17 C 0.59669(14) 0.8764(4) -0.05394(19) 0.0920(13) Uani 1 1 d . . . H17B H 0.6168 0.8810 -0.0761 0.110 Uiso 1 1 calc R . . C18 C 0.60792(13) 0.9143(4) -0.00276(19) 0.0886(13) Uani 1 1 d . . . H18A H 0.6361 0.9454 0.0099 0.106 Uiso 1 1 calc R . . C19 C 0.37323(14) 0.4765(4) 0.18209(16) 0.0900(12) Uani 1 1 d . . . H19A H 0.3427 0.4872 0.1790 0.108 Uiso 1 1 calc R . . C20 C 0.39068(17) 0.3684(4) 0.19407(17) 0.0960(14) Uani 1 1 d . . . H20A H 0.3729 0.3060 0.1983 0.115 Uiso 1 1 calc R . . C21 C 0.43519(18) 0.3585(4) 0.19929(16) 0.0924(14) Uani 1 1 d . . . H21A H 0.4480 0.2869 0.2086 0.111 Uiso 1 1 calc R . . C22 C 0.44099(14) 0.5444(3) 0.18016(12) 0.0594(9) Uani 1 1 d . . . C23 C 0.50958(13) 0.6303(3) 0.17505(13) 0.0627(9) Uani 1 1 d . . . H23A H 0.5238 0.5621 0.1876 0.075 Uiso 1 1 calc R . . C24 C 0.57814(13) 0.6983(4) 0.16668(14) 0.0671(10) Uani 1 1 d . . . C25 C 0.64288(18) 0.6053(5) 0.18793(19) 0.1078(16) Uani 1 1 d . . . H25A H 0.6595 0.5413 0.2017 0.129 Uiso 1 1 calc R . . C26 C 0.66451(15) 0.6945(5) 0.16930(19) 0.1020(16) Uani 1 1 d . . . H26A H 0.6951 0.6920 0.1710 0.122 Uiso 1 1 calc R . . C27 C 0.63929(13) 0.7878(4) 0.14797(15) 0.0831(12) Uani 1 1 d . . . H27A H 0.6526 0.8493 0.1343 0.100 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 Zn1 0.0559(2) 0.0670(3) 0.0651(3) -0.0088(2) 0.0106(2) 0.0043(2) Zn2 0.0657(3) 0.0475(2) 0.0683(3) -0.0023(2) 0.0090(2) 0.00416(19) I1 0.05673(15) 0.0902(2) 0.0999(2) 0.02709(16) 0.01343(14) -0.00692(13) I2 0.1125(3) 0.1198(3) 0.1206(3) -0.0109(2) 0.0297(2) -0.0229(2) I3 0.07032(19) 0.1066(2) 0.1443(3) -0.0032(2) 0.03260(18) 0.00494(16) N1 0.0623(18) 0.053(2) 0.067(2) -0.0032(15) 0.0245(16) -0.0075(15) N2 0.0627(19) 0.059(2) 0.0623(19) -0.0084(16) 0.0212(15) -0.0028(15) N3 0.0516(17) 0.0466(18) 0.0579(18) -0.0018(13) 0.0168(14) -0.0003(14) N4 0.0500(16) 0.0464(18) 0.0597(18) -0.0062(13) 0.0114(15) -0.0033(14) N5 0.068(2) 0.050(2) 0.072(2) -0.0003(16) 0.0112(16) -0.0041(16) N6 0.0513(17) 0.067(2) 0.0622(19) -0.0002(15) 0.0106(15) -0.0056(16) N7 0.0467(18) 0.0588(19) 0.067(2) 0.0067(15) 0.0208(16) -0.0030(13) N8 0.056(2) 0.101(3) 0.063(2) 0.0132(18) 0.0020(17) -0.0143(17) N9 0.0456(16) 0.0526(18) 0.0538(17) 0.0015(14) 0.0092(14) -0.0025(13) N10 0.0461(17) 0.0564(19) 0.0580(18) 0.0002(14) 0.0131(15) -0.0036(13) N11 0.0590(19) 0.091(2) 0.055(2) -0.0002(17) 0.0178(17) 0.0066(16) N12 0.0553(19) 0.087(2) 0.078(2) -0.0016(18) 0.0236(18) -0.0068(17) N13 0.076(2) 0.056(2) 0.092(2) 0.0146(17) 0.0323(19) -0.0010(18) N14 0.100(2) 0.050(2) 0.093(2) 0.0204(18) 0.0373(19) 0.0090(19) N15 0.0637(19) 0.0467(19) 0.0619(19) 0.0050(14) 0.0122(15) 0.0037(15) N16 0.0563(19) 0.062(2) 0.067(2) 0.0028(16) 0.0077(16) 0.0053(16) N17 0.064(2) 0.092(3) 0.109(3) 0.010(2) 0.001(2) 0.027(2) N18 0.0474(19) 0.075(2) 0.074(2) -0.0102(18) 0.0098(16) -0.0023(15) C1 0.074(3) 0.066(3) 0.077(3) -0.003(2) 0.025(2) -0.015(2) C2 0.065(2) 0.088(3) 0.082(3) -0.005(2) 0.035(2) -0.012(2) C3 0.072(3) 0.075(3) 0.065(2) -0.013(2) 0.018(2) 0.012(2) C4 0.053(2) 0.050(2) 0.051(2) 0.0023(18) 0.0096(17) 0.0031(18) C5 0.056(2) 0.049(2) 0.051(2) -0.0003(17) 0.0105(18) 0.0018(18) C6 0.045(2) 0.056(3) 0.057(2) -0.0021(19) 0.0018(18) -0.0027(19) C7 0.084(3) 0.056(3) 0.090(3) -0.001(2) 0.003(3) -0.003(2) C8 0.078(3) 0.080(3) 0.093(3) 0.008(3) 0.016(3) -0.025(2) C9 0.063(2) 0.097(4) 0.065(3) 0.003(2) 0.012(2) -0.012(2) C10 0.060(3) 0.083(3) 0.081(3) 0.011(2) 0.023(2) -0.003(2) C11 0.051(2) 0.118(4) 0.101(4) 0.021(3) 0.012(3) -0.017(2) C12 0.065(3) 0.116(4) 0.073(3) 0.017(3) -0.010(2) -0.012(2) C13 0.055(2) 0.048(2) 0.065(3) 0.0034(19) 0.012(2) -0.0002(17) C14 0.058(2) 0.053(2) 0.051(2) 0.0033(17) 0.0144(19) 0.0032(17) C15 0.048(2) 0.055(2) 0.070(3) 0.010(2) 0.018(2) 0.0053(17) C16 0.074(3) 0.105(3) 0.064(3) 0.013(2) 0.022(2) 0.018(2) C17 0.071(3) 0.122(4) 0.093(4) 0.023(3) 0.041(3) 0.014(3) C18 0.063(3) 0.109(4) 0.100(4) -0.003(3) 0.030(3) -0.009(2) C19 0.088(3) 0.080(4) 0.112(4) 0.017(3) 0.043(3) 0.001(3) C20 0.117(4) 0.066(3) 0.121(4) 0.017(3) 0.061(3) -0.014(3) C21 0.133(4) 0.049(3) 0.108(4) 0.025(2) 0.055(3) 0.021(3) C22 0.086(3) 0.044(2) 0.053(2) 0.0073(18) 0.023(2) -0.003(2) C23 0.070(3) 0.057(3) 0.060(2) 0.0043(19) 0.011(2) 0.010(2) C24 0.069(3) 0.071(3) 0.056(2) -0.008(2) 0.003(2) 0.007(2) C25 0.089(4) 0.105(4) 0.119(4) -0.001(3) -0.003(3) 0.029(3) C26 0.059(3) 0.128(5) 0.113(4) -0.033(3) 0.003(3) 0.021(3) C27 0.058(3) 0.102(4) 0.087(3) -0.021(3) 0.012(2) -0.006(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 Zn1 N10 1.967(3) . ? Zn1 N4 2.045(3) . ? Zn1 N18 2.053(3) . ? Zn1 N6 2.283(3) . ? Zn1 N16 2.323(3) . ? Zn2 N15 1.948(3) . ? Zn2 N3 2.016(3) . ? Zn2 N7 2.025(3) . ? Zn2 N9 2.340(3) . ? Zn2 N1 2.387(3) . ? I1 I3 2.8949(5) . ? I1 I2 2.9191(5) . ? N1 C1 1.320(4) . ? N1 C4 1.332(4) . ? N2 C4 1.326(4) . ? N2 C3 1.336(4) . ? N3 C5 1.305(4) . ? N3 C4 1.389(4) . ? N4 C5 1.310(3) . ? N4 C6 1.384(4) . ? N5 C6 1.326(4) . ? N5 C7 1.346(4) . ? N6 C9 1.334(4) . ? N6 C6 1.337(4) . ? N7 C10 1.312(4) . ? N7 C13 1.353(4) . ? N8 C12 1.330(4) . ? N8 C13 1.337(4) . ? N9 C14 1.322(4) . ? N9 C13 1.376(4) . ? N10 C14 1.317(4) . ? N10 C15 1.398(4) . ? N11 C16 1.332(4) . ? N11 C15 1.334(4) . ? N12 C15 1.329(4) . ? N12 C18 1.332(4) . ? N13 C19 1.323(4) . ? N13 C22 1.325(4) . ? N14 C21 1.327(5) . ? N14 C22 1.341(4) . ? N15 C23 1.319(4) . ? N15 C22 1.397(4) . ? N16 C23 1.305(4) . ? N16 C24 1.375(4) . ? N17 C25 1.315(5) . ? N17 C24 1.324(4) . ? N18 C27 1.328(4) . ? N18 C24 1.340(4) . ? C1 C2 1.361(5) . ? C2 C3 1.375(5) . ? C7 C8 1.386(5) . ? C8 C9 1.347(5) . ? C10 C11 1.371(5) . ? C11 C12 1.376(5) . ? C16 C17 1.370(5) . ? C17 C18 1.370(5) . ? C19 C20 1.375(5) . ? C20 C21 1.349(5) . ? C25 C26 1.373(6) . ? C26 C27 1.378(6) . ? 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 N10 Zn1 N4 118.44(10) . . ? N10 Zn1 N18 114.91(11) . . ? N4 Zn1 N18 126.63(10) . . ? N10 Zn1 N6 112.05(10) . . ? N4 Zn1 N6 61.75(10) . . ? N18 Zn1 N6 99.55(11) . . ? N10 Zn1 N16 105.51(10) . . ? N4 Zn1 N16 102.60(10) . . ? N18 Zn1 N16 60.68(11) . . ? N6 Zn1 N16 142.34(9) . . ? N15 Zn2 N3 122.66(11) . . ? N15 Zn2 N7 116.26(11) . . ? N3 Zn2 N7 121.07(10) . . ? N15 Zn2 N9 106.24(10) . . ? N3 Zn2 N9 101.54(10) . . ? N7 Zn2 N9 61.04(10) . . ? N15 Zn2 N1 118.00(10) . . ? N3 Zn2 N1 60.52(10) . . ? N7 Zn2 N1 91.93(10) . . ? N9 Zn2 N1 135.24(9) . . ? I3 I1 I2 177.914(12) . . ? C1 N1 C4 116.7(3) . . ? C1 N1 Zn2 155.1(2) . . ? C4 N1 Zn2 86.5(2) . . ? C4 N2 C3 114.7(3) . . ? C5 N3 C4 120.5(3) . . ? C5 N3 Zn2 137.6(2) . . ? C4 N3 Zn2 101.3(2) . . ? C5 N4 C6 120.4(3) . . ? C5 N4 Zn1 140.7(2) . . ? C6 N4 Zn1 98.6(2) . . ? C6 N5 C7 113.9(3) . . ? C9 N6 C6 117.3(3) . . ? C9 N6 Zn1 152.6(3) . . ? C6 N6 Zn1 89.5(2) . . ? C10 N7 C13 117.6(3) . . ? C10 N7 Zn2 140.1(3) . . ? C13 N7 Zn2 101.9(2) . . ? C12 N8 C13 114.5(3) . . ? C14 N9 C13 119.7(3) . . ? C14 N9 Zn2 151.6(2) . . ? C13 N9 Zn2 87.2(2) . . ? C14 N10 C15 119.3(3) . . ? C14 N10 Zn1 124.2(2) . . ? C15 N10 Zn1 116.5(2) . . ? C16 N11 C15 114.8(3) . . ? C15 N12 C18 115.9(3) . . ? C19 N13 C22 115.2(3) . . ? C21 N14 C22 113.8(3) . . ? C23 N15 C22 120.5(3) . . ? C23 N15 Zn2 123.4(2) . . ? C22 N15 Zn2 115.9(2) . . ? C23 N16 C24 118.3(3) . . ? C23 N16 Zn1 152.1(2) . . ? C24 N16 Zn1 88.1(2) . . ? C25 N17 C24 115.0(4) . . ? C27 N18 C24 118.0(3) . . ? C27 N18 Zn1 140.6(3) . . ? C24 N18 Zn1 101.2(2) . . ? N1 C1 C2 122.0(3) . . ? C1 C2 C3 117.0(3) . . ? N2 C3 C2 122.9(3) . . ? N2 C4 N1 126.7(3) . . ? N2 C4 N3 122.3(3) . . ? N1 C4 N3 110.9(3) . . ? N3 C5 N4 123.0(3) . . ? N5 C6 N6 126.8(3) . . ? N5 C6 N4 123.1(3) . . ? N6 C6 N4 110.0(3) . . ? N5 C7 C8 123.3(4) . . ? C9 C8 C7 117.5(4) . . ? N6 C9 C8 121.2(4) . . ? N7 C10 C11 121.4(4) . . ? C10 C11 C12 117.0(3) . . ? N8 C12 C11 123.9(4) . . ? N8 C13 N7 125.6(3) . . ? N8 C13 N9 124.5(3) . . ? N7 C13 N9 109.8(3) . . ? N10 C14 N9 120.5(3) . . ? N12 C15 N11 127.5(3) . . ? N12 C15 N10 112.5(3) . . ? N11 C15 N10 120.0(3) . . ? N11 C16 C17 122.4(4) . . ? C16 C17 C18 117.9(4) . . ? N12 C18 C17 121.4(4) . . ? N13 C19 C20 123.0(4) . . ? C21 C20 C19 116.0(4) . . ? N14 C21 C20 124.6(4) . . ? N13 C22 N14 127.6(3) . . ? N13 C22 N15 114.1(3) . . ? N14 C22 N15 118.3(4) . . ? N16 C23 N15 121.6(3) . . ? N17 C24 N18 126.1(4) . . ? N17 C24 N16 124.0(4) . . ? N18 C24 N16 109.9(3) . . ? N17 C25 C26 123.7(4) . . ? C25 C26 C27 117.6(4) . . ? N18 C27 C26 119.6(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.600 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.060 #===END data_1c _database_code_depnum_ccdc_archive 'CCDC 640643' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H21 Cl N18 O4 Zn2' _chemical_formula_weight 827.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.287(2) _cell_length_b 12.424(3) _cell_length_c 31.198(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.391(5) _cell_angle_gamma 90.00 _cell_volume 4347.