# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Liu, Qingxiang' _publ_contact_author_email tjnulqx@163.com _publ_section_title ; N-Heterocyclic carbene copper(I), mercury(II) and silver(I) complexes containing durene linker: synthesis and structural studies ; _publ_author_name 'Qingxiang Liu' data_2b _database_code_depnum_ccdc_archive 'CCDC 757348' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H71 Cu4 I4 N9' _chemical_formula_weight 1704.04 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7099(19) _cell_length_b 17.216(3) _cell_length_c 19.642(4) _cell_angle_alpha 72.85(3) _cell_angle_beta 86.38(3) _cell_angle_gamma 88.62(3) _cell_volume 3131.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6636 _cell_measurement_theta_min 1.386 _cell_measurement_theta_max 27.876 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 3.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6507 _exptl_absorpt_correction_T_max 0.7300 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _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 19291 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10999 _reflns_number_gt 8699 _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^)+(0.0531P)^2^+12.8773P] 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 10999 _refine_ls_number_parameters 725 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.003 _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 I1 I 0.43270(6) 0.72177(3) 0.39089(3) 0.04031(17) Uani 1 1 d . . . I2 I 0.78089(7) 0.79343(4) 0.25340(3) 0.05082(19) Uani 1 1 d . . . I3 I -0.09190(6) 0.28799(4) 0.11174(4) 0.05013(19) Uani 1 1 d . . . I4 I 0.21421(7) 0.22346(4) 0.25914(3) 0.05311(19) Uani 1 1 d . . . Cu1 Cu 0.65976(11) 0.81117(6) 0.36978(6) 0.0383(3) Uani 1 1 d . . . Cu2 Cu 0.65698(12) 0.66774(6) 0.34362(5) 0.0378(3) Uani 1 1 d . . . Cu3 Cu 0.11323(11) 0.34513(6) 0.15798(6) 0.0381(3) Uani 1 1 d . . . Cu4 Cu 0.13321(12) 0.19640(6) 0.14619(7) 0.0472(3) Uani 1 1 d . . . N1 N 0.6351(8) 0.9690(4) 0.4000(4) 0.044(2) Uani 1 1 d . . . N2 N 0.7546(7) 0.8842(4) 0.4799(4) 0.0353(17) Uani 1 1 d . . . N3 N 0.7574(6) 0.4966(3) 0.3982(3) 0.0235(13) Uani 1 1 d . . . N4 N 0.6640(9) 0.5222(5) 0.2980(4) 0.050(2) Uani 1 1 d D . . N5 N 0.1150(8) 0.4989(4) 0.1909(4) 0.0373(17) Uani 1 1 d . . . N6 N 0.2360(7) 0.5109(3) 0.0925(3) 0.0289(15) Uani 1 1 d . . . N7 N 0.2479(8) 0.1089(4) 0.0440(5) 0.050(2) Uani 1 1 d . . . N8 N 0.0908(9) 0.0419(4) 0.1184(5) 0.056(2) Uani 1 1 d . . . C1 C 0.6666(9) 1.0089(5) 0.4489(5) 0.041(2) Uani 1 1 d . . . C2 C 0.6328(11) 1.0869(5) 0.4532(6) 0.061(3) Uani 1 1 d . . . H2 H 0.5816 1.1228 0.4189 0.074 Uiso 1 1 calc R . . C3 C 0.6779(13) 1.1084(6) 0.5095(6) 0.064(4) Uani 1 1 d . . . H3 H 0.6578 1.1598 0.5138 0.077 Uiso 1 1 calc R . . C4 C 0.7519(13) 1.0551(6) 0.5593(6) 0.066(4) Uani 1 1 d . . . H4 H 0.7797 1.0714 0.5973 0.079 Uiso 1 1 calc R . . C5 C 0.7888(12) 0.9765(5) 0.5565(6) 0.059(3) Uani 1 1 d . . . H5 H 0.8405 0.9408 0.5907 0.071 Uiso 1 1 calc R . . C6 C 0.7419(10) 0.9564(5) 0.4985(5) 0.044(2) Uani 1 1 d . . . C7 C 0.6885(9) 0.8916(4) 0.4204(5) 0.038(2) Uani 1 1 d . . . C8 C 0.5621(12) 1.0048(6) 0.3361(6) 0.060(3) Uani 1 1 d . . . H8A H 0.4863 1.0381 0.3464 0.072 Uiso 1 1 calc R . . H8B H 0.5241 0.9622 0.3199 0.072 Uiso 1 1 calc R . . C9 C 0.6596(15) 1.0566(8) 0.2780(7) 0.089(5) Uani 1 1 d . . . H9A H 0.6868 1.1031 0.2913 0.134 Uiso 1 1 calc R . . H9B H 0.6138 1.0744 0.2341 0.134 Uiso 1 1 calc R . . H9C H 0.7398 1.0252 0.2717 0.134 Uiso 1 1 calc R . . C10 C 0.8305(9) 0.8143(4) 0.5200(5) 0.036(2) Uani 1 1 d . . . H10A H 0.8002 0.8025 0.5700 0.043 Uiso 1 1 calc R . . H10B H 0.9274 0.8284 0.5156 0.043 Uiso 1 1 calc R . . C11 C 0.8172(8) 0.7379(4) 0.4984(4) 0.0323(18) Uani 1 1 d . . . C12 C 0.7093(7) 0.6830(4) 0.5314(4) 0.0252(16) Uani 1 1 d . . . C13 C 0.7077(8) 0.6067(4) 0.5195(4) 0.0265(16) Uani 1 1 d . . . C14 C 0.8082(7) 0.5860(4) 0.4736(4) 0.0247(16) Uani 1 1 d . . . C15 C 0.9125(8) 0.6424(4) 0.4390(4) 0.0314(18) Uani 1 1 d . . . C16 C 0.9146(8) 0.7187(4) 0.4504(4) 0.0286(17) Uani 1 1 d . . . C17 C 1.0217(9) 0.7809(5) 0.4098(5) 0.038(2) Uani 1 1 d . . . H17A H 0.9921 0.8341 0.4108 0.057 Uiso 1 1 calc R . . H17B H 1.0324 0.7797 0.3611 0.057 Uiso 1 1 calc R . . H17C H 1.1084 0.7681 0.4316 0.057 Uiso 1 1 calc R . . C18 C 0.5959(9) 0.7074(5) 0.5779(5) 0.038(2) Uani 1 1 d . . . H18A H 0.5078 0.6942 0.5648 0.057 Uiso 1 1 calc R . . H18B H 0.6002 0.7648 0.5712 0.057 Uiso 1 1 calc R . . H18C H 0.6079 0.6786 0.6271 0.057 Uiso 1 1 calc R . . C19 C 0.5902(8) 0.5499(5) 0.5559(5) 0.037(2) Uani 1 1 d . . . H19A H 0.5059 0.5702 0.5340 0.055 Uiso 1 1 calc R . . H19B H 0.5812 0.5468 0.6056 0.055 Uiso 1 1 calc R . . H19C H 0.6095 0.4967 0.5512 0.055 Uiso 1 1 calc R . . C20 C 1.0171(8) 0.6239(5) 0.3849(4) 0.0308(18) Uani 1 1 d . . . H20A H 1.0006 0.6589 0.3382 0.046 Uiso 1 1 calc R . . H20B H 1.0081 0.5682 0.3856 0.046 Uiso 1 1 calc R . . H20C H 1.1086 0.6327 0.3969 0.046 Uiso 1 1 calc R . . C21 C 0.8128(8) 0.5027(4) 0.4642(4) 0.0308(17) Uani 1 1 d . . . H21A H 0.9079 0.4841 0.4655 0.037 Uiso 1 1 calc R . . H21B H 0.7615 0.4662 0.5044 0.037 Uiso 1 1 calc R . . C22 C 0.6970(9) 0.5561(5) 0.3483(5) 0.037(2) Uani 1 1 d . . . C23 C 0.6263(14) 0.5681(7) 0.2250(7) 0.130(8) Uani 1 1 d D . . H23A H 0.6609 0.5418 0.1899 0.156 Uiso 1 1 calc R . . H23B H 0.6590 0.6237 0.2113 0.156 Uiso 1 1 calc R . . C24 C 0.4717(16) 0.5640(9) 0.2354(7) 0.125(8) Uani 1 1 d D . . H24A H 0.4432 0.5083 0.2486 0.187 Uiso 1 1 calc R . . H24B H 0.4316 0.5936 0.1918 0.187 Uiso 1 1 calc R . . H24C H 0.4417 0.5875 0.2725 0.187 Uiso 1 1 calc R . . C25 C 0.7006(10) 0.4398(5) 0.3162(5) 0.040(2) Uani 1 1 d . . . C26 C 0.6926(11) 0.3800(6) 0.2807(6) 0.055(3) Uani 1 1 d . . . H26 H 0.6513 0.3907 0.2374 0.066 Uiso 1 1 calc R . . C27 C 0.7482(10) 0.3057(5) 0.3127(6) 0.050(3) Uani 1 1 d . . . H27 H 0.7451 0.2652 0.2902 0.060 Uiso 1 1 calc R . . C28 C 0.8103(9) 0.2878(5) 0.3789(5) 0.039(2) Uani 1 1 d . . . H28 H 0.8456 0.2361 0.3994 0.046 Uiso 1 1 calc R . . C29 C 0.8188(8) 0.3476(4) 0.4136(4) 0.0292(18) Uani 1 1 d . . . H29 H 0.8609 0.3374 0.4567 0.035 Uiso 1 1 calc R . . C30 C 0.7618(8) 0.4224(4) 0.3810(4) 0.0269(17) Uani 1 1 d . . . C31 C 0.1607(11) 0.5781(5) 0.1678(5) 0.047(2) Uani 1 1 d . . . C32 C 0.1395(15) 0.6419(6) 0.1955(6) 0.084(5) Uani 1 1 d . . . H32 H 0.0883 0.6362 0.2384 0.101 Uiso 1 1 calc R . . C33 C 0.1980(16) 0.7152(6) 0.1567(7) 0.094(6) Uani 1 1 d . . . H33 H 0.1802 0.7609 0.1720 0.113 Uiso 1 1 calc R . . C34 C 0.2833(15) 0.7226(6) 0.0951(6) 0.080(5) Uani 1 1 d . . . H34 H 0.3272 0.7717 0.0725 0.096 Uiso 1 1 calc R . . C35 C 0.3031(11) 0.6579(5) 0.0674(5) 0.052(3) Uani 1 1 d . . . H35 H 0.3571 0.6625 0.0256 0.063 Uiso 1 1 calc R . . C36 C 0.2389(10) 0.5864(5) 0.1047(4) 0.043(2) Uani 1 1 d . . . C37 C 0.1576(8) 0.4564(4) 0.1459(4) 0.0298(17) Uani 1 1 d . . . C38 C 0.0376(9) 0.4626(5) 0.2601(4) 0.040(2) Uani 1 1 d . . . H38A H -0.0104 0.4145 0.2585 0.048 Uiso 1 1 calc R . . H38B H -0.0305 0.5012 0.2689 0.048 Uiso 1 1 calc R . . C39 C 0.1348(9) 0.4405(5) 0.3188(5) 0.042(2) Uani 1 1 d . . . H39A H 0.1978 0.3993 0.3119 0.063 Uiso 1 1 calc R . . H39B H 0.0835 0.4203 0.3638 0.063 Uiso 1 1 calc R . . H39C H 0.1856 0.4878 0.3186 0.063 Uiso 1 1 calc R . . C40 C 0.3064(8) 0.4974(4) 0.0293(4) 0.0288(17) Uani 1 1 d . . . H40A H 0.4007 0.5162 0.0258 0.035 Uiso 1 1 calc R . . H40B H 0.2618 0.5304 -0.0124 0.035 Uiso 1 1 calc R . . C41 C 0.3095(8) 0.4100(4) 0.0276(4) 0.0308(18) Uani 1 1 d . . . C42 C 0.2252(8) 0.3862(5) -0.0166(5) 0.037(2) Uani 1 1 d . . . C43 C 0.2342(9) 0.3071(5) -0.0221(5) 0.042(2) Uani 1 1 d . . . C44 C 0.3321(8) 0.2537(5) 0.0184(5) 0.038(2) Uani 1 1 d . . . C45 C 0.4108(8) 0.2766(4) 0.0653(4) 0.0330(19) Uani 1 1 d . . . C46 C 0.4014(8) 0.3559(5) 0.0705(4) 0.0344(19) Uani 1 1 d . . . C47 C 0.4893(9) 0.3806(6) 0.1208(5) 0.045(2) Uani 1 1 d . . . H47A H 0.4532 0.3571 0.1689 0.067 Uiso 1 1 calc R . . H47B H 0.4887 0.4388 0.1097 0.067 Uiso 1 1 calc R . . H47C H 0.5822 0.3618 0.1157 0.067 Uiso 1 1 calc R . . C48 C 0.1157(10) 0.4428(6) -0.0582(6) 0.053(3) Uani 1 1 d . . . H48A H 0.0266 0.4179 -0.0454 0.079 Uiso 1 1 calc R . . H48B H 0.1364 0.4526 -0.1085 0.079 Uiso 1 1 calc R . . H48C H 0.1153 0.4934 -0.0470 0.079 Uiso 1 1 calc R . . C49 C 0.1357(11) 0.2792(6) -0.0687(6) 0.059(3) Uani 1 1 d . . . H49A H 0.0422 0.2907 -0.0556 0.089 Uiso 1 1 calc R . . H49B H 0.1470 0.2219 -0.0614 0.089 Uiso 1 1 calc R . . H49C H 0.1568 0.3078 -0.1180 0.089 Uiso 1 1 calc R . . C50 C 0.5063(9) 0.2167(5) 0.1133(6) 0.051(3) Uani 1 1 d . . . H50A H 0.4813 0.1622 0.1158 0.076 Uiso 1 1 calc R . . H50B H 0.4981 0.2232 0.1603 0.076 Uiso 1 1 calc R . . H50C H 0.5998 0.2267 0.0942 0.076 Uiso 1 1 calc R . . C51 C 0.3526(10) 0.1699(5) 0.0065(6) 0.055(3) Uani 1 1 d . . . H51A H 0.3523 0.1765 -0.0442 0.066 Uiso 1 1 calc R . . H51B H 0.4428 0.1492 0.0220 0.066 Uiso 1 1 calc R . . C52 C 0.1651(10) 0.1114(5) 0.1014(6) 0.050(3) Uani 1 1 d . . . C53 C -0.0130(12) 0.0188(6) 0.1796(7) 0.071(4) Uani 1 1 d . . . H53A H -0.0810 -0.0166 0.1703 0.085 Uiso 1 1 calc R . . H53B H -0.0603 0.0672 0.1846 0.085 Uiso 1 1 calc R . . C54 C 0.0529(16) -0.0242(8) 0.2483(7) 0.097(5) Uani 1 1 d . . . H54A H 0.0961 -0.0735 0.2443 0.146 Uiso 1 1 calc R . . H54B H -0.0166 -0.0368 0.2868 0.146 Uiso 1 1 calc R . . H54C H 0.1209 0.0104 0.2574 0.146 Uiso 1 1 calc R . . C55 C 0.1281(10) -0.0049(5) 0.0740(7) 0.059(3) Uani 1 1 d . . . C56 C 0.0765(11) -0.0781(6) 0.0669(7) 0.064(3) Uani 1 1 d . . . H56 H 0.0059 -0.1064 0.0978 0.076 Uiso 1 1 calc R . . C57 C 0.1334(11) -0.1052(6) 0.0135(7) 0.069(4) Uani 1 1 d . . . H57 H 0.1023 -0.1536 0.0081 0.082 Uiso 1 1 calc R . . C58 C 0.2388(12) -0.0619(6) -0.0340(8) 0.070(4) Uani 1 1 d . . . H58 H 0.2754 -0.0827 -0.0700 0.084 Uiso 1 1 calc R . . C59 C 0.2901(11) 0.0106(5) -0.0290(7) 0.058(3) Uani 1 1 d . . . H59 H 0.3602 0.0390 -0.0603 0.070 Uiso 1 1 calc R . . C60 C 0.2294(10) 0.0379(5) 0.0259(6) 0.054(3) Uani 1 1 d . . . N9 N 0.432(2) 1.0056(6) 0.1756(10) 0.156(8) Uani 1 1 d . . . C61 C 0.441(2) 0.9414(16) 0.1775(12) 0.143(9) Uani 1 1 d . . . C62 C 0.4135(15) 0.8538(9) 0.1724(10) 0.132(8) Uani 1 1 d . . . H62A H 0.3433 0.8280 0.2080 0.198 Uiso 1 1 calc R . . H62B H 0.4969 0.8221 0.1802 0.198 Uiso 1 1 calc R . . H62C H 0.3833 0.8576 0.1259 0.198 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 I1 0.0358(3) 0.0376(3) 0.0512(4) -0.0196(3) 0.0012(3) 0.0023(2) I2 0.0618(4) 0.0442(3) 0.0354(3) 0.0018(3) 0.0104(3) 0.0114(3) I3 0.0306(3) 0.0468(4) 0.0761(5) -0.0224(3) -0.0049(3) -0.0022(3) I4 0.0604(4) 0.0449(4) 0.0405(3) 0.0081(3) -0.0006(3) -0.0034(3) Cu1 0.0441(6) 0.0245(5) 0.0463(6) -0.0105(4) -0.0037(5) 0.0067(4) Cu2 0.0537(7) 0.0275(5) 0.0332(5) -0.0105(4) -0.0093(5) 0.0172(4) Cu3 0.0354(6) 0.0335(5) 0.0413(6) -0.0058(4) 0.0055(5) -0.0075(4) Cu4 0.0457(7) 0.0305(6) 0.0592(7) -0.0057(5) 0.0094(6) -0.0039(5) N1 0.048(5) 0.026(4) 0.053(5) -0.008(3) 0.018(4) -0.002(3) N2 0.045(4) 0.023(3) 0.039(4) -0.011(3) 0.000(4) -0.001(3) N3 0.029(3) 0.017(3) 0.025(3) -0.007(2) -0.002(3) 0.002(2) N4 0.069(6) 0.050(5) 0.045(5) -0.030(4) -0.041(4) 0.040(4) N5 0.045(4) 0.027(3) 0.029(4) 0.005(3) 0.012(3) -0.002(3) N6 0.033(4) 0.023(3) 0.023(3) 0.002(3) 0.008(3) 0.006(3) N7 0.044(5) 0.026(4) 0.078(6) -0.013(4) 0.011(5) -0.004(3) N8 0.055(5) 0.032(4) 0.072(6) -0.003(4) 0.013(5) -0.010(4) C1 0.046(5) 0.020(4) 0.056(6) -0.012(4) 0.028(5) -0.008(4) C2 0.064(7) 0.027(5) 0.086(8) -0.015(5) 0.039(6) -0.003(4) C3 0.093(9) 0.023(5) 0.077(8) -0.024(5) 0.043(7) -0.015(5) C4 0.094(9) 0.040(6) 0.071(7) -0.034(6) 0.034(7) -0.025(6) C5 0.087(8) 0.033(5) 0.064(6) -0.027(5) 0.029(6) -0.028(5) C6 0.056(6) 0.021(4) 0.055(6) -0.015(4) 0.021(5) -0.012(4) C7 0.038(5) 0.013(3) 0.057(6) -0.005(3) 0.015(5) 0.000(3) C8 0.066(7) 0.035(5) 0.072(8) -0.008(5) 0.013(6) 0.009(5) C9 0.091(10) 0.083(9) 0.063(8) 0.025(7) -0.003(8) 0.022(7) C10 0.042(5) 0.026(4) 0.042(5) -0.012(4) -0.005(4) -0.003(3) C11 0.036(5) 0.025(4) 0.039(5) -0.014(3) -0.007(4) 0.001(3) C12 0.021(4) 0.020(3) 0.035(4) -0.009(3) -0.005(3) -0.002(3) C13 0.025(4) 0.027(4) 0.030(4) -0.011(3) -0.009(3) 0.002(3) C14 0.024(4) 0.019(3) 0.032(4) -0.009(3) -0.010(3) 0.008(3) C15 0.035(4) 0.029(4) 0.031(4) -0.010(3) 0.005(4) -0.005(3) C16 0.026(4) 0.022(4) 0.034(4) -0.002(3) -0.007(4) 0.000(3) C17 0.034(5) 0.030(4) 0.045(5) -0.003(4) 0.000(4) -0.001(3) C18 0.035(5) 0.033(4) 0.046(5) -0.014(4) 0.007(4) -0.002(4) C19 0.027(4) 0.031(4) 0.054(5) -0.016(4) 0.002(4) -0.009(3) C20 0.035(4) 0.031(4) 0.026(4) -0.009(3) -0.002(4) 0.008(3) C21 0.032(4) 0.026(4) 0.035(4) -0.009(3) -0.007(4) 0.003(3) C22 0.047(5) 0.032(4) 0.038(5) -0.020(4) -0.010(4) 0.013(4) C23 0.080(10) 0.051(8) 0.28(3) -0.070(13) -0.073(14) 0.017(7) C24 0.23(2) 0.094(11) 0.052(8) -0.023(7) 0.027(11) -0.068(13) C25 0.049(5) 0.042(5) 0.037(5) -0.025(4) -0.004(4) 0.001(4) C26 0.068(7) 0.057(6) 0.057(6) -0.040(5) -0.015(6) 0.009(5) C27 0.052(6) 0.036(5) 0.071(7) -0.031(5) 0.006(5) -0.009(4) C28 0.041(5) 0.029(4) 0.047(5) -0.016(4) 0.009(4) -0.005(4) C29 0.034(4) 0.023(4) 0.030(4) -0.008(3) 0.004(4) -0.001(3) C30 0.023(4) 0.024(4) 0.035(4) -0.012(3) 0.006(4) -0.003(3) C31 0.073(7) 0.028(4) 0.034(5) -0.004(4) 0.010(5) 0.006(4) C32 0.151(13) 0.036(5) 0.059(7) -0.017(5) 0.059(8) 0.004(6) C33 0.177(14) 0.024(5) 0.077(8) -0.022(5) 0.068(9) -0.024(7) C34 0.144(12) 0.023(5) 0.065(7) -0.010(5) 0.046(8) -0.012(6) C35 0.078(7) 0.033(5) 0.040(5) -0.007(4) 0.024(5) -0.001(4) C36 0.064(6) 0.028(4) 0.032(4) -0.007(3) 0.019(5) -0.001(4) C37 0.029(4) 0.032(4) 0.023(4) 0.001(3) -0.002(4) 0.008(3) C38 0.043(5) 0.039(5) 0.032(5) -0.004(4) 0.011(4) 0.002(4) C39 0.036(5) 0.043(5) 0.042(5) -0.006(4) 0.012(4) -0.001(4) C40 0.028(4) 0.027(4) 0.029(4) -0.005(3) 0.004(4) 0.003(3) C41 0.025(4) 0.029(4) 0.034(4) -0.004(3) 0.008(4) -0.003(3) C42 0.023(4) 0.034(4) 0.052(5) -0.011(4) -0.004(4) -0.002(3) C43 0.036(5) 0.039(5) 0.050(5) -0.013(4) 0.005(5) -0.005(4) C44 0.029(4) 0.027(4) 0.054(6) -0.009(4) 0.009(4) 0.004(3) C45 0.022(4) 0.028(4) 0.040(5) 0.003(3) 0.006(4) 0.003(3) C46 0.026(4) 0.033(4) 0.036(5) 0.000(3) 0.006(4) -0.002(3) C47 0.027(5) 0.057(6) 0.043(5) -0.005(4) 0.003(4) -0.009(4) C48 0.046(6) 0.046(5) 0.072(7) -0.024(5) -0.017(5) 0.014(4) C49 0.064(7) 0.057(6) 0.069(7) -0.036(6) -0.015(6) -0.002(5) C50 0.026(5) 0.032(5) 0.076(7) 0.011(4) -0.001(5) 0.009(3) C51 0.041(5) 0.029(4) 0.095(8) -0.022(5) 0.020(6) -0.011(4) C52 0.040(5) 0.026(4) 0.074(7) 0.000(4) -0.001(5) -0.002(4) C53 0.064(7) 0.043(6) 0.092(9) -0.003(6) 0.019(7) -0.022(5) C54 0.099(11) 0.070(8) 0.087(10) 0.031(7) 0.002(9) -0.022(8) C55 0.043(6) 0.018(4) 0.107(9) -0.008(5) 0.008(6) -0.001(4) C56 0.056(7) 0.036(5) 0.096(9) -0.015(6) -0.004(7) -0.010(5) C57 0.053(6) 0.036(5) 0.121(11) -0.031(6) -0.002(7) -0.002(5) C58 0.061(7) 0.038(6) 0.115(11) -0.029(6) -0.005(7) 0.010(5) C59 0.050(6) 0.027(5) 0.095(8) -0.020(5) 0.010(6) 0.002(4) C60 0.043(5) 0.026(4) 0.092(8) -0.019(5) 0.002(6) 0.003(4) N9 0.27(2) 0.033(6) 0.191(16) -0.041(8) -0.165(16) 0.054(9) C61 0.111(15) 0.21(2) 0.149(19) -0.121(19) -0.005(14) 0.000(15) C62 0.080(10) 0.104(12) 0.171(17) 0.039(11) -0.070(11) -0.060(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 I1 Cu2 2.5741(13) . ? I1 Cu1 2.6597(14) . ? I2 Cu1 2.5996(13) . ? I2 Cu2 2.6202(16) . ? I3 Cu3 2.5710(14) . ? I3 Cu4 2.6670(16) . ? I4 Cu4 2.5701(16) . ? I4 Cu3 2.6437(17) . ? Cu1 C7 1.962(8) . ? Cu1 Cu2 2.6676(14) . ? Cu2 C22 1.929(7) . ? Cu3 C37 1.916(8) . ? Cu3 Cu4 2.6397(15) . ? Cu4 C52 1.927(10) . ? N1 C7 1.373(10) . ? N1 C1 1.388(12) . ? N1 C8 1.447(15) . ? N2 C7 1.341(12) . ? N2 C6 1.396(9) . ? N2 C10 1.444(11) . ? N3 C22 1.344(11) . ? N3 C30 1.412(8) . ? N3 C21 1.468(10) . ? N4 C22 1.344(10) . ? N4 C25 1.398(11) . ? N4 C23 1.483(9) . ? N5 C37 1.345(10) . ? N5 C31 1.379(10) . ? N5 C38 1.480(9) . ? N6 C37 1.383(9) . ? N6 C36 1.391(10) . ? N6 C40 1.455(9) . ? N7 C52 1.354(12) . ? N7 C60 1.389(11) . ? N7 C51 1.476(10) . ? N8 C52 1.357(11) . ? N8 C55 1.379(13) . ? N8 C53 1.485(13) . ? C1 C6 1.356(14) . ? C1 C2 1.400(11) . ? C2 C3 1.364(17) . ? C2 H2 0.9300 . ? C3 C4 1.357(18) . ? C3 H3 0.9300 . ? C4 C5 1.408(13) . ? C4 H4 0.9300 . ? C5 C6 1.388(14) . ? C5 H5 0.9300 . ? C8 C9 1.515(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.507(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.394(10) . ? C11 C12 1.419(10) . ? C12 C13 1.401(9) . ? C12 C18 1.516(10) . ? C13 C14 1.398(10) . ? C13 C19 1.518(10) . ? C14 C15 1.414(10) . ? C14 C21 1.498(9) . ? C15 C16 1.398(10) . ? C15 C20 1.520(10) . ? C16 C17 1.520(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 C24 1.502(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.388(12) . ? C25 C26 1.411(11) . ? C26 C27 1.363(15) . ? C26 H26 0.9300 . ? C27 C28 1.416(14) . ? C27 H27 0.9300 . ? C28 C29 1.400(10) . ? C28 H28 0.9300 . ? C29 C30 1.378(11) . ? C29 H29 0.9300 . ? C31 C32 1.369(12) . ? C31 C36 1.383(11) . ? C32 C33 1.382(13) . ? C32 H32 0.9300 . ? C33 C34 1.397(14) . ? C33 H33 0.9300 . ? C34 C35 1.381(12) . ? C34 H34 0.9300 . ? C35 C36 1.374(11) . ? C35 H35 0.9300 . ? C38 C39 1.493(14) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.515(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.381(12) . ? C41 C46 1.401(12) . ? C42 C43 1.397(11) . ? C42 C48 1.529(13) . ? C43 C44 1.416(14) . ? C43 C49 1.541(13) . ? C44 C45 1.379(13) . ? C44 C51 1.534(11) . ? C45 C46 1.398(11) . ? C45 C50 1.518(12) . ? C46 C47 1.503(12) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C53 C54 1.507(19) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C60 1.382(13) . ? C55 C56 1.414(13) . ? C56 C57 1.351(15) . ? C56 H56 0.9300 . ? C57 C58 1.407(16) . ? C57 H57 0.9300 . ? C58 C59 1.387(13) . ? C58 H58 0.9300 . ? C59 C60 1.392(14) . ? C59 H59 0.9300 . ? N9 C61 1.10(2) . ? C61 C62 1.57(3) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I1 Cu1 61.26(4) . . ? Cu1 I2 Cu2 61.47(4) . . ? Cu3 I3 Cu4 60.49(4) . . ? Cu4 I4 Cu3 60.82(4) . . ? C7 Cu1 I2 130.6(2) . . ? C7 Cu1 I1 122.9(2) . . ? I2 Cu1 I1 104.65(5) . . ? C7 Cu1 Cu2 159.4(3) . . ? I2 Cu1 Cu2 59.65(4) . . ? I1 Cu1 Cu2 57.79(4) . . ? C22 Cu2 I1 126.2(3) . . ? C22 Cu2 I2 124.5(3) . . ? I1 Cu2 I2 106.53(5) . . ? C22 Cu2 Cu1 161.5(3) . . ? I1 Cu2 Cu1 60.95(4) . . ? I2 Cu2 Cu1 58.89(4) . . ? C37 Cu3 I3 128.5(3) . . ? C37 Cu3 Cu4 159.8(2) . . ? I3 Cu3 Cu4 61.55(5) . . ? C37 Cu3 I4 122.6(3) . . ? I3 Cu3 I4 106.59(5) . . ? Cu4 Cu3 I4 58.21(4) . . ? C52 Cu4 I4 134.9(3) . . ? C52 Cu4 Cu3 158.5(3) . . ? I4 Cu4 Cu3 60.97(5) . . ? C52 Cu4 I3 116.7(3) . . ? I4 Cu4 I3 105.93(5) . . ? Cu3 Cu4 I3 57.95(4) . . ? C7 N1 C1 109.3(9) . . ? C7 N1 C8 125.5(8) . . ? C1 N1 C8 125.1(7) . . ? C7 N2 C6 109.7(8) . . ? C7 N2 C10 127.0(6) . . ? C6 N2 C10 123.3(8) . . ? C22 N3 C30 111.8(6) . . ? C22 N3 C21 127.0(6) . . ? C30 N3 C21 121.2(6) . . ? C22 N4 C25 111.5(8) . . ? C22 N4 C23 124.8(8) . . ? C25 N4 C23 122.1(7) . . ? C37 N5 C31 112.2(6) . . ? C37 N5 C38 123.6(6) . . ? C31 N5 C38 124.1(7) . . ? C37 N6 C36 111.0(6) . . ? C37 N6 C40 128.0(6) . . ? C36 N6 C40 121.0(6) . . ? C52 N7 C60 111.6(7) . . ? C52 N7 C51 125.9(7) . . ? C60 N7 C51 122.4(7) . . ? C52 N8 C55 111.7(8) . . ? C52 N8 C53 123.1(9) . . ? C55 N8 C53 125.1(8) . . ? C6 C1 N1 107.0(7) . . ? C6 C1 C2 121.6(10) . . ? N1 C1 C2 131.5(11) . . ? C3 C2 C1 117.5(11) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C4 C3 C2 120.5(9) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 123.6(11) . . ? C3 C4 H4 118.2 . . ? C5 C4 H4 118.2 . . ? C6 C5 C4 114.6(12) . . ? C6 C5 H5 122.7 . . ? C4 C5 H5 122.7 . . ? C1 C6 C5 122.2(8) . . ? C1 C6 N2 107.4(8) . . ? C5 C6 N2 130.5(10) . . ? N2 C7 N1 106.7(7) . . ? N2 C7 Cu1 129.9(6) . . ? N1 C7 Cu1 123.4(8) . . ? N1 C8 C9 110.0(10) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 116.0(8) . . ? N2 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? N2 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C16 C11 C12 120.5(6) . . ? C16 C11 C10 120.6(7) . . ? C12 C11 C10 118.7(7) . . ? C13 C12 C11 119.1(6) . . ? C13 C12 C18 120.6(6) . . ? C11 C12 C18 120.3(6) . . ? C14 C13 C12 120.5(6) . . ? C14 C13 C19 122.1(6) . . ? C12 C13 C19 117.4(6) . . ? C13 C14 C15 119.8(6) . . ? C13 C14 C21 120.8(6) . . ? C15 C14 C21 119.2(6) . . ? C16 C15 C14 120.1(6) . . ? C16 C15 C20 118.8(6) . . ? C14 C15 C20 120.9(6) . . ? C11 C16 C15 119.8(6) . . ? C11 C16 C17 120.4(6) . . ? C15 C16 C17 119.8(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C14 115.4(7) . . ? N3 C21 H21A 108.4 . . ? C14 C21 H21A 108.4 . . ? N3 C21 H21B 108.4 . . ? C14 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? N3 C22 N4 105.6(6) . . ? N3 C22 Cu2 130.8(6) . . ? N4 C22 Cu2 123.6(7) . . ? N4 C23 C24 99.9(12) . . ? N4 C23 H23A 111.8 . . ? C24 C23 H23A 111.8 . . ? N4 C23 H23B 111.8 . . ? C24 C23 H23B 111.8 . . ? H23A C23 H23B 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 N4 106.3(6) . . ? C30 C25 C26 120.6(9) . . ? N4 C25 C26 132.9(9) . . ? C27 C26 C25 117.0(10) . . ? C27 C26 H26 121.5 . . ? C25 C26 H26 121.5 . . ? C26 C27 C28 122.4(8) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C29 C28 C27 120.3(8) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 116.8(8) . . ? C30 C29 H29 121.6 . . ? C28 C29 H29 121.6 . . ? C29 C30 C25 122.8(7) . . ? C29 C30 N3 132.3(8) . . ? C25 C30 N3 104.7(7) . . ? C32 C31 N5 131.7(8) . . ? C32 C31 C36 121.6(8) . . ? N5 C31 C36 106.7(7) . . ? C31 C32 C33 116.6(8) . . ? C31 C32 H32 121.7 . . ? C33 C32 H32 121.7 . . ? C32 C33 C34 121.8(8) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C35 C34 C33 120.8(9) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 116.6(8) . . ? C36 C35 H35 121.7 . . ? C34 C35 H35 121.7 . . ? C35 C36 C31 122.4(7) . . ? C35 C36 N6 131.9(7) . . ? C31 C36 N6 105.7(7) . . ? N5 C37 N6 104.4(6) . . ? N5 C37 Cu3 125.1(5) . . ? N6 C37 Cu3 130.5(5) . . ? N5 C38 C39 109.9(7) . . ? N5 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? N5 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 C41 115.1(6) . . ? N6 C40 H40A 108.5 . . ? C41 C40 H40A 108.5 . . ? N6 C40 H40B 108.5 . . ? C41 C40 H40B 108.5 . . ? H40A C40 H40B 107.5 . . ? C42 C41 C46 122.0(7) . . ? C42 C41 C40 119.8(8) . . ? C46 C41 C40 118.2(7) . . ? C41 C42 C43 120.1(8) . . ? C41 C42 C48 122.2(7) . . ? C43 C42 C48 117.7(8) . . ? C42 C43 C44 117.8(8) . . ? C42 C43 C49 120.2(9) . . ? C44 C43 C49 121.9(8) . . ? C45 C44 C43 121.6(7) . . ? C45 C44 C51 120.5(9) . . ? C43 C44 C51 117.8(9) . . ? C44 C45 C46 120.1(8) . . ? C44 C45 C50 121.3(8) . . ? C46 C45 C50 118.5(8) . . ? C45 C46 C41 118.1(8) . . ? C45 C46 C47 119.7(8) . . ? C41 C46 C47 122.2(7) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C48 H48A 109.5 . . ? C42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C43 C49 H49A 109.5 . . ? C43 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C43 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N7 C51 C44 115.0(7) . . ? N7 C51 H51A 108.5 . . ? C44 C51 H51A 108.5 . . ? N7 C51 H51B 108.5 . . ? C44 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? N7 C52 N8 104.7(8) . . ? N7 C52 Cu4 130.9(6) . . ? N8 C52 Cu4 124.1(7) . . ? N8 C53 C54 111.7(10) . . ? N8 C53 H53A 109.3 . . ? C54 C53 H53A 109.3 . . ? N8 C53 H53B 109.3 . . ? C54 