# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email tjnulqx@163.com _publ_contact_author_name 'Qingxiang Liu' _publ_author_name 'Qingxiang Liu' # Attachment '- complex 6.cif' data_n100824d _database_code_depnum_ccdc_archive 'CCDC 794736' #TrackingRef '- complex 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H40 Hg1.50 I3 N4' _chemical_formula_weight 1174.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.235(2) _cell_length_b 18.637(3) _cell_length_c 18.650(3) _cell_angle_alpha 109.493(3) _cell_angle_beta 104.117(2) _cell_angle_gamma 92.378(2) _cell_volume 3537.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2180 _exptl_absorpt_coefficient_mu 9.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.400 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17852 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12497 _reflns_number_gt 11091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+64.0387P] 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 12279 _refine_ls_number_parameters 758 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.059 _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 Hg3 Hg 0.03606(4) 0.19317(3) 0.84639(3) 0.02047(14) Uani 1 1 d . . . Hg2 Hg 0.67555(4) 0.89480(2) 0.76034(3) 0.01503(13) Uani 1 1 d . . . Hg1 Hg 0.03621(4) 0.60516(2) 0.29873(3) 0.01592(13) Uani 1 1 d . . . I1 I -0.07511(7) 0.45314(4) 0.29679(5) 0.02223(19) Uani 1 1 d . . . I2 I 0.51493(7) 0.81241(5) 0.59779(5) 0.0258(2) Uani 1 1 d . . . I3 I 0.11384(7) 0.13566(4) 0.70753(5) 0.02171(19) Uani 1 1 d . . . I4 I -0.12575(7) 0.29960(5) 0.82544(5) 0.02231(19) Uani 1 1 d . . . I5 I 0.24869(7) 0.25815(5) 0.97056(5) 0.02244(19) Uani 1 1 d . . . I6 I -0.10657(7) 0.08470(4) 0.87659(5) 0.02054(19) Uani 1 1 d . . . N1 N -0.2199(9) 0.6502(5) 0.2442(6) 0.017(2) Uani 1 1 d . . . N2 N -0.1520(9) 0.7034(5) 0.3729(6) 0.019(2) Uani 1 1 d . . . N3 N 0.3205(9) 0.5978(5) 0.3489(5) 0.0136(19) Uani 1 1 d U . . N4 N 0.2333(9) 0.5239(6) 0.2252(6) 0.017(2) Uani 1 1 d . . . N5 N 0.4467(9) 0.9693(5) 0.8025(6) 0.017(2) Uani 1 1 d . . . N6 N 0.5181(9) 0.9051(5) 0.8784(6) 0.016(2) Uani 1 1 d . . . N7 N 0.9148(9) 0.8186(5) 0.7333(6) 0.016(2) Uani 1 1 d . . . N8 N 0.8878(9) 0.9120(5) 0.6865(6) 0.017(2) Uani 1 1 d . . . C1 C -0.3156(10) 0.6867(6) 0.2706(7) 0.014(2) Uani 1 1 d U . . C2 C -0.2717(10) 0.7209(6) 0.3493(7) 0.015(2) Uani 1 1 d . . . C3 C -0.3434(11) 0.7635(7) 0.3984(9) 0.024(3) Uani 1 1 d . . . H3 H -0.3152 0.7854 0.4532 0.029 Uiso 1 1 calc R . . C4 C -0.4633(12) 0.7686(7) 0.3534(8) 0.023(3) Uani 1 1 d . . . H4 H -0.5149 0.7973 0.3805 0.028 Uiso 1 1 calc R . . C5 C -0.5068(11) 0.7345(7) 0.2740(9) 0.027(3) Uani 1 1 d . . . H5 H -0.5870 0.7391 0.2489 0.032 Uiso 1 1 calc R . . C6 C -0.4341(11) 0.6930(7) 0.2295(7) 0.020(2) Uani 1 1 d . . . H6 H -0.4627 0.6703 0.1747 0.024 Uiso 1 1 calc R . . C7 C -0.1226(10) 0.6607(6) 0.3056(8) 0.018(2) Uani 1 1 d . . . C8 C -0.2215(11) 0.6162(7) 0.1591(7) 0.018(2) Uani 1 1 d . . . H8A H -0.1367 0.6165 0.1556 0.021 Uiso 1 1 calc R . . H8B H -0.2609 0.6486 0.1316 0.021 Uiso 1 1 calc R . . C9 C -0.2882(11) 0.5349(7) 0.1172(8) 0.021(3) Uani 1 1 d . . . H9A H -0.2492 0.5016 0.1437 0.025 Uiso 1 1 calc R . . H9B H -0.3738 0.5338 0.1191 0.025 Uiso 1 1 calc R . . C10 C -0.2833(13) 0.5063(8) 0.0320(8) 0.029(3) Uani 1 1 d . . . H10A H -0.3204 0.5408 0.0066 0.035 Uiso 1 1 calc R . . H10B H -0.1973 0.5074 0.0309 0.035 Uiso 1 1 calc R . . C11 C -0.3495(14) 0.4257(9) -0.0145(10) 0.040(4) Uani 1 1 d . . . H11A H -0.3190 0.3921 0.0130 0.060 Uiso 1 1 calc R . . H11B H -0.3348 0.4082 -0.0658 0.060 Uiso 1 1 calc R . . H11C H -0.4368 0.4256 -0.0204 0.060 Uiso 1 1 calc R . . C12 C -0.0668(11) 0.7423(7) 0.4512(7) 0.018(2) Uani 1 1 d U . . H12A H -0.1125 0.7508 0.4905 0.021 Uiso 1 1 calc R . . H12B H -0.0324 0.7922 0.4541 0.021 Uiso 1 1 calc R . . C13 C 0.0373(11) 0.6983(7) 0.4706(7) 0.020(2) Uani 1 1 d . . . C14 C 0.1489(11) 0.7098(7) 0.4516(7) 0.020(3) Uani 1 1 d . . . C15 C 0.2377(11) 0.6601(6) 0.4598(7) 0.015(2) Uani 1 1 d U . . C16 C 0.2243(11) 0.6079(7) 0.4987(8) 0.024(3) Uani 1 1 d . . . C17 C 0.1154(11) 0.6017(7) 0.5212(7) 0.018(2) Uani 1 1 d U . . H17 H 0.1066 0.5686 0.5479 0.022 Uiso 1 1 calc R . . C18 C 0.0209(12) 0.6435(7) 0.5047(8) 0.024(3) Uani 1 1 d . . . C19 C 0.1764(12) 0.7733(7) 0.4220(8) 0.024(3) Uani 1 1 d . . . H19A H 0.1028 0.7965 0.4101 0.035 Uiso 1 1 calc R . . H19B H 0.2033 0.7524 0.3750 0.035 Uiso 1 1 calc R . . H19C H 0.2404 0.8115 0.4620 0.035 Uiso 1 1 calc R . . C20 C 0.3232(13) 0.5598(8) 0.5169(10) 0.036(3) Uani 1 1 d . . . H20A H 0.2993 0.5312 0.5466 0.053 Uiso 1 1 calc R . . H20B H 0.3998 0.5925 0.5473 0.053 Uiso 1 1 calc R . . H20C H 0.3337 0.5249 0.4683 0.053 Uiso 1 1 calc R . . C21 C -0.0977(12) 0.6290(9) 0.5248(8) 0.029(3) Uani 1 1 d . . . H21A H -0.0915 0.5894 0.5473 0.044 Uiso 1 1 calc R . . H21B H -0.1655 0.6131 0.4776 0.044 Uiso 1 1 calc R . . H21C H -0.1118 0.6754 0.5623 0.044 Uiso 1 1 calc R . . C22 C 0.3463(11) 0.6587(7) 0.4272(7) 0.020(2) Uani 1 1 d . . . H22A H 0.3653 0.7081 0.4228 0.024 Uiso 1 1 calc R . . H22B H 0.4179 0.6499 0.4629 0.024 Uiso 1 1 calc R . . C23 C 0.4141(11) 0.5617(7) 0.3185(9) 0.023(3) Uani 1 1 d . . . C24 C 0.3588(11) 0.5152(6) 0.2422(7) 0.016(2) Uani 1 1 d . . . C25 C 0.4251(13) 0.4695(7) 0.1908(9) 0.026(3) Uani 1 1 d . . . H25 H 0.3885 0.4392 0.1382 0.031 Uiso 1 1 calc R . . C26 C 0.5513(13) 0.4754(8) 0.2285(9) 0.028(3) Uani 1 1 d . . . H26 H 0.6001 0.4464 0.1992 0.033 Uiso 1 1 calc R . . C27 C 0.6097(12) 0.5225(7) 0.3082(8) 0.024(3) Uani 1 1 d . . . H27 H 0.6937 0.5232 0.3303 0.029 Uiso 1 1 calc R . . C28 C 0.5398(12) 0.5667(7) 0.3516(9) 0.028(3) Uani 1 1 d . . . H28 H 0.5767 0.5999 0.4031 0.033 Uiso 1 1 calc R . . C29 C 0.2120(11) 0.5739(6) 0.2900(7) 0.015(2) Uani 1 1 d . . . C30 C 0.1399(12) 0.4852(6) 0.1498(7) 0.018(2) Uani 1 1 d . . . H30A H 0.1735 0.4874 0.1072 0.022 Uiso 1 1 calc R . . H30B H 0.0684 0.5127 0.1485 0.022 Uiso 1 1 calc R . . C31 C 0.0981(10) 0.4016(6) 0.1354(7) 0.015(2) Uani 1 1 d U . . H31A H 0.1645 0.3714 0.1254 0.018 Uiso 1 1 calc R . . H31B H 0.0791 0.3978 0.1821 0.018 Uiso 1 1 calc R . . C32 C -0.0147(14) 0.3705(8) 0.0658(8) 0.032(3) Uani 1 1 d . . . H32A H 0.0077 0.3696 0.0184 0.038 Uiso 1 1 calc R . . H32B H -0.0766 0.4050 0.0733 0.038 Uiso 1 1 calc R . . C33 C -0.0708(14) 0.2907(8) 0.0534(9) 0.036(3) Uani 1 1 d . . . H33A H -0.0127 0.2553 0.0412 0.054 Uiso 1 1 calc R . . H33B H -0.1451 0.2754 0.0104 0.054 Uiso 1 1 calc R . . H33C H -0.0904 0.2906 0.1007 0.054 Uiso 1 1 calc R . . C34 C 0.3632(11) 0.9696(6) 0.8482(7) 0.015(2) Uani 1 1 d . . . C35 C 0.4080(11) 0.9291(7) 0.8957(8) 0.019(2) Uani 1 1 d . . . C36 C 0.3455(12) 0.9157(7) 0.9460(8) 0.023(3) Uani 1 1 d . . . H36 H 0.3777 0.8891 0.9790 0.028 Uiso 1 1 calc R . . C37 C 0.2323(13) 0.9434(8) 0.9455(8) 0.028(3) Uani 1 1 d . . . H37 H 0.1866 0.9344 0.9778 0.034 Uiso 1 1 calc R . . C38 C 0.1873(12) 0.9843(8) 0.8972(8) 0.026(3) Uani 1 1 d . . . H38 H 0.1119 1.0028 0.8984 0.031 Uiso 1 1 calc R . . C39 C 0.2512(11) 0.9991(7) 0.8465(8) 0.021(3) Uani 1 1 d . . . H39 H 0.2208 1.0266 0.8141 0.025 Uiso 1 1 calc R . . C40 C 0.5391(10) 0.9292(6) 0.8205(6) 0.012(2) Uani 1 1 d U . . C41 C 0.4419(10) 1.0109(6) 0.7477(7) 0.013(2) Uani 1 1 d U . . H41A H 0.3571 1.0190 0.7282 0.016 Uiso 1 1 calc R . . H41B H 0.4692 0.9804 0.7028 0.016 Uiso 1 1 calc R . . C42 C 0.5243(12) 1.0884(7) 0.7887(8) 0.024(3) Uani 1 1 d . . . H42A H 0.5218 1.1134 0.7504 0.029 Uiso 1 1 calc R . . H42B H 0.6090 1.0795 0.8067 0.029 Uiso 1 1 calc R . . C43 C 0.4869(12) 1.1435(7) 0.8605(9) 0.029(3) Uani 1 1 d . . . H43A H 0.4103 1.1618 0.8415 0.035 Uiso 1 1 calc R . . H43B H 0.4721 1.1153 0.8935 0.035 Uiso 1 1 calc R . . C44 C 0.5850(13) 1.2114(8) 0.9097(8) 0.029(3) Uani 1 1 d . . . H44A H 0.6529 1.1952 0.9404 0.044 Uiso 1 1 calc R . . H44B H 0.5505 1.2500 0.9444 0.044 Uiso 1 1 calc R . . H44C H 0.6142 1.2323 0.8755 0.044 Uiso 1 1 calc R . . C45 C 0.5929(11) 0.8585(7) 0.9165(7) 0.016(2) Uani 1 1 d U . . H45A H 0.5444 0.8361 0.9422 0.019 Uiso 1 1 calc R . . H45B H 0.6646 0.8910 0.9568 0.019 Uiso 1 1 calc R . . C46 C 0.6352(11) 0.7956(6) 0.8575(8) 0.022(3) Uani 1 1 d . . . C47 C 0.7552(11) 0.8015(7) 0.8486(7) 0.017(2) Uani 1 1 d U . . C48 C 0.7826(11) 0.7480(6) 0.7813(8) 0.020(3) Uani 1 1 d . . . C49 C 0.6936(12) 0.6879(7) 0.7303(8) 0.020(3) Uani 1 1 d . . . C50 C 0.5769(12) 0.6806(7) 0.7422(8) 0.022(3) Uani 1 1 d . . . H50 H 0.5191 0.6385 0.7081 0.026 Uiso 1 1 calc R . . C51 C 0.5450(10) 0.7347(6) 0.8037(6) 0.012(2) Uani 1 1 d U . . C52 C 0.8537(11) 0.8649(7) 0.9121(7) 0.022(3) Uani 1 1 d . . . H52A H 0.8225 0.9134 0.9214 0.033 Uiso 1 1 calc R . . H52B H 0.9269 0.8669 0.8946 0.033 Uiso 1 1 calc R . . H52C H 0.8735 0.8541 0.9602 0.033 Uiso 1 1 calc R . . C53 C 0.7145(14) 0.6295(8) 0.6558(10) 0.036(3) Uani 1 1 d . . . H53A H 0.7278 0.6553 0.6211 0.053 Uiso 1 1 calc R . . H53B H 0.6431 0.5912 0.6293 0.053 Uiso 1 1 calc R . . H53C H 0.7859 0.6054 0.6702 0.053 Uiso 1 1 calc R . . C54 C 0.4142(12) 0.7251(7) 0.8102(8) 0.025(3) Uani 1 1 d . . . H54A H 0.4165 0.7288 0.8631 0.038 Uiso 1 1 calc R . . H54B H 0.3721 0.6757 0.7738 0.038 Uiso 1 1 calc R . . H54C H 0.3709 0.7646 0.7978 0.038 Uiso 1 1 calc R . . C55 C 0.9063(11) 0.7602(7) 0.7701(8) 0.021(3) Uani 1 1 d . . . H55A H 0.9249 0.7120 0.7369 0.025 Uiso 1 1 calc R . . H55B H 0.9678 0.7764 0.8210 0.025 Uiso 1 1 calc R . . C56 C 1.0134(11) 0.8258(7) 0.7014(7) 0.017(2) Uani 1 1 d . . . C57 C 0.9955(11) 0.8843(7) 0.6710(7) 0.018(2) Uani 1 1 d . . . C58 C 1.0791(11) 0.9070(7) 0.6353(7) 0.016(2) Uani 1 1 d U . . H58 H 1.0670 0.9462 0.6150 0.020 Uiso 1 1 calc R . . C59 C 1.1806(11) 0.8676(7) 0.6322(7) 0.016(2) Uani 1 1 d U . . H59 H 1.2382 0.8800 0.6084 0.019 Uiso 1 1 calc R . . C60 C 1.1989(12) 0.8079(7) 0.6652(8) 0.026(3) Uani 1 1 d . . . H60 H 1.2705 0.7847 0.6650 0.032 Uiso 1 1 calc R . . C61 C 1.1142(11) 0.7847(7) 0.6966(7) 0.022(3) Uani 1 1 d . . . H61 H 1.1229 0.7434 0.7140 0.026 Uiso 1 1 calc R . . C62 C 0.8389(10) 0.8731(7) 0.7242(6) 0.015(2) Uani 1 1 d . . . C63 C 0.8329(11) 0.9735(7) 0.6630(6) 0.015(2) Uani 1 1 d . . . H63A H 0.7685 0.9890 0.6891 0.018 Uiso 1 1 calc R . . H63B H 0.8961 1.0176 0.6813 0.018 Uiso 1 1 calc R . . C64 C 0.7800(13) 0.9518(7) 0.5778(8) 0.025(3) Uani 1 1 d . . . H64A H 0.7174 0.9074 0.5590 0.030 Uiso 1 1 calc R . . H64B H 0.8445 0.9375 0.5514 0.030 Uiso 1 1 calc R . . C65 C 0.7218(15) 1.0172(8) 0.5562(11) 0.040(3) Uani 1 1 d U . . H65A H 0.6567 1.0307 0.5823 0.048 Uiso 1 1 calc R . . H65B H 0.7844 1.0618 0.5765 0.048 Uiso 1 1 calc R . . C66 C 0.6680(18) 0.9985(10) 0.4688(12) 0.054(4) Uani 1 1 d U . . H66A H 0.7297 0.9806 0.4418 0.081 Uiso 1 1 calc R . . H66B H 0.6420 1.0438 0.4594 0.081 Uiso 1 1 calc R . . H66C H 0.5981 0.9592 0.4495 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg3 0.0202(2) 0.0183(2) 0.0263(3) 0.0115(2) 0.0072(2) 0.00348(18) Hg2 0.0158(2) 0.0137(2) 0.0205(3) 0.00950(18) 0.00833(18) 0.00547(16) Hg1 0.0163(2) 0.0155(2) 0.0153(2) 0.00419(18) 0.00441(18) 0.00486(17) I1 0.0234(4) 0.0181(4) 0.0317(5) 0.0129(3) 0.0129(3) 0.0066(3) I2 0.0208(4) 0.0298(4) 0.0197(4) 0.0013(3) 0.0040(3) 0.0004(3) I3 0.0258(4) 0.0167(4) 0.0269(4) 0.0099(3) 0.0119(3) 0.0021(3) I4 0.0196(4) 0.0247(4) 0.0304(5) 0.0180(4) 0.0086(3) 0.0076(3) I5 0.0212(4) 0.0245(4) 0.0247(4) 0.0139(3) 0.0045(3) 0.0040(3) I6 0.0213(4) 0.0174(4) 0.0248(4) 0.0091(3) 0.0075(3) 0.0021(3) N1 0.020(5) 0.009(4) 0.017(5) 0.002(4) 0.004(4) 0.000(4) N2 0.012(5) 0.011(5) 0.030(6) 0.004(4) 0.003(4) 0.003(4) N3 0.019(4) 0.018(4) 0.006(3) 0.008(3) 0.003(3) 0.002(3) N4 0.021(5) 0.018(5) 0.014(5) 0.007(4) 0.005(4) 0.005(4) N5 0.015(5) 0.015(5) 0.020(5) 0.007(4) 0.003(4) 0.003(4) N6 0.020(5) 0.014(5) 0.014(5) 0.005(4) 0.006(4) 0.005(4) N7 0.013(5) 0.011(5) 0.025(5) 0.007(4) 0.005(4) 0.001(4) N8 0.021(5) 0.012(5) 0.024(5) 0.007(4) 0.013(4) 0.005(4) C1 0.015(2) 0.014(2) 0.014(2) 0.0056(12) 0.0040(11) 0.0016(10) C2 0.017(6) 0.013(5) 0.018(6) 0.010(5) 0.001(5) 0.001(4) C3 0.019(6) 0.013(6) 0.046(8) 0.010(6) 0.017(6) 0.004(5) C4 0.025(6) 0.023(6) 0.025(7) 0.006(5) 0.017(5) 0.008(5) C5 0.014(6) 0.024(7) 0.046(9) 0.019(6) 0.007(6) 0.007(5) C6 0.025(6) 0.024(6) 0.007(5) 0.007(5) -0.003(5) 0.000(5) C7 0.015(5) 0.013(5) 0.029(7) 0.012(5) 0.008(5) 0.001(4) C8 0.018(6) 0.015(6) 0.019(6) 0.005(5) 0.004(5) 0.000(5) C9 0.013(5) 0.016(6) 0.031(7) 0.007(5) 0.006(5) 0.003(4) C10 0.034(7) 0.023(7) 0.030(8) 0.007(6) 0.011(6) 0.010(6) C11 0.032(8) 0.034(8) 0.040(9) 0.002(7) 0.001(7) -0.002(6) C12 0.022(4) 0.021(4) 0.009(4) 0.005(3) 0.003(3) 0.004(3) C13 0.021(6) 0.016(6) 0.018(6) 0.001(5) 0.002(5) 0.000(5) C14 0.021(6) 0.013(5) 0.016(6) -0.004(5) 0.000(5) -0.003(5) C15 0.018(4) 0.017(4) 0.009(4) 0.007(3) 0.002(3) 0.001(3) C16 0.021(6) 0.012(6) 0.028(7) 0.001(5) 0.000(5) 0.000(5) C17 0.026(4) 0.020(4) 0.013(4) 0.012(3) 0.004(3) -0.001(3) C18 0.021(6) 0.012(6) 0.033(7) 0.001(5) 0.009(5) -0.003(5) C19 0.026(7) 0.026(7) 0.025(7) 0.012(5) 0.015(6) 0.001(5) C20 0.031(8) 0.027(7) 0.046(9) 0.015(7) 0.001(7) 0.007(6) C21 0.025(7) 0.043(8) 0.025(7) 0.018(6) 0.007(6) 0.000(6) C22 0.020(6) 0.020(6) 0.015(6) 0.003(5) 0.002(5) 0.001(5) C23 0.015(6) 0.016(6) 0.045(8) 0.014(6) 0.016(6) 0.006(5) C24 0.023(6) 0.016(6) 0.019(6) 0.011(5) 0.013(5) 0.006(5) C25 0.036(7) 0.020(6) 0.037(8) 0.014(6) 0.029(6) 0.011(5) C26 0.033(7) 0.027(7) 0.045(9) 0.026(6) 0.028(7) 0.015(6) C27 0.018(6) 0.027(7) 0.039(8) 0.023(6) 0.009(6) 0.006(5) C28 0.024(7) 0.019(6) 0.042(8) 0.017(6) 0.005(6) 0.001(5) C29 0.025(6) 0.014(5) 0.012(6) 0.011(5) 0.006(5) 0.002(4) C30 0.028(6) 0.016(6) 0.012(6) 0.007(5) 0.006(5) 0.005(5) C31 0.015(2) 0.015(2) 0.014(2) 0.0052(12) 0.0042(11) 0.0022(10) C32 0.039(8) 0.027(7) 0.024(7) 0.008(6) 0.000(6) 0.007(6) C33 0.036(8) 0.029(7) 0.031(8) 0.007(6) -0.006(6) 0.001(6) C34 0.018(6) 0.012(5) 0.012(6) -0.001(4) 0.007(5) 0.003(4) C35 0.022(6) 0.013(5) 0.025(7) 0.010(5) 0.009(5) 0.005(5) C36 0.030(7) 0.025(6) 0.026(7) 0.019(6) 0.009(6) 0.011(5) C37 0.029(7) 0.029(7) 0.032(8) 0.006(6) 0.021(6) 0.010(6) C38 0.024(7) 0.031(7) 0.025(7) 0.007(6) 0.013(6) 0.014(5) C39 0.020(6) 0.017(6) 0.024(7) 0.003(5) 0.007(5) 0.007(5) C40 0.012(2) 0.012(2) 0.012(2) 0.0044(10) 0.0033(9) 0.0018(8) C41 0.014(2) 0.014(2) 0.013(2) 0.0050(12) 0.0037(11) 0.0019(10) C42 0.024(6) 0.023(6) 0.030(7) 0.023(6) -0.004(5) 0.000(5) C43 0.025(7) 0.020(6) 0.043(9) 0.009(6) 0.013(6) 0.004(5) C44 0.038(8) 0.026(7) 0.023(7) 0.013(6) 0.002(6) 0.003(6) C45 0.021(4) 0.019(4) 0.011(4) 0.010(3) 0.003(3) 0.006(3) C46 0.022(6) 0.009(5) 0.044(8) 0.014(5) 0.017(6) 0.010(5) C47 0.017(3) 0.017(3) 0.018(3) 0.0067(13) 0.0044(12) 0.0024(10) C48 0.020(6) 0.009(5) 0.036(7) 0.012(5) 0.010(5) 0.006(4) C49 0.030(7) 0.017(6) 0.028(7) 0.019(5) 0.015(6) 0.013(5) C50 0.024(6) 0.018(6) 0.028(7) 0.014(5) 0.007(5) 0.000(5) C51 0.019(4) 0.014(4) 0.009(4) 0.008(3) 0.004(3) 0.005(3) C52 0.023(6) 0.026(6) 0.019(6) 0.016(5) -0.001(5) 0.004(5) C53 0.032(8) 0.024(7) 0.051(10) 0.007(7) 0.022(7) 0.007(6) C54 0.021(6) 0.022(6) 0.033(8) 0.008(6) 0.011(6) 0.004(5) C55 0.024(6) 0.023(6) 0.022(6) 0.014(5) 0.010(5) 0.010(5) C56 0.017(6) 0.018(6) 0.012(6) 0.004(5) 0.002(5) -0.003(4) C57 0.016(6) 0.019(6) 0.016(6) 0.002(5) 0.009(5) -0.004(5) C58 0.020(4) 0.018(4) 0.010(4) 0.004(3) 0.004(3) -0.002(3) C59 0.020(4) 0.021(4) 0.009(4) 0.004(3) 0.009(3) -0.002(3) C60 0.018(6) 0.020(6) 0.034(8) 0.003(6) 0.006(6) -0.002(5) C61 0.019(6) 0.019(6) 0.022(7) -0.001(5) 0.009(5) 0.004(5) C62 0.016(5) 0.019(6) 0.008(5) 0.009(5) -0.002(4) 0.001(4) C63 0.020(6) 0.020(6) 0.009(5) 0.010(5) 0.003(5) -0.001(5) C64 0.031(7) 0.020(6) 0.027(7) 0.011(5) 0.011(6) 0.002(5) C65 0.039(8) 0.025(7) 0.062(8) 0.026(7) 0.009(7) 0.005(6) C66 0.057(11) 0.037(9) 0.065(9) 0.027(9) 0.000(9) 0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg3 I5 2.7795(10) . ? Hg3 I4 2.8039(9) . ? Hg3 I6 2.8113(9) . ? Hg3 I3 2.8191(10) . ? Hg2 C40 2.112(11) . ? Hg2 C62 2.114(12) . ? Hg2 I2 2.9663(10) . ? Hg1 C7 2.109(11) . ? Hg1 C29 2.111(12) . ? Hg1 I1 3.0345(10) . ? N1 C7 1.329(16) . ? N1 C1 1.399(15) . ? N1 C8 1.495(15) . ? N2 C7 1.370(16) . ? N2 C2 1.397(15) . ? N2 C12 1.458(15) . ? N3 C29 1.366(15) . ? N3 C23 1.405(15) . ? N3 C22 1.472(15) . ? N4 C29 1.339(15) . ? N4 C24 1.397(16) . ? N4 C30 1.462(15) . ? N5 C40 1.346(14) . ? N5 C34 1.411(15) . ? N5 C41 1.469(15) . ? N6 C40 1.364(15) . ? N6 C35 1.406(15) . ? N6 C45 1.466(14) . ? N7 C62 1.380(15) . ? N7 C56 1.401(15) . ? N7 C55 1.479(15) . ? N8 C62 1.349(15) . ? N8 C57 1.392(15) . ? N8 C63 1.465(15) . ? C1 C2 1.342(17) . ? C1 C6 1.396(16) . ? C2 C3 1.429(17) . ? C3 C4 1.429(19) . ? C3 H3 0.9300 . ? C4 C5 1.35(2) . ? C4 H4 0.9300 . ? C5 C6 1.382(19) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.517(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.514(19) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.512(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.498(17) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.399(18) . ? C13 C14 1.411(18) . ? C14 C15 1.404(17) . ? C14 C19 1.514(17) . ? C15 C16 1.418(17) . ? C15 C22 1.487(16) . ? C16 C17 1.399(18) . ? C16 C20 1.502(18) . ? C17 C18 1.377(18) . ? C17 H17 0.9300 . ? C18 C21 1.506(18) . ? 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 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.365(19) . ? C23 C28 1.382(18) . ? C24 C25 1.433(16) . ? C25 C26 1.40(2) . ? C25 H25 0.9300 . ? C26 C27 1.42(2) . ? C26 H26 0.9300 . ? C27 C28 1.37(2) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C30 C31 1.523(15) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.504(17) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.51(2) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.365(17) . ? C34 C39 1.392(17) . ? C35 C36 1.378(18) . ? C36 C37 1.392(18) . ? C36 H36 0.9300 . ? C37 C38 1.38(2) . ? C37 H37 0.9300 . ? C38 C39 1.406(19) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C41 C42 1.527(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.55(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.508(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.501(16) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.403(17) . ? C46 C51 1.403(17) . ? C47 C48 1.429(17) . ? C47 C52 1.531(17) . ? C48 C49 1.375(18) . ? C48 C55 1.475(17) . ? C49 C50 1.390(18) . ? C49 C53 1.531(19) . ? C50 C51 1.385(17) . ? C50 H50 0.9300 . ? C51 C54 1.513(16) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.388(17) . ? C56 C61 1.398(17) . ? C57 C58 1.400(16) . ? C58 C59 1.384(17) . ? C58 H58 0.9300 . ? C59 C60 1.440(18) . ? C59 H59 0.9300 . ? C60 C61 1.356(19) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C63 C64 1.461(17) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.530(18) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.51(3) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 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 I5 Hg3 I4 113.21(3) . . ? I5 Hg3 I6 110.83(3) . . ? I4 Hg3 I6 103.78(3) . . ? I5 Hg3 I3 106.73(3) . . ? I4 Hg3 I3 107.27(3) . . ? I6 Hg3 I3 115.15(3) . . ? C40 Hg2 C62 167.7(4) . . ? C40 Hg2 I2 100.0(3) . . ? C62 Hg2 I2 92.3(3) . . ? C7 Hg1 C29 166.4(4) . . ? C7 Hg1 I1 96.3(3) . . ? C29 Hg1 I1 97.2(3) . . ? C7 N1 C1 109.5(10) . . ? C7 N1 C8 125.6(10) . . ? C1 N1 C8 124.1(10) . . ? C7 N2 C2 106.9(10) . . ? C7 N2 C12 127.1(10) . . ? C2 N2 C12 123.9(10) . . ? C29 N3 C23 108.0(10) . . ? C29 N3 C22 128.7(10) . . ? C23 N3 C22 122.8(10) . . ? C29 N4 C24 108.4(10) . . ? C29 N4 C30 125.3(10) . . ? C24 N4 C30 126.3(10) . . ? C40 N5 C34 109.9(10) . . ? C40 N5 C41 123.6(10) . . ? C34 N5 C41 126.3(9) . . ? C40 N6 C35 109.9(9) . . ? C40 N6 C45 127.0(10) . . ? C35 N6 C45 123.1(10) . . ? C62 N7 C56 108.7(9) . . ? C62 N7 C55 130.7(10) . . ? C56 N7 C55 120.6(9) . . ? C62 N8 C57 110.7(10) . . ? C62 N8 C63 124.5(10) . . ? C57 N8 C63 124.8(10) . . ? C2 C1 C6 122.3(11) . . ? C2 C1 N1 106.4(10) . . ? C6 C1 N1 131.3(11) . . ? C1 C2 N2 108.8(11) . . ? C1 C2 C3 123.2(11) . . ? N2 C2 C3 127.9(11) . . ? C4 C3 C2 112.2(12) . . ? C4 C3 H3 123.9 . . ? C2 C3 H3 123.9 . . ? C5 C4 C3 124.2(12) . . ? C5 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? C4 C5 C6 121.1(12) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 116.8(11) . . ? C5 C6 H6 121.6 . . ? C1 C6 H6 121.6 . . ? N1 C7 N2 108.3(10) . . ? N1 C7 Hg1 124.1(9) . . ? N2 C7 Hg1 126.9(9) . . ? N1 C8 C9 114.2(10) . . ? N1 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 109.6(11) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 113.1(12) . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? 