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7692 _exptl_absorpt_correction_T_max 0.9998 _exptl_absorpt_process_details ? _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_decay_% ? _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _diffrn_reflns_number 23775 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0929 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 24.75 _reflns_number_total 7364 _reflns_number_gt 3891 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0322P)^2^+10.1225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00029(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7364 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Zn1 Zn 0.71065(8) 0.80361(6) -0.07992(3) 0.0646(3) Uani 1 1 d . . . Zn2 Zn 0.86389(8) 0.71987(6) 0.02824(3) 0.0647(3) Uani 1 1 d . . . Cl1 Cl 0.9590(3) 1.3582(3) -0.22534(8) 0.1085(8) Uani 1 1 d . . . O1 O 1.0328(18) 1.2750(17) -0.2249(6) 0.365(12) Uani 1 1 d . . . O2 O 0.8449(11) 1.3330(15) -0.2365(4) 0.294(8) Uani 1 1 d . . . O3 O 0.9813(14) 1.3877(13) -0.1877(3) 0.328(10) Uani 1 1 d . . . O4 O 0.9908(15) 1.3999(13) -0.2593(4) 0.306(9) Uani 1 1 d . . . C1 C 1.1466(8) 0.7345(6) 0.0858(2) 0.076(2) Uani 1 1 d . . . H1A H 1.1416 0.6865 0.1084 0.091 Uiso 1 1 calc R . . C2 C 1.2527(7) 0.7857(7) 0.0818(3) 0.083(2) Uani 1 1 d . . . H2A H 1.3200 0.7719 0.1011 0.100 Uiso 1 1 calc R . . C3 C 1.2566(7) 0.8581(7) 0.0485(3) 0.080(2) Uani 1 1 d . . . H3A H 1.3274 0.8948 0.0461 0.096 Uiso 1 1 calc R . . C4 C 1.0656(6) 0.8230(5) 0.0256(2) 0.0572(17) Uani 1 1 d . . . C5 C 0.9567(6) 0.8851(5) -0.0377(2) 0.0576(17) Uani 1 1 d . . . H5A H 1.0208 0.9300 -0.0413 0.069 Uiso 1 1 calc R . . C6 C 0.8656(7) 0.9475(5) -0.1045(2) 0.0570(17) Uani 1 1 d . . . C7 C 0.9408(8) 1.0656(6) -0.1489(3) 0.082(2) Uani 1 1 d . . . H7A H 1.0023 1.1090 -0.1564 0.098 Uiso 1 1 calc R . . C8 C 0.8360(10) 1.0632(7) -0.1757(3) 0.094(3) Uani 1 1 d . . . H8A H 0.8255 1.1056 -0.2004 0.113 Uiso 1 1 calc R . . C9 C 0.7473(8) 0.9965(7) -0.1650(2) 0.083(2) Uani 1 1 d . . . H9A H 0.6763 0.9918 -0.1831 0.100 Uiso 1 1 calc R . . C10 C 0.7891(8) 0.7366(6) 0.1225(3) 0.078(2) Uani 1 1 d . . . H10A H 0.8579 0.7046 0.1359 0.094 Uiso 1 1 calc R . . C11 C 0.6972(10) 0.7692(8) 0.1472(3) 0.103(3) Uani 1 1 d . . . H11A H 0.7057 0.7628 0.1771 0.124 Uiso 1 1 calc R . . C12 C 0.5948(9) 0.8108(8) 0.1252(3) 0.106(3) Uani 1 1 d . . . H12A H 0.5330 0.8307 0.1409 0.127 Uiso 1 1 calc R . . C13 C 0.6722(7) 0.7936(5) 0.0616(2) 0.0625(18) Uani 1 1 d . . . C14 C 0.5805(6) 0.8389(5) -0.0067(2) 0.0568(17) Uani 1 1 d . . . H14A H 0.5142 0.8609 0.0063 0.068 Uiso 1 1 calc R . . C15 C 0.4738(6) 0.8784(5) -0.0730(2) 0.0596(18) Uani 1 1 d . . . C16 C 0.2826(7) 0.9416(7) -0.0794(3) 0.084(2) Uani 1 1 d . . . H16A H 0.2169 0.9666 -0.0668 0.101 Uiso 1 1 calc R . . C17 C 0.2757(8) 0.9333(7) -0.1230(4) 0.095(3) Uani 1 1 d . . . H17A H 0.2061 0.9510 -0.1404 0.114 Uiso 1 1 calc R . . C18 C 0.3753(10) 0.8978(8) -0.1404(3) 0.105(3) Uani 1 1 d . . . H18A H 0.3722 0.8929 -0.1702 0.126 Uiso 1 1 calc R . . C19 C 0.9318(8) 0.4481(8) 0.1041(2) 0.096(3) Uani 1 1 d . . . H19A H 0.9693 0.4669 0.1311 0.115 Uiso 1 1 calc R . . C20 C 0.8977(9) 0.3427(7) 0.0959(3) 0.094(3) Uani 1 1 d . . . H20A H 0.9065 0.2906 0.1174 0.112 Uiso 1 1 calc R . . C21 C 0.8522(8) 0.3190(6) 0.0565(3) 0.084(2) Uani 1 1 d . . . H21A H 0.8320 0.2475 0.0506 0.101 Uiso 1 1 calc R . . C22 C 0.8649(6) 0.4898(5) 0.0348(2) 0.0555(17) Uani 1 1 d . . . C23 C 0.8070(6) 0.5515(5) -0.0354(2) 0.0582(17) Uani 1 1 d . . . H23A H 0.8066 0.4804 -0.0448 0.070 Uiso 1 1 calc R . . C24 C 0.7391(7) 0.6019(5) -0.1055(2) 0.0628(18) Uani 1 1 d . . . C25 C 0.7036(9) 0.4967(7) -0.1643(3) 0.103(3) Uani 1 1 d . . . H25A H 0.7123 0.4312 -0.1780 0.124 Uiso 1 1 calc R . . C26 C 0.6484(9) 0.5797(8) -0.1886(3) 0.102(3) Uani 1 1 d . . . H26A H 0.6135 0.5692 -0.2167 0.123 Uiso 1 1 calc R . . C27 C 0.6480(8) 0.6792(7) -0.1685(2) 0.084(2) Uani 1 1 d . . . H27A H 0.6182 0.7391 -0.1840 0.100 Uiso 1 1 calc R . . N1 N 1.0501(5) 0.7528(4) 0.05763(18) 0.0607(15) Uani 1 1 d . . . N2 N 1.1630(6) 0.8776(4) 0.01953(18) 0.0647(15) Uani 1 1 d . . . N3 N 0.9610(5) 0.8283(4) -0.00270(17) 0.0541(13) Uani 1 1 d . . . N4 N 0.8687(5) 0.8832(4) -0.06804(16) 0.0575(14) Uani 1 1 d . . . N5 N 0.9588(6) 1.0083(5) -0.11240(19) 0.0704(16) Uani 1 1 d . . . N6 N 0.7614(6) 0.9384(4) -0.12888(18) 0.0676(16) Uani 1 1 d . . . N7 N 0.7760(6) 0.7522(4) 0.07969(19) 0.0661(15) Uani 1 1 d . . . N8 N 0.5800(6) 0.8241(5) 0.0824(2) 0.0813(18) Uani 1 1 d . . . N9 N 0.6755(6) 0.8025(4) 0.01762(18) 0.0644(15) Uani 1 1 d . . . N10 N 0.5781(5) 0.8446(4) -0.04930(18) 0.0585(14) Uani 1 1 d . . . N11 N 0.3817(6) 0.9145(5) -0.0541(2) 0.0764(18) Uani 1 1 d . . . N12 N 0.4790(5) 0.8693(5) -0.1158(2) 0.0750(17) Uani 1 1 d . . . N13 N 0.9114(6) 0.5232(4) 0.07364(19) 0.0751(18) Uani 1 1 d . . . N14 N 0.8329(5) 0.3888(4) 0.02432(18) 0.0686(16) Uani 1 1 d . . . N15 N 0.8413(5) 0.5727(4) 0.00499(16) 0.0565(14) Uani 1 1 d . . . N16 N 0.7733(5) 0.6271(4) -0.06321(16) 0.0550(13) Uani 1 1 d . . . N17 N 0.7450(6) 0.5040(5) -0.12280(19) 0.083(2) Uani 1 1 d . . . N18 N 0.6902(5) 0.6892(4) -0.12727(17) 0.0648(15) 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 Zn1 0.0655(6) 0.0603(5) 0.0677(5) -0.0092(4) 0.0060(4) -0.0016(4) Zn2 0.0782(6) 0.0493(5) 0.0658(5) -0.0055(4) 0.0054(4) -0.0083(4) Cl1 0.135(2) 0.118(2) 0.0683(15) -0.0020(14) -0.0074(15) -0.0199(18) O1 0.38(3) 0.40(3) 0.31(2) 0.003(18) 0.049(16) 0.20(2) O2 0.153(10) 0.52(3) 0.204(11) -0.068(13) -0.002(8) -0.079(13) O3 0.42(2) 0.42(2) 0.110(7) -0.138(10) -0.095(10) 0.122(17) O4 0.37(2) 0.330(18) 0.196(11) 0.147(12) -0.051(11) -0.148(15) C1 0.089(6) 0.058(5) 0.075(5) -0.008(4) -0.014(5) 0.025(4) C2 0.063(6) 0.085(6) 0.096(6) -0.018(5) -0.019(5) 0.010(5) C3 0.060(5) 0.078(6) 0.101(6) -0.025(5) 0.008(5) 0.004(4) C4 0.058(5) 0.050(4) 0.062(4) -0.011(3) -0.001(4) 0.010(3) C5 0.058(5) 0.048(4) 0.066(5) 0.000(4) 0.006(4) 0.004(3) C6 0.060(5) 0.053(4) 0.058(4) -0.004(3) 0.009(4) 0.003(4) C7 0.100(7) 0.080(6) 0.066(5) 0.009(4) 0.012(5) -0.010(5) C8 0.136(9) 0.081(6) 0.064(5) 0.013(4) 0.011(6) -0.001(6) C9 0.099(7) 0.085(6) 0.061(5) 0.002(4) -0.011(5) 0.004(5) C10 0.082(6) 0.078(5) 0.072(5) 0.002(4) -0.002(5) -0.006(4) C11 0.113(8) 0.125(8) 0.073(6) -0.022(5) 0.012(6) -0.009(7) C12 0.100(8) 0.147(9) 0.074(6) 0.001(6) 0.031(6) -0.011(7) C13 0.067(5) 0.058(4) 0.063(5) -0.005(4) 0.010(4) -0.006(4) C14 0.055(5) 0.043(4) 0.073(5) -0.002(3) 0.009(4) -0.002(3) C15 0.057(5) 0.049(4) 0.074(5) 0.011(3) 0.008(4) 0.007(3) C16 0.054(5) 0.085(6) 0.114(7) 0.024(5) 0.010(5) 0.006(4) C17 0.058(6) 0.094(6) 0.128(9) 0.024(6) -0.010(6) 0.013(5) C18 0.105(8) 0.103(7) 0.101(7) 0.012(6) -0.012(6) 0.007(6) C19 0.128(8) 0.097(7) 0.061(5) 0.023(5) -0.001(5) -0.004(6) C20 0.150(9) 0.056(5) 0.076(6) 0.017(4) 0.022(6) 0.008(5) C21 0.135(8) 0.053(5) 0.068(5) 0.003(4) 0.036(5) 0.013(5) C22 0.060(4) 0.054(4) 0.052(4) 0.005(3) 0.005(3) 0.012(3) C23 0.065(5) 0.046(4) 0.062(5) -0.005(3) 0.003(4) 0.003(3) C24 0.085(5) 0.055(4) 0.048(4) -0.003(3) 0.009(4) 0.004(4) C25 0.165(10) 0.076(6) 0.065(6) -0.022(5) 0.001(6) -0.001(6) C26 0.136(9) 0.104(7) 0.061(5) -0.012(5) -0.014(5) 0.014(6) C27 0.104(7) 0.085(6) 0.057(5) 0.004(4) -0.013(4) 0.016(5) N1 0.071(4) 0.045(3) 0.066(4) -0.002(3) 0.007(3) 0.007(3) N2 0.055(4) 0.061(4) 0.077(4) -0.010(3) 0.004(3) -0.005(3) N3 0.059(4) 0.044(3) 0.057(3) -0.001(3) -0.004(3) 0.000(2) N4 0.071(4) 0.052(3) 0.049(3) 0.004(3) 0.002(3) 0.006(3) N5 0.077(4) 0.069(4) 0.065(4) 0.006(3) 0.008(3) -0.008(3) N6 0.083(5) 0.062(4) 0.054(3) 0.004(3) -0.005(3) -0.002(3) N7 0.077(4) 0.055(3) 0.064(4) 0.003(3) -0.005(3) -0.010(3) N8 0.081(5) 0.093(5) 0.073(4) -0.010(4) 0.025(4) -0.002(4) N9 0.083(4) 0.054(3) 0.056(4) -0.004(3) 0.009(3) -0.005(3) N10 0.052(4) 0.059(3) 0.065(4) 0.006(3) 0.008(3) -0.001(3) N11 0.067(4) 0.066(4) 0.099(5) 0.025(3) 0.018(4) 0.008(3) N12 0.066(4) 0.085(4) 0.071(4) 0.001(3) -0.006(3) 0.013(3) N13 0.103(5) 0.054(4) 0.063(4) 0.006(3) -0.017(3) 0.001(3) N14 0.092(5) 0.047(3) 0.067(4) 0.000(3) 0.012(3) 0.002(3) N15 0.075(4) 0.046(3) 0.048(3) -0.005(3) 0.004(3) -0.008(3) N16 0.064(4) 0.051(3) 0.048(3) -0.001(3) -0.003(3) 0.000(3) N17 0.126(6) 0.062(4) 0.057(4) -0.014(3) -0.010(4) 0.017(4) N18 0.084(4) 0.054(3) 0.055(3) 0.005(3) 0.002(3) 0.011(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 Zn1 N10 1.931(5) . ? Zn1 N4 2.037(6) . ? Zn1 N18 2.045(5) . ? Zn1 N16 2.345(5) . ? Zn1 N6 2.379(6) . ? Zn2 N15 1.973(5) . ? Zn2 N7 2.019(6) . ? Zn2 N3 2.045(5) . ? Zn2 N1 2.235(6) . ? Zn2 N9 2.351(6) . ? Cl1 O3 1.228(8) . ? Cl1 O4 1.267(11) . ? Cl1 O1 1.326(16) . ? Cl1 O2 1.333(11) . ? C1 N1 1.341(9) . ? C1 C2 1.374(11) . ? C1 H1A 0.9300 . ? C2 C3 1.380(11) . ? C2 H2A 0.9300 . ? C3 N2 1.334(9) . ? C3 H3A 0.9300 . ? C4 N2 1.323(8) . ? C4 N1 1.353(8) . ? C4 N3 1.394(8) . ? C5 N4 1.293(8) . ? C5 N3 1.297(8) . ? C5 H5A 0.9300 . ? C6 N6 1.332(8) . ? C6 N5 1.340(8) . ? C6 N4 1.387(8) . ? C7 N5 1.338(9) . ? C7 C8 1.371(11) . ? C7 H7A 0.9300 . ? C8 C9 1.369(11) . ? C8 H8A 0.9300 . ? C9 N6 1.332(9) . ? C9 H9A 0.9300 . ? C10 N7 1.342(9) . ? C10 C11 1.418(11) . ? C10 H10A 0.9300 . ? C11 C12 1.376(13) . ? C11 H11A 0.9300 . ? C12 N8 1.338(10) . ? C12 H12A 0.9300 . ? C13 N8 1.341(9) . ? C13 N7 1.345(9) . ? C13 N9 1.381(8) . ? C14 N9 1.322(8) . ? C14 N10 1.329(8) . ? C14 H14A 0.9300 . ? C15 N11 1.328(9) . ? C15 N12 1.350(8) . ? C15 N10 1.383(8) . ? C16 N11 1.337(10) . ? C16 C17 1.357(11) . ? C16 H16A 0.9300 . ? C17 C18 1.374(12) . ? C17 H17A 0.9300 . ? C18 N12 1.372(10) . ? C18 H18A 0.9300 . ? C19 N13 1.334(9) . ? C19 C20 1.381(11) . ? C19 H19A 0.9300 . ? C20 C21 1.312(10) . ? C20 H20A 0.9300 . ? C21 N14 1.326(8) . ? C21 H21A 0.9300 . ? C22 N13 1.331(8) . ? C22 N14 1.336(8) . ? C22 N15 1.394(7) . ? C23 N15 1.305(7) . ? C23 N16 1.305(7) . ? C23 