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N8 C55 C60 106.2(7) . . ? N8 C55 C56 133.2(9) . . ? C60 C55 C56 120.3(10) . . ? C57 C56 C55 117.5(10) . . ? C57 C56 H56 121.2 . . ? C55 C56 H56 121.2 . . ? C56 C57 C58 121.5(9) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C59 C58 C57 122.3(11) . . ? C59 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C58 C59 C60 115.4(9) . . ? C58 C59 H59 122.3 . . ? C60 C59 H59 122.3 . . ? C55 C60 N7 105.8(8) . . ? C55 C60 C59 123.0(8) . . ? N7 C60 C59 131.2(8) . . ? N9 C61 C62 164(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu2 I2 Cu1 C7 158.0(4) . . . . ? Cu2 I2 Cu1 I1 -37.67(4) . . . . ? Cu2 I1 Cu1 C7 -155.5(3) . . . . ? Cu2 I1 Cu1 I2 38.55(4) . . . . ? Cu1 I1 Cu2 C22 159.7(3) . . . . ? Cu1 I1 Cu2 I2 -38.61(4) . . . . ? Cu1 I2 Cu2 C22 -158.4(3) . . . . ? Cu1 I2 Cu2 I1 39.58(5) . . . . ? C7 Cu1 Cu2 C22 -19.6(10) . . . . ? I2 Cu1 Cu2 C22 106.3(8) . . . . ? I1 Cu1 Cu2 C22 -118.0(8) . . . . ? C7 Cu1 Cu2 I1 98.4(6) . . . . ? I2 Cu1 Cu2 I1 -135.68(5) . . . . ? C7 Cu1 Cu2 I2 -125.9(6) . . . . ? I1 Cu1 Cu2 I2 135.68(5) . . . . ? Cu4 I3 Cu3 C37 158.9(3) . . . . ? Cu4 I3 Cu3 I4 -38.14(4) . . . . ? Cu4 I4 Cu3 C37 -156.1(3) . . . . ? Cu4 I4 Cu3 I3 39.71(4) . . . . ? Cu3 I4 Cu4 C52 161.6(4) . . . . ? Cu3 I4 Cu4 I3 -37.86(4) . . . . ? C37 Cu3 Cu4 C52 -43.7(11) . . . . ? I3 Cu3 Cu4 C52 81.7(8) . . . . ? I4 Cu3 Cu4 C52 -142.4(8) . . . . ? C37 Cu3 Cu4 I4 98.7(8) . . . . ? I3 Cu3 Cu4 I4 -135.87(5) . . . . ? C37 Cu3 Cu4 I3 -125.4(8) . . . . ? I4 Cu3 Cu4 I3 135.87(5) . . . . ? Cu3 I3 Cu4 C52 -156.0(3) . . . . ? Cu3 I3 Cu4 I4 39.28(4) . . . . ? C7 N1 C1 C6 1.3(8) . . . . ? C8 N1 C1 C6 -176.5(8) . . . . ? C7 N1 C1 C2 -178.0(8) . . . . ? C8 N1 C1 C2 4.2(13) . . . . ? C6 C1 C2 C3 -0.3(12) . . . . ? N1 C1 C2 C3 178.9(8) . . . . ? C1 C2 C3 C4 -0.4(14) . . . . ? C2 C3 C4 C5 1.0(15) . . . . ? C3 C4 C5 C6 -0.8(14) . . . . ? N1 C1 C6 C5 -178.8(7) . . . . ? C2 C1 C6 C5 0.5(12) . . . . ? N1 C1 C6 N2 -0.7(8) . . . . ? C2 C1 C6 N2 178.7(7) . . . . ? C4 C5 C6 C1 0.0(12) . . . . ? C4 C5 C6 N2 -177.6(8) . . . . ? C7 N2 C6 C1 -0.2(9) . . . . ? C10 N2 C6 C1 178.9(7) . . . . ? C7 N2 C6 C5 177.8(8) . . . . ? C10 N2 C6 C5 -3.1(13) . . . . ? C6 N2 C7 N1 1.0(8) . . . . ? C10 N2 C7 N1 -178.1(7) . . . . ? C6 N2 C7 Cu1 -176.6(6) . . . . ? C10 N2 C7 Cu1 4.3(12) . . . . ? C1 N1 C7 N2 -1.4(8) . . . . ? C8 N1 C7 N2 176.4(7) . . . . ? C1 N1 C7 Cu1 176.4(5) . . . . ? C8 N1 C7 Cu1 -5.8(11) . . . . ? I2 Cu1 C7 N2 -103.0(7) . . . . ? I1 Cu1 C7 N2 95.1(7) . . . . ? Cu2 Cu1 C7 N2 9.9(12) . . . . ? I2 Cu1 C7 N1 79.7(7) . . . . ? I1 Cu1 C7 N1 -82.2(6) . . . . ? Cu2 Cu1 C7 N1 -167.3(4) . . . . ? C7 N1 C8 C9 -98.0(11) . . . . ? C1 N1 C8 C9 79.4(11) . . . . ? C7 N2 C10 C11 -9.2(11) . . . . ? C6 N2 C10 C11 171.9(7) . . . . ? N2 C10 C11 C16 94.9(10) . . . . ? N2 C10 C11 C12 -89.5(10) . . . . ? C16 C11 C12 C13 4.7(13) . . . . ? C10 C11 C12 C13 -170.9(8) . . . . ? C16 C11 C12 C18 -174.1(8) . . . . ? C10 C11 C12 C18 10.3(13) . . . . ? C11 C12 C13 C14 -2.3(12) . . . . ? C18 C12 C13 C14 176.5(8) . . . . ? C11 C12 C13 C19 -179.9(8) . . . . ? C18 C12 C13 C19 -1.1(12) . . . . ? C12 C13 C14 C15 0.2(12) . . . . ? C19 C13 C14 C15 177.7(8) . . . . ? C12 C13 C14 C21 176.0(8) . . . . ? C19 C13 C14 C21 -6.5(12) . . . . ? C13 C14 C15 C16 -0.4(13) . . . . ? C21 C14 C15 C16 -176.3(8) . . . . ? C13 C14 C15 C20 -175.7(8) . . . . ? C21 C14 C15 C20 8.4(12) . . . . ? C12 C11 C16 C15 -5.0(13) . . . . ? C10 C11 C16 C15 170.6(8) . . . . ? C12 C11 C16 C17 174.2(8) . . . . ? C10 C11 C16 C17 -10.3(13) . . . . ? C14 C15 C16 C11 2.8(13) . . . . ? C20 C15 C16 C11 178.2(8) . . . . ? C14 C15 C16 C17 -176.3(8) . . . . ? C20 C15 C16 C17 -0.9(12) . . . . ? C22 N3 C21 C14 -4.0(11) . . . . ? C30 N3 C21 C14 176.8(6) . . . . ? C13 C14 C21 N3 102.7(8) . . . . ? C15 C14 C21 N3 -81.5(9) . . . . ? C30 N3 C22 N4 -1.0(9) . . . . ? C21 N3 C22 N4 179.7(7) . . . . ? C30 N3 C22 Cu2 178.0(6) . . . . ? C21 N3 C22 Cu2 -1.3(12) . . . . ? C25 N4 C22 N3 1.2(10) . . . . ? C23 N4 C22 N3 -164.6(10) . . . . ? C25 N4 C22 Cu2 -177.8(6) . . . . ? C23 N4 C22 Cu2 16.4(14) . . . . ? I1 Cu2 C22 N3 -90.8(8) . . . . ? I2 Cu2 C22 N3 110.7(7) . . . . ? Cu1 Cu2 C22 N3 16.2(15) . . . . ? I1 Cu2 C22 N4 88.0(8) . . . . ? I2 Cu2 C22 N4 -70.5(9) . . . . ? Cu1 Cu2 C22 N4 -165.0(6) . . . . ? C22 N4 C23 C24 -97.8(12) . . . . ? C25 N4 C23 C24 97.9(12) . . . . ? C22 N4 C25 C30 -1.0(11) . . . . ? C23 N4 C25 C30 165.3(9) . . . . ? C22 N4 C25 C26 -177.1(10) . . . . ? C23 N4 C25 C26 -10.9(17) . . . . ? C30 C25 C26 C27 -0.4(14) . . . . ? N4 C25 C26 C27 175.3(10) . . . . ? C25 C26 C27 C28 0.6(14) . . . . ? C26 C27 C28 C29 -1.1(13) . . . . ? C27 C28 C29 C30 1.3(11) . . . . ? C28 C29 C30 C25 -1.2(11) . . . . ? C28 C29 C30 N3 -176.3(7) . . . . ? N4 C25 C30 C29 -176.0(7) . . . . ? C26 C25 C30 C29 0.7(12) . . . . ? N4 C25 C30 N3 0.3(9) . . . . ? C26 C25 C30 N3 177.0(8) . . . . ? C22 N3 C30 C29 176.2(8) . . . . ? C21 N3 C30 C29 -4.5(11) . . . . ? C22 N3 C30 C25 0.4(8) . . . . ? C21 N3 C30 C25 179.7(6) . . . . ? C37 N5 C31 C32 178.3(14) . . . . ? C38 N5 C31 C32 -6.4(19) . . . . ? C37 N5 C31 C36 -0.9(12) . . . . ? C38 N5 C31 C36 174.4(9) . . . . ? N5 C31 C32 C33 -177.9(13) . . . . ? C36 C31 C32 C33 1(2) . . . . ? C31 C32 C33 C34 -5(3) . . . . ? C32 C33 C34 C35 5(3) . . . . ? C33 C34 C35 C36 -2(2) . . . . ? C34 C35 C36 C31 -1.5(18) . . . . ? C34 C35 C36 N6 179.8(12) . . . . ? C32 C31 C36 C35 2.0(19) . . . . ? N5 C31 C36 C35 -178.7(10) . . . . ? C32 C31 C36 N6 -179.0(12) . . . . ? N5 C31 C36 N6 0.3(12) . . . . ? C37 N6 C36 C35 179.3(12) . . . . ? C40 N6 C36 C35 -2.2(17) . . . . ? C37 N6 C36 C31 0.4(11) . . . . ? C40 N6 C36 C31 178.9(8) . . . . ? C31 N5 C37 N6 1.1(10) . . . . ? C38 N5 C37 N6 -174.2(8) . . . . ? C31 N5 C37 Cu3 -178.8(7) . . . . ? C38 N5 C37 Cu3 5.9(13) . . . . ? C36 N6 C37 N5 -0.9(10) . . . . ? C40 N6 C37 N5 -179.3(8) . . . . ? C36 N6 C37 Cu3 179.0(7) . . . . ? C40 N6 C37 Cu3 0.5(13) . . . . ? I3 Cu3 C37 N5 90.7(8) . . . . ? Cu4 Cu3 C37 N5 -155.7(5) . . . . ? I4 Cu3 C37 N5 -69.9(8) . . . . ? I3 Cu3 C37 N6 -89.2(8) . . . . ? Cu4 Cu3 C37 N6 24.4(14) . . . . ? I4 Cu3 C37 N6 110.3(8) . . . . ? C37 N5 C38 C39 96.1(10) . . . . ? C31 N5 C38 C39 -78.7(11) . . . . ? C37 N6 C40 C41 -9.0(12) . . . . ? C36 N6 C40 C41 172.7(8) . . . . ? N6 C40 C41 C42 105.5(9) . . . . ? N6 C40 C41 C46 -75.9(9) . . . . ? C46 C41 C42 C43 -3.0(11) . . . . ? C40 C41 C42 C43 175.6(7) . . . . ? C46 C41 C42 C48 174.3(7) . . . . ? C40 C41 C42 C48 -7.1(11) . . . . ? C41 C42 C43 C44 -0.4(11) . . . . ? C48 C42 C43 C44 -177.8(8) . . . . ? C41 C42 C43 C49 177.2(8) . . . . ? C48 C42 C43 C49 -0.2(12) . . . . ? C42 C43 C44 C45 3.9(12) . . . . ? C49 C43 C44 C45 -173.7(8) . . . . ? C42 C43 C44 C51 -173.8(7) . . . . ? C49 C43 C44 C51 8.7(12) . . . . ? C43 C44 C45 C46 -4.1(11) . . . . ? C51 C44 C45 C46 173.5(7) . . . . ? C43 C44 C45 C50 174.5(7) . . . . ? C51 C44 C45 C50 -7.9(11) . . . . ? C44 C45 C46 C41 0.7(10) . . . . ? C50 C45 C46 C41 -177.9(7) . . . . ? C44 C45 C46 C47 -178.9(7) . . . . ? C50 C45 C46 C47 2.5(10) . . . . ? C42 C41 C46 C45 2.8(10) . . . . ? C40 C41 C46 C45 -175.8(6) . . . . ? C42 C41 C46 C47 -177.6(7) . . . . ? C40 C41 C46 C47 3.8(10) . . . . ? C52 N7 C51 C44 -20.6(16) . . . . ? C60 N7 C51 C44 163.4(10) . . . . ? C45 C44 C51 N7 101.9(10) . . . . ? C43 C44 C51 N7 -80.4(12) . . . . ? C60 N7 C52 N8 -1.6(12) . . . . ? C51 N7 C52 N8 -177.9(10) . . . . ? C60 N7 C52 Cu4 -174.3(9) . . . . ? C51 N7 C52 Cu4 9.3(17) . . . . ? C55 N8 C52 N7 1.5(13) . . . . ? C53 N8 C52 N7 179.0(10) . . . . ? C55 N8 C52 Cu4 175.0(8) . . . . ? C53 N8 C52 Cu4 -7.6(16) . . . . ? I4 Cu4 C52 N7 -102.4(10) . . . . ? Cu3 Cu4 C52 N7 28.8(17) . . . . ? I3 Cu4 C52 N7 98.6(10) . . . . ? I4 Cu4 C52 N8 86.1(10) . . . . ? Cu3 Cu4 C52 N8 -142.8(7) . . . . ? I3 Cu4 C52 N8 -72.9(10) . . . . ? C52 N8 C53 C54 -84.9(14) . . . . ? C55 N8 C53 C54 92.2(14) . . . . ? C52 N8 C55 C60 -1.0(13) . . . . ? C53 N8 C55 C60 -178.4(11) . . . . ? C52 N8 C55 C56 -175.1(13) . . . . ? C53 N8 C55 C56 7(2) . . . . ? N8 C55 C56 C57 175.9(13) . . . . ? C60 C55 C56 C57 2.4(18) . . . . ? C55 C56 C57 C58 -0.9(19) . . . . ? C56 C57 C58 C59 0(2) . . . . ? C57 C58 C59 C60 -0.4(19) . . . . ? N8 C55 C60 N7 0.0(13) . . . . ? C56 C55 C60 N7 175.0(11) . . . . ? N8 C55 C60 C59 -178.1(11) . . . . ? C56 C55 C60 C59 -3.1(19) . . . . ? C52 N7 C60 C55 1.0(13) . . . . ? C51 N7 C60 C55 177.5(10) . . . . ? C52 N7 C60 C59 178.9(12) . . . . ? C51 N7 C60 C59 -4.7(19) . . . . ? C58 C59 C60 C55 2.0(18) . . . . ? C58 C59 C60 N7 -175.6(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.105 _refine_diff_density_min -2.150 _refine_diff_density_rms 0.155 data_2c _database_code_depnum_ccdc_archive 'CCDC 757349' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H73 Br6 Hg3 N8 O S' _chemical_formula_weight 2059.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0172(18) _cell_length_b 16.221(2) _cell_length_c 18.554(2) _cell_angle_alpha 89.714(2) _cell_angle_beta 69.778(2) _cell_angle_gamma 72.194(2) _cell_volume 3745.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7600 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 22.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1950 _exptl_absorpt_coefficient_mu 9.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.108 _exptl_absorpt_correction_T_max 0.152 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 20719 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14714 _reflns_number_gt 10178 _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^)+(0.0555P)^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 14562 _refine_ls_number_parameters 783 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.033 _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 0.93942(2) 0.083489(19) 0.296469(14) 0.04795(9) Uani 1 1 d . . . Hg2 Hg 0.58696(2) 0.400278(17) 0.204522(14) 0.04433(8) Uani 1 1 d . . . Hg3 Hg 0.12838(3) 0.49179(2) 0.218414(18) 0.06071(10) Uani 1 1 d . . . Br1 Br 1.15366(8) -0.01961(6) 0.31291(5) 0.0716(2) Uani 1 1 d . . . Br2 Br 0.75280(6) 0.25891(5) 0.24537(4) 0.0572(2) Uani 1 1 d . . . Br3 Br 0.32145(7) 0.50553(5) 0.19259(5) 0.0603(2) Uani 1 1 d . . . Br4 Br 0.01758(7) 0.63459(6) 0.17788(6) 0.0796(3) Uani 1 1 d . . . Br5 Br 0.15556(10) 0.35645(7) 0.13260(8) 0.1139(5) Uani 1 1 d . . . Br6 Br 0.01954(15) 0.48642(10) 0.36204(6) 0.1431(7) Uani 1 1 d . . . N1 N 1.0571(5) 0.0378(4) 0.1240(3) 0.0427(13) Uani 1 1 d . . . N2 N 0.9778(4) -0.0582(3) 0.1652(3) 0.0376(12) Uani 1 1 d . . . N3 N 0.9241(5) 0.2301(4) 0.4039(3) 0.0463(14) Uani 1 1 d . . . N4 N 0.8253(4) 0.1566(3) 0.4727(3) 0.0379(12) Uani 1 1 d . . . N5 N 0.6018(5) 0.2658(4) 0.0858(3) 0.0452(14) Uani 1 1 d . . . N6 N 0.6856(4) 0.3528(3) 0.0234(3) 0.0396(13) Uani 1 1 d . . . N7 N 0.4319(5) 0.4525(4) 0.3713(3) 0.0575(16) Uani 1 1 d D . . N8 N 0.5267(4) 0.5408(3) 0.3421(3) 0.0417(13) Uani 1 1 d . . . C1 C 0.9904(5) 0.0161(4) 0.1866(4) 0.0414(16) Uani 1 1 d . . . C2 C 1.0870(5) -0.0231(4) 0.0600(4) 0.0392(15) Uani 1 1 d . . . C3 C 1.0391(5) -0.0848(4) 0.0865(3) 0.0384(16) Uani 1 1 d . . . C4 C 1.0497(6) -0.1548(4) 0.0394(4) 0.0475(17) Uani 1 1 d . . . H4 H 1.0151 -0.1954 0.0579 0.057 Uiso 1 1 calc R . . C5 C 1.1158(6) -0.1611(5) -0.0380(4) 0.0512(19) Uani 1 1 d . . . H5 H 1.1278 -0.2082 -0.0721 0.061 Uiso 1 1 calc R . . C6 C 1.1635(6) -0.0988(5) -0.0644(4) 0.0529(19) Uani 1 1 d . . . H6 H 1.2059 -0.1045 -0.1164 0.064 Uiso 1 1 calc R . . C7 C 1.1509(6) -0.0280(5) -0.0165(4) 0.0509(18) Uani 1 1 d . . . H7 H 1.1836 0.0138 -0.0349 0.061 Uiso 1 1 calc R . . C8 C 1.0907(7) 0.1153(5) 0.1191(4) 0.064(2) Uani 1 1 d . . . H8A H 1.0392 0.1595 0.1610 0.077 Uiso 1 1 calc R . . H8B H 1.0915 0.1386 0.0707 0.077 Uiso 1 1 calc R . . C9 C 1.1989(8) 0.0949(6) 0.1235(5) 0.078(3) Uani 1 1 d . . . H9A H 1.2010 0.0644 0.1678 0.117 Uiso 1 1 calc R . . H9B H 1.2140 0.1480 0.1283 0.117 Uiso 1 1 calc R . . H9C H 1.2517 0.0590 0.0775 0.117 Uiso 1 1 calc R . . C10 C 0.9092(6) -0.1081(5) 0.2104(4) 0.0483(17) Uani 1 1 d . . . H10A H 0.9529 -0.1682 0.2075 0.058 Uiso 1 1 calc R . . H10B H 0.8554 -0.1076 0.1885 0.058 Uiso 1 1 calc R . . C11 C 0.8543(5) -0.0686(4) 0.2943(4) 0.0391(15) Uani 1 1 d . . . C12 C 0.9070(5) -0.0977(4) 0.3466(4) 0.0434(16) Uani 1 1 d . . . C13 C 0.8695(6) -0.0466(5) 0.4180(4) 0.0449(16) Uani 1 1 d . . . C14 C 0.7834(5) 0.0301(4) 0.4360(4) 0.0402(15) Uani 1 1 d . . . C15 C 0.7208(5) 0.0517(4) 0.3869(4) 0.0414(16) Uani 1 1 d . . . C16 C 0.7576(5) 0.0010(4) 0.3162(4) 0.0393(15) Uani 1 1 d . . . C17 C 1.0036(7) -0.1787(5) 0.3257(5) 0.072(2) Uani 1 1 d . . . H17A H 0.9984 -0.2189 0.2906 0.107 Uiso 1 1 calc R . . H17B H 1.0063 -0.2051 0.3717 0.107 Uiso 1 1 calc R . . H17C H 1.0677 -0.1636 0.3015 0.107 Uiso 1 1 calc R . . C18 C 0.9289(7) -0.0754(6) 0.4735(5) 0.073(3) Uani 1 1 d . . . H18A H 0.8809 -0.0527 0.5254 0.109 Uiso 1 1 calc R . . H18B H 0.9886 -0.0537 0.4606 0.109 Uiso 1 1 calc R . . H18C H 0.9547 -0.1379 0.4694 0.109 Uiso 1 1 calc R . . C19 C 0.6205(6) 0.1292(5) 0.4096(5) 0.067(2) Uani 1 1 d . . . H19A H 0.6395 0.1813 0.3988 0.100 Uiso 1 1 calc R . . H19B H 0.5805 0.1328 0.4638 0.100 Uiso 1 1 calc R . . H19C H 0.5775 0.1233 0.3806 0.100 Uiso 1 1 calc R . . C20 C 0.6954(7) 0.0283(5) 0.2633(5) 0.066(2) Uani 1 1 d . . . H20A H 0.6239 0.0261 0.2881 0.098 Uiso 1 1 calc R . . H20B H 0.7306 -0.0106 0.2161 0.098 Uiso 1 1 calc R . . H20C H 0.6923 0.0866 0.2518 0.098 Uiso 1 1 calc R . . C21 C 0.7635(6) 0.0959(5) 0.4998(4) 0.0494(18) Uani 1 1 d . . . H21A H 0.6874 0.1288 0.5213 0.059 Uiso 1 1 calc R . . H21B H 0.7834 0.0662 0.5405 0.059 Uiso 1 1 calc R . . C22 C 0.8887(6) 0.1635(4) 0.4003(4) 0.0438(16) Uani 1 1 d . . . C23 C 0.8855(6) 0.2674(4) 0.4800(4) 0.0435(16) Uani 1 1 d . . . C24 C 0.8210(5) 0.2221(4) 0.5239(4) 0.0390(15) Uani 1 1 d . . . C25 C 0.7671(6) 0.2435(5) 0.6017(4) 0.0474(17) Uani 1 1 d . . . H25 H 0.7234 0.2127 0.6302 0.057 Uiso 1 1 calc R . . C26 C 0.7795(6) 0.3116(5) 0.6363(4) 0.0519(19) Uani 1 1 d . . . H26 H 0.7444 0.3272 0.6893 0.062 Uiso 1 1 calc R . . C27 C 0.8447(6) 0.3583(5) 0.5928(5) 0.055(2) Uani 1 1 d . . . H27 H 0.8519 0.4044 0.6177 0.066 Uiso 1 1 calc R . . C28 C 0.8995(6) 0.3371(4) 0.5125(4) 0.0517(19) Uani 1 1 d . . . H28 H 0.9424 0.3681 0.4832 0.062 Uiso 1 1 calc R . . C29 C 0.9963(7) 0.2603(5) 0.3397(4) 0.061(2) Uani 1 1 d . . . H29 H 0.9737 0.2940 0.3043 0.074 Uiso 1 1 calc R . . C30 C 1.1096(7) 0.2315(6) 0.3367(6) 0.084(3) Uani 1 1 d . . . H30A H 1.1132 0.2605 0.3802 0.126 Uiso 1 1 calc R . . H30B H 1.1546 0.2459 0.2897 0.126 Uiso 1 1 calc R . . H30C H 1.1337 0.1697 0.3383 0.126 Uiso 1 1 calc R . . C31 C 0.6306(5) 0.3363(4) 0.0948(3) 0.0394(15) Uani 1 1 d . . . C32 C 0.6394(6) 0.2357(4) 0.0070(4) 0.0438(16) Uani 1 1 d . . . C33 C 0.6937(5) 0.2907(4) -0.0332(4) 0.0403(16) Uani 1 1 d . . . C34 C 0.7427(6) 0.2785(5) -0.1120(4) 0.0463(17) Uani 1 1 d . . . H34 H 0.7781 0.3157 -0.1385 0.056 Uiso 1 1 calc R . . C35 C 0.7370(6) 0.2080(5) -0.1504(4) 0.0519(19) Uani 1 1 d . . . H35 H 0.7712 0.1967 -0.2038 0.062 Uiso 1 1 calc R . . C36 C 0.6809(8) 0.1532(5) -0.1108(5) 0.067(2) Uani 1 1 d . . . H36 H 0.6767 0.1079 -0.1387 0.080 Uiso 1 1 calc R . . C37 C 0.6312(7) 0.1652(5) -0.0304(4) 0.056(2) Uani 1 1 d . . . H37 H 0.5951 0.1286 -0.0036 0.067 Uiso 1 1 calc R . . C38 C 0.5427(6) 0.2236(5) 0.1485(4) 0.057(2) Uani 1 1 d . . . H38A H 0.5464 0.2415 0.1970 0.068 Uiso 1 1 calc R . . H38B H 0.5754 0.1608 0.1376 0.068 Uiso 1 1 calc R . . C39 C 0.4264(7) 0.2492(6) 0.1550(6) 0.088(3) Uani 1 1 d . . . H39A H 0.3942 0.3113 0.1663 0.132 Uiso 1 1 calc R . . H39B H 0.3883 0.2216 0.1958 0.132 Uiso 1 1 calc R . . H39C H 0.4231 0.2308 0.1071 0.132 Uiso 1 1 calc R . . C40 C 0.7330(6) 0.4227(5) -0.0002(4) 0.0474(17) Uani 1 1 d . . . H40A H 0.7006 0.4569 -0.0338 0.057 Uiso 1 1 calc R . . H40B H 0.8095 0.3973 -0.0290 0.057 Uiso 1 1 calc R . . C41 C 0.7150(5) 0.4810(4) 0.0693(4) 0.0398(15) Uani 1 1 d . . . C42 C 0.6202(5) 0.5515(4) 0.0984(4) 0.0415(16) Uani 1 1 d . . . C43 C 0.5879(5) 0.5916(4) 0.1737(4) 0.0440(16) Uani 1 1 d . . . C44 C 0.6532(6) 0.5586(4) 0.2185(4) 0.0427(16) Uani 1 1 d . . . C45 C 0.7568(5) 0.4990(4) 0.1834(4) 0.0416(16) Uani 1 1 d . . . C46 C 0.7876(5) 0.4593(4) 0.1092(4) 0.0415(15) Uani 1 1 d . . . C47 C 0.5490(6) 0.5814(6) 0.0508(4) 0.063(2) Uani 1 1 d . . . H47A H 0.5135 0.6432 0.0624 0.095 Uiso 1 1 calc R . . H47B H 0.4963 0.5521 0.0632 0.095 Uiso 1 1 calc R . . H47C H 0.5923 0.5678 -0.0032 0.095 Uiso 1 1 calc R . . C48 C 0.4816(6) 0.6645(5) 0.2094(5) 0.064(2) Uani 1 1 d . . . H48A H 0.4677 0.6778 0.2632 0.096 Uiso 1 1 calc R . . H48B H 0.4249 0.6465 0.2043 0.096 Uiso 1 1 calc R . . H48C H 0.4850 0.7154 0.1834 0.096 Uiso 1 1 calc R . . C49 C 0.8341(6) 0.4736(5) 0.2262(4) 0.060(2) Uani 1 1 d . . . H49A H 0.8008 0.5052 0.2770 0.090 Uiso 1 1 calc R . . H49B H 0.8981 0.4874 0.1983 0.090 Uiso 1 1 calc R . . H49C H 0.8524 0.4122 0.2304 0.090 Uiso 1 1 calc R . . C50 C 0.8993(6) 0.3912(5) 0.0725(5) 0.069(2) Uani 1 1 d . . . H50A H 0.9454 0.4160 0.0343 0.104 Uiso 1 1 calc R . . H50B H 0.8936 0.3416 0.0485 0.104 Uiso 1 1 calc R . . H50C H 0.9290 0.3733 0.1118 0.104 Uiso 1 1 calc R . . C51 C 0.6056(6) 0.5836(5) 0.3048(4) 0.0522(18) Uani 1 1 d . . . H51A H 0.6625 0.5673 0.3257 0.063 Uiso 1 1 calc R . . H51B H 0.5715 0.6462 0.3157 0.063 Uiso 1 1 calc R . . C52 C 0.5099(6) 0.4718(5) 0.3145(4) 0.0444(16) Uani 1 1 d . . . C53 C 0.3973(6) 0.5103(5) 0.4385(4) 0.0492(18) Uani 1 1 d . . . C54 C 0.4564(5) 0.5659(5) 0.4198(4) 0.0441(17) Uani 1 1 d . . . C55 C 0.4436(6) 0.6318(5) 0.4731(4) 0.0522(19) Uani 1 1 d . . . H55 H 0.4839 0.6694 0.4608 0.063 Uiso 1 1 calc R . . C56 C 0.3663(7) 0.6381(5) 0.5463(4) 0.064(2) Uani 1 1 d . . . H56 H 0.3549 0.6811 0.5841 0.076 Uiso 1 1 calc R . . C57 C 0.3070(7) 0.5835(6) 0.5641(4) 0.066(2) Uani 1 1 d . . . H57 H 0.2561 0.5904 0.6136 0.079 Uiso 1 1 calc R . . C58 C 0.3202(7) 0.5183(6) 0.5111(4) 0.067(2) Uani 1 1 d . . . H58 H 0.2791 0.4812 0.5235 0.080 Uiso 1 1 calc R . . C59 C 0.3643(9) 0.3975(7) 0.3615(7) 0.120(4) Uani 1 1 d DU . . H59A H 0.2913 0.4179 0.3988 0.144 Uiso 1 1 calc R . . H59B H 0.3633 0.3948 0.3095 0.144 Uiso 1 1 calc R . . C60 C 0.4278(11) 0.3145(8) 0.3774(8) 0.149(5) Uani 1 1 d DU . . H60A H 0.5025 0.3038 0.3480 0.224 Uiso 1 1 calc R . . H60B H 0.4059 0.2684 0.3632 0.224 Uiso 1 1 calc R . . H60C H 0.4165 0.3168 0.4315 0.224 Uiso 1 1 calc R . . O1 O 0.7777(15) 0.8553(9) 0.0940(11) 0.112(7) Uani 0.514(11) 1 d PDU A 1 S1 S 0.7218(5) 0.7906(4) 0.1156(4) 0.095(3) Uani 0.514(11) 1 d PD A 1 C61 C 0.8188(14) 0.6873(7) 0.0703(12) 0.070(6) Uani 0.514(11) 1 d PDU A 1 H61A H 0.8827 0.6799 0.0814 0.105 Uiso 0.514(11) 1 calc PR A 1 H61B H 0.8360 0.6848 0.0154 0.105 Uiso 0.514(11) 1 calc PR A 1 H61C H 0.7899 0.6417 0.0897 0.105 Uiso 0.514(11) 1 calc PR A 1 C62 C 0.642(3) 0.802(2) 0.056(2) 0.19(2) Uani 0.514(11) 1 d PDU A 1 H62A H 0.6541 0.8460 0.0220 0.280 Uiso 0.514(11) 1 calc PR A 1 H62B H 0.5676 0.8184 0.0876 0.280 Uiso 0.514(11) 1 calc PR A 1 H62C H 0.6628 0.7474 0.0250 0.280 Uiso 0.514(11) 1 calc PR A 1 O1' O 0.7418(19) 0.8592(12) 0.1187(13) 0.169(13) Uani 0.486(11) 1 d PDU A 2 S1' S 0.7709(6) 0.7898(4) 0.0568(5) 0.093(3) Uani 0.486(11) 1 d PD A 2 C61' C 0.800(3) 0.6895(11) 0.0986(16) 0.141(16) Uani 0.486(11) 1 d PDU A 2 H61D H 0.8735 0.6548 0.0716 0.211 Uiso 0.486(11) 1 calc PR A 2 H61E H 0.7536 0.6583 0.0944 0.211 Uiso 0.486(11) 1 calc PR A 2 H61F H 0.7883 0.7018 0.1521 0.211 Uiso 0.486(11) 1 calc PR A 2 C62' C 0.6456(13) 0.7901(15) 0.0506(14) 0.068(7) Uani 0.486(11) 1 d PDU A 2 H62D H 0.5941 0.8475 0.0672 0.102 Uiso 0.486(11) 1 calc PR A 2 H62E H 0.6193 0.7496 0.0832 0.102 Uiso 0.486(11) 1 calc PR A 2 H62F H 0.6565 0.7732 -0.0019 0.102 Uiso 0.486(11) 1 calc PR A 2 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 0.05433(18) 0.05762(18) 0.03285(14) -0.00578(12) -0.00488(12) -0.03173(15) Hg2 0.05176(17) 0.04904(16) 0.03298(14) -0.00059(11) -0.00893(12) -0.02465(14) Hg3 0.0684(2) 0.0610(2) 0.0573(2) 0.00336(15) -0.02173(16) -0.02836(18) Br1 0.0826(6) 0.0715(5) 0.0612(5) 0.0006(4) -0.0348(5) -0.0155(5) Br2 0.0645(5) 0.0570(5) 0.0417(4) -0.0010(3) -0.0190(4) -0.0084(4) Br3 0.0641(5) 0.0628(5) 0.0621(5) 0.0125(4) -0.0305(4) -0.0232(4) Br4 0.0569(5) 0.0684(6) 0.0995(7) 0.0078(5) -0.0182(5) -0.0128(5) Br5 0.0970(8) 0.0951(8) 0.1476(11) -0.0571(7) -0.0687(8) 0.0008(7) Br6 0.2397(18) 0.1588(12) 0.0621(7) 0.0111(7) -0.0118(8) -0.1565(13) N1 0.046(3) 0.047(3) 0.035(3) -0.002(3) -0.013(3) -0.015(3) N2 0.036(3) 0.039(3) 0.036(3) -0.002(2) -0.014(2) -0.008(3) N3 0.055(4) 0.047(3) 0.040(3) 0.001(3) -0.015(3) -0.023(3) N4 0.037(3) 0.041(3) 0.032(3) 0.002(2) -0.011(2) -0.010(3) N5 0.053(4) 0.046(3) 0.041(3) 0.006(3) -0.017(3) -0.023(3) N6 0.046(3) 0.041(3) 0.031(3) -0.002(2) -0.015(3) -0.013(3) N7 0.063(4) 0.065(4) 0.046(4) -0.001(3) -0.008(3) -0.035(4) N8 0.045(3) 0.044(3) 0.034(3) -0.005(2) -0.015(3) -0.011(3) C1 0.041(4) 0.046(4) 0.040(4) 0.002(3) -0.017(3) -0.014(3) C2 0.038(4) 0.047(4) 0.032(3) 0.003(3) -0.014(3) -0.012(3) C3 0.037(4) 0.042(4) 0.029(3) -0.005(3) -0.018(3) 0.005(3) C4 0.048(4) 0.039(4) 0.052(4) -0.001(3) -0.026(4) -0.001(3) C5 0.060(5) 0.046(4) 0.038(4) -0.006(3) -0.026(4) 0.004(4) C6 0.044(4) 0.064(5) 0.035(4) 0.002(4) -0.012(3) 0.003(4) C7 0.048(4) 0.062(5) 0.037(4) 0.004(3) -0.013(3) -0.013(4) C8 0.079(6) 0.074(6) 0.039(4) 0.002(4) -0.011(4) -0.037(5) C9 0.091(7) 0.081(6) 0.095(7) 0.033(5) -0.053(6) -0.051(6) C10 0.053(4) 0.056(4) 0.037(4) -0.006(3) -0.010(3) -0.026(4) C11 0.040(4) 0.041(4) 0.038(4) 0.001(3) -0.009(3) -0.021(3) C12 0.040(4) 0.046(4) 0.047(4) 0.001(3) -0.019(3) -0.013(3) C13 0.044(4) 0.053(4) 0.044(4) 0.009(3) -0.020(3) -0.021(4) C14 0.037(4) 0.050(4) 0.033(3) 0.005(3) -0.006(3) -0.022(3) C15 0.038(4) 0.041(4) 0.050(4) 0.010(3) -0.014(3) -0.022(3) C16 0.044(4) 0.042(4) 0.038(4) 0.006(3) -0.015(3) -0.023(3) C17 0.055(5) 0.065(5) 0.083(6) -0.011(5) -0.033(5) 0.005(4) C18 0.078(6) 0.092(7) 0.056(5) 0.007(5) -0.041(5) -0.018(5) C19 0.051(5) 0.062(5) 0.074(6) 0.005(4) -0.018(4) -0.005(4) C20 0.071(6) 0.064(5) 0.071(6) 0.006(4) -0.039(5) -0.019(5) C21 0.054(5) 0.058(5) 0.041(4) 0.005(3) -0.012(3) -0.032(4) C22 0.040(4) 0.049(4) 0.043(4) 0.002(3) -0.015(3) -0.016(3) C23 0.044(4) 0.043(4) 0.042(4) -0.005(3) -0.022(3) -0.004(3) C24 0.035(4) 0.039(4) 0.040(4) -0.005(3) -0.020(3) -0.001(3) C25 0.043(4) 0.053(4) 0.037(4) -0.003(3) -0.010(3) -0.008(4) C26 0.054(5) 0.051(4) 0.045(4) -0.010(3) -0.021(4) -0.006(4) C27 0.060(5) 0.044(4) 0.064(5) -0.009(4) -0.031(4) -0.012(4) C28 0.065(5) 0.035(4) 0.061(5) 0.001(3) -0.027(4) -0.018(4) C29 0.074(6) 0.068(5) 0.052(5) 0.012(4) -0.016(4) -0.045(5) C30 0.063(6) 0.079(6) 0.090(7) 0.007(5) 0.002(5) -0.031(5) C31 0.039(4) 0.047(4) 0.031(3) 0.000(3) -0.011(3) -0.016(3) C32 0.043(4) 0.040(4) 0.048(4) -0.002(3) -0.023(3) -0.005(3) C33 0.038(4) 0.039(4) 0.047(4) 0.001(3) -0.026(3) -0.005(3) C34 0.043(4) 0.054(4) 0.037(4) -0.001(3) -0.016(3) -0.007(4) C35 0.057(5) 0.052(4) 0.050(4) -0.007(4) -0.031(4) -0.009(4) C36 0.091(7) 0.054(5) 0.057(5) -0.010(4) -0.040(5) -0.012(5) C37 0.077(6) 0.044(4) 0.056(5) 0.001(4) -0.031(4) -0.022(4) C38 0.064(5) 0.054(5) 0.058(5) 0.000(4) -0.017(4) -0.033(4) C39 0.073(7) 0.064(6) 0.119(9) 0.021(6) -0.022(6) -0.025(5) C40 0.049(4) 0.057(4) 0.035(4) 0.004(3) -0.008(3) -0.024(4) C41 0.037(4) 0.045(4) 0.041(4) 0.007(3) -0.012(3) -0.020(3) C42 0.040(4) 0.052(4) 0.040(4) 0.013(3) -0.018(3) -0.021(3) C43 0.033(4) 0.045(4) 0.049(4) 0.000(3) -0.009(3) -0.013(3) C44 0.049(4) 0.044(4) 0.037(4) -0.002(3) -0.011(3) -0.022(4) C45 0.041(4) 0.050(4) 0.047(4) 0.010(3) -0.020(3) -0.029(4) C46 0.033(4) 0.046(4) 0.044(4) 0.006(3) -0.010(3) -0.016(3) C47 0.046(4) 0.094(6) 0.061(5) 0.017(5) -0.033(4) -0.022(5) C48 0.051(5) 0.064(5) 0.065(5) 0.004(4) -0.017(4) -0.008(4) C49 0.059(5) 0.070(5) 0.064(5) 0.018(4) -0.035(4) -0.025(4) C50 0.047(5) 0.068(5) 0.070(6) -0.002(4) -0.010(4) 0.002(4) C51 0.053(4) 0.065(5) 0.042(4) 0.000(4) -0.014(3) -0.029(4) C52 0.042(4) 0.053(4) 0.036(4) 0.001(3) -0.012(3) -0.014(3) C53 0.044(4) 0.057(4) 0.040(4) -0.001(3) -0.014(3) -0.009(4) C54 0.038(4) 0.052(4) 0.031(4) -0.002(3) -0.014(3) 0.002(3) C55 0.052(4) 0.053(4) 0.039(4) -0.007(3) -0.015(3) -0.001(4) C56 0.076(6) 0.061(5) 0.031(4) -0.006(4) -0.019(4) 0.010(5) C57 0.057(5) 0.068(5) 0.038(4) -0.003(4) -0.001(4) 0.007(5) C58 0.058(5) 0.084(6) 0.044(5) 0.009(4) -0.007(4) -0.018(5) C59 0.162(9) 0.096(7) 0.079(6) -0.002(5) -0.029(6) -0.026(7) C60 0.133(9) 0.174(9) 0.143(9) 0.015(7) -0.058(7) -0.044(7) O1 0.129(10) 0.104(10) 0.133(11) 0.003(7) -0.055(8) -0.069(8) S1 0.091(5) 0.107(5) 0.089(6) 0.006(4) -0.028(4) -0.039(4) C61 0.072(9) 0.074(9) 0.066(9) 0.012(7) -0.029(7) -0.023(7) C62 0.19(2) 0.19(2) 0.19(2) 0.016(10) -0.072(13) -0.067(12) O1' 0.170(16) 0.172(16) 0.179(16) -0.010(9) -0.071(10) -0.063(10) S1' 0.103(5) 0.106(5) 0.093(6) 0.020(4) -0.033(4) -0.068(4) C61' 0.139(18) 0.141(18) 0.139(18) 0.017(9) -0.048(11) -0.044(10) C62' 0.065(10) 0.074(10) 0.072(10) 0.007(7) -0.028(7) -0.030(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C1 2.097(6) . ? Hg1 C22 2.101(6) . ? Hg1 Br1 3.0764(10) . ? Hg2 C31 2.090(6) . ? Hg2 C52 2.100(6) . ? Hg2 Br2 3.0294(8) . ? Hg3 Br5 2.5699(10) . ? Hg3 Br6 2.5893(12) . ? Hg3 Br4 2.6332(10) . ? Hg3 Br3 2.6599(9) . ? N1 C1 1.340(8) . ? N1 C2 1.406(8) . ? N1 C8 1.463(9) . ? N2 C1 1.350(8) . ? N2 C3 1.404(8) . ? N2 C10 1.481(8) . ? N3 C22 1.331(8) . ? N3 C23 1.389(8) . ? N3 C29 1.465(9) . ? N4 C22 1.356(8) . ? N4 C24 1.401(8) . ? N4 C21 1.479(8) . ? N5 C31 1.352(8) . ? N5 C32 1.403(8) . ? N5 C38 1.476(9) . ? N6 C31 1.355(8) . ? N6 C33 1.411(8) . ? N6 C40 1.475(8) . ? N7 C52 1.346(9) . ? N7 C53 1.407(9) . ? N7 C59 1.539(8) . ? N8 C52 1.349(8) . ? N8 C54 1.412(8) . ? N8 C51 1.456(9) . ? C2 C3 1.367(9) . ? C2 C7 1.380(9) . ? C3 C4 1.376(9) . ? C4 C5 1.398(10) . ? C4 H4 0.9300 . ? C5 C6 1.375(11) . ? C5 H5 0.9300 . ? C6 C7 1.384(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.482(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.518(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.402(9) . ? C11 C12 1.411(9) . ? C12 C13 1.407(9) . ? C12 C17 1.504(9) . ? C13 C14 1.387(9) . ? C13 C18 1.523(9) . ? C14 C15 1.443(9) . ? C14 C21 1.491(9) . ? C15 C16 1.396(9) . ? C15 C19 1.500(10) . ? C16 C20 1.507(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 C28 1.381(9) . ? C23 C24 1.383(10) . ? C24 C25 1.366(9) . ? C25 C26 1.366(9) . ? C25 H25 0.9300 . ? C26 C27 1.402(11) . ? C26 H26 0.9300 . ? C27 C28 1.408(10) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.492(12) . