# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Mir Wais Hosseini' 'Ernest Graf' 'Nathalie Kyritsakas' 'Guillaume Laugel' 'Jean-Marc Planeix' _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur Institut Le Bel, 4 Strasbourg F-67000 FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: on the formation of tubular coordination networks ; # Attachment 'New CIF for 2-Ag.cif' data_e304a _database_code_depnum_ccdc_archive 'CCDC 616017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C39 H37 Ag N2 O7 S), 3(CH Cl3), 0.5(C2 O2)' _chemical_formula_sum 'C85 H80 Ag2 Cl18 N4 O15 S2' _chemical_formula_weight 2315.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.609(2) _cell_length_b 23.520(5) _cell_length_c 35.590(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.59(3) _cell_angle_gamma 90.00 _cell_volume 9672(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4680 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8553 _exptl_absorpt_correction_T_max 0.9237 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58562 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.55 _reflns_number_total 11092 _reflns_number_gt 7655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1454P)^2^+68.3497P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11092 _refine_ls_number_parameters 523 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2545 _refine_ls_wR_factor_gt 0.2230 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.38518(4) 0.45635(2) 1.003044(12) 0.03793(17) Uani 1 1 d . . . C1 C 0.4042(4) 0.4146(2) 0.76674(14) 0.0225(10) Uani 1 1 d . . . C2 C 0.3724(5) 0.4301(2) 0.80240(14) 0.0258(11) Uani 1 1 d . . . C3 C 0.2834(4) 0.4002(2) 0.81616(13) 0.0230(10) Uani 1 1 d . . . C4 C 0.2244(4) 0.3554(2) 0.79768(14) 0.0242(10) Uani 1 1 d . . . C5 C 0.2561(4) 0.3406(2) 0.76144(14) 0.0231(10) Uani 1 1 d . . . C6 C 0.3441(4) 0.3715(2) 0.74610(13) 0.0209(10) Uani 1 1 d . . . C7 C 0.4309(7) 0.4779(3) 0.82577(18) 0.0419(15) Uani 1 1 d . . . H7A H 0.4919 0.4947 0.8121 0.063 Uiso 0.50 1 calc PR . . H7B H 0.4650 0.4628 0.8500 0.063 Uiso 0.50 1 calc PR . . H7C H 0.3736 0.5071 0.8303 0.063 Uiso 0.50 1 calc PR . . H7D H 0.3951 0.4817 0.8495 0.063 Uiso 0.50 1 calc PR . . H7E H 0.4220 0.5136 0.8116 0.063 Uiso 0.50 1 calc PR . . H7F H 0.5134 0.4693 0.8313 0.063 Uiso 0.50 1 calc PR . . O1 O 0.2563(3) 0.41461(15) 0.85327(9) 0.0256(8) Uani 1 1 d . . . C8 C 0.1729(5) 0.4536(2) 0.85544(14) 0.0263(11) Uani 1 1 d . . . O2 O 0.1115(4) 0.4709(2) 0.82896(11) 0.0418(11) Uani 1 1 d . . . C9 C 0.1657(5) 0.4727(2) 0.89525(14) 0.0229(10) Uani 1 1 d . . . C10 C 0.2541(5) 0.4629(2) 0.92337(14) 0.0260(11) Uani 1 1 d . . . H10 H 0.3216 0.4437 0.9171 0.031 Uiso 1 1 calc R . . N1 N 0.2484(4) 0.4796(2) 0.95949(12) 0.0292(10) Uani 1 1 d . . . C11 C 0.1511(5) 0.5062(3) 0.96802(16) 0.0353(13) Uani 1 1 d . . . H11 H 0.1449 0.5171 0.9934 0.042 Uiso 1 1 calc R . . C12 C 0.0615(5) 0.5181(3) 0.94154(16) 0.0328(12) Uani 1 1 d . . . H12 H -0.0048 0.5377 0.9485 0.039 Uiso 1 1 calc R . . C13 C 0.0674(5) 0.5014(2) 0.90428(14) 0.0250(10) Uani 1 1 d . . . H13 H 0.0058 0.5095 0.8855 0.030 Uiso 1 1 calc R . . C14 C 0.1288(5) 0.3264(3) 0.81604(18) 0.0385(14) Uani 1 1 d . . . H14A H 0.1216 0.3436 0.8408 0.058 Uiso 1 1 calc R . . H14B H 0.1468 0.2859 0.8193 0.058 Uiso 1 1 calc R . . H14C H 0.0557 0.3308 0.8000 0.058 Uiso 1 1 calc R . . C15 C 0.3735(5) 0.3582(2) 0.70643(14) 0.0268(11) Uani 1 1 d . . . H15A H 0.4046 0.3924 0.6953 0.040 Uiso 1 1 calc R . . H15B H 0.3035 0.3459 0.6910 0.040 Uiso 1 1 calc R . . H15C H 0.4315 0.3278 0.7074 0.040 Uiso 1 1 calc R . . C16 C 0.1900(4) 0.2937(3) 0.73895(15) 0.0288(12) Uani 1 1 d . . . H16A H 0.1402 0.3122 0.7183 0.035 Uiso 1 1 calc R . . H16B H 0.1378 0.2755 0.7558 0.035 Uiso 1 1 calc R . . C17 C 0.2573(4) 0.2464(2) 0.72140(14) 0.0240(10) Uani 1 1 d . . . C18 C 0.2301(4) 0.2324(2) 0.68291(15) 0.0259(11) Uani 1 1 d . . . C19 C 0.2898(5) 0.1873(2) 0.66893(14) 0.0248(11) Uani 1 1 d . . . C20 C 0.3778(5) 0.1576(2) 0.68893(15) 0.0269(11) Uani 1 1 d . . . C21 C 0.4058(5) 0.1724(2) 0.72672(15) 0.0271(11) Uani 1 1 d . . . C22 C 0.3420(4) 0.2151(2) 0.74356(14) 0.0246(10) Uani 1 1 d . . . C23 C 0.1392(5) 0.2629(3) 0.65733(16) 0.0346(13) Uani 1 1 d . . . H23A H 0.1401 0.2486 0.6315 0.052 Uiso 1 1 calc R . . H23B H 0.1554 0.3038 0.6578 0.052 Uiso 1 1 calc R . . H23C H 0.0628 0.2560 0.6660 0.052 Uiso 1 1 calc R . . O3 O 0.2630(3) 0.17339(16) 0.63004(10) 0.0264(8) Uani 1 1 d . . . C24 C 0.1761(5) 0.1357(2) 0.62183(15) 0.0285(11) Uani 1 1 d . . . O4 O 0.1200(5) 0.1146(2) 0.64428(11) 0.0521(14) Uani 1 1 d . . . C25 C 0.1599(5) 0.1253(2) 0.58026(14) 0.0257(11) Uani 1 1 d . . . C26 C 0.0650(5) 0.0937(2) 0.56559(15) 0.0284(11) Uani 1 1 d . . . H26 H 0.0149 0.0781 0.5825 0.034 Uiso 1 1 calc R . . N2 N 0.0416(4) 0.0844(2) 0.52849(13) 0.0303(10) Uani 1 1 d . . . C27 C 0.1151(6) 0.1055(3) 0.50513(16) 0.0374(14) Uani 1 1 d . . . H27 H 0.1000 0.0982 0.4789 0.045 Uiso 1 1 calc R . . C28 C 0.2109(6) 0.1370(3) 0.51741(17) 0.0446(16) Uani 1 1 d . . . H28 H 0.2602 0.1517 0.5000 0.054 Uiso 1 1 calc R . . C29 C 0.2342(5) 0.1470(3) 0.55575(16) 0.0335(13) Uani 1 1 d . . . H29 H 0.3003 0.1684 0.5651 0.040 Uiso 1 1 calc R . . C30 C 0.4395(6) 0.1103(3) 0.66918(19) 0.0448(16) Uani 1 1 d . . . H30A H 0.4165 0.0732 0.6786 0.067 Uiso 1 1 calc R . . H30B H 0.5234 0.1149 0.6744 0.067 Uiso 1 1 calc R . . H30C H 0.4180 0.1123 0.6419 0.067 Uiso 1 1 calc R . . C31 C 0.3602(5) 0.2247(3) 0.78559(15) 0.0311(12) Uani 1 1 d . . . H31A H 0.4164 0.2553 0.7911 0.047 Uiso 1 1 calc R . . H31B H 0.3895 0.1897 0.7981 0.047 Uiso 1 1 calc R . . H31C H 0.2865 0.2352 0.7950 0.047 Uiso 1 1 calc R . . C32 C 0.5000 0.1400(3) 0.7500 0.0342(19) Uani 1 2 d S . . H32A H 0.4619 0.1150 0.7674 0.041 Uiso 0.50 1 calc PR . . H32B H 0.5381 0.1150 0.7326 0.041 Uiso 0.50 1 calc PR . . C33 C 0.5000 0.4477(3) 0.7500 0.0283(16) Uani 1 2 d S . . H33A H 0.5370 0.4727 0.7701 0.034 Uiso 0.50 1 calc PR . . H33B H 0.4630 0.4727 0.7299 0.034 Uiso 0.50 1 calc PR . . S1 S 0.29531(14) 0.52315(6) 1.07708(4) 0.0340(3) Uani 1 1 d . . . O5 O 0.2673(5) 0.4687(2) 1.05828(15) 0.0579(8) Uani 1 1 d . . . O6 O 0.2248(5) 0.5677(2) 1.05953(15) 0.0579(8) Uani 1 1 d . . . O7 O 0.4177(5) 0.5354(2) 1.07971(15) 0.0579(8) Uani 1 1 d . . . C34 C 0.2559(8) 0.5154(4) 1.1234(2) 0.0649(9) Uani 1 1 d . . . C35 C 0.1928(8) 0.5577(4) 1.1393(2) 0.0649(9) Uani 1 1 d . . . H35 H 0.1710 0.5906 1.1249 0.078 Uiso 1 1 calc R . . C36 C 0.1619(8) 0.5530(4) 1.1746(2) 0.0649(9) Uani 1 1 d . . . H36 H 0.1192 0.5827 1.1848 0.078 Uiso 1 1 calc R . . C37 C 0.1909(8) 0.5066(4) 1.1956(2) 0.0649(9) Uani 1 1 d D . . C38 C 0.2550(8) 0.4630(4) 1.1806(2) 0.0649(9) Uani 1 1 d . . . H38 H 0.2761 0.4304 1.1954 0.078 Uiso 1 1 calc R . . C39 C 0.2880(8) 0.4670(4) 1.1442(2) 0.0649(9) Uani 1 1 d . . . H39 H 0.3312 0.4375 1.1339 0.078 Uiso 1 1 calc R . . C40 C 0.1517(8) 0.5010(4) 1.2356(2) 0.0649(9) Uani 1 1 d D . . H40A H 0.1801 0.4649 1.2468 0.097 Uiso 0.50 1 calc PR . . H40B H 0.0670 0.5017 1.2341 0.097 Uiso 0.50 1 calc PR . . H40C H 0.1833 0.5326 1.2512 0.097 Uiso 0.50 1 calc PR . . H40D H 0.1068 0.5346 1.2413 0.097 Uiso 0.50 1 calc PR . . H40E H 0.2199 0.4978 1.2540 0.097 Uiso 0.50 1 calc PR . . H40F H 0.1036 0.4669 1.2368 0.097 Uiso 0.50 1 calc PR . . C41 C 0.5088(8) 0.3298(4) 0.9088(3) 0.061(2) Uani 1 1 d . . . H41 H 0.5299 0.3705 0.9054 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.4061(2) 0.32609(11) 0.94240(7) 0.0745(6) Uani 1 1 d . . . Cl2 Cl 0.6352(2) 0.29184(13) 0.92670(9) 0.0943(9) Uani 1 1 d . . . Cl3 Cl 0.4556(3) 0.30280(14) 0.86628(7) 0.0943(9) Uani 1 1 d . . . C42 C 0.2442(9) 0.1599(4) 0.9203(3) 0.080(3) Uani 1 1 d . . . H42 H 0.2277 0.1184 0.9229 0.096 Uiso 1 1 calc R . . Cl4 Cl 0.3886(3) 0.16642(15) 0.91226(9) 0.1014(7) Uani 1 1 d . . . Cl5 Cl 0.1525(4) 0.18528(13) 0.88214(11) 0.1237(14) Uani 1 1 d . . . Cl6 Cl 0.2106(3) 0.19290(15) 0.96154(9) 0.1014(7) Uani 1 1 d . . . C43 C 0.4676(7) 0.8392(3) 0.9520(2) 0.0491(17) Uani 1 1 d . . . H43 H 0.3970 0.8613 0.9426 0.059 Uiso 1 1 calc R . . Cl7 Cl 0.5585(2) 0.83585(10) 0.91569(7) 0.0776(7) Uani 1 1 d . . . Cl8 Cl 0.4236(2) 0.77078(10) 0.96338(10) 0.0900(9) Uani 1 1 d . . . Cl9 Cl 0.5330(3) 0.87380(15) 0.99098(8) 0.1058(11) Uani 1 1 d . . . O9 O -0.0309(13) 0.1668(6) 0.7116(3) 0.080(4) Uani 0.50 1 d PD . . C44 C 0.0465(17) 0.1326(8) 0.7374(5) 0.080(4) Uani 0.50 1 d PD . . 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 0.0435(3) 0.0439(3) 0.0239(2) 0.00393(18) -0.00952(18) 0.0117(2) C1 0.024(2) 0.021(2) 0.022(2) -0.0019(18) 0.0006(19) 0.0057(19) C2 0.031(3) 0.024(3) 0.022(2) -0.005(2) -0.001(2) 0.006(2) C3 0.027(3) 0.027(3) 0.014(2) -0.0042(18) -0.0027(18) 0.009(2) C4 0.021(2) 0.030(3) 0.021(2) -0.006(2) -0.0009(19) 0.004(2) C5 0.017(2) 0.033(3) 0.018(2) -0.010(2) -0.0046(18) 0.007(2) C6 0.019(2) 0.028(2) 0.015(2) -0.0065(18) -0.0030(17) 0.0104(19) C7 0.061(4) 0.032(3) 0.034(3) -0.014(3) 0.007(3) -0.012(3) O1 0.034(2) 0.0294(19) 0.0132(16) -0.0077(14) -0.0002(14) 0.0094(16) C8 0.032(3) 0.026(3) 0.020(2) -0.003(2) -0.001(2) 0.002(2) O2 0.052(3) 0.050(3) 0.0212(19) -0.0086(18) -0.0066(18) 0.026(2) C9 0.033(3) 0.018(2) 0.017(2) -0.0025(18) 0.000(2) 0.005(2) C10 0.031(3) 0.027(3) 0.020(2) -0.0030(19) 0.001(2) 0.010(2) N1 0.037(3) 0.033(2) 0.017(2) -0.0042(18) -0.0036(18) 0.010(2) C11 0.043(3) 0.042(3) 0.022(3) -0.008(2) 0.004(2) 0.014(3) C12 0.036(3) 0.036(3) 0.026(3) -0.006(2) 0.003(2) 0.012(2) C13 0.023(2) 0.031(3) 0.020(2) -0.005(2) 0.0003(19) 0.006(2) C14 0.034(3) 0.046(4) 0.037(3) -0.016(3) 0.014(3) -0.005(3) C15 0.022(2) 0.038(3) 0.020(2) -0.009(2) -0.0001(19) 0.004(2) C16 0.017(2) 0.042(3) 0.027(3) -0.016(2) 0.002(2) 0.000(2) C17 0.017(2) 0.032(3) 0.023(2) -0.012(2) 0.0001(19) -0.005(2) C18 0.021(2) 0.032(3) 0.024(3) -0.009(2) -0.004(2) 0.000(2) C19 0.027(3) 0.025(3) 0.022(2) -0.0093(19) 0.000(2) -0.010(2) C20 0.034(3) 0.017(2) 0.029(3) -0.0081(19) -0.001(2) -0.001(2) C21 0.037(3) 0.018(2) 0.024(3) -0.0021(19) -0.004(2) -0.005(2) C22 0.025(3) 0.025(3) 0.023(2) -0.0069(19) 0.000(2) -0.008(2) C23 0.027(3) 0.044(3) 0.030(3) -0.015(2) -0.011(2) 0.006(2) O3 0.032(2) 0.0296(19) 0.0175(17) -0.0101(14) -0.0010(14) -0.0066(15) C24 0.036(3) 0.026(3) 0.022(3) -0.009(2) -0.003(2) -0.007(2) O4 0.072(3) 0.065(3) 0.019(2) -0.007(2) 