H23A 0.9300 . ? C24 N17 1.336(8) . ? C24 N18 1.363(8) . ? C24 N16 1.368(8) . ? C25 N17 1.330(9) . ? C25 C26 1.386(11) . ? C25 H25A 0.9300 . ? C26 C27 1.385(11) . ? C26 H26A 0.9300 . ? C27 N18 1.328(8) . ? C27 H27A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Zn1 N4 119.5(2) . . ? N10 Zn1 N18 120.6(2) . . ? N4 Zn1 N18 119.7(2) . . ? N10 Zn1 N16 111.6(2) . . ? N4 Zn1 N16 100.2(2) . . ? N18 Zn1 N16 61.13(19) . . ? N10 Zn1 N6 112.8(2) . . ? N4 Zn1 N6 60.4(2) . . ? N18 Zn1 N6 92.4(2) . . ? N16 Zn1 N6 135.5(2) . . ? N15 Zn2 N7 115.0(2) . . ? N15 Zn2 N3 119.4(2) . . ? N7 Zn2 N3 125.5(2) . . ? N15 Zn2 N1 113.4(2) . . ? N7 Zn2 N1 99.2(2) . . ? N3 Zn2 N1 62.9(2) . . ? N15 Zn2 N9 106.0(2) . . ? N7 Zn2 N9 60.6(2) . . ? N3 Zn2 N9 99.8(2) . . ? N1 Zn2 N9 140.57(18) . . ? O3 Cl1 O4 129.0(11) . . ? O3 Cl1 O1 99.2(10) . . ? O4 Cl1 O1 95.3(11) . . ? O3 Cl1 O2 114.2(10) . . ? O4 Cl1 O2 103.5(8) . . ? O1 Cl1 O2 114.1(13) . . ? N1 C1 C2 120.9(8) . . ? N1 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C1 C2 C3 118.1(7) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? N2 C3 C2 122.7(8) . . ? N2 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? N2 C4 N1 127.9(6) . . ? N2 C4 N3 123.0(6) . . ? N1 C4 N3 109.2(6) . . ? N4 C5 N3 124.1(7) . . ? N4 C5 H5A 118.0 . . ? N3 C5 H5A 118.0 . . ? N6 C6 N5 127.2(6) . . ? N6 C6 N4 111.1(6) . . ? N5 C6 N4 121.7(6) . . ? N5 C7 C8 123.1(8) . . ? N5 C7 H7A 118.5 . . ? C8 C7 H7A 118.5 . . ? C9 C8 C7 118.0(8) . . ? C9 C8 H8A 121.0 . . ? C7 C8 H8A 121.0 . . ? N6 C9 C8 120.8(8) . . ? N6 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? N7 C10 C11 119.6(8) . . ? N7 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 117.5(8) . . ? C12 C11 H11A 121.3 . . ? C10 C11 H11A 121.3 . . ? N8 C12 C11 123.3(9) . . ? N8 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N8 C13 N7 126.3(7) . . ? N8 C13 N9 124.5(7) . . ? N7 C13 N9 109.2(6) . . ? N9 C14 N10 121.1(6) . . ? N9 C14 H14A 119.4 . . ? N10 C14 H14A 119.4 . . ? N11 C15 N12 126.1(7) . . ? N11 C15 N10 121.8(7) . . ? N12 C15 N10 112.1(6) . . ? N11 C16 C17 121.5(8) . . ? N11 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C16 C17 C18 117.5(8) . . ? C16 C17 H17A 121.2 . . ? C18 C17 H17A 121.2 . . ? N12 C18 C17 123.2(9) . . ? N12 C18 H18A 118.4 . . ? C17 C18 H18A 118.4 . . ? N13 C19 C20 120.6(8) . . ? N13 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C21 C20 C19 117.3(7) . . ? C21 C20 H20A 121.4 . . ? C19 C20 H20A 121.4 . . ? C20 C21 N14 125.2(8) . . ? C20 C21 H21A 117.4 . . ? N14 C21 H21A 117.4 . . ? N13 C22 N14 125.7(6) . . ? N13 C22 N15 113.8(6) . . ? N14 C22 N15 120.3(6) . . ? N15 C23 N16 122.0(6) . . ? N15 C23 H23A 119.0 . . ? N16 C23 H23A 119.0 . . ? N17 C24 N18 123.9(6) . . ? N17 C24 N16 125.2(6) . . ? N18 C24 N16 110.7(6) . . ? N17 C25 C26 124.8(8) . . ? N17 C25 H25A 117.6 . . ? C26 C25 H25A 117.6 . . ? C27 C26 C25 116.1(7) . . ? C27 C26 H26A 121.9 . . ? C25 C26 H26A 121.9 . . ? N18 C27 C26 120.2(7) . . ? N18 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C1 N1 C4 115.6(6) . . ? C1 N1 Zn2 153.6(5) . . ? C4 N1 Zn2 90.4(4) . . ? C4 N2 C3 114.7(7) . . ? C5 N3 C4 120.6(6) . . ? C5 N3 Zn2 141.6(5) . . ? C4 N3 Zn2 97.5(4) . . ? C5 N4 C6 122.5(6) . . ? C5 N4 Zn1 136.7(5) . . ? C6 N4 Zn1 100.8(4) . . ? C7 N5 C6 114.1(7) . . ? C6 N6 C9 116.8(7) . . ? C6 N6 Zn1 87.3(4) . . ? C9 N6 Zn1 155.4(6) . . ? C10 N7 C13 117.8(7) . . ? C10 N7 Zn2 138.9(6) . . ? C13 N7 Zn2 103.0(4) . . ? C12 N8 C13 115.5(7) . . ? C14 N9 C13 119.2(6) . . ? C14 N9 Zn2 153.3(5) . . ? C13 N9 Zn2 87.1(4) . . ? C14 N10 C15 118.2(6) . . ? C14 N10 Zn1 123.4(5) . . ? C15 N10 Zn1 118.4(5) . . ? C15 N11 C16 117.9(7) . . ? C15 N12 C18 113.7(7) . . ? C22 N13 C19 116.7(7) . . ? C21 N14 C22 114.3(6) . . ? C23 N15 C22 120.7(5) . . ? C23 N15 Zn2 123.7(4) . . ? C22 N15 Zn2 115.6(4) . . ? C23 N16 C24 120.4(6) . . ? C23 N16 Zn1 151.5(4) . . ? C24 N16 Zn1 87.3(4) . . ? C25 N17 C24 115.3(6) . . ? C27 N18 C24 119.4(6) . . ? C27 N18 Zn1 139.9(5) . . ? C24 N18 Zn1 100.7(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.721 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.093 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 640644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H21 Cd2 N19 O3' _chemical_formula_weight 884.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3194(12) _cell_length_b 29.1565(19) _cell_length_c 12.6256(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.187(9) _cell_angle_gamma 90.00 _cell_volume 4155.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.24 _cell_measurement_theta_max 12.51 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8594 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8756 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7236 _reflns_number_gt 4798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0373P)^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 7236 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Cd1 Cd 0.72513(3) 0.091265(10) 0.20310(2) 0.06260(11) Uani 1 1 d . . . Cd2 Cd 0.82759(3) -0.036380(10) 0.27582(2) 0.06457(11) Uani 1 1 d . . . N1 N 0.3842(4) 0.05109(14) 0.0968(3) 0.0837(11) Uani 1 1 d . . . N2 N 0.5211(3) 0.11079(13) 0.1477(3) 0.0752(10) Uani 1 1 d . . . N3 N 0.5827(3) 0.03743(12) 0.1588(3) 0.0660(9) Uani 1 1 d . . . N4 N 0.6474(3) -0.03658(13) 0.1853(3) 0.0690(9) Uani 1 1 d . . . N5 N 0.5240(3) -0.09932(12) 0.1294(3) 0.0806(11) Uani 1 1 d . . . N6 N 0.7159(3) -0.10766(14) 0.2193(3) 0.0810(10) Uani 1 1 d . . . N7 N 0.8220(4) 0.14482(14) 0.5041(3) 0.0866(11) Uani 1 1 d . . . N8 N 0.7390(3) 0.15582(14) 0.3275(3) 0.0798(10) Uani 1 1 d . . . N9 N 0.7902(3) 0.08436(12) 0.3783(3) 0.0685(9) Uani 1 1 d . . . N10 N 0.8225(3) 0.00913(12) 0.4227(2) 0.0675(9) Uani 1 1 d . . . N11 N 0.8317(4) -0.01532(13) 0.6035(3) 0.0871(12) Uani 1 1 d . . . N12 N 0.8570(4) -0.06508(14) 0.4561(3) 0.0816(11) Uani 1 1 d . . . N13 N 1.0014(3) 0.11818(13) 0.0059(3) 0.0762(10) Uani 1 1 d . . . N14 N 0.8187(3) 0.14251(14) 0.0701(3) 0.0779(10) Uani 1 1 d . . . N15 N 0.8882(3) 0.07233(12) 0.1178(2) 0.0628(8) Uani 1 1 d . . . N16 N 0.9524(3) 0.00060(12) 0.1685(2) 0.0632(8) Uani 1 1 d . . . N17 N 1.1431(3) -0.02516(12) 0.1277(3) 0.0745(10) Uani 1 1 d . . . N18 N 1.0156(3) -0.06750(13) 0.2347(3) 0.0724(10) Uani 1 1 d . . . C1 C 0.4361(5) 0.14182(18) 0.1308(4) 0.0904(14) Uani 1 1 d . . . H1B H 0.4541 0.1727 0.1415 0.108 Uiso 1 1 calc R . . C2 C 0.3223(5) 0.1296(2) 0.0981(4) 0.1019(17) Uani 1 1 d . . . H2A H 0.2619 0.1512 0.0890 0.122 Uiso 1 1 calc R . . C3 C 0.3024(5) 0.0835(2) 0.0792(4) 0.0964(16) Uani 1 1 d . . . H3A H 0.2272 0.0745 0.0525 0.116 Uiso 1 1 calc R . . C4 C 0.4895(4) 0.06648(16) 0.1321(3) 0.0674(11) Uani 1 1 d . . . C5 C 0.5661(4) -0.00705(16) 0.1512(3) 0.0689(11) Uani 1 1 d . . . H5B H 0.4943 -0.0179 0.1207 0.083 Uiso 1 1 calc R . . C6 C 0.6247(4) -0.08332(16) 0.1761(3) 0.0691(11) Uani 1 1 d . . . C7 C 0.5152(5) -0.14468(19) 0.1249(5) 0.0980(16) Uani 1 1 d . . . H7B H 0.4473 -0.1577 0.0915 0.118 Uiso 1 1 calc R . . C8 C 0.6026(6) -0.17297(19) 0.1679(5) 0.1137(19) Uani 1 1 d . . . H8A H 0.5933 -0.2047 0.1655 0.136 Uiso 1 1 calc R . . C9 C 0.7040(5) -0.1537(2) 0.2146(4) 0.0995(16) Uani 1 1 d . . . H9A H 0.7649 -0.1724 0.2432 0.119 Uiso 1 1 calc R . . C10 C 0.7266(5) 0.2005(2) 0.3480(5) 0.1079(18) Uani 1 1 d . . . H10A H 0.6937 0.2197 0.2949 0.130 Uiso 1 1 calc R . . C11 C 0.7607(6) 0.21851(19) 0.4440(5) 0.1114(19) Uani 1 1 d . . . H11B H 0.7518 0.2496 0.4577 0.134 Uiso 1 1 calc R . . C12 C 0.8085(6) 0.1896(2) 0.5200(4) 0.1084(19) Uani 1 1 d . . . H12A H 0.8329 0.2017 0.5862 0.130 Uiso 1 1 calc R . . C13 C 0.7841(4) 0.12958(16) 0.4067(3) 0.0702(11) Uani 1 1 d . . . C14 C 0.8145(4) 0.05248(16) 0.4498(3) 0.0685(11) Uani 1 1 d . . . H14A H 0.8263 0.0607 0.5210 0.082 Uiso 1 1 calc R . . C15 C 0.8398(4) -0.02408(15) 0.4992(3) 0.0703(11) Uani 1 1 d . . . C16 C 0.8455(5) -0.0516(2) 0.6663(4) 0.1045(18) Uani 1 1 d . . . H16A H 0.8388 -0.0473 0.7386 0.125 Uiso 1 1 calc R . . C17 C 0.8689(6) -0.0949(2) 0.6317(5) 0.116(2) Uani 1 1 d . . . H17B H 0.8807 -0.1193 0.6787 0.139 Uiso 1 1 calc R . . C18 C 0.8742(5) -0.10063(18) 0.5231(5) 0.1031(17) Uani 1 1 d . . . H18A H 0.8898 -0.1295 0.4963 0.124 Uiso 1 1 calc R . . C19 C 0.8282(5) 0.18255(18) 0.0191(4) 0.0948(16) Uani 1 1 d . . . H19A H 0.7707 0.2050 0.0251 0.114 Uiso 1 1 calc R . . C20 C 0.9213(6) 0.19092(19) -0.0415(5) 0.1039(17) Uani 1 1 d . . . H20A H 0.9262 0.2182 -0.0792 0.125 Uiso 1 1 calc R . . C21 C 1.0068(5) 0.15791(19) -0.0449(4) 0.0914(14) Uani 1 1 d . . . H21A H 1.0715 0.1635 -0.0844 0.110 Uiso 1 1 calc R . . C22 C 0.9057(4) 0.11210(15) 0.0609(3) 0.0658(11) Uani 1 1 d . . . C23 C 0.9649(4) 0.03847(15) 0.1150(3) 0.0632(10) Uani 1 1 d . . . H23A H 1.0295 0.0416 0.0741 0.076 Uiso 1 1 calc R . . C24 C 1.0430(4) -0.03151(15) 0.1749(3) 0.0649(11) Uani 1 1 d . . . C25 C 1.2236(5) -0.0577(2) 0.1471(4) 0.0891(14) Uani 1 1 d . . . H25A H 1.2953 -0.0550 0.1162 0.107 Uiso 1 1 calc R . . C26 C 1.2070(5) -0.0949(2) 0.2101(4) 0.0932(15) Uani 1 1 d . . . H26A H 1.2665 -0.1166 0.2237 0.112 Uiso 1 1 calc R . . C27 C 1.0987(5) -0.09921(17) 0.2529(4) 0.0877(14) Uani 1 1 d . . . H27A H 1.0839 -0.1245 0.2947 0.105 Uiso 1 1 calc R . . N19 N 1.0857(5) 0.2324(2) 0.6086(5) 0.1096(16) Uani 1 1 d . . . O1 O 1.1622(7) 0.2097(2) 0.5742(5) 0.209(3) Uani 1 1 d . . . O2 O 