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C32 C37 1.395(9) . ? C32 C33 1.397(10) . ? C33 C34 1.368(9) . ? C34 C35 1.389(9) . ? C34 H34 0.9300 . ? C35 C36 1.403(11) . ? C35 H35 0.9300 . ? C36 C37 1.395(11) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.515(11) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.504(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.395(9) . ? C41 C46 1.417(9) . ? C42 C43 1.404(9) . ? C42 C47 1.524(9) . ? C43 C44 1.427(9) . ? C43 C48 1.518(9) . ? C44 C45 1.401(9) . ? C44 C51 1.508(9) . ? C45 C46 1.388(9) . ? C45 C49 1.514(9) . ? C46 C50 1.533(9) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C53 C54 1.370(10) . ? C53 C58 1.382(10) . ? C54 C55 1.387(9) . ? C55 C56 1.394(11) . ? C55 H55 0.9300 . ? C56 C57 1.356(12) . ? C56 H56 0.9300 . ? C57 C58 1.373(11) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 C60 1.462(9) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? O1 S1 1.469(9) . ? S1 C61 1.787(9) . ? S1 C62 1.802(10) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? O1' S1' 1.471(10) . ? S1' C61' 1.794(10) . ? S1' C62' 1.798(9) . ? C61' H61D 0.9600 . ? C61' H61E 0.9600 . ? C61' H61F 0.9600 . ? C62' H62D 0.9600 . ? C62' H62E 0.9600 . ? C62' H62F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # . . ? C1 Hg1 C22 173.7(3) . . ? C1 Hg1 Br1 90.38(18) . . ? C22 Hg1 Br1 92.24(18) . . ? C31 Hg2 C52 167.8(3) . . ? C31 Hg2 Br2 93.30(18) . . ? C52 Hg2 Br2 96.37(18) . . ? Br5 Hg3 Br6 111.67(5) . . ? Br5 Hg3 Br4 110.97(4) . . ? Br6 Hg3 Br4 105.99(5) . . ? Br5 Hg3 Br3 107.32(4) . . ? Br6 Hg3 Br3 114.47(4) . . ? Br4 Hg3 Br3 106.32(3) . . ? C1 N1 C2 109.7(5) . . ? C1 N1 C8 126.8(6) . . ? C2 N1 C8 123.4(6) . . ? C1 N2 C3 109.6(5) . . ? C1 N2 C10 130.1(5) . . ? C3 N2 C10 120.3(5) . . ? C22 N3 C23 109.9(6) . . ? C22 N3 C29 127.0(6) . . ? C23 N3 C29 123.0(6) . . ? C22 N4 C24 108.8(5) . . ? C22 N4 C21 129.9(5) . . ? C24 N4 C21 121.3(5) . . ? C31 N5 C32 110.0(5) . . ? C31 N5 C38 126.1(6) . . ? C32 N5 C38 123.9(6) . . ? C31 N6 C33 110.0(6) . . ? C31 N6 C40 130.2(5) . . ? C33 N6 C40 119.8(5) . . ? C52 N7 C53 109.7(6) . . ? C52 N7 C59 126.5(7) . . ? C53 N7 C59 121.3(7) . . ? C52 N8 C54 108.6(6) . . ? C52 N8 C51 129.4(6) . . ? C54 N8 C51 121.9(5) . . ? N1 C1 N2 107.5(5) . . ? N1 C1 Hg1 121.6(5) . . ? N2 C1 Hg1 130.4(5) . . ? C3 C2 C7 121.6(6) . . ? C3 C2 N1 106.6(5) . . ? C7 C2 N1 131.8(7) . . ? C2 C3 C4 123.0(6) . . ? C2 C3 N2 106.5(5) . . ? C4 C3 N2 130.4(7) . . ? C3 C4 C5 115.8(7) . . ? C3 C4 H4 122.1 . . ? C5 C4 H4 122.1 . . ? C6 C5 C4 121.0(7) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 122.6(7) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C2 C7 C6 116.0(7) . . ? C2 C7 H7 122.0 . . ? C6 C7 H7 122.0 . . ? N1 C8 C9 111.5(7) . . ? N1 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 110.4(5) . . ? N2 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N2 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C16 C11 C12 121.6(6) . . ? C16 C11 C10 119.3(6) . . ? C12 C11 C10 118.9(6) . . ? C13 C12 C11 118.1(6) . . ? C13 C12 C17 120.6(6) . . ? C11 C12 C17 121.2(6) . . ? C14 C13 C12 120.7(6) . . ? C14 C13 C18 120.8(6) . . ? C12 C13 C18 118.4(6) . . ? C13 C14 C15 120.1(6) . . ? C13 C14 C21 120.3(6) . . ? C15 C14 C21 119.2(6) . . ? C16 C15 C14 118.7(6) . . ? C16 C15 C19 120.3(6) . . ? C14 C15 C19 121.0(6) . . ? C15 C16 C11 119.5(6) . . ? C15 C16 C20 118.0(6) . . ? C11 C16 C20 122.3(6) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 C14 111.8(5) . . ? N4 C21 H21A 109.2 . . ? C14 C21 H21A 109.2 . . ? N4 C21 H21B 109.2 . . ? C14 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N3 C22 Hg1 121.6(5) . . ? N4 C22 Hg1 130.0(5) . . ? C28 C23 C24 121.8(6) . . ? C28 C23 N3 131.5(7) . . ? C24 C23 N3 106.7(6) . . ? C25 C24 C23 122.3(6) . . ? C25 C24 N4 131.3(7) . . ? C23 C24 N4 106.3(5) . . ? C24 C25 C26 117.8(7) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? C25 C26 C27 120.7(7) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 121.7(6) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C23 C28 C27 115.6(7) . . ? C23 C28 H28 122.2 . . ? C27 C28 H28 122.2 . . ? N3 C29 C30 113.4(7) . . ? N3 C29 H29 123.3 . . ? C30 C29 H29 123.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 N6 107.5(5) . . ? N5 C31 Hg2 121.0(5) . . ? N6 C31 Hg2 131.5(5) . . ? C37 C32 C33 122.2(7) . . ? C37 C32 N5 131.2(7) . . ? C33 C32 N5 106.6(5) . . ? C34 C33 C32 122.0(6) . . ? C34 C33 N6 132.2(7) . . ? C32 C33 N6 105.8(6) . . ? C33 C34 C35 116.8(7) . . ? C33 C34 H34 121.6 . . ? C35 C34 H34 121.6 . . ? C34 C35 C36 121.7(7) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 121.6(7) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C32 C37 C36 115.7(7) . . ? C32 C37 H37 122.2 . . ? C36 C37 H37 122.2 . . ? N5 C38 C39 109.7(7) . . ? N5 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? N5 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 C41 110.7(5) . . ? N6 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C46 120.5(6) . . ? C42 C41 C40 118.8(6) . . ? C46 C41 C40 120.4(6) . . ? C41 C42 C43 119.4(6) . . ? C41 C42 C47 120.3(6) . . ? C43 C42 C47 120.2(6) . . ? C42 C43 C44 118.8(6) . . ? C42 C43 C48 121.0(6) . . ? C44 C43 C48 120.0(6) . . ? C45 C44 C43 120.2(6) . . ? C45 C44 C51 120.8(6) . . ? C43 C44 C51 118.8(6) . . ? C46 C45 C44 119.4(6) . . ? C46 C45 C49 119.2(6) . . ? C44 C45 C49 121.4(6) . . ? C45 C46 C41 119.7(6) . . ? C45 C46 C50 119.1(6) . . ? C41 C46 C50 121.2(6) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C46 C50 H50A 109.5 . . ? C46 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C46 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N8 C51 C44 111.3(5) . . ? N8 C51 H51A 109.4 . . ? C44 C51 H51A 109.4 . . ? N8 C51 H51B 109.4 . . ? C44 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? N7 C52 N8 108.2(6) . . ? N7 C52 Hg2 122.5(5) . . ? N8 C52 Hg2 129.3(5) . . ? C54 C53 C58 121.5(7) . . ? C54 C53 N7 106.1(6) . . ? C58 C53 N7 132.4(8) . . ? C53 C54 C55 121.8(7) . . ? C53 C54 N8 107.4(6) . . ? C55 C54 N8 130.7(7) . . ? C54 C55 C56 115.7(8) . . ? C54 C55 H55 122.1 . . ? C56 C55 H55 122.1 . . ? C57 C56 C55 122.2(7) . . ? C57 C56 H56 118.9 . . ? C55 C56 H56 118.9 . . ? C56 C57 C58 121.9(8) . . ? C56 C57 H57 119.1 . . ? C58 C57 H57 119.1 . . ? C57 C58 C53 116.9(8) . . ? C57 C58 H58 121.5 . . ? C53 C58 H58 121.5 . . ? C60 C59 N7 97.6(9) . . ? C60 C59 H59A 112.2 . . ? N7 C59 H59A 112.2 . . ? C60 C59 H59B 112.2 . . ? N7 C59 H59B 112.2 . . ? H59A C59 H59B 109.8 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O1 S1 C61 106.3(8) . . ? O1 S1 C62 105.3(9) . . ? C61 S1 C62 97.7(10) . . ? O1' S1' C61' 105.7(9) . . ? O1' S1' C62' 105.3(9) . . ? C61' S1' C62' 97.5(10) . . ? S1' C61' H61D 109.5 . . ? S1' C61' H61E 109.5 . . ? H61D C61' H61E 109.5 . . ? S1' C61' H61F 109.5 . . ? H61D C61' H61F 109.5 . . ? H61E C61' H61F 109.5 . . ? S1' C62' H62D 109.5 . . ? S1' C62' H62E 109.5 . . ? H62D C62' H62E 109.5 . . ? S1' C62' H62F 109.5 . . ? H62D C62' H62F 109.5 . . ? H62E C62' H62F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 1.1(7) . . . . ? C8 N1 C1 N2 177.7(6) . . . . ? C2 N1 C1 Hg1 173.8(4) . . . . ? C8 N1 C1 Hg1 -9.6(10) . . . . ? C3 N2 C1 N1 0.4(7) . . . . ? C10 N2 C1 N1 -176.8(6) . . . . ? C3 N2 C1 Hg1 -171.5(5) . . . . ? C10 N2 C1 Hg1 11.4(10) . . . . ? C22 Hg1 C1 N1 35(3) . . . . ? Br1 Hg1 C1 N1 -79.8(5) . . . . ? C22 Hg1 C1 N2 -154(2) . . . . ? Br1 Hg1 C1 N2 91.1(6) . . . . ? C1 N1 C2 C3 -2.1(7) . . . . ? C8 N1 C2 C3 -178.9(6) . . . . ? C1 N1 C2 C7 178.1(7) . . . . ? C8 N1 C2 C7 1.4(11) . . . . ? C7 C2 C3 C4 -0.9(10) . . . . ? N1 C2 C3 C4 179.3(6) . . . . ? C7 C2 C3 N2 -178.0(6) . . . . ? N1 C2 C3 N2 2.3(7) . . . . ? C1 N2 C3 C2 -1.7(7) . . . . ? C10 N2 C3 C2 175.8(6) . . . . ? C1 N2 C3 C4 -178.5(6) . . . . ? C10 N2 C3 C4 -1.0(10) . . . . ? C2 C3 C4 C5 1.9(9) . . . . ? N2 C3 C4 C5 178.2(6) . . . . ? C3 C4 C5 C6 -2.0(10) . . . . ? C4 C5 C6 C7 1.2(11) . . . . ? C3 C2 C7 C6 -0.1(10) . . . . ? N1 C2 C7 C6 179.7(7) . . . . ? C5 C6 C7 C2 -0.1(10) . . . . ? C1 N1 C8 C9 100.0(9) . . . . ? C2 N1 C8 C9 -83.8(8) . . . . ? C1 N2 C10 C11 -5.1(10) . . . . ? C3 N2 C10 C11 178.0(5) . . . . ? N2 C10 C11 C16 85.1(7) . . . . ? N2 C10 C11 C12 -89.1(7) . . . . ? C16 C11 C12 C13 -9.8(10) . . . . ? C10 C11 C12 C13 164.3(6) . . . . ? C16 C11 C12 C17 172.8(7) . . . . ? C10 C11 C12 C17 -13.1(10) . . . . ? C11 C12 C13 C14 -0.3(10) . . . . ? C17 C12 C13 C14 177.2(7) . . . . ? C11 C12 C13 C18 -177.4(7) . . . . ? C17 C12 C13 C18 0.0(11) . . . . ? C12 C13 C14 C15 9.6(10) . . . . ? C18 C13 C14 C15 -173.3(7) . . . . ? C12 C13 C14 C21 -162.5(6) . . . . ? C18 C13 C14 C21 14.6(10) . . . . ? C13 C14 C15 C16 -9.1(9) . . . . ? C21 C14 C15 C16 163.1(6) . . . . ? C13 C14 C15 C19 173.4(6) . . . . ? C21 C14 C15 C19 -14.4(9) . . . . ? C14 C15 C16 C11 -0.7(9) . . . . ? C19 C15 C16 C11 176.9(6) . . . . ? C14 C15 C16 C20 -175.8(6) . . . . ? C19 C15 C16 C20 1.7(9) . . . . ? C12 C11 C16 C15 10.2(9) . . . . ? C10 C11 C16 C15 -163.8(6) . . . . ? C12 C11 C16 C20 -174.9(7) . . . . ? C10 C11 C16 C20 11.1(9) . . . . ? C22 N4 C21 C14 4.7(10) . . . . ? C24 N4 C21 C14 -178.0(5) . . . . ? C13 C14 C21 N4 86.6(8) . . . . ? C15 C14 C21 N4 -85.6(7) . . . . ? C23 N3 C22 N4 1.1(8) . . . . ? C29 N3 C22 N4 178.9(7) . . . . ? C23 N3 C22 Hg1 -175.0(4) . . . . ? C29 N3 C22 Hg1 2.9(10) . . . . ? C24 N4 C22 N3 0.0(7) . . . . ? C21 N4 C22 N3 177.6(6) . . . . ? C24 N4 C22 Hg1 175.7(5) . . . . ? C21 N4 C22 Hg1 -6.8(10) . . . . ? C1 Hg1 C22 N3 -35(3) . . . . ? Br1 Hg1 C22 N3 79.2(5) . . . . ? C1 Hg1 C22 N4 150(2) . . . . ? Br1 Hg1 C22 N4 -95.9(6) . . . . ? C22 N3 C23 C28 -179.8(7) . . . . ? C29 N3 C23 C28 2.2(12) . . . . ? C22 N3 C23 C24 -1.7(8) . . . . ? C29 N3 C23 C24 -179.7(6) . . . . ? C28 C23 C24 C25 0.2(10) . . . . ? N3 C23 C24 C25 -178.1(6) . . . . ? C28 C23 C24 N4 180.0(6) . . . . ? N3 C23 C24 N4 1.7(7) . . . . ? C22 N4 C24 C25 178.6(7) . . . . ? C21 N4 C24 C25 0.9(10) . . . . ? C22 N4 C24 C23 -1.1(7) . . . . ? C21 N4 C24 C23 -178.9(6) . . . . ? C23 C24 C25 C26 -0.8(10) . . . . ? N4 C24 C25 C26 179.5(6) . . . . ? C24 C25 C26 C27 0.7(10) . . . . ? C25 C26 C27 C28 0.0(11) . . . . ? C24 C23 C28 C27 0.4(10) . . . . ? N3 C23 C28 C27 178.2(7) . . . . ? C26 C27 C28 C23 -0.5(11) . . . . ? C22 N3 C29 C30 -101.4(9) . . . . ? C23 N3 C29 C30 76.2(9) . . . . ? C32 N5 C31 N6 0.4(7) . . . . ? C38 N5 C31 N6 178.4(6) . . . . ? C32 N5 C31 Hg2 179.3(4) . . . . ? C38 N5 C31 Hg2 -2.7(9) . . . . ? C33 N6 C31 N5 -0.7(7) . . . . ? C40 N6 C31 N5 178.5(6) . . . . ? C33 N6 C31 Hg2 -179.5(5) . . . . ? C40 N6 C31 Hg2 -0.3(11) . . . . ? C52 Hg2 C31 N5 -67.4(14) . . . . ? Br2 Hg2 C31 N5 75.1(5) . . . . ? C52 Hg2 C31 N6 111.2(13) . . . . ? Br2 Hg2 C31 N6 -106.3(6) . . . . ? C31 N5 C32 C37 179.0(7) . . . . ? C38 N5 C32 C37 0.9(12) . . . . ? C31 N5 C32 C33 0.1(7) . . . . ? C38 N5 C32 C33 -178.0(6) . . . . ? C37 C32 C33 C34 -0.3(10) . . . . ? N5 C32 C33 C34 178.7(6) . . . . ? C37 C32 C33 N6 -179.5(6) . . . . ? N5 C32 C33 N6 -0.5(7) . . . . ? C31 N6 C33 C34 -178.4(7) . . . . ? C40 N6 C33 C34 2.3(10) . . . . ? C31 N6 C33 C32 0.8(7) . . . . ? C40 N6 C33 C32 -178.5(6) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? N6 C33 C34 C35 178.4(6) . . . . ? C33 C34 C35 C36 1.9(10) . . . . ? C34 C35 C36 C37 -2.3(12) . . . . ? C33 C32 C37 C36 0.0(11) . . . . ? N5 C32 C37 C36 -178.8(7) . . . . ? C35 C36 C37 C32 1.3(12) . . . . ? C31 N5 C38 C39 103.1(8) . . . . ? C32 N5 C38 C39 -79.2(9) . . . . ? C31 N6 C40 C41 1.0(10) . . . . ? C33 N6 C40 C41 -179.9(5) . . . . ? N6 C40 C41 C42 -87.5(7) . . . . ? N6 C40 C41 C46 85.9(7) . . . . ? C46 C41 C42 C43 -11.0(10) . . . . ? C40 C41 C42 C43 162.5(6) . . . . ? C46 C41 C42 C47 172.6(6) . . . . ? C40 C41 C42 C47 -13.9(9) . . . . ? C41 C42 C43 C44 -0.1(10) . . . . ? C47 C42 C43 C44 176.2(6) . . . . ? C41 C42 C43 C48 -175.9(6) . . . . ? C47 C42 C43 C48 0.5(10) . . . . ? C42 C43 C44 C45 12.0(10) . . . . ? C48 C43 C44 C45 -172.2(6) . . . . ? C42 C43 C44 C51 -163.2(6) . . . . ? C48 C43 C44 C51 12.5(10) . . . . ? C43 C44 C45 C46 -12.6(9) . . . . ? C51 C44 C45 C46 162.5(6) . . . . ? C43 C44 C45 C49 170.4(6) . . . . ? C51 C44 C45 C49 -14.4(10) . . . . ? C44 C45 C46 C41 1.5(10) . . . . ? C49 C45 C46 C41 178.5(6) . . . . ? C44 C45 C46 C50 -177.4(6) . . . . ? C49 C45 C46 C50 -0.4(10) . . . . ? C42 C41 C46 C45 10.4(10) . . . . ? C40 C41 C46 C45 -162.9(6) . . . . ? C42 C41 C46 C50 -170.7(7) . . . . ? C40 C41 C46 C50 15.9(10) . . . . ? C52 N8 C51 C44 16.1(10) . . . . ? C54 N8 C51 C44 -167.7(6) . . . . ? C45 C44 C51 N8 -103.9(7) . . . . ? C43 C44 C51 N8 71.3(8) . . . . ? C53 N7 C52 N8 -0.6(8) . . . . ? C59 N7 C52 N8 161.7(8) . . . . ? C53 N7 C52 Hg2 178.8(5) . . . . ? C59 N7 C52 Hg2 -19.0(11) . . . . ? C54 N8 C52 N7 0.2(8) . . . . ? C51 N8 C52 N7 176.8(7) . . . . ? C54 N8 C52 Hg2 -179.1(5) . . . . ? C51 N8 C52 Hg2 -2.5(10) . . . . ? C31 Hg2 C52 N7 57.5(15) . . . . ? Br2 Hg2 C52 N7 -84.8(6) . . . . ? C31 Hg2 C52 N8 -123.3(12) . . . . ? Br2 Hg2 C52 N8 94.4(6) . . . . ? C52 N7 C53 C54 0.7(8) . . . . ? C59 N7 C53 C54 -162.6(7) . . . . ? C52 N7 C53 C58 179.6(8) . . . . ? C59 N7 C53 C58 16.3(13) . . . . ? C58 C53 C54 C55 1.3(11) . . . . ? N7 C53 C54 C55 -179.7(6) . . . . ? C58 C53 C54 N8 -179.6(7) . . . . ? N7 C53 C54 N8 -0.6(7) . . . . ? C52 N8 C54 C53 0.3(7) . . . . ? C51 N8 C54 C53 -176.7(6) . . . . ? C52 N8 C54 C55 179.2(7) . . . . ? C51 N8 C54 C55 2.3(11) . . . . ? C53 C54 C55 C56 -0.5(10) . . . . ? N8 C54 C55 C56 -179.4(7) . . . . ? C54 C55 C56 C57 -0.3(11) . . . . ? C55 C56 C57 C58 0.4(13) . . . . ? C56 C57 C58 C53 0.3(12) . . . . ? C54 C53 C58 C57 -1.2(12) . . . . ? N7 C53 C58 C57 -179.9(8) . . . . ? C52 N7 C59 C60 96.4(11) . . . . ? C53 N7 C59 C60 -103.3(10) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.486 659.3 185.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.912 _refine_diff_density_min -1.889 _refine_diff_density_rms 0.127 data_2d _database_code_depnum_ccdc_archive 'CCDC 757350' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Hg3 I4 N6' _chemical_formula_weight 1696.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2129(8) _cell_length_b 13.3117(8) _cell_length_c 16.6923(10) _cell_angle_alpha 71.1610(10) _cell_angle_beta 75.7010(10) _cell_angle_gamma 62.9880(10) _cell_volume 2271.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5491 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.34 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 12.862 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.047 _exptl_absorpt_correction_T_max 0.076 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 11724 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7972 _reflns_number_gt 6636 _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^)+(0.0569P)^2^+3.2148P] 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 8015 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.76219(4) 0.39716(3) 0.75117(2) 0.05042(12) Uani 1 1 d . . . Hg2 Hg 1.00046(3) 0.57607(3) 0.64115(2) 0.03815(10) Uani 1 1 d . . . Hg3 Hg 0.76388(3) 0.71955(3) 0.76925(2) 0.04415(11) Uani 1 1 d . . . I1 I 0.83667(6) 0.43105(7) 0.57696(4) 0.05876(18) Uani 1 1 d . . . I2 I 0.91758(6) 0.43118(6) 0.83416(4) 0.05147(16) Uani 1 1 d . . . I3 I 0.53628(7) 0.57991(7) 0.76572(6) 0.0749(2) Uani 1 1 d . . . I4 I 0.76989(9) 0.18475(7) 0.82567(6) 0.0861(3) Uani 1 1 d . . . N1 N 0.6379(7) 0.7386(6) 0.9546(4) 0.0432(17) Uani 1 1 d . . . N2 N 0.7602(7) 0.8298(6) 0.9038(4) 0.0459(17) Uani 1 1 d . . . N3 N 1.2812(6) 0.4921(6) 0.6366(5) 0.0396(16) Uani 1 1 d . . . N4 N 1.2395(6) 0.3554(6) 0.6248(5) 0.0423(17) Uani 1 1 d . . . N5 N 0.7671(10) 0.8894(8) 0.5316(6) 0.082(3) Uani 1 1 d . . . N6 N 0.5042(13) 0.9221(12) 0.7175(10) 0.115(5) Uani 1 1 d . . . C1 C 0.2278(14) 0.7523(15) 0.9483(10) 0.114(6) Uani 1 1 d . . . H1A H 0.1984 0.8238 0.9647 0.172 Uiso 1 1 calc R . . H1B H 0.1736 0.7139 0.9768 0.172 Uiso 1 1 calc R . . H1C H 0.2296 0.7684 0.8877 0.172 Uiso 1 1 calc R . . C2 C 0.3586(10) 0.6736(10) 0.9731(7) 0.065(3) Uani 1 1 d . . . H2A H 0.3545 0.6417 1.0344 0.079 Uiso 1 1 calc R . . H2B H 0.3956 0.6093 0.9459 0.079 Uiso 1 1 calc R . . C3 C 0.4386(9) 0.7427(9) 0.9457(6) 0.053(2) Uani 1 1 d . . . H3A H 0.4374 0.7788 0.8851 0.064 Uiso 1 1 calc R . . H3B H 0.4033 0.8042 0.9756 0.064 Uiso 1 1 calc R . . C4 C 0.5697(9) 0.6688(8) 0.9635(6) 0.053(2) Uani 1 1 d . . . H4A H 0.5706 0.6198 1.0210 0.064 Uiso 1 1 calc R . . H4B H 0.6107 0.6185 0.9244 0.064 Uiso 1 1 calc R . . C5 C 0.6279(9) 0.7932(8) 1.0152(6) 0.049(2) Uani 1 1 d . . . C6 C 0.5585(9) 0.7962(9) 1.0941(6) 0.059(3) Uani 1 1 d . . . H6 H 0.5081 0.7557 1.1160 0.071 Uiso 1 1 calc R . . C7 C 0.5677(12) 0.8628(11) 1.1392(6) 0.073(3) Uani 1 1 d . . . H7 H 0.5224 0.8671 1.1926 0.088 Uiso 1 1 calc R . . C8 C 0.6423(11) 0.9225(10) 1.1066(7) 0.070(3) Uani 1 1 d . . . H8 H 0.6459 0.9661 1.1389 0.084 Uiso 1 1 calc R . . C9 C 0.7118(10) 0.9200(9) 1.0282(6) 0.058(3) Uani 1 1 d . . . H9 H 0.7618 0.9609 1.0065 0.069 Uiso 1 1 calc R . . C10 C 0.7033(9) 0.8529(7) 0.9832(5) 0.045(2) Uani 1 1 d . . . C11 C 0.7180(9) 0.7617(8) 0.8866(6) 0.049(2) Uani 1 1 d . . . C12 C 0.8517(10) 0.8739(9) 0.8514(6) 0.061(3) Uani 1 1 d . . . H12A H 0.8916 0.8859 0.8889 0.073 Uiso 1 1 calc R . . H12B H 0.8082 0.9492 0.8149 0.073 Uiso 1 1 calc R . . C13 C 0.9509(8) 0.7980(7) 0.7961(5) 0.0396(19) Uani 1 1 d . . . C14 C 0.9702(8) 0.8440(7) 0.7092(5) 0.0404(19) Uani 1 1 d . . . C15 C 1.0724(8) 0.7792(7) 0.6578(5) 0.0384(18) Uani 1 1 d . . . C16 C 1.1537(7) 0.6680(7) 0.6974(6) 0.0408(19) Uani 1 1 d . . . C17 C 1.1336(8) 0.6204(7) 0.7858(5) 0.042(2) Uani 1 1 d . . . C18 C 1.0330(9) 0.6850(8) 0.8339(5) 0.046(2) Uani 1 1 d . . . C19 C 0.8851(10) 0.9673(8) 0.6686(6) 0.067(3) Uani 1 1 d . . . H19A H 0.8032 0.9852 0.6986 0.101 Uiso 1 1 calc R . . H19B H 0.8829 0.9736 0.6101 0.101 Uiso 1 1 calc R . . H19C H 0.9155 1.0209 0.6717 0.101 Uiso 1 1 calc R . . C20 C 1.0904(10) 0.8286(9) 0.5644(6) 0.061(3) Uani 1 1 d . . . H20A H 1.1308 0.8798 0.5534 0.091 Uiso 1 1 calc R . . H20B H 1.0114 0.8712 0.5431 0.091 Uiso 1 1 calc R . . H20C H 1.1406 0.7666 0.5365 0.091 Uiso 1 1 calc R . . C21 C 1.2238(10) 0.5002(8) 0.8264(7) 0.064(3) Uani 1 1 d . . . H21A H 1.3067 0.4954 0.8098 0.095 Uiso 1 1 d R . . H21B H 1.2160 0.4428 0.8078 0.095 Uiso 1 1 d R . . H21C H 1.2058 0.4862 0.8873 0.095 Uiso 1 1 d R . . C22 C 1.0134(11) 0.6348(10) 0.9288(6) 0.066(3) Uani 1 1 d . . . H22A H 0.9664 0.5893 0.9396 0.099 Uiso 1 1 calc R . . H22B H 0.9691 0.6968 0.9573 0.099 Uiso 1 1 calc R . . H22C H 1.0922 0.5863 0.9498 0.099 Uiso 1 1 calc R . . C23 C 1.2712(8) 0.6016(8) 0.6459(7) 0.051(2) Uani 1 1 d . . . H23A H 1.2770 0.6516 0.5895 0.062 Uiso 1 1 calc R . . H23B H 1.3415 0.5852 0.6727 0.062 Uiso 1 1 calc R . . C24 C 1.3946(8) 0.4008(8) 0.6229(5) 0.043(2) Uani 1 1 d . . . C25 C 1.5157(8) 0.3877(9) 0.6159(7) 0.056(2) Uani 1 1 d . . . H25 H 1.5342 0.4462 0.6201 0.067 Uiso 1 1 calc R . . C26 C 1.6071(9) 0.2831(10) 0.6025(8) 0.065(3) Uani 1 1 d . . . H26 H 1.6895 0.2703 0.5986 0.078 Uiso 1 1 calc R . . C27 C 1.5797(9) 0.1961(10) 0.5946(7) 0.068(3) Uani 1 1 d . . . H27 H 1.6439 0.1270 0.5850 0.082 Uiso 1 1 calc R . . C28 C 1.4601(9) 0.2108(9) 0.6006(6) 0.057(2) Uani 1 1 d . . . H28 H 1.4418 0.1526 0.5956 0.069 Uiso 1 1 calc R . . C29 C 1.3672(8) 0.3145(8) 0.6144(5) 0.044(2) Uani 1 1 d . . . C30 C 1.1874(7) 0.4644(7) 0.6371(5) 0.0369(18) Uani 1 1 d . . . C31 C 1.1738(9) 0.2883(9) 0.6228(7) 0.053(2) Uani 1 1 d . . . H31A H 1.2073 0.2573 0.5726 0.064 Uiso 1 1 calc R . . H31B H 1.0871 0.3395 0.6182 0.064 Uiso 1 1 calc R . . C32 C 1.1836(9) 0.1891(8) 0.7012(6) 0.053(2) Uani 1 1 d . . . H32A H 1.2702 0.1395 0.7071 0.064 Uiso 1 1 calc R . . H32B H 1.1469 0.2203 0.7513 0.064 Uiso 1 1 calc R . . C33 C 1.1196(11) 0.1173(10) 0.6970(9) 0.078(3) Uani 1 1 d . . . H33A H 1.0323 0.1664 0.6938 0.093 Uiso 1 1 calc R . . H33B H 1.1534 0.0898 0.6453 0.093 Uiso 1 1 calc R . . C34 