0.003(2) -0.042(3) C25 0.030(3) 0.026(3) 0.020(2) -0.0042(19) 0.000(2) -0.002(2) C26 0.035(3) 0.030(3) 0.020(2) -0.004(2) -0.002(2) -0.007(2) N2 0.035(3) 0.033(2) 0.022(2) -0.0057(18) -0.0013(19) -0.004(2) C27 0.046(4) 0.047(4) 0.019(3) -0.006(2) 0.002(2) 0.002(3) C28 0.047(4) 0.064(4) 0.024(3) -0.004(3) 0.012(3) -0.018(3) C29 0.029(3) 0.041(3) 0.030(3) -0.006(2) 0.002(2) -0.007(2) C30 0.053(4) 0.034(3) 0.045(4) -0.020(3) -0.009(3) 0.017(3) C31 0.034(3) 0.040(3) 0.019(2) -0.006(2) -0.004(2) -0.003(2) C32 0.052(5) 0.018(4) 0.030(4) 0.000 -0.010(4) 0.000 C33 0.039(4) 0.021(4) 0.025(4) 0.000 0.003(3) 0.000 S1 0.0435(8) 0.0339(7) 0.0245(7) 0.0015(5) 0.0024(6) 0.0063(6) O5 0.069(2) 0.063(2) 0.0429(16) 0.0087(14) 0.0120(15) 0.0074(16) O6 0.069(2) 0.063(2) 0.0429(16) 0.0087(14) 0.0120(15) 0.0074(16) O7 0.069(2) 0.063(2) 0.0429(16) 0.0087(14) 0.0120(15) 0.0074(16) C34 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C35 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C36 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C37 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C38 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C39 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C40 0.072(2) 0.083(2) 0.0408(16) -0.0188(14) 0.0144(14) -0.0391(19) C41 0.070(5) 0.044(4) 0.072(5) -0.004(4) 0.015(4) -0.004(4) Cl1 0.0839(16) 0.0695(14) 0.0733(15) -0.0047(11) 0.0239(12) -0.0037(12) Cl2 0.0812(17) 0.0883(18) 0.109(2) -0.0319(16) -0.0144(15) 0.0292(14) Cl3 0.123(2) 0.113(2) 0.0450(12) 0.0129(13) 0.0007(13) 0.0050(18) C42 0.090(7) 0.060(6) 0.087(7) 0.002(5) -0.008(6) -0.002(5) Cl4 0.0976(15) 0.1130(17) 0.0978(15) 0.0093(13) 0.0316(12) 0.0145(13) Cl5 0.159(3) 0.0726(18) 0.125(3) 0.0112(17) -0.058(2) 0.0231(19) Cl6 0.0976(15) 0.1130(17) 0.0978(15) 0.0093(13) 0.0316(12) 0.0145(13) C43 0.053(4) 0.046(4) 0.049(4) 0.001(3) 0.008(3) 0.009(3) Cl7 0.0974(18) 0.0639(13) 0.0784(16) -0.0017(11) 0.0444(14) -0.0052(12) Cl8 0.0789(16) 0.0548(13) 0.145(3) 0.0248(14) 0.0545(17) 0.0079(11) Cl9 0.118(2) 0.119(2) 0.0749(18) -0.0396(17) -0.0189(16) 0.0177(19) O9 0.111(9) 0.085(8) 0.047(5) -0.011(5) 0.023(5) -0.046(7) C44 0.111(9) 0.085(8) 0.047(5) -0.011(5) 0.023(5) -0.046(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.171(5) 8_556 ? Ag1 N1 2.178(4) . ? Ag1 O5 2.519(5) . ? C1 C6 1.397(7) . ? C1 C2 1.404(7) . ? C1 C33 1.526(6) . ? C2 C3 1.380(8) . ? C2 C7 1.519(8) . ? C3 C4 1.387(7) . ? C3 O1 1.428(6) . ? C4 C5 1.419(7) . ? C4 C14 1.506(8) . ? C5 C6 1.407(8) . ? C5 C16 1.525(7) . ? C6 C15 1.517(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C7 H7E 0.9800 . ? C7 H7F 0.9800 . ? O1 C8 1.341(6) . ? C8 O2 1.196(7) . ? C8 C9 1.497(7) . ? C9 C10 1.381(7) . ? C9 C13 1.390(7) . ? C10 N1 1.352(7) . ? C10 H10 0.9500 . ? N1 C11 1.352(7) . ? C11 C12 1.362(8) . ? C11 H11 0.9500 . ? C12 C13 1.391(7) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.528(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.406(8) . ? C17 C18 1.414(7) . ? C18 C19 1.387(7) . ? C18 C23 1.506(7) . ? C19 C20 1.377(8) . ? C19 O3 1.427(6) . ? C20 C21 1.396(7) . ? C20 C30 1.531(8) . ? C21 C22 1.415(8) . ? C21 C32 1.512(7) . ? C22 C31 1.507(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O3 C24 1.353(6) . ? C24 O4 1.187(7) . ? C24 C25 1.494(7) . ? C25 C29 1.383(8) . ? C25 C26 1.388(7) . ? C26 N2 1.340(7) . ? C26 H26 0.9500 . ? N2 C27 1.343(8) . ? N2 Ag1 2.171(5) 8_455 ? C27 C28 1.372(9) . ? C27 H27 0.9500 . ? C28 C29 1.385(8) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C21 1.512(7) 2_656 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C1 1.526(6) 2_656 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? S1 O6 1.434(6) . ? S1 O7 1.444(6) . ? S1 O5 1.466(6) . ? S1 C34 1.764(8) . ? C34 C35 1.386(13) . ? C34 C39 1.390(14) . ? C35 C36 1.346(11) . ? C35 H35 0.9500 . ? C36 C37 1.346(14) . ? C36 H36 0.9500 . ? C37 C38 1.403(13) . ? C37 C40 1.541(9) . ? C38 C39 1.386(11) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C40 H40D 0.9800 . ? C40 H40E 0.9800 . ? C40 H40F 0.9800 . ? C41 Cl3 1.701(9) . ? C41 Cl1 1.770(9) . ? C41 Cl2 1.781(9) . ? C41 H41 1.0000 . ? C42 Cl4 1.735(12) . ? C42 Cl6 1.737(12) . ? C42 Cl5 1.747(11) . ? C42 H42 1.0000 . ? C43 Cl9 1.719(8) . ? C43 Cl8 1.748(8) . ? C43 Cl7 1.749(8) . ? C43 H43 1.0000 . ? O9 C44 1.463(17) . ? C44 C44 1.47(4) 2_556 ? 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 N2 Ag1 N1 158.37(18) 8_556 . ? N2 Ag1 O5 102.79(18) 8_556 . ? N1 Ag1 O5 96.47(19) . . ? C6 C1 C2 120.1(5) . . ? C6 C1 C33 120.7(4) . . ? C2 C1 C33 119.0(4) . . ? C3 C2 C1 117.4(5) . . ? C3 C2 C7 119.6(5) . . ? C1 C2 C7 123.0(5) . . ? C2 C3 C4 124.9(5) . . ? C2 C3 O1 116.6(4) . . ? C4 C3 O1 118.4(5) . . ? C3 C4 C5 117.3(5) . . ? C3 C4 C14 119.3(5) . . ? C5 C4 C14 123.4(5) . . ? C6 C5 C4 119.2(4) . . ? C6 C5 C16 121.2(4) . . ? C4 C5 C16 119.5(5) . . ? C1 C6 C5 121.0(4) . . ? C1 C6 C15 119.5(5) . . ? C5 C6 C15 119.5(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C7 H7D 109.5 . . ? H7A C7 H7D 141.1 . . ? H7B C7 H7D 56.3 . . ? H7C C7 H7D 56.3 . . ? C2 C7 H7E 109.5 . . ? H7A C7 H7E 56.3 . . ? H7B C7 H7E 141.1 . . ? H7C C7 H7E 56.3 . . ? H7D