1.0514(6) 0.26278(18) 0.5536(5) 0.174(2) Uani 1 1 d . . . O3 O 1.0482(5) 0.2210(2) 0.6908(5) 0.192(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.05749(19) 0.06772(19) 0.06148(18) -0.00306(14) -0.00326(13) -0.00174(16) Cd2 0.0641(2) 0.0670(2) 0.06237(18) -0.00216(14) 0.00286(14) 0.00109(16) N1 0.060(2) 0.096(3) 0.092(3) 0.018(2) -0.014(2) -0.012(2) N2 0.071(3) 0.071(2) 0.082(2) 0.0010(19) -0.004(2) -0.006(2) N3 0.056(2) 0.070(2) 0.071(2) -0.0011(17) -0.0054(17) -0.0079(19) N4 0.058(2) 0.079(2) 0.069(2) -0.0064(18) 0.0010(17) -0.005(2) N5 0.075(3) 0.065(2) 0.102(3) -0.008(2) 0.001(2) -0.006(2) N6 0.074(3) 0.082(3) 0.087(3) 0.003(2) 0.008(2) 0.000(2) N7 0.106(3) 0.078(3) 0.073(2) -0.008(2) -0.008(2) -0.005(2) N8 0.081(3) 0.087(3) 0.069(2) 0.007(2) -0.011(2) -0.008(2) N9 0.073(2) 0.073(2) 0.0590(19) -0.0003(19) -0.0010(17) -0.0104(19) N10 0.074(2) 0.068(2) 0.059(2) -0.0042(17) 0.0030(18) -0.0038(19) N11 0.115(3) 0.082(3) 0.063(2) 0.002(2) -0.009(2) -0.023(2) N12 0.087(3) 0.074(3) 0.083(3) -0.006(2) 0.005(2) -0.004(2) N13 0.067(3) 0.081(3) 0.079(2) 0.011(2) 0.001(2) -0.003(2) N14 0.069(3) 0.079(3) 0.084(2) -0.013(2) -0.0053(19) 0.000(2) N15 0.054(2) 0.073(2) 0.0614(19) -0.0010(17) 0.0032(16) 0.0012(19) N16 0.059(2) 0.075(2) 0.0553(18) -0.0005(17) 0.0045(16) 0.0019(19) N17 0.057(2) 0.084(3) 0.082(2) -0.0085(19) 0.005(2) 0.004(2) N18 0.081(3) 0.078(2) 0.058(2) -0.0008(18) -0.0035(18) 0.008(2) C1 0.085(4) 0.082(3) 0.104(4) 0.004(3) 0.007(3) 0.004(3) C2 0.077(4) 0.103(4) 0.124(4) 0.022(3) 0.000(3) 0.024(3) C3 0.060(3) 0.126(5) 0.102(4) 0.023(3) -0.010(3) -0.011(3) C4 0.057(3) 0.078(3) 0.067(2) 0.003(2) 0.002(2) -0.009(2) C5 0.063(3) 0.074(3) 0.069(3) -0.003(2) -0.002(2) -0.006(3) C6 0.058(3) 0.077(3) 0.072(3) 0.001(2) 0.003(2) 0.001(3) C7 0.078(4) 0.081(4) 0.135(5) -0.015(3) 0.008(3) -0.010(3) C8 0.103(5) 0.075(4) 0.166(6) 0.000(4) 0.028(4) -0.012(4) C9 0.086(4) 0.097(4) 0.116(4) 0.013(3) 0.014(3) 0.017(3) C10 0.123(5) 0.100(4) 0.099(4) 0.015(3) -0.005(4) 0.001(4) C11 0.153(6) 0.076(3) 0.106(4) -0.002(3) 0.011(4) 0.002(4) C12 0.150(6) 0.084(4) 0.089(4) -0.014(3) -0.006(4) -0.009(4) C13 0.065(3) 0.083(3) 0.063(3) -0.005(2) -0.001(2) -0.014(2) C14 0.065(3) 0.079(3) 0.060(2) -0.006(2) -0.001(2) -0.008(2) C15 0.063(3) 0.076(3) 0.071(3) -0.007(2) -0.008(2) -0.011(2) C16 0.134(5) 0.096(4) 0.079(3) 0.002(3) -0.026(3) -0.031(4) C17 0.145(6) 0.100(4) 0.098(4) 0.017(3) -0.025(4) -0.012(4) C18 0.107(4) 0.073(3) 0.129(5) -0.002(3) 0.002(4) 0.001(3) C19 0.094(4) 0.078(4) 0.110(4) -0.001(3) -0.011(3) 0.016(3) C20 0.110(5) 0.087(4) 0.113(4) 0.016(3) 0.001(4) -0.005(4) C21 0.082(4) 0.097(4) 0.096(3) 0.016(3) 0.005(3) -0.011(3) C22 0.058(3) 0.074(3) 0.064(2) -0.008(2) -0.003(2) 0.000(2) C23 0.054(3) 0.078(3) 0.058(2) -0.007(2) 0.0050(19) -0.002(2) C24 0.062(3) 0.076(3) 0.056(2) -0.012(2) -0.002(2) -0.001(3) C25 0.063(3) 0.104(4) 0.099(4) -0.016(3) 0.000(3) 0.001(3) C26 0.078(4) 0.098(4) 0.101(4) -0.015(3) -0.019(3) 0.016(3) C27 0.100(4) 0.084(3) 0.076(3) 0.002(2) -0.010(3) 0.008(3) N19 0.111(5) 0.087(4) 0.130(5) -0.014(3) 0.000(4) 0.014(3) O1 0.255(8) 0.194(6) 0.180(5) 0.020(4) 0.024(5) 0.093(6) O2 0.187(5) 0.103(3) 0.233(6) 0.007(4) 0.015(5) 0.033(4) O3 0.146(5) 0.301(8) 0.127(4) 0.015(5) 0.000(4) -0.061(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N15 2.272(3) . ? Cd1 N9 2.289(3) . ? Cd1 N3 2.290(3) . ? Cd1 N2 2.431(4) . ? Cd1 N8 2.449(4) . ? Cd1 N14 2.536(4) . ? Cd2 N4 2.264(4) . ? Cd2 N10 2.285(3) . ? Cd2 N16 2.297(3) . ? Cd2 N18 2.405(4) . ? Cd2 N12 2.425(4) . ? Cd2 N6 2.509(4) . ? N1 C4 1.321(5) . ? N1 C3 1.330(6) . ? N2 C1 1.327(6) . ? N2 C4 1.351(5) . ? N3 C5 1.313(5) . ? N3 C4 1.375(5) . ? N4 C5 1.310(5) . ? N4 C6 1.390(5) . ? N5 C7 1.327(6) . ? N5 C6 1.329(5) . ? N6 C6 1.336(5) . ? N6 C9 1.349(6) . ? N7 C12 1.332(6) . ? N7 C13 1.347(5) . ? N8 C13 1.331(5) . ? N8 C10 1.339(6) . ? N9 C14 1.311(5) . ? N9 C13 1.370(5) . ? N10 C14 1.314(5) . ? N10 C15 1.372(5) . ? N11 C16 1.323(6) . ? N11 C15 1.350(5) . ? N12 C15 1.334(5) . ? N12 C18 1.343(6) . ? N13 C21 1.328(6) . ? N13 C22 1.340(5) . ? N14 C22 1.337(5) . ? N14 C19 1.341(6) . ? N15 C23 1.317(5) . ? N15 C22 1.386(5) . ? N16 C23 1.307(5) . ? N16 C24 1.386(5) . ? N17 C25 1.325(6) . ? N17 C24 1.332(5) . ? N18 C27 1.327(6) . ? N18 C24 1.342(5) . ? C1 C2 1.370(7) . ? C2 C3 1.381(7) . ? C7 C8 1.369(8) . ? C8 C9 1.373(8) . ? C10 C11 1.351(7) . ? C11 C12 1.359(7) . ? C16 C17 1.369(7) . ? C17 C18 1.387(8) . ? C19 C20 1.368(7) . ? C20 C21 1.368(7) . ? C25 C26 1.368(7) . ? C26 C27 1.381(7) . ? N19 O2 1.175(6) . ? N19 O1 1.195(7) . ? N19 O3 1.197(7) . ? 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 N15 Cd1 N9 102.79(12) . . ? N15 Cd1 N3 107.43(12) . . ? N9 Cd1 N3 110.31(12) . . ? N15 Cd1 N2 135.09(12) . . ? N9 Cd1 N2 122.03(13) . . ? N3 Cd1 N2 56.85(12) . . ? N15 Cd1 N8 118.33(12) . . ? N9 Cd1 N8 56.41(12) . . ? N3 Cd1 N8 133.98(13) . . ? N2 Cd1 N8 91.11(13) . . ? N15 Cd1 N14 55.70(12) . . ? N9 Cd1 N14 124.83(12) . . ? N3 Cd1 N14 124.24(11) . . ? N2 Cd1 N14 96.06(12) . . ? N8 Cd1 N14 87.79(12) . . ? N4 Cd2 N10 109.65(12) . . ? N4 Cd2 N16 105.90(12) . . ? N10 Cd2 N16 105.02(12) . . ? N4 Cd2 N18 131.98(12) . . ? N10 Cd2 N18 118.00(12) . . ? N16 Cd2 N18 57.15(12) . . ? N4 Cd2 N12 121.98(13) . . ? N10 Cd2 N12 56.52(12) . . ? N16 Cd2 N12 131.88(12) . . ? N18 Cd2 N12 90.55(12) . . ? N4 Cd2 N6 55.78(13) . . ? N10 Cd2 N6 132.05(12) . . ? N16 Cd2 N6 122.71(11) . . ? N18 Cd2 N6 93.54(13) . . ? N12 Cd2 N6 90.72(13) . . ? C4 N1 C3 114.5(4) . . ? C1 N2 C4 116.6(4) . . ? C1 N2 Cd1 150.3(3) . . ? C4 N2 Cd1 93.1(3) . . ? C5 N3 C4 119.2(4) . . ? C5 N3 Cd1 142.1(3) . . ? C4 N3 Cd1 98.7(3) . . ? C5 N4 C6 119.7(4) . . ? C5 N4 Cd2 138.6(3) . . ? C6 N4 Cd2 101.5(3) . . ? C7 N5 C6 115.4(4) . . ? C6 N6 C9 116.1(4) . . ? C6 N6 Cd2 92.0(3) . . ? C9 N6 Cd2 151.9(4) . . ? C12 N7 C13 115.4(4) . . ? C13 N8 C10 117.0(4) . . ? C13 N8 Cd1 92.5(3) . . ? C10 N8 Cd1 150.5(3) . . ? C14 N9 C13 120.9(4) . . ? C14 N9 Cd1 139.9(3) . . ? C13 N9 Cd1 98.6(3) . . ? C14 N10 C15 120.3(3) . . ? C14 N10 Cd2 140.9(3) . . ? C15 N10 Cd2 98.7(3) . . ? C16 N11 C15 114.8(4) . . ? C15 N12 C18 116.9(4) . . ? C15 N12 Cd2 93.4(3) . . ? C18 N12 Cd2 149.5(4) . . ? C21 N13 C22 115.7(4) . . ? C22 N14 C19 116.7(4) . . ? C22 N14 Cd1 90.7(3) . . ? C19 N14 Cd1 152.0(4) . . ? C23 N15 C22 119.6(4) . . ? C23 N15 Cd1 139.0(3) . . ? C22 N15 Cd1 101.2(3) . . ? C23 N16 C24 119.5(4) . . ? C23 N16 Cd2 142.7(3) . . ? C24 N16 Cd2 97.6(3) . . ? C25 N17 C24 114.5(4) . . ? C27 N18 C24 116.9(4) . . ? C27 N18 Cd2 148.5(3) . . ? C24 N18 Cd2 94.1(3) . . ? N2 C1 C2 121.7(5) . . ? C1 C2 C3 116.3(5) . . ? N1 C3 C2 124.0(5) . . ? N1 C4 N2 126.7(4) . . ? N1 C4 N3 122.0(4) . . ? N2 C4 N3 111.3(4) . . ? N4 C5 N3 122.2(4) . . ? N5 C6 N6 127.3(4) . . ? N5 C6 N4 121.9(4) . . ? N6 C6 N4 110.7(4) . . ? N5 C7 C8 122.2(5) . . ? C7 C8 C9 118.7(5) . . ? N6 C9 C8 120.2(5) . . ? N8 C10 C11 121.6(5) . . ? C10 C11 C12 117.8(5) . . ? N7 C12 C11 123.0(5) . . ? N8 C13 N7 125.1(4) . . ? N8 C13 N9 112.3(4) . . ? N7 C13 N9 122.5(4) . . ? N9 C14 N10 121.2(4) . . ? N12 C15 N11 126.2(4) . . ? N12 C15 N10 111.3(4) . . ? N11 C15 N10 122.5(4) . . ? N11 C16 C17 124.3(5) . . ? C16 C17 C18 116.7(5) . . ? N12 C18 C17 121.0(5) . . ? N14 C19 C20 121.1(5) . . ? C19 C20 C21 117.9(5) . . ? N13 C21 C20 122.8(5) . . ? N14 C22 N13 125.9(4) . . ? N14 C22 N15 112.1(4) . . ? N13 C22 N15 122.1(4) . . ? N16 C23 N15 121.5(4) . . ? N17 C24 N18 126.8(4) . . ? N17 C24 N16 122.0(4) . . ? N18 C24 N16 111.2(4) . . ? N17 C25 C26 123.7(5) . . ? C25 C26 C27 117.5(5) . . ? N18 C27 C26 120.5(5) . . ? O2 N19 O1 114.8(7) . . ? O2 N19 O3 126.8(8) . . ? O1 N19 O3 118.3(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.380 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.060 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 640645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H21 Cd2 Cl N18 O4' _chemical_formula_weight 921.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.002(3) _cell_length_b 12.6232(16) _cell_length_c 32.299(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.264(8) _cell_angle_gamma 90.00 _cell_volume 9119.9(18) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.16 _cell_measurement_theta_max 12.