Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #======================================================== # SUBMISSION DETAILS _publ_contact_author ; Prof. Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_contact_letter ; This CIF file contains details of the 13 crystal structure in the paper: Structural studies on complexes of Ag(I), Hg(I) and Hg(II) with multidentate ligands ... by S. P. Argent et al, submitted to Dalton Trans. for publication. ; _publ_contact_author_name 'Prof. Mike Ward' loop_ _publ_author_name 'Stephen P. Argent' 'Harry Adams' W.Clegg 'Lindsay P. Harding' 'Ross W. Harrington' ; J.Jeffery ; T.Riis-Johannessen 'Mike Ward' #======================================================== data_imw259m _database_code_depnum_ccdc_archive 'CCDC 609491' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C24 H20 Ag N6), 2(C6 H14 O), 4(B F4)' _chemical_formula_sum 'C108 H108 Ag4 B4 F16 N24 O2' _chemical_formula_weight 2552.90 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _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 10.565(3) _cell_length_b 11.280(4) _cell_length_c 23.344(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.500(5) _cell_angle_gamma 90.00 _cell_volume 2779.3(15) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6487 _cell_measurement_theta_min 5.031 _cell_measurement_theta_max 54.986 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8285 _exptl_absorpt_correction_T_max 0.9619 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22834 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6259 _reflns_number_gt 4240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^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 6259 _refine_ls_number_parameters 388 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 1.046 _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 Ag1 Ag 0.61589(3) 0.57437(3) 0.140066(15) 0.04473(15) Uani 1 1 d . . . N11 N 0.7250(3) 0.7321(3) 0.10955(14) 0.0341(7) Uani 1 1 d . . . C12 C 0.8429(3) 0.7472(3) 0.13276(16) 0.0313(8) Uani 1 1 d . . . C13 C 0.9265(4) 0.8286(4) 0.1102(2) 0.0432(10) Uani 1 1 d . . . H13 H 1.0102 0.8371 0.1263 0.052 Uiso 1 1 calc R . . C14 C 0.8851(5) 0.8964(4) 0.0641(2) 0.0538(13) Uani 1 1 d . . . H14 H 0.9403 0.9529 0.0482 0.065 Uiso 1 1 calc R . . C15 C 0.7630(5) 0.8824(5) 0.0408(2) 0.0603(14) Uani 1 1 d . . . H15 H 0.7331 0.9288 0.0091 0.072 Uiso 1 1 calc R . . C16 C 0.6871(4) 0.7996(4) 0.06499(19) 0.0513(12) Uani 1 1 d . . . H16 H 0.6033 0.7897 0.0493 0.062 Uiso 1 1 calc R . . N21 N 0.8096(3) 0.5807(3) 0.19640(14) 0.0301(7) Uani 1 1 d . . . N22 N 0.8651(3) 0.5357(3) 0.24439(14) 0.0345(7) Uani 1 1 d . . . C23 C 0.9700(4) 0.5988(4) 0.2611(2) 0.0423(10) Uani 1 1 d . . . H23 H 1.0241 0.5836 0.2938 0.051 Uiso 1 1 calc R . . C24 C 0.9832(4) 0.6870(4) 0.22254(18) 0.0394(10) Uani 1 1 d . . . H24 H 1.0480 0.7454 0.2225 0.047 Uiso 1 1 calc R . . C25 C 0.8805(3) 0.6739(3) 0.18255(16) 0.0301(8) Uani 1 1 d . . . C31 C 0.8170(4) 0.4271(4) 0.2698(2) 0.0428(10) Uani 1 1 d . . . H31A H 0.7237 0.4247 0.2638 0.051 Uiso 1 1 calc R . . H31B H 0.8368 0.4282 0.3116 0.051 Uiso 1 1 calc R . . C32 C 0.8725(4) 0.3180(4) 0.24474(17) 0.0365(9) Uani 1 1 d . . . C33 C 0.9838(3) 0.2689(3) 0.26894(16) 0.0317(8) Uani 1 1 d . . . H33 H 1.0228 0.3039 0.3022 0.038 Uiso 1 1 calc R . . C34 C 1.0386(3) 0.1692(3) 0.24495(17) 0.0319(8) Uani 1 1 d . . . C35 C 0.9815(4) 0.1171(4) 0.19690(18) 0.0395(9) Uani 1 1 d . . . H35 H 1.0188 0.0494 0.1803 0.047 Uiso 1 1 calc R . . C36 C 0.8698(4) 0.1635(4) 0.1729(2) 0.0485(11) Uani 1 1 d . . . H36 H 0.8302 0.1271 0.1401 0.058 Uiso 1 1 calc R . . C37 C 0.8158(4) 0.2631(4) 0.19675(19) 0.0454(11) Uani 1 1 d . . . H37 H 0.7392 0.2942 0.1801 0.054 Uiso 1 1 calc R . . C38 C 1.1619(3) 0.1210(4) 0.27159(18) 0.0343(9) Uani 1 1 d . . . H38A H 1.2259 0.1179 0.2419 0.041 Uiso 1 1 calc R . . H38B H 1.1935 0.1760 0.3020 0.041 Uiso 1 1 calc R . . N41 N 1.0598(3) -0.0180(3) 0.33494(13) 0.0291(7) Uani 1 1 d . . . N42 N 1.1485(3) 0.0034(3) 0.29616(13) 0.0298(7) Uani 1 1 d . . . C43 C 1.2271(4) -0.0911(3) 0.29188(18) 0.0329(9) Uani 1 1 d . . . H43 H 1.2970 -0.0967 0.2677 0.039 Uiso 1 1 calc R . . C44 C 1.1880(3) -0.1761(3) 0.32831(16) 0.0326(9) Uani 1 1 d . . . H44 H 1.2243 -0.2522 0.3348 0.039 Uiso 1 1 calc R . . C45 C 1.0819(3) -0.1274(3) 0.35436(15) 0.0291(8) Uani 1 1 d . . . N51 N 0.9052(3) -0.1081(3) 0.41443(15) 0.0423(9) Uani 1 1 d . . . C52 C 0.9987(3) -0.1788(4) 0.39704(16) 0.0323(9) Uani 1 1 d . . . C53 C 1.0139(4) -0.2933(4) 0.41675(18) 0.0418(10) Uani 1 1 d . . . H53 H 1.0796 -0.3422 0.4034 0.050 Uiso 1 1 calc R . . C54 C 0.9316(4) -0.3355(5) 0.4563(2) 0.0545(13) Uani 1 1 d . . . H54 H 0.9409 -0.4138 0.4708 0.065 Uiso 1 1 calc R . . C55 C 0.8366(4) -0.2643(5) 0.4747(2) 0.0593(14) Uani 1 1 d . . . H55 H 0.7791 -0.2919 0.5019 0.071 Uiso 1 1 calc R . . C56 C 0.8271(4) -0.1524(5) 0.4527(2) 0.0580(14) Uani 1 1 d . . . H56 H 0.7611 -0.1029 0.4654 0.070 Uiso 1 1 calc R . . B1 B 0.7219(4) 0.0640(4) 0.8828(2) 0.0359(10) Uani 1 1 d . . . F1 F 0.8009(3) 0.0458(3) 0.92929(13) 0.0756(10) Uani 1 1 d . . . F2 F 0.5998(3) 0.0804(3) 0.89994(17) 0.0827(11) Uani 1 1 d . . . F3 F 0.7628(3) 0.1602(3) 0.85346(16) 0.0858(11) Uani 1 1 d . . . F4 F 0.7188(3) -0.0291(3) 0.84568(16) 0.0880(12) Uani 1 1 d . . . C1 C 1.1281(9) 0.5465(9) 0.0791(4) 0.063(2) Uani 0.50 1 d PDU A -1 H1A H 1.1371 0.6235 0.0603 0.095 Uiso 0.50 1 calc PR A -1 H1B H 1.2122 0.5129 0.0881 0.095 Uiso 0.50 1 calc PR A -1 H1C H 1.0834 0.5570 0.1147 0.095 Uiso 0.50 1 calc PR A -1 C2 C 1.0560(12) 0.4661(11) 0.0410(5) 0.083(4) Uani 0.50 1 d PDU A -1 H2A H 1.1200 0.4511 0.0115 0.099 Uiso 0.50 1 calc PR A -1 C3 C 1.0432(13) 0.3425(10) 0.0651(7) 0.100(4) Uani 0.50 1 d PDU A -1 H3A H 0.9985 0.2919 0.0366 0.151 Uiso 0.50 1 calc PR A -1 H3B H 0.9951 0.3457 0.1000 0.151 Uiso 0.50 1 calc PR A -1 H3C H 1.1276 0.3097 0.0741 0.151 Uiso 0.50 1 calc PR A -1 O4 O 0.9515(6) 0.4795(9) 0.0068(4) 0.090(2) Uani 0.50 1 d PDU A -1 C5 C 0.9950(19) 0.510(2) -0.0794(6) 0.161(8) Uani 0.50 1 d PDU A -1 H5A H 1.0845 0.4896 -0.0731 0.241 Uiso 0.50 1 calc PR A -1 H5B H 0.9838 0.5569 -0.1147 0.241 Uiso 0.50 1 calc PR A -1 H5C H 0.9442 0.4379 -0.0828 0.241 Uiso 0.50 1 calc PR A -1 C6 C 0.9549(16) 0.5784(15) -0.0324(6) 0.120(5) Uani 0.50 1 d PDU A -1 H6A H 1.0160 0.6420 -0.0200 0.144 Uiso 0.50 1 calc PR A -1 C7 C 0.8233(16) 0.6145(18) -0.0318(7) 0.154(8) Uani 0.50 1 d PDU A -1 H7A H 0.8096 0.6833 -0.0570 0.231 Uiso 0.50 1 calc PR A -1 H7B H 0.8024 0.6356 0.0074 0.231 Uiso 0.50 1 calc PR A -1 H7C H 0.7690 0.5490 -0.0455 0.231 Uiso 0.50 1 calc PR A -1 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 Ag1 0.02885(19) 0.0500(2) 0.0558(2) -0.00559(16) 0.00705(14) -0.01715(14) N11 0.0245(15) 0.0409(19) 0.0371(18) 0.0056(15) 0.0044(13) -0.0001(14) C12 0.0241(17) 0.033(2) 0.038(2) -0.0007(17) 0.0121(16) -0.0027(15) C13 0.036(2) 0.037(2) 0.058(3) 0.004(2) 0.013(2) -0.0084(18) C14 0.054(3) 0.044(3) 0.065(3) 0.020(2) 0.021(3) -0.008(2) C15 0.054(3) 0.068(3) 0.060(3) 0.029(3) 0.006(2) 0.007(3) C16 0.038(2) 0.068(3) 0.048(3) 0.018(2) 0.004(2) 0.004(2) N21 0.0224(15) 0.0307(17) 0.0375(17) 0.0047(14) 0.0065(13) 0.0018(13) N22 0.0268(16) 0.0377(18) 0.0394(19) 0.0091(15) 0.0054(14) 0.0041(14) C23 0.029(2) 0.053(3) 0.043(2) -0.001(2) -0.0060(18) 0.0052(18) C24 0.0244(18) 0.043(2) 0.050(2) -0.001(2) -0.0017(18) -0.0033(17) C25 0.0196(16) 0.032(2) 0.039(2) 0.0005(17) 0.0058(15) -0.0019(14) C31 0.037(2) 0.044(2) 0.049(3) 0.015(2) 0.0179(19) 0.0084(18) C32 0.0289(19) 0.038(2) 0.043(2) 0.0156(19) 0.0086(17) 0.0009(17) C33 0.0256(17) 0.036(2) 0.034(2) 0.0072(17) 0.0048(16) -0.0040(16) C34 0.0211(17) 0.035(2) 0.040(2) 0.0087(17) 0.0071(16) -0.0020(15) C35 0.039(2) 0.037(2) 0.043(2) 0.0013(19) 0.0031(19) -0.0003(19) C36 0.049(3) 0.051(3) 0.044(2) 0.004(2) -0.009(2) -0.006(2) C37 0.033(2) 0.051(3) 0.052(3) 0.019(2) -0.001(2) 0.000(2) C38 0.0215(17) 0.035(2) 0.047(2) 0.0012(18) 0.0052(16) -0.0009(16) N41 0.0185(14) 0.0351(18) 0.0341(17) 0.0027(14) 0.0053(12) 0.0044(13) N42 0.0189(14) 0.0353(18) 0.0355(17) 0.0008(14) 0.0042(13) 0.0019(12) C43 0.0242(18) 0.034(2) 0.041(2) -0.0076(17) 0.0074(16) 0.0056(15) C44 0.0245(18) 0.032(2) 0.041(2) -0.0054(17) -0.0005(16) 0.0069(15) C45 0.0231(17) 0.036(2) 0.0278(18) -0.0008(16) -0.0037(15) 0.0015(16) N51 0.0324(18) 0.054(2) 0.0415(19) 0.0130(17) 0.0097(15) 0.0110(16) C52 0.0223(17) 0.044(2) 0.0309(19) 0.0053(17) -0.0011(15) 0.0024(16) C53 0.032(2) 0.049(3) 0.044(2) 0.012(2) -0.0027(18) 0.0038(18) C54 0.046(3) 0.060(3) 0.057(3) 0.026(2) -0.005(2) -0.004(2) C55 0.041(3) 0.084(4) 0.054(3) 0.034(3) 0.010(2) 0.002(3) C56 0.039(2) 0.081(4) 0.056(3) 0.025(3) 0.021(2) 0.016(2) B1 0.031(2) 0.037(3) 0.040(3) -0.005(2) 0.004(2) -0.0069(19) F1 0.073(2) 0.101(3) 0.0521(17) 0.0289(17) -0.0131(16) -0.0088(18) F2 0.0518(19) 0.087(3) 0.112(3) -0.020(2) 0.0342(19) -0.0015(16) F3 0.0575(18) 0.076(2) 0.122(3) 0.057(2) -0.0231(19) -0.0209(16) F4 0.077(2) 0.095(2) 0.095(2) -0.055(2) 0.034(2) -0.032(2) C1 0.045(5) 0.083(6) 0.061(6) 0.022(5) -0.001(4) 0.021(4) C2 0.041(5) 0.138(8) 0.068(8) 0.034(5) -0.014(5) -0.021(6) C3 0.067(8) 0.110(7) 0.119(11) 0.023(7) -0.048(8) -0.009(7) O4 0.045(4) 0.142(7) 0.081(5) 0.017(5) -0.015(3) 0.026(5) C5 0.143(16) 0.23(2) 0.107(8) 0.011(11) 0.039(12) 0.045(15) C6 0.114(10) 0.169(12) 0.075(8) 0.030(7) -0.011(8) 0.036(9) C7 0.156(12) 0.206(16) 0.095(11) -0.008(11) -0.040(10) 0.114(13) _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 Ag1 N41 2.228(3) 2_655 ? Ag1 N11 2.252(3) . ? Ag1 N21 2.385(3) . ? Ag1 N51 2.425(4) 2_655 ? N11 C16 1.337(5) . ? N11 C12 1.348(5) . ? C12 C13 1.392(5) . ? C12 C25 1.467(5) . ? C13 C14 1.377(6) . ? C14 C15 1.387(7) . ? C15 C16 1.369(7) . ? N21 C25 1.339(5) . ? N21 N22 1.341(4) . ? N22 C23 1.359(5) . ? N22 C31 1.462(5) . ? C23 C24 1.353(6) . ? C24 C25 1.408(5) . ? C31 C32 1.493(6) . ? C32 C37 1.392(6) . ? C32 C33 1.397(5) . ? C33 C34 1.393(5) . ? C34 C35 1.381(6) . ? C34 C38 1.520(5) . ? C35 C36 1.387(6) . ? C36 C37 1.387(6) . ? C38 N42 1.455(5) . ? N41 C45 1.332(5) . ? N41 N42 1.352(4) . ? N41 Ag1 2.228(3) 2_645 ? N42 C43 1.357(5) . ? C43 C44 1.358(5) . ? C44 C45 1.410(5) . ? C45 C52 1.476(5) . ? N51 C56 1.340(5) . ? N51 C52 1.346(5) . ? N51 Ag1 2.425(4) 2_645 ? C52 C53 1.379(6) . ? C53 C54 1.381(6) . ? C54 C55 1.369(7) . ? C55 C56 1.364(7) . ? B1 F1 1.356(6) . ? B1 F4 1.361(5) . ? B1 F3 1.363(5) . ? B1 F2 1.379(5) . ? C1 C2 1.463(11) . ? C2 O4 1.341(11) . ? C2 C3 1.512(11) . ? O4 C6 1.445(13) . ? C5 C6 1.416(12) . ? C6 C7 1.450(12) . ? 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 N41 Ag1 N11 153.60(11) 2_655 . ? N41 Ag1 N21 125.03(11) 2_655 . ? N11 Ag1 N21 73.28(11) . . ? N41 Ag1 N51 71.48(11) 2_655 2_655 ? N11 Ag1 N51 122.75(12) . 2_655 ? N21 Ag1 N51 111.80(11) . 2_655 ? C16 N11 C12 118.7(3) . . ? C16 N11 Ag1 123.8(3) . . ? C12 N11 Ag1 116.7(2) . . ? N11 C12 C13 121.5(4) . . ? N11 C12 C25 117.4(3) . . ? C13 C12 C25 121.1(4) . . ? C14 C13 C12 118.5(4) . . ? C13 C14 C15 120.1(4) . . ? C16 C15 C14 117.9(4) . . ? N11 C16 C15 123.3(4) . . ? C25 N21 N22 105.6(3) . . ? C25 N21 Ag1 111.5(2) . . ? N22 N21 Ag1 141.5(2) . . ? N21 N22 C23 111.3(3) . . ? N21 N22 C31 120.6(3) . . ? C23 N22 C31 128.0(4) . . ? C24 C23 N22 107.5(4) . . ? C23 C24 C25 105.4(4) . . ? N21 C25 C24 110.2(3) . . ? N21 C25 C12 119.9(3) . . ? C24 C25 C12 129.8(3) . . ? N22 C31 C32 112.5(3) . . ? C37 C32 C33 118.3(4) . . ? C37 C32 C31 121.3(4) . . ? C33 C32 C31 120.4(4) . . ? C34 C33 C32 121.0(4) . . ? C35 C34 C33 119.7(4) . . ? C35 C34 C38 121.1(4) . . ? C33 C34 C38 119.2(4) . . ? C34 C35 C36 120.0(4) . . ? C35 C36 C37 120.1(4) . . ? C36 C37 C32 120.8(4) . . ? N42 C38 C34 113.0(3) . . ? C45 N41 N42 106.1(3) . . ? C45 N41 Ag1 118.7(2) . 2_645 ? N42 N41 Ag1 134.5(2) . 2_645 ? N41 N42 C43 110.7(3) . . ? N41 N42 C38 120.6(3) . . ? C43 N42 C38 128.0(3) . . ? N42 C43 C44 107.7(3) . . ? C43 C44 C45 105.3(3) . . ? N41 C45 C44 110.2(3) . . ? N41 C45 C52 119.6(3) . . ? C44 C45 C52 130.2(4) . . ? C56 N51 C52 117.5(4) . . ? C56 N51 Ag1 128.5(3) . 2_645 ? C52 N51 Ag1 113.3(3) . 2_645 ? N51 C52 C53 122.1(4) . . ? N51 C52 C45 115.9(3) . . ? C53 C52 C45 122.0(3) . . ? C52 C53 C54 118.6(4) . . ? C55 C54 C53 120.0(5) . . ? C56 C55 C54 117.9(4) . . ? N51 C56 C55 124.0(4) . . ? F1 B1 F4 112.9(4) . . ? F1 B1 F3 109.0(4) . . ? F4 B1 F3 107.1(4) . . ? F1 B1 F2 109.7(4) . . ? F4 B1 F2 107.0(4) . . ? F3 B1 F2 111.1(4) . . ? O4 C2 C1 133.3(12) . . ? O4 C2 C3 103.9(9) . . ? C1 C2 C3 113.4(9) . . ? C2 O4 C6 114.9(10) . . ? C5 C6 O4 95.2(12) . . ? C5 C6 C7 118.6(14) . . ? O4 C6 C7 99.2(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N41 Ag1 N11 C16 -46.8(5) 2_655 . . . ? N21 Ag1 N11 C16 175.2(4) . . . . ? N51 Ag1 N11 C16 69.7(4) 2_655 . . . ? N41 Ag1 N11 C12 143.0(3) 2_655 . . . ? N21 Ag1 N11 C12 5.0(3) . . . . ? N51 Ag1 N11 C12 -100.5(3) 2_655 . . . ? C16 N11 C12 C13 -2.0(6) . . . . ? Ag1 N11 C12 C13 168.7(3) . . . . ? C16 N11 C12 C25 178.4(4) . . . . ? Ag1 N11 C12 C25 -10.8(4) . . . . ? N11 C12 C13 C14 1.6(6) . . . . ? C25 C12 C13 C14 -178.9(4) . . . . ? C12 C13 C14 C15 -0.5(7) . . . . ? C13 C14 C15 C16 -0.2(8) . . . . ? C12 N11 C16 C15 1.3(7) . . . . ? Ag1 N11 C16 C15 -168.7(4) . . . . ? C14 C15 C16 N11 -0.2(8) . . . . ? N41 Ag1 N21 C25 -157.0(2) 2_655 . . . ? N11 Ag1 N21 C25 1.7(2) . . . . ? N51 Ag1 N21 C25 120.9(2) 2_655 . . . ? N41 Ag1 N21 N22 6.8(4) 2_655 . . . ? N11 Ag1 N21 N22 165.5(4) . . . . ? N51 Ag1 N21 N22 -75.3(4) 2_655 . . . ? C25 N21 N22 C23 -0.1(4) . . . . ? Ag1 N21 N22 C23 -164.5(3) . . . . ? C25 N21 N22 C31 -175.9(3) . . . . ? Ag1 N21 N22 C31 19.7(6) . . . . ? N21 N22 C23 C24 -0.3(5) . . . . ? C31 N22 C23 C24 175.2(4) . . . . ? N22 C23 C24 C25 0.5(5) . . . . ? N22 N21 C25 C24 0.4(4) . . . . ? Ag1 N21 C25 C24 170.1(2) . . . . ? N22 N21 C25 C12 -177.5(3) . . . . ? Ag1 N21 C25 C12 -7.9(4) . . . . ? C23 C24 C25 N21 -0.6(5) . . . . ? C23 C24 C25 C12 177.1(4) . . . . ? N11 C12 C25 N21 13.0(5) . . . . ? C13 C12 C25 N21 -166.6(4) . . . . ? N11 C12 C25 C24 -164.5(4) . . . . ? C13 C12 C25 C24 15.9(6) . . . . ? N21 N22 C31 C32 86.7(4) . . . . ? C23 N22 C31 C32 -88.3(5) . . . . ? N22 C31 C32 C37 -89.5(5) . . . . ? N22 C31 C32 C33 90.1(5) . . . . ? C37 C32 C33 C34 1.5(5) . . . . ? C31 C32 C33 C34 -178.1(3) . . . . ? C32 C33 C34 C35 -0.7(5) . . . . ? C32 C33 C34 C38 178.1(3) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C38 C34 C35 C36 -179.2(4) . . . . ? C34 C35 C36 C37 0.6(7) . . . . ? C35 C36 C37 C32 0.2(7) . . . . ? C33 C32 C37 C36 -1.2(6) . . . . ? C31 C32 C37 C36 178.3(4) . . . . ? C35 C34 C38 N42 -66.3(5) . . . . ? C33 C34 C38 N42 114.8(4) . . . . ? C45 N41 N42 C43 -1.0(4) . . . . ? Ag1 N41 N42 C43 -170.5(3) 2_645 . . . ? C45 N41 N42 C38 -172.3(3) . . . . ? Ag1 N41 N42 C38 18.2(5) 2_645 . . . ? C34 C38 N42 N41 -53.8(5) . . . . ? C34 C38 N42 C43 136.6(4) . . . . ? N41 N42 C43 C44 0.6(4) . . . . ? C38 N42 C43 C44 171.0(4) . . . . ? N42 C43 C44 C45 0.1(4) . . . . ? N42 N41 C45 C44 1.1(4) . . . . ? Ag1 N41 C45 C44 172.6(2) 2_645 . . . ? N42 N41 C45 C52 -178.8(3) . . . . ? Ag1 N41 C45 C52 -7.3(4) 2_645 . . . ? C43 C44 C45 N41 -0.7(4) . . . . ? C43 C44 C45 C52 179.1(4) . . . . ? C56 N51 C52 C53 1.0(6) . . . . ? Ag1 N51 C52 C53 -170.3(3) 2_645 . . . ? C56 N51 C52 C45 179.4(4) . . . . ? Ag1 N51 C52 C45 8.1(4) 2_645 . . . ? N41 C45 C52 N51 -1.2(5) . . . . ? C44 C45 C52 N51 179.0(4) . . . . ? N41 C45 C52 C53 177.2(4) . . . . ? C44 C45 C52 C53 -2.6(6) . . . . ? N51 C52 C53 C54 -1.2(6) . . . . ? C45 C52 C53 C54 -179.4(4) . . . . ? C52 C53 C54 C55 0.7(7) . . . . ? C53 C54 C55 C56 0.0(8) . . . . ? C52 N51 C56 C55 -0.3(7) . . . . ? Ag1 N51 C56 C55 169.5(4) 2_645 . . . ? C54 C55 C56 N51 -0.2(8) . . . . ? C1 C2 O4 C6 52(2) . . . . ? C3 C2 O4 C6 -165.3(11) . . . . ? C2 O4 C6 C5 96.0(14) . . . . ? C2 O4 C6 C7 -143.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.149 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.102 #===END data_imw205m _database_code_depnum_ccdc_archive 'CCDC 609492' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H44 Ag2 Cl2 N12 O8' _chemical_formula_weight 1227.61 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' Cl Cl 0.1484 0.1585 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3886(13) _cell_length_b 14.0381(15) _cell_length_c 14.2908(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.946(2) _cell_angle_gamma 90.00 _cell_volume 2479.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8156 _exptl_absorpt_correction_T_max 0.8687 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 ' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27544 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5651 _reflns_number_gt 3647 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0357P)^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 5651 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 Ag1 Ag 0.26269(2) 0.895733(18) 0.219197(16) 0.04067(9) Uani 1 1 d . . . N11 N 0.29205(17) 0.74512(16) 0.16096(15) 0.0280(5) Uani 1 1 d . . . C12 C 0.3278(2) 0.7406(2) 0.07388(19) 0.0271(6) Uani 1 1 d . . . C13 C 0.3513(2) 0.6544(2) 0.0326(2) 0.0379(8) Uani 1 1 d . . . H13 H 0.3724 0.6524 -0.0300 0.045 Uiso 1 1 calc R . . C14 C 0.3435(3) 0.5710(2) 0.0840(3) 0.0466(9) Uani 1 1 d . . . H14 H 0.3620 0.5114 0.0579 0.056 Uiso 1 1 calc R . . C15 C 0.3086(3) 0.5760(2) 0.1729(3) 0.0456(9) Uani 1 1 d . . . H15 H 0.3027 0.5201 0.2096 0.055 Uiso 1 1 calc R . . C16 C 0.2824(2) 0.6635(2) 0.2078(2) 0.0374(8) Uani 1 1 d . . . H16 H 0.2560 0.6661 0.2686 0.045 Uiso 1 1 calc R . . N21 N 0.31307(17) 0.91300(16) 0.06737(15) 0.0264(5) Uani 1 1 d . . . N22 N 0.34341(17) 0.98366(16) 0.01094(16) 0.0291(5) Uani 1 1 d . . . C23 C 0.3905(2) 0.9486(2) -0.06392(19) 0.0351(7) Uani 1 1 d . . . H23 H 0.4179 0.9849 -0.1132 0.042 Uiso 1 1 calc R . . C24 C 0.3921(2) 0.8519(2) -0.05662(19) 0.0324(7) Uani 1 1 d . . . H24 H 0.4201 0.8076 -0.0989 0.039 Uiso 1 1 calc R . . C25 C 0.3435(2) 0.8320(2) 0.02676(18) 0.0252(6) Uani 1 1 d . . . C31 C 0.3194(2) 1.08231(19) 0.0333(2) 0.0321(7) Uani 1 1 d . . . H31A H 0.3676 1.1248 -0.0001 0.039 Uiso 1 1 calc R . . H31B H 0.3345 1.0927 0.1015 0.039 Uiso 1 1 calc R . . C32 C 0.2025(2) 1.10831(18) 0.00614(19) 0.0272(6) Uani 1 1 d . . . C33 C 0.1751(2) 1.14188(18) -0.08310(19) 0.0268(6) Uani 1 1 d . . . H33 H 0.2289 1.1470 -0.1271 0.032 Uiso 1 1 calc R . . C34 C 0.0686(2) 1.16833(18) -0.10888(18) 0.0261(6) Uani 1 1 d . . . C35 C -0.0094(2) 1.15907(19) -0.04421(19) 0.0279(6) Uani 1 1 d . . . H35 H -0.0820 1.1765 -0.0619 0.033 Uiso 1 1 calc R . . C36 C 0.0164(2) 1.12495(19) 0.04553(19) 0.0292(7) Uani 1 1 d . . . C37 C 0.1236(2) 1.10026(19) 0.07004(19) 0.0290(6) Uani 1 1 d . . . H37 H 0.1430 1.0776 0.1315 0.035 Uiso 1 1 calc R . . C38 C 0.0397(2) 1.2074(2) -0.20587(19) 0.0327(7) Uani 1 1 d . . . H38A H 0.0986 1.2417 -0.2275 0.049 Uiso 1 1 d R . . H38B H -0.0223 1.2479 -0.2027 0.049 Uiso 1 1 d R . . C39 C -0.0701(2) 1.1143(2) 0.1140(2) 0.0399(8) Uani 1 1 d . . . H39A H -0.1015 1.1768 0.1260 0.060 Uiso 1 1 calc R . . H39B H -0.0382 1.0876 0.1730 0.060 Uiso 1 1 calc R . . H39C H -0.1268 1.0716 0.0876 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.57578(6) 0.80929(5) 0.27252(5) 0.03301(18) Uani 1 1 d . . . O1 O 0.53565(19) 0.71464(14) 0.26841(15) 0.0503(6) Uani 1 1 d . . . O2 O 0.5606(2) 0.85069(18) 0.18154(17) 0.0678(8) Uani 1 1 d . . . O3 O 0.5195(2) 0.86067(17) 0.33978(19) 0.0758(9) Uani 1 1 d . . . O4 O 0.68830(19) 0.8085(2) 0.29927(18) 0.0804(9) Uani 1 1 d . . . N41 N -0.08658(18) 1.09456(16) -0.28260(15) 0.0271(5) Uani 1 1 d . . . N42 N 0.01427(18) 1.13130(17) -0.27435(15) 0.0302(6) Uani 1 1 d . . . C43 C 0.0817(2) 1.0836(2) -0.3271(2) 0.0404(8) Uani 1 1 d . . . H43 H 0.1564 1.0965 -0.3315 0.048 Uiso 1 1 calc R . . C44 C 0.0235(2) 1.0133(2) -0.3732(2) 0.0374(8) Uani 1 1 d . . . H44 H 0.0488 0.9680 -0.4161 0.045 Uiso 1 1 calc R . . C45 C -0.0813(2) 1.02232(19) -0.34360(17) 0.0259(6) Uani 1 1 d . . . N51 N -0.27047(18) 0.99030(16) -0.33000(15) 0.0289(5) Uani 1 1 d . . . C52 C -0.1793(2) 0.96766(19) -0.37184(18) 0.0259(6) Uani 1 1 d . . . C53 C -0.1780(2) 0.89737(19) -0.44034(19) 0.0313(7) Uani 1 1 d . . . H53 H -0.1130 0.8831 -0.4691 0.038 Uiso 1 1 calc R . . C54 C -0.2722(3) 0.8486(2) -0.4662(2) 0.0352(7) Uani 1 1 d . . . H54 H -0.2734 0.8014 -0.5139 0.042 Uiso 1 1 calc R . . C55 C -0.3642(3) 0.8696(2) -0.4215(2) 0.0387(8) Uani 1 1 d . . . H55 H -0.4295 0.8357 -0.4363 0.046 Uiso 1 1 calc R . . C56 C -0.3596(2) 0.9408(2) -0.3549(2) 0.0361(7) Uani 1 1 d . . . H56 H -0.4238 0.9554 -0.3250 0.043 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 Ag1 0.04132(16) 0.05294(17) 0.02880(13) -0.00931(11) 0.01010(10) 0.01115(13) N11 0.0203(13) 0.0336(14) 0.0305(14) -0.0012(11) 0.0041(10) 0.0011(10) C12 0.0139(14) 0.0366(17) 0.0303(16) -0.0052(13) -0.0025(12) 0.0020(12) C13 0.0336(18) 0.0407(19) 0.0394(18) -0.0124(15) 0.0020(14) 0.0031(15) C14 0.043(2) 0.0301(18) 0.065(2) -0.0144(17) -0.0074(18) -0.0023(15) C15 0.036(2) 0.0361(19) 0.064(2) 0.0072(17) -0.0023(17) -0.0089(15) C16 0.0282(18) 0.045(2) 0.0391(18) 0.0062(15) 0.0042(14) -0.0034(14) N21 0.0221(13) 0.0318(14) 0.0253(12) 0.0003(10) 0.0022(10) -0.0001(10) N22 0.0215(13) 0.0362(14) 0.0297(13) 0.0023(11) 0.0029(10) 0.0009(11) C23 0.0212(16) 0.058(2) 0.0267(16) 0.0091(15) 0.0067(13) 0.0028(15) C24 0.0259(17) 0.0451(19) 0.0265(16) -0.0040(14) 0.0044(13) 0.0064(14) C25 0.0141(14) 0.0365(17) 0.0247(15) -0.0046(12) -0.0003(11) 0.0050(12) C31 0.0241(16) 0.0339(17) 0.0378(17) 0.0039(13) -0.0027(13) -0.0036(13) C32 0.0266(15) 0.0219(14) 0.0329(16) -0.0036(13) -0.0008(12) -0.0032(13) C33 0.0255(16) 0.0251(15) 0.0302(16) -0.0016(12) 0.0048(12) -0.0029(12) C34 0.0289(16) 0.0235(15) 0.0256(15) -0.0046(12) -0.0012(12) -0.0040(12) C35 0.0210(15) 0.0307(16) 0.0316(16) -0.0058(13) -0.0008(12) -0.0020(12) C36 0.0273(16) 0.0321(17) 0.0282(15) -0.0062(12) 0.0025(13) -0.0058(13) C37 0.0339(17) 0.0278(15) 0.0246(15) -0.0009(12) -0.0025(12) -0.0038(13) C38 0.0323(17) 0.0336(17) 0.0317(16) -0.0008(13) -0.0022(13) -0.0076(14) C39 0.0328(18) 0.052(2) 0.0360(18) -0.0041(15) 0.0078(14) -0.0068(15) Cl1 0.0310(4) 0.0387(4) 0.0301(4) -0.0007(3) 0.0074(3) -0.0096(3) O1 0.0607(16) 0.0347(13) 0.0586(15) -0.0055(11) 0.0269(12) -0.0137(11) O2 0.0737(19) 0.0757(18) 0.0551(16) 0.0350(14) 0.0129(14) 0.0022(15) O3 0.094(2) 0.0556(16) 0.084(2) -0.0251(15) 0.0523(17) -0.0057(15) O4 0.0325(15) 0.148(3) 0.0598(17) -0.0073(17) -0.0043(12) -0.0270(16) N41 0.0230(13) 0.0357(14) 0.0227(12) -0.0004(10) 0.0030(10) 0.0010(11) N42 0.0229(13) 0.0437(15) 0.0241(13) -0.0005(11) 0.0014(10) -0.0024(11) C43 0.0242(17) 0.071(2) 0.0262(16) -0.0016(16) 0.0073(13) 0.0020(16) C44 0.0294(18) 0.055(2) 0.0284(16) -0.0102(15) 0.0047(14) 0.0035(15) C45 0.0278(16) 0.0338(16) 0.0160(13) 0.0002(12) 0.0017(12) 0.0048(13) N51 0.0285(14) 0.0361(14) 0.0223(12) -0.0013(10) 0.0026(10) -0.0010(11) C52 0.0301(16) 0.0264(15) 0.0214(14) 0.0042(12) 0.0026(12) 0.0036(12) C53 0.0348(17) 0.0303(16) 0.0291(15) 0.0026(13) 0.0048(13) 0.0090(14) C54 0.051(2) 0.0235(16) 0.0299(16) -0.0007(13) -0.0040(15) 0.0038(15) C55 0.039(2) 0.0370(18) 0.0387(19) 0.0068(14) -0.0050(15) -0.0108(15) C56 0.0268(17) 0.0458(19) 0.0361(18) 0.0021(15) 0.0058(14) -0.0069(15) _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 Ag1 N51 2.248(2) 3_575 ? Ag1 N11 2.310(2) . ? Ag1 N21 2.311(2) . ? Ag1 N41 2.423(2) 3_575 ? N11 C16 1.337(4) . ? N11 C12 1.351(3) . ? C12 C13 1.385(4) . ? C12 C25 1.469(4) . ? C13 C14 1.390(4) . ? C14 C15 1.371(5) . ? C15 C16 1.373(4) . ? N21 C25 1.342(3) . ? N21 N22 1.348(3) . ? N22 C23 1.347(3) . ? N22 C31 1.457(3) . ? C23 C24 1.360(4) . ? C24 C25 1.400(4) . ? C31 C32 1.518(4) . ? C32 C33 1.380(4) . ? C32 C37 1.387(4) . ? C33 C34 1.396(4) . ? C34 C35 1.388(4) . ? C34 C38 1.510(4) . ? C35 C36 1.385(4) . ? C36 C37 1.394(4) . ? C36 C39 1.507(4) . ? C38 N42 1.468(3) . ? Cl1 O1 1.418(2) . ? Cl1 O4 1.420(2) . ? Cl1 O3 1.422(2) . ? Cl1 O2 1.425(2) . ? N41 C45 1.342(3) . ? N41 N42 1.349(3) . ? N41 Ag1 2.423(2) 3_575 ? N42 C43 1.342(4) . ? C43 C44 1.365(4) . ? C44 C45 1.399(4) . ? C45 C52 1.470(4) . ? N51 C56 1.333(3) . ? N51 C52 1.352(3) . ? N51 Ag1 2.248(2) 3_575 ? C52 C53 1.391(4) . ? C53 C54 1.381(4) . ? C54 C55 1.375(4) . ? C55 C56 1.379(4) . ? 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 N51 Ag1 N11 154.79(8) 3_575 . ? N51 Ag1 N21 125.82(8) 3_575 . ? N11 Ag1 N21 72.45(8) . . ? N51 Ag1 N41 72.10(8) 3_575 3_575 ? N11 Ag1 N41 110.75(8) . 3_575 ? N21 Ag1 N41 130.80(7) . 3_575 ? C16 N11 C12 117.9(2) . . ? C16 N11 Ag1 125.62(19) . . ? C12 N11 Ag1 116.41(18) . . ? N11 C12 C13 121.7(3) . . ? N11 C12 C25 116.3(2) . . ? C13 C12 C25 122.0(3) . . ? C12 C13 C14 119.2(3) . . ? C15 C14 C13 118.9(3) . . ? C14 C15 C16 118.7(3) . . ? N11 C16 C15 123.6(3) . . ? C25 N21 N22 105.5(2) . . ? C25 N21 Ag1 114.78(17) . . ? N22 N21 Ag1 138.00(17) . . ? C23 N22 N21 111.1(2) . . ? C23 N22 C31 128.9(2) . . ? N21 N22 C31 119.9(2) . . ? N22 C23 C24 108.0(3) . . ? C23 C24 C25 105.0(3) . . ? N21 C25 C24 110.4(2) . . ? N21 C25 C12 119.5(2) . . ? C24 C25 C12 130.0(3) . . ? N22 C31 C32 112.2(2) . . ? C33 C32 C37 119.8(3) . . ? C33 C32 C31 119.2(3) . . ? C37 C32 C31 121.0(3) . . ? C32 C33 C34 120.2(3) . . ? C35 C34 C33 119.2(3) . . ? C35 C34 C38 120.9(3) . . ? C33 C34 C38 119.9(2) . . ? C36 C35 C34 121.5(3) . . ? C35 C36 C37 118.3(3) . . ? C35 C36 C39 120.4(3) . . ? C37 C36 C39 121.3(3) . . ? C32 C37 C36 121.1(3) . . ? N42 C38 C34 112.0(2) . . ? O1 Cl1 O4 109.80(17) . . ? O1 Cl1 O3 108.44(14) . . ? O4 Cl1 O3 109.88(17) . . ? O1 Cl1 O2 108.69(15) . . ? O4 Cl1 O2 108.32(16) . . ? O3 Cl1 O2 111.70(17) . . ? C45 N41 N42 105.0(2) . . ? C45 N41 Ag1 111.79(17) . 3_575 ? N42 N41 Ag1 142.94(17) . 3_575 ? C43 N42 N41 111.6(2) . . ? C43 N42 C38 128.6(2) . . ? N41 N42 C38 119.4(2) . . ? N42 C43 C44 107.7(3) . . ? C43 C44 C45 105.0(3) . . ? N41 C45 C44 110.7(3) . . ? N41 C45 C52 119.8(2) . . ? C44 C45 C52 129.5(3) . . ? C56 N51 C52 117.5(2) . . ? C56 N51 Ag1 123.64(19) . 3_575 ? C52 N51 Ag1 118.83(18) . 3_575 ? N51 C52 C53 121.9(3) . . ? N51 C52 C45 117.1(2) . . ? C53 C52 C45 120.9(2) . . ? C54 C53 C52 119.3(3) . . ? C55 C54 C53 118.8(3) . . ? C54 C55 C56 118.7(3) . . ? N51 C56 C55 123.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N51 Ag1 N11 C16 39.1(3) 3_575 . . . ? N21 Ag1 N11 C16 179.4(2) . . . . ? N41 Ag1 N11 C16 -52.8(2) 3_575 . . . ? N51 Ag1 N11 C12 -137.0(2) 3_575 . . . ? N21 Ag1 N11 C12 3.29(17) . . . . ? N41 Ag1 N11 C12 131.10(18) 3_575 . . . ? C16 N11 C12 C13 1.7(4) . . . . ? Ag1 N11 C12 C13 178.1(2) . . . . ? C16 N11 C12 C25 -176.5(2) . . . . ? Ag1 N11 C12 C25 -0.2(3) . . . . ? N11 C12 C13 C14 -3.6(4) . . . . ? C25 C12 C13 C14 174.6(3) . . . . ? C12 C13 C14 C15 2.5(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C12 N11 C16 C15 1.1(4) . . . . ? Ag1 N11 C16 C15 -174.9(2) . . . . ? C14 C15 C16 N11 -2.1(5) . . . . ? N51 Ag1 N21 C25 154.11(17) 3_575 . . . ? N11 Ag1 N21 C25 -6.28(17) . . . . ? N41 Ag1 N21 C25 -108.86(19) 3_575 . . . ? N51 Ag1 N21 N22 -7.9(3) 3_575 . . . ? N11 Ag1 N21 N22 -168.3(3) . . . . ? N41 Ag1 N21 N22 89.1(3) 3_575 . . . ? C25 N21 N22 C23 0.7(3) . . . . ? Ag1 N21 N22 C23 163.8(2) . . . . ? C25 N21 N22 C31 178.2(2) . . . . ? Ag1 N21 N22 C31 -18.7(4) . . . . ? N21 N22 C23 C24 -0.4(3) . . . . ? C31 N22 C23 C24 -177.6(3) . . . . ? N22 C23 C24 C25 -0.1(3) . . . . ? N22 N21 C25 C24 -0.8(3) . . . . ? Ag1 N21 C25 C24 -168.42(17) . . . . ? N22 N21 C25 C12 176.4(2) . . . . ? Ag1 N21 C25 C12 8.8(3) . . . . ? C23 C24 C25 N21 0.6(3) . . . . ? C23 C24 C25 C12 -176.2(3) . . . . ? N11 C12 C25 N21 -5.9(4) . . . . ? C13 C12 C25 N21 175.8(3) . . . . ? N11 C12 C25 C24 170.6(3) . . . . ? C13 C12 C25 C24 -7.6(4) . . . . ? C23 N22 C31 C32 98.4(3) . . . . ? N21 N22 C31 C32 -78.6(3) . . . . ? N22 C31 C32 C33 -88.5(3) . . . . ? N22 C31 C32 C37 92.6(3) . . . . ? C37 C32 C33 C34 0.5(4) . . . . ? C31 C32 C33 C34 -178.5(2) . . . . ? C32 C33 C34 C35 -1.0(4) . . . . ? C32 C33 C34 C38 178.4(2) . . . . ? C33 C34 C35 C36 0.6(4) . . . . ? C38 C34 C35 C36 -178.8(2) . . . . ? C34 C35 C36 C37 0.3(4) . . . . ? C34 C35 C36 C39 -179.2(3) . . . . ? C33 C32 C37 C36 0.5(4) . . . . ? C31 C32 C37 C36 179.4(2) . . . . ? C35 C36 C37 C32 -0.9(4) . . . . ? C39 C36 C37 C32 178.6(3) . . . . ? C35 C34 C38 N42 -94.1(3) . . . . ? C33 C34 C38 N42 86.5(3) . . . . ? C45 N41 N42 C43 -0.8(3) . . . . ? Ag1 N41 N42 C43 172.3(2) 3_575 . . . ? C45 N41 N42 C38 -174.7(2) . . . . ? Ag1 N41 N42 C38 -1.7(4) 3_575 . . . ? C34 C38 N42 C43 -88.7(3) . . . . ? C34 C38 N42 N41 84.1(3) . . . . ? N41 N42 C43 C44 0.8(3) . . . . ? C38 N42 C43 C44 174.1(3) . . . . ? N42 C43 C44 C45 -0.5(3) . . . . ? N42 N41 C45 C44 0.4(3) . . . . ? Ag1 N41 C45 C44 -175.07(18) 3_575 . . . ? N42 N41 C45 C52 -177.8(2) . . . . ? Ag1 N41 C45 C52 6.7(3) 3_575 . . . ? C43 C44 C45 N41 0.0(3) . . . . ? C43 C44 C45 C52 178.1(3) . . . . ? C56 N51 C52 C53 1.8(4) . . . . ? Ag1 N51 C52 C53 179.46(19) 3_575 . . . ? C56 N51 C52 C45 -179.7(2) . . . . ? Ag1 N51 C52 C45 -2.0(3) 3_575 . . . ? N41 C45 C52 N51 -3.6(4) . . . . ? C44 C45 C52 N51 178.5(3) . . . . ? N41 C45 C52 C53 175.0(2) . . . . ? C44 C45 C52 C53 -3.0(4) . . . . ? N51 C52 C53 C54 -0.5(4) . . . . ? C45 C52 C53 C54 -178.9(2) . . . . ? C52 C53 C54 C55 -1.5(4) . . . . ? C53 C54 C55 C56 2.1(4) . . . . ? C52 N51 C56 C55 -1.2(4) . . . . ? Ag1 N51 C56 C55 -178.7(2) 3_575 . . . ? C54 C55 C56 N51 -0.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.495 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.073 #===END data_argentm _database_code_depnum_ccdc_archive 'CCDC 609493' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 Ag2 N12, 2(B F4)' _chemical_formula_sum 'C48 H40 Ag2 B2 F8 N12' _chemical_formula_weight 1174.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 '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 11.5905(2) _cell_length_b 21.4560(4) _cell_length_c 18.4922(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.6510(10) _cell_angle_gamma 90.00 _cell_volume 4576.40(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 8.242 _cell_measurement_theta_max 139.824 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 7.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.145322 _exptl_absorpt_correction_T_max 0.322063 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21250 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 70.06 _reflns_number_total 7220 _reflns_number_gt 6046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0581P)^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 7220 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Ag1 Ag 0.52013(2) 0.237732(11) -0.055395(17) 0.02858(9) Uani 1 1 d . . . Ag2 Ag 0.54676(2) 0.246378(12) 0.400058(17) 0.03125(10) Uani 1 1 d . . . N11 N 0.6359(2) 0.15616(12) -0.07676(18) 0.0240(7) Uani 1 1 d . . . C12 C 0.7366(3) 0.15022(15) -0.0342(2) 0.0234(8) Uani 1 1 d . . . C13 C 0.8009(3) 0.09531(15) -0.0330(2) 0.0265(8) Uani 1 1 d . . . H13 H 0.8690 0.0918 -0.0022 0.032 Uiso 1 1 calc R . . C14 C 0.7636(3) 0.04635(16) -0.0773(2) 0.0292(9) Uani 1 1 d . . . H14 H 0.8060 0.0095 -0.0769 0.035 Uiso 1 1 calc R . . C15 C 0.6619(3) 0.05281(16) -0.1225(2) 0.0294(8) Uani 1 1 d . . . H15 H 0.6351 0.0208 -0.1536 0.035 Uiso 1 1 calc R . . C16 C 0.6008(3) 0.10825(16) -0.1202(2) 0.0290(8) Uani 1 1 d . . . H16 H 0.5321 0.1125 -0.1503 0.035 Uiso 1 1 calc R . . N21 N 0.7143(2) 0.25572(12) 0.00925(18) 0.0243(7) Uani 1 1 d . . . C22 C 0.7771(3) 0.20353(15) 0.0108(2) 0.0238(8) Uani 1 1 d . . . C23 C 0.8780(3) 0.20917(16) 0.0594(2) 0.0270(8) Uani 1 1 d . . . H23 H 0.9354 0.1794 0.0702 0.032 Uiso 1 1 calc R . . C24 C 0.8732(3) 0.26849(16) 0.0874(2) 0.0288(8) Uani 1 1 d . . . H24 H 0.9276 0.2870 0.1210 0.035 Uiso 1 1 calc R . . N25 N 0.7743(2) 0.29461(13) 0.05669(18) 0.0239(7) Uani 1 1 d . . . C26 C 0.7290(3) 0.35640(15) 0.0699(2) 0.0266(8) Uani 1 1 d . . . H26A H 0.6934 0.3731 0.0243 0.032 Uiso 1 1 calc R . . H26B H 0.7933 0.3834 0.0865 0.032 Uiso 1 1 calc R . . C31 C 0.6409(3) 0.35828(15) 0.1251(2) 0.0238(8) Uani 1 1 d . . . C32 C 0.5682(3) 0.30823(16) 0.1366(2) 0.0279(8) Uani 1 1 d . . . H32 H 0.5767 0.2708 0.1124 0.034 Uiso 1 1 calc R . . C33 C 0.4830(3) 0.31401(16) 0.1841(2) 0.0289(9) Uani 1 1 d . . . H33 H 0.4349 0.2803 0.1913 0.035 Uiso 1 1 calc R . . C34 C 0.4687(3) 0.36969(15) 0.2211(2) 0.0247(8) Uani 1 1 d . . . C35 C 0.5429(3) 0.41943(16) 0.2098(2) 0.0282(8) Uani 1 1 d . . . H35 H 0.5348 0.4569 0.2340 0.034 Uiso 1 1 calc R . . C36 C 0.6284(3) 0.41324(15) 0.1630(2) 0.0275(8) Uani 1 1 d . . . H36 H 0.6781 0.4464 0.1568 0.033 Uiso 1 1 calc R . . N41 N 0.3657(2) 0.27702(13) 0.32864(18) 0.0240(6) Uani 1 1 d . . . C42 C 0.2910(3) 0.22920(16) 0.3235(2) 0.0249(8) Uani 1 1 d . . . C43 C 0.1913(3) 0.24392(16) 0.2774(2) 0.0288(8) Uani 1 1 d . . . H43 H 0.1272 0.2187 0.2651 0.035 Uiso 1 1 calc R . . C44 C 0.2091(3) 0.30346(16) 0.2547(2) 0.0274(8) Uani 1 1 d . . . H44 H 0.1585 0.3269 0.2233 0.033 Uiso 1 1 calc R . . N45 N 0.3138(2) 0.32200(13) 0.28620(18) 0.0245(7) Uani 1 1 d . . . C46 C 0.3761(3) 0.37880(15) 0.2727(2) 0.0284(9) Uani 1 1 d . . . H46A H 0.4122 0.3947 0.3186 0.034 Uiso 1 1 calc R . . H46B H 0.3212 0.4099 0.2525 0.034 Uiso 1 1 calc R . . N51 N 0.4151(2) 0.17073(13) 0.41264(18) 0.0260(7) Uani 1 1 d . . . C52 C 0.3207(3) 0.17088(15) 0.3628(2) 0.0247(8) Uani 1 1 d . . . C53 C 0.2564(3) 0.11679(16) 0.3468(2) 0.0263(8) Uani 1 1 d . . . H53 H 0.1933 0.1174 0.3116 0.032 Uiso 1 1 calc R . . C54 C 0.2873(3) 0.06212(16) 0.3837(2) 0.0297(9) Uani 1 1 d . . . H54 H 0.2461 0.0255 0.3731 0.036 Uiso 1 1 calc R . . C55 C 0.3814(3) 0.06298(17) 0.4372(2) 0.0330(9) Uani 1 1 d . . . H55 H 0.4026 0.0274 0.4640 0.040 Uiso 1 1 calc R . . C56 C 0.4420(3) 0.11804(16) 0.4490(2) 0.0286(8) Uani 1 1 d . . . H56 H 0.5050 0.1185 0.4842 0.034 Uiso 1 1 calc R . . N61 N 0.4350(2) 0.33460(12) -0.05349(18) 0.0243(7) Uani 1 1 d . . . C62 C 0.3463(3) 0.34231(15) -0.0123(2) 0.0241(8) Uani 1 1 d . . . C63 C 0.3008(3) 0.40115(16) 0.0006(2) 0.0293(8) Uani 1 1 d . . . H63 H 0.2399 0.4054 0.0294 0.035 Uiso 1 1 calc R . . C64 C 0.3477(3) 0.45293(17) -0.0301(3) 0.0351(10) Uani 1 1 d . . . H64 H 0.3182 0.4925 -0.0226 0.042 Uiso 1 1 calc R . . C65 C 0.4387(3) 0.44523(16) -0.0723(2) 0.0336(9) Uani 1 1 d . . . H65 H 0.4722 0.4794 -0.0931 0.040 Uiso 1 1 calc R . . C66 C 0.4788(3) 0.38558(16) -0.0826(2) 0.0305(9) Uani 1 1 d . . . H66 H 0.5396 0.3805 -0.1113 0.037 Uiso 1 1 calc R . . N71 N 0.3563(2) 0.23132(12) 0.01441(18) 0.0231(6) Uani 1 1 d . . . C72 C 0.3006(3) 0.28599(15) 0.0197(2) 0.0232(8) Uani 1 1 d . . . C73 C 0.2038(3) 0.27899(17) 0.0592(2) 0.0296(8) Uani 1 1 d . . . H73 H 0.1511 0.3095 0.0702 0.036 Uiso 1 1 calc R . . C74 C 0.2044(3) 0.21683(17) 0.0781(2) 0.0291(9) Uani 1 1 d . . . H74 H 0.1517 0.1970 0.1052 0.035 Uiso 1 1 calc R . . N75 N 0.2948(2) 0.19017(13) 0.05016(18) 0.0246(7) Uani 1 1 d . . . C76 C 0.3348(3) 0.12574(15) 0.0591(2) 0.0266(8) Uani 1 1 d . . . H76A H 0.3604 0.1110 0.0137 0.032 Uiso 1 1 calc R . . H76B H 0.2709 0.0996 0.0707 0.032 Uiso 1 1 calc R . . C81 C 0.4335(3) 0.12013(14) 0.1187(2) 0.0238(8) Uani 1 1 d . . . C82 C 0.4110(3) 0.10961(16) 0.1904(2) 0.0286(9) Uani 1 1 d . . . H82 H 0.3350 0.1039 0.2012 0.034 Uiso 1 1 calc R . . C83 C 0.5017(3) 0.10757(16) 0.2459(2) 0.0295(9) Uani 1 1 d . . . H83 H 0.4860 0.1004 0.2936 0.035 Uiso 1 1 calc R . . C84 C 0.6151(3) 0.11628(14) 0.2301(2) 0.0234(8) Uani 1 1 d . . . C85 C 0.6379(3) 0.12484(18) 0.1585(2) 0.0318(9) Uani 1 1 d . . . H85 H 0.7139 0.1296 0.1474 0.038 Uiso 1 1 calc R . . C86 C 0.5469(3) 0.12633(17) 0.1028(2) 0.0307(9) Uani 1 1 d . . . H86 H 0.5628 0.1315 0.0549 0.037 Uiso 1 1 calc R . . N91 N 0.7083(2) 0.22588(13) 0.33121(18) 0.0240(6) Uani 1 1 d . . . C92 C 0.7710(3) 0.27769(16) 0.3224(2) 0.0250(8) Uani 1 1 d . . . C93 C 0.8667(3) 0.26422(16) 0.2839(2) 0.0286(8) Uani 1 1 d . . . H93 H 0.9233 0.2918 0.2713 0.034 Uiso 1 1 calc R . . C94 C 0.8589(3) 0.20170(17) 0.2687(2) 0.0294(9) Uani 1 1 d . . . H94 H 0.9091 0.1785 0.2431 0.035 Uiso 1 1 calc R . . N95 N 0.7647(2) 0.18020(13) 0.29801(18) 0.0247(7) Uani 1 1 d . . . C96 C 0.7132(3) 0.11797(15) 0.2901(2) 0.0254(8) Uani 1 1 d . . . H96A H 0.6844 0.1058 0.3355 0.031 Uiso 1 1 calc R . . H96B H 0.7723 0.0882 0.2794 0.031 Uiso 1 1 calc R . . N101 N 0.6526(2) 0.33574(13) 0.39847(18) 0.0268(7) Uani 1 1 d . . . C102 C 0.7355(3) 0.33745(16) 0.3521(2) 0.0267(8) Uani 1 1 d . . . C103 C 0.7841(3) 0.39342(16) 0.3315(2) 0.0315(9) Uani 1 1 d . . . H103 H 0.8404 0.3935 0.2989 0.038 Uiso 1 1 calc R . . C104 C 0.7476(3) 0.44886(17) 0.3601(2) 0.0365(10) Uani 1 1 d . . . H104 H 0.7794 0.4867 0.3474 0.044 Uiso 1 1 calc R . . C105 C 0.6629(3) 0.44706(17) 0.4080(2) 0.0357(10) Uani 1 1 d . . . H105 H 0.6366 0.4835 0.4282 0.043 Uiso 1 1 calc R . . C106 C 0.6191(3) 0.39022(17) 0.4249(2) 0.0333(9) Uani 1 1 d . . . H106 H 0.5620 0.3894 0.4569 0.040 Uiso 1 1 calc R . . B1 B 0.5132(3) 0.06522(17) 0.6616(3) 0.0273(9) Uani 1 1 d . . . F1A F 0.4253(2) 0.02816(11) 0.63059(17) 0.0497(7) Uani 1 1 d . . . F1B F 0.5859(2) 0.03323(11) 0.71142(15) 0.0506(7) Uani 1 1 d . . . F1C F 0.4663(2) 0.11686(10) 0.69539(15) 0.0412(6) Uani 1 1 d . . . F1D F 0.5778(2) 0.08789(12) 0.60778(16) 0.0505(7) Uani 1 1 d . . . B2 B 0.0339(3) 0.07367(18) 0.1676(3) 0.0265(10) Uani 1 1 d . . . F2A F 0.07101(18) 0.13323(9) 0.18997(13) 0.0323(5) Uani 1 1 d . . . F2B F 0.03759(18) 0.06929(9) 0.09210(13) 0.0337(5) Uani 1 1 d . . . F2C F 0.1060(2) 0.02961(10) 0.20251(14) 0.0400(6) Uani 1 1 d . . . F2D F -0.07940(18) 0.06573(10) 0.18480(16) 0.0414(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 Ag1 0.02487(14) 0.03198(14) 0.0291(2) -0.00082(11) 0.00387(11) 0.00643(8) Ag2 0.02392(15) 0.03871(15) 0.0313(2) -0.00133(11) 0.00333(11) -0.00363(8) N11 0.0240(15) 0.0285(14) 0.020(2) -0.0009(13) 0.0059(12) 0.0022(10) C12 0.0249(17) 0.0318(17) 0.015(2) 0.0042(15) 0.0102(14) 0.0020(11) C13 0.0253(18) 0.0308(17) 0.024(3) 0.0036(15) 0.0081(15) 0.0023(12) C14 0.0332(19) 0.0283(17) 0.028(3) 0.0020(16) 0.0104(16) 0.0044(12) C15 0.043(2) 0.0266(17) 0.020(3) -0.0010(15) 0.0086(17) -0.0015(13) C16 0.0313(19) 0.0332(18) 0.023(3) 0.0008(16) 0.0055(16) -0.0008(12) N21 0.0245(15) 0.0284(14) 0.020(2) -0.0007(12) 0.0025(12) -0.0025(9) C22 0.0207(17) 0.0318(17) 0.020(2) 0.0031(15) 0.0087(14) 0.0002(11) C23 0.0242(18) 0.0317(17) 0.025(3) 0.0019(15) 0.0020(15) 0.0018(12) C24 0.0266(18) 0.0338(18) 0.026(3) 0.0032(16) 0.0006(15) -0.0010(12) N25 0.0264(15) 0.0280(14) 0.018(2) -0.0021(12) 0.0050(12) -0.0023(10) C26 0.0294(18) 0.0251(17) 0.026(3) 0.0000(15) 0.0060(15) 0.0000(11) C31 0.0235(17) 0.0301(17) 0.018(2) 0.0021(15) 0.0020(14) 0.0007(11) C32 0.0299(19) 0.0290(17) 0.026(3) -0.0074(15) 0.0062(16) -0.0035(12) C33 0.0286(19) 0.0298(18) 0.029(3) -0.0027(16) 0.0067(16) -0.0046(12) C34 0.0257(17) 0.0290(17) 0.019(2) 0.0006(15) 0.0014(14) 0.0035(11) C35 0.0322(19) 0.0270(17) 0.026(3) -0.0023(15) 0.0063(16) 0.0032(12) C36 0.0275(18) 0.0278(17) 0.027(3) 0.0012(15) 0.0032(15) -0.0022(11) N41 0.0230(14) 0.0328(14) 0.0166(19) -0.0021(13) 0.0037(12) 0.0027(10) C42 0.0247(17) 0.0320(17) 0.019(2) -0.0050(15) 0.0091(15) 0.0013(12) C43 0.0238(18) 0.0341(18) 0.028(3) -0.0066(16) 0.0013(15) 0.0012(12) C44 0.0253(18) 0.0340(18) 0.023(2) -0.0036(15) 0.0012(15) 0.0038(12) N45 0.0256(15) 0.0291(14) 0.020(2) -0.0008(13) 0.0067(12) 0.0020(10) C46 0.0300(19) 0.0274(17) 0.028(3) -0.0003(15) 0.0062(16) 0.0017(12) N51 0.0270(15) 0.0361(16) 0.016(2) -0.0016(13) 0.0088(13) 0.0018(10) C52 0.0230(17) 0.0330(17) 0.019(2) -0.0041(15) 0.0061(15) 0.0011(11) C53 0.0228(17) 0.0364(18) 0.021(2) -0.0043(16) 0.0076(15) 0.0003(12) C54 0.0301(19) 0.0298(18) 0.031(3) -0.0050(16) 0.0122(16) -0.0023(12) C55 0.036(2) 0.0348(19) 0.030(3) 0.0040(17) 0.0106(18) 0.0057(13) C56 0.0322(19) 0.0349(18) 0.020(2) 0.0003(16) 0.0076(16) 0.0057(13) N61 0.0231(14) 0.0291(14) 0.021(2) 0.0004(12) 0.0044(12) 0.0003(10) C62 0.0230(17) 0.0285(16) 0.020(2) 0.0021(15) 0.0006(14) -0.0013(11) C63 0.0281(19) 0.0347(18) 0.026(3) -0.0041(16) 0.0050(16) 0.0003(12) C64 0.038(2) 0.0278(18) 0.039(3) 0.0001(17) 0.0029(18) 0.0022(13) C65 0.032(2) 0.0318(18) 0.037(3) 0.0062(17) 0.0063(17) -0.0031(13) C66 0.0255(18) 0.0350(19) 0.032(3) 0.0041(16) 0.0081(16) -0.0003(12) N71 0.0213(14) 0.0270(13) 0.0211(19) -0.0002(12) 0.0028(12) -0.0030(9) C72 0.0222(17) 0.0293(17) 0.018(2) 0.0006(14) 0.0020(14) 0.0003(11) C73 0.0274(19) 0.0323(18) 0.030(3) 0.0020(16) 0.0059(16) 0.0023(12) C74 0.0258(18) 0.0350(19) 0.027(3) 0.0019(16) 0.0043(16) -0.0017(12) N75 0.0269(15) 0.0276(15) 0.019(2) 0.0024(12) 0.0020(12) -0.0012(10) C76 0.0313(19) 0.0242(16) 0.024(3) 0.0018(15) 0.0014(16) -0.0026(11) C81 0.0287(18) 0.0199(15) 0.023(3) -0.0012(14) 0.0011(15) -0.0020(11) C82 0.0234(17) 0.0366(18) 0.026(3) -0.0009(16) 0.0036(16) -0.0021(12) C83 0.034(2) 0.0339(18) 0.021(3) -0.0029(16) 0.0071(16) -0.0028(13) C84 0.0271(17) 0.0221(15) 0.021(3) 0.0007(14) 0.0037(15) 0.0001(11) C85 0.0233(18) 0.046(2) 0.027(3) 0.0072(17) 0.0048(16) 0.0011(13) C86 0.033(2) 0.043(2) 0.016(3) 0.0060(16) 0.0046(16) -0.0012(14) N91 0.0221(14) 0.0313(14) 0.0191(19) -0.0022(13) 0.0039(12) 0.0033(10) C92 0.0195(16) 0.0327(17) 0.022(2) 0.0041(15) -0.0001(14) 0.0005(11) C93 0.0274(18) 0.0325(18) 0.027(3) 0.0027(16) 0.0060(16) -0.0014(12) C94 0.0228(18) 0.0388(19) 0.027(3) 0.0023(17) 0.0061(15) 0.0010(12) N95 0.0247(15) 0.0290(14) 0.021(2) -0.0008(13) 0.0028(12) 0.0022(10) C96 0.0301(18) 0.0260(16) 0.020(2) 0.0003(14) 0.0023(15) 0.0014(11) N101 0.0244(15) 0.0332(15) 0.022(2) -0.0028(13) -0.0010(13) 0.0006(10) C102 0.0259(18) 0.0318(18) 0.021(2) -0.0021(15) -0.0024(15) 0.0012(12) C103 0.0276(19) 0.0346(19) 0.031(3) 0.0044(17) -0.0012(16) 0.0016(13) C104 0.041(2) 0.0281(18) 0.038(3) 0.0028(17) -0.0088(19) 0.0025(13) C105 0.041(2) 0.0344(19) 0.030(3) -0.0064(17) -0.0064(19) 0.0111(14) C106 0.030(2) 0.039(2) 0.029(3) -0.0061(17) -0.0048(17) 0.0084(13) B1 0.031(2) 0.0258(19) 0.025(3) 0.0018(17) 0.0043(18) 0.0013(13) F1A 0.0366(13) 0.0449(13) 0.067(2) -0.0175(12) 0.0029(12) -0.0069(9) F1B 0.0715(18) 0.0464(14) 0.0311(17) 0.0043(12) -0.0086(13) 0.0184(11) F1C 0.0447(13) 0.0382(12) 0.0406(18) -0.0106(11) 0.0032(11) 0.0081(9) F1D 0.0608(16) 0.0562(15) 0.038(2) 0.0065(13) 0.0226(13) -0.0077(11) B2 0.024(2) 0.0256(18) 0.031(3) 0.0010(17) 0.0064(17) 0.0003(12) F2A 0.0363(11) 0.0296(10) 0.0312(15) -0.0024(9) 0.0043(10) -0.0061(7) F2B 0.0390(12) 0.0383(11) 0.0238(15) -0.0028(9) 0.0032(10) 0.0051(8) F2C 0.0481(14) 0.0380(11) 0.0343(17) 0.0109(10) 0.0050(11) 0.0139(9) F2D 0.0297(11) 0.0396(12) 0.058(2) -0.0122(11) 0.0175(11) -0.0080(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.264(3) . ? Ag1 N61 2.302(3) . ? Ag1 N71 2.403(3) . ? Ag1 N21 2.472(3) . ? Ag2 N51 2.255(3) . ? Ag2 N101 2.278(3) . ? Ag2 N91 2.406(3) . ? Ag2 N41 2.456(3) . ? N11 C16 1.343(5) . ? N11 C12 1.348(5) . ? C12 C13 1.393(5) . ? C12 C22 1.464(5) . ? C13 C14 1.376(5) . ? C14 C15 1.383(5) . ? C15 C16 1.387(5) . ? N21 C22 1.335(4) . ? N21 N25 1.353(4) . ? C22 C23 1.409(5) . ? C23 C24 1.377(5) . ? C24 N25 1.350(5) . ? N25 C26 1.455(4) . ? C26 C31 1.515(5) . ? C31 C36 1.386(5) . ? C31 C32 1.394(5) . ? C32 C33 1.390(6) . ? C33 C34 1.394(5) . ? C34 C35 1.399(5) . ? C34 C46 1.518(5) . ? C35 C36 1.386(6) . ? N41 C42 1.340(4) . ? N41 N45 1.348(4) . ? C42 C43 1.402(5) . ? C42 C52 1.471(5) . ? C43 C44 1.367(5) . ? C44 N45 1.354(5) . ? N45 C46 1.451(4) . ? N51 C56 1.336(5) . ? N51 C52 1.360(5) . ? C52 C53 1.395(5) . ? C53 C54 1.386(5) . ? C54 C55 1.399(6) . ? C55 C56 1.380(5) . ? N61 C66 1.341(5) . ? N61 C62 1.349(5) . ? C62 C63 1.397(5) . ? C62 C72 1.467(5) . ? C63 C64 1.383(5) . ? C64 C65 1.382(6) . ? C65 C66 1.381(5) . ? N71 C72 1.347(4) . ? N71 N75 1.348(4) . ? C72 C73 1.407(5) . ? C73 C74 1.379(6) . ? C74 N75 1.342(5) . ? N75 C76 1.462(4) . ? C76 C81 1.513(5) . ? C81 C86 1.381(5) . ? C81 C82 1.394(6) . ? C82 C83 1.397(5) . ? C83 C84 1.387(5) . ? C84 C85 1.388(6) . ? C84 C96 1.508(5) . ? C85 C86 1.400(5) . ? N91 C92 1.347(4) . ? N91 N95 1.358(4) . ? C92 C93 1.406(5) . ? C92 C102 1.470(5) . ? C93 C94 1.371(5) . ? C94 N95 1.347(5) . ? N95 C96 1.464(4) . ? N101 C106 1.339(5) . ? N101 C102 1.350(5) . ? C102 C103 1.396(5) . ? C103 C104 1.385(6) . ? C104 C105 1.386(6) . ? C105 C106 1.369(6) . ? B1 F1B 1.370(5) . ? B1 F1A 1.373(5) . ? B1 F1D 1.390(5) . ? B1 F1C 1.408(5) . ? B2 F2C 1.379(4) . ? B2 F2D 1.392(4) . ? B2 F2A 1.398(4) . ? B2 F2B 1.404(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 N11 Ag1 N61 164.33(11) . . ? N11 Ag1 N71 124.26(10) . . ? N61 Ag1 N71 71.40(10) . . ? N11 Ag1 N21 71.22(10) . . ? N61 Ag1 N21 102.86(9) . . ? N71 Ag1 N21 118.63(11) . . ? N51 Ag2 N101 167.89(11) . . ? N51 Ag2 N91 119.51(10) . . ? N101 Ag2 N91 72.48(10) . . ? N51 Ag2 N41 72.38(10) . . ? N101 Ag2 N41 101.56(10) . . ? N91 Ag2 N41 115.62(10) . . ? C16 N11 C12 118.1(3) . . ? C16 N11 Ag1 123.1(2) . . ? C12 N11 Ag1 117.7(2) . . ? N11 C12 C13 121.3(3) . . ? N11 C12 C22 118.0(3) . . ? C13 C12 C22 120.7(3) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 118.8(3) . . ? C14 C15 C16 118.4(3) . . ? N11 C16 C15 123.3(3) . . ? C22 N21 N25 105.0(3) . . ? C22 N21 Ag1 110.4(2) . . ? N25 N21 Ag1 142.7(2) . . ? N21 C22 C23 111.0(3) . . ? N21 C22 C12 120.0(3) . . ? C23 C22 C12 129.0(3) . . ? C24 C23 C22 104.9(3) . . ? N25 C24 C23 106.8(3) . . ? C24 N25 N21 112.2(3) . . ? C24 N25 C26 127.8(3) . . ? N21 N25 C26 120.0(3) . . ? N25 C26 C31 114.6(3) . . ? C36 C31 C32 118.9(4) . . ? C36 C31 C26 118.3(3) . . ? C32 C31 C26 122.7(3) . . ? C33 C32 C31 120.3(3) . . ? C32 C33 C34 120.8(3) . . ? C33 C34 C35 118.5(4) . . ? C33 C34 C46 123.0(3) . . ? C35 C34 C46 118.6(3) . . ? C36 C35 C34 120.5(3) . . ? C35 C36 C31 120.9(3) . . ? C42 N41 N45 105.0(3) . . ? C42 N41 Ag2 110.2(2) . . ? N45 N41 Ag2 144.4(2) . . ? N41 C42 C43 111.0(3) . . ? N41 C42 C52 119.9(3) . . ? C43 C42 C52 129.1(3) . . ? C44 C43 C42 104.9(3) . . ? N45 C44 C43 107.3(3) . . ? N41 N45 C44 111.7(3) . . ? N41 N45 C46 120.0(3) . . ? C44 N45 C46 127.8(3) . . ? N45 C46 C34 113.3(3) . . ? C56 N51 C52 118.3(3) . . ? C56 N51 Ag2 122.3(2) . . ? C52 N51 Ag2 115.9(2) . . ? N51 C52 C53 121.3(3) . . ? N51 C52 C42 118.1(3) . . ? C53 C52 C42 120.6(3) . . ? C54 C53 C52 119.5(3) . . ? C53 C54 C55 118.8(3) . . ? C56 C55 C54 118.2(4) . . ? N51 C56 C55 123.7(4) . . ? C66 N61 C62 117.8(3) . . ? C66 N61 Ag1 123.4(2) . . ? C62 N61 Ag1 118.1(2) . . ? N61 C62 C63 121.9(3) . . ? N61 C62 C72 116.9(3) . . ? C63 C62 C72 121.2(3) . . ? C64 C63 C62 119.1(4) . . ? C65 C64 C63 119.2(3) . . ? C66 C65 C64 118.3(3) . . ? N61 C66 C65 123.7(4) . . ? C72 N71 N75 104.8(3) . . ? C72 N71 Ag1 113.5(2) . . ? N75 N71 Ag1 141.7(2) . . ? N71 C72 C73 110.9(3) . . ? N71 C72 C62 119.6(3) . . ? C73 C72 C62 129.5(3) . . ? C74 C73 C72 104.5(3) . . ? N75 C74 C73 107.4(3) . . ? C74 N75 N71 112.4(3) . . ? C74 N75 C76 127.6(3) . . ? N71 N75 C76 119.8(3) . . ? N75 C76 C81 111.5(3) . . ? C86 C81 C82 119.2(3) . . ? C86 C81 C76 120.3(4) . . ? C82 C81 C76 120.5(3) . . ? C81 C82 C83 120.4(3) . . ? C84 C83 C82 120.1(4) . . ? C83 C84 C85 119.5(3) . . ? C83 C84 C96 120.6(4) . . ? C85 C84 C96 119.9(3) . . ? C84 C85 C86 120.3(3) . . ? C81 C86 C85 120.4(4) . . ? C92 N91 N95 104.5(3) . . ? C92 N91 Ag2 111.8(2) . . ? N95 N91 Ag2 143.7(2) . . ? N91 C92 C93 110.8(3) . . ? N91 C92 C102 120.0(3) . . ? C93 C92 C102 129.3(3) . . ? C94 C93 C92 105.3(3) . . ? N95 C94 C93 107.0(3) . . ? C94 N95 N91 112.3(3) . . ? C94 N95 C96 127.6(3) . . ? N91 N95 C96 119.6(3) . . ? N95 C96 C84 111.5(3) . . ? C106 N101 C102 117.3(3) . . ? C106 N101 Ag2 123.6(3) . . ? C102 N101 Ag2 116.7(2) . . ? N101 C102 C103 122.0(3) . . ? N101 C102 C92 117.2(3) . . ? C103 C102 C92 120.8(4) . . ? C104 C103 C102 119.2(4) . . ? C105 C104 C103 118.9(4) . . ? C106 C105 C104 118.2(4) . . ? N101 C106 C105 124.5(4) . . ? F1B B1 F1A 111.9(3) . . ? F1B B1 F1D 108.5(3) . . ? F1A B1 F1D 109.5(4) . . ? F1B B1 F1C 109.5(4) . . ? F1A B1 F1C 109.7(3) . . ? F1D B1 F1C 107.5(3) . . ? F2C B2 F2D 110.5(3) . . ? F2C B2 F2A 109.5(3) . . ? F2D B2 F2A 108.3(3) . . ? F2C B2 F2B 110.1(3) . . ? F2D B2 F2B 110.0(3) . . ? F2A B2 F2B 108.5(3) . . ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 70.06 _diffrn_measured_fraction_theta_full 0.830 _refine_diff_density_max 0.755 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.089 #===END data_imw284m _database_code_depnum_ccdc_archive 'CCDC 609494' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H27 Ag B F4 N7 O2' _chemical_formula_weight 724.28 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 16.607(5) _cell_length_b 28.742(9) _cell_length_c 52.334(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 24980(13) _cell_formula_units_Z 32 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11712 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6751 _exptl_absorpt_correction_T_max 0.8423 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46972 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4091 _reflns_number_gt 2374 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2000P)^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 4091 _refine_ls_number_parameters 418 _refine_ls_number_restraints 294 _refine_ls_R_factor_all 0.1758 _refine_ls_R_factor_gt 0.1311 _refine_ls_wR_factor_ref 0.4523 _refine_ls_wR_factor_gt 0.4124 _refine_ls_goodness_of_fit_ref 1.703 _refine_ls_restrained_S_all 1.660 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 1.1250 0.55405(7) 0.6250 0.1043(9) Uani 1 2 d SU . . Ag2 Ag 0.8750 0.3750 0.72767(6) 0.1435(11) Uani 1 2 d SU . . N11 N 1.2381(7) 0.5843(5) 0.6026(3) 0.097(4) Uani 1 1 d U . . C12 C 1.2414(13) 0.6161(6) 0.5839(4) 0.115(5) Uani 1 1 d U . . H12A H 1.1918 0.6294 0.5786 0.138 Uiso 1 1 calc R . . C13 C 1.3071(14) 0.6308(7) 0.5724(4) 0.140(7) Uani 1 1 d U . . H13A H 1.3050 0.6525 0.5587 0.168 Uiso 1 1 calc R . . C14 C 1.3867(11) 0.6113(8) 0.5821(5) 0.128(6) Uani 1 1 d U . . H14A H 1.4364 0.6221 0.5753 0.154 Uiso 1 1 calc R . . C15 C 1.3853(9) 0.5800(7) 0.5994(4) 0.108(5) Uani 1 1 d U . . H15A H 1.4340 0.5662 0.6052 0.130 Uiso 1 1 calc R . . C16 C 1.3098(10) 0.5660(6) 0.6102(3) 0.098(5) Uani 1 1 d U . . N21 N 1.2410(7) 0.5179(4) 0.6401(2) 0.085(3) Uani 1 1 d U . . N22 N 1.2606(5) 0.4867(4) 0.6585(3) 0.095(4) Uani 1 1 d U . . C23 C 1.3392(9) 0.4819(6) 0.6597(3) 0.104(5) Uani 1 1 d U . . H23A H 1.3661 0.4617 0.6713 0.125 Uiso 1 1 calc R . . C24 C 1.3773(8) 0.5097(6) 0.6424(3) 0.106(5) Uani 1 1 d U . . H24 H 1.4331 0.5135 0.6391 0.127 Uiso 1 1 calc R . . C25 C 1.3077(10) 0.5321(6) 0.6305(3) 0.094(4) Uani 1 1 d U . . C31 C 1.1939(10) 0.4636(5) 0.6730(3) 0.103(5) Uani 1 1 d U . . H31A H 1.1546 0.4506 0.6607 0.123 Uiso 1 1 calc R . . H31B H 1.2165 0.4374 0.6830 0.123 Uiso 1 1 calc R . . C32 C 1.1519(10) 0.4952(6) 0.6904(3) 0.099(4) Uani 1 1 d U . . C33 C 1.0715(9) 0.4953(5) 0.6923(3) 0.092(4) Uani 1 1 d U . . H33A H 1.0421 0.4754 0.6812 0.110 Uiso 1 1 calc R . . C34 C 1.0289(10) 0.5222(6) 0.7091(3) 0.101(5) Uani 1 1 d U . . C35 C 1.0669(13) 0.5545(7) 0.7237(4) 0.132(6) Uani 1 1 d U . . H35 H 1.0387 0.5751 0.7347 0.158 Uiso 1 1 calc R . . C36 C 1.1553(15) 0.5551(10) 0.7213(5) 0.173(10) Uani 1 1 d U . . H36A H 1.1857 0.5771 0.7308 0.208 Uiso 1 1 calc R . . C37 C 1.1928(12) 0.5257(9) 0.7062(5) 0.154(8) Uani 1 1 d U . . H37A H 1.2500 0.5254 0.7061 0.184 Uiso 1 1 calc R . . C41 C 0.7702(11) 0.4506(8) 0.6801(4) 0.135(7) Uani 1 1 d U . . H41A H 0.8105 0.4322 0.6705 0.162 Uiso 1 1 calc R . . H41B H 0.7365 0.4677 0.6676 0.162 Uiso 1 1 calc R . . C42 C 0.8103(11) 0.4831(7) 0.6963(4) 0.134(7) Uani 1 1 d U . . C43 C 0.7716(12) 0.5133(9) 0.7133(6) 0.179(10) Uani 1 1 d U . . H43A H 0.7145 0.5159 0.7134 0.215 Uiso 1 1 calc R . . C44 C 0.8199(17) 0.5401(9) 0.7303(6) 0.186(12) Uani 1 1 d U . . H44A H 0.7939 0.5544 0.7444 0.223 Uiso 1 1 calc R . . C45 C 0.8956(15) 0.5461(8) 0.7279(5) 0.171(10) Uani 1 1 d U . . H45A H 0.9225 0.5691 0.7378 0.205 Uiso 1 1 calc R . . C46 C 0.9379(9) 0.5190(5) 0.7109(3) 0.096(4) Uani 1 1 d U . . C47 C 0.8974(10) 0.4872(6) 0.6966(3) 0.107(5) Uani 1 1 d U . . H47A H 0.9278 0.4665 0.6863 0.129 Uiso 1 1 calc R . . N51 N 0.7493(7) 0.3897(5) 0.7126(3) 0.110(5) Uani 1 1 d U . . N52 N 0.7177(8) 0.4183(7) 0.6956(4) 0.133(6) Uani 1 1 d U . . C53 C 0.6391(9) 0.4187(9) 0.6936(5) 0.140(8) Uani 1 1 d U . . H53A H 0.6064 0.4374 0.6829 0.168 Uiso 1 1 calc R . . C54 C 0.6160(10) 0.3859(9) 0.7108(5) 0.144(9) Uani 1 1 d U . . H54 H 0.5620 0.3769 0.7140 0.172 Uiso 1 1 calc R . . C55 C 0.6880(11) 0.3663(8) 0.7236(5) 0.120(6) Uani 1 1 d U . . N61 N 0.7791(11) 0.3302(7) 0.7522(5) 0.164(7) Uani 1 1 d U . . C62 C 0.7031(13) 0.3328(9) 0.7446(5) 0.141(8) Uani 1 1 d U . . C63 C 0.6396(16) 0.3078(12) 0.7556(7) 0.182(12) Uani 1 1 d U . . H63A H 0.5866 0.3163 0.7506 0.218 Uiso 1 1 calc R . . C64 C 0.646(2) 0.2761(15) 0.7711(8) 0.211(16) Uani 1 1 d U . . H64A H 0.6029 0.2565 0.7764 0.254 Uiso 1 1 calc R . . C65 C 0.730(3) 0.2725(12) 0.7802(8) 0.26(2) Uani 1 1 d U . . H65A H 0.7415 0.2489 0.7923 0.313 Uiso 1 1 calc R . . C66 C 0.793(2) 0.3014(12) 0.7724(8) 0.228(16) Uani 1 1 d U . . H66 H 0.8434 0.3009 0.7808 0.273 Uiso 1 1 calc R . . C100 C 0.5113(17) 0.1091(10) 0.8661(5) 0.177(10) Uani 1 1 d U . . H10A H 0.5542 0.1181 0.8542 0.265 Uiso 1 1 calc R . . H10B H 0.4608 0.1050 0.8567 0.265 Uiso 1 1 calc R . . H10C H 0.5258 0.0799 0.8745 0.265 Uiso 1 1 calc R . . N100 N 0.5011(13) 0.1452(8) 0.8852(4) 0.139(6) Uani 1 1 d DU . . O100 O 0.4381(16) 0.1496(13) 0.8952(7) 0.322(18) Uani 1 1 d DU . . O101 O 0.5590(16) 0.1646(10) 0.8923(4) 0.251(12) Uani 1 1 d DU . . B1 B 0.1250 0.1250 0.9589(4) 0.092(7) Uani 1 2 d SDU . . F1 F 0.1751(8) 0.1035(6) 0.9421(3) 0.224(8) Uani 1 1 d DU . . F2 F 0.1733(8) 0.1535(6) 0.9715(3) 0.215(8) Uani 1 1 d DU . . B2 B 0.8750 0.2510(13) 0.8750 0.31(5) Uani 1 2 d SDU . . F3 F 0.9147(13) 0.2384(10) 0.8986(5) 0.40(2) Uani 1 1 d DU . . F4 F 0.9338(8) 0.2842(8) 0.8678(4) 0.250(10) Uani 1 1 d DU . . 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 Ag1 0.0581(11) 0.1360(16) 0.1189(15) 0.000 -0.0080(8) 0.000 Ag2 0.0631(13) 0.151(2) 0.217(3) 0.000 0.000 0.0242(10) N11 0.081(9) 0.103(9) 0.106(9) -0.016(8) -0.006(7) 0.004(7) C12 0.114(15) 0.113(13) 0.119(13) 0.015(12) -0.005(11) -0.008(10) C13 0.116(16) 0.164(18) 0.141(16) 0.022(13) 0.014(13) -0.051(14) C14 0.079(12) 0.151(17) 0.154(17) 0.001(15) 0.032(11) -0.006(11) C15 0.063(9) 0.115(12) 0.147(15) 0.012(12) 0.012(9) -0.010(8) C16 0.085(11) 0.107(11) 0.101(11) -0.026(10) 0.021(9) -0.015(9) N21 0.073(8) 0.083(8) 0.100(8) -0.001(7) 0.004(7) -0.003(6) N22 0.028(5) 0.119(9) 0.137(10) 0.004(8) -0.006(5) 0.008(5) C23 0.073(10) 0.110(11) 0.129(13) 0.011(10) -0.002(9) -0.002(8) C24 0.050(8) 0.126(13) 0.142(13) 0.011(11) 0.000(9) 0.008(8) C25 0.077(10) 0.086(9) 0.120(12) -0.007(9) -0.019(9) -0.009(8) C31 0.097(11) 0.096(10) 0.114(11) 0.022(10) 0.024(9) -0.004(9) C32 0.085(10) 0.104(11) 0.108(11) -0.004(10) 0.017(9) -0.001(9) C33 0.079(10) 0.088(10) 0.109(11) 0.009(9) 0.000(8) -0.003(8) C34 0.096(11) 0.096(11) 0.111(11) -0.008(10) -0.005(9) 0.023(9) C35 0.107(14) 0.144(16) 0.145(15) -0.028(13) -0.008(12) 0.012(12) C36 0.129(18) 0.23(3) 0.16(2) -0.094(19) -0.007(15) -0.062(17) C37 0.090(13) 0.21(2) 0.164(19) -0.057(17) 0.007(12) -0.043(14) C41 0.081(12) 0.174(19) 0.150(16) -0.033(15) -0.005(11) 0.013(12) C42 0.084(12) 0.142(15) 0.177(18) -0.048(14) 0.003(12) 0.043(11) C43 0.072(12) 0.164(19) 0.30(3) -0.02(2) 0.041(16) -0.023(13) C44 0.127(19) 0.17(2) 0.26(3) -0.11(2) 0.04(2) -0.007(16) C45 0.137(18) 0.161(19) 0.21(2) -0.076(17) 0.092(17) -0.058(15) C46 0.066(9) 0.105(11) 0.117(12) -0.010(10) 0.008(8) 0.014(8) C47 0.097(11) 0.118(13) 0.107(11) 0.001(10) -0.006(9) 0.016(10) N51 0.047(7) 0.128(11) 0.154(12) -0.033(9) -0.027(8) 0.016(7) N52 0.059(9) 0.166(15) 0.173(15) -0.073(13) 0.000(9) 0.000(9) C53 0.026(8) 0.22(2) 0.179(19) -0.011(17) -0.009(9) 0.004(10) C54 0.040(9) 0.20(2) 0.19(2) -0.104(18) 0.012(11) -0.001(11) C55 0.058(11) 0.147(16) 0.156(17) -0.056(14) 0.004(10) -0.017(10) N61 0.095(12) 0.161(15) 0.24(2) 0.006(15) 0.064(13) 0.037(11) C62 0.090(15) 0.164(19) 0.17(2) -0.083(17) 0.017(14) 0.023(13) C63 0.105(17) 0.21(3) 0.23(3) 0.00(2) 0.087(19) 0.028(18) C64 0.17(3) 0.23(4) 0.24(4) -0.02(3) 0.01(2) 0.10(3) C65 0.31(5) 0.20(3) 0.27(3) 0.10(3) 0.19(4) 0.07(3) C66 0.15(3) 0.22(3) 0.31(4) 0.10(3) -0.03(3) 0.03(2) C100 0.18(2) 0.21(2) 0.135(16) -0.078(18) -0.014(16) 0.01(2) N100 0.098(12) 0.168(15) 0.151(15) -0.008(13) -0.007(11) -0.004(12) O100 0.140(18) 0.43(4) 0.39(4) -0.16(3) -0.04(2) 0.05(2) O101 0.21(2) 0.35(3) 0.199(18) -0.067(18) -0.022(16) -0.09(2) B1 0.056(12) 0.090(15) 0.13(2) 0.000 0.000 -0.006(12) F1 0.142(11) 0.267(16) 0.262(16) -0.158(14) 0.060(10) -0.041(10) F2 0.116(9) 0.308(18) 0.220(13) -0.154(13) 0.021(9) -0.059(11) B2 0.37(10) 0.33(9) 0.23(6) 0.000 -0.06(7) 0.000 F3 0.21(2) 0.34(3) 0.66(6) 0.23(4) 0.13(3) 0.02(2) F4 0.082(8) 0.30(2) 0.37(2) 0.119(18) -0.039(10) -0.073(11) _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 Ag1 N21 2.327(12) . ? Ag1 N21 2.328(12) 11_655 ? Ag1 N11 2.380(13) 11_655 ? Ag1 N11 2.380(14) . ? Ag2 N51 2.271(13) . ? Ag2 N51 2.271(13) 2_655 ? Ag2 N61 2.417(19) 2_655 ? Ag2 N61 2.417(19) . ? N11 C12 1.34(2) . ? N11 C16 1.36(2) . ? C12 C13 1.32(3) . ? C13 C14 1.52(3) . ? C14 C15 1.28(3) . ? C15 C16 1.43(2) . ? C16 C25 1.44(2) . ? N21 C25 1.283(19) . ? N21 N22 1.354(15) . ? N22 C23 1.314(18) . ? N22 C31 1.499(18) . ? C23 C24 1.36(2) . ? C24 C25 1.46(2) . ? C31 C32 1.46(2) . ? C32 C33 1.34(2) . ? C32 C37 1.38(2) . ? C33 C34 1.37(2) . ? C34 C35 1.36(2) . ? C34 C46 1.52(2) . ? C35 C36 1.47(3) . ? C36 C37 1.31(3) . ? C41 C42 1.43(2) . ? C41 N52 1.51(3) . ? C42 C43 1.40(3) . ? C42 C47 1.45(2) . ? C43 C44 1.43(3) . ? C44 C45 1.27(3) . ? C45 C46 1.38(2) . ? C46 C47 1.36(2) . ? N51 N52 1.32(2) . ? N51 C55 1.35(2) . ? N52 C53 1.31(2) . ? C53 C54 1.36(3) . ? C54 C55 1.48(3) . ? C55 C62 1.48(3) . ? N61 C62 1.32(3) . ? N61 C66 1.36(4) . ? C62 C63 1.40(3) . ? C63 C64 1.22(4) . ? C64 C65 1.47(6) . ? C65 C66 1.40(4) . ? C100 N100 1.45(3) . ? N100 O101 1.173(19) . ? N100 O100 1.18(2) . ? B1 F2 1.324(13) . ? B1 F2 1.324(13) 14_445 ? B1 F1 1.356(14) 14_445 ? B1 F1 1.356(14) . ? B2 F4 1.42(2) 3_656 ? B2 F4 1.42(2) . ? B2 F3 1.444(17) . ? B2 F3 1.444(17) 3_656 ? 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 N21 Ag1 N21 126.9(6) . 11_655 ? N21 Ag1 N11 130.5(4) . 11_655 ? N21 Ag1 N11 71.2(5) 11_655 11_655 ? N21 Ag1 N11 71.2(5) . . ? N21 Ag1 N11 130.4(4) 11_655 . ? N11 Ag1 N11 137.1(6) 11_655 . ? N51 Ag2 N51 139.3(8) . 2_655 ? N51 Ag2 N61 133.7(6) . 2_655 ? N51 Ag2 N61 71.2(7) 2_655 2_655 ? N51 Ag2 N61 71.2(7) . . ? N51 Ag2 N61 133.7(6) 2_655 . ? N61 Ag2 N61 115.9(12) 2_655 . ? C12 N11 C16 116.3(15) . . ? C12 N11 Ag1 129.9(12) . . ? C16 N11 Ag1 113.9(11) . . ? C13 C12 N11 126(2) . . ? C12 C13 C14 117(2) . . ? C15 C14 C13 118.6(17) . . ? C14 C15 C16 119.6(18) . . ? N11 C16 C15 122.8(17) . . ? N11 C16 C25 117.1(13) . . ? C15 C16 C25 120.0(16) . . ? C25 N21 N22 106.3(12) . . ? C25 N21 Ag1 116.1(10) . . ? N22 N21 Ag1 137.4(8) . . ? C23 N22 N21 110.1(13) . . ? C23 N22 C31 131.5(15) . . ? N21 N22 C31 118.4(10) . . ? N22 C23 C24 111.5(16) . . ? C23 C24 C25 100.1(14) . . ? N21 C25 C16 121.6(14) . . ? N21 C25 C24 112.1(15) . . ? C16 C25 C24 126.3(16) . . ? C32 C31 N22 113.3(13) . . ? C33 C32 C37 116.3(16) . . ? C33 C32 C31 121.6(16) . . ? C37 C32 C31 122.0(17) . . ? C32 C33 C34 124.4(16) . . ? C35 C34 C33 120.5(17) . . ? C35 C34 C46 118.1(15) . . ? C33 C34 C46 121.3(16) . . ? C34 C35 C36 115.1(18) . . ? C37 C36 C35 121.0(19) . . ? C36 C37 C32 122.3(19) . . ? C42 C41 N52 110.6(18) . . ? C43 C42 C41 124.6(18) . . ? C43 C42 C47 113.5(19) . . ? C41 C42 C47 121.8(17) . . ? C42 C43 C44 118.3(19) . . ? C45 C44 C43 125(2) . . ? C44 C45 C46 119(2) . . ? C47 C46 C45 119.0(17) . . ? C47 C46 C34 120.0(14) . . ? C45 C46 C34 120.9(17) . . ? C46 C47 C42 123.7(16) . . ? N52 N51 C55 107.3(15) . . ? N52 N51 Ag2 135.6(12) . . ? C55 N51 Ag2 117.0(15) . . ? C53 N52 N51 117(2) . . ? C53 N52 C41 122(2) . . ? N51 N52 C41 121.1(14) . . ? N52 C53 C54 103(2) . . ? C53 C54 C55 109.6(18) . . ? N51 C55 C54 103(2) . . ? N51 C55 C62 120.8(19) . . ? C54 C55 C62 136(2) . . ? C62 N61 C66 115(2) . . ? C62 N61 Ag2 116(2) . . ? C66 N61 Ag2 129(2) . . ? N61 C62 C63 124(3) . . ? N61 C62 C55 115(2) . . ? C63 C62 C55 121(2) . . ? C64 C63 C62 126(4) . . ? C63 C64 C65 110(4) . . ? C66 C65 C64 125(3) . . ? N61 C66 C65 118(3) . . ? O101 N100 O100 122(3) . . ? O101 N100 C100 118(2) . . ? O100 N100 C100 119(3) . . ? F2 B1 F2 120(2) . 14_445 ? F2 B1 F1 114.4(11) . 14_445 ? F2 B1 F1 103.5(8) 14_445 14_445 ? F2 B1 F1 103.5(8) . . ? F2 B1 F1 114.4(11) 14_445 . ? F1 B1 F1 100(2) 14_445 . ? F4 B2 F4 95(3) 3_656 . ? F4 B2 F3 104.9(18) 3_656 . ? F4 B2 F3 94.6(13) . . ? F4 B2 F3 94.6(12) 3_656 3_656 ? F4 B2 F3 104.9(18) . 3_656 ? F3 B2 F3 151(4) . 3_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.121 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.141 #===END data_imw619 _database_code_depnum_ccdc_archive 'CCDC 609495' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C135 H131 Ag4 B4 F16 N25 O3' _chemical_formula_weight 2930.37 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 18.6570(10) _cell_length_b 14.6839(7) _cell_length_c 24.3229(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.321(3) _cell_angle_gamma 90.00 _cell_volume 6593.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4741 _cell_measurement_theta_min 5.16 _cell_measurement_theta_max 42.86 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9061 _exptl_absorpt_correction_T_max 0.9360 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42909 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 21.57 _reflns_number_total 7638 _reflns_number_gt 5361 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1100P)^2^+29.8000P] 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 7638 _refine_ls_number_parameters 819 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.011 _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 Ag1 Ag 0.66395(5) 0.53082(6) 0.05401(3) 0.0585(3) Uani 1 1 d . . . Ag2 Ag 0.83604(4) 0.99063(5) -0.09695(3) 0.0538(3) Uani 1 1 d . . . N11A N 0.8962(4) 1.0792(5) -0.1562(3) 0.0395(18) Uani 1 1 d . . . C12A C 0.9283(5) 1.0312(6) -0.1936(4) 0.038(2) Uani 1 1 d . . . C13A C 0.9613(5) 1.0738(6) -0.2343(4) 0.044(2) Uani 1 1 d . . . H13A H 0.9847 1.0388 -0.2593 0.053 Uiso 1 1 calc R . . C14A C 0.9598(5) 1.1674(7) -0.2380(4) 0.054(3) Uani 1 1 d . . . H14A H 0.9805 1.1977 -0.2664 0.065 Uiso 1 1 calc R . . C15A C 0.9280(6) 1.2163(7) -0.2001(5) 0.059(3) Uani 1 1 d . . . H15A H 0.9277 1.2810 -0.2011 0.071 Uiso 1 1 calc R . . C16A C 0.8959(5) 1.1698(7) -0.1597(4) 0.050(3) Uani 1 1 d . . . H16A H 0.8732 1.2039 -0.1339 0.060 Uiso 1 1 calc R . . N21A N 0.8898(4) 0.8936(5) -0.1522(3) 0.0332(17) Uani 1 1 d . . . N22A N 0.9000(4) 0.8030(5) -0.1563(3) 0.0372(18) Uani 1 1 d . . . C23A C 0.9456(5) 0.7854(7) -0.1941(4) 0.046(2) Uani 1 1 d . . . H23A H 0.9618 0.7270 -0.2038 0.055 Uiso 1 1 calc R . . C24A C 0.9635(5) 0.8663(6) -0.2152(4) 0.041(2) Uani 1 1 d . . . H24A H 0.9942 0.8759 -0.2426 0.049 Uiso 1 1 calc R . . C25A C 0.9280(4) 0.9317(6) -0.1887(3) 0.034(2) Uani 1 1 d . . . C31A C 0.8661(5) 0.7403(6) -0.1220(3) 0.041(2) Uani 1 1 d . . . H31A H 0.8677 0.6781 -0.1374 0.049 Uiso 1 1 calc R . . H31B H 0.8146 0.7574 -0.1231 0.049 Uiso 1 1 calc R . . C32A C 0.9024(5) 0.7400(5) -0.0626(4) 0.039(2) Uani 1 1 d . . . C33A C 0.8642(5) 0.7656(5) -0.0201(4) 0.037(2) Uani 1 1 d . . . H33A H 0.8155 0.7854 -0.0294 0.044 Uiso 1 1 calc R . . C34A C 0.8949(5) 0.7631(5) 0.0358(3) 0.035(2) Uani 1 1 d . . . C35A C 0.9670(5) 0.7361(6) 0.0481(4) 0.043(2) Uani 1 1 d . . . H35A H 0.9896 0.7341 0.0856 0.052 Uiso 1 1 calc R . . C36A C 1.0059(5) 0.7121(6) 0.0060(4) 0.051(3) Uani 1 1 d . . . H36A H 1.0552 0.6945 0.0151 0.061 Uiso 1 1 calc R . . C37A C 0.9742(5) 0.7132(6) -0.0490(4) 0.044(2) Uani 1 1 d . . . H37A H 1.0014 0.6958 -0.0774 0.053 Uiso 1 1 calc R . . C41A C 0.6547(5) 0.7801(6) 0.1046(4) 0.046(2) Uani 1 1 d . . . H41A H 0.6300 0.8377 0.1118 0.055 Uiso 1 1 calc R . . H41B H 0.6401 0.7642 0.0650 0.055 Uiso 1 1 calc R . . C42A C 0.7348(5) 0.7954(6) 0.1147(4) 0.042(2) Uani 1 1 d . . . C43A C 0.7774(5) 0.7705(5) 0.0732(3) 0.035(2) Uani 1 1 d . . . H43A H 0.7548 0.7422 0.0401 0.042 Uiso 1 1 calc R . . C44A C 0.8516(5) 0.7868(5) 0.0800(3) 0.035(2) Uani 1 1 d . . . C45A C 0.8830(5) 0.8264(6) 0.1297(4) 0.045(2) Uani 1 1 d . . . H45A H 0.9336 0.8377 0.1355 0.053 Uiso 1 1 calc R . . C46A C 0.8420(6) 0.8499(6) 0.1714(4) 0.051(3) Uani 1 1 d . . . H46A H 0.8647 0.8764 0.2052 0.062 Uiso 1 1 calc R . . C47A C 0.7691(5) 0.8346(6) 0.1632(4) 0.047(2) Uani 1 1 d . . . H47A H 0.7412 0.8513 0.1914 0.056 Uiso 1 1 calc R . . N51A N 0.6244(4) 0.6224(5) 0.1221(3) 0.0405(18) Uani 1 1 d . . . N52A N 0.6299(4) 0.7086(5) 0.1389(3) 0.0420(19) Uani 1 1 d . . . C53A C 0.6102(5) 0.7173(7) 0.1904(4) 0.052(3) Uani 1 1 d . . . H53A H 0.6110 0.7718 0.2116 0.063 Uiso 1 1 calc R . . C54A C 0.5894(5) 0.6346(7) 0.2058(4) 0.051(3) Uani 1 1 d . . . H54A H 0.5717 0.6194 0.2394 0.061 Uiso 1 1 calc R . . C55A C 0.5991(5) 0.5755(6) 0.1624(4) 0.038(2) Uani 1 1 d . . . N61A N 0.6057(4) 0.4388(5) 0.1106(3) 0.053(2) Uani 1 1 d . . . C62A C 0.5852(5) 0.4770(6) 0.1555(4) 0.038(2) Uani 1 1 d . . . C63A C 0.5525(5) 0.4283(7) 0.1934(4) 0.045(2) Uani 1 1 d . . . H63A H 0.5381 0.4574 0.2249 0.054 Uiso 1 1 calc R . . C64A C 0.5412(6) 0.3363(7) 0.1846(4) 0.057(3) Uani 1 1 d . . . H64A H 0.5198 0.3010 0.2106 0.068 Uiso 1 1 calc R . . C65A C 0.5605(6) 0.2964(7) 0.1389(5) 0.066(3) Uani 1 1 d . . . H65A H 0.5526 0.2332 0.1322 0.080 Uiso 1 1 calc R . . C66A C 0.5924(6) 0.3502(7) 0.1019(5) 0.072(3) Uani 1 1 d . . . H66A H 0.6051 0.3228 0.0692 0.087 Uiso 1 1 calc R . . N11B N 0.8578(4) 1.0241(5) -0.0007(3) 0.0432(19) Uani 1 1 d . . . C12B C 0.8008(5) 1.0139(6) 0.0267(4) 0.041(2) Uani 1 1 d . . . C13B C 0.8039(6) 1.0324(6) 0.0823(4) 0.047(2) Uani 1 1 d . . . H13B H 0.7626 1.0234 0.1004 0.057 Uiso 1 1 calc R . . C14B C 0.8669(6) 1.0637(7) 0.1110(4) 0.055(3) Uani 1 1 d . . . H14B H 0.8703 1.0768 0.1496 0.066 Uiso 1 1 calc R . . C15B C 0.9254(6) 1.0762(7) 0.0837(4) 0.056(3) Uani 1 1 d . . . H15B H 0.9700 1.0984 0.1030 0.068 Uiso 1 1 calc R . . C16B C 0.9186(5) 1.0563(6) 0.0286(4) 0.051(3) Uani 1 1 d . . . H16B H 0.9592 1.0658 0.0099 0.061 Uiso 1 1 calc R . . N21B N 0.7289(4) 0.9829(5) -0.0632(3) 0.0369(18) Uani 1 1 d . . . N22B N 0.6591(4) 0.9646(5) -0.0829(3) 0.0405(19) Uani 1 1 d . . . C23B C 0.6191(6) 0.9558(7) -0.0417(4) 0.054(3) Uani 1 1 d . . . H23B H 0.5688 0.9422 -0.0458 0.065 Uiso 1 1 calc R . . C24B C 0.6634(5) 0.9697(6) 0.0070(4) 0.050(3) Uani 1 1 d . . . H24B H 0.6506 0.9684 0.0434 0.060 Uiso 1 1 calc R . . C25B C 0.7322(5) 0.9866(6) -0.0078(4) 0.039(2) Uani 1 1 d . . . C31B C 0.6376(5) 0.9554(6) -0.1427(4) 0.048(2) Uani 1 1 d . . . H31C H 0.5843 0.9618 -0.1512 0.057 Uiso 1 1 calc R . . H31D H 0.6596 1.0057 -0.1617 0.057 Uiso 1 1 calc R . . C32B C 0.6593(5) 0.8670(6) -0.1654(4) 0.043(2) Uani 1 1 d . . . C33B C 0.7067(5) 0.8643(6) -0.2042(4) 0.040(2) Uani 1 1 d . . . H33B H 0.7276 0.9198 -0.2143 0.049 Uiso 1 1 calc R . . C34B C 0.7253(5) 0.7840(6) -0.2290(4) 0.042(2) Uani 1 1 d . . . C35B C 0.6940(6) 0.7046(7) -0.2115(5) 0.061(3) Uani 1 1 d . . . H35B H 0.7046 0.6480 -0.2274 0.073 Uiso 1 1 calc R . . C36B C 0.6487(6) 0.7059(7) -0.1723(5) 0.067(3) Uani 1 1 d . . . H36B H 0.6295 0.6503 -0.1607 0.080 Uiso 1 1 calc R . . C37B C 0.6310(6) 0.7844(7) -0.1499(4) 0.058(3) Uani 1 1 d . . . H37B H 0.5986 0.7840 -0.1232 0.070 Uiso 1 1 calc R . . C41B C 0.8565(5) 0.5529(6) 0.1348(4) 0.050(3) Uani 1 1 d . . . H41C H 0.8217 0.6007 0.1423 0.061 Uiso 1 1 calc R . . H41D H 0.9058 0.5741 0.1499 0.061 Uiso 1 1 calc R . . C42B C 0.8404(5) 0.4670(6) 0.1642(4) 0.041(2) Uani 1 1 d . . . C43B C 0.7902(5) 0.4659(6) 0.2009(4) 0.039(2) Uani 1 1 d . . . H43B H 0.7647 0.5201 0.2069 0.047 Uiso 1 1 calc R . . C44B C 0.7763(5) 0.3870(6) 0.2293(4) 0.038(2) Uani 1 1 d . . . C45B C 0.8133(5) 0.3077(6) 0.2193(4) 0.049(3) Uani 1 1 d . . . H45B H 0.8038 0.2530 0.2377 0.058 Uiso 1 1 calc R . . C46B C 0.8636(5) 0.3077(7) 0.1830(4) 0.055(3) Uani 1 1 d . . . H46B H 0.8889 0.2534 0.1768 0.066 Uiso 1 1 calc R . . C47B C 0.8769(5) 0.3865(7) 0.1560(4) 0.052(3) Uani 1 1 d . . . H47B H 0.9117 0.3862 0.1311 0.062 Uiso 1 1 calc R . . N51B N 0.7860(4) 0.5365(5) 0.0429(3) 0.0432(19) Uani 1 1 d . . . N52B N 0.8519(5) 0.5407(5) 0.0748(3) 0.046(2) Uani 1 1 d . . . C53B C 0.9054(6) 0.5243(6) 0.0434(5) 0.052(3) Uani 1 1 d . . . H53B H 0.9560 0.5225 0.0563 0.062 Uiso 1 1 calc R . . C54B C 0.8737(6) 0.5114(6) -0.0089(4) 0.051(3) Uani 1 1 d . . . H54B H 0.8973 0.4994 -0.0402 0.061 Uiso 1 1 calc R . . C55B C 0.7990(5) 0.5190(6) -0.0086(4) 0.044(2) Uani 1 1 d . . . N61B N 0.6704(5) 0.5108(5) -0.0392(3) 0.048(2) Uani 1 1 d . . . C62B C 0.7379(6) 0.5062(6) -0.0528(4) 0.048(3) Uani 1 1 d . . . C63B C 0.7492(6) 0.4900(6) -0.1078(4) 0.055(3) Uani 1 1 d . . . H63B H 0.7967 0.4899 -0.1176 0.066 Uiso 1 1 calc R . . C64B C 0.6895(7) 0.4741(7) -0.1476(4) 0.062(3) Uani 1 1 d . . . H64B H 0.6957 0.4633 -0.1852 0.074 Uiso 1 1 calc R . . C65B C 0.6226(7) 0.4739(7) -0.1331(4) 0.060(3) Uani 1 1 d . . . H65B H 0.5817 0.4601 -0.1598 0.072 Uiso 1 1 calc R . . C66B C 0.6140(6) 0.4937(7) -0.0793(5) 0.058(3) Uani 1 1 d . . . H66B H 0.5664 0.4956 -0.0699 0.070 Uiso 1 1 calc R . . B10 B 0.0855(5) 0.9874(6) 0.6585(4) 0.053(3) Uiso 0.328(16) 1 d PD A 1 F11 F 0.051(2) 0.950(3) 0.6104(11) 0.26(3) Uiso 0.328(16) 1 d PD A 1 F12 F 0.0611(11) 1.0715(9) 0.6694(8) 0.067(7) Uiso 0.328(16) 1 d PD A 1 F13 F 0.1583(8) 0.9847(19) 0.6559(12) 0.101(10) Uiso 0.328(16) 1 d PD A 1 F14 F 0.0741(14) 0.9227(12) 0.6987(9) 0.089(8) Uiso 0.328(16) 1 d PD A 1 B10' B 0.0855(5) 0.9874(6) 0.6585(4) 0.053(3) Uiso 0.67 1 d PD A 2 F11' F 0.0467(7) 1.0198(10) 0.6086(5) 0.126(5) Uiso 0.672(16) 1 d PD A 2 F12' F 0.1011(7) 1.0599(7) 0.6936(4) 0.086(4) Uiso 0.672(16) 1 d PD A 2 F13' F 0.1476(6) 0.9581(9) 0.6411(5) 0.087(4) Uiso 0.672(16) 1 d PD A 2 F14' F 0.0418(5) 0.9222(5) 0.6736(4) 0.053(3) Uiso 0.672(16) 1 d PD A 2 B20 B 0.4251(4) 0.5159(5) 0.3144(3) 0.036(3) Uiso 0.436(14) 1 d PD B 1 F21 F 0.4334(9) 0.4288(8) 0.2911(7) 0.090(6) Uiso 0.436(14) 1 d PD B 1 F22 F 0.4451(8) 0.4998(11) 0.3695(5) 0.085(6) Uiso 0.436(14) 1 d PD B 1 F23 F 0.4825(7) 0.5625(7) 0.2962(6) 0.041(4) Uiso 0.436(14) 1 d PD B 1 F24 F 0.3585(6) 0.5453(12) 0.2964(6) 0.070(5) Uiso 0.436(14) 1 d PD B 1 B20' B 0.4251(4) 0.5159(5) 0.3144(3) 0.036(3) Uiso 0.56 1 d PD B 2 F21' F 0.4539(7) 0.4349(8) 0.3312(7) 0.107(5) Uiso 0.564(14) 1 d PD B 2 F22' F 0.4568(7) 0.5629(7) 0.2766(5) 0.058(3) Uiso 0.564(14) 1 d PD B 2 F23' F 0.4236(6) 0.5692(8) 0.3621(4) 0.082(4) Uiso 0.564(14) 1 d PD B 2 F24' F 0.3538(5) 0.4977(10) 0.2921(5) 0.072(4) Uiso 0.564(14) 1 d PD B 2 O1 O 0.3523(4) 0.7338(5) 0.0171(3) 0.073(2) Uani 1 1 d . . . C2 C 0.2805(6) 0.7684(7) 0.0015(5) 0.074(3) Uani 1 1 d . . . H2 H 0.2846 0.8326 -0.0115 0.089 Uiso 1 1 calc R . . C3 C 0.2381(7) 0.7699(9) 0.0505(6) 0.096(4) Uani 1 1 d . . . H3A H 0.2325 0.7075 0.0636 0.144 Uiso 1 1 calc R . . H3B H 0.1902 0.7967 0.0388 0.144 Uiso 1 1 calc R . . H3C H 0.2644 0.8064 0.0806 0.144 Uiso 1 1 calc R . . C4 C 0.2412(7) 0.7152(9) -0.0455(6) 0.096(4) Uani 1 1 d . . . H4A H 0.2628 0.7271 -0.0792 0.143 Uiso 1 1 calc R . . H4B H 0.1902 0.7334 -0.0516 0.143 Uiso 1 1 calc R . . H4C H 0.2448 0.6501 -0.0366 0.143 Uiso 1 1 calc R . . C5 C 0.4039(7) 0.7974(8) 0.0453(5) 0.076(3) Uani 1 1 d . . . H5 H 0.3774 0.8522 0.0563 0.091 Uiso 1 1 calc R . . C6 C 0.4437(8) 0.7523(10) 0.0978(5) 0.108(5) Uani 1 1 d . . . H6A H 0.4084 0.7309 0.1210 0.162 Uiso 1 1 calc R . . H6B H 0.4763 0.7966 0.1186 0.162 Uiso 1 1 calc R . . H6C H 0.4720 0.7005 0.0873 0.162 Uiso 1 1 calc R . . C7 C 0.4604(8) 0.8282(9) 0.0073(6) 0.105(5) Uani 1 1 d . . . H7A H 0.4900 0.7759 -0.0005 0.157 Uiso 1 1 calc R . . H7B H 0.4918 0.8756 0.0263 0.157 Uiso 1 1 calc R . . H7C H 0.4349 0.8525 -0.0277 0.157 Uiso 1 1 calc R . . O1S O 0.7403(10) 0.0671(10) 0.7653(7) 0.084(5) Uiso 0.50 1 d PD C -1 C2S C 0.7500 0.1386(12) 0.7500 0.111(7) Uiso 1 2 d SD C -1 H2S H 0.7706 0.1259 0.7173 0.134 Uiso 0.50 1 calc PR C -1 N3S N 0.7500 0.2241(8) 0.7500 0.062(3) Uiso 1 2 d SD . . C4S C 0.7225(10) 0.2698(12) 0.7943(7) 0.150 Uiso 1 1 d D C . H4S1 H 0.7125 0.2372 0.8266 0.225 Uiso 1 1 d R . . H4S2 H 0.6797 0.3017 0.7780 0.225 Uiso 1 1 d R . . H4S3 H 0.7608 0.3127 0.8049 0.225 Uiso 1 1 d 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 Ag1 0.0682(6) 0.0644(6) 0.0525(5) -0.0053(4) 0.0413(4) -0.0068(4) Ag2 0.0546(5) 0.0661(6) 0.0472(5) -0.0084(4) 0.0291(4) 0.0025(4) N11A 0.040(4) 0.043(5) 0.035(5) -0.002(4) 0.008(4) 0.002(4) C12A 0.028(5) 0.050(6) 0.036(6) 0.000(5) 0.003(4) -0.006(4) C13A 0.051(6) 0.051(6) 0.033(6) 0.004(5) 0.007(5) -0.008(5) C14A 0.057(7) 0.061(7) 0.045(6) 0.014(6) 0.006(5) -0.011(5) C15A 0.060(7) 0.040(6) 0.071(8) 0.010(6) -0.006(6) -0.009(5) C16A 0.047(6) 0.042(6) 0.063(7) -0.006(5) 0.012(5) -0.002(5) N21A 0.035(4) 0.039(5) 0.028(4) -0.002(3) 0.012(3) 0.002(3) N22A 0.045(5) 0.039(5) 0.032(4) -0.001(3) 0.018(4) 0.005(3) C23A 0.049(6) 0.057(7) 0.033(6) -0.013(5) 0.006(5) 0.003(5) C24A 0.048(6) 0.052(6) 0.027(5) -0.001(5) 0.016(4) -0.007(5) C25A 0.030(5) 0.046(6) 0.026(5) -0.003(4) 0.005(4) 0.002(4) C31A 0.050(6) 0.037(5) 0.037(6) -0.005(4) 0.013(5) 0.002(4) C32A 0.047(6) 0.028(5) 0.045(6) 0.001(4) 0.015(5) -0.004(4) C33A 0.034(5) 0.036(5) 0.041(6) -0.001(4) 0.008(5) 0.003(4) C34A 0.043(6) 0.028(5) 0.034(6) 0.005(4) 0.009(4) 0.005(4) C35A 0.050(6) 0.038(5) 0.041(6) 0.008(4) 0.006(5) 0.003(5) C36A 0.034(5) 0.054(6) 0.066(8) 0.003(5) 0.014(6) 0.003(5) C37A 0.049(6) 0.046(6) 0.041(6) -0.003(5) 0.019(5) 0.002(5) C41A 0.060(7) 0.039(5) 0.045(6) 0.005(5) 0.026(5) 0.007(5) C42A 0.058(7) 0.028(5) 0.043(6) 0.010(4) 0.020(5) 0.003(4) C43A 0.055(6) 0.024(5) 0.028(5) 0.002(4) 0.012(4) 0.004(4) C44A 0.046(6) 0.029(5) 0.031(5) 0.000(4) 0.013(4) 0.006(4) C45A 0.055(6) 0.037(5) 0.041(6) 0.008(5) 0.007(5) 0.002(4) C46A 0.074(8) 0.051(6) 0.030(6) -0.004(5) 0.010(5) -0.005(5) C47A 0.058(7) 0.055(6) 0.032(6) 0.003(5) 0.018(5) 0.000(5) N51A 0.049(5) 0.038(5) 0.039(5) -0.001(4) 0.022(4) 0.005(4) N52A 0.050(5) 0.036(5) 0.046(5) 0.000(4) 0.027(4) 0.006(4) C53A 0.068(7) 0.053(7) 0.043(6) -0.006(5) 0.033(5) -0.001(5) C54A 0.061(7) 0.056(7) 0.043(6) 0.004(5) 0.030(5) -0.003(5) C55A 0.039(5) 0.047(6) 0.033(6) 0.004(5) 0.019(4) 0.004(4) N61A 0.065(6) 0.042(5) 0.058(6) -0.008(4) 0.034(5) -0.010(4) C62A 0.038(5) 0.041(6) 0.038(6) 0.008(5) 0.015(4) 0.004(4) C63A 0.050(6) 0.054(7) 0.032(6) 0.004(5) 0.015(5) -0.005(5) C64A 0.067(7) 0.064(8) 0.041(6) 0.008(6) 0.014(5) -0.018(6) C65A 0.085(8) 0.048(6) 0.070(8) -0.001(6) 0.026(7) -0.018(6) C66A 0.095(9) 0.054(7) 0.078(8) -0.018(6) 0.049(7) -0.023(6) N11B 0.042(5) 0.043(5) 0.046(5) -0.007(4) 0.011(4) 0.009(4) C12B 0.051(6) 0.030(5) 0.044(6) 0.001(4) 0.010(5) 0.008(4) C13B 0.070(7) 0.036(5) 0.035(6) 0.001(4) 0.005(5) -0.001(5) C14B 0.080(8) 0.049(6) 0.036(6) 0.001(5) 0.006(6) -0.002(6) C15B 0.073(8) 0.047(6) 0.043(7) -0.001(5) -0.014(6) 0.006(5) C16B 0.048(7) 0.037(6) 0.067(8) -0.003(5) 0.012(6) 0.005(5) N21B 0.034(5) 0.043(4) 0.037(5) 0.002(3) 0.016(4) 0.005(3) N22B 0.034(5) 0.053(5) 0.036(5) 0.006(4) 0.011(4) -0.002(4) C23B 0.043(6) 0.067(7) 0.055(7) 0.012(5) 0.019(6) 0.005(5) C24B 0.053(7) 0.055(6) 0.046(7) 0.012(5) 0.021(6) 0.003(5) C25B 0.040(6) 0.039(5) 0.040(6) 0.006(4) 0.010(5) 0.004(4) C31B 0.048(6) 0.058(6) 0.036(6) 0.007(5) 0.003(5) -0.004(5) C32B 0.040(6) 0.049(6) 0.040(6) 0.006(5) 0.004(5) -0.003(5) C33B 0.042(6) 0.036(6) 0.038(6) 0.009(4) -0.010(5) -0.010(4) C34B 0.045(6) 0.038(5) 0.039(6) 0.000(4) -0.002(4) -0.001(4) C35B 0.076(8) 0.039(6) 0.069(8) 0.003(5) 0.011(7) -0.010(5) C36B 0.085(9) 0.047(7) 0.069(8) 0.009(6) 0.014(7) -0.017(6) C37B 0.062(7) 0.051(7) 0.064(7) 0.012(6) 0.015(6) -0.014(6) C41B 0.055(6) 0.048(6) 0.053(7) -0.010(5) 0.026(5) -0.008(5) C42B 0.046(6) 0.038(6) 0.039(6) -0.003(4) 0.007(5) 0.000(4) C43B 0.040(5) 0.038(5) 0.038(6) -0.003(4) 0.005(5) 0.004(4) C44B 0.038(5) 0.041(6) 0.035(6) 0.001(4) 0.005(4) 0.001(4) C45B 0.050(6) 0.040(6) 0.055(7) -0.001(5) 0.009(5) 0.003(5) C46B 0.053(7) 0.044(6) 0.066(7) -0.007(5) 0.005(6) 0.016(5) C47B 0.058(7) 0.055(7) 0.046(6) -0.008(5) 0.020(5) -0.001(5) N51B 0.057(6) 0.041(5) 0.038(5) -0.002(4) 0.026(4) -0.001(4) N52B 0.057(6) 0.044(5) 0.041(5) -0.003(4) 0.018(5) -0.001(4) C53B 0.049(6) 0.054(6) 0.061(8) 0.004(5) 0.033(6) 0.004(5) C54B 0.063(7) 0.049(6) 0.047(7) 0.003(5) 0.033(6) 0.019(5) C55B 0.060(7) 0.037(5) 0.042(6) 0.004(4) 0.031(5) 0.003(5) N61B 0.060(6) 0.044(5) 0.046(5) 0.008(4) 0.028(5) 0.004(4) C62B 0.078(8) 0.028(5) 0.044(7) 0.010(4) 0.025(6) 0.005(5) C63B 0.084(8) 0.048(6) 0.044(7) 0.013(5) 0.043(6) 0.020(5) C64B 0.105(10) 0.049(7) 0.033(6) 0.005(5) 0.015(7) 0.015(6) C65B 0.087(9) 0.051(7) 0.042(7) 0.002(5) 0.008(6) 0.007(6) C66B 0.070(8) 0.053(6) 0.054(8) 0.017(5) 0.018(6) 0.006(5) O1 0.075(6) 0.063(5) 0.081(6) 0.001(4) 0.007(4) 0.004(4) C2 0.076(9) 0.046(7) 0.100(10) 0.001(6) 0.015(8) 0.019(6) C3 0.091(10) 0.074(9) 0.126(12) 0.013(8) 0.030(9) 0.011(7) C4 0.097(10) 0.071(8) 0.108(11) -0.014(8) -0.019(8) -0.001(7) C5 0.085(9) 0.061(7) 0.080(9) -0.002(7) 0.007(7) -0.006(7) C6 0.106(11) 0.122(12) 0.085(10) 0.032(9) -0.022(9) -0.012(9) C7 0.127(12) 0.094(10) 0.099(11) -0.008(9) 0.034(9) -0.028(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 Ag1 N61B 2.306(8) . ? Ag1 N61A 2.309(8) . ? Ag1 N51B 2.332(8) . ? Ag1 N51A 2.335(7) . ? Ag2 N21B 2.271(7) . ? Ag2 N21A 2.288(7) . ? Ag2 N11A 2.344(7) . ? Ag2 N11B 2.369(8) . ? N11A C16A 1.332(11) . ? N11A C12A 1.358(11) . ? C12A C13A 1.388(12) . ? C12A C25A 1.466(12) . ? C13A C14A 1.378(13) . ? C14A C15A 1.370(14) . ? C15A C16A 1.400(14) . ? N21A C25A 1.339(10) . ? N21A N22A 1.349(9) . ? N22A C23A 1.363(11) . ? N22A C31A 1.449(11) . ? C23A C24A 1.356(12) . ? C24A C25A 1.378(12) . ? C31A C32A 1.505(12) . ? C32A C33A 1.388(12) . ? C32A C37A 1.389(12) . ? C33A C34A 1.398(11) . ? C34A C35A 1.392(12) . ? C34A C44A 1.477(11) . ? C35A C36A 1.382(12) . ? C36A C37A 1.384(12) . ? C41A N52A 1.456(11) . ? C41A C42A 1.497(13) . ? C42A C47A 1.384(13) . ? C42A C43A 1.420(12) . ? C43A C44A 1.390(12) . ? C44A C45A 1.392(12) . ? C45A C46A 1.399(13) . ? C46A C47A 1.365(13) . ? N51A C55A 1.339(10) . ? N51A N52A 1.329(9) . ? N52A C53A 1.363(11) . ? C53A C54A 1.345(13) . ? C54A C55A 1.398(12) . ? C55A C62A 1.475(12) . ? N61A C62A 1.333(11) . ? N61A C66A 1.336(12) . ? C62A C63A 1.375(12) . ? C63A C64A 1.379(13) . ? C64A C65A 1.350(14) . ? C65A C66A 1.394(14) . ? N11B C16B 1.335(12) . ? N11B C12B 1.343(12) . ? C12B C13B 1.372(13) . ? C12B C25B 1.480(13) . ? C13B C14B 1.358(13) . ? C14B C15B 1.370(14) . ? C15B C16B 1.361(13) . ? N21B N22B 1.348(10) . ? N21B C25B 1.342(11) . ? N22B C23B 1.340(12) . ? N22B C31B 1.458(11) . ? C23B C24B 1.359(14) . ? C24B C25B 1.404(13) . ? C31B C32B 1.490(13) . ? C32B C37B 1.396(13) . ? C32B C33B 1.384(12) . ? C33B C34B 1.391(12) . ? C34B C35B 1.398(13) . ? C34B C34B 1.474(18) 2_654 ? C35B C36B 1.362(15) . ? C36B C37B 1.336(14) . ? C41B N52B 1.459(12) . ? C41B C42B 1.501(12) . ? C42B C43B 1.386(12) . ? C42B C47B 1.393(13) . ? C43B C44B 1.392(12) . ? C44B C45B 1.392(12) . ? C44B C44B 1.504(17) 2_655 ? C45B C46B 1.378(13) . ? C46B C47B 1.371(13) . ? N51B C55B 1.335(11) . ? N51B N52B 1.358(10) . ? N52B C53B 1.364(12) . ? C53B C54B 1.336(14) . ? C54B C55B 1.400(13) . ? C55B C62B 1.462(14) . ? N61B C66B 1.351(13) . ? N61B C62B 1.349(12) . ? C62B C63B 1.405(14) . ? C63B C64B 1.386(15) . ? C64B C65B 1.346(15) . ? C65B C66B 1.372(15) . ? B10 F12 1.355(12) . ? B10 F11 1.367(14) . ? B10 F13 1.369(13) . ? B10 F14 1.401(13) . ? B20 F24 1.328(11) . ? B20 F22 1.359(11) . ? B20 F23 1.397(10) . ? B20 F21 1.415(11) . ? O1 C5 1.442(13) . ? O1 C2 1.432(13) . ? C2 C4 1.486(16) . ? C2 C3 1.523(17) . ? C5 C6 1.531(16) . ? C5 C7 1.567(17) . ? O1S C2S 1.137(14) . ? C2S N3S 1.256(15) . ? N3S C4S 1.427(14) . ? N3S C4S 1.427(14) 2_656 ? 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 N61B Ag1 N61A 127.4(3) . . ? N61B Ag1 N51B 72.5(3) . . ? N61A Ag1 N51B 129.9(3) . . ? N61B Ag1 N51A 146.9(3) . . ? N61A Ag1 N51A 71.9(3) . . ? N51B Ag1 N51A 118.4(3) . . ? N21B Ag2 N21A 131.7(2) . . ? N21B Ag2 N11A 140.8(2) . . ? N21A Ag2 N11A 72.2(2) . . ? N21B Ag2 N11B 71.8(3) . . ? N21A Ag2 N11B 133.1(2) . . ? N11A Ag2 N11B 117.6(3) . . ? C16A N11A C12A 118.3(8) . . ? C16A N11A Ag2 126.5(6) . . ? C12A N11A Ag2 114.9(6) . . ? N11A C12A C13A 121.9(8) . . ? N11A C12A C25A 117.2(8) . . ? C13A C12A C25A 120.9(8) . . ? C14A C13A C12A 119.2(9) . . ? C13A C14A C15A 119.1(9) . . ? C14A C15A C16A 119.2(9) . . ? N11A C16A C15A 122.2(9) . . ? C25A N21A N22A 105.6(6) . . ? C25A N21A Ag2 116.7(5) . . ? N22A N21A Ag2 137.4(5) . . ? N21A N22A C23A 110.2(7) . . ? N21A N22A C31A 120.4(7) . . ? C23A N22A C31A 129.4(8) . . ? C24A C23A N22A 107.5(8) . . ? C23A C24A C25A 105.8(8) . . ? N21A C25A C24A 110.9(8) . . ? N21A C25A C12A 118.6(7) . . ? C24A C25A C12A 130.5(8) . . ? N22A C31A C32A 112.5(7) . . ? C33A C32A C37A 118.8(8) . . ? C33A C32A C31A 120.3(8) . . ? C37A C32A C31A 120.9(8) . . ? C32A C33A C34A 122.3(8) . . ? C35A C34A C33A 117.6(8) . . ? C35A C34A C44A 121.6(8) . . ? C33A C34A C44A 120.8(8) . . ? C36A C35A C34A 120.5(9) . . ? C35A C36A C37A 121.1(9) . . ? C36A C37A C32A 119.6(9) . . ? N52A C41A C42A 114.0(7) . . ? C47A C42A C43A 118.4(9) . . ? C47A C42A C41A 121.9(8) . . ? C43A C42A C41A 119.6(8) . . ? C44A C43A C42A 121.4(8) . . ? C43A C44A C45A 117.5(8) . . ? C43A C44A C34A 120.9(8) . . ? C45A C44A C34A 121.6(8) . . ? C44A C45A C46A 121.8(9) . . ? C47A C46A C45A 119.4(9) . . ? C46A C47A C42A 121.4(9) . . ? C55A N51A N52A 106.6(7) . . ? C55A N51A Ag1 113.8(6) . . ? N52A N51A Ag1 138.4(5) . . ? N51A N52A C53A 110.6(7) . . ? N51A N52A C41A 121.9(7) . . ? C53A N52A C41A 127.5(8) . . ? C54A C53A N52A 107.4(8) . . ? C53A C54A C55A 106.1(8) . . ? N51A C55A C54A 109.3(8) . . ? N51A C55A C62A 119.8(8) . . ? C54A C55A C62A 130.9(8) . . ? C62A N61A C66A 118.0(8) . . ? C62A N61A Ag1 117.3(6) . . ? C66A N61A Ag1 124.6(7) . . ? N61A C62A C63A 122.6(8) . . ? N61A C62A C55A 116.0(7) . . ? C63A C62A C55A 121.4(8) . . ? C62A C63A C64A 118.5(9) . . ? C65A C64A C63A 120.0(9) . . ? C64A C65A C66A 118.4(10) . . ? N61A C66A C65A 122.4(10) . . ? C16B N11B C12B 116.5(8) . . ? C16B N11B Ag2 127.7(7) . . ? C12B N11B Ag2 115.7(6) . . ? C13B C12B N11B 123.0(9) . . ? C13B C12B C25B 121.4(9) . . ? N11B C12B C25B 115.5(8) . . ? C12B C13B C14B 118.9(10) . . ? C15B C14B C13B 119.2(10) . . ? C14B C15B C16B 118.7(10) . . ? N11B C16B C15B 123.6(10) . . ? N22B N21B C25B 105.5(7) . . ? N22B N21B Ag2 137.5(6) . . ? C25B N21B Ag2 116.5(6) . . ? C23B N22B N21B 111.6(7) . . ? C23B N22B C31B 129.4(8) . . ? N21B N22B C31B 119.0(7) . . ? N22B C23B C24B 107.6(9) . . ? C23B C24B C25B 105.5(9) . . ? N21B C25B C24B 109.8(8) . . ? N21B C25B C12B 119.4(8) . . ? C24B C25B C12B 130.5(9) . . ? C32B C31B N22B 113.6(7) . . ? C37B C32B C33B 117.5(9) . . ? C37B C32B C31B 121.6(9) . . ? C33B C32B C31B 120.8(8) . . ? C34B C33B C32B 122.9(8) . . ? C33B C34B C35B 115.7(9) . . ? C33B C34B C34B 121.4(5) . 2_654 ? C35B C34B C34B 122.9(6) . 2_654 ? C36B C35B C34B 122.0(10) . . ? C37B C36B C35B 120.8(10) . . ? C36B C37B C32B 121.0(10) . . ? N52B C41B C42B 112.7(7) . . ? C43B C42B C47B 118.2(8) . . ? C43B C42B C41B 121.2(8) . . ? C47B C42B C41B 120.6(9) . . ? C42B C43B C44B 121.4(8) . . ? C43B C44B C45B 118.5(8) . . ? C43B C44B C44B 121.2(5) . 2_655 ? C45B C44B C44B 120.3(6) . 2_655 ? C46B C45B C44B 120.9(9) . . ? C45B C46B C47B 119.6(9) . . ? C46B C47B C42B 121.4(9) . . ? C55B N51B N52B 105.8(7) . . ? C55B N51B Ag1 114.5(7) . . ? N52B N51B Ag1 139.0(6) . . ? N51B N52B C53B 110.4(8) . . ? N51B N52B C41B 119.6(8) . . ? C53B N52B C41B 129.8(9) . . ? C54B C53B N52B 107.4(9) . . ? C53B C54B C55B 106.7(9) . . ? N51B C55B C54B 109.7(9) . . ? N51B C55B C62B 119.1(9) . . ? C54B C55B C62B 131.1(9) . . ? C66B N61B C62B 118.1(9) . . ? C66B N61B Ag1 126.0(7) . . ? C62B N61B Ag1 115.6(7) . . ? N61B C62B C63B 121.1(10) . . ? N61B C62B C55B 117.9(8) . . ? C63B C62B C55B 121.0(10) . . ? C62B C63B C64B 118.5(10) . . ? C65B C64B C63B 119.9(10) . . ? C64B C65B C66B 119.4(11) . . ? N61B C66B C65B 122.8(11) . . ? F12 B10 F11 114.1(19) . . ? F12 B10 F13 113.5(14) . . ? F11 B10 F13 107.0(19) . . ? F12 B10 F14 113.1(12) . . ? F11 B10 F14 102.9(18) . . ? F13 B10 F14 105.3(14) . . ? F24 B20 F22 119.5(11) . . ? F24 B20 F23 117.4(10) . . ? F22 B20 F23 106.5(10) . . ? F24 B20 F21 108.2(11) . . ? F22 B20 F21 102.0(10) . . ? F23 B20 F21 100.5(9) . . ? C5 O1 C2 115.6(9) . . ? O1 C2 C4 110.8(10) . . ? O1 C2 C3 111.6(10) . . ? C4 C2 C3 110.8(11) . . ? O1 C5 C6 109.1(10) . . ? O1 C5 C7 111.5(10) . . ? C6 C5 C7 109.3(11) . . ? O1S C2S N3S 157.4(8) . . ? C2S N3S C4S 118.0(9) . . ? C2S N3S C4S 118.0(9) . 2_656 ? C4S N3S C4S 124.0(18) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21B Ag2 N11A C16A 41.0(9) . . . . ? N21A Ag2 N11A C16A 176.4(8) . . . . ? N11B Ag2 N11A C16A -53.7(8) . . . . ? N21B Ag2 N11A C12A -132.4(6) . . . . ? N21A Ag2 N11A C12A 2.9(5) . . . . ? N11B Ag2 N11A C12A 132.8(5) . . . . ? C16A N11A C12A C13A 1.0(12) . . . . ? Ag2 N11A C12A C13A 175.1(6) . . . . ? C16A N11A C12A C25A 179.7(7) . . . . ? Ag2 N11A C12A C25A -6.2(9) . . . . ? N11A C12A C13A C14A -2.0(13) . . . . ? C25A C12A C13A C14A 179.4(8) . . . . ? C12A C13A C14A C15A 2.4(14) . . . . ? C13A C14A C15A C16A -2.0(14) . . . . ? C12A N11A C16A C15A -0.6(13) . . . . ? Ag2 N11A C16A C15A -173.9(7) . . . . ? C14A C15A C16A N11A 1.1(15) . . . . ? N21B Ag2 N21A C25A 144.4(5) . . . . ? N11A Ag2 N21A C25A 0.9(5) . . . . ? N11B Ag2 N21A C25A -110.6(6) . . . . ? N21B Ag2 N21A N22A -42.8(9) . . . . ? N11A Ag2 N21A N22A 173.7(8) . . . . ? N11B Ag2 N21A N22A 62.2(8) . . . . ? C25A N21A N22A C23A 1.5(9) . . . . ? Ag2 N21A N22A C23A -171.9(6) . . . . ? C25A N21A N22A C31A 179.8(7) . . . . ? Ag2 N21A N22A C31A 6.4(12) . . . . ? N21A N22A C23A C24A -1.2(10) . . . . ? C31A N22A C23A C24A -179.3(8) . . . . ? N22A C23A C24A C25A 0.5(10) . . . . ? N22A N21A C25A C24A -1.2(9) . . . . ? Ag2 N21A C25A C24A 173.8(5) . . . . ? N22A N21A C25A C12A -179.5(7) . . . . ? Ag2 N21A C25A C12A -4.5(9) . . . . ? C23A C24A C25A N21A 0.4(10) . . . . ? C23A C24A C25A C12A 178.5(8) . . . . ? N11A C12A C25A N21A 7.3(11) . . . . ? C13A C12A C25A N21A -174.0(8) . . . . ? N11A C12A C25A C24A -170.6(8) . . . . ? C13A C12A C25A C24A 8.1(14) . . . . ? N21A N22A C31A C32A -74.5(10) . . . . ? C23A N22A C31A C32A 103.4(10) . . . . ? N22A C31A C32A C33A 118.3(9) . . . . ? N22A C31A C32A C37A -62.5(10) . . . . ? C37A C32A C33A C34A -1.6(13) . . . . ? C31A C32A C33A C34A 177.6(7) . . . . ? C32A C33A C34A C35A 1.7(12) . . . . ? C32A C33A C34A C44A -177.2(8) . . . . ? C33A C34A C35A C36A -0.5(12) . . . . ? C44A C34A C35A C36A 178.4(8) . . . . ? C34A C35A C36A C37A -0.8(14) . . . . ? C35A C36A C37A C32A 0.9(14) . . . . ? C33A C32A C37A C36A 0.3(13) . . . . ? C31A C32A C37A C36A -178.9(8) . . . . ? N52A C41A C42A C47A -70.6(11) . . . . ? N52A C41A C42A C43A 110.5(9) . . . . ? C47A C42A C43A C44A -1.5(12) . . . . ? C41A C42A C43A C44A 177.5(7) . . . . ? C42A C43A C44A C45A 1.5(12) . . . . ? C42A C43A C44A C34A -178.2(7) . . . . ? C35A C34A C44A C43A -148.2(8) . . . . ? C33A C34A C44A C43A 30.6(12) . . . . ? C35A C34A C44A C45A 32.1(12) . . . . ? C33A C34A C44A C45A -149.1(8) . . . . ? C43A C44A C45A C46A -0.5(12) . . . . ? C34A C44A C45A C46A 179.2(8) . . . . ? C44A C45A C46A C47A -0.6(14) . . . . ? C45A C46A C47A C42A 0.7(14) . . . . ? C43A C42A C47A C46A 0.3(13) . . . . ? C41A C42A C47A C46A -178.6(8) . . . . ? N61B Ag1 N51A C55A 141.2(6) . . . . ? N61A Ag1 N51A C55A 9.2(6) . . . . ? N51B Ag1 N51A C55A -116.9(6) . . . . ? N61B Ag1 N51A N52A -53.3(11) . . . . ? N61A Ag1 N51A N52A 174.7(9) . . . . ? N51B Ag1 N51A N52A 48.5(9) . . . . ? C55A N51A N52A C53A 1.7(10) . . . . ? Ag1 N51A N52A C53A -164.5(7) . . . . ? C55A N51A N52A C41A -178.8(8) . . . . ? Ag1 N51A N52A C41A 15.1(13) . . . . ? C42A C41A N52A N51A -90.7(10) . . . . ? C42A C41A N52A C53A 88.8(11) . . . . ? N51A N52A C53A C54A -2.0(11) . . . . ? C41A N52A C53A C54A 178.5(9) . . . . ? N52A C53A C54A C55A 1.5(11) . . . . ? N52A N51A C55A C54A -0.7(10) . . . . ? Ag1 N51A C55A C54A 169.3(6) . . . . ? N52A N51A C55A C62A 178.5(7) . . . . ? Ag1 N51A C55A C62A -11.6(10) . . . . ? C53A C54A C55A N51A -0.5(11) . . . . ? C53A C54A C55A C62A -179.6(9) . . . . ? N61B Ag1 N61A C62A -155.7(6) . . . . ? N51B Ag1 N61A C62A 105.9(7) . . . . ? N51A Ag1 N61A C62A -6.4(7) . . . . ? N61B Ag1 N61A C66A 25.5(10) . . . . ? N51B Ag1 N61A C66A -72.9(10) . . . . ? N51A Ag1 N61A C66A 174.8(10) . . . . ? C66A N61A C62A C63A 1.3(14) . . . . ? Ag1 N61A C62A C63A -177.5(7) . . . . ? C66A N61A C62A C55A -178.2(9) . . . . ? Ag1 N61A C62A C55A 3.0(10) . . . . ? N51A C55A C62A N61A 6.1(12) . . . . ? C54A C55A C62A N61A -175.0(9) . . . . ? N51A C55A C62A C63A -173.5(8) . . . . ? C54A C55A C62A C63A 5.5(15) . . . . ? N61A C62A C63A C64A 0.6(14) . . . . ? C55A C62A C63A C64A -179.9(8) . . . . ? C62A C63A C64A C65A -1.5(15) . . . . ? C63A C64A C65A C66A 0.6(17) . . . . ? C62A N61A C66A C65A -2.3(17) . . . . ? Ag1 N61A C66A C65A 176.4(9) . . . . ? C64A C65A C66A N61A 1.4(19) . . . . ? N21B Ag2 N11B C16B -170.0(8) . . . . ? N21A Ag2 N11B C16B 59.4(8) . . . . ? N11A Ag2 N11B C16B -31.6(8) . . . . ? N21B Ag2 N11B C12B 6.1(6) . . . . ? N21A Ag2 N11B C12B -124.5(6) . . . . ? N11A Ag2 N11B C12B 144.5(6) . . . . ? C16B N11B C12B C13B -2.0(12) . . . . ? Ag2 N11B C12B C13B -178.5(6) . . . . ? C16B N11B C12B C25B 174.3(7) . . . . ? Ag2 N11B C12B C25B -2.2(9) . . . . ? N11B C12B C13B C14B 1.0(13) . . . . ? C25B C12B C13B C14B -175.1(8) . . . . ? C12B C13B C14B C15B 0.2(14) . . . . ? C13B C14B C15B C16B -0.3(14) . . . . ? C12B N11B C16B C15B 1.8(13) . . . . ? Ag2 N11B C16B C15B 177.9(7) . . . . ? C14B C15B C16B N11B -0.7(14) . . . . ? N21A Ag2 N21B N22B -47.6(9) . . . . ? N11A Ag2 N21B N22B 68.8(9) . . . . ? N11B Ag2 N21B N22B -179.6(8) . . . . ? N21A Ag2 N21B C25B 122.4(6) . . . . ? N11A Ag2 N21B C25B -121.2(6) . . . . ? N11B Ag2 N21B C25B -9.6(6) . . . . ? C25B N21B N22B C23B -0.7(9) . . . . ? Ag2 N21B N22B C23B 170.1(7) . . . . ? C25B N21B N22B C31B -179.5(7) . . . . ? Ag2 N21B N22B C31B -8.8(12) . . . . ? N21B N22B C23B C24B 0.8(11) . . . . ? C31B N22B C23B C24B 179.4(8) . . . . ? N22B C23B C24B C25B -0.5(11) . . . . ? N22B N21B C25B C24B 0.4(9) . . . . ? Ag2 N21B C25B C24B -172.7(6) . . . . ? N22B N21B C25B C12B -174.6(7) . . . . ? Ag2 N21B C25B C12B 12.4(10) . . . . ? C23B C24B C25B N21B 0.1(10) . . . . ? C23B C24B C25B C12B 174.3(9) . . . . ? C13B C12B C25B N21B 169.7(8) . . . . ? N11B C12B C25B N21B -6.7(11) . . . . ? C13B C12B C25B C24B -4.0(14) . . . . ? N11B C12B C25B C24B 179.6(9) . . . . ? C23B N22B C31B C32B -102.2(11) . . . . ? N21B N22B C31B C32B 76.4(10) . . . . ? N22B C31B C32B C37B 64.4(12) . . . . ? N22B C31B C32B C33B -117.7(9) . . . . ? C37B C32B C33B C34B 1.9(13) . . . . ? C31B C32B C33B C34B -176.1(8) . . . . ? C32B C33B C34B C35B -1.3(13) . . . . ? C32B C33B C34B C34B 178.6(10) . . . 2_654 ? C33B C34B C35B C36B -0.5(15) . . . . ? C34B C34B C35B C36B 179.6(11) 2_654 . . . ? C34B C35B C36B C37B 1.7(17) . . . . ? C35B C36B C37B C32B -1.1(17) . . . . ? C33B C32B C37B C36B -0.6(15) . . . . ? C31B C32B C37B C36B 177.3(10) . . . . ? N52B C41B C42B C43B -129.0(9) . . . . ? N52B C41B C42B C47B 52.4(12) . . . . ? C47B C42B C43B C44B 0.3(13) . . . . ? C41B C42B C43B C44B -178.4(8) . . . . ? C42B C43B C44B C45B -1.1(13) . . . . ? C42B C43B C44B C44B 177.9(9) . . . 2_655 ? C43B C44B C45B C46B 1.3(14) . . . . ? C44B C44B C45B C46B -177.7(10) 2_655 . . . ? C44B C45B C46B C47B -0.7(15) . . . . ? C45B C46B C47B C42B -0.2(15) . . . . ? C43B C42B C47B C46B 0.4(14) . . . . ? C41B C42B C47B C46B 179.1(9) . . . . ? N61B Ag1 N51B C55B -4.8(6) . . . . ? N61A Ag1 N51B C55B 119.7(6) . . . . ? N51A Ag1 N51B C55B -150.8(6) . . . . ? N61B Ag1 N51B N52B -173.4(9) . . . . ? N61A Ag1 N51B N52B -48.9(9) . . . . ? N51A Ag1 N51B N52B 40.7(9) . . . . ? C55B N51B N52B C53B -1.1(9) . . . . ? Ag1 N51B N52B C53B 168.1(7) . . . . ? C55B N51B N52B C41B -175.8(7) . . . . ? Ag1 N51B N52B C41B -6.6(12) . . . . ? C42B C41B N52B N51B 76.7(10) . . . . ? C42B C41B N52B C53B -96.8(11) . . . . ? N51B N52B C53B C54B 1.2(10) . . . . ? C41B N52B C53B C54B 175.3(8) . . . . ? N52B C53B C54B C55B -0.9(10) . . . . ? N52B N51B C55B C54B 0.5(9) . . . . ? Ag1 N51B C55B C54B -171.7(6) . . . . ? N52B N51B C55B C62B 177.3(7) . . . . ? Ag1 N51B C55B C62B 5.1(10) . . . . ? C53B C54B C55B N51B 0.2(11) . . . . ? C53B C54B C55B C62B -176.1(9) . . . . ? N61A Ag1 N61B C66B 49.3(8) . . . . ? N51B Ag1 N61B C66B 176.6(8) . . . . ? N51A Ag1 N61B C66B -67.9(9) . . . . ? N61A Ag1 N61B C62B -123.1(6) . . . . ? N51B Ag1 N61B C62B 4.1(6) . . . . ? N51A Ag1 N61B C62B 119.6(7) . . . . ? C66B N61B C62B C63B 4.0(12) . . . . ? Ag1 N61B C62B C63B 177.1(6) . . . . ? C66B N61B C62B C55B -176.2(8) . . . . ? Ag1 N61B C62B C55B -3.1(10) . . . . ? N51B C55B C62B N61B -1.4(12) . . . . ? C54B C55B C62B N61B 174.5(9) . . . . ? N51B C55B C62B C63B 178.4(8) . . . . ? C54B C55B C62B C63B -5.6(15) . . . . ? N61B C62B C63B C64B -3.2(13) . . . . ? C55B C62B C63B C64B 177.0(8) . . . . ? C62B C63B C64B C65B -0.4(14) . . . . ? C63B C64B C65B C66B 3.0(15) . . . . ? C62B N61B C66B C65B -1.3(14) . . . . ? Ag1 N61B C66B C65B -173.6(7) . . . . ? C64B C65B C66B N61B -2.3(15) . . . . ? C5 O1 C2 C4 156.6(10) . . . . ? C5 O1 C2 C3 -79.4(12) . . . . ? C2 O1 C5 C6 130.7(11) . . . . ? C2 O1 C5 C7 -108.5(12) . . . . ? O1S C2S N3S C4S 0(3) . . . . ? O1S C2S N3S C4S -180(3) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.864 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.102 #===END data_sse1270 _database_code_depnum_ccdc_archive 'CCDC 609496' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H99 Ag4 N27 4+, 4 B F4 -' _chemical_formula_sum 'C108 H99 Ag4 B4 F16 N27' _chemical_formula_weight 2553.86 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.281(11) _cell_length_b 18.300(12) _cell_length_c 23.280(15) _cell_angle_alpha 72.910(6) _cell_angle_beta 78.379(6) _cell_angle_gamma 76.302(6) _cell_volume 6376(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5887 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 21.3 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.002 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6712 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX2 CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 35172 _diffrn_reflns_av_R_equivalents 0.1346 _diffrn_reflns_av_sigmaI/netI 0.1689 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 20.69 _reflns_number_total 15451 _reflns_number_gt 7538 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.2000P)^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 0.0136(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15451 _refine_ls_number_parameters 1118 _refine_ls_number_restraints 2662 _refine_ls_R_factor_all 0.1945 _refine_ls_R_factor_gt 0.1414 _refine_ls_wR_factor_ref 0.3919 _refine_ls_wR_factor_gt 0.3683 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.002 _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 Ag1 Ag 0.91026(11) 0.28494(8) 0.40611(7) 0.0755(6) Uani 1 1 d U . . Ag2 Ag 1.48404(10) -0.19215(8) 0.17931(7) 0.0723(6) Uani 1 1 d U . . Ag3 Ag 0.49126(10) 0.67722(8) 0.31347(7) 0.0682(6) Uani 1 1 d U . . Ag4 Ag 1.17763(11) 0.27523(9) 0.12345(8) 0.0905(7) Uani 1 1 d U . . N11A N 0.3596(5) 0.6767(6) 0.2883(4) 0.059(3) Uani 1 1 d GDU . . C12A C 0.3495(6) 0.6059(5) 0.2826(5) 0.057(3) Uani 1 1 d GDU . . C13A C 0.2752(7) 0.6004(6) 0.2648(5) 0.081(5) Uani 1 1 d GDU . . H13A H 0.2683 0.5520 0.2609 0.098 Uiso 1 1 calc R . . C14A C 0.2109(6) 0.6657(8) 0.2527(6) 0.083(5) Uani 1 1 d GDU . . H14A H 0.1600 0.6619 0.2405 0.100 Uiso 1 1 calc R . . C15A C 0.2209(6) 0.7364(6) 0.2584(6) 0.084(5) Uani 1 1 d GDU . . H15A H 0.1769 0.7811 0.2501 0.101 Uiso 1 1 calc R . . C16A C 0.2952(7) 0.7419(5) 0.2762(5) 0.074(5) Uani 1 1 d GDU . . H16A H 0.3021 0.7903 0.2801 0.089 Uiso 1 1 calc R . . N21A N 0.4886(6) 0.5513(4) 0.3132(5) 0.056(3) Uani 1 1 d GDU . . N22A N 0.5447(5) 0.4779(5) 0.3230(5) 0.064(3) Uani 1 1 d GDU . . C23A C 0.5044(7) 0.4237(4) 0.3117(6) 0.071(4) Uani 1 1 d GDU . . H23A H 0.5276 0.3701 0.3149 0.085 Uiso 1 1 calc R . . C24A C 0.4233(7) 0.4637(6) 0.2948(6) 0.071(4) Uani 1 1 d GDU . . H24A H 0.3827 0.4415 0.2847 0.085 Uiso 1 1 calc R . . C25A C 0.4135(5) 0.5426(5) 0.2957(6) 0.065(4) Uani 1 1 d GDU . . N31A N 0.3704(5) 0.2926(5) 0.7109(4) 0.060(3) Uani 1 1 d GDU . . C32A C 0.3484(6) 0.2592(6) 0.6711(4) 0.059(4) Uani 1 1 d GDU . . C33A C 0.2699(6) 0.2361(7) 0.6829(5) 0.070(4) Uani 1 1 d GDU . . H33A H 0.2548 0.2133 0.6557 0.084 Uiso 1 1 calc R . . C34A C 0.2134(5) 0.2464(7) 0.7345(5) 0.075(5) Uani 1 1 d GDU . . H34A H 0.1598 0.2307 0.7426 0.091 Uiso 1 1 calc R . . C35A C 0.2355(6) 0.2798(7) 0.7744(4) 0.069(4) Uani 1 1 d GDU . . H35A H 0.1969 0.2869 0.8097 0.083 Uiso 1 1 calc R . . C36A C 0.3139(7) 0.3029(6) 0.7625(4) 0.060(4) Uani 1 1 d GDU . . H36A H 0.3290 0.3257 0.7898 0.072 Uiso 1 1 calc R . . N41A N 0.4854(6) 0.2747(6) 0.6122(4) 0.059(3) Uani 1 1 d GDU . . N42A N 0.5338(5) 0.2580(7) 0.5580(4) 0.072(4) Uani 1 1 d GDU . . C43A C 0.4866(8) 0.2194(8) 0.5352(4) 0.080(5) Uani 1 1 d GDU . . H43A H 0.5038 0.2015 0.4995 0.096 Uiso 1 1 calc R . . C44A C 0.4090(7) 0.2122(8) 0.5753(6) 0.077(5) Uani 1 1 d GDU . . H44A H 0.3652 0.1886 0.5711 0.092 Uiso 1 1 calc R . . C45A C 0.4083(5) 0.2464(7) 0.6229(4) 0.061(4) Uani 1 1 d GDU . . N51A N 1.0267(6) 0.1930(5) 0.4387(5) 0.074(4) Uani 1 1 d GDU . . C52A C 1.0297(7) 0.1188(6) 0.4333(6) 0.066(4) Uani 1 1 d GDU . . C53A C 1.0957(8) 0.0584(5) 0.4535(6) 0.076(5) Uani 1 1 d GDU . . H53A H 1.0977 0.0076 0.4499 0.091 Uiso 1 1 calc R . . C54A C 1.1586(7) 0.0723(6) 0.4792(7) 0.094(6) Uani 1 1 d GDU . . H54A H 1.2037 0.0310 0.4930 0.113 Uiso 1 1 calc R . . C55A C 1.1557(8) 0.1466(7) 0.4846(7) 0.099(6) Uani 1 1 d GDU . . H55A H 1.1987 0.1561 0.5021 0.119 Uiso 1 1 calc R . . C56A C 1.0897(8) 0.2069(5) 0.4644(6) 0.090(6) Uani 1 1 d GDU . . H56A H 1.0876 0.2577 0.4681 0.108 Uiso 1 1 calc R . . N61A N 0.8944(6) 0.1691(4) 0.3960(5) 0.064(3) Uani 1 1 d GDU . . N62A N 0.8388(5) 0.1418(6) 0.3708(5) 0.066(3) Uani 1 1 d GDU . . C63A C 0.8761(7) 0.0643(6) 0.3679(7) 0.093(6) Uani 1 1 d GDU . . H63A H 0.8525 0.0319 0.3529 0.111 Uiso 1 1 calc R . . C64A C 0.9548(7) 0.0437(5) 0.3914(6) 0.077(5) Uani 1 1 d GDU . . H64A H 0.9932 -0.0049 0.3948 0.092 Uiso 1 1 calc R . . C65A C 0.9662(6) 0.1084(6) 0.4087(5) 0.058(3) Uani 1 1 d GDU . . C71A C 0.6242(9) 0.4688(8) 0.3385(9) 0.077(5) Uani 1 1 d DU . . H71A H 0.6227 0.5053 0.3630 0.093 Uiso 1 1 calc R . . H71B H 0.6657 0.4811 0.3012 0.093 Uiso 1 1 calc R . . C72A C 0.6164(9) 0.2702(11) 0.5398(6) 0.077(5) Uani 1 1 d DU . . H72A H 0.6557 0.2227 0.5584 0.092 Uiso 1 1 calc R . . H72B H 0.6231 0.3131 0.5553 0.092 Uiso 1 1 calc R . . C73A C 0.7646(9) 0.1882(8) 0.3511(7) 0.067(4) Uani 1 1 d DU . . H73A H 0.7235 0.1541 0.3555 0.080 Uiso 1 1 calc R . . H73B H 0.7777 0.2130 0.3072 0.080 Uiso 1 1 calc R . . C81A C 0.6524(7) 0.3853(4) 0.3748(4) 0.063(4) Uani 1 1 d GDU . . C82A C 0.6226(7) 0.3665(5) 0.4367(4) 0.069(5) Uani 1 1 d GDU . . C83A C 0.6420(7) 0.2902(5) 0.4714(3) 0.063(4) Uani 1 1 d GDU . . C84A C 0.6912(7) 0.2328(4) 0.4443(4) 0.067(5) Uani 1 1 d GDU . . C85A C 0.7210(6) 0.2516(4) 0.3825(4) 0.051(4) Uani 1 1 d GDU . . C86A C 0.7016(7) 0.3278(5) 0.3477(3) 0.058(4) Uani 1 1 d GDU . . C91A C 0.5594(14) 0.4263(11) 0.4672(9) 0.099(7) Uani 1 1 d DU . . H91A H 0.5885 0.4671 0.4678 0.149 Uiso 1 1 calc R . . H91B H 0.5384 0.4000 0.5089 0.149 Uiso 1 1 calc R . . H91C H 0.5112 0.4497 0.4443 0.149 Uiso 1 1 calc R . . C92A C 0.7089(13) 0.1452(8) 0.4813(8) 0.072(5) Uani 1 1 d DU . . H92A H 0.7169 0.1116 0.4539 0.108 Uiso 1 1 calc R . . H92B H 0.6602 0.1346 0.5129 0.108 Uiso 1 1 calc R . . H92C H 0.7605 0.1346 0.5002 0.108 Uiso 1 1 calc R . . C93A C 0.7344(15) 0.3494(12) 0.2793(7) 0.109(9) Uani 1 1 d DU . . H93A H 0.7427 0.4034 0.2665 0.163 Uiso 1 1 calc R . . H93B H 0.6925 