C 1.1334(13) 0.0146(12) 0.7721(11) 0.113(6) Uani 1 1 d . . . H34A H 1.2192 -0.0378 0.7730 0.169 Uiso 1 1 calc R . . H34B H 1.0869 -0.0248 0.7675 0.169 Uiso 1 1 calc R . . H34C H 1.1029 0.0408 0.8238 0.169 Uiso 1 1 calc R . . C35 C 0.8134(7) 0.6965(7) 0.6452(5) 0.041(2) Uani 1 1 d . . . H35 H 0.7644 0.6595 0.6378 0.049 Uiso 1 1 calc R . . C36 C 0.7898(9) 0.8007(9) 0.5823(6) 0.051(2) Uani 1 1 d . . . C37 C 0.4735(15) 0.9033(14) 0.6669(10) 0.097(5) Uani 1 1 d . . . C38 C 0.4308(19) 0.8769(16) 0.6085(13) 0.168(10) Uani 1 1 d . . . H38A H 0.4661 0.7942 0.6157 0.253 Uiso 1 1 calc R . . H38B H 0.4550 0.9132 0.5514 0.253 Uiso 1 1 calc R . . H38C H 0.3422 0.9054 0.6186 0.253 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 0.0634(2) 0.0461(2) 0.0446(2) -0.01329(16) -0.00109(17) -0.02599(18) Hg2 0.03622(18) 0.03379(18) 0.03936(18) -0.00889(14) -0.01109(13) -0.00674(14) Hg3 0.0535(2) 0.0416(2) 0.03517(18) -0.01468(15) -0.00622(15) -0.01361(16) I1 0.0647(4) 0.0768(5) 0.0399(3) -0.0133(3) -0.0070(3) -0.0334(4) I2 0.0690(4) 0.0526(4) 0.0397(3) -0.0048(3) -0.0129(3) -0.0318(3) I3 0.0614(4) 0.0779(5) 0.0873(6) -0.0446(5) -0.0118(4) -0.0122(4) I4 0.1087(7) 0.0557(5) 0.0934(6) -0.0270(4) 0.0256(5) -0.0462(5) N1 0.052(4) 0.044(4) 0.034(4) -0.016(3) -0.002(3) -0.017(4) N2 0.066(5) 0.038(4) 0.033(4) -0.011(3) -0.001(3) -0.022(4) N3 0.035(4) 0.030(4) 0.048(4) -0.008(3) -0.009(3) -0.007(3) N4 0.033(4) 0.038(4) 0.048(4) -0.003(3) -0.012(3) -0.010(3) N5 0.101(8) 0.054(6) 0.064(6) -0.015(5) -0.033(6) 0.003(5) N6 0.100(10) 0.076(9) 0.116(12) 0.000(8) -0.014(9) -0.005(7) C1 0.116(12) 0.161(16) 0.102(11) 0.011(10) -0.032(9) -0.104(12) C2 0.077(7) 0.069(7) 0.061(7) -0.015(6) 0.001(5) -0.043(6) C3 0.064(6) 0.056(6) 0.042(5) -0.009(4) -0.002(4) -0.030(5) C4 0.059(6) 0.046(6) 0.049(5) -0.019(4) -0.001(4) -0.015(5) C5 0.058(6) 0.047(6) 0.040(5) -0.016(4) -0.006(4) -0.016(5) C6 0.059(6) 0.067(7) 0.038(5) -0.014(5) 0.007(4) -0.019(5) C7 0.095(9) 0.082(8) 0.033(5) -0.016(5) -0.006(5) -0.028(7) C8 0.098(9) 0.068(7) 0.044(6) -0.028(5) -0.003(6) -0.027(7) C9 0.079(7) 0.053(6) 0.044(5) -0.019(5) -0.003(5) -0.027(5) C10 0.061(6) 0.029(5) 0.038(5) -0.008(4) -0.006(4) -0.012(4) C11 0.056(6) 0.049(6) 0.037(5) -0.019(4) -0.007(4) -0.012(5) C12 0.098(8) 0.047(6) 0.046(5) -0.020(5) 0.015(5) -0.044(6) C13 0.066(6) 0.028(4) 0.031(4) -0.008(3) -0.006(4) -0.022(4) C14 0.061(5) 0.024(4) 0.033(4) -0.002(3) -0.010(4) -0.016(4) C15 0.051(5) 0.026(4) 0.032(4) -0.005(3) -0.008(4) -0.009(4) C16 0.038(4) 0.040(5) 0.048(5) -0.009(4) -0.011(4) -0.017(4) C17 0.058(5) 0.035(5) 0.045(5) 0.001(4) -0.021(4) -0.028(4) C18 0.069(6) 0.060(6) 0.024(4) 0.002(4) -0.013(4) -0.043(5) C19 0.081(8) 0.040(6) 0.043(5) -0.003(4) -0.017(5) 0.008(5) C20 0.073(7) 0.050(6) 0.036(5) 0.003(4) 0.001(5) -0.019(5) C21 0.074(7) 0.042(6) 0.070(7) 0.015(5) -0.042(6) -0.022(5) C22 0.095(8) 0.081(8) 0.029(5) 0.013(5) -0.022(5) -0.053(7) C23 0.044(5) 0.044(5) 0.067(6) -0.014(5) -0.004(4) -0.019(4) C24 0.042(5) 0.049(5) 0.040(5) -0.013(4) -0.006(4) -0.019(4) C25 0.039(5) 0.054(6) 0.071(7) -0.020(5) -0.014(5) -0.011(4) C26 0.038(5) 0.068(7) 0.088(8) -0.032(6) -0.018(5) -0.008(5) C27 0.041(6) 0.065(7) 0.083(8) -0.032(6) -0.014(5) 0.004(5) C28 0.059(6) 0.048(6) 0.059(6) -0.019(5) -0.007(5) -0.013(5) C29 0.039(5) 0.045(5) 0.041(5) -0.011(4) -0.008(4) -0.009(4) C30 0.034(4) 0.030(4) 0.039(4) -0.004(3) -0.010(3) -0.007(4) C31 0.048(5) 0.055(6) 0.065(6) -0.019(5) -0.018(5) -0.019(5) C32 0.056(6) 0.043(5) 0.059(6) -0.019(5) 0.002(5) -0.018(5) C33 0.074(8) 0.055(7) 0.100(9) 0.002(6) -0.018(7) -0.033(6) C34 0.079(9) 0.078(10) 0.167(16) 0.014(10) -0.029(9) -0.042(8) C35 0.037(4) 0.040(5) 0.043(5) -0.021(4) -0.018(4) -0.001(4) C36 0.055(6) 0.045(6) 0.042(5) -0.014(5) -0.011(4) -0.007(5) C37 0.091(11) 0.074(10) 0.067(9) 0.001(8) -0.018(8) 0.007(8) C38 0.19(2) 0.109(15) 0.134(17) -0.047(13) -0.087(16) 0.041(14) _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 I4 2.6637(8) . ? Hg1 I3 2.7464(8) . ? Hg1 I1 2.7760(7) . ? Hg1 I2 2.8653(7) . ? Hg2 C30 2.082(8) . ? Hg2 C35 2.112(8) . ? Hg2 Hg3 3.3380(5) . ? Hg3 C11 2.084(8) . ? Hg3 C35 2.090(8) . ? N1 C11 1.357(12) . ? N1 C5 1.379(11) . ? N1 C4 1.459(12) . ? N2 C11 1.354(12) . ? N2 C10 1.396(11) . ? N2 C12 1.463(12) . ? N3 C30 1.351(10) . ? N3 C24 1.393(11) . ? N3 C23 1.463(11) . ? N4 C30 1.356(11) . ? N4 C29 1.385(10) . ? N4 C31 1.458(11) . ? N5 C36 1.167(13) . ? N6 C37 1.14(2) . ? C1 C2 1.532(18) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.527(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.496(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.381(13) . ? C5 C10 1.384(13) . ? C6 C7 1.387(15) . ? C6 H6 0.9300 . ? C7 C8 1.375(16) . ? C7 H7 0.9300 . ? C8 C9 1.374(14) . ? C8 H8 0.9300 . ? C9 C10 1.389(13) . ? C9 H9 0.9300 . ? C12 C13 1.511(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.387(11) . ? C13 C18 1.412(12) . ? C14 C15 1.417(12) . ? C14 C19 1.520(12) . ? C15 C16 1.404(11) . ? C15 C20 1.487(12) . ? C16 C17 1.414(12) . ? C16 C23 1.520(12) . ? C17 C18 1.375(13) . ? C17 C21 1.517(12) . ? C18 C22 1.514(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.387(12) . ? C24 C29 1.388(12) . ? C25 C26 1.378(14) . ? C25 H25 0.9300 . ? C26 C27 1.394(15) . ? C26 H26 0.9300 . ? C27 C28 1.365(14) . ? C27 H27 0.9300 . ? C28 C29 1.378(13) . ? C28 H28 0.9300 . ? C31 C32 1.513(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.509(14) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.502(18) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.398(13) . ? C35 H35 0.9800 . ? C37 C38 1.41(2) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I4 Hg1 I3 116.60(3) . . ? I4 Hg1 I1 113.15(3) . . ? I3 Hg1 I1 104.36(3) . . ? I4 Hg1 I2 107.26(3) . . ? I3 Hg1 I2 104.53(2) . . ? I1 Hg1 I2 110.59(2) . . ? C30 Hg2 C35 176.9(3) . . ? C30 Hg2 Hg3 141.9(2) . . ? C35 Hg2 Hg3 37.2(2) . . ? C11 Hg3 C35 172.8(4) . . ? C11 Hg3 Hg2 143.0(3) . . ? C35 Hg3 Hg2 37.6(2) . . ? C11 N1 C5 109.6(8) . . ? C11 N1 C4 126.3(7) . . ? C5 N1 C4 124.1(8) . . ? C11 N2 C10 109.3(7) . . ? C11 N2 C12 128.0(7) . . ? C10 N2 C12 122.7(7) . . ? C30 N3 C24 110.2(7) . . ? C30 N3 C23 127.1(7) . . ? C24 N3 C23 122.7(7) . . ? C30 N4 C29 110.0(7) . . ? C30 N4 C31 126.4(7) . . ? C29 N4 C31 123.6(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 110.2(10) . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 112.7(9) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N1 C4 C3 112.0(8) . . ? N1 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N1 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C6 131.2(9) . . ? N1 C5 C10 107.2(8) . . ? C6 C5 C10 121.6(9) . . ? C5 C6 C7 116.6(10) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? C8 C7 C6 121.5(10) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 122.4(10) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C8 C9 C10 116.2(10) . . ? C8 C9 H9 121.9 . . ? C10 C9 H9 121.9 . . ? C5 C10 C9 121.7(9) . . ? C5 C10 N2 106.4(8) . . ? C9 C10 N2 131.9(9) . . ? N2 C11 N1 107.5(7) . . ? N2 C11 Hg3 122.5(7) . . ? N1 C11 Hg3 129.8(7) . . ? N2 C12 C13 116.1(7) . . ? N2 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? N2 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C14 C13 C18 119.9(8) . . ? C14 C13 C12 119.7(8) . . ? C18 C13 C12 120.0(8) . . ? C13 C14 C15 120.6(8) . . ? C13 C14 C19 120.1(8) . . ? C15 C14 C19 119.1(7) . . ? C16 C15 C14 118.2(7) . . ? C16 C15 C20 121.7(8) . . ? C14 C15 C20 120.1(7) . . ? C15 C16 C17 121.3(8) . . ? C15 C16 C23 119.4(8) . . ? C17 C16 C23 119.1(8) . . ? C18 C17 C16 119.2(8) . . ? C18 C17 C21 121.1(8) . . ? C16 C17 C21 119.8(9) . . ? C17 C18 C13 120.8(7) . . ? C17 C18 C22 119.0(9) . . ? C13 C18 C22 120.2(9) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.4 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 C16 115.8(7) . . ? N3 C23 H23A 108.3 . . ? C16 C23 H23A 108.3 . . ? N3 C23 H23B 108.3 . . ? C16 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C29 121.8(8) . . ? C25 C24 N3 132.1(8) . . ? C29 C24 N3 106.1(7) . . ? C26 C25 C24 116.3(9) . . ? C26 C25 H25 121.8 . . ? C24 C25 H25 121.8 . . ? C25 C26 C27 122.0(9) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C28 C27 C26 121.0(9) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 117.9(10) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? C28 C29 N4 132.2(9) . . ? C28 C29 C24 121.0(8) . . ? N4 C29 C24 106.8(7) . . ? N3 C30 N4 106.9(7) . . ? N3 C30 Hg2 125.9(6) . . ? N4 C30 Hg2 126.8(6) . . ? N4 C31 C32 112.6(7) . . ? N4 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N4 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C31 112.2(9) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 113.3(11) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 Hg3 113.5(6) . . ? C36 C35 Hg2 114.7(7) . . ? Hg3 C35 Hg2 105.2(3) . . ? C36 C35 H35 107.7 . . ? Hg3 C35 H35 107.7 . . ? Hg2 C35 H35 107.7 . . ? N5 C36 C35 177.9(11) . . ? N6 C37 C38 176(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 Hg2 Hg3 C11 7.1(6) . . . . ? C35 Hg2 Hg3 C11 -168.2(6) . . . . ? C30 Hg2 Hg3 C35 175.2(5) . . . . ? C1 C2 C3 C4 -176.5(10) . . . . ? C11 N1 C4 C3 -100.5(10) . . . . ? C5 N1 C4 C3 78.3(11) . . . . ? C2 C3 C4 N1 -167.5(8) . . . . ? C11 N1 C5 C6 179.7(10) . . . . ? C4 N1 C5 C6 0.7(16) . . . . ? C11 N1 C5 C10 0.6(10) . . . . ? C4 N1 C5 C10 -178.4(8) . . . . ? N1 C5 C6 C7 -178.5(10) . . . . ? C10 C5 C6 C7 0.4(15) . . . . ? C5 C6 C7 C8 0.0(17) . . . . ? C6 C7 C8 C9 0.0(19) . . . . ? C7 C8 C9 C10 -0.3(17) . . . . ? N1 C5 C10 C9 178.4(9) . . . . ? C6 C5 C10 C9 -0.8(15) . . . . ? N1 C5 C10 N2 -1.6(10) . . . . ? C6 C5 C10 N2 179.3(9) . . . . ? C8 C9 C10 C5 0.7(15) . . . . ? C8 C9 C10 N2 -179.4(10) . . . . ? C11 N2 C10 C5 2.0(10) . . . . ? C12 N2 C10 C5 -177.2(9) . . . . ? C11 N2 C10 C9 -177.9(10) . . . . ? C12 N2 C10 C9 2.9(16) . . . . ? C10 N2 C11 N1 -1.6(10) . . . . ? C12 N2 C11 N1 177.5(9) . . . . ? C10 N2 C11 Hg3 173.5(6) . . . . ? C12 N2 C11 Hg3 -7.3(13) . . . . ? C5 N1 C11 N2 0.6(10) . . . . ? C4 N1 C11 N2 179.6(8) . . . . ? C5 N1 C11 Hg3 -174.0(7) . . . . ? C4 N1 C11 Hg3 4.9(14) . . . . ? C35 Hg3 C11 N2 -25(3) . . . . ? Hg2 Hg3 C11 N2 65.3(9) . . . . ? C35 Hg3 C11 N1 149(2) . . . . ? Hg2 Hg3 C11 N1 -120.7(7) . . . . ? C11 N2 C12 C13 -30.7(15) . . . . ? C10 N2 C12 C13 148.4(8) . . . . ? N2 C12 C13 C14 125.7(9) . . . . ? N2 C12 C13 C18 -61.6(12) . . . . ? C18 C13 C14 C15 -0.6(13) . . . . ? C12 C13 C14 C15 172.1(8) . . . . ? C18 C13 C14 C19 -177.6(9) . . . . ? C12 C13 C14 C19 -4.9(13) . . . . ? C13 C14 C15 C16 -0.5(12) . . . . ? C19 C14 C15 C16 176.5(9) . . . . ? C13 C14 C15 C20 178.7(9) . . . . ? C19 C14 C15 C20 -4.3(13) . . . . ? C14 C15 C16 C17 1.1(12) . . . . ? C20 C15 C16 C17 -178.0(8) . . . . ? C14 C15 C16 C23 -173.6(8) . . . . ? C20 C15 C16 C23 7.3(13) . . . . ? C15 C16 C17 C18 -0.7(12) . . . . ? C23 C16 C17 C18 174.1(7) . . . . ? C15 C16 C17 C21 -179.7(8) . . . . ? C23 C16 C17 C21 -4.9(12) . . . . ? C16 C17 C18 C13 -0.5(12) . . . . ? C21 C17 C18 C13 178.5(8) . . . . ? C16 C17 C18 C22 -178.7(8) . . . . ? C21 C17 C18 C22 0.3(12) . . . . ? C14 C13 C18 C17 1.1(12) . . . . ? C12 C13 C18 C17 -171.6(8) . . . . ? C14 C13 C18 C22 179.3(8) . . . . ? C12 C13 C18 C22 6.7(12) . . . . ? C30 N3 C23 C16 28.2(13) . . . . ? C24 N3 C23 C16 -153.9(8) . . . . ? C15 C16 C23 N3 -117.5(9) . . . . ? C17 C16 C23 N3 67.6(11) . . . . ? C30 N3 C24 C25 179.0(10) . . . . ? C23 N3 C24 C25 0.8(15) . . . . ? C30 N3 C24 C29 0.2(9) . . . . ? C23 N3 C24 C29 -178.0(8) . . . . ? C29 C24 C25 C26 -1.7(14) . . . . ? N3 C24 C25 C26 179.7(10) . . . . ? C24 C25 C26 C27 1.3(17) . . . . ? C25 C26 C27 C28 -0.6(18) . . . . ? C26 C27 C28 C29 0.3(16) . . . . ? C27 C28 C29 N4 -178.8(10) . . . . ? C27 C28 C29 C24 -0.8(15) . . . . ? C30 N4 C29 C28 179.8(10) . . . . ? C31 N4 C29 C28 0.0(15) . . . . ? C30 N4 C29 C24 1.6(10) . . . . ? C31 N4 C29 C24 -178.2(8) . . . . ? C25 C24 C29 C28 1.5(14) . . . . ? N3 C24 C29 C28 -179.6(8) . . . . ? C25 C24 C29 N4 180.0(8) . . . . ? N3 C24 C29 N4 -1.1(9) . . . . ? C24 N3 C30 N4 0.7(9) . . . . ? C23 N3 C30 N4 178.9(8) . . . . ? C24 N3 C30 Hg2 -172.6(6) . . . . ? C23 N3 C30 Hg2 5.5(12) . . . . ? C29 N4 C30 N3 -1.5(9) . . . . ? C31 N4 C30 N3 178.4(8) . . . . ? C29 N4 C30 Hg2 171.8(6) . . . . ? C31 N4 C30 Hg2 -8.4(12) . . . . ? C35 Hg2 C30 N3 1(6) . . . . ? Hg3 Hg2 C30 N3 -68.5(8) . . . . ? C35 Hg2 C30 N4 -171(6) . . . . ? Hg3 Hg2 C30 N4 119.4(6) . . . . ? C30 N4 C31 C32 -108.0(10) . . . . ? C29 N4 C31 C32 71.9(11) . . . . ? N4 C31 C32 C33 -177.7(9) . . . . ? C31 C32 C33 C34 177.1(11) . . . . ? C11 Hg3 C35 C36 -26(3) . . . . ? Hg2 Hg3 C35 C36 -126.2(9) . . . . ? C11 Hg3 C35 Hg2 100(3) . . . . ? C30 Hg2 C35 C36 52(6) . . . . ? Hg3 Hg2 C35 C36 125.4(8) . . . . ? C30 Hg2 C35 Hg3 -74(6) . . . . ? Hg3 C35 C36 N5 -28(32) . . . . ? Hg2 C35 C36 N5 -149(31) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.686 _refine_diff_density_min -2.135 _refine_diff_density_rms 0.183 data_2e(2) _database_code_depnum_ccdc_archive 'CCDC 757351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Ag2 N6' _chemical_formula_weight 702.43 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' Ag Ag -0.8971 1.1015 '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 10.9505(6) _cell_length_b 14.8255(7) _cell_length_c 19.4605(9) _cell_angle_alpha 98.1050(10) _cell_angle_beta 95.9220(10) _cell_angle_gamma 107.0280(10) _cell_volume 2955.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4518 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 23.27 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398.0 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.763 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 15297 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10444 _reflns_number_gt 6554 _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^)+(0.0911P)^2^+2.0297P] 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 10382 _refine_ls_number_parameters 690 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.037 _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 0.76019(5) 0.99796(3) 0.09961(3) 0.07945(19) Uani 1 1 d . . . Ag2 Ag 0.90056(6) 1.01068(4) 0.26863(3) 0.0845(2) Uani 1 1 d . . . Ag3 Ag -0.06140(6) 0.50148(4) 0.24826(3) 0.0876(2) Uani 1 1 d . . . Ag4 Ag 0.22736(6) 0.64773(4) 0.32159(4) 0.0981(2) Uani 1 1 d . . . N1 N 0.4819(7) 1.0081(5) 0.0893(3) 0.0838(16) Uani 1 1 d . . . N2 N 0.4788(5) 0.8642(4) 0.0913(3) 0.0750(14) Uani 1 1 d . . . N3 N 1.0924(5) 0.8914(4) 0.2625(3) 0.0691(13) Uani 1 1 d . . . N4 N 1.1931(5) 1.0415(4) 0.2804(3) 0.0734(14) Uani 1 1 d . . . N5 N 1.1709(7) 1.0859(8) 0.1098(5) 0.134(3) Uani 1 1 d . . . N6 N 0.5879(14) 1.0819(14) 0.3377(9) 0.281(10) Uani 1 1 d D . . N7 N 0.3270(7) 0.6136(5) 0.4669(4) 0.104(2) Uani 1 1 d . A . N8 N 0.2918(8) 0.7431(5) 0.4790(5) 0.126(3) Uani 1 1 d D . . N9 N -0.1052(5) 0.4262(4) 0.0894(3) 0.0752(14) Uani 1 1 d . . . N10 N -0.0496(6) 0.3266(4) 0.1439(3) 0.0771(15) Uani 1 1 d . . . N11 N 0.2053(10) 0.6255(9) 0.1164(6) 0.158(4) Uani 1 1 d . . . N12 N -0.2757(11) 0.5604(9) 0.3940(5) 0.163(4) Uani 1 1 d . . . C1 C 0.5713(10) 1.3078(7) 0.2494(5) 0.131(4) Uani 1 1 d . . . H1A H 0.4858 1.2972 0.2613 0.197 Uiso 1 1 calc R . . H1B H 0.6123 1.3753 0.2522 0.197 Uiso 1 1 calc R . . H1C H 0.6209 1.2839 0.2817 0.197 Uiso 1 1 calc R . . C2 C 0.5631(13) 1.2565(9) 0.1762(6) 0.161(5) Uani 1 1 d . . . H2A H 0.4999 1.2732 0.1460 0.193 Uiso 1 1 calc R . . H2B H 0.6460 1.2817 0.1610 0.193 Uiso 1 1 calc R . . C3 C 0.5330(15) 1.1634(8) 0.1652(5) 0.174(6) Uani 1 1 d . . . H3A H 0.4484 1.1381 0.1786 0.209 Uiso 1 1 calc R . . H3B H 0.5939 1.1467 0.1969 0.209 Uiso 1 1 calc R . . C4 C 0.5297(10) 1.1113(6) 0.0920(4) 0.108(3) Uani 1 1 d . . . H4A H 0.4740 1.1298 0.0585 0.130 Uiso 1 1 calc R . . H4B H 0.6160 1.1288 0.0794 0.130 Uiso 1 1 calc R . . C5 C 0.3550(8) 0.9549(8) 0.0876(4) 0.099(3) Uani 1 1 d . . . H5 H 0.2845 0.9777 0.0856 0.119 Uiso 1 1 calc R . . C6 C 0.3517(8) 0.8653(7) 0.0894(4) 0.100(2) Uani 1 1 d . . . H6 H 0.2791 0.8135 0.0894 0.120 Uiso 1 1 calc R . . C7 C 0.5620(7) 0.9524(5) 0.0922(3) 0.0739(17) Uani 1 1 d . . . C8 C 0.5120(7) 0.7743(5) 0.0858(4) 0.0811(19) Uani 1 1 d . . . H8A H 0.5162 0.7522 0.0370 0.097 Uiso 1 1 calc R . . H8B H 0.4437 0.7259 0.1002 0.097 Uiso 1 1 calc R . . C9 C 0.6384(6) 0.7842(4) 0.1295(3) 0.0628(15) Uani 1 1 d . . . C10 C 0.6447(6) 0.7895(4) 0.2006(3) 0.0655(15) Uani 1 1 d . . . C11 C 0.7594(6) 0.7931(4) 0.2420(3) 0.0677(16) Uani 1 1 d . . . C12 C 0.8676(6) 0.7941(4) 0.2094(3) 0.0646(15) Uani 1 1 d . . . C13 C 0.8627(6) 0.7914(4) 0.1377(4) 0.0667(16) Uani 1 1 d . . . C14 C 0.7455(7) 0.7848(4) 0.0966(3) 0.0660(16) Uani 1 1 d . . . C15 C 0.7414(8) 0.7786(6) 0.0171(4) 0.092(2) Uani 1 1 d . . . H15A H 0.7997 0.8363 0.0077 0.138 Uiso 1 1 d R . . H15B H 0.6552 0.7712 -0.0043 0.138 Uiso 1 1 d R . . H15C H 0.7665 0.7245 -0.0018 0.138 Uiso 1 1 d R . . C16 C 0.5302(7) 0.7945(6) 0.2372(4) 0.091(2) Uani 1 1 d . . . H16A H 0.4514 0.7576 0.2068 0.137 Uiso 1 1 d R . . H16B H 0.5318 0.8601 0.2482 0.137 Uiso 1 1 d R . . H16C H 0.5351 0.7690 0.2797 0.137 Uiso 1 1 d R . . C17 C 0.7617(8) 0.7960(6) 0.3213(4) 0.097(2) Uani 1 1 d . . . H17A H 0.7259 0.7322 0.3300 0.145 Uiso 1 1 calc R . . H17B H 0.7115 0.8351 0.3386 0.145 Uiso 1 1 calc R . . H17C H 0.8493 0.8226 0.3448 0.145 Uiso 1 1 calc R . . C18 C 0.9821(7) 0.7959(6) 0.1043(4) 0.092(2) Uani 1 1 d . . . H18A H 0.9594 0.7507 0.0609 0.138 Uiso 1 1 d R . . H18B H 1.0436 0.7803 0.1355 0.138 Uiso 1 1 d R . . H18C H 1.0195 0.8594 0.0952 0.138 Uiso 1 1 d R . . C19 C 0.9928(6) 0.7983(5) 0.2541(4) 0.082(2) Uani 1 1 d . . . H19A H 0.9748 0.7851 0.3000 0.099 Uiso 1 1 calc R . . H19B H 1.0252 0.7488 0.2323 0.099 Uiso 1 1 calc R . . C20 C 1.2227(7) 0.9024(5) 0.2681(4) 0.0806(19) Uani 1 1 d . . . H20 H 1.2606 0.8537 0.2651 0.097 Uiso 1 1 calc R . . C21 C 1.2834(7) 0.9961(6) 0.2788(4) 0.0808(19) Uani 1 1 d . . . H21 H 1.3723 1.0252 0.2842 0.097 Uiso 1 1 calc R . . C22 C 1.0719(6) 0.9785(4) 0.2698(3) 0.0684(16) Uani 1 1 d . . . C23 C 1.2204(8) 1.1471(5) 0.2895(4) 0.092(2) Uani 1 1 d . . . H23A H 1.2732 1.1709 0.2548 0.111 Uiso 1 1 calc R . . H23B H 1.1394 1.1606 0.2802 0.111 Uiso 1 1 calc R . . C24 C 1.2863(11) 1.1991(7) 0.3590(5) 0.128(3) Uani 1 1 d . . . H24A H 1.3676 1.1856 0.3669 0.154 Uiso 1 1 calc R . . H24B H 1.3074 1.2671 0.3576 0.154 Uiso 1 1 calc R . . C25 C 1.2253(16) 1.1831(9) 0.4178(6) 0.184(6) Uani 1 1 d . . . H25A H 1.2075 1.1158 0.4209 0.221 Uiso 1 1 calc R . . H25B H 1.1426 1.1945 0.4097 0.221 Uiso 1 1 calc R . . C26 C 1.2965(17) 1.2420(10) 0.4884(6) 0.207(7) Uani 1 1 d . . . H26A H 1.3626 1.2164 0.5050 0.310 Uiso 1 1 calc R . . H26B H 1.2367 1.2396 0.5214 0.310 Uiso 1 1 calc R . . H26C H 1.3352 1.3073 0.4833 0.310 Uiso 1 1 calc R . . C27 C 0.9475(7) 1.0530(5) 0.0992(4) 0.086(2) Uani 1 1 d D . . C28 C 1.0680(8) 1.0694(5) 0.1046(4) 0.085(2) Uani 1 1 d D . . C29 C 0.7507(10) 1.0503(6) 0.2771(6) 0.110(3) Uani 1 1 d D . . C30 C 0.6590(11) 1.0699(7) 0.3051(5) 0.116(4) Uani 1 1 d D . . C31 C -0.1109(8) 0.3485(6) 0.0394(4) 0.092(2) Uani 1 1 d . . . H31 H -0.1340 0.3416 -0.0088 0.111 Uiso 1 1 calc R . . C32 C -0.0771(8) 0.2853(5) 0.0732(4) 0.087(2) Uani 1 1 d . . . H32 H -0.0727 0.2256 0.0534 0.105 Uiso 1 1 calc R . . C33 C -0.0684(6) 0.4135(4) 0.1545(4) 0.0717(17) Uani 1 1 d . . . C34 C -0.0067(9) 0.2769(5) 0.1972(4) 0.099(2) Uani 1 1 d . . . H34A H 0.0360 0.2337 0.1757 0.119 Uiso 1 1 calc R . . H34B H -0.0815 0.2386 0.2142 0.119 Uiso 1 1 calc R . . C35 C 0.0861(8) 0.3467(4) 0.2591(4) 0.0749(18) Uani 1 1 d . . . C36 C 0.0432(7) 0.3567(5) 0.3241(4) 0.0785(19) Uani 1 1 d . . . C37 C 0.1285(8) 0.4155(5) 0.3826(4) 0.084(2) Uani 1 1 d . . . C38 C 0.2544(8) 0.4638(5) 0.3741(4) 0.082(2) Uani 1 1 d . . . C39 C 0.2966(7) 0.4572(5) 0.3085(4) 0.084(2) Uani 1 1 d . . . C40 C 0.2100(8) 0.3949(5) 0.2502(4) 0.0786(18) Uani 1 1 d . . . C41 C 0.2514(9) 0.3834(7) 0.1798(5) 0.119(3) Uani 1 1 d . . . H41A H 0.2095 0.3190 0.1552 0.178 Uiso 1 1 calc R . . H41B H 0.3434 0.3964 0.1853 0.178 Uiso 1 1 calc R . . H41C H 0.2279 0.4275 0.1534 0.178 Uiso 1 1 calc R . . C42 C -0.0948(9) 0.3082(7) 0.3347(5) 0.125(3) Uani 1 1 d . . . H42A H -0.0952 0.2621 0.3648 0.187 Uiso 1 1 calc R . . H42B H -0.1462 0.2763 0.2901 0.187 Uiso 1 1 calc R . . H42C H -0.1300 0.3555 0.3559 0.187 Uiso 1 1 calc R . . C43 C 0.0839(11) 0.4271(7) 0.4529(4) 0.125(3) Uani 1 1 d . . . H43A H 0.1574 0.4481 0.4894 0.188 Uiso 1 1 calc R . . H43B H 0.0270 0.3668 0.4590 0.188 Uiso 1 1 calc R . . H43C H 0.0388 0.4739 0.4551 0.188 Uiso 1 1 calc R . . C44 C 0.4310(8) 0.5154(7) 0.2991(6) 0.126(3) Uani 1 1 d . . . H44A H 0.4624 0.5715 0.3352 0.189 Uiso 1 1 calc R . . H44B H 0.4278 0.5342 0.2539 0.189 Uiso 1 1 calc R . . H44C H 0.4879 0.4772 0.3023 0.189 Uiso 1 1 calc R . . C45 C 0.3508(9) 0.5215(6) 0.4385(5) 0.113(3) Uani 1 1 d . . . H45A H 0.3463 0.4827 0.4749 0.135 Uiso 1 1 calc R . . H45B H 0.4373 0.5361 0.4264 0.135 Uiso 1 1 calc R . . C46 C 0.3561(11) 0.6509(8) 0.5374(5) 0.131(4) Uani 1 1 d . . . H46 H 0.3866 0.6237 0.5730 0.158 Uiso 1 1 calc R A . C47 C 0.3319(11) 0.7337(7) 0.5442(6) 0.136(4) Uani 1 1 d D A . H47 H 0.3408 0.7765 0.5856 0.163 Uiso 1 1 calc R . . C48 C 0.2860(9) 0.6699(6) 0.4297(5) 0.101(2) Uani 1 1 d D A . C49 C 0.2637(14) 0.8318(10) 0.4643(9) 0.185(5) Uiso 0.688(11) 1 d PDU A 1 C50 C 0.1245(14) 0.8235(11) 0.4771(11) 0.189(6) Uiso 0.688(11) 1 d PDU A 1 C51 C 0.093(2) 0.9138(15) 0.4629(10) 0.225(8) Uiso 0.688(11) 1 d PDU A 1 C52 C 0.084(3) 0.9747(17) 0.5319(14) 0.269(11) Uiso 0.688(11) 1 d PDU A 1 C53 C -0.3906(17) 0.5212(12) 0.1275(9) 0.222(6) Uani 1 1 d U . . H53A H -0.3873 0.4939 0.1693 0.333 Uiso 1 1 calc R . . H53B H -0.4734 0.5302 0.1172 0.333 Uiso 1 1 calc R . . H53C H -0.3240 0.5820 0.1345 0.333 Uiso 1 1 calc R . . C54 C -0.3710(15) 0.4569(11) 0.0690(9) 0.184(4) Uani 1 1 d U . . H54A H -0.3620 0.3996 0.0847 0.221 Uiso 1 1 calc R . . H54B H -0.4454 0.4379 0.0324 0.221 Uiso 1 1 calc R . . C55 C -0.2615(12) 0.5020(9) 0.0427(7) 0.155(3) Uani 1 1 d U . . H55A H -0.2642 0.5663 0.0402 0.186 Uiso 1 1 calc R . . H55B H -0.2720 0.4694 -0.0054 0.186 Uiso 1 1 calc R . . C57 C 0.1901(8) 0.6448(6) 0.2199(5) 0.087(2) Uani 1 1 d U . . C56 C -0.1289(8) 0.5126(6) 0.0744(5) 0.102(2) Uani 1 1 d U . . H56A H -0.0705 0.5393 0.0429 0.122 Uiso 1 1 calc R . . H56B H -0.1075 0.5588 0.1178 0.122 Uiso 1 1 calc R . . C58 C 0.1966(9) 0.6374(7) 0.1679(7) 0.095(2) Uani 1 1 d U . . C59 C -0.0858(10) 0.5845(7) 0.3376(5) 0.105(3) Uani 1 1 d U . . C60 C -0.1700(15) 0.5731(8) 0.3618(7) 0.130(3) Uani 1 1 d U . . C49' C 0.242(2) 0.8236(12) 0.4655(13) 0.186(7) Uiso 0.312(11) 1 d PDU A 2 C50' C 0.357(4) 0.9111(14) 0.461(2) 0.198(8) Uiso 0.312(11) 1 d PDU A 2 C51' C 0.332(5) 1.0037(13) 0.493(3) 0.226(11) Uiso 0.312(11) 1 d PDU A 2 C52' C 0.202(5) 0.978(3) 0.522(3) 0.238(12) Uiso 0.312(11) 1 d PDU A 2 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 0.0821(4) 0.0599(3) 0.0902(4) 0.0070(3) 0.0087(3) 0.0174(2) Ag2 0.0845(4) 0.0655(3) 0.1017(4) 0.0108(3) -0.0032(3) 0.0286(3) Ag3 0.1053(5) 0.0663(3) 0.0881(4) 0.0037(3) 0.0062(3) 0.0294(3) Ag4 0.1011(5) 0.0738(4) 0.1155(5) 0.0155(3) -0.0049(4) 0.0291(3) N1 0.102(5) 0.094(4) 0.066(3) 0.005(3) 0.006(3) 0.052(4) N2 0.064(3) 