C7 H7E 109.5 . . ? C2 C7 H7F 109.5 . . ? H7A C7 H7F 56.3 . . ? H7B C7 H7F 56.3 . . ? H7C C7 H7F 141.1 . . ? H7D C7 H7F 109.5 . . ? H7E C7 H7F 109.5 . . ? C8 O1 C3 116.2(4) . . ? O2 C8 O1 124.5(5) . . ? O2 C8 C9 124.0(5) . . ? O1 C8 C9 111.5(4) . . ? C10 C9 C13 118.8(5) . . ? C10 C9 C8 122.0(5) . . ? C13 C9 C8 119.2(5) . . ? N1 C10 C9 122.6(5) . . ? N1 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 N1 C11 117.8(5) . . ? C10 N1 Ag1 120.3(4) . . ? C11 N1 Ag1 121.6(4) . . ? N1 C11 C12 122.5(5) . . ? N1 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C13 119.8(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C9 C13 C12 118.3(5) . . ? C9 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6 C15 H15A 109.5 . . ? C6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C5 C16 C17 119.3(4) . . ? C5 C16 H16A 107.5 . . ? C17 C16 H16A 107.5 . . ? C5 C16 H16B 107.5 . . ? C17 C16 H16B 107.5 . . ? H16A C16 H16B 107.0 . . ? C22 C17 C18 120.0(5) . . ? C22 C17 C16 120.6(4) . . ? C18 C17 C16 119.3(5) . . ? C19 C18 C17 116.9(5) . . ? C19 C18 C23 119.5(5) . . ? C17 C18 C23 123.6(5) . . ? C20 C19 C18 125.0(5) . . ? C20 C19 O3 117.8(5) . . ? C18 C19 O3 117.0(5) . . ? C19 C20 C21 117.6(5) . . ? C19 C20 C30 119.2(5) . . ? C21 C20 C30 123.2(5) . . ? C20 C21 C22 120.2(5) . . ? C20 C21 C32 119.4(5) . . ? C22 C21 C32 120.4(4) . . ? C17 C22 C21 120.0(5) . . ? C17 C22 C31 120.1(5) . . ? C21 C22 C31 119.8(5) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 O3 C19 116.5(4) . . ? O4 C24 O3 125.1(5) . . ? O4 C24 C25 125.0(5) . . ? O3 C24 C25 109.9(5) . . ? C29 C25 C26 118.8(5) . . ? C29 C25 C24 122.5(5) . . ? C26 C25 C24 118.7(5) . . ? N2 C26 C25 122.4(5) . . ? N2 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C26 N2 C27 118.0(5) . . ? C26 N2 Ag1 124.3(4) . 8_455 ? C27 N2 Ag1 117.4(4) . 8_455 ? N2 C27 C28 123.1(5) . . ? N2 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C27 C28 C29 118.7(6) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C25 C29 C28 119.0(5) . . ? C25 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C20 C30 H30A 109.5 . . ? C20 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C20 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 C31 H31A 109.5 . . ? C22 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C22 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C21 C32 C21 119.6(6) 2_656 . ? C21 C32 H32A 107.4 2_656 . ? C21 C32 H32A 107.4 . . ? C21 C32 H32B 107.4 2_656 . ? C21 C32 H32B 107.4 . . ? H32A C32 H32B 107.0 . . ? C1 C33 C1 118.5(6) . 2_656 ? C1 C33 H33A 107.7 . . ? C1 C33 H33A 107.7 2_656 . ? C1 C33 H33B 107.7 . . ? C1 C33 H33B 107.7 2_656 . ? H33A C33 H33B 107.1 . . ? O6 S1 O7 113.5(3) . . ? O6 S1 O5 110.3(3) . . ? O7 S1 O5 112.1(3) . . ? O6 S1 C34 107.1(4) . . ? O7 S1 C34 107.7(4) . . ? O5 S1 C34 105.7(4) . . ? S1 O5 Ag1 110.1(3) . . ? C35 C34 C39 119.8(8) . . ? C35 C34 S1 120.1(8) . . ? C39 C34 S1 120.2(7) . . ? C36 C35 C34 121.3(10) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C37 C36 C35 120.7(10) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.6(8) . . ? C36 C37 C40 120.1(9) . . ? C38 C37 C40 120.3(9) . . ? C39 C38 C37 120.7(10) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C34 C39 C38 117.9(9) . . ? C34 C39 H39 121.1 . . ? C38 C39 H39 121.1 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C40 H40D 109.5 . . ? H40A C40 H40D 141.1 . . ? H40B C40 H40D 56.3 . . ? H40C C40 H40D 56.3 . . ? C37 C40 H40E 109.5 . . ? H40A C40 H40E 56.3 . . ? H40B C40 H40E 141.1 . . ? H40C C40 H40E 56.3 . . ? H40D C40 H40E 109.5 . . ? C37 C40 H40F 109.5 . . ? H40A C40 H40F 56.3 . . ? H40B C40 H40F 56.3 . . ? H40C C40 H40F 141.1 . . ? H40D C40 H40F 109.5 . . ? H40E C40 H40F 109.5 . . ? Cl3 C41 Cl1 111.9(5) . . ? Cl3 C41 Cl2 110.2(5) . . ? Cl1 C41 Cl2 108.7(5) . . ? Cl3 C41 H41 108.7 . . ? Cl1 C41 H41 108.7 . . ? Cl2 C41 H41 108.7 . . ? Cl4 C42 Cl6 113.6(6) . . ? Cl4 C42 Cl5 111.5(6) . . ? Cl6 C42 Cl5 109.5(6) . . ? Cl4 C42 H42 107.3 . . ? Cl6 C42 H42 107.3 . . ? Cl5 C42 H42 107.3 . . ? Cl9 C43 Cl8 111.4(4) . . ? Cl9 C43 Cl7 111.5(5) . . ? Cl8 C43 Cl7 109.8(4) . . ? Cl9 C43 H43 108.0 . . ? Cl8 C43 H43 108.0 . . ? Cl7 C43 H43 108.0 . . ? O9 C44 C44 86.5(15) . 2_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.764 _refine_diff_density_min -1.250 _refine_diff_density_rms 0.245 # Attachment 'New CIF for 2 .cif' data_e100a _database_code_depnum_ccdc_archive 'CCDC 616018' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C64 H60 N4 O8), (C6), 2(O0.25), 0.25(O4)' _chemical_formula_sum 'C70 H60 N4 O9.50' _chemical_formula_weight 1109.22 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pban _symmetry_space_group_name_Hall '-P 2ab 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' _cell_length_a 17.0505(6) _cell_length_b 17.6067(6) _cell_length_c 12.0448(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3615.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4985 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.86 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.009 _exptl_crystal_density_diffrn 1.