0.3436 0.2568 0.163 Uiso 1 1 calc R . . H93C H 0.7888 0.3148 0.2710 0.163 Uiso 1 1 calc R . . N11B N 1.4628(7) -0.2971(5) 0.1527(5) 0.070(3) Uani 1 1 d GDU . . C12B C 1.3898(7) -0.2881(5) 0.1269(5) 0.078(4) Uani 1 1 d GDU . . C13B C 1.3735(8) -0.3501(7) 0.1108(6) 0.094(5) Uani 1 1 d GDU . . H13B H 1.3236 -0.3440 0.0933 0.112 Uiso 1 1 calc R . . C14B C 1.4301(9) -0.4211(6) 0.1204(6) 0.093(6) Uani 1 1 d GDU . . H14B H 1.4189 -0.4635 0.1094 0.112 Uiso 1 1 calc R . . C15B C 1.5030(8) -0.4301(5) 0.1462(6) 0.080(5) Uani 1 1 d GDU . . H15B H 1.5417 -0.4786 0.1527 0.095 Uiso 1 1 calc R . . C16B C 1.5194(7) -0.3681(6) 0.1623(5) 0.071(4) Uani 1 1 d GDU . . H16B H 1.5692 -0.3742 0.1798 0.086 Uiso 1 1 calc R . . N21B N 1.3543(6) -0.1566(6) 0.1371(5) 0.073(3) Uani 1 1 d GDU . . N22B N 1.2876(8) -0.0908(5) 0.1247(6) 0.084(4) Uani 1 1 d GDU . . C23B C 1.2277(8) -0.1106(7) 0.0979(7) 0.113(7) Uani 1 1 d GDU . . H23B H 1.1767 -0.0775 0.0850 0.135 Uiso 1 1 calc R . . C24B C 1.2575(9) -0.1886(7) 0.0938(8) 0.105(6) Uani 1 1 d GDU . . H24B H 1.2299 -0.2169 0.0776 0.126 Uiso 1 1 calc R . . C25B C 1.3357(8) -0.2170(5) 0.1180(6) 0.078(4) Uani 1 1 d GDU . . N31B N 1.1180(7) 0.4055(5) 0.1130(6) 0.093(4) Uani 1 1 d GDU . . C32B C 1.0401(8) 0.4289(6) 0.0910(6) 0.088(4) Uani 1 1 d GDU . . C33B C 0.9990(7) 0.5064(7) 0.0810(6) 0.097(6) Uani 1 1 d GDU . . H33B H 0.9458 0.5224 0.0659 0.117 Uiso 1 1 calc R . . C34B C 1.0359(9) 0.5605(5) 0.0930(7) 0.112(7) Uani 1 1 d GDU . . H34B H 1.0078 0.6135 0.0862 0.135 Uiso 1 1 calc R . . C35B C 1.1138(10) 0.5371(7) 0.1151(8) 0.123(7) Uani 1 1 d GDU . . H35B H 1.1390 0.5741 0.1233 0.147 Uiso 1 1 calc R . . C36B C 1.1549(8) 0.4596(8) 0.1251(7) 0.110(6) Uani 1 1 d GDU . . H36B H 1.2081 0.4436 0.1401 0.132 Uiso 1 1 calc R . . N41B N 1.0524(6) 0.2963(6) 0.0872(5) 0.077(3) Uani 1 1 d GDU . . N42B N 1.0029(8) 0.2529(5) 0.0712(6) 0.091(4) Uani 1 1 d GDU . . C43B C 0.9251(8) 0.3031(8) 0.0558(8) 0.119(6) Uani 1 1 d GDU . . H43B H 0.8800 0.2894 0.0434 0.143 Uiso 1 1 calc R . . C44B C 0.9266(8) 0.3776(7) 0.0622(8) 0.120(7) Uani 1 1 d GDU . . H44B H 0.8826 0.4224 0.0548 0.144 Uiso 1 1 calc R . . C45B C 1.0053(8) 0.3734(6) 0.0816(6) 0.086(4) Uani 1 1 d GDU . . N51B N 1.5139(7) 0.1226(6) -0.2492(4) 0.067(4) Uani 1 1 d GDU . . C52B C 1.4437(6) 0.0868(7) -0.2374(4) 0.077(5) Uani 1 1 d GDU . . C53B C 1.4339(7) 0.0460(7) -0.2765(6) 0.085(5) Uani 1 1 d GDU . . H53B H 1.3859 0.0215 -0.2685 0.102 Uiso 1 1 calc R . . C54B C 1.4942(9) 0.0409(7) -0.3275(5) 0.093(6) Uani 1 1 d GDU . . H54B H 1.4875 0.0129 -0.3542 0.112 Uiso 1 1 calc R . . C55B C 1.5644(8) 0.0767(7) -0.3392(4) 0.080(5) Uani 1 1 d GDU . . H55B H 1.6056 0.0732 -0.3741 0.096 Uiso 1 1 calc R . . C56B C 1.5742(6) 0.1175(6) -0.3001(5) 0.069(4) Uani 1 1 d GDU . . H56B H 1.6222 0.1420 -0.3082 0.083 Uiso 1 1 calc R . . N61B N 1.3967(6) 0.1374(6) -0.1476(5) 0.066(4) Uani 1 1 d GDU . . N62B N 1.3253(7) 0.1365(7) -0.1011(4) 0.079(4) Uani 1 1 d GDU . . C63B C 1.2708(7) 0.0926(9) -0.1111(6) 0.095(6) Uani 1 1 d GDU . . H63B H 1.2183 0.0825 -0.0869 0.114 Uiso 1 1 calc R . . C64B C 1.3086(9) 0.0665(9) -0.1639(6) 0.096(6) Uani 1 1 d GDU . . H64B H 1.2858 0.0358 -0.1811 0.116 Uiso 1 1 calc R . . C65B C 1.3864(8) 0.0942(8) -0.1864(4) 0.079(5) Uani 1 1 d GDU . . C71B C 1.2853(14) -0.0250(7) 0.1423(8) 0.090(5) Uani 1 1 d DU . . H71C H 1.3439 -0.0216 0.1455 0.107 Uiso 1 1 calc R . . H71D H 1.2506 -0.0280 0.1828 0.107 Uiso 1 1 calc R . . C72B C 1.0300(9) 0.1757(9) 0.0735(10) 0.095(5) Uani 1 1 d DU . . H72C H 1.0052 0.1648 0.0420 0.114 Uiso 1 1 calc R . . H72D H 1.0052 0.1456 0.1133 0.114 Uiso 1 1 calc R . . C73B C 1.3151(12) 0.1763(9) -0.0577(6) 0.075(5) Uani 1 1 d DU . . H73C H 1.2878 0.2311 -0.0739 0.090 Uiso 1 1 calc R . . H73D H 1.3718 0.1759 -0.0484 0.090 Uiso 1 1 calc R . . C81B C 1.2472(7) 0.0468(6) 0.0970(4) 0.070(4) Uani 1 1 d GDU . . C82B C 1.1614(6) 0.0802(7) 0.1080(4) 0.082(5) Uani 1 1 d GDU . . C83B C 1.1252(5) 0.1437(7) 0.0649(5) 0.076(5) Uani 1 1 d GDU . . C84B C 1.1749(6) 0.1740(6) 0.0109(4) 0.074(5) Uani 1 1 d GDU . . C85B C 1.2607(6) 0.1407(6) 0.0000(4) 0.067(4) Uani 1 1 d GDU . . C86B C 1.2968(5) 0.0771(6) 0.0431(5) 0.071(5) Uani 1 1 d GDU . . C91B C 1.1049(14) 0.0496(13) 0.1687(8) 0.115(9) Uani 1 1 d DU . . H91D H 1.0603 0.0926 0.1782 0.173 Uiso 1 1 calc R . . H91E H 1.1405 0.0283 0.2014 0.173 Uiso 1 1 calc R . . H91F H 1.0784 0.0088 0.1650 0.173 Uiso 1 1 calc R . . C92B C 1.1328(11) 0.2424(10) -0.0383(7) 0.078(6) Uani 1 1 d DU . . H92D H 1.0732 0.2388 -0.0363 0.116 Uiso 1 1 calc R . . H92E H 1.1638 0.2395 -0.0786 0.116 Uiso 1 1 calc R . . H92F H 1.1351 0.2920 -0.0312 0.116 Uiso 1 1 calc R . . C93B C 1.3899(9) 0.0318(13) 0.0304(10) 0.097(7) Uani 1 1 d DU . . H93D H 1.4177 0.0183 0.0668 0.146 Uiso 1 1 calc R . . H93E H 1.4222 0.0646 -0.0034 0.146 Uiso 1 1 calc R . . H93F H 1.3884 -0.0159 0.0199 0.146 Uiso 1 1 calc R . . N11C N 0.8252(7) 0.3606(5) 0.4699(4) 0.059(3) Uani 1 1 d GDU . . C12C C 0.8044(7) 0.4394(5) 0.4411(3) 0.052(4) Uani 1 1 d GDU . . C13C C 0.7577(8) 0.4914(5) 0.4743(5) 0.073(5) Uani 1 1 d GDU . . H13C H 0.7435 0.5452 0.4546 0.088 Uiso 1 1 calc R . . C14C C 0.7316(9) 0.4647(7) 0.5362(5) 0.104(7) Uani 1 1 d GDU . . H14C H 0.6997 0.5002 0.5588 0.125 Uiso 1 1 calc R . . C15C C 0.7524(10) 0.3859(7) 0.5649(3) 0.097(6) Uani 1 1 d GDU . . H15C H 0.7346 0.3677 0.6072 0.116 Uiso 1 1 calc R . . C16C C 0.7991(9) 0.3339(5) 0.5318(4) 0.078(5) Uani 1 1 d GDU . . H16C H 0.8133 0.2801 0.5514 0.094 Uiso 1 1 calc R . . N21C N 0.8852(7) 0.4081(4) 0.3497(4) 0.056(3) Uani 1 1 d GDU . . N22C N 0.9035(7) 0.4474(5) 0.2876(3) 0.060(4) Uani 1 1 d GDU . . C23C C 0.8597(8) 0.5259(5) 0.2794(4) 0.064(5) Uani 1 1 d GDU . . H23C H 0.8605 0.5654 0.2422 0.076 Uiso 1 1 calc R . . C24C C 0.8143(8) 0.5351(5) 0.3365(4) 0.069(5) Uani 1 1 d GDU . . H24C H 0.7795 0.5817 0.3442 0.083 Uiso 1 1 calc R . . C25C C 0.8301(7) 0.4622(6) 0.3799(3) 0.057(4) Uani 1 1 d GDU . . N31C N 1.3202(6) 0.2523(6) 0.0778(5) 0.072(4) Uani 1 1 d GDU . . C32C C 1.3724(7) 0.1915(7) 0.1132(4) 0.073(5) Uani 1 1 d GDU . . C33C C 1.4595(7) 0.1745(8) 0.0933(6) 0.112(8) Uani 1 1 d GDU . . H33C H 1.4951 0.1330 0.1175 0.134 Uiso 1 1 calc R . . C34C C 1.4944(6) 0.2184(10) 0.0382(6) 0.129(9) Uani 1 1 d GDU . . H34C H 1.5539 0.2068 0.0246 0.155 Uiso 1 1 calc R . . C35C C 1.4422(9) 0.2792(9) 0.0028(5) 0.108(7) Uani 1 1 d GDU . . H35C H 1.4660 0.3091 -0.0349 0.129 Uiso 1 1 calc R . . C36C C 1.3551(8) 0.2961(7) 0.0227(5) 0.091(6) Uani 1 1 d GDU . . H36C H 1.3194 0.3377 -0.0015 0.109 Uiso 1 1 calc R . . N41C N 1.2490(6) 0.1800(5) 0.1894(4) 0.067(4) Uani 1 1 d GDU . . N42C N 1.2261(5) 0.1276(6) 0.2458(4) 0.073(4) Uani 1 1 d GDU . . C43C C 1.2982(7) 0.0674(6) 0.2588(5) 0.084(6) Uani 1 1 d GDU . . H43C H 1.3008 0.0245 0.2938 0.100 Uiso 1 1 calc R . . C44C C 1.3657(5) 0.0826(6) 0.2104(5) 0.079(6) Uani 1 1 d GDU . . H44C H 1.4214 0.0517 0.2073 0.095 Uiso 1 1 calc R . . C45C C 1.3353(6) 0.1522(6) 0.1675(4) 0.064(5) Uani 1 1 d GDU . . N51C N 1.1273(8) 0.3565(9) 0.5803(7) 0.121(6) Uani 1 1 d GDU . . C52C C 1.1012(9) 0.3758(9) 0.5235(6) 0.107(6) Uani 1 1 d GDU . . C53C C 1.0155(10) 0.4042(10) 0.5173(6) 0.107(6) Uani 1 1 d GDU . . H53C H 0.9976 0.4174 0.4785 0.129 Uiso 1 1 calc R . . C54C C 0.9559(7) 0.4135(10) 0.5678(8) 0.122(7) Uani 1 1 d GDU . . H54C H 0.8973 0.4330 0.5635 0.147 Uiso 1 1 calc R . . C55C C 0.9820(10) 0.3943(11) 0.6245(6) 0.117(7) Uani 1 1 d GDU . . H55C H 0.9413 0.4007 0.6590 0.141 Uiso 1 1 calc R . . C56C C 1.0677(12) 0.3658(10) 0.6308(5) 0.127(7) Uani 1 1 d GDU . . H56C H 1.0855 0.3527 0.6696 0.153 Uiso 1 1 calc R . . N61C N 1.1543(7) 0.3751(8) 0.4279(6) 0.091(4) Uani 1 1 d GDU . . N62C N 1.2315(8) 0.3522(8) 0.3911(5) 0.102(5) Uani 1 1 d GDU . . C63C C 1.2969(7) 0.3214(9) 0.4287(7) 0.111(6) Uani 1 1 d GDU . . H63C H 1.3550 0.3017 0.4159 0.133 Uiso 1 1 calc R . . C64C C 1.2600(9) 0.3251(10) 0.4887(6) 0.113(6) Uani 1 1 d GDU . . H64C H 1.2892 0.3083 0.5231 0.136 Uiso 1 1 calc R . . C65C C 1.1719(9) 0.3583(10) 0.4882(5) 0.105(6) Uani 1 1 d GDU . . C71C C 0.9588(10) 0.4095(9) 0.2485(6) 0.074(5) Uani 1 1 d DU . . H71E H 0.9764 0.4494 0.2118 0.088 Uiso 1 1 calc R . . H71F H 0.9265 0.3787 0.2358 0.088 Uiso 1 1 calc R . . C72C C 1.1491(9) 0.1435(7) 0.2825(7) 0.066(4) Uani 1 1 d DU . . H72E H 1.1523 0.1081 0.3237 0.079 Uiso 1 1 calc R . . H72F H 1.1030 0.1328 0.2660 0.079 Uiso 1 1 calc R . . C73C C 1.2389(12) 0.3579(13) 0.3302(8) 0.106(6) Uani 1 1 d DU . . H73E H 1.2954 0.3277 0.3180 0.128 Uiso 1 1 calc R . . H73F H 1.2387 0.4131 0.3081 0.128 Uiso 1 1 calc R . . C81C C 1.0393(6) 0.3553(5) 0.2698(5) 0.067(4) Uani 1 1 d GDU . . C82C C 1.0532(6) 0.2779(6) 0.2684(5) 0.059(4) Uani 1 1 d GDU . . C83C C 1.1265(7) 0.2269(4) 0.2873(6) 0.071(4) Uani 1 1 d GDU . . C84C C 1.1859(6) 0.2533(6) 0.3075(6) 0.078(4) Uani 1 1 d GDU . . C85C C 1.1720(7) 0.3307(7) 0.3089(6) 0.083(5) Uani 1 1 d GDU . . C86C C 1.0987(8) 0.3817(5) 0.2900(6) 0.081(5) Uani 1 1 d GDU . . C91C C 0.9891(10) 0.2440(9) 0.2467(8) 0.065(4) Uani 1 1 d DU . . H91G H 0.9925 0.1888 0.2680 0.097 Uiso 1 1 calc R . . H91H H 1.0036 0.2494 0.2029 0.097 Uiso 1 1 calc R . . H91I H 0.9310 0.2725 0.2555 0.097 Uiso 1 1 calc R . . C92C C 1.2675(11) 0.1988(12) 0.3332(11) 0.100(7) Uani 1 1 d DU . . H92G H 1.3179 0.2073 0.3028 0.149 Uiso 1 1 calc R . . H92H H 1.2614 0.1444 0.3427 0.149 Uiso 1 1 calc R . . H92I H 1.2741 0.2109 0.3702 0.149 Uiso 1 1 calc R . . C93C C 1.0837(16) 0.4703(8) 0.2862(12) 0.110(8) Uani 1 1 d DU . . H93G H 1.0287 0.4963 0.2720 0.165 Uiso 1 1 calc R . . H93H H 1.1297 0.4932 0.2577 0.165 Uiso 1 1 calc R . . H93I H 1.0832 0.4772 0.3265 0.165 Uiso 1 1 calc R . . B1 B 0.8096(10) 0.0996(8) 0.6349(7) 0.103(6) Uani 1 1 d DU . . F11 F 0.8844(9) 0.1070(9) 0.5961(9) 0.174(7) Uani 1 1 d DU . . F12 F 0.7577(8) 0.1709(6) 0.6257(5) 0.106(4) Uani 1 1 d DU . . F13 F 0.7711(9) 0.0490(7) 0.6218(6) 0.127(4) Uani 1 1 d DU . . F14 F 0.8249(13) 0.0755(9) 0.6932(7) 0.200(8) Uani 1 1 d DU . . B2 B 0.5195(12) 0.2062(11) 0.3404(10) 0.088(8) Uani 0.50 1 d PDU . . F21 F 0.5132(14) 0.1450(12) 0.3238(11) 0.111(8) Uani 0.50 1 d PDU . . F22 F 0.531(2) 0.1849(18) 0.3983(10) 0.171(12) Uani 0.50 1 d PDU . . F23 F 0.5859(11) 0.2356(11) 0.3068(10) 0.087(6) Uani 0.50 1 d PDU . . F24 F 0.4496(13) 0.2597(13) 0.3332(15) 0.142(10) Uani 0.50 1 d PDU . . 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 Ag1 0.0885(12) 0.0425(8) 0.0757(11) -0.0051(7) -0.0088(9) 0.0102(7) Ag2 0.0791(11) 0.0592(9) 0.0608(10) -0.0042(7) -0.0047(8) 0.0019(8) Ag3 0.0725(11) 0.0524(9) 0.0676(10) -0.0064(7) -0.0070(8) -0.0025(7) Ag4 0.0855(12) 0.0698(11) 0.0751(11) 0.0036(8) -0.0042(9) 0.0293(9) N11A 0.048(7) 0.077(7) 0.031(7) -0.008(7) 0.009(6) 0.007(5) C12A 0.053(8) 0.078(7) 0.024(8) 0.000(8) 0.002(7) -0.004(6) C13A 0.068(10) 0.095(10) 0.066(12) 0.012(10) -0.018(9) -0.020(8) C14A 0.055(10) 0.115(12) 0.061(11) 0.002(11) -0.006(9) -0.014(9) C15A 0.060(10) 0.107(11) 0.059(11) -0.009(11) -0.007(9) 0.017(10) C16A 0.073(9) 0.072(9) 0.054(10) 0.005(9) -0.005(9) 0.003(8) N21A 0.045(7) 0.048(5) 0.055(8) 0.008(6) 0.001(6) -0.006(5) N22A 0.057(7) 0.051(6) 0.070(9) -0.006(7) -0.004(7) -0.003(5) C23A 0.070(10) 0.058(8) 0.072(12) -0.011(9) 0.007(9) -0.010(7) C24A 0.060(10) 0.078(8) 0.071(12) -0.015(10) 0.001(9) -0.019(7) C25A 0.052(8) 0.066(7) 0.064(10) -0.005(8) 0.002(8) -0.012(6) N31A 0.051(8) 0.043(8) 0.065(8) -0.001(6) -0.010(6) 0.014(6) C32A 0.049(8) 0.059(10) 0.057(9) -0.006(7) 0.003(6) -0.006(8) C33A 0.046(8) 0.079(12) 0.073(10) -0.019(9) 0.000(7) 0.002(8) C34A 0.049(9) 0.083(13) 0.077(12) -0.002(9) 0.005(7) -0.013(9) C35A 0.047(8) 0.069(12) 0.066(10) -0.011(8) 0.005(8) 0.017(8) C36A 0.060(9) 0.037(9) 0.064(9) -0.003(7) -0.006(7) 0.011(7) N41A 0.044(7) 0.080(10) 0.040(7) -0.009(6) -0.001(5) -0.002(6) N42A 0.065(8) 0.079(10) 0.056(8) -0.014(7) 0.004(6) 0.003(7) C43A 0.075(11) 0.089(13) 0.067(11) -0.024(9) -0.006(8) 0.000(10) C44A 0.065(10) 0.091(13) 0.076(11) -0.033(9) -0.009(8) -0.005(9) C45A 0.028(7) 0.078(11) 0.069(9) -0.021(8) -0.015(6) 0.017(7) N51A 0.075(9) 0.047(6) 0.083(11) 0.001(7) -0.013(7) -0.001(6) C52A 0.072(10) 0.047(7) 0.062(11) -0.002(8) -0.001(8) 0.000(6) C53A 0.083(12) 0.039(8) 0.089(13) 0.004(9) -0.013(9) -0.005(7) C54A 0.080(13) 0.073(9) 0.121(16) -0.025(12) -0.025(11) 0.012(10) C55A 0.095(14) 0.070(10) 0.131(17) -0.014(12) -0.042(12) -0.004(10) C56A 0.104(13) 0.058(9) 0.105(15) -0.010(10) -0.035(11) -0.009(8) N61A 0.064(8) 0.045(6) 0.066(9) -0.017(6) 0.010(6) 0.008(5) N62A 0.060(8) 0.048(7) 0.078(10) -0.027(7) 0.014(7) 0.008(5) C63A 0.079(12) 0.051(9) 0.144(17) -0.033(10) -0.012(11) 0.004(8) C64A 0.087(11) 0.048(8) 0.085(13) -0.020(9) -0.010(10) 0.009(7) C65A 0.060(9) 0.047(7) 0.047(9) -0.010(7) 0.018(7) 0.003(6) C71A 0.052(9) 0.051(8) 0.111(12) -0.005(8) -0.012(10) 0.005(7) C72A 0.051(8) 0.084(12) 0.071(8) -0.016(8) 0.014(8) 0.008(8) C73A 0.064(10) 0.055(8) 0.074(11) -0.023(8) 0.006(8) -0.001(7) C81A 0.038(9) 0.044(7) 0.086(8) 0.001(6) 0.005(7) -0.001(6) C82A 0.040(10) 0.056(8) 0.091(8) -0.016(6) 0.008(9) 0.009(8) C83A 0.055(10) 0.061(7) 0.064(7) -0.017(6) -0.006(7) 0.003(7) C84A 0.051(10) 0.066(8) 0.063(7) -0.014(6) -0.005(8) 0.023(8) C85A 0.026(8) 0.049(7) 0.067(7) -0.013(5) 0.000(7) 0.006(6) C86A 0.036(9) 0.050(7) 0.077(8) -0.011(6) 0.000(8) 0.000(7) C91A 0.092(16) 0.073(12) 0.109(15) -0.033(12) 0.008(13) 0.023(11) C92A 0.074(13) 0.064(8) 0.065(11) -0.010(7) 0.000(10) -0.005(10) C93A 0.087(16) 0.084(15) 0.095(11) 0.012(9) 0.038(13) 0.010(13) N11B 0.108(10) 0.048(6) 0.032(7) 0.008(6) 0.002(7) -0.006(6) C12B 0.101(11) 0.068(8) 0.049(10) -0.008(8) 0.001(9) -0.004(7) C13B 0.124(15) 0.074(9) 0.072(13) -0.003(10) -0.007(11) -0.022(9) C14B 0.129(16) 0.072(9) 0.078(13) -0.019(10) -0.002(11) -0.030(10) C15B 0.125(14) 0.052(8) 0.047(11) -0.006(8) 0.004(10) -0.010(10) C16B 0.093(12) 0.061(8) 0.046(10) -0.005(8) 0.007(9) -0.013(7) N21B 0.070(8) 0.072(7) 0.058(9) -0.010(7) 0.006(7) 0.001(6) N22B 0.091(10) 0.077(7) 0.065(10) -0.009(7) -0.012(8) 0.009(7) C23B 0.123(15) 0.094(12) 0.114(16) -0.007(13) -0.062(13) 0.005(10) C24B 0.109(14) 0.086(11) 0.113(16) 0.002(12) -0.047(12) -0.017(10) C25B 0.068(10) 0.076(8) 0.075(12) -0.011(9) 0.003(8) -0.009(7) N31B 0.097(10) 0.069(7) 0.072(10) 0.005(8) 0.003(8) 0.019(6) C32B 0.101(11) 0.068(7) 0.048(10) 0.014(9) 0.006(9) 0.022(7) C33B 0.098(13) 0.075(9) 0.069(12) -0.003(10) 0.020(10) 0.030(9) C34B 0.119(16) 0.074(11) 0.098(16) 0.006(12) 0.002(12) 0.020(11) C35B 0.149(18) 0.069(9) 0.119(17) -0.002(12) -0.034(14) 0.023(11) C36B 0.117(15) 0.069(8) 0.108(16) 0.002(12) -0.012(12) 0.014(9) N41B 0.074(7) 0.076(7) 0.036(8) 0.004(7) 0.016(6) 0.025(6) N42B 0.076(9) 0.096(8) 0.062(10) -0.004(8) 0.020(7) 0.010(7) C43B 0.092(12) 0.109(12) 0.126(17) -0.008(14) -0.019(13) 0.012(9) C44B 0.091(12) 0.107(11) 0.129(17) -0.024(14) -0.018(13) 0.037(10) C45B 0.088(10) 0.078(8) 0.049(10) 0.010(9) 0.004(9) 0.023(7) N51B 0.070(9) 0.057(9) 0.053(8) -0.009(7) -0.009(6) 0.024(6) C52B 0.081(11) 0.066(11) 0.066(10) -0.015(8) 0.001(8) 0.007(8) C53B 0.090(12) 0.083(13) 0.068(11) -0.017(9) -0.008(8) 0.003(10) C54B 0.105(15) 0.088(14) 0.080(12) -0.038(11) -0.004(10) 0.009(10) C55B 0.099(13) 0.069(12) 0.045(10) 0.000(7) -0.006(9) 0.012(9) C56B 0.067(10) 0.051(10) 0.061(10) -0.004(7) 0.003(7) 0.021(8) N61B 0.065(8) 0.053(8) 0.061(8) -0.009(6) 0.022(6) -0.008(7) N62B 0.074(10) 0.073(10) 0.082(9) -0.032(7) 0.028(7) -0.018(8) C63B 0.084(12) 0.099(15) 0.107(14) -0.050(11) 0.028(10) -0.033(10) C64B 0.107(13) 0.104(15) 0.085(13) -0.039(11) 0.007(10) -0.033(11) C65B 0.084(11) 0.077(12) 0.060(10) -0.015(8) 0.000(7) 0.003(9) C71B 0.109(14) 0.078(9) 0.070(11) -0.013(7) -0.026(10) 0.009(9) C72B 0.066(9) 0.105(10) 0.088(13) -0.021(11) 0.008(9) 0.012(8) C73B 0.075(11) 0.069(11) 0.077(9) -0.031(7) 0.012(8) -0.008(9) C81B 0.070(9) 0.073(8) 0.066(9) -0.021(7) -0.021(7) 0.003(8) C82B 0.092(10) 0.069(11) 0.064(10) -0.012(7) 0.000(8) 0.010(9) C83B 0.063(8) 0.091(11) 0.057(9) -0.010(7) -0.010(7) 0.005(8) C84B 0.053(8) 0.086(12) 0.061(9) -0.011(7) -0.003(7) 0.013(8) C85B 0.057(8) 0.060(10) 0.076(8) -0.025(6) 0.005(7) 0.003(7) C86B 0.071(9) 0.058(10) 0.075(10) -0.030(6) -0.006(7) 0.017(8) C91B 0.110(16) 0.093(16) 0.082(13) 0.000(10) 0.018(11) 0.041(14) C92B 0.065(12) 0.071(12) 0.063(11) 0.015(8) 0.012(9) -0.008(9) C93B 0.045(10) 0.123(18) 0.116(17) -0.036(14) -0.017(9) 0.010(10) N11C 0.063(9) 0.062(6) 0.053(6) -0.014(5) -0.007(6) -0.017(6) C12C 0.042(9) 0.062(7) 0.054(6) -0.018(5) -0.010(7) -0.005(7) C13C 0.070(12) 0.081(9) 0.075(9) -0.035(7) -0.005(9) -0.011(9) C14C 0.120(17) 0.096(10) 0.089(11) -0.047(10) 0.038(13) -0.023(13) C15C 0.132(17) 0.097(11) 0.075(11) -0.038(8) 0.038(11) -0.071(12) C16C 0.110(15) 0.070(9) 0.057(8) -0.013(6) 0.000(9) -0.036(10) N21C 0.055(8) 0.047(5) 0.054(6) -0.004(5) -0.004(6) 0.000(6) N22C 0.079(9) 0.045(6) 0.048(6) -0.006(5) -0.012(6) 0.000(6) C23C 0.066(11) 0.045(7) 0.063(8) -0.003(6) -0.016(8) 0.014(8) C24C 0.082(13) 0.048(8) 0.064(8) -0.011(6) -0.011(9) 0.009(8) C25C 0.047(9) 0.050(7) 0.063(6) -0.009(5) 0.001(7) -0.003(7) N31C 0.080(6) 0.065(9) 0.054(8) -0.009(6) 0.008(6) -0.006(6) C32C 0.059(7) 0.079(11) 0.071(10) -0.010(7) 0.003(7) -0.012(8) C33C 0.069(9) 0.145(18) 0.081(13) -0.017(11) 0.025(9) 0.013(11) C34C 0.084(13) 0.19(2) 0.082(14) -0.026(12) 0.031(10) -0.013(13) C35C 0.110(12) 0.144(18) 0.059(12) -0.022(10) 0.025(10) -0.040(13) C36C 0.108(11) 0.084(13) 0.069(11) -0.003(8) 0.007(9) -0.031(11) N41C 0.059(7) 0.049(7) 0.062(8) 0.005(5) 0.005(5) 0.012(6) N42C 0.061(8) 0.063(8) 0.064(8) 0.005(6) 0.006(6) 0.006(6) C43C 0.055(10) 0.065(11) 0.091(12) 0.016(8) -0.005(8) 0.015(8) C44C 0.064(9) 0.054(10) 0.091(12) -0.009(7) 0.001(8) 0.018(8) C45C 0.058(8) 0.042(8) 0.074(9) -0.011(6) 0.010(6) 0.005(7) N51C 0.135(14) 0.103(13) 0.140(11) -0.037(13) -0.048(10) -0.023(12) C52C 0.121(11) 0.086(14) 0.136(11) -0.048(13) -0.039(9) -0.020(13) C53C 0.116(11) 0.103(15) 0.123(13) -0.054(14) -0.034(10) -0.014(14) C54C 0.135(14) 0.119(17) 0.115(15) -0.036(16) -0.025(10) -0.016(15) C55C 0.147(15) 0.107(17) 0.111(12) -0.032(14) -0.022(13) -0.040(15) C56C 0.152(17) 0.108(17) 0.127(12) -0.019(15) -0.040(12) -0.033(17) N61C 0.087(9) 0.064(10) 0.132(10) -0.029(10) -0.028(8) -0.019(8) N62C 0.092(10) 0.083(11) 0.142(10) -0.047(11) -0.039(8) 0.003(10) C63C 0.097(10) 0.095(15) 0.154(14) -0.035(15) -0.050(9) -0.011(12) C64C 0.117(11) 0.088(14) 0.158(13) -0.048(14) -0.062(11) -0.007(13) C65C 0.108(11) 0.084(13) 0.138(10) -0.033(13) -0.042(9) -0.020(12) C71C 0.106(11) 0.044(8) 0.055(9) -0.012(7) -0.006(8) 0.009(8) C72C 0.052(9) 0.063(8) 0.060(10) 0.005(8) -0.004(7) 0.005(7) C73C 0.096(13) 0.106(14) 0.122(11) -0.024(13) -0.018(10) -0.034(12) C81C 0.077(9) 0.067(8) 0.052(10) -0.020(8) 0.005(8) -0.009(6) C82C 0.064(9) 0.051(7) 0.049(10) -0.007(7) 0.009(7) -0.006(6) C83C 0.069(10) 0.074(8) 0.061(11) -0.015(8) 0.000(8) -0.007(6) C84C 0.077(11) 0.075(8) 0.071(12) -0.005(9) -0.006(9) -0.016(8) C85C 0.072(10) 0.084(8) 0.091(12) -0.021(10) 0.002(9) -0.021(8) C86C 0.082(11) 0.064(8) 0.092(14) -0.019(10) 0.007(9) -0.025(7) C91C 0.066(11) 0.054(10) 0.062(11) -0.014(9) -0.004(9) 0.008(8) C92C 0.072(13) 0.104(14) 0.113(18) -0.030(14) -0.013(12) 0.003(11) C93C 0.12(2) 0.065(9) 0.15(2) -0.016(14) -0.046(18) -0.021(10) B1 0.123(17) 0.050(11) 0.104(13) -0.002(13) 0.004(12) 0.003(9) F11 0.106(10) 0.119(12) 0.264(17) -0.060(13) 0.045(12) -0.007(8) F12 0.113(9) 0.074(7) 0.090(8) -0.006(6) 0.001(7) 0.028(6) F13 0.139(12) 0.083(8) 0.136(11) -0.016(8) 0.015(9) -0.021(8) F14 0.28(2) 0.136(14) 0.154(11) 0.051(11) -0.115(12) -0.023(14) B2 0.056(18) 0.11(2) 0.13(2) -0.07(2) -0.02(2) -0.027(12) F21 0.11(2) 0.088(15) 0.16(2) -0.064(16) -0.018(18) -0.033(12) F22 0.20(3) 0.24(4) 0.124(16) -0.07(2) -0.022(18) -0.12(2) F23 0.038(10) 0.095(15) 0.146(17) -0.041(14) -0.041(11) -0.010(10) F24 0.061(12) 0.114(18) 0.26(3) -0.10(2) 0.014(17) -0.010(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 Ag1 N51A 2.306(8) . ? Ag1 N61A 2.280(8) . ? Ag1 N11C 2.348(8) . ? Ag1 N21C 2.238(7) . ? Ag2 N11B 2.301(9) . ? Ag2 N21B 2.378(9) . ? Ag2 N51B 2.350(9) 2_855 ? Ag2 N61B 2.286(9) 2_855 ? Ag3 N11A 2.337(8) . ? Ag3 N21A 2.317(8) . ? Ag3 N31A 2.364(8) 2_666 ? Ag3 N41A 2.287(8) 2_666 ? Ag4 N31B 2.311(9) . ? Ag4 N41B 2.269(10) . ? Ag4 N31C 2.345(9) . ? Ag4 N41C 2.221(7) . ? N11A C12A 1.390 . ? N11A C16A 1.390 . ? C12A C13A 1.390 . ? C12A C25A 1.367(8) . ? C13A C14A 1.390 . ? C14A C15A 1.390 . ? C15A C16A 1.390 . ? N21A N22A 1.420 . ? N21A C25A 1.420 . ? N22A C23A 1.420 . ? N22A C71A 1.372(13) . ? C23A C24A 1.420 . ? C24A C25A 1.420 . ? N31A Ag3 2.365(8) 2_666 ? N31A C32A 1.390 . ? N31A C36A 1.390 . ? C32A C33A 1.390 . ? C32A C45A 1.367(8) . ? C33A C34A 1.390 . ? C34A C35A 1.390 . ? C35A C36A 1.390 . ? N41A Ag3 2.287(8) 2_666 ? N41A N42A 1.420 . ? N41A C45A 1.420 . ? N42A C43A 1.420 . ? N42A C72A 1.375(13) . ? C43A C44A 1.420 . ? C44A C45A 1.420 . ? N51A C52A 1.390 . ? N51A C56A 1.390 . ? C52A C53A 1.390 . ? C52A C65A 1.352(9) . ? C53A C54A 1.390 . ? C54A C55A 1.390 . ? C55A C56A 1.390 . ? N61A N62A 1.420 . ? N61A C65A 1.420 . ? N62A C63A 1.420 . ? N62A C73A 1.377(12) . ? C63A C64A 1.420 . ? C64A C65A 1.420 . ? C71A C81A 1.526(12) . ? C72A C83A 1.519(12) . ? C73A C85A 1.510(12) . ? C81A C82A 1.390 . ? C81A C86A 1.390 . ? C82A C83A 1.390 . ? C82A C91A 1.547(12) . ? C83A C84A 1.390 . ? C84A C85A 1.390 . ? C84A C92A 1.570(12) . ? C85A C86A 1.390 . ? C86A C93A 1.538(13) . ? N11B C12B 1.390 . ? N11B C16B 1.390 . ? C12B C13B 1.390 . ? C12B C25B 1.372(9) . ? C13B C14B 1.390 . ? C14B C15B 1.390 . ? C15B C16B 1.390 . ? N21B N22B 1.420 . ? N21B C25B 1.420 . ? N22B C23B 1.420 . ? N22B C71B 1.372(13) . ? C23B C24B 1.420 . ? C24B C25B 1.420 . ? N31B C32B 1.390 . ? N31B C36B 1.390 . ? C32B C33B 1.390 . ? C32B C45B 1.362(10) . ? C33B C34B 1.390 . ? C34B C35B 1.390 . ? C35B C36B 1.390 . ? N41B N42B 1.420 . ? N41B C45B 1.420 . ? N42B C43B 1.420 . ? N42B C72B 1.365(13) . ? C43B C44B 1.420 . ? C44B C45B 1.420 . ? N51B Ag2 2.350(9) 2_855 ? N51B C52B 1.390 . ? N51B C56B 1.390 . ? C52B C53B 1.390 . ? C52B C65B 1.373(9) . ? C53B C54B 1.390 . ? C54B C55B 1.390 . ? C55B C56B 1.390 . ? N61B Ag2 2.286(9) 2_855 ? N61B N62B 1.420 . ? N61B C65B 1.420 . ? N62B C63B 1.420 . ? N62B C73B 1.371(12) . ? C63B C64B 1.420 . ? C64B C65B 1.420 . ? C71B C81B 1.513(12) . ? C72B C83B 1.517(12) . ? C73B C85B 1.515(12) . ? C81B C82B 1.390 . ? C81B C86B 1.390 . ? C82B C83B 1.390 . ? C82B C91B 1.554(13) . ? C83B C84B 1.390 . ? C84B C85B 1.390 . ? C84B C92B 1.555(12) . ? C85B C86B 1.390 . ? C86B C93B 1.562(12) . ? N11C C12C 1.390 . ? N11C C16C 1.390 . ? C12C C13C 1.390 . ? C12C C25C 1.368(8) . ? C13C C14C 1.390 . ? C14C C15C 1.390 . ? C15C C16C 1.390 . ? N21C N22C 1.420 . ? N21C C25C 1.420 . ? N22C C23C 1.420 . ? N22C C71C 1.367(12) . ? C23C C24C 1.420 . ? C24C C25C 1.420 . ? N31C C32C 1.390 . ? N31C C36C 1.390 . ? C32C C33C 1.390 . ? C32C C45C 1.358(8) . ? C33C C34C 1.390 . ? C34C C35C 1.390 . ? C35C C36C 1.390 . ? N41C N42C 1.420 . ? N41C C45C 1.420 . ? N42C C43C 1.420 . ? N42C C72C 1.388(12) . ? C43C C44C 1.420 . ? C44C C45C 1.420 . ? N51C C52C 1.390 . ? N51C C56C 1.390 . ? C52C C53C 1.390 . ? C52C C65C 1.305(11) . ? C53C C54C 1.390 . ? C54C C55C 1.390 . ? C55C C56C 1.390 . ? N61C N62C 1.420 . ? N61C C65C 1.420 . ? N62C C63C 1.420 . ? N62C C73C 1.372(13) . ? C63C C64C 1.420 . ? C64C C65C 1.420 . ? C71C C81C 1.518(12) . ? C72C C83C 1.514(12) . ? C73C C85C 1.516(13) . ? C81C C82C 1.390 . ? C81C C86C 1.390 . ? C82C C83C 1.390 . ? C82C C91C 1.559(12) . ? C83C C84C 1.390 . ? C84C C85C 1.390 . ? C84C C92C 1.568(13) . ? C85C C86C 1.390 . ? C86C C93C 1.559(13) . ? B1 F11 1.370(14) . ? B1 F12 1.360(14) . ? B1 F13 1.366(14) . ? B1 F14 1.351(14) . ? B2 F21 1.318(18) . ? B2 F22 1.328(18) . ? B2 F23 1.326(18) . ? B2 F24 1.317(18) . ? 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 N51A Ag1 N61A 72.7(3) . . ? N51A Ag1 N11C 120.2(4) . . ? N51A Ag1 N21C 137.4(4) . . ? N61A Ag1 N11C 128.8(4) . . ? N61A Ag1 N21C 134.0(4) . . ? N11C Ag1 N21C 72.8(3) . . ? Ag3 Ag2 N11B 81.0(3) 1_645 . ? Ag3 Ag2 N21B 118.0(3) 1_645 . ? Ag3 Ag2 N51B 74.1(3) 1_645 2_855 ? Ag3 Ag2 N61B 112.4(3) 1_645 2_855 ? N11B Ag2 N21B 71.2(4) . . ? N11B Ag2 N51B 153.8(4) . 2_855 ? N11B Ag2 N61B 125.6(4) . 2_855 ? N21B Ag2 N51B 113.5(4) . 2_855 ? N21B Ag2 N61B 129.0(4) . 2_855 ? N51B Ag2 N61B 73.1(4) 2_855 2_855 ? Ag2 Ag3 N11A 76.6(2) 1_465 . ? Ag2 Ag3 N21A 115.3(3) 1_465 . ? Ag2 Ag3 N31A 77.0(2) 1_465 2_666 ? Ag2 Ag3 N41A 113.4(3) 1_465 2_666 ? N11A Ag3 N21A 71.7(3) . . ? N11A Ag3 N31A 152.5(3) . 2_666 ? N11A Ag3 N41A 127.2(3) . 2_666 ? N21A Ag3 N31A 113.9(3) . 2_666 ? N21A Ag3 N41A 130.8(4) . 2_666 ? N31A Ag3 N41A 71.1(3) 2_666 2_666 ? N31B Ag4 N41B 73.3(4) . . ? N31B Ag4 N31C 114.1(4) . . ? N31B Ag4 N41C 137.0(5) . . ? N41B Ag4 N31C 131.9(4) . . ? N41B Ag4 N41C 135.8(4) . . ? N31C Ag4 N41C 72.7(3) . . ? Ag3 N11A C12A 115.5(5) . . ? Ag3 N11A C16A 124.4(5) . . ? C12A N11A C16A 120.0 . . ? N11A C12A C13A 120.0 . . ? N11A C12A C25A 118.5(8) . . ? C13A C12A C25A 121.5(8) . . ? C12A C13A C14A 120.0 . . ? C13A C14A C15A 120.0 . . ? C14A C15A C16A 120.0 . . ? N11A C16A C15A 120.0 . . ? Ag3 N21A N22A 137.2(5) . . ? Ag3 N21A C25A 114.7(5) . . ? N22A N21A C25A 108.0 . . ? N21A N22A C23A 108.0 . . ? N21A N22A C71A 121.4(9) . . ? C23A N22A C71A 130.6(9) . . ? N22A C23A C24A 108.0 . . ? C23A C24A C25A 108.0 . . ? C12A C25A N21A 119.3(8) . . ? C12A C25A C24A 132.7(8) . . ? N21A C25A C24A 108.0 . . ? Ag3 N31A C32A 115.6(5) 2_666 . ? Ag3 N31A C36A 124.3(5) 2_666 . ? C32A N31A C36A 120.0 . . ? N31A C32A C33A 120.0 . . ? N31A C32A C45A 117.5(8) . . ? C33A C32A C45A 122.4(8) . . ? C32A C33A C34A 120.0 . . ? C33A C34A C35A 120.0 . . ? C34A C35A C36A 120.0 . . ? N31A C36A C35A 120.0 . . ? Ag3 N41A N42A 135.5(5) 2_666 . ? Ag3 N41A C45A 116.1(5) 2_666 . ? N42A N41A C45A 108.0 . . ? N41A N42A C43A 108.0 . . ? N41A N42A C72A 121.4(9) . . ? C43A N42A C72A 130.0(9) . . ? N42A C43A C44A 108.0 . . ? C43A C44A C45A 108.0 . . ? C32A C45A N41A 119.2(8) . . ? C32A C45A C44A 132.7(8) . . ? N41A C45A C44A 108.0 . . ? Ag1 N51A C52A 115.3(6) . . ? Ag1 N51A C56A 124.6(6) . . ? C52A N51A C56A 120.0 . . ? N51A C52A C53A 120.0 . . ? N51A C52A C65A 117.4(8) . . ? C53A C52A C65A 122.6(8) . . ? C52A C53A C54A 120.0 . . ? C53A C54A C55A 120.0 . . ? C54A C55A C56A 120.0 . . ? N51A C56A C55A 120.0 . . ? Ag1 N61A N62A 137.6(5) . . ? Ag1 N61A C65A 113.4(5) . . ? N62A N61A C65A 108.0 . . ? N61A N62A C63A 108.0 . . ? N61A N62A C73A 122.3(9) . . ? C63A N62A C73A 129.6(9) . . ? N62A C63A C64A 108.0 . . ? C63A C64A C65A 108.0 . . ? C52A C65A N61A 120.5(8) . . ? C52A C65A C64A 131.5(8) . . ? N61A C65A C64A 108.0 . . ? N22A C71A C81A 110.0(11) . . ? N42A C72A C83A 113.7(11) . . ? N62A C73A C85A 117.1(11) . . ? C71A C81A C82A 117.5(9) . . ? C71A C81A C86A 122.4(9) . . ? C82A C81A C86A 120.0 . . ? C81A C82A C83A 120.0 . . ? C81A C82A C91A 121.6(10) . . ? C83A C82A C91A 118.0(10) . . ? C72A C83A C82A 120.5(9) . . ? C72A C83A C84A 119.3(9) . . ? C82A C83A C84A 120.0 . . ? C83A C84A C85A 120.0 . . ? C83A C84A C92A 121.2(8) . . ? C85A C84A C92A 118.6(8) . . ? C73A C85A C84A 120.3(8) . . ? C73A C85A C86A 119.2(8) . . ? C84A C85A C86A 120.0 . . ? C81A C86A C85A 120.0 . . ? C81A C86A C93A 119.5(9) . . ? C85A C86A C93A 120.5(9) . . ? Ag2 N11B C12B 117.8(6) . . ? Ag2 N11B C16B 122.2(6) . . ? C12B N11B C16B 120.0 . . ? N11B C12B C13B 120.0 . . ? N11B C12B C25B 118.2(9) . . ? C13B C12B C25B 121.8(9) . . ? C12B C13B C14B 120.0 . . ? C13B C14B C15B 120.0 . . ? C14B C15B C16B 120.0 . . ? N11B C16B C15B 120.0 . . ? Ag2 N21B N22B 138.5(6) . . ? Ag2 N21B C25B 113.5(6) . . ? N22B N21B C25B 108.0 . . ? N21B N22B C23B 108.0 . . ? N21B N22B C71B 121.1(10) . . ? C23B N22B C71B 130.7(10) . . ? N22B C23B C24B 108.0 . . ? C23B C24B C25B 108.0 . . ? C12B C25B N21B 119.3(9) . . ? C12B C25B C24B 132.7(9) . . ? N21B C25B C24B 108.0 . . ? Ag4 N31B C32B 114.6(6) . . ? Ag4 N31B C36B 125.4(7) . . ? C32B N31B C36B 120.0 . . ? N31B C32B C33B 120.0 . . ? N31B C32B C45B 117.8(9) . . ? C33B C32B C45B 122.1(9) . . ? C32B C33B C34B 120.0 . . ? C33B C34B C35B 120.0 . . ? C34B C35B C36B 120.0 . . ? N31B C36B C35B 120.0 . . ? Ag4 N41B N42B 138.3(6) . . ? Ag4 N41B C45B 113.5(6) . . ? N42B N41B C45B 108.0 . . ? N41B N42B C43B 108.0 . . ? N41B N42B C72B 122.2(11) . . ? C43B N42B C72B 129.7(11) . . ? N42B C43B C44B 108.0 . . ? C43B C44B C45B 108.0 . . ? C32B C45B N41B 120.4(9) . . ? C32B C45B C44B 131.5(9) . . ? N41B C45B C44B 108.0 . . ? Ag2 N51B C52B 114.6(5) 2_855 . ? Ag2 N51B C56B 125.4(5) 2_855 . ? C52B N51B C56B 120.0 . . ? N51B C52B C53B 120.0 . . ? N51B C52B C65B 117.1(8) . . ? C53B C52B C65B 122.9(8) . . ? C52B C53B C54B 120.0 . . ? C53B C54B C55B 120.0 . . ? C54B C55B C56B 120.0 . . ? N51B C56B C55B 120.0 . . ? Ag2 N61B N62B 138.7(6) 2_855 . ? Ag2 N61B C65B 113.2(6) 2_855 . ? N62B N61B C65B 108.0 . . ? N61B N62B C63B 108.0 . . ? N61B N62B C73B 121.8(9) . . ? C63B N62B C73B 130.1(9) . . ? N62B C63B C64B 108.0 . . ? C63B C64B C65B 108.0 . . ? C52B C65B N61B 122.1(9) . . ? C52B C65B C64B 129.9(9) . . ? N61B C65B C64B 108.0 . . ? N22B C71B C81B 110.5(12) . . ? N42B C72B C83B 118.6(13) . . ? N62B C73B C85B 111.8(11) . . ? C71B C81B C82B 119.9(10) . . ? C71B C81B C86B 120.0(10) . . ? C82B C81B C86B 120.0 . . ? C81B C82B C83B 120.0 . . ? C81B C82B C91B 121.3(9) . . ? C83B C82B C91B 118.7(9) . . ? C72B C83B C82B 120.5(9) . . ? C72B C83B C84B 119.2(9) . . ? C82B C83B C84B 120.0 . . ? C83B C84B C85B 120.0 . . ? C83B C84B C92B 119.6(9) . . ? C85B C84B C92B 120.3(8) . . ? C73B C85B C84B 119.5(9) . . ? C73B C85B C86B 120.4(9) . . ? C84B C85B C86B 120.0 . . ? C81B C86B C85B 120.0 . . ? C81B C86B C93B 117.5(10) . . ? C85B C86B C93B 122.2(10) . . ? Ag1 N11C C12C 114.0(5) . . ? Ag1 N11C C16C 125.9(5) . . ? C12C N11C C16C 120.0 . . ? N11C C12C C13C 120.0 . . ? N11C C12C C25C 117.5(7) . . ? C13C C12C C25C 122.4(7) . . ? C12C C13C C14C 120.0 . . ? C13C C14C C15C 120.0 . . ? C14C C15C C16C 120.0 . . ? N11C C16C C15C 120.0 . . ? Ag1 N21C N22C 136.2(5) . . ? Ag1 N21C C25C 115.4(5) . . ? N22C N21C C25C 108.0 . . ? N21C N22C C23C 108.0 . . ? N21C N22C C71C 120.2(8) . . ? C23C N22C C71C 131.7(9) . . ? N22C C23C C24C 108.0 . . ? C23C C24C C25C 108.0 . . ? C12C C25C N21C 119.8(7) . . ? C12C C25C C24C 132.2(7) . . ? N21C C25C C24C 108.0 . . ? Ag4 N31C C32C 113.9(5) . . ? Ag4 N31C C36C 126.0(5) . . ? C32C N31C C36C 120.0 . . ? N31C C32C C33C 120.0 . . ? N31C C32C C45C 117.5(8) . . ? C33C C32C C45C 122.5(8) . . ? C32C C33C C34C 120.0 . . ? C33C C34C C35C 120.0 . . ? C34C C35C C36C 120.0 . . ? N31C C36C C35C 120.0 . . ? Ag4 N41C N42C 135.0(5) . . ? Ag4 N41C C45C 115.6(5) . . ? N42C N41C C45C 108.0 . . ? N41C N42C C43C 108.0 . . ? N41C N42C C72C 122.0(8) . . ? C43C N42C C72C 129.4(9) . . ? N42C C43C C44C 108.0 . . ? C43C C44C C45C 108.0 . . ? C32C C45C N41C 119.7(7) . . ? C32C C45C C44C 132.3(7) . . ? N41C C45C C44C 108.0 . . ? C52C N51C C56C 120.0 . . ? N51C C52C C53C 120.0 . . ? N51C C52C C65C 103.2(10) . . ? C53C C52C C65C 136.7(10) . . ? C52C C53C C54C 120.0 . . ? C53C C54C C55C 120.0 . . ? C54C C55C C56C 120.0 . . ? N51C C56C C55C 120.0 . . ? N62C N61C C65C 108.0 . . ? N61C N62C C63C 108.0 . . ? N61C N62C C73C 124.6(12) . . ? C63C N62C C73C 127.3(12) . . ? N62C C63C C64C 108.0 . . ? C63C C64C C65C 108.0 . . ? C52C C65C N61C 109.3(10) . . ? C52C C65C C64C 142.6(10) . . ? N61C C65C C64C 108.0 . . ? N22C C71C C81C 118.9(11) . . ? N42C C72C C83C 113.1(11) . . ? N62C C73C C85C 117.9(14) . . ? C71C C81C C82C 118.6(9) . . ? C71C C81C C86C 121.4(9) . . ? C82C C81C C86C 120.0 . . ? C81C C82C C83C 120.0 . . ? C81C C82C C91C 122.9(8) . . ? C83C C82C C91C 117.1(8) . . ? C72C C83C C82C 122.8(9) . . ? C72C C83C C84C 117.0(9) . . ? C82C C83C C84C 120.0 . . ? C83C C84C C85C 120.0 . . ? C83C C84C C92C 123.4(10) . . ? C85C C84C C92C 116.5(10) . . ? C73C C85C C84C 118.6(11) . . ? C73C C85C C86C 121.4(11) . . ? C84C C85C C86C 120.0 . . ? C81C C86C C85C 120.0 . . ? C81C C86C C93C 118.1(10) . . ? C85C C86C C93C 121.8(10) . . ? F11 B1 F12 107.6(11) . . ? F11 B1 F13 109.5(11) . . ? F11 B1 F14 110.3(12) . . ? F12 B1 F13 108.8(11) . . ? F12 B1 F14 109.2(11) . . ? F13 B1 F14 111.2(11) . . ? F21 B2 F22 109.6(13) . . ? F21 B2 F23 109.5(13) . . ? F21 B2 F24 110.3(13) . . ? F22 B2 F23 108.9(13) . . ? F22 B2 F24 109.4(13) . . ? F23 B2 F24 109.2(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag2 Ag3 N11A C12A 119.1(5) 1_465 . . . ? Ag2 Ag3 N11A C16A -57.5(5) 1_465 . . . ? N21A Ag3 N11A C12A -3.7(5) . . . . ? N21A Ag3 N11A C16A 179.7(6) . . . . ? N31A Ag3 N11A C12A 103.2(8) 2_666 . . . ? N31A Ag3 N11A C16A -73.5(9) 2_666 . . . ? N41A Ag3 N11A C12A -131.5(6) 2_666 . . . ? N41A Ag3 N11A C16A 51.9(7) 2_666 . . . ? Ag3 N11A C12A C13A -176.8(6) . . . . ? Ag3 N11A C12A C25A 4.1(10) . . . . ? C16A N11A C12A C13A 0.0 . . . . ? C16A N11A C12A C25A -179.1(11) . . . . ? N11A C12A C13A C14A 0.0 . . . . ? C25A C12A C13A C14A 179.1(11) . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C13A C14A C15A C16A 0.0 . . . . ? C14A C15A C16A N11A 0.0 . . . . ? Ag3 N11A C16A C15A 176.5(7) . . . . ? C12A N11A C16A C15A 0.0 . . . . ? Ag2 Ag3 N21A N22A 114.1(9) 1_465 . . . ? Ag2 Ag3 N21A C25A -61.9(6) 1_465 . . . ? N11A Ag3 N21A N22A 178.8(10) . . . . ? N11A Ag3 N21A C25A 2.9(6) . . . . ? N31A Ag3 N21A N22A 27.7(10) 2_666 . . . ? N31A Ag3 N21A C25A -148.3(6) 2_666 . . . ? N41A Ag3 N21A N22A -57.3(10) 2_666 . . . ? N41A Ag3 N21A C25A 126.7(6) 2_666 . . . ? Ag3 N21A N22A C23A -176.2(10) . . . . ? Ag3 N21A N22A C71A 1.5(17) . . . . ? C25A N21A N22A C23A 0.0 . . . . ? C25A N21A N22A C71A 177.7(15) . . . . ? N21A N22A C23A C24A 0.0 . . . . ? C71A N22A C23A C24A -177.4(16) . . . . ? N22A C23A C24A C25A 0.0 . . . . ? N11A C12A C25A N21A -1.5(13) . . . . ? N11A C12A C25A C24A 179.7(8) . . . . ? C13A C12A C25A N21A 179.4(7) . . . . ? C13A C12A C25A C24A 0.7(15) . . . . ? C23A C24A C25A C12A 178.9(15) . . . . ? C23A C24A C25A N21A 0.0 . . . . ? Ag3 N21A C25A C12A -1.9(11) . . . . ? Ag3 N21A C25A C24A 177.1(7) . . . . ? N22A N21A C25A C12A -179.0(12) . . . . ? N22A N21A C25A C24A 0.0 . . . . ? Ag3 N31A C32A C33A 177.1(6) 2_666 . . . ? Ag3 N31A C32A C45A 0.8(10) 2_666 . . . ? C36A N31A C32A C33A 0.0 . . . . ? C36A N31A C32A C45A -176.4(11) . . . . ? N31A C32A C33A C34A 0.0 . . . . ? C45A C32A C33A C34A 176.2(11) . . . . ? C32A C33A C34A C35A 0.0 . . . . ? C33A C34A C35A C36A 0.0 . . . . ? C34A C35A C36A N31A 0.0 . . . . ? Ag3 N31A C36A C35A -176.9(7) 2_666 . . . ? C32A N31A C36A C35A 0.0 . . . . ? Ag3 N41A N42A C43A 172.6(10) 2_666 . . . ? Ag3 N41A N42A C72A 0.5(16) 2_666 . . . ? C45A N41A N42A C43A 0.0 . . . . ? C45A N41A N42A C72A -172.1(14) . . . . ? N41A N42A C43A C44A 0.0 . . . . ? C72A N42A C43A C44A 171.2(15) . . . . ? N42A C43A C44A C45A 0.0 . . . . ? N31A C32A C45A N41A -6.5(13) . . . . ? N31A C32A C45A C44A 177.9(8) . . . . ? C33A C32A C45A N41A 177.2(7) . . . . ? C33A C32A C45A C44A 1.6(15) . . . . ? C43A C44A C45A C32A 176.0(14) . . . . ? C43A C44A C45A N41A 0.0 . . . . ? Ag3 N41A C45A C32A 9.1(11) 2_666 . . . ? Ag3 N41A C45A C44A -174.3(8) 2_666 . . . ? N42A N41A C45A C32A -176.6(12) . . . . ? N42A N41A C45A C44A 0.0 . . . . ? N61A Ag1 N51A C52A 2.6(6) . . . . ? N61A Ag1 N51A C56A -175.0(8) . . . . ? N11C Ag1 N51A C52A 127.9(6) . . . . ? N11C Ag1 N51A C56A -49.8(8) . . . . ? N21C Ag1 N51A C52A -134.8(7) . . . . ? N21C Ag1 N51A C56A 47.5(10) . . . . ? Ag1 N51A C52A C53A -177.8(8) . . . . ? Ag1 N51A C52A C65A 1.4(11) . . . . ? C56A N51A C52A C53A 0.0 . . . . ? C56A N51A C52A C65A 179.2(13) . . . . ? N51A C52A C53A C54A 0.0 . . . . ? C65A C52A C53A C54A -179.1(14) . . . . ? C52A C53A C54A C55A 0.0 . . . . ? C53A C54A C55A C56A 0.0 . . . . ? C54A C55A C56A N51A 0.0 . . . . ? Ag1 N51A C56A C55A 177.6(9) . . . . ? C52A N51A C56A C55A 0.0 . . . . ? N51A Ag1 N61A N62A -172.6(11) . . . . ? N51A Ag1 N61A C65A -6.0(6) . . . . ? N11C Ag1 N61A N62A 72.2(11) . . . . ? N11C Ag1 N61A C65A -121.2(6) . . . . ? N21C Ag1 N61A N62A -32.2(12) . . . . ? N21C Ag1 N61A C65A 134.4(6) . . . . ? Ag1 N61A N62A C63A 167.1(11) . . . . ? Ag1 N61A N62A C73A -10.2(17) . . . . ? C65A N61A N62A C63A 0.0 . . . . ? C65A N61A N62A C73A -177.3(14) . . . . ? N61A N62A C63A C64A 0.0 . . . . ? C73A N62A C63A C64A 177.0(15) . . . . ? N62A C63A C64A C65A 0.0 . . . . ? N51A C52A C65A N61A -7.4(14) . . . . ? N51A C52A C65A C64A 172.7(9) . . . . ? C53A C52A C65A N61A 171.7(8) . . . . ? C53A C52A C65A C64A -8.2(17) . . . . ? Ag1 N61A C65A C52A 9.5(12) . . . . ? Ag1 N61A C65A C64A -170.5(8) . . . . ? N62A N61A C65A C52A -179.9(13) . . . . ? N62A N61A C65A C64A 0.0 . . . . ? C63A C64A C65A C52A 179.9(15) . . . . ? C63A C64A C65A N61A 0.0 . . . . ? N21A N22A C71A C81A 152.8(10) . . . . ? C23A N22A C71A C81A -30(2) . . . . ? N41A N42A C72A C83A -150.0(10) . . . . ? C43A N42A C72A C83A 40(2) . . . . ? N61A N62A C73A C85A -29(2) . . . . ? C63A N62A C73A C85A 154.2(11) . . . . ? N22A C71A C81A C82A -82.5(16) . . . . ? N22A C71A C81A C86A 93.6(15) . . . . ? C71A C81A C82A C83A 176.2(11) . . . . ? C71A C81A C82A C91A 3.3(16) . . . . ? C86A C81A C82A C83A 0.0 . . . . ? C86A C81A C82A C91A -172.9(15) . . . . ? C81A C82A C83A C72A 174.8(12) . . . . ? C81A C82A C83A C84A 0.0 . . . . ? C91A C82A C83A C72A -12.1(16) . . . . ? C91A C82A C83A C84A 173.1(15) . . . . ? N42A C72A C83A C82A 84.2(16) . . . . ? N42A C72A C83A C84A -101.0(14) . . . . ? C72A C83A C84A C85A -174.8(12) . . . . ? C72A C83A C84A C92A 9.5(14) . . . . ? C82A C83A C84A C85A 0.0 . . . . ? C82A C83A C84A C92A -175.7(13) . . . . ? C83A C84A C85A C73A -172.1(12) . . . . ? C83A C84A C85A C86A 0.0 . . . . ? C92A C84A C85A C73A 3.7(14) . . . . ? C92A C84A C85A C86A 175.8(13) . . . . ? N62A C73A C85A C84A -61.3(17) . . . . ? N62A C73A C85A C86A 126.5(13) . . . . ? C73A C85A C86A C81A 172.2(12) . . . . ? C73A C85A C86A C93A -8.0(17) . . . . ? C84A C85A C86A C81A 0.0 . . . . ? C84A C85A C86A C93A 179.8(16) . . . . ? C71A C81A C86A C85A -176.0(12) . . . . ? C71A C81A C86A C93A 4.2(16) . . . . ? C82A C81A C86A C85A 0.0 . . . . ? C82A C81A C86A C93A -179.8(15) . . . . ? Ag3 Ag2 N11B C12B 123.8(6) 1_645 . . . ? Ag3 Ag2 N11B C16B -55.3(5) 1_645 . . . ? N21B Ag2 N11B C12B 0.0(6) . . . . ? N21B Ag2 N11B C16B -179.1(7) . . . . ? N51B Ag2 N11B C12B 105.1(9) 2_855 . . . ? N51B Ag2 N11B C16B -74.0(11) 2_855 . . . ? N61B Ag2 N11B C12B -125.0(6) 2_855 . . . ? N61B Ag2 N11B C16B 55.9(7) 2_855 . . . ? Ag2 N11B C12B C13B -179.1(7) . . . . ? Ag2 N11B C12B C25B 1.1(11) . . . . ? C16B N11B C12B C13B 0.0 . . . . ? C16B N11B C12B C25B -179.8(12) . . . . ? N11B C12B C13B C14B 0.0 . . . . ? C25B C12B C13B C14B 179.8(12) . . . . ? C12B C13B C14B C15B 0.0 . . . . ? C13B C14B C15B C16B 0.0 . . . . ? C14B C15B C16B N11B 0.0 . . . . ? Ag2 N11B C16B C15B 179.1(7) . . . . ? C12B N11B C16B C15B 0.0 . . . . ? Ag3 Ag2 N21B N22B 110.7(11) 1_645 . . . ? Ag3 Ag2 N21B C25B -69.5(7) 1_645 . . . ? N11B Ag2 N21B N22B 179.1(12) . . . . ? N11B Ag2 N21B C25B -1.1(7) . . . . ? N51B Ag2 N21B N22B 26.8(12) 2_855 . . . ? N51B Ag2 N21B C25B -153.4(7) 2_855 . . . ? N61B Ag2 N21B N22B -59.9(12) 2_855 . . . ? N61B Ag2 N21B C25B 119.9(7) 2_855 . . . ? Ag2 N21B N22B C23B 179.8(13) . . . . ? Ag2 N21B N22B C71B -4.8(19) . . . . ? C25B N21B N22B C23B 0.0 . . . . ? C25B N21B N22B C71B 175.4(16) . . . . ? N21B N22B C23B C24B 0.0 . . . . ? C71B N22B C23B C24B -174.8(18) . . . . ? N22B C23B C24B C25B 0.0 . . . . ? N11B C12B C25B N21B -2.2(15) . . . . ? N11B C12B C25B C24B -179.6(10) . . . . ? C13B C12B C25B N21B 178.0(8) . . . . ? C13B C12B C25B C24B 0.6(17) . . . . ? Ag2 N21B C25B C12B 2.2(13) . . . . ? Ag2 N21B C25B C24B -179.9(9) . . . . ? N22B N21B C25B C12B -178.0(14) . . . . ? N22B N21B C25B C24B 0.0 . . . . ? C23B C24B C25B C12B 177.6(16) . . . . ? C23B C24B C25B N21B 0.0 . . . . ? N41B Ag4 N31B C32B 0.0(6) . . . . ? N41B Ag4 N31B C36B -178.0(8) . . . . ? N31C Ag4 N31B C32B 129.0(6) . . . . ? N31C Ag4 N31B C36B -48.9(9) . . . . ? N41C Ag4 N31B C32B -140.9(7) . . . . ? N41C Ag4 N31B C36B 41.1(10) . . . . ? Ag4 N31B C32B C33B -178.1(8) . . . . ? Ag4 N31B C32B C45B 3.8(12) . . . . ? C36B N31B C32B C33B 0.0 . . . . ? C36B N31B C32B C45B -178.1(14) . . . . ? N31B C32B C33B C34B 0.0 . . . . ? C45B C32B C33B C34B 178.0(14) . . . . ? C32B C33B C34B C35B 0.0 . . . . ? C33B C34B C35B C36B 0.0 . . . . ? C34B C35B C36B N31B 0.0 . . . . ? Ag4 N31B C36B C35B 177.9(9) . . . . ? C32B N31B C36B C35B 0.0 . . . . ? N31B Ag4 N41B N42B -178.4(12) . . . . ? N31B Ag4 N41B C45B -3.5(7) . . . . ? N31C Ag4 N41B N42B 74.0(12) . . . . ? N31C Ag4 N41B C45B -111.1(8) . . . . ? N41C Ag4 N41B N42B -36.5(13) . . . . ? N41C Ag4 N41B C45B 138.4(7) . . . . ? Ag4 N41B N42B C43B 175.1(12) . . . . ? Ag4 N41B N42B C72B -3(2) . . . . ? C45B N41B N42B C43B 0.0 . . . . ? C45B N41B N42B C72B -178.4(16) . . . . ? N41B N42B C43B C44B 0.0 . . . . ? C72B N42B C43B C44B 178.2(18) . . . . ? N42B C43B C44B C45B 0.0 . . . . ? N31B C32B C45B N41B -7.5(16) . . . . ? N31B C32B C45B C44B 177.1(10) . . . . ? C33B C32B C45B N41B 174.5(8) . . . . ? C33B C32B C45B C44B -0.9(18) . . . . ? C43B C44B C45B C32B 175.8(17) . . . . ? C43B C44B C45B N41B 0.0 . . . . ? Ag4 N41B C45B C32B 7.2(14) . . . . ? Ag4 N41B C45B C44B -176.5(9) . . . . ? N42B N41B C45B C32B -176.4(15) . . . . ? N42B N41B C45B C44B 0.0 . . . . ? Ag2 N51B C52B C53B 178.0(7) 2_855 . . . ? Ag2 N51B C52B C65B -1.9(11) 2_855 . . . ? C56B N51B C52B C53B 0.0 . . . . ? C56B N51B C52B C65B -179.9(12) . . . . ? N51B C52B C53B C54B 0.0 . . . . ? C65B C52B C53B C54B 179.9(13) . . . . ? C52B C53B C54B C55B 0.0 . . . . ? C53B C54B C55B C56B 0.0 . . . . ? C54B C55B C56B N51B 0.0 . . . . ? Ag2 N51B C56B C55B -177.8(7) 2_855 . . . ? C52B N51B C56B C55B 0.0 . . . . ? Ag2 N61B N62B C63B 176.0(12) 2_855 . . . ? Ag2 N61B N62B C73B -1.2(19) 2_855 . . . ? C65B N61B N62B C63B 0.0 . . . . ? C65B N61B N62B C73B -177.2(16) . . . . ? N61B N62B C63B C64B 0.0 . . . . ? C73B N62B C63B C64B 176.9(18) . . . . ? N62B C63B C64B C65B 0.0 . . . . ? N51B C52B C65B N61B 1.1(15) . . . . ? N51B C52B C65B C64B 177.9(9) . . . . ? C53B C52B C65B N61B -178.8(8) . . . . ? C53B C52B C65B C64B -2.0(16) . . . . ? C63B C64B C65B C52B -177.2(16) . . . . ? C63B C64B C65B N61B 0.0 . . . . ? Ag2 N61B C65B C52B 0.3(14) 2_855 . . . ? Ag2 N61B C65B C64B -177.2(9) 2_855 . . . ? N62B N61B C65B C52B 177.4(14) . . . . ? N62B N61B C65B C64B 0.0 . . . . ? N21B N22B C71B C81B 146.7(12) . . . . ? C23B N22B C71B C81B -39(2) . . . . ? N41B N42B C72B C83B -28(2) . . . . ? C43B N42B C72B C83B 154.3(12) . . . . ? N61B N62B C73B C85B -154.9(11) . . . . ? C63B N62B C73B C85B 29(2) . . . . ? N22B C71B C81B C82B 97.4(16) . . . . ? N22B C71B C81B C86B -79.2(18) . . . . ? C71B C81B C82B C83B -176.6(13) . . . . ? C71B C81B C82B C91B 5.6(18) . . . . ? C86B C81B C82B C83B 0.0 . . . . ? C86B C81B C82B C91B -177.8(17) . . . . ? C81B C82B C83B C72B 174.0(14) . . . . ? C81B C82B C83B C84B 0.0 . . . . ? C91B C82B C83B C72B -8.1(19) . . . . ? C91B C82B C83B C84B 177.9(17) . . . . ? N42B C72B C83B C82B 125.7(15) . . . . ? N42B C72B C83B C84B -60(2) . . . . ? C72B C83B C84B C85B -174.1(14) . . . . ? C72B C83B C84B C92B 2.8(17) . . . . ? C82B C83B C84B C85B 0.0 . . . . ? C82B C83B C84B C92B 176.9(15) . . . . ? C83B C84B C85B C73B -177.4(13) . . . . ? C83B C84B C85B C86B 0.0 . . . . ? C92B C84B C85B C73B 5.7(16) . . . . ? C92B C84B C85B C86B -176.9(15) . . . . ? N62B C73B C85B C84B -99.8(15) . . . . ? N62B C73B C85B C86B 82.8(17) . . . . ? C73B C85B C86B C81B 177.4(13) . . . . ? C73B C85B C86B C93B -9.4(17) . . . . ? C84B C85B C86B C81B 0.0 . . . . ? C84B C85B C86B C93B 173.3(15) . . . . ? C71B C81B C86B C85B 176.6(13) . . . . ? C71B C81B C86B C93B 3.0(16) . . . . ? C82B C81B C86B C85B 0.0 . . . . ? C82B C81B C86B C93B -173.6(14) . . . . ? N51A Ag1 N11C C12C 135.0(6) . . . . ? N51A Ag1 N11C C16C -41.8(8) . . . . ? N61A Ag1 N11C C12C -133.5(6) . . . . ? N61A Ag1 N11C C16C 49.7(8) . . . . ? N21C Ag1 N11C C12C -0.3(6) . . . . ? N21C Ag1 N11C C16C -177.1(8) . . . . ? Ag1 N11C C12C C13C -177.0(7) . . . . ? Ag1 N11C C12C C25C 4.4(11) . . . . ? C16C N11C C12C C13C 0.0 . . . . ? C16C N11C C12C C25C -178.6(12) . . . . ? N11C C12C C13C C14C 0.0 . . . . ? C25C C12C C13C C14C 178.6(13) . . . . ? C12C C13C C14C C15C 0.0 . . . . ? C13C C14C C15C C16C 0.0 . . . . ? C14C C15C C16C N11C 0.0 . . . . ? Ag1 N11C C16C C15C 176.6(8) . . . . ? C12C N11C C16C C15C 0.0 . . . . ? N51A Ag1 N21C N22C 68.3(11) . . . . ? N51A Ag1 N21C C25C -119.7(7) . . . . ? N61A Ag1 N21C N22C -47.8(11) . . . . ? N61A Ag1 N21C C25C 124.2(7) . . . . ? N11C Ag1 N21C N22C -175.6(10) . . . . ? N11C Ag1 N21C C25C -3.5(7) . . . . ? Ag1 N21C N22C C23C 172.4(11) . . . . ? Ag1 N21C N22C C71C -10.7(17) . . . . ? C25C N21C N22C C23C 0.0 . . . . ? C25C N21C N22C C71C 176.9(15) . . . . ? N21C N22C C23C C24C 0.0 . . . . ? C71C N22C C23C C24C -176.4(17) . . . . ? N22C C23C C24C C25C 0.0 . . . . ? N11C C12C C25C N21C -8.0(14) . . . . ? N11C C12C C25C C24C 174.2(9) . . . . ? C13C C12C C25C N21C 173.4(8) . . . . ? C13C C12C C25C C24C -4.4(17) . . . . ? Ag1 N21C C25C C12C 7.5(12) . . . . ? Ag1 N21C C25C C24C -174.2(8) . . . . ? N22C N21C C25C C12C -178.3(13) . . . . ? N22C N21C C25C C24C 0.0 . . . . ? C23C C24C C25C C12C 178.0(15) . . . . ? C23C C24C C25C N21C 0.0 . . . . ? N31B Ag4 N31C C32C 136.9(7) . . . . ? N31B Ag4 N31C C36C -38.9(9) . . . . ? N41B Ag4 N31C C32C -134.4(7) . . . . ? N41B Ag4 N31C C36C 49.8(10) . . . . ? N41C Ag4 N31C C32C 2.4(7) . . . . ? N41C Ag4 N31C C36C -173.4(9) . . . . ? Ag4 N31C C32C C33C -176.1(9) . . . . ? Ag4 N31C C32C C45C 1.9(13) . . . . ? C36C N31C C32C C33C 0.0 . . . . ? C36C N31C C32C C45C 178.0(14) . . . . ? N31C C32C C33C C34C 0.0 . . . . ? C45C C32C C33C C34C -177.9(15) . . . . ? C32C C33C C34C C35C 0.0 . . . . ? C33C C34C C35C C36C 0.0 . . . . ? C34C C35C C36C N31C 0.0 . . . . ? Ag4 N31C C36C C35C 175.6(10) . . . . ? C32C N31C C36C C35C 0.0 . . . . ? N31B Ag4 N41C N42C 82.1(12) . . . . ? N31B Ag4 N41C C45C -113.2(8) . . . . ? N41B Ag4 N41C N42C -37.7(13) . . . . ? N41B Ag4 N41C C45C 127.0(7) . . . . ? N31C Ag4 N41C N42C -170.9(11) . . . . ? N31C Ag4 N41C C45C -6.2(7) . . . . ? Ag4 N41C N42C C43C 165.5(12) . . . . ? Ag4 N41C N42C C72C -22.6(18) . . . . ? C45C N41C N42C C43C 0.0 . . . . ? C45C N41C N42C C72C 172.0(15) . . . . ? N41C N42C C43C C44C 0.0 . . . . ? C72C N42C C43C C44C -171.2(16) . . . . ? N42C C43C C44C C45C 0.0 . . . . ? N31C C32C C45C N41C -7.8(17) . . . . ? N31C C32C C45C C44C 170.5(11) . . . . ? C33C C32C C45C N41C 170.1(9) . . . . ? C33C C32C C45C C44C -11.6(19) . . . . ? Ag4 N41C C45C C32C 10.0(14) . . . . ? Ag4 N41C C45C C44C -168.7(10) . . . . ? N42C N41C C45C C32C 178.7(15) . . . . ? N42C N41C C45C C44C 0.0 . . . . ? C43C C44C C45C C32C -178.5(18) . . . . ? C43C C44C C45C N41C 0.0 . . . . ? C56C N51C C52C C53C 0.0 . . . . ? C56C N51C C52C C65C -178.6(15) . . . . ? N51C C52C C53C C54C 0.0 . . . . ? C65C C52C C53C C54C 178(2) . . . . ? C52C C53C C54C C55C 0.0 . . . . ? C53C C54C C55C C56C 0.0 . . . . ? C54C C55C C56C N51C 0.0 . . . . ? C52C N51C C56C C55C 0.0 . . . . ? C65C N61C N62C C63C 0.0 . . . . ? C65C N61C N62C C73C 178.3(18) . . . . ? N61C N62C C63C C64C 0.0 . . . . ? C73C N62C C63C C64C -178.3(18) . . . . ? N62C C63C C64C C65C 0.0 . . . . ? N51C C52C C65C N61C 179.8(9) . . . . ? N51C C52C C65C C64C 4(2) . . . . ? C53C C52C C65C N61C 2(2) . . . . ? C53C C52C C65C C64C -174.3(14) . . . . ? C63C C64C C65C C52C 176(3) . . . . ? C63C C64C C65C N61C 0.0 . . . . ? N62C N61C C65C C52C -177.4(16) . . . . ? N62C N61C C65C C64C 0.0 . . . . ? N21C N22C C71C C81C -41(2) . . . . ? C23C N22C C71C C81C 135.4(12) . . . . ? N41C N42C C72C C83C -43.1(18) . . . . ? C43C N42C C72C C83C 127.0(12) . . . . ? N61C N62C C73C C85C -45(2) . . . . ? C63C N62C C73C C85C 132.7(14) . . . . ? N22C C71C C81C C82C 122.2(14) . . . . ? N22C C71C C81C C86C -58.2(18) . . . . ? C71C C81C C82C C83C 179.6(12) . . . . ? C71C C81C C82C C91C -0.8(14) . . . . ? C86C C81C C82C C83C 0.0 . . . . ? C86C C81C C82C C91C 179.6(13) . . . . ? C81C C82C C83C C72C -175.2(12) . . . . ? C81C C82C C83C C84C 0.0 . . . . ? C91C C82C C83C C72C 5.2(14) . . . . ? C91C C82C C83C C84C -179.6(12) . . . . ? N42C C72C C83C C82C 119.1(12) . . . . ? N42C C72C C83C C84C -56.2(15) . . . . ? C72C C83C C84C C85C 175.5(11) . . . . ? C72C C83C C84C C92C -8.3(16) . . . . ? C82C C83C C84C C85C 0.0 . . . . ? C82C C83C C84C C92C 176.2(15) . . . . ? C83C C84C C85C C73C -179.0(13) . . . . ? C83C C84C C85C C86C 0.0 . . . . ? C92C C84C C85C C73C 4.5(15) . . . . ? C92C C84C C85C C86C -176.5(14) . . . . ? N62C C73C C85C C84C -89.6(19) . . . . ? N62C C73C C85C C86C 91.4(19) . . . . ? C73C C85C C86C C81C 179.0(13) . . . . ? C73C C85C C86C C93C 3.6(18) . . . . ? C84C C85C C86C C81C 0.0 . . . . ? C84C C85C C86C C93C -175.4(16) . . . . ? C71C C81C C86C C85C -179.6(12) . . . . ? C71C C81C C86C C93C -4.1(16) . . . . ? C82C C81C C86C C85C 0.0 . . . . ? C82C C81C C86C C93C 175.5(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.69 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.215 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.182 #===END data_imw620 _database_code_depnum_ccdc_archive 'CCDC 609497' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Hg N6, 2(Cl O4)' _chemical_formula_sum 'C24 H20 Cl2 Hg N6 O8' _chemical_formula_weight 791.95 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' 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 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 34.5280(17) _cell_length_b 14.1848(6) _cell_length_c 16.4180(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.7320(10) _cell_angle_gamma 90.00 _cell_volume 7181.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6077 _cell_measurement_theta_min 4.96 _cell_measurement_theta_max 40.08 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 4.