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 113.3(10) . . ? N2 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N2 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C18 C13 C14 120.4(11) . . ? C18 C13 C12 119.4(11) . . ? C14 C13 C12 120.1(11) . . ? C15 C14 C13 118.9(11) . . ? C15 C14 C19 118.6(11) . . ? C13 C14 C19 122.5(11) . . ? C14 C15 C16 120.1(11) . . ? C14 C15 C22 122.2(10) . . ? C16 C15 C22 117.7(11) . . ? C17 C16 C15 118.5(11) . . ? C17 C16 C20 119.3(12) . . ? C15 C16 C20 122.2(12) . . ? C18 C17 C16 121.7(11) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C13 119.6(11) . . ? C17 C18 C21 118.6(12) . . ? C13 C18 C21 121.7(12) . . ? 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 . . ? 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 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C15 110.5(9) . . ? N3 C22 H22A 109.5 . . ? C15 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C28 121.2(12) . . ? C24 C23 N3 106.7(10) . . ? C28 C23 N3 132.1(13) . . ? C23 C24 N4 107.9(10) . . ? C23 C24 C25 123.4(12) . . ? N4 C24 C25 128.6(12) . . ? C26 C25 C24 112.7(13) . . ? C26 C25 H25 123.7 . . ? C24 C25 H25 123.7 . . ? C25 C26 C27 124.6(12) . . ? C25 C26 H26 117.7 . . ? C27 C26 H26 117.7 . . ? C28 C27 C26 118.5(12) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C23 119.6(14) . . ? C27 C28 H28 120.2 . . ? C23 C28 H28 120.2 . . ? N4 C29 N3 108.9(10) . . ? N4 C29 Hg1 124.5(9) . . ? N3 C29 Hg1 126.5(8) . . ? N4 C30 C31 113.5(9) . . ? N4 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? N4 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 110.3(10) . . ? C32 C31 H31A 109.6 . . ? C30 C31 H31A 109.6 . . ? C32 C31 H31B 109.6 . . ? C30 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C31 C32 C33 113.5(11) . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 122.5(11) . . ? C35 C34 N5 106.9(10) . . ? C39 C34 N5 130.5(11) . . ? C34 C35 C36 121.9(11) . . ? C34 C35 N6 106.5(10) . . ? C36 C35 N6 131.5(11) . . ? C35 C36 C37 117.4(12) . . ? C35 C36 H36 121.3 . . ? C37 C36 H36 121.3 . . ? C38 C37 C36 120.4(12) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 122.5(12) . . ? C37 C38 H38 118.7 . . ? C39 C38 H38 118.7 . . ? C34 C39 C38 115.2(12) . . ? C34 C39 H39 122.4 . . ? C38 C39 H39 122.4 . . ? N5 C40 N6 106.8(10) . . ? N5 C40 Hg2 127.2(8) . . ? N6 C40 Hg2 125.4(8) . . ? N5 C41 C42 110.8(9) . . ? N5 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? N5 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C41 C42 C43 114.2(11) . . ? C41 C42 H42A 108.7 . . ? C43 C42 H42A 108.7 . . ? C41 C42 H42B 108.7 . . ? C43 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C42 112.4(11) . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? C42 C43 H43B 109.1 . . ? H43A C43 H43B 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N6 C45 C46 111.2(10) . . ? N6 C45 H45A 109.4 . . ? C46 C45 H45A 109.4 . . ? N6 C45 H45B 109.4 . . ? C46 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C47 C46 C51 120.3(11) . . ? C47 C46 C45 121.9(11) . . ? C51 C46 C45 117.2(10) . . ? C46 C47 C48 119.4(11) . . ? C46 C47 C52 118.7(11) . . ? C48 C47 C52 121.9(11) . . ? C49 C48 C47 119.1(11) . . ? C49 C48 C55 123.1(12) . . ? C47 C48 C55 117.8(11) . . ? C48 C49 C50 120.7(12) . . ? C48 C49 C53 122.2(12) . . ? C50 C49 C53 117.0(12) . . ? C51 C50 C49 121.4(12) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C50 C51 C46 118.9(11) . . ? C50 C51 C54 118.3(11) . . ? C46 C51 C54 122.8(11) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 N7 112.2(10) . . ? C48 C55 H55A 109.2 . . ? N7 C55 H55A 109.2 . . ? C48 C55 H55B 109.2 . . ? N7 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C57 C56 C61 122.0(11) . . ? C57 C56 N7 107.3(10) . . ? C61 C56 N7 130.7(11) . . ? C56 C57 N8 106.3(10) . . ? C56 C57 C58 122.0(11) . . ? N8 C57 C58 131.7(11) . . ? C59 C58 C57 116.1(11) . . ? C59 C58 H58 122.0 . . ? C57 C58 H58 122.0 . . ? C58 C59 C60 121.2(11) . . ? C58 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? C61 C60 C59 121.7(12) . . ? C61 C60 H60 119.2 . . ? C59 C60 H60 119.2 . . ? C60 C61 C56 116.8(12) . . ? C60 C61 H61 121.6 . . ? C56 C61 H61 121.6 . . ? N8 C62 N7 107.1(10) . . ? N8 C62 Hg2 124.6(8) . . ? N7 C62 Hg2 128.4(8) . . ? C64 C63 N8 113.7(10) . . ? C64 C63 H63A 108.8 . . ? N8 C63 H63A 108.8 . . ? C64 C63 H63B 108.8 . . ? N8 C63 H63B 108.8 . . ? H63A C63 H63B 107.7 . . ? C63 C64 C65 111.9(12) . . ? C63 C64 H64A 109.2 . . ? C65 C64 H64A 109.2 . . ? C63 C64 H64B 109.2 . . ? C65 C64 H64B 109.2 . . ? H64A C64 H64B 107.9 . . ? C66 C65 C64 114.2(14) . . ? C66 C65 H65A 108.7 . . ? C64 C65 H65A 108.7 . . ? C66 C65 H65B 108.7 . . ? C64 C65 H65B 108.7 . . ? H65A C65 H65B 107.6 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 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 1.5(13) . . . . ? C8 N1 C1 C2 -169.3(10) . . . . ? C7 N1 C1 C6 179.1(12) . . . . ? C8 N1 C1 C6 8.2(19) . . . . ? C6 C1 C2 N2 179.5(10) . . . . ? N1 C1 C2 N2 -2.7(12) . . . . ? C6 C1 C2 C3 3.0(18) . . . . ? N1 C1 C2 C3 -179.1(10) . . . . ? C7 N2 C2 C1 2.9(12) . . . . ? C12 N2 C2 C1 167.5(10) . . . . ? C7 N2 C2 C3 179.1(11) . . . . ? C12 N2 C2 C3 -16.3(18) . . . . ? C1 C2 C3 C4 -3.1(16) . . . . ? N2 C2 C3 C4 -178.9(11) . . . . ? C2 C3 C4 C5 2.7(18) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C4 C5 C6 C1 1.5(18) . . . . ? C2 C1 C6 C5 -2.0(18) . . . . ? N1 C1 C6 C5 -179.2(12) . . . . ? C1 N1 C7 N2 0.3(12) . . . . ? C8 N1 C7 N2 170.9(10) . . . . ? C1 N1 C7 Hg1 171.6(7) . . . . ? C8 N1 C7 Hg1 -17.7(15) . . . . ? C2 N2 C7 N1 -1.9(12) . . . . ? C12 N2 C7 N1 -165.8(10) . . . . ? C2 N2 C7 Hg1 -172.9(8) . . . . ? C12 N2 C7 Hg1 23.1(16) . . . . ? C29 Hg1 C7 N1 97(2) . . . . ? I1 Hg1 C7 N1 -79.1(9) . . . . ? C29 Hg1 C7 N2 -94(2) . . . . ? I1 Hg1 C7 N2 90.6(9) . . . . ? C7 N1 C8 C9 105.8(12) . . . . ? C1 N1 C8 C9 -84.9(13) . . . . ? N1 C8 C9 C10 -179.6(10) . . . . ? C8 C9 C10 C11 -179.1(11) . . . . ? C7 N2 C12 C13 -36.8(16) . . . . ? C2 N2 C12 C13 161.7(11) . . . . ? N2 C12 C13 C18 -87.2(14) . . . . ? N2 C12 C13 C14 90.1(13) . . . . ? C18 C13 C14 C15 6.5(17) . . . . ? C12 C13 C14 C15 -170.8(10) . . . . ? C18 C13 C14 C19 -174.0(11) . . . . ? C12 C13 C14 C19 8.7(17) . . . . ? C13 C14 C15 C16 -10.4(17) . . . . ? C19 C14 C15 C16 170.1(11) . . . . ? C13 C14 C15 C22 168.3(11) . . . . ? C19 C14 C15 C22 -11.2(17) . . . . ? C14 C15 C16 C17 6.4(17) . . . . ? C22 C15 C16 C17 -172.3(11) . . . . ? C14 C15 C16 C20 -173.2(12) . . . . ? C22 C15 C16 C20 8.1(18) . . . . ? C15 C16 C17 C18 1.6(18) . . . . ? C20 C16 C17 C18 -178.8(12) . . . . ? C16 C17 C18 C13 -5.5(19) . . . . ? C16 C17 C18 C21 175.1(12) . . . . ? C14 C13 C18 C17 1.3(18) . . . . ? C12 C13 C18 C17 178.7(11) . . . . ? C14 C13 C18 C21 -179.2(12) . . . . ? C12 C13 C18 C21 -1.9(18) . . . . ? C29 N3 C22 C15 37.0(16) . . . . ? C23 N3 C22 C15 -153.0(10) . . . . ? C14 C15 C22 N3 -95.7(13) . . . . ? C16 C15 C22 N3 83.1(13) . . . . ? C29 N3 C23 C24 -1.5(12) . . . . ? C22 N3 C23 C24 -173.3(10) . . . . ? C29 N3 C23 C28 178.2(13) . . . . ? C22 N3 C23 C28 6(2) . . . . ? C28 C23 C24 N4 -178.3(11) . . . . ? N3 C23 C24 N4 1.4(13) . . . . ? C28 C23 C24 C25 -0.9(19) . . . . ? N3 C23 C24 C25 178.9(10) . . . . ? C29 N4 C24 C23 -0.8(13) . . . . ? C30 N4 C24 C23 179.4(10) . . . . ? C29 N4 C24 C25 -178.1(11) . . . . ? C30 N4 C24 C25 2.1(19) . . . . ? C23 C24 C25 C26 2.5(17) . . . . ? N4 C24 C25 C26 179.5(11) . . . . ? C24 C25 C26 C27 -1.4(17) . . . . ? C25 C26 C27 C28 -1.3(19) . . . . ? C26 C27 C28 C23 3.2(18) . . . . ? C24 C23 C28 C27 -2.2(19) . . . . ? N3 C23 C28 C27 178.2(12) . . . . ? C24 N4 C29 N3 -0.1(12) . . . . ? C30 N4 C29 N3 179.6(10) . . . . ? C24 N4 C29 Hg1 -177.6(7) . . . . ? C30 N4 C29 Hg1 2.2(15) . . . . ? C23 N3 C29 N4 1.0(12) . . . . ? C22 N3 C29 N4 172.2(10) . . . . ? C23 N3 C29 Hg1 178.4(8) . . . . ? C22 N3 C29 Hg1 -10.5(16) . . . . ? C7 Hg1 C29 N4 -106(2) . . . . ? I1 Hg1 C29 N4 70.1(9) . . . . ? C7 Hg1 C29 N3 77(2) . . . . ? I1 Hg1 C29 N3 -106.9(9) . . . . ? C29 N4 C30 C31 -103.5(13) . . . . ? C24 N4 C30 C31 76.2(14) . . . . ? N4 C30 C31 C32 168.6(11) . . . . ? C30 C31 C32 C33 -173.3(12) . . . . ? C40 N5 C34 C35 0.8(13) . . . . ? C41 N5 C34 C35 -174.7(10) . . . . ? C40 N5 C34 C39 -175.5(12) . . . . ? C41 N5 C34 C39 9.1(19) . . . . ? C39 C34 C35 C36 -0.8(19) . . . . ? N5 C34 C35 C36 -177.4(11) . . . . ? C39 C34 C35 N6 176.8(11) . . . . ? N5 C34 C35 N6 0.2(13) . . . . ? C40 N6 C35 C34 -1.1(13) . . . . ? C45 N6 C35 C34 -178.8(10) . . . . ? C40 N6 C35 C36 176.2(13) . . . . ? C45 N6 C35 C36 -1(2) . . . . ? C34 C35 C36 C37 2(2) . . . . ? N6 C35 C36 C37 -175.4(13) . . . . ? C35 C36 C37 C38 -1(2) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C35 C34 C39 C38 0.0(18) . . . . ? N5 C34 C39 C38 175.7(12) . . . . ? C37 C38 C39 C34 0.0(19) . . . . ? C34 N5 C40 N6 -1.4(12) . . . . ? C41 N5 C40 N6 174.2(10) . . . . ? C34 N5 C40 Hg2 170.1(8) . . . . ? C41 N5 C40 Hg2 -14.3(15) . . . . ? C35 N6 C40 N5 1.5(13) . . . . ? C45 N6 C40 N5 179.1(10) . . . . ? C35 N6 C40 Hg2 -170.1(8) . . . . ? C45 N6 C40 Hg2 7.5(16) . . . . ? C62 Hg2 C40 N5 124.2(19) . . . . ? I2 Hg2 C40 N5 -54.4(10) . . . . ? C62 Hg2 C40 N6 -66(2) . . . . ? I2 Hg2 C40 N6 115.5(9) . . . . ? C40 N5 C41 C42 -80.3(13) . . . . ? C34 N5 C41 C42 94.6(13) . . . . ? N5 C41 C42 C43 -60.8(13) . . . . ? C41 C42 C43 C44 167.6(11) . . . . ? C40 N6 C45 C46 -40.7(16) . . . . ? C35 N6 C45 C46 136.6(11) . . . . ? N6 C45 C46 C47 100.4(14) . . . . ? N6 C45 C46 C51 -70.9(13) . . . . ? C51 C46 C47 C48 4.1(17) . . . . ? C45 C46 C47 C48 -167.1(11) . . . . ? C51 C46 C47 C52 -175.1(10) . . . . ? C45 C46 C47 C52 13.8(17) . . . . ? C46 C47 C48 C49 -5.4(17) . . . . ? C52 C47 C48 C49 173.7(11) . . . . ? C46 C47 C48 C55 174.6(11) . . . . ? C52 C47 C48 C55 -6.2(17) . . . . ? C47 C48 C49 C50 2.3(17) . . . . ? C55 C48 C49 C50 -177.8(11) . . . . ? C47 C48 C49 C53 178.2(12) . . . . ? C55 C48 C49 C53 -1.8(18) . . . . ? C48 C49 C50 C51 2.3(18) . . . . ? C53 C49 C50 C51 -173.8(11) . . . . ? C49 C50 C51 C46 -3.7(17) . . . . ? C49 C50 C51 C54 176.8(11) . . . . ? C47 C46 C51 C50 0.5(17) . . . . ? C45 C46 C51 C50 172.0(10) . . . . ? C47 C46 C51 C54 179.9(11) . . . . ? C45 C46 C51 C54 -8.5(17) . . . . ? C49 C48 C55 N7 99.1(13) . . . . ? C47 C48 C55 N7 -81.0(14) . . . . ? C62 N7 C55 C48 15.8(18) . . . . ? C56 N7 C55 C48 -165.3(11) . . . . ? C62 N7 C56 C57 -1.3(13) . . . . ? C55 N7 C56 C57 179.5(10) . . . . ? C62 N7 C56 C61 179.7(12) . . . . ? C55 N7 C56 C61 0.5(19) . . . . ? C61 C56 C57 N8 -179.8(11) . . . . ? N7 C56 C57 N8 1.1(13) . . . . ? C61 C56 C57 C58 -1.7(18) . . . . ? N7 C56 C57 C58 179.2(11) . . . . ? C62 N8 C57 C56 -0.5(13) . . . . ? C63 N8 C57 C56 -178.8(10) . . . . ? C62 N8 C57 C58 -178.4(12) . . . . ? C63 N8 C57 C58 3(2) . . . . ? C56 C57 C58 C59 0.0(17) . . . . ? N8 C57 C58 C59 177.6(12) . . . . ? C57 C58 C59 C60 -1.0(17) . . . . ? C58 C59 C60 C61 3.8(19) . . . . ? C59 C60 C61 C56 -5.2(18) . . . . ? C57 C56 C61 C60 4.2(18) . . . . ? N7 C56 C61 C60 -176.9(12) . . . . ? C57 N8 C62 N7 -0.3(13) . . . . ? C63 N8 C62 N7 178.0(10) . . . . ? C57 N8 C62 Hg2 179.8(8) . . . . ? C63 N8 C62 Hg2 -1.9(16) . . . . ? C56 N7 C62 N8 1.0(12) . . . . ? C55 N7 C62 N8 -179.9(11) . . . . ? C56 N7 C62 Hg2 -179.1(8) . . . . ? C55 N7 C62 Hg2 -0.1(18) . . . . ? C40 Hg2 C62 N8 -101(2) . . . . ? I2 Hg2 C62 N8 78.1(9) . . . . ? C40 Hg2 C62 N7 80(2) . . . . ? I2 Hg2 C62 N7 -101.7(10) . . . . ? C62 N8 C63 C64 -108.7(13) . . . . ? C57 N8 C63 C64 69.4(15) . . . . ? N8 C63 C64 C65 179.0(11) . . . . ? C63 C64 C65 C66 178.