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7746 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9324 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7908 _reflns_number_gt 3856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7908 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Cd1 Cd 0.326854(19) 0.03609(4) 0.041390(13) 0.07568(17) Uani 1 1 d . . . Cd2 Cd 0.33775(2) -0.03741(4) -0.072584(14) 0.08413(18) Uani 1 1 d . . . N1 N 0.3422(2) 0.3673(4) 0.03461(16) 0.0782(13) Uani 1 1 d . . . N2 N 0.3224(2) 0.2242(4) 0.07585(19) 0.0855(14) Uani 1 1 d . . . N3 N 0.32567(19) 0.1899(4) 0.00793(16) 0.0723(12) Uani 1 1 d . . . N4 N 0.3272(2) 0.1458(4) -0.05986(17) 0.0743(12) Uani 1 1 d . . . N5 N 0.3214(3) 0.2762(4) -0.11504(18) 0.0984(17) Uani 1 1 d . . . N6 N 0.3295(2) 0.0926(4) -0.12536(19) 0.0866(14) Uani 1 1 d . . . N7 N 0.1710(3) -0.1335(4) 0.02032(19) 0.1001(16) Uani 1 1 d . . . N8 N 0.2488(2) -0.0212(4) 0.06594(18) 0.0786(13) Uani 1 1 d . . . N9 N 0.2546(2) -0.0799(4) 0.00214(17) 0.0721(12) Uani 1 1 d . . . N10 N 0.2607(2) -0.1265(4) -0.06445(18) 0.0806(13) Uani 1 1 d . . . N11 N 0.1927(3) -0.2460(5) -0.1141(2) 0.1067(18) Uani 1 1 d . . . N12 N 0.2719(3) -0.1630(4) -0.1296(2) 0.0983(16) Uani 1 1 d . . . N13 N 0.4990(3) -0.0713(5) 0.1141(2) 0.1058(18) Uani 1 1 d . . . N14 N 0.4074(2) 0.0108(4) 0.10892(18) 0.0797(13) Uani 1 1 d . . . N15 N 0.4176(2) -0.0424(4) 0.04617(18) 0.0789(13) Uani 1 1 d . . . N16 N 0.4223(2) -0.0908(4) -0.02083(18) 0.0781(13) Uani 1 1 d . . . N17 N 0.5012(2) -0.2020(5) -0.0228(2) 0.1000(17) Uani 1 1 d . . . N18 N 0.4225(3) -0.1354(4) -0.0875(2) 0.1000(16) Uani 1 1 d . . . C1 C 0.3291(3) 0.2901(8) 0.1099(2) 0.111(2) Uani 1 1 d . . . H1B H 0.3249 0.2643 0.1355 0.134 Uiso 1 1 calc R . . C2 C 0.3423(3) 0.3962(7) 0.1073(3) 0.106(2) Uani 1 1 d . . . H2A H 0.3462 0.4428 0.1305 0.127 Uiso 1 1 calc R . . C3 C 0.3494(3) 0.4300(5) 0.0686(2) 0.0879(19) Uani 1 1 d . . . H3A H 0.3597 0.5004 0.0667 0.106 Uiso 1 1 calc R . . C4 C 0.3292(2) 0.2668(5) 0.0396(2) 0.0726(16) Uani 1 1 d . . . C5 C 0.3273(2) 0.2160(5) -0.0308(2) 0.0722(15) Uani 1 1 d . . . H5B H 0.3285 0.2874 -0.0376 0.087 Uiso 1 1 calc R . . C6 C 0.3257(3) 0.1760(5) -0.1011(2) 0.0767(16) Uani 1 1 d . . . C7 C 0.3210(3) 0.2910(6) -0.1555(3) 0.116(2) Uani 1 1 d . . . H7B H 0.3183 0.3600 -0.1662 0.139 Uiso 1 1 calc R . . C8 C 0.3244(4) 0.2099(8) -0.1825(3) 0.127(3) Uani 1 1 d . . . H8A H 0.3245 0.2219 -0.2109 0.153 Uiso 1 1 calc R . . C9 C 0.3275(4) 0.1106(8) -0.1655(3) 0.122(3) Uani 1 1 d . . . H9A H 0.3282 0.0532 -0.1834 0.146 Uiso 1 1 calc R . . C10 C 0.2213(4) -0.0144(5) 0.0950(2) 0.103(2) Uani 1 1 d . . . H10A H 0.2382 0.0263 0.1205 0.124 Uiso 1 1 calc R . . C11 C 0.1686(4) -0.0667(7) 0.0879(3) 0.118(3) Uani 1 1 d . . . H11B H 0.1494 -0.0627 0.1083 0.142 Uiso 1 1 calc R . . C12 C 0.1456(4) -0.1237(7) 0.0507(4) 0.123(3) Uani 1 1 d . . . H12A H 0.1096 -0.1587 0.0456 0.147 Uiso 1 1 calc R . . C13 C 0.2232(3) -0.0806(5) 0.0303(2) 0.0761(16) Uani 1 1 d . . . C14 C 0.2351(3) -0.1351(4) -0.0356(2) 0.0741(15) Uani 1 1 d . . . H14A H 0.2026 -0.1804 -0.0413 0.089 Uiso 1 1 calc R . . C15 C 0.2395(3) -0.1823(5) -0.1038(2) 0.0881(18) Uani 1 1 d . . . C16 C 0.1775(4) -0.2982(6) -0.1526(3) 0.132(3) Uani 1 1 d . . . H16A H 0.1455 -0.3452 -0.1608 0.159 Uiso 1 1 calc R . . C17 C 0.2093(5) -0.2824(7) -0.1804(3) 0.146(4) Uani 1 1 d . . . H17B H 0.1987 -0.3192 -0.2071 0.175 Uiso 1 1 calc R . . C18 C 0.2550(5) -0.2147(7) -0.1690(3) 0.128(3) Uani 1 1 d . . . H18A H 0.2754 -0.2028 -0.1882 0.154 Uiso 1 1 calc R . . C19 C 0.4281(4) 0.0255(6) 0.1521(3) 0.108(2) Uani 1 1 d . . . H19A H 0.4039 0.0582 0.1652 0.130 Uiso 1 1 calc R . . C20 C 0.4844(4) -0.0063(7) 0.1782(3) 0.131(3) Uani 1 1 d . . . H20A H 0.4995 0.0049 0.2087 0.157 Uiso 1 1 calc R . . C21 C 0.5170(4) -0.0552(7) 0.1570(3) 0.130(3) Uani 1 1 d . . . H21A H 0.5550 -0.0791 0.1743 0.156 Uiso 1 1 calc R . . C22 C 0.4442(3) -0.0356(5) 0.0914(2) 0.0781(16) Uani 1 1 d . . . C23 C 0.4456(3) -0.0861(4) 0.0227(3) 0.0787(17) Uani 1 1 d . . . H23A H 0.4833 -0.1149 0.0373 0.094 Uiso 1 1 calc R . . C24 C 0.4521(3) -0.1444(5) -0.0431(2) 0.0815(17) Uani 1 1 d . . . C25 C 0.5220(3) -0.2544(7) -0.0496(4) 0.122(3) Uani 1 1 d . . . H25A H 0.5554 -0.2975 -0.0372 0.147 Uiso 1 1 calc R . . C26 C 0.4958(5) -0.2476(7) -0.0957(4) 0.132(3) Uani 1 1 d . . . H26A H 0.5121 -0.2827 -0.1139 0.158 Uiso 1 1 calc R . . C27 C 0.4452(4) -0.1870(7) -0.1132(3) 0.118(2) Uani 1 1 d . . . H27A H 0.4264 -0.1822 -0.1439 0.142 Uiso 1 1 calc R . . Cl1 Cl 0.33842(10) -0.08438(17) -0.26370(6) 0.0985(5) Uani 1 1 d . . . O1 O 0.3519(6) -0.1353(6) -0.2266(3) 0.281(6) Uani 1 1 d . . . O2 O 0.3296(4) -0.1382(7) -0.3004(2) 0.233(4) Uani 1 1 d . . . O3 O 0.3732(4) 0.0047(7) -0.2585(2) 0.200(3) Uani 1 1 d . . . O4 O 0.2832(4) -0.0409(10) -0.2691(4) 0.292(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 Cd1 0.0776(3) 0.0755(3) 0.0741(3) -0.0001(2) 0.0276(2) 0.0093(2) Cd2 0.0979(4) 0.0757(3) 0.0812(3) -0.0022(3) 0.0355(3) 0.0161(3) N1 0.083(3) 0.062(3) 0.078(3) -0.001(3) 0.016(3) 0.019(3) N2 0.081(3) 0.092(4) 0.076(3) 0.004(3) 0.020(3) 0.016(3) N3 0.072(3) 0.070(3) 0.073(3) -0.002(3) 0.023(3) 0.008(2) N4 0.085(3) 0.064(3) 0.072(3) 0.001(3) 0.026(3) 0.011(3) N5 0.143(5) 0.076(4) 0.080(4) 0.009(3) 0.045(3) 0.026(3) N6 0.100(4) 0.077(4) 0.083(4) -0.010(3) 0.034(3) 0.016(3) N7 0.120(5) 0.079(4) 0.114(4) -0.003(3) 0.058(4) -0.009(4) N8 0.088(3) 0.067(3) 0.078(3) -0.002(3) 0.026(3) 0.006(3) N9 0.075(3) 0.065(3) 0.075(3) 0.006(3) 0.026(3) 0.007(2) N10 0.086(3) 0.071(3) 0.077(3) -0.006(3) 0.020(3) 0.004(3) N11 0.130(5) 0.087(4) 0.092(4) -0.004(4) 0.025(4) -0.015(4) N12 0.127(5) 0.084(4) 0.087(4) 0.000(3) 0.042(4) 0.001(3) N13 0.082(4) 0.126(5) 0.094(4) -0.003(4) 0.014(3) 0.020(4) N14 0.081(3) 0.079(3) 0.082(4) -0.002(3) 0.032(3) 0.001(3) N15 0.067(3) 0.076(3) 0.094(4) -0.001(3) 0.030(3) 0.004(3) N16 0.094(4) 0.068(3) 0.078(3) -0.001(3) 0.038(3) 0.011(3) N17 0.072(4) 0.110(4) 0.125(5) -0.033(4) 0.044(4) -0.001(3) N18 0.117(5) 0.080(4) 0.115(5) -0.009(4) 0.058(4) 0.002(3) C1 0.090(5) 0.158(8) 0.086(5) -0.001(6) 0.032(4) 0.019(5) C2 0.113(6) 0.108(6) 0.085(5) -0.020(5) 0.020(4) 0.032(5) C3 0.081(4) 0.076(4) 0.095(5) -0.005(4) 0.017(4) 0.021(3) C4 0.071(4) 0.081(4) 0.061(4) 0.009(4) 0.017(3) 0.020(3) C5 0.073(4) 0.061(4) 0.078(4) 0.005(4) 0.022(3) 0.008(3) C6 0.080(4) 0.073(4) 0.074(4) -0.003(4) 0.025(3) 0.006(3) C7 0.152(7) 0.103(6) 0.091(5) 0.024(5) 0.041(5) 0.021(5) C8 0.180(8) 0.128(7) 0.089(5) -0.003(6) 0.067(5) 0.021(6) C9 0.147(7) 0.109(7) 0.105(6) -0.033(6) 0.040(5) 0.025(6) C10 0.150(7) 0.076(5) 0.100(5) -0.001(4) 0.065(5) 0.021(5) C11 0.144(8) 0.104(6) 0.138(7) 0.003(6) 0.090(6) -0.012(5) C12 0.142(7) 0.093(6) 0.158(8) 0.017(6) 0.085(7) -0.015(5) C13 0.088(5) 0.052(3) 0.091(5) 0.021(4) 0.036(4) 0.012(3) C14 0.077(4) 0.061(4) 0.079(4) 0.003(3) 0.022(4) 0.008(3) C15 0.105(5) 0.056(4) 0.093(5) 0.008(4) 0.023(5) 0.013(4) C16 0.187(9) 0.093(6) 0.100(6) -0.007(5) 0.032(6) -0.028(6) C17 0.259(12) 0.101(6) 0.074(5) -0.016(5) 0.055(7) -0.012(7) C18 0.197(9) 0.087(6) 0.099(6) -0.007(5) 0.053(6) -0.002(6) C19 0.108(6) 0.117(6) 0.109(6) -0.006(5) 0.052(5) -0.005(5) C20 0.125(7) 0.179(9) 0.076(5) -0.004(5) 0.023(5) 0.002(7) C21 0.092(5) 0.167(8) 0.109(7) -0.007(6) 0.010(5) 0.019(6) C22 0.070(4) 0.072(4) 0.090(4) -0.006(4) 0.027(4) -0.008(4) C23 0.064(4) 0.060(4) 0.114(6) 0.003(4) 0.034(4) 0.001(3) C24 0.086(5) 0.067(4) 0.096(5) -0.011(4) 0.038(4) -0.018(4) C25 0.084(5) 0.126(7) 0.168(9) -0.036(7) 0.058(6) -0.001(4) C26 0.154(8) 0.128(7) 0.150(8) -0.031(7) 0.101(7) -0.005(7) C27 0.147(8) 0.101(6) 0.120(6) -0.008(5) 0.066(6) -0.002(6) Cl1 0.1196(15) 0.1068(13) 0.0738(11) -0.0032(11) 0.0408(10) 0.0017(13) O1 0.523(18) 0.182(7) 0.137(6) 0.065(6) 0.119(8) 0.027(9) O2 0.305(9) 0.291(10) 0.156(5) -0.109(7) 0.146(6) -0.108(8) O3 0.229(8) 0.194(7) 0.143(5) 0.000(5) 0.029(5) -0.081(7) O4 0.194(9) 0.384(15) 0.314(13) -0.115(11) 0.112(8) 0.026(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 Cd1 N3 2.217(5) . ? Cd1 N9 2.272(5) . ? Cd1 N15 2.346(5) . ? Cd1 N14 2.354(5) . ? Cd1 N8 2.396(5) . ? Cd1 N2 2.641(6) . ? Cd2 N16 2.215(5) . ? Cd2 N10 2.260(5) . ? Cd2 N6 2.322(6) . ? Cd2 N4 2.378(5) . ? Cd2 N12 2.508(6) . ? Cd2 N18 2.572(6) . ? N1 C3 1.314(7) . ? N1 C4 1.330(7) . ? N2 C1 1.340(9) . ? N2 C4 1.350(7) . ? N3 C5 1.307(7) . ? N3 C4 1.391(7) . ? N4 C5 1.291(7) . ? N4 C6 1.375(7) . ? N5 C7 1.317(8) . ? N5 C6 1.334(7) . ? N6 C9 1.301(9) . ? N6 C6 1.334(7) . ? N7 C12 1.336(9) . ? N7 C13 1.350(7) . ? N8 C13 1.324(7) . ? N8 C10 1.332(8) . ? N9 C14 1.333(7) . ? N9 C13 1.377(7) . ? N10 C14 1.293(7) . ? N10 C15 1.378(8) . ? N11 C15 1.323(8) . ? N11 C16 1.337(9) . ? N12 C15 1.354(8) . ? N12 C18 1.354(9) . ? N13 C21 1.309(9) . ? N13 C22 1.331(7) . ? N14 C19 1.313(8) . ? N14 C22 1.342(7) . ? N15 C23 1.304(7) . ? N15 C22 1.368(7) . ? N16 C23 1.313(7) . ? N16 C24 1.363(7) . ? N17 C25 1.325(9) . ? N17 C24 1.336(8) . ? N18 C27 1.318(9) . ? N18 C24 1.354(8) . ? C1 C2 1.386(10) . ? C2 C3 1.386(9) . ? C7 C8 1.367(10) . ? C8 C9 1.360(11) . ? C10 C11 1.372(10) . ? C11 C12 1.335(10) . ? C16 C17 1.387(11) . ? C17 C18 1.333(11) . ? C19 C20 1.368(10) . ? C20 C21 1.362(10) . ? C25 C26 1.392(10) . ? C26 C27 1.373(10) . ? Cl1 O1 1.294(7) . ? Cl1 O2 1.315(6) . ? Cl1 O3 1.374(7) . ? Cl1 O4 1.385(9) . ? 