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6154 _exptl_absorpt_correction_T_max 0.8070 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 44595 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7850 _reflns_number_gt 5191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^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 7850 _refine_ls_number_parameters 370 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.009 _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 0.231751(6) 0.153657(14) 0.264972(12) 0.03428(8) Uani 1 1 d . . . N11 N 0.20541(13) 0.1116(3) 0.3588(3) 0.0358(10) Uani 1 1 d . . . C12 C 0.23120(18) 0.1190(4) 0.4499(4) 0.0390(13) Uani 1 1 d . . . C13 C 0.2159(2) 0.0901(3) 0.5115(3) 0.0455(15) Uani 1 1 d . . . H13A H 0.2338 0.0942 0.5739 0.055 Uiso 1 1 calc R . . C14 C 0.1749(2) 0.0562(4) 0.4808(4) 0.0478(15) Uani 1 1 d . . . H14A H 0.1644 0.0381 0.5215 0.057 Uiso 1 1 calc R . . C15 C 0.14950(18) 0.0492(4) 0.3885(4) 0.0473(14) Uani 1 1 d . . . H15A H 0.1216 0.0246 0.3664 0.057 Uiso 1 1 calc R . . C16 C 0.16474(17) 0.0781(4) 0.3281(4) 0.0419(13) Uani 1 1 d . . . H16A H 0.1468 0.0745 0.2657 0.050 Uiso 1 1 calc R . . N21 N 0.28547(14) 0.1835(3) 0.4133(3) 0.0392(11) Uani 1 1 d . . . N22 N 0.32748(14) 0.2098(3) 0.4577(3) 0.0418(11) Uani 1 1 d . . . C23 C 0.34230(19) 0.1996(4) 0.5481(4) 0.0479(15) Uani 1 1 d . . . H23A H 0.3702 0.2137 0.5922 0.058 Uiso 1 1 calc R . . C24 C 0.30980(19) 0.1654(3) 0.5644(4) 0.0435(14) Uani 1 1 d . . . H24A H 0.3106 0.1516 0.6205 0.052 Uiso 1 1 calc R . . C25 C 0.27494(17) 0.1558(3) 0.4782(3) 0.0354(12) Uani 1 1 d . . . C31 C 0.35000(16) 0.2459(4) 0.4065(4) 0.0469(14) Uani 1 1 d . . . H31A H 0.3556 0.3126 0.4189 0.056 Uiso 1 1 calc R . . H31B H 0.3313 0.2386 0.3417 0.056 Uiso 1 1 calc R . . C32 C 0.39195(17) 0.1960(4) 0.4304(3) 0.0528(15) Uani 1 1 d DU . . C33 C 0.4300(2) 0.2490(5) 0.4751(4) 0.083(2) Uani 1 1 d DU . . H33A H 0.4288 0.3109 0.4926 0.100 Uiso 1 1 calc R . . C34 C 0.4695(2) 0.2083(6) 0.4929(5) 0.117(3) Uani 1 1 d DU . . H34A H 0.4948 0.2432 0.5229 0.141 Uiso 1 1 calc R . . C35 C 0.4720(2) 0.1167(6) 0.4669(5) 0.102(3) Uani 1 1 d DU . . H35 H 0.4987 0.0907 0.4786 0.123 Uiso 1 1 calc R . . C36 C 0.43471(18) 0.0640(5) 0.4235(4) 0.077(2) Uani 1 1 d DU . . H36A H 0.4362 0.0022 0.4063 0.092 Uiso 1 1 calc R . . C37 C 0.39442(16) 0.1038(4) 0.4054(3) 0.0508(15) Uani 1 1 d DU . . C38 C 0.35469(15) 0.0405(4) 0.3600(3) 0.0410(13) Uani 1 1 d . . . H38A H 0.3640 -0.0249 0.3688 0.049 Uiso 1 1 calc R . . H38B H 0.3361 0.0499 0.3895 0.049 Uiso 1 1 calc R . . N41 N 0.29007(12) 0.1012(3) 0.2287(3) 0.0327(10) Uani 1 1 d . . . N42 N 0.32963(12) 0.0590(3) 0.2620(3) 0.0384(10) Uani 1 1 d . . . C43 C 0.34047(17) 0.0404(4) 0.1948(4) 0.0491(15) Uani 1 1 d . . . H43A H 0.3662 0.0127 0.2020 0.059 Uiso 1 1 calc R . . C44 C 0.30744(17) 0.0689(4) 0.1140(4) 0.0409(13) Uani 1 1 d . . . H44A H 0.3058 0.0647 0.0560 0.049 Uiso 1 1 calc R . . C45 C 0.27643(15) 0.1061(3) 0.1385(3) 0.0317(11) Uani 1 1 d . . . N51 N 0.21032(12) 0.1807(3) 0.1219(3) 0.0316(10) Uani 1 1 d . . . C52 C 0.23414(15) 0.1488(3) 0.0814(3) 0.0312(12) Uani 1 1 d . . . C53 C 0.21889(17) 0.1591(3) -0.0121(3) 0.0357(12) Uani 1 1 d . . . H53A H 0.2353 0.1368 -0.0401 0.043 Uiso 1 1 calc R . . C54 C 0.17987(16) 0.2019(4) -0.0633(4) 0.0394(13) Uani 1 1 d . . . H54A H 0.1692 0.2080 -0.1261 0.047 Uiso 1 1 calc R . . C55 C 0.15690(16) 0.2357(4) -0.0198(3) 0.0449(14) Uani 1 1 d . . . H55A H 0.1306 0.2663 -0.0529 0.054 Uiso 1 1 calc R . . C56 C 0.17287(15) 0.2243(4) 0.0724(3) 0.0375(13) Uani 1 1 d . . . H56A H 0.1571 0.2476 0.1014 0.045 Uiso 1 1 calc R . . Cl10 Cl 0.24138(4) 0.90010(9) 0.27504(8) 0.0332(3) Uani 1 1 d . . . O11 O 0.21213(10) 0.9662(2) 0.2084(2) 0.0397(9) Uani 1 1 d . . . O12 O 0.26741(10) 0.9484(2) 0.3592(2) 0.0399(8) Uani 1 1 d . . . O13 O 0.26914(11) 0.8583(2) 0.2403(2) 0.0456(10) Uani 1 1 d . . . O14 O 0.21695(12) 0.8269(2) 0.2917(2) 0.0436(9) Uani 1 1 d . . . Cl20 Cl 0.09440(4) 0.28571(11) 0.18260(10) 0.0516(4) Uani 1 1 d . . . O21 O 0.07356(15) 0.2038(4) 0.1879(4) 0.1070(19) Uani 1 1 d . . . O22 O 0.14047(11) 0.2713(3) 0.2268(2) 0.0656(12) Uani 1 1 d . . . O23 O 0.08359(18) 0.3594(3) 0.2273(4) 0.1001(17) Uani 1 1 d . . . O24 O 0.08165(14) 0.3123(3) 0.0905(3) 0.0765(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03626(13) 0.03780(15) 0.02784(12) 0.00071(9) 0.01358(9) 0.00312(10) N11 0.039(3) 0.039(3) 0.030(2) 0.0055(19) 0.016(2) 0.010(2) C12 0.053(4) 0.027(3) 0.039(3) 0.002(2) 0.022(3) 0.014(3) C13 0.073(4) 0.032(4) 0.032(3) 0.006(2) 0.024(3) 0.022(3) C14 0.066(4) 0.042(4) 0.048(4) 0.009(3) 0.036(3) 0.013(3) C15 0.045(3) 0.041(4) 0.064(4) 0.006(3) 0.032(3) 0.010(3) C16 0.038(3) 0.053(4) 0.037(3) -0.003(3) 0.019(3) 0.003(3) N21 0.045(3) 0.030(3) 0.035(3) -0.0047(19) 0.011(2) -0.002(2) N22 0.041(3) 0.031(3) 0.039(3) -0.003(2) 0.005(2) 0.002(2) C23 0.050(4) 0.039(4) 0.033(3) -0.007(3) -0.001(3) 0.012(3) C24 0.054(4) 0.036(3) 0.031(3) 0.000(2) 0.012(3) 0.004(3) C25 0.045(3) 0.027(3) 0.028(3) -0.001(2) 0.010(2) 0.007(2) C31 0.037(3) 0.035(3) 0.054(4) -0.002(3) 0.006(3) 0.003(3) C32 0.033(3) 0.041(3) 0.064(4) -0.004(3) 0.005(3) -0.006(3) C33 0.049(4) 0.051(4) 0.109(6) 0.001(4) -0.001(4) -0.011(3) C34 0.037(4) 0.066(5) 0.182(9) 0.019(5) -0.010(5) -0.010(4) C35 0.029(3) 0.075(5) 0.174(8) 0.008(5) 0.020(4) 0.001(3) C36 0.024(3) 0.064(4) 0.121(6) -0.001(4) 0.014(3) 0.002(3) C37 0.030(3) 0.047(4) 0.060(4) 0.002(3) 0.007(3) 0.004(3) C38 0.028(3) 0.038(3) 0.046(3) 0.003(3) 0.007(2) -0.001(2) N41 0.018(2) 0.040(3) 0.040(3) -0.003(2) 0.0136(19) -0.0019(19) N42 0.025(2) 0.037(3) 0.047(3) 0.000(2) 0.011(2) 0.0026(19) C43 0.036(3) 0.048(4) 0.072(4) -0.007(3) 0.033(3) 0.005(3) C44 0.042(3) 0.035(3) 0.051(3) -0.003(3) 0.026(3) -0.002(3) C45 0.031(3) 0.028(3) 0.035(3) -0.005(2) 0.014(2) -0.009(2) N51 0.025(2) 0.036(3) 0.031(2) 0.0055(18) 0.0097(19) 0.0031(18) C52 0.029(3) 0.030(3) 0.036(3) 0.000(2) 0.016(2) -0.006(2) C53 0.041(3) 0.033(3) 0.037(3) -0.004(2) 0.022(3) -0.008(2) C54 0.035(3) 0.045(3) 0.036(3) 0.001(3) 0.013(3) -0.010(3) C55 0.034(3) 0.053(4) 0.039(3) 0.013(3) 0.009(3) 0.006(3) C56 0.030(3) 0.046(4) 0.036(3) 0.000(2) 0.014(2) 0.000(2) Cl10 0.0389(7) 0.0299(8) 0.0328(7) -0.0021(5) 0.0179(6) -0.0022(5) O11 0.042(2) 0.041(2) 0.0293(19) 0.0041(16) 0.0104(17) 0.0038(17) O12 0.038(2) 0.044(2) 0.0326(19) -0.0066(16) 0.0108(16) -0.0043(16) O13 0.055(3) 0.044(3) 0.046(2) 0.0019(17) 0.030(2) 0.0078(18) O14 0.052(2) 0.041(2) 0.040(2) -0.0036(16) 0.0224(19) -0.0124(17) Cl20 0.0367(8) 0.0626(11) 0.0532(9) -0.0003(7) 0.0183(7) -0.0045(7) O21 0.067(3) 0.089(4) 0.153(5) 0.034(4) 0.039(3) -0.031(3) O22 0.034(2) 0.108(4) 0.047(2) 0.001(2) 0.0110(19) -0.003(2) O23 0.099(4) 0.108(4) 0.115(4) -0.019(3) 0.067(4) 0.019(3) O24 0.057(3) 0.111(4) 0.047(3) 0.014(2) 0.011(2) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N51 2.157(4) . ? Hg1 N11 2.196(4) . ? Hg1 N21 2.342(4) . ? Hg1 N41 2.458(4) . ? N11 C16 1.347(6) . ? N11 C12 1.356(6) . ? C12 C13 1.397(7) . ? C12 C25 1.462(7) . ? C13 C14 1.358(7) . ? C14 C15 1.371(7) . ? C15 C16 1.378(7) . ? N21 C25 1.330(6) . ? N21 N22 1.350(6) . ? N22 C23 1.342(6) . ? N22 C31 1.471(6) . ? C23 C24 1.355(8) . ? C24 C25 1.392(7) . ? C31 C32 1.497(7) . ? C32 C37 1.385(8) . ? C32 C33 1.402(8) . ? C33 C34 1.386(9) . ? C34 C35 1.382(10) . ? C35 C36 1.377(8) . ? C36 C37 1.403(7) . ? C37 C38 1.525(7) . ? C38 N42 1.469(6) . ? N41 C45 1.339(6) . ? N41 N42 1.361(5) . ? N42 C43 1.341(6) . ? C43 C44 1.365(7) . ? C44 C45 1.405(6) . ? C45 C52 1.465(7) . ? N51 C56 1.330(6) . ? N51 C52 1.346(6) . ? C52 C53 1.389(7) . ? C53 C54 1.368(7) . ? C54 C55 1.370(7) . ? C55 C56 1.368(6) . ? Cl10 O12 1.439(3) . ? Cl10 O14 1.440(3) . ? Cl10 O13 1.445(3) . ? Cl10 O11 1.450(3) . ? Cl20 O21 1.390(4) . ? Cl20 O23 1.419(5) . ? Cl20 O24 1.423(4) . ? Cl20 O22 1.436(4) . ? 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 N51 Hg1 N11 139.96(15) . . ? N51 Hg1 N21 145.48(15) . . ? N11 Hg1 N21 72.75(16) . . ? N51 Hg1 N41 72.95(14) . . ? N11 Hg1 N41 136.97(14) . . ? N21 Hg1 N41 87.40(14) . . ? C16 N11 C12 119.8(5) . . ? C16 N11 Hg1 121.6(3) . . ? C12 N11 Hg1 118.6(4) . . ? N11 C12 C13 120.0(5) . . ? N11 C12 C25 116.8(5) . . ? C13 C12 C25 123.2(5) . . ? C14 C13 C12 120.3(5) . . ? C13 C14 C15 118.6(5) . . ? C14 C15 C16 120.8(5) . . ? N11 C16 C15 120.5(5) . . ? C25 N21 N22 105.3(4) . . ? C25 N21 Hg1 113.9(3) . . ? N22 N21 Hg1 140.1(3) . . ? C23 N22 N21 110.5(5) . . ? C23 N22 C31 129.3(5) . . ? N21 N22 C31 120.2(4) . . ? N22 C23 C24 108.6(5) . . ? C23 C24 C25 104.4(5) . . ? N21 C25 C24 111.2(5) . . ? N21 C25 C12 117.8(4) . . ? C24 C25 C12 131.0(5) . . ? N22 C31 C32 112.5(4) . . ? C37 C32 C33 119.6(5) . . ? C37 C32 C31 123.4(5) . . ? C33 C32 C31 116.9(6) . . ? C34 C33 C32 119.3(7) . . ? C35 C34 C33 121.2(6) . . ? C36 C35 C34 119.8(6) . . ? C35 C36 C37 119.9(7) . . ? C32 C37 C36 120.3(5) . . ? C32 C37 C38 122.6(5) . . ? C36 C37 C38 117.0(5) . . ? N42 C38 C37 112.8(4) . . ? C45 N41 N42 104.9(4) . . ? C45 N41 Hg1 109.5(3) . . ? N42 N41 Hg1 145.1(3) . . ? C43 N42 N41 110.9(4) . . ? C43 N42 C38 128.5(4) . . ? N41 N42 C38 120.6(4) . . ? N42 C43 C44 108.7(5) . . ? C43 C44 C45 104.2(5) . . ? N41 C45 C44 111.3(4) . . ? N41 C45 C52 118.8(4) . . ? C44 C45 C52 129.9(5) . . ? C56 N51 C52 119.8(4) . . ? C56 N51 Hg1 120.7(3) . . ? C52 N51 Hg1 119.4(3) . . ? N51 C52 C53 119.9(4) . . ? N51 C52 C45 118.5(4) . . ? C53 C52 C45 121.6(4) . . ? C54 C53 C52 120.3(5) . . ? C53 C54 C55 118.5(5) . . ? C56 C55 C54 119.7(5) . . ? N51 C56 C55 121.9(5) . . ? O12 Cl10 O14 109.1(2) . . ? O12 Cl10 O13 109.6(2) . . ? O14 Cl10 O13 109.2(2) . . ? O12 Cl10 O11 109.8(2) . . ? O14 Cl10 O11 110.0(2) . . ? O13 Cl10 O11 109.1(2) . . ? O21 Cl20 O23 108.6(3) . . ? O21 Cl20 O24 111.5(3) . . ? O23 Cl20 O24 109.0(3) . . ? O21 Cl20 O22 109.7(3) . . ? O23 Cl20 O22 109.4(3) . . ? O24 Cl20 O22 108.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N51 Hg1 N11 C16 12.0(5) . . . . ? N21 Hg1 N11 C16 178.3(4) . . . . ? N41 Hg1 N11 C16 -115.4(4) . . . . ? N51 Hg1 N11 C12 -168.6(3) . . . . ? N21 Hg1 N11 C12 -2.3(3) . . . . ? N41 Hg1 N11 C12 64.0(4) . . . . ? C16 N11 C12 C13 1.3(7) . . . . ? Hg1 N11 C12 C13 -178.1(3) . . . . ? C16 N11 C12 C25 179.9(4) . . . . ? Hg1 N11 C12 C25 0.5(6) . . . . ? N11 C12 C13 C14 -1.2(7) . . . . ? C25 C12 C13 C14 -179.7(5) . . . . ? C12 C13 C14 C15 1.4(8) . . . . ? C13 C14 C15 C16 -1.6(8) . . . . ? C12 N11 C16 C15 -1.6(7) . . . . ? Hg1 N11 C16 C15 177.8(4) . . . . ? C14 C15 C16 N11 1.8(8) . . . . ? N51 Hg1 N21 C25 168.4(3) . . . . ? N11 Hg1 N21 C25 3.9(3) . . . . ? N41 Hg1 N21 C25 -137.4(3) . . . . ? N51 Hg1 N21 N22 -23.2(6) . . . . ? N11 Hg1 N21 N22 172.4(5) . . . . ? N41 Hg1 N21 N22 31.1(5) . . . . ? C25 N21 N22 C23 -0.8(5) . . . . ? Hg1 N21 N22 C23 -169.9(4) . . . . ? C25 N21 N22 C31 -179.3(4) . . . . ? Hg1 N21 N22 C31 11.6(7) . . . . ? N21 N22 C23 C24 0.4(6) . . . . ? C31 N22 C23 C24 178.7(5) . . . . ? N22 C23 C24 C25 0.2(6) . . . . ? N22 N21 C25 C24 0.9(5) . . . . ? Hg1 N21 C25 C24 173.2(3) . . . . ? N22 N21 C25 C12 -177.4(4) . . . . ? Hg1 N21 C25 C12 -5.1(5) . . . . ? C23 C24 C25 N21 -0.7(6) . . . . ? C23 C24 C25 C12 177.4(5) . . . . ? N11 C12 C25 N21 3.3(7) . . . . ? C13 C12 C25 N21 -178.2(4) . . . . ? N11 C12 C25 C24 -174.7(5) . . . . ? C13 C12 C25 C24 3.9(8) . . . . ? C23 N22 C31 C32 53.4(7) . . . . ? N21 N22 C31 C32 -128.4(5) . . . . ? N22 C31 C32 C37 71.1(6) . . . . ? N22 C31 C32 C33 -113.4(4) . . . . ? C37 C32 C33 C34 0.4(2) . . . . ? C31 C32 C33 C34 -175.3(5) . . . . ? C32 C33 C34 C35 0.4(3) . . . . ? C33 C34 C35 C36 -0.9(6) . . . . ? C34 C35 C36 C37 0.5(7) . . . . ? C33 C32 C37 C36 -0.8(5) . . . . ? C31 C32 C37 C36 174.7(5) . . . . ? C33 C32 C37 C38 177.5(5) . . . . ? C31 C32 C37 C38 -7.1(7) . . . . ? C35 C36 C37 C32 0.3(7) . . . . ? C35 C36 C37 C38 -178.0(5) . . . . ? C32 C37 C38 N42 79.9(6) . . . . ? C36 C37 C38 N42 -101.8(5) . . . . ? N51 Hg1 N41 C45 -7.2(3) . . . . ? N11 Hg1 N41 C45 140.5(3) . . . . ? N21 Hg1 N41 C45 -158.4(3) . . . . ? N51 Hg1 N41 N42 -176.4(6) . . . . ? N11 Hg1 N41 N42 -28.7(6) . . . . ? N21 Hg1 N41 N42 32.4(5) . . . . ? C45 N41 N42 C43 1.4(5) . . . . ? Hg1 N41 N42 C43 170.8(4) . . . . ? C45 N41 N42 C38 -179.3(4) . . . . ? Hg1 N41 N42 C38 -9.9(8) . . . . ? C37 C38 N42 C43 70.0(7) . . . . ? C37 C38 N42 N41 -109.1(5) . . . . ? N41 N42 C43 C44 -1.1(6) . . . . ? C38 N42 C43 C44 179.7(4) . . . . ? N42 C43 C44 C45 0.3(6) . . . . ? N42 N41 C45 C44 -1.2(5) . . . . ? Hg1 N41 C45 C44 -174.8(3) . . . . ? N42 N41 C45 C52 -179.9(4) . . . . ? Hg1 N41 C45 C52 6.5(5) . . . . ? C43 C44 C45 N41 0.6(6) . . . . ? C43 C44 C45 C52 179.1(5) . . . . ? N11 Hg1 N51 C56 38.6(5) . . . . ? N21 Hg1 N51 C56 -117.9(4) . . . . ? N41 Hg1 N51 C56 -175.9(4) . . . . ? N11 Hg1 N51 C52 -138.0(3) . . . . ? N21 Hg1 N51 C52 65.5(4) . . . . ? N41 Hg1 N51 C52 7.4(3) . . . . ? C56 N51 C52 C53 -1.9(7) . . . . ? Hg1 N51 C52 C53 174.8(3) . . . . ? C56 N51 C52 C45 176.4(4) . . . . ? Hg1 N51 C52 C45 -6.9(5) . . . . ? N41 C45 C52 N51 -0.7(7) . . . . ? C44 C45 C52 N51 -179.1(5) . . . . ? N41 C45 C52 C53 177.6(4) . . . . ? C44 C45 C52 C53 -0.9(8) . . . . ? N51 C52 C53 C54 0.3(7) . . . . ? C45 C52 C53 C54 -177.9(4) . . . . ? C52 C53 C54 C55 1.3(7) . . . . ? C53 C54 C55 C56 -1.4(8) . . . . ? C52 N51 C56 C55 1.8(7) . . . . ? Hg1 N51 C56 C55 -174.8(4) . . . . ? C54 C55 C56 N51 -0.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.908 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.132 #===END data_imw397m _database_code_depnum_ccdc_archive 'CCDC 609498' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl2 Hg2 N8 O12' _chemical_formula_weight 1114.63 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.543(6) _cell_length_b 14.122(11) _cell_length_c 16.669(13) _cell_angle_alpha 103.677(13) _cell_angle_beta 93.039(13) _cell_angle_gamma 101.174(13) _cell_volume 1684(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 9.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2567 _exptl_absorpt_correction_T_max 0.6524 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14973 _diffrn_reflns_av_R_equivalents 0.1767 _diffrn_reflns_av_sigmaI/netI 0.1563 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5889 _reflns_number_gt 4028 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0360P)^2^+194.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5889 _refine_ls_number_parameters 431 _refine_ls_number_restraints 447 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.1110 _refine_ls_wR_factor_ref 0.2611 _refine_ls_wR_factor_gt 0.2466 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _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 0.56879(13) 0.82511(8) 0.84945(6) 0.0233(3) Uani 1 1 d U . . Hg2 Hg 0.41772(13) 0.71239(8) 0.71264(6) 0.0258(3) Uani 1 1 d U . . N11 N 0.683(3) 0.9745(16) 0.9431(13) 0.023(4) Uani 1 1 d U . . C12 C 0.771(3) 0.9788(18) 1.0207(16) 0.019(5) Uiso 1 1 d U . . C13 C 0.832(3) 1.061(2) 1.0770(17) 0.026(5) Uani 1 1 d U . . H13 H 0.8868 1.0608 1.1296 0.031 Uiso 1 1 calc R . . C14 C 0.812(4) 1.155(2) 1.0567(17) 0.029(5) Uani 1 1 d U . . H14 H 0.8626 1.2175 1.0943 0.035 Uiso 1 1 calc R . . C15 C 0.722(4) 1.149(2) 0.9836(17) 0.027(5) Uani 1 1 d U . . H15 H 0.6991 1.2073 0.9694 0.033 Uiso 1 1 calc R . . C16 C 0.663(3) 1.057(2) 0.9301(16) 0.023(4) Uani 1 1 d U . . H16 H 0.6022 1.0542 0.8781 0.028 Uiso 1 1 calc R . . N21 N 0.719(3) 0.7965(17) 0.9707(13) 0.024(4) Uani 1 1 d U . . N22 N 0.758(3) 0.7203(17) 0.9964(14) 0.025(4) Uani 1 1 d U . . C23 C 0.843(4) 0.750(2) 1.0748(16) 0.027(5) Uani 1 1 d U . . H23 H 0.8786 0.7093 1.1074 0.032 Uiso 1 1 calc R . . C24 C 0.867(4) 0.853(2) 1.0974(17) 0.027(5) Uani 1 1 d U . . H24 H 0.9280 0.8961 1.1478 0.032 Uiso 1 1 calc R . . C25 C 0.781(3) 0.881(2) 1.0308(15) 0.019(4) Uani 1 1 d U . . C31 C 0.719(4) 0.620(2) 0.9416(18) 0.031(5) Uani 1 1 d U . . H31A H 0.7678 0.5749 0.9697 0.038 Uiso 1 1 calc R . . H31B H 0.7806 0.6212 0.8907 0.038 Uiso 1 1 calc R . . C32 C 0.508(3) 0.580(2) 0.9173(16) 0.025(4) Uani 1 1 d U . . C33 C 0.394(3) 0.610(2) 0.9792(17) 0.025(5) Uani 1 1 d U . . H33 H 0.4450 0.6503 1.0325 0.030 Uiso 1 1 calc R . . C34 C 0.201(4) 0.577(2) 0.9602(18) 0.028(5) Uani 1 1 d U . . H34 H 0.1217 0.5961 1.0005 0.034 Uiso 1 1 calc R . . C35 C 0.135(4) 0.519(2) 0.8850(18) 0.029(5) Uani 1 1 d U . . H35 H 0.0072 0.4980 0.8729 0.034 Uiso 1 1 calc R . . C36 C 0.243(4) 0.489(2) 0.8234(19) 0.029(5) Uani 1 1 d U . . H36 H 0.1912 0.4479 0.7703 0.035 Uiso 1 1 calc R . . C37 C 0.435(4) 0.520(2) 0.8427(17) 0.026(4) Uani 1 1 d U . . C38 C 0.555(4) 0.486(2) 0.7737(17) 0.029(5) Uani 1 1 d U . . H38A H 0.6642 0.5399 0.7784 0.034 Uiso 1 1 calc R . . H38B H 0.5968 0.4268 0.7826 0.034 Uiso 1 1 calc R . . N41 N 0.418(3) 0.5391(17) 0.6617(14) 0.024(4) Uani 1 1 d U . . N42 N 0.461(3) 0.4615(18) 0.6888(15) 0.030(4) Uani 1 1 d U . . C43 C 0.408(4) 0.375(2) 0.6349(18) 0.032(5) Uani 1 1 d U . . H43 H 0.4219 0.3112 0.6411 0.038 Uiso 1 1 calc R . . C44 C 0.324(4) 0.397(2) 0.565(2) 0.037(6) Uani 1 1 d U . . H44 H 0.2688 0.3509 0.5145 0.045 Uiso 1 1 calc R . . C45 C 0.339(3) 0.496(2) 0.5838(17) 0.027(4) Uani 1 1 d U . . N51 N 0.310(3) 0.6633(17) 0.5776(13) 0.026(4) Uani 1 1 d U . . C52 C 0.281(4) 0.566(2) 0.5351(19) 0.036(6) Uiso 1 1 d U . . C53 C 0.196(4) 0.529(2) 0.4565(18) 0.035(5) Uani 1 1 d U . . H53 H 0.1705 0.4596 0.4311 0.043 Uiso 1 1 calc R . . C54 C 0.149(4) 0.595(2) 0.4162(19) 0.038(6) Uani 1 1 d U . . H54 H 0.1015 0.5722 0.3595 0.046 Uiso 1 1 calc R . . C55 C 0.171(4) 0.694(2) 0.4563(18) 0.038(6) Uani 1 1 d U . . H55 H 0.1339 0.7395 0.4282 0.046 Uiso 1 1 calc R . . C56 C 0.249(4) 0.728(2) 0.5411(18) 0.033(5) Uani 1 1 d U . . H56 H 0.2573 0.7953 0.5711 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.0533(8) 0.2766(5) 0.2814(4) 0.0274(14) Uani 1 1 d U . . O11 O -0.089(3) 0.1930(15) 0.2832(12) 0.038(4) Uani 1 1 d U . . O12 O 0.197(3) 0.2887(17) 0.3468(12) 0.041(5) Uani 1 1 d U . . O13 O -0.023(2) 0.3643(15) 0.2937(12) 0.035(4) Uani 1 1 d U . . O14 O 0.132(2) 0.2675(17) 0.1997(11) 0.036(5) Uani 1 1 d U . . Cl2 Cl 0.724(2) 0.2371(11) 0.7671(9) 0.028(4) Uiso 0.50 1 d PDU A 1 O21 O 0.817(4) 0.161(2) 0.7682(18) 0.026(8) Uiso 0.50 1 d PDU A 1 O22 O 0.630(4) 0.221(2) 0.6884(17) 0.029(8) Uiso 0.50 1 d PDU A 1 O23 O 0.599(5) 0.239(3) 0.827(2) 0.080(17) Uiso 0.50 1 d PDU A 1 O24 O 0.849(4) 0.329(2) 0.785(2) 0.050 Uiso 0.50 1 d PDU A 1 Cl2' Cl 0.774(2) 0.2479(12) 0.7634(10) 0.034(5) Uiso 0.50 1 d PDU B 2 O21' O 0.802(8) 0.312(3) 0.717(3) 0.14(3) Uiso 0.50 1 d PDU B 2 O22' O 0.917(6) 0.206(4) 0.764(3) 0.15(3) Uiso 0.50 1 d PDU B 2 O23' O 0.631(5) 0.178(3) 0.733(2) 0.050 Uiso 0.50 1 d PDU B 2 O24' O 0.758(6) 0.295(3) 0.840(2) 0.074(15) Uiso 0.50 1 d PDU B 2 C1A C 0.269(8) 0.056(4) 0.386(3) 0.106(17) Uani 1 1 d U . . H1A1 H 0.1898 0.1030 0.3994 0.159 Uiso 1 1 calc R . . H1A2 H 0.3805 0.0785 0.4245 0.159 Uiso 1 1 calc R . . H1A3 H 0.2065 -0.0102 0.3905 0.159 Uiso 1 1 calc R . . N2A N 0.319(3) 0.048(2) 0.2967(17) 0.045(6) Uani 1 1 d DU . . O3A O 0.196(3) 0.0482(16) 0.2454(13) 0.042(5) Uani 1 1 d DU . . O4A O 0.473(3) 0.044(2) 0.277(2) 0.085(9) Uani 1 1 d DU . . C1B C 0.215(4) 0.155(2) 0.5704(17) 0.034(7) Uiso 1 1 d DU . . H1B1 H 0.2973 0.1561 0.5271 0.051 Uiso 1 1 calc R . . H1B2 H 0.2568 0.2135 0.6169 0.051 Uiso 1 1 calc R . . H1B3 H 0.0921 0.1546 0.5476 0.051 Uiso 1 1 calc R . . N2B N 0.211(6) 0.067(3) 0.5988(17) 0.095(12) Uani 1 1 d DU . . O3B O 0.218(6) 0.068(2) 0.6811(18) 0.117(13) Uani 1 1 d DU . . O4B O 0.240(5) -0.020(2) 0.553(2) 0.093(10) Uani 1 1 d DU . . 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 0.0206(5) 0.0297(6) 0.0169(6) 0.0018(4) -0.0021(4) 0.0049(4) Hg2 0.0246(5) 0.0314(6) 0.0179(6) -0.0003(4) 0.0000(4) 0.0060(4) N11 0.020(10) 0.024(7) 0.023(9) -0.004(6) -0.004(8) 0.016(8) C13 0.022(11) 0.031(9) 0.020(10) 0.006(8) 0.008(9) -0.007(10) C14 0.026(12) 0.026(11) 0.025(11) -0.010(9) -0.002(9) 0.002(10) C15 0.027(12) 0.024(8) 0.029(11) 0.001(8) 0.004(9) 0.008(10) C16 0.027(8) 0.027(6) 0.015(8) 0.007(6) -0.003(7) 0.005(7) N21 0.026(10) 0.031(8) 0.021(8) 0.012(6) 0.000(7) 0.014(8) N22 0.026(10) 0.031(7) 0.020(9) 0.010(6) -0.006(7) 0.009(8) C23 0.030(12) 0.037(10) 0.017(10) 0.010(8) -0.007(9) 0.014(11) C24 0.026(12) 0.037(10) 0.017(10) 0.007(8) 0.001(8) 0.007(10) C25 0.011(10) 0.032(7) 0.015(8) 0.007(7) 0.005(7) 0.004(8) C31 0.025(8) 0.034(9) 0.034(13) 0.003(9) -0.015(9) 0.017(10) C32 0.025(8) 0.036(12) 0.018(9) 0.021(8) -0.001(7) 0.002(8) C33 0.027(9) 0.037(14) 0.016(10) 0.022(9) -0.001(7) 0.002(9) C34 0.026(9) 0.028(13) 0.030(11) 0.013(9) -0.003(9) -0.001(10) C35 0.027(10) 0.028(13) 0.033(12) 0.015(10) -0.003(7) 0.002(9) C36 0.028(8) 0.022(13) 0.038(12) 0.009(10) -0.003(8) 0.007(9) C37 0.027(8) 0.029(12) 0.027(8) 0.011(9) -0.007(7) 0.013(9) C38 0.024(10) 0.025(13) 0.034(9) 0.006(8) -0.003(7) 0.003(9) N41 0.015(9) 0.033(7) 0.023(9) 0.004(6) 0.004(7) 0.004(8) N42 0.024(10) 0.031(7) 0.035(8) 0.002(7) 0.003(7) 0.011(8) C43 0.028(12) 0.033(8) 0.031(11) -0.004(7) 0.016(9) 0.012(10) C44 0.030(13) 0.032(9) 0.042(12) -0.006(9) 0.001(10) 0.010(11) C45 0.014(10) 0.028(7) 0.030(9) -0.002(7) 0.001(8) -0.003(9) N51 0.019(10) 0.036(9) 0.022(7) 0.018(7) 0.001(7) -0.011(8) C53 0.036(14) 0.041(11) 0.029(11) 0.001(8) 0.006(10) 0.016(11) C54 0.040(9) 0.045(8) 0.027(9) 0.007(6) 0.001(7) 0.010(8) C55 0.051(15) 0.047(10) 0.017(10) 0.008(10) -0.008(11) 0.012(13) C56 0.028(13) 0.050(13) 0.022(9) 0.004(8) -0.007(10) 0.015(11) Cl1 0.019(3) 0.042(4) 0.018(3) 0.001(3) 0.003(2) 0.006(3) O11 0.030(9) 0.036(9) 0.032(11) -0.014(9) -0.007(8) -0.002(7) O12 0.030(9) 0.064(15) 0.022(9) 0.011(10) -0.005(7) 0.003(8) O13 0.025(9) 0.040(9) 0.032(11) -0.006(9) -0.002(8) 0.004(7) O14 0.008(8) 0.075(15) 0.019(7) -0.007(9) -0.004(6) 0.017(8) C1A 0.15(4) 0.11(4) 0.035(14) 0.03(2) -0.002(16) -0.05(3) N2A 0.045(11) 0.052(16) 0.037(13) 0.023(13) -0.006(9) -0.002(12) O3A 0.048(10) 0.034(12) 0.037(11) 0.006(10) -0.016(9) 0.000(10) O4A 0.038(10) 0.08(2) 0.11(2) -0.017(18) -0.013(12) 0.011(14) N2B 0.11(3) 0.10(2) 0.048(14) -0.025(18) 0.014(19) 0.02(2) O3B 0.20(4) 0.07(2) 0.061(14) 0.007(16) -0.06(2) 0.02(2) O4B 0.14(3) 0.054(17) 0.086(19) 0.020(14) -0.01(2) 0.024(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N11 2.28(2) . ? Hg1 N21 2.42(2) . ? Hg1 Hg2 2.518(2) . ? Hg2 N51 2.25(2) . ? Hg2 N41 2.39(2) . ? N11 C16 1.26(3) . ? N11 C12 1.41(3) . ? C12 C13 1.29(4) . ? C12 C25 1.44(4) . ? C13 C14 1.48(4) . ? C14 C15 1.34(4) . ? C15 C16 1.37(4) . ? N21 N22 1.32(3) . ? N21 C25 1.35(3) . ? N22 C23 1.36(3) . ? N22 C31 1.45(4) . ? C23 C24 1.38(4) . ? C24 C25 1.43(4) . ? C31 C32 1.58(4) . ? C32 C37 1.35(4) . ? C32 C33 1.41(4) . ? C33 C34 1.43(4) . ? C34 C35 1.33(4) . ? C35 C36 1.38(4) . ? C36 C37 1.42(4) . ? C37 C38 1.55(4) . ? C38 N42 1.48(4) . ? N41 C45 1.35(3) . ? N41 N42 1.37(3) . ? N42 C43 1.31(4) . ? C43 C44 1.43(4) . ? C44 C45 1.34(4) . ? C45 C52 1.53(4) . ? N51 C52 1.35(4) . ? N51 C56 1.35(4) . ? C52 C53 1.36(4) . ? C53 C54 1.36(4) . ? C54 C55 1.38(4) . ? C55 C56 1.43(4) . ? Cl1 O13 1.44(2) . ? Cl1 O11 1.44(2) . ? Cl1 O12 1.45(2) . ? Cl1 O14 1.500(19) . ? Cl2 O21 1.40(2) . ? Cl2 O23 1.40(3) . ? Cl2 O22 1.41(2) . ? Cl2 O24 1.41(3) . ? Cl2' O23' 1.30(3) . ? Cl2' O21' 1.31(4) . ? Cl2' O24' 1.32(3) . ? Cl2' O22' 1.33(4) . ? C1A N2A 1.53(5) . ? N2A O3A 1.23(2) . ? N2A O4A 1.24(2) . ? C1B N2B 1.43(6) . ? N2B O4B 1.35(4) . ? N2B O3B 1.37(4) . ? 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 N11 Hg1 N21 70.6(8) . . ? N11 Hg1 Hg2 155.7(5) . . ? N21 Hg1 Hg2 133.5(5) . . ? N51 Hg2 N41 71.1(8) . . ? N51 Hg2 Hg1 159.5(6) . . ? N41 Hg2 Hg1 126.7(5) . . ? C16 N11 C12 116(2) . . ? C16 N11 Hg1 122.6(18) . . ? C12 N11 Hg1 121.0(16) . . ? C13 C12 N11 123(2) . . ? C13 C12 C25 124(3) . . ? N11 C12 C25 112(2) . . ? C12 C13 C14 118(3) . . ? C15 C14 C13 118(3) . . ? C14 C15 C16 118(3) . . ? N11 C16 C15 127(3) . . ? N22 N21 C25 109(2) . . ? N22 N21 Hg1 138.2(18) . . ? C25 N21 Hg1 112.7(16) . . ? N21 N22 C23 111(2) . . ? N21 N22 C31 121(2) . . ? C23 N22 C31 128(2) . . ? N22 C23 C24 106(2) . . ? C23 C24 C25 107(2) . . ? N21 C25 C24 106(2) . . ? N21 C25 C12 123(2) . . ? C24 C25 C12 130(2) . . ? N22 C31 C32 111(2) . . ? C37 C32 C33 120(2) . . ? C37 C32 C31 123(2) . . ? C33 C32 C31 116(2) . . ? C32 C33 C34 119(3) . . ? C35 C34 C33 119(3) . . ? C34 C35 C36 124(3) . . ? C35 C36 C37 117(3) . . ? C32 C37 C36 121(3) . . ? C32 C37 C38 121(2) . . ? C36 C37 C38 117(2) . . ? N42 C38 C37 114(2) . . ? C45 N41 N42 104(2) . . ? C45 N41 Hg2 115.8(18) . . ? N42 N41 Hg2 140.1(18) . . ? C43 N42 N41 114(3) . . ? C43 N42 C38 130(3) . . ? N41 N42 C38 117(2) . . ? N42 C43 C44 104(3) . . ? C45 C44 C43 107(3) . . ? C44 C45 N41 111(3) . . ? C44 C45 C52 132(3) . . ? N41 C45 C52 116(2) . . ? C52 N51 C56 119(2) . . ? C52 N51 Hg2 121.2(19) . . ? C56 N51 Hg2 120(2) . . ? N51 C52 C53 125(3) . . ? N51 C52 C45 115(3) . . ? C53 C52 C45 120(3) . . ? C54 C53 C52 118(3) . . ? C53 C54 C55 121(3) . . ? C54 C55 C56 119(3) . . ? N51 C56 C55 119(3) . . ? O13 Cl1 O11 108.4(12) . . ? O13 Cl1 O12 110.5(13) . . ? O11 Cl1 O12 109.1(13) . . ? O13 Cl1 O14 105.5(13) . . ? O11 Cl1 O14 113.8(12) . . ? O12 Cl1 O14 109.5(11) . . ? O21 Cl2 O23 109.6(11) . . ? O21 Cl2 O22 110.2(11) . . ? O23 Cl2 O22 108.9(11) . . ? O21 Cl2 O24 109.7(11) . . ? O23 Cl2 O24 109.7(11) . . ? O22 Cl2 O24 108.7(11) . . ? O23' Cl2' O21' 110.8(13) . . ? O23' Cl2' O24' 111.2(13) . . ? O21' Cl2' O24' 109.6(13) . . ? O23' Cl2' O22' 108.4(13) . . ? O21' Cl2' O22' 108.4(13) . . ? O24' Cl2' O22' 108.3(12) . . ? O3A N2A O4A 121(3) . . ? O3A N2A C1A 116(3) . . ? O4A N2A C1A 123(3) . . ? O4B N2B O3B 111(4) . . ? O4B N2B C1B 125(3) . . ? O3B N2B C1B 122(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Hg1 Hg2 N51 17(2) . . . . ? N21 Hg1 Hg2 N51 -155.1(17) . . . . ? N11 Hg1 Hg2 N41 164.0(14) . . . . ? N21 Hg1 Hg2 N41 -8.0(9) . . . . ? N21 Hg1 N11 C16 -179(2) . . . . ? Hg2 Hg1 N11 C16 7(3) . . . . ? N21 Hg1 N11 C12 -2.3(17) . . . . ? Hg2 Hg1 N11 C12 -176.2(12) . . . . ? C16 N11 C12 C13 0(4) . . . . ? Hg1 N11 C12 C13 -177(2) . . . . ? C16 N11 C12 C25 178(2) . . . . ? Hg1 N11 C12 C25 1(3) . . . . ? N11 C12 C13 C14 -2(4) . . . . ? C25 C12 C13 C14 179(2) . . . . ? C12 C13 C14 C15 5(4) . . . . ? C13 C14 C15 C16 -4(4) . . . . ? C12 N11 C16 C15 1(4) . . . . ? Hg1 N11 C16 C15 178(2) . . . . ? C14 C15 C16 N11 2(4) . . . . ? N11 Hg1 N21 N22 -177(3) . . . . ? Hg2 Hg1 N21 N22 -1(3) . . . . ? N11 Hg1 N21 C25 3.3(16) . . . . ? Hg2 Hg1 N21 C25 179.8(13) . . . . ? C25 N21 N22 C23 2(3) . . . . ? Hg1 N21 N22 C23 -177.8(19) . . . . ? C25 N21 N22 C31 -175(2) . . . . ? Hg1 N21 N22 C31 5(4) . . . . ? N21 N22 C23 C24 -3(3) . . . . ? C31 N22 C23 C24 173(3) . . . . ? N22 C23 C24 C25 4(3) . . . . ? N22 N21 C25 C24 1(3) . . . . ? Hg1 N21 C25 C24 -179.7(15) . . . . ? N22 N21 C25 C12 176(2) . . . . ? Hg1 N21 C25 C12 -4(3) . . . . ? C23 C24 C25 N21 -3(3) . . . . ? C23 C24 C25 C12 -178(2) . . . . ? C13 C12 C25 N21 -179(2) . . . . ? N11 C12 C25 N21 3(3) . . . . ? C13 C12 C25 C24 -5(4) . . . . ? N11 C12 C25 C24 177(2) . . . . ? N21 N22 C31 C32 -64(3) . . . . ? C23 N22 C31 C32 119(3) . . . . ? N22 C31 C32 C37 146(3) . . . . ? N22 C31 C32 C33 -35(3) . . . . ? C37 C32 C33 C34 -2(4) . . . . ? C31 C32 C33 C34 179(2) . . . . ? C32 C33 C34 C35 1(4) . . . . ? C33 C34 C35 C36 0(4) . . . . ? C34 C35 C36 C37 1(4) . . . . ? C33 C32 C37 C36 3(4) . . . . ? C31 C32 C37 C36 -178(2) . . . . ? C33 C32 C37 C38 -180(2) . . . . ? C31 C32 C37 C38 -1(4) . . . . ? C35 C36 C37 C32 -2(4) . . . . ? C35 C36 C37 C38 -180(2) . . . . ? C32 C37 C38 N42 -154(2) . . . . ? C36 C37 C38 N42 24(3) . . . . ? N51 Hg2 N41 C45 -6.8(17) . . . . ? Hg1 Hg2 N41 C45 -175.2(14) . . . . ? N51 Hg2 N41 N42 -179(3) . . . . ? Hg1 Hg2 N41 N42 12(3) . . . . ? C45 N41 N42 C43 -3(3) . . . . ? Hg2 N41 N42 C43 170.5(19) . . . . ? C45 N41 N42 C38 179(2) . . . . ? Hg2 N41 N42 C38 -8(4) . . . . ? C37 C38 N42 C43 -111(3) . . . . ? C37 C38 N42 N41 68(3) . . . . ? N41 N42 C43 C44 1(3) . . . . ? C38 N42 C43 C44 179(2) . . . . ? N42 C43 C44 C45 1(3) . . . . ? C43 C44 C45 N41 -3(3) . . . . ? C43 C44 C45 C52 178(3) . . . . ? N42 N41 C45 C44 3(3) . . . . ? Hg2 N41 C45 C44 -171.8(18) . . . . ? N42 N41 C45 C52 -178(2) . . . . ? Hg2 N41 C45 C52 7(3) . . . . ? N41 Hg2 N51 C52 5.6(19) . . . . ? Hg1 Hg2 N51 C52 158.2(16) . . . . ? N41 Hg2 N51 C56 176(2) . . . . ? Hg1 Hg2 N51 C56 -31(3) . . . . ? C56 N51 C52 C53 1(4) . . . . ? Hg2 N51 C52 C53 172(2) . . . . ? C56 N51 C52 C45 -174(2) . . . . ? Hg2 N51 C52 C45 -4(3) . . . . ? C44 C45 C52 N51 176(3) . . . . ? N41 C45 C52 N51 -3(3) . . . . ? C44 C45 C52 C53 1(5) . . . . ? N41 C45 C52 C53 -178(3) . . . . ? N51 C52 C53 C54 5(5) . . . . ? C45 C52 C53 C54 -180(3) . . . . ? C52 C53 C54 C55 -7(5) . . . . ? C53 C54 C55 C56 2(5) . . . . ? C52 N51 C56 C55 -6(4) . . . . ? Hg2 N51 C56 C55 -176(2) . . . . ? C54 C55 C56 N51 4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.040 _refine_diff_density_min -3.436 _refine_diff_density_rms 0.417 #===END data_imw278b _database_code_depnum_ccdc_archive 'CCDC 609499' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Hg2 N7 O, C3 H7 N O, 2(Cl O4)' _chemical_formula_sum 'C30 H34 Cl2 Hg2 N8 O10' _chemical_formula_weight 1138.73 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.319(6) _cell_length_b 11.656(3) _cell_length_c 15.942(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.757(5) _cell_angle_gamma 90.00 _cell_volume 3582.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4763 _cell_measurement_theta_min 4.747 _cell_measurement_theta_max 55.077 _exptl_crystal_description PLATE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 8.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1101 _exptl_absorpt_correction_T_max 0.5786 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24519 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6273 _reflns_number_gt 4953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^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 6273 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.132129(17) 0.14569(2) 0.223452(17) 0.03103(11) Uani 1 1 d . . . Hg2 Hg 0.195767(17) 0.24995(2) 0.343945(17) 0.02806(11) Uani 1 1 d . . . N11 N 0.0819(3) 0.1873(5) 0.0883(4) 0.0263(15) Uani 1 1 d . . . C12 C 0.0814(4) 0.1009(5) 0.0305(4) 0.0215(16) Uani 1 1 d . . . C13 C 0.0598(4) 0.1201(6) -0.0517(4) 0.0243(17) Uani 1 1 d . . . H13 H 0.0604 0.0593 -0.0913 0.029 Uiso 1 1 calc R . . C14 C 0.0373(4) 0.2274(6) -0.0772(5) 0.0291(18) Uani 1 1 d . . . H14 H 0.0216 0.2410 -0.1341 0.035 Uiso 1 1 calc R . . C15 C 0.0378(4) 0.3162(6) -0.0181(5) 0.0308(19) Uani 1 1 d . . . H15 H 0.0232 0.3914 -0.0341 0.037 Uiso 1 1 calc R . . C16 C 0.0596(4) 0.2923(6) 0.0630(5) 0.0318(19) Uani 1 1 d . . . H16 H 0.0591 0.3521 0.1035 0.038 Uiso 1 1 calc R . . N21 N 0.1157(3) -0.0240(4) 0.1463(3) 0.0237(14) Uani 1 1 d . . . N22 N 0.1341(3) -0.1361(5) 0.1579(4) 0.0268(14) Uani 1 1 d . . . C24 C 0.1328(4) -0.1917(6) 0.0837(5) 0.0311(18) Uani 1 1 d . . . H24 H 0.1435 -0.2705 0.0762 0.037 Uiso 1 1 calc R . . C25 C 0.1134(4) -0.1154(6) 0.0205(5) 0.0267(17) Uani 1 1 d . . . H25 H 0.1078 -0.1296 -0.0382 0.032 Uiso 1 1 calc R . . C26 C 0.1039(4) -0.0113(6) 0.0633(4) 0.0247(16) Uani 1 1 d . . . C31 C 0.1412(5) -0.1836(6) 0.2429(5) 0.0331(19) Uani 1 1 d . . . H31A H 0.1562 -0.2647 0.2401 0.040 Uiso 1 1 calc R . . H31B H 0.0955 -0.1820 0.2676 0.040 Uiso 1 1 calc R . . C32 C 0.1933(4) -0.1176(5) 0.2995(5) 0.0263(18) Uani 1 1 d . . . C33 C 0.2592(5) -0.0957(6) 0.2749(5) 0.035(2) Uani 1 1 d . . . H33 H 0.2718 -0.1194 0.2210 0.042 Uiso 1 1 calc R . . C34 C 0.3069(5) -0.0394(6) 0.3286(5) 0.037(2) Uani 1 1 d . . . H34 H 0.3523 -0.0249 0.3115 0.045 Uiso 1 1 calc R . . C35 C 0.2890(5) -0.0040(6) 0.4071(5) 0.0337(19) Uani 1 1 d . . . H35 H 0.3223 0.0346 0.4433 0.040 Uiso 1 1 calc R . . C36 C 0.2236(4) -0.0239(6) 0.4336(4) 0.0284(18) Uani 1 1 d . . . C37 C 0.1743(4) -0.0809(5) 0.3785(4) 0.0245(17) Uani 1 1 d . . . H37 H 0.1287 -0.0941 0.3951 0.029 Uiso 1 1 calc R . . C38 C 0.2019(4) 0.0129(6) 0.5172(4) 0.0279(18) Uani 1 1 d . . . H38A H 0.1506 0.0158 0.5155 0.033 Uiso 1 1 calc R . . H38B H 0.2177 -0.0449 0.5598 0.033 Uiso 1 1 calc R . . N41 N 0.2250(3) 0.2166(5) 0.4888(4) 0.0247(14) Uani 1 1 d . . . N42 N 0.2300(4) 0.1266(5) 0.5434(4) 0.0273(15) Uani 1 1 d . . . C43 C 0.2587(4) 0.1586(6) 0.6175(5) 0.0318(19) Uani 1 1 d . . . H43 H 0.2668 0.1104 0.6652 0.038 Uiso 1 1 calc R . . C44 C 0.2748(4) 0.2742(6) 0.6137(5) 0.0299(18) Uani 1 1 d . . . H44 H 0.2960 0.3211 0.6569 0.036 Uiso 1 1 calc R . . C45 C 0.2530(4) 0.3060(6) 0.5320(5) 0.0264(17) Uani 1 1 d . . . N51 N 0.2299(3) 0.4202(5) 0.4082(4) 0.0252(14) Uani 1 1 d . . . C52 C 0.2564(4) 0.4172(6) 0.4879(4) 0.0247(17) Uani 1 1 d . . . C53 C 0.2863(4) 0.5132(6) 0.5268(5) 0.0298(18) Uani 1 1 d . . . H53 H 0.3053 0.5091 0.5832 0.036 Uiso 1 1 calc R . . C54 C 0.2882(5) 0.6140(6) 0.4828(5) 0.036(2) Uani 1 1 d . . . H54 H 0.3077 0.6807 0.5092 0.043 Uiso 1 1 calc R . . C55 C 0.2619(4) 0.6189(6) 0.4005(5) 0.0318(19) Uani 1 1 d . . . H55 H 0.2636 0.6878 0.3688 0.038 Uiso 1 1 calc R . . C56 C 0.2325(4) 0.5188(6) 0.3651(5) 0.0274(18) Uani 1 1 d . . . H56 H 0.2137 0.5208 0.3085 0.033 Uiso 1 1 calc R . . O61 O 0.3253(3) 0.2529(5) 0.3138(4) 0.0417(15) Uani 1 1 d . . . C62 C 0.3705(5) 0.3282(7) 0.3203(5) 0.037(2) Uani 1 1 d . . . H62 H 0.3590 0.3993 0.3451 0.044 Uiso 1 1 calc R . . N63 N 0.4335(4) 0.3154(6) 0.2948(5) 0.0462(19) Uani 1 1 d . . . C64 C 0.4545(6) 0.2062(9) 0.2606(9) 0.080(4) Uani 1 1 d . . . H64A H 0.4216 0.1464 0.2749 0.121 Uiso 1 1 calc R . . H64B H 0.5010 0.1862 0.2845 0.121 Uiso 1 1 calc R . . H64C H 0.4552 0.2122 0.1993 0.121 Uiso 1 1 calc R . . C65 C 0.4844(6) 0.4074(9) 0.3014(8) 0.070(3) Uani 1 1 d . . . H65A H 0.4626 0.4772 0.3216 0.105 Uiso 1 1 calc R . . H65B H 0.5019 0.4219 0.2461 0.105 Uiso 1 1 calc R . . H65C H 0.5230 0.3851 0.3410 0.105 Uiso 1 1 calc R . . O71 O 0.4293(4) 0.4025(6) 0.5024(6) 0.085(3) Uani 1 1 d . . . C72 C 0.4833(6) 0.3536(8) 0.5262(7) 0.061(3) Uani 1 1 d . . . H72 H 0.5215 0.4013 0.5431 0.074 Uiso 1 1 calc R . . N73 N 0.4941(4) 0.2404(6) 0.5311(5) 0.045(2) Uani 1 1 d . . . C74 C 0.4380(6) 0.1633(8) 0.5059(8) 0.071(3) Uani 1 1 d . . . H74A H 0.3958 0.2078 0.4914 0.106 Uiso 1 1 calc R . . H74B H 0.4297 0.1111 0.5524 0.106 Uiso 1 1 calc R . . H74C H 0.4503 0.1188 0.4569 0.106 Uiso 1 1 calc R . . C75 C 0.5605(5) 0.1919(9) 0.5587(7) 0.059(3) Uani 1 1 d . . . H75A H 0.5923 0.2536 0.5776 0.088 Uiso 1 1 calc R . . H75B H 0.5797 0.1504 0.5121 0.088 Uiso 1 1 calc R . . H75C H 0.5546 0.1388 0.6054 0.088 Uiso 1 1 calc R . . Cl1 Cl 0.04337(10) 0.52630(13) 0.22827(11) 0.0276(4) Uani 1 1 d . . . O11 O 0.0559(5) 0.4123(5) 0.2535(3) 0.069(2) Uani 1 1 d . . . O12 O 0.0470(4) 0.5996(5) 0.3000(4) 0.062(2) Uani 1 1 d . . . O13 O 0.0909(4) 0.5602(6) 0.1687(4) 0.0566(19) Uani 1 1 d . . . O14 O -0.0239(4) 0.5318(7) 0.1880(4) 0.072(2) Uani 1 1 d . . . Cl2 Cl 0.34477(11) 0.64542(15) 0.17929(13) 0.0351(5) Uani 1 1 d . . . O21 O 0.3747(4) 0.6389(8) 0.2634(5) 0.079(3) Uani 1 1 d . . . O22 O 0.3629(4) 0.7528(5) 0.1453(5) 0.061(2) Uani 1 1 d . . . O23 O 0.3704(4) 0.5554(6) 0.1313(6) 0.091(3) Uani 1 1 d . . . O24 O 0.2704(3) 0.6390(5) 0.1806(4) 0.0477(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0360(2) 0.03406(18) 0.02256(17) -0.00662(12) -0.00139(14) -0.00459(14) Hg2 0.0321(2) 0.02797(17) 0.02344(17) -0.00519(11) -0.00326(14) 0.00010(12) N11 0.037(4) 0.021(3) 0.021(3) 0.003(2) 0.007(3) 0.001(3) C12 0.019(4) 0.019(3) 0.026(4) 0.002(3) -0.006(3) -0.003(3) C13 0.021(4) 0.031(4) 0.021(4) -0.004(3) 0.000(3) -0.002(3) C14 0.038(5) 0.026(4) 0.023(4) 0.001(3) 0.000(4) -0.001(3) C15 0.042(5) 0.020(4) 0.030(4) 0.003(3) -0.003(4) -0.002(3) C16 0.037(5) 0.022(4) 0.036(4) -0.006(3) -0.005(4) -0.001(3) N21 0.034(4) 0.014(3) 0.023(3) -0.002(2) -0.003(3) -0.001(3) N22 0.035(4) 0.020(3) 0.024(3) -0.001(2) -0.006(3) 0.000(3) C24 0.036(5) 0.024(4) 0.034(4) -0.009(3) 0.002(4) -0.004(3) C25 0.032(5) 0.024(4) 0.024(4) 0.000(3) 0.000(4) -0.004(3) C26 0.023(4) 0.022(4) 0.030(4) 0.000(3) 0.004(3) -0.005(3) C31 0.046(6) 0.016(3) 0.035(4) 0.006(3) -0.010(4) 0.003(3) C32 0.035(5) 0.009(3) 0.034(4) 0.003(3) -0.002(4) 0.003(3) C33 0.055(6) 0.017(4) 0.033(4) 0.004(3) 0.008(4) 0.007(4) C34 0.039(5) 0.026(4) 0.048(5) -0.001(4) 0.010(4) 0.002(4) C35 0.040(6) 0.028(4) 0.031(4) -0.001(3) -0.010(4) -0.006(4) C36 0.040(5) 0.018(3) 0.027(4) 0.007(3) -0.005(4) 0.005(3) C37 0.030(5) 0.014(3) 0.028(4) 0.009(3) -0.007(3) 0.007(3) C38 0.031(5) 0.020(3) 0.032(4) 0.010(3) -0.005(4) 0.002(3) N41 0.031(4) 0.018(3) 0.024(3) 0.005(2) -0.006(3) 0.002(3) N42 0.043(4) 0.019(3) 0.019(3) 0.006(2) 0.000(3) 0.004(3) C43 0.041(5) 0.033(4) 0.021(4) 0.003(3) -0.001(4) 0.005(4) C44 0.034(5) 0.024(4) 0.030(4) 0.004(3) -0.009(4) 0.002(3) C45 0.030(5) 0.020(4) 0.030(4) -0.002(3) 0.005(4) 0.002(3) N51 0.028(4) 0.020(3) 0.028(3) -0.002(2) 0.007(3) 0.003(3) C52 0.024(5) 0.026(4) 0.024(4) 0.001(3) 0.000(3) 0.010(3) C53 0.029(5) 0.031(4) 0.029(4) -0.006(3) -0.005(4) 0.000(3) C54 0.039(6) 0.024(4) 0.045(5) -0.005(3) 0.002(4) -0.006(4) C55 0.040(5) 0.014(3) 0.042(5) -0.001(3) 0.006(4) 0.000(3) C56 0.037(5) 0.021(4) 0.024(4) 0.005(3) 0.001(4) 0.010(3) O61 0.036(4) 0.044(3) 0.045(4) -0.012(3) 0.003(3) -0.003(3) C62 0.027(5) 0.042(5) 0.041(5) 0.003(4) -0.007(4) 0.009(4) N63 0.031(5) 0.040(4) 0.069(5) 0.004(4) 0.010(4) 0.003(3) C64 0.059(8) 0.071(7) 0.117(11) -0.024(7) 0.044(8) 0.004(6) C65 0.041(7) 0.063(7) 0.108(10) 0.000(6) 0.014(7) -0.004(5) O71 0.053(5) 0.054(4) 0.147(8) 0.008(5) -0.004(5) 0.017(4) C72 0.058(8) 0.043(6) 0.084(8) -0.016(5) 0.010(6) -0.012(5) N73 0.041(5) 0.034(4) 0.060(5) -0.003(3) -0.001(4) -0.005(3) C74 0.058(8) 0.049(6) 0.101(9) 0.010(6) -0.018(7) -0.016(5) C75 0.050(7) 0.062(6) 0.064(7) 0.013(5) -0.001(6) 0.004(5) Cl1 0.0365(12) 0.0190(8) 0.0272(9) 0.0006(7) 0.0014(9) 0.0010(7) O11 0.145(8) 0.032(3) 0.027(3) 0.002(3) -0.007(4) 0.038(4) O12 0.104(6) 0.038(3) 0.047(4) -0.018(3) 0.031(4) -0.025(4) O13 0.057(5) 0.065(4) 0.051(4) -0.026(3) 0.021(4) -0.022(3) O14 0.043(5) 0.120(6) 0.053(4) 0.028(4) 0.000(4) 0.008(4) Cl2 0.0382(13) 0.0283(10) 0.0390(11) -0.0016(8) 0.0048(10) -0.0003(9) O21 0.041(5) 0.135(8) 0.060(5) 0.039(5) -0.006(4) 0.005(5) O22 0.056(5) 0.046(4) 0.081(5) 0.020(3) 0.006(4) -0.006(3) O23 0.084(6) 0.051(4) 0.144(8) -0.045(5) 0.059(6) -0.006(4) O24 0.038(4) 0.056(4) 0.049(4) -0.017(3) 0.006(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N21 2.340(5) . ? Hg1 N11 2.354(6) . ? Hg1 Hg2 2.5237(6) . ? Hg2 N51 2.310(6) . ? Hg2 N41 2.373(6) . ? Hg2 O61 2.579(6) . ? N11 C16 1.351(9) . ? N11 C12 1.365(9) . ? C12 C13 1.368(10) . ? C12 C26 1.464(9) . ? C13 C14 1.377(10) . ? C14 C15 1.400(10) . ? C15 C16 1.361(11) . ? N21 C26 1.336(9) . ? N21 N22 1.363(7) . ? N22 C24 1.348(9) . ? N22 C31 1.463(9) . ? C24 C25 1.377(10) . ? C25 C26 1.410(9) . ? C31 C32 1.516(11) . ? C32 C33 1.381(11) . ? C32 C37 1.401(10) . ? C33 C34 1.381(12) . ? C34 C35 1.384(11) . ? C35 C36 1.377(11) . ? C36 C37 1.417(10) . ? C36 C38 1.487(10) . ? C38 N42 1.482(9) . ? N41 C45 1.344(9) . ? N41 N42 1.362(8) . ? N42 C43 1.324(10) . ? C43 C44 1.386(10) . ? C44 C45 1.392(11) . ? C45 C52 1.478(10) . ? N51 C52 1.338(9) . ? N51 C56 1.342(9) . ? C52 C53 1.387(10) . ? C53 C54 1.370(10) . ? C54 C55 1.377(11) . ? C55 C56 1.400(10) . ? O61 C62 1.237(10) . ? C62 N63 1.317(11) . ? N63 C64 1.454(12) . ? N63 C65 1.454(12) . ? O71 C72 1.226(13) . ? C72 N73 1.338(11) . ? N73 C74 1.444(12) . ? N73 C75 1.445(12) . ? Cl1 O11 1.405(5) . ? Cl1 O14 1.413(7) . ? Cl1 O13 1.419(6) . ? Cl1 O12 1.426(6) . ? Cl2 O23 1.408(6) . ? Cl2 O22 1.417(6) . ? Cl2 O21 1.427(7) . ? Cl2 O24 1.441(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 N21 Hg1 N11 70.09(19) . . ? N21 Hg1 Hg2 148.19(15) . . ? N11 Hg1 Hg2 138.43(14) . . ? N51 Hg2 N41 70.5(2) . . ? N51 Hg2 Hg1 149.56(15) . . ? N41 Hg2 Hg1 137.28(14) . . ? N51 Hg2 O61 79.56(19) . . ? N41 Hg2 O61 90.7(2) . . ? Hg1 Hg2 O61 107.16(13) . . ? C16 N11 C12 118.6(6) . . ? C16 N11 Hg1 124.4(5) . . ? C12 N11 Hg1 116.8(4) . . ? N11 C12 C13 121.0(6) . . ? N11 C12 C26 115.4(6) . . ? C13 C12 C26 123.6(6) . . ? C12 C13 C14 120.2(7) . . ? C13 C14 C15 119.0(7) . . ? C16 C15 C14 118.4(7) . . ? N11 C16 C15 122.8(7) . . ? C26 N21 N22 105.5(5) . . ? C26 N21 Hg1 115.8(4) . . ? N22 N21 Hg1 135.5(4) . . ? C24 N22 N21 110.6(6) . . ? C24 N22 C31 128.8(6) . . ? N21 N22 C31 119.8(6) . . ? N22 C24 C25 108.7(6) . . ? C24 C25 C26 103.9(6) . . ? N21 C26 C25 111.4(6) . . ? N21 C26 C12 118.7(6) . . ? C25 C26 C12 129.9(7) . . ? N22 C31 C32 112.2(6) . . ? C33 C32 C37 119.9(7) . . ? C33 C32 C31 120.9(7) . . ? C37 C32 C31 119.2(7) . . ? C32 C33 C34 120.2(7) . . ? C33 C34 C35 120.3(8) . . ? C36 C35 C34 121.1(8) . . ? C35 C36 C37 118.7(7) . . ? C35 C36 C38 123.0(7) . . ? C37 C36 C38 118.3(7) . . ? C32 C37 C36 119.7(7) . . ? N42 C38 C36 113.0(6) . . ? C45 N41 N42 105.1(6) . . ? C45 N41 Hg2 115.7(5) . . ? N42 N41 Hg2 138.6(4) . . ? C43 N42 N41 111.2(6) . . ? C43 N42 C38 128.8(6) . . ? N41 N42 C38 119.9(6) . . ? N42 C43 C44 108.5(6) . . ? C43 C44 C45 104.1(7) . . ? N41 C45 C44 111.1(6) . . ? N41 C45 C52 117.7(7) . . ? C44 C45 C52 131.2(7) . . ? C52 N51 C56 119.0(6) . . ? C52 N51 Hg2 118.6(4) . . ? C56 N51 Hg2 121.8(5) . . ? N51 C52 C53 121.7(7) . . ? N51 C52 C45 116.7(6) . . ? C53 C52 C45 121.7(7) . . ? C54 C53 C52 119.2(7) . . ? C53 C54 C55 120.2(7) . . ? C54 C55 C56 117.6(7) . . ? N51 C56 C55 122.3(7) . . ? C62 O61 Hg2 133.0(5) . . ? O61 C62 N63 123.7(8) . . ? C62 N63 C64 120.1(8) . . ? C62 N63 C65 121.9(8) . . ? C64 N63 C65 117.9(8) . . ? O71 C72 N73 127.1(10) . . ? C72 N73 C74 119.1(9) . . ? C72 N73 C75 122.4(9) . . ? C74 N73 C75 118.5(8) . . ? O11 Cl1 O14 108.0(5) . . ? O11 Cl1 O13 110.4(4) . . ? O14 Cl1 O13 107.5(4) . . ? O11 Cl1 O12 109.8(4) . . ? O14 Cl1 O12 109.4(5) . . ? O13 Cl1 O12 111.7(4) . . ? O23 Cl2 O22 110.3(5) . . ? O23 Cl2 O21 109.6(6) . . ? O22 Cl2 O21 108.1(5) . . ? O23 Cl2 O24 110.8(4) . . ? O22 Cl2 O24 108.9(4) . . ? O21 Cl2 O24 109.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Hg1 Hg2 N51 160.6(4) . . . . ? N11 Hg1 Hg2 N51 13.0(4) . . . . ? N21 Hg1 Hg2 N41 -48.7(4) . . . . ? N11 Hg1 Hg2 N41 163.7(3) . . . . ? N21 Hg1 Hg2 O61 61.9(3) . . . . ? N11 Hg1 Hg2 O61 -85.7(3) . . . . ? N21 Hg1 N11 C16 173.7(7) . . . . ? Hg2 Hg1 N11 C16 -23.8(7) . . . . ? N21 Hg1 N11 C12 -12.3(5) . . . . ? Hg2 Hg1 N11 C12 150.2(4) . . . . ? C16 N11 C12 C13 1.0(11) . . . . ? Hg1 N11 C12 C13 -173.3(5) . . . . ? C16 N11 C12 C26 -177.8(7) . . . . ? Hg1 N11 C12 C26 7.8(8) . . . . ? N11 C12 C13 C14 -0.9(11) . . . . ? C26 C12 C13 C14 177.9(7) . . . . ? C12 C13 C14 C15 0.9(12) . . . . ? C13 C14 C15 C16 -1.1(12) . . . . ? C12 N11 C16 C15 -1.2(12) . . . . ? Hg1 N11 C16 C15 172.7(6) . . . . ? C14 C15 C16 N11 1.3(13) . . . . ? N11 Hg1 N21 C26 15.9(5) . . . . ? Hg2 Hg1 N21 C26 -141.9(4) . . . . ? N11 Hg1 N21 N22 172.1(7) . . . . ? Hg2 Hg1 N21 N22 14.4(9) . . . . ? C26 N21 N22 C24 -0.8(8) . . . . ? Hg1 N21 N22 C24 -158.7(6) . . . . ? C26 N21 N22 C31 -171.4(7) . . . . ? Hg1 N21 N22 C31 30.7(11) . . . . ? N21 N22 C24 C25 0.3(9) . . . . ? C31 N22 C24 C25 169.8(8) . . . . ? N22 C24 C25 C26 0.3(9) . . . . ? N22 N21 C26 C25 1.0(8) . . . . ? Hg1 N21 C26 C25 164.0(5) . . . . ? N22 N21 C26 C12 178.7(6) . . . . ? Hg1 N21 C26 C12 -18.4(9) . . . . ? C24 C25 C26 N21 -0.8(9) . . . . ? C24 C25 C26 C12 -178.2(8) . . . . ? N11 C12 C26 N21 7.1(10) . . . . ? C13 C12 C26 N21 -171.7(7) . . . . ? N11 C12 C26 C25 -175.7(7) . . . . ? C13 C12 C26 C25 5.5(13) . . . . ? C24 N22 C31 C32 134.3(8) . . . . ? N21 N22 C31 C32 -57.1(10) . . . . ? N22 C31 C32 C33 -51.6(9) . . . . ? N22 C31 C32 C37 130.0(7) . . . . ? C37 C32 C33 C34 1.1(10) . . . . ? C31 C32 C33 C34 -177.4(7) . . . . ? C32 C33 C34 C35 -0.3(11) . . . . ? C33 C34 C35 C36 0.0(12) . . . . ? C34 C35 C36 C37 -0.5(11) . . . . ? C34 C35 C36 C38 -179.7(7) . . . . ? C33 C32 C37 C36 -1.5(10) . . . . ? C31 C32 C37 C36 176.9(6) . . . . ? C35 C36 C37 C32 1.2(10) . . . . ? C38 C36 C37 C32 -179.5(6) . . . . ? C35 C36 C38 N42 38.6(9) . . . . ? C37 C36 C38 N42 -140.7(6) . . . . ? N51 Hg2 N41 C45 -7.0(5) . . . . ? Hg1 Hg2 N41 C45 -171.7(4) . . . . ? O61 Hg2 N41 C45 71.7(5) . . . . ? N51 Hg2 N41 N42 -176.6(8) . . . . ? Hg1 Hg2 N41 N42 18.7(9) . . . . ? O61 Hg2 N41 N42 -97.9(7) . . . . ? C45 N41 N42 C43 1.0(8) . . . . ? Hg2 N41 N42 C43 171.3(6) . . . . ? C45 N41 N42 C38 178.2(7) . . . . ? Hg2 N41 N42 C38 -11.5(11) . . . . ? C36 C38 N42 C43 -135.3(8) . . . . ? C36 C38 N42 N41 48.1(9) . . . . ? N41 N42 C43 C44 -0.8(9) . . . . ? C38 N42 C43 C44 -177.7(7) . . . . ? N42 C43 C44 C45 0.3(9) . . . . ? N42 N41 C45 C44 -0.8(9) . . . . ? Hg2 N41 C45 C44 -173.7(5) . . . . ? N42 N41 C45 C52 178.7(6) . . . . ? Hg2 N41 C45 C52 5.8(9) . . . . ? C43 C44 C45 N41 0.4(9) . . . . ? C43 C44 C45 C52 -179.0(8) . . . . ? N41 Hg2 N51 C52 7.9(5) . . . . ? Hg1 Hg2 N51 C52 167.2(4) . . . . ? O61 Hg2 N51 C52 -86.6(5) . . . . ? N41 Hg2 N51 C56 178.9(6) . . . . ? Hg1 Hg2 N51 C56 -21.7(7) . . . . ? O61 Hg2 N51 C56 84.5(6) . . . . ? C56 N51 C52 C53 0.0(11) . . . . ? Hg2 N51 C52 C53 171.3(5) . . . . ? C56 N51 C52 C45 -179.2(7) . . . . ? Hg2 N51 C52 C45 -7.9(9) . . . . ? N41 C45 C52 N51 1.2(10) . . . . ? C44 C45 C52 N51 -179.5(8) . . . . ? N41 C45 C52 C53 -178.0(7) . . . . ? C44 C45 C52 C53 1.3(13) . . . . ? N51 C52 C53 C54 0.7(12) . . . . ? C45 C52 C53 C54 179.8(7) . . . . ? C52 C53 C54 C55 -1.3(12) . . . . ? C53 C54 C55 C56 1.2(12) . . . . ? C52 N51 C56 C55 -0.1(11) . . . . ? Hg2 N51 C56 C55 -171.1(6) . . . . ? C54 C55 C56 N51 -0.5(12) . . . . ? N51 Hg2 O61 C62 -12.5(8) . . . . ? N41 Hg2 O61 C62 -82.6(8) . . . . ? Hg1 Hg2 O61 C62 136.8(7) . . . . ? Hg2 O61 C62 N63 -174.1(6) . . . . ? O61 C62 N63 C64 -3.3(14) . . . . ? O61 C62 N63 C65 178.2(9) . . . . ? O71 C72 N73 C74 0.3(18) . . . . ? O71 C72 N73 C75 178.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.198 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.213 #===END data_imw322m _database_code_depnum_ccdc_archive 'CCDC 609500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Cl2 Hg2 N6 O8, C24 H20 Hg2 N6, 2(Cl O4)' _chemical_formula_sum 'C48 H40 Cl4 Hg4 N12 O16' _chemical_formula_weight 1985.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.744(4) _cell_length_b 14.504(4) _cell_length_c 15.839(5) _cell_angle_alpha 84.768(5) _cell_angle_beta 87.466(5) _cell_angle_gamma 89.353(5) _cell_volume 2684.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 942 _cell_measurement_theta_min 5.170 _cell_measurement_theta_max 53.580 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 11.