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9865 _exptl_absorpt_correction_T_max 0.9932 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43812 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 29.99 _reflns_number_total 5262 _reflns_number_gt 2270 _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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5262 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1995 _refine_ls_R_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.2845 _refine_ls_wR_factor_gt 0.2533 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _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 C1 C 0.1046(2) 0.39941(17) 0.2929(2) 0.0549(8) Uani 1 1 d . . . C2 C 0.1645(2) 0.36547(17) 0.2340(2) 0.0546(8) Uani 1 1 d . . . C3 C 0.18573(18) 0.29056(17) 0.2630(2) 0.0511(8) Uani 1 1 d . . . C4 C 0.14437(17) 0.25237(16) 0.3473(2) 0.0472(7) Uani 1 1 d . . . C5 C 0.08513(17) 0.29037(16) 0.4080(2) 0.0475(7) Uani 1 1 d . . . C6 C 0.06400(18) 0.36493(17) 0.3793(2) 0.0519(8) Uani 1 1 d . . . C7 C 0.2034(2) 0.4072(2) 0.1385(3) 0.0780(11) Uani 1 1 d . . . H7A H 0.1940 0.3802 0.0705 0.117 Uiso 1 1 calc R . . H7B H 0.2588 0.4103 0.1516 0.117 Uiso 1 1 calc R . . H7C H 0.1820 0.4575 0.1329 0.117 Uiso 1 1 calc R . . C8 C 0.2500 0.2500 0.1976(3) 0.0577(11) Uani 1 2 d S . . H8A H 0.2750 0.2871 0.1497 0.069 Uiso 0.50 1 calc PR . . H8B H 0.2250 0.2129 0.1497 0.069 Uiso 0.50 1 calc PR . . C9 C 0.1589(2) 0.16889(15) 0.3684(2) 0.0533(8) Uani 1 1 d . . . H9A H 0.1981 0.1633 0.4250 0.080 Uiso 1 1 calc R . . H9B H 0.1767 0.1452 0.3012 0.080 Uiso 1 1 calc R . . H9C H 0.1111 0.1452 0.3924 0.080 Uiso 1 1 calc R . . C10 C 0.0404(3) 0.2500 0.5000 0.0520(10) Uani 1 2 d S . . H10A H 0.0065 0.2127 0.4651 0.062 Uiso 0.50 1 calc PR . . H10B H 0.0065 0.2873 0.5349 0.062 Uiso 0.50 1 calc PR . . C11 C -0.0035(2) 0.4066(2) 0.4359(3) 0.0720(10) Uani 1 1 d . . . H11A H -0.0515 0.3794 0.4237 0.108 Uiso 1 1 calc R . . H11B H -0.0080 0.4569 0.4056 0.108 Uiso 1 1 calc R . . H11C H 0.0066 0.4099 0.5142 0.108 Uiso 1 1 calc R . . O1 O 0.08624(14) 0.47648(12) 0.26832(19) 0.0645(7) Uani 1 1 d . . . C12 C 0.0281(2) 0.4899(2) 0.1950(3) 0.0655(9) Uani 1 1 d . . . O2 O -0.00781(19) 0.44038(18) 0.1487(2) 0.0923(10) Uani 1 1 d . . . C13 C 0.0148(2) 0.5725(2) 0.1806(3) 0.0666(10) Uani 1 1 d . . . C14 C -0.0454(3) 0.5959(3) 0.1102(3) 0.0889(14) Uani 1 1 d . . . H14 H -0.0751 0.5592 0.0738 0.107 Uiso 1 1 calc R . . N1 N -0.0620(3) 0.6696(3) 0.0931(4) 0.1251(19) Uani 1 1 d . . . C15 C -0.0163(4) 0.7225(3) 0.1470(5) 0.122(2) Uani 1 1 d . . . H15 H -0.0267 0.7738 0.1355 0.146 Uiso 1 1 calc R . . C16 C 0.0416(3) 0.7035(2) 0.2143(4) 0.1012(16) Uani 1 1 d . . . H16 H 0.0713 0.7411 0.2485 0.121 Uiso 1 1 calc R . . C17 C 0.0587(3) 0.6265(2) 0.2346(3) 0.0800(12) Uani 1 1 d . . . H17 H 0.0986 0.6126 0.2832 0.096 Uiso 1 1 calc R . . C18 C 0.2771(9) 0.5336(11) 0.4598(15) 0.178(6) Uiso 0.50 1 d PU . . C19 C 0.2834(7) 0.5464(8) 0.3546(11) 0.120(3) Uiso 0.50 1 d PU . . C20 C 0.2774(18) 0.6068(17) 0.318(3) 0.266(12) Uiso 0.50 1 d PU . . O3 O 0.1938(14) 0.6104(14) 0.970(2) 0.184(8) Uiso 0.25 1 d P . . O4 O 0.2500 0.7500 0.0000 0.324(19) Uiso 0.50 4 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.074(2) 0.0418(16) 0.0485(16) 0.0030(12) -0.0041(14) 0.0115(15) C2 0.071(2) 0.0505(17) 0.0422(15) 0.0098(12) -0.0024(14) 0.0075(15) C3 0.0659(18) 0.0508(17) 0.0366(13) 0.0027(12) -0.0042(12) 0.0082(14) C4 0.0611(17) 0.0402(14) 0.0402(13) -0.0015(11) -0.0064(13) 0.0050(12) C5 0.0614(17) 0.0407(15) 0.0405(14) -0.0024(11) -0.0041(12) 0.0033(13) C6 0.0671(18) 0.0423(16) 0.0464(15) -0.0022(12) -0.0026(13) 0.0080(14) C7 0.098(3) 0.073(2) 0.062(2) 0.0309(17) 0.0113(19) 0.020(2) C8 0.075(3) 0.058(3) 0.040(2) 0.000 0.000 0.011(2) C9 0.0730(19) 0.0404(15) 0.0464(15) -0.0018(12) -0.0039(13) 0.0074(14) C10 0.067(3) 0.040(2) 0.050(2) -0.0016(17) 0.000 0.000 C11 0.096(3) 0.056(2) 0.064(2) 0.0011(15) 0.0141(19) 0.0246(18) O1 0.0828(15) 0.0453(13) 0.0653(14) 0.0111(10) -0.0050(11) 0.0115(11) C12 0.085(2) 0.065(2) 0.0468(17) 0.0054(16) 0.0047(17) 0.0156(19) O2 0.122(2) 0.078(2) 0.0762(17) -0.0053(14) -0.0297(17) 0.0233(17) C13 0.086(2) 0.065(2) 0.0488(17) 0.0135(15) 0.0185(17) 0.0263(19) C14 0.118(3) 0.089(3) 0.060(2) 0.0153(19) 0.010(2) 0.047(3) N1 0.180(5) 0.118(4) 0.077(3) 0.040(3) 0.037(3) 0.096(4) C15 0.184(6) 0.075(3) 0.107(4) 0.046(3) 0.071(4) 0.071(4) C16 0.140(4) 0.051(2) 0.113(4) 0.017(2) 0.049(3) 0.021(3) C17 0.098(3) 0.063(2) 0.079(2) 0.018(2) 0.028(2) 0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(5) . ? C1 C6 1.390(4) . ? C1 O1 1.424(4) . ? C2 C3 1.412(4) . ? C2 C7 1.517(4) . ? C3 C4 1.408(4) . ? C3 C8 1.527(4) . ? C4 C5 1.415(4) . ? C4 C9 1.512(4) . ? C5 C6 1.404(4) . ? C5 C10 1.522(3) . ? C6 C11 1.526(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C3 1.527(4) 2 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C5 1.522(3) 4_556 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? O1 C12 1.348(4) . ? C12 O2 1.202(4) . ? C12 C13 1.483(5) . ? C13 C17 1.374(6) . ? C13 C14 1.394(6) . ? C14 N1 1.344(6) . ? C14 H14 0.9300 . ? N1 C15 1.378(8) . ? C15 C16 1.321(8) . ? C15 H15 0.9300 . ? C16 C17 1.408(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.291(19) . ? C18 C18 1.34(3) 3_556 ? C19 C20 1.16(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 124.4(3) . . ? C2 C1 O1 117.9(3) . . ? C6 C1 O1 117.6(3) . . ? C1 C2 C3 117.8(3) . . ? C1 C2 C7 120.3(3) . . ? C3 C2 C7 121.9(3) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 C8 120.6(2) . . ? C2 C3 C8 119.5(2) . . ? C3 C4 C5 120.3(3) . . ? C3 C4 C9 120.2(3) . . ? C5 C4 C9 119.3(3) . . ? C6 C5 C4 119.9(3) . . ? C6 C5 C10 119.1(2) . . ? C4 C5 C10 120.9(2) . . ? C1 C6 C5 117.7(3) . . ? C1 C6 C11 120.0(3) . . ? C5 C6 C11 122.2(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 C3 117.9(3) . 