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.992 _refine_diff_density_min -3.869 _refine_diff_density_rms 0.413 # Attachment '- complex 7.cif' data_090319a _database_code_depnum_ccdc_archive 'CCDC 794737' #TrackingRef '- complex 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38.50 Br4 Hg2 N7.50' _chemical_formula_weight 1345.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 15.9630(11) _cell_length_b 15.4870(10) _cell_length_c 34.670(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.6010(10) _cell_angle_gamma 90.00 _cell_volume 8451.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6524 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.22 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5048 _exptl_absorpt_coefficient_mu 11.079 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.063 _exptl_absorpt_correction_T_max 0.087 _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 21420 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7465 _reflns_number_gt 5797 _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^)+(0.0398P)^2^+64.5414P] 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 7461 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.005 _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 0.840456(17) 0.366756(17) 0.624824(7) 0.02877(9) Uani 1 1 d . . . Hg2 Hg 0.62764(2) 0.13705(2) 0.649612(9) 0.04506(10) Uani 1 1 d . . . Br1 Br 0.66481(5) 0.29276(5) 0.61809(2) 0.0456(2) Uani 1 1 d . . . Br2 Br 0.59053(6) 0.17778(7) 0.71651(2) 0.0605(3) Uani 1 1 d . . . Br3 Br 0.48777(6) 0.08896(7) 0.60460(2) 0.0652(3) Uani 1 1 d . . . Br4 Br 0.74663(8) 0.02800(8) 0.64577(3) 0.0867(4) Uani 1 1 d . . . N1 N 0.8868(4) 0.3484(4) 0.55129(18) 0.0396(15) Uani 1 1 d . . . N2 N 0.8885(4) 0.1906(3) 0.59604(15) 0.0295(13) Uani 1 1 d . . . N3 N 0.9548(4) 0.2075(4) 0.65567(14) 0.0292(13) Uani 1 1 d . . . N4 N 0.8130(3) 0.5507(3) 0.65514(15) 0.0271(12) Uani 1 1 d . . . N5 N 0.7419(4) 0.5324(3) 0.59642(15) 0.0281(13) Uani 1 1 d . . . N6 N 0.7262(4) 0.4804(4) 0.49217(17) 0.0460(17) Uani 1 1 d . . . C1 C 0.8838(5) 0.2516(5) 0.4979(2) 0.0448(19) Uani 1 1 d . . . H1 H 0.8702 0.1972 0.4873 0.054 Uiso 1 1 calc R . . C2 C 0.9197(6) 0.3128(6) 0.4772(2) 0.058(2) Uani 1 1 d . . . H2 H 0.9301 0.3010 0.4522 0.069 Uiso 1 1 calc R . . C3 C 0.9399(6) 0.3911(6) 0.4940(3) 0.059(2) Uani 1 1 d . . . H3 H 0.9645 0.4336 0.4805 0.071 Uiso 1 1 calc R . . C4 C 0.9236(6) 0.4065(6) 0.5310(2) 0.054(2) Uani 1 1 d . . . H4 H 0.9388 0.4598 0.5424 0.065 Uiso 1 1 calc R . . C5 C 0.8684(4) 0.2722(4) 0.53476(18) 0.0309(16) Uani 1 1 d . . . C6 C 0.8310(4) 0.2074(4) 0.55918(18) 0.0312(16) Uani 1 1 d . . . H6A H 0.7772 0.2289 0.5648 0.037 Uiso 1 1 calc R . . H6B H 0.8201 0.1539 0.5447 0.037 Uiso 1 1 calc R . . C7 C 0.9421(4) 0.1197(4) 0.6041(2) 0.0312(16) Uani 1 1 d . . . C8 C 0.9570(5) 0.0498(5) 0.5813(2) 0.0364(17) Uani 1 1 d . . . H8 H 0.9289 0.0431 0.5557 0.044 Uiso 1 1 calc R . . C9 C 1.0160(5) -0.0093(5) 0.5987(2) 0.0417(19) Uani 1 1 d . . . H9 H 1.0292 -0.0567 0.5844 0.050 Uiso 1 1 calc R . . C10 C 1.0568(5) 0.0007(5) 0.6376(2) 0.046(2) Uani 1 1 d . . . H10 H 1.0948 -0.0415 0.6486 0.055 Uiso 1 1 calc R . . C11 C 1.0422(5) 0.0709(5) 0.6600(2) 0.0390(18) Uani 1 1 d . . . H11 H 1.0698 0.0777 0.6856 0.047 Uiso 1 1 calc R . . C12 C 0.9833(4) 0.1312(4) 0.64176(19) 0.0291(15) Uani 1 1 d . . . C13 C 0.8978(4) 0.2438(4) 0.62715(18) 0.0289(15) Uani 1 1 d . . . C14 C 0.9846(5) 0.2388(5) 0.69581(19) 0.0349(17) Uani 1 1 d . . . H14A H 1.0406 0.2642 0.6971 0.042 Uiso 1 1 calc R . . H14B H 0.9897 0.1901 0.7137 0.042 Uiso 1 1 calc R . . C15 C 0.9261(4) 0.3041(4) 0.70851(17) 0.0279(15) Uani 1 1 d . . . C16 C 0.9387(4) 0.3923(5) 0.70184(17) 0.0292(15) Uani 1 1 d . . . C17 C 0.8751(4) 0.4505(4) 0.70687(17) 0.0306(16) Uani 1 1 d . . . C18 C 0.8046(5) 0.4232(4) 0.72326(18) 0.0329(16) Uani 1 1 d . . . C19 C 0.7970(5) 0.3363(5) 0.73157(19) 0.0346(16) Uani 1 1 d . . . H19 H 0.7515 0.3182 0.7432 0.041 Uiso 1 1 calc R . . C20 C 0.8549(4) 0.2758(4) 0.72317(18) 0.0305(16) Uani 1 1 d . . . C21 C 0.8378(5) 0.1815(5) 0.7293(2) 0.048(2) Uani 1 1 d . . . H21A H 0.7845 0.1754 0.7384 0.072 Uiso 1 1 calc R . . H21B H 0.8825 0.1579 0.7483 0.072 Uiso 1 1 calc R . . H21C H 0.8353 0.1511 0.7050 0.072 Uiso 1 1 calc R . . C22 C 1.0191(5) 0.4219(5) 0.6883(2) 0.0423(19) Uani 1 1 d . . . H22A H 1.0100 0.4244 0.6603 0.063 Uiso 1 1 calc R . . H22B H 1.0641 0.3820 0.6973 0.063 Uiso 1 1 calc R . . H22C H 1.0344 0.4782 0.6988 0.063 Uiso 1 1 calc R . . C23 C 0.7366(5) 0.4847(5) 0.7316(2) 0.050(2) Uani 1 1 d . . . H23A H 0.6929 0.4531 0.7414 0.074 Uiso 1 1 calc R . . H23B H 0.7126 0.5140 0.7079 0.074 Uiso 1 1 calc R . . H23C H 0.7611 0.5263 0.7507 0.074 Uiso 1 1 calc R . . C24 C 0.8753(5) 0.5416(4) 0.69169(19) 0.0345(17) Uani 1 1 d . . . H24A H 0.8611 0.5813 0.7113 0.041 Uiso 1 1 calc R . . H24B H 0.9316 0.5560 0.6867 0.041 Uiso 1 1 calc R . . C25 C 0.7975(4) 0.4943(4) 0.62545(18) 0.0262(14) Uani 1 1 d . . . C26 C 0.7667(5) 0.6268(4) 0.6458(2) 0.0333(16) Uani 1 1 d . . . C27 C 0.7593(5) 0.7012(5) 0.6666(2) 0.047(2) Uani 1 1 d . . . H27 H 0.7907 0.7100 0.6914 0.056 Uiso 1 1 calc R . . C28 C 0.7024(6) 0.7623(5) 0.6486(3) 0.055(2) Uani 1 1 d . . . H28 H 0.6960 0.8138 0.6615 0.066 Uiso 1 1 calc R . . C29 C 0.6550(6) 0.7492(5) 0.6119(3) 0.052(2) Uani 1 1 d . . . H29 H 0.6159 0.7910 0.6015 0.062 Uiso 1 1 calc R . . C30 C 0.6640(5) 0.6751(5) 0.5902(2) 0.0447(19) Uani 1 1 d . . . H30 H 0.6342 0.6674 0.5650 0.054 Uiso 1 1 calc R . . C31 C 0.7199(4) 0.6138(4) 0.6084(2) 0.0307(16) Uani 1 1 d . . . C32 C 0.7086(4) 0.4944(5) 0.55902(18) 0.0324(16) Uani 1 1 d . . . H32A H 0.6479 0.5054 0.5533 0.039 Uiso 1 1 calc R . . H32B H 0.7165 0.4324 0.5610 0.039 Uiso 1 1 calc R . . C33 C 0.7485(5) 0.5270(5) 0.52495(19) 0.0358(17) Uani 1 1 d . . . C34 C 0.8008(5) 0.5976(5) 0.5273(2) 0.0421(18) Uani 1 1 d . . . H34 H 0.8141 0.6286 0.5505 0.051 Uiso 1 1 calc R . . C35 C 0.8337(6) 0.6222(6) 0.4938(3) 0.060(2) Uani 1 1 d . . . H35 H 0.8697 0.6695 0.4944 0.072 Uiso 1 1 calc R . . C36 C 0.8117(6) 0.5752(7) 0.4606(2) 0.067(3) Uani 1 1 d . . . H36 H 0.8321 0.5900 0.4379 0.081 Uiso 1 1 calc R . . C37 C 0.7594(6) 0.5059(6) 0.4611(2) 0.064(3) Uani 1 1 d . . . H37 H 0.7457 0.4740 0.4382 0.077 Uiso 1 1 calc R . . N7 N 0.9176(12) 0.8463(12) 0.5177(5) 0.162(8) Uani 1 1 d . . . C38 C 0.9021(10) 0.8285(11) 0.5490(7) 0.115(7) Uani 1 1 d . . . C39 C 0.8866(13) 0.8123(11) 0.5870(8) 0.170(9) Uani 1 1 d . . . H39A H 0.9355 0.7852 0.6020 0.255 Uiso 1 1 calc R . . H39B H 0.8383 0.7748 0.5858 0.255 Uiso 1 1 calc R . . H39C H 0.8754 0.8658 0.5991 0.255 Uiso 1 1 calc R . . N8 N 0.0000 1.0175(11) 0.7500 0.094(4) Uani 1 2 d S . . C40 C 0.0227(16) 0.9565(15) 0.7654(7) 0.079(7) Uani 0.50 1 d P . . C41 C 0.057(2) 0.8767(17) 0.7899(10) 0.132(12) Uani 0.50 1 d P . . H41A H 0.1085 0.8924 0.8074 0.198 Uiso 0.50 1 calc PR . . H41B H 0.0699 0.8315 0.7728 0.198 Uiso 0.50 1 calc PR . . H41C H 0.0157 0.8569 0.8049 0.198 Uiso 0.50 1 calc PR . . 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 0.03585(16) 0.02491(15) 0.02404(13) -0.00284(11) 0.00056(10) 0.00473(12) Hg2 0.04543(19) 0.0480(2) 0.04185(17) 0.00014(14) 0.00757(14) -0.00816(15) Br1 0.0435(4) 0.0345(4) 0.0613(5) 0.0015(4) 0.0159(4) -0.0061(4) Br2 0.0638(6) 0.0780(7) 0.0426(4) -0.0046(4) 0.0176(4) -0.0054(5) Br3 0.0582(5) 0.0948(8) 0.0397(4) 0.0073(5) -0.0001(4) -0.0350(5) Br4 0.0989(9) 0.0913(9) 0.0690(7) -0.0184(6) 0.0113(6) 0.0280(7) N1 0.055(4) 0.028(4) 0.039(3) -0.003(3) 0.018(3) -0.009(3) N2 0.036(3) 0.026(3) 0.025(3) -0.002(2) 0.001(2) 0.004(3) N3 0.035(3) 0.028(3) 0.023(3) -0.005(2) 0.001(2) 0.008(3) N4 0.032(3) 0.022(3) 0.028(3) -0.002(2) 0.006(2) 0.003(2) N5 0.038(3) 0.021(3) 0.024(3) 0.003(2) 0.000(2) -0.002(2) N6 0.057(4) 0.049(4) 0.032(3) -0.007(3) 0.006(3) -0.019(3) C1 0.056(5) 0.047(5) 0.031(4) -0.011(3) 0.004(4) -0.007(4) C2 0.066(6) 0.072(7) 0.039(4) -0.002(4) 0.020(4) -0.006(5) C3 0.072(6) 0.058(6) 0.052(5) 0.010(4) 0.024(5) -0.011(5) C4 0.071(6) 0.040(5) 0.054(5) 0.000(4) 0.020(5) -0.010(5) C5 0.031(4) 0.032(4) 0.028(3) -0.003(3) -0.002(3) 0.001(3) C6 0.037(4) 0.028(4) 0.027(3) -0.006(3) 0.000(3) 0.003(3) C7 0.028(4) 0.029(4) 0.038(4) 0.002(3) 0.007(3) 0.002(3) C8 0.037(4) 0.034(4) 0.039(4) -0.009(3) 0.009(3) -0.005(3) C9 0.037(4) 0.034(4) 0.057(5) -0.013(4) 0.015(4) 0.002(4) C10 0.037(4) 0.033(5) 0.068(5) 0.001(4) 0.008(4) 0.012(4) C11 0.035(4) 0.041(5) 0.039(4) -0.002(3) 0.001(3) 0.010(3) C12 0.027(4) 0.026(4) 0.035(4) -0.003(3) 0.007(3) 0.000(3) C13 0.033(4) 0.025(4) 0.028(3) -0.001(3) 0.002(3) 0.003(3) C14 0.041(4) 0.036(4) 0.025(3) -0.006(3) 0.000(3) 0.005(3) C15 0.032(4) 0.034(4) 0.016(3) -0.001(3) -0.004(3) 0.004(3) C16 0.032(4) 0.038(4) 0.015(3) 0.002(3) -0.003(3) 0.002(3) C17 0.040(4) 0.033(4) 0.018(3) 0.000(3) 0.002(3) -0.003(3) C18 0.040(4) 0.032(4) 0.025(3) -0.004(3) 0.001(3) 0.001(3) C19 0.033(4) 0.041(4) 0.031(4) -0.002(3) 0.008(3) -0.004(3) C20 0.034(4) 0.032(4) 0.023(3) 0.000(3) -0.004(3) -0.005(3) C21 0.058(5) 0.034(5) 0.048(5) 0.007(4) -0.002(4) -0.009(4) C22 0.033(4) 0.048(5) 0.045(4) 0.005(4) 0.004(3) -0.008(4) C23 0.050(5) 0.047(5) 0.054(5) -0.002(4) 0.016(4) 0.009(4) C24 0.047(4) 0.027(4) 0.027(3) -0.005(3) 0.001(3) -0.007(3) C25 0.028(4) 0.023(4) 0.028(3) -0.001(3) 0.007(3) -0.002(3) C26 0.042(4) 0.024(4) 0.036(4) 0.003(3) 0.014(3) 0.005(3) C27 0.062(5) 0.032(5) 0.048(4) -0.004(4) 0.014(4) 0.003(4) C28 0.076(6) 0.031(5) 0.066(6) 0.000(4) 0.029(5) 0.005(4) C29 0.060(6) 0.031(5) 0.068(6) 