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1054 _exptl_absorpt_correction_T_max 0.3878 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30500 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.57 _reflns_number_total 11992 _reflns_number_gt 8480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^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 11992 _refine_ls_number_parameters 772 _refine_ls_number_restraints 146 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 0.20053(3) 0.23219(3) 0.13732(2) 0.03066(11) Uani 1 1 d . A . Hg2 Hg 0.12531(4) 0.14299(3) 0.27206(2) 0.03416(12) Uani 1 1 d . . . Hg3 Hg 0.25544(3) 0.29284(3) 0.63634(2) 0.03225(12) Uani 1 1 d . . . Hg4 Hg 0.36099(4) 0.22797(3) 0.76346(2) 0.03326(12) Uani 1 1 d . . . N11A N 0.3867(7) 0.2925(6) 0.0984(5) 0.0310(19) Uani 1 1 d . . . C12A C 0.3955(8) 0.3426(7) 0.0236(6) 0.028(2) Uani 1 1 d . A . C13A C 0.4986(9) 0.3863(7) -0.0071(6) 0.034(2) Uani 1 1 d . . . H13A H 0.5034 0.4206 -0.0611 0.041 Uiso 1 1 calc R A . C14A C 0.5913(9) 0.3779(7) 0.0431(7) 0.036(2) Uani 1 1 d . A . H14A H 0.6612 0.4069 0.0243 0.043 Uiso 1 1 calc R . . C15A C 0.5821(10) 0.3273(8) 0.1205(7) 0.041(3) Uani 1 1 d . . . H15A H 0.6452 0.3205 0.1561 0.049 Uiso 1 1 calc R A . C16A C 0.4770(9) 0.2855(8) 0.1459(6) 0.034(2) Uani 1 1 d . A . H16A H 0.4705 0.2507 0.1997 0.041 Uiso 1 1 calc R . . N21A N 0.1996(7) 0.3036(5) 0.0045(5) 0.0255(17) Uani 1 1 d . . . N22A N 0.1171(7) 0.3285(6) -0.0505(5) 0.0286(19) Uani 1 1 d . A . C23A C 0.1556(9) 0.3886(7) -0.1130(6) 0.033(2) Uani 1 1 d . . . H23A H 0.1131 0.4159 -0.1586 0.040 Uiso 1 1 calc R A . C24A C 0.2690(9) 0.4041(7) -0.0996(6) 0.032(2) Uani 1 1 d . A . H24A H 0.3201 0.4429 -0.1344 0.039 Uiso 1 1 calc R . . C25A C 0.2926(8) 0.3519(7) -0.0256(6) 0.026(2) Uani 1 1 d . A . C31A C 0.0063(8) 0.2818(7) -0.0447(6) 0.030(2) Uani 1 1 d . . . H31A H 0.0147 0.2237 -0.0727 0.036 Uiso 1 1 calc R A . H31B H -0.0487 0.3218 -0.0769 0.036 Uiso 1 1 calc R . . C32A C -0.0430(8) 0.2590(7) 0.0434(6) 0.027(2) Uani 1 1 d . A . C33A C -0.0629(8) 0.3246(7) 0.1009(6) 0.027(2) Uani 1 1 d . . . H33A H -0.0418 0.3872 0.0859 0.032 Uiso 1 1 calc R A . C34A C -0.1135(8) 0.2993(7) 0.1803(6) 0.029(2) Uani 1 1 d . A . H34A H -0.1255 0.3447 0.2195 0.035 Uiso 1 1 calc R . . C35A C -0.1469(8) 0.2084(7) 0.2034(6) 0.029(2) Uani 1 1 d . . . C36A C -0.1283(8) 0.1427(7) 0.1463(7) 0.036(3) Uani 1 1 d . A . H36A H -0.1522 0.0807 0.1610 0.043 Uiso 1 1 calc R . . C37A C -0.0746(9) 0.1669(7) 0.0676(6) 0.033(2) Uani 1 1 d . . . H37A H -0.0591 0.1207 0.0297 0.040 Uiso 1 1 calc R A . C38A C -0.2145(9) 0.1814(8) 0.2869(6) 0.038(3) Uani 1 1 d . A . H38A H -0.2786 0.2256 0.2924 0.046 Uiso 1 1 calc R . . H38B H -0.2473 0.1192 0.2843 0.046 Uiso 1 1 calc R . . N41A N -0.0403(7) 0.1460(6) 0.3651(5) 0.0311(19) Uani 1 1 d . A . N42A N -0.1469(6) 0.1801(6) 0.3625(5) 0.0289(18) Uani 1 1 d . . . C43A C -0.1897(9) 0.1910(7) 0.4416(6) 0.034(2) Uani 1 1 d . A . H43A H -0.2639 0.2130 0.4558 0.041 Uiso 1 1 calc R . . C44A C -0.1087(9) 0.1651(7) 0.4968(6) 0.033(2) Uani 1 1 d . . . H44A H -0.1137 0.1655 0.5568 0.040 Uiso 1 1 calc R A . C45A C -0.0168(9) 0.1377(6) 0.4471(6) 0.027(2) Uani 1 1 d . A . N51A N 0.1728(7) 0.0875(5) 0.4083(5) 0.0281(18) Uani 1 1 d . A . C52A C 0.0952(8) 0.1039(7) 0.4716(6) 0.025(2) Uani 1 1 d . . . C53A C 0.1229(9) 0.0855(7) 0.5559(6) 0.036(3) Uani 1 1 d . A . H53A H 0.0685 0.0961 0.6003 0.043 Uiso 1 1 calc R . . C54A C 0.2314(9) 0.0513(8) 0.5750(6) 0.037(3) Uani 1 1 d . . . H54A H 0.2525 0.0406 0.6323 0.044 Uiso 1 1 calc R A . C55A C 0.3071(9) 0.0334(8) 0.5096(7) 0.037(3) Uani 1 1 d . A . H55A H 0.3800 0.0076 0.5215 0.045 Uiso 1 1 calc R . . C56A C 0.2765(9) 0.0531(8) 0.4266(7) 0.036(3) Uani 1 1 d . . . H56A H 0.3297 0.0422 0.3816 0.044 Uiso 1 1 calc R A . N11B N 0.0890(7) 0.3454(6) 0.5802(5) 0.0309(19) Uani 1 1 d . . . C12B C 0.0848(9) 0.3598(7) 0.4957(6) 0.031(2) Uani 1 1 d . . . C13B C -0.0174(10) 0.3904(8) 0.4588(7) 0.042(3) Uani 1 1 d . . . H13B H -0.0218 0.4003 0.3989 0.050 Uiso 1 1 calc R . . C14B C -0.1107(10) 0.4055(8) 0.5112(7) 0.042(3) Uani 1 1 d . . . H14B H -0.1805 0.4260 0.4875 0.050 Uiso 1 1 calc R . . C15B C -0.1040(9) 0.3912(8) 0.5974(7) 0.043(3) Uani 1 1 d . . . H15B H -0.1686 0.4012 0.6337 0.052 Uiso 1 1 calc R . . C16B C -0.0024(9) 0.3622(8) 0.6306(7) 0.036(2) Uani 1 1 d . . . H16B H 0.0035 0.3538 0.6904 0.043 Uiso 1 1 calc R . . N21B N 0.2763(7) 0.3001(6) 0.4831(5) 0.035(2) Uani 1 1 d . . . N22B N 0.3629(8) 0.3049(6) 0.4232(5) 0.035(2) Uani 1 1 d . . . C23B C 0.3325(12) 0.3507(9) 0.3500(7) 0.049(3) Uani 1 1 d . . . H23B H 0.3788 0.3622 0.2995 0.059 Uiso 1 1 calc R . . C24B C 0.2224(12) 0.3773(9) 0.3627(7) 0.048(3) Uani 1 1 d . . . H24B H 0.1768 0.4112 0.3225 0.058 Uiso 1 1 calc R . . C25B C 0.1888(9) 0.3459(7) 0.4450(6) 0.031(2) Uani 1 1 d . . . C31B C 0.4677(9) 0.2539(8) 0.4384(7) 0.038(3) Uani 1 1 d . . . H31C H 0.5237 0.2721 0.3915 0.046 Uiso 1 1 calc R . . H31D H 0.4524 0.1871 0.4370 0.046 Uiso 1 1 calc R . . C32B C 0.5203(8) 0.2682(7) 0.5211(6) 0.031(2) Uani 1 1 d . . . C33B C 0.5343(8) 0.3580(7) 0.5460(6) 0.032(2) Uani 1 1 d . . . H33B H 0.5130 0.4105 0.5096 0.039 Uiso 1 1 calc R . . C34B C 0.5790(9) 0.3695(9) 0.6231(7) 0.043(3) Uani 1 1 d . . . H34B H 0.5857 0.4299 0.6407 0.051 Uiso 1 1 calc R . . C35B C 0.6147(8) 0.2928(8) 0.6758(6) 0.033(2) Uani 1 1 d . . . C36B C 0.6047(9) 0.2058(8) 0.6513(7) 0.034(2) Uani 1 1 d . . . H36B H 0.6317 0.1540 0.6861 0.040 Uiso 1 1 calc R . . C37B C 0.5552(9) 0.1930(8) 0.5759(7) 0.038(3) Uani 1 1 d . . . H37B H 0.5447 0.1318 0.5608 0.045 Uiso 1 1 calc R . . C38B C 0.6654(10) 0.3131(8) 0.7595(7) 0.043(3) Uani 1 1 d . . . H38C H 0.7496 0.3105 0.7531 0.052 Uiso 1 1 calc R . . H38D H 0.6435 0.3767 0.7721 0.052 Uiso 1 1 calc R . . N41B N 0.5194(7) 0.2221(6) 0.8437(5) 0.0300(19) Uani 1 1 d . . . N42B N 0.6279(7) 0.2482(6) 0.8309(5) 0.034(2) Uani 1 1 d . . . C43B C 0.6914(9) 0.2171(8) 0.8985(7) 0.036(2) Uani 1 1 d . . . H43B H 0.7703 0.2275 0.9043 0.043 Uiso 1 1 calc R . . C44B C 0.6194(8) 0.1680(7) 0.9559(6) 0.032(2) Uani 1 1 d . . . H44B H 0.6376 0.1379 1.0094 0.038 Uiso 1 1 calc R . . C45B C 0.5127(8) 0.1718(7) 0.9188(6) 0.027(2) Uani 1 1 d . . . N51B N 0.3200(7) 0.1401(6) 0.8923(5) 0.0253(17) Uani 1 1 d . . . C52B C 0.4030(8) 0.1284(7) 0.9480(6) 0.025(2) Uani 1 1 d . . . C53B C 0.3875(9) 0.0818(7) 1.0276(7) 0.036(2) Uani 1 1 d . . . H53B H 0.4477 0.0768 1.0659 0.044 Uiso 1 1 calc R . . C54B C 0.2833(9) 0.0428(7) 1.0501(6) 0.034(2) Uani 1 1 d . . . H54B H 0.2705 0.0086 1.1037 0.041 Uiso 1 1 calc R . . C55B C 0.1962(8) 0.0546(7) 0.9923(6) 0.030(2) Uani 1 1 d . . . H55B H 0.1226 0.0301 1.0069 0.036 Uiso 1 1 calc R . . C56B C 0.2183(9) 0.1015(7) 0.9151(6) 0.030(2) Uani 1 1 d . . . H56B H 0.1594 0.1072 0.8756 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.1774(2) 0.50093(17) 0.13953(15) 0.0326(6) Uani 1 1 d . . . O11 O 0.1495(8) 0.4084(5) 0.1745(5) 0.048(2) Uani 1 1 d . . . O12 O 0.1344(9) 0.5162(6) 0.0570(5) 0.059(2) Uani 1 1 d . . . O13 O 0.1257(6) 0.5656(5) 0.1933(5) 0.0418(19) Uani 1 1 d . . . O14 O 0.2985(7) 0.5100(7) 0.1361(6) 0.068(3) Uani 1 1 d . . . Cl2 Cl 0.0526(2) -0.10179(19) 0.22705(15) 0.0352(6) Uani 0.37(2) 1 d PD A 1 O21 O -0.0666(11) -0.1285(17) 0.2518(11) 0.047(7) Uiso 0.37(2) 1 d PDU A 1 O22 O 0.1185(19) -0.1854(12) 0.2334(14) 0.068(9) Uiso 0.37(2) 1 d PDU A 1 O23 O 0.0880(17) -0.0380(10) 0.2825(9) 0.029(5) Uiso 0.37(2) 1 d PDU A 1 O24 O 0.0509(17) -0.0620(14) 0.1406(7) 0.032(6) Uiso 0.37(2) 1 d PDU A 1 Cl2' Cl 0.0526(2) -0.10179(19) 0.22705(15) 0.0352(6) Uani 0.357(19) 1 d PD B 2 O21' O -0.0363(16) -0.1704(13) 0.2469(12) 0.045(7) Uiso 0.357(19) 1 d PDU B 2 O22' O 0.1552(14) -0.1375(17) 0.2642(15) 0.093(11) Uiso 0.357(19) 1 d PDU B 2 O23' O 0.0180(18) -0.0186(9) 0.2645(11) 0.039(7) Uiso 0.357(19) 1 d PDU B 2 O24' O 0.068(2) -0.0851(17) 0.1377(7) 0.040(18) Uiso 0.357(19) 1 d PDU B 2 Cl2$ Cl 0.0526(2) -0.10179(19) 0.22705(15) 0.0352(6) Uani 0.273(19) 1 d PD C 3 O21$ O -0.0556(16) -0.061(2) 0.2510(18) 0.070(12) Uiso 0.273(19) 1 d PDU C 3 O22$ O 0.142(2) -0.0513(17) 0.2609(17) 0.054(10) Uiso 0.273(19) 1 d PDU C 3 O23$ O 0.055(3) -0.1963(10) 0.2568(16) 0.055(10) Uiso 0.273(19) 1 d PDU C 3 O24$ O 0.065(3) -0.092(2) 0.1356(8) 0.04(2) Uiso 0.273(19) 1 d PDU C 3 Cl3 Cl 0.3109(2) 0.52899(18) 0.67154(15) 0.0339(6) Uani 1 1 d . . . O31 O 0.2053(6) 0.5033(6) 0.7150(5) 0.0423(19) Uani 1 1 d . . . O32 O 0.3254(6) 0.4785(5) 0.5973(4) 0.0383(18) Uani 1 1 d . . . O33 O 0.3075(8) 0.6264(6) 0.6452(5) 0.060(3) Uani 1 1 d . . . O34 O 0.4034(7) 0.5085(7) 0.7261(5) 0.056(2) Uani 1 1 d . . . Cl4 Cl 0.47052(19) 0.96625(16) 0.75095(14) 0.0281(5) Uani 1 1 d . . . O41 O 0.4745(7) 0.9041(6) 0.6865(5) 0.057(2) Uani 1 1 d . . . O42 O 0.4131(8) 1.0480(6) 0.7190(5) 0.053(2) Uani 1 1 d . . . O43 O 0.4096(6) 0.9259(6) 0.8255(5) 0.049(2) Uani 1 1 d . . . O44 O 0.5844(6) 0.9886(6) 0.7710(5) 0.052(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0382(2) 0.0290(2) 0.0239(2) -0.00018(15) 0.00424(16) -0.00197(17) Hg2 0.0458(3) 0.0323(2) 0.0235(2) -0.00087(16) 0.00618(17) -0.00492(18) Hg3 0.0360(2) 0.0328(2) 0.0283(2) 0.00026(16) -0.01084(16) -0.00224(17) Hg4 0.0393(2) 0.0355(2) 0.0259(2) -0.00454(17) -0.01019(16) 0.00520(18) N11A 0.032(5) 0.035(5) 0.026(4) -0.001(4) -0.001(3) -0.006(4) C12A 0.031(5) 0.031(6) 0.025(5) -0.017(4) 0.006(4) 0.003(4) C13A 0.041(6) 0.031(6) 0.029(5) 0.004(4) 0.000(4) 0.001(5) C14A 0.025(5) 0.033(6) 0.048(7) 0.003(5) 0.002(5) -0.001(4) C15A 0.040(7) 0.034(7) 0.049(7) -0.005(5) -0.013(5) 0.005(5) C16A 0.036(6) 0.038(6) 0.028(5) -0.002(5) 0.004(4) -0.001(5) N21A 0.025(4) 0.024(4) 0.029(4) -0.008(3) -0.003(3) 0.004(3) N22A 0.028(4) 0.038(5) 0.020(4) -0.001(4) -0.005(3) -0.007(4) C23A 0.036(6) 0.034(6) 0.028(5) 0.002(4) -0.001(4) 0.001(5) C24A 0.040(6) 0.029(6) 0.027(5) 0.004(4) 0.000(4) 0.000(5) C25A 0.029(5) 0.024(5) 0.027(5) -0.007(4) -0.003(4) -0.005(4) C31A 0.022(5) 0.038(6) 0.029(5) 0.001(4) -0.004(4) -0.002(4) C32A 0.025(5) 0.028(6) 0.027(5) 0.001(4) -0.003(4) -0.001(4) C33A 0.028(5) 0.029(6) 0.025(5) -0.005(4) -0.009(4) 0.001(4) C34A 0.023(5) 0.034(6) 0.033(5) -0.009(4) -0.005(4) 0.002(4) C35A 0.023(5) 0.033(6) 0.029(5) 0.004(4) 0.000(4) -0.003(4) C36A 0.027(5) 0.031(6) 0.051(7) -0.005(5) -0.001(5) -0.010(5) C37A 0.034(6) 0.029(6) 0.038(6) -0.008(5) -0.007(4) -0.007(5) C38A 0.028(6) 0.052(7) 0.034(6) 0.000(5) -0.006(4) -0.012(5) N41A 0.024(4) 0.042(5) 0.028(4) -0.004(4) 0.002(3) -0.004(4) N42A 0.021(4) 0.032(5) 0.033(5) 0.002(4) -0.004(3) -0.001(3) C43A 0.032(6) 0.040(7) 0.030(5) -0.010(5) 0.008(4) 0.004(5) C44A 0.040(6) 0.030(6) 0.028(5) 0.004(4) 0.003(4) 0.005(5) C45A 0.041(6) 0.019(5) 0.022(5) -0.007(4) 0.005(4) -0.006(4) N51A 0.036(5) 0.021(4) 0.026(4) 0.002(3) 0.001(3) 0.000(4) C52A 0.024(5) 0.029(5) 0.020(5) 0.012(4) 0.001(4) -0.007(4) C53A 0.043(6) 0.037(6) 0.026(5) 0.002(4) 0.008(4) -0.009(5) C54A 0.042(7) 0.039(7) 0.028(5) 0.012(5) -0.015(5) -0.006(5) C55A 0.028(6) 0.038(7) 0.047(7) -0.006(5) -0.006(5) 0.003(5) C56A 0.029(6) 0.040(7) 0.040(6) -0.008(5) 0.006(5) 0.006(5) N11B 0.028(5) 0.039(5) 0.027(4) 0.000(4) -0.008(3) -0.003(4) C12B 0.034(6) 0.026(6) 0.033(5) -0.006(4) -0.009(4) -0.002(4) C13B 0.048(7) 0.041(7) 0.037(6) -0.002(5) -0.006(5) -0.009(5) C14B 0.037(6) 0.039(7) 0.050(7) 0.003(5) -0.021(5) -0.001(5) C15B 0.026(6) 0.050(8) 0.052(7) -0.003(6) -0.004(5) -0.003(5) C16B 0.030(6) 0.043(7) 0.033(6) 0.006(5) -0.005(4) -0.006(5) N21B 0.035(5) 0.042(6) 0.028(5) -0.008(4) 0.004(4) -0.003(4) N22B 0.041(5) 0.036(5) 0.028(5) -0.009(4) 0.006(4) -0.002(4) C23B 0.077(9) 0.051(8) 0.020(5) -0.001(5) 0.003(5) -0.011(7) C24B 0.067(9) 0.051(8) 0.028(6) -0.006(5) -0.004(5) 0.012(6) C25B 0.044(6) 0.032(6) 0.018(5) -0.005(4) -0.006(4) -0.002(5) C31B 0.042(7) 0.038(6) 0.036(6) -0.014(5) 0.013(5) -0.009(5) C32B 0.022(5) 0.039(6) 0.032(5) -0.008(5) 0.009(4) -0.002(4) C33B 0.028(5) 0.031(6) 0.039(6) -0.005(5) 0.004(4) -0.006(4) C34B 0.038(6) 0.052(8) 0.040(6) -0.014(6) 0.005(5) -0.020(6) C35B 0.027(5) 0.037(6) 0.034(6) 0.005(5) 0.006(4) -0.007(5) C36B 0.033(6) 0.031(6) 0.036(6) 0.000(5) 0.003(4) -0.004(5) C37B 0.034(6) 0.027(6) 0.051(7) -0.006(5) 0.006(5) -0.004(5) C38B 0.046(7) 0.040(7) 0.042(6) 0.009(5) -0.011(5) -0.018(5) N41B 0.024(4) 0.032(5) 0.034(5) 0.001(4) -0.008(3) -0.008(4) N42B 0.025(5) 0.033(5) 0.043(5) -0.004(4) -0.007(4) -0.006(4) C43B 0.035(6) 0.036(6) 0.040(6) -0.009(5) -0.013(5) 0.002(5) C44B 0.032(6) 0.032(6) 0.032(5) -0.001(4) -0.013(4) 0.001(4) C45B 0.024(5) 0.032(6) 0.025(5) -0.009(4) 0.000(4) -0.007(4) N51B 0.025(4) 0.030(5) 0.022(4) -0.007(3) -0.002(3) -0.003(3) C52B 0.029(5) 0.022(5) 0.024(5) -0.004(4) -0.001(4) -0.001(4) C53B 0.032(6) 0.029(6) 0.050(7) -0.011(5) -0.003(5) 0.008(5) C54B 0.044(6) 0.031(6) 0.028(5) -0.004(4) -0.002(4) 0.003(5) C55B 0.026(5) 0.030(6) 0.035(6) -0.006(4) -0.001(4) 0.000(4) C56B 0.033(6) 0.029(6) 0.028(5) -0.005(4) -0.004(4) 0.002(4) Cl1 0.0387(14) 0.0299(14) 0.0304(12) -0.0086(10) -0.0028(10) -0.0051(11) O11 0.078(6) 0.028(4) 0.037(4) -0.001(3) -0.004(4) -0.009(4) O12 0.106(8) 0.044(5) 0.025(4) -0.001(4) -0.011(4) 0.010(5) O13 0.045(5) 0.043(5) 0.040(4) -0.018(4) 0.000(3) 0.005(4) O14 0.042(5) 0.086(7) 0.083(7) -0.041(6) 0.015(5) -0.010(5) Cl2 0.0355(14) 0.0443(16) 0.0270(12) -0.0097(11) -0.0021(10) 0.0026(11) Cl2' 0.0355(14) 0.0443(16) 0.0270(12) -0.0097(11) -0.0021(10) 0.0026(11) Cl2$ 0.0355(14) 0.0443(16) 0.0270(12) -0.0097(11) -0.0021(10) 0.0026(11) Cl3 0.0386(14) 0.0341(14) 0.0284(12) -0.0003(10) -0.0001(10) -0.0045(11) O31 0.038(4) 0.050(5) 0.037(4) 0.000(4) 0.005(3) -0.004(4) O32 0.040(4) 0.045(5) 0.029(4) -0.005(3) -0.002(3) 0.007(4) O33 0.089(7) 0.031(5) 0.057(6) 0.006(4) 0.021(5) -0.003(5) O34 0.046(5) 0.079(7) 0.046(5) -0.013(5) -0.011(4) 0.005(5) Cl4 0.0267(12) 0.0294(13) 0.0286(12) -0.0031(10) -0.0034(9) -0.0024(10) O41 0.042(5) 0.067(6) 0.067(6) -0.043(5) 0.015(4) -0.009(4) O42 0.072(6) 0.038(5) 0.050(5) 0.002(4) -0.022(4) 0.012(4) O43 0.035(4) 0.065(6) 0.044(5) 0.006(4) 0.001(3) -0.007(4) O44 0.031(4) 0.076(7) 0.048(5) 0.005(4) -0.014(3) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N21A 2.259(8) . ? Hg1 N11A 2.398(8) . ? Hg1 Hg2 2.5227(7) . ? Hg2 N51A 2.322(8) . ? Hg2 N41A 2.390(8) . ? Hg2 O23 2.656(14) . ? Hg3 N11B 2.279(8) . ? Hg3 N21B 2.421(8) . ? Hg3 Hg4 2.5149(8) . ? Hg4 N41B 2.295(8) . ? Hg4 N51B 2.340(8) . ? N11A C16A 1.325(13) . ? N11A C12A 1.334(13) . ? C12A C13A 1.418(13) . ? C12A C25A 1.465(13) . ? C13A C14A 1.374(14) . ? C14A C15A 1.371(15) . ? C15A C16A 1.408(14) . ? N21A C25A 1.350(12) . ? N21A N22A 1.356(11) . ? N22A C23A 1.326(12) . ? N22A C31A 1.469(12) . ? C23A C24A 1.383(14) . ? C24A C25A 1.374(14) . ? C31A C32A 1.497(13) . ? C32A C33A 1.387(13) . ? C32A C37A 1.405(13) . ? C33A C34A 1.386(13) . ? C34A C35A 1.392(13) . ? C35A C36A 1.381(14) . ? C35A C38A 1.533(13) . ? C36A C37A 1.390(14) . ? C38A N42A 1.464(12) . ? N41A C45A 1.334(12) . ? N41A N42A 1.342(11) . ? N42A C43A 1.350(12) . ? C43A C44A 1.347(14) . ? C44A C45A 1.383(14) . ? C45A C52A 1.454(14) . ? N51A C56A 1.344(13) . ? N51A C52A 1.360(12) . ? C52A C53A 1.390(13) . ? C53A C54A 1.397(15) . ? C54A C55A 1.376(15) . ? C55A C56A 1.383(15) . ? N11B C12B 1.338(12) . ? N11B C16B 1.342(13) . ? C12B C13B 1.408(15) . ? C12B C25B 1.454(14) . ? C13B C14B 1.373(16) . ? C14B C15B 1.367(15) . ? C15B C16B 1.371(15) . ? N21B C25B 1.352(13) . ? N21B N22B 1.358(11) . ? N22B C23B 1.344(14) . ? N22B C31B 1.447(14) . ? C23B C24B 1.356(18) . ? C24B C25B 1.382(15) . ? C31B C32B 1.505(14) . ? C32B C37B 1.400(16) . ? C32B C33B 1.408(14) . ? C33B C34B 1.375(14) . ? C34B C35B 1.400(16) . ? C35B C36B 1.362(14) . ? C35B C38B 1.531(14) . ? C36B C37B 1.380(15) . ? C38B N42B 1.460(13) . ? N41B N42B 1.335(10) . ? N41B C45B 1.337(12) . ? N42B C43B 1.371(13) . ? C43B C44B 1.370(15) . ? C44B C45B 1.406(13) . ? C45B C52B 1.478(12) . ? N51B C52B 1.342(12) . ? N51B C56B 1.345(12) . ? C52B C53B 1.380(14) . ? C53B C54B 1.373(14) . ? C54B C55B 1.401(14) . ? C55B C56B 1.360(14) . ? Cl1 O12 1.419(8) . ? Cl1 O14 1.429(9) . ? Cl1 O13 1.436(7) . ? Cl1 O11 1.440(8) . ? Cl2 O23 1.410(11) . ? Cl2 O22 1.430(12) . ? Cl2 O24 1.437(11) . ? Cl2 O21 1.483(11) . ? Cl3 O31 1.427(7) . ? Cl3 O34 1.430(8) . ? Cl3 O33 1.437(8) . ? Cl3 O32 1.444(7) . ? Cl4 O42 1.421(8) . ? Cl4 O41 1.421(7) . ? Cl4 O43 1.435(8) . ? Cl4 O44 1.436(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 N21A Hg1 N11A 70.9(3) . . ? N21A Hg1 Hg2 158.43(19) . . ? N11A Hg1 Hg2 130.7(2) . . ? N51A Hg2 N41A 70.8(3) . . ? N51A Hg2 Hg1 143.5(2) . . ? N41A Hg2 Hg1 137.3(2) . . ? N51A Hg2 O23 74.5(4) . . ? N41A Hg2 O23 84.2(5) . . ? Hg1 Hg2 O23 122.4(3) . . ? N11B Hg3 N21B 71.1(3) . . ? N11B Hg3 Hg4 148.9(2) . . ? N21B Hg3 Hg4 138.6(2) . . ? N41B Hg4 N51B 70.9(3) . . ? N41B Hg4 Hg3 150.7(2) . . ? N51B Hg4 Hg3 137.79(19) . . ? C16A N11A C12A 118.3(8) . . ? C16A N11A Hg1 126.4(7) . . ? C12A N11A Hg1 115.2(6) . . ? N11A C12A C13A 122.1(9) . . ? N11A C12A C25A 116.7(8) . . ? C13A C12A C25A 121.1(9) . . ? C14A C13A C12A 118.6(9) . . ? C15A C14A C13A 119.4(10) . . ? C14A C15A C16A 118.5(10) . . ? N11A C16A C15A 123.1(10) . . ? C25A N21A N22A 105.4(8) . . ? C25A N21A Hg1 118.4(6) . . ? N22A N21A Hg1 134.4(6) . . ? C23A N22A N21A 111.4(8) . . ? C23A N22A C31A 126.5(8) . . ? N21A N22A C31A 121.6(8) . . ? N22A C23A C24A 107.3(9) . . ? C25A C24A C23A 105.8(9) . . ? N21A C25A C24A 110.1(9) . . ? N21A C25A C12A 118.1(9) . . ? C24A C25A C12A 131.9(9) . . ? N22A C31A C32A 115.4(8) . . ? C33A C32A C37A 118.6(9) . . ? C33A C32A C31A 123.4(9) . . ? C37A C32A C31A 118.0(9) . . ? C34A C33A C32A 120.3(9) . . ? C33A C34A C35A 120.9(9) . . ? C36A C35A C34A 119.2(9) . . ? C36A C35A C38A 119.0(9) . . ? C34A C35A C38A 121.6(9) . . ? C35A C36A C37A 120.2(10) . . ? C36A C37A C32A 120.7(9) . . ? N42A C38A C35A 114.2(8) . . ? C45A N41A N42A 105.2(8) . . ? C45A N41A Hg2 113.5(6) . . ? N42A N41A Hg2 137.7(6) . . ? N41A N42A C43A 110.6(8) . . ? N41A N42A C38A 122.7(8) . . ? C43A N42A C38A 125.0(8) . . ? C44A C43A N42A 108.1(9) . . ? C43A C44A C45A 105.0(9) . . ? N41A C45A C44A 111.1(10) . . ? N41A C45A C52A 119.0(8) . . ? C44A C45A C52A 129.9(9) . . ? C56A N51A C52A 120.4(9) . . ? C56A N51A Hg2 122.9(7) . . ? C52A N51A Hg2 116.0(6) . . ? N51A C52A C53A 120.1(9) . . ? N51A C52A C45A 117.5(8) . . ? C53A C52A C45A 122.4(9) . . ? C52A C53A C54A 119.5(9) . . ? C55A C54A C53A 119.1(10) . . ? C54A C55A C56A 119.6(10) . . ? N51A C56A C55A 121.3(9) . . ? C12B N11B C16B 120.9(9) . . ? C12B N11B Hg3 118.3(7) . . ? C16B N11B Hg3 120.8(7) . . ? N11B C12B C13B 119.8(10) . . ? N11B C12B C25B 118.1(9) . . ? C13B C12B C25B 122.1(9) . . ? C14B C13B C12B 118.6(10) . . ? C15B C14B C13B 120.5(11) . . ? C14B C15B C16B 119.0(11) . . ? N11B C16B C15B 121.3(10) . . ? C25B N21B N22B 104.6(8) . . ? C25B N21B Hg3 112.2(6) . . ? N22B N21B Hg3 137.3(7) . . ? C23B N22B N21B 112.2(10) . . ? C23B N22B C31B 127.1(9) . . ? N21B N22B C31B 120.3(9) . . ? N22B C23B C24B 106.1(10) . . ? C23B C24B C25B 107.5(11) . . ? N21B C25B C24B 109.6(10) . . ? N21B C25B C12B 118.1(9) . . ? C24B C25B C12B 132.1(11) . . ? N22B C31B C32B 114.8(8) . . ? C37B C32B C33B 118.2(10) . . ? C37B C32B C31B 121.2(10) . . ? C33B C32B C31B 120.6(10) . . ? C34B C33B C32B 119.7(11) . . ? C33B C34B C35B 120.6(11) . . ? C36B C35B C34B 120.1(10) . . ? C36B C35B C38B 123.3(10) . . ? C34B C35B C38B 116.6(10) . . ? C35B C36B C37B 119.8(11) . . ? C36B C37B C32B 121.4(10) . . ? N42B C38B C35B 113.0(8) . . ? N42B N41B C45B 106.5(8) . . ? N42B N41B Hg4 135.6(6) . . ? C45B N41B Hg4 117.4(6) . . ? N41B N42B C43B 111.1(8) . . ? N41B N42B C38B 122.2(8) . . ? C43B N42B C38B 126.0(8) . . ? C44B C43B N42B 106.8(9) . . ? C43B C44B C45B 105.4(9) . . ? N41B C45B C44B 110.2(8) . . ? N41B C45B C52B 118.9(8) . . ? C44B C45B C52B 130.9(9) . . ? C52B N51B C56B 117.6(8) . . ? C52B N51B Hg4 117.9(6) . . ? C56B N51B Hg4 124.5(6) . . ? N51B C52B C53B 123.2(9) . . ? N51B C52B C45B 114.8(8) . . ? C53B C52B C45B 121.9(9) . . ? C54B C53B C52B 118.6(10) . . ? C53B C54B C55B 118.5(10) . . ? C56B C55B C54B 119.3(9) . . ? N51B C56B C55B 122.7(9) . . ? O12 Cl1 O14 110.6(6) . . ? O12 Cl1 O13 109.6(5) . . ? O14 Cl1 O13 110.3(5) . . ? O12 Cl1 O11 109.2(5) . . ? O14 Cl1 O11 108.3(6) . . ? O13 Cl1 O11 108.8(5) . . ? O23 Cl2 O22 112.3(8) . . ? O23 Cl2 O24 112.3(8) . . ? O22 Cl2 O24 111.1(9) . . ? O23 Cl2 O21 108.3(8) . . ? O22 Cl2 O21 106.4(8) . . ? O24 Cl2 O21 106.0(8) . . ? Cl2 O23 Hg2 136.0(10) . . ? O31 Cl3 O34 110.2(5) . . ? O31 Cl3 O33 108.7(5) . . ? O34 Cl3 O33 110.1(6) . . ? O31 Cl3 O32 109.1(4) . . ? O34 Cl3 O32 109.8(5) . . ? O33 Cl3 O32 108.9(5) . . ? O42 Cl4 O41 107.8(5) . . ? O42 Cl4 O43 109.4(5) . . ? O41 Cl4 O43 110.5(5) . . ? O42 Cl4 O44 109.6(5) . . ? O41 Cl4 O44 109.6(5) . . ? O43 Cl4 O44 110.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21A Hg1 Hg2 N51A -176.0(6) . . . . ? N11A Hg1 Hg2 N51A 4.7(4) . . . . ? N21A Hg1 Hg2 N41A -45.7(6) . . . . ? N11A Hg1 Hg2 N41A 135.0(4) . . . . ? N21A Hg1 Hg2 O23 75.0(7) . . . . ? N11A Hg1 Hg2 O23 -104.4(6) . . . . ? N11B Hg3 Hg4 N41B -139.0(6) . . . . ? N21B Hg3 Hg4 N41B 61.9(5) . . . . ? N11B Hg3 Hg4 N51B 27.0(5) . . . . ? N21B Hg3 Hg4 N51B -132.1(4) . . . . ? N21A Hg1 N11A C16A -179.7(9) . . . . ? Hg2 Hg1 N11A C16A 0.0(10) . . . . ? N21A Hg1 N11A C12A 4.9(6) . . . . ? Hg2 Hg1 N11A C12A -175.4(5) . . . . ? C16A N11A C12A C13A 1.6(14) . . . . ? Hg1 N11A C12A C13A 177.4(7) . . . . ? C16A N11A C12A C25A -177.6(8) . . . . ? Hg1 N11A C12A C25A -1.8(11) . . . . ? N11A C12A C13A C14A -1.4(15) . . . . ? C25A C12A C13A C14A 177.8(9) . . . . ? C12A C13A C14A C15A 0.6(16) . . . . ? C13A C14A C15A C16A -0.1(16) . . . . ? C12A N11A C16A C15A -1.0(15) . . . . ? Hg1 N11A C16A C15A -176.3(8) . . . . ? C14A C15A C16A N11A 0.3(16) . . . . ? N11A Hg1 N21A C25A -7.8(6) . . . . ? Hg2 Hg1 N21A C25A 172.8(5) . . . . ? N11A Hg1 N21A N22A -170.2(9) . . . . ? Hg2 Hg1 N21A N22A 10.4(12) . . . . ? C25A N21A N22A C23A 0.8(10) . . . . ? Hg1 N21A N22A C23A 164.7(7) . . . . ? C25A N21A N22A C31A 172.5(8) . . . . ? Hg1 N21A N22A C31A -23.6(13) . . . . ? N21A N22A C23A C24A 0.4(11) . . . . ? C31A N22A C23A C24A -170.8(9) . . . . ? N22A C23A C24A C25A -1.4(12) . . . . ? N22A N21A C25A C24A -1.7(10) . . . . ? Hg1 N21A C25A C24A -168.7(7) . . . . ? N22A N21A C25A C12A 177.0(8) . . . . ? Hg1 N21A C25A C12A 10.0(11) . . . . ? C23A C24A C25A N21A 1.9(12) . . . . ? C23A C24A C25A C12A -176.6(10) . . . . ? N11A C12A C25A N21A -5.2(13) . . . . ? C13A C12A C25A N21A 175.7(9) . . . . ? N11A C12A C25A C24A 173.2(10) . . . . ? C13A C12A C25A C24A -6.0(16) . . . . ? C23A N22A C31A C32A -149.4(10) . . . . ? N21A N22A C31A C32A 40.3(13) . . . . ? N22A C31A C32A C33A 56.4(13) . . . . ? N22A C31A C32A C37A -126.1(10) . . . . ? C37A C32A C33A C34A -0.3(14) . . . . ? C31A C32A C33A C34A 177.1(9) . . . . ? C32A C33A C34A C35A -1.1(14) . . . . ? C33A C34A C35A C36A 0.6(15) . . . . ? C33A C34A C35A C38A -173.3(9) . . . . ? C34A C35A C36A C37A 1.3(15) . . . . ? C38A C35A C36A C37A 175.3(9) . . . . ? C35A C36A C37A C32A -2.8(15) . . . . ? C33A C32A C37A C36A 2.3(15) . . . . ? C31A C32A C37A C36A -175.4(9) . . . . ? C36A C35A C38A N42A 112.6(11) . . . . ? C34A C35A C38A N42A -73.5(13) . . . . ? N51A Hg2 N41A C45A 15.8(6) . . . . ? Hg1 Hg2 N41A C45A -135.5(6) . . . . ? O23 Hg2 N41A C45A 91.4(7) . . . . ? N51A Hg2 N41A N42A 170.2(10) . . . . ? Hg1 Hg2 N41A N42A 18.9(11) . . . . ? O23 Hg2 N41A N42A -114.2(10) . . . . ? C45A N41A N42A C43A -1.2(11) . . . . ? Hg2 N41A N42A C43A -157.0(8) . . . . ? C45A N41A N42A C38A -166.8(8) . . . . ? Hg2 N41A N42A C38A 37.5(14) . . . . ? C35A C38A N42A N41A -41.1(14) . . . . ? C35A C38A N42A C43A 155.4(10) . . . . ? N41A N42A C43A C44A 1.1(12) . . . . ? C38A N42A C43A C44A 166.2(9) . . . . ? N42A C43A C44A C45A -0.5(12) . . . . ? N42A N41A C45A C44A 0.9(11) . . . . ? Hg2 N41A C45A C44A 163.4(7) . . . . ? N42A N41A C45A C52A -178.7(8) . . . . ? Hg2 N41A C45A C52A -16.2(11) . . . . ? C43A C44A C45A N41A -0.3(11) . . . . ? C43A C44A C45A C52A 179.3(10) . . . . ? N41A Hg2 N51A C56A 175.2(8) . . . . ? Hg1 Hg2 N51A C56A -38.0(9) . . . . ? O23 Hg2 N51A C56A 86.1(9) . . . . ? N41A Hg2 N51A C52A -14.1(6) . . . . ? Hg1 Hg2 N51A C52A 132.6(6) . . . . ? O23 Hg2 N51A C52A -103.3(8) . . . . ? C56A N51A C52A C53A 0.3(14) . . . . ? Hg2 N51A C52A C53A -170.6(7) . . . . ? C56A N51A C52A C45A -177.7(9) . . . . ? Hg2 N51A C52A C45A 11.4(11) . . . . ? N41A C45A C52A N51A 3.8(13) . . . . ? C44A C45A C52A N51A -175.8(9) . . . . ? N41A C45A C52A C53A -174.1(9) . . . . ? C44A C45A C52A C53A 6.3(16) . . . . ? N51A C52A C53A C54A 0.9(15) . . . . ? C45A C52A C53A C54A 178.7(9) . . . . ? C52A C53A C54A C55A -2.4(16) . . . . ? C53A C54A C55A C56A 2.8(16) . . . . ? C52A N51A C56A C55A 0.1(15) . . . . ? Hg2 N51A C56A C55A 170.4(8) . . . . ? C54A C55A C56A N51A -1.7(16) . . . . ? N21B Hg3 N11B C12B -3.9(7) . . . . ? Hg4 Hg3 N11B C12B -169.5(5) . . . . ? N21B Hg3 N11B C16B 176.6(8) . . . . ? Hg4 Hg3 N11B C16B 11.0(10) . . . . ? C16B N11B C12B C13B -1.8(15) . . . . ? Hg3 N11B C12B C13B 178.6(7) . . . . ? C16B N11B C12B C25B 176.2(9) . . . . ? Hg3 N11B C12B C25B -3.4(12) . . . . ? N11B C12B C13B C14B 0.5(16) . . . . ? C25B C12B C13B C14B -177.4(10) . . . . ? C12B C13B C14B C15B 0.1(17) . . . . ? C13B C14B C15B C16B 0.4(17) . . . . ? C12B N11B C16B C15B 2.5(16) . . . . ? Hg3 N11B C16B C15B -178.0(8) . . . . ? C14B C15B C16B N11B -1.7(17) . . . . ? N11B Hg3 N21B C25B 11.0(6) . . . . ? Hg4 Hg3 N21B C25B 179.7(5) . . . . ? N11B Hg3 N21B N22B 158.7(11) . . . . ? Hg4 Hg3 N21B N22B -32.6(11) . . . . ? C25B N21B N22B C23B -0.5(11) . . . . ? Hg3 N21B N22B C23B -149.7(9) . . . . ? C25B N21B N22B C31B -172.9(8) . . . . ? Hg3 N21B N22B C31B 37.8(14) . . . . ? N21B N22B C23B C24B 0.4(13) . . . . ? C31B N22B C23B C24B 172.2(10) . . . . ? N22B C23B C24B C25B -0.1(13) . . . . ? N22B N21B C25B C24B 0.4(11) . . . . ? Hg3 N21B C25B C24B 158.4(7) . . . . ? N22B N21B C25B C12B -174.9(8) . . . . ? Hg3 N21B C25B C12B -16.9(11) . . . . ? C23B C24B C25B N21B -0.2(13) . . . . ? C23B C24B C25B C12B 174.2(11) . . . . ? N11B C12B C25B N21B 14.4(14) . . . . ? C13B C12B C25B N21B -167.7(9) . . . . ? N11B C12B C25B C24B -159.6(11) . . . . ? C13B C12B C25B C24B 18.3(18) . . . . ? C23B N22B C31B C32B 137.7(11) . . . . ? N21B N22B C31B C32B -51.1(12) . . . . ? N22B C31B C32B C37B 131.0(10) . . . . ? N22B C31B C32B C33B -48.2(12) . . . . ? C37B C32B C33B C34B -1.4(14) . . . . ? C31B C32B C33B C34B 177.8(9) . . . . ? C32B C33B C34B C35B 2.4(15) . . . . ? C33B C34B C35B C36B -0.5(16) . . . . ? C33B C34B C35B C38B 178.8(9) . . . . ? C34B C35B C36B C37B -2.5(15) . . . . ? C38B C35B C36B C37B 178.3(10) . . . . ? C35B C36B C37B C32B 3.5(16) . . . . ? C33B C32B C37B C36B -1.5(15) . . . . ? C31B C32B C37B C36B 179.2(9) . . . . ? C36B C35B C38B N42B -41.8(15) . . . . ? C34B C35B C38B N42B 138.9(10) . . . . ? N51B Hg4 N41B N42B 172.1(10) . . . . ? Hg3 Hg4 N41B N42B -17.8(12) . . . . ? N51B Hg4 N41B C45B 2.2(7) . . . . ? Hg3 Hg4 N41B C45B 172.3(5) . . . . ? C45B N41B N42B C43B -1.5(11) . . . . ? Hg4 N41B N42B C43B -172.2(7) . . . . ? C45B N41B N42B C38B -172.9(9) . . . . ? Hg4 N41B N42B C38B 16.4(15) . . . . ? C35B C38B N42B N41B -44.0(14) . . . . ? C35B C38B N42B C43B 145.8(10) . . . . ? N41B N42B C43B C44B 0.7(12) . . . . ? C38B N42B C43B C44B 171.8(10) . . . . ? N42B C43B C44B C45B 0.3(11) . . . . ? N42B N41B C45B C44B 1.6(11) . . . . ? Hg4 N41B C45B C44B 174.3(6) . . . . ? N42B N41B C45B C52B -176.5(8) . . . . ? Hg4 N41B C45B C52B -3.8(12) . . . . ? C43B C44B C45B N41B -1.2(12) . . . . ? C43B C44B C45B C52B 176.6(10) . . . . ? N41B Hg4 N51B C52B -0.3(6) . . . . ? Hg3 Hg4 N51B C52B -173.1(5) . . . . ? N41B Hg4 N51B C56B 178.7(8) . . . . ? Hg3 Hg4 N51B C56B 5.9(9) . . . . ? C56B N51B C52B C53B -2.2(14) . . . . ? Hg4 N51B C52B C53B 176.8(7) . . . . ? C56B N51B C52B C45B 179.5(8) . . . . ? Hg4 N51B C52B C45B -1.4(10) . . . . ? N41B C45B C52B N51B 3.5(13) . . . . ? C44B C45B C52B N51B -174.2(10) . . . . ? N41B C45B C52B C53B -174.8(9) . . . . ? C44B C45B C52B C53B 7.5(16) . . . . ? N51B C52B C53B C54B 2.2(15) . . . . ? C45B C52B C53B C54B -179.7(9) . . . . ? C52B C53B C54B C55B -2.0(15) . . . . ? C53B C54B C55B C56B 2.1(15) . . . . ? C52B N51B C56B C55B 2.3(14) . . . . ? Hg4 N51B C56B C55B -176.7(7) . . . . ? C54B C55B C56B N51B -2.2(15) . . . . ? O22 Cl2 O23 Hg2 136.4(18) . . . . ? O24 Cl2 O23 Hg2 10(2) . . . . ? O21 Cl2 O23 Hg2 -106.4(19) . . . . ? N51A Hg2 O23 Cl2 -177.5(18) . . . . ? N41A Hg2 O23 Cl2 110.9(17) . . . . ? Hg1 Hg2 O23 Cl2 -33.1(19) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.845 _refine_diff_density_min -2.065 _refine_diff_density_rms 0.282 #===END data_imw325m _database_code_depnum_ccdc_archive 'CCDC 609501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C180 H144 Hg4 N36, 8(Cl O4), 3(C H3 N O2)' _chemical_formula_sum 'C183 H153 Cl8 Hg4 N39 O38' _chemical_formula_weight 4592.40 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.823(11) _cell_length_b 19.008(10) _cell_length_c 30.656(17) _cell_angle_alpha 86.704(9) _cell_angle_beta 89.145(9) _cell_angle_gamma 66.948(9) _cell_volume 10075(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 973 _cell_measurement_theta_min 4.950 _cell_measurement_theta_max 53.817 _exptl_crystal_description PLATE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 3.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4995 _exptl_absorpt_correction_T_max 0.7825 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 83866 _diffrn_reflns_av_R_equivalents 0.1431 _diffrn_reflns_av_sigmaI/netI 0.2799 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 35266 _reflns_number_gt 12585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 35266 _refine_ls_number_parameters 1294 _refine_ls_number_restraints 3513 _refine_ls_R_factor_all 0.2199 _refine_ls_R_factor_gt 0.1184 _refine_ls_wR_factor_ref 0.3528 _refine_ls_wR_factor_gt 0.2981 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.785 _refine_ls_shift/su_max 0.004 _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 0.16514(5) 0.11557(5) 0.02853(3) 0.0654(3) Uani 1 1 d U . . Hg2 Hg 0.25739(5) 0.42505(4) 0.34046(2) 0.0565(2) Uani 1 1 d U . . Hg3 Hg -0.36553(5) 0.57187(5) 0.21077(2) 0.0651(3) Uani 1 1 d U . . Hg4 Hg -0.02225(6) -0.05804(5) 0.37226(2) 0.0755(3) Uani 1 1 d U . . N11A N 0.1819(10) -0.0061(8) 0.0040(4) 0.081(5) Uiso 1 1 d DU . . C12A C 0.2037(13) -0.0648(9) 0.0350(4) 0.080(6) Uiso 1 1 d DU . . C13A C 0.2201(15) -0.1390(10) 0.0224(6) 0.107(8) Uiso 1 1 d DU . . H13A H 0.2347 -0.1806 0.0437 0.128 Uiso 1 1 calc R . . C14A C 0.2150(16) -0.1516(12) -0.0208(6) 0.115(9) Uiso 1 1 d DU . . H14A H 0.2268 -0.2022 -0.0293 0.137 Uiso 1 1 calc R . . C15A C 0.1931(15) -0.0923(12) -0.0518(6) 0.104(8) Uiso 1 1 d DU . . H15A H 0.1896 -0.1015 -0.0816 0.125 Uiso 1 1 calc R . . C16A C 0.1760(15) -0.0177(11) -0.0390(5) 0.101(8) Uiso 1 1 d DU . . H16A H 0.1604 0.0242 -0.0601 0.121 Uiso 1 1 calc R . . N21A N 0.2035(8) 0.0245(7) 0.0868(4) 0.054(4) Uiso 1 1 d DU . . N22A N 0.2204(10) 0.0242(8) 0.1298(4) 0.072(5) Uiso 1 1 d DU . . C23A C 0.2400(14) -0.0484(10) 0.1495(5) 0.092(7) Uiso 1 1 d DU . . H23A H 0.2554 -0.0642 0.1790 0.111 Uiso 1 1 calc R . . C24A C 0.2323(13) -0.0932(10) 0.1173(5) 0.089(7) Uiso 1 1 d DU . . H24A H 0.2385 -0.1452 0.1212 0.107 Uiso 1 1 calc R . . C25A C 0.2143(12) -0.0491(9) 0.0784(4) 0.071(6) Uiso 1 1 d DU . . C31A C 0.2203(10) 0.0927(11) 0.1489(6) 0.068(5) Uiso 1 1 d DU . . H31A H 0.2040 0.0936 0.1798 0.082 Uiso 1 1 calc R . . H31B H 0.1832 0.1389 0.1329 0.082 Uiso 1 1 calc R . . C32A C 0.3014(9) 0.0929(9) 0.1462(6) 0.059(5) Uiso 1 1 d DU . . C33A C 0.3131(9) 0.1487(9) 0.1689(5) 0.058(5) Uiso 1 1 d DU . . H33A H 0.2712 0.1852 0.1836 0.070 Uiso 1 1 calc R . . C34A C 0.3850(8) 0.1516(9) 0.1701(5) 0.060(5) Uiso 1 1 d DU . . C35A C 0.4432(9) 0.1036(10) 0.1443(6) 0.065(5) Uiso 1 1 d DU . . H35A H 0.4915 0.1085 0.1427 0.077 Uiso 1 1 calc R . . C36A C 0.4315(11) 0.0480(12) 0.1206(7) 0.096(7) Uiso 1 1 d DU . . H36A H 0.4716 0.0151 0.1032 0.115 Uiso 1 1 calc R . . C37A C 0.3601(10) 0.0418(11) 0.1228(7) 0.086(7) Uiso 1 1 d DU . . H37A H 0.3521 0.0026 0.1082 0.103 Uiso 1 1 calc R . . C41A C 0.3047(10) 0.4215(9) 0.2151(6) 0.059(5) Uiso 1 1 d DU . . H41A H 0.2977 0.4401 0.1840 0.071 Uiso 1 1 calc R . . H41B H 0.2541 0.4246 0.2264 0.071 Uiso 1 1 calc R . . C42A C 0.3630(9) 0.3370(8) 0.2185(5) 0.053(4) Uiso 1 1 d DU . . C43A C 0.3474(9) 0.2848(8) 0.1945(5) 0.058(5) Uiso 1 1 d DU . . H43A H 0.3013 0.3008 0.1776 0.070 Uiso 1 1 calc R . . C44A C 0.3992(9) 0.2096(8) 0.1954(5) 0.057(5) Uiso 1 1 d DU . . C45A C 0.4640(9) 0.1854(9) 0.2219(5) 0.061(5) Uiso 1 1 d DU . . H45A H 0.4991 0.1334 0.2223 0.073 Uiso 1 1 calc R . . C46A C 0.4787(10) 0.2356(9) 0.2479(6) 0.069(5) Uiso 1 1 d DU . . H46A H 0.5224 0.2183 0.2669 0.083 Uiso 1 1 calc R . . C47A C 0.4277(9) 0.3117(9) 0.2455(6) 0.065(5) Uiso 1 1 d DU . . H47A H 0.4373 0.3473 0.2626 0.078 Uiso 1 1 calc R . . N51A N 0.3175(8) 0.4767(8) 0.2830(3) 0.052(4) Uiso 1 1 d DU . . N52A N 0.3303(8) 0.4700(8) 0.2392(4) 0.055(4) Uiso 1 1 d DU . . C53A C 0.3740(11) 0.5104(11) 0.2243(5) 0.077(6) Uiso 1 1 d DU . . H53A H 0.3903 0.5142 0.1951 0.092 Uiso 1 1 calc R . . C54A C 0.3893(12) 0.5437(11) 0.2593(5) 0.078(6) Uiso 1 1 d DU . . H54A H 0.4174 0.5757 0.2589 0.094 Uiso 1 1 calc R . . C55A C 0.3558(10) 0.5218(10) 0.2960(4) 0.060(5) Uiso 1 1 d DU . . N61A N 0.3185(9) 0.5076(9) 0.3688(4) 0.065(4) Uiso 1 1 d DU . . C62A C 0.3554(11) 0.5390(11) 0.3401(4) 0.069(5) Uiso 1 1 d DU . . C63A C 0.3928(12) 0.5846(12) 0.3541(6) 0.084(6) Uiso 1 1 d DU . . H63A H 0.4167 0.6081 0.3340 0.101 Uiso 1 1 calc R . . C64A C 0.3935(15) 0.5940(14) 0.3980(6) 0.113(9) Uiso 1 1 d DU . . H64A H 0.4172 0.6259 0.4084 0.136 Uiso 1 1 calc R . . C65A C 0.3607(16) 0.5583(15) 0.4276(6) 0.122(9) Uiso 1 1 d DU . . H65A H 0.3654 0.5621 0.4581 0.147 Uiso 1 1 calc R . . C66A C 0.3202(11) 0.5165(11) 0.4120(5) 0.067(5) Uiso 1 1 d DU . . H66A H 0.2942 0.4946 0.4318 0.080 Uiso 1 1 calc R . . N11B N 0.2891(9) 0.1023(9) 0.0065(6) 0.090(6) Uiso 1 1 d DU . . C12B C 0.3172(9) 0.1537(10) 0.0190(6) 0.081(6) Uiso 1 1 d DU . . C13B C 0.3921(11) 0.1461(13) 0.0078(8) 0.111(8) Uiso 1 1 d DU . . H13B H 0.4138 0.1791 0.0188 0.134 Uiso 1 1 calc R . . C14B C 0.4333(12) 0.0900(13) -0.0195(8) 0.106(8) Uiso 1 1 d DU . . H14B H 0.4826 0.0868 -0.0291 0.128 Uiso 1 1 calc R . . C15B C 0.4056(12) 0.0386(13) -0.0332(8) 0.106(8) Uiso 1 1 d DU . . H15B H 0.4343 0.0008 -0.0527 0.127 Uiso 1 1 calc R . . C16B C 0.3330(11) 0.0431(11) -0.0176(7) 0.095(7) Uiso 1 1 d DU . . H16B H 0.3148 0.0046 -0.0240 0.114 Uiso 1 1 calc R . . N21B N 0.1932(8) 0.2215(8) 0.0530(5) 0.065(4) Uiso 1 1 d DU . . N22B N 0.1610(8) 0.2859(8) 0.0753(5) 0.064(4) Uiso 1 1 d DU . . C23B C 0.2168(11) 0.3149(12) 0.0831(8) 0.110(8) Uiso 1 1 d DU . . H23B H 0.2099 0.3579 0.0996 0.132 Uiso 1 1 calc R . . C24B C 0.2834(10) 0.2705(11) 0.0627(7) 0.094(7) Uiso 1 1 d DU . . H24B H 0.3304 0.2782 0.0615 0.113 Uiso 1 1 calc R . . C25B C 0.2692(9) 0.2116(10) 0.0441(7) 0.083(6) Uiso 1 1 d DU . . C31B C 0.0834(10) 0.3111(10) 0.0858(5) 0.062(5) Uiso 1 1 d DU . . H31C H 0.0748 0.3391 0.1129 0.074 Uiso 1 1 calc R . . H31D H 0.0703 0.2659 0.0919 0.074 Uiso 1 1 calc R . . C32B C 0.0284(8) 0.3635(10) 0.0502(5) 0.060(5) Uiso 1 1 d DU . . C33B C -0.0479(8) 0.4062(9) 0.0605(5) 0.061(5) Uiso 1 1 d DU . . H33B H -0.0648 0.4024 0.0895 0.073 Uiso 1 1 calc R . . C34B C -0.1002(8) 0.4543(9) 0.0296(5) 0.059(5) Uiso 1 1 d DU . . C35B C -0.0728(9) 0.4588(10) -0.0126(5) 0.062(5) Uiso 1 1 d DU . . H35B H -0.1065 0.4927 -0.0343 0.074 Uiso 1 1 calc R . . C36B C 0.0035(9) 0.4143(10) -0.0236(5) 0.068(5) Uiso 1 1 d DU . . H36B H 0.0204 0.4162 -0.0528 0.081 Uiso 1 1 calc R . . C37B C 0.0549(9) 0.3674(9) 0.0084(4) 0.056(5) Uiso 1 1 d DU . . H37B H 0.1073 0.3385 0.0014 0.068 Uiso 1 1 calc R . . C41B C -0.3415(12) 0.4632(12) 0.1037(7) 0.080(6) Uiso 1 1 d DU . . H41C H -0.3402 0.4182 0.0885 0.096 Uiso 1 1 calc R . . H41D H -0.3133 0.4444 0.1318 0.096 Uiso 1 1 calc R . . C42B C -0.2997(9) 0.5052(9) 0.0754(6) 0.066(5) Uiso 1 1 d DU . . C43B C -0.2228(9) 0.4647(10) 0.0665(6) 0.072(6) Uiso 1 1 d DU . . H43B H -0.1975 0.4136 0.0783 0.086 Uiso 1 1 calc R . . C44B C -0.1822(8) 0.4981(9) 0.0407(6) 0.065(5) Uiso 1 1 d DU . . C45B C -0.2192(9) 0.5739(9) 0.0246(6) 0.073(6) Uiso 1 1 d DU . . H45B H -0.1913 0.5974 0.0074 0.087 Uiso 1 1 calc R . . C46B C -0.2970(10) 0.6156(10) 0.0335(7) 0.085(6) Uiso 1 1 d DU . . H46B H -0.3223 0.6670 0.0222 0.102 Uiso 1 1 calc R . . C47B C -0.3364(10) 0.5806(9) 0.0589(6) 0.073(6) Uiso 1 1 d DU . . H47B H -0.3893 0.6084 0.0652 0.088 Uiso 1 1 calc R . . N51B N -0.4358(7) 0.5576(8) 0.1461(4) 0.058(4) Uiso 1 1 d DU . . N52B N -0.4172(9) 0.5095(9) 0.1120(5) 0.075(5) Uiso 1 1 d DU . . C53B C -0.4834(11) 0.5282(13) 0.0868(6) 0.110(8) Uiso 1 1 d DU . . H53B H -0.4865 0.5059 0.0603 0.132 Uiso 1 1 calc R . . C54B C -0.5440(10) 0.5844(12) 0.1063(6) 0.092(7) Uiso 1 1 d DU . . H54B H -0.5956 0.6085 0.0958 0.110 Uiso 1 1 calc R . . C55B C -0.5143(9) 0.5989(10) 0.1447(5) 0.075(6) Uiso 1 1 d DU . . N61B N -0.5068(8) 0.6566(9) 0.2100(4) 0.072(5) Uiso 1 1 d DU . . C62B C -0.5508(9) 0.6532(11) 0.1759(6) 0.085(6) Uiso 1 1 d DU . . C63B C -0.6277(9) 0.7022(11) 0.1725(6) 0.085(7) Uiso 1 1 d DU . . H63B H -0.6573 0.7017 0.1478 0.102 Uiso 1 1 calc R . . C64B C -0.6614(11) 0.7514(13) 0.2048(7) 0.108(8) Uiso 1 1 d DU . . H64B H -0.7154 0.7812 0.2040 0.130 Uiso 1 1 calc R . . C65B C -0.6169(11) 0.7574(12) 0.2382(7) 0.100(8) Uiso 1 1 d DU . . H65B H -0.6385 0.7952 0.2589 0.120 Uiso 1 1 calc R . . C66B C -0.5385(11) 0.7067(11) 0.2415(6) 0.088(7) Uiso 1 1 d DU . . H66B H -0.5081 0.7078 0.2657 0.106 Uiso 1 1 calc R . . N11C N 0.1133(8) 0.1751(8) -0.0447(4) 0.107(7) Uiso 1 1 d GDU . . C12C C 0.0370(8) 0.2274(9) -0.0449(4) 0.110(8) Uiso 1 1 d GDU . . C13C C 0.0049(8) 0.2723(8) -0.0826(5) 0.088(7) Uiso 1 1 d GDU . . H13C H -0.0473 0.3081 -0.0827 0.105 Uiso 1 1 calc R . . C14C C 0.0490(11) 0.2648(10) -0.1201(4) 0.132(10) Uiso 1 1 d GDU . . H14C H 0.0270 0.2955 -0.1459 0.158 Uiso 1 1 calc R . . C15C C 0.1252(11) 0.2124(11) -0.1200(4) 0.143(11) Uiso 1 1 d GDU . . H15C H 0.1554 0.2073 -0.1456 0.171 Uiso 1 1 calc R . . C16C C 0.1574(8) 0.1676(9) -0.0823(6) 0.125(10) Uiso 1 1 d GDU . . H16C H 0.2095 0.1318 -0.0822 0.150 Uiso 1 1 calc R . . N21C N 0.0331(9) 0.1813(10) 0.0305(5) 0.096(6) Uiso 1 1 d DU . . N22C N -0.0224(10) 0.1909(11) 0.0612(5) 0.100(6) Uiso 1 1 d DU . . C23C C -0.0922(10) 0.2400(11) 0.0444(6) 0.080(6) Uiso 1 1 d DU . . H23C H -0.1399 0.2570 0.0595 0.096 Uiso 1 1 calc R . . C24C C -0.0816(10) 0.2608(15) 0.0013(6) 0.127(10) Uiso 1 1 d DU . . H24C H -0.1202 0.2941 -0.0184 0.152 Uiso 1 1 calc R . . C25C C -0.0027(10) 0.2229(12) -0.0071(5) 0.090(7) Uiso 1 1 d DU . . C31C C -0.0040(12) 0.1506(9) 0.0971(6) 0.067(5) Uiso 1 1 d DU . . H31E H -0.0437 0.1766 0.1188 0.080 Uiso 1 1 calc R . . H31F H 0.0452 0.1516 0.1073 0.080 Uiso 1 1 calc R . . C32C C 0.0057(11) 0.0662(7) 0.0984(5) 0.105(8) Uiso 1 1 d GDU . . C33C C 0.0130(11) 0.0245(10) 0.1380(4) 0.125(10) Uiso 1 1 d GDU . . H33C H 0.0123 0.0479 0.1646 0.150 Uiso 1 1 calc R . . C34C C 0.0213(12) -0.0516(9) 0.1387(5) 0.126(9) Uiso 1 1 d GDU . . C35C C 0.0223(12) -0.0859(8) 0.0997(6) 0.128(10) Uiso 1 1 d GDU . . H35C H 0.0280 -0.1378 0.1001 0.154 Uiso 1 1 calc R . . C36C C 0.0150(11) -0.0442(10) 0.0601(5) 0.132(10) Uiso 1 1 d GDU . . H36C H 0.0157 -0.0676 0.0334 0.159 Uiso 1 1 calc R . . C37C C 0.0067(11) 0.0318(10) 0.0594(4) 0.112(9) Uiso 1 1 d GDU . . H37C H 0.0017 0.0603 0.0323 0.134 Uiso 1 1 calc R . . C41C C 0.1377(16) -0.1458(18) 0.2858(9) 0.142(11) Uiso 1 1 d DU . . H41E H 0.1872 -0.1615 0.2700 0.171 Uiso 1 1 calc R . . H41F H 0.1264 -0.0940 0.2960 0.171 Uiso 1 1 calc R . . C42C C 0.0736(10) -0.1385(11) 0.2520(5) 0.127(9) Uiso 1 1 d GDU . . C43C C 0.0719(10) -0.0981(11) 0.2125(6) 0.136(10) Uiso 1 1 d GDU . . H43C H 0.1070 -0.0737 0.2076 0.163 Uiso 1 1 calc R . . C44C C 0.0188(11) -0.0932(10) 0.1803(5) 0.125(9) Uiso 1 1 d GDU . . C45C C -0.0326(10) -0.1288(11) 0.1875(5) 0.140(11) Uiso 1 1 d GDU . . H45C H -0.0689 -0.1255 0.1655 0.167 Uiso 1 1 calc R . . C46C C -0.0310(10) -0.1692(11) 0.2270(6) 0.135(10) Uiso 1 1 d GDU . . H46C H -0.0661 -0.1935 0.2320 0.162 Uiso 1 1 calc R . . C47C C 0.0221(12) -0.1740(10) 0.2593(5) 0.131(10) Uiso 1 1 d GDU . . H47C H 0.0233 -0.2016 0.2863 0.158 Uiso 1 1 calc R . . N51C N 0.0866(8) -0.1765(7) 0.3533(4) 0.081(5) Uiso 1 1 d GDU . . N52C N 0.1497(10) -0.1969(11) 0.3239(4) 0.125(8) Uiso 1 1 d GDU . . C53C C 0.2037(9) -0.2709(11) 0.3376(7) 0.181(14) Uiso 1 1 d GDU . . H53C H 0.2513 -0.2986 0.3239 0.217 Uiso 1 1 calc R . . C54C C 0.1741(10) -0.2963(8) 0.3755(7) 0.163(13) Uiso 1 1 d GDU . . H54C H 0.1985 -0.3439 0.3915 0.196 Uiso 1 1 calc R . . C55C C 0.1018(9) -0.2379(9) 0.3852(5) 0.088(7) Uiso 1 1 d GDU . . N61C N -0.0161(7) -0.1694(7) 0.4189(4) 0.047(3) Uiso 1 1 d DU . . C62C C 0.0487(9) -0.2353(9) 0.4180(5) 0.070(5) Uiso 1 1 d DU . . C63C C 0.0559(11) -0.2979(10) 0.4459(6) 0.092(7) Uiso 1 1 d DU . . H63C H 0.0993 -0.3449 0.4439 0.110 Uiso 1 1 calc R . . C64C C 0.0006(11) -0.2916(11) 0.4762(7) 0.097(7) Uiso 1 1 d DU . . H64C H 0.0070 -0.3334 0.4965 0.116 Uiso 1 1 calc R . . C65C C -0.0643(11) -0.2254(10) 0.4776(6) 0.081(6) Uiso 1 1 d DU . . H65C H -0.1038 -0.2214 0.4981 0.097 Uiso 1 1 calc R . . C66C C -0.0717(9) -0.1626(9) 0.4478(5) 0.055(5) Uiso 1 1 d DU . . H66C H -0.1160 -0.1161 0.4486 0.065 Uiso 1 1 calc R . . N11D N 0.3625(8) 0.3161(7) 0.3572(4) 0.056(4) Uiso 1 1 d DU . . C12D C 0.3645(9) 0.2483(9) 0.3418(5) 0.058(5) Uiso 1 1 d DU . . C13D C 0.4277(9) 0.1794(9) 0.3495(6) 0.062(5) Uiso 1 1 d DU . . H13D H 0.4274 0.1327 0.3402 0.074 Uiso 1 1 calc R . . C14D C 0.4916(11) 0.1812(12) 0.3713(7) 0.087(7) Uiso 1 1 d DU . . H14D H 0.5362 0.1352 0.3755 0.104 Uiso 1 1 calc R . . C15D C 0.4918(11) 0.2461(11) 0.3865(7) 0.078(6) Uiso 1 1 d DU . . H15D H 0.5356 0.2462 0.4014 0.093 Uiso 1 1 calc R . . C16D C 0.4267(11) 0.3127(11) 0.3799(7) 0.081(6) Uiso 1 1 d DU . . H16D H 0.4260 0.3582 0.3915 0.097 Uiso 1 1 calc R . . N21D N 0.2452(7) 0.3231(7) 0.3033(4) 0.046(3) Uiso 1 1 d DU . . N22D N 0.1902(8) 0.3092(8) 0.2818(4) 0.057(4) Uiso 1 1 d DU . . C23D C 0.2089(10) 0.2340(9) 0.2807(6) 0.068(5) Uiso 1 1 d DU . . H23D H 0.1797 0.2102 0.2671 0.081 Uiso 1 1 calc R . . C24D C 0.2781(10) 0.1970(9) 0.3027(6) 0.062(5) Uiso 1 1 d DU . . H24D H 0.3056 0.1433 0.3076 0.075 Uiso 1 1 calc R . . C25D C 0.2986(9) 0.2542(9) 0.3160(6) 0.060(5) Uiso 1 1 d DU . . C31D C 0.1258(9) 0.3707(9) 0.2593(5) 0.053(4) Uiso 1 1 d DU . . H31G H 0.1056 0.3491 0.2362 0.064 Uiso 1 1 calc R . . H31H H 0.1446 0.4082 0.2451 0.064 Uiso 1 1 calc R . . C32D C 0.0613(9) 0.4113(9) 0.2901(5) 0.054(4) Uiso 1 1 d DU . . C33D C 0.0004(9) 0.4773(9) 0.2734(5) 0.061(5) Uiso 1 1 d DU . . H33D H 0.0027 0.4961 0.2442 0.074 Uiso 1 1 calc R . . C34D C -0.0634(9) 0.5156(9) 0.2988(5) 0.057(5) Uiso 1 1 d DU . . C35D C -0.0659(10) 0.4884(9) 0.3403(5) 0.057(5) Uiso 1 1 d DU . . H35D H -0.1069 0.5175 0.3585 0.068 Uiso 1 1 calc R . . C36D C -0.0122(10) 0.4211(10) 0.3570(6) 0.068(5) Uiso 1 1 d DU . . H36D H -0.0185 0.4012 0.3852 0.081 Uiso 1 1 calc R . . C37D C 0.0542(10) 0.3806(10) 0.3313(5) 0.060(5) Uiso 1 1 d DU . . H37D H 0.0926 0.3336 0.3423 0.072 Uiso 1 1 calc R . . C41D C -0.3416(10) 0.7057(11) 0.2982(7) 0.075(6) Uiso 1 1 d DU . . H41G H -0.3458 0.7409 0.3217 0.090 Uiso 1 1 calc R . . H41H H -0.3783 0.7352 0.2746 0.090 Uiso 1 1 calc R . . C42D C -0.2585(9) 0.6761(9) 0.2800(6) 0.062(5) Uiso 1 1 d DU . . C43D C -0.2005(8) 0.6111(9) 0.2968(5) 0.056(5) Uiso 1 1 d DU . . H43D H -0.2110 0.5808 0.3197 0.067 Uiso 1 1 calc R . . C44D C -0.1258(8) 0.5893(8) 0.2802(5) 0.054(4) Uiso 1 1 d DU . . C45D C -0.1100(9) 0.6340(9) 0.2474(5) 0.057(5) Uiso 1 1 d DU . . H45D H -0.0600 0.6178 0.2349 0.069 Uiso 1 1 calc R . . C46D C -0.1692(10) 0.7044(11) 0.2327(6) 0.077(6) Uiso 1 1 d DU . . H46D H -0.1581 0.7390 0.2129 0.093 Uiso 1 1 calc R . . C47D C -0.2436(10) 0.7216(10) 0.2479(6) 0.071(6) Uiso 1 1 d DU . . H47D H -0.2849 0.7656 0.2359 0.085 Uiso 1 1 calc R . . N51D N -0.3691(9) 0.5935(8) 0.2872(4) 0.068(4) Uiso 1 1 d DU . . N52D N -0.3631(9) 0.6441(8) 0.3156(4) 0.062(4) Uiso 1 1 d DU . . C53D C -0.3769(12) 0.6227(10) 0.3575(5) 0.070(5) Uiso 1 1 d DU . . H53D H -0.3756 0.6483 0.3830 0.083 Uiso 1 1 calc R . . C54D C -0.3929(11) 0.5578(9) 0.3562(4) 0.062(5) Uiso 1 1 d DU . . H54D H -0.4050 0.5308 0.3802 0.075 Uiso 1 1 calc R . . C55D C -0.3875(11) 0.5400(9) 0.3121(4) 0.065(5) Uiso 1 1 d DU . . N61D N -0.3899(8) 0.4747(7) 0.2480(4) 0.055(4) Uiso 1 1 d DU . . C62D C -0.4010(11) 0.4808(8) 0.2919(4) 0.057(5) Uiso 1 1 d DU . . C63D C -0.4142(11) 0.4221(9) 0.3158(5) 0.069(5) Uiso 1 1 d DU . . H63D H -0.4139 0.4204 0.3469 0.083 Uiso 1 1 calc R . . C64D C -0.4276(11) 0.3668(9) 0.2942(5) 0.064(5) Uiso 1 1 d DU . . H64D H -0.4427 0.3308 0.3103 0.077 Uiso 1 1 calc R . . C65D C -0.4193(11) 0.3633(9) 0.2499(5) 0.060(5) Uiso 1 1 d DU . . H65D H -0.4251 0.3231 0.2353 0.072 Uiso 1 1 calc R . . C66D C -0.4023(11) 0.4201(9) 0.2262(5) 0.066(5) Uiso 1 1 d DU . . H66D H -0.3994 0.4205 0.1952 0.079 Uiso 1 1 calc R . . N11E N -0.3312(7) 0.6520(7) 0.1700(4) 0.052(4) Uiso 1 1 d DU . . C12E C -0.2563(10) 0.6304(9) 0.1561(6) 0.076(6) Uiso 1 1 d DU . . C13E C -0.2376(11) 0.6787(10) 0.1252(6) 0.072(6) Uiso 1 1 d DU . . H13E H -0.1880 0.6623 0.1122 0.087 Uiso 1 1 calc R . . C14E C -0.2935(11) 0.7504(11) 0.1145(7) 0.080(6) Uiso 1 1 d DU . . H14E H -0.2806 0.7827 0.0939 0.096 Uiso 1 1 calc R . . C15E C -0.3646(11) 0.7772(11) 0.1311(7) 0.082(6) Uiso 1 1 d DU . . H15E H -0.4008 0.8283 0.1255 0.099 Uiso 1 1 calc R . . C16E C -0.3806(11) 0.7235(10) 0.1574(7) 0.081(6) Uiso 1 1 d DU . . H16E H -0.4320 0.7387 0.1677 0.097 Uiso 1 1 calc R . . N21E N -0.2303(8) 0.5027(7) 0.1859(5) 0.061(4) Uiso 1 1 d DU . . N22E N -0.1681(8) 0.4375(8) 0.1948(5) 0.067(4) Uiso 1 1 d DU . . C23E C -0.1036(9) 0.4466(9) 0.1838(6) 0.063(5) Uiso 1 1 d DU . . H23E H -0.0525 0.4091 0.1871 0.075 Uiso 1 1 calc R . . C24E C -0.1248(9) 0.5207(9) 0.1666(6) 0.060(5) Uiso 1 1 d DU . . H24E H -0.0912 0.5436 0.1550 0.072 Uiso 1 1 calc R . . C25E C -0.2026(8) 0.5546(8) 0.1693(5) 0.052(4) Uiso 1 1 d DU . . C31E C -0.1798(11) 0.3686(10) 0.2070(5) 0.059(5) Uiso 1 1 d DU . . H31I H -0.1329 0.3240 0.1994 0.070 Uiso 1 1 calc R . . H31J H -0.2232 0.3679 0.1894 0.070 Uiso 1 1 calc R . . C32E C -0.1968(11) 0.3592(10) 0.2549(5) 0.062(5) Uiso 1 1 d DU . . C33E C -0.2155(11) 0.2958(9) 0.2660(5) 0.060(5) Uiso 1 1 d DU . . H33E H -0.2183 0.2635 0.2441 0.072 Uiso 1 1 calc R . . C34E C -0.2300(11) 0.2808(10) 0.3094(5) 0.067(5) Uiso 1 1 d DU . . C35E C -0.2239(11) 0.3265(10) 0.3395(6) 0.070(6) Uiso 1 1 d DU . . H35E H -0.2403 0.3199 0.3684 0.084 Uiso 1 1 calc R . . C36E C -0.1955(12) 0.3821(11) 0.3312(6) 0.080(6) Uiso 1 1 d DU . . H36E H -0.1828 0.4066 0.3543 0.096 Uiso 1 1 calc R . . C37E C -0.1856(12) 0.4019(11) 0.2864(5) 0.070(6) Uiso 1 1 d DU . . H37E H -0.1716 0.4439 0.2788 0.084 Uiso 1 1 calc R . . C41E C -0.2285(17) 0.0641(15) 0.4157(7) 0.116(9) Uiso 1 1 d DU . . H41I H -0.2749 0.0772 0.4343 0.139 Uiso 1 1 calc R . . H41J H -0.2102 0.0092 0.4099 0.139 Uiso 1 1 calc R . . C42E C -0.2500(14) 0.1126(12) 0.3722(6) 0.094(7) Uiso 1 1 d DU . . C43E C -0.2298(13) 0.1737(11) 0.3622(6) 0.085(7) Uiso 1 1 d DU . . H43E H -0.2012 0.1886 0.3824 0.103 Uiso 1 1 calc R . . C44E C -0.2525(11) 0.2134(10) 0.3216(5) 0.069(5) Uiso 1 1 d DU . . C45E C -0.2906(11) 0.1903(10) 0.2912(5) 0.065(5) Uiso 1 1 d DU . . H45E H -0.3029 0.2160 0.2631 0.078 Uiso 1 1 calc R . . C46E C -0.3114(13) 0.1273(11) 0.3025(6) 0.087(7) Uiso 1 1 d DU . . H46E H -0.3380 0.1104 0.2822 0.104 Uiso 1 1 calc R . . C47E C -0.2922(13) 0.0910(12) 0.3437(6) 0.085(7) Uiso 1 1 d DU . . H47E H -0.3085 0.0509 0.3523 0.103 Uiso 1 1 calc R . . N51E N -0.0947(8) 0.0369(9) 0.4256(5) 0.082(5) Uiso 1 1 d DU . . N52E N -0.1674(8) 0.0780(9) 0.4392(5) 0.075(5) Uiso 1 1 d DU . . C53E C -0.1677(10) 0.1310(12) 0.4681(7) 0.097(7) Uiso 1 1 d DU . . H53E H -0.2117 0.1676 0.4812 0.117 Uiso 1 1 calc R . . C54E C -0.0918(9) 0.1203(10) 0.4743(6) 0.079(6) Uiso 1 1 d DU . . H54E H -0.0735 0.1478 0.4930 0.095 Uiso 1 1 calc R . . C55E C -0.0460(7) 0.0614(10) 0.4479(6) 0.070(5) Uiso 1 1 d DU . . N61E N 0.0626(7) -0.0254(8) 0.4114(5) 0.069(4) Uiso 1 1 d DU . . C62E C 0.0337(7) 0.0287(9) 0.4415(5) 0.059(5) Uiso 1 1 d DU . . C63E C 0.0837(8) 0.0508(10) 0.4651(5) 0.065(5) Uiso 1 1 d DU . . H63E H 0.0637 0.0896 0.4854 0.079 Uiso 1 1 calc R . . C64E C 0.1622(9) 0.0163(10) 0.4587(6) 0.066(5) Uiso 1 1 d DU . . H64E H 0.1964 0.0320 0.4741 0.079 Uiso 1 1 calc R . . C65E C 0.1907(9) -0.0411(10) 0.4298(6) 0.076(6) Uiso 1 1 d DU . . H65E H 0.2449 -0.0674 0.4266 0.091 Uiso 1 1 calc R . . C66E C 0.1396(8) -0.0607(10) 0.4052(6) 0.072(6) Uiso 1 1 d DU . . H66E H 0.1590 -0.0986 0.3843 0.086 Uiso 1 1 calc R . . N11F N -0.1104(9) -0.0721(8) 0.3281(5) 0.067(4) Uiso 1 1 d DU . . C12F C -0.1309(11) -0.0267(10) 0.2895(6) 0.071(5) Uiso 1 1 d DU . . C13F C -0.1824(13) -0.0357(13) 0.2602(7) 0.104(8) Uiso 1 1 d DU . . H13F H -0.1960 -0.0056 0.2335 0.124 Uiso 1 1 calc R . . C14F C -0.2135(14) -0.0902(13) 0.2711(7) 0.103(8) Uiso 1 1 d DU . . H14F H -0.2450 -0.0998 0.2502 0.124 Uiso 1 1 calc R . . C15F C -0.2001(13) -0.1295(13) 0.3103(7) 0.091(7) Uiso 1 1 d DU . . H15F H -0.2279 -0.1599 0.3195 0.110 Uiso 1 1 calc R . . C16F C -0.1438(11) -0.1230(11) 0.3362(6) 0.072(6) Uiso 1 1 d DU . . H16F H -0.1273 -0.1566 0.3616 0.086 Uiso 1 1 calc R . . N21F N -0.0298(9) 0.0201(8) 0.3052(5) 0.069(4) Uiso 1 1 d DU . . N22F N -0.0122(8) 0.0783(8) 0.2878(5) 0.061(4) Uiso 1 1 d DU . . C23F C -0.0558(11) 0.1135(11) 0.2534(6) 0.072(6) Uiso 1 1 d DU . . H23F H -0.0499 0.1527 0.2349 0.087 Uiso 1 1 calc R . . C24F C -0.1110(12) 0.0838(11) 0.2490(6) 0.086(7) Uiso 1 1 d DU . . H24F H -0.1519 0.0991 0.2282 0.103 Uiso 1 1 calc R . . C25F C -0.0934(10) 0.0266(10) 0.2820(6) 0.066(5) Uiso 1 1 d DU . . C31F C 0.0597(11) 0.0849(11) 0.3021(6) 0.074(6) Uiso 1 1 d DU . . H31K H 0.0818 0.1044 0.2770 0.089 Uiso 1 1 calc R . . H31L H 0.0978 0.0334 0.3115 0.089 Uiso 1 1 calc R . . C32F C 0.0463(9) 0.1374(10) 0.3390(5) 0.063(5) Uiso 1 1 d DU . . C33F C 0.1121(9) 0.1400(9) 0.3579(5) 0.055(5) Uiso 1 1 d DU . . H33F H 0.1616 0.1064 0.3487 0.066 Uiso 1 1 calc R . . C34F C 0.1072(8) 0.1904(9) 0.3898(5) 0.054(4) Uiso 1 1 d DU . . C35F C 0.0373(9) 0.2325(10) 0.4059(6) 0.068(5) Uiso 1 1 d DU . . H35F H 0.0334 0.2651 0.4290 0.082 Uiso 1 1 calc R . . C36F C -0.0275(10) 0.2285(11) 0.3896(6) 0.070(5) Uiso 1 1 d DU . . H36F H -0.0762 0.2595 0.4011 0.084 Uiso 1 1 calc R . . C37F C -0.0246(9) 0.1793(10) 0.3556(5) 0.062(5) Uiso 1 1 d DU . . H37F H -0.0702 0.1756 0.3450 0.075 Uiso 1 1 calc R . . C41F C 0.2468(12) 0.3331(10) 0.4610(7) 0.072(6) Uiso 1 1 d DU . . H41K H 0.2458 0.3265 0.4933 0.087 Uiso 1 1 calc R . . H41L H 0.2953 0.3390 0.4528 0.087 Uiso 1 1 calc R . . C42F C 0.2450(9) 0.2614(9) 0.4406(6) 0.055(5) Uiso 1 1 d DU . . C43F C 0.1783(10) 0.2606(10) 0.4246(6) 0.066(5) Uiso 1 1 d DU . . H43F H 0.1313 0.3047 0.4245 0.079 Uiso 1 1 calc R . . C44F C 0.1817(9) 0.1911(9) 0.4079(6) 0.063(5) Uiso 1 1 d DU . . C45F C 0.2497(10) 0.1272(10) 0.4092(7) 0.076(6) Uiso 1 1 d DU . . H45F H 0.2506 0.0803 0.3994 0.092 Uiso 1 1 calc R . . C46F C 0.3176(11) 0.1307(11) 0.4248(7) 0.078(6) Uiso 1 1 d DU . . H46F H 0.3654 0.0877 0.4241 0.093 Uiso 1 1 calc R . . C47F C 0.3133(11) 0.1988(10) 0.4415(7) 0.082(6) Uiso 1 1 d DU . . H47F H 0.3582 0.2017 0.4536 0.098 Uiso 1 1 calc R . . N51F N 0.1803(7) 0.4381(7) 0.4069(4) 0.053(4) Uiso 1 1 d DU . . N52F N 0.1829(8) 0.4000(8) 0.4466(4) 0.070(4) Uiso 1 1 d DU . . C53F C 0.1119(10) 0.4342(11) 0.4662(5) 0.084(6) Uiso 1 1 d DU . . H53F H 0.0975 0.4188 0.4938 0.101 Uiso 1 1 calc R . . C54F C 0.0654(9) 0.4945(10) 0.4389(5) 0.073(6) Uiso 1 1 d DU . . H54F H 0.0136 0.5280 0.4442 0.088 Uiso 1 1 calc R . . C55F C 0.1090(8) 0.4971(9) 0.4020(4) 0.062(5) Uiso 1 1 d DU . . N61F N 0.1437(7) 0.5271(7) 0.3300(4) 0.053(4) Uiso 1 1 d DU . . C62F C 0.0906(8) 0.5467(8) 0.3637(4) 0.051(4) Uiso 1 1 d DU . . C63F C 0.0216(8) 0.6107(8) 0.3593(4) 0.051(4) Uiso 1 1 d DU . . H63F H -0.0143 0.6232 0.3826 0.061 Uiso 1 1 calc R . . C64F C 0.0052(9) 0.6562(9) 0.3209(5) 0.056(5) Uiso 1 1 d DU . . H64F H -0.0424 0.6991 0.3173 0.067 Uiso 1 1 calc R . . C65F C 0.0589(9) 0.6384(9) 0.2878(5) 0.061(5) Uiso 1 1 d DU . . H65F H 0.0495 0.6709 0.2619 0.074 Uiso 1 1 calc R . . C66F C 0.1272(8) 0.5726(8) 0.2923(4) 0.046(4) Uiso 1 1 d DU . . H66F H 0.1627 0.5593 0.2688 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.0484(3) 0.2345(3) 0.19844(15) 0.0709(14) Uani 1 1 d DU . . O11 O 0.1141(6) 0.2506(7) 0.1856(4) 0.064(3) Uani 1 1 d DU . . O12 O -0.0106(7) 0.2693(9) 0.1656(4) 0.097(4) Uani 1 1 d DU . . O13 O 0.0690(9) 0.1536(6) 0.2012(5) 0.105(5) Uani 1 1 d DU . . O14 O 0.0195(8) 0.2668(8) 0.2396(4) 0.090(5) Uani 1 1 d DU . . Cl2 Cl 0.8105(3) 0.6931(3) 0.41313(15) 0.0725(14) Uani 1 1 d DU . . O21 O 0.8641(8) 0.6204(7) 0.4293(5) 0.095(4) Uani 1 1 d DU . . O22 O 0.7446(8) 0.6869(11) 0.3939(6) 0.132(6) Uani 1 1 d DU . . O23 O 0.8468(9) 0.7268(8) 0.3814(4) 0.101(5) Uani 1 1 d DU . . O24 O 0.7859(10) 0.7415(8) 0.4493(4) 0.102(5) Uani 1 1 d DU . . Cl3 Cl -0.3807(7) 0.3620(7) 0.4484(4) 0.091(3) Uiso 0.25 1 d PDU A 1 O31 O -0.399(3) 0.353(3) 0.4932(6) 0.15(3) Uiso 0.25 1 d PDU A 1 O32 O -0.327(2) 0.2913(15) 0.4341(15) 0.101(19) Uiso 0.25 1 d PDU A 1 O33 O -0.351(2) 0.421(2) 0.4434(15) 0.088(17) Uiso 0.25 1 d PDU A 1 O34 O -0.4503(16) 0.386(2) 0.4225(12) 0.078(15) Uiso 0.25 1 d PDU A 1 Cl3' Cl -0.3807(7) 0.3620(7) 0.4484(4) 0.091(3) Uiso 0.25 1 d PDU B 2 O31' O -0.389(3) 0.327(3) 0.4901(9) 0.150 Uiso 0.25 1 d PDU B 2 O32' O -0.385(3) 0.315(2) 0.4147(12) 0.099(18) Uiso 0.25 1 d PDU B 2 O33' O -0.441(2) 0.4359(15) 0.4432(17) 0.11(2) Uiso 0.25 1 d PDU B 2 O34' O -0.3073(15) 0.368(3) 0.4477(14) 0.076(15) Uiso 0.25 1 d PDU B 2 Cl4 Cl 0.2747(4) -0.0302(3) 0.28447(19) 0.0898(17) Uiso 0.50 1 d PDU C 1 O41 O 0.3535(7) -0.0830(11) 0.2824(8) 0.089(9) Uiso 0.50 1 d PDU C 1 O42 O 0.2445(12) -0.0357(14) 0.3269(5) 0.068(9) Uiso 0.50 1 d PDU C 1 O43 O 0.2691(14) 0.0457(7) 0.2746(7) 0.075(8) Uiso 0.50 1 d PDU C 1 O44 O 0.2309(13) -0.0502(13) 0.2529(6) 0.082(8) Uiso 0.50 1 d PDU C 1 Cl4' Cl 0.2747(4) -0.0302(3) 0.28447(19) 0.0898(17) Uiso 0.50 1 d PDU D 2 O41' O 0.2894(17) -0.0846(13) 0.2526(7) 0.101(10) Uiso 0.50 1 d PDU D 2 O42' O 0.2214(17) 0.0433(10) 0.2667(10) 0.151(15) Uiso 0.50 1 d PDU D 2 O43' O 0.3430(12) -0.022(2) 0.2976(10) 0.150 Uiso 0.50 1 d PDU D 2 O44' O 0.2398(19) -0.0517(19) 0.3220(7) 0.14(2) Uiso 0.50 1 d PDU D 2 Cl5 Cl 0.1012(3) 0.5122(3) 0.15411(16) 0.0724(14) Uiso 0.50 1 d PDU E 1 O51 O 0.1221(12) 0.5308(11) 0.1953(4) 0.043(6) Uiso 0.50 1 d PDU E 1 O52 O 0.1636(11) 0.4956(15) 0.1246(6) 0.113(11) Uiso 0.50 1 d PDU E 1 O53 O 0.0828(14) 0.4450(10) 0.1616(7) 0.085(8) Uiso 0.50 1 d PDU E 1 O54 O 0.0333(11) 0.5736(11) 0.1374(8) 0.125(12) Uiso 0.50 1 d PDU E 1 Cl5' Cl 0.1012(3) 0.5122(3) 0.15411(16) 0.0724(14) Uiso 0.50 1 d PDU F 2 O51' O 0.0847(16) 0.5517(14) 0.1928(5) 0.109(12) Uiso 0.50 1 d PDU F 2 O52' O 0.1587(13) 0.4359(8) 0.1612(8) 0.111(11) Uiso 0.50 1 d PDU F 2 O53' O 0.1321(15) 0.5519(14) 0.1218(6) 0.093(9) Uiso 0.50 1 d PDU F 2 O54' O 0.0334(11) 0.5087(18) 0.1356(9) 0.148(15) Uiso 0.50 1 d PDU F 2 Cl6 Cl -0.2709(9) 0.2522(9) 0.1362(5) 0.126(4) Uiso 0.50 1 d PDU G 1 O61 O -0.2114(16) 0.1904(15) 0.1599(11) 0.150 Uiso 0.50 1 d PDU G 1 O62 O -0.3247(16) 0.3002(16) 0.1661(8) 0.096(12) Uiso 0.50 1 d PDU G 1 O63 O -0.2373(18) 0.2954(17) 0.1102(10) 0.150 Uiso 0.50 1 d PDU G 1 O64 O -0.3103(17) 0.2194(18) 0.1092(10) 0.150 Uiso 0.50 1 d PDU G 1 Cl6' Cl -0.2429(10) 0.2321(9) 0.1475(5) 0.126(4) Uiso 0.50 1 d PDU H 2 O61' O -0.1659(12) 0.2199(19) 0.1592(11) 0.150 Uiso 0.50 1 d PDU H 2 O62' O -0.2962(16) 0.2938(14) 0.1718(9) 0.090(11) Uiso 0.50 1 d PDU H 2 O63' O -0.256(2) 0.2550(18) 0.1018(6) 0.150 Uiso 0.50 1 d PDU H 2 O64' O -0.2576(18) 0.1650(13) 0.1565(10) 0.127(13) Uiso 0.50 1 d PDU H 2 Cl7 Cl -0.4548(6) 0.6986(6) 0.4771(3) 0.083(3) Uiso 0.50 1 d PDU . . O71 O -0.4178(16) 0.7432(14) 0.4563(9) 0.150 Uiso 0.50 1 d PDU . . O72 O -0.4007(12) 0.6380(11) 0.5049(7) 0.094(9) Uiso 0.50 1 d PDU . . O73 O -0.4808(15) 0.6611(14) 0.4450(7) 0.106(11) Uiso 0.50 1 d PDU . . O74 O -0.5184(12) 0.7442(14) 0.5019(8) 0.128(13) Uiso 0.50 1 d PDU . . Cl8 Cl 0.2990(9) 0.0516(8) -0.1568(4) 0.115(4) Uiso 0.25 1 d PDU I 1 O81 O 0.312(3) 0.058(3) -0.1114(6) 0.084(17) Uiso 0.25 1 d PDU I 1 O82 O 0.302(3) -0.0235(15) -0.1629(15) 0.11(2) Uiso 0.25 1 d PDU I 1 O83 O 0.356(2) 0.066(3) -0.1822(13) 0.100 Uiso 0.25 1 d PDU I 1 O84 O 0.2237(15) 0.107(2) -0.1687(14) 0.109(19) Uiso 0.25 1 d PDU I 1 Cl8' Cl 0.2990(9) 0.0516(8) -0.1568(4) 0.115(4) Uiso 0.25 1 d PDU J 2 O81' O 0.348(2) 0.043(2) -0.1204(9) 0.063(14) Uiso 0.25 1 d PDU J 2 O82' O 0.341(2) -0.003(2) -0.1883(12) 0.11(2) Uiso 0.25 1 d PDU J 2 O83' O 0.275(3) 0.1269(14) -0.1767(14) 0.11(2) Uiso 0.25 1 d PDU J 2 O84' O 0.2333(18) 0.037(3) -0.1432(14) 0.100(18) Uiso 0.25 1 d PDU J 2 Cl9 Cl -0.4172(6) 0.0682(6) 0.4940(3) 0.075(3) Uiso 0.25 1 d PDU K 1 O91 O -0.401(2) -0.0012(14) 0.4717(11) 0.047(11) Uiso 0.25 1 d PDU K 1 O92 O -0.424(3) 0.1284(17) 0.4622(11) 0.13(2) Uiso 0.25 1 d PDU K 1 O93 O -0.3539(16) 0.056(2) 0.5227(11) 0.074(16) Uiso 0.25 1 d PDU K 1 O94 O -0.4860(15) 0.085(2) 0.5179(13) 0.099(19) Uiso 0.25 1 d PDU K 1 Cl9' Cl -0.4172(6) 0.0682(6) 0.4940(3) 0.075(3) Uiso 0.25 1 d PDU L 2 O91' O -0.4936(11) 0.118(2) 0.5035(15) 0.15(3) Uiso 0.25 1 d PDU L 2 O92' O -0.406(2) 0.070(3) 0.4473(5) 0.078(15) Uiso 0.25 1 d PDU L 2 O93' O -0.403(3) -0.0082(14) 0.5091(15) 0.150 Uiso 0.25 1 d PDU L 2 O94' O -0.3625(17) 0.093(2) 0.5132(10) 0.041(10) Uiso 0.25 1 d PDU L 2 Cl10 Cl 0.3480(7) -0.3455(7) 0.0012(4) 0.095(4) Uiso 0.50 1 d PDU . . O101 O 0.3874(15) -0.3047(13) -0.0219(8) 0.133(13) Uiso 0.50 1 d PDU . . O102 O 0.3303(15) -0.3181(13) 0.0441(5) 0.102(10) Uiso 0.50 1 d PDU . . O103 O 0.3951(12) -0.4254(8) 0.0043(7) 0.069(7) Uiso 0.50 1 d PDU . . O104 O 0.2774(11) -0.3338(15) -0.0207(9) 0.140(14) Uiso 0.50 1 d PDU . . Cl11 Cl 0.4328(7) -0.1801(6) 0.0797(4) 0.094(4) Uiso 0.50 1 d PDU . . O111 O 0.3801(12) -0.2182(12) 0.0828(8) 0.089(9) Uiso 0.50 1 d PDU . . O112 O 0.5028(10) -0.2311(12) 0.0610(8) 0.114(11) Uiso 0.50 1 d PDU . . O113 O 0.4002(13) -0.1115(10) 0.0531(7) 0.086(9) Uiso 0.50 1 d PDU . . O114 O 0.4482(15) -0.1642(14) 0.1225(5) 0.115(11) Uiso 0.50 1 d PDU . . C11S C 0.2553(13) 0.4916(13) 0.5568(7) 0.100(8) Uiso 1 1 d DU . . H11A H 0.2905 0.5168 0.5627 0.150 Uiso 1 1 d R . . H11B H 0.2819 0.4474 0.5393 0.150 Uiso 1 1 d R . . H11C H 0.2390 0.4744 0.5845 0.150 Uiso 1 1 d R . . N12S N 0.1872(11) 0.5449(10) 0.5320(6) 0.106(7) Uiso 1 1 d DU . . O13S O 0.1934(10) 0.5510(9) 0.4925(5) 0.103(5) Uiso 1 1 d DU . . O14S O 0.1248(12) 0.5808(12) 0.5474(7) 0.150 Uiso 1 1 d DU . . C21S C 0.264(2) 0.5338(18) 0.0575(9) 0.056(9) Uiso 0.50 1 d PDU . . H21A H 0.2384 0.4992 0.0658 0.084 Uiso 0.50 1 d PR . . H21B H 0.3192 0.5038 0.0530 0.084 Uiso 0.50 1 d PR . . H21C H 0.2410 0.5635 0.0305 0.084 Uiso 0.50 1 d PR . . N22S N 0.2503(15) 0.5881(15) 0.0918(8) 0.078(10) Uiso 0.50 1 d PDU . . O23S O 0.197(2) 0.6497(18) 0.0878(12) 0.145(15) Uiso 0.50 1 d PDU . . O24S O 0.2881(18) 0.5773(17) 0.1252(9) 0.106(11) Uiso 0.50 1 d PDU . . C31S C -0.387(2) -0.104(2) 0.3933(15) 0.123(19) Uiso 0.50 1 d PDU M 1 H31M H -0.3460 -0.1373 0.3745 0.185 Uiso 0.50 1 d PR M 1 H31N H -0.4132 -0.1345 0.4078 0.185 Uiso 0.50 1 d PR M 1 H31O H -0.3634 -0.0845 0.4154 0.185 Uiso 0.50 1 d PR M 1 N32S N -0.4428(17) -0.0371(16) 0.3686(9) 0.090(11) Uiso 0.50 1 d PDU M 1 O33S O -0.5100(18) -0.020(2) 0.3781(11) 0.127(13) Uiso 0.50 1 d PDU M 1 O34S O -0.431(2) 0.0000(19) 0.3386(11) 0.122(12) Uiso 0.50 1 d PDU M 1 C41S C -0.358(2) 0.878(3) 0.4468(16) 0.13(2) Uiso 0.50 1 d PDU N 2 H41M H -0.3414 0.8293 0.4646 0.200 Uiso 0.50 1 d PR N 2 H41N H -0.3785 0.8714 0.4188 0.200 Uiso 0.50 1 d PR N 2 H41O H -0.3974 0.9181 0.4622 0.200 Uiso 0.50 1 d PR N 2 N42S N -0.2923(15) 0.9004(14) 0.4396(8) 0.094(12) Uiso 0.50 1 d PDU N 2 O43S O -0.2744(19) 0.9073(19) 0.4018(9) 0.107(11) Uiso 0.50 1 d PDU N 2 O44S O -0.2530(11) 0.9128(11) 0.4658(6) 0.042(5) Uiso 0.50 1 d PDU N 2 C51S C -0.523(3) 0.9822(19) 0.2407(16) 0.121(19) Uiso 0.50 1 d PDU . . H51A H -0.4924 0.9964 0.2183 0.182 Uiso 0.50 1 d PR . . H51B H -0.5301 1.0143 0.2656 0.182 Uiso 0.50 1 d PR . . H51C H -0.5734 0.9900 0.2284 0.182 Uiso 0.50 1 d PR . . N52S N -0.4838(17) 0.9013(18) 0.2556(10) 0.140(17) Uiso 0.50 1 d PDU . . O53S O -0.458(2) 0.887(2) 0.2928(10) 0.134(14) Uiso 0.50 1 d PDU . . O54S O -0.4738(19) 0.8479(17) 0.2335(10) 0.101(10) Uiso 0.50 1 d PDU . . 