2 ? C3 C8 H8A 107.8 . . ? C3 C8 H8A 107.8 2 . ? C3 C8 H8B 107.8 . . ? C3 C8 H8B 107.8 2 . ? H8A C8 H8B 107.2 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 C5 119.8(3) . 4_556 ? C5 C10 H10A 107.4 . . ? C5 C10 H10A 107.4 4_556 . ? C5 C10 H10B 107.4 . . ? C5 C10 H10B 107.4 4_556 . ? H10A C10 H10B 106.9 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 O1 C1 117.7(3) . . ? O2 C12 O1 123.5(3) . . ? O2 C12 C13 125.4(3) . . ? O1 C12 C13 111.1(3) . . ? C17 C13 C14 119.0(4) . . ? C17 C13 C12 122.7(3) . . ? C14 C13 C12 118.3(4) . . ? N1 C14 C13 122.3(5) . . ? N1 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 N1 C15 117.5(5) . . ? C16 C15 N1 122.7(4) . . ? C16 C15 H15 118.7 . . ? N1 C15 H15 118.7 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C13 C17 C16 118.1(5) . . ? C13 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C19 C18 C18 140(2) . 3_556 ? C20 C19 C18 122(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.500 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.150 # Attachment 'New CIF for 2-Hg.cif' data_e266a _database_code_depnum_ccdc_archive 'CCDC 616019' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H60 Cl4.50 Hg2 N4 O11' _chemical_formula_weight 1705.94 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 22.5845(10) _cell_length_b 12.3139(5) _cell_length_c 17.2598(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4800.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5844 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.89 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1677 _exptl_absorpt_coefficient_mu 3.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7296 _exptl_absorpt_correction_T_max 0.8498 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45965 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10976 _reflns_number_gt 7950 _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^)+(0.1916P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.068(13) _refine_ls_number_reflns 10976 _refine_ls_number_parameters 415 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2744 _refine_ls_wR_factor_gt 0.2468 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 N2 N 0.7889(4) 1.4036(9) 0.9451(5) 0.060(2) Uani 1 1 d . . . C11 C 0.7974(4) 1.3822(11) 0.8693(6) 0.054(3) Uani 1 1 d . . . H11 H 0.7757 1.4228 0.8321 0.065 Uiso 1 1 calc R . . Hg1 Hg 0.71938(2) 0.54243(5) -0.01271(3) 0.0729(2) Uani 1 1 d . . . Cl1 Cl 0.6885(2) 0.4739(4) 0.1083(2) 0.1019(15) Uani 1 1 d . . . Cl2 Cl 0.70490(17) 0.6186(4) -0.1357(2) 0.0908(13) Uani 1 1 d . . . C1 C 0.9523(3) 1.2305(7) 0.5469(6) 0.0369(18) Uani 1 1 d . . . C2 C 0.9196(3) 1.1516(7) 0.5085(5) 0.0316(15) Uani 1 1 d . . . C3 C 0.8768(3) 1.0886(7) 0.5482(5) 0.0344(17) Uani 1 1 d . . . C4 C 0.8630(4) 1.1103(8) 0.6256(5) 0.0385(19) Uani 1 1 d . . . C5 C 0.8953(4) 1.1963(8) 0.6614(5) 0.040(2) Uani 1 1 d . . . C6 C 0.9397(4) 1.2562(7) 0.6249(6) 0.0383(19) Uani 1 1 d . . . C7 C 0.9285(4) 1.1351(8) 0.4230(5) 0.043(2) Uani 1 1 d . . . H7A H 0.9401 1.2041 0.3990 0.065 Uiso 1 1 calc R . . H7B H 0.8916 1.1093 0.3996 0.065 Uiso 1 1 calc R . . H7C H 0.9598 1.0812 0.4146 0.065 Uiso 1 1 calc R . . C8 C 0.8167(4) 1.0528(9) 0.6730(6) 0.048(2) Uani 1 1 d . . . H8A H 0.7782 1.0878 0.6651 0.072 Uiso 1 1 calc R . . H8B H 0.8274 1.0565 0.7279 0.072 Uiso 1 1 calc R . . H8C H 0.8144 0.9766 0.6568 0.072 Uiso 1 1 calc R . . C9 C 0.8433(4) 1.2909(10) 0.7574(6) 0.050(2) Uani 1 1 d . . . C10 C 0.8353(4) 1.3062(9) 0.8440(6) 0.048(2) Uani 1 1 d . . . C12 C 0.8213(6) 1.3466(11) 0.9960(6) 0.064(3) Uani 1 1 d . . . H12 H 0.8146 1.3576 1.0498 0.077 Uiso 1 1 calc R . . C13 C 0.8606(7) 1.2785(13) 0.9752(7) 0.077(4) Uani 1 1 d . . . H13 H 0.8852 1.2473 1.0139 0.092 Uiso 1 1 calc R . . C14 C 0.8696(5) 1.2466(12) 0.8962(8) 0.063(3) Uani 1 1 d . . . H14 H 0.8961 1.1907 0.8809 0.075 Uiso 1 1 calc R . . C15 C 0.9690(5) 1.3524(9) 0.6682(7) 0.053(3) Uani 1 1 d . . . H15A H 0.9639 1.4191 0.6381 0.080 Uiso 1 1 calc R . . H15B H 1.0114 1.3377 0.6750 0.080 Uiso 1 1 calc R . . H15C H 0.9504 1.3611 0.7191 0.080 Uiso 1 1 calc R . . C16 C 0.8419(3) 1.0020(8) 0.5063(5) 0.0409(18) Uani 1 1 d . . . H16A H 0.8155 1.0384 0.4687 0.049 Uiso 1 1 calc R . . H16B H 0.8164 0.9649 0.5447 0.049 Uiso 1 1 calc R . . C17 C 0.8779(3) 0.9135(7) 0.4620(5) 0.0361(17) Uani 1 1 d . . . C18 C 0.8646(4) 0.8942(8) 0.3826(6) 0.041(2) Uani 1 1 d . . . C19 C 0.8989(3) 0.8103(9) 0.3476(6) 0.042(2) Uani 1 1 d . . . C20 C 0.9409(4) 0.7494(8) 0.3835(6) 0.044(2) Uani 1 1 d . . . C21 C 0.9527(3) 0.7696(7) 0.4625(5) 0.0368(18) Uani 1 1 d . . . C22 C 0.9191(3) 0.8505(7) 0.5003(5) 0.0365(18) Uani 1 1 d . . . C23 C 0.8195(4) 0.9573(10) 0.3350(6) 0.050(2) Uani 1 1 d . . . H23A H 0.7798 0.9286 0.3451 0.074 Uiso 1 1 calc R . . H23B H 0.8287 0.9496 0.2798 0.074 Uiso 1 1 calc R . . H23C H 0.8209 1.0342 0.3495 0.074 Uiso 1 1 calc R . . C24 C 0.8464(4) 0.7296(10) 0.2427(6) 0.050(2) Uani 1 1 d . . . C25 C 0.8421(4) 0.7311(9) 0.1562(5) 0.045(2) Uani 1 1 d . . . C26 C 0.8771(5) 0.8011(11) 0.1093(7) 0.057(3) Uani 1 1 d . . . H26 H 0.9044 0.8496 0.1329 0.069 Uiso 1 1 calc R . . C27 C 0.8718(7) 0.7990(14) 0.0336(10) 0.082(4) Uani 1 1 d . . . H27 H 0.8949 0.8449 0.0013 0.099 Uiso 1 1 calc R . . C28 C 0.8287(6) 0.7224(11) 0.0012(7) 0.065(3) Uani 1 1 d . . . H28 H 0.8247 0.7183 -0.0535 0.077 Uiso 1 1 calc R . . C29 C 0.8024(5) 0.6632(9) 0.1209(6) 0.050(2) Uani 1 1 d . . . H29 H 0.7790 0.6167 0.1524 0.060 Uiso 1 1 calc R . . C30 C 0.9710(5) 0.6553(11) 0.3386(8) 0.066(4) Uani 1 1 d . . . H30A H 0.9466 0.6357 0.2938 0.099 Uiso 1 1 calc R . . H30B H 0.9751 0.5922 0.3728 0.099 Uiso 1 1 calc R . . H30C H 1.0102 0.6785 0.3210 0.099 Uiso 1 1 calc R . . C31 C 0.9271(4) 0.8650(9) 0.5874(5) 0.043(2) Uani 1 1 d . . . H31A H 0.9612 0.9123 0.5972 0.065 Uiso 1 1 calc R . . H31B H 0.9339 0.7940 0.6115 0.065 Uiso 1 1 calc R . . H31C H 0.8913 0.8979 0.6094 0.065 Uiso 1 1 calc R . . C32 C 1.0008(4) 1.2963(7) 0.5055(6) 0.043(2) Uani 1 1 d . . . H32A H 0.9815 1.3458 0.4680 0.052 Uiso 1 1 calc R . . H32B H 1.0212 1.3420 0.5444 0.052 Uiso 1 1 calc R . . N1 N 0.7952(4) 0.6593(8) 0.0443(5) 0.052(2) Uani 1 1 d . . . O1 O 0.8834(3) 1.2161(6) 0.7404(4) 0.0479(16) Uani 1 1 d . . . O2 O 0.8158(4) 1.3407(9) 0.7096(5) 0.073(3) Uani 1 1 d . . . O3 O 0.8897(3) 0.7970(8) 0.2657(4) 0.0559(19) Uani 1 1 d . . . O4 O 0.8160(5) 0.6756(10) 0.2850(5) 0.083(3) Uani 1 1 d . . . O5 O 0.8746(11) 0.5021(19) 0.4940(14) 0.095(6) Uiso 0.50 1 d P . . C33 C 0.922(2) 0.596(4) 0.842(3) 0.104(14) Uiso 0.40 1 d PD . . C34 C 0.930(2) 0.520(3) 0.914(2) 0.089(11) Uiso 0.40 1 d PD . . O6 O 0.8791(15) 0.609(3) 0.785(2) 0.105(9) Uiso 0.40 1 d P . . C35 C 0.0000 1.0000 0.0897(16) 0.085(5) Uiso 0.50 2 d SPD . . C38 C 0.0000 1.0000 0.2514(17) 0.085(5) Uiso 0.50 2 d SPD . . C37 C 0.0422(7) 0.9384(16) 0.2127(14) 0.085(5) Uiso 0.50 1 d PD . . C36 C 0.0437(7) 0.9408(17) 0.1305(14) 0.085(5) Uiso 0.50 1 d PD . . Cl3 Cl 0.0000 1.0000 -0.0134(16) 0.177(9) Uiso 0.50 2 d SPD . . C39 C 0.8871(16) 0.758(3) 0.778(2) 0.103(9) Uiso 0.60 1 d P . . C40 C 0.9336(15) 0.811(3) 0.809(2) 0.107(10) Uiso 0.60 1 d P . . O7 O 0.9506(7) 0.9307(14) 0.7917(11) 0.080(4) Uiso 0.60 1 d P . . 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 N2 0.060(5) 0.084(6) 0.038(4) -0.021(4) 0.016(4) -0.026(5) C11 0.041(5) 0.081(8) 0.041(5) -0.025(5) 0.013(4) -0.018(5) Hg1 0.0723(3) 0.1036(4) 0.0428(3) -0.0338(2) 0.0023(2) -0.0038(3) Cl1 0.129(3) 0.113(3) 0.064(2) -0.042(2) 0.038(2) -0.042(3) Cl2 0.089(2) 0.136(3) 0.0471(16) -0.0277(19) -0.0146(15) 0.035(2) C1 0.023(3) 0.040(5) 0.047(5) -0.004(4) 0.005(3) -0.002(3) C2 0.027(3) 0.037(4) 0.030(4) -0.003(3) 0.000(3) 0.001(3) C3 0.024(3) 0.040(4) 0.039(4) -0.003(4) 0.003(3) 0.005(3) C4 0.032(4) 0.049(5) 0.035(4) -0.002(4) 0.007(3) 0.001(4) C5 0.030(4) 0.052(5) 0.037(5) -0.011(4) -0.001(3) 0.010(4) C6 0.029(4) 0.041(5) 0.045(5) -0.012(4) -0.003(3) 0.003(3) C7 0.047(5) 0.051(6) 0.033(4) -0.004(4) 0.011(4) -0.005(4) C8 0.042(4) 0.065(6) 0.037(5) 0.004(4) 0.017(4) -0.004(5) C9 0.038(4) 0.071(7) 0.041(5) -0.011(5) 0.000(4) 0.000(5) C10 0.036(4) 0.059(6) 0.049(6) -0.008(5) 0.008(4) -0.015(4) C12 0.072(7) 0.092(8) 0.029(5) -0.007(5) -0.004(5) -0.018(6) C13 0.095(10) 0.100(10) 0.035(6) 0.015(6) 0.007(6) 0.021(8) C14 0.047(5) 0.091(9) 0.051(6) -0.002(6) 0.008(5) -0.005(6) C15 0.055(5) 0.047(6) 0.058(7) -0.019(5) -0.004(5) -0.016(5) C16 0.025(3) 0.052(4) 0.046(5) -0.008(4) -0.001(3) 0.001(3) C17 0.029(3) 0.043(4) 0.037(4) 0.001(4) -0.001(3) -0.009(3) C18 0.032(4) 0.045(5) 0.047(5) -0.007(4) -0.006(4) -0.004(4) C19 0.024(4) 0.057(6) 0.044(5) -0.015(4) -0.002(3) -0.007(4) C20 0.034(4) 0.052(6) 0.047(5) -0.021(4) 0.001(4) -0.008(4) C21 0.026(3) 0.044(5) 0.041(4) -0.009(4) -0.008(3) -0.009(3) C22 0.024(3) 0.046(5) 0.040(5) -0.006(4) 0.001(3) -0.008(3) C23 0.042(4) 0.066(6) 0.040(5) -0.003(5) -0.016(4) -0.003(5) C24 0.038(5) 0.081(7) 0.031(4) -0.014(5) 0.000(4) -0.008(5) C25 0.030(4) 0.072(6) 0.033(4) -0.013(4) -0.005(3) 0.010(4) C26 0.045(5) 0.071(7) 0.055(6) -0.014(6) -0.011(5) 0.000(5) C27 0.081(9) 0.087(9) 0.080(11) -0.020(8) 0.008(8) 0.005(8) C28 0.067(7) 0.092(8) 0.034(6) -0.009(5) -0.004(5) 0.007(6) C29 0.052(5) 0.061(6) 0.036(5) -0.009(4) 0.002(4) 0.003(5) C30 0.046(5) 0.073(8) 0.079(9) -0.046(7) -0.008(5) 0.009(5) C31 0.032(4) 0.060(6) 0.037(5) 0.004(4) -0.006(3) -0.003(4) C32 0.040(4) 0.033(4) 0.057(6) -0.001(4) 0.012(5) -0.002(3) N1 0.058(5) 0.060(5) 0.038(4) -0.016(4) -0.006(4) 0.003(4) O1 0.041(3) 0.065(4) 0.038(4) -0.012(3) -0.002(3) 0.005(3) O2 0.067(5) 0.114(7) 0.039(4) -0.015(5) -0.003(4) 0.050(5) O3 0.041(3) 0.090(5) 0.037(4) -0.019(4) 0.000(3) -0.007(4) O4 0.082(6) 