0.021(4) 0.019(5) 0.015(4) C30 0.047(5) 0.040(5) 0.047(4) 0.015(4) 0.011(4) 0.006(4) C31 0.033(4) 0.021(4) 0.040(4) 0.003(3) 0.010(3) 0.001(3) C32 0.034(4) 0.036(4) 0.026(3) 0.002(3) 0.003(3) -0.001(3) C33 0.042(4) 0.037(4) 0.026(3) 0.007(3) -0.002(3) -0.003(3) C34 0.043(4) 0.042(5) 0.039(4) -0.003(4) 0.002(3) -0.012(4) C35 0.063(6) 0.057(6) 0.062(6) 0.004(5) 0.019(5) -0.022(5) C36 0.085(7) 0.083(7) 0.035(4) 0.010(5) 0.014(5) -0.031(6) C37 0.083(7) 0.076(7) 0.036(4) -0.007(4) 0.017(5) -0.035(6) N7 0.148(14) 0.174(16) 0.148(14) -0.071(13) -0.019(12) 0.070(11) C38 0.071(9) 0.077(11) 0.182(19) -0.056(14) -0.017(13) 0.002(8) C39 0.144(17) 0.076(11) 0.30(3) -0.002(16) 0.06(2) -0.029(10) N8 0.111(13) 0.086(12) 0.089(10) 0.000 0.033(9) 0.000 C40 0.080(19) 0.059(14) 0.11(2) -0.006(12) 0.033(14) -0.008(12) C41 0.15(3) 0.08(2) 0.18(3) -0.02(2) 0.08(3) -0.019(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C25 2.093(6) . ? Hg1 C13 2.108(7) . ? Hg1 Br1 3.0018(9) . ? Hg2 Br4 2.5617(12) . ? Hg2 Br2 2.5666(9) . ? Hg2 Br3 2.6102(9) . ? Hg2 Br1 2.7527(8) . ? N1 C5 1.324(9) . ? N1 C4 1.338(10) . ? N2 C13 1.346(8) . ? N2 C7 1.392(8) . ? N2 C6 1.467(8) . ? N3 C13 1.349(8) . ? N3 C12 1.383(8) . ? N3 C14 1.475(8) . ? N4 C25 1.341(8) . ? N4 C26 1.400(8) . ? N4 C24 1.482(8) . ? N5 C25 1.361(8) . ? N5 C31 1.391(8) . ? N5 C32 1.442(8) . ? N6 C37 1.336(10) . ? N6 C33 1.344(9) . ? C1 C2 1.371(12) . ? C1 C5 1.377(10) . ? C1 H1 0.9300 . ? C2 C3 1.360(13) . ? C2 H2 0.9300 . ? C3 C4 1.371(12) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.500(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.372(9) . ? C7 C8 1.385(10) . ? C8 C9 1.378(10) . ? C8 H8 0.9300 . ? C9 C10 1.405(11) . ? C9 H9 0.9300 . ? C10 C11 1.378(10) . ? C10 H10 0.9300 . ? C11 C12 1.398(9) . ? C11 H11 0.9300 . ? C14 C15 1.493(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.391(10) . ? C15 C16 1.406(10) . ? C16 C17 1.389(10) . ? C16 C22 1.510(10) . ? C17 C18 1.408(10) . ? C17 C24 1.506(10) . ? C18 C19 1.385(10) . ? C18 C23 1.509(10) . ? C19 C20 1.381(10) . ? C19 H19 0.9300 . ? C20 C21 1.507(10) . ? 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 0.9700 . ? C24 H24B 0.9700 . ? C26 C27 1.374(10) . ? C26 C31 1.399(10) . ? C27 C28 1.387(11) . ? C27 H27 0.9300 . ? C28 C29 1.380(12) . ? C28 H28 0.9300 . ? C29 C30 1.393(12) . ? C29 H29 0.9300 . ? C30 C31 1.381(10) . ? C30 H30 0.9300 . ? C32 C33 1.519(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.370(10) . ? C34 C35 1.403(11) . ? C34 H34 0.9300 . ? C35 C36 1.358(12) . ? C35 H35 0.9300 . ? C36 C37 1.362(12) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? N7 C38 1.18(3) . ? C38 C39 1.40(2) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? N8 C40 1.12(2) 2_556 ? N8 C40 1.12(2) . ? C40 C40 1.19(5) 2_556 ? C40 C41 1.55(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 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 C25 Hg1 C13 173.3(3) . . ? C25 Hg1 Br1 93.30(18) . . ? C13 Hg1 Br1 93.01(19) . . ? Br4 Hg2 Br2 119.60(4) . . ? Br4 Hg2 Br3 110.40(4) . . ? Br2 Hg2 Br3 107.88(3) . . ? Br4 Hg2 Br1 110.25(4) . . ? Br2 Hg2 Br1 103.94(3) . . ? Br3 Hg2 Br1 103.43(3) . . ? Hg2 Br1 Hg1 124.33(3) . . ? C5 N1 C4 117.2(7) . . ? C13 N2 C7 109.9(5) . . ? C13 N2 C6 124.0(5) . . ? C7 N2 C6 126.1(5) . . ? C13 N3 C12 108.7(5) . . ? C13 N3 C14 128.8(5) . . ? C12 N3 C14 122.4(5) . . ? C25 N4 C26 110.4(5) . . ? C25 N4 C24 127.3(5) . . ? C26 N4 C24 122.1(5) . . ? C25 N5 C31 109.8(5) . . ? C25 N5 C32 125.8(6) . . ? C31 N5 C32 124.4(6) . . ? C37 N6 C33 116.0(7) . . ? C2 C1 C5 118.7(8) . . ? C2 C1 H1 120.7 . . ? C5 C1 H1 120.7 . . ? C3 C2 C1 118.9(8) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.0(8) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? N1 C4 C3 123.0(8) . . ? N1 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? N1 C5 C1 123.2(7) . . ? N1 C5 C6 115.7(6) . . ? C1 C5 C6 121.2(6) . . ? N2 C6 C5 111.0(6) . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C12 C7 C8 122.9(6) . . ? C12 C7 N2 105.7(6) . . ? C8 C7 N2 131.4(6) . . ? C9 C8 C7 116.1(7) . . ? C9 C8 H8 122.0 . . ? C7 C8 H8 122.0 . . ? C8 C9 C10 121.3(7) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C10 C9 122.2(7) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 115.9(7) . . ? C10 C11 H11 122.1 . . ? C12 C11 H11 122.1 . . ? C7 C12 N3 108.0(6) . . ? C7 C12 C11 121.5(6) . . ? N3 C12 C11 130.5(6) . . ? N2 C13 N3 107.7(6) . . ? N2 C13 Hg1 122.2(4) . . ? N3 C13 Hg1 129.8(5) . . ? N3 C14 C15 112.4(5) . . ? N3 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N3 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C20 C15 C16 120.9(6) . . ? C20 C15 C14 118.9(6) . . ? C16 C15 C14 119.8(6) . . ? C17 C16 C15 118.8(6) . . ? C17 C16 C22 121.3(7) . . ? C15 C16 C22 119.9(6) . . ? C16 C17 C18 120.4(6) . . ? C16 C17 C24 121.3(6) . . ? C18 C17 C24 118.1(6) . . ? C19 C18 C17 118.7(7) . . ? C19 C18 C23 118.9(7) . . ? C17 C18 C23 122.4(7) . . ? C20 C19 C18 122.0(7) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C15 118.7(6) . . ? C19 C20 C21 119.0(7) . . ? C15 C20 C21 122.4(7) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C17 110.4(5) . . ? N4 C24 H24A 109.6 . . ? C17 C24 H24A 109.6 . . ? N4 C24 H24B 109.6 . . ? C17 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? N4 C25 N5 107.5(5) . . ? N4 C25 Hg1 127.1(5) . . ? N5 C25 Hg1 125.2(4) . . ? C27 C26 C31 121.8(7) . . ? C27 C26 N4 132.3(7) . . ? C31 C26 N4 105.9(6) . . ? C26 C27 C28 116.3(8) . . ? C26 C27 H27 121.8 . . ? C28 C27 H27 121.8 . . ? C29 C28 C27 122.1(8) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 122.0(8) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C31 C30 C29 115.8(7) . . ? C31 C30 H30 122.1 . . ? C29 C30 H30 122.1 . . ? C30 C31 N5 131.5(7) . . ? C30 C31 C26 122.0(7) . . ? N5 C31 C26 106.5(6) . . ? N5 C32 C33 115.1(6) . . ? N5 C32 H32A 108.5 . . ? C33 C32 H32A 108.5 . . ? N5 C32 H32B 108.5 . . ? C33 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? N6 C33 C34 123.5(7) . . ? N6 C33 C32 113.1(6) . . ? C34 C33 C32 123.4(6) . . ? C33 C34 C35 118.4(7) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C36 C35 C34 118.5(8) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C37 118.8(8) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? N6 C37 C36 124.8(8) . . ? N6 C37 H37 117.6 . . ? C36 C37 H37 117.6 . . ? N7 C38 C39 176(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 . . ? C40 N8 C40 64(3) 2_556 . ? N8 C40 C40 57.9(13) . 2_556 ? N8 C40 C41 175(2) . . ? C40 C40 C41 127.1(15) 2_556 . ? 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 . . ? 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 Br4 Hg2 Br1 Hg1 -35.53(5) . . . . ? Br2 Hg2 Br1 Hg1 93.82(4) . . . . ? Br3 Hg2 Br1 Hg1 -153.56(4) . . . . ? C25 Hg1 Br1 Hg2 -147.80(17) . . . . ? C13 Hg1 Br1 Hg2 29.92(17) . . . . ? C5 C1 C2 C3 1.0(13) . . . . ? C1 C2 C3 C4 -0.2(14) . . . . ? C5 N1 C4 C3 2.1(13) . . . . ? C2 C3 C4 N1 -1.4(15) . . . . ? C4 N1 C5 C1 -1.3(11) . . . . ? C4 N1 C5 C6 177.3(7) . . . . ? C2 C1 C5 N1 -0.2(12) . . . . ? C2 C1 C5 C6 -178.7(7) . . . . ? C13 N2 C6 C5 78.1(8) . . . . ? C7 N2 C6 C5 -100.7(7) . . . . ? N1 C5 C6 N2 -58.8(8) . . . . ? C1 C5 C6 N2 119.9(7) . . . . ? C13 N2 C7 C12 1.1(8) . . . . ? C6 N2 C7 C12 -179.9(6) . . . . ? C13 N2 C7 C8 -177.8(8) . . . . ? C6 N2 C7 C8 1.1(12) . . . . ? C12 C7 C8 C9 0.4(11) . . . . ? N2 C7 C8 C9 179.3(7) . . . . ? C7 C8 C9 C10 1.4(11) . . . . ? C8 C9 C10 C11 -2.1(13) . . . . ? C9 C10 C11 C12 0.9(12) . . . . ? C8 C7 C12 N3 178.9(7) . . . . ? N2 C7 C12 N3 -0.1(7) . . . . ? C8 C7 C12 C11 -1.7(11) . . . . ? N2 C7 C12 C11 179.3(6) . . . . ? C13 N3 C12 C7 -0.9(8) . . . . ? C14 N3 C12 C7 178.5(6) . . . . ? C13 N3 C12 C11 179.8(7) . . . . ? C14 N3 C12 C11 -0.8(12) . . . . ? C10 C11 C12 C7 0.9(11) . . . . ? C10 C11 C12 N3 -179.8(7) . . . . ? C7 N2 C13 N3 -1.7(8) . . . . ? C6 N2 C13 N3 179.3(6) . . . . ? C7 N2 C13 Hg1 171.9(5) . . . . ? C6 N2 C13 Hg1 -7.2(9) . . . . ? C12 N3 C13 N2 1.6(8) . . . . ? C14 N3 C13 N2 -177.8(7) . . . . ? C12 N3 C13 Hg1 -171.3(5) . . . . ? C14 N3 C13 Hg1 9.4(11) . . . . ? C25 Hg1 C13 N2 -130.7(19) . . . . ? Br1 Hg1 C13 N2 69.1(6) . . . . ? C25 Hg1 C13 N3 41(2) . . . . ? Br1 Hg1 C13 N3 -118.9(6) . . . . ? C13 N3 C14 C15 18.4(10) . . . . ? C12 N3 C14 C15 -160.8(6) . . . . ? N3 C14 C15 C20 83.1(7) . . . . ? N3 C14 C15 C16 -90.5(7) . . . . ? C20 C15 C16 C17 -5.6(9) . . . . ? C14 C15 C16 C17 167.8(5) . . . . ? C20 C15 C16 C22 176.2(6) . . . . ? C14 C15 C16 C22 -10.5(9) . . . . ? C15 C16 C17 C18 8.3(9) . . . . ? C22 C16 C17 C18 -173.5(6) . . . . ? C15 C16 C17 C24 -166.0(6) . . . . ? C22 C16 C17 C24 12.3(9) . . . . ? C16 C17 C18 C19 -4.6(9) . . . . ? C24 C17 C18 C19 169.8(6) . . . . ? C16 C17 C18 C23 176.3(6) . . . . ? C24 C17 C18 C23 -9.3(9) . . . . ? C17 C18 C19 C20 -2.0(10) . . . . ? C23 C18 C19 C20 177.2(6) . . . . ? C18 C19 C20 C15 4.7(10) . . . . ? C18 C19 C20 C21 -173.9(6) . . . . ? C16 C15 C20 C19 -0.8(9) . . . . ? C14 C15 C20 C19 -174.2(6) . . . . ? C16 C15 C20 C21 177.7(6) . . . . ? C14 C15 C20 C21 4.2(9) . . . . ? C25 N4 C24 C17 -40.9(9) . . . . ? C26 N4 C24 C17 145.3(6) . . . . ? C16 C17 C24 N4 102.6(7) . . . . ? C18 C17 C24 N4 -71.8(7) . . . . ? C26 N4 C25 N5 0.4(7) . . . . ? C24 N4 C25 N5 -174.0(6) . . . . ? C26 N4 C25 Hg1 -174.3(5) . . . . ? C24 N4 C25 Hg1 11.3(10) . . . . ? C31 N5 C25 N4 -1.6(7) . . . . ? C32 N5 C25 N4 179.6(6) . . . . ? C31 N5 C25 Hg1 173.2(5) . . . . ? C32 N5 C25 Hg1 -5.6(9) . . . . ? C13 Hg1 C25 N4 -46(2) . . . . ? Br1 Hg1 C25 N4 114.0(6) . . . . ? C13 Hg1 C25 N5 140.1(19) . . . . ? Br1 Hg1 C25 N5 -59.8(5) . . . . ? C25 N4 C26 C27 177.9(8) . . . . ? C24 N4 C26 C27 -7.4(12) . . . . ? C25 N4 C26 C31 0.9(8) . . . . ? C24 N4 C26 C31 175.7(6) . . . . ? C31 C26 C27 C28 0.5(12) . . . . ? N4 C26 C27 C28 -176.0(8) . . . . ? C26 C27 C28 C29 0.7(13) . . . . ? C27 C28 C29 C30 -2.7(14) . . . . ? C28 C29 C30 C31 3.3(12) . . . . ? C29 C30 C31 N5 177.2(7) . . . . ? C29 C30 C31 C26 -2.1(11) . . . . ? C25 N5 C31 C30 -177.2(7) . . . . ? C32 N5 C31 C30 1.5(12) . . . . ? C25 N5 C31 C26 2.2(8) . . . . ? C32 N5 C31 C26 -179.0(6) . . . . ? C27 C26 C31 C30 0.3(11) . . . . ? N4 C26 C31 C30 177.6(7) . . . . ? C27 C26 C31 N5 -179.2(7) . . . . ? N4 C26 C31 N5 -1.8(7) . . . . ? C25 N5 C32 C33 -103.0(8) . . . . ? C31 N5 C32 C33 78.5(8) . . . . ? C37 N6 C33 C34 1.1(12) . . . . ? C37 N6 C33 C32 -179.9(7) . . . . ? N5 C32 C33 N6 169.6(6) . . . . ? N5 