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 0.0720(6) 0.0694(6) 0.0619(5) -0.0067(4) 0.0033(4) -0.0351(5) Hg2 0.0722(5) 0.0577(5) 0.0503(4) -0.0013(3) -0.0018(4) -0.0372(4) Hg3 0.0767(6) 0.0734(6) 0.0569(5) -0.0036(4) 0.0074(4) -0.0421(5) Hg4 0.1173(8) 0.0965(7) 0.0467(4) 0.0104(4) -0.0127(4) -0.0801(6) Cl1 0.099(4) 0.078(3) 0.054(3) -0.019(3) 0.028(3) -0.054(3) O11 0.071(8) 0.088(9) 0.055(7) -0.016(7) 0.015(6) -0.053(8) O12 0.077(9) 0.153(12) 0.074(8) -0.055(8) 0.015(6) -0.055(9) O13 0.139(14) 0.084(7) 0.123(13) -0.038(8) 0.071(10) -0.073(9) O14 0.109(12) 0.122(11) 0.058(7) -0.046(8) 0.031(7) -0.062(10) Cl2 0.087(4) 0.090(4) 0.044(3) -0.004(2) -0.002(2) -0.040(3) O21 0.105(11) 0.089(8) 0.089(11) 0.019(7) 0.010(8) -0.038(7) O22 0.090(11) 0.192(19) 0.123(14) -0.046(12) -0.016(9) -0.058(11) O23 0.134(14) 0.092(11) 0.075(9) 0.007(8) 0.031(9) -0.044(10) O24 0.149(15) 0.109(11) 0.056(8) -0.026(7) 0.022(8) -0.057(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 N21C 2.306(15) . ? Hg1 N21A 2.327(12) . ? Hg1 N11B 2.340(15) . ? Hg1 N11A 2.375(14) . ? Hg1 N21B 2.432(13) . ? Hg1 N11C 2.487(12) . ? Hg2 N61F 2.268(12) . ? Hg2 N11D 2.272(13) . ? Hg2 N21D 2.390(12) . ? Hg2 N51A 2.442(11) . ? Hg2 N51F 2.449(11) . ? Hg2 N61A 2.477(13) . ? Hg3 N11E 2.196(12) . ? Hg3 N61D 2.308(12) . ? Hg3 N51D 2.398(12) . ? Hg3 N51B 2.485(12) . ? Hg3 N21E 2.495(13) . ? Hg3 N61B 2.512(14) . ? Hg4 N11F 2.262(14) . ? Hg4 N61E 2.301(13) . ? Hg4 N21F 2.438(14) . ? Hg4 N61C 2.451(11) . ? Hg4 N51C 2.471(12) . ? Hg4 N51E 2.476(14) . ? N11A C12A 1.359(13) . ? N11A C16A 1.362(13) . ? C12A C13A 1.398(13) . ? C12A C25A 1.414(13) . ? C13A C14A 1.370(14) . ? C14A C15A 1.365(14) . ? C15A C16A 1.403(14) . ? N21A N22A 1.359(12) . ? N21A C25A 1.372(12) . ? N22A C23A 1.384(13) . ? N22A C31A 1.46(2) . ? C23A C24A 1.385(14) . ? C24A C25A 1.383(13) . ? C31A C32A 1.529(17) . ? C32A C37A 1.378(14) . ? C32A C33A 1.389(14) . ? C33A C34A 1.378(14) . ? C34A C35A 1.390(14) . ? C34A C44A 1.491(15) . ? C35A C36A 1.404(15) . ? C36A C37A 1.394(15) . ? C41A N52A 1.44(2) . ? C41A C42A 1.548(17) . ? C42A C47A 1.388(14) . ? C42A C43A 1.389(14) . ? C43A C44A 1.378(14) . ? C44A C45A 1.380(14) . ? C45A C46A 1.388(14) . ? C46A C47A 1.386(14) . ? N51A N52A 1.363(12) . ? N51A C55A 1.395(12) . ? N52A C53A 1.384(13) . ? C53A C54A 1.365(14) . ? C54A C55A 1.403(13) . ? C55A C62A 1.406(13) . ? N61A C66A 1.348(12) . ? N61A C62A 1.364(12) . ? C62A C63A 1.400(13) . ? C63A C64A 1.368(14) . ? C64A C65A 1.380(14) . ? C65A C66A 1.404(14) . ? N11B C12B 1.353(13) . ? N11B C16B 1.359(13) . ? C12B C25B 1.386(13) . ? C12B C13B 1.400(14) . ? C13B C14B 1.368(14) . ? C14B C15B 1.362(14) . ? C15B C16B 1.414(14) . ? N21B N22B 1.354(12) . ? N21B C25B 1.392(13) . ? N22B C31B 1.39(2) . ? N22B C23B 1.394(14) . ? C23B C24B 1.373(14) . ? C24B C25B 1.401(13) . ? C31B C32B 1.536(17) . ? C32B C37B 1.377(14) . ? C32B C33B 1.387(14) . ? C33B C34B 1.386(14) . ? C34B C35B 1.397(14) . ? C34B C44B 1.483(15) . ? C35B C36B 1.399(14) . ? C36B C37B 1.393(14) . ? C41B N52B 1.38(2) . ? C41B C42B 1.548(18) . ? C42B C43B 1.379(14) . ? C42B C47B 1.393(14) . ? C43B C44B 1.386(14) . ? C44B C45B 1.395(14) . ? C45B C46B 1.395(15) . ? C46B C47B 1.382(15) . ? N51B C55B 1.375(13) . ? N51B N52B 1.376(12) . ? N52B C53B 1.389(14) . ? C53B C54B 1.378(14) . ? C54B C55B 1.397(13) . ? C55B C62B 1.411(13) . ? N61B C66B 1.356(13) . ? N61B C62B 1.364(13) . ? C62B C63B 1.382(13) . ? C63B C64B 1.372(14) . ? C64B C65B 1.369(14) . ? C65B C66B 1.412(14) . ? N11C C12C 1.3900 . ? N11C C16C 1.3900 . ? C12C C25C 1.385(12) . ? C12C C13C 1.3900 . ? C13C C14C 1.3900 . ? C14C C15C 1.3900 . ? C15C C16C 1.3900 . ? N21C N22C 1.359(13) . ? N21C C25C 1.382(13) . ? N22C C31C 1.27(2) . ? N22C C23C 1.368(14) . ? C23C C24C 1.390(14) . ? C24C C25C 1.402(14) . ? C31C C32C 1.541(15) . ? C32C C33C 1.3900 . ? C32C C37C 1.3900 . ? C33C C34C 1.3900 . ? C34C C35C 1.3900 . ? C34C C44C 1.473(13) . ? C35C C36C 1.3900 . ? C36C C37C 1.3900 . ? C41C N52C 1.44(3) . ? C41C C42C 1.562(18) . ? C42C C43C 1.3900 . ? C42C C47C 1.3900 . ? C43C C44C 1.3900 . ? C44C C45C 1.3900 . ? C45C C46C 1.3900 . ? C46C C47C 1.3900 . ? N51C C55C 1.4200 . ? N51C N52C 1.4200 . ? N52C C53C 1.4200 . ? C53C C54C 1.4200 . ? C54C C55C 1.4200 . ? C55C C62C 1.395(12) . ? N61C C66C 1.333(12) . ? N61C C62C 1.366(12) . ? C62C C63C 1.389(13) . ? C63C C64C 1.358(14) . ? C64C C65C 1.372(14) . ? C65C C66C 1.422(13) . ? N11D C16D 1.380(17) . ? N11D C12D 1.384(15) . ? C12D C13D 1.393(18) . ? C12D C25D 1.445(17) . ? C13D C14D 1.397(19) . ? C14D C15D 1.346(19) . ? C15D C16D 1.382(19) . ? N21D C25D 1.342(15) . ? N21D N22D 1.354(14) . ? N22D C23D 1.333(16) . ? N22D C31D 1.46(2) . ? C23D C24D 1.379(18) . ? C24D C25D 1.372(17) . ? C31D C32D 1.508(16) . ? C32D C37D 1.388(17) . ? C32D C33D 1.403(17) . ? C33D C34D 1.391(17) . ? C34D C35D 1.351(16) . ? C34D C44D 1.518(17) . ? C35D C36D 1.359(18) . ? C36D C37D 1.435(18) . ? C41D N52D 1.45(2) . ? C41D C42D 1.548(18) . ? C42D C43D 1.367(17) . ? C42D C47D 1.371(18) . ? C43D C44D 1.397(17) . ? C44D C45D 1.384(17) . ? C45D C46D 1.418(18) . ? C46D C47D 1.389(19) . ? N51D N52D 1.371(12) . ? N51D C55D 1.383(12) . ? N52D C53D 1.375(13) . ? C53D C54D 1.382(13) . ? C54D C55D 1.405(13) . ? C55D C62D 1.421(13) . ? N61D C66D 1.361(12) . ? N61D C62D 1.364(12) . ? C62D C63D 1.399(13) . ? C63D C64D 1.378(13) . ? C64D C65D 1.370(13) . ? C65D C66D 1.403(13) . ? N11E C16E 1.350(17) . ? N11E C12E 1.374(16) . ? C12E C13E 1.419(18) . ? C12E C25E 1.437(17) . ? C13E C14E 1.381(19) . ? C14E C15E 1.337(19) . ? C15E C16E 1.386(19) . ? N21E N22E 1.348(15) . ? N21E C25E 1.356(15) . ? N22E C23E 1.328(16) . ? N22E C31E 1.44(2) . ? C23E C24E 1.379(18) . ? C24E C25E 1.353(17) . ? C31E C32E 1.514(17) . ? C32E C37E 1.367(17) . ? C32E C33E 1.405(17) . ? C33E C34E 1.392(17) . ? C34E C35E 1.337(17) . ? C34E C44E 1.526(17) . ? C35E C36E 1.371(18) . ? C36E C37E 1.431(18) . ? C41E N52E 1.48(3) . ? C41E C42E 1.54(2) . ? C42E C47E 1.370(19) . ? C42E C43E 1.374(18) . ? C43E C44E 1.399(18) . ? C44E C45E 1.375(17) . ? C45E C46E 1.422(18) . ? C46E C47E 1.386(19) . ? N51E N52E 1.357(12) . ? N51E C55E 1.384(13) . ? N52E C53E 1.378(14) . ? C53E C54E 1.377(14) . ? C54E C55E 1.406(13) . ? C55E C62E 1.397(13) . ? N61E C66E 1.353(13) . ? N61E C62E 1.364(12) . ? C62E C63E 1.397(13) . ? C63E C64E 1.377(13) . ? C64E C65E 1.379(13) . ? C65E C66E 1.403(14) . ? N11F C16F 1.355(17) . ? N11F C12F 1.388(16) . ? C12F C13F 1.396(19) . ? C12F C25F 1.452(17) . ? C13F C14F 1.40(2) . ? C14F C15F 1.35(2) . ? C15F C16F 1.383(19) . ? N21F N22F 1.355(15) . ? N21F C25F 1.359(16) . ? N22F C23F 1.322(16) . ? N22F C31F 1.48(2) . ? C23F C24F 1.375(18) . ? C24F C25F 1.385(18) . ? C31F C32F 1.505(17) . ? C32F C37F 1.368(17) . ? C32F C33F 1.395(17) . ? C33F C34F 1.384(16) . ? C34F C35F 1.350(17) . ? C34F C44F 1.520(17) . ? C35F C36F 1.354(18) . ? C36F C37F 1.427(18) . ? C41F N52F 1.42(2) . ? C41F C42F 1.544(18) . ? C42F C43F 1.362(18) . ? C42F C47F 1.368(18) . ? C43F C44F 1.421(17) . ? C44F C45F 1.377(18) . ? C45F C46F 1.397(19) . ? C46F C47F 1.392(19) . ? N51F C55F 1.374(12) . ? N51F N52F 1.374(12) . ? N52F C53F 1.381(13) . ? C53F C54F 1.380(14) . ? C54F C55F 1.396(13) . ? C55F C62F 1.420(12) . ? N61F C66F 1.366(12) . ? N61F C62F 1.388(12) . ? C62F C63F 1.391(13) . ? C63F C64F 1.383(13) . ? C64F C65F 1.381(13) . ? C65F C66F 1.402(13) . ? Cl1 O13 1.429(10) . ? Cl1 O11 1.432(9) . ? Cl1 O12 1.437(10) . ? Cl1 O14 1.438(9) . ? Cl2 O21 1.421(10) . ? Cl2 O22 1.431(10) . ? Cl2 O24 1.435(10) . ? Cl2 O23 1.441(10) . ? Cl3 O33 1.423(11) . ? Cl3 O32 1.420(11) . ? Cl3 O31 1.431(11) . ? Cl3 O34 1.442(11) . ? Cl4 O43 1.420(10) . ? Cl4 O42 1.426(10) . ? Cl4 O41 1.432(10) . ? Cl4 O44 1.441(10) . ? Cl5 O52 1.418(10) . ? Cl5 O54 1.428(10) . ? Cl5 O51 1.432(10) . ? Cl5 O53 1.453(10) . ? Cl6 O63 1.422(11) . ? Cl6 O62 1.429(11) . ? Cl6 O61 1.433(11) . ? Cl6 O64 1.437(11) . ? Cl6' O64' 1.420(11) . ? Cl6' O61' 1.423(11) . ? Cl6' O63' 1.439(11) . ? Cl6' O62' 1.447(11) . ? Cl7 O74 1.413(10) . ? Cl7 O71 1.414(11) . ? Cl7 O72 1.443(10) . ? Cl7 O73 1.445(10) . ? Cl8 O83 1.414(11) . ? Cl8 O82 1.428(11) . ? Cl8 O84 1.431(11) . ? Cl8 O81 1.436(11) . ? Cl9 O94 1.412(11) . ? Cl9 O92 1.426(11) . ? Cl9 O93 1.431(11) . ? Cl9 O91 1.442(11) . ? Cl10 O101 1.424(10) . ? Cl10 O103 1.426(10) . ? Cl10 O104 1.428(11) . ? Cl10 O102 1.432(10) . ? Cl11 O113 1.415(10) . ? Cl11 O114 1.424(10) . ? Cl11 O112 1.430(10) . ? Cl11 O111 1.439(10) . ? C11S N12S 1.47(2) . ? N12S O14S 1.208(15) . ? N12S O13S 1.221(14) . ? C21S N22S 1.46(2) . ? N22S O23S 1.208(17) . ? N22S O24S 1.215(16) . ? C31S N32S 1.48(2) . ? N32S O34S 1.198(16) . ? N32S O33S 1.212(17) . ? C41S N42S 1.47(2) . ? N42S O44S 1.194(16) . ? N42S O43S 1.216(17) . ? C51S N52S 1.47(2) . ? N52S O54S 1.204(17) . ? N52S O53S 1.220(17) . ? 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 N21C Hg1 N21A 109.1(5) . . ? N21C Hg1 N11B 152.6(6) . . ? N21A Hg1 N11B 96.8(6) . . ? N21C Hg1 N11A 104.2(7) . . ? N21A Hg1 N11A 70.4(4) . . ? N11B Hg1 N11A 92.6(6) . . ? N21C Hg1 N21B 94.3(6) . . ? N21A Hg1 N21B 104.3(5) . . ? N11B Hg1 N21B 70.1(4) . . ? N11A Hg1 N21B 161.4(5) . . ? N21C Hg1 N11C 69.0(5) . . ? N21A Hg1 N11C 159.1(5) . . ? N11B Hg1 N11C 90.0(6) . . ? N11A Hg1 N11C 89.6(5) . . ? N21B Hg1 N11C 96.6(5) . . ? N61F Hg2 N11D 172.3(5) . . ? N61F Hg2 N21D 106.1(5) . . ? N11D Hg2 N21D 71.7(4) . . ? N61F Hg2 N51A 90.8(4) . . ? N11D Hg2 N51A 96.9(5) . . ? N21D Hg2 N51A 99.7(4) . . ? N61F Hg2 N51F 71.2(4) . . ? N11D Hg2 N51F 102.0(4) . . ? N21D Hg2 N51F 106.0(4) . . ? N51A Hg2 N51F 151.8(4) . . ? N61F Hg2 N61A 91.1(5) . . ? N11D Hg2 N61A 92.7(5) . . ? N21D Hg2 N61A 159.0(5) . . ? N51A Hg2 N61A 67.4(4) . . ? N51F Hg2 N61A 90.7(4) . . ? N11E Hg3 N61D 172.2(5) . . ? N11E Hg3 N51D 113.3(5) . . ? N61D Hg3 N51D 72.3(4) . . ? N11E Hg3 N51B 87.8(5) . . ? N61D Hg3 N51B 89.7(4) . . ? N51D Hg3 N51B 147.1(5) . . ? N11E Hg3 N21E 71.3(4) . . ? N61D Hg3 N21E 101.7(5) . . ? N51D Hg3 N21E 111.2(5) . . ? N51B Hg3 N21E 99.1(4) . . ? N11E Hg3 N61B 95.0(5) . . ? N61D Hg3 N61B 90.8(5) . . ? N51D Hg3 N61B 85.8(5) . . ? N51B Hg3 N61B 66.7(4) . . ? N21E Hg3 N61B 161.2(5) . . ? N11F Hg4 N61E 171.0(5) . . ? N11F Hg4 N21F 72.6(5) . . ? N61E Hg4 N21F 99.3(5) . . ? N11F Hg4 N61C 91.0(5) . . ? N61E Hg4 N61C 97.8(5) . . ? N21F Hg4 N61C 158.2(5) . . ? N11F Hg4 N51C 96.3(5) . . ? N61E Hg4 N51C 88.8(5) . . ? N21F Hg4 N51C 99.2(5) . . ? N61C Hg4 N51C 67.7(4) . . ? N11F Hg4 N51E 107.0(5) . . ? N61E Hg4 N51E 70.6(4) . . ? N21F Hg4 N51E 103.6(6) . . ? N61C Hg4 N51E 94.8(5) . . ? N51C Hg4 N51E 151.3(5) . . ? C12A N11A C16A 121.9(13) . . ? C12A N11A Hg1 115.8(9) . . ? C16A N11A Hg1 122.1(11) . . ? N11A C12A C13A 118.9(12) . . ? N11A C12A C25A 118.5(13) . . ? C13A C12A C25A 122.4(13) . . ? C14A C13A C12A 119.8(15) . . ? C15A C14A C13A 120.9(16) . . ? C14A C15A C16A 119.4(15) . . ? N11A C16A C15A 119.2(15) . . ? N22A N21A C25A 107.0(10) . . ? N22A N21A Hg1 135.8(9) . . ? C25A N21A Hg1 117.1(8) . . ? N21A N22A C23A 110.4(11) . . ? N21A N22A C31A 121.2(13) . . ? C23A N22A C31A 128.4(14) . . ? N22A C23A C24A 105.8(12) . . ? C25A C24A C23A 108.2(12) . . ? N21A C25A C24A 108.4(11) . . ? N21A C25A C12A 118.1(12) . . ? C24A C25A C12A 133.5(13) . . ? N22A C31A C32A 109.4(14) . . ? C37A C32A C33A 120.9(13) . . ? C37A C32A C31A 123.1(14) . . ? C33A C32A C31A 115.9(13) . . ? C34A C33A C32A 120.4(13) . . ? C33A C34A C35A 118.9(12) . . ? C33A C34A C44A 121.1(12) . . ? C35A C34A C44A 119.8(13) . . ? C34A C35A C36A 120.8(14) . . ? C37A C36A C35A 119.2(16) . . ? C32A C37A C36A 119.4(15) . . ? N52A C41A C42A 111.9(13) . . ? C47A C42A C43A 119.6(12) . . ? C47A C42A C41A 122.6(13) . . ? C43A C42A C41A 117.8(12) . . ? C44A C43A C42A 119.6(13) . . ? C43A C44A C45A 120.1(12) . . ? C43A C44A C34A 121.6(13) . . ? C45A C44A C34A 118.2(12) . . ? C44A C45A C46A 121.3(14) . . ? C47A C46A C45A 118.1(14) . . ? C46A C47A C42A 121.2(14) . . ? N52A N51A C55A 105.5(9) . . ? N52A N51A Hg2 137.6(8) . . ? C55A N51A Hg2 116.7(8) . . ? N51A N52A C53A 110.9(11) . . ? N51A N52A C41A 121.1(12) . . ? C53A N52A C41A 127.8(13) . . ? C54A C53A N52A 107.3(12) . . ? C53A C54A C55A 107.4(12) . . ? N51A C55A C54A 108.9(10) . . ? N51A C55A C62A 120.5(11) . . ? C54A C55A C62A 130.6(12) . . ? C66A N61A C62A 120.7(12) . . ? C66A N61A Hg2 120.6(10) . . ? C62A N61A Hg2 118.5(8) . . ? N61A C62A C63A 121.3(12) . . ? N61A C62A C55A 116.8(12) . . ? C63A C62A C55A 121.8(12) . . ? C64A C63A C62A 117.5(14) . . ? C63A C64A C65A 121.5(16) . . ? C64A C65A C66A 119.1(15) . . ? N61A C66A C65A 119.6(14) . . ? C12B N11B C16B 120.4(14) . . ? C12B N11B Hg1 119.0(10) . . ? C16B N11B Hg1 120.6(12) . . ? N11B C12B C25B 116.7(13) . . ? N11B C12B C13B 120.6(13) . . ? C25B C12B C13B 122.6(14) . . ? C14B C13B C12B 118.3(15) . . ? C15B C14B C13B 121.8(16) . . ? C14B C15B C16B 118.2(15) . . ? N11B C16B C15B 120.0(15) . . ? N22B N21B C25B 107.4(10) . . ? N22B N21B Hg1 141.0(10) . . ? C25B N21B Hg1 111.4(9) . . ? N21B N22B C31B 118.8(14) . . ? N21B N22B C23B 109.2(12) . . ? C31B N22B C23B 132.0(15) . . ? C24B C23B N22B 107.9(13) . . ? C23B C24B C25B 107.0(13) . . ? C12B C25B N21B 122.3(13) . . ? C12B C25B C24B 129.3(14) . . ? N21B C25B C24B 108.3(11) . . ? N22B C31B C32B 114.4(14) . . ? C37B C32B C33B 120.6(13) . . ? C37B C32B C31B 119.9(13) . . ? C33B C32B C31B 119.5(12) . . ? C32B C33B C34B 122.0(13) . . ? C33B C34B C35B 117.2(12) . . ? C33B C34B C44B 121.5(12) . . ? C35B C34B C44B 121.3(13) . . ? C34B C35B C36B 121.2(14) . . ? C37B C36B C35B 120.1(14) . . ? C32B C37B C36B 118.8(13) . . ? N52B C41B C42B 112.7(16) . . ? C43B C42B C47B 119.7(13) . . ? C43B C42B C41B 117.3(14) . . ? C47B C42B C41B 123.0(14) . . ? C42B C43B C44B 120.5(14) . . ? C43B C44B C45B 119.4(13) . . ? C43B C44B C34B 120.9(13) . . ? C45B C44B C34B 119.7(13) . . ? C44B C45B C46B 120.7(14) . . ? C47B C46B C45B 118.7(15) . . ? C46B C47B C42B 121.0(15) . . ? C55B N51B N52B 107.7(10) . . ? C55B N51B Hg3 116.6(8) . . ? N52B N51B Hg3 135.1(9) . . ? N51B N52B C41B 121.1(15) . . ? N51B N52B C53B 107.6(11) . . ? C41B N52B C53B 130.3(16) . . ? C54B C53B N52B 109.0(13) . . ? C53B C54B C55B 106.3(13) . . ? N51B C55B C54B 108.9(11) . . ? N51B C55B C62B 120.9(12) . . ? C54B C55B C62B 129.6(13) . . ? C66B N61B C62B 120.4(13) . . ? C66B N61B Hg3 121.5(11) . . ? C62B N61B Hg3 118.1(9) . . ? N61B C62B C63B 120.2(12) . . ? N61B C62B C55B 117.3(12) . . ? C63B C62B C55B 122.5(13) . . ? C64B C63B C62B 120.2(14) . . ? C65B C64B C63B 119.7(16) . . ? C64B C65B C66B 119.4(15) . . ? N61B C66B C65B 119.8(14) . . ? C12C N11C C16C 120.0 . . ? C12C N11C Hg1 114.6(8) . . ? C16C N11C Hg1 124.7(8) . . ? C25C C12C N11C 113.9(11) . . ? C25C C12C C13C 125.7(11) . . ? N11C C12C C13C 120.0 . . ? C14C C13C C12C 120.0 . . ? C15C C14C C13C 120.0 . . ? C14C C15C C16C 120.0 . . ? C15C C16C N11C 120.0 . . ? N22C N21C C25C 107.7(12) . . ? N22C N21C Hg1 135.2(11) . . ? C25C N21C Hg1 117.1(10) . . ? C31C N22C N21C 118.6(17) . . ? C31C N22C C23C 131.7(17) . . ? N21C N22C C23C 109.4(12) . . ? N22C C23C C24C 108.4(13) . . ? C23C C24C C25C 106.2(13) . . ? N21C C25C C12C 123.3(13) . . ? N21C C25C C24C 108.3(11) . . ? C12C C25C C24C 128.3(14) . . ? N22C C31C C32C 119.4(16) . . ? C33C C32C C37C 120.0 . . ? C33C C32C C31C 120.6(12) . . ? C37C C32C C31C 119.4(12) . . ? C32C C33C C34C 120.0 . . ? C33C C34C C35C 120.0 . . ? C33C C34C C44C 120.4(12) . . ? C35C C34C C44C 119.1(12) . . ? C34C C35C C36C 120.0 . . ? C37C C36C C35C 120.0 . . ? C36C C37C C32C 120.0 . . ? N52C C41C C42C 119(2) . . ? C43C C42C C47C 120.0 . . ? C43C C42C C41C 117.5(14) . . ? C47C C42C C41C 122.4(14) . . ? C42C C43C C44C 120.0 . . ? C43C C44C C45C 120.0 . . ? C43C C44C C34C 117.5(13) . . ? C45C C44C C34C 122.4(13) . . ? C46C C45C C44C 120.0 . . ? C45C C46C C47C 120.0 . . ? C46C C47C C42C 120.0 . . ? C55C N51C N52C 108.0 . . ? C55C N51C Hg4 113.5(8) . . ? N52C N51C Hg4 136.9(8) . . ? C53C N52C N51C 108.0 . . ? C53C N52C C41C 136.4(18) . . ? N51C N52C C41C 114.7(18) . . ? C54C C53C N52C 108.0 . . ? C53C C54C C55C 108.0 . . ? C62C C55C C54C 130.7(11) . . ? C62C C55C N51C 121.2(11) . . ? C54C C55C N51C 108.0 . . ? C66C N61C C62C 121.0(11) . . ? C66C N61C Hg4 119.9(9) . . ? C62C N61C Hg4 118.7(8) . . ? N61C C62C C63C 120.1(12) . . ? N61C C62C C55C 116.5(11) . . ? C63C C62C C55C 123.1(12) . . ? C64C C63C C62C 119.7(14) . . ? C63C C64C C65C 120.4(15) . . ? C64C C65C C66C 119.0(14) . . ? N61C C66C C65C 119.7(13) . . ? C16D N11D C12D 116.9(13) . . ? C16D N11D Hg2 124.9(11) . . ? C12D N11D Hg2 118.0(9) . . ? N11D C12D C13D 121.7(13) . . ? N11D C12D C25D 115.9(13) . . ? C13D C12D C25D 122.3(14) . . ? C12D C13D C14D 117.8(15) . . ? C15D C14D C13D 122.0(18) . . ? C14D C15D C16D 118.3(17) . . ? N11D C16D C15D 123.1(16) . . ? C25D N21D N22D 105.8(11) . . ? C25D N21D Hg2 112.9(9) . . ? N22D N21D Hg2 138.4(10) . . ? C23D N22D N21D 110.5(12) . . ? C23D N22D C31D 127.4(14) . . ? N21D N22D C31D 121.7(13) . . ? N22D C23D C24D 107.8(14) . . ? C25D C24D C23D 105.3(14) . . ? N21D C25D C24D 110.5(12) . . ? N21D C25D C12D 120.2(13) . . ? C24D C25D C12D 129.2(14) . . ? N22D C31D C32D 112.1(13) . . ? C37D C32D C33D 118.9(13) . . ? C37D C32D C31D 123.0(13) . . ? C33D C32D C31D 117.4(13) . . ? C34D C33D C32D 121.0(14) . . ? C35D C34D C33D 118.9(13) . . ? C35D C34D C44D 122.0(13) . . ? C33D C34D C44D 119.1(13) . . ? C34D C35D C36D 122.7(15) . . ? C35D C36D C37D 119.1(15) . . ? C32D C37D C36D 118.9(14) . . ? N52D C41D C42D 112.5(15) . . ? C43D C42D C47D 120.5(15) . . ? C43D C42D C41D 122.8(14) . . ? C47D C42D C41D 116.5(14) . . ? C42D C43D C44D 120.0(14) . . ? C45D C44D C43D 120.2(13) . . ? C45D C44D C34D 121.4(13) . . ? C43D C44D C34D 118.4(12) . . ? C44D C45D C46D 119.3(14) . . ? C47D C46D C45D 118.6(16) . . ? C42D C47D C46D 121.0(16) . . ? N52D N51D C55D 106.5(10) . . ? N52D N51D Hg3 141.5(9) . . ? C55D N51D Hg3 111.8(8) . . ? N51D N52D C53D 109.6(11) . . ? N51D N52D C41D 118.3(13) . . ? C53D N52D C41D 132.0(14) . . ? N52D C53D C54D 108.5(12) . . ? C53D C54D C55D 106.0(11) . . ? N51D C55D C54D 109.3(10) . . ? N51D C55D C62D 120.7(11) . . ? C54D C55D C62D 130.0(12) . . ? C66D N61D C62D 122.0(11) . . ? C66D N61D Hg3 121.0(9) . . ? C62D N61D Hg3 116.5(8) . . ? N61D C62D C63D 118.2(11) . . ? N61D C62D C55D 118.3(11) . . ? C63D C62D C55D 122.8(12) . . ? C64D C63D C62D 119.8(13) . . ? C65D C64D C63D 120.7(13) . . ? C64D C65D C66D 119.0(13) . . ? N61D C66D C65D 119.4(13) . . ? C16E N11E C12E 116.6(13) . . ? C16E N11E Hg3 123.2(11) . . ? C12E N11E Hg3 120.2(10) . . ? N11E C12E C13E 119.2(14) . . ? N11E C12E C25E 117.6(13) . . ? C13E C12E C25E 122.6(14) . . ? C14E C13E C12E 118.1(16) . . ? C15E C14E C13E 124.3(17) . . ? C14E C15E C16E 113.7(17) . . ? N11E C16E C15E 127.3(17) . . ? N22E N21E C25E 106.1(12) . . ? N22E N21E Hg3 140.4(10) . . ? C25E N21E Hg3 109.0(9) . . ? C23E N22E N21E 110.6(13) . . ? C23E N22E C31E 129.7(15) . . ? N21E N22E C31E 118.8(14) . . ? N22E C23E C24E 107.2(14) . . ? C25E C24E C23E 106.6(13) . . ? C24E C25E N21E 109.4(12) . . ? C24E C25E C12E 131.6(14) . . ? N21E C25E C12E 118.9(13) . . ? N22E C31E C32E 114.7(14) . . ? C37E C32E C33E 121.1(14) . . ? C37E C32E C31E 123.7(14) . . ? C33E C32E C31E 114.7(13) . . ? C34E C33E C32E 119.1(14) . . ? C35E C34E C33E 118.8(14) . . ? C35E C34E C44E 121.7(14) . . ? C33E C34E C44E 119.5(13) . . ? C34E C35E C36E 124.0(16) . . ? C35E C36E C37E 117.3(16) . . ? C32E C37E C36E 118.6(15) . . ? N52E C41E C42E 110.9(18) . . ? C47E C42E C43E 121.5(17) . . ? C47E C42E C41E 115.0(16) . . ? C43E C42E C41E 123.5(17) . . ? C42E C43E C44E 118.3(16) . . ? C45E C44E C43E 121.6(14) . . ? C45E C44E C34E 118.8(14) . . ? C43E C44E C34E 119.4(14) . . ? C44E C45E C46E 118.7(15) . . ? C47E C46E C45E 119.0(16) . . ? C42E C47E C46E 120.6(17) . . ? N52E N51E C55E 106.7(11) . . ? N52E N51E Hg4 142.0(10) . . ? C55E N51E Hg4 111.1(9) . . ? N51E N52E C53E 111.0(12) . . ? N51E N52E C41E 114.3(17) . . ? C53E N52E C41E 134.0(17) . . ? C54E C53E N52E 106.4(13) . . ? C53E C54E C55E 107.9(12) . . ? N51E C55E C62E 120.6(12) . . ? N51E C55E C54E 107.9(11) . . ? C62E C55E C54E 131.5(13) . . ? C66E N61E C62E 121.1(12) . . ? C66E N61E Hg4 120.3(10) . . ? C62E N61E Hg4 118.6(9) . . ? N61E C62E C55E 119.0(12) . . ? N61E C62E C63E 119.8(11) . . ? C55E C62E C63E 121.2(12) . . ? C64E C63E C62E 119.8(13) . . ? C63E C64E C65E 119.6(14) . . ? C64E C65E C66E 119.8(14) . . ? N61E C66E C65E 119.7(14) . . ? C16F N11F C12F 117.4(13) . . ? C16F N11F Hg4 124.5(11) . . ? C12F N11F Hg4 118.1(10) . . ? N11F C12F C13F 120.2(15) . . ? N11F C12F C25F 115.5(13) . . ? C13F C12F C25F 124.3(15) . . ? C12F C13F C14F 118.5(17) . . ? C15F C14F C13F 122.0(19) . . ? C14F C15F C16F 116.4(18) . . ? N11F C16F C15F 124.6(16) . . ? N22F N21F C25F 103.4(12) . . ? N22F N21F Hg4 143.0(11) . . ? C25F N21F Hg4 108.9(10) . . ? C23F N22F N21F 112.2(13) . . ? C23F N22F C31F 127.4(15) . . ? N21F N22F C31F 119.0(14) . . ? N22F C23F C24F 108.3(14) . . ? C23F C24F C25F 104.1(14) . . ? N21F C25F C24F 111.6(13) . . ? N21F C25F C12F 121.9(14) . . ? C24F C25F C12F 126.2(15) . . ? N22F C31F C32F 112.4(14) . . ? C37F C32F C33F 119.3(14) . . ? C37F C32F C31F 124.4(14) . . ? C33F C32F C31F 116.3(14) . . ? C34F C33F C32F 121.7(14) . . ? C35F C34F C33F 118.9(14) . . ? C35F C34F C44F 122.4(13) . . ? C33F C34F C44F 118.5(13) . . ? C34F C35F C36F 120.6(15) . . ? C35F C36F C37F 121.9(16) . . ? C32F C37F C36F 117.3(14) . . ? N52F C41F C42F 111.1(15) . . ? C43F C42F C47F 122.8(15) . . ? C43F C42F C41F 121.3(14) . . ? C47F C42F C41F 115.8(14) . . ? C42F C43F C44F 117.3(14) . . ? C45F C44F C43F 120.6(14) . . ? C45F C44F C34F 122.1(14) . . ? C43F C44F C34F 117.3(13) . . ? C44F C45F C46F 120.5(16) . . ? C47F C46F C45F 118.3(16) . . ? C42F C47F C46F 120.4(16) . . ? C55F N51F N52F 108.4(10) . . ? C55F N51F Hg2 111.8(8) . . ? N52F N51F Hg2 139.4(9) . . ? N51F N52F C53F 107.8(11) . . ? N51F N52F C41F 123.2(14) . . ? C53F N52F C41F 128.7(14) . . ? C54F C53F N52F 108.6(12) . . ? C53F C54F C55F 106.9(12) . . ? N51F C55F C54F 108.2(10) . . ? N51F C55F C62F 120.4(11) . . ? C54F C55F C62F 131.4(12) . . ? C66F N61F C62F 118.6(11) . . ? C66F N61F Hg2 122.0(9) . . ? C62F N61F Hg2 119.3(8) . . ? N61F C62F C63F 121.0(10) . . ? N61F C62F C55F 116.9(11) . . ? C63F C62F C55F 122.1(11) . . ? C64F C63F C62F 120.0(12) . . ? C65F C64F C63F 119.3(13) . . ? C64F C65F C66F 120.0(13) . . ? N61F C66F C65F 121.0(12) . . ? O13 Cl1 O11 109.6(8) . . ? O13 Cl1 O12 109.3(9) . . ? O11 Cl1 O12 107.9(8) . . ? O13 Cl1 O14 110.8(9) . . ? O11 Cl1 O14 110.2(8) . . ? O12 Cl1 O14 108.9(9) . . ? O21 Cl2 O22 111.0(10) . . ? O21 Cl2 O24 107.8(9) . . ? O22 Cl2 O24 109.1(10) . . ? O21 Cl2 O23 110.3(9) . . ? O22 Cl2 O23 109.8(10) . . ? O24 Cl2 O23 108.8(9) . . ? O33 Cl3 O32 111.3(10) . . ? O33 Cl3 O31 109.6(10) . . ? O32 Cl3 O31 109.7(10) . . ? O33 Cl3 O34 108.2(10) . . ? O32 Cl3 O34 109.2(10) . . ? O31 Cl3 O34 108.8(10) . . ? O43 Cl4 O42 110.0(9) . . ? O43 Cl4 O41 110.2(9) . . ? O42 Cl4 O41 110.1(9) . . ? O43 Cl4 O44 109.6(9) . . ? O42 Cl4 O44 108.8(9) . . ? O41 Cl4 O44 108.0(9) . . ? O52 Cl5 O54 111.8(9) . . ? O52 Cl5 O51 110.2(9) . . ? O54 Cl5 O51 109.6(9) . . ? O52 Cl5 O53 109.4(9) . . ? O54 Cl5 O53 107.8(9) . . ? O51 Cl5 O53 107.8(8) . . ? O63 Cl6 O62 110.1(10) . . ? O63 Cl6 O61 109.6(10) . . ? O62 Cl6 O61 109.9(10) . . ? O63 Cl6 O64 110.6(10) . . ? O62 Cl6 O64 109.0(10) . . ? O61 Cl6 O64 107.6(10) . . ? O64' Cl6' O61' 111.3(10) . . ? O64' Cl6' O63' 109.7(10) . . ? O61' Cl6' O63' 109.7(10) . . ? O64' Cl6' O62' 109.3(10) . . ? O61' Cl6' O62' 109.2(10) . . ? O63' Cl6' O62' 107.6(10) . . ? O74 Cl7 O71 111.1(10) . . ? O74 Cl7 O72 110.0(9) . . ? O71 Cl7 O72 110.1(10) . . ? O74 Cl7 O73 109.5(9) . . ? O71 Cl7 O73 110.1(9) . . ? O72 Cl7 O73 105.9(9) . . ? O83 Cl8 O82 110.7(10) . . ? O83 Cl8 O84 110.3(10) . . ? O82 Cl8 O84 109.1(10) . . ? O83 Cl8 O81 109.6(10) . . ? O82 Cl8 O81 109.1(10) . . ? O84 Cl8 O81 108.1(10) . . ? O94 Cl9 O92 111.1(10) . . ? O94 Cl9 O93 110.3(10) . . ? O92 Cl9 O93 109.1(10) . . ? O94 Cl9 O91 109.3(10) . . ? O92 Cl9 O91 108.6(10) . . ? O93 Cl9 O91 108.5(10) . . ? O101 Cl10 O103 110.3(9) . . ? O101 Cl10 O104 110.5(10) . . ? O103 Cl10 O104 109.1(9) . . ? O101 Cl10 O102 109.1(9) . . ? O103 Cl10 O102 109.3(9) . . ? O104 Cl10 O102 108.6(9) . . ? O113 Cl11 O114 110.6(9) . . ? O113 Cl11 O112 110.5(9) . . ? O114 Cl11 O112 109.5(9) . . ? O113 Cl11 O111 109.9(9) . . ? O114 Cl11 O111 108.6(9) . . ? O112 Cl11 O111 107.8(9) . . ? O14S N12S O13S 117(2) . . ? O14S N12S C11S 125.5(19) . . ? O13S N12S C11S 117.2(18) . . ? O23S N22S O24S 115(2) . . ? O23S N22S C21S 119(2) . . ? O24S N22S C21S 126(2) . . ? O34S N32S O33S 116(3) . . ? O34S N32S C31S 128(3) . . ? O33S N32S C31S 116(2) . . ? O44S N42S O43S 115(2) . . ? O44S N42S C41S 129(2) . . ? O43S N42S C41S 116(2) . . ? O54S N52S O53S 117(3) . . ? O54S N52S C51S 125(3) . . ? O53S N52S C51S 118(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21C Hg1 N11A C12A -104.9(15) . . . . ? N21A Hg1 N11A C12A 0.6(15) . . . . ? N11B Hg1 N11A C12A 96.9(16) . . . . ? N21B Hg1 N11A C12A 77(2) . . . . ? N11C Hg1 N11A C12A -173.1(16) . . . . ? N21C Hg1 N11A C16A 80.0(18) . . . . ? N21A Hg1 N11A C16A -174.4(19) . . . . ? N11B Hg1 N11A C16A -78.1(18) . . . . ? N21B Hg1 N11A C16A -98(2) . . . . ? N11C Hg1 N11A C16A 11.8(18) . . . . ? C16A N11A C12A C13A 0(3) . . . . ? Hg1 N11A C12A C13A -175.4(17) . . . . ? C16A N11A C12A C25A 175(2) . . . . ? Hg1 N11A C12A C25A 0(3) . . . . ? N11A C12A C13A C14A 1(4) . . . . ? C25A C12A C13A C14A -174(2) . . . . ? C12A C13A C14A C15A -1(4) . . . . ? C13A C14A C15A C16A 0(4) . . . . ? C12A N11A C16A C15A 0(4) . . . . ? Hg1 N11A C16A C15A 174.5(18) . . . . ? C14A C15A C16A N11A 0(4) . . . . ? N21C Hg1 N21A N22A -83.8(17) . . . . ? N11B Hg1 N21A N22A 87.1(17) . . . . ? N11A Hg1 N21A N22A 177.4(18) . . . . ? N21B Hg1 N21A N22A 16.0(17) . . . . ? N11C Hg1 N21A N22A -164.9(15) . . . . ? N21C Hg1 N21A C25A 97.5(14) . . . . ? N11B Hg1 N21A C25A -91.6(13) . . . . ? N11A Hg1 N21A C25A -1.3(13) . . . . ? N21B Hg1 N21A C25A -162.7(13) . . . . ? N11C Hg1 N21A C25A 16(2) . . . . ? C25A N21A N22A C23A -2(2) . . . . ? Hg1 N21A N22A C23A 179.6(14) . . . . ? C25A N21A N22A C31A 175.5(16) . . . . ? Hg1 N21A N22A C31A -3(3) . . . . ? N21A N22A C23A C24A -2(2) . . . . ? C31A N22A C23A C24A -178.6(18) . . . . ? N22A C23A C24A C25A 4(3) . . . . ? N22A N21A C25A C24A 4(2) . . . . ? Hg1 N21A C25A C24A -176.6(14) . . . . ? N22A N21A C25A C12A -177.2(18) . . . . ? Hg1 N21A C25A C12A 2(2) . . . . ? C23A C24A C25A N21A -6(3) . . . . ? C23A C24A C25A C12A 176(2) . . . . ? N11A C12A C25A N21A -1(3) . . . . ? C13A C12A C25A N21A 174(2) . . . . ? N11A C12A C25A C24A 177(2) . . . . ? C13A C12A C25A C24A -8(4) . . . . ? N21A N22A C31A C32A -92(2) . . . . ? C23A N22A C31A C32A 85(2) . . . . ? N22A C31A C32A C37A 10(3) . . . . ? N22A C31A C32A C33A -170.8(15) . . . . ? C37A C32A C33A C34A -3(3) . . . . ? C31A C32A C33A C34A 177.2(17) . . . . ? C32A C33A C34A C35A 7(3) . . . . ? C32A C33A C34A C44A -178.1(16) . . . . ? C33A C34A C35A C36A -6(3) . . . . ? C44A C34A C35A C36A 179.4(17) . . . . ? C34A C35A C36A C37A 1(3) . . . . ? C33A C32A C37A C36A -2(3) . . . . ? C31A C32A C37A C36A 177(2) . . . . ? C35A C36A C37A C32A 4(3) . . . . ? N52A C41A C42A C47A 6(2) . . . . ? N52A C41A C42A C43A -176.3(15) . . . . ? C47A C42A C43A C44A -5(3) . . . . ? C41A C42A C43A C44A 177.5(16) . . . . ? C42A C43A C44A C45A 4(3) . . . . ? C42A C43A C44A C34A -179.9(15) . . . . ? C33A C34A C44A C43A -43(3) . . . . ? C35A C34A C44A C43A 131.8(19) . . . . ? C33A C34A C44A C45A 133.8(19) . . . . ? C35A C34A C44A C45A -52(2) . . . . ? C43A C44A C45A C46A 0(3) . . . . ? C34A C44A C45A C46A -176.8(16) . . . . ? C44A C45A C46A C47A -2(3) . . . . ? C45A C46A C47A C42A 1(3) . . . . ? C43A C42A C47A C46A 2(3) . . . . ? C41A C42A C47A C46A 179.8(17) . . . . ? N61F Hg2 N51A N52A -93.3(16) . . . . ? N11D Hg2 N51A N52A 85.8(16) . . . . ? N21D Hg2 N51A N52A 13.3(16) . . . . ? N51F Hg2 N51A N52A -142.3(14) . . . . ? N61A Hg2 N51A N52A 175.9(17) . . . . ? N61F Hg2 N51A C55A 93.0(13) . . . . ? N11D Hg2 N51A C55A -87.9(12) . . . . ? N21D Hg2 N51A C55A -160.5(12) . . . . ? N51F Hg2 N51A C55A 43.9(17) . . . . ? N61A Hg2 N51A C55A 2.2(12) . . . . ? C55A N51A N52A C53A -1(2) . . . . ? Hg2 N51A N52A C53A -175.3(13) . . . . ? C55A N51A N52A C41A 174.6(15) . . . . ? Hg2 N51A N52A C41A 0(2) . . . . ? C42A C41A N52A N51A -83.7(19) . . . . ? C42A C41A N52A C53A 91(2) . . . . ? N51A N52A C53A C54A 0(2) . . . . ? C41A N52A C53A C54A -175.4(17) . . . . ? N52A C53A C54A C55A 1(2) . . . . ? N52A N51A C55A C54A 2(2) . . . . ? Hg2 N51A C55A C54A 177.5(13) . . . . ? N52A N51A C55A C62A -178.8(17) . . . . ? Hg2 N51A C55A C62A -3(2) . . . . ? C53A C54A C55A N51A -2(2) . . . . ? C53A C54A C55A C62A 179(2) . . . . ? N61F Hg2 N61A C66A 93.3(14) . . . . ? N11D Hg2 N61A C66A -80.0(15) . . . . ? N21D Hg2 N61A C66A -121.3(15) . . . . ? N51A Hg2 N61A C66A -176.2(16) . . . . ? N51F Hg2 N61A C66A 22.1(14) . . . . ? N61F Hg2 N61A C62A -91.7(14) . . . . ? N11D Hg2 N61A C62A 95.1(14) . . . . ? N21D Hg2 N61A C62A 54(2) . . . . ? N51A Hg2 N61A C62A -1.2(13) . . . . ? N51F Hg2 N61A C62A -162.9(14) . . . . ? C66A N61A C62A C63A -3(3) . . . . ? Hg2 N61A C62A C63A -178.4(16) . . . . ? C66A N61A C62A C55A 175.1(18) . . . . ? Hg2 N61A C62A C55A 0(2) . . . . ? N51A C55A C62A N61A 2(3) . . . . ? C54A C55A C62A N61A -179(2) . . . . ? N51A C55A C62A C63A -179.5(18) . . . . ? C54A C55A C62A C63A 0(4) . . . . ? N61A C62A C63A C64A 3(3) . . . . ? C55A C62A C63A C64A -176(2) . . . . ? C62A C63A C64A C65A 2(4) . . . . ? C63A C64A C65A C66A -5(4) . . . . ? C62A N61A C66A C65A 0(3) . . . . ? Hg2 N61A C66A C65A 174.7(17) . . . . ? C64A C65A C66A N61A 4(4) . . . . ? N21C Hg1 N11B C12B 62(2) . . . . ? N21A Hg1 N11B C12B -99.3(16) . . . . ? N11A Hg1 N11B C12B -169.9(16) . . . . ? N21B Hg1 N11B C12B 3.5(15) . . . . ? N11C Hg1 N11B C12B 100.5(16) . . . . ? N21C Hg1 N11B C16B -119.8(18) . . . . ? N21A Hg1 N11B C16B 79.1(18) . . . . ? N11A Hg1 N11B C16B 8.6(18) . . . . ? N21B Hg1 N11B C16B -178.1(19) . . . . ? N11C Hg1 N11B C16B -81.0(18) . . . . ? C16B N11B C12B C25B -179(2) . . . . ? Hg1 N11B C12B C25B -1(3) . . . . ? C16B N11B C12B C13B -1(3) . . . . ? Hg1 N11B C12B C13B 177.8(18) . . . . ? N11B C12B C13B C14B 6(4) . . . . ? C25B C12B C13B C14B -176(2) . . . . ? C12B C13B C14B C15B -5(4) . . . . ? C13B C14B C15B C16B -2(4) . . . . ? C12B N11B C16B C15B -6(3) . . . . ? Hg1 N11B C16B C15B 175.7(17) . . . . ? C14B C15B C16B N11B 7(4) . . . . ? N21C Hg1 N21B N22B 23.2(19) . . . . ? N21A Hg1 N21B N22B -87.7(19) . . . . ? N11B Hg1 N21B N22B -180(2) . . . . ? N11A Hg1 N21B N22B -158.5(16) . . . . ? N11C Hg1 N21B N22B 92.6(18) . . . . ? N21C Hg1 N21B C25B -162.7(14) . . . . ? N21A Hg1 N21B C25B 86.4(14) . . . . ? N11B Hg1 N21B C25B -5.7(13) . . . . ? N11A Hg1 N21B C25B 16(2) . . . . ? N11C Hg1 N21B C25B -93.3(14) . . . . ? C25B N21B N22B C31B 176.1(16) . . . . ? Hg1 N21B N22B C31B -10(3) . . . . ? C25B N21B N22B C23B -4(2) . . . . ? Hg1 N21B N22B C23B 170.7(16) . . . . ? N21B N22B C23B C24B 4(3) . . . . ? C31B N22B C23B C24B -175.6(19) . . . . ? N22B C23B C24B C25B -3(3) . . . . ? N11B C12B C25B N21B -6(3) . . . . ? C13B C12B C25B N21B 176(2) . . . . ? N11B C12B C25B C24B 178(2) . . . . ? C13B C12B C25B C24B -1(4) . . . . ? N22B N21B C25B C12B -176(2) . . . . ? Hg1 N21B C25B C12B 8(3) . . . . ? N22B N21B C25B C24B 2(2) . . . . ? Hg1 N21B C25B C24B -174.3(14) . . . . ? C23B C24B C25B C12B 178(2) . . . . ? C23B C24B C25B N21B 1(3) . . . . ? N21B N22B C31B C32B -87(2) . . . . ? C23B N22B C31B C32B 93(3) . . . . ? N22B C31B C32B C37B 15(3) . . . . ? N22B C31B C32B C33B -165.1(17) . . . . ? C37B C32B C33B C34B 0(3) . . . . ? C31B C32B C33B C34B -179.8(17) . . . . ? C32B C33B C34B C35B -1(3) . . . . ? C32B C33B C34B C44B 178.4(17) . . . . ? C33B C34B C35B C36B 2(3) . . . . ? C44B C34B C35B C36B -176.6(17) . . . . ? C34B C35B C36B C37B -3(3) . . . . ? C33B C32B C37B C36B -1(3) . . . . ? C31B C32B C37B C36B 178.9(17) . . . . ? C35B C36B C37B C32B 2(3) . . . . ? N52B C41B C42B C43B 177.7(18) . . . . ? N52B C41B C42B C47B -2(3) . . . . ? C47B C42B C43B C44B -1(3) . . . . ? C41B C42B C43B C44B 178.7(19) . . . . ? C42B C43B C44B C45B 2(3) . . . . ? C42B C43B C44B C34B -177.8(18) . . . . ? C33B C34B C44B C43B -42(3) . . . . ? C35B C34B C44B C43B 137(2) . . . . ? C33B C34B C44B C45B 139(2) . . . . ? C35B C34B C44B C45B -42(3) . . . . ? C43B C44B C45B C46B -1(3) . . . . ? C34B C44B C45B C46B 178.0(18) . . . . ? C44B C45B C46B C47B 1(3) . . . . ? C45B C46B C47B C42B 0(3) . . . . ? C43B C42B C47B C46B 0(3) . . . . ? C41B C42B C47B C46B -179(2) . . . . ? N11E Hg3 N51B C55B -100.1(14) . . . . ? N61D Hg3 N51B C55B 87.4(14) . . . . ? N51D Hg3 N51B C55B 32.0(18) . . . . ? N21E Hg3 N51B C55B -170.8(13) . . . . ? N61B Hg3 N51B C55B -3.7(13) . . . . ? N11E Hg3 N51B N52B 90.1(16) . . . . ? N61D Hg3 N51B N52B -82.4(16) . . . . ? N51D Hg3 N51B N52B -137.7(15) . . . . ? N21E Hg3 N51B N52B 19.4(17) . . . . ? N61B Hg3 N51B N52B -173.4(18) . . . . ? C55B N51B N52B C41B 176.8(17) . . . . ? Hg3 N51B N52B C41B -13(3) . . . . ? C55B N51B N52B C53B 7(2) . . . . ? Hg3 N51B N52B C53B 177.4(15) . . . . ? C42B C41B N52B N51B -84(2) . . . . ? C42B C41B N52B C53B 83(3) . . . . ? N51B N52B C53B C54B -4(3) . . . . ? C41B N52B C53B C54B -172(2) . . . . ? N52B C53B C54B C55B -1(3) . . . . ? N52B N51B C55B C54B -8(2) . . . . ? Hg3 N51B C55B C54B 179.6(14) . . . . ? N52B N51B C55B C62B 179.8(19) . . . . ? Hg3 N51B C55B C62B 7(3) . . . . ? C53B C54B C55B N51B 6(3) . . . . ? C53B C54B C55B C62B 177(2) . . . . ? N11E Hg3 N61B C66B -91.8(16) . . . . ? N61D Hg3 N61B C66B 93.4(16) . . . . ? N51D Hg3 N61B C66B 21.2(16) . . . . ? N51B Hg3 N61B C66B -177.3(18) . . . . ? N21E Hg3 N61B C66B -134.2(17) . . . . ? N11E Hg3 N61B C62B 85.4(16) . . . . ? N61D Hg3 N61B C62B -89.4(16) . . . . ? N51D Hg3 N61B C62B -161.5(16) . . . . ? N51B Hg3 N61B C62B -0.1(15) . . . . ? N21E Hg3 N61B C62B 43(2) . . . . ? C66B N61B C62B C63B 1(3) . . . . ? Hg3 N61B C62B C63B -175.8(17) . . . . ? C66B N61B C62B C55B -179(2) . . . . ? Hg3 N61B C62B C55B 4(3) . . . . ? N51B C55B C62B N61B -8(3) . . . . ? C54B C55B C62B N61B -178(2) . . . . ? N51B C55B C62B C63B 172(2) . . . . ? C54B C55B C62B C63B 2(4) . . . . ? N61B C62B C63B C64B -4(4) . . . . ? C55B C62B C63B C64B 177(2) . . . . ? C62B C63B C64B C65B 7(4) . . . . ? C63B C64B C65B C66B -7(4) . . . . ? C62B N61B C66B C65B -2(3) . . . . ? Hg3 N61B C66B C65B 175.2(17) . . . . ? C64B C65B C66B N61B 5(4) . . . . ? N21C Hg1 N11C C12C 11.6(8) . . . . ? N21A Hg1 N11C C12C 100.4(14) . . . . ? N11B Hg1 N11C C12C -150.4(8) . . . . ? N11A Hg1 N11C C12C 117.1(8) . . . . ? N21B Hg1 N11C C12C -80.5(8) . . . . ? N21C Hg1 N11C C16C -177.9(11) . . . . ? N21A Hg1 N11C C16C -89.1(16) . . . . ? N11B Hg1 N11C C16C 20.1(10) . . . . ? N11A Hg1 N11C C16C -72.4(10) . . . . ? N21B Hg1 N11C C16C 90.1(9) . . . . ? C16C N11C C12C C25C 173.0(17) . . . . ? Hg1 N11C C12C C25C -16.0(15) . . . . ? C16C N11C C12C C13C 0.0 . . . . ? Hg1 N11C C12C C13C 171.0(10) . . . . ? C25C C12C C13C C14C -172(2) . . . . ? N11C C12C C13C C14C 0.0 . . . . ? C12C C13C C14C C15C 0.0 . . . . ? C13C C14C C15C C16C 0.0 . . . . ? C14C C15C C16C N11C 0.0 . . . . ? C12C N11C C16C C15C 0.0 . . . . ? Hg1 N11C C16C C15C -170.1(11) . . . . ? N21A Hg1 N21C N22C 17(2) . . . . ? N11B Hg1 N21C N22C -142.7(18) . . . . ? N11A Hg1 N21C N22C 91(2) . . . . ? N21B Hg1 N21C N22C -89(2) . . . . ? N11C Hg1 N21C N22C 175(2) . . . . ? N21A Hg1 N21C C25C -163.3(16) . . . . ? N11B Hg1 N21C C25C 37(2) . . . . ? N11A Hg1 N21C C25C -89.5(17) . . . . ? N21B Hg1 N21C C25C 90.0(17) . . . . ? N11C Hg1 N21C C25C -5.5(16) . . . . ? C25C N21C N22C C31C 171.9(19) . . . . ? Hg1 N21C N22C C31C -9(3) . . . . ? C25C N21C N22C C23C -2(3) . . . . ? Hg1 N21C N22C C23C 177.2(16) . . . . ? C31C N22C C23C C24C -171(2) . . . . ? N21C N22C C23C C24C 2(3) . . . . ? N22C C23C C24C C25C 0(3) . . . . ? N22C N21C C25C C12C 178(2) . . . . ? Hg1 N21C C25C C12C -1(3) . . . . ? N22C N21C C25C C24C 2(3) . . . . ? Hg1 N21C C25C C24C -177.6(17) . . . . ? N11C C12C C25C N21C 12(3) . . . . ? C13C C12C C25C N21C -175.4(17) . . . . ? N11C C12C C25C C24C -172(2) . . . . ? C13C C12C C25C C24C 0(4) . . . . ? C23C C24C C25C N21C -1(3) . . . . ? C23C C24C C25C C12C -177(2) . . . . ? N21C N22C C31C C32C -77(3) . . . . ? C23C N22C C31C C32C 95(3) . . . . ? N22C C31C C32C C33C -169.3(16) . . . . ? N22C C31C C32C C37C 10(3) . . . . ? C37C C32C C33C C34C 0.0 . . . . ? C31C C32C C33C C34C 179.7(18) . . . . ? C32C C33C C34C C35C 0.0 . . . . ? C32C C33C C34C C44C -171.9(17) . . . . ? C33C C34C C35C C36C 0.0 . . . . ? C44C C34C C35C C36C 172.0(17) . . . . ? C34C C35C C36C C37C 0.0 . . . . ? C35C C36C C37C C32C 0.0 . . . . ? C33C C32C C37C C36C 0.0 . . . . ? C31C C32C C37C C36C -179.7(17) . . . . ? N52C C41C C42C C43C -170(2) . . . . ? N52C C41C C42C C47C 6(4) . . . . ? C47C C42C C43C C44C 0.0 . . . . ? C41C C42C C43C C44C 176(2) . . . . ? C42C C43C C44C C45C 0.0 . . . . ? C42C C43C C44C C34C -178.3(16) . . . . ? C33C C34C C44C C43C -57.5(17) . . . . ? C35C C34C C44C C43C 130.5(12) . . . . ? C33C C34C C44C C45C 124.3(13) . . . . ? C35C C34C C44C C45C -47.7(19) . . . . ? C43C C44C C45C C46C 0.0 . . . . ? C34C C44C C45C C46C 178.2(17) . . . . ? C44C C45C C46C C47C 0.0 . . . . ? C45C C46C C47C C42C 0.0 . . . . ? C43C C42C C47C C46C 0.0 . . . . ? C41C C42C C47C C46C -176(2) . . . . ? N11F Hg4 N51C C55C -101.2(10) . . . . ? N61E Hg4 N51C C55C 86.2(10) . . . . ? N21F Hg4 N51C C55C -174.6(9) . . . . ? N61C Hg4 N51C C55C -12.7(9) . . . . ? N51E Hg4 N51C C55C 43.2(15) . . . . ? N11F Hg4 N51C N52C 95.8(14) . . . . ? N61E Hg4 N51C N52C -76.8(14) . . . . ? N21F Hg4 N51C N52C 22.4(14) . . . . ? N61C Hg4 N51C N52C -175.8(15) . . . . ? N51E Hg4 N51C N52C -119.9(14) . . . . ? C55C N51C N52C C53C 0.0 . . . . ? Hg4 N51C N52C C53C 163.6(16) . . . . ? C55C N51C N52C C41C 170.8(19) . . . . ? Hg4 N51C N52C C41C -26(2) . . . . ? C42C C41C N52C C53C 102(3) . . . . ? C42C C41C N52C N51C -65(3) . . . . ? N51C N52C C53C C54C 0.0 . . . . ? C41C N52C C53C C54C -168(2) . . . . ? N52C C53C C54C C55C 0.0 . . . . ? C53C C54C C55C C62C 178(2) . . . . ? C53C C54C C55C N51C 0.0 . . . . ? N52C N51C C55C C62C -178(2) . . . . ? Hg4 N51C C55C C62C 13.9(19) . . . . ? N52C N51C C55C C54C 0.0 . . . . ? Hg4 N51C C55C C54C -167.9(12) . . . . ? N11F Hg4 N61C C66C -78.3(13) . . . . ? N61E Hg4 N61C C66C 99.8(12) . . . . ? N21F Hg4 N61C C66C -118.7(15) . . . . ? N51C Hg4 N61C C66C -174.7(14) . . . . ? N51E Hg4 N61C C66C 28.8(13) . . . . ? N11F Hg4 N61C C62C 108.7(13) . . . . ? N61E Hg4 N61C C62C -73.1(13) . . . . ? N21F Hg4 N61C C62C 68.4(19) . . . . ? N51C Hg4 N61C C62C 12.3(13) . . . . ? N51E Hg4 N61C C62C -144.1(13) . . . . ? C66C N61C C62C C63C 3(3) . . . . ? Hg4 N61C C62C C63C 176.1(16) . . . . ? C66C N61C C62C C55C 177.1(17) . . . . ? Hg4 N61C C62C C55C -10(2) . . . . ? C54C C55C C62C N61C 179.2(15) . . . . ? N51C C55C C62C N61C -3(3) . . . . ? C54C C55C C62C C63C -7(3) . . . . ? N51C C55C C62C C63C 170.6(18) . . . . ? N61C C62C C63C C64C -4(3) . . . . ? C55C C62C C63C C64C -178(2) . . . . ? C62C C63C C64C C65C 4(4) . . . . ? C63C C64C C65C C66C -2(4) . . . . ? C62C N61C C66C C65C -1(3) . . . . ? Hg4 N61C C66C C65C -174.2(14) . . . . ? C64C C65C C66C N61C 1(3) . . . . ? N61F Hg2 N11D C16D -113(3) . . . . ? N21D Hg2 N11D C16D 171.7(16) . . . . ? N51A Hg2 N11D C16D 73.7(15) . . . . ? N51F Hg2 N11D C16D -85.2(15) . . . . ? N61A Hg2 N11D C16D 6.2(15) . . . . ? N61F Hg2 N11D C12D 70(4) . . . . ? N21D Hg2 N11D C12D -4.9(11) . . . . ? N51A Hg2 N11D C12D -102.9(12) . . . . ? N51F Hg2 N11D C12D 98.2(12) . . . . ? N61A Hg2 N11D C12D -170.5(12) . . . . ? C16D N11D C12D C13D 1(3) . . . . ? Hg2 N11D C12D C13D 178.1(13) . . . . ? C16D N11D C12D C25D -176.5(17) . . . . ? Hg2 N11D C12D C25D 0(2) . . . . ? N11D C12D C13D C14D -4(3) . . . . ? C25D C12D C13D C14D 174.0(18) . . . . ? C12D C13D C14D C15D 3(3) . . . . ? C13D C14D C15D C16D 0(3) . . . . ? C12D N11D C16D C15D 2(3) . . . . ? Hg2 N11D C16D C15D -174.9(15) . . . . ? C14D C15D C16D N11D -2(3) . . . . ? N61F Hg2 N21D C25D -163.1(11) . . . . ? N11D Hg2 N21D C25D 9.1(11) . . . . ? N51A Hg2 N21D C25D 103.2(12) . . . . ? N51F Hg2 N21D C25D -88.5(12) . . . . ? N61A Hg2 N21D C25D 53.1(18) . . . . ? N61F Hg2 N21D N22D -5.9(16) . . . . ? N11D Hg2 N21D N22D 166.3(16) . . . . ? N51A Hg2 N21D N22D -99.6(15) . . . . ? N51F Hg2 N21D N22D 68.6(15) . . . . ? N61A Hg2 N21D N22D -149.7(14) . . . . ? C25D N21D N22D C23D -0.6(19) . . . . ? Hg2 N21D N22D C23D -158.8(13) . . . . ? C25D N21D N22D C31D -173.9(14) . . . . ? Hg2 N21D N22D C31D 28(2) . . . . ? N21D N22D C23D C24D 1(2) . . . . ? C31D N22D C23D C24D 173.6(16) . . . . ? N22D C23D C24D C25D -1(2) . . . . ? N22D N21D C25D C24D 0(2) . . . . ? Hg2 N21D C25D C24D 164.6(12) . . . . ? N22D N21D C25D C12D -177.2(16) . . . . ? Hg2 N21D C25D C12D -13(2) . . . . ? C23D C24D C25D N21D 0(2) . . . . ? C23D C24D C25D C12D 177.4(19) . . . . ? N11D C12D C25D N21D 9(3) . . . . ? C13D C12D C25D N21D -168.9(17) . . . . ? N11D C12D C25D C24D -168.0(18) . . . . ? C13D C12D C25D C24D 14(3) . . . . ? C23D N22D C31D C32D 105(2) . . . . ? N21D N22D C31D C32D -82.7(19) . . . . ? N22D C31D C32D C37D -17(2) . . . . ? N22D C31D C32D C33D 172.5(15) . . . . ? C37D C32D C33D C34D 6(3) . . . . ? C31D C32D C33D C34D 176.4(17) . . . . ? C32D C33D C34D C35D 0(3) . . . . ? C32D C33D C34D C44D 176.6(16) . . . . ? C33D C34D C35D C36D -6(3) . . . . ? C44D C34D C35D C36D 177.4(17) . . . . ? C34D C35D C36D C37D 6(3) . . . . ? C33D C32D C37D C36D -5(3) . . . . ? C31D C32D C37D C36D -175.7(17) . . . . ? C35D C36D C37D C32D 0(3) . . . . ? N52D C41D C42D C43D -31(3) . . . . ? N52D C41D C42D C47D 153.5(18) . . . . ? C47D C42D C43D C44D -2(3) . . . . ? C41D C42D C43D C44D -177.1(17) . . . . ? C42D C43D C44D C45D 1(3) . . . . ? C42D C43D C44D C34D -178.4(16) . . . . ? C35D C34D C44D C45D 151.8(18) . . . . ? C33D C34D C44D C45D -24(3) . . . . ? C35D C34D C44D C43D -29(3) . . . . ? C33D C34D C44D C43D 155.2(17) . . . . ? C43D C44D C45D C46D 4(3) . . . . ? C34D C44D C45D C46D -176.6(17) . . . . ? C44D C45D C46D C47D -8(3) . . . . ? C43D C42D C47D C46D -2(3) . . . . ? C41D C42D C47D C46D 173.1(19) . . . . ? C45D C46D C47D C42D 7(3) . . . . ? N11E Hg3 N51D N52D 8(2) . . . . ? N61D Hg3 N51D N52D -178(2) . . . . ? N51B Hg3 N51D N52D -118.5(18) . . . . ? N21E Hg3 N51D N52D 85.7(19) . . . . ? N61B Hg3 N51D N52D -86.0(19) . . . . ? N11E Hg3 N51D C55D -177.3(12) . . . . ? N61D Hg3 N51D C55D -3.2(13) . . . . ? N51B Hg3 N51D C55D 56.5(17) . . . . ? N21E Hg3 N51D C55D -99.3(13) . . . . ? N61B Hg3 N51D C55D 89.0(14) . . . . ? C55D N51D N52D C53D 0(2) . . . . ? Hg3 N51D N52D C53D 175.6(15) . . . . ? C55D N51D N52D C41D 178.1(16) . . . . ? Hg3 N51D N52D C41D -7(3) . . . . ? C42D C41D N52D N51D -66(2) . . . . ? C42D C41D N52D C53D 111(2) . . . . ? N51D N52D C53D C54D -1(2) . . . . ? C41D N52D C53D C54D -177.9(18) . . . . ? N52D C53D C54D C55D 1(2) . . . . ? N52D N51D C55D C54D 0(2) . . . . ? Hg3 N51D C55D C54D -176.8(12) . . . . ? N52D N51D C55D C62D 177.3(17) . . . . ? Hg3 N51D C55D C62D 1(2) . . . . ? C53D C54D C55D N51D 0(2) . . . . ? C53D C54D