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 Cd1 N9 114.82(16) . . ? N3 Cd1 N15 104.45(16) . . ? N9 Cd1 N15 105.49(17) . . ? N3 Cd1 N14 115.57(16) . . ? N9 Cd1 N14 129.35(16) . . ? N15 Cd1 N14 56.66(18) . . ? N3 Cd1 N8 123.53(16) . . ? N9 Cd1 N8 57.31(17) . . ? N15 Cd1 N8 132.01(16) . . ? N14 Cd1 N8 97.51(17) . . ? N3 Cd1 N2 54.74(17) . . ? N9 Cd1 N2 132.47(15) . . ? N15 Cd1 N2 122.02(16) . . ? N14 Cd1 N2 82.91(16) . . ? N8 Cd1 N2 88.63(17) . . ? N16 Cd2 N10 109.02(17) . . ? N16 Cd2 N6 125.42(18) . . ? N10 Cd2 N6 125.54(17) . . ? N16 Cd2 N4 106.93(17) . . ? N10 Cd2 N4 108.70(17) . . ? N6 Cd2 N4 56.88(18) . . ? N16 Cd2 N12 121.51(18) . . ? N10 Cd2 N12 56.42(19) . . ? N6 Cd2 N12 92.54(19) . . ? N4 Cd2 N12 131.56(16) . . ? N16 Cd2 N18 54.83(19) . . ? N10 Cd2 N18 121.27(17) . . ? N6 Cd2 N18 93.75(18) . . ? N4 Cd2 N18 129.88(16) . . ? N12 Cd2 N18 83.6(2) . . ? C3 N1 C4 116.0(6) . . ? C1 N2 C4 116.5(6) . . ? C1 N2 Cd1 153.2(5) . . ? C4 N2 Cd1 87.5(4) . . ? C5 N3 C4 120.8(5) . . ? C5 N3 Cd1 133.5(4) . . ? C4 N3 Cd1 105.4(4) . . ? C5 N4 C6 120.5(5) . . ? C5 N4 Cd2 145.2(4) . . ? C6 N4 Cd2 94.0(4) . . ? C7 N5 C6 116.2(6) . . ? C9 N6 C6 117.4(6) . . ? C9 N6 Cd2 144.9(6) . . ? C6 N6 Cd2 97.6(4) . . ? C12 N7 C13 114.2(7) . . ? C13 N8 C10 117.2(6) . . ? C13 N8 Cd1 93.2(4) . . ? C10 N8 Cd1 149.4(5) . . ? C14 N9 C13 120.4(5) . . ? C14 N9 Cd1 142.3(4) . . ? C13 N9 Cd1 97.2(4) . . ? C14 N10 C15 120.6(6) . . ? C14 N10 Cd2 138.4(4) . . ? C15 N10 Cd2 101.0(5) . . ? C15 N11 C16 117.0(7) . . ? C15 N12 C18 116.7(7) . . ? C15 N12 Cd2 90.6(4) . . ? C18 N12 Cd2 152.7(6) . . ? C21 N13 C22 114.4(6) . . ? C19 N14 C22 117.2(6) . . ? C19 N14 Cd1 146.3(5) . . ? C22 N14 Cd1 96.5(4) . . ? C23 N15 C22 120.5(6) . . ? C23 N15 Cd1 143.4(4) . . ? C22 N15 Cd1 96.1(4) . . ? C23 N16 C24 119.1(6) . . ? C23 N16 Cd2 135.4(4) . . ? C24 N16 Cd2 105.4(4) . . ? C25 N17 C24 115.2(7) . . ? C27 N18 C24 116.7(7) . . ? C27 N18 Cd2 153.0(6) . . ? C24 N18 Cd2 89.4(4) . . ? N2 C1 C2 120.8(7) . . ? C1 C2 C3 117.2(7) . . ? N1 C3 C2 123.0(7) . . ? N1 C4 N2 126.3(6) . . ? N1 C4 N3 122.0(6) . . ? N2 C4 N3 111.4(6) . . ? N4 C5 N3 122.0(5) . . ? N5 C6 N6 124.3(6) . . ? N5 C6 N4 124.2(6) . . ? N6 C6 N4 111.5(6) . . ? N5 C7 C8 123.1(7) . . ? C9 C8 C7 116.1(7) . . ? N6 C9 C8 122.8(7) . . ? N8 C10 C11 120.9(7) . . ? C12 C11 C10 117.7(8) . . ? C11 C12 N7 124.1(8) . . ? N8 C13 N7 125.9(6) . . ? N8 C13 N9 112.2(6) . . ? N7 C13 N9 121.9(6) . . ? N10 C14 N9 121.0(6) . . ? N11 C15 N12 125.4(7) . . ? N11 C15 N10 122.6(7) . . ? N12 C15 N10 112.0(7) . . ? N11 C16 C17 120.2(8) . . ? C18 C17 C16 120.3(8) . . ? C17 C18 N12 120.3(8) . . ? N14 C19 C20 121.4(7) . . ? C21 C20 C19 116.3(7) . . ? N13 C21 C20 124.9(7) . . ? N13 C22 N14 125.7(6) . . ? N13 C22 N15 123.5(6) . . ? N14 C22 N15 110.8(6) . . ? N15 C23 N16 122.2(6) . . ? N17 C24 N18 126.5(6) . . ? N17 C24 N16 123.3(6) . . ? N18 C24 N16 110.1(7) . . ? N17 C25 C26 122.5(8) . . ? C27 C26 C25 117.6(8) . . ? N18 C27 C26 121.4(8) . . ? O1 Cl1 O2 118.9(6) . . ? O1 Cl1 O3 110.9(6) . . ? O2 Cl1 O3 115.1(5) . . ? O1 Cl1 O4 102.8(7) . . ? O2 Cl1 O4 104.9(6) . . ? O3 Cl1 O4 101.6(7) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.561 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.071 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 640646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 Cl2 Hg2 N12' _chemical_formula_weight 870.49 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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.2507(17) _cell_length_b 15.775(2) _cell_length_c 10.3758(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2332.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 13.02 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 13.412 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8955 _exptl_absorpt_correction_T_max 0.9869 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2784 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2406 _reflns_number_gt 1865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0218P)^2^+6.3902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(19) _refine_ls_number_reflns 2406 _refine_ls_number_parameters 308 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.26717(4) 0.94594(3) 0.04323(5) 0.0525(2) Uani 1 1 d . . . Hg2 Hg 0.26753(4) 1.15837(3) 0.12967(7) 0.0516(2) Uani 1 1 d . . . Cl1 Cl 0.4041(3) 0.9732(3) -0.0682(7) 0.0762(17) Uani 1 1 d . . . Cl2 Cl 0.4117(3) 1.1334(3) 0.2234(8) 0.0815(18) Uani 1 1 d . . . N1 N 0.2053(9) 0.7794(7) 0.116(2) 0.063(4) Uani 1 1 d . . . N2 N 0.1259(10) 0.7945(10) 0.3145(19) 0.058(5) Uani 1 1 d . . . N3 N 0.1879(9) 0.9105(8) 0.2013(16) 0.045(4) Uani 1 1 d . . . N4 N 0.1751(10) 1.0484(8) 0.2687(14) 0.047(3) Uani 1 1 d . . . N5 N 0.1610(12) 1.1869(10) 0.3144(18) 0.055(5) Uani 1 1 d . . . N6 N 0.0829(10) 1.0889(8) 0.4506(18) 0.058(4) Uani 1 1 d . . . N7 N 0.1137(9) 1.3108(9) -0.1334(18) 0.057(4) Uani 1 1 d . . . N8 N 0.2005(10) 1.3261(8) 0.060(2) 0.066(4) Uani 1 1 d . . . N9 N 0.1768(11) 1.1943(9) -0.0195(19) 0.053(4) Uani 1 1 d . . . N10 N 0.1620(10) 1.0567(7) -0.0811(13) 0.039(4) Uani 1 1 d . . . N11 N 0.0663(9) 1.0152(8) -0.2635(16) 0.049(3) Uani 1 1 d . . . N12 N 0.1572(12) 0.9165(11) -0.1374(16) 0.050(5) Uani 1 1 d . . . C1 C 0.1703(11) 0.8228(10) 0.213(2) 0.047(5) Uani 1 1 d . . . C2 C 0.1902(12) 0.6955(10) 0.126(3) 0.068(5) Uani 1 1 d . . . H2B H 0.2131 0.6611 0.0603 0.081 Uiso 1 1 calc R . . C3 C 0.1460(13) 0.6589(12) 0.220(3) 0.074(8) Uani 1 1 d . . . H3A H 0.1370 0.6005 0.2219 0.089 Uiso 1 1 calc R . . C4 C 0.1123(11) 0.7115(11) 0.320(2) 0.055(6) Uani 1 1 d . . . H4A H 0.0804 0.6879 0.3893 0.065 Uiso 1 1 calc R . . C5 C 0.1550(13) 0.9672(11) 0.285(2) 0.049(5) Uani 1 1 d . . . H5A H 0.1186 0.9499 0.3550 0.059 Uiso 1 1 calc R . . C6 C 0.1378(13) 1.1066(13) 0.351(2) 0.050(5) Uani 1 1 d . . . C7 C 0.0466(13) 1.1512(11) 0.515(2) 0.068(6) Uani 1 1 d . . . H7B H 0.0082 1.1396 0.5850 0.081 Uiso 1 1 calc R . . C8 C 0.0640(12) 1.2365(11) 0.480(2) 0.067(6) Uani 1 1 d . . . H8B H 0.0360 1.2810 0.5244 0.081 Uiso 1 1 calc R . . C9 C 0.1227(12) 1.2510(12) 0.381(2) 0.065(6) Uani 1 1 d . . . H9A H 0.1369 1.3065 0.3579 0.078 Uiso 1 1 calc R . . C10 C 0.1616(11) 1.2816(10) -0.0326(19) 0.044(4) Uani 1 1 d . . . C11 C 0.1030(14) 1.3949(12) -0.136(3) 0.077(7) Uani 1 1 d . . . H11B H 0.0711 1.4194 -0.2045 0.092 Uiso 1 1 calc R . . C12 C 0.1375(14) 1.4464(10) -0.041(3) 0.077(8) Uani 1 1 d . . . H12A H 0.1281 1.5047 -0.0435 0.092 Uiso 1 1 calc R . . C13 C 0.1860(12) 1.4101(9) 0.058(3) 0.069(6) Uani 1 1 d . . . H13A H 0.2091 1.4438 0.1248 0.083 Uiso 1 1 calc R . . C14 C 0.1407(13) 1.1372(11) -0.097(2) 0.047(5) Uani 1 1 d . . . H14A H 0.1002 1.1535 -0.1627 0.056 Uiso 1 1 calc R . . C15 C 0.1243(11) 0.9964(10) -0.1686(19) 0.036(4) Uani 1 1 d . . . C16 C 0.0402(11) 0.9496(8) -0.338(2) 0.052(5) Uani 1 1 d . . . H16A H 0.0011 0.9599 -0.4083 0.063 Uiso 1 1 calc R . . C17 C 0.0690(11) 0.8690(9) -0.315(2) 0.058(5) Uani 1 1 d . . . H17A H 0.0504 0.8245 -0.3680 0.069 Uiso 1 1 calc R . . C18 C 0.1259(12) 0.8552(11) -0.211(2) 0.055(5) Uani 1 1 d . . . H18A H 0.1434 0.7998 -0.1923 0.066 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 0.0590(3) 0.0366(3) 0.0620(5) -0.0019(4) 0.0070(11) -0.0004(3) Hg2 0.0591(3) 0.0374(3) 0.0583(4) -0.0026(4) -0.0080(11) -0.0007(3) Cl1 0.064(3) 0.050(2) 0.114(5) -0.003(3) 0.026(3) -0.007(2) Cl2 0.069(3) 0.054(3) 0.122(5) -0.002(4) -0.029(4) 0.003(2) N1 0.073(9) 0.030(6) 0.087(13) -0.012(9) 0.002(10) 0.003(6) N2 0.056(9) 0.061(11) 0.057(13) 0.002(10) 0.003(9) 0.008(8) N3 0.048(8) 0.035(7) 0.053(10) 0.000(7) 0.001(8) -0.003(6) N4 0.050(8) 0.039(8) 0.053(9) -0.008(9) 0.001(7) -0.005(6) N5 0.067(11) 0.031(8) 0.069(14) -0.003(9) 0.001(10) -0.006(8) N6 0.067(9) 0.040(7) 0.067(12) -0.016(9) 0.007(9) 0.012(7) N7 0.054(8) 0.044(8) 0.074(12) 0.002(8) -0.010(9) 0.012(7) N8 0.079(9) 0.039(7) 0.079(12) 0.001(10) -0.005(11) -0.007(7) N9 0.050(9) 0.037(8) 0.071(12) -0.011(9) -0.009(9) -0.006(7) N10 0.054(8) 0.037(8) 0.026(8) 0.000(9) -0.013(6) 0.003(6) N11 0.054(8) 0.050(7) 0.042(9) 0.009(7) -0.005(7) 0.000(7) N12 0.067(11) 0.045(8) 0.038(11) -0.012(9) 0.015(9) 0.006(9) C1 0.030(8) 0.036(9) 0.074(16) -0.004(11) -0.020(10) 0.005(7) C2 0.077(12) 0.041(9) 0.085(15) 0.008(14) 0.006(16) -0.005(8) C3 0.064(12) 0.052(11) 0.11(2) 0.019(14) -0.008(16) 0.006(10) C4 0.045(11) 0.052(11) 0.067(16) 0.031(11) -0.011(10) -0.007(8) C5 0.040(11) 0.049(11) 0.058(14) -0.004(12) 0.001(9) 0.007(9) C6 0.048(11) 0.067(13) 0.035(13) 0.003(11) -0.004(10) -0.013(10) C7 0.084(13) 0.067(12) 0.053(16) 0.001(10) 0.000(12) -0.004(10) C8 0.068(12) 0.064(12) 0.069(15) -0.039(12) 0.009(12) 0.013(10) C9 0.070(13) 0.037(10) 0.089(17) -0.009(12) -0.002(12) 0.001(10) C10 0.039(9) 0.049(10) 0.044(12) 0.006(10) 0.003(9) 0.001(7) C11 0.072(14) 0.055(12) 0.10(2) -0.001(14) 0.001(14) 0.002(10) C12 0.089(14) 0.029(9) 0.11(2) 0.019(12) 0.007(18) 0.022(9) C13 0.089(12) 0.021(7) 0.098(16) 0.002(13) 0.006(17) 0.011(8) C14 0.044(10) 0.042(9) 0.055(14) 0.006(12) -0.003(10) 0.005(8) C15 0.044(10) 0.030(8) 0.035(12) -0.007(8) 0.016(9) -0.010(7) C16 0.059(10) 0.050(9) 0.048(13) 0.002(9) -0.009(11) -0.007(7) C17 0.071(11) 0.038(9) 0.064(14) -0.006(9) 0.017(11) 0.001(8) C18 0.065(12) 0.052(11) 0.049(13) 0.002(11) -0.001(10) 0.016(10) _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 2.068(16) . ? Hg1 Cl1 2.308(5) . ? Hg1 N12 2.487(18) . ? Hg1 N10 2.639(13) . ? Hg1 Hg2 3.4689(9) . ? Hg2 N9 2.095(18) . ? Hg2 Cl2 2.307(5) . ? Hg2 N5 2.486(18) . ? Hg2 N4 2.613(13) . ? N1 C1 1.32(3) . ? N1 C2 1.344(19) . ? N2 C1 1.30(3) . ? N2 C4 1.32(2) . ? N3 C5 1.33(2) . ? N3 C1 1.41(2) . ? N4 C5 1.32(2) . ? N4 C6 1.36(2) . ? N5 C9 1.34(2) . ? N5 C6 1.36(2) . ? N6 C7 1.29(2) . ? N6 C6 1.32(2) . ? N7 C10 1.33(2) . ? N7 C11 1.34(2) . ? N8 C10 1.32(2) . ? N8 C13 1.341(18) . ? N9 C14 1.31(3) . ? N9 C10 1.40(2) . ? N10 C14 1.315(18) . ? N10 C15 1.42(2) . ? N11 C15 1.32(2) . ? N11 C16 1.34(2) . ? N12 C18 1.31(2) . ? N12 C15 1.38(2) . ? C2 C3 1.30(4) . ? C3 C4 1.41(3) . ? C7 C8 1.42(2) . ? C8 C9 1.35(3) . ? C11 C12 1.37(4) . ? C12 C13 1.36(4) . ? C16 C17 1.358(19) . ? C17 C18 1.36(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 N3 Hg1 Cl1 155.4(4) . . ? N3 Hg1 N12 101.7(5) . . ? Cl1 Hg1 N12 101.0(4) . . ? N3 Hg1 N10 104.9(5) . . ? Cl1 Hg1 N10 96.4(3) . . ? N12 Hg1 N10 52.9(5) . . ? N3 Hg1 Hg2 93.2(4) . . ? Cl1 Hg1 Hg2 87.03(12) . . ? N12 Hg1 Hg2 112.1(4) . . ? N10 Hg1 