C32 C33 C34 -11.4(10) . . . . ? N6 C33 C34 C35 -0.8(12) . . . . ? C32 C33 C34 C35 -179.7(7) . . . . ? C33 C34 C35 C36 0.5(13) . . . . ? C34 C35 C36 C37 -0.5(15) . . . . ? C33 N6 C37 C36 -1.1(15) . . . . ? C35 C36 C37 N6 0.9(17) . . . . ? C40 N8 C40 C41 -173(31) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.415 _refine_diff_density_min -1.816 _refine_diff_density_rms 0.136 data_90509c _database_code_depnum_ccdc_archive 'CCDC 818678' #TrackingRef '- complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Ag2 Cl2 N4 O2' _chemical_formula_weight 817.29 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' 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 9.7774(6) _cell_length_b 11.1171(7) _cell_length_c 15.9735(10) _cell_angle_alpha 102.3410(10) _cell_angle_beta 91.0380(10) _cell_angle_gamma 108.9110(10) _cell_volume 1597.40(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6058 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.431 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 0.773 _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 8201 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5640 _reflns_number_gt 4964 _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^)+(0.0384P)^2^+3.0699P] 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 5615 _refine_ls_number_parameters 419 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.067 _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 0.72508(3) 0.15390(3) 0.706070(19) 0.04601(11) Uani 1 1 d . . . Ag2 Ag 0.43906(6) 0.05170(7) 0.59936(3) 0.1084(2) Uani 1 1 d U . . C1 C 0.9733(4) 0.5591(4) 0.7246(3) 0.0443(9) Uani 1 1 d . A . C2 C 0.8770(4) 0.5767(3) 0.7843(2) 0.0372(8) Uani 1 1 d . A . C3 C 0.8775(5) 0.7009(4) 0.8244(3) 0.0461(9) Uani 1 1 d . . . H3 H 0.8113 0.7132 0.8636 0.055 Uiso 1 1 calc R . . C4 C 0.9811(5) 0.8046(4) 0.8032(3) 0.0568(11) Uani 1 1 d . . . H4 H 0.9837 0.8890 0.8281 0.068 Uiso 1 1 calc R . . C5 C 1.0816(5) 0.7876(4) 0.7459(3) 0.0612(12) Uani 1 1 d . . . H5 H 1.1517 0.8608 0.7351 0.073 Uiso 1 1 calc R . . C6 C 1.0802(5) 0.6651(4) 0.7045(3) 0.0593(11) Uani 1 1 d . . . H6 H 1.1466 0.6534 0.6654 0.071 Uiso 1 1 calc R . . C7 C 0.8237(4) 0.3586(3) 0.7326(2) 0.0415(8) Uani 1 1 d . A . C8 C 1.0288(19) 0.371(2) 0.6347(8) 0.067(6) Uani 0.494(13) 1 d PD A 1 H8A H 1.0062 0.2787 0.6315 0.081 Uiso 0.494(13) 1 calc PR A 1 H8B H 1.1305 0.4157 0.6554 0.081 Uiso 0.494(13) 1 calc PR A 1 C9 C 0.9994(15) 0.3931(15) 0.5474(7) 0.103(5) Uani 0.494(13) 1 d PD A 1 H9A H 0.8965 0.3673 0.5335 0.154 Uiso 0.494(13) 1 calc PR A 1 H9B H 1.0392 0.3419 0.5051 0.154 Uiso 0.494(13) 1 calc PR A 1 H9C H 1.0437 0.4840 0.5479 0.154 Uiso 0.494(13) 1 calc PR A 1 C8' C 0.9803(17) 0.354(2) 0.6155(7) 0.056(4) Uani 0.506(13) 1 d PD A 2 H8'1 H 1.0048 0.4082 0.5742 0.068 Uiso 0.506(13) 1 calc PR A 2 H8'2 H 0.9018 0.2741 0.5891 0.068 Uiso 0.506(13) 1 calc PR A 2 C9' C 1.1099(14) 0.3230(17) 0.6429(8) 0.107(6) Uani 0.506(13) 1 d PD A 2 H9'1 H 1.1858 0.4026 0.6702 0.160 Uiso 0.506(13) 1 calc PR A 2 H9'2 H 1.1435 0.2790 0.5934 0.160 Uiso 0.506(13) 1 calc PR A 2 H9'3 H 1.0835 0.2676 0.6828 0.160 Uiso 0.506(13) 1 calc PR A 2 C10 C 0.6706(4) 0.4256(3) 0.8443(2) 0.0371(8) Uani 1 1 d . A . H10A H 0.6191 0.3322 0.8313 0.045 Uiso 1 1 calc R . . H10B H 0.6028 0.4674 0.8304 0.045 Uiso 1 1 calc R . . C11 C 0.7174(3) 0.4719(3) 0.9395(2) 0.0327(7) Uani 1 1 d . . . C12 C 0.7992(4) 0.4148(3) 0.9803(2) 0.0333(7) Uani 1 1 d . . . C13 C 0.8357(4) 0.4545(3) 1.0688(2) 0.0398(8) Uani 1 1 d . . . H13 H 0.8922 0.4176 1.0953 0.048 Uiso 1 1 calc R . . C14 C 0.7875(4) 0.5490(4) 1.1173(3) 0.0454(9) Uani 1 1 d . . . H14 H 0.8107 0.5746 1.1766 0.055 Uiso 1 1 calc R . . C15 C 0.7057(4) 0.6056(4) 1.0786(3) 0.0463(9) Uani 1 1 d . . . H15 H 0.6730 0.6688 1.1114 0.056 Uiso 1 1 calc R . . C16 C 0.6725(4) 0.5675(4) 0.9903(3) 0.0417(8) Uani 1 1 d . . . H16 H 0.6186 0.6070 0.9643 0.050 Uiso 1 1 calc R . . C17 C 0.9186(4) 0.2567(3) 0.9668(2) 0.0359(8) Uani 1 1 d . . . H17A H 0.8694 0.2237 1.0136 0.043 Uiso 1 1 calc R . . H17B H 1.0140 0.3186 0.9898 0.043 Uiso 1 1 calc R . . C18 C 0.9326(4) 0.1465(3) 0.8989(3) 0.0377(8) Uani 1 1 d . . . H18A H 0.9785 0.1810 0.8517 0.045 Uiso 1 1 calc R . . H18B H 0.9952 0.1076 0.9228 0.045 Uiso 1 1 calc R . . C19 C 0.7172(4) -0.0224(3) 0.9207(2) 0.0319(7) Uani 1 1 d . . . C20 C 0.5715(4) -0.0896(3) 0.8916(2) 0.0333(7) Uani 1 1 d . . . C21 C 0.4859(4) -0.1611(3) 0.9440(3) 0.0416(8) Uani 1 1 d . . . H21 H 0.3889 -0.2083 0.9251 0.050 Uiso 1 1 calc R . . C22 C 0.5399(5) -0.1647(4) 1.0235(3) 0.0465(9) Uani 1 1 d . . . H22 H 0.4795 -0.2123 1.0580 0.056 Uiso 1 1 calc R . . C23 C 0.6837(4) -0.0972(4) 1.0513(3) 0.0444(9) Uani 1 1 d . . . H23 H 0.7208 -0.0987 1.1050 0.053 Uiso 1 1 calc R . . C24 C 0.7732(4) -0.0272(3) 0.9997(2) 0.0389(8) Uani 1 1 d . . . H24 H 0.8711 0.0167 1.0181 0.047 Uiso 1 1 calc R . . C25 C 0.5072(4) -0.0774(4) 0.8085(2) 0.0395(8) Uani 1 1 d . . . H25A H 0.4035 -0.1247 0.8019 0.047 Uiso 1 1 calc R . . H25B H 0.5206 0.0139 0.8120 0.047 Uiso 1 1 calc R . . C26 C 0.6565(4) -0.0518(3) 0.6849(2) 0.0386(8) Uani 1 1 d . . . C27 C 0.5577(4) -0.2584(3) 0.7025(2) 0.0400(8) Uani 1 1 d . . . C28 C 0.4810(5) -0.3709(4) 0.7286(3) 0.0511(10) Uani 1 1 d . . . H28 H 0.4243 -0.3685 0.7746 0.061 Uiso 1 1 calc R . . C29 C 0.4932(6) -0.4870(4) 0.6826(3) 0.0623(13) Uani 1 1 d . . . H29 H 0.4437 -0.5645 0.6982 0.075 Uiso 1 1 calc R . . C30 C 0.5772(6) -0.4906(4) 0.6140(3) 0.0668(14) Uani 1 1 d . . . H30 H 0.5835 -0.5704 0.5851 0.080 Uiso 1 1 calc R . . C31 C 0.6520(6) -0.3792(4) 0.5871(3) 0.0604(12) Uani 1 1 d . . . H31 H 0.7074 -0.3822 0.5405 0.072 Uiso 1 1 calc R . . C32 C 0.6403(4) -0.2624(4) 0.6332(2) 0.0443(9) Uani 1 1 d . . . C33 C 0.7993(5) -0.0924(5) 0.5616(3) 0.0554(11) Uani 1 1 d . . . H33A H 0.7984 -0.0086 0.5535 0.066 Uiso 1 1 calc R . . H33B H 0.7681 -0.1553 0.5067 0.066 Uiso 1 1 calc R . . C34 C 0.9511(6) -0.0805(7) 0.5907(4) 0.092(2) Uani 1 1 d . . . H34A H 0.9505 -0.1605 0.6046 0.137 Uiso 1 1 calc R . . H34B H 0.9872 -0.0098 0.6408 0.137 Uiso 1 1 calc R . . H34C H 1.0127 -0.0635 0.5454 0.137 Uiso 1 1 calc R . . Cl1 Cl 0.34534(16) 0.15021(12) 0.72279(8) 0.0717(3) Uani 1 1 d . . . Cl2 Cl 0.37225(17) -0.17128(14) 0.49889(10) 0.0829(4) Uani 1 1 d . . . N1 N 0.9366(4) 0.4238(3) 0.6938(2) 0.0516(9) Uani 1 1 d D . . N2 N 0.7889(3) 0.4518(3) 0.78888(19) 0.0346(6) Uani 1 1 d . . . N3 N 0.5709(3) -0.1273(3) 0.73246(19) 0.0372(7) Uani 1 1 d . . . N4 N 0.6986(4) -0.1339(3) 0.6241(2) 0.0425(7) Uani 1 1 d . . . O1 O 0.8367(3) 0.3188(2) 0.92757(16) 0.0382(5) Uani 1 1 d . . . O2 O 0.7966(3) 0.0477(2) 0.86637(16) 0.0382(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0628(2) 0.02907(15) 0.04372(18) 0.00704(12) 0.00469(14) 0.01308(13) Ag2 0.1176(4) 0.1571(5) 0.0596(3) -0.0146(3) -0.0200(3) 0.0851(4) C1 0.052(2) 0.038(2) 0.046(2) 0.0167(17) 0.0044(18) 0.0136(17) C2 0.0408(19) 0.0321(18) 0.038(2) 0.0122(15) -0.0061(16) 0.0093(15) C3 0.059(2) 0.0342(19) 0.044(2) 0.0073(16) -0.0044(18) 0.0166(17) C4 0.070(3) 0.031(2) 0.063(3) 0.0111(19) -0.011(2) 0.0095(19) C5 0.057(3) 0.043(2) 0.077(3) 0.029(2) -0.012(2) -0.001(2) C6 0.055(3) 0.058(3) 0.069(3) 0.033(2) 0.010(2) 0.013(2) C7 0.058(2) 0.0316(18) 0.037(2) 0.0104(15) 0.0050(17) 0.0165(17) C8 0.067(12) 0.056(8) 0.079(10) 0.009(8) 0.031(9) 0.024(9) C9 0.108(10) 0.125(12) 0.053(8) 0.003(7) 0.028(7) 0.019(8) C8' 0.063(10) 0.061(8) 0.042(6) 0.011(5) 0.013(6) 0.016(8) C9' 0.089(9) 0.162(14) 0.066(8) -0.028(8) -0.001(6) 0.072(10) C10 0.0337(18) 0.0366(18) 0.042(2) 0.0118(15) -0.0010(15) 0.0112(14) C11 0.0278(16) 0.0297(17) 0.0379(19) 0.0078(14) 0.0028(14) 0.0061(13) C12 0.0304(16) 0.0271(16) 0.040(2) 0.0078(14) 0.0032(14) 0.0061(13) C13 0.0389(19) 0.0374(19) 0.039(2) 0.0108(16) -0.0009(16) 0.0070(15) C14 0.049(2) 0.040(2) 0.038(2) 0.0045(16) 0.0081(17) 0.0052(17) C15 0.047(2) 0.039(2) 0.050(2) 0.0031(17) 0.0155(18) 0.0130(17) C16 0.0348(19) 0.0384(19) 0.053(2) 0.0102(17) 0.0080(17) 0.0142(15) C17 0.0326(17) 0.0314(17) 0.045(2) 0.0133(15) -0.0019(15) 0.0094(14) C18 0.0301(17) 0.0327(18) 0.052(2) 0.0142(16) 0.0044(16) 0.0097(14) C19 0.0359(17) 0.0238(15) 0.0377(19) 0.0079(13) 0.0088(14) 0.0116(13) C20 0.0360(18) 0.0266(16) 0.0369(19) 0.0037(14) 0.0075(15) 0.0122(14) C21 0.0379(19) 0.0332(18) 0.049(2) 0.0060(16) 0.0112(17) 0.0076(15) C22 0.058(2) 0.0353(19) 0.047(2) 0.0158(17) 0.0203(19) 0.0129(17) C23 0.061(2) 0.0364(19) 0.042(2) 0.0151(16) 0.0063(18) 0.0205(18) C24 0.0414(19) 0.0320(18) 0.045(2) 0.0106(15) 0.0011(16) 0.0135(15) C25 0.0370(19) 0.0377(19) 0.044(2) 0.0070(16) 0.0046(16) 0.0142(15) C26 0.046(2) 0.0322(18) 0.0340(19) 0.0055(15) -0.0038(16) 0.0107(15) C27 0.046(2) 0.0293(17) 0.039(2) 0.0019(15) -0.0082(16) 0.0092(15) C28 0.055(2) 0.035(2) 0.055(3) 0.0105(18) -0.011(2) 0.0050(17) C29 0.078(3) 0.032(2) 0.066(3) 0.008(2) -0.026(3) 0.008(2) C30 0.096(4) 0.035(2) 0.062(3) -0.010(2) -0.024(3) 0.028(2) C31 0.086(3) 0.047(2) 0.048(3) -0.0034(19) -0.004(2) 0.032(2) C32 0.059(2) 0.0364(19) 0.037(2) 0.0035(16) -0.0069(18) 0.0196(17) C33 0.076(3) 0.063(3) 0.038(2) 0.019(2) 0.015(2) 0.033(2) C34 0.074(4) 0.133(6) 0.095(5) 0.067(4) 0.029(3) 0.044(4) Cl1 0.0888(9) 0.0602(7) 0.0602(7) 0.0051(6) 0.0057(6) 0.0227(6) Cl2 0.0927(10) 0.0636(8) 0.0783(9) -0.0005(7) -0.0143(7) 0.0192(7) N1 0.069(2) 0.0414(18) 0.049(2) 0.0160(15) 0.0217(17) 0.0207(16) N2 0.0414(16) 0.0283(14) 0.0342(16) 0.0094(12) 0.0001(13) 0.0106(12) N3 0.0425(16) 0.0296(15) 0.0356(16) 0.0030(12) 0.0000(13) 0.0099(12) N4 0.0568(19) 0.0371(16) 0.0342(17) 0.0060(13) 0.0035(14) 0.0178(14) O1 0.0443(14) 0.0343(13) 0.0392(14) 0.0078(10) -0.0019(11) 0.0184(11) O2 0.0358(13) 0.0328(12) 0.0423(14) 0.0133(11) 0.0034(11) 0.0037(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C7 2.107(4) . ? Ag1 C26 2.112(3) . ? Ag1 Ag2 2.9928(6) . ? Ag2 Cl1 2.3916(14) . ? Ag2 Cl2 2.5217(15) . ? Ag2 Cl2 2.6533(18) 2_656 ? C1 C2 1.380(5) . ? C1 N1 1.400(5) . ? C1 C6 1.400(6) . ? C2 C3 1.391(5) . ? C2 N2 1.395(4) . ? C3 C4 1.376(6) . ? C3 H3 0.9300 . ? C4 C5 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.376(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N1 1.352(5) . ? C7 N2 1.357(5) . ? C8 N1 1.476(9) . ? C8 C9 1.504(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C8' N1 1.473(9) . ? C8' C9' 1.497(10) . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C10 N2 1.461(5) . ? C10 C11 1.508(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.389(5) . ? C11 C12 1.398(5) . ? C12 O1 1.365(4) . ? C12 C13 1.392(5) . ? C13 C14 1.382(5) . ? C13 H13 0.9300 . ? C14 C15 1.376(6) . ? C14 H14 0.9300 . ? C15 C16 1.383(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O1 1.426(4) . ? C17 C18 1.497(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O2 1.424(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O2 1.372(4) . ? C19 C24 1.386(5) . ? C19 C20 1.394(5) . ? C20 C21 1.384(5) . ? C20 C25 1.508(5) . ? C21 C22 1.380(6) . ? C21 H21 0.9300 . ? C22 C23 1.374(6) . ? C22 H22 0.9300 . ? C23 C24 1.382(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N3 1.461(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N3 1.350(5) . ? C26 N4 1.350(5) . ? C27 C32 1.385(6) . ? C27 C28 1.388(5) . ? C27 N3 1.396(4) . ? C28 C29 1.385(6) . ? C28 H28 0.9300 . ? C29 C30 1.383(7) . ? C29 H29 0.9300 . ? C30 C31 1.379(7) . ? C30 H30 0.9300 . ? C31 C32 1.390(6) . ? C31 H31 0.9300 . ? C32 N4 1.397(5) . ? C33 N4 1.455(5) . ? C33 C34 1.503(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? Cl2 Ag2 2.6534(18) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ag1 C26 171.61(15) . . ? C7 Ag1 Ag2 114.40(11) . . ? C26 Ag1 Ag2 73.65(10) . . ? Cl1 Ag2 Cl2 136.41(6) . . ? Cl1 Ag2 Cl2 127.62(5) . 2_656 ? Cl2 Ag2 Cl2 94.79(5) . 2_656 ? Cl1 Ag2 Ag1 86.49(4) . . ? Cl2 Ag2 Ag1 117.61(4) . . ? Cl2 Ag2 Ag1 75.19(4) 2_656 . ? C2 C1 N1 106.2(3) . . ? C2 C1 C6 121.7(4) . . ? N1 C1 C6 132.1(4) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 N2 106.2(3) . . ? C3 C2 N2 132.3(4) . . ? C4 C3 C2 116.5(4) . . ? C4 C3 H3 121.7 . . ? C2 C3 H3 121.7 . . ? C3 C4 C5 122.3(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 116.4(4) . . ? C5 C6 H6 121.8 . . ? C1 C6 H6 121.8 . . ? N1 C7 N2 105.7(3) . . ? N1 C7 Ag1 125.4(3) . . ? N2 C7 Ag1 128.9(3) . . ? N1 C8 C9 107.9(9) . . ? N1 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? N1 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? N1 C8' C9' 106.7(9) . . ? N1 C8' H8'1 110.4 . . ? C9' C8' H8'1 110.4 . . ? N1 C8' H8'2 110.4 . . ? C9' C8' H8'2 110.4 . . ? H8'1 C8' H8'2 108.6 . . ? C8' C9' H9'1 109.5 . . ? C8' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C8' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? N2 C10 C11 114.8(3) . . ? N2 C10 H10A 108.6 . . ? C11 C10 H10A 108.6 . . ? N2 C10 H10B 108.6 . . ? C11 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? C16 C11 C12 117.8(3) . . ? C16 C11 C10 120.6(3) . . ? C12 C11 C10 121.4(3) . . ? O1 C12 C13 124.0(3) . . ? O1 C12 C11 115.3(3) . . ? C13 C12 C11 120.7(3) . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.6(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.3(4) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C11 121.9(4) . . ? C15 C16 H16 119.0 . . ? C11 C16 H16 119.0 . . ? O1 C17 C18 107.5(3) . . ? O1 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O1 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? O2 C18 C17 113.0(3) . . ? O2 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? O2 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O2 C19 C24 124.1(3) . . ? O2 C19 C20 115.2(3) . . ? C24 C19 C20 120.7(3) . . ? C21 C20 C19 117.7(3) . . ? C21 C20 C25 121.1(3) . . ? C19 C20 C25 121.1(3) . . ? C22 C21 C20 122.1(4) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C23 C22 C21 119.4(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.0(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? N3 C25 C20 113.6(3) . . ? N3 C25 H25A 108.8 . . ? C20 C25 H25A 108.8 . . ? N3 C25 H25B 108.8 . . ? C20 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N3 C26 N4 105.9(3) . . ? N3 C26 Ag1 127.5(3) . . ? N4 C26 Ag1 126.5(3) . . ? C32 C27 C28 121.7(4) . . ? C32 C27 N3 105.7(3) . . ? C28 C27 N3 132.6(4) . . ? C29 C28 C27 116.6(4) . . ? C29 C28 H28 121.7 . . ? C27 C28 H28 121.7 . . ? C30 C29 C28 121.6(4) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C31 C30 C29 121.9(4) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 116.7(4) . . ? C30 C31 H31 121.7 . . ? C32 C31 H31 121.7 . . ? C27 C32 C31 121.4(4) . . ? C27 C32 N4 106.3(3) . . ? C31 C32 N4 132.2(4) . . ? N4 C33 C34 111.3(4) . . ? N4 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? N4 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? 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 . . ? Ag2 Cl2 Ag2 85.21(5) . 2_656 ? C7 N1 C1 110.9(3) . . ? C7 N1 C8' 119.5(9) . . ? C1 N1 C8' 127.7(9) . . ? C7 N1 C8 128.9(10) . . ? C1 N1 C8 119.8(10) . . ? C8' N1 C8 20.2(9) . . ? C7 N2 C2 111.0(3) . . ? C7 N2 C10 124.7(3) . . ? C2 N2 C10 124.3(3) . . ? C26 N3 C27 111.3(3) . . ? C26 N3 C25 124.5(3) . . ? C27 N3 C25 124.2(3) . . ? C26 N4 C32 110.8(3) . . ? C26 N4 C33 124.4(3) . . ? C32 N4 C33 124.7(3) . . ? C12 O1 C17 117.2(3) . . ? C19 O2 C18 119.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Ag1 Ag2 Cl1 -70.02(12) . . . . ? C26 Ag1 Ag2 Cl1 112.49(11) . . . . ? C7 Ag1 Ag2 Cl2 148.10(12) . . . . ? C26 Ag1 Ag2 Cl2 -29.40(12) . . . . ? C7 Ag1 Ag2 Cl2 60.43(12) . . . 2_656 ? C26 Ag1 Ag2 Cl2 -117.06(11) . . . 2_656 ? N1 C1 C2 C3 -176.4(3) . . . . ? C6 C1 C2 C3 3.0(6) . . . . ? N1 C1 C2 N2 1.6(4) . . . . ? C6 C1 C2 N2 -179.1(4) . . . . ? C1 C2 C3 C4 -1.6(6) . . . . ? N2 C2 C3 C4 -179.0(4) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C3 C4 C5 C6 2.3(7) . . . . ? C4 C5 C6 C1 -1.0(7) . . . . ? C2 C1 C6 C5 -1.6(6) . . . . ? N1 C1 C6 C5 177.5(4) . . . . ? C26 Ag1 C7 N1 59.7(11) . . . . ? Ag2 Ag1 C7 N1 -103.6(3) . . . . ? C26 Ag1 C7 N2 -121.6(9) . . . . ? Ag2 Ag1 C7 N2 75.1(3) . . . . ? N2 C10 C11 C16 116.8(3) . . . . ? N2 C10 C11 C12 -67.3(4) . . . . ? C16 C11 C12 O1 178.2(3) . . . . ? C10 C11 C12 O1 2.1(4) . . . . ? C16 C11 C12 C13 -0.9(5) . . . . ? C10 C11 C12 C13 -177.0(3) . . . . ? O1 C12 C13 C14 -177.4(3) . . . . ? C11 C12 C13 C14 1.6(5) . . . . ? C12 C13 C14 C15 -1.0(5) . . . . ? C13 C14 C15 C16 -0.4(6) . . . . ? C14 C15 C16 C11 1.1(6) . . . . ? C12 C11 C16 C15 -0.4(5) . . . . ? C10 C11 C16 C15 175.6(3) . . . . ? O1 C17 C18 O2 -63.7(4) . . . . ? O2 C19 C20 C21 -179.5(3) . . . . ? C24 C19 C20 C21 -0.3(5) . . . . ? O2 C19 C20 C25 -3.5(4) . . . . ? C24 C19 C20 C25 175.7(3) . . . . ? C19 C20 C21 C22 1.5(5) . . . . ? C25 C20 C21 C22 -174.5(3) . . . . ? C20 C21 C22 C23 -1.2(6) . . . . ? C21 C22 C23 C24 -0.4(6) . . . . ? C22 C23 C24 C19 1.5(5) . . . . ? O2 C19 C24 C23 177.9(3) . . . . ? C20 C19 C24 C23 -1.2(5) . . . . ? C21 C20 C25 N3 -120.5(4) . . . . ? C19 C20 C25 N3 63.6(4) . . . . ? C7 Ag1 C26 N3 108.2(10) . . . . ? Ag2 Ag1 C26 N3 -87.6(3) . . . . ? C7 Ag1 C26 N4 -66.5(11) . . . . ? Ag2 Ag1 C26 N4 97.7(3) . . . . ? C32 C27 C28 C29 1.0(6) . . . . ? N3 C27 C28 C29 179.7(4) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C28 C29 C30 C31 -0.7(7) . . . . ? C29 C30 C31 C32 0.8(7) . . . . ? C28 C27 C32 C31 -1.0(6) . . . . ? N3 C27 C32 C31 -180.0(4) . . . . ? C28 C27 C32 N4 178.6(4) . . . . ? N3 C27 C32 N4 -0.4(4) . . . . ? C30 C31 C32 C27 0.1(6) . . . . ? C30 C31 C32 N4 -179.4(4) . . . . ? Cl1 Ag2 Cl2 Ag2 167.53(6) . . . 2_656 ? Cl2 Ag2 Cl2 Ag2 0.0 2_656 . . 2_656 ? Ag1 Ag2 Cl2 Ag2 -75.78(5) . . . 2_656 ? N2 C7 N1 C1 -0.6(4) . . . . ? Ag1 C7 N1 C1 178.4(3) . . . . ? N2 C7 N1 C8' -166.4(8) . . . . ? Ag1 C7 N1 C8' 12.6(9) . . . . ? N2 C7 N1 C8 171.9(8) . . . . ? Ag1 C7 N1 C8 -9.1(10) . . . . ? C2 C1 N1 C7 -0.7(5) . . . . ? C6 C1 N1 C7 -179.9(4) . . . . ? C2 C1 N1 C8' 163.6(8) . . . . ? C6 C1 N1 C8' -15.6(10) . . . . ? C2 C1 N1 C8 -173.9(7) . . . . ? C6 C1 N1 C8 6.8(9) . . . . ? C9' C8' N1 C7 -100.6(13) . . . . ? C9' C8' N1 C1 96.3(14) . . . . ? C9' C8' N1 C8 23(4) . . . . ? C9 C8 N1 C7 112.8(13) . . . . ? C9 C8 N1 C1 -75.2(15) . . . . ? C9 C8 N1 C8' 44(4) . . . . ? N1 C7 N2 C2 1.6(4) . . . . ? Ag1 C7 N2 C2 -177.2(3) . . . . ? N1 C7 N2 C10 179.0(3) . . . . ? Ag1 C7 N2 C10 0.1(5) . . . . ? C1 C2 N2 C7 -2.1(4) . . . . ? C3 C2 N2 C7 175.6(4) . . . . ? C1 C2 N2 C10 -179.5(3) . . . . ? C3 C2 N2 C10 -1.8(6) . . . . ? C11 C10 N2 C7 118.3(4) . . . . ? C11 C10 N2 C2 -64.6(4) . . . . ? N4 C26 N3 C27 0.1(4) . . . . ? Ag1 C26 N3 C27 -175.5(3) . . . . ? N4 C26 N3 C25 176.7(3) . . . . ? Ag1 C26 N3 C25 1.2(5) . . . . ? C32 C27 N3 C26 0.2(4) . . . . ? C28 C27 N3 C26 -178.6(4) . . . . ? C32 C27 N3 C25 -176.5(3) . . . . ? C28 C27 N3 C25 4.7(6) . . . . ? C20 C25 N3 C26 -110.5(4) . . . . ? C20 C25 N3 C27 65.7(4) . . . . ? N3 C26 N4 C32 -0.3(4) . . . . ? Ag1 C26 N4 C32 175.3(3) . . . . ? N3 C26 N4 C33 -176.3(3) . . . . ? Ag1 C26 N4 C33 -0.6(5) . . . . ? C27 C32 N4 C26 0.4(4) . . . . ? C31 C32 N4 C26 180.0(4) . . . . ? C27 C32 N4 C33 176.4(4) . . . . ? C31 C32 N4 C33 -4.1(7) . . . . ? C34 C33 N4 C26 96.8(5) . . . . ? C34 C33 N4 C32 -78.6(6) . . . . ? C13 C12 O1 C17 -0.2(5) . . . . ? C11 C12 O1 C17 -179.2(3) . . . . ? C18 C17 O1 C12 173.9(3) . . . . ? C24 C19 O2 C18 -16.3(5) . . . . ? C20 C19 O2 C18 162.9(3) . . . . ? C17 C18 O2 C19 -63.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.740 _refine_diff_density_min -1.797 _refine_diff_density_rms 0.072 # Attachment '- complex 2.cif' data_91204b _database_code_depnum_ccdc_archive 'CCDC 818679' #TrackingRef '- complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 Cl4 N6 O3 Pd2' _chemical_formula_weight 1041.48 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8237(10) _cell_length_b 20.2191(10) _cell_length_c 12.4370(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.5070(10) _cell_angle_gamma 90.00 _cell_volume 4602.