C55D C62D -177(2) . . . . ? N11E Hg3 N61D C66D -46(4) . . . . ? N51D Hg3 N61D C66D 177.5(15) . . . . ? N51B Hg3 N61D C66D 25.5(13) . . . . ? N21E Hg3 N61D C66D -73.8(14) . . . . ? N61B Hg3 N61D C66D 92.2(13) . . . . ? N11E Hg3 N61D C62D 142(3) . . . . ? N51D Hg3 N61D C62D 5.8(12) . . . . ? N51B Hg3 N61D C62D -146.3(13) . . . . ? N21E Hg3 N61D C62D 114.5(13) . . . . ? N61B Hg3 N61D C62D -79.6(13) . . . . ? C66D N61D C62D C63D 10(3) . . . . ? Hg3 N61D C62D C63D -178.6(14) . . . . ? C66D N61D C62D C55D -179.4(17) . . . . ? Hg3 N61D C62D C55D -8(2) . . . . ? N51D C55D C62D N61D 5(3) . . . . ? C54D C55D C62D N61D -178.5(19) . . . . ? N51D C55D C62D C63D 175.1(19) . . . . ? C54D C55D C62D C63D -8(3) . . . . ? N61D C62D C63D C64D -10(3) . . . . ? C55D C62D C63D C64D 179.4(18) . . . . ? C62D C63D C64D C65D 8(3) . . . . ? C63D C64D C65D C66D -4(3) . . . . ? C62D N61D C66D C65D -7(3) . . . . ? Hg3 N61D C66D C65D -178.0(13) . . . . ? C64D C65D C66D N61D 4(3) . . . . ? N61D Hg3 N11E C16E 144(3) . . . . ? N51D Hg3 N11E C16E -81.4(16) . . . . ? N51B Hg3 N11E C16E 72.6(15) . . . . ? N21E Hg3 N11E C16E 173.0(16) . . . . ? N61B Hg3 N11E C16E 6.3(15) . . . . ? N61D Hg3 N11E C12E -36(4) . . . . ? N51D Hg3 N11E C12E 98.4(14) . . . . ? N51B Hg3 N11E C12E -107.6(14) . . . . ? N21E Hg3 N11E C12E -7.2(13) . . . . ? N61B Hg3 N11E C12E -174.0(14) . . . . ? C16E N11E C12E C13E -9(3) . . . . ? Hg3 N11E C12E C13E 171.7(14) . . . . ? C16E N11E C12E C25E 179.7(17) . . . . ? Hg3 N11E C12E C25E 0(2) . . . . ? N11E C12E C13E C14E 8(3) . . . . ? C25E C12E C13E C14E 179.5(19) . . . . ? C12E C13E C14E C15E 0(3) . . . . ? C13E C14E C15E C16E -6(3) . . . . ? C12E N11E C16E C15E 2(3) . . . . ? Hg3 N11E C16E C15E -178.6(18) . . . . ? C14E C15E C16E N11E 6(3) . . . . ? N11E Hg3 N21E N22E 165.1(19) . . . . ? N61D Hg3 N21E N22E -18.7(18) . . . . ? N51D Hg3 N21E N22E 56.6(18) . . . . ? N51B Hg3 N21E N22E -110.3(18) . . . . ? N61B Hg3 N21E N22E -149.8(17) . . . . ? N11E Hg3 N21E C25E 13.7(11) . . . . ? N61D Hg3 N21E C25E -170.1(11) . . . . ? N51D Hg3 N21E C25E -94.8(11) . . . . ? N51B Hg3 N21E C25E 98.3(12) . . . . ? N61B Hg3 N21E C25E 59(2) . . . . ? C25E N21E N22E C23E -1(2) . . . . ? Hg3 N21E N22E C23E -153.1(14) . . . . ? C25E N21E N22E C31E -171.1(14) . . . . ? Hg3 N21E N22E C31E 37(3) . . . . ? N21E N22E C23E C24E 0(2) . . . . ? C31E N22E C23E C24E 168.1(17) . . . . ? N22E C23E C24E C25E 2(2) . . . . ? C23E C24E C25E N21E -3(2) . . . . ? C23E C24E C25E C12E -179(2) . . . . ? N22E N21E C25E C24E 2(2) . . . . ? Hg3 N21E C25E C24E 163.9(12) . . . . ? N22E N21E C25E C12E 179.3(16) . . . . ? Hg3 N21E C25E C12E -19(2) . . . . ? N11E C12E C25E C24E -169.2(19) . . . . ? C13E C12E C25E C24E 19(3) . . . . ? N11E C12E C25E N21E 15(3) . . . . ? C13E C12E C25E N21E -156.8(19) . . . . ? C23E N22E C31E C32E 108(2) . . . . ? N21E N22E C31E C32E -84(2) . . . . ? N22E C31E C32E C37E -14(3) . . . . ? N22E C31E C32E C33E 174.1(16) . . . . ? C37E C32E C33E C34E 6(3) . . . . ? C31E C32E C33E C34E 178.2(17) . . . . ? C32E C33E C34E C35E -1(3) . . . . ? C32E C33E C34E C44E 178.4(17) . . . . ? C33E C34E C35E C36E -8(3) . . . . ? C44E C34E C35E C36E 172.2(19) . . . . ? C34E C35E C36E C37E 12(3) . . . . ? C33E C32E C37E C36E -2(3) . . . . ? C31E C32E C37E C36E -173.0(19) . . . . ? C35E C36E C37E C32E -7(3) . . . . ? N52E C41E C42E C47E 166(2) . . . . ? N52E C41E C42E C43E -15(4) . . . . ? C47E C42E C43E C44E -1(4) . . . . ? C41E C42E C43E C44E 180(2) . . . . ? C42E C43E C44E C45E -3(3) . . . . ? C42E C43E C44E C34E -179(2) . . . . ? C35E C34E C44E C45E 151(2) . . . . ? C33E C34E C44E C45E -29(3) . . . . ? C35E C34E C44E C43E -33(3) . . . . ? C33E C34E C44E C43E 147(2) . . . . ? C43E C44E C45E C46E 4(3) . . . . ? C34E C44E C45E C46E 179.9(18) . . . . ? C44E C45E C46E C47E 0(3) . . . . ? C43E C42E C47E C46E 5(4) . . . . ? C41E C42E C47E C46E -176(2) . . . . ? C45E C46E C47E C42E -4(4) . . . . ? N11F Hg4 N51E N52E 7(2) . . . . ? N61E Hg4 N51E N52E 178(2) . . . . ? N21F Hg4 N51E N52E 83(2) . . . . ? N61C Hg4 N51E N52E -86(2) . . . . ? N51C Hg4 N51E N52E -135.8(19) . . . . ? N11F Hg4 N51E C55E -167.2(13) . . . . ? N61E Hg4 N51E C55E 3.7(13) . . . . ? N21F Hg4 N51E C55E -91.5(14) . . . . ? N61C Hg4 N51E C55E 100.3(14) . . . . ? N51C Hg4 N51E C55E 50.1(19) . . . . ? C55E N51E N52E C53E 3(2) . . . . ? Hg4 N51E N52E C53E -171.5(17) . . . . ? C55E N51E N52E C41E 175.0(16) . . . . ? Hg4 N51E N52E C41E 1(3) . . . . ? C42E C41E N52E N51E -83(2) . . . . ? C42E C41E N52E C53E 87(3) . . . . ? N51E N52E C53E C54E -3(3) . . . . ? C41E N52E C53E C54E -173(2) . . . . ? N52E C53E C54E C55E 1(3) . . . . ? N52E N51E C55E C62E 178.9(18) . . . . ? Hg4 N51E C55E C62E -5(2) . . . . ? N52E N51E C55E C54E -2(2) . . . . ? Hg4 N51E C55E C54E 174.3(13) . . . . ? C53E C54E C55E N51E 0(3) . . . . ? C53E C54E C55E C62E 179(2) . . . . ? N11F Hg4 N61E C66E -108(3) . . . . ? N21F Hg4 N61E C66E -82.8(15) . . . . ? N61C Hg4 N61E C66E 83.7(15) . . . . ? N51C Hg4 N61E C66E 16.4(15) . . . . ? N51E Hg4 N61E C66E 176.0(16) . . . . ? N11F Hg4 N61E C62E 73(4) . . . . ? N21F Hg4 N61E C62E 98.8(14) . . . . ? N61C Hg4 N61E C62E -94.8(14) . . . . ? N51C Hg4 N61E C62E -162.1(14) . . . . ? N51E Hg4 N61E C62E -2.5(13) . . . . ? C66E N61E C62E C55E -177.6(18) . . . . ? Hg4 N61E C62E C55E 1(2) . . . . ? C66E N61E C62E C63E 3(3) . . . . ? Hg4 N61E C62E C63E -178.6(13) . . . . ? N51E C55E C62E N61E 3(3) . . . . ? C54E C55E C62E N61E -176(2) . . . . ? N51E C55E C62E C63E -177.5(18) . . . . ? C54E C55E C62E C63E 4(4) . . . . ? N61E C62E C63E C64E -2(3) . . . . ? C55E C62E C63E C64E 178.6(18) . . . . ? C62E C63E C64E C65E -2(3) . . . . ? C63E C64E C65E C66E 4(3) . . . . ? C62E N61E C66E C65E 0(3) . . . . ? Hg4 N61E C66E C65E -178.9(14) . . . . ? C64E C65E C66E N61E -3(3) . . . . ? N61E Hg4 N11F C16F -162(3) . . . . ? N21F Hg4 N11F C16F 172.0(17) . . . . ? N61C Hg4 N11F C16F 6.6(16) . . . . ? N51C Hg4 N11F C16F 74.3(16) . . . . ? N51E Hg4 N11F C16F -88.7(16) . . . . ? N61E Hg4 N11F C12F 20(4) . . . . ? N21F Hg4 N11F C12F -6.5(14) . . . . ? N61C Hg4 N11F C12F -172.0(14) . . . . ? N51C Hg4 N11F C12F -104.3(14) . . . . ? N51E Hg4 N11F C12F 92.7(14) . . . . ? C16F N11F C12F C13F -2(3) . . . . ? Hg4 N11F C12F C13F 177.0(17) . . . . ? C16F N11F C12F C25F -179.6(18) . . . . ? Hg4 N11F C12F C25F -1(2) . . . . ? N11F C12F C13F C14F 1(4) . . . . ? C25F C12F C13F C14F 179(2) . . . . ? C12F C13F C14F C15F 5(4) . . . . ? C13F C14F C15F C16F -11(4) . . . . ? C12F N11F C16F C15F -4(3) . . . . ? Hg4 N11F C16F C15F 177.1(17) . . . . ? C14F C15F C16F N11F 10(4) . . . . ? N11F Hg4 N21F N22F 163(2) . . . . ? N61E Hg4 N21F N22F -13(2) . . . . ? N61C Hg4 N21F N22F -154.6(16) . . . . ? N51C Hg4 N21F N22F -104(2) . . . . ? N51E Hg4 N21F N22F 59(2) . . . . ? N11F Hg4 N21F C25F 13.2(12) . . . . ? N61E Hg4 N21F C25F -162.7(12) . . . . ? N61C Hg4 N21F C25F 56(2) . . . . ? N51C Hg4 N21F C25F 107.0(13) . . . . ? N51E Hg4 N21F C25F -90.7(13) . . . . ? C25F N21F N22F C23F -6(2) . . . . ? Hg4 N21F N22F C23F -156.9(16) . . . . ? C25F N21F N22F C31F -173.9(15) . . . . ? Hg4 N21F N22F C31F 36(3) . . . . ? N21F N22F C23F C24F 6(2) . . . . ? C31F N22F C23F C24F 172.2(17) . . . . ? N22F C23F C24F C25F -3(2) . . . . ? N22F N21F C25F C24F 4(2) . . . . ? Hg4 N21F C25F C24F 166.1(14) . . . . ? N22F N21F C25F C12F 178.5(18) . . . . ? Hg4 N21F C25F C12F -20(2) . . . . ? C23F C24F C25F N21F -1(3) . . . . ? C23F C24F C25F C12F -175(2) . . . . ? N11F C12F C25F N21F 15(3) . . . . ? C13F C12F C25F N21F -163(2) . . . . ? N11F C12F C25F C24F -171(2) . . . . ? C13F C12F C25F C24F 11(4) . . . . ? C23F N22F C31F C32F 101(2) . . . . ? N21F N22F C31F C32F -94(2) . . . . ? N22F C31F C32F C37F -5(3) . . . . ? N22F C31F C32F C33F 172.7(16) . . . . ? C37F C32F C33F C34F -8(3) . . . . ? C31F C32F C33F C34F 175.0(17) . . . . ? C32F C33F C34F C35F 7(3) . . . . ? C32F C33F C34F C44F -178.4(16) . . . . ? C33F C34F C35F C36F -4(3) . . . . ? C44F C34F C35F C36F -178.2(18) . . . . ? C34F C35F C36F C37F 1(3) . . . . ? C33F C32F C37F C36F 5(3) . . . . ? C31F C32F C37F C36F -177.7(18) . . . . ? C35F C36F C37F C32F -2(3) . . . . ? N52F C41F C42F C43F -21(2) . . . . ? N52F C41F C42F C47F 161.4(17) . . . . ? C47F C42F C43F C44F -1(3) . . . . ? C41F C42F C43F C44F -177.7(16) . . . . ? C42F C43F C44F C45F 2(3) . . . . ? C42F C43F C44F C34F -179.6(16) . . . . ? C35F C34F C44F C45F 146(2) . . . . ? C33F C34F C44F C45F -28(3) . . . . ? C35F C34F C44F C43F -32(3) . . . . ? C33F C34F C44F C43F 152.9(17) . . . . ? C43F C44F C45F C46F -3(3) . . . . ? C34F C44F C45F C46F 177.9(18) . . . . ? C44F C45F C46F C47F 4(3) . . . . ? C43F C42F C47F C46F 1(3) . . . . ? C41F C42F C47F C46F 178.6(18) . . . . ? C45F C46F C47F C42F -3(3) . . . . ? N61F Hg2 N51F C55F 2.7(12) . . . . ? N11D Hg2 N51F C55F -173.5(12) . . . . ? N21D Hg2 N51F C55F -99.3(12) . . . . ? N51A Hg2 N51F C55F 55.6(16) . . . . ? N61A Hg2 N51F C55F 93.5(12) . . . . ? N61F Hg2 N51F N52F 174.1(18) . . . . ? N11D Hg2 N51F N52F -2.1(17) . . . . ? N21D Hg2 N51F N52F 72.1(17) . . . . ? N51A Hg2 N51F N52F -133.0(15) . . . . ? N61A Hg2 N51F N52F -95.0(17) . . . . ? C55F N51F N52F C53F 2(2) . . . . ? Hg2 N51F N52F C53F -170.1(14) . . . . ? C55F N51F N52F C41F 176.3(16) . . . . ? Hg2 N51F N52F C41F 5(3) . . . . ? C42F C41F N52F N51F -80(2) . . . . ? C42F C41F N52F C53F 93(2) . . . . ? N51F N52F C53F C54F -1(2) . . . . ? C41F N52F C53F C54F -175.3(18) . . . . ? N52F C53F C54F C55F 0(2) . . . . ? N52F N51F C55F C54F -2(2) . . . . ? Hg2 N51F C55F C54F 172.6(12) . . . . ? N52F N51F C55F C62F 179.6(16) . . . . ? Hg2 N51F C55F C62F -6(2) . . . . ? C53F C54F C55F N51F 1(2) . . . . ? C53F C54F C55F C62F 180(2) . . . . ? N11D Hg2 N61F C66F -153(3) . . . . ? N21D Hg2 N61F C66F -80.7(13) . . . . ? N51A Hg2 N61F C66F 19.7(12) . . . . ? N51F Hg2 N61F C66F 177.5(13) . . . . ? N61A Hg2 N61F C66F 87.1(12) . . . . ? N11D Hg2 N61F C62F 30(4) . . . . ? N21D Hg2 N61F C62F 102.9(12) . . . . ? N51A Hg2 N61F C62F -156.8(12) . . . . ? N51F Hg2 N61F C62F 1.1(12) . . . . ? N61A Hg2 N61F C62F -89.4(12) . . . . ? C66F N61F C62F C63F 1(2) . . . . ? Hg2 N61F C62F C63F 177.2(12) . . . . ? C66F N61F C62F C55F 178.7(15) . . . . ? Hg2 N61F C62F C55F -5(2) . . . . ? N51F C55F C62F N61F 8(3) . . . . ? C54F C55F C62F N61F -171(2) . . . . ? N51F C55F C62F C63F -174.4(17) . . . . ? C54F C55F C62F C63F 7(3) . . . . ? N61F C62F C63F C64F 0(3) . . . . ? C55F C62F C63F C64F -178.3(17) . . . . ? C62F C63F C64F C65F -2(3) . . . . ? C63F C64F C65F C66F 4(3) . . . . ? C62F N61F C66F C65F 1(2) . . . . ? Hg2 N61F C66F C65F -175.4(13) . . . . ? C64F C65F C66F N61F -3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.655 _refine_diff_density_min -2.386 _refine_diff_density_rms 0.210 #===END data_imw546 _database_code_depnum_ccdc_archive 'CCDC 609502' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H70 Hg3 N22, 6(C2 H3 N), 6(Cl O4)' _chemical_formula_sum 'C98 H88 Cl6 Hg3 N28 O24' _chemical_formula_weight 2856.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2863(3) _cell_length_b 25.3101(4) _cell_length_c 22.8779(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.6130(10) _cell_angle_gamma 90.00 _cell_volume 10567.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9628 _cell_measurement_theta_min 4.616 _cell_measurement_theta_max 49.361 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5624 _exptl_absorpt_coefficient_mu 4.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3399 _exptl_absorpt_correction_T_max 0.5462 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 197417 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 24.81 _reflns_number_total 18231 _reflns_number_gt 14761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+59.7677P] 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 18231 _refine_ls_number_parameters 1438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.830 _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 0.695407(10) 0.419330(7) 0.886611(8) 0.02269(5) Uani 1 1 d . . . Hg2 Hg 0.342146(9) 0.322629(6) 0.701261(7) 0.01671(5) Uani 1 1 d . . . Hg3 Hg -0.004517(10) 0.332390(7) 0.497349(9) 0.02544(5) Uani 1 1 d . . . N11A N 0.7348(2) 0.35852(15) 0.94706(17) 0.0249(9) Uani 1 1 d . . . C12A C 0.7405(2) 0.30816(18) 0.9267(2) 0.0214(10) Uani 1 1 d . . . C13A C 0.7661(3) 0.26763(19) 0.9632(2) 0.0301(12) Uani 1 1 d . . . H13A H 0.7701 0.2327 0.9487 0.036 Uiso 1 1 calc R . . C14A C 0.7856(3) 0.2791(2) 1.0214(2) 0.0406(14) Uani 1 1 d . . . H14A H 0.8032 0.2518 1.0471 0.049 Uiso 1 1 calc R . . C15A C 0.7794(3) 0.3302(2) 1.0418(2) 0.0386(14) Uani 1 1 d . . . H15A H 0.7928 0.3385 1.0815 0.046 Uiso 1 1 calc R . . C16A C 0.7536(3) 0.3690(2) 1.0037(2) 0.0303(12) Uani 1 1 d . . . H16A H 0.7490 0.4041 1.0177 0.036 Uiso 1 1 calc R . . N21A N 0.7006(2) 0.33950(14) 0.83011(16) 0.0196(8) Uani 1 1 d . . . N22A N 0.68517(19) 0.31918(14) 0.77634(15) 0.0181(8) Uani 1 1 d . . . C23A C 0.6944(2) 0.26647(18) 0.7763(2) 0.0249(10) Uani 1 1 d . . . H23A H 0.6872 0.2438 0.7434 0.030 Uiso 1 1 calc R . . C24A C 0.7160(3) 0.25138(17) 0.8321(2) 0.0245(10) Uani 1 1 d . . . H24A H 0.7265 0.2167 0.8460 0.029 Uiso 1 1 calc R . . C25A C 0.7194(2) 0.29868(17) 0.86426(19) 0.0198(10) Uani 1 1 d . . . C31A C 0.6637(2) 0.35502(18) 0.72903(19) 0.0217(10) Uani 1 1 d . . . H31A H 0.6593 0.3349 0.6919 0.026 Uiso 1 1 calc R . . H31B H 0.7028 0.3817 0.7257 0.026 Uiso 1 1 calc R . . C32A C 0.5919(2) 0.38315(17) 0.73722(18) 0.0173(9) Uani 1 1 d . . . C33A C 0.5737(2) 0.42672(17) 0.70212(19) 0.0199(10) Uani 1 1 d . . . H33A H 0.6069 0.4386 0.6746 0.024 Uiso 1 1 calc R . . C34A C 0.5080(2) 0.45285(17) 0.70679(18) 0.0181(9) Uani 1 1 d . . . H34A H 0.4956 0.4817 0.6816 0.022 Uiso 1 1 calc R . . C35A C 0.4598(2) 0.43713(16) 0.74815(18) 0.0160(9) Uani 1 1 d . . . C36A C 0.4784(2) 0.39441(17) 0.78395(19) 0.0183(9) Uani 1 1 d . . . H36A H 0.4462 0.3835 0.8126 0.022 Uiso 1 1 calc R . . C37A C 0.5439(2) 0.36730(17) 0.77826(18) 0.0177(9) Uani 1 1 d . . . H37A H 0.5557 0.3378 0.8027 0.021 Uiso 1 1 calc R . . C38A C 0.3903(2) 0.46830(16) 0.7531(2) 0.0187(9) Uani 1 1 d . . . H38A H 0.4024 0.5019 0.7736 0.022 Uiso 1 1 calc R . . H38B H 0.3697 0.4771 0.7133 0.022 Uiso 1 1 calc R . . N41A N 0.30792(19) 0.39402(14) 0.76383(15) 0.0175(8) Uani 1 1 d . . . N42A N 0.33495(19) 0.44071(14) 0.78428(16) 0.0183(8) Uani 1 1 d . . . C43A C 0.3025(2) 0.45568(18) 0.8333(2) 0.0223(10) Uani 1 1 d . . . H43A H 0.3128 0.4869 0.8554 0.027 Uiso 1 1 calc R . . C44A C 0.2524(3) 0.41789(18) 0.8453(2) 0.0237(10) Uani 1 1 d . . . H44A H 0.2211 0.4172 0.8769 0.028 Uiso 1 1 calc R . . C45A C 0.2572(2) 0.38028(16) 0.80067(18) 0.0159(9) Uani 1 1 d . . . N51A N 0.24394(18) 0.29681(13) 0.75064(15) 0.0157(8) Uani 1 1 d . . . C52A C 0.2176(2) 0.33039(17) 0.79044(18) 0.0167(9) Uani 1 1 d . . . C53A C 0.1559(2) 0.31789(18) 0.8204(2) 0.0210(10) Uani 1 1 d . . . H53A H 0.1377 0.3418 0.8479 0.025 Uiso 1 1 calc R . . C54A C 0.1219(2) 0.27010(18) 0.80919(19) 0.0218(10) Uani 1 1 d . . . H54A H 0.0796 0.2609 0.8290 0.026 Uiso 1 1 calc R . . C55A C 0.1491(2) 0.23561(18) 0.76936(19) 0.0216(10) Uani 1 1 d . . . H55A H 0.1267 0.2022 0.7624 0.026 Uiso 1 1 calc R . . C56A C 0.2100(2) 0.25040(17) 0.73936(19) 0.0176(9) Uani 1 1 d . . . N61A N 0.28721(19) 0.23474(14) 0.65754(15) 0.0174(8) Uani 1 1 d . . . N62A N 0.3010(2) 0.19347(14) 0.62285(16) 0.0210(8) Uani 1 1 d . . . C63A C 0.2629(3) 0.14995(18) 0.6367(2) 0.0250(11) Uani 1 1 d . . . H63A H 0.2644 0.1165 0.6181 0.030 Uiso 1 1 calc R . . C64A C 0.2223(3) 0.16280(18) 0.6823(2) 0.0248(11) Uani 1 1 d . . . H64A H 0.1897 0.1407 0.7018 0.030 Uiso 1 1 calc R . . C65A C 0.2391(2) 0.21633(17) 0.69427(18) 0.0177(9) Uani 1 1 d . . . C71A C 0.3443(2) 0.20059(18) 0.57145(19) 0.0216(10) Uani 1 1 d . . . H71A H 0.3560 0.1656 0.5551 0.026 Uiso 1 1 calc R . . H71B H 0.3910 0.2184 0.5835 0.026 Uiso 1 1 calc R . . C72A C 0.3029(2) 0.23312(17) 0.52509(19) 0.0188(9) Uani 1 1 d . . . C73A C 0.3321(2) 0.28047(17) 0.50585(19) 0.0209(10) Uani 1 1 d . . . H73A H 0.3794 0.2913 0.5206 0.025 Uiso 1 1 calc R . . C74A C 0.2926(3) 0.31184(17) 0.46535(19) 0.0219(10) Uani 1 1 d . . . H74A H 0.3133 0.3439 0.4526 0.026 Uiso 1 1 calc R . . C75A C 0.2234(3) 0.29683(17) 0.44337(19) 0.0209(10) Uani 1 1 d . . . C76A C 0.1951(3) 0.24874(18) 0.46092(19) 0.0218(10) Uani 1 1 d . . . H76A H 0.1483 0.2375 0.4453 0.026 Uiso 1 1 calc R . . C77A C 0.2346(3) 0.21712(18) 0.50108(19) 0.0219(10) Uani 1 1 d . . . H77A H 0.2148 0.1842 0.5123 0.026 Uiso 1 1 calc R . . C78A C 0.1791(3) 0.33303(18) 0.4020(2) 0.0246(10) Uani 1 1 d . . . H78A H 0.2083 0.3424 0.3686 0.030 Uiso 1 1 calc R . . H78B H 0.1343 0.3145 0.3865 0.030 Uiso 1 1 calc R . . N81A N 0.10386(19) 0.38010(14) 0.46910(15) 0.0183(8) Uani 1 1 d . . . N82A N 0.1587(2) 0.38125(14) 0.43257(15) 0.0208(8) Uani 1 1 d . . . C83A C 0.1942(3) 0.42822(18) 0.4350(2) 0.0243(10) Uani 1 1 d . . . H83A H 0.2348 0.4378 0.4134 0.029 Uiso 1 1 calc R . . C84A C 0.1606(2) 0.45929(17) 0.47429(19) 0.0210(10) Uani 1 1 d . . . H84A H 0.1727 0.4945 0.4854 0.025 Uiso 1 1 calc R . . C85A C 0.1046(2) 0.42772(16) 0.49447(18) 0.0174(9) Uani 1 1 d . . . N91A N -0.00392(19) 0.40578(14) 0.54517(16) 0.0177(8) Uani 1 1 d . . . C92A C 0.0505(2) 0.44070(16) 0.53689(19) 0.0166(9) Uani 1 1 d . . . C93A C 0.0543(2) 0.48794(17) 0.56797(19) 0.0184(9) Uani 1 1 d . . . H93A H 0.0929 0.5122 0.5623 0.022 Uiso 1 1 calc R . . C94A C 0.0022(2) 0.49968(18) 0.6070(2) 0.0221(10) Uani 1 1 d . . . H94A H 0.0045 0.5318 0.6286 0.027 Uiso 1 1 calc R . . C95A C -0.0533(2) 0.46377(18) 0.6141(2) 0.0233(10) Uani 1 1 d . . . H95A H -0.0904 0.4713 0.6402 0.028 Uiso 1 1 calc R . . C96A C -0.0548(2) 0.41702(18) 0.5832(2) 0.0232(10) Uani 1 1 d . . . H96A H -0.0927 0.3922 0.5889 0.028 Uiso 1 1 calc R . . N11B N 0.6640(2) 0.48478(14) 0.83059(16) 0.0209(8) Uani 1 1 d . . . C12B C 0.6013(2) 0.51124(16) 0.83874(19) 0.0186(10) Uani 1 1 d . . . C13B C 0.5835(3) 0.55594(18) 0.8061(2) 0.0241(10) Uani 1 1 d . . . H13B H 0.5397 0.5747 0.8123 0.029 Uiso 1 1 calc R . . C14B C 0.6294(3) 0.57320(19) 0.7645(2) 0.0272(11) Uani 1 1 d . . . H14B H 0.6179 0.6042 0.7425 0.033 Uiso 1 1 calc R . . C15B C 0.6922(3) 0.54497(19) 0.7552(2) 0.0283(11) Uani 1 1 d . . . H15B H 0.7240 0.5556 0.7261 0.034 Uiso 1 1 calc R . . C16B C 0.7075(3) 0.50123(19) 0.7891(2) 0.0279(11) Uani 1 1 d . . . H16B H 0.7507 0.4817 0.7830 0.033 Uiso 1 1 calc R . . N21B N 0.5718(2) 0.44771(14) 0.91374(16) 0.0195(8) Uani 1 1 d . . . N22B N 0.5166(2) 0.44020(14) 0.94947(16) 0.0219(8) Uani 1 1 d . . . C23B C 0.4639(3) 0.47733(18) 0.9406(2) 0.0242(10) Uani 1 1 d . . . H23B H 0.4197 0.4798 0.9602 0.029 Uiso 1 1 calc R . . C24B C 0.4859(2) 0.51066(18) 0.8980(2) 0.0231(10) Uani 1 1 d . . . H24B H 0.4607 0.5408 0.8824 0.028 Uiso 1 1 calc R . . C25B C 0.5536(2) 0.49095(16) 0.88236(19) 0.0183(9) Uani 1 1 d . . . C31B C 0.5145(3) 0.39334(18) 0.9869(2) 0.0272(11) Uani 1 1 d . . . H31C H 0.4849 0.4009 1.0206 0.033 Uiso 1 1 calc R . . H31D H 0.5649 0.3844 1.0022 0.033 Uiso 1 1 calc R . . C32B C 0.4819(3) 0.34694(18) 0.95289(19) 0.0219(10) Uani 1 1 d . . . C33B C 0.5240(3) 0.30283(18) 0.9406(2) 0.0270(11) Uani 1 1 d . . . H33B H 0.5734 0.3004 0.9559 0.032 Uiso 1 1 calc R . . C34B C 0.4934(3) 0.26235(19) 0.9061(2) 0.0271(11) Uani 1 1 d . . . H34B H 0.5222 0.2324 0.8978 0.033 Uiso 1 1 calc R . . C35B C 0.4212(2) 0.26516(17) 0.88343(19) 0.0200(10) Uani 1 1 d . . . C36B C 0.3789(2) 0.30820(18) 0.89747(19) 0.0210(10) Uani 1 1 d . . . H36B H 0.3290 0.3100 0.8832 0.025 Uiso 1 1 calc R . . C37B C 0.4087(2) 0.34870(18) 0.93216(19) 0.0219(10) Uani 1 1 d . . . H37B H 0.3791 0.3778 0.9418 0.026 Uiso 1 1 calc R . . C38B C 0.3899(2) 0.22268(17) 0.84268(19) 0.0208(10) Uani 1 1 d . . . H38C H 0.3903 0.1885 0.8637 0.025 Uiso 1 1 calc R . . H38D H 0.3384 0.2314 0.8305 0.025 Uiso 1 1 calc R . . N41B N 0.42998(19) 0.25637(13) 0.74992(15) 0.0170(8) Uani 1 1 d . . . N42B N 0.43209(19) 0.21783(14) 0.79085(15) 0.0182(8) Uani 1 1 d . . . C43B C 0.4854(3) 0.18255(18) 0.7820(2) 0.0245(10) Uani 1 1 d . . . H43B H 0.4979 0.1528 0.8059 0.029 Uiso 1 1 calc R . . C44B C 0.5181(3) 0.19728(18) 0.7327(2) 0.0249(11) Uani 1 1 d . . . H44B H 0.5571 0.1799 0.7150 0.030 Uiso 1 1 calc R . . C45B C 0.4818(2) 0.24352(17) 0.71378(19) 0.0185(9) Uani 1 1 d . . . N51B N 0.44648(19) 0.31685(14) 0.65156(15) 0.0163(8) Uani 1 1 d . . . C52B C 0.4942(2) 0.27710(16) 0.66299(18) 0.0170(9) Uani 1 1 d . . . C53B C 0.5526(2) 0.26877(18) 0.6278(2) 0.0232(10) Uani 1 1 d . . . H53B H 0.5860 0.2405 0.6358 0.028 Uiso 1 1 calc R . . C54B C 0.5614(2) 0.30244(19) 0.5807(2) 0.0241(10) Uani 1 1 d . . . H54B H 0.6004 0.2969 0.5559 0.029 Uiso 1 1 calc R . . C55B C 0.5133(2) 0.34389(19) 0.57016(19) 0.0227(10) Uani 1 1 d . . . H55B H 0.5193 0.3676 0.5386 0.027 Uiso 1 1 calc R . . C56B C 0.4558(2) 0.35023(17) 0.60678(18) 0.0181(9) Uani 1 1 d . . . N61B N 0.33830(19) 0.38702(14) 0.62575(15) 0.0183(8) Uani 1 1 d . . . N62B N 0.2959(2) 0.42833(14) 0.60847(16) 0.0207(8) Uani 1 1 d . . . C63B C 0.3300(3) 0.45904(19) 0.5703(2) 0.0267(11) Uani 1 1 d . . . H63B H 0.3111 0.4905 0.5525 0.032 Uiso 1 1 calc R . . C64B C 0.3973(3) 0.43660(19) 0.5617(2) 0.0261(11) Uani 1 1 d . . . H64B H 0.4336 0.4489 0.5370 0.031 Uiso 1 1 calc R . . C65B C 0.4000(2) 0.39151(17) 0.59755(18) 0.0175(9) Uani 1 1 d . . . C71B C 0.2254(2) 0.43756(17) 0.6333(2) 0.0217(10) Uani 1 1 d . . . H71C H 0.1990 0.4654 0.6101 0.026 Uiso 1 1 calc R . . H71D H 0.2344 0.4509 0.6737 0.026 Uiso 1 1 calc R . . C72B C 0.1770(2) 0.38908(17) 0.63455(19) 0.0192(10) Uani 1 1 d . . . C73B C 0.1208(2) 0.38874(18) 0.6734(2) 0.0232(10) Uani 1 1 d . . . H73B H 0.1151 0.4178 0.6989 0.028 Uiso 1 1 calc R . . C74B C 0.0735(2) 0.34635(18) 0.6746(2) 0.0229(10) Uani 1 1 d . . . H74B H 0.0346 0.3471 0.7002 0.028 Uiso 1 1 calc R . . C75B C 0.0818(2) 0.30269(18) 0.63904(19) 0.0206(10) Uani 1 1 d . . . C76B C 0.1380(2) 0.30302(18) 0.60110(19) 0.0221(10) Uani 1 1 d . . . H76B H 0.1449 0.2732 0.5768 0.026 Uiso 1 1 calc R . . C77B C 0.1844(2) 0.34603(17) 0.59794(19) 0.0190(10) Uani 1 1 d . . . H77B H 0.2214 0.3460 0.5706 0.023 Uiso 1 1 calc R . . C78B C 0.0311(3) 0.2556(2) 0.6443(2) 0.0279(11) Uani 1 1 d . . . H78C H 0.0525 0.2316 0.6750 0.034 Uiso 1 1 calc R . . H78D H -0.0165 0.2683 0.6572 0.034 Uiso 1 1 calc R . . N81B N -0.0019(2) 0.24917(14) 0.53854(17) 0.0226(9) Uani 1 1 d . . . N82B N 0.0182(2) 0.22581(15) 0.59003(18) 0.0299(10) Uani 1 1 d . . . C83B C 0.0171(4) 0.1730(2) 0.5841(3) 0.061(2) Uani 1 1 d . . . H83B H 0.0293 0.1480 0.6141 0.073 Uiso 1 1 calc R . . C84B C -0.0048(4) 0.1614(2) 0.5272(3) 0.067(2) Uani 1 1 d . . . H84B H -0.0114 0.1275 0.5100 0.080 Uiso 1 1 calc R . . C85B C -0.0152(3) 0.21044(19) 0.5000(2) 0.0323(12) Uani 1 1 d . . . N91B N -0.0313(2) 0.27570(14) 0.42403(17) 0.0222(8) Uani 1 1 d . . . C92B C -0.0378(3) 0.22402(18) 0.4394(2) 0.0272(11) Uani 1 1 d . . . C93B C -0.0637(3) 0.1864(2) 0.3991(2) 0.0367(13) Uani 1 1 d . . . H93B H -0.0671 0.1503 0.4099 0.044 Uiso 1 1 calc R . . C94B C -0.0845(3) 0.2029(2) 0.3427(2) 0.0337(12) Uani 1 1 d . . . H94B H -0.1043 0.1782 0.3147 0.040 Uiso 1 1 calc R . . C95B C -0.0766(3) 0.2546(2) 0.3272(2) 0.0293(11) Uani 1 1 d . . . H95B H -0.0892 0.2658 0.2882 0.035 Uiso 1 1 calc R . . C96B C -0.0499(3) 0.29032(19) 0.3691(2) 0.0285(11) Uani 1 1 d . . . H96B H -0.0446 0.3263 0.3584 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.05514(6) 0.40826(4) 0.25960(5) 0.0260(2) Uani 1 1 d . . . O11 O 0.0535(4) 0.3859(2) 0.3160(2) 0.0907(19) Uani 1 1 d . . . O12 O 0.0002(2) 0.44851(14) 0.25453(18) 0.0461(10) Uani 1 1 d . . . O13 O 0.0404(2) 0.36791(18) 0.2177(2) 0.0652(14) Uani 1 1 d . . . O14 O 0.1254(3) 0.4297(2) 0.2538(3) 0.110(3) Uani 1 1 d . . . Cl2 Cl 0.17026(6) 0.70936(4) 0.33527(5) 0.0240(2) Uani 1 1 d . . . O21 O 0.1276(2) 0.69107(15) 0.38209(16) 0.0411(9) Uani 1 1 d . . . O22 O 0.14456(19) 0.76082(13) 0.31749(16) 0.0358(9) Uani 1 1 d . . . O23 O 0.1624(2) 0.67399(16) 0.28630(18) 0.0509(11) Uani 1 1 d . . . O24 O 0.24577(18) 0.71175(14) 0.35641(15) 0.0333(8) Uani 1 1 d . . . Cl3 Cl 0.41634(6) 0.42738(4) 0.39828(5) 0.0244(2) Uani 1 1 d . . . O31 O 0.4066(3) 0.47813(14) 0.42410(17) 0.0555(12) Uani 1 1 d . . . O32 O 0.34702(18) 0.40835(15) 0.37196(15) 0.0352(9) Uani 1 1 d . . . O33 O 0.46744(18) 0.43097(13) 0.35336(14) 0.0309(8) Uani 1 1 d . . . O34 O 0.44260(19) 0.38983(13) 0.44178(15) 0.0339(8) Uani 1 1 d . . . Cl4 Cl 0.65453(6) 0.11906(4) 0.65414(5) 0.0216(2) Uani 1 1 d . . . O41 O 0.61463(19) 0.09027(13) 0.69649(15) 0.0323(8) Uani 1 1 d . . . O42 O 0.6049(2) 0.13485(15) 0.60662(16) 0.0460(10) Uani 1 1 d . . . O43 O 0.7111(2) 0.08582(13) 0.63324(16) 0.0380(9) Uani 1 1 d . . . O44 O 0.68635(18) 0.16522(13) 0.68154(16) 0.0334(8) Uani 1 1 d . . . Cl5 Cl 0.72843(6) 0.53955(4) 0.98634(5) 0.0223(2) Uani 1 1 d . . . O51 O 0.66219(19) 0.56664(14) 0.96651(16) 0.0359(9) Uani 1 1 d . . . O52 O 0.7130(2) 0.50412(15) 1.03341(17) 0.0452(10) Uani 1 1 d . . . O53 O 0.7829(2) 0.57665(15) 1.00712(17) 0.0466(10) Uani 1 1 d . . . O54 O 0.7552(2) 0.51007(16) 0.93889(16) 0.0437(10) Uani 1 1 d . . . Cl6 Cl 0.83445(6) 0.38348(4) 0.43458(5) 0.0192(2) Uani 1 1 d . . . O61 O 0.79480(17) 0.43173(12) 0.44457(14) 0.0244(7) Uani 1 1 d . . . O62 O 0.84085(17) 0.35263(12) 0.48771(14) 0.0265(7) Uani 1 1 d . . . O63 O 0.90744(16) 0.39648(12) 0.41789(14) 0.0237(7) Uani 1 1 d . . . O64 O 0.79704(17) 0.35342(12) 0.38879(14) 0.0253(7) Uani 1 1 d . . . N11 N 0.0622(3) 0.4287(3) 0.8773(4) 0.086(2) Uani 1 1 d . . . C12 C 0.0878(4) 0.4701(3) 0.8756(3) 0.0581(18) Uani 1 1 d . . . C13 C 0.1198(3) 0.5239(3) 0.8744(3) 0.0576(18) Uani 1 1 d . . . H13C H 0.1190 0.5399 0.9134 0.086 Uiso 1 1 calc R . . H13D H 0.0911 0.5457 0.8459 0.086 Uiso 1 1 calc R . . H13E H 0.1706 0.5217 0.8631 0.086 Uiso 1 1 calc R . . N21 N 0.2151(4) 0.5322(2) 0.7282(2) 0.0710(19) Uani 1 1 d . . . C22 C 0.1900(3) 0.5718(2) 0.7374(2) 0.0404(14) Uani 1 1 d . . . C23 C 0.1602(3) 0.6236(2) 0.7491(2) 0.0335(12) Uani 1 1 d . . . H23C H 0.1819 0.6368 0.7866 0.050 Uiso 1 1 calc R . . H23D H 0.1069 0.6210 0.7511 0.050 Uiso 1 1 calc R . . H23E H 0.1716 0.6480 0.7177 0.050 Uiso 1 1 calc R . . N31 N 0.6258(3) 0.3430(2) 0.4472(2) 0.0495(13) Uani 1 1 d . . . C32 C 0.6317(3) 0.3683(2) 0.4070(3) 0.0358(13) Uani 1 1 d . . . C33 C 0.6397(3) 0.4005(2) 0.3545(3) 0.0449(15) Uani 1 1 d . . . H33C H 0.6843 0.4219 0.3597 0.067 Uiso 1 1 calc R . . H33D H 0.5971 0.4237 0.3482 0.067 Uiso 1 1 calc R . . H33E H 0.6431 0.3773 0.3205 0.067 Uiso 1 1 calc R . . N41 N 0.7743(2) 0.45679(19) 0.6586(2) 0.0420(12) Uani 1 1 d . . . C42 C 0.7447(3) 0.4364(2) 0.6197(3) 0.0322(12) Uani 1 1 d . . . C43 C 0.7061(3) 0.4095(2) 0.5707(2) 0.0410(14) Uani 1 1 d . . . H43C H 0.7049 0.3715 0.5785 0.061 Uiso 1 1 calc R . . H43D H 0.7316 0.4160 0.5349 0.061 Uiso 1 1 calc R . . H43E H 0.6559 0.4230 0.5656 0.061 Uiso 1 1 calc R . . N51 N 0.8361(3) 0.42559(18) 0.8445(2) 0.0425(12) Uani 1 1 d . . . C52 C 0.8792(3) 0.4268(2) 0.8090(2) 0.0341(12) Uani 1 1 d . . . C53 C 0.9325(4) 0.4289(2) 0.7651(3) 0.0471(15) Uani 1 1 d . . . H53C H 0.9374 0.4654 0.7516 0.071 Uiso 1 1 calc R . . H53D H 0.9163 0.4064 0.7319 0.071 Uiso 1 1 calc R . . H53E H 0.9800 0.4164 0.7819 0.071 Uiso 1 1 calc R . . N61 N 0.9198(3) 0.0490(2) 0.4842(3) 0.0672(17) Uani 1 1 d . . . C62 C 0.9196(3) 0.0121(3) 0.4547(3) 0.0487(16) Uani 1 1 d . . . C63 C 0.9191(3) -0.0341(2) 0.4183(3) 0.0497(16) Uani 1 1 d . . . H63C H 0.8873 -0.0610 0.4342 0.075 Uiso 1 1 calc R . . H63D H 0.9690 -0.0480 0.4174 0.075 Uiso 1 1 calc R . . H63E H 0.9006 -0.0248 0.3785 0.075 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 0.02426(10) 0.01490(9) 0.02835(10) -0.00101(7) -0.00274(7) 0.00704(7) Hg2 0.01591(9) 0.01504(9) 0.01977(9) 0.00162(7) 0.00590(6) 0.00008(6) Hg3 0.02182(10) 0.01280(9) 0.04072(11) -0.00615(8) -0.00565(8) 0.00019(7) N11A 0.027(2) 0.022(2) 0.026(2) -0.0001(17) -0.0007(17) 0.0064(17) C12A 0.020(2) 0.021(2) 0.023(2) -0.0003(19) 0.0015(19) 0.0091(19) C13A 0.038(3) 0.022(3) 0.031(3) 0.006(2) 0.006(2) 0.011(2) C14A 0.055(4) 0.041(3) 0.027(3) 0.014(2) 0.004(3) 0.020(3) C15A 0.054(4) 0.041(3) 0.020(3) -0.001(2) 0.001(2) 0.019(3) C16A 0.036(3) 0.030(3) 0.024(3) -0.007(2) -0.001(2) 0.011(2) N21A 0.019(2) 0.019(2) 0.021(2) 0.0011(16) -0.0009(16) 0.0041(15) N22A 0.0191(19) 0.0162(19) 0.0189(19) 0.0002(15) 0.0007(15) 0.0046(15) C23A 0.025(3) 0.018(2) 0.032(3) -0.004(2) 0.000(2) 0.002(2) C24A 0.027(3) 0.012(2) 0.034(3) 0.002(2) 0.003(2) 0.0041(19) C25A 0.017(2) 0.018(2) 0.024(2) -0.0006(19) 0.0053(19) 0.0028(18) C31A 0.022(2) 0.022(2) 0.021(2) -0.0001(19) 0.0011(19) 0.0049(19) C32A 0.015(2) 0.020(2) 0.017(2) -0.0033(18) 0.0015(17) 0.0002(18) C33A 0.019(2) 0.020(2) 0.020(2) 0.0014(19) 0.0027(18) -0.0002(19) C34A 0.021(2) 0.015(2) 0.018(2) 0.0020(18) -0.0027(18) -0.0045(18) C35A 0.017(2) 0.012(2) 0.018(2) -0.0014(17) -0.0011(18) -0.0026(17) C36A 0.017(2) 0.018(2) 0.019(2) -0.0014(18) 0.0018(18) -0.0065(18) C37A 0.019(2) 0.013(2) 0.021(2) 0.0021(18) -0.0033(18) -0.0001(18) C38A 0.022(2) 0.011(2) 0.023(2) 0.0007(18) 0.0032(19) -0.0015(18) N41A 0.0160(19) 0.0176(19) 0.0191(19) -0.0020(15) 0.0033(15) 0.0003(15) N42A 0.0191(19) 0.0128(18) 0.023(2) -0.0035(15) 0.0011(16) 0.0009(15) C43A 0.026(3) 0.019(2) 0.023(2) -0.0049(19) 0.005(2) 0.0061(19) C44A 0.026(3) 0.024(2) 0.023(2) -0.002(2) 0.007(2) 0.006(2) C45A 0.012(2) 0.014(2) 0.022(2) 0.0015(18) 0.0020(18) 0.0031(17) N51A 0.0151(18) 0.0147(18) 0.0173(18) 0.0035(15) 0.0019(15) 0.0006(15) C52A 0.017(2) 0.018(2) 0.015(2) 0.0064(18) 0.0001(17) 0.0010(18) C53A 0.020(2) 0.024(2) 0.020(2) 0.0050(19) 0.0046(18) 0.0025(19) C54A 0.017(2) 0.025(2) 0.025(2) 0.010(2) 0.0087(19) 0.0011(19) C55A 0.018(2) 0.023(2) 0.024(2) 0.008(2) -0.0030(19) -0.0031(19) C56A 0.015(2) 0.017(2) 0.021(2) 0.0039(18) -0.0027(18) 0.0015(17) N61A 0.0181(19) 0.0161(19) 0.0179(19) 0.0007(16) -0.0003(15) 0.0002(15) N62A 0.026(2) 0.018(2) 0.020(2) -0.0022(16) 0.0037(16) 0.0021(16) C63A 0.036(3) 0.012(2) 0.027(3) 0.0010(19) 0.002(2) -0.005(2) C64A 0.030(3) 0.018(2) 0.028(3) 0.003(2) 0.007(2) -0.005(2) C65A 0.015(2) 0.018(2) 0.020(2) 0.0046(18) -0.0030(18) -0.0009(18) C71A 0.022(2) 0.018(2) 0.026(2) -0.0017(19) 0.003(2) 0.0035(19) C72A 0.021(2) 0.017(2) 0.019(2) -0.0043(18) 0.0044(18) 0.0040(18) C73A 0.020(2) 0.021(2) 0.022(2) -0.0073(19) 0.0044(19) -0.0030(19) C74A 0.031(3) 0.014(2) 0.022(2) -0.0028(19) 0.011(2) 0.0001(19) C75A 0.027(3) 0.018(2) 0.018(2) -0.0046(19) 0.0058(19) 0.0037(19) C76A 0.023(2) 0.022(2) 0.021(2) -0.0068(19) 0.0012(19) -0.0008(19) C77A 0.029(3) 0.017(2) 0.019(2) -0.0051(19) 0.004(2) -0.0009(19) C78A 0.037(3) 0.019(2) 0.018(2) -0.0040(19) 0.003(2) 0.006(2) N81A 0.019(2) 0.0146(19) 0.0211(19) 0.0007(15) 0.0004(16) 0.0018(15) N82A 0.028(2) 0.0170(19) 0.0177(19) -0.0020(16) 0.0024(16) 0.0036(16) C83A 0.027(3) 0.019(2) 0.027(3) 0.002(2) 0.005(2) 0.003(2) C84A 0.023(2) 0.015(2) 0.025(2) 0.0019(19) -0.001(2) 0.0005(18) C85A 0.020(2) 0.013(2) 0.019(2) -0.0003(18) -0.0025(18) 0.0041(18) N91A 0.0174(19) 0.0125(18) 0.023(2) -0.0007(15) -0.0021(16) -0.0005(15) C92A 0.016(2) 0.013(2) 0.021(2) 0.0047(18) -0.0043(18) 0.0016(17) C93A 0.015(2) 0.014(2) 0.026(2) 0.0001(18) -0.0003(18) -0.0004(17) C94A 0.023(2) 0.018(2) 0.025(2) -0.0049(19) -0.001(2) 0.0033(19) C95A 0.021(2) 0.027(3) 0.022(2) 0.003(2) 0.0060(19) 0.003(2) C96A 0.016(2) 0.023(3) 0.030(3) 0.006(2) -0.001(2) -0.0014(19) N11B 0.023(2) 0.0171(19) 0.022(2) -0.0004(16) -0.0027(16) 0.0014(16) C12B 0.021(2) 0.013(2) 0.022(2) -0.0057(18) -0.0047(19) -0.0007(18) C13B 0.029(3) 0.018(2) 0.025(2) -0.001(2) -0.004(2) 0.005(2) C14B 0.035(3) 0.019(2) 0.026(3) 0.004(2) -0.004(2) -0.001(2) C15B 0.034(3) 0.025(3) 0.026(3) 0.001(2) 0.002(2) -0.002(2) C16B 0.022(3) 0.029(3) 0.033(3) -0.005(2) 0.004(2) 0.000(2) N21B 0.021(2) 0.0168(19) 0.020(2) -0.0005(16) -0.0005(16) 0.0009(15) N22B 0.028(2) 0.0164(19) 0.022(2) -0.0017(16) -0.0013(17) -0.0005(16) C23B 0.022(2) 0.021(2) 0.030(3) -0.004(2) 0.002(2) 0.004(2) C24B 0.022(2) 0.018(2) 0.029(3) -0.004(2) -0.005(2) 0.0038(19) C25B 0.021(2) 0.013(2) 0.020(2) -0.0009(18) -0.0044(18) 0.0027(18) C31B 0.039(3) 0.022(3) 0.020(2) 0.002(2) -0.001(2) -0.001(2) C32B 0.030(3) 0.021(2) 0.016(2) 0.0023(19) 0.0029(19) 0.001(2) C33B 0.023(3) 0.022(3) 0.035(3) 0.002(2) -0.004(2) 0.003(2) C34B 0.026(3) 0.021(2) 0.033(3) -0.003(2) 0.000(2) 0.005(2) C35B 0.024(2) 0.018(2) 0.018(2) 0.0045(19) 0.0042(19) -0.0010(19) C36B 0.019(2) 0.024(2) 0.020(2) 0.0068(19) 0.0064(19) 0.0006(19) C37B 0.026(3) 0.018(2) 0.022(2) 0.0017(19) 0.007(2) 0.0032(19) C38B 0.023(2) 0.017(2) 0.023(2) 0.0076(19) 0.0052(19) -0.0035(18) N41B 0.0193(19) 0.0131(18) 0.0187(19) 0.0021(15) 0.0009(15) -0.0019(15) N42B 0.0187(19) 0.0148(19) 0.0214(19) 0.0022(16) 0.0030(15) -0.0006(15) C43B 0.026(3) 0.015(2) 0.032(3) 0.001(2) 0.003(2) 0.0027(19) C44B 0.023(3) 0.017(2) 0.035(3) 0.001(2) 0.006(2) 0.0060(19) C45B 0.017(2) 0.017(2) 0.022(2) -0.0045(19) 0.0034(19) -0.0018(18) N51B 0.0175(19) 0.0154(19) 0.0160(18) -0.0010(15) 0.0001(15) -0.0016(15) C52B 0.016(2) 0.015(2) 0.020(2) -0.0055(18) 0.0010(18) -0.0044(17) C53B 0.018(2) 0.023(2) 0.029(3) -0.006(2) 0.007(2) -0.0021(19) C54B 0.021(2) 0.029(3) 0.024(2) -0.005(2) 0.011(2) -0.007(2) C55B 0.023(2) 0.028(3) 0.017(2) 0.0005(19) 0.0053(19) -0.010(2) C56B 0.019(2) 0.020(2) 0.015(2) -0.0028(18) 0.0005(18) -0.0034(18) N61B 0.021(2) 0.0159(19) 0.0173(19) 0.0030(15) -0.0003(16) -0.0007(15) N62B 0.022(2) 0.0174(19) 0.022(2) 0.0018(16) -0.0035(16) -0.0001(16) C63B 0.033(3) 0.022(3) 0.025(3) 0.009(2) -0.001(2) -0.004(2) C64B 0.026(3) 0.031(3) 0.022(2) 0.007(2) 0.004(2) -0.005(2) C65B 0.023(2) 0.018(2) 0.011(2) -0.0015(17) 0.0020(18) -0.0053(18) C71B 0.024(2) 0.018(2) 0.024(2) 0.0019(19) 0.0035(19) 0.0023(19) C72B 0.016(2) 0.021(2) 0.020(2) 0.0035(19) -0.0038(18) 0.0052(18) C73B 0.025(3) 0.023(2) 0.022(2) -0.001(2) -0.001(2) 0.008(2) C74B 0.019(2) 0.027(3) 0.023(2) 0.005(2) 0.0066(19) 0.007(2) C75B 0.016(2) 0.022(2) 0.023(2) 0.005(2) -0.0031(19) 0.0058(18) C76B 0.025(3) 0.019(2) 0.021(2) -0.0028(19) -0.0035(19) 0.0040(19) C77B 0.014(2) 0.024(2) 0.018(2) -0.0010(19) 0.0003(18) 0.0020(18) C78B 0.024(3) 0.036(3) 0.023(2) 0.005(2) -0.003(2) -0.002(2) N81B 0.019(2) 0.019(2) 0.029(2) 0.0041(17) -0.0027(17) -0.0040(16) N82B 0.031(2) 0.021(2) 0.036(2) 0.0077(19) -0.0096(19) -0.0055(18) C83B 0.103(6) 0.024(3) 0.052(4) 0.013(3) -0.030(4) -0.007(3) C84B 0.116(6) 0.016(3) 0.063(4) 0.003(3) -0.039(4) -0.007(3) C85B 0.039(3) 0.017(2) 0.038(3) 0.000(2) -0.015(2) -0.009(2) N91B 0.021(2) 0.0152(19) 0.029(2) -0.0033(16) -0.0047(17) 0.0051(16) C92B 0.024(3) 0.020(2) 0.036(3) -0.002(2) -0.006(2) 0.000(2) C93B 0.041(3) 0.021(3) 0.047(3) -0.006(2) -0.012(3) -0.001(2) C94B 0.028(3) 0.031(3) 0.041(3) -0.015(2) -0.009(2) 0.000(2) C95B 0.027(3) 0.032(3) 0.028(3) -0.007(2) -0.003(2) 0.013(2) C96B 0.031(3) 0.020(2) 0.034(3) -0.004(2) -0.002(2) 0.011(2) Cl1 0.0242(6) 0.0225(6) 0.0316(6) -0.0054(5) 0.0042(5) 0.0033(5) O11 0.145(5) 0.079(4) 0.048(3) 0.022(3) 0.003(3) 0.050(4) O12 0.043(2) 0.029(2) 0.066(3) -0.0079(19) -0.001(2) 0.0146(17) O13 0.063(3) 0.053(3) 0.077(3) -0.042(2) -0.019(2) 0.020(2) O14 0.044(3) 0.083(4) 0.211(7) -0.072(4) 0.058(4) -0.025(3) Cl2 0.0274(6) 0.0195(6) 0.0247(6) -0.0002(5) -0.0001(5) 0.0001(5) O21 0.038(2) 0.043(2) 0.043(2) 0.0200(18) 0.0043(17) -0.0102(18) O22 0.034(2) 0.0234(18) 0.050(2) 0.0146(17) 0.0046(17) 0.0021(15) O23 0.053(3) 0.048(3) 0.049(2) -0.025(2) -0.018(2) 0.008(2) O24 0.0262(19) 0.041(2) 0.0324(19) -0.0086(17) 0.0004(15) 0.0050(16) Cl3 0.0346(6) 0.0161(5) 0.0234(6) 0.0022(5) 0.0085(5) 0.0040(5) O31 0.106(4) 0.021(2) 0.041(2) -0.0059(18) 0.016(2) 0.013(2) O32 0.0267(19) 0.046(2) 0.034(2) 0.0119(17) 0.0083(15) 0.0008(16) O33 0.0320(19) 0.0315(19) 0.0306(19) 0.0014(15) 0.0134(15) -0.0058(15) O34 0.042(2) 0.0291(19) 0.0302(19) 0.0108(16) -0.0023(16) 0.0025(16) Cl4 0.0270(6) 0.0132(5) 0.0248(6) -0.0028(4) 0.0017(5) -0.0011(4) O41 0.036(2) 0.0232(18) 0.038(2) 0.0025(16) 0.0113(16) -0.0037(15) O42 0.057(3) 0.040(2) 0.038(2) 0.0055(18) -0.0184(19) 0.0050(19) O43 0.052(2) 0.0237(19) 0.041(2) -0.0008(16) 0.0213(18) 0.0098(17) O44 0.0267(19) 0.0214(18) 0.052(2) -0.0149(16) 0.0015(16) -0.0070(14) Cl5 0.0248(6) 0.0196(5) 0.0229(6) -0.0016(4) 0.0037(5) 0.0008(4) O51 0.031(2) 0.033(2) 0.044(2) 0.0125(17) 0.0054(16) 0.0110(16) O52 0.048(2) 0.042(2) 0.046(2) 0.0188(19) 0.0107(19) 0.0048(19) O53 0.045(2) 0.044(2) 0.051(2) -0.016(2) -0.0026(19) -0.0097(19) O54 0.037(2) 0.057(3) 0.038(2) -0.0221(19) 0.0078(17) 0.0009(19) Cl6 0.0197(5) 0.0133(5) 0.0246(6) -0.0019(4) 0.0016(4) -0.0019(4) O61 0.0247(17) 0.0163(16) 0.0325(18) -0.0032(14) 0.0057(14) 0.0027(13) O62 0.0290(18) 0.0231(17) 0.0271(18) 0.0058(14) -0.0007(14) -0.0043(14) O63 0.0190(16) 0.0155(16) 0.0373(19) -0.0019(14) 0.0075(14) -0.0023(13) O64 0.0266(18) 0.0189(17) 0.0296(18) -0.0061(14) -0.0041(14) -0.0036(14) N11 0.046(4) 0.072(5) 0.141(7) -0.024(5) 0.011(4) 0.001(3) C12 0.038(4) 0.069(5) 0.068(5) -0.015(4) 0.008(3) 0.007(4) C13 0.040(4) 0.076(5) 0.057(4) -0.006(4) 0.008(3) 0.010(3) N21 0.117(5) 0.049(4) 0.046(3) -0.017(3) -0.006(3) 0.034(4) C22 0.056(4) 0.037(3) 0.027(3) -0.005(2) 0.001(3) 0.010(3) C23 0.034(3) 0.028(3) 0.037(3) -0.001(2) -0.001(2) 0.007(2) N31 0.040(3) 0.062(4) 0.048(3) -0.001(3) 0.012(2) -0.009(3) C32 0.019(3) 0.042(3) 0.046(3) -0.009(3) 0.001(2) -0.004(2) C33 0.025(3) 0.048(4) 0.061(4) 0.007(3) -0.005(3) 0.001(3) N41 0.029(3) 0.044(3) 0.054(3) -0.003(3) 0.012(2) -0.007(2) C42 0.022(3) 0.030(3) 0.046(3) 0.008(3) 0.015(2) 0.000(2) C43 0.043(3) 0.044(3) 0.037(3) 0.000(3) 0.012(3) -0.003(3) N51 0.032(3) 0.035(3) 0.061(3) -0.001(2) 0.004(2) 0.004(2) C52 0.032(3) 0.025(3) 0.045(3) -0.001(2) -0.006(3) 0.000(2) C53 0.071(4) 0.033(3) 0.040(3) 0.003(3) 0.018(3) -0.014(3) N61 0.071(4) 0.053(4) 0.076(4) -0.009(3) -0.011(3) -0.013(3) C62 0.040(4) 0.043(4) 0.062(4) 0.004(3) -0.003(3) -0.004(3) C63 0.035(3) 0.040(3) 0.074(5) -0.010(3) 0.007(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N11B 2.151(4) . ? Hg1 N11A 2.162(4) . ? Hg1 N21A 2.404(4) . ? Hg1 N21B 2.488(4) . ? Hg2 N51A 2.277(3) . ? Hg2 N51B 2.286(3) . ? Hg2 N61B 2.373(3) . ? Hg2 N41A 2.412(3) . ? Hg2 N41B 2.531(3) . ? Hg2 N61A 2.614(3) . ? Hg3 N91A 2.155(3) . ? Hg3 N91B 2.238(4) . ? Hg3 N81B 2.307(4) . ? Hg3 N81A 2.442(4) . ? N11A C16A 1.346(6) . ? N11A C12A 1.364(6) . ? C12A C13A 1.386(6) . ? C12A C25A 1.475(6) . ? C13A C14A 1.386(7) . ? C14A C15A 1.384(8) . ? C15A C16A 1.376(7) . ? N21A C25A 1.327(6) . ? N21A N22A 1.347(5) . ? N22A C23A 1.345(6) . ? N22A C31A 1.447(5) . ? C23A C24A 1.367(7) . ? C24A C25A 1.405(6) . ? C31A C32A 1.516(6) . ? C32A C37A 1.384(6) . ? C32A C33A 1.392(6) . ? C33A C34A 1.382(6) . ? C34A C35A 1.391(6) . ? C35A C36A 1.386(6) . ? C35A C38A 1.506(6) . ? C36A C37A 1.394(6) . ? C38A N42A 1.453(5) . ? N41A C45A 1.338(5) . ? N41A N42A 1.353(5) . ? N42A C43A 1.356(6) . ? C43A C44A 1.365(7) . ? C44A C45A 1.403(6) . ? C45A C52A 1.467(6) . ? N51A C56A 1.345(5) . ? N51A C52A 1.356(5) . ? C52A C53A 1.392(6) . ? C53A C54A 1.377(6) . ? C54A C55A 1.377(6) . ? C55A C56A 1.396(6) . ? C56A C65A 1.469(6) . ? N61A C65A 1.338(5) . ? N61A N62A 1.345(5) . ? N62A C63A 1.351(6) . ? N62A C71A 1.470(6) . ? C63A C64A 1.357(7) . ? C64A C65A 1.412(6) . ? C71A C72A 1.509(6) . ? C72A C77A 1.393(6) . ? C72A C73A 1.395(6) . ? C73A C74A 1.388(6) . ? C74A C75A 1.386(6) . ? C75A C76A 1.392(6) . ? C75A C78A 1.514(6) . ? C76A C77A 1.387(6) . ? C78A N82A 1.466(5) . ? N81A C85A 1.338(5) . ? N81A N82A 1.345(5) . ? N82A C83A 1.354(6) . ? C83A C84A 1.369(6) . ? C84A C85A 1.400(6) . ? C85A C92A 1.467(6) . ? N91A C96A 1.344(6) . ? N91A C92A 1.353(5) . ? C92A C93A 1.391(6) . ? C93A C94A 1.378(6) . ? C94A C95A 1.380(6) . ? C95A C96A 1.378(6) . ? N11B C16B 1.343(6) . ? N11B C12B 1.351(6) . ? C12B C13B 1.383(6) . ? C12B C25B 1.459(6) . ? C13B C14B 1.377(7) . ? C14B C15B 1.382(7) . ? C15B C16B 1.371(7) . ? N21B C25B 1.339(5) . ? N21B N22B 1.352(5) . ? N22B C23B 1.353(6) . ? N22B C31B 1.464(6) . ? C23B C24B 1.368(7) . ? C24B C25B 1.402(6) . ? C31B C32B 1.510(6) . ? C32B C37B 1.391(6) . ? C32B C33B 1.394(6) . ? C33B C34B 1.390(7) . ? C34B C35B 1.388(6) . ? C35B C36B 1.386(6) . ? C35B C38B 1.512(6) . ? C36B C37B 1.387(6) . ? C38B N42B 1.460(6) . ? N41B C45B 1.336(5) . ? N41B N42B 1.351(5) . ? N42B C43B 1.347(6) . ? C43B C44B 1.362(7) . ? C44B C45B 1.401(6) . ? C45B C52B 1.469(6) . ? N51B C56B 1.347(5) . ? N51B C52B 1.347(5) . ? C52B C53B 1.393(6) . ? C53B C54B 1.390(7) . ? C54B C55B 1.380(7) . ? C55B C56B 1.394(6) . ? C56B C65B 1.467(6) . ? N61B C65B 1.339(6) . ? N61B N62B 1.346(5) . ? N62B C63B 1.351(6) . ? N62B C71B 1.459(6) . ? C63B C64B 1.380(7) . ? C64B C65B 1.405(6) . ? C71B C72B 1.515(6) . ? C72B C77B 1.386(6) . ? C72B C73B 1.401(6) . ? C73B C74B 1.379(7) . ? C74B C75B 1.386(6) . ? C75B C76B 1.387(6) . ? C75B C78B 1.520(6) . ? C76B C77B 1.384(6) . ? C78B N82B 1.460(6) . ? N81B C85B 1.331(6) . ? N81B N82B 1.348(5) . ? N82B C83B 1.344(7) . ? C83B C84B 1.368(9) . ? C84B C85B 1.396(7) . ? C85B C92B 1.462(7) . ? N91B C96B 1.334(6) . ? N91B C92B 1.362(6) . ? C92B C93B 1.387(7) . ? C93B C94B 1.386(7) . ? C94B C95B 1.365(7) . ? C95B C96B 1.385(7) . ? Cl1 O14 1.409(5) . ? Cl1 O11 1.411(5) . ? Cl1 O13 1.415(4) . ? Cl1 O12 1.430(4) . ? Cl2 O23 1.434(4) . ? Cl2 O22 1.435(3) . ? Cl2 O24 1.435(3) . ? Cl2 O21 1.441(4) . ? Cl3 O31 1.430(4) . ? Cl3 O33 1.435(3) . ? Cl3 O34 1.437(3) . ? Cl3 O32 1.451(4) . ? Cl4 O42 1.429(4) . ? Cl4 O44 1.432(3) . ? Cl4 O43 1.438(3) . ? Cl4 O41 1.446(3) . ? Cl5 O53 1.428(4) . ? Cl5 O54 1.429(4) . ? Cl5 O51 1.440(3) . ? Cl5 O52 1.443(4) . ? Cl6 O64 1.433(3) . ? Cl6 O62 1.443(3) . ? Cl6 O61 1.446(3) . ? Cl6 O63 1.449(3) . ? N11 C12 1.150(9) . ? C12 C13 1.483(10) . ? N21 C22 1.128(7) . ? C22 C23 1.451(7) . ? N31 C32 1.133(7) . ? C32 C33 1.466(8) . ? N41 C42 1.137(7) . ? C42 C43 1.455(8) . ? N51 C52 1.166(7) . ? C52 C53 1.446(8) . ? N61 C62 1.153(8) . ? C62 C63 1.433(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 N11B Hg1 N11A 174.46(15) . . ? N11B Hg1 N21A 110.19(13) . . ? N11A Hg1 N21A 73.91(13) . . ? N11B Hg1 N21B 73.34(13) . . ? N11A Hg1 N21B 108.52(13) . . ? N21A Hg1 N21B 116.35(12) . . ? N51A Hg2 N51B 159.61(12) . . ? N51A Hg2 N61B 124.77(12) . . ? N51B Hg2 N61B 70.68(12) . . ? N51A Hg2 N41A 71.23(12) . . ? N51B Hg2 N41A 126.80(12) . . ? N61B Hg2 N41A 85.45(12) . . ? N51A Hg2 N41B 95.17(11) . . ? N51B Hg2 N41B 69.52(12) . . ? N61B Hg2 N41B 139.83(12) . . ? N41A Hg2 N41B 114.62(11) . . ? N51A Hg2 N61A 69.48(12) . . ? N51B Hg2 N61A 93.89(11) . . ? N61B Hg2 N61A 108.24(11) . . ? N41A Hg2 N61A 139.18(11) . . ? N41B Hg2 N61A 79.76(11) . . ? N91A Hg3 N91B 157.94(13) . . ? N91A Hg3 N81B 125.46(13) . . ? N91B Hg3 N81B 73.66(13) . . ? N91A Hg3 N81A 74.34(13) . . ? N91B Hg3 N81A 105.15(13) . . ? N81B Hg3 N81A 124.30(12) . . ? C16A N11A C12A 119.5(4) . . ? C16A N11A Hg1 122.0(3) . . ? C12A N11A Hg1 118.4(3) . . ? N11A C12A C13A 121.0(4) . . ? N11A C12A C25A 117.5(4) . . ? C13A C12A C25A 121.5(4) . . ? C14A C13A C12A 118.8(5) . . ? C15A C14A C13A 119.9(5) . . ? C16A C15A C14A 119.1(5) . . ? N11A C16A C15A 121.7(5) . . ? C25A N21A N22A 105.8(3) . . ? C25A N21A Hg1 110.8(3) . . ? N22A N21A Hg1 143.1(3) . . ? C23A N22A N21A 111.1(4) . . ? C23A N22A C31A 130.5(4) . . ? N21A N22A C31A 118.4(3) . . ? N22A C23A C24A 107.8(4) . . ? C23A C24A C25A 104.6(4) . . ? N21A C25A C24A 110.7(4) . . ? N21A C25A C12A 119.0(4) . . ? C24A C25A C12A 130.2(4) . . ? N22A C31A C32A 113.5(4) . . ? C37A C32A C33A 118.8(4) . . ? C37A C32A C31A 122.6(4) . . ? C33A C32A C31A 118.6(4) . . ? C34A C33A C32A 120.8(4) . . ? C33A C34A C35A 120.5(4) . . ? C36A C35A C34A 118.9(4) . . ? C36A C35A C38A 122.7(4) . . ? C34A C35A C38A 118.4(4) . . ? C35A C36A C37A 120.6(4) . . ? C32A C37A C36A 120.4(4) . . ? N42A C38A C35A 113.7(3) . . ? C45A N41A N42A 105.2(3) . . ? C45A N41A Hg2 113.3(3) . . ? N42A N41A Hg2 139.2(3) . . ? N41A N42A C43A 111.1(4) . . ? N41A N42A C38A 120.1(3) . . ? C43A N42A C38A 128.8(4) . . ? N42A C43A C44A 107.8(4) . . ? C43A C44A C45A 104.8(4) . . ? N41A C45A C44A 111.1(4) . . ? N41A C45A C52A 118.6(4) . . ? C44A C45A C52A 130.3(4) . . ? C56A N51A C52A 119.8(4) . . ? C56A N51A Hg2 121.6(3) . . ? C52A N51A Hg2 118.6(3) . . ? N51A C52A C53A 121.4(4) . . ? N51A C52A C45A 117.0(4) . . ? C53A C52A C45A 121.6(4) . . ? C54A C53A C52A 118.6(4) . . ? C53A C54A C55A 120.1(4) . . ? C54A C55A C56A 119.2(4) . . ? N51A C56A C55A 120.8(4) . . ? N51A C56A C65A 117.7(4) . . ? C55A C56A C65A 121.5(4) . . ? C65A N61A N62A 104.8(3) . . ? C65A N61A Hg2 108.0(3) . . ? N62A N61A Hg2 143.6(3) . . ? N61A N62A C63A 112.1(4) . . ? N61A N62A C71A 120.5(4) . . ? C63A N62A C71A 126.8(4) . . ? N62A C63A C64A 107.5(4) . . ? C63A C64A C65A 104.9(4) . . ? N61A C65A C64A 110.8(4) . . ? N61A C65A C56A 121.2(4) . . ? C64A C65A C56A 128.0(4) . . ? N62A C71A C72A 110.9(4) . . ? C77A C72A C73A 118.5(4) . . ? C77A C72A C71A 121.1(4) . . ? C73A C72A C71A 120.4(4) . . ? C74A C73A C72A 120.6(4) . . ? C75A C74A C73A 120.7(4) . . ? C74A C75A C76A 118.9(4) . . ? C74A C75A C78A 120.1(4) . . ? C76A C75A C78A 121.0(4) . . ? C77A C76A C75A 120.5(4) . . ? C76A C77A C72A 120.7(4) . . ? N82A C78A C75A 110.4(4) . . ? C85A N81A N82A 105.2(3) . . ? C85A N81A Hg3 108.5(3) . . ? N82A N81A Hg3 145.5(3) . . ? N81A N82A C83A 111.6(4) . . ? N81A N82A C78A 120.0(4) . . ? C83A N82A C78A 127.9(4) . . ? N82A C83A C84A 107.3(4) . . ? C83A C84A C85A 104.9(4) . . ? N81A C85A C84A 111.0(4) . . ? N81A C85A C92A 120.0(4) . . ? C84A C85A C92A 129.0(4) . . ? C96A N91A C92A 119.9(4) . . ? C96A N91A Hg3 122.0(3) . . ? C92A N91A Hg3 118.2(3) . . ? N91A C92A C93A 120.2(4) . . ? N91A C92A C85A 118.6(4) . . ? C93A C92A C85A 121.1(4) . . ? C94A C93A C92A 120.2(4) . . ? C93A C94A C95A 118.5(4) . . ? C96A C95A C94A 119.8(4) . . ? N91A C96A C95A 121.4(4) . . ? C16B N11B C12B 119.3(4) . . ? C16B N11B Hg1 120.8(3) . . ? C12B N11B Hg1 119.8(3) . . ? N11B C12B C13B 120.2(4) . . ? N11B C12B C25B 118.0(4) . . ? C13B C12B C25B 121.8(4) . . ? C14B C13B C12B 120.0(4) . . ? C13B C14B C15B 119.4(4) . . ? C16B C15B C14B 118.2(5) . . ? N11B C16B C15B 122.8(5) . . ? C25B N21B N22B 105.6(3) . . ? C25B N21B Hg1 107.5(3) . . ? N22B N21B Hg1 146.6(3) . . ? N21B N22B C23B 111.3(4) . . ? N21B N22B C31B 121.0(4) . . ? C23B N22B C31B 127.3(4) . . ? N22B C23B C24B 107.2(4) . . ? C23B C24B C25B 105.5(4) . . ? N21B C25B C24B 110.3(4) . . ? N21B C25B C12B 121.0(4) . . ? C24B C25B C12B 128.7(4) . . ? N22B C31B C32B 110.7(4) . . ? C37B C32B C33B 119.2(4) . . ? C37B C32B C31B 119.4(4) . . ? C33B C32B C31B 121.4(4) . . ? C34B C33B C32B 119.8(4) . . ? C35B C34B C33B 120.9(4) . . ? C36B C35B C34B 119.1(4) . . ? C36B C35B C38B 120.4(4) . . ? C34B C35B C38B 120.5(4) . . ? C35B C36B C37B 120.5(4) . . ? C36B C37B C32B 120.5(4) . . ? N42B C38B C35B 111.2(4) . . ? C45B N41B N42B 105.2(3) . . ? C45B N41B Hg2 110.1(3) . . ? N42B N41B Hg2 140.6(3) . . ? C43B N42B N41B 111.4(4) . . ? C43B N42B C38B 127.0(4) . . ? N41B N42B C38B 120.6(3) . . ? N42B C43B C44B 107.6(4) . . ? C43B C44B C45B 105.1(4) . . ? N41B C45B C44B 110.7(4) . . ? N41B C45B C52B 120.0(4) . . ? C44B C45B C52B 129.3(4) . . ? C56B N51B C52B 120.3(4) . . ? C56B N51B Hg2 119.2(3) . . ? C52B N51B Hg2 120.2(3) . . ? N51B C52B C53B 120.8(4) . . ? N51B C52B C45B 117.0(4) . . ? C53B C52B C45B 122.2(4) . . ? C54B C53B C52B 119.0(4) . . ? C55B C54B C53B 119.9(4) . . ? C54B C55B C56B 118.6(4) . . ? N51B C56B C55B 121.4(4) . . ? N51B C56B C65B 115.8(4) . . ? C55B C56B C65B 122.7(4) . . ? C65B N61B N62B 106.2(3) . . ? C65B N61B Hg2 115.0(3) . . ? N62B N61B Hg2 137.5(3) . . ? N61B N62B C63B 110.8(4) . . ? N61B N62B C71B 121.1(3) . . ? C63B N62B C71B 127.9(4) . . ? N62B C63B C64B 107.9(4) . . ? C63B C64B C65B 104.5(4) . . ? N61B C65B C64B 110.5(4) . . ? N61B C65B C56B 118.0(4) . . ? C64B C65B C56B 131.4(4) . . ? N62B C71B C72B 114.2(4) . . ? C77B C72B C73B 118.8(4) . . ? C77B C72B C71B 123.1(4) . . ? C73B C72B C71B 118.1(4) . . ? C74B C73B C72B 120.3(4) . . ? C73B C74B C75B 121.1(4) . . ? C74B C75B C76B 118.4(4) . . ? C74B C75B C78B 119.2(4) . . ? C76B C75B C78B 122.3(4) . . ? C77B C76B C75B 121.2(4) . . ? C76B C77B C72B 120.2(4) . . ? N82B C78B C75B 113.8(4) . . ? C85B N81B N82B 106.5(4) . . ? C85B N81B Hg3 113.8(3) . . ? N82B N81B Hg3 139.0(3) . . ? C83B N82B N81B 110.3(4) . . ? C83B N82B C78B 126.9(4) . . ? N81B N82B C78B 122.5(4) . . ? N82B C83B C84B 108.1(5) . . ? C83B C84B C85B 104.9(5) . . ? N81B C85B C84B 110.1(5) . . ? N81B C85B C92B 119.0(4) . . ? C84B C85B C92B 130.9(5) . . ? C96B N91B C92B 119.2(4) . . ? C96B N91B Hg3 124.0(3) . . ? C92B N91B Hg3 116.2(3) . . ? N91B C92B C93B 121.3(5) . . ? N91B C92B C85B 116.5(4) . . ? C93B C92B C85B 122.2(4) . . ? C94B C93B C92B 118.3(5) . . ? C95B C94B C93B 120.2(5) . . ? C94B C95B C96B 119.0(5) . . ? N91B C96B C95B 122.0(5) . . ? O14 Cl1 O11 108.1(4) . . ? O14 Cl1 O13 110.6(3) . . ? O11 Cl1 O13 108.4(3) . . ? O14 Cl1 O12 111.0(3) . . ? O11 Cl1 O12 107.7(3) . . ? O13 Cl1 O12 110.9(2) . . ? O23 Cl2 O22 109.3(2) . . ? O23 Cl2 O24 109.7(2) . . ? O22 Cl2 O24 110.4(2) . . ? O23 Cl2 O21 110.4(3) . . ? O22 Cl2 O21 108.6(2) . . ? O24 Cl2 O21 108.5(2) . . ? O31 Cl3 O33 110.0(2) . . ? O31 Cl3 O34 110.7(2) . . ? O33 Cl3 O34 109.5(2) . . ? O31 Cl3 O32 110.0(3) . . ? O33 Cl3 O32 108.4(2) . . ? O34 Cl3 O32 108.2(2) . . ? O42 Cl4 O44 109.0(2) . . ? O42 Cl4 O43 110.3(2) . . ? O44 Cl4 O43 110.0(2) . . ? O42 Cl4 O41 109.1(2) . . ? O44 Cl4 O41 109.0(2) . . ? O43 Cl4 O41 109.4(2) . . ? O53 Cl5 O54 109.4(2) . . ? O53 Cl5 O51 110.3(2) . . ? O54 Cl5 O51 109.3(2) . . ? O53 Cl5 O52 109.0(2) . . ? O54 Cl5 O52 109.6(2) . . ? O51 Cl5 O52 109.3(2) . . ? O64 Cl6 O62 109.77(19) . . ? O64 Cl6 O61 110.06(19) . . ? O62 Cl6 O61 109.79(19) . . ? O64 Cl6 O63 109.46(19) . . ? O62 Cl6 O63 108.52(19) . . ? O61 Cl6 O63 109.22(18) . . ? N11 C12 C13 178.8(8) . . ? N21 C22 C23 178.0(7) . . ? N31 C32 C33 179.2(7) . . ? N41 C42 C43 178.9(6) . . ? N51 C52 C53 179.3(6) . . ? N61 C62 C63 179.6(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11B Hg1 N11A C16A 39.4(17) . . . . ? N21A Hg1 N11A C16A 177.7(4) . . . . ? N21B Hg1 N11A C16A -69.3(4) . . . . ? N11B