Hg2 59.2(3) . . ? N9 Hg2 Cl2 155.1(5) . . ? N9 Hg2 N5 98.3(5) . . ? Cl2 Hg2 N5 104.5(5) . . ? N9 Hg2 N4 106.0(5) . . ? Cl2 Hg2 N4 95.9(3) . . ? N5 Hg2 N4 52.2(4) . . ? N9 Hg2 Hg1 94.0(4) . . ? Cl2 Hg2 Hg1 86.86(12) . . ? N5 Hg2 Hg1 111.9(4) . . ? N4 Hg2 Hg1 60.0(3) . . ? C1 N1 C2 113(2) . . ? C1 N2 C4 116.3(18) . . ? C5 N3 C1 122.4(19) . . ? C5 N3 Hg1 122.0(13) . . ? C1 N3 Hg1 115.6(13) . . ? C5 N4 C6 119.0(17) . . ? C5 N4 Hg2 145.5(13) . . ? C6 N4 Hg2 95.5(10) . . ? C9 N5 C6 117.2(19) . . ? C9 N5 Hg2 141.5(14) . . ? C6 N5 Hg2 101.3(13) . . ? C7 N6 C6 118.4(17) . . ? C10 N7 C11 114.6(18) . . ? C10 N8 C13 117(2) . . ? C14 N9 C10 124(2) . . ? C14 N9 Hg2 120.5(13) . . ? C10 N9 Hg2 115.7(13) . . ? C14 N10 C15 118.7(16) . . ? C14 N10 Hg1 146.2(12) . . ? C15 N10 Hg1 94.8(9) . . ? C15 N11 C16 115.5(14) . . ? C18 N12 C15 114.8(17) . . ? C18 N12 Hg1 142.4(13) . . ? C15 N12 Hg1 102.7(12) . . ? N2 C1 N1 128.5(15) . . ? N2 C1 N3 119.5(19) . . ? N1 C1 N3 112.0(18) . . ? C3 C2 N1 125(3) . . ? C2 C3 C4 117.1(19) . . ? N2 C4 C3 120.1(19) . . ? N4 C5 N3 119(2) . . ? N6 C6 N4 125.3(17) . . ? N6 C6 N5 123.9(19) . . ? N4 C6 N5 110.8(18) . . ? N6 C7 C8 121(2) . . ? C9 C8 C7 117.7(18) . . ? N5 C9 C8 121.3(18) . . ? N8 C10 N7 127.3(16) . . ? N8 C10 N9 112.9(17) . . ? N7 C10 N9 119.8(18) . . ? N7 C11 C12 122(2) . . ? C13 C12 C11 118.4(17) . . ? N8 C13 C12 120(3) . . ? N9 C14 N10 120(2) . . ? N11 C15 N12 126.3(16) . . ? N11 C15 N10 124.2(14) . . ? N12 C15 N10 109.4(17) . . ? N11 C16 C17 122.3(18) . . ? C16 C17 C18 118.0(18) . . ? N12 C18 C17 123.0(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.001 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.153 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 640647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 Br2 Hg2 N12' _chemical_formula_weight 959.41 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.466(2) _cell_length_b 16.1116(15) _cell_length_c 10.3394(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2409.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 12.73 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 16.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5828 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2864 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2473 _reflns_number_gt 1572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0460P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.19(5) _refine_ls_number_reflns 2473 _refine_ls_number_parameters 298 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.73533(6) 0.65570(6) 1.04530(11) 0.0528(3) Uani 1 1 d . . . Hg2 Hg 0.73699(6) 0.44713(6) 0.95303(9) 0.0534(3) Uani 1 1 d . . . Br1 Br 0.5837(2) 0.63324(19) 1.1398(5) 0.0774(11) Uani 1 1 d . . . Br2 Br 0.5918(2) 0.47117(19) 0.8415(5) 0.0785(11) Uani 1 1 d . . . N1 N 0.8039(15) 0.8169(13) 0.976(3) 0.064(7) Uani 1 1 d . . . N2 N 0.8852(17) 0.8037(14) 0.779(2) 0.060(7) Uani 1 1 d . . . N3 N 0.8234(15) 0.6891(14) 0.888(3) 0.050(7) Uani 1 1 d . . . N4 N 0.8409(18) 0.5563(15) 0.836(2) 0.053(7) Uani 1 1 d . . . N5 N 0.8443(18) 0.4192(16) 0.773(3) 0.054(8) Uani 1 1 d . . . N6 N 0.9304(16) 0.5145(13) 0.652(2) 0.058(6) Uani 1 1 d . . . N7 N 0.8765(17) 0.3012(15) 1.230(3) 0.063(9) Uani 1 1 d . . . N8 N 0.7965(15) 0.2858(14) 1.033(3) 0.065(6) Uiso 1 1 d . . . N9 N 0.8165(13) 0.4125(15) 1.115(2) 0.035(5) Uani 1 1 d . . . N10 N 0.8283(13) 0.5472(12) 1.182(2) 0.036(5) Uani 1 1 d . . . N11 N 0.9197(17) 0.5846(14) 1.361(2) 0.060(7) Uani 1 1 d . . . N12 N 0.8391(17) 0.6841(17) 1.225(2) 0.048(7) Uani 1 1 d . . . C1 C 0.8382(18) 0.7740(17) 0.879(3) 0.047(7) Uiso 1 1 d . . . C2 C 0.814(2) 0.9046(16) 0.953(5) 0.069(8) Uani 1 1 d . . . H2B H 0.7848 0.9396 1.0115 0.083 Uiso 1 1 calc R . . C3 C 0.856(2) 0.939(2) 0.862(4) 0.080(12) Uani 1 1 d . . . H3A H 0.8627 0.9963 0.8556 0.095 Uiso 1 1 calc R . . C4 C 0.893(2) 0.886(2) 0.775(4) 0.082(13) Uani 1 1 d . . . H4A H 0.9261 0.9086 0.7072 0.099 Uiso 1 1 calc R . . C5 C 0.860(2) 0.635(2) 0.812(3) 0.041(8) Uani 1 1 d . . . H5A H 0.8983 0.6502 0.7432 0.049 Uiso 1 1 calc R . . C6 C 0.8770(18) 0.4994(18) 0.747(3) 0.040(7) Uani 1 1 d . . . C7 C 0.9599(16) 0.4503(19) 0.575(3) 0.069(10) Uani 1 1 d . . . H7B H 1.0022 0.4598 0.5091 0.082 Uiso 1 1 calc R . . C8 C 0.9263(19) 0.3719(14) 0.597(3) 0.062(9) Uani 1 1 d . . . H8B H 0.9396 0.3295 0.5387 0.074 Uiso 1 1 calc R . . C9 C 0.874(2) 0.356(2) 0.703(3) 0.065(9) Uani 1 1 d . . . H9A H 0.8590 0.3018 0.7257 0.078 Uiso 1 1 calc R . . C10 C 0.834(2) 0.330(2) 1.135(4) 0.061(10) Uani 1 1 d . . . C11 C 0.8864(19) 0.217(2) 1.238(4) 0.073(11) Uani 1 1 d . . . H11B H 0.9129 0.1926 1.3101 0.087 Uiso 1 1 calc R . . C12 C 0.857(2) 0.1694(18) 1.137(4) 0.066(10) Uani 1 1 d . . . H12A H 0.8682 0.1127 1.1400 0.079 Uiso 1 1 calc R . . C13 C 0.810(2) 0.2010(16) 1.028(4) 0.072(10) Uani 1 1 d . . . H13A H 0.7898 0.1681 0.9593 0.086 Uiso 1 1 calc R . . C14 C 0.845(2) 0.468(2) 1.204(3) 0.055(9) Uani 1 1 d . . . H14A H 0.8766 0.4510 1.2777 0.065 Uiso 1 1 calc R . . C15 C 0.8649(15) 0.611(2) 1.265(3) 0.048(9) Uani 1 1 d . . . C16 C 0.9512(19) 0.6448(19) 1.425(3) 0.068(9) Uani 1 1 d . . . H16A H 0.9872 0.6322 1.4965 0.081 Uiso 1 1 calc R . . C17 C 0.9364(19) 0.732(2) 1.396(3) 0.073(11) Uani 1 1 d . . . H17A H 0.9658 0.7745 1.4404 0.088 Uiso 1 1 calc R . . C18 C 0.879(3) 0.7443(19) 1.304(4) 0.088(14) Uani 1 1 d . . . H18A H 0.8626 0.7991 1.2884 0.105 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 0.0580(6) 0.0415(5) 0.0589(6) -0.0009(6) 0.0086(13) -0.0010(5) Hg2 0.0577(5) 0.0423(5) 0.0601(6) -0.0010(7) -0.0089(12) -0.0011(5) Br1 0.0685(19) 0.055(2) 0.108(3) -0.002(2) 0.029(2) -0.0079(17) Br2 0.0646(17) 0.0537(18) 0.117(3) 0.000(2) -0.033(2) -0.0001(17) N1 0.075(13) 0.054(14) 0.065(17) -0.012(14) 0.009(14) 0.001(12) N2 0.088(18) 0.052(17) 0.039(14) -0.001(14) 0.007(14) 0.012(14) N3 0.042(14) 0.024(13) 0.08(2) 0.015(15) 0.005(15) 0.002(10) N4 0.061(15) 0.052(17) 0.046(16) -0.011(18) -0.006(14) 0.002(13) N5 0.061(17) 0.037(14) 0.065(19) 0.003(15) 0.038(15) 0.011(14) N6 0.082(17) 0.045(13) 0.046(15) 0.003(13) 0.019(15) 0.010(13) N7 0.067(16) 0.037(15) 0.08(2) 0.021(16) -0.019(17) 0.005(13) N9 0.032(12) 0.053(15) 0.021(11) -0.007(12) -0.003(11) -0.007(11) N10 0.032(11) 0.028(12) 0.047(13) -0.025(13) 0.000(10) 0.009(9) N11 0.081(17) 0.056(14) 0.041(15) -0.026(15) -0.003(14) -0.026(14) N12 0.066(16) 0.040(15) 0.038(16) 0.025(14) 0.031(13) 0.028(14) C2 0.08(2) 0.043(16) 0.08(2) 0.00(2) 0.00(3) 0.024(15) C3 0.07(2) 0.06(2) 0.11(3) 0.06(2) 0.01(2) 0.008(17) C4 0.054(19) 0.06(2) 0.13(4) 0.02(3) 0.02(2) 0.022(18) C5 0.051(17) 0.07(2) 0.005(13) 0.001(17) -0.010(13) -0.010(17) C6 0.052(17) 0.053(19) 0.014(16) 0.008(15) -0.007(15) -0.002(15) C7 0.034(13) 0.11(3) 0.06(2) 0.04(2) 0.000(17) -0.002(15) C8 0.11(2) 0.018(13) 0.06(2) -0.013(15) -0.04(2) -0.005(14) C9 0.10(2) 0.08(2) 0.018(16) 0.000(18) -0.003(17) 0.02(2) C10 0.044(15) 0.06(2) 0.08(3) 0.00(2) -0.008(18) 0.011(14) C11 0.047(17) 0.09(3) 0.08(3) 0.03(3) -0.031(18) 0.013(18) C12 0.08(2) 0.039(18) 0.08(3) -0.01(2) 0.03(2) -0.010(17) C13 0.10(2) 0.030(16) 0.08(3) 0.006(18) -0.01(2) 0.022(15) C14 0.049(19) 0.06(2) 0.05(2) 0.00(2) -0.010(17) 0.012(17) C15 0.006(12) 0.11(3) 0.027(18) 0.01(2) -0.006(12) 0.003(15) C16 0.08(2) 0.07(2) 0.05(2) 0.031(19) -0.029(19) 0.014(16) C17 0.052(17) 0.11(3) 0.05(2) 0.00(2) -0.012(17) 0.002(19) C18 0.10(3) 0.021(16) 0.14(4) 0.00(2) 0.06(3) 0.03(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 Hg1 N3 2.13(3) . ? Hg1 Br1 2.429(3) . ? Hg1 N12 2.43(3) . ? Hg1 N10 2.62(2) . ? Hg1 Hg2 3.4933(13) . ? Hg2 N9 2.11(2) . ? Hg2 Br2 2.427(3) . ? Hg2 N5 2.47(3) . ? Hg2 N4 2.61(3) . ? N1 C1 1.32(4) . ? N1 C2 1.44(3) . ? N2 C1 1.33(3) . ? N2 C4 1.33(3) . ? N3 C5 1.30(4) . ? N3 C1 1.39(3) . ? N4 C5 1.32(3) . ? N4 C6 1.40(3) . ? N5 C9 1.32(4) . ? N5 C6 1.40(4) . ? N6 C6 1.27(3) . ? N6 C7 1.37(4) . ? N7 C10 1.25(4) . ? N7 C11 1.37(4) . ? N8 C13 1.38(3) . ? N8 C10 1.39(4) . ? N9 C14 1.34(4) . ? N9 C10 1.37(4) . ? N10 C14 1.32(3) . ? N10 C15 1.44(4) . ? N11 C16 1.26(3) . ? N11 C15 1.34(4) . ? N12 C15 1.30(4) . ? N12 C18 1.40(5) . ? C2 C3 1.25(5) . ? C3 C4 1.35(5) . ? C7 C8 1.37(3) . ? C8 C9 1.36(4) . ? C11 C12 1.36(5) . ? C12 C13 1.41(5) . ? C16 C17 1.45(4) . ? C17 C18 1.27(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 N3 Hg1 Br1 152.1(7) . . ? N3 Hg1 N12 99.5(7) . . ? Br1 Hg1 N12 106.2(5) . . ? N3 Hg1 N10 105.8(7) . . ? Br1 Hg1 N10 98.5(4) . . ? N12 Hg1 N10 52.9(7) . . ? N3 Hg1 Hg2 91.8(7) . . ? Br1 Hg1 Hg2 88.44(8) . . ? N12 Hg1 Hg2 112.7(6) . . ? N10 Hg1 Hg2 60.1(4) . . ? N9 Hg2 Br2 153.1(5) . . ? N9 Hg2 N5 102.1(8) . . ? Br2 Hg2 N5 102.4(7) . . ? N9 Hg2 N4 103.5(8) . . ? Br2 Hg2 N4 99.8(5) . . ? N5 Hg2 N4 53.8(8) . . ? N9 Hg2 Hg1 92.4(6) . . ? Br2 Hg2 Hg1 88.30(8) . . ? N5 Hg2 Hg1 112.7(6) . . ? N4 Hg2 Hg1 58.9(5) . . ? C1 N1 C2 110(3) . . ? C1 N2 C4 115(3) . . ? C5 N3 C1 124(3) . . ? C5 N3 Hg1 123(2) . . ? C1 N3 Hg1 113(2) . . ? C5 N4 C6 115(3) . . ? C5 N4 Hg2 149(2) . . ? C6 N4 Hg2 94.5(17) . . ? C9 N5 C6 120(3) . . ? C9 N5 Hg2 139(2) . . ? C6 N5 Hg2 100.8(19) . . ? C6 N6 C7 120(3) . . ? C10 N7 C11 118(3) . . ? C13 N8 C10 119(3) . . ? C14 N9 C10 119(3) . . ? C14 N9 Hg2 122(2) . . ? C10 N9 Hg2 119(2) . . ? C14 N10 C15 121(3) . . ? C14 N10 Hg1 147(2) . . ? C15 N10 Hg1 91.8(16) . . ? C16 N11 C15 111(3) . . ? C15 N12 C18 109(3) . . ? C15 N12 Hg1 104(2) . . ? C18 N12 Hg1 147(2) . . ? N1 C1 N2 127(3) . . ? N1 C1 N3 114(3) . . ? N2 C1 N3 119(3) . . ? C3 C2 N1 128(4) . . ? C2 C3 C4 114(3) . . ? N2 C4 C3 126(3) . . ? N3 C5 N4 116(3) . . ? N6 C6 N4 127(3) . . ? N6 C6 N5 122(3) . . ? N4 C6 N5 111(3) . . ? C8 C7 N6 119(3) . . ? C9 C8 C7 120(3) . . ? N5 C9 C8 118(3) . . ? N7 C10 N9 125(3) . . ? N7 C10 N8 127(3) . . ? N9 C10 N8 108(3) . . ? C12 C11 N7 119(3) . . ? C11 C12 C13 124(3) . . ? N8 C13 C12 113(3) . . ? N10 C14 N9 118(3) . . ? N12 C15 N11 134(3) . . ? N12 C15 N10 111(3) . . ? N11 C15 N10 115(3) . . ? N11 C16 C17 126(3) . . ? C18 C17 C16 114(3) . . ? C17 C18 N12 127(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.970 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.219 #===END data_3c _database_code_depnum_ccdc_archive 'CCDC 640648' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 Hg2 I2 N12' _chemical_formula_weight 1053.