0.082(4) 0.076(4) 0.014(3) 0.003(3) 0.021(3) N3 0.064(3) 0.064(3) 0.079(3) 0.014(3) 0.003(3) 0.022(3) N4 0.075(4) 0.067(3) 0.070(3) 0.010(3) 0.005(3) 0.013(3) N5 0.072(5) 0.189(9) 0.152(7) 0.047(6) 0.025(5) 0.049(5) N6 0.204(18) 0.245(18) 0.32(3) -0.025(17) -0.083(15) 0.030(14) N7 0.109(5) 0.086(4) 0.097(5) -0.012(4) -0.017(4) 0.026(4) N8 0.164(8) 0.087(5) 0.116(6) -0.011(4) -0.008(5) 0.047(5) N9 0.072(3) 0.068(3) 0.083(4) 0.019(3) 0.008(3) 0.016(3) N10 0.092(4) 0.061(3) 0.074(4) 0.008(3) 0.000(3) 0.022(3) N11 0.133(8) 0.188(11) 0.143(8) 0.067(8) -0.005(7) 0.025(7) N12 0.163(9) 0.208(11) 0.127(7) 0.041(7) 0.004(6) 0.071(8) C1 0.123(8) 0.121(7) 0.133(8) -0.031(6) -0.003(6) 0.046(6) C2 0.216(13) 0.155(10) 0.127(9) -0.028(7) -0.025(8) 0.122(10) C3 0.295(17) 0.123(8) 0.109(8) -0.018(6) -0.064(9) 0.124(10) C4 0.160(8) 0.086(5) 0.092(6) 0.003(4) -0.009(5) 0.075(6) C5 0.086(6) 0.144(8) 0.083(5) 0.010(5) 0.014(4) 0.063(6) C6 0.068(5) 0.127(7) 0.108(6) 0.022(5) 0.007(4) 0.037(5) C7 0.079(4) 0.080(4) 0.064(4) 0.009(3) 0.002(3) 0.033(4) C8 0.082(5) 0.063(4) 0.087(5) 0.003(3) -0.003(4) 0.015(3) C9 0.061(4) 0.052(3) 0.071(4) 0.011(3) 0.002(3) 0.013(3) C10 0.060(4) 0.056(3) 0.076(4) 0.012(3) 0.014(3) 0.010(3) C11 0.073(4) 0.055(3) 0.071(4) 0.014(3) 0.010(3) 0.013(3) C12 0.066(4) 0.051(3) 0.077(4) 0.013(3) 0.006(3) 0.020(3) C13 0.075(4) 0.045(3) 0.080(4) 0.008(3) 0.020(3) 0.017(3) C14 0.084(5) 0.046(3) 0.064(4) 0.009(3) 0.008(3) 0.016(3) C15 0.118(6) 0.088(5) 0.077(5) 0.016(4) 0.016(4) 0.042(5) C16 0.068(4) 0.111(6) 0.096(5) 0.031(4) 0.023(4) 0.020(4) C17 0.102(6) 0.119(6) 0.077(5) 0.029(4) 0.015(4) 0.039(5) C18 0.095(5) 0.087(5) 0.098(5) 0.004(4) 0.039(4) 0.032(4) C19 0.072(4) 0.066(4) 0.112(6) 0.024(4) 0.005(4) 0.026(3) C20 0.068(4) 0.088(5) 0.089(5) 0.020(4) 0.012(4) 0.027(4) C21 0.061(4) 0.091(5) 0.084(5) 0.018(4) 0.012(3) 0.014(4) C22 0.077(4) 0.061(4) 0.061(4) 0.011(3) 0.006(3) 0.014(3) C23 0.105(6) 0.064(4) 0.092(5) 0.011(4) 0.006(4) 0.007(4) C24 0.164(10) 0.091(6) 0.114(8) 0.016(6) -0.010(7) 0.028(6) C25 0.283(18) 0.142(10) 0.100(8) 0.021(7) 0.041(10) 0.022(11) C26 0.33(2) 0.174(12) 0.097(8) -0.010(8) 0.043(10) 0.056(13) C27 0.074(5) 0.060(4) 0.110(6) 0.004(4) 0.014(4) 0.007(3) C28 0.124(7) 0.062(4) 0.075(5) 0.018(3) 0.017(5) 0.036(5) C29 0.093(6) 0.080(5) 0.147(9) 0.000(5) -0.014(6) 0.030(5) C30 0.144(12) 0.070(5) 0.090(7) 0.013(5) -0.044(7) -0.011(6) C31 0.101(6) 0.094(5) 0.079(5) 0.015(4) 0.006(4) 0.030(5) C32 0.111(6) 0.070(4) 0.070(4) -0.005(4) -0.004(4) 0.025(4) C33 0.070(4) 0.054(3) 0.083(5) 0.011(3) 0.006(3) 0.010(3) C34 0.140(7) 0.067(4) 0.084(5) 0.007(4) -0.012(5) 0.036(4) C35 0.103(6) 0.058(4) 0.067(4) 0.007(3) 0.001(4) 0.036(4) C36 0.083(5) 0.060(4) 0.089(5) 0.011(3) 0.002(4) 0.021(3) C37 0.104(6) 0.074(4) 0.080(5) 0.017(4) 0.013(4) 0.036(4) C38 0.093(5) 0.067(4) 0.085(5) 0.006(4) -0.016(4) 0.036(4) C39 0.082(5) 0.084(5) 0.097(6) 0.019(4) 0.009(4) 0.044(4) C40 0.091(5) 0.078(4) 0.078(5) 0.011(4) 0.014(4) 0.044(4) C41 0.135(8) 0.143(8) 0.103(7) 0.013(6) 0.030(6) 0.082(7) C42 0.125(8) 0.101(6) 0.130(8) 0.024(6) 0.025(6) 0.004(6) C43 0.170(10) 0.126(7) 0.072(5) 0.008(5) 0.026(6) 0.037(7) C44 0.085(6) 0.116(7) 0.177(10) 0.012(7) 0.022(6) 0.037(5) C45 0.125(7) 0.099(6) 0.102(6) -0.012(5) -0.037(5) 0.047(5) C46 0.147(9) 0.114(8) 0.094(7) -0.015(6) -0.031(6) 0.015(7) C47 0.173(11) 0.093(7) 0.115(8) -0.020(6) 0.000(7) 0.026(7) C48 0.106(6) 0.079(5) 0.111(6) 0.007(5) -0.002(5) 0.028(5) C53 0.264(10) 0.193(9) 0.207(9) 0.040(7) 0.072(8) 0.054(7) C54 0.180(7) 0.163(7) 0.217(7) 0.045(6) 0.033(6) 0.058(6) C55 0.149(6) 0.139(6) 0.190(6) 0.046(5) 0.024(5) 0.057(5) C57 0.086(4) 0.081(4) 0.092(5) 0.023(4) 0.002(4) 0.023(3) C56 0.094(5) 0.099(5) 0.127(5) 0.044(4) 0.013(4) 0.041(4) C58 0.080(4) 0.085(4) 0.113(6) 0.008(5) 0.017(5) 0.019(3) C59 0.118(6) 0.101(5) 0.108(5) 0.023(4) 0.032(4) 0.046(5) C60 0.154(7) 0.119(5) 0.124(6) 0.035(5) -0.006(5) 0.055(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 Ag1 C27 1.975(7) . ? Ag1 C7 2.058(7) . ? Ag2 C29 1.913(10) . ? Ag2 C22 2.066(7) . ? Ag3 C33 2.068(7) . ? Ag3 C59 2.072(10) . ? Ag3 Ag4 3.3041(9) . ? Ag4 C57 1.970(9) . ? Ag4 C48 2.086(9) . ? N1 C7 1.372(8) . ? N1 C5 1.377(10) . ? N1 C4 1.456(10) . ? N2 C7 1.353(8) . ? N2 C6 1.393(9) . ? N2 C8 1.473(9) . ? N3 C22 1.365(8) . ? N3 C20 1.378(8) . ? N3 C19 1.462(8) . ? N4 C21 1.350(9) . ? N4 C22 1.356(8) . ? N4 C23 1.486(9) . ? N5 C28 1.071(9) . ? N6 C30 1.092(5) . ? N7 C48 1.321(10) . ? N7 C46 1.372(11) . ? N7 C45 1.505(10) . ? N8 C48 1.324(10) . ? N8 C47 1.341(12) . ? N8 C49' 1.491(9) . ? N8 C49 1.493(8) . ? N9 C33 1.346(8) . ? N9 C31 1.380(9) . ? N9 C56 1.442(9) . ? N10 C33 1.353(8) . ? N10 C32 1.389(8) . ? N10 C34 1.469(9) . ? N11 C58 1.012(12) . ? N12 C60 1.351(16) . ? C1 C2 1.499(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.303(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.513(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.323(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.505(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.368(9) . ? C9 C14 1.392(9) . ? C10 C11 1.403(9) . ? C10 C16 1.520(9) . ? C11 C12 1.397(9) . ? C11 C17 1.536(9) . ? C12 C13 1.386(9) . ? C12 C19 1.526(9) . ? C13 C14 1.410(9) . ? C13 C18 1.508(9) . ? C14 C15 1.531(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.328(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C23 C24 1.458(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.397(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.517(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.259(5) . ? C29 C30 1.276(5) . ? C31 C32 1.332(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C34 C35 1.528(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C40 1.378(10) . ? C35 C36 1.399(10) . ? C36 C37 1.397(10) . ? C36 C42 1.520(11) . ? C37 C38 1.393(11) . ? C37 C43 1.504(11) . ? C38 C39 1.403(10) . ? C38 C45 1.521(10) . ? C39 C40 1.417(10) . ? C39 C44 1.517(11) . ? C40 C41 1.490(10) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.321(14) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C49 C50 1.543(10) . ? C50 C51 1.531(10) . ? C51 C52 1.536(10) . ? C53 C54 1.453(18) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.378(16) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.471(13) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C57 C58 1.015(11) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C59 C60 1.060(15) . ? C49' C50' 1.545(10) . ? C50' C51' 1.540(10) . ? C51' C52' 1.545(10) . ? 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 C27 Ag1 C7 173.0(3) . . ? C29 Ag2 C22 173.6(3) . . ? C33 Ag3 C59 170.9(3) . . ? C33 Ag3 Ag4 115.96(18) . . ? C59 Ag3 Ag4 72.8(3) . . ? C57 Ag4 C48 171.8(3) . . ? C57 Ag4 Ag3 66.6(2) . . ? C48 Ag4 Ag3 120.9(2) . . ? C7 N1 C5 111.4(7) . . ? C7 N1 C4 122.8(7) . . ? C5 N1 C4 125.7(7) . . ? C7 N2 C6 112.0(7) . . ? C7 N2 C8 125.7(6) . . ? C6 N2 C8 122.1(7) . . ? C22 N3 C20 110.7(5) . . ? C22 N3 C19 125.8(5) . . ? C20 N3 C19 123.4(6) . . ? C21 N4 C22 111.6(6) . . ? C21 N4 C23 125.0(6) . . ? C22 N4 C23 123.3(6) . . ? C48 N7 C46 112.6(8) . . ? C48 N7 C45 126.4(7) . . ? C46 N7 C45 120.8(8) . . ? C48 N8 C47 114.2(8) . . ? C48 N8 C49' 123.7(11) . . ? C47 N8 C49' 121.6(11) . . ? C48 N8 C49 124.0(10) . . ? C47 N8 C49 121.7(9) . . ? C49' N8 C49 9.1(12) . . ? C33 N9 C31 111.4(6) . . ? C33 N9 C56 123.6(6) . . ? C31 N9 C56 125.0(7) . . ? C33 N10 C32 111.5(6) . . ? C33 N10 C34 127.5(6) . . ? C32 N10 C34 121.0(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 118.3(12) . . ? C3 C2 H2A 107.7 . . ? C1 C2 H2A 107.7 . . ? C3 C2 H2B 107.7 . . ? C1 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? C2 C3 C4 118.6(11) . . ? C2 C3 H3A 107.7 . . ? C4 C3 H3A 107.7 . . ? C2 C3 H3B 107.7 . . ? C4 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? N1 C4 C3 109.9(8) . . ? N1 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N1 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 N1 107.6(7) . . ? C6 C5 H5 126.2 . . ? N1 C5 H5 126.2 . . ? C5 C6 N2 106.2(8) . . ? C5 C6 H6 126.9 . . ? N2 C6 H6 126.9 . . ? N2 C7 N1 102.8(6) . . ? N2 C7 Ag1 130.5(5) . . ? N1 C7 Ag1 126.8(5) . . ? N2 C8 C9 113.6(5) . . ? N2 C8 H8A 108.8 . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 121.3(6) . . ? C10 C9 C8 119.4(6) . . ? C14 C9 C8 119.3(6) . . ? C9 C10 C11 120.4(6) . . ? C9 C10 C16 121.4(6) . . ? C11 C10 C16 118.2(6) . . ? C12 C11 C10 118.7(6) . . ? C12 C11 C17 122.4(6) . . ? C10 C11 C17 118.9(6) . . ? C13 C12 C11 121.1(6) . . ? C13 C12 C19 119.9(6) . . ? C11 C12 C19 119.0(6) . . ? C12 C13 C14 119.4(6) . . ? C12 C13 C18 120.0(6) . . ? C14 C13 C18 120.6(6) . . ? C9 C14 C13 119.1(6) . . ? C9 C14 C15 122.5(6) . . ? C13 C14 C15 118.4(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C12 112.6(5) . . ? N3 C19 H19A 109.1 . . ? C12 C19 H19A 109.1 . . ? N3 C19 H19B 109.1 . . ? C12 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C21 C20 N3 106.6(7) . . ? C21 C20 H20 126.7 . . ? N3 C20 H20 126.7 . . ? C20 C21 N4 107.8(6) . . ? C20 C21 H21 126.1 . . ? N4 C21 H21 126.1 . . ? N4 C22 N3 103.3(6) . . ? N4 C22 Ag2 127.0(5) . . ? N3 C22 Ag2 129.6(5) . . ? C24 C23 N4 114.3(7) . . ? C24 C23 H23A 108.7 . . ? N4 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? N4 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C23 119.8(10) . . ? C25 C24 H24A 107.4 . . ? C23 C24 H24A 107.4 . . ? C25 C24 H24B 107.4 . . ? C23 C24 H24B 107.4 . . ? H24A C24 H24B 106.9 . . ? C24 C25 C26 117.4(13) . . ? C24 C25 H25A 108.0 . . ? C26 C25 H25A 108.0 . . ? C24 C25 H25B 108.0 . . ? C26 C25 H25B 108.0 . . ? H25A C25 H25B 107.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Ag1 165.7(6) . . ? N5 C28 C27 178.2(10) . . ? C30 C29 Ag2 158.9(10) . . ? N6 C30 C29 169.1(18) . . ? C32 C31 N9 107.3(7) . . ? C32 C31 H31 126.4 . . ? N9 C31 H31 126.4 . . ? C31 C32 N10 106.0(7) . . ? C31 C32 H32 127.0 . . ? N10 C32 H32 127.0 . . ? N9 C33 N10 103.8(6) . . ? N9 C33 Ag3 127.0(5) . . ? N10 C33 Ag3 128.9(5) . . ? N10 C34 C35 112.2(6) . . ? N10 C34 H34A 109.2 . . ? C35 C34 H34A 109.2 . . ? N10 C34 H34B 109.2 . . ? C35 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C40 C35 C36 122.0(6) . . ? C40 C35 C34 119.6(7) . . ? C36 C35 C34 118.4(7) . . ? C37 C36 C35 119.5(7) . . ? C37 C36 C42 117.3(7) . . ? C35 C36 C42 123.1(7) . . ? C38 C37 C36 118.8(7) . . ? C38 C37 C43 121.0(8) . . ? C36 C37 C43 120.2(8) . . ? C37 C38 C39 122.0(7) . . ? C37 C38 C45 119.0(8) . . ? C39 C38 C45 118.9(8) . . ? C38 C39 C40 118.4(7) . . ? C38 C39 C44 121.5(8) . . ? C40 C39 C44 120.1(8) . . ? C35 C40 C39 119.2(7) . . ? C35 C40 C41 120.3(7) . . ? C39 C40 C41 120.5(8) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C37 C43 H43A 109.5 . . ? C37 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C37 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 C45 C38 113.0(6) . . ? N7 C45 H45A 109.0 . . ? C38 C45 H45A 109.0 . . ? N7 C45 H45B 109.0 . . ? C38 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? C47 C46 N7 105.6(10) . . ? C47 C46 H46 127.2 . . ? N7 C46 H46 127.2 . . ? C46 C47 N8 105.6(9) . . ? C46 C47 H47 127.2 . . ? N8 C47 H47 127.2 . . ? N7 C48 N8 101.9(8) . . ? N7 C48 Ag4 128.6(6) . . ? N8 C48 Ag4 129.6(7) . . ? N8 C49 C50 108.3(9) . . ? C51 C50 C49 109.6(9) . . ? C50 C51 C52 110.5(10) . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C53 110.1(14) . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54B 109.6 . . ? C53 C54 H54B 109.6 . . ? H54A C54 H54B 108.2 . . ? C54 C55 C56 124.3(12) . . ? C54 C55 H55A 106.2 . . ? C56 C55 H55A 106.2 . . ? C54 C55 H55B 106.2 . . ? C56 C55 H55B 106.2 . . ? H55A C55 H55B 106.4 . . ? C58 C57 Ag4 162.0(10) . . ? N9 C56 C55 116.1(8) . . ? N9 C56 H56A 108.3 . . ? C55 C56 H56A 108.3 . . ? N9 C56 H56B 108.3 . . ? C55 C56 H56B 108.3 . . ? H56A C56 H56B 107.4 . . ? N11 C58 C57 175.6(16) . . ? C60 C59 Ag3 126.8(11) . . ? C59 C60 N12 178.5(17) . . ? N8 C49' C50' 108.9(10) . . ? C51' C50' C49' 109.4(9) . . ? C50' C51' C52' 109.5(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 Ag3 Ag4 C57 45.3(3) . . . . ? C59 Ag3 Ag4 C57 -131.9(4) . . . . ? C33 Ag3 Ag4 C48 -138.3(3) . . . . ? C59 Ag3 Ag4 C48 44.5(4) . . . . ? C1 C2 C3 C4 -177.6(10) . . . . ? C7 N1 C4 C3 -100.6(9) . . . . ? C5 N1 C4 C3 75.5(10) . . . . ? C2 C3 C4 N1 -174.4(12) . . . . ? C7 N1 C5 C6 0.0(9) . . . . ? C4 N1 C5 C6 -176.5(7) . . . . ? N1 C5 C6 N2 -0.7(9) . . . . ? C7 N2 C6 C5 1.3(9) . . . . ? C8 N2 C6 C5 -173.1(7) . . . . ? C6 N2 C7 N1 -1.2(7) . . . . ? C8 N2 C7 N1 172.9(6) . . . . ? C6 N2 C7 Ag1 176.8(5) . . . . ? C8 N2 C7 Ag1 -9.1(10) . . . . ? C5 N1 C7 N2 0.7(7) . . . . ? C4 N1 C7 N2 177.4(6) . . . . ? C5 N1 C7 Ag1 -177.4(5) . . . . ? C4 N1 C7 Ag1 -0.7(9) . . . . ? C27 Ag1 C7 N2 147(2) . . . . ? C27 Ag1 C7 N1 -36(3) . . . . ? C7 N2 C8 C9 41.6(9) . . . . ? C6 N2 C8 C9 -144.8(7) . . . . ? N2 C8 C9 C10 75.8(8) . . . . ? N2 C8 C9 C14 -106.1(7) . . . . ? C14 C9 C10 C11 -1.8(9) . . . . ? C8 C9 C10 C11 176.3(5) . . . . ? C14 C9 C10 C16 176.5(6) . . . . ? C8 C9 C10 C16 -5.5(9) . . . . ? C9 C10 C11 C12 1.9(9) . . . . ? C16 C10 C11 C12 -176.4(6) . . . . ? C9 C10 C11 C17 -178.2(6) . . . . ? C16 C10 C11 C17 3.5(9) . . . . ? C10 C11 C12 C13 -0.1(9) . . . . ? C17 C11 C12 C13 -180.0(6) . . . . ? C10 C11 C12 C19 179.9(5) . . . . ? C17 C11 C12 C19 0.0(9) . . . . ? C11 C12 C13 C14 -1.8(8) . . . . ? C19 C12 C13 C14 178.2(5) . . . . ? C11 C12 C13 C18 178.0(6) . . . . ? C19 C12 C13 C18 -2.0(8) . . . . ? C10 C9 C14 C13 -0.2(8) . . . . ? C8 C9 C14 C13 -178.3(5) . . . . ? C10 C9 C14 C15 179.8(6) . . . . ? C8 C9 C14 C15 1.7(9) . . . . ? C12 C13 C14 C9 2.0(8) . . . . ? C18 C13 C14 C9 -177.8(5) . . . . ? C12 C13 C14 C15 -178.0(5) . . . . ? C18 C13 C14 C15 2.2(8) . . . . ? C22 N3 C19 C12 36.9(9) . . . . ? C20 N3 C19 C12 -147.1(6) . . . . ? C13 C12 C19 N3 71.6(8) . . . . ? C11 C12 C19 N3 -108.3(7) . . . . ? C22 N3 C20 C21 -0.2(8) . . . . ? C19 N3 C20 C21 -176.7(6) . . . . ? N3 C20 C21 N4 0.6(8) . . . . ? C22 N4 C21 C20 -0.8(8) . . . . ? C23 N4 C21 C20 -178.5(6) . . . . ? C21 N4 C22 N3 0.7(7) . . . . ? C23 N4 C22 N3 178.4(6) . . . . ? C21 N4 C22 Ag2 179.1(5) . . . . ? C23 N4 C22 Ag2 -3.2(9) . . . . ? C20 N3 C22 N4 -0.3(7) . . . . ? C19 N3 C22 N4 176.2(6) . . . . ? C20 N3 C22 Ag2 -178.7(5) . . . . ? C19 N3 C22 Ag2 -2.2(9) . . . . ? C29 Ag2 C22 N4 -48(3) . . . . ? C29 Ag2 C22 N3 130(3) . . . . ? C21 N4 C23 C24 -68.8(10) . . . . ? C22 N4 C23 C24 113.9(9) . . . . ? N4 C23 C24 C25 -63.3(14) . . . . ? C23 C24 C25 C26 -177.8(11) . . . . ? C7 Ag1 C27 C28 -164(2) . . . . ? Ag1 C27 C28 N5 -144(30) . . . . ? C22 Ag2 C29 C30 -50(5) . . . . ? Ag2 C29 C30 N6 -3(10) . . . . ? C33 N9 C31 C32 -0.1(9) . . . . ? C56 N9 C31 C32 177.0(7) . . . . ? N9 C31 C32 N10 -0.7(9) . . . . ? C33 N10 C32 C31 1.2(9) . . . . ? C34 N10 C32 C31 -179.1(7) . . . . ? C31 N9 C33 N10 0.8(8) . . . . ? C56 N9 C33 N10 -176.3(6) . . . . ? C31 N9 C33 Ag3 -173.7(5) . . . . ? C56 N9 C33 Ag3 9.2(9) . . . . ? C32 N10 C33 N9 -1.2(8) . . . . ? C34 N10 C33 N9 179.1(7) . . . . ? C32 N10 C33 Ag3 173.1(5) . . . . ? C34 N10 C33 Ag3 -6.5(11) . . . . ? C59 Ag3 C33 N9 62(2) . . . . ? Ag4 Ag3 C33 N9 -100.8(6) . . . . ? C59 Ag3 C33 N10 -111(2) . . . . ? Ag4 Ag3 C33 N10 86.1(6) . . . . ? C33 N10 C34 C35 -32.5(11) . . . . ? C32 N10 C34 C35 147.8(7) . . . . ? N10 C34 C35 C40 -71.8(9) . . . . ? N10 C34 C35 C36 110.6(8) . . . . ? C40 C35 C36 C37 -1.5(10) . . . . ? C34 C35 C36 C37 176.1(6) . . . . ? C40 C35 C36 C42 177.0(7) . . . . ? C34 C35 C36 C42 -5.5(10) . . . . ? C35 C36 C37 C38 0.8(10) . . . . ? C42 C36 C37 C38 -177.7(7) . . . . ? C35 C36 C37 C43 180.0(7) . . . . ? C42 C36 C37 C43 1.4(11) . . . . ? C36 C37 C38 C39 1.9(10) . . . . ? C43 C37 C38 C39 -177.3(7) . . . . ? C36 C37 C38 C45 -175.1(6) . . . . ? C43 C37 C38 C45 5.7(11) . . . . ? C37 C38 C39 C40 -3.9(10) . . . . ? C45 C38 C39 C40 173.1(6) . . . . ? C37 C38 C39 C44 175.8(7) . . . . ? C45 C38 C39 C44 -7.2(10) . . . . ? C36 C35 C40 C39 -0.5(10) . . . . ? C34 C35 C40 C39 -178.1(6) . . . . ? C36 C35 C40 C41 -179.0(7) . . . . ? C34 C35 C40 C41 3.4(10) . . . . ? C38 C39 C40 C35 3.1(10) . . . . ? C44 C39 C40 C35 -176.5(7) . . . . ? C38 C39 C40 C41 -178.4(7) . . . . ? C44 C39 C40 C41 2.0(11) . . . . ? C48 N7 C45 C38 -36.1(14) . . . . ? C46 N7 C45 C38 148.5(9) . . . . ? C37 C38 C45 N7 -73.7(10) . . . . ? C39 C38 C45 N7 109.2(9) . . . . ? C48 N7 C46 C47 0.2(13) . . . . ? C45 N7 C46 C47 176.2(10) . . . . ? N7 C46 C47 N8 -0.8(13) . . . . ? C48 N8 C47 C46 1.2(14) . . . . ? C49' N8 C47 C46 173.7(14) . . . . ? C49 N8 C47 C46 -175.6(10) . . . . ? C46 N7 C48 N8 0.5(11) . . . . ? C45 N7 C48 N8 -175.2(9) . . . . ? C46 N7 C48 Ag4 -179.3(7) . . . . ? C45 N7 C48 Ag4 5.0(14) . . . . ? C47 N8 C48 N7 -1.1(12) . . . . ? C49' N8 C48 N7 -173.4(13) . . . . ? C49 N8 C48 N7 175.6(9) . . . . ? C47 N8 C48 Ag4 178.7(8) . . . . ? C49' N8 C48 Ag4 6.4(17) . . . . ? C49 N8 C48 Ag4 -4.5(15) . . . . ? C57 Ag4 C48 N7 -126(2) . . . . ? Ag3 Ag4 C48 N7 77.6(9) . . . . ? C57 Ag4 C48 N8 54(3) . . . . ? Ag3 Ag4 C48 N8 -102.1(9) . . . . ? C48 N8 C49 C50 99.5(15) . . . . ? C47 N8 C49 C50 -84.0(16) . . . . ? C49' N8 C49 C50 8(7) . . . . ? N8 C49 C50 C51 179.7(13) . . . . ? C49 C50 C51 C52 -109(2) . . . . ? C53 C54 C55 C56 79.8(18) . . . . ? C48 Ag4 C57 C58 79(4) . . . . ? Ag3 Ag4 C57 C58 -123(3) . . . . ? C33 N9 C56 C55 -117.7(10) . . . . ? C31 N9 C56 C55 65.6(11) . . . . ? C54 C55 C56 N9 50.9(17) . . . . ? Ag4 C57 C58 N11 39(20) . . . . ? C33 Ag3 C59 C60 28(3) . . . . ? Ag4 Ag3 C59 C60 -167.9(13) . . . . ? Ag3 C59 C60 N12 172(100) . . . . ? C48 N8 C49' C50' -101(2) . . . . ? C47 N8 C49' C50' 87(3) . . . . ? C49 N8 C49' C50' -6(7) . . . . ? N8 C49' C50' C51' -145(3) . . . . ? C49' C50' C51' C52' 3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.682 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.084 data_2f _database_code_depnum_ccdc_archive 'CCDC 757352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 Ag2 Br2 N6 O S' _chemical_formula_weight 1030.42 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 10.097(2) _cell_length_b 13.533(3) _cell_length_c 15.409(3) _cell_angle_alpha 104.053(3) _cell_angle_beta 97.686(3) _cell_angle_gamma 94.555(4) _cell_volume 2010.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4235 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.67 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 3.053 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.451 _exptl_absorpt_correction_T_max 0.543 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 10282 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7090 _reflns_number_gt 5335 _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^)+(0.0623P)^2^+0.2164P] 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 7035 _refine_ls_number_parameters 510 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.11331(3) 0.20561(3) 0.11554(2) 0.05426(12) Uani 1 1 d . . . Ag2 Ag 0.23956(4) 0.26920(3) 0.31958(2) 0.06348(13) Uani 1 1 d . . . Br1 Br -0.05815(5) 0.17237(4) 0.21044(3) 0.06875(16) Uani 1 1 d . . . Br2 Br 0.30368(7) 0.39414(4) 0.23784(4) 0.0872(2) Uani 1 1 d . . . N1 N 0.1868(3) 0.2716(3) -0.0542(2) 0.0513(8) Uani 1 1 d . . . N2 N 0.2871(3) 0.1412(2) -0.0385(2) 0.0422(7) Uani 1 1 d . . . N3 N 0.2817(3) 0.1006(3) 0.42208(19) 0.0440(8) Uani 1 1 d . . . N4 N 0.1365(3) 0.1961(3) 0.4757(2) 0.0501(8) Uani 1 1 d . . . N6 N 0.1349(6) 0.5229(5) -0.0683(4) 0.118(2) Uani 1 1 d . . . C2 C 0.2015(12) 0.6198(7) -0.0536(8) 0.135(4) Uani 1 1 d . . . H2 H 0.1722 0.6650 -0.0870 0.162 Uiso 1 1 calc R . . C3 C 0.3110(14) 0.6463(8) 0.0112(8) 0.151(4) Uani 1 1 d . . . H3 H 0.3498 0.7141 0.0252 0.181 Uiso 1 1 calc R . . C4 C 0.3690(11) 0.5862(8) 0.0569(6) 0.146(4) Uani 1 1 d . . . H4 H 0.4484 0.6082 0.0978 0.175 Uiso 1 1 calc R . . C5 C 0.3025(9) 0.4876(6) 0.0395(5) 0.109(2) Uani 1 1 d . . . H5 H 0.3373 0.4405 0.0688 0.131 Uiso 1 1 calc R . . C6 C 0.1854(7) 0.4604(4) -0.0212(4) 0.0772(17) Uani 1 1 d . . . C7 C 0.1057(5) 0.3558(4) -0.0386(4) 0.0711(14) Uani 1 1 d . . . H7A H 0.0612 0.3539 0.0131 0.085 Uiso 1 1 calc R . . H7B H 0.0365 0.3464 -0.0909 0.085 Uiso 1 1 calc R . . C8 C 0.2597(4) 0.2494(3) -0.1257(3) 0.0512(10) Uani 1 1 d . . . C9 C 0.2756(5) 0.2947(4) -0.1957(3) 0.0684(13) Uani 1 1 d . . . H9 H 0.2323 0.3511 -0.2028 0.082 Uiso 1 1 calc R . . C10 C 0.3592(6) 0.2514(4) -0.2542(3) 0.0724(14) Uani 1 1 d . . . H10 H 0.3719 0.2790 -0.3025 0.087 Uiso 1 1 calc R . . C11 C 0.4244(5) 0.1687(4) -0.2437(3) 0.0688(13) Uani 1 1 d . . . H11 H 0.4807 0.1428 -0.2847 0.083 Uiso 1 1 calc R . . C12 C 0.4091(5) 0.1237(4) -0.1751(3) 0.0563(11) Uani 1 1 d . . . H12 H 0.4534 0.0677 -0.1683 0.068 Uiso 1 1 calc R . . C13 C 0.3243(4) 0.1655(3) -0.1158(3) 0.0458(9) Uani 1 1 d . . . C14 C 0.2024(4) 0.2051(3) -0.0012(3) 0.0449(9) Uani 1 1 d . . . C15 C 0.3307(5) 0.0514(3) -0.0094(3) 0.0525(10) Uani 1 1 d . . . H15A H 0.4183 0.0398 -0.0265 0.063 Uiso 1 1 calc R . . H15B H 0.2682 -0.0084 -0.0421 0.063 Uiso 1 1 calc R . . C16 C 0.3398(4) 0.0600(3) 0.0908(2) 0.0416(9) Uani 1 1 d . . . C17 C 0.4418(4) 0.1267(3) 0.1513(3) 0.0484(10) Uani 1 1 d . . . C18 C 0.4569(4) 0.1309(3) 0.2438(3) 0.0452(9) Uani 1 1 d . . . C19 C 0.3704(4) 0.0641(3) 0.2747(2) 0.0435(9) Uani 1 1 d . . . C20 C 0.2689(4) -0.0036(3) 0.2129(3) 0.0440(9) Uani 1 1 d . . . C21 C 0.2518(4) -0.0040(3) 0.1211(3) 0.0449(9) Uani 1 1 d . . . C22 C 0.1350(5) -0.0733(4) 0.0583(3) 0.0703(13) Uani 1 1 d . . . H22A H 0.1526 -0.1434 0.0495 0.105 Uiso 1 1 calc R . . H22B H 0.1239 -0.0563 0.0010 0.105 Uiso 1 1 calc R . . H22C H 0.0544 -0.0641 0.0845 0.105 Uiso 1 1 calc R . . C23 C 0.5361(5) 0.1978(4) 0.1190(3) 0.0680(13) Uani 1 1 d . . . H23A H 0.5200 0.1815 0.0540 0.102 Uiso 1 1 calc R . . H23B H 0.6275 0.1895 0.1396 0.102 Uiso 1 1 calc R . . H23C H 0.5204 0.2675 0.1430 0.102 Uiso 1 1 calc R . . C24 C 0.5641(5) 0.2090(4) 0.3076(3) 0.0694(13) Uani 1 1 d . . . H24A H 0.5536 0.2116 0.3691 0.104 Uiso 1 1 calc R . . H24B H 0.5555 0.2753 0.2968 0.104 Uiso 1 1 calc R . . H24C H 0.6514 0.1898 0.2976 0.104 Uiso 1 1 calc R . . C25 C 0.1765(5) -0.0757(4) 0.2448(3) 0.0680(13) Uani 1 1 d . . . H25A H 0.0872 -0.0559 0.2392 0.102 Uiso 1 1 calc R . . H25B H 0.2083 -0.0728 0.3070 0.102 Uiso 1 1 calc R . . H25C H 0.1753 -0.1444 0.2084 0.102 Uiso 1 1 calc R . . C26 C 0.3896(4) 0.0612(4) 0.3723(3) 0.0517(10) Uani 1 1 d . . . H26A H 0.3958 -0.0091 0.3752 0.062 Uiso 1 1 calc R . . H26B H 0.4744 0.1011 0.4027 0.062 Uiso 1 1 calc R . . C27 C 0.2406(4) 0.0627(3) 0.4916(2) 0.0472(10) Uani 1 1 d . . . C28 C 0.2725(4) -0.0204(4) 0.5247(3) 0.0559(11) Uani 1 1 d . . . H28 H 0.3345 -0.0626 0.5012 0.067 Uiso 1 1 calc R . . C29 C 0.2084(5) -0.0377(4) 0.5938(3) 0.0690(13) Uani 1 1 d . . . H29 H 0.2275 -0.0929 0.6175 0.083 Uiso 1 1 calc R . . C30 C 0.1163(6) 0.0246(5) 0.6291(4) 0.0777(15) Uani 1 1 d . . . H30 H 0.0753 0.0106 0.6761 0.093 Uiso 1 1 calc R . . C31 C 0.0840(5) 0.1070(4) 0.5963(3) 0.0671(13) Uani 1 1 d . . . H31 H 0.0222 0.1490 0.6202 0.081 Uiso 1 1 calc R . . C32 C 0.1473(4) 0.1250(3) 0.5261(3) 0.0498(10) Uani 1 1 d . . . C33 C 0.2193(4) 0.1823(3) 0.4124(3) 0.0464(9) Uani 1 1 d . . . C34 C 0.0473(5) 0.2761(4) 0.4889(3) 0.0610(12) Uani 1 1 d . . . H34A H -0.0350 0.2488 0.5052 0.073 Uiso 1 1 calc R . . H34B H 