Hg1 N11A C12A -140.6(14) . . . . ? N21A Hg1 N11A C12A -2.3(3) . . . . ? N21B Hg1 N11A C12A 110.7(3) . . . . ? C16A N11A C12A C13A -0.6(7) . . . . ? Hg1 N11A C12A C13A 179.4(4) . . . . ? C16A N11A C12A C25A -179.9(4) . . . . ? Hg1 N11A C12A C25A 0.1(5) . . . . ? N11A C12A C13A C14A 0.2(7) . . . . ? C25A C12A C13A C14A 179.6(5) . . . . ? C12A C13A C14A C15A 0.0(8) . . . . ? C13A C14A C15A C16A 0.1(9) . . . . ? C12A N11A C16A C15A 0.7(8) . . . . ? Hg1 N11A C16A C15A -179.3(4) . . . . ? C14A C15A C16A N11A -0.5(9) . . . . ? N11B Hg1 N21A C25A -179.5(3) . . . . ? N11A Hg1 N21A C25A 4.4(3) . . . . ? N21B Hg1 N21A C25A -98.6(3) . . . . ? N11B Hg1 N21A N22A -7.9(5) . . . . ? N11A Hg1 N21A N22A 176.1(5) . . . . ? N21B Hg1 N21A N22A 73.0(5) . . . . ? C25A N21A N22A C23A -0.3(5) . . . . ? Hg1 N21A N22A C23A -172.2(4) . . . . ? C25A N21A N22A C31A -179.1(4) . . . . ? Hg1 N21A N22A C31A 9.0(7) . . . . ? N21A N22A C23A C24A 0.5(5) . . . . ? C31A N22A C23A C24A 179.1(4) . . . . ? N22A C23A C24A C25A -0.5(5) . . . . ? N22A N21A C25A C24A 0.0(5) . . . . ? Hg1 N21A C25A C24A 174.8(3) . . . . ? N22A N21A C25A C12A 179.2(4) . . . . ? Hg1 N21A C25A C12A -6.0(5) . . . . ? C23A C24A C25A N21A 0.3(5) . . . . ? C23A C24A C25A C12A -178.8(5) . . . . ? N11A C12A C25A N21A 4.4(6) . . . . ? C13A C12A C25A N21A -174.9(4) . . . . ? N11A C12A C25A C24A -176.5(5) . . . . ? C13A C12A C25A C24A 4.1(8) . . . . ? C23A N22A C31A C32A 117.1(5) . . . . ? N21A N22A C31A C32A -64.4(5) . . . . ? N22A C31A C32A C37A -14.0(6) . . . . ? N22A C31A C32A C33A 165.8(4) . . . . ? C37A C32A C33A C34A -1.9(6) . . . . ? C31A C32A C33A C34A 178.2(4) . . . . ? C32A C33A C34A C35A 2.2(6) . . . . ? C33A C34A C35A C36A -1.0(6) . . . . ? C33A C34A C35A C38A 177.5(4) . . . . ? C34A C35A C36A C37A -0.6(6) . . . . ? C38A C35A C36A C37A -179.0(4) . . . . ? C33A C32A C37A C36A 0.4(6) . . . . ? C31A C32A C37A C36A -179.8(4) . . . . ? C35A C36A C37A C32A 0.9(6) . . . . ? C36A C35A C38A N42A -18.5(6) . . . . ? C34A C35A C38A N42A 163.0(4) . . . . ? N51A Hg2 N41A C45A 8.7(3) . . . . ? N51B Hg2 N41A C45A -160.5(3) . . . . ? N61B Hg2 N41A C45A 137.8(3) . . . . ? N41B Hg2 N41A C45A -78.4(3) . . . . ? N61A Hg2 N41A C45A 25.0(4) . . . . ? N51A Hg2 N41A N42A 167.7(4) . . . . ? N51B Hg2 N41A N42A -1.4(5) . . . . ? N61B Hg2 N41A N42A -63.1(4) . . . . ? N41B Hg2 N41A N42A 80.7(4) . . . . ? N61A Hg2 N41A N42A -175.9(3) . . . . ? C45A N41A N42A C43A 0.7(5) . . . . ? Hg2 N41A N42A C43A -159.4(3) . . . . ? C45A N41A N42A C38A -177.9(4) . . . . ? Hg2 N41A N42A C38A 21.9(6) . . . . ? C35A C38A N42A N41A -60.2(5) . . . . ? C35A C38A N42A C43A 121.4(5) . . . . ? N41A N42A C43A C44A -0.3(5) . . . . ? C38A N42A C43A C44A 178.1(4) . . . . ? N42A C43A C44A C45A -0.2(5) . . . . ? N42A N41A C45A C44A -0.8(5) . . . . ? Hg2 N41A C45A C44A 165.2(3) . . . . ? N42A N41A C45A C52A -179.5(3) . . . . ? Hg2 N41A C45A C52A -13.6(5) . . . . ? C43A C44A C45A N41A 0.6(5) . . . . ? C43A C44A C45A C52A 179.2(4) . . . . ? N51B Hg2 N51A C56A -31.4(5) . . . . ? N61B Hg2 N51A C56A 104.0(3) . . . . ? N41A Hg2 N51A C56A 174.2(3) . . . . ? N41B Hg2 N51A C56A -71.5(3) . . . . ? N61A Hg2 N51A C56A 5.5(3) . . . . ? N51B Hg2 N51A C52A 151.5(3) . . . . ? N61B Hg2 N51A C52A -73.1(3) . . . . ? N41A Hg2 N51A C52A -2.8(3) . . . . ? N41B Hg2 N51A C52A 111.4(3) . . . . ? N61A Hg2 N51A C52A -171.5(3) . . . . ? C56A N51A C52A C53A 0.3(6) . . . . ? Hg2 N51A C52A C53A 177.4(3) . . . . ? C56A N51A C52A C45A 179.9(4) . . . . ? Hg2 N51A C52A C45A -2.9(5) . . . . ? N41A C45A C52A N51A 11.6(6) . . . . ? C44A C45A C52A N51A -166.9(4) . . . . ? N41A C45A C52A C53A -168.7(4) . . . . ? C44A C45A C52A C53A 12.8(7) . . . . ? N51A C52A C53A C54A 0.5(6) . . . . ? C45A C52A C53A C54A -179.2(4) . . . . ? C52A C53A C54A C55A 0.4(6) . . . . ? C53A C54A C55A C56A -1.9(6) . . . . ? C52A N51A C56A C55A -1.9(6) . . . . ? Hg2 N51A C56A C55A -178.9(3) . . . . ? C52A N51A C56A C65A 177.7(4) . . . . ? Hg2 N51A C56A C65A 0.7(5) . . . . ? C54A C55A C56A N51A 2.7(6) . . . . ? C54A C55A C56A C65A -176.9(4) . . . . ? N51A Hg2 N61A C65A -11.2(3) . . . . ? N51B Hg2 N61A C65A 156.7(3) . . . . ? N61B Hg2 N61A C65A -132.4(3) . . . . ? N41A Hg2 N61A C65A -27.7(3) . . . . ? N41B Hg2 N61A C65A 88.3(3) . . . . ? N51A Hg2 N61A N62A -164.3(5) . . . . ? N51B Hg2 N61A N62A 3.6(5) . . . . ? N61B Hg2 N61A N62A 74.5(5) . . . . ? N41A Hg2 N61A N62A 179.2(4) . . . . ? N41B Hg2 N61A N62A -64.8(4) . . . . ? C65A N61A N62A C63A 0.0(5) . . . . ? Hg2 N61A N62A C63A 153.5(4) . . . . ? C65A N61A N62A C71A 171.7(4) . . . . ? Hg2 N61A N62A C71A -34.7(6) . . . . ? N61A N62A C63A C64A 0.2(5) . . . . ? C71A N62A C63A C64A -170.9(4) . . . . ? N62A C63A C64A C65A -0.2(5) . . . . ? N62A N61A C65A C64A -0.2(5) . . . . ? Hg2 N61A C65A C64A -164.0(3) . . . . ? N62A N61A C65A C56A -179.6(4) . . . . ? Hg2 N61A C65A C56A 16.5(5) . . . . ? C63A C64A C65A N61A 0.3(5) . . . . ? C63A C64A C65A C56A 179.7(4) . . . . ? N51A C56A C65A N61A -13.4(6) . . . . ? C55A C56A C65A N61A 166.2(4) . . . . ? N51A C56A C65A C64A 167.2(4) . . . . ? C55A C56A C65A C64A -13.2(7) . . . . ? N61A N62A C71A C72A -68.6(5) . . . . ? C63A N62A C71A C72A 101.8(5) . . . . ? N62A C71A C72A C77A -58.3(5) . . . . ? N62A C71A C72A C73A 120.9(4) . . . . ? C77A C72A C73A C74A 2.4(6) . . . . ? C71A C72A C73A C74A -176.8(4) . . . . ? C72A C73A C74A C75A 0.2(6) . . . . ? C73A C74A C75A C76A -2.4(6) . . . . ? C73A C74A C75A C78A 176.3(4) . . . . ? C74A C75A C76A C77A 1.9(6) . . . . ? C78A C75A C76A C77A -176.7(4) . . . . ? C75A C76A C77A C72A 0.7(7) . . . . ? C73A C72A C77A C76A -2.9(6) . . . . ? C71A C72A C77A C76A 176.3(4) . . . . ? C74A C75A C78A N82A -66.7(5) . . . . ? C76A C75A C78A N82A 112.0(5) . . . . ? N91A Hg3 N81A C85A -4.1(3) . . . . ? N91B Hg3 N81A C85A 153.0(3) . . . . ? N81B Hg3 N81A C85A -126.6(3) . . . . ? N91A Hg3 N81A N82A -171.1(5) . . . . ? N91B Hg3 N81A N82A -14.0(5) . . . . ? N81B Hg3 N81A N82A 66.3(5) . . . . ? C85A N81A N82A C83A 0.6(5) . . . . ? Hg3 N81A N82A C83A 167.9(4) . . . . ? C85A N81A N82A C78A 173.2(4) . . . . ? Hg3 N81A N82A C78A -19.6(7) . . . . ? C75A C78A N82A N81A -76.8(5) . . . . ? C75A C78A N82A C83A 94.4(5) . . . . ? N81A N82A C83A C84A -0.6(5) . . . . ? C78A N82A C83A C84A -172.4(4) . . . . ? N82A C83A C84A C85A 0.3(5) . . . . ? N82A N81A C85A C84A -0.4(5) . . . . ? Hg3 N81A C85A C84A -172.8(3) . . . . ? N82A N81A C85A C92A 179.1(4) . . . . ? Hg3 N81A C85A C92A 6.6(4) . . . . ? C83A C84A C85A N81A 0.1(5) . . . . ? C83A C84A C85A C92A -179.4(4) . . . . ? N91B Hg3 N91A C96A 90.4(5) . . . . ? N81B Hg3 N91A C96A -56.5(4) . . . . ? N81A Hg3 N91A C96A -177.8(3) . . . . ? N91B Hg3 N91A C92A -90.7(5) . . . . ? N81B Hg3 N91A C92A 122.3(3) . . . . ? N81A Hg3 N91A C92A 1.0(3) . . . . ? C96A N91A C92A C93A 0.6(6) . . . . ? Hg3 N91A C92A C93A -178.2(3) . . . . ? C96A N91A C92A C85A -179.1(4) . . . . ? Hg3 N91A C92A C85A 2.1(5) . . . . ? N81A C85A C92A N91A -6.5(6) . . . . ? C84A C85A C92A N91A 172.9(4) . . . . ? N81A C85A C92A C93A 173.9(4) . . . . ? C84A C85A C92A C93A -6.8(7) . . . . ? N91A C92A C93A C94A -0.6(6) . . . . ? C85A C92A C93A C94A 179.1(4) . . . . ? C92A C93A C94A C95A -0.3(7) . . . . ? C93A C94A C95A C96A 1.2(7) . . . . ? C92A N91A C96A C95A 0.3(6) . . . . ? Hg3 N91A C96A C95A 179.1(3) . . . . ? C94A C95A C96A N91A -1.2(7) . . . . ? N11A Hg1 N11B C16B 72.1(16) . . . . ? N21A Hg1 N11B C16B -65.0(4) . . . . ? N21B Hg1 N11B C16B -177.5(4) . . . . ? N11A Hg1 N11B C12B -105.0(15) . . . . ? N21A Hg1 N11B C12B 118.0(3) . . . . ? N21B Hg1 N11B C12B 5.4(3) . . . . ? C16B N11B C12B C13B -2.3(6) . . . . ? Hg1 N11B C12B C13B 174.8(3) . . . . ? C16B N11B C12B C25B 177.3(4) . . . . ? Hg1 N11B C12B C25B -5.6(5) . . . . ? N11B C12B C13B C14B 0.8(7) . . . . ? C25B C12B C13B C14B -178.7(4) . . . . ? C12B C13B C14B C15B 1.2(7) . . . . ? C13B C14B C15B C16B -1.7(7) . . . . ? C12B N11B C16B C15B 1.8(7) . . . . ? Hg1 N11B C16B C15B -175.3(4) . . . . ? C14B C15B C16B N11B 0.2(7) . . . . ? N11B Hg1 N21B C25B -4.6(3) . . . . ? N11A Hg1 N21B C25B 170.0(3) . . . . ? N21A Hg1 N21B C25B -109.3(3) . . . . ? N11B Hg1 N21B N22B -177.9(5) . . . . ? N11A Hg1 N21B N22B -3.4(5) . . . . ? N21A Hg1 N21B N22B 77.4(5) . . . . ? C25B N21B N22B C23B 0.8(5) . . . . ? Hg1 N21B N22B C23B 174.3(4) . . . . ? C25B N21B N22B C31B 174.5(4) . . . . ? Hg1 N21B N22B C31B -12.1(7) . . . . ? N21B N22B C23B C24B -0.8(5) . . . . ? C31B N22B C23B C24B -173.9(4) . . . . ? N22B C23B C24B C25B 0.4(5) . . . . ? N22B N21B C25B C24B -0.6(5) . . . . ? Hg1 N21B C25B C24B -176.8(3) . . . . ? N22B N21B C25B C12B 179.8(4) . . . . ? Hg1 N21B C25B C12B 3.6(5) . . . . ? C23B C24B C25B N21B 0.1(5) . . . . ? C23B C24B C25B C12B 179.7(4) . . . . ? N11B C12B C25B N21B 0.6(6) . . . . ? C13B C12B C25B N21B -179.8(4) . . . . ? N11B C12B C25B C24B -178.9(4) . . . . ? C13B C12B C25B C24B 0.7(7) . . . . ? N21B N22B C31B C32B -83.0(5) . . . . ? C23B N22B C31B C32B 89.5(5) . . . . ? N22B C31B C32B C37B -65.4(6) . . . . ? N22B C31B C32B C33B 113.0(5) . . . . ? C37B C32B C33B C34B 2.6(7) . . . . ? C31B C32B C33B C34B -175.9(4) . . . . ? C32B C33B C34B C35B 0.0(7) . . . . ? C33B C34B C35B C36B -2.3(7) . . . . ? C33B C34B C35B C38B 176.0(4) . . . . ? C34B C35B C36B C37B 2.0(6) . . . . ? C38B C35B C36B C37B -176.3(4) . . . . ? C35B C36B C37B C32B 0.6(7) . . . . ? C33B C32B C37B C36B -2.9(7) . . . . ? C31B C32B C37B C36B 175.6(4) . . . . ? C36B C35B C38B N42B 120.1(4) . . . . ? C34B C35B C38B N42B -58.2(5) . . . . ? N51A Hg2 N41B C45B 151.1(3) . . . . ? N51B Hg2 N41B C45B -15.1(3) . . . . ? N61B Hg2 N41B C45B -23.2(4) . . . . ? N41A Hg2 N41B C45B -137.2(3) . . . . ? N61A Hg2 N41B C45B 83.0(3) . . . . ? N51A Hg2 N41B N42B -1.5(4) . . . . ? N51B Hg2 N41B N42B -167.6(4) . . . . ? N61B Hg2 N41B N42B -175.7(4) . . . . ? N41A Hg2 N41B N42B 70.2(4) . . . . ? N61A Hg2 N41B N42B -69.5(4) . . . . ? C45B N41B N42B C43B 2.1(5) . . . . ? Hg2 N41B N42B C43B 155.4(3) . . . . ? C45B N41B N42B C38B 171.2(4) . . . . ? Hg2 N41B N42B C38B -35.5(6) . . . . ? C35B C38B N42B C43B 97.5(5) . . . . ? C35B C38B N42B N41B -69.8(5) . . . . ? N41B N42B C43B C44B -1.9(5) . . . . ? C38B N42B C43B C44B -170.2(4) . . . . ? N42B C43B C44B C45B 0.9(5) . . . . ? N42B N41B C45B C44B -1.4(5) . . . . ? Hg2 N41B C45B C44B -163.8(3) . . . . ? N42B N41B C45B C52B 179.4(4) . . . . ? Hg2 N41B C45B C52B 17.0(5) . . . . ? C43B C44B C45B N41B 0.3(5) . . . . ? C43B C44B C45B C52B 179.5(4) . . . . ? N51A Hg2 N51B C56B 142.7(3) . . . . ? N61B Hg2 N51B C56B 0.4(3) . . . . ? N41A Hg2 N51B C56B -68.1(3) . . . . ? N41B Hg2 N51B C56B -174.1(3) . . . . ? N61A Hg2 N51B C56B 108.3(3) . . . . ? N51A Hg2 N51B C52B -30.5(5) . . . . ? N61B Hg2 N51B C52B -172.8(3) . . . . ? N41A Hg2 N51B C52B 118.7(3) . . . . ? N41B Hg2 N51B C52B 12.7(3) . . . . ? N61A Hg2 N51B C52B -64.9(3) . . . . ? C56B N51B C52B C53B -2.0(6) . . . . ? Hg2 N51B C52B C53B 171.1(3) . . . . ? C56B N51B C52B C45B 177.9(4) . . . . ? Hg2 N51B C52B C45B -9.0(5) . . . . ? N41B C45B C52B N51B -7.2(6) . . . . ? C44B C45B C52B N51B 173.8(4) . . . . ? N41B C45B C52B C53B 172.7(4) . . . . ? C44B C45B C52B C53B -6.3(7) . . . . ? N51B C52B C53B C54B 0.5(6) . . . . ? C45B C52B C53B C54B -179.4(4) . . . . ? C52B C53B C54B C55B 1.1(7) . . . . ? C53B C54B C55B C56B -1.2(7) . . . . ? C52B N51B C56B C55B 1.9(6) . . . . ? Hg2 N51B C56B C55B -171.3(3) . . . . ? C52B N51B C56B C65B 179.0(4) . . . . ? Hg2 N51B C56B C65B 5.8(5) . . . . ? C54B C55B C56B N51B -0.3(6) . . . . ? C54B C55B C56B C65B -177.1(4) . . . . ? N51A Hg2 N61B C65B -172.0(3) . . . . ? N51B Hg2 N61B C65B -7.0(3) . . . . ? N41A Hg2 N61B C65B 124.6(3) . . . . ? N41B Hg2 N61B C65B 1.0(4) . . . . ? N61A Hg2 N61B C65B -94.7(3) . . . . ? N51A Hg2 N61B N62B 23.3(4) . . . . ? N51B Hg2 N61B N62B -171.7(4) . . . . ? N41A Hg2 N61B N62B -40.1(4) . . . . ? N41B Hg2 N61B N62B -163.7(3) . . . . ? N61A Hg2 N61B N62B 100.6(4) . . . . ? C65B N61B N62B C63B -0.6(5) . . . . ? Hg2 N61B N62B C63B 165.0(3) . . . . ? C65B N61B N62B C71B -176.6(4) . . . . ? Hg2 N61B N62B C71B -11.0(6) . . . . ? N61B N62B C63B C64B 0.7(5) . . . . ? C71B N62B C63B C64B 176.4(4) . . . . ? N62B C63B C64B C65B -0.5(5) . . . . ? N62B N61B C65B C64B 0.2(5) . . . . ? Hg2 N61B C65B C64B -169.1(3) . . . . ? N62B N61B C65B C56B -178.0(4) . . . . ? Hg2 N61B C65B C56B 12.7(5) . . . . ? C63B C64B C65B N61B 0.2(5) . . . . ? C63B C64B C65B C56B 178.1(4) . . . . ? N51B C56B C65B N61B -12.5(6) . . . . ? C55B C56B C65B N61B 164.5(4) . . . . ? N51B C56B C65B C64B 169.7(4) . . . . ? C55B C56B C65B C64B -13.3(7) . . . . ? N61B N62B C71B C72B -48.3(5) . . . . ? C63B N62B C71B C72B 136.4(4) . . . . ? N62B C71B C72B C77B -22.5(6) . . . . ? N62B C71B C72B C73B 159.6(4) . . . . ? C77B C72B C73B C74B -0.4(6) . . . . ? C71B C72B C73B C74B 177.6(4) . . . . ? C72B C73B C74B C75B 2.0(7) . . . . ? C73B C74B C75B C76B -1.4(7) . . . . ? C73B C74B C75B C78B 176.5(4) . . . . ? C74B C75B C76B C77B -0.9(6) . . . . ? C78B C75B C76B C77B -178.7(4) . . . . ? C75B C76B C77B C72B 2.4(7) . . . . ? C73B C72B C77B C76B -1.8(6) . . . . ? C71B C72B C77B C76B -179.6(4) . . . . ? C74B C75B C78B N82B 150.6(4) . . . . ? C76B C75B C78B N82B -31.5(6) . . . . ? N91A Hg3 N81B C85B 169.2(3) . . . . ? N91B Hg3 N81B C85B 1.5(3) . . . . ? N81A Hg3 N81B C85B -96.0(3) . . . . ? N91A Hg3 N81B N82B -21.8(5) . . . . ? N91B Hg3 N81B N82B 170.5(5) . . . . ? N81A Hg3 N81B N82B 73.0(5) . . . . ? C85B N81B N82B C83B -0.4(6) . . . . ? Hg3 N81B N82B C83B -169.9(5) . . . . ? C85B N81B N82B C78B -174.6(4) . . . . ? Hg3 N81B N82B C78B 15.9(7) . . . . ? C75B C78B N82B C83B 137.0(6) . . . . ? C75B C78B N82B N81B -49.8(6) . . . . ? N81B N82B C83B C84B -0.4(8) . . . . ? C78B N82B C83B C84B 173.5(6) . . . . ? N82B C83B C84B C85B 1.0(9) . . . . ? N82B N81B C85B C84B 1.1(6) . . . . ? Hg3 N81B C85B C84B 173.5(5) . . . . ? N82B N81B C85B C92B -179.5(4) . . . . ? Hg3 N81B C85B C92B -7.0(6) . . . . ? C83B C84B C85B N81B -1.3(8) . . . . ? C83B C84B C85B C92B 179.4(6) . . . . ? N91A Hg3 N91B C96B 23.1(6) . . . . ? N81B Hg3 N91B C96B 175.6(4) . . . . ? N81A Hg3 N91B C96B -62.5(4) . . . . ? N91A Hg3 N91B C92B -148.0(4) . . . . ? N81B Hg3 N91B C92B 4.4(3) . . . . ? N81A Hg3 N91B C92B 126.3(3) . . . . ? C96B N91B C92B C93B -0.3(7) . . . . ? Hg3 N91B C92B C93B 171.3(4) . . . . ? C96B N91B C92B C85B 178.9(4) . . . . ? Hg3 N91B C92B C85B -9.5(6) . . . . ? N81B C85B C92B N91B 11.2(7) . . . . ? C84B C85B C92B N91B -169.5(7) . . . . ? N81B C85B C92B C93B -169.5(5) . . . . ? C84B C85B C92B C93B 9.8(10) . . . . ? N91B C92B C93B C94B -1.4(8) . . . . ? C85B C92B C93B C94B 179.4(5) . . . . ? C92B C93B C94B C95B 2.6(8) . . . . ? C93B C94B C95B C96B -2.1(8) . . . . ? C92B N91B C96B C95B 0.9(7) . . . . ? Hg3 N91B C96B C95B -170.1(3) . . . . ? C94B C95B C96B N91B 0.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.246 _refine_diff_density_min -1.833 _refine_diff_density_rms 0.099 #===END data_imw574 _database_code_depnum_ccdc_archive 'CCDC 609503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H77 Cl4 Hg3 N25 O22' _chemical_formula_weight 2592.33 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' 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 13.9421(4) _cell_length_b 49.7930(14) _cell_length_c 14.8980(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.458(2) _cell_angle_gamma 90.00 _cell_volume 10099.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5080 _exptl_absorpt_coefficient_mu 4.737 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3307 _exptl_absorpt_correction_T_max 0.5368 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 186222 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -64 _diffrn_reflns_limit_k_max 66 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.26 _reflns_number_total 24955 _reflns_number_gt 21551 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0650P)^2^+201.0000P] 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 24955 _refine_ls_number_parameters 1265 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2099 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.004 _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 0.74455(3) 0.365294(7) 0.17399(2) 0.02325(9) Uani 1 1 d . . . Hg2 Hg 0.45456(3) 0.292647(9) 0.57168(3) 0.03413(11) Uani 1 1 d . . . Hg3 Hg 1.26839(3) 0.446343(9) 0.24275(3) 0.03440(11) Uani 1 1 d . . . N11A N 0.3015(8) 0.2842(2) 0.5329(6) 0.039(2) Uani 1 1 d . . . C12A C 0.2604(9) 0.2703(2) 0.4555(7) 0.032(2) Uani 1 1 d . . . C13A C 0.1595(9) 0.2648(2) 0.4352(8) 0.039(3) Uani 1 1 d . . . H13A H 0.1311 0.2545 0.3824 0.046 Uiso 1 1 calc R . . C14A C 0.1015(9) 0.2744(3) 0.4929(9) 0.044(3) Uani 1 1 d . . . H14A H 0.0330 0.2707 0.4803 0.053 Uiso 1 1 calc R . . C15A C 0.1447(10) 0.2896(2) 0.5698(9) 0.043(3) Uani 1 1 d . . . H15A H 0.1058 0.2970 0.6087 0.051 Uiso 1 1 calc R . . C16A C 0.2441(10) 0.2936(3) 0.5881(8) 0.041(3) Uani 1 1 d . . . H16A H 0.2738 0.3034 0.6416 0.049 Uiso 1 1 calc R . . N21A N 0.4121(8) 0.2715(2) 0.4024(6) 0.040(2) Uani 1 1 d . . . N22A N 0.4519(8) 0.2576(2) 0.3423(6) 0.038(2) Uani 1 1 d . . . C23A C 0.3873(10) 0.2391(2) 0.2963(8) 0.043(3) Uani 1 1 d . . . H23A H 0.3982 0.2273 0.2493 0.051 Uiso 1 1 calc R . . C24A C 0.3057(10) 0.2406(2) 0.3295(8) 0.039(3) Uani 1 1 d . . . H24A H 0.2474 0.2303 0.3115 0.047 Uiso 1 1 calc R . . C25A C 0.3250(9) 0.2609(2) 0.3970(7) 0.035(2) Uani 1 1 d . . . C31A C 0.5514(10) 0.2637(4) 0.3270(8) 0.053(4) Uani 1 1 d . . . H31A H 0.5857 0.2467 0.3200 0.064 Uiso 1 1 calc R . . H31B H 0.5897 0.2732 0.3814 0.064 Uiso 1 1 calc R . . C32A C 0.5468(9) 0.2811(3) 0.2413(7) 0.038(3) Uani 1 1 d . . . C33A C 0.5997(11) 0.2737(2) 0.1776(8) 0.042(3) Uani 1 1 d . . . H33A H 0.6371 0.2576 0.1863 0.050 Uiso 1 1 calc R . . C34A C 0.5992(10) 0.2895(2) 0.1006(8) 0.037(3) Uani 1 1 d . . . H34A H 0.6365 0.2840 0.0574 0.045 Uiso 1 1 calc R . . C35A C 0.5451(8) 0.3130(2) 0.0860(7) 0.029(2) Uani 1 1 d . . . C36A C 0.4925(8) 0.3207(3) 0.1512(7) 0.038(3) Uani 1 1 d . . . H36A H 0.4552 0.3369 0.1429 0.046 Uiso 1 1 calc R . . C37A C 0.4944(9) 0.3048(3) 0.2284(8) 0.048(3) Uani 1 1 d . . . H37A H 0.4591 0.3104 0.2730 0.058 Uiso 1 1 calc R . . C38A C 0.5436(9) 0.3301(2) 0.0008(7) 0.033(2) Uani 1 1 d . . . H38A H 0.4936 0.3229 -0.0510 0.039 Uiso 1 1 calc R . . H38B H 0.5241 0.3487 0.0128 0.039 Uiso 1 1 calc R . . N41A N 0.7148(7) 0.34098(16) 0.0345(6) 0.0260(17) Uani 1 1 d . . . N42A N 0.6371(7) 0.33084(18) -0.0251(6) 0.0308(19) Uani 1 1 d . . . C43A C 0.6655(9) 0.3202(2) -0.1003(7) 0.033(2) Uani 1 1 d . . . H43A H 0.6239 0.3119 -0.1519 0.040 Uiso 1 1 calc R . . C44A C 0.7635(11) 0.3236(2) -0.0870(8) 0.041(3) Uani 1 1 d . . . H44A H 0.8049 0.3180 -0.1264 0.050 Uiso 1 1 calc R . . C45A C 0.7918(8) 0.33736(19) -0.0024(7) 0.027(2) Uani 1 1 d . . . N51A N 0.8872(6) 0.36225(16) 0.1214(6) 0.0241(16) Uani 1 1 d . . . C52A C 0.8888(8) 0.3474(2) 0.0466(7) 0.029(2) Uani 1 1 d . . . C53A C 0.9750(9) 0.3420(2) 0.0174(8) 0.035(2) Uani 1 1 d . . . H53A H 0.9743 0.3314 -0.0357 0.042 Uiso 1 1 calc R . . C54A C 1.0619(9) 0.3525(2) 0.0680(8) 0.037(3) Uani 1 1 d . . . H54A H 1.1220 0.3489 0.0501 0.045 Uiso 1 1 calc R . . C55A C 1.0614(8) 0.3682(2) 0.1444(8) 0.033(2) Uani 1 1 d . . . H55A H 1.1207 0.3754 0.1795 0.040 Uiso 1 1 calc R . . C56A C 0.9722(7) 0.3731(2) 0.1690(7) 0.027(2) Uani 1 1 d . . . N61A N 0.8774(6) 0.39417(16) 0.2693(6) 0.0247(16) Uani 1 1 d . . . N62A N 0.8951(6) 0.41254(17) 0.3385(6) 0.0277(17) Uani 1 1 d . . . C63A C 0.9896(8) 0.4200(2) 0.3590(8) 0.034(2) Uani 1 1 d . . . H63A H 1.0185 0.4324 0.4055 0.041 Uiso 1 1 calc R . . C64A C 1.0369(8) 0.4068(2) 0.3017(8) 0.033(2) Uani 1 1 d . . . H64A H 1.1045 0.4079 0.2998 0.040 Uiso 1 1 calc R . . C65A C 0.9644(7) 0.3911(2) 0.2460(7) 0.028(2) Uani 1 1 d . . . C71A C 0.8183(8) 0.4197(2) 0.3863(7) 0.027(2) Uani 1 1 d . . . H71A H 0.7540 0.4191 0.3424 0.033 Uiso 1 1 calc R . . H71B H 0.8291 0.4384 0.4093 0.033 Uiso 1 1 calc R . . C72A C 0.8150(7) 0.4011(2) 0.4671(7) 0.028(2) Uani 1 1 d . . . C73A C 0.8669(7) 0.3772(2) 0.4816(7) 0.028(2) Uani 1 1 d . . . H73A H 0.9070 0.3718 0.4407 0.033 Uiso 1 1 calc R . . C74A C 0.8601(8) 0.3612(2) 0.5567(7) 0.029(2) Uani 1 1 d . . . H74A H 0.8951 0.3447 0.5661 0.035 Uiso 1 1 calc R . . C75A C 0.8030(8) 0.3689(2) 0.6178(7) 0.032(2) Uani 1 1 d . . . C76A C 0.7520(9) 0.3927(2) 0.6022(8) 0.036(2) Uani 1 1 d . . . H76A H 0.7123 0.3981 0.6434 0.043 Uiso 1 1 calc R . . C77A C 0.7571(8) 0.4090(2) 0.5276(8) 0.033(2) Uani 1 1 d . . . H77A H 0.7215 0.4254 0.5180 0.040 Uiso 1 1 calc R . . C78A C 0.7964(9) 0.3516(2) 0.6978(8) 0.036(2) Uani 1 1 d . . . H78A H 0.8624 0.3444 0.7255 0.043 Uiso 1 1 calc R . . H78B H 0.7744 0.3626 0.7449 0.043 Uiso 1 1 calc R . . N81A N 0.7617(7) 0.30521(19) 0.6471(6) 0.0315(19) Uani 1 1 d . . . N82A N 0.7274(7) 0.32894(18) 0.6712(6) 0.0309(19) Uani 1 1 d . . . C83A C 0.6284(8) 0.3300(2) 0.6554(7) 0.033(2) Uani 1 1 d . . . H83A H 0.5897 0.3448 0.6674 0.040 Uiso 1 1 calc R . . C84A C 0.5942(9) 0.3054(2) 0.6183(7) 0.033(2) Uani 1 1 d . . . C85A C 0.6797(9) 0.2907(2) 0.6160(6) 0.032(2) Uani 1 1 d . . . N91A N 0.6020(10) 0.2501(2) 0.5547(6) 0.047(3) Uani 1 1 d . . . C92A C 0.6867(11) 0.2629(2) 0.5793(7) 0.040(3) Uani 1 1 d . . . C93A C 0.7770(12) 0.2524(3) 0.5686(8) 0.047(3) Uani 1 1 d . . . H93A H 0.8362 0.2623 0.5879 0.056 Uiso 1 1 calc R . . C94A C 0.7772(16) 0.2273(3) 0.5290(10) 0.066(5) Uani 1 1 d . . . H94A H 0.8367 0.2195 0.5206 0.080 Uiso 1 1 calc R . . C95A C 0.6904(15) 0.2141(3) 0.5021(9) 0.061(5) Uani 1 1 d . . . H95A H 0.6891 0.1968 0.4745 0.073 Uiso 1 1 calc R . . C96A C 0.6031(14) 0.2257(3) 0.5151(8) 0.059(4) Uani 1 1 d . . . H96A H 0.5431 0.2162 0.4956 0.070 Uiso 1 1 calc R . . N11B N 1.2458(7) 0.48852(19) 0.2423(6) 0.034(2) Uani 1 1 d . . . C12B C 1.1945(8) 0.5011(2) 0.1671(8) 0.030(2) Uani 1 1 d . . . C13B C 1.1848(8) 0.5292(2) 0.1675(8) 0.035(2) Uani 1 1 d . . . H13B H 1.1486 0.5382 0.1146 0.043 Uiso 1 1 calc R . . C14B C 1.2272(10) 0.5437(3) 0.2438(9) 0.046(3) Uani 1 1 d . . . H14B H 1.2218 0.5628 0.2440 0.056 Uiso 1 1 calc R . . C15B C 1.2782(11) 0.5301(3) 0.3211(10) 0.052(3) Uani 1 1 d . . . H15B H 1.3064 0.5397 0.3756 0.062 Uiso 1 1 calc R . . C16B C 1.2873(9) 0.5030(3) 0.3176(9) 0.042(3) Uani 1 1 d . . . H16B H 1.3241 0.4938 0.3698 0.050 Uiso 1 1 calc R . . N21B N 1.1301(6) 0.45953(18) 0.0985(6) 0.0300(18) Uani 1 1 d . . . N22B N 1.0924(6) 0.45041(17) 0.0135(6) 0.0285(18) Uani 1 1 d . . . C23B C 1.0889(7) 0.4698(2) -0.0509(8) 0.031(2) Uani 1 1 d . . . H23B H 1.0654 0.4679 -0.1153 0.038 Uiso 1 1 calc R . . C24B C 1.1252(9) 0.4925(2) -0.0057(8) 0.035(2) Uani 1 1 d . . . H24B H 1.1327 0.5097 -0.0316 0.042 Uiso 1 1 calc R . . C25B C 1.1495(8) 0.4852(2) 0.0878(8) 0.030(2) Uani 1 1 d . . . C31B C 1.0585(7) 0.4227(2) -0.0004(8) 0.028(2) Uani 1 1 d . . . H31C H 1.0961 0.4113 0.0495 0.034 Uiso 1 1 calc R . . H31D H 1.0712 0.4160 -0.0594 0.034 Uiso 1 1 calc R . . C32B C 0.9486(7) 0.4201(2) -0.0020(7) 0.0253(19) Uani 1 1 d . . . C33B C 0.9074(7) 0.43297(19) 0.0643(7) 0.0233(18) Uani 1 1 d . . . H33B H 0.9480 0.4432 0.1115 0.028 Uiso 1 1 calc R . . C34B C 0.8081(8) 0.4309(2) 0.0613(7) 0.029(2) Uani 1 1 d . . . H34B H 0.7810 0.4398 0.1065 0.034 Uiso 1 1 calc R . . C35B C 0.7472(7) 0.4160(2) -0.0067(7) 0.0257(19) Uani 1 1 d . . . C36B C 0.7883(7) 0.40295(19) -0.0720(7) 0.0249(19) Uani 1 1 d . . . H36B H 0.7476 0.3925 -0.1184 0.030 Uiso 1 1 calc R . . C37B C 0.8879(8) 0.40505(19) -0.0703(7) 0.028(2) Uani 1 1 d . . . H37B H 0.9148 0.3962 -0.1157 0.033 Uiso 1 1 calc R . . C38B C 0.6373(7) 0.4151(2) -0.0164(6) 0.0258(19) Uani 1 1 d . . . H38C H 0.6069 0.4295 -0.0586 0.031 Uiso 1 1 calc R . . H38D H 0.6124 0.3977 -0.0445 0.031 Uiso 1 1 calc R . . N41B N 0.6224(6) 0.39819(17) 0.1326(6) 0.0254(17) Uani 1 1 d . . . N42B N 0.6068(6) 0.41808(17) 0.0708(6) 0.0272(17) Uani 1 1 d . . . C43B C 0.5597(8) 0.4387(2) 0.1007(8) 0.035(2) Uani 1 1 d . . . H43B H 0.5411 0.4551 0.0686 0.042 Uiso 1 1 calc R . . C44B C 0.5431(9) 0.4321(2) 0.1852(8) 0.038(3) Uani 1 1 d . . . H44B H 0.5108 0.4426 0.2231 0.045 Uiso 1 1 calc R . . C45B C 0.5843(7) 0.4066(2) 0.2034(7) 0.028(2) Uani 1 1 d . . . N51B N 0.6517(6) 0.36752(17) 0.2852(5) 0.0251(16) Uani 1 1 d . . . C52B C 0.5914(7) 0.3884(2) 0.2825(7) 0.027(2) Uani 1 1 d . . . C53B C 0.5385(8) 0.3923(3) 0.3508(8) 0.037(3) Uani 1 1 d . . . H53B H 0.4961 0.4073 0.3486 0.045 Uiso 1 1 calc R . . C54B C 0.5485(8) 0.3740(3) 0.4213(8) 0.038(3) Uani 1 1 d . . . H54B H 0.5142 0.3765 0.4692 0.046 Uiso 1 1 calc R . . C55B C 0.6099(8) 0.3517(3) 0.4221(7) 0.034(2) Uani 1 1 d . . . H55B H 0.6157 0.3384 0.4688 0.040 Uiso 1 1 calc R . . C56B C 0.6623(7) 0.3495(2) 0.3521(7) 0.027(2) Uani 1 1 d . . . N61B N 0.7731(7) 0.32551(17) 0.2771(6) 0.0295(18) Uani 1 1 d . . . N62B N 0.8271(7) 0.30293(16) 0.2904(6) 0.0313(19) Uani 1 1 d . . . C63B C 0.8182(9) 0.2904(2) 0.3691(7) 0.036(3) Uani 1 1 d . . . H63B H 0.8499 0.2742 0.3930 0.044 Uiso 1 1 calc R . . C64B C 0.7552(9) 0.3052(2) 0.4073(7) 0.034(2) Uani 1 1 d . . . H64B H 0.7336 0.3015 0.4623 0.041 Uiso 1 1 calc R . . C65B C 0.7289(8) 0.3272(2) 0.3481(7) 0.031(2) Uani 1 1 d . . . C71B C 0.8945(9) 0.2963(2) 0.2308(8) 0.036(3) Uani 1 1 d . . . H71C H 0.8677 0.3037 0.1687 0.044 Uiso 1 1 calc R . . H71D H 0.8977 0.2766 0.2251 0.044 Uiso 1 1 calc R . . C72B C 0.9964(9) 0.30690(19) 0.2643(7) 0.031(2) Uani 1 1 d . . . C73B C 1.0714(10) 0.2975(2) 0.2242(8) 0.038(3) Uani 1 1 d . . . H73B H 1.0571 0.2841 0.1778 0.046 Uiso 1 1 calc R . . C74B C 1.1651(10) 0.3070(2) 0.2500(9) 0.045(3) Uani 1 1 d . . . H74B H 1.2147 0.3002 0.2213 0.054 Uiso 1 1 calc R . . C75B C 1.1890(10) 0.3268(2) 0.3187(8) 0.040(3) Uani 1 1 d . . . C76B C 1.1160(10) 0.3362(2) 0.3611(8) 0.040(3) Uani 1 1 d . . . H76B H 1.1312 0.3494 0.4081 0.048 Uiso 1 1 calc R . . C77B C 1.0198(9) 0.3263(2) 0.3346(7) 0.034(2) Uani 1 1 d . . . H77B H 0.9703 0.3326 0.3643 0.041 Uiso 1 1 calc R . . C78B C 1.2933(10) 0.3384(3) 0.3463(10) 0.049(3) Uani 1 1 d . . . H78C H 1.3096 0.3416 0.4135 0.059 Uiso 1 1 calc R . . H78D H 1.3407 0.3252 0.3319 0.059 Uiso 1 1 calc R . . N81B N 1.3144(7) 0.3637(2) 0.2109(7) 0.039(2) Uani 1 1 d . . . N82B N 1.3028(8) 0.3636(2) 0.2985(7) 0.040(2) Uani 1 1 d . . . C83B C 1.2872(8) 0.3887(3) 0.3278(8) 0.039(3) Uani 1 1 d . . . H83B H 1.2757 0.3934 0.3863 0.047 Uiso 1 1 calc R . . C84B C 1.2912(8) 0.4060(2) 0.2576(8) 0.033(2) Uani 1 1 d . . . C85B C 1.3090(7) 0.3892(2) 0.1868(8) 0.031(2) Uani 1 1 d . . . N91B N 1.3134(7) 0.4248(2) 0.0807(7) 0.036(2) Uani 1 1 d . . . C92B C 1.3181(8) 0.3981(2) 0.0953(8) 0.035(2) Uani 1 1 d . . . C93B C 1.3281(10) 0.3803(3) 0.0263(9) 0.048(3) Uani 1 1 d . . . H93B H 1.3283 0.3615 0.0370 0.058 Uiso 1 1 calc R . . C94B C 1.3377(13) 0.3901(4) -0.0586(9) 0.065(5) Uani 1 1 d . . . H94B H 1.3454 0.3783 -0.1066 0.078 Uiso 1 1 calc R . . C95B C 1.3356(10) 0.4180(3) -0.0709(9) 0.053(4) Uani 1 1 d . . . H95B H 1.3442 0.4256 -0.1272 0.063 Uiso 1 1 calc R . . C96B C 1.3209(8) 0.4343(3) -0.0010(9) 0.042(3) Uani 1 1 d . . . H96B H 1.3160 0.4531 -0.0113 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.5786(2) 0.16049(8) 0.3017(2) 0.0519(8) Uani 1 1 d . . . O11 O 0.5206(9) 0.1834(2) 0.3253(7) 0.061(3) Uani 1 1 d . . . O12 O 0.5774(10) 0.1622(2) 0.2059(7) 0.069(3) Uani 1 1 d . . . O13 O 0.5276(10) 0.1354(3) 0.3171(9) 0.077(3) Uani 1 1 d . . . O14 O 0.6721(10) 0.1595(3) 0.3590(9) 0.079(4) Uani 1 1 d . . . Cl2 Cl 0.9199(3) 0.22130(7) 0.3039(2) 0.0477(7) Uani 1 1 d . . . O21 O 0.8223(11) 0.2325(3) 0.2745(11) 0.103(5) Uani 1 1 d . . . O22 O 0.9742(16) 0.2347(2) 0.2504(10) 0.120(7) Uani 1 1 d . . . O23 O 0.9545(8) 0.2268(2) 0.3956(7) 0.055(2) Uani 1 1 d . . . O24 O 0.9200(7) 0.19328(17) 0.2845(6) 0.046(2) Uani 1 1 d . . . Cl3 Cl 0.0255(3) 0.09926(11) 0.2364(3) 0.0758(12) Uani 1 1 d . . . O31 O 0.1067(10) 0.0852(4) 0.2490(10) 0.119(7) Uani 1 1 d . . . O32 O -0.0491(12) 0.0885(4) 0.2673(14) 0.144(9) Uani 1 1 d . . . O33 O -0.0023(15) 0.1084(4) 0.1385(11) 0.133(7) Uani 1 1 d . . . O34 O 0.0508(19) 0.1231(4) 0.2934(13) 0.164(11) Uani 1 1 d . . . Cl4 Cl 0.5536(4) 0.47165(12) 0.4213(4) 0.0448(13) Uani 0.50 1 d PD . . O41 O 0.4743(14) 0.4627(4) 0.3651(14) 0.080 Uiso 0.50 1 d PD . . O42 O 0.5653(15) 0.4547(4) 0.4951(13) 0.080 Uiso 0.50 1 d PD . . O43 O 0.6331(13) 0.4702(4) 0.3922(14) 0.080 Uiso 0.50 1 d PD . . O44 O 0.5379(15) 0.4954(4) 0.4532(14) 0.080 Uiso 0.50 1 d PD . . C1A C 0.7973(13) 0.1347(4) 0.1974(11) 0.069(5) Uani 1 1 d . . . H111 H 0.8537 0.1434 0.2374 0.103 Uiso 1 1 calc R . . H112 H 0.7936 0.1159 0.2160 0.103 Uiso 1 1 calc R . . H113 H 0.7369 0.1440 0.2027 0.103 Uiso 1 1 calc R . . N2A N 0.8083(13) 0.1358(3) 0.1039(11) 0.068(4) Uani 1 1 d . . . O3A O 0.8565(16) 0.1502(4) 0.0734(12) 0.130(8) Uani 1 1 d . . . O4A O 0.7551(13) 0.1187(4) 0.0523(11) 0.116(6) Uani 1 1 d . . . C1B C 0.5437(13) 0.0931(4) 0.1495(10) 0.064(4) Uani 1 1 d . . . H121 H 0.4777 0.0888 0.1140 0.095 Uiso 1 1 calc R . . H122 H 0.5922 0.0888 0.1128 0.095 Uiso 1 1 calc R . . H123 H 0.5475 0.1122 0.1652 0.095 Uiso 1 1 calc R . . N2B N 0.5637(10) 0.0774(3) 0.2320(9) 0.061(3) Uani 1 1 d . . . O3B O 0.6473(11) 0.0758(4) 0.2738(11) 0.109(6) Uani 1 1 d . . . O4B O 0.4960(13) 0.0682(3) 0.2585(10) 0.098(5) Uani 1 1 d . . . Cl5 Cl 0.5678(5) 0.49147(12) -0.0956(5) 0.0531(17) Uani 0.50 1 d PD . . O51 O 0.5871(15) 0.5147(4) -0.1349(14) 0.080 Uiso 0.50 1 d PD . . O52 O 0.6490(13) 0.4803(4) -0.0443(14) 0.080 Uiso 0.50 1 d PD . . O53 O 0.5271(15) 0.4732(4) -0.1641(13) 0.080 Uiso 0.50 1 d PD . . O54 O 0.4971(14) 0.4955(4) -0.0454(14) 0.080 Uiso 0.50 1 d PD . . C200 C 1.3206(17) 0.4468(5) 0.5512(14) 0.100 Uiso 1 1 d DU . . H20A H 1.3375 0.4652 0.5729 0.150 Uiso 1 1 calc R . . H20B H 1.3614 0.4416 0.5082 0.150 Uiso 1 1 calc R . . H20C H 1.3324 0.4345 0.6037 0.150 Uiso 1 1 calc R . . N200 N 1.2330(8) 0.4459(2) 0.5119(7) 0.040(2) Uiso 1 1 d DU . . O201 O 1.2110(11) 0.4470(3) 0.4304(9) 0.100 Uiso 1 1 d DU . . O200 O 1.1706(10) 0.4496(3) 0.5511(11) 0.100 Uiso 1 1 d DU . . 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 0.02949(18) 0.02302(17) 0.01836(17) 0.00019(13) 0.00765(13) 0.00225(13) Hg2 0.0431(2) 0.0352(2) 0.02262(19) 0.00029(16) 0.00381(16) -0.01572(17) Hg3 0.0297(2) 0.0338(2) 0.0409(2) 0.00157(17) 0.01022(17) 0.00557(16) N11A 0.046(6) 0.044(6) 0.023(4) 0.007(4) 0.000(4) -0.015(4) C12A 0.048(6) 0.022(5) 0.021(5) 0.006(4) 0.000(4) -0.011(4) C13A 0.048(7) 0.028(6) 0.035(6) 0.013(5) 0.000(5) -0.007(5) C14A 0.040(6) 0.041(7) 0.045(7) 0.019(6) -0.002(5) -0.009(5) C15A 0.054(7) 0.031(6) 0.046(7) 0.014(5) 0.017(6) 0.004(5) C16A 0.051(7) 0.044(7) 0.029(6) 0.004(5) 0.009(5) -0.014(5) N21A 0.048(6) 0.048(6) 0.019(4) 0.004(4) -0.002(4) -0.018(5) N22A 0.044(6) 0.052(6) 0.019(4) 0.001(4) 0.007(4) -0.011(5) C23A 0.067(8) 0.032(6) 0.029(6) -0.004(5) 0.013(5) -0.013(6) C24A 0.054(7) 0.031(6) 0.029(6) 0.003(5) 0.001(5) -0.015(5) C25A 0.043(6) 0.030(5) 0.026(5) 0.011(4) -0.002(4) -0.013(4) C31A 0.041(7) 0.096(12) 0.019(5) 0.007(6) -0.001(5) -0.010(7) C32A 0.041(6) 0.052(7) 0.021(5) 0.005(5) 0.005(4) -0.008(5) C33A 0.077(9) 0.021(5) 0.029(6) -0.001(4) 0.016(6) -0.002(5) C34A 0.061(8) 0.030(6) 0.025(5) -0.003(4) 0.018(5) 0.004(5) C35A 0.029(5) 0.033(5) 0.024(5) -0.003(4) 0.004(4) -0.004(4) C36A 0.035(6) 0.055(7) 0.025(5) -0.007(5) 0.005(4) 0.012(5) C37A 0.034(6) 0.084(10) 0.030(6) -0.004(6) 0.015(5) 0.002(6) C38A 0.049(6) 0.024(5) 0.022(5) 0.000(4) 0.002(4) 0.007(4) N41A 0.040(5) 0.019(4) 0.021(4) -0.001(3) 0.010(3) -0.001(3) N42A 0.048(5) 0.025(4) 0.019(4) -0.002(3) 0.007(4) -0.004(4) C43A 0.055(7) 0.026(5) 0.019(5) -0.008(4) 0.009(4) -0.006(5) C44A 0.073(9) 0.031(6) 0.026(6) -0.004(5) 0.023(6) -0.003(6) C45A 0.048(6) 0.018(4) 0.018(4) 0.006(4) 0.012(4) 0.004(4) N51A 0.031(4) 0.022(4) 0.022(4) 0.005(3) 0.010(3) 0.003(3) C52A 0.044(6) 0.022(5) 0.025(5) 0.009(4) 0.016(4) 0.003(4) C53A 0.052(7) 0.022(5) 0.037(6) 0.005(4) 0.024(5) 0.014(4) C54A 0.044(6) 0.031(6) 0.046(7) 0.014(5) 0.030(5) 0.014(5) C55A 0.036(6) 0.031(6) 0.035(6) 0.013(4) 0.011(4) 0.005(4) C56A 0.031(5) 0.022(5) 0.027(5) 0.014(4) 0.006(4) 0.006(4) N61A 0.024(4) 0.023(4) 0.025(4) 0.003(3) 0.002(3) 0.002(3) N62A 0.032(4) 0.023(4) 0.028(4) 0.001(3) 0.007(3) 0.002(3) C63A 0.027(5) 0.034(6) 0.042(6) 0.001(5) 0.009(4) -0.003(4) C64A 0.027(5) 0.036(6) 0.035(6) 0.006(5) 0.003(4) -0.004(4) C65A 0.025(5) 0.032(5) 0.025(5) 0.009(4) 0.001(4) 0.002(4) C71A 0.033(5) 0.022(5) 0.027(5) -0.007(4) 0.004(4) 0.001(4) C72A 0.028(5) 0.028(5) 0.028(5) -0.002(4) 0.006(4) -0.003(4) C73A 0.024(5) 0.032(5) 0.028(5) -0.003(4) 0.007(4) 0.003(4) C74A 0.034(5) 0.028(5) 0.025(5) 0.000(4) 0.001(4) -0.001(4) C75A 0.030(5) 0.040(6) 0.023(5) -0.007(4) 0.002(4) -0.015(4) C76A 0.039(6) 0.038(6) 0.035(6) -0.011(5) 0.020(5) -0.007(5) C77A 0.027(5) 0.031(5) 0.043(6) -0.006(5) 0.012(4) 0.002(4) C78A 0.041(6) 0.036(6) 0.029(5) -0.006(5) 0.007(4) -0.016(5) N81A 0.041(5) 0.036(5) 0.016(4) 0.003(3) 0.002(3) -0.005(4) N82A 0.039(5) 0.032(5) 0.021(4) -0.003(4) 0.004(3) -0.010(4) C83A 0.042(6) 0.037(6) 0.020(5) -0.003(4) 0.009(4) -0.012(5) C84A 0.044(6) 0.041(6) 0.015(4) 0.001(4) 0.006(4) -0.014(5) C85A 0.049(6) 0.036(6) 0.009(4) 0.004(4) 0.001(4) -0.008(5) N91A 0.087(8) 0.033(5) 0.020(4) 0.004(4) 0.008(5) -0.025(5) C92A 0.078(9) 0.031(6) 0.011(4) 0.006(4) 0.008(5) -0.017(6) C93A 0.074(9) 0.040(7) 0.027(6) 0.004(5) 0.014(6) 0.005(6) C94A 0.122(15) 0.038(8) 0.040(8) 0.010(6) 0.018(9) 0.011(9) C95A 0.127(15) 0.026(6) 0.030(7) -0.006(5) 0.019(8) -0.007(8) C96A 0.121(14) 0.031(7) 0.023(6) 0.004(5) 0.014(7) -0.027(8) N11B 0.033(5) 0.036(5) 0.033(5) 0.002(4) 0.008(4) 0.008(4) C12B 0.026(5) 0.031(5) 0.035(6) 0.000(4) 0.008(4) 0.001(4) C13B 0.035(6) 0.034(6) 0.037(6) -0.001(5) 0.008(5) 0.000(4) C14B 0.048(7) 0.034(6) 0.052(8) -0.006(6) -0.001(6) 0.005(5) C15B 0.062(9) 0.046(8) 0.046(8) -0.023(6) 0.009(6) -0.005(6) C16B 0.040(6) 0.039(6) 0.043(7) 0.002(5) 0.003(5) 0.007(5) N21B 0.027(4) 0.029(4) 0.033(5) -0.001(4) 0.004(3) -0.001(3) N22B 0.027(4) 0.026(4) 0.034(5) 0.004(4) 0.010(3) -0.001(3) C23B 0.022(5) 0.039(6) 0.032(5) 0.004(4) 0.003(4) 0.003(4) C24B 0.044(6) 0.026(5) 0.038(6) 0.003(4) 0.016(5) -0.008(4) C25B 0.026(5) 0.030(5) 0.036(6) 0.000(4) 0.011(4) 0.005(4) C31B 0.027(5) 0.021(5) 0.037(6) 0.003(4) 0.008(4) 0.002(4) C32B 0.025(5) 0.024(5) 0.028(5) 0.008(4) 0.009(4) 0.004(4) C33B 0.023(4) 0.023(5) 0.024(5) -0.002(4) 0.005(3) -0.004(3) C34B 0.038(6) 0.022(5) 0.027(5) 0.003(4) 0.009(4) 0.008(4) C35B 0.026(5) 0.025(5) 0.024(5) 0.007(4) 0.001(4) 0.006(4) C36B 0.033(5) 0.018(4) 0.023(5) -0.001(4) 0.005(4) -0.001(4) C37B 0.050(6) 0.014(4) 0.022(5) 0.002(4) 0.014(4) 0.002(4) C38B 0.030(5) 0.028(5) 0.020(4) 0.002(4) 0.006(4) -0.001(4) N41B 0.023(4) 0.028(4) 0.024(4) -0.001(3) 0.001(3) 0.001(3) N42B 0.025(4) 0.028(4) 0.027(4) 0.003(3) 0.003(3) 0.004(3) C43B 0.029(5) 0.038(6) 0.038(6) 0.006(5) 0.006(4) 0.016(4) C44B 0.039(6) 0.041(6) 0.035(6) 0.003(5) 0.012(5) 0.015(5) C45B 0.026(5) 0.033(5) 0.023(5) -0.001(4) 0.003(4) 0.001(4) N51B 0.027(4) 0.029(4) 0.019(4) -0.002(3) 0.003(3) -0.004(3) C52B 0.023(5) 0.035(5) 0.021(5) -0.004(4) 0.002(4) 0.000(4) C53B 0.025(5) 0.055(7) 0.032(6) -0.005(5) 0.008(4) 0.001(5) C54B 0.032(6) 0.060(8) 0.025(5) -0.009(5) 0.012(4) -0.008(5) C55B 0.032(5) 0.052(7) 0.018(5) -0.003(4) 0.008(4) -0.012(5) C56B 0.029(5) 0.028(5) 0.022(5) -0.006(4) 0.003(4) -0.003(4) N61B 0.044(5) 0.023(4) 0.023(4) 0.001(3) 0.011(4) -0.003(4) N62B 0.056(6) 0.015(4) 0.024(4) 0.007(3) 0.013(4) 0.002(4) C63B 0.056(7) 0.029(5) 0.021(5) 0.006(4) 0.002(5) -0.007(5) C64B 0.049(7) 0.035(6) 0.019(5) 0.008(4) 0.008(4) -0.005(5) C65B 0.038(6) 0.030(5) 0.022(5) 0.002(4) 0.002(4) -0.008(4) C71B 0.058(7) 0.022(5) 0.032(6) 0.009(4) 0.016(5) 0.010(5) C72B 0.061(7) 0.017(4) 0.020(5) 0.009(4) 0.018(5) 0.008(4) C73B 0.069(8) 0.026(5) 0.028(5) 0.005(4) 0.026(5) 0.015(5) C74B 0.065(8) 0.039(6) 0.040(7) 0.021(5) 0.031(6) 0.032(6) C75B 0.057(7) 0.029(6) 0.037(6) 0.015(5) 0.020(5) 0.015(5) C76B 0.066(8) 0.025(5) 0.035(6) 0.012(5) 0.021(6) 0.016(5) C77B 0.053(7) 0.025(5) 0.027(5) 0.002(4) 0.015(5) 0.010(5) C78B 0.047(7) 0.047(8) 0.055(8) 0.018(6) 0.015(6) 0.020(6) N81B 0.032(5) 0.040(5) 0.045(6) 0.008(4) 0.010(4) 0.014(4) N82B 0.041(5) 0.037(5) 0.045(6) 0.016(4) 0.013(4) 0.017(4) C83B 0.026(5) 0.051(7) 0.038(6) 0.009(5) 0.005(4) 0.007(5) C84B 0.023(5) 0.037(6) 0.037(6) 0.010(5) 0.001(4) 0.004(4) C85B 0.020(5) 0.038(6) 0.036(6) 0.006(5) 0.005(4) 0.007(4) N91B 0.031(5) 0.040(5) 0.042(5) 0.003(4) 0.018(4) -0.001(4) C92B 0.027(5) 0.042(6) 0.035(6) 0.010(5) 0.007(4) 0.011(4) C93B 0.055(8) 0.045(7) 0.041(7) 0.002(6) 0.000(6) 0.017(6) C94B 0.085(12) 0.080(11) 0.025(6) -0.003(7) 0.002(7) 0.029(9) C95B 0.039(7) 0.086(11) 0.034(7) 0.015(7) 0.009(5) 0.017(7) C96B 0.029(6) 0.051(7) 0.050(7) 0.008(6) 0.015(5) 0.001(5) Cl1 0.0446(17) 0.074(2) 0.0388(16) -0.0074(15) 0.0127(13) 0.0031(15) O11 0.082(8) 0.055(6) 0.045(6) 0.005(5) 0.010(5) 0.010(5) O12 0.099(9) 0.075(8) 0.040(6) -0.002(5) 0.030(6) -0.015(7) O13 0.086(9) 0.070(8) 0.083(9) 0.009(6) 0.039(7) -0.011(6) O14 0.079(8) 0.072(8) 0.076(8) -0.017(6) -0.004(6) 0.012(6) Cl2 0.063(2) 0.0399(16) 0.0378(16) -0.0008(13) 0.0054(14) 0.0006(14) O21 0.100(11) 0.075(9) 0.105(11) -0.022(8) -0.041(9) 0.029(8) O22 0.27(2) 0.036(6) 0.087(9) -0.001(6) 0.122(13) -0.005(9) O23 0.061(6) 0.055(6) 0.043(5) -0.011(4) 0.000(4) -0.004(5) O24 0.058(6) 0.032(4) 0.043(5) -0.001(4) 0.000(4) 0.002(4) Cl3 0.057(2) 0.105(4) 0.064(3) 0.017(2) 0.0106(19) 0.005(2) O31 0.054(8) 0.22(2) 0.078(10) 0.002(11) 0.013(7) 0.036(10) O32 0.088(11) 0.19(2) 0.174(18) 0.114(16) 0.082(12) 0.035(12) O33 0.157(17) 0.158(17) 0.078(10) 0.035(11) 0.014(11) -0.053(14) O34 0.24(3) 0.104(14) 0.097(13) 0.028(11) -0.069(15) -0.057(15) Cl4 0.039(3) 0.045(3) 0.049(3) 0.001(3) 0.006(2) 0.012(2) C1A 0.059(10) 0.103(14) 0.051(9) 0.007(9) 0.026(7) 0.010(9) N2A 0.095(11) 0.052(8) 0.067(9) -0.014(7) 0.037(8) -0.014(7) O3A 0.184(19) 0.119(14) 0.112(13) -0.052(11) 0.086(13) -0.075(14) O4A 0.116(13) 0.157(17) 0.078(10) -0.005(11) 0.024(9) -0.017(12) C1B 0.078(11) 0.072(11) 0.036(7) 0.007(7) 0.002(7) 0.003(8) N2B 0.056(8) 0.067(9) 0.054(8) 0.003(6) 0.000(6) 0.003(6) O3B 0.081(10) 0.130(14) 0.091(10) 0.002(9) -0.039(8) 0.018(9) O4B 0.124(13) 0.097(11) 0.076(9) 0.020(8) 0.031(9) -0.036(9) Cl5 0.059(4) 0.027(3) 0.075(5) 0.016(3) 0.017(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N51A 2.294(8) . ? Hg1 N51B 2.315(8) . ? Hg1 N41B 2.348(8) . ? Hg1 N41A 2.363(8) . ? Hg1 N61B 2.486(8) . ? Hg1 N61A 2.526(8) . ? Hg2 C84A 2.024(11) . ? Hg2 N11A 2.130(10) . ? Hg2 N21A 2.680(9) . ? Hg3 C84B 2.040(11) . ? Hg3 N11B 2.124(10) . ? Hg3 N21B 2.642(9) . ? N11A C16A 1.350(17) . ? N11A C12A 1.359(14) . ? C12A C13A 1.402(16) . ? C12A C25A 1.460(17) . ? C13A C14A 1.386(19) . ? C14A C15A 1.396(19) . ? C15A C16A 1.367(18) . ? N21A C25A 1.312(14) . ? N21A N22A 1.342(15) . ? N22A C23A 1.366(15) . ? N22A C31A 1.484(16) . ? C23A C24A 1.337(19) . ? C24A C25A 1.408(16) . ? C31A C32A 1.532(17) . ? C32A C33A 1.372(17) . ? C32A C37A 1.380(19) . ? C33A C34A 1.388(16) . ? C34A C35A 1.385(16) . ? C35A C36A 1.391(15) . ? C35A C38A 1.526(15) . ? C36A C37A 1.392(18) . ? C38A N42A 1.437(15) . ? N41A C45A 1.321(13) . ? N41A N42A 1.342(12) . ? N42A C43A 1.373(13) . ? C43A C44A 1.349(18) . ? C44A C45A 1.414(15) . ? C45A C52A 1.479(16) . ? N51A C52A 1.341(13) . ? N51A C56A 1.355(13) . ? C52A C53A 1.389(15) . ? C53A C54A 1.383(18) . ? C54A C55A 1.381(17) . ? C55A C56A 1.391(15) . ? C56A C65A 1.479(15) . ? N61A C65A 1.340(13) . ? N61A N62A 1.360(12) . ? N62A C63A 1.340(14) . ? N62A C71A 1.454(13) . ? C63A C64A 1.356(16) . ? C64A C65A 1.400(15) . ? C71A C72A 1.529(14) . ? C72A C73A 1.382(14) . ? C72A C77A 1.391(14) . ? C73A C74A 1.394(15) . ? C74A C75A 1.386(15) . ? C75A C76A 1.376(17) . ? C75A C78A 1.490(15) . ? C76A C77A 1.391(16) . ? C78A N82A 1.480(13) . ? N81A C85A 1.347(14) . ? N81A N82A 1.352(13) . ? N82A C83A 1.351(15) . ? C83A C84A 1.387(15) . ? C84A C85A 1.404(17) . ? C85A C92A 1.502(16) . ? N91A C92A 1.322(16) . ? N91A C96A 1.353(17) . ? C92A C93A 1.40(2) . ? C93A C94A 1.38(2) . ? C94A C95A 1.36(3) . ? C95A C96A 1.40(2) . ? N11B C12B 1.347(14) . ? N11B C16B 1.353(16) . ? C12B C13B 1.405(15) . ? C12B C25B 1.447(15) . ? C13B C14B 1.369(17) . ? C14B C15B 1.39(2) . ? C15B C16B 1.362(18) . ? N21B C25B 1.325(14) . ? N21B N22B 1.340(13) . ? N22B C23B 1.356(14) . ? N22B C31B 1.460(13) . ? C23B C24B 1.358(16) . ? C24B C25B 1.409(16) . ? C31B C32B 1.532(13) . ? C32B C37B 1.394(15) . ? C32B C33B 1.399(13) . ? C33B C34B 1.380(14) . ? C34B C35B 1.387(15) . ? C35B C36B 1.394(14) . ? C35B C38B 1.508(14) . ? C36B C37B 1.387(15) . ? C38B N42B 1.459(12) . ? N41B N42B 1.337(12) . ? N41B C45B 1.347(13) . ? N42B C43B 1.347(13) . ? C43B C44B 1.368(16) . ? C44B C45B 1.396(15) . ? C45B C52B 1.473(14) . ? N51B C56B 1.326(13) . ? N51B C52B 1.333(13) . ? C52B C53B 1.393(14) . ? C53B C54B 1.373(18) . ? C54B C55B 1.403(18) . ? C55B C56B 1.401(14) . ? C56B C65B 1.457(15) . ? N61B C65B 1.335(14) . ? N61B N62B 1.344(12) . ? N62B C63B 1.358(13) . ? N62B C71B 1.464(14) . ? C63B C64B 1.364(17) . ? C64B C65B 1.403(15) . ? C71B C72B 1.496(18) . ? C72B C73B 1.392(15) . ? C72B C77B 1.409(15) . ? C73B C74B 1.36(2) . ? C74B C75B 1.408(19) . ? C75B C76B 1.389(16) . ? C75B C78B 1.54(2) . ? C76B C77B 1.403(18) . ? C78B N82B 1.461(16) . ? N81B C85B 1.318(15) . ? N81B N82B 1.348(14) . ? N82B C83B 1.359(16) . ? C83B C84B 1.364(16) . ? C84B C85B 1.408(16) . ? C85B C92B 1.465(15) . ? N91B C96B 1.329(16) . ? N91B C92B 1.349(15) . ? C92B C93B 1.386(18) . ? C93B C94B 1.39(2) . ? C94B C95B 1.40(2) . ? C95B C96B 1.37(2) . ? Cl1 O14 1.396(13) . ? Cl1 O12 1.427(10) . ? Cl1 O13 1.482(12) . ? Cl1 O11 1.484(11) . ? Cl2 O23 1.374(10) . ? Cl2 O22 1.383(13) . ? Cl2 O24 1.425(9) . ? Cl2 O21 1.448(14) . ? Cl3 O31 1.310(15) . ? Cl3 O32 1.338(14) . ? Cl3 O34 1.46(2) . ? Cl3 O33 1.498(16) . ? Cl4 O43 1.276(17) . ? Cl4 O41 1.312(17) . ? Cl4 O44 1.312(17) . ? Cl4 O42 1.370(17) . ? C1A N2A 1.44(2) . ? N2A O3A 1.143(19) . ? N2A O4A 1.27(2) . ? C1B N2B 1.430(19) . ? N2B O4B 1.192(18) . ? N2B O3B 1.200(17) . ? Cl5 O52 1.342(17) . ? Cl5 O51 1.349(17) . ? Cl5 O54 1.376(17) . ? Cl5 O53 1.393(17) . ? O54 O54 1.41(4) 3_665 ? C200 N200 1.24(2) . ? N200 O200 1.162(13) . ? N200 O201 1.187(13) . ? 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 N51A Hg1 N51B 155.1(3) . . ? N51A Hg1 N41B 126.1(3) . . ? N51B Hg1 N41B 70.7(3) . . ? N51A Hg1 N41A 70.5(3) . . ? N51B Hg1 N41A 129.4(3) . . ? N41B Hg1 N41A 98.4(3) . . ? N51A Hg1 N61B 97.1(3) . . ? N51B Hg1 N61B 68.6(3) . . ? N41B Hg1 N61B 136.8(3) . . ? N41A Hg1 N61B 96.3(3) . . ? N51A Hg1 N61A 69.2(3) . . ? N51B Hg1 N61A 91.5(3) . . ? N41B Hg1 N61A 98.8(3) . . ? N41A Hg1 N61A 139.0(3) . . ? N61B Hg1 N61A 96.1(3) . . ? C84A Hg2 N11A 171.6(5) . . ? C84A Hg2 N21A 116.5(4) . . ? N11A Hg2 N21A 70.2(4) . . ? C84B Hg3 N11B 174.0(4) . . ? C84B Hg3 N21B 113.7(4) . . ? N11B Hg3 N21B 70.7(3) . . ? C16A N11A C12A 119.8(11) . . ? C16A N11A Hg2 117.2(8) . . ? C12A N11A Hg2 123.0(9) . . ? N11A C12A C13A 120.2(11) . . ? N11A C12A C25A 118.0(10) . . ? C13A C12A C25A 121.8(10) . . ? C14A C13A C12A 119.4(11) . . ? C13A C14A C15A 119.3(12) . . ? C16A C15A C14A 118.8(12) . . ? N11A C16A C15A 122.4(12) . . ? C25A N21A N22A 105.2(10) . . ? C25A N21A Hg2 103.2(7) . . ? N22A N21A Hg2 142.3(8) . . ? N21A N22A C23A 111.1(10) . . ? N21A N22A C31A 122.0(10) . . ? C23A N22A C31A 126.8(11) . . ? C24A C23A N22A 107.3(11) . . ? C23A C24A C25A 105.0(11) . . ? N21A C25A C24A 111.3(11) . . ? N21A C25A C12A 121.0(10) . . ? C24A C25A C12A 127.6(10) . . ? N22A C31A C32A 111.8(10) . . ? C33A C32A C37A 118.7(11) . . ? C33A C32A C31A 119.6(12) . . ? C37A C32A C31A 121.7(12) . . ? C32A C33A C34A 120.9(12) . . ? C35A C34A C33A 120.8(11) . . ? C34A C35A C36A 118.5(10) . . ? C34A C35A C38A 120.8(9) . . ? C36A C35A C38A 120.7(10) . . ? C35A C36A C37A 120.0(11) . . ? C32A C37A C36A 121.2(11) . . ? N42A C38A C35A 112.8(9) . . ? C45A N41A N42A 106.6(8) . . ? C45A N41A Hg1 115.6(7) . . ? N42A N41A Hg1 137.6(7) . . ? N41A N42A C43A 110.6(9) . . ? N41A N42A C38A 118.7(8) . . ? C43A N42A C38A 130.3(9) . . ? C44A C43A N42A 107.0(10) . . ? C43A C44A C45A 105.8(10) . . ? N41A C45A C44A 109.9(10) . . ? N41A C45A C52A 119.2(9) . . ? C44A C45A C52A 130.8(10) . . ? C52A N51A C56A 118.9(9) . . ? C52A N51A Hg1 119.4(7) . . ? C56A N51A Hg1 121.3(6) . . ? N51A C52A C53A 122.5(11) . . ? N51A C52A C45A 114.7(9) . . ? C53A C52A C45A 122.8(10) . . ? C54A C53A C52A 118.2(10) . . ? C55A C54A C53A 120.1(10) . . ? C54A C55A C56A 118.7(11) . . ? N51A C56A C55A 121.5(10) . . ? N51A C56A C65A 116.4(9) . . ? C55A C56A C65A 122.1(10) . . ? C65A N61A N62A 104.3(8) . . ? C65A N61A Hg1 112.6(7) . . ? N62A N61A Hg1 143.1(6) . . ? C63A N62A N61A 111.6(9) . . ? C63A N62A C71A 127.8(9) . . ? N61A N62A C71A 120.3(8) . . ? N62A C63A C64A 108.0(10) . . ? C63A C64A C65A 104.9(10) . . ? N61A C65A C64A 111.2(10) . . ? N61A C65A C56A 119.5(9) . . ? C64A C65A C56A 129.3(10) . . ? N62A C71A C72A 112.7(8) . . ? C73A C72A C77A 120.0(10) . . ? C73A C72A C71A 122.8(9) . . ? C77A C72A C71A 117.1(9) . . ? C72A C73A C74A 119.6(9) . . ? C75A C74A C73A 121.0(10) . . ? C76A C75A C74A 118.5(10) . . ? C76A C75A C78A 121.0(10) . . ? C74A C75A C78A 120.5(11) . . ? C75A C76A C77A 121.6(10) . . ? C76A C77A C72A 119.2(10) . . ? N82A C78A C75A 112.0(9) . . ? C85A N81A N82A 103.6(9) . . ? C83A N82A N81A 113.4(9) . . ? C83A N82A C78A 126.6(10) . . ? N81A N82A C78A 119.3(9) . . ? N82A C83A C84A 106.5(10) . . ? C83A C84A C85A 104.5(10) . . ? C83A C84A Hg2 129.5(10) . . ? C85A C84A Hg2 126.0(8) . . ? N81A C85A C84A 112.1(10) . . ? N81A C85A C92A 120.2(11) . . ? C84A C85A C92A 127.7(11) . . ? C92A N91A C96A 117.5(14) . . ? N91A C92A C93A 123.9(12) . . ? N91A C92A C85A 115.0(12) . . ? C93A C92A C85A 121.0(11) . . ? C94A C93A C92A 118.0(15) . . ? C95A C94A C93A 118.7(17) . . ? C94A C95A C96A 120.3(13) . . ? N91A C96A C95A 121.6(15) . . ? C12B N11B C16B 119.9(10) . . ? C12B N11B Hg3 121.0(8) . . ? C16B N11B Hg3 119.1(8) . . ? N11B C12B C13B 119.6(10) . . ? N11B C12B C25B 118.9(10) . . ? C13B C12B C25B 121.5(10) . . ? C14B C13B C12B 120.3(11) . . ? C13B C14B C15B 118.8(12) . . ? C16B C15B C14B 119.2(12) . . ? N11B C16B C15B 122.2(12) . . ? C25B N21B N22B 105.2(9) . . ? C25B N21B Hg3 101.8(7) . . ? N22B N21B Hg3 138.8(7) . . ? N21B N22B C23B 111.9(9) . . ? N21B N22B C31B 120.3(8) . . ? C23B N22B C31B 127.7(9) . . ? N22B C23B C24B 106.9(10) . . ? C23B C24B C25B 105.0(10) . . ? N21B C25B C24B 110.9(10) . . ? N21B C25B C12B 119.6(10) . . ? C24B C25B C12B 129.4(10) . . ? N22B C31B C32B 111.9(8) . . ? C37B C32B C33B 118.9(9) . . ? C37B C32B C31B 120.2(9) . . ? C33B C32B C31B 120.9(9) . . ? C34B C33B C32B 120.3(9) . . ? C33B C34B C35B 121.1(9) . . ? C34B C35B C36B 118.7(9) . . ? C34B C35B C38B 122.5(9) . . ? C36B C35B C38B 118.7(9) . . ? C37B C36B C35B 120.8(9) . . ? C36B C37B C32B 120.2(9) . . ? N42B C38B C35B 113.3(8) . . ? N42B N41B C45B 105.9(8) . . ? N42B N41B Hg1 134.3(6) . . ? C45B N41B Hg1 113.5(6) . . ? N41B N42B C43B 110.9(9) . . ? N41B N42B C38B 120.0(8) . . ? C43B N42B C38B 129.0(9) . . ? N42B C43B C44B 108.1(10) . . ? C43B C44B C45B 104.7(10) . . ? N41B C45B C44B 110.3(9) . . ? N41B C45B C52B 117.7(9) . . ? C44B C45B C52B 132.0(10) . . ? C56B N51B C52B 121.3(9) . . ? C56B N51B Hg1 121.1(7) . . ? C52B N51B Hg1 117.5(7) . . ? N51B C52B C53B 121.0(10) . . ? N51B C52B C45B 116.0(9) . . ? C53B C52B C45B 123.0(10) . . ? C54B C53B C52B 119.1(11) . . ? C53B C54B C55B 119.5(10) . . ? C56B C55B C54B 118.0(10) . . ? N51B C56B C55B 121.1(10) . . ? N51B C56B C65B 117.0(9) . . ? C55B C56B C65B 122.0(10) . . ? C65B N61B N62B 106.0(8) . . ? C65B N61B Hg1 113.5(7) . . ? N62B N61B Hg1 140.2(6) . . ? N61B N62B C63B 111.1(9) . . ? N61B N62B C71B 120.8(8) . . ? C63B N62B C71B 127.6(10) . . ? N62B C63B C64B 107.3(10) . . ? C63B C64B C65B 105.3(9) . . ? N61B C65B C64B 110.3(10) . . ? N61B C65B C56B 119.2(9) . . ? C64B C65B C56B 130.5(10) . . ? N62B C71B C72B 114.0(10) . . ? C73B C72B C77B 118.2(12) . . ? C73B C72B C71B 119.1(10) . . ? C77B C72B C71B 122.7(10) . . ? C74B C73B C72B 121.7(11) . . ? C73B C74B C75B 120.6(11) . . ? C76B C75B C74B 119.0(13) . . ? C76B C75B C78B 119.7(12) . . ? C74B C75B C78B 121.3(11) . . ? C75B C76B C77B 120.1(12) . . ? C76B C77B C72B 120.3(11) . . ? N82B C78B C75B 111.9(10) . . ? C85B N81B N82B 104.8(10) . . ? N81B N82B C83B 111.6(9) . . ? N81B N82B C78B 121.2(11) . . ? C83B N82B C78B 126.5(11) . . ? N82B C83B C84B 107.3(11) . . ? C83B C84B C85B 104.1(10) . . ? C83B C84B Hg3 132.3(10) . . ? C85B C84B Hg3 123.5(8) . . ? N81B C85B C84B 112.2(10) . . ? N81B C85B C92B 122.3(11) . . ? C84B C85B C92B 125.6(10) . . ? C96B N91B C92B 119.0(11) . . ? N91B C92B C93B 121.3(11) . . ? N91B C92B C85B 116.0(10) . . ? C93B C92B C85B 122.7(11) . . ? C92B C93B C94B 119.8(13) . . ? C93B C94B C95B 117.6(13) . . ? C96B C95B C94B 119.3(13) . . ? N91B C96B C95B 122.9(13) . . ? O14 Cl1 O12 114.9(8) . . ? O14 Cl1 O13 107.0(8) . . ? O12 Cl1 O13 107.6(7) . . ? O14 Cl1 O11 111.5(7) . . ? O12 Cl1 O11 107.7(7) . . ? O13 Cl1 O11 107.9(7) . . ? O23 Cl2 O22 111.1(9) . . ? O23 Cl2 O24 112.3(6) . . ? O22 Cl2 O24 109.3(7) . . ? O23 Cl2 O21 109.3(8) . . ? O22 Cl2 O21 103.6(11) . . ? O24 Cl2 O21 110.9(7) . . ? O31 Cl3 O32 116.6(12) . . ? O31 Cl3 O34 105.1(13) . . ? O32 Cl3 O34 103.6(15) . . ? O31 Cl3 O33 109.7(12) . . ? O32 Cl3 O33 113.6(12) . . ? O34 Cl3 O33 107.3(11) . . ? O43 Cl4 O41 116.0(11) . . ? O43 Cl4 O44 113.6(11) . . ? O41 Cl4 O44 110.7(10) . . ? O43 Cl4 O42 106.0(10) . . ? O41 Cl4 O42 103.9(10) . . ? O44 Cl4 O42 105.5(10) . . ? O3A N2A O4A 119.7(17) . . ? O3A N2A C1A 127.3(17) . . ? O4A N2A C1A 113.0(15) . . ? O4B N2B O3B 123.4(17) . . ? O4B N2B C1B 118.3(15) . . ? O3B N2B C1B 118.1(16) . . ? O52 Cl5 O51 112.4(10) . . ? O52 Cl5 O54 111.5(10) . . ? O51 Cl5 O54 110.1(10) . . ? O52 Cl5 O53 107.9(10) . . ? O51 Cl5 O53 109.2(10) . . ? O54 Cl5 O53 105.5(10) . . ? Cl5 O54 O54 132(2) . 3_665 ? O200 N200 O201 116.7(15) . . ? O200 N200 C200 121.8(13) . . ? O201 N200 C200 119.6(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.354 _refine_diff_density_min -3.429 _refine_diff_density_rms 0.250 #===END