0.136(9) 0.032(4) -0.026(5) 0.000(4) -0.051(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N2 C12 1.342(17) . ? N2 C11 1.349(13) . ? N2 Hg1 2.433(11) 1_566 ? C11 C10 1.340(16) . ? C11 H11 0.9500 . ? Hg1 Cl2 2.343(4) . ? Hg1 Cl1 2.358(4) . ? Hg1 N2 2.433(11) 1_544 ? Hg1 N1 2.444(8) . ? C1 C2 1.389(12) . ? C1 C6 1.412(14) . ? C1 C32 1.540(12) . ? C2 C3 1.415(12) . ? C2 C7 1.503(12) . ? C3 C4 1.398(13) . ? C3 C16 1.510(13) . ? C4 C5 1.427(14) . ? C4 C8 1.504(12) . ? C5 C6 1.396(14) . ? C5 O1 1.412(11) . ? C6 C15 1.549(12) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O2 1.200(14) . ? C9 O1 1.324(13) . ? C9 C10 1.518(15) . ? C10 C14 1.396(18) . ? C12 C13 1.27(2) . ? C12 H12 0.9500 . ? C13 C14 1.434(18) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.560(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.379(13) . ? C17 C18 1.422(14) . ? C18 C19 1.425(14) . ? C18 C23 1.522(13) . ? C19 C20 1.360(15) . ? C19 O3 1.437(12) . ? C20 C21 1.411(13) . ? C20 C30 1.551(14) . ? C21 C22 1.412(13) . ? C21 C32 1.521(12) 2_775 ? C22 C31 1.524(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O4 1.203(14) . ? C24 O3 1.344(13) . ? C24 C25 1.496(13) . ? C25 C29 1.368(15) . ? C25 C26 1.422(17) . ? C26 C27 1.31(2) . ? C26 H26 0.9500 . ? C27 C28 1.47(2) . ? C27 H27 0.9500 . ? C28 N1 1.315(15) . ? C28 H28 0.9500 . ? C29 N1 1.333(14) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C21 1.521(12) 2_775 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O6 1.40(6) . ? C33 C34 1.558(19) . ? O6 C39 1.85(5) . ? C35 C36 1.415(12) . ? C35 C36 1.415(12) 2_575 ? C35 Cl3 1.78(4) . ? C38 C37 1.389(13) 2_575 ? C38 C37 1.389(13) . ? C37 C36 1.418(16) . ? C39 C40 1.35(5) . ? C40 O7 1.55(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 C12 N2 C11 117.1(11) . . ? C12 N2 Hg1 121.5(8) . 1_566 ? C11 N2 Hg1 121.4(9) . 1_566 ? C10 C11 N2 122.9(13) . . ? C10 C11 H11 118.5 . . ? N2 C11 H11 118.5 . . ? Cl2 Hg1 Cl1 154.73(18) . . ? Cl2 Hg1 N2 95.7(3) . 1_544 ? Cl1 Hg1 N2 101.8(3) . 1_544 ? Cl2 Hg1 N1 103.1(3) . . ? Cl1 Hg1 N1 93.5(3) . . ? N2 Hg1 N1 94.7(3) 1_544 . ? C2 C1 C6 120.4(8) . . ? C2 C1 C32 121.7(8) . . ? C6 C1 C32 117.9(8) . . ? C1 C2 C3 121.0(8) . . ? C1 C2 C7 119.4(8) . . ? C3 C2 C7 119.5(8) . . ? C4 C3 C2 120.7(8) . . ? C4 C3 C16 118.4(8) . . ? C2 C3 C16 120.8(8) . . ? C3 C4 C5 116.2(8) . . ? C3 C4 C8 125.8(9) . . ? C5 C4 C8 118.0(8) . . ? C6 C5 O1 118.9(8) . . ? C6 C5 C4 124.4(8) . . ? O1 C5 C4 116.7(9) . . ? C5 C6 C1 117.1(8) . . ? C5 C6 C15 119.5(8) . . ? C1 C6 C15 123.1(9) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 O1 123.8(10) . . ? O2 C9 C10 123.5(10) . . ? O1 C9 C10 112.7(10) . . ? C11 C10 C14 120.8(11) . . ? C11 C10 C9 118.9(11) . . ? C14 C10 C9 120.2(10) . . ? C13 C12 N2 122.7(11) . . ? C13 C12 H12 118.7 . . ? N2 C12 H12 118.7 . . ? C12 C13 C14 123.2(13) . . ? C12 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C10 C14 C13 113.0(12) . . ? C10 C14 H14 123.5 . . ? C13 C14 H14 123.5 . . ? C6 C15 H15A 109.5 . . ? C6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 C16 C17 117.2(7) . . ? C3 C16 H16A 108.0 . . ? C17 C16 H16A 108.0 . . ? C3 C16 H16B 108.0 . . ? C17 C16 H16B 108.0 . . ? H16A C16 H16B 107.3 . . ? C22 C17 C18 120.7(8) . . ? C22 C17 C16 120.6(8) . . ? C18 C17 C16 118.6(8) . . ? C17 C18 C19 114.6(8) . . ? C17 C18 C23 125.2(9) . . ? C19 C18 C23 120.2(9) . . ? C20 C19 C18 125.8(9) . . ? C20 C19 O3 119.0(9) . . ? C18 C19 O3 115.0(9) . . ? C19 C20 C21 118.4(9) . . ? C19 C20 C30 119.4(9) . . ? C21 C20 C30 122.1(10) . . ? C20 C21 C22 118.0(8) . . ? C20 C21 C32 120.5(9) . 2_775 ? C22 C21 C32 121.5(8) . 2_775 ? C17 C22 C21 122.5(8) . . ? C17 C22 C31 119.1(8) . . ? C21 C22 C31 118.3(8) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 O3 125.2(9) . . ? O4 C24 C25 125.2(9) . . ? O3 C24 C25 109.6(9) . . ? C29 C25 C26 118.8(9) . . ? C29 C25 C24 118.6(10) . . ? C26 C25 C24 122.6(9) . . ? C27 C26 C25 120.2(12) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 116.9(15) . . ? C26 C27 H27 121.6 . . ? C28 C27 H27 121.6 . . ? N1 C28 C27 123.1(11) . . ? N1 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? N1 C29 C25 122.9(11) . . ? N1 C29 H29 118.5 . . ? C25 C29 H29 118.5 . . ? C20 C30 H30A 109.5 . . ? C20 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C20 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 C31 H31A 109.5 . . ? C22 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C22 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C21 C32 C1 115.9(7) 2_775 . ? C21 C32 H32A 108.3 2_775 . ? C1 C32 H32A 108.3 . . ? C21 C32 H32B 108.3 2_775 . ? C1 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C28 N1 C29 118.0(9) . . ? C28 N1 Hg1 121.5(7) . . ? C29 N1 Hg1 120.4(8) . . ? C9 O1 C5 117.7(8) . . ? C24 O3 C19 117.8(8) . . ? O6 C33 C34 135(4) . . ? C33 O6 C39 95(3) . . ? C36 C35 C36 120.3(16) . 2_575 ? C36 C35 Cl3 119.9(8) . . ? C36 C35 Cl3 119.9(8) 2_575 . ? C37 C38 C37 122.5(18) 2_575 . ? C38 C37 C36 119.1(11) . . ? C35 C36 C37 119.4(10) . . ? C40 C39 O6 122(3) . . ? C39 C40 O7 125(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.935 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.353