0.0237 0.2938 0.4319 0.073 Uiso 1 1 calc R . . C35 C 0.1062(4) 0.3731(3) 0.5612(3) 0.0549(11) Uani 1 1 d . . . C36 C 0.2405(5) 0.4041(4) 0.5850(3) 0.0654(12) Uani 1 1 d . . . H36 H 0.3022 0.3653 0.5569 0.078 Uiso 1 1 calc R . . C37 C 0.2836(6) 0.4931(4) 0.6506(4) 0.0815(15) Uani 1 1 d . . . H37 H 0.3750 0.5140 0.6701 0.098 Uiso 1 1 calc R . . C38 C 0.1916(8) 0.5497(5) 0.6865(5) 0.103(2) Uani 1 1 d . . . H38 H 0.2179 0.6118 0.7296 0.124 Uiso 1 1 calc R . . C39 C 0.0590(7) 0.5145(5) 0.6584(6) 0.121(3) Uani 1 1 d . . . H39 H -0.0042 0.5541 0.6836 0.145 Uiso 1 1 calc R . . N5 N 0.0147(5) 0.4269(4) 0.5970(4) 0.0991(17) Uani 1 1 d . . . S1 S 0.5970(3) 0.3252(2) 0.61343(18) 0.0786(10) Uani 0.564(5) 1 d PD A 1 O1 O 0.5653(16) 0.2141(8) 0.5648(13) 0.125(9) Uani 0.564(5) 1 d PD A 1 C42 C 0.652(2) 0.3910(14) 0.5372(14) 0.087(6) Uani 0.564(5) 1 d PD A 1 H42A H 0.5772 0.3929 0.4922 0.130 Uiso 0.564(5) 1 calc PR A 1 H42B H 0.7198 0.3563 0.5082 0.130 Uiso 0.564(5) 1 calc PR A 1 H42C H 0.6885 0.4598 0.5694 0.130 Uiso 0.564(5) 1 calc PR A 1 C41 C 0.7516(16) 0.3369(18) 0.6861(11) 0.099(7) Uani 0.564(5) 1 d PD A 1 H41A H 0.7392 0.3033 0.7331 0.148 Uiso 0.564(5) 1 calc PR A 1 H41B H 0.7825 0.4082 0.7128 0.148 Uiso 0.564(5) 1 calc PR A 1 H41C H 0.8170 0.3056 0.6520 0.148 Uiso 0.564(5) 1 calc PR A 1 S1' S 0.6904(4) 0.2832(3) 0.5798(3) 0.0968(16) Uani 0.436(5) 1 d PD A 2 O1' O 0.5517(15) 0.2256(14) 0.5633(14) 0.117(10) Uani 0.436(5) 1 d PD A 2 C42' C 0.667(3) 0.4041(14) 0.558(2) 0.114(12) Uani 0.436(5) 1 d PD A 2 H42D H 0.6390 0.3949 0.4939 0.171 Uiso 0.436(5) 1 calc PR A 2 H42E H 0.7497 0.4488 0.5771 0.171 Uiso 0.436(5) 1 calc PR A 2 H42F H 0.5987 0.4338 0.5902 0.171 Uiso 0.436(5) 1 calc PR A 2 C41' C 0.734(2) 0.328(2) 0.6993(8) 0.107(12) Uani 0.436(5) 1 d PD A 2 H41D H 0.7508 0.2708 0.7245 0.161 Uiso 0.436(5) 1 calc PR A 2 H41E H 0.6613 0.3603 0.7239 0.161 Uiso 0.436(5) 1 calc PR A 2 H41F H 0.8135 0.3762 0.7140 0.161 Uiso 0.436(5) 1 calc PR A 2 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 0.0559(2) 0.0628(2) 0.04867(19) 0.01377(15) 0.01943(14) 0.01717(15) Ag2 0.0914(3) 0.0556(2) 0.0516(2) 0.01986(16) 0.01852(17) 0.02570(19) Br1 0.0563(3) 0.0982(4) 0.0567(3) 0.0230(3) 0.0202(2) 0.0103(2) Br2 0.1338(5) 0.0526(3) 0.0766(4) 0.0193(3) 0.0189(3) 0.0064(3) N1 0.052(2) 0.048(2) 0.061(2) 0.0207(17) 0.0155(16) 0.0184(16) N2 0.0529(18) 0.0394(18) 0.0377(16) 0.0114(14) 0.0117(14) 0.0133(14) N3 0.0486(18) 0.052(2) 0.0333(16) 0.0101(14) 0.0083(13) 0.0138(15) N4 0.0517(19) 0.051(2) 0.0477(19) 0.0088(16) 0.0118(15) 0.0150(16) N6 0.140(5) 0.111(5) 0.165(5) 0.090(4) 0.100(4) 0.081(4) C2 0.208(10) 0.090(6) 0.181(9) 0.096(7) 0.132(8) 0.092(7) C3 0.225(13) 0.107(7) 0.168(10) 0.068(8) 0.124(9) 0.038(8) C4 0.185(9) 0.123(8) 0.111(6) 0.015(6) 0.026(6) -0.045(7) C5 0.145(7) 0.085(5) 0.097(5) 0.032(4) 0.018(5) -0.012(4) C6 0.112(4) 0.064(3) 0.088(4) 0.042(3) 0.065(4) 0.046(3) C7 0.069(3) 0.069(3) 0.091(4) 0.031(3) 0.029(3) 0.035(3) C8 0.056(2) 0.054(3) 0.048(2) 0.017(2) 0.0147(19) 0.014(2) C9 0.081(3) 0.070(3) 0.069(3) 0.034(3) 0.021(3) 0.024(3) C10 0.092(4) 0.079(4) 0.060(3) 0.035(3) 0.025(3) 0.014(3) C11 0.090(4) 0.072(3) 0.057(3) 0.023(2) 0.036(3) 0.022(3) C12 0.071(3) 0.060(3) 0.043(2) 0.014(2) 0.021(2) 0.022(2) C13 0.056(2) 0.043(2) 0.041(2) 0.0140(17) 0.0104(17) 0.0111(18) C14 0.046(2) 0.043(2) 0.047(2) 0.0101(18) 0.0103(17) 0.0100(17) C15 0.076(3) 0.044(2) 0.045(2) 0.0164(19) 0.019(2) 0.023(2) C16 0.053(2) 0.035(2) 0.043(2) 0.0145(17) 0.0130(17) 0.0163(17) C17 0.046(2) 0.046(2) 0.061(3) 0.021(2) 0.0194(19) 0.0138(18) C18 0.048(2) 0.041(2) 0.048(2) 0.0117(18) 0.0062(17) 0.0144(17) C19 0.048(2) 0.046(2) 0.040(2) 0.0116(17) 0.0114(17) 0.0192(18) C20 0.047(2) 0.043(2) 0.048(2) 0.0165(18) 0.0164(17) 0.0108(17) C21 0.049(2) 0.045(2) 0.040(2) 0.0079(17) 0.0076(17) 0.0146(18) C22 0.073(3) 0.072(3) 0.057(3) 0.012(2) -0.004(2) -0.008(3) C23 0.060(3) 0.075(3) 0.077(3) 0.031(3) 0.020(2) 0.003(2) C24 0.062(3) 0.066(3) 0.072(3) 0.012(3) 0.000(2) -0.006(2) C25 0.077(3) 0.064(3) 0.067(3) 0.022(2) 0.024(2) -0.001(2) C26 0.056(2) 0.062(3) 0.039(2) 0.0110(19) 0.0118(18) 0.020(2) C27 0.048(2) 0.054(3) 0.036(2) 0.0084(18) 0.0012(17) 0.0073(19) C28 0.059(3) 0.060(3) 0.050(2) 0.021(2) 0.002(2) 0.010(2) C29 0.073(3) 0.079(4) 0.066(3) 0.040(3) 0.008(2) 0.007(3) C30 0.076(3) 0.106(5) 0.064(3) 0.040(3) 0.021(3) 0.009(3) C31 0.061(3) 0.085(4) 0.058(3) 0.017(3) 0.022(2) 0.009(3) C32 0.046(2) 0.063(3) 0.040(2) 0.0119(19) 0.0056(17) 0.0073(19) C33 0.047(2) 0.051(2) 0.041(2) 0.0085(18) 0.0062(17) 0.0143(18) C34 0.059(3) 0.066(3) 0.061(3) 0.013(2) 0.015(2) 0.024(2) C35 0.065(3) 0.050(3) 0.059(3) 0.020(2) 0.023(2) 0.018(2) C36 0.066(3) 0.061(3) 0.072(3) 0.016(3) 0.021(2) 0.015(2) C37 0.085(4) 0.061(3) 0.096(4) 0.014(3) 0.023(3) 0.001(3) C38 0.123(6) 0.053(3) 0.126(5) -0.001(3) 0.044(4) -0.005(3) C39 0.111(5) 0.066(4) 0.174(7) -0.018(4) 0.073(5) 0.019(4) N5 0.070(3) 0.081(3) 0.134(4) -0.012(3) 0.043(3) 0.015(2) S1 0.0751(17) 0.0775(18) 0.0792(18) 0.0054(14) 0.0268(13) 0.0065(13) O1 0.165(17) 0.064(9) 0.141(17) -0.002(9) 0.074(12) -0.016(10) C42 0.128(13) 0.062(8) 0.059(11) -0.001(7) 0.006(8) 0.005(8) C41 0.106(12) 0.101(15) 0.107(13) 0.068(12) 0.010(10) 0.004(10) S1' 0.111(3) 0.063(2) 0.111(3) -0.0064(19) 0.060(2) -0.0007(19) O1' 0.112(15) 0.120(17) 0.082(14) -0.028(12) 0.020(11) -0.053(12) C42' 0.15(2) 0.11(2) 0.055(12) -0.003(12) 0.000(12) 0.000(15) C41' 0.16(3) 0.053(12) 0.109(18) 0.025(13) 0.039(16) 0.001(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 C14 2.115(4) . ? Ag1 Br1 2.4921(6) . ? Ag1 Ag2 3.1130(7) . ? Ag2 C33 2.081(4) . ? Ag2 Br2 2.4378(7) . ? N1 C14 1.359(5) . ? N1 C8 1.391(5) . ? N1 C7 1.447(5) . ? N2 C14 1.347(5) . ? N2 C13 1.399(5) . ? N2 C15 1.474(5) . ? N3 C33 1.344(5) . ? N3 C27 1.391(5) . ? N3 C26 1.475(5) . ? N4 C33 1.356(5) . ? N4 C32 1.378(5) . ? N4 C34 1.456(5) . ? N6 C6 1.331(7) . ? N6 C2 1.378(11) . ? C2 C3 1.348(14) . ? C2 H2 0.9300 . ? C3 C4 1.321(14) . ? C3 H3 0.9300 . ? C4 C5 1.393(10) . ? C4 H4 0.9300 . ? C5 C6 1.369(9) . ? C5 H5 0.9300 . ? C6 C7 1.517(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.383(6) . ? C8 C9 1.384(6) . ? C9 C10 1.376(7) . ? C9 H9 0.9300 . ? C10 C11 1.374(7) . ? C10 H10 0.9300 . ? C11 C12 1.362(6) . ? C11 H11 0.9300 . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C15 C16 1.510(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.390(6) . ? C16 C21 1.394(6) . ? C17 C18 1.399(6) . ? C17 C23 1.514(6) . ? C18 C19 1.415(6) . ? C18 C24 1.512(6) . ? C19 C20 1.401(6) . ? C19 C26 1.501(5) . ? C20 C21 1.400(5) . ? C20 C25 1.509(6) . ? C21 C22 1.512(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.386(6) . ? C27 C32 1.386(6) . ? C28 C29 1.375(6) . ? C28 H28 0.9300 . ? C29 C30 1.381(7) . ? C29 H29 0.9300 . ? C30 C31 1.376(7) . ? C30 H30 0.9300 . ? C31 C32 1.388(6) . ? C31 H31 0.9300 . ? C34 C35 1.518(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N5 1.318(6) . ? C35 C36 1.361(6) . ? C36 C37 1.367(7) . ? C36 H36 0.9300 . ? C37 C38 1.342(8) . ? C37 H37 0.9300 . ? C38 C39 1.360(9) . ? C38 H38 0.9300 . ? C39 N5 1.325(8) . ? C39 H39 0.9300 . ? S1 O1 1.495(9) . ? S1 C42 1.756(9) . ? S1 C41 1.767(9) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? S1' O1' 1.505(9) . ? S1' C41' 1.774(10) . ? S1' C42' 1.778(10) . ? C42' H42D 0.9600 . ? C42' H42E 0.9600 . ? C42' H42F 0.9600 . ? C41' H41D 0.9600 . ? C41' H41E 0.9600 . ? C41' H41F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ag1 Br1 159.60(11) . . ? C14 Ag1 Ag2 130.38(11) . . ? Br1 Ag1 Ag2 69.76(2) . . ? C33 Ag2 Br2 166.92(11) . . ? C33 Ag2 Ag1 125.91(11) . . ? Br2 Ag2 Ag1 66.88(2) . . ? C14 N1 C8 111.6(3) . . ? C14 N1 C7 124.7(4) . . ? C8 N1 C7 123.8(4) . . ? C14 N2 C13 111.4(3) . . ? C14 N2 C15 126.8(3) . . ? C13 N2 C15 121.7(3) . . ? C33 N3 C27 111.3(3) . . ? C33 N3 C26 125.1(3) . . ? C27 N3 C26 123.4(3) . . ? C33 N4 C32 111.5(3) . . ? C33 N4 C34 124.4(4) . . ? C32 N4 C34 124.1(4) . . ? C6 N6 C2 118.5(8) . . ? C3 C2 N6 117.0(8) . . ? C3 C2 H2 121.5 . . ? N6 C2 H2 121.5 . . ? C4 C3 C2 126.9(11) . . ? C4 C3 H3 116.6 . . ? C2 C3 H3 116.6 . . ? C3 C4 C5 115.2(10) . . ? C3 C4 H4 122.4 . . ? C5 C4 H4 122.4 . . ? C6 C5 C4 119.4(8) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N6 C6 C5 122.7(7) . . ? N6 C6 C7 116.1(6) . . ? C5 C6 C7 121.2(5) . . ? N1 C7 C6 113.8(4) . . ? N1 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C13 C8 C9 121.6(4) . . ? C13 C8 N1 105.8(4) . . ? C9 C8 N1 132.6(4) . . ? C10 C9 C8 116.0(5) . . ? C10 C9 H9 122.0 . . ? C8 C9 H9 122.0 . . ? C11 C10 C9 122.3(4) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C13 116.7(4) . . ? C11 C12 H12 121.6 . . ? C13 C12 H12 121.6 . . ? C8 C13 C12 121.4(4) . . ? C8 C13 N2 106.1(3) . . ? C12 C13 N2 132.5(4) . . ? N2 C14 N1 105.2(3) . . ? N2 C14 Ag1 128.4(3) . . ? N1 C14 Ag1 126.5(3) . . ? N2 C15 C16 115.1(3) . . ? N2 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? N2 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C21 120.6(4) . . ? C17 C16 C15 119.6(4) . . ? C21 C16 C15 119.7(4) . . ? C16 C17 C18 120.3(4) . . ? C16 C17 C23 120.8(4) . . ? C18 C17 C23 118.9(4) . . ? C17 C18 C19 119.4(4) . . ? C17 C18 C24 118.3(4) . . ? C19 C18 C24 122.3(4) . . ? C20 C19 C18 119.7(3) . . ? C20 C19 C26 119.3(4) . . ? C18 C19 C26 121.0(4) . . ? C21 C20 C19 120.2(4) . . ? C21 C20 C25 119.5(4) . . ? C19 C20 C25 120.3(4) . . ? C16 C21 C20 119.7(4) . . ? C16 C21 C22 122.2(4) . . ? C20 C21 C22 118.1(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 C19 114.6(3) . . ? N3 C26 H26A 108.6 . . ? C19 C26 H26A 108.6 . . ? N3 C26 H26B 108.6 . . ? C19 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C32 121.5(4) . . ? C28 C27 N3 132.5(4) . . ? C32 C27 N3 105.9(4) . . ? C29 C28 C27 116.9(4) . . ? C29 C28 H28 121.5 . . ? C27 C28 H28 121.5 . . ? C28 C29 C30 121.9(5) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C31 C30 C29 121.3(5) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 117.4(5) . . ? C30 C31 H31 121.3 . . ? C32 C31 H31 121.3 . . ? N4 C32 C27 106.0(4) . . ? N4 C32 C31 133.1(4) . . ? C27 C32 C31 120.9(4) . . ? N3 C33 N4 105.3(3) . . ? N3 C33 Ag2 128.4(3) . . ? N4 C33 Ag2 126.3(3) . . ? N4 C34 C35 114.5(4) . . ? N4 C34 H34A 108.6 . . ? C35 C34 H34A 108.6 . . ? N4 C34 H34B 108.6 . . ? C35 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? N5 C35 C36 122.6(5) . . ? N5 C35 C34 113.7(4) . . ? C36 C35 C34 123.6(4) . . ? C35 C36 C37 119.2(5) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 118.8(6) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C38 C39 118.6(6) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? N5 C39 C38 123.7(5) . . ? N5 C39 H39 118.1 . . ? C38 C39 H39 118.1 . . ? C35 N5 C39 116.9(5) . . ? O1 S1 C42 107.9(7) . . ? O1 S1 C41 106.4(7) . . ? C42 S1 C41 98.6(6) . . ? S1 C42 H42A 109.5 . . ? S1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? S1 C41 H41A 109.5 . . ? S1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O1' S1' C41' 105.5(8) . . ? O1' S1' C42' 105.6(8) . . ? C41' S1' C42' 97.2(6) . . ? S1' C42' H42D 109.5 . . ? S1' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? S1' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? S1' C41' H41D 109.5 . . ? S1' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? S1' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Ag1 Ag2 C33 -129.45(19) . . . . ? Br1 Ag1 Ag2 C33 46.77(13) . . . . ? C14 Ag1 Ag2 Br2 47.35(14) . . . . ? Br1 Ag1 Ag2 Br2 -136.44(2) . . . . ? C6 N6 C2 C3 -3.0(11) . . . . ? N6 C2 C3 C4 6.6(16) . . . . ? C2 C3 C4 C5 -4.8(15) . . . . ? C3 C4 C5 C6 -0.4(12) . . . . ? C2 N6 C6 C5 -1.7(8) . . . . ? C2 N6 C6 C7 178.5(5) . . . . ? C4 C5 C6 N6 3.5(10) . . . . ? C4 C5 C6 C7 -176.7(6) . . . . ? C14 N1 C7 C6 118.1(5) . . . . ? C8 N1 C7 C6 -61.3(6) . . . . ? N6 C6 C7 N1 131.8(5) . . . . ? C5 C6 C7 N1 -48.1(7) . . . . ? C14 N1 C8 C13 -0.4(5) . . . . ? C7 N1 C8 C13 179.0(4) . . . . ? C14 N1 C8 C9 -179.7(5) . . . . ? C7 N1 C8 C9 -0.2(8) . . . . ? C13 C8 C9 C10 -0.1(7) . . . . ? N1 C8 C9 C10 179.1(5) . . . . ? C8 C9 C10 C11 -0.6(8) . . . . ? C9 C10 C11 C12 0.8(9) . . . . ? C10 C11 C12 C13 -0.1(8) . . . . ? C9 C8 C13 C12 0.8(7) . . . . ? N1 C8 C13 C12 -178.6(4) . . . . ? C9 C8 C13 N2 179.3(4) . . . . ? N1 C8 C13 N2 -0.1(4) . . . . ? C11 C12 C13 C8 -0.6(7) . . . . ? C11 C12 C13 N2 -178.7(5) . . . . ? C14 N2 C13 C8 0.6(5) . . . . ? C15 N2 C13 C8 176.4(4) . . . . ? C14 N2 C13 C12 178.9(5) . . . . ? C15 N2 C13 C12 -5.3(7) . . . . ? C13 N2 C14 N1 -0.8(4) . . . . ? C15 N2 C14 N1 -176.4(4) . . . . ? C13 N2 C14 Ag1 180.0(3) . . . . ? C15 N2 C14 Ag1 4.4(6) . . . . ? C8 N1 C14 N2 0.8(5) . . . . ? C7 N1 C14 N2 -178.7(4) . . . . ? C8 N1 C14 Ag1 180.0(3) . . . . ? C7 N1 C14 Ag1 0.6(6) . . . . ? Br1 Ag1 C14 N2 -97.7(4) . . . . ? Ag2 Ag1 C14 N2 72.1(4) . . . . ? Br1 Ag1 C14 N1 83.2(5) . . . . ? Ag2 Ag1 C14 N1 -107.0(3) . . . . ? C14 N2 C15 C16 -31.6(6) . . . . ? C13 N2 C15 C16 153.3(4) . . . . ? N2 C15 C16 C17 -71.0(5) . . . . ? N2 C15 C16 C21 113.5(4) . . . . ? C21 C16 C17 C18 -0.5(6) . . . . ? C15 C16 C17 C18 -176.0(3) . . . . ? C21 C16 C17 C23 -178.9(4) . . . . ? C15 C16 C17 C23 5.7(6) . . . . ? C16 C17 C18 C19 2.3(5) . . . . ? C23 C17 C18 C19 -179.3(4) . . . . ? C16 C17 C18 C24 -176.5(4) . . . . ? C23 C17 C18 C24 1.9(6) . . . . ? C17 C18 C19 C20 -1.5(5) . . . . ? C24 C18 C19 C20 177.2(4) . . . . ? C17 C18 C19 C26 175.7(4) . . . . ? C24 C18 C19 C26 -5.7(6) . . . . ? C18 C19 C20 C21 -1.0(5) . . . . ? C26 C19 C20 C21 -178.2(3) . . . . ? C18 C19 C20 C25 179.6(4) . . . . ? C26 C19 C20 C25 2.4(6) . . . . ? C17 C16 C21 C20 -2.0(5) . . . . ? C15 C16 C21 C20 173.4(3) . . . . ? C17 C16 C21 C22 176.6(4) . . . . ? C15 C16 C21 C22 -8.0(6) . . . . ? C19 C20 C21 C16 2.8(5) . . . . ? C25 C20 C21 C16 -177.8(4) . . . . ? C19 C20 C21 C22 -175.9(4) . . . . ? C25 C20 C21 C22 3.5(6) . . . . ? C33 N3 C26 C19 -39.0(6) . . . . ? C27 N3 C26 C19 147.2(4) . . . . ? C20 C19 C26 N3 -70.7(5) . . . . ? C18 C19 C26 N3 112.1(4) . . . . ? C33 N3 C27 C28 177.8(4) . . . . ? C26 N3 C27 C28 -7.7(7) . . . . ? C33 N3 C27 C32 0.1(4) . . . . ? C26 N3 C27 C32 174.7(4) . . . . ? C32 C27 C28 C29 -0.5(6) . . . . ? N3 C27 C28 C29 -177.9(4) . . . . ? C27 C28 C29 C30 -0.1(7) . . . . ? C28 C29 C30 C31 0.3(8) . . . . ? C29 C30 C31 C32 0.2(8) . . . . ? C33 N4 C32 C27 -0.8(5) . . . . ? C34 N4 C32 C27 179.3(4) . . . . ? C33 N4 C32 C31 -179.1(5) . . . . ? C34 N4 C32 C31 1.0(7) . . . . ? C28 C27 C32 N4 -177.6(4) . . . . ? N3 C27 C32 N4 0.4(4) . . . . ? C28 C27 C32 C31 1.0(6) . . . . ? N3 C27 C32 C31 179.0(4) . . . . ? C30 C31 C32 N4 177.3(5) . . . . ? C30 C31 C32 C27 -0.8(7) . . . . ? C27 N3 C33 N4 -0.6(4) . . . . ? C26 N3 C33 N4 -175.1(3) . . . . ? C27 N3 C33 Ag2 -179.5(3) . . . . ? C26 N3 C33 Ag2 6.1(6) . . . . ? C32 N4 C33 N3 0.9(4) . . . . ? C34 N4 C33 N3 -179.2(4) . . . . ? C32 N4 C33 Ag2 179.8(3) . . . . ? C34 N4 C33 Ag2 -0.3(6) . . . . ? Br2 Ag2 C33 N3 -90.1(6) . . . . ? Ag1 Ag2 C33 N3 76.7(4) . . . . ? Br2 Ag2 C33 N4 91.2(6) . . . . ? Ag1 Ag2 C33 N4 -102.0(3) . . . . ? C33 N4 C34 C35 -94.3(5) . . . . ? C32 N4 C34 C35 85.6(5) . . . . ? N4 C34 C35 N5 -155.5(5) . . . . ? N4 C34 C35 C36 26.7(7) . . . . ? N5 C35 C36 C37 2.1(8) . . . . ? C34 C35 C36 C37 179.7(5) . . . . ? C35 C36 C37 C38 -3.3(9) . . . . ? C36 C37 C38 C39 2.3(10) . . . . ? C37 C38 C39 N5 -0.1(13) . . . . ? C36 C35 N5 C39 0.1(9) . . . . ? C34 C35 N5 C39 -177.7(6) . . . . ? C38 C39 N5 C35 -1.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.586 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.083 data_2g _database_code_depnum_ccdc_archive 'CCDC 757353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H35 Ag F6 N4 O0.50 P' _chemical_formula_weight 712.46 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3684(14) _cell_length_b 13.897(2) _cell_length_c 14.595(2) _cell_angle_alpha 103.651(2) _cell_angle_beta 102.976(2) _cell_angle_gamma 104.986(2) _cell_volume 1699.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5756 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.66 _exptl_crystal_description BLOCK _exptl_crystal_colour PALE-YELLOW _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724.0 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.811 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 8589 _diffrn_reflns_av_R_equivalents 0.0121 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5984 _reflns_number_gt 5151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _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^)+(0.1038P)^2^+1.0933P] 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 5920 _refine_ls_number_parameters 431 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.124 _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 0.50531(4) 0.79252(3) 0.70270(2) 0.05613(17) Uani 1 1 d . . . P1 P 0.1748(2) 0.28176(13) 0.77221(15) 0.0833(5) Uani 1 1 d D . . F1 F 0.2124(6) 0.4051(3) 0.8049(4) 0.1228(15) Uani 1 1 d U A . F2 F 0.1347(8) 0.2852(5) 0.6597(4) 0.129(2) Uani 0.853(10) 1 d PDU A 1 F3 F -0.0060(5) 0.2593(5) 0.7520(5) 0.123(2) Uani 0.853(10) 1 d PDU A 1 F4 F 0.3444(5) 0.2959(5) 0.7707(6) 0.127(2) Uani 0.853(10) 1 d PDU A 1 F5 F 0.2050(12) 0.2834(7) 0.8801(5) 0.180(4) Uani 0.853(10) 1 d PDU A 1 F5' F 0.087(3) 0.2909(19) 0.8498(17) 0.130(13) Uani 0.147(10) 1 d PDU A 2 F4' F 0.330(2) 0.312(2) 0.8576(17) 0.118(12) Uani 0.147(10) 1 d PDU A 2 F2' F 0.269(3) 0.290(3) 0.6985(19) 0.158(17) Uani 0.147(10) 1 d PDU A 2 F3' F 0.027(3) 0.269(3) 0.6910(18) 0.167(18) Uani 0.147(10) 1 d PDU A 2 F6 F 0.1421(7) 0.1622(4) 0.7458(6) 0.171(2) Uani 1 1 d U A . N1 N 0.2640(4) 0.6664(3) 0.4898(3) 0.0571(9) Uani 1 1 d . . . N2 N 0.3026(5) 0.5676(3) 0.5798(3) 0.0620(10) Uani 1 1 d . . . N3 N 0.7457(5) 1.0094(3) 0.8480(3) 0.0591(9) Uani 1 1 d . . . N4 N 0.6894(5) 0.8970(4) 0.9238(3) 0.0646(10) Uani 1 1 d . . . C1 C 0.1708(6) 0.5647(4) 0.4325(4) 0.0629(12) Uani 1 1 d . . . C2 C 0.1950(6) 0.5021(4) 0.4898(4) 0.0646(12) Uani 1 1 d . . . C3 C 0.1165(8) 0.3944(4) 0.4562(5) 0.0828(17) Uani 1 1 d . . . H3 H 0.1310 0.3508 0.4944 0.099 Uiso 1 1 calc R . . C4 C 0.0133(8) 0.3577(5) 0.3596(6) 0.100(2) Uani 1 1 d . . . H4 H -0.0437 0.2866 0.3332 0.120 Uiso 1 1 calc R . . C5 C -0.0077(8) 0.4210(5) 0.3019(5) 0.0896(19) Uani 1 1 d . . . H5 H -0.0753 0.3911 0.2377 0.107 Uiso 1 1 calc R . . C6 C 0.0675(6) 0.5259(5) 0.3361(4) 0.0746(14) Uani 1 1 d . . . H6 H 0.0516 0.5694 0.2980 0.090 Uiso 1 1 calc R . . C7 C 0.3450(5) 0.6684(4) 0.5799(4) 0.0561(10) Uani 1 1 d . . . C8 C 0.3698(7) 0.5322(4) 0.6597(5) 0.0781(15) Uani 1 1 d . . . H8A H 0.2945 0.4697 0.6603 0.094 Uiso 1 1 calc R . . H8B H 0.3956 0.5860 0.7225 0.094 Uiso 1 1 calc R . . C9 C 0.5144(10) 0.5082(7) 0.6479(7) 0.114(3) Uani 1 1 d U . . H9A H 0.4890 0.4551 0.5857 0.171 Uiso 1 1 calc R . . H9B H 0.5556 0.4837 0.7009 0.171 Uiso 1 1 calc R . . H9C H 0.5903 0.5707 0.6497 0.171 Uiso 1 1 calc R . . C10 C 0.2643(7) 0.7562(4) 0.4513(4) 0.0734(14) Uani 1 1 d . . . H10A H 0.1651 0.7675 0.4445 0.088 Uiso 1 1 calc R . . H10B H 0.2790 0.7403 0.3864 0.088 Uiso 1 1 calc R . . C11 C 0.3921(6) 0.8541(3) 0.5204(3) 0.0569(11) Uani 1 1 d . . . C12 C 0.5431(6) 0.8647(4) 0.5205(3) 0.0585(11) Uani 1 1 d . . . C13 C 0.6664(6) 0.9397(4) 0.5989(3) 0.0584(11) Uani 1 1 d . . . C14 C 0.6338(5) 1.0024(4) 0.6758(3) 0.0565(11) Uani 1 1 d . . . C15 C 0.4823(6) 0.9999(4) 0.6705(3) 0.0583(11) Uani 1 1 d . . . C16 C 0.3604(6) 0.9250(4) 0.5917(4) 0.0608(11) Uani 1 1 d . . . C17 C 0.5759(9) 0.7906(5) 0.4407(5) 0.0892(18) Uani 1 1 d . . . H17A H 0.6229 0.7460 0.4685 0.134 Uiso 1 1 calc R . . H17B H 0.6451 0.8300 0.4131 0.134 Uiso 1 1 calc R . . H17C H 0.4805 0.7483 0.3896 0.134 Uiso 1 1 calc R . . C18 C 0.8316(7) 0.9453(7) 0.6057(5) 0.098(2) Uani 1 1 d . . . H18A H 0.8797 0.9363 0.6671 0.147 Uiso 1 1 calc R . . H18B H 0.8879 1.0123 0.6029 0.147 Uiso 1 1 calc R . . H18C H 0.8323 0.8908 0.5515 0.147 Uiso 1 1 calc R . . C19 C 0.4505(8) 1.0701(5) 0.7559(5) 0.0877(17) Uani 1 1 d . . . H19A H 0.3711 1.0969 0.7298 0.132 Uiso 1 1 calc R . . H19B H 0.5437 1.1274 0.7944 0.132 Uiso 1 1 calc R . . H19C H 0.4169 1.0301 0.7970 0.132 Uiso 1 1 calc R . . C20 C 0.1953(7) 0.9160(6) 0.5899(6) 0.0948(19) Uani 1 1 d . . . H20A H 0.1645 0.8748 0.6308 0.142 Uiso 1 1 calc R . . H20B H 0.1278 0.8828 0.5232 0.142 Uiso 1 1 calc R . . H20C H 0.1890 0.9848 0.6145 0.142 Uiso 1 1 calc R . . C21 C 0.7599(7) 1.0649(5) 0.7736(4) 0.0733(14) Uani 1 1 d . . . H21A H 0.8611 1.0741 0.7637 0.088 Uiso 1 1 calc R . . H21B H 0.7510 1.1337 0.7974 0.088 Uiso 1 1 calc R . . C22 C 0.8271(6) 1.0593(4) 0.9471(3) 0.0628(12) Uani 1 1 d . . . C23 C 0.7901(6) 0.9867(5) 0.9943(4) 0.0659(13) Uani 1 1 d . . . C24 C 0.8545(9) 1.0128(7) 1.0985(4) 0.092(2) Uani 1 1 d . . . H24 H 0.8296 0.9651 1.1324 0.110 Uiso 1 1 calc R . . C25 C 0.9568(9) 1.1139(7) 1.1463(5) 0.104(3) Uani 1 1 d . . . H25 H 1.0030 1.1337 1.2143 0.125 Uiso 1 1 calc R . . C26 C 0.9935(9) 1.1864(6) 1.0981(5) 0.095(2) Uani 1 1 d . . . H26 H 1.0618 1.2536 1.1338 0.114 Uiso 1 1 calc R . . C27 C 0.9289(7) 1.1597(5) 0.9967(4) 0.0792(15) Uani 1 1 d . . . H27 H 0.9533 1.2078 0.9631 0.095 Uiso 1 1 calc R . . C28 C 0.6610(6) 0.9106(4) 0.8341(3) 0.0595(11) Uani 1 1 d . . . C29 C 0.6113(9) 0.8010(6) 0.9424(5) 0.095(2) Uani 1 1 d . . . H29A H 0.6774 0.7945 1.0006 0.114 Uiso 1 1 calc R . . H29B H 0.5946 0.7408 0.8866 0.114 Uiso 1 1 calc R . . C30 C 0.4577(11) 0.8010(9) 0.9581(7) 0.140(3) Uani 1 1 d U . . H30A H 0.4751 0.8537 1.0191 0.210 Uiso 1 1 calc R . . H30B H 0.4035 0.7335 0.9610 0.210 Uiso 1 1 calc R . . H30C H 0.3968 0.8157 0.9042 0.210 Uiso 1 1 calc R . . O1 O 0.7426(13) 0.3839(11) 0.8796(11) 0.142(4) Uani 0.50 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 Ag1 0.0597(2) 0.0580(2) 0.0557(2) 0.03137(17) 0.01484(16) 0.01768(17) P1 0.0831(10) 0.0796(10) 0.1151(13) 0.0524(9) 0.0465(10) 0.0384(8) F1 0.165(4) 0.093(3) 0.123(3) 0.040(2) 0.051(3) 0.053(3) F2 0.122(5) 0.147(5) 0.103(4) 0.038(3) 0.030(3) 0.022(3) F3 0.087(3) 0.154(4) 0.176(6) 0.104(4) 0.057(3) 0.052(3) F4 0.075(3) 0.128(4) 0.161(6) 0.020(4) 0.035(3) 0.031(3) F5 0.229(8) 0.224(7) 0.142(5) 0.129(5) 0.059(5) 0.098(6) F5' 0.125(15) 0.137(16) 0.137(16) 0.037(9) 0.076(11) 0.032(9) F4' 0.109(14) 0.110(14) 0.129(15) 0.047(10) 0.025(9) 0.028(9) F2' 0.160(19) 0.162(19) 0.157(19) 0.048(11) 0.061(12) 0.051(11) F3' 0.16(2) 0.18(2) 0.16(2) 0.056(11) 0.049(11) 0.052(12) F6 0.129(4) 0.085(3) 0.294(7) 0.055(4) 0.053(4) 0.040(3) N1 0.055(2) 0.051(2) 0.063(2) 0.0196(17) 0.0130(18) 0.0154(17) N2 0.066(2) 0.056(2) 0.079(3) 0.034(2) 0.033(2) 0.0222(19) N3 0.058(2) 0.069(2) 0.050(2) 0.0235(18) 0.0147(17) 0.0181(19) N4 0.068(2) 0.084(3) 0.055(2) 0.035(2) 0.0195(19) 0.031(2) C1 0.058(3) 0.058(3) 0.077(3) 0.019(2) 0.028(2) 0.021(2) C2 0.064(3) 0.056(3) 0.082(3) 0.021(2) 0.035(3) 0.020(2) C3 0.088(4) 0.054(3) 0.106(5) 0.018(3) 0.044(4) 0.016(3) C4 0.094(5) 0.058(3) 0.124(6) -0.005(4) 0.044(4) 0.006(3) C5 0.082(4) 0.074(4) 0.087(4) -0.002(3) 0.017(3) 0.015(3) C6 0.066(3) 0.074(3) 0.071(3) 0.010(3) 0.014(3) 0.021(3) C7 0.055(2) 0.054(2) 0.070(3) 0.031(2) 0.025(2) 0.020(2) C8 0.091(4) 0.063(3) 0.087(4) 0.042(3) 0.028(3) 0.018(3) C9 0.119(5) 0.112(5) 0.138(6) 0.071(4) 0.027(4) 0.063(4) C10 0.075(3) 0.067(3) 0.071(3) 0.032(3) 0.000(3) 0.021(3) C11 0.067(3) 