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 15.6846(16) _cell_length_b 10.1364(15) _cell_length_c 16.822(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.659(7) _cell_angle_gamma 90.00 _cell_volume 2575.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 16.39 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 14.338 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3204 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5499 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4404 _reflns_number_gt 2525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0542P)^2^+16.3130P] 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 4404 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.48976(4) 0.79190(7) 0.14269(4) 0.0559(2) Uani 1 1 d . . . Hg2 Hg 0.49354(5) 0.69330(7) 0.34499(4) 0.0574(2) Uani 1 1 d . . . I1 I 0.33896(9) 0.90412(17) 0.13121(8) 0.0861(5) Uani 1 1 d . . . I2 I 0.33875(9) 0.58661(18) 0.29653(8) 0.0931(5) Uani 1 1 d . . . N1 N 0.5505(9) 0.7122(17) 0.0013(7) 0.066(4) Uani 1 1 d . . . N2 N 0.6335(9) 0.5141(15) 0.0384(9) 0.059(4) Uani 1 1 d . . . N3 N 0.5692(9) 0.6279(13) 0.1288(8) 0.052(3) Uani 1 1 d . . . N4 N 0.5828(8) 0.5631(13) 0.2621(7) 0.052(4) Uani 1 1 d . . . N5 N 0.5976(10) 0.5087(14) 0.3966(9) 0.062(4) Uani 1 1 d . . . N6 N 0.6759(10) 0.3772(14) 0.3207(8) 0.061(4) Uani 1 1 d . . . N7 N 0.6355(10) 0.9855(16) 0.5110(9) 0.074(5) Uani 1 1 d . . . N8 N 0.5521(10) 0.7853(17) 0.5107(8) 0.071(4) Uani 1 1 d . . . N9 N 0.5801(9) 0.8555(13) 0.3939(7) 0.053(4) Uani 1 1 d . . . N10 N 0.5941(8) 0.9156(13) 0.2660(7) 0.049(3) Uani 1 1 d . . . N11 N 0.6855(10) 1.0938(15) 0.2494(9) 0.068(4) Uani 1 1 d . . . N12 N 0.5944(9) 0.9726(15) 0.1363(8) 0.058(4) Uani 1 1 d . . . C1 C 0.5864(10) 0.6159(17) 0.0527(9) 0.044(4) Uani 1 1 d . . . C2 C 0.5620(15) 0.705(2) -0.0732(12) 0.084(6) Uani 1 1 d . . . H2B H 0.5354 0.7673 -0.1125 0.101 Uiso 1 1 calc R . . C3 C 0.6116(16) 0.607(3) -0.0943(12) 0.094(8) Uani 1 1 d . . . H3A H 0.6231 0.6079 -0.1457 0.113 Uiso 1 1 calc R . . C4 C 0.6449(13) 0.508(2) -0.0379(12) 0.079(6) Uani 1 1 d . . . H4A H 0.6750 0.4369 -0.0529 0.094 Uiso 1 1 calc R . . C5 C 0.6036(10) 0.5437(15) 0.1940(9) 0.047(4) Uani 1 1 d . . . H5A H 0.6409 0.4747 0.1890 0.057 Uiso 1 1 calc R . . C6 C 0.6227(11) 0.4783(17) 0.3271(10) 0.051(4) Uani 1 1 d . . . C7 C 0.7081(12) 0.3125(19) 0.3909(13) 0.077(6) Uani 1 1 d . . . H7B H 0.7478 0.2442 0.3911 0.093 Uiso 1 1 calc R . . C8 C 0.6861(15) 0.340(2) 0.4654(13) 0.086(7) Uani 1 1 d . . . H8A H 0.7097 0.2916 0.5132 0.103 Uiso 1 1 calc R . . C9 C 0.6306(14) 0.438(2) 0.4637(10) 0.073(6) Uani 1 1 d . . . H9A H 0.6141 0.4583 0.5114 0.087 Uiso 1 1 calc R . . C10 C 0.5896(10) 0.8778(19) 0.4766(9) 0.053(4) Uani 1 1 d . . . C11 C 0.6379(12) 0.996(2) 0.5916(12) 0.077(6) Uani 1 1 d . . . H11B H 0.6664 1.0689 0.6202 0.092 Uiso 1 1 calc R . . C12 C 0.6011(15) 0.905(2) 0.6356(12) 0.087(7) Uani 1 1 d . . . H12A H 0.6048 0.9159 0.6913 0.105 Uiso 1 1 calc R . . C13 C 0.5606(16) 0.804(3) 0.5918(10) 0.095(8) Uani 1 1 d . . . H13A H 0.5361 0.7403 0.6191 0.114 Uiso 1 1 calc R . . C14 C 0.6121(11) 0.9335(17) 0.3447(9) 0.053(4) Uani 1 1 d . . . H14A H 0.6487 1.0034 0.3681 0.063 Uiso 1 1 calc R . . C15 C 0.6287(11) 1.0001(18) 0.2178(10) 0.056(5) Uani 1 1 d . . . C16 C 0.7113(11) 1.1706(15) 0.1944(11) 0.055(4) Uani 1 1 d . . . H16A H 0.7522 1.2377 0.2134 0.065 Uiso 1 1 calc R . . C17 C 0.6789(15) 1.151(2) 0.1122(13) 0.082(6) Uani 1 1 d . . . H17A H 0.6968 1.2048 0.0747 0.098 Uiso 1 1 calc R . . C18 C 0.6191(12) 1.052(2) 0.0854(11) 0.068(5) Uani 1 1 d . . . H18A H 0.5952 1.0407 0.0289 0.081 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 0.0566(4) 0.0626(5) 0.0518(4) 0.0036(4) 0.0204(3) 0.0115(4) Hg2 0.0582(4) 0.0654(5) 0.0533(4) -0.0016(4) 0.0229(3) -0.0075(4) I1 0.0730(9) 0.1197(12) 0.0711(8) 0.0094(8) 0.0290(7) 0.0408(9) I2 0.0701(9) 0.1468(15) 0.0669(7) -0.0085(9) 0.0262(7) -0.0414(10) N1 0.064(9) 0.104(13) 0.036(7) -0.008(8) 0.024(7) -0.001(10) N2 0.051(9) 0.057(10) 0.073(10) -0.022(8) 0.022(7) -0.013(8) N3 0.055(9) 0.049(8) 0.062(8) -0.006(7) 0.034(7) 0.006(7) N4 0.056(9) 0.060(9) 0.045(7) -0.008(7) 0.026(6) 0.011(7) N5 0.076(10) 0.053(9) 0.061(9) 0.008(8) 0.022(8) -0.010(8) N6 0.076(10) 0.045(9) 0.062(9) 0.014(7) 0.018(8) 0.012(8) N7 0.076(11) 0.079(11) 0.057(9) -0.020(9) 0.002(8) -0.021(10) N8 0.069(10) 0.104(13) 0.050(8) 0.004(9) 0.032(7) -0.014(10) N9 0.066(9) 0.046(8) 0.043(7) 0.007(6) 0.005(7) -0.004(7) N10 0.059(8) 0.053(9) 0.040(7) -0.001(6) 0.021(6) 0.009(7) N11 0.081(11) 0.054(10) 0.075(10) -0.006(8) 0.034(9) -0.013(9) N12 0.063(9) 0.067(10) 0.045(8) 0.002(7) 0.019(7) 0.010(8) C1 0.038(9) 0.057(11) 0.040(8) -0.007(8) 0.016(7) -0.010(8) C2 0.099(16) 0.093(17) 0.066(12) -0.015(12) 0.031(12) -0.017(14) C3 0.102(17) 0.13(2) 0.061(12) -0.038(15) 0.048(13) -0.062(17) C4 0.078(14) 0.094(16) 0.057(11) -0.029(12) 0.005(11) 0.001(13) C5 0.043(9) 0.042(10) 0.059(10) 0.009(8) 0.018(8) 0.012(8) C6 0.057(11) 0.045(11) 0.058(10) 0.013(9) 0.026(9) -0.008(9) C7 0.065(12) 0.059(13) 0.089(14) 0.004(12) -0.011(11) 0.021(10) C8 0.092(16) 0.080(16) 0.071(14) 0.025(12) -0.001(12) -0.010(14) C9 0.090(15) 0.081(15) 0.045(10) 0.022(10) 0.015(10) 0.001(13) C10 0.034(9) 0.078(13) 0.048(9) 0.005(9) 0.015(8) 0.010(9) C11 0.064(13) 0.087(15) 0.071(13) -0.015(12) 0.004(11) 0.012(12) C12 0.111(18) 0.109(19) 0.050(11) -0.015(13) 0.034(12) -0.009(16) C13 0.14(2) 0.13(2) 0.036(9) 0.016(12) 0.058(11) -0.021(18) C14 0.058(11) 0.049(11) 0.050(10) 0.004(8) 0.014(8) 0.011(9) C15 0.053(11) 0.057(11) 0.059(11) 0.019(9) 0.015(9) -0.003(10) C16 0.049(10) 0.035(10) 0.080(12) 0.016(9) 0.019(9) -0.004(8) C17 0.088(15) 0.083(15) 0.080(14) 0.031(12) 0.034(12) -0.005(13) C18 0.072(13) 0.090(15) 0.053(10) 0.008(11) 0.037(10) -0.003(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 Hg1 N3 2.128(13) . ? Hg1 N12 2.481(15) . ? Hg1 I1 2.5844(15) . ? Hg1 N10 2.592(12) . ? Hg2 N9 2.150(13) . ? Hg2 N5 2.481(15) . ? Hg2 I2 2.5807(15) . ? Hg2 N4 2.588(13) . ? N1 C2 1.32(2) . ? N1 C1 1.32(2) . ? N2 C1 1.33(2) . ? N2 C4 1.34(2) . ? N3 C5 1.381(18) . ? N3 C1 1.383(19) . ? N4 C5 1.288(19) . ? N4 C6 1.399(19) . ? N5 C9 1.32(2) . ? N5 C6 1.37(2) . ? N6 C7 1.33(2) . ? N6 C6 1.34(2) . ? N7 C10 1.35(2) . ? N7 C11 1.35(2) . ? N8 C10 1.32(2) . ? N8 C13 1.35(2) . ? N9 C14 1.34(2) . ? N9 C10 1.378(19) . ? N10 C14 1.290(18) . ? N10 C15 1.39(2) . ? N11 C15 1.31(2) . ? N11 C16 1.35(2) . ? N12 C18 1.31(2) . ? N12 C15 1.359(19) . ? C2 C3 1.36(3) . ? C3 C4 1.39(3) . ? C7 C8 1.42(3) . ? C8 C9 1.32(3) . ? C11 C12 1.39(3) . ? C12 C13 1.33(3) . ? C16 C17 1.35(2) . ? C17 C18 1.37(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 N3 Hg1 N12 99.1(5) . . ? N3 Hg1 I1 152.5(4) . . ? N12 Hg1 I1 105.9(3) . . ? N3 Hg1 N10 101.8(4) . . ? N12 Hg1 N10 52.8(4) . . ? I1 Hg1 N10 102.4(3) . . ? N9 Hg2 N5 98.9(5) . . ? N9 Hg2 I2 152.2(4) . . ? N5 Hg2 I2 105.6(3) . . ? N9 Hg2 N4 102.6(5) . . ? N5 Hg2 N4 53.4(4) . . ? I2 Hg2 N4 102.4(3) . . ? C2 N1 C1 115.8(18) . . ? C1 N2 C4 115.7(16) . . ? C5 N3 C1 123.3(14) . . ? C5 N3 Hg1 120.7(10) . . ? C1 N3 Hg1 115.9(11) . . ? C5 N4 C6 115.7(14) . . ? C5 N4 Hg2 149.4(11) . . ? C6 N4 Hg2 94.9(10) . . ? C9 N5 C6 118.2(17) . . ? C9 N5 Hg2 141.1(14) . . ? C6 N5 Hg2 100.6(10) . . ? C7 N6 C6 113.7(16) . . ? C10 N7 C11 111.0(17) . . ? C10 N8 C13 114.1(17) . . ? C14 N9 C10 125.0(14) . . ? C14 N9 Hg2 121.3(10) . . ? C10 N9 Hg2 113.4(12) . . ? C14 N10 C15 120.1(15) . . ? C14 N10 Hg1 143.7(12) . . ? C15 N10 Hg1 95.3(9) . . ? C15 N11 C16 115.8(15) . . ? C18 N12 C15 115.3(16) . . ? C18 N12 Hg1 143.1(12) . . ? C15 N12 Hg1 101.2(11) . . ? N1 C1 N2 127.9(15) . . ? N1 C1 N3 112.5(15) . . ? N2 C1 N3 119.6(15) . . ? N1 C2 C3 122(2) . . ? C2 C3 C4 119.0(19) . . ? N2 C4 C3 120(2) . . ? N4 C5 N3 118.3(14) . . ? N6 C6 N5 124.7(15) . . ? N6 C6 N4 124.2(15) . . ? N5 C6 N4 111.0(15) . . ? N6 C7 C8 124.4(18) . . ? C9 C8 C7 116.6(19) . . ? N5 C9 C8 122(2) . . ? N8 C10 N7 129.7(15) . . ? N8 C10 N9 112.6(15) . . ? N7 C10 N9 117.7(16) . . ? N7 C11 C12 125.4(19) . . ? C13 C12 C11 114.9(18) . . ? C12 C13 N8 125(2) . . ? N10 C14 N9 122.5(16) . . ? N11 C15 N12 126.7(16) . . ? N11 C15 N10 122.7(15) . . ? N12 C15 N10 110.6(15) . . ? C17 C16 N11 121.2(16) . . ? C16 C17 C18 118.6(18) . . ? N12 C18 C17 122.4(17) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.079 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.223 #===END