0.053(2) 0.052(2) 0.030(2) 0.008(2) 0.018(2) C12 0.075(3) 0.063(3) 0.054(2) 0.032(2) 0.028(2) 0.030(2) C13 0.064(3) 0.069(3) 0.058(3) 0.035(2) 0.029(2) 0.024(2) C14 0.065(3) 0.053(2) 0.055(2) 0.031(2) 0.019(2) 0.011(2) C15 0.074(3) 0.055(2) 0.060(3) 0.030(2) 0.026(2) 0.029(2) C16 0.063(3) 0.066(3) 0.073(3) 0.041(2) 0.024(2) 0.034(2) C17 0.112(5) 0.091(4) 0.067(3) 0.018(3) 0.038(3) 0.035(4) C18 0.069(4) 0.138(6) 0.095(4) 0.045(4) 0.039(3) 0.029(4) C19 0.104(5) 0.088(4) 0.089(4) 0.027(3) 0.043(4) 0.048(4) C20 0.065(3) 0.102(5) 0.132(6) 0.051(4) 0.028(4) 0.041(3) C21 0.076(3) 0.076(3) 0.055(3) 0.027(2) 0.015(2) 0.002(3) C22 0.061(3) 0.079(3) 0.050(2) 0.019(2) 0.016(2) 0.028(2) C23 0.065(3) 0.091(4) 0.051(3) 0.024(3) 0.018(2) 0.039(3) C24 0.104(5) 0.141(6) 0.055(3) 0.040(4) 0.027(3) 0.070(5) C25 0.108(5) 0.141(7) 0.052(3) 0.001(4) 0.004(3) 0.068(5) C26 0.097(5) 0.104(5) 0.064(4) 0.002(3) 0.009(3) 0.037(4) C27 0.078(4) 0.086(4) 0.064(3) 0.015(3) 0.015(3) 0.027(3) C28 0.061(3) 0.078(3) 0.055(3) 0.036(2) 0.023(2) 0.029(2) C29 0.108(5) 0.101(5) 0.074(4) 0.054(4) 0.014(3) 0.020(4) C30 0.133(6) 0.167(7) 0.130(6) 0.075(5) 0.067(5) 0.016(5) O1 0.090(7) 0.155(11) 0.169(12) 0.072(9) 0.031(7) 0.007(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 C7 2.106(5) . ? Ag1 C28 2.125(5) . ? P1 F5 1.529(6) . ? P1 F2' 1.541(11) . ? P1 F5' 1.543(10) . ? P1 F6 1.545(5) . ? P1 F3' 1.548(11) . ? P1 F4 1.556(5) . ? P1 F4' 1.568(10) . ? P1 F3 1.585(5) . ? P1 F1 1.586(5) . ? P1 F2 1.616(5) . ? N1 C7 1.353(6) . ? N1 C1 1.391(6) . ? N1 C10 1.483(6) . ? N2 C7 1.352(6) . ? N2 C2 1.392(7) . ? N2 C8 1.450(7) . ? N3 C28 1.338(7) . ? N3 C22 1.383(6) . ? N3 C21 1.482(6) . ? N4 C28 1.344(6) . ? N4 C23 1.361(7) . ? N4 C29 1.465(8) . ? C1 C2 1.367(7) . ? C1 C6 1.403(8) . ? C2 C3 1.393(7) . ? C3 C4 1.407(10) . ? C3 H3 0.9300 . ? C4 C5 1.373(11) . ? C4 H4 0.9300 . ? C5 C6 1.356(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.512(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.506(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.384(7) . ? C11 C16 1.396(7) . ? C12 C13 1.397(7) . ? C12 C17 1.507(7) . ? C13 C14 1.394(7) . ? C13 C18 1.509(7) . ? C14 C15 1.395(7) . ? C14 C21 1.521(7) . ? C15 C16 1.393(7) . ? C15 C19 1.528(7) . ? C16 C20 1.513(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.367(8) . ? C22 C27 1.380(8) . ? C23 C24 1.422(7) . ? C24 C25 1.386(11) . ? C24 H24 0.9300 . ? C25 C26 1.375(12) . ? C25 H25 0.9300 . ? C26 C27 1.385(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C30 1.507(11) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ag1 C28 175.31(16) . . ? F5 P1 F2' 137.3(11) . . ? F5 P1 F5' 43.5(10) . . ? F2' P1 F5' 171.9(16) . . ? F5 P1 F6 86.5(5) . . ? F2' P1 F6 91.4(15) . . ? F5' P1 F6 96.7(10) . . ? F5 P1 F3' 132.7(11) . . ? F2' P1 F3' 90.0(5) . . ? F5' P1 F3' 90.0(5) . . ? F6 P1 F3' 92.8(16) . . ? F5 P1 F4 95.7(4) . . ? F2' P1 F4 41.6(11) . . ? F5' P1 F4 137.8(10) . . ? F6 P1 F4 89.0(3) . . ? F3' P1 F4 131.6(11) . . ? F5 P1 F4' 48.5(10) . . ? F2' P1 F4' 89.4(5) . . ? F5' P1 F4' 89.5(5) . . ? F6 P1 F4' 95.2(12) . . ? F3' P1 F4' 172.0(15) . . ? F4 P1 F4' 48.4(10) . . ? F5 P1 F3 94.4(4) . . ? F2' P1 F3 128.2(11) . . ? F5' P1 F3 52.8(10) . . ? F6 P1 F3 88.0(3) . . ? F3' P1 F3 38.4(11) . . ? F4 P1 F3 169.3(4) . . ? F4' P1 F3 142.2(11) . . ? F5 P1 F1 90.8(4) . . ? F2' P1 F1 90.1(15) . . ? F5' P1 F1 81.9(9) . . ? F6 P1 F1 177.1(4) . . ? F3' P1 F1 89.7(16) . . ? F4 P1 F1 90.4(3) . . ? F4' P1 F1 82.3(12) . . ? F3 P1 F1 93.1(3) . . ? F5 P1 F2 175.8(4) . . ? F2' P1 F2 46.0(11) . . ? F5' P1 F2 132.8(11) . . ? F6 P1 F2 96.3(4) . . ? F3' P1 F2 44.2(12) . . ? F4 P1 F2 87.5(4) . . ? F4' P1 F2 134.0(11) . . ? F3 P1 F2 82.6(3) . . ? F1 P1 F2 86.5(3) . . ? C7 N1 C1 110.9(4) . . ? C7 N1 C10 128.0(4) . . ? C1 N1 C10 121.1(4) . . ? C7 N2 C2 110.8(4) . . ? C7 N2 C8 124.3(5) . . ? C2 N2 C8 124.8(4) . . ? C28 N3 C22 110.3(4) . . ? C28 N3 C21 128.7(4) . . ? C22 N3 C21 120.9(4) . . ? C28 N4 C23 110.7(4) . . ? C28 N4 C29 123.7(5) . . ? C23 N4 C29 125.5(4) . . ? C2 C1 N1 106.3(5) . . ? C2 C1 C6 122.9(5) . . ? N1 C1 C6 130.8(5) . . ? C1 C2 N2 106.5(4) . . ? C1 C2 C3 121.9(6) . . ? N2 C2 C3 131.6(6) . . ? C2 C3 C4 114.0(6) . . ? C2 C3 H3 123.0 . . ? C4 C3 H3 123.0 . . ? C5 C4 C3 123.6(6) . . ? C5 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? C6 C5 C4 121.7(7) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 115.8(6) . . ? C5 C6 H6 122.1 . . ? C1 C6 H6 122.1 . . ? N2 C7 N1 105.5(4) . . ? N2 C7 Ag1 122.7(4) . . ? N1 C7 Ag1 131.8(3) . . ? N2 C8 C9 111.0(5) . . ? N2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 110.5(4) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C16 120.8(4) . . ? C12 C11 C10 118.6(5) . . ? C16 C11 C10 120.0(5) . . ? C11 C12 C13 119.8(4) . . ? C11 C12 C17 120.4(5) . . ? C13 C12 C17 119.6(5) . . ? C14 C13 C12 118.8(4) . . ? C14 C13 C18 120.3(5) . . ? C12 C13 C18 120.6(5) . . ? C13 C14 C15 121.3(4) . . ? C13 C14 C21 120.5(5) . . ? C15 C14 C21 117.7(5) . . ? C16 C15 C14 118.9(4) . . ? C16 C15 C19 120.7(5) . . ? C14 C15 C19 120.0(5) . . ? C15 C16 C11 119.6(4) . . ? C15 C16 C20 119.2(5) . . ? C11 C16 C20 121.1(5) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C14 110.3(4) . . ? N3 C21 H21A 109.6 . . ? C14 C21 H21A 109.6 . . ? N3 C21 H21B 109.6 . . ? C14 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C27 122.4(5) . . ? C23 C22 N3 106.0(5) . . ? C27 C22 N3 131.6(5) . . ? N4 C23 C22 106.9(4) . . ? N4 C23 C24 132.4(6) . . ? C22 C23 C24 120.6(6) . . ? C25 C24 C23 115.7(7) . . ? C25 C24 H24 122.2 . . ? C23 C24 H24 122.2 . . ? C26 C25 C24 123.3(6) . . ? C26 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C25 C26 C27 120.2(7) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C22 C27 C26 117.8(7) . . ? C22 C27 H27 121.1 . . ? C26 C27 H27 121.1 . . ? N3 C28 N4 106.1(4) . . ? N3 C28 Ag1 130.2(3) . . ? N4 C28 Ag1 123.7(4) . . ? N4 C29 C30 111.7(6) . . ? N4 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N4 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 C1 C2 0.2(5) . . . . ? C10 N1 C1 C2 -178.7(5) . . . . ? C7 N1 C1 C6 179.3(5) . . . . ? C10 N1 C1 C6 0.4(8) . . . . ? N1 C1 C2 N2 -0.2(5) . . . . ? C6 C1 C2 N2 -179.4(5) . . . . ? N1 C1 C2 C3 178.4(5) . . . . ? C6 C1 C2 C3 -0.8(8) . . . . ? C7 N2 C2 C1 0.1(5) . . . . ? C8 N2 C2 C1 -175.2(5) . . . . ? C7 N2 C2 C3 -178.3(5) . . . . ? C8 N2 C2 C3 6.3(9) . . . . ? C1 C2 C3 C4 0.5(8) . . . . ? N2 C2 C3 C4 178.7(5) . . . . ? C2 C3 C4 C5 0.9(10) . . . . ? C3 C4 C5 C6 -2.1(11) . . . . ? C4 C5 C6 C1 1.8(9) . . . . ? C2 C1 C6 C5 -0.4(8) . . . . ? N1 C1 C6 C5 -179.3(5) . . . . ? C2 N2 C7 N1 0.0(5) . . . . ? C8 N2 C7 N1 175.4(5) . . . . ? C2 N2 C7 Ag1 179.7(3) . . . . ? C8 N2 C7 Ag1 -4.9(7) . . . . ? C1 N1 C7 N2 -0.2(5) . . . . ? C10 N1 C7 N2 178.7(5) . . . . ? C1 N1 C7 Ag1 -179.8(3) . . . . ? C10 N1 C7 Ag1 -1.0(8) . . . . ? C28 Ag1 C7 N2 -29(2) . . . . ? C28 Ag1 C7 N1 150.5(18) . . . . ? C7 N2 C8 C9 -86.4(7) . . . . ? C2 N2 C8 C9 88.3(7) . . . . ? C7 N1 C10 C11 10.2(8) . . . . ? C1 N1 C10 C11 -171.0(4) . . . . ? N1 C10 C11 C12 75.8(6) . . . . ? N1 C10 C11 C16 -95.5(5) . . . . ? C16 C11 C12 C13 7.4(6) . . . . ? C10 C11 C12 C13 -163.9(4) . . . . ? C16 C11 C12 C17 -177.4(5) . . . . ? C10 C11 C12 C17 11.3(7) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? C17 C12 C13 C14 -175.3(5) . . . . ? C11 C12 C13 C18 173.8(5) . . . . ? C17 C12 C13 C18 -1.5(7) . . . . ? C12 C13 C14 C15 -7.1(6) . . . . ? C18 C13 C14 C15 179.0(5) . . . . ? C12 C13 C14 C21 164.6(4) . . . . ? C18 C13 C14 C21 -9.3(7) . . . . ? C13 C14 C15 C16 6.9(6) . . . . ? C21 C14 C15 C16 -165.0(4) . . . . ? C13 C14 C15 C19 -179.7(5) . . . . ? C21 C14 C15 C19 8.4(7) . . . . ? C14 C15 C16 C11 0.4(6) . . . . ? C19 C15 C16 C11 -172.9(5) . . . . ? C14 C15 C16 C20 175.1(5) . . . . ? C19 C15 C16 C20 1.8(7) . . . . ? C12 C11 C16 C15 -7.6(6) . . . . ? C10 C11 C16 C15 163.5(4) . . . . ? C12 C11 C16 C20 177.8(5) . . . . ? C10 C11 C16 C20 -11.0(7) . . . . ? C28 N3 C21 C14 13.3(8) . . . . ? C22 N3 C21 C14 -167.4(4) . . . . ? C13 C14 C21 N3 -99.7(5) . . . . ? C15 C14 C21 N3 72.3(6) . . . . ? C28 N3 C22 C23 0.4(6) . . . . ? C21 N3 C22 C23 -179.1(5) . . . . ? C28 N3 C22 C27 179.6(6) . . . . ? C21 N3 C22 C27 0.1(9) . . . . ? C28 N4 C23 C22 -0.3(6) . . . . ? C29 N4 C23 C22 -175.5(5) . . . . ? C28 N4 C23 C24 179.4(6) . . . . ? C29 N4 C23 C24 4.2(9) . . . . ? C27 C22 C23 N4 -179.3(5) . . . . ? N3 C22 C23 N4 -0.1(5) . . . . ? C27 C22 C23 C24 0.9(8) . . . . ? N3 C22 C23 C24 -179.8(5) . . . . ? N4 C23 C24 C25 179.1(6) . . . . ? C22 C23 C24 C25 -1.2(8) . . . . ? C23 C24 C25 C26 1.2(10) . . . . ? C24 C25 C26 C27 -0.9(11) . . . . ? C23 C22 C27 C26 -0.6(9) . . . . ? N3 C22 C27 C26 -179.6(5) . . . . ? C25 C26 C27 C22 0.5(10) . . . . ? C22 N3 C28 N4 -0.6(5) . . . . ? C21 N3 C28 N4 178.8(5) . . . . ? C22 N3 C28 Ag1 178.0(3) . . . . ? C21 N3 C28 Ag1 -2.6(8) . . . . ? C23 N4 C28 N3 0.6(5) . . . . ? C29 N4 C28 N3 175.9(5) . . . . ? C23 N4 C28 Ag1 -178.2(3) . . . . ? C29 N4 C28 Ag1 -2.8(7) . . . . ? C7 Ag1 C28 N3 -168.4(18) . . . . ? C7 Ag1 C28 N4 10(2) . . . . ? C28 N4 C29 C30 -84.5(8) . . . . ? C23 N4 C29 C30 90.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.865 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.095 data_2h _database_code_depnum_ccdc_archive 'CCDC 757354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H43.88 Ag2 I0.1 N4 O1.88' _chemical_formula_weight 768.56 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' I I -0.4742 1.8119 '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 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 13.133(4) _cell_length_b 18.772(4) _cell_length_c 15.872(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.706(5) _cell_angle_gamma 90.00 _cell_volume 3784.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6944 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 22.5 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1566.0 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 3350 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0143 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3344 _reflns_number_gt 2887 _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^)+(0.0717P)^2^+3.5445P] 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 3344 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 0.40440(2) 0.624657(14) 0.558777(19) 0.05647(15) Uani 1 1 d . . . N1 N 0.6403(2) 0.66512(14) 0.59287(17) 0.0446(6) Uani 1 1 d . . . N2 N 0.5452(2) 0.76080(13) 0.57281(17) 0.0434(6) Uani 1 1 d . . . C1 C 0.5393(3) 0.68851(17) 0.5741(2) 0.0464(7) Uani 1 1 d . A . C2 C 0.7110(3) 0.72197(18) 0.60386(19) 0.0430(7) Uani 1 1 d . A . C3 C 0.6495(2) 0.78339(16) 0.59027(19) 0.0408(6) Uani 1 1 d . A . C4 C 0.6933(3) 0.85089(19) 0.5949(2) 0.0484(7) Uani 1 1 d . . . H4 H 0.6520 0.8917 0.5849 0.058 Uiso 1 1 calc R A . C5 C 0.8024(3) 0.8542(2) 0.6152(2) 0.0562(9) Uani 1 1 d . A . H5 H 0.8353 0.8983 0.6187 0.067 Uiso 1 1 calc R . . C6 C 0.8633(3) 0.7931(2) 0.6304(3) 0.0608(9) Uani 1 1 d . . . H6 H 0.9362 0.7976 0.6454 0.073 Uiso 1 1 calc R A . C7 C 0.8196(3) 0.7256(2) 0.6243(2) 0.0527(8) Uani 1 1 d . A . H7 H 0.8612 0.6848 0.6334 0.063 Uiso 1 1 calc R . . C8 C 0.6703(3) 0.58960(18) 0.6009(2) 0.0546(8) Uani 1 1 d . A . H8A H 0.7342 0.5832 0.5816 0.066 Uiso 1 1 calc R . . H8B H 0.6152 0.5616 0.5629 0.066 Uiso 1 1 calc R . . C9 C 0.6884(4) 0.5625(2) 0.6926(3) 0.0806(13) Uani 1 1 d . . . H9A H 0.6291 0.5760 0.7151 0.097 Uiso 1 1 calc R A . H9B H 0.7507 0.5852 0.7286 0.097 Uiso 1 1 calc R . . C10 C 0.7024(5) 0.4828(3) 0.6999(4) 0.1021(18) Uani 1 1 d . A . H10A H 0.7545 0.4687 0.6694 0.123 Uiso 1 1 calc R . . H10B H 0.7298 0.4705 0.7608 0.123 Uiso 1 1 calc R . . C11 C 0.6046(6) 0.4414(3) 0.6644(4) 0.121(2) Uani 1 1 d . . . H11A H 0.5503 0.4578 0.6904 0.182 Uiso 1 1 calc R A . H11B H 0.6179 0.3918 0.6775 0.182 Uiso 1 1 calc R . . H11C H 0.5823 0.4477 0.6024 0.182 Uiso 1 1 calc R . . C12 C 0.4577(3) 0.81204(19) 0.5579(3) 0.0571(9) Uani 1 1 d . A . H12A H 0.4661 0.8462 0.5142 0.068 Uiso 1 1 calc R . . H12B H 0.4617 0.8380 0.6114 0.068 Uiso 1 1 calc R . . C13 C 0.3503(2) 0.77819(17) 0.5282(2) 0.0445(7) Uani 1 1 d . . . C14 C 0.3073(3) 0.76550(17) 0.4387(2) 0.0454(7) Uani 1 1 d . A . C15 C 0.3694(3) 0.7837(3) 0.3732(3) 0.0722(11) Uani 1 1 d . . . H15A H 0.3552 0.7490 0.3273 0.108 Uiso 1 1 calc R A . H15B H 0.4433 0.7836 0.4016 0.108 Uiso 1 1 calc R . . H15C H 0.3492 0.8300 0.3492 0.108 Uiso 1 1 calc R . . C16 C 0.2062(3) 0.73815(18) 0.4107(2) 0.0450(7) Uani 1 1 d . . . C17 C 0.1565(4) 0.7281(3) 0.3140(2) 0.0762(12) Uani 1 1 d . A . H17A H 0.1816 0.7645 0.2818 0.114 Uiso 1 1 calc R . . H17B H 0.0814 0.7314 0.3031 0.114 Uiso 1 1 calc R . . H17C H 0.1753 0.6822 0.2962 0.114 Uiso 1 1 calc R . . O1 O 0.2630(2) 0.55214(14) 0.5481(2) 0.0644(7) Uani 0.9414(8) 1 d P A 1 H1 H 0.2783 0.5204 0.5847 0.097 Uiso 0.9414(8) 1 calc PR A 1 I1 I 0.1969(4) 0.5313(2) 0.5372(4) 0.0644(7) Uani 0.0586(8) 1 d P A 2 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 0.0518(2) 0.0419(2) 0.0744(2) 0.00148(11) 0.01351(15) -0.00528(10) N1 0.0461(15) 0.0411(14) 0.0465(14) 0.0060(11) 0.0116(11) 0.0049(12) N2 0.0389(14) 0.0376(13) 0.0516(14) 0.0019(11) 0.0075(11) 0.0006(11) C1 0.0430(17) 0.0444(17) 0.0491(17) 0.0034(14) 0.0067(14) -0.0006(14) C2 0.0432(17) 0.0500(17) 0.0357(14) 0.0012(13) 0.0100(12) 0.0016(14) C3 0.0399(16) 0.0447(16) 0.0367(14) -0.0018(12) 0.0075(12) 0.0003(13) C4 0.0484(19) 0.0452(17) 0.0507(18) -0.0048(14) 0.0107(15) -0.0024(15) C5 0.053(2) 0.0565(19) 0.061(2) -0.0117(17) 0.0184(17) -0.0147(17) C6 0.0403(18) 0.080(3) 0.062(2) -0.0084(19) 0.0132(16) -0.0051(18) C7 0.0432(18) 0.064(2) 0.0520(18) -0.0020(16) 0.0142(15) 0.0067(16) C8 0.057(2) 0.0440(18) 0.062(2) 0.0053(15) 0.0144(17) 0.0090(16) C9 0.108(4) 0.057(2) 0.065(2) 0.0142(19) 0.000(2) 0.000(2) C10 0.125(5) 0.063(3) 0.108(4) 0.033(3) 0.011(3) 0.004(3) C11 0.173(7) 0.075(4) 0.115(5) 0.016(3) 0.033(4) -0.031(4) C12 0.0412(18) 0.0429(18) 0.083(2) -0.0010(17) 0.0082(17) 0.0051(15) C13 0.0384(16) 0.0397(16) 0.0521(17) 0.0010(13) 0.0054(13) 0.0045(13) C14 0.0471(18) 0.0463(17) 0.0455(16) 0.0078(13) 0.0162(14) 0.0119(14) C15 0.070(3) 0.085(3) 0.071(3) 0.019(2) 0.036(2) 0.014(2) C16 0.0456(17) 0.0486(17) 0.0378(15) -0.0004(13) 0.0051(13) 0.0072(14) C17 0.079(3) 0.096(3) 0.045(2) -0.007(2) -0.0010(19) 0.005(2) O1 0.0589(16) 0.0408(13) 0.0935(17) -0.0028(11) 0.0191(15) 0.0028(11) I1 0.0589(16) 0.0408(13) 0.0935(17) -0.0028(11) 0.0191(15) 0.0028(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 C1 2.101(3) . ? Ag1 O1 2.274(3) . ? Ag1 I1 3.185(5) . ? N1 C1 1.356(4) . ? N1 C2 1.396(4) . ? N1 C8 1.469(4) . ? N2 C1 1.360(4) . ? N2 C3 1.393(4) . ? N2 C12 1.470(4) . ? C2 C7 1.382(5) . ? C2 C3 1.393(4) . ? C3 C4 1.386(5) . ? C4 C5 1.387(5) . ? C4 H4 0.9300 . ? C5 C6 1.383(6) . ? C5 H5 0.9300 . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.504(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.508(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.485(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.510(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C16 1.396(5) 7_566 ? C13 C14 1.409(5) . ? C14 C16 1.387(5) . ? C14 C15 1.514(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C13 1.396(5) 7_566 ? C16 C17 1.519(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? O1 H1 0.8200 . ? 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 C1 Ag1 O1 177.06(12) . . ? C1 Ag1 I1 178.50(12) . . ? O1 Ag1 I1 3.74(11) . . ? C1 N1 C2 111.3(3) . . ? C1 N1 C8 123.9(3) . . ? C2 N1 C8 124.8(3) . . ? C1 N2 C3 111.0(3) . . ? C1 N2 C12 127.6(3) . . ? C3 N2 C12 121.4(3) . . ? N1 C1 N2 105.7(3) . . ? N1 C1 Ag1 126.1(2) . . ? N2 C1 Ag1 128.1(2) . . ? C7 C2 C3 121.3(3) . . ? C7 C2 N1 132.9(3) . . ? C3 C2 N1 105.8(3) . . ? C4 C3 C2 122.1(3) . . ? C4 C3 N2 131.5(3) . . ? C2 C3 N2 106.3(3) . . ? C3 C4 C5 116.3(3) . . ? C3 C4 H4 121.8 . . ? C5 C4 H4 121.8 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 122.4(3) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C2 C7 C6 116.4(3) . . ? C2 C7 H7 121.8 . . ? C6 C7 H7 121.8 . . ? N1 C8 C9 112.5(3) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 113.3(4) . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 114.5(5) . . ? C11 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 113.9(3) . . ? N2 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? N2 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C16 C13 C14 121.0(3) 7_566 . ? C16 C13 C12 119.7(3) 7_566 . ? C14 C13 C12 119.2(3) . . ? C16 C14 C13 119.4(3) . . ? C16 C14 C15 120.1(3) . . ? C13 C14 C15 120.4(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 C13 119.5(3) . 7_566 ? C14 C16 C17 120.0(3) . . ? C13 C16 C17 120.4(3) 7_566 . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Ag1 O1 H1 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 0.2(4) . . . . ? C8 N1 C1 N2 179.9(3) . . . . ? C2 N1 C1 Ag1 -176.3(2) . . . . ? C8 N1 C1 Ag1 3.4(4) . . . . ? C3 N2 C1 N1 0.2(4) . . . . ? C12 N2 C1 N1 -178.2(3) . . . . ? C3 N2 C1 Ag1 176.7(2) . . . . ? C12 N2 C1 Ag1 -1.8(5) . . . . ? O1 Ag1 C1 N1 41(2) . . . . ? I1 Ag1 C1 N1 151(5) . . . . ? O1 Ag1 C1 N2 -135(2) . . . . ? I1 Ag1 C1 N2 -25(5) . . . . ? C1 N1 C2 C7 179.0(3) . . . . ? C8 N1 C2 C7 -0.7(5) . . . . ? C1 N1 C2 C3 -0.5(3) . . . . ? C8 N1 C2 C3 179.8(3) . . . . ? C7 C2 C3 C4 1.2(5) . . . . ? N1 C2 C3 C4 -179.2(3) . . . . ? C7 C2 C3 N2 -179.0(3) . . . . ? N1 C2 C3 N2 0.7(3) . . . . ? C1 N2 C3 C4 179.3(3) . . . . ? C12 N2 C3 C4 -2.2(5) . . . . ? C1 N2 C3 C2 -0.6(3) . . . . ? C12 N2 C3 C2 178.0(3) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? N2 C3 C4 C5 179.2(3) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C4 C5 C6 C7 1.7(6) . . . . ? C3 C2 C7 C6 0.1(5) . . . . ? N1 C2 C7 C6 -179.4(3) . . . . ? C5 C6 C7 C2 -1.4(5) . . . . ? C1 N1 C8 C9 -91.0(4) . . . . ? C2 N1 C8 C9 88.7(4) . . . . ? N1 C8 C9 C10 170.8(4) . . . . ? C8 C9 C10 C11 -71.7(7) . . . . ? C1 N2 C12 C13 -9.4(5) . . . . ? C3 N2 C12 C13 172.3(3) . . . . ? N2 C12 C13 C16 95.4(4) . . . 7_566 ? N2 C12 C13 C14 -86.4(4) . . . . ? C16 C13 C14 C16 1.8(5) 7_566 . . . ? C12 C13 C14 C16 -176.4(3) . . . . ? C16 C13 C14 C15 179.8(3) 7_566 . . . ? C12 C13 C14 C15 1.7(5) . . . . ? C13 C14 C16 C13 -1.7(5) . . . 7_566 ? C15 C14 C16 C13 -179.8(3) . . . 7_566 ? C13 C14 C16 C17 176.5(3) . . . . ? C15 C14 C16 C17 -1.6(5) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.481 0.250 112 31 ' ' 2 0.000 0.519 0.750 112 31 ' ' 3 0.500 0.981 0.250 112 31 ' ' 4 0.500 0.019 0.750 112 31 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.918 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.082 data_1e _database_code_depnum_ccdc_archive 'CCDC 757355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H41 Br2 N7' _chemical_formula_weight 779.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.7807(7) _cell_length_b 14.6784(7) _cell_length_c 18.5397(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.0320(10) _cell_angle_gamma 90.00 _cell_volume 3754.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6603 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.95 _exptl_crystal_description BLOCK _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 2.197 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6435 _exptl_absorpt_correction_T_max 0.7484 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 18776 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6616 _reflns_number_gt 4554 _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^)+(0.0733P)^2^+1.6636P] 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 6616 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Br1 Br 0.25655(3) 0.79382(3) 0.32118(3) 0.06850(16) Uani 1 1 d . . . Br2 Br 0.42225(4) 0.21335(3) 0.24727(3) 0.07578(18) Uani 1 1 d . . . N1 N 0.1066(3) 0.3251(3) 0.1738(2) 0.0796(11) Uani 1 1 d . . . N2 N 0.2447(2) 0.4143(2) 0.13643(17) 0.0554(8) Uani 1 1 d . . . N3 N 0.3118(2) 0.51724(19) 0.22386(16) 0.0485(7) Uani 1 1 d . . . N4 N 0.4261(2) 0.19774(18) 0.50309(16) 0.0444(7) Uani 1 1 d . . . N5 N 0.3453(2) 0.09730(19) 0.41683(16) 0.0467(7) Uani 1 1 d . . . N6 N 0.1578(2) 0.1624(2) 0.3679(2) 0.0721(10) Uani 1 1 d . . . C1 C 0.1296(3) 0.2876(3) 0.1180(2) 0.0613(10) Uani 1 1 d . . . C2 C 0.0311(5) 0.2885(4) 0.1884(4) 0.0986(17) Uani 1 1 d . . . H2 H 0.0136 0.3147 0.2272 0.118 Uiso 1 1 calc R . . C3 C -0.0202(4) 0.2166(4) 0.1503(4) 0.1044(19) Uani 1 1 d . . . H3 H -0.0712 0.1937 0.1631 0.125 Uiso 1 1 calc R . . C4 C 0.0033(4) 0.1774(4) 0.0928(4) 0.110(2) Uani 1 1 d . . . H4 H -0.0309 0.1272 0.0661 0.132 Uiso 1 1 calc R . . C5 C 0.0796(4) 0.2140(3) 0.0743(3) 0.0925(16) Uani 1 1 d . . . H5 H 0.0964 0.1901 0.0344 0.111 Uiso 1 1 calc R . . C6 C 0.2157(3) 0.3253(3) 0.1023(2) 0.0652(11) Uani 1 1 d . . . H6A H 0.2698 0.2835 0.1227 0.078 Uiso 1 1 calc R . . H6B H 0.1999 0.3295 0.0469 0.078 Uiso 1 1 calc R . . C7 C 0.2125(3) 0.4977(3) 0.1021(2) 0.0548(9) Uani 1 1 d . . . C8 C 0.2566(3) 0.5643(3) 0.1567(2) 0.0508(9) Uani 1 1 d . . . C9 C 0.2461(3) 0.6567(3) 0.1408(2) 0.0666(11) Uani 1 1 d . . . H9 H 0.2766 0.7008 0.1775 0.080 Uiso 1 1 calc R . . C10 C 0.1870(4) 0.6784(4) 0.0664(3) 0.0887(15) Uani 1 1 d . . . H10 H 0.1778 0.7394 0.0522 0.106 Uiso 1 1 calc R . . C11 C 0.1402(4) 0.6117(4) 0.0114(3) 0.0950(16) Uani 1 1 d . . . H11 H 0.0998 0.6299 -0.0377 0.114 Uiso 1 1 calc R . . C12 C 0.1522(3) 0.5212(4) 0.0279(2) 0.0740(12) Uani 1 1 d . . . H12 H 0.1215 0.4772 -0.0088 0.089 Uiso 1 1 calc R . . C13 C 0.3025(3) 0.4290(3) 0.2083(2) 0.0533(9) Uani 1 1 d . . . H13 H 0.3328 0.3834 0.2435 0.064 Uiso 1 1 calc R . . C14 C 0.3714(3) 0.5604(2) 0.2982(2) 0.0539(9) Uani 1 1 d . . . H14A H 0.3353 0.6098 0.3098 0.065 Uiso 1 1 calc R . . H14B H 0.4298 0.5857 0.2937 0.065 Uiso 1 1 calc R . . C15 C 0.3986(2) 0.4910(2) 0.36337(19) 0.0459(8) Uani 1 1 d . . . C16 C 0.4893(2) 0.4492(2) 0.38762(19) 0.0470(8) Uani 1 1 d . . . C17 C 0.5120(2) 0.3820(2) 0.44542(19) 0.0469(8) Uani 1 1 d . . . C18 C 0.4441(3) 0.3599(2) 0.47945(19) 0.0468(8) Uani 1 1 d . . . C19 C 0.3524(3) 0.4013(2) 0.4540(2) 0.0497(9) Uani 1 1 d . . . C20 C 0.3290(2) 0.4670(2) 0.3958(2) 0.0486(8) Uani 1 1 d . . . C21 C 0.5630(3) 0.4712(3) 0.3511(3) 0.0740(12) Uani 1 1 d . . . H21A H 0.5629 0.4240 0.3152 0.111 Uiso 1 1 calc R . . H21B H 0.6263 0.4753 0.3905 0.111 Uiso 1 1 calc R . . H21C H 0.5468 0.5283 0.3243 0.111 Uiso 1 1 calc R . . C22 C 0.6078(3) 0.3320(3) 0.4667(3) 0.0683(11) Uani 1 1 d . . . H22A H 0.6116 0.2862 0.5046 0.102 Uiso 1 1 calc R . . H22B H 0.6601 0.3745 0.4875 0.102 Uiso 1 1 calc R . . H22C H 0.6123 0.3037 0.4214 0.102 Uiso 1 1 calc R . . C23 C 0.2774(3) 0.3723(3) 0.4881(3) 0.0721(12) Uani 1 1 d . . . H23A H 0.2398 0.3226 0.4585 0.108 Uiso 1 1 calc R . . H23B H 0.2353 0.4226 0.4866 0.108 Uiso 1 1 calc R . . H23C H 0.3096 0.3533 0.5406 0.108 Uiso 1 1 calc R . . C24 C 0.2288(3) 0.5096(3) 0.3648(3) 0.0717(12) Uani 1 1 d . . . H24A H 0.1823 0.4645 0.3372 0.108 Uiso 1 1 calc R . . H24B H 0.2285 0.5588 0.3306 0.108 Uiso 1 1 calc R . . H24C H 0.2124 0.5324 0.4071 0.108 Uiso 1 1 calc R . . C25 C 0.4667(3) 0.2848(2) 0.5392(2) 0.0518(9) Uani 1 1 d . . . H25A H 0.5364 0.2791 0.5644 0.062 Uiso 1 1 calc R . . H25B H 0.4398 0.3003 0.5782 0.062 Uiso 1 1 calc R . . C26 C 0.4336(2) 0.1148(2) 0.54184(19) 0.0439(8) Uani 1 1 d . . . C27 C 0.3819(2) 0.0511(2) 0.4869(2) 0.0443(8) Uani 1 1 d . . . C28 C 0.3771(3) -0.0406(2) 0.5046(2) 0.0531(9) Uani 1 1 d . . . H28 H 0.3422 -0.0829 0.4678 0.064 Uiso 1 1 calc R . . C29 C 0.4276(3) -0.0643(3) 0.5803(2) 0.0577(10) Uani 1 1 d . . . H29 H 0.4266 -0.1247 0.5952 0.069 Uiso 1 1 calc R . . C30 C 0.4800(3) -0.0009(3) 0.6352(2) 0.0571(10) Uani 1 1 d . . . H30 H 0.5133 -0.0205 0.6855 0.069 Uiso 1 1 calc R . . C31 C 0.4844(3) 0.0905(2) 0.6178(2) 0.0511(9) Uani 1 1 d . . . H31 H 0.5193 0.1327 0.6547 0.061 Uiso 1 1 calc R . . C32 C 0.3731(2) 0.1839(2) 0.4293(2) 0.0490(8) Uani 1 1 d . . . H32 H 0.3573 0.2288 0.3914 0.059 Uiso 1 1 calc R . . C33 C 0.2744(3) 0.0626(3) 0.3450(2) 0.0554(9) Uani 1 1 d . . . H33A H 0.2836 -0.0024 0.3412 0.066 Uiso 1 1 calc R . . H33B H 0.2839 0.0919 0.3013 0.066 Uiso 1 1 calc R . . C34 C 0.1727(3) 0.0809(3) 0.3424(2) 0.0540(9) Uani 1 1 d . . . C35 C 0.0672(4) 0.1802(4) 0.3649(3) 0.0884(15) Uani 1 1 d . . . H35 H 0.0551 0.2365 0.3826 0.106 Uiso 1 1 calc R . . C36 C -0.0074(4) 0.1206(4) 0.3375(3) 0.0904(15) Uani 1 1 d . . . H36 H -0.0693 0.1368 0.3349 0.108 Uiso 1 1 calc R . . C37 C 0.0093(3) 0.0374(4) 0.3141(3) 0.0825(14) Uani 1 1 d . . . H37 H -0.0406 -0.0050 0.2965 0.099 Uiso 1 1 calc R . . C38 C 0.1016(3) 0.0157(3) 0.3166(2) 0.0693(11) Uani 1 1 d . . . H38 H 0.1151 -0.0415 0.3013 0.083 Uiso 1 1 calc R . . N7 N 1.0030(5) 0.0806(5) 0.8983(4) 0.155(3) Uani 1 1 d . . . C39 C 0.9244(6) 0.0669(5) 0.8843(4) 0.131(2) Uani 1 1 d . . . C40 C 0.8264(5) 0.0441(6) 0.8680(6) 0.188(4) Uani 1 1 d . . . H40A H 0.8134 -0.0149 0.8441 0.282 Uiso 1 1 calc R . . H40B H 0.7855 0.0885 0.8336 0.282 Uiso 1 1 calc R . . H40C H 0.8135 0.0430 0.9152 0.282 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 Br1 0.0700(3) 0.0516(2) 0.0799(3) -0.0100(2) 0.0220(2) 0.00851(19) Br2 0.1091(4) 0.0598(3) 0.0682(3) 0.0165(2) 0.0437(3) 0.0305(2) N1 0.093(3) 0.074(2) 0.086(3) -0.001(2) 0.048(2) 0.002(2) N2 0.0557(19) 0.063(2) 0.0450(18) -0.0057(15) 0.0151(15) 0.0007(15) N3 0.0525(17) 0.0482(17) 0.0410(16) 0.0029(13) 0.0124(14) 0.0027(14) N4 0.0475(16) 0.0439(16) 0.0400(16) 0.0024(12) 0.0134(13) -0.0031(13) N5 0.0447(16) 0.0476(17) 0.0453(17) -0.0023(13) 0.0133(14) -0.0017(13) N6 0.060(2) 0.068(2) 0.082(3) -0.0109(19) 0.0185(19) 0.0067(18) C1 0.065(3) 0.057(2) 0.057(2) -0.0012(19) 0.015(2) 0.007(2) C2 0.121(5) 0.077(4) 0.119(5) 0.015(3) 0.070(4) 0.006(3) C3 0.097(4) 0.096(4) 0.131(5) 0.033(4) 0.054(4) 0.000(3) C4 0.098(4) 0.085(4) 0.133(6) 0.009(4) 0.025(4) -0.026(3) C5 0.098(4) 0.080(3) 0.094(4) -0.012(3) 0.028(3) -0.007(3) C6 0.067(3) 0.068(3) 0.058(2) -0.017(2) 0.019(2) 0.003(2) C7 0.049(2) 0.071(3) 0.045(2) 0.0027(19) 0.0180(18) 0.0090(19) C8 0.047(2) 0.061(2) 0.045(2) 0.0094(17) 0.0178(17) 0.0076(18) C9 0.073(3) 0.067(3) 0.060(3) 0.014(2) 0.023(2) 0.015(2) C10 0.105(4) 0.085(3) 0.074(3) 0.033(3) 0.030(3) 0.030(3) C11 0.104(4) 0.115(4) 0.054(3) 0.015(3) 0.013(3) 0.031(3) C12 0.070(3) 0.094(4) 0.050(2) 0.006(2) 0.012(2) 0.017(3) C13 0.059(2) 0.052(2) 0.046(2) -0.0005(17) 0.0167(19) 0.0033(18) C14 0.058(2) 0.049(2) 0.048(2) -0.0017(16) 0.0101(18) -0.0061(17) C15 0.051(2) 0.0393(18) 0.0411(19) -0.0034(14) 0.0093(16) -0.0038(16) C16 0.049(2) 0.0487(19) 0.0421(19) -0.0033(16) 0.0147(16) -0.0062(16) C17 0.049(2) 0.0437(19) 0.0418(19) -0.0043(15) 0.0085(16) -0.0002(16) C18 0.052(2) 0.0438(19) 0.0390(18) -0.0034(15) 0.0102(17) -0.0053(16) C19 0.051(2) 0.051(2) 0.048(2) -0.0065(17) 0.0183(17) -0.0075(17) C20 0.047(2) 0.0469(19) 0.047(2) -0.0073(16) 0.0108(17) -0.0018(16) C21 0.068(3) 0.087(3) 0.074(3) 0.023(2) 0.033(2) 0.011(2) C22 0.059(2) 0.071(3) 0.074(3) 0.013(2) 0.022(2) 0.011(2) C23 0.065(3) 0.079(3) 0.078(3) 0.006(2) 0.034(2) -0.005(2) C24 0.052(2) 0.078(3) 0.079(3) 0.008(2) 0.016(2) 0.010(2) C25 0.059(2) 0.048(2) 0.043(2) -0.0009(16) 0.0113(17) -0.0063(17) C26 0.0457(19) 0.0465(19) 0.0435(19) 0.0023(16) 0.0207(16) 0.0046(15) C27 0.0417(19) 0.0458(19) 0.050(2) 0.0021(16) 0.0224(17) 0.0011(15) C28 0.053(2) 0.051(2) 0.065(2) -0.0004(19) 0.032(2) 0.0010(17) C29 0.066(2) 0.049(2) 0.072(3) 0.012(2) 0.042(2) 0.0110(19) C30 0.066(2) 0.062(2) 0.052(2) 0.0138(19) 0.031(2) 0.013(2) C31 0.056(2) 0.056(2) 0.045(2) 0.0023(16) 0.0231(18) 0.0052(17) C32 0.050(2) 0.051(2) 0.043(2) 0.0057(16) 0.0118(17) -0.0012(17) C33 0.054(2) 0.058(2) 0.048(2) -0.0076(17) 0.0121(18) -0.0046(18) C34 0.053(2) 0.059(2) 0.045(2) 0.0009(17) 0.0107(18) -0.0024(18) C35 0.065(3) 0.096(4) 0.096(4) -0.013(3) 0.019(3) 0.014(3) C36 0.056(3) 0.118(4) 0.095(4) 0.009(3) 0.024(3) 0.011(3) C37 0.056(3) 0.094(4) 0.088(3) 0.003(3) 0.014(2) -0.012(3) C38 0.062(3) 0.068(3) 0.068(3) -0.008(2) 0.011(2) -0.010(2) N7 0.109(4) 0.141(5) 0.219(8) -0.041(5) 0.065(5) -0.032(4) C39 0.136(6) 0.136(6) 0.139(6) -0.020(5) 0.071(6) -0.017(5) C40 0.096(5) 0.178(8) 0.298(13) 0.030(8) 0.080(7) -0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.320(5) . ? N1 C2 1.350(6) . ? N2 C13 1.318(5) . ? N2 C7 1.383(5) . ? N2 C6 1.448(5) . ? N3 C13 1.323(4) . ? N3 C8 1.401(4) . ? N3 C14 1.485(4) . ? N4 C32 1.325(4) . ? N4 C26 1.397(4) . ? N4 C25 1.468(4) . ? N5 C32 1.331(4) . ? N5 C27 1.390(4) . ? N5 C33 1.459(4) . ? N6 C34 1.333(5) . ? N6 C35 1.347(6) . ? C1 C5 1.392(6) . ? C1 C6 1.510(6) . ? C2 C3 1.344(8) . ? C2 H2 0.9300 . ? C3 C4 1.362(8) . ? C3 H3 0.9300 . ? C4 C5 1.398(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.388(5) . ? C7 C8 1.389(5) . ? C8 C9 1.385(5) . ? C9 C10 1.379(6) . ? C9 H9 0.9300 . ? C10 C11 1.403(7) . ? C10 H10 0.9300 . ? C11 C12 1.361(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.520(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.394(5) . ? C15 C20 1.410(5) . ? C16 C17 1.406(5) . ? C16 C21 1.511(5) . ? C17 C18 1.401(5) . ? C17 C22 1.516(5) . ? C18 C19 1.403(5) . ? C18 C25 1.512(5) . ? C19 C20 1.395(5) . ? C19 C23 1.521(5) . ? C20 C24 1.518(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C31 1.383(5) . ? C26 C27 1.392(5) . ? C27 C28 1.394(5) . ? C28 C29 1.376(5) . ? C28 H28 0.9300 . ? C29 C30 1.392(5) . ? C29 H29 0.9300 . ? C30 C31 1.387(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.511(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C38 1.374(5) . ? C35 C36 1.355(7) . ? C35 H35 0.9300 . ? C36 C37 1.348(7) . ? C36 H36 0.9300 . ? C37 C38 1.385(6) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? N7 C39 1.114(8) . ? C39 C40 1.411(10) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 117.1(4) . . ? C13 N2 C7 108.1(3) . . ? C13 N2 C6 124.9(3) . . ? C7 N2 C6 126.8(3) . . ? C13 N3 C8 107.9(3) . . ? C13 N3 C14 126.9(3) . . ? C8 N3 C14 125.2(3) . . ? C32 N4 C26 107.8(3) . . ? C32 N4 C25 126.7(3) . . ? C26 N4 C25 125.5(3) . . ? C32 N5 C27 108.1(3) . . ? C32 N5 C33 124.6(3) . . ? C27 N5 C33 126.4(3) . . ? C34 N6 C35 116.6(4) . . ? N1 C1 C5 123.2(5) . . ? N1 C1 C6 118.1(4) . . ? C5 C1 C6 118.7(4) . . ? C3 C2 N1 123.9(6) . . ? C3 C2 H2 118.0 . . ? N1 C2 H2 118.0 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.0(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C1 C5 C4 117.5(5) . . ? C1 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? N2 C6 C1 112.6(3) . . ? N2 C6 H6A 109.1 . . ? C1 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C1 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C12 131.9(4) . . ? N2 C7 C8 107.1(3) . . ? C12 C7 C8 121.0(4) . . ? C9 C8 C7 123.1(4) . . ? C9 C8 N3 131.0(4) . . ? C7 C8 N3 105.8(3) . . ? C10 C9 C8 114.9(4) . . ? C10 C9 H9 122.6 . . ? C8 C9 H9 122.6 . . ? C9 C10 C11 122.5(5) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 121.8(5) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 116.8(5) . . ? C11 C12 H12 121.6 . . ? C7 C12 H12 121.6 . . ? N2 C13 N3 111.1(3) . . ? N2 C13 H13 124.5 . . ? N3 C13 H13 124.5 . . ? N3 C14 C15 110.6(3) . . ? N3 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C20 121.1(3) . . ? C16 C15 C14 120.1(3) . . ? C20 C15 C14 118.8(3) . . ? C15 C16 C17 119.6(3) . . ? C15 C16 C21 121.7(3) . . ? C17 C16 C21 118.6(3) . . ? C18 C17 C16 119.5(3) . . ? C18 C17 C22 121.6(3) . . ? C16 C17 C22 118.9(3) . . ? C17 C18 C19 120.7(3) . . ? C17 C18 C25 119.5(3) . . ? C19 C18 C25 119.6(3) . . ? C20 C19 C18 120.0(3) . . ? C20 C19 C23 120.0(3) . . ? C18 C19 C23 119.9(3) . . ? C19 C20 C15 119.1(3) . . ? C19 C20 C24 121.0(3) . . ? C15 C20 C24 119.9(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C18 110.7(3) . . ? N4 C25 H25A 109.5 . . ? C18 C25 H25A 109.5 . . ? N4 C25 H25B 109.5 . . ? C18 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C31 C26 C27 121.8(3) . . ? C31 C26 N4 131.5(3) . . ? C27 C26 N4 106.7(3) . . ? N5 C27 C26 106.5(3) . . ? N5 C27 C28 131.0(3) . . ? C26 C27 C28 122.5(3) . . ? C29 C28 C27 115.5(4) . . ? C29 C28 H28 122.3 . . ? C27 C28 H28 122.3 . . ? C28 C29 C30 122.2(4) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 122.4(4) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C26 C31 C30 115.7(3) . . ? C26 C31 H31 122.2 . . ? C30 C31 H31 122.2 . . ? N4 C32 N5 110.9(3) . . ? N4 C32 H32 124.5 . . ? N5 C32 H32 124.5 . . ? N5 C33 C34 110.3(3) . . ? N5 C33 H33A 109.6 . . ? C34 C33 H33A 109.6 . . ? N5 C33 H33B 109.6 . . ? C34 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? N6 C34 C38 123.1(4) . . ? N6 C34 C33 115.9(3) . . ? C38 C34 C33 121.0(4) . . ? N6 C35 C36 123.6(5) . . ? N6 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? C37 C36 C35 119.1(5) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C34 C38 C37 118.2(4) . . ? C34 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? N7 C39 C40 176.5(10) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 C5 0.5(7) . . . . ? C2 N1 C1 C6 -178.0(4) . . . . ? C1 N1 C2 C3 0.8(8) . . . . ? N1 C2 C3 C4 -0.6(10) . . . . ? C2 C3 C4 C5 -0.7(9) . . . . ? N1 C1 C5 C4 -1.8(7) . . . . ? C6 C1 C5 C4 176.7(5) . . . . ? C3 C4 C5 C1 1.9(9) . . . . ? C13 N2 C6 C1 84.8(5) . . . . ? C7 N2 C6 C1 -90.6(4) . . . . ? N1 C1 C6 N2 -16.5(5) . . . . ? C5 C1 C6 N2 164.8(4) . . . . ? C13 N2 C7 C12 178.9(4) . . . . ? C6 N2 C7 C12 -5.0(7) . . . . ? C13 N2 C7 C8 1.9(4) . . . . ? C6 N2 C7 C8 177.9(3) . . . . ? N2 C7 C8 C9 175.6(4) . . . . ? C12 C7 C8 C9 -1.8(6) . . . . ? N2 C7 C8 N3 -2.2(4) . . . . ? C12 C7 C8 N3 -179.7(3) . . . . ? C13 N3 C8 C9 -175.8(4) . . . . ? C14 N3 C8 C9 2.9(6) . . . . ? C13 N3 C8 C7 1.8(4) . . . . ? C14 N3 C8 C7 -179.5(3) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? N3 C8 C9 C10 178.1(4) . . . . ? C8 C9 C10 C11 0.8(7) . . . . ? C9 C10 C11 C12 -1.5(9) . . . . ? C10 C11 C12 C7 0.5(8) . . . . ? N2 C7 C12 C11 -175.7(4) . . . . ? C8 C7 C12 C11 1.0(6) . . . . ? C7 N2 C13 N3 -0.7(4) . . . . ? C6 N2 C13 N3 -176.9(3) . . . . ? C8 N3 C13 N2 -0.7(4) . . . . ? C14 N3 C13 N2 -179.4(3) . . . . ? C13 N3 C14 C15 -16.9(5) . . . . ? C8 N3 C14 C15 164.7(3) . . . . ? N3 C14 C15 C16 98.3(4) . . . . ? N3 C14 C15 C20 -78.7(4) . . . . ? C20 C15 C16 C17 -0.1(5) . . . . ? C14 C15 C16 C17 -177.0(3) . . . . ? C20 C15 C16 C21 177.3(3) . . . . ? C14 C15 C16 C21 0.4(5) . . . . ? C15 C16 C17 C18 -1.9(5) . . . . ? C21 C16 C17 C18 -179.4(3) . . . . ? C15 C16 C17 C22 175.3(3) . . . . ? C21 C16 C17 C22 -2.2(5) . . . . ? C16 C17 C18 C19 2.9(5) . . . . ? C22 C17 C18 C19 -174.2(3) . . . . ? C16 C17 C18 C25 177.4(3) . . . . ? C22 C17 C18 C25 0.3(5) . . . . ? C17 C18 C19 C20 -1.9(5) . . . . ? C25 C18 C19 C20 -176.4(3) . . . . ? C17 C18 C19 C23 176.2(3) . . . . ? C25 C18 C19 C23 1.7(5) . . . . ? C18 C19 C20 C15 0.0(5) . . . . ? C23 C19 C20 C15 -178.1(3) . . . . ? C18 C19 C20 C24 177.3(3) . . . . ? C23 C19 C20 C24 -0.8(5) . . . . ? C16 C15 C20 C19 1.0(5) . . . . ? C14 C15 C20 C19 178.0(3) . . . . ? C16 C15 C20 C24 -176.3(3) . . . . ? C14 C15 C20 C24 0.7(5) . . . . ? C32 N4 C25 C18 -2.7(5) . . . . ? C26 N4 C25 C18 -179.8(3) . . . . ? C17 C18 C25 N4 -94.4(4) . . . . ? C19 C18 C25 N4 80.1(4) . . . . ? C32 N4 C26 C31 176.2(3) . . . . ? C25 N4 C26 C31 -6.2(6) . . . . ? C32 N4 C26 C27 -0.1(4) . . . . ? C25 N4 C26 C27 177.5(3) . . . . ? C32 N5 C27 C26 -0.4(4) . . . . ? C33 N5 C27 C26 -170.0(3) . . . . ? C32 N5 C27 C28 -177.0(3) . . . . ? C33 N5 C27 C28 13.4(6) . . . . ? C31 C26 C27 N5 -176.4(3) . . . . ? N4 C26 C27 N5 0.3(3) . . . . ? C31 C26 C27 C28 0.5(5) . . . . ? N4 C26 C27 C28 177.3(3) . . . . ? N5 C27 C28 C29 175.8(3) . . . . ? C26 C27 C28 C29 -0.4(5) . . . . ? C27 C28 C29 C30 -0.2(5) . . . . ? C28 C29 C30 C31 0.5(6) . . . . ? C27 C26 C31 C30 -0.2(5) . . . . ? N4 C26 C31 C30 -176.0(3) . . . . ? C29 C30 C31 C26 -0.3(5) . . . . ? C26 N4 C32 N5 -0.2(4) . . . . ? C25 N4 C32 N5 -177.8(3) . . . . ? C27 N5 C32 N4 0.4(4) . . . . ? C33 N5 C32 N4 170.2(3) . . . . ? C32 N5 C33 C34 -81.1(4) . . . . ? C27 N5 C33 C34 86.9(4) . . . . ? C35 N6 C34 C38 -2.3(6) . . . . ? C35 N6 C34 C33 179.0(4) . . . . ? N5 C33 C34 N6 41.4(5) . . . . ? N5 C33 C34 C38 -137.3(4) . . . . ? C34 N6 C35 C36 -0.3(8) . . . . ? N6 C35 C36 C37 2.3(9) . . . . ? C35 C36 C37 C38 -1.7(8) . . . . ? N6 C34 C38 C37 2.8(6) . . . . ? C33 C34 C38 C37 -178.6(4) . . . . ? C36 C37 C38 C34 -0.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.676 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.056 data_2a _database_code_depnum_ccdc_archive 'CCDC 775637' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 Cl6 N4 O2 Pd2 S2' _chemical_formula_weight 1062.46 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 8.8850(11) _cell_length_b 10.6269(13) _cell_length_c 13.0417(16) _cell_angle_alpha 78.793(2) _cell_angle_beta 80.799(2) _cell_angle_gamma 66.276(2) _cell_volume 1101.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3004 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 29.11 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 5682 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3893 _reflns_number_gt 3280 _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^)+(0.1110P)^2^+4.4272P] 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 contr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3868 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.003 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 Pd1 Pd -0.01620(5) 0.48098(5) 0.32167(4) 0.0361(2) Uani 1 1 d . . . Cl1 Cl -0.28746(18) 0.49264(18) 0.33658(14) 0.0459(4) Uani 1 1 d . . . Cl2 Cl -0.0714(2) 0.67083(19) 0.18915(14) 0.0498(4) Uani 1 1 d . . . Cl3 Cl 0.04815(19) 0.28195(16) 0.44866(15) 0.0470(4) Uani 1 1 d . . . S1 S 0.24776(19) 0.45909(17) 0.30190(13) 0.0395(4) Uani 1 1 d . . . O1 O 0.3459(7) 0.3764(8) 0.2215(6) 0.088(2) Uani 1 1 d . . . N1 N 0.7578(7) 0.8807(5) 0.8609(4) 0.0389(12) Uani 1 1 d . . . N2 N 0.5742(7) 1.0478(6) 0.7665(4) 0.0404(12) Uani 1 1 d . . . C1 C 1.1842(11) 0.6120(9) 0.9217(8) 0.072(3) Uani 1 1 d . . . H1A H 1.1697 0.6089 0.9965 0.107 Uiso 1 1 calc R . . H1B H 1.2940 0.6060 0.8963 0.107 Uiso 1 1 calc R . . H1C H 1.1673 0.5354 0.9039 0.107 Uiso 1 1 calc R . . C2 C 1.0606(10) 0.7469(9) 0.8717(8) 0.066(2) Uani 1 1 d . . . H2A H 1.0890 0.7593 0.7965 0.079 Uiso 1 1 calc R . . H2B H 1.0633 0.8241 0.8996 0.079 Uiso 1 1 calc R . . C3 C 0.8842(8) 0.7445(7) 0.8948(6) 0.0428(15) Uani 1 1 d . . . H3A H 0.8780 0.6755 0.8585 0.051 Uiso 1 1 calc R . . H3B H 0.8630 0.7180 0.9695 0.051 Uiso 1 1 calc R . . C4 C 0.6934(8) 0.9944(7) 0.9157(5) 0.0382(14) Uani 1 1 d . . . C5 C 0.7247(9) 1.0126(7) 1.0119(5) 0.0461(16) Uani 1 1 d . . . H5 H 0.8037 0.9427 1.0520 0.055 Uiso 1 1 calc R . . C6 C 0.6330(10) 1.1390(7) 1.0444(5) 0.0486(17) Uani 1 1 d . . . H6 H 0.6498 1.1549 1.1085 0.058 Uiso 1 1 calc R . . C7 C 0.5153(9) 1.2443(7) 0.9842(6) 0.0449(16) Uani 1 1 d . . . H7 H 0.4564 1.3285 1.0094 0.054 Uiso 1 1 calc R . . C8 C 0.4832(8) 1.2285(7) 0.8900(5) 0.0420(15) Uani 1 1 d . . . H8 H 0.4042 1.2991 0.8504 0.050 Uiso 1 1 calc R . . C9 C 0.5765(8) 1.0992(6) 0.8559(5) 0.0347(13) Uani 1 1 d . . . C10 C 0.6833(8) 0.9180(7) 0.7727(5) 0.0414(15) Uani 1 1 d . . . H10 H 0.7050 0.8606 0.7222 0.050 Uiso 1 1 calc R . . C11 C 0.4643(10) 1.1300(8) 0.6828(6) 0.057(2) Uani 1 1 d . . . H11A H 0.4834 1.2149 0.6577 0.068 Uiso 1 1 calc R . . H11B H 0.3506 1.1559 0.7128 0.068 Uiso 1 1 calc R . . C12 C 0.4877(8) 1.0552(6) 0.5905(5) 0.0398(15) Uani 1 1 d . . . C13 C 0.3752(9) 0.9974(7) 0.5800(5) 0.0436(15) Uani 1 1 d . . . C14 C 0.2395(12) 0.9944(12) 0.6661(7) 0.077(3) Uani 1 1 d . . . H14A H 0.2755 0.9898 0.7328 0.115 Uiso 1 1 calc R . . H14B H 0.2147 0.9143 0.6662 0.115 Uiso 1 1 calc R . . H14C H 0.1423 1.0770 0.6537 0.115 Uiso 1 1 calc R . . C15 C 0.6140(9) 1.0571(7) 0.5118(5) 0.0419(15) Uani 1 1 d . . . C16 C 0.7366(12) 1.1149(10) 0.5235(7) 0.068(2) Uani 1 1 d . . . H16A H 0.6867 1.2145 0.5121 0.102 Uiso 1 1 calc R . . H16B H 0.8301 1.0837 0.4731 0.102 Uiso 1 1 calc R . . H16C H 0.7721 1.0839 0.5931 0.102 Uiso 1 1 calc R . . C17 C 0.3456(12) 0.3928(13) 0.4191(8) 0.088(3) Uani 1 1 d . . . H17A H 0.3981 0.2935 0.4249 0.133 Uiso 1 1 calc R . . H17B H 0.2650 0.4178 0.4779 0.133 Uiso 1 1 calc R . . H17C H 0.4271 0.4310 0.4184 0.133 Uiso 1 1 calc R . . C18 C 0.2679(13) 0.6213(10) 0.2763(12) 0.101(4) Uani 1 1 d . . . H18A H 0.3372 0.6260 0.2124 0.151 Uiso 1 1 calc R . . H18B H 0.3164 0.6316 0.3332 0.151 Uiso 1 1 calc R . . H18C H 0.1609 0.6945 0.2694 0.151 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 Pd1 0.0325(3) 0.0353(3) 0.0391(3) -0.0033(2) -0.0068(2) -0.0110(2) Cl1 0.0255(7) 0.0544(10) 0.0566(10) -0.0040(8) -0.0067(7) -0.0149(7) Cl2 0.0419(9) 0.0517(10) 0.0438(9) 0.0118(8) -0.0141(7) -0.0103(7) Cl3 0.0346(8) 0.0316(8) 0.0639(11) 0.0269(7) -0.0127(7) -0.0136(6) S1 0.0342(8) 0.0441(9) 0.0417(9) -0.0067(7) -0.0061(7) -0.0154(7) O1 0.054(3) 0.135(6) 0.094(5) -0.075(5) 0.018(3) -0.038(4) N1 0.040(3) 0.036(3) 0.039(3) -0.007(2) -0.012(2) -0.008(2) N2 0.046(3) 0.039(3) 0.034(3) -0.007(2) -0.013(2) -0.009(2) C1 0.057(5) 0.058(5) 0.087(7) -0.018(5) -0.028(5) 0.003(4) C2 0.051(5) 0.057(5) 0.089(6) -0.019(5) -0.005(4) -0.016(4) C3 0.043(4) 0.038(3) 0.046(4) 0.000(3) -0.018(3) -0.011(3) C4 0.044(3) 0.038(3) 0.035(3) -0.004(3) -0.008(3) -0.017(3) C5 0.058(4) 0.050(4) 0.034(3) 0.004(3) -0.020(3) -0.023(3) C6 0.066(5) 0.052(4) 0.037(4) -0.007(3) -0.017(3) -0.027(4) C7 0.051(4) 0.039(3) 0.047(4) -0.015(3) -0.008(3) -0.014(3) C8 0.043(4) 0.041(3) 0.041(4) -0.005(3) -0.013(3) -0.012(3) C9 0.038(3) 0.039(3) 0.028(3) -0.005(3) -0.010(2) -0.013(3) C10 0.046(4) 0.044(4) 0.035(3) -0.009(3) -0.013(3) -0.011(3) C11 0.063(5) 0.050(4) 0.045(4) -0.015(3) -0.031(4) 0.004(4) C12 0.045(4) 0.036(3) 0.032(3) -0.003(3) -0.021(3) -0.003(3) C13 0.045(4) 0.046(4) 0.033(3) 0.003(3) -0.010(3) -0.013(3) C14 0.073(6) 0.108(8) 0.049(5) 0.003(5) 0.002(4) -0.045(6) C15 0.048(4) 0.037(3) 0.042(4) 0.005(3) -0.024(3) -0.015(3) C16 0.077(6) 0.070(5) 0.074(6) 0.006(4) -0.030(5) -0.044(5) C17 0.063(6) 0.134(9) 0.067(6) 0.027(6) -0.035(5) -0.045(6) C18 0.075(6) 0.066(6) 0.181(13) 0.020(7) -0.049(7) -0.051(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.2388(16) . ? Pd1 Cl2 2.3275(17) . ? Pd1 Cl1 2.3411(15) . ? Pd1 Cl3 2.3477(15) . ? S1 O1 1.443(6) . ? S1 C17 1.761(9) . ? S1 C18 1.766(9) . ? N1 C10 1.332(8) . ? N1 C4 1.395(8) . ? N1 C3 1.468(8) . ? N2 C10 1.324(8) . ? N2 C9 1.387(8) . ? N2 C11 1.481(8) . ? C1 C2 1.511(12) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.557(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.385(9) . ? C4 C5 1.393(9) . ? C5 C6 1.370(10) . ? C5 H5 0.9300 . ? C6 C7 1.393(10) . ? C6 H6 0.9300 . ? C7 C8 1.360(9) . ? C7 H7 0.9300 . ? C8 C9 1.405(9) . ? C8 H8 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.511(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C15 1.399(10) . ? C12 C13 1.402(10) . ? C13 C15 1.402(9) 2_676 ? C13 C14 1.517(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C13 1.402(9) 2_676 ? C15 C16 1.489(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pd1 Cl2 88.62(6) . . ? S1 Pd1 Cl1 176.53(6) . . ? Cl2 Pd1 Cl1 92.11(6) . . ? S1 Pd1 Cl3 90.16(6) . . ? Cl2 Pd1 Cl3 176.95(7) . . ? Cl1 Pd1 Cl3 88.95(6) . . ? O1 S1 C17 109.1(5) . . ? O1 S1 C18 109.2(6) . . ? C17 S1 C18 98.5(6) . . ? O1 S1 Pd1 113.2(3) . . ? C17 S1 Pd1 113.4(3) . . ? C18 S1 Pd1 112.4(4) . . ? C10 N1 C4 107.6(5) . . ? C10 N1 C3 126.3(5) . . ? C4 N1 C3 126.1(5) . . ? C10 N2 C9 107.8(5) . . ? C10 N2 C11 129.0(5) . . ? C9 N2 C11 123.2(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 109.7(8) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N1 C3 C2 111.4(6) . . ? N1 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C9 C4 C5 121.5(6) . . ? C9 C4 N1 106.4(5) . . ? C5 C4 N1 132.0(6) . . ? C6 C5 C4 116.5(6) . . ? C6 C5 H5 121.8 . . ? C4 C5 H5 121.8 . . ? C5 C6 C7 121.9(6) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 122.4(6) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C9 116.1(6) . . ? C7 C8 H8 121.9 . . ? C9 C8 H8 121.9 . . ? C4 C9 N2 107.2(5) . . ? C4 C9 C8 121.5(6) . . ? N2 C9 C8 131.3(6) . . ? N2 C10 N1 111.0(6) . . ? N2 C10 H10 124.5 . . ? N1 C10 H10 124.5 . . ? N2 C11 C12 114.2(5) . . ? N2 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N2 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C15 C12 C13 121.3(6) . . ? C15 C12 C11 118.2(7) . . ? C13 C12 C11 120.3(7) . . ? C12 C13 C15 120.0(6) . 2_676 ? C12 C13 C14 121.0(7) . . ? C15 C13 C14 119.0(7) 2_676 . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 C13 118.8(6) . 2_676 ? C12 C15 C16 121.6(7) . . ? C13 C15 C16 119.6(7) 2_676 . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S1 C17 H17A 109.5 . . ? S1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S1 C18 H18A 109.5 . . ? S1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Pd1 S1 O1 -86.5(4) . . . . ? Cl1 Pd1 S1 O1 15.6(12) . . . . ? Cl3 Pd1 S1 O1 90.7(4) . . . . ? Cl2 Pd1 S1 C17 148.5(5) . . . . ? Cl1 Pd1 S1 C17 -109.4(11) . . . . ? Cl3 Pd1 S1 C17 -34.3(5) . . . . ? Cl2 Pd1 S1 C18 37.8(6) . . . . ? Cl1 Pd1 S1 C18 139.9(11) . . . . ? Cl3 Pd1 S1 C18 -145.0(6) . . . . ? C10 N1 C3 C2 100.2(8) . . . . ? C4 N1 C3 C2 -80.1(9) . . . . ? C1 C2 C3 N1 171.8(7) . . . . ? C10 N1 C4 C9 0.7(7) . . . . ? C3 N1 C4 C9 -179.1(6) . . . . ? C10 N1 C4 C5 179.0(7) . . . . ? C3 N1 C4 C5 -0.7(12) . . . . ? C9 C4 C5 C6 0.5(10) . . . . ? N1 C4 C5 C6 -177.6(7) . . . . ? C4 C5 C6 C7 -0.4(11) . . . . ? C5 C6 C7 C8 0.3(12) . . . . ? C6 C7 C8 C9 -0.3(11) . . . . ? C5 C4 C9 N2 -179.3(6) . . . . ? N1 C4 C9 N2 -0.7(7) . . . . ? C5 C4 C9 C8 -0.5(10) . . . . ? N1 C4 C9 C8 178.1(6) . . . . ? C10 N2 C9 C4 0.5(8) . . . . ? C11 N2 C9 C4 -179.9(7) . . . . ? C10 N2 C9 C8 -178.1(7) . . . . ? C11 N2 C9 C8 1.4(12) . . . . ? C7 C8 C9 C4 0.3(10) . . . . ? C7 C8 C9 N2 178.8(7) . . . . ? C9 N2 C10 N1 -0.1(8) . . . . ? C11 N2 C10 N1 -179.6(7) . . . . ? C4 N1 C10 N2 -0.4(8) . . . . ? C3 N1 C10 N2 179.4(6) . . . . ? C10 N2 C11 C12 -3.0(12) . . . . ? C9 N2 C11 C12 177.6(6) . . . . ? N2 C11 C12 C15 -83.5(9) . . . . ? N2 C11 C12 C13 102.5(8) . . . . ? C15 C12 C13 C15 -1.4(10) . . . 2_676 ? C11 C12 C13 C15 172.3(6) . . . 2_676 ? C15 C12 C13 C14 179.4(7) . . . . ? C11 C12 C13 C14 -6.8(10) . . . . ? C13 C12 C15 C13 1.4(10) . . . 2_676 ? C11 C12 C15 C13 -172.5(6) . . . 2_676 ? C13 C12 C15 C16 -178.4(7) . . . . ? C11 C12 C15 C16 7.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.646 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.156