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.93 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.836 _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 23202 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8082 _reflns_number_gt 6555 _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^)+(0.0492P)^2^+4.7142P] 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 8082 _refine_ls_number_parameters 520 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.073 _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 Pd1 Pd 0.830749(16) 0.653908(13) 0.37260(2) 0.05018(10) Uani 1 1 d . . . Pd2 Pd 0.731167(15) 0.347597(13) 0.97728(2) 0.04985(10) Uani 1 1 d . . . Cl1 Cl 0.92246(6) 0.63950(6) 0.52949(9) 0.0739(3) Uani 1 1 d . . . Cl2 Cl 0.73376(7) 0.66508(6) 0.22374(9) 0.0733(3) Uani 1 1 d . . . Cl3 Cl 0.63164(7) 0.34120(8) 0.83131(12) 0.0975(4) Uani 1 1 d . . . Cl4 Cl 0.83643(6) 0.35246(5) 1.11443(8) 0.0666(3) Uani 1 1 d . . . O1 O 0.67715(14) 0.67287(14) 0.7250(2) 0.0591(6) Uani 1 1 d . . . O2 O 0.73865(13) 0.61989(11) 0.9261(2) 0.0540(6) Uani 1 1 d . . . N1 N 0.74508(15) 0.56963(15) 0.4901(2) 0.0485(7) Uani 1 1 d . . . N2 N 0.78458(16) 0.51538(14) 0.3656(2) 0.0501(7) Uani 1 1 d . . . N3 N 0.80097(15) 0.43641(13) 0.8460(2) 0.0439(6) Uani 1 1 d . . . N4 N 0.82338(16) 0.33338(13) 0.8181(2) 0.0464(6) Uani 1 1 d . . . N5 N 0.8852(2) 0.73754(18) 0.3340(3) 0.0686(9) Uani 1 1 d . . . N6 N 0.6675(2) 0.32464(19) 1.0883(3) 0.0730(10) Uani 1 1 d . . . C1 C 0.72267(19) 0.50503(19) 0.4957(3) 0.0536(9) Uani 1 1 d . . . C2 C 0.74840(19) 0.46944(18) 0.4172(3) 0.0536(8) Uani 1 1 d . . . C3 C 0.7387(2) 0.4021(2) 0.4037(4) 0.0728(12) Uani 1 1 d . . . H3 H 0.7557 0.3788 0.3503 0.087 Uiso 1 1 calc R . . C4 C 0.7023(3) 0.3713(3) 0.4739(5) 0.0914(16) Uani 1 1 d . . . H4 H 0.6951 0.3258 0.4681 0.110 Uiso 1 1 calc R . . C5 C 0.6760(3) 0.4062(3) 0.5535(5) 0.0882(16) Uani 1 1 d . . . H5 H 0.6518 0.3832 0.5990 0.106 Uiso 1 1 calc R . . C6 C 0.6847(2) 0.4734(2) 0.5666(3) 0.0699(12) Uani 1 1 d . . . H6 H 0.6666 0.4966 0.6190 0.084 Uiso 1 1 calc R . . C7 C 0.78330(18) 0.57546(17) 0.4112(3) 0.0463(8) Uani 1 1 d . . . C8 C 0.8232(2) 0.4995(2) 0.2782(3) 0.0611(10) Uani 1 1 d . . . H8A H 0.8247 0.5385 0.2334 0.073 Uiso 1 1 calc R . . H8B H 0.7965 0.4653 0.2306 0.073 Uiso 1 1 calc R . . C9 C 0.8992(2) 0.4763(2) 0.3256(4) 0.0744(12) Uani 1 1 d . . . H9A H 0.9266 0.5110 0.3692 0.112 Uiso 1 1 calc R . . H9B H 0.9220 0.4646 0.2667 0.112 Uiso 1 1 calc R . . H9C H 0.8980 0.4383 0.3715 0.112 Uiso 1 1 calc R . . C10 C 0.73257(19) 0.6223(2) 0.5633(3) 0.0549(9) Uani 1 1 d . . . H10A H 0.7640 0.6594 0.5568 0.066 Uiso 1 1 calc R . . H10B H 0.7463 0.6066 0.6390 0.066 Uiso 1 1 calc R . . C11 C 0.65379(19) 0.64608(17) 0.5389(3) 0.0493(8) Uani 1 1 d . . . C12 C 0.62846(19) 0.67308(18) 0.6262(3) 0.0502(8) Uani 1 1 d . . . C13 C 0.5576(2) 0.6979(2) 0.6067(4) 0.0682(11) Uani 1 1 d . . . H13 H 0.5408 0.7172 0.6641 0.082 Uiso 1 1 calc R . . C14 C 0.5126(2) 0.6940(3) 0.5033(4) 0.0822(14) Uani 1 1 d . . . H14 H 0.4650 0.7099 0.4912 0.099 Uiso 1 1 calc R . . C15 C 0.5368(3) 0.6667(3) 0.4165(4) 0.0808(13) Uani 1 1 d . . . H15 H 0.5058 0.6643 0.3464 0.097 Uiso 1 1 calc R . . C16 C 0.6079(2) 0.6429(2) 0.4348(3) 0.0645(10) Uani 1 1 d . . . H16 H 0.6246 0.6247 0.3766 0.077 Uiso 1 1 calc R . . C17 C 0.6546(2) 0.69441(19) 0.8220(3) 0.0560(9) Uani 1 1 d . . . H17A H 0.6151 0.6669 0.8344 0.067 Uiso 1 1 calc R . . H17B H 0.6378 0.7399 0.8134 0.067 Uiso 1 1 calc R . . C18 C 0.7189(2) 0.68862(17) 0.9154(3) 0.0543(9) Uani 1 1 d . . . H18A H 0.7591 0.7147 0.9013 0.065 Uiso 1 1 calc R . . H18B H 0.7073 0.7045 0.9829 0.065 Uiso 1 1 calc R . . C19 C 0.80807(18) 0.60301(17) 0.9804(3) 0.0464(8) Uani 1 1 d . . . C20 C 0.82730(18) 0.53785(16) 0.9623(3) 0.0439(7) Uani 1 1 d . . . C21 C 0.8955(2) 0.51601(19) 1.0153(3) 0.0536(9) Uani 1 1 d . . . H21 H 0.9091 0.4727 1.0049 0.064 Uiso 1 1 calc R . . C22 C 0.9443(2) 0.5578(2) 1.0844(3) 0.0646(10) Uani 1 1 d . . . H22 H 0.9906 0.5427 1.1194 0.078 Uiso 1 1 calc R . . C23 C 0.9240(2) 0.6210(2) 1.1007(3) 0.0686(11) Uani 1 1 d . . . H23 H 0.9567 0.6488 1.1473 0.082 Uiso 1 1 calc R . . C24 C 0.8566(2) 0.64415(19) 1.0499(3) 0.0586(9) Uani 1 1 d . . . H24 H 0.8433 0.6874 1.0619 0.070 Uiso 1 1 calc R . . C25 C 0.77135(18) 0.49550(16) 0.8869(3) 0.0496(8) Uani 1 1 d . . . H25A H 0.7349 0.4821 0.9263 0.059 Uiso 1 1 calc R . . H25B H 0.7469 0.5220 0.8242 0.059 Uiso 1 1 calc R . . C26 C 0.84471(17) 0.43588(17) 0.7697(3) 0.0443(7) Uani 1 1 d . . . C27 C 0.85887(19) 0.37053(17) 0.7521(3) 0.0469(8) Uani 1 1 d . . . C28 C 0.9004(2) 0.3518(2) 0.6782(3) 0.0586(10) Uani 1 1 d . . . H28 H 0.9096 0.3075 0.6662 0.070 Uiso 1 1 calc R . . C29 C 0.9269(2) 0.4015(2) 0.6241(3) 0.0669(11) Uani 1 1 d . . . H29 H 0.9561 0.3910 0.5755 0.080 Uiso 1 1 calc R . . C30 C 0.9114(2) 0.4675(2) 0.6400(3) 0.0672(11) Uani 1 1 d . . . H30 H 0.9291 0.4998 0.6000 0.081 Uiso 1 1 calc R . . C31 C 0.87033(19) 0.4867(2) 0.7135(3) 0.0563(9) Uani 1 1 d . . . H31 H 0.8605 0.5309 0.7246 0.068 Uiso 1 1 calc R . . C32 C 0.78850(17) 0.37370(16) 0.8739(3) 0.0428(7) Uani 1 1 d . . . C33 C 0.8265(2) 0.26148(17) 0.8278(4) 0.0647(10) Uani 1 1 d . . . H33A H 0.8180 0.2423 0.7544 0.078 Uiso 1 1 calc R . . H33B H 0.7877 0.2466 0.8613 0.078 Uiso 1 1 calc R . . C34 C 0.8978(3) 0.2372(2) 0.8951(4) 0.0892(15) Uani 1 1 d . . . H34A H 0.9363 0.2505 0.8609 0.134 Uiso 1 1 calc R . . H34B H 0.8968 0.1899 0.8997 0.134 Uiso 1 1 calc R . . H34C H 0.9063 0.2557 0.9681 0.134 Uiso 1 1 calc R . . C35 C 0.9181(2) 0.7828(2) 0.3279(3) 0.0607(10) Uani 1 1 d . . . C36 C 0.9612(3) 0.8420(2) 0.3237(4) 0.0762(13) Uani 1 1 d . . . H36A H 0.9470 0.8759 0.3685 0.114 Uiso 1 1 calc R . . H36B H 0.9530 0.8571 0.2487 0.114 Uiso 1 1 calc R . . H36C H 1.0121 0.8320 0.3512 0.114 Uiso 1 1 calc R . . C37 C 0.6278(2) 0.3218(2) 1.1431(4) 0.0688(11) Uani 1 1 d . . . C38 C 0.5770(3) 0.3186(3) 1.2142(4) 0.0921(15) Uani 1 1 d . . . H38A H 0.5871 0.2801 1.2603 0.138 Uiso 1 1 calc R . . H38B H 0.5280 0.3163 1.1697 0.138 Uiso 1 1 calc R . . H38C H 0.5822 0.3575 1.2598 0.138 Uiso 1 1 calc R . . O3 O 0.4669(4) 0.4381(4) 0.1225(7) 0.207(3) Uani 1 1 d DU . . C40 C 0.4949(6) 0.4794(5) 0.3157(9) 0.209(4) Uani 1 1 d DU . . H40A H 0.4958 0.4357 0.3465 0.313 Uiso 1 1 calc R . . H40B H 0.4795 0.5105 0.3639 0.313 Uiso 1 1 calc R . . H40C H 0.5429 0.4909 0.3078 0.313 Uiso 1 1 calc R . . C41 C 0.4211(6) 0.4412(6) 0.0024(9) 0.204(4) Uani 1 1 d DU . . H41A H 0.3698 0.4343 0.0000 0.245 Uiso 1 1 calc R . . H41B H 0.4266 0.4840 -0.0302 0.245 Uiso 1 1 calc R . . C39 C 0.4439(6) 0.4808(5) 0.2073(9) 0.202(4) Uani 1 1 d DU . . H39A H 0.4389 0.5261 0.1808 0.243 Uiso 1 1 calc R . . H39B H 0.3963 0.4663 0.2154 0.243 Uiso 1 1 calc R . . C42 C 0.4492(7) 0.3880(6) -0.0579(10) 0.227(5) Uani 1 1 d DU . . H42A H 0.4404 0.3459 -0.0277 0.341 Uiso 1 1 calc R . . H42B H 0.5007 0.3939 -0.0504 0.341 Uiso 1 1 calc R . . H42C H 0.4246 0.3897 -0.1347 0.341 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 0.05825(19) 0.04786(17) 0.04887(17) -0.00401(11) 0.02150(13) -0.00207(12) Pd2 0.05371(18) 0.04764(17) 0.05206(17) -0.00085(11) 0.02013(13) -0.00324(12) Cl1 0.0660(6) 0.0873(8) 0.0641(6) -0.0005(5) 0.0067(5) -0.0165(5) Cl2 0.0784(7) 0.0864(8) 0.0543(5) 0.0065(5) 0.0137(5) 0.0128(6) Cl3 0.0627(7) 0.1417(13) 0.0815(8) 0.0009(8) 0.0032(6) -0.0155(7) Cl4 0.0716(6) 0.0770(7) 0.0498(5) 0.0057(4) 0.0112(5) -0.0077(5) O1 0.0523(15) 0.0738(17) 0.0542(15) -0.0075(13) 0.0186(12) 0.0143(12) O2 0.0521(14) 0.0407(13) 0.0671(15) -0.0053(11) 0.0099(12) 0.0046(11) N1 0.0458(15) 0.0557(18) 0.0459(15) -0.0050(13) 0.0146(13) -0.0011(13) N2 0.0542(17) 0.0499(17) 0.0482(16) -0.0070(13) 0.0156(13) -0.0005(13) N3 0.0465(15) 0.0384(14) 0.0464(15) 0.0003(12) 0.0101(12) 0.0031(12) N4 0.0561(17) 0.0393(15) 0.0463(15) -0.0028(12) 0.0168(13) 0.0010(12) N5 0.080(2) 0.063(2) 0.070(2) 0.0002(17) 0.0330(19) -0.0042(19) N6 0.068(2) 0.084(3) 0.076(2) 0.000(2) 0.033(2) -0.0104(19) C1 0.0424(19) 0.064(2) 0.051(2) 0.0045(17) 0.0050(16) -0.0062(16) C2 0.047(2) 0.053(2) 0.057(2) -0.0019(17) 0.0068(17) -0.0025(16) C3 0.069(3) 0.056(2) 0.090(3) -0.003(2) 0.010(2) -0.007(2) C4 0.085(3) 0.065(3) 0.117(4) 0.012(3) 0.008(3) -0.019(3) C5 0.069(3) 0.096(4) 0.093(4) 0.032(3) 0.007(3) -0.030(3) C6 0.049(2) 0.098(4) 0.061(2) 0.009(2) 0.0106(19) -0.014(2) C7 0.0451(18) 0.052(2) 0.0410(17) -0.0066(15) 0.0087(14) 0.0015(15) C8 0.075(3) 0.060(2) 0.052(2) -0.0127(17) 0.0233(19) 0.0025(19) C9 0.069(3) 0.094(3) 0.066(3) -0.011(2) 0.027(2) 0.005(2) C10 0.049(2) 0.068(2) 0.050(2) -0.0115(17) 0.0149(16) 0.0012(17) C11 0.0444(19) 0.052(2) 0.052(2) 0.0065(15) 0.0140(16) -0.0021(15) C12 0.0475(19) 0.051(2) 0.056(2) 0.0080(16) 0.0197(17) 0.0029(15) C13 0.055(2) 0.079(3) 0.076(3) 0.014(2) 0.024(2) 0.016(2) C14 0.051(2) 0.098(4) 0.097(4) 0.028(3) 0.016(2) 0.020(2) C15 0.060(3) 0.095(4) 0.077(3) 0.018(3) -0.004(2) 0.003(2) C16 0.056(2) 0.079(3) 0.055(2) 0.0053(19) 0.0075(19) 0.0044(19) C17 0.063(2) 0.052(2) 0.060(2) -0.0002(17) 0.0308(19) 0.0170(17) C18 0.070(2) 0.0399(19) 0.058(2) -0.0062(16) 0.0263(19) 0.0093(17) C19 0.0498(19) 0.0480(19) 0.0438(18) -0.0008(14) 0.0158(15) 0.0009(15) C20 0.0468(18) 0.0455(18) 0.0405(17) 0.0016(14) 0.0127(14) 0.0015(14) C21 0.055(2) 0.055(2) 0.050(2) 0.0041(16) 0.0107(17) 0.0065(17) C22 0.052(2) 0.087(3) 0.052(2) 0.002(2) 0.0048(18) 0.005(2) C23 0.064(3) 0.085(3) 0.053(2) -0.015(2) 0.007(2) -0.012(2) C24 0.066(2) 0.056(2) 0.055(2) -0.0118(17) 0.0152(19) -0.0069(18) C25 0.0464(19) 0.0393(18) 0.061(2) -0.0017(15) 0.0094(16) 0.0048(14) C26 0.0409(17) 0.0506(19) 0.0386(16) 0.0065(14) 0.0035(14) 0.0006(14) C27 0.0502(19) 0.051(2) 0.0377(17) -0.0010(14) 0.0072(15) 0.0018(15) C28 0.060(2) 0.072(3) 0.046(2) -0.0042(17) 0.0143(17) 0.0082(19) C29 0.057(2) 0.099(3) 0.048(2) 0.000(2) 0.0176(18) 0.000(2) C30 0.057(2) 0.094(3) 0.051(2) 0.018(2) 0.0124(18) -0.012(2) C31 0.049(2) 0.057(2) 0.058(2) 0.0135(17) 0.0030(17) -0.0029(17) C32 0.0460(18) 0.0405(17) 0.0412(17) -0.0014(14) 0.0091(14) -0.0016(14) C33 0.086(3) 0.0375(19) 0.077(3) -0.0058(18) 0.033(2) 0.0001(19) C34 0.115(4) 0.057(3) 0.095(4) 0.010(2) 0.023(3) 0.023(3) C35 0.068(2) 0.060(2) 0.058(2) 0.0079(18) 0.0225(19) 0.002(2) C36 0.085(3) 0.072(3) 0.073(3) 0.010(2) 0.020(2) -0.014(2) C37 0.067(3) 0.071(3) 0.073(3) -0.002(2) 0.026(2) -0.010(2) C38 0.080(3) 0.112(4) 0.100(4) -0.002(3) 0.052(3) -0.006(3) O3 0.199(6) 0.191(6) 0.233(6) 0.019(5) 0.056(5) 0.021(5) C40 0.238(9) 0.150(7) 0.234(8) -0.030(7) 0.048(7) 0.003(6) C41 0.168(7) 0.207(8) 0.239(9) 0.013(7) 0.049(7) -0.042(6) C39 0.202(8) 0.171(7) 0.239(9) -0.042(7) 0.064(7) 0.057(6) C42 0.228(9) 0.256(9) 0.205(8) -0.041(7) 0.065(7) -0.017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C7 1.935(3) . ? Pd1 N5 2.090(4) . ? Pd1 Cl2 2.2876(11) . ? Pd1 Cl1 2.3019(11) . ? Pd2 C32 1.935(3) . ? Pd2 N6 2.081(3) . ? Pd2 Cl3 2.2878(13) . ? Pd2 Cl4 2.2948(11) . ? O1 C12 1.351(4) . ? O1 C17 1.436(4) . ? O2 C19 1.367(4) . ? O2 C18 1.437(4) . ? N1 C7 1.351(4) . ? N1 C1 1.380(5) . ? N1 C10 1.455(4) . ? N2 C7 1.343(4) . ? N2 C2 1.393(5) . ? N2 C8 1.478(4) . ? N3 C32 1.349(4) . ? N3 C26 1.394(4) . ? N3 C25 1.459(4) . ? N4 C32 1.338(4) . ? N4 C27 1.393(4) . ? N4 C33 1.459(4) . ? N5 C35 1.118(5) . ? N6 C37 1.124(5) . ? C1 C2 1.388(5) . ? C1 C6 1.411(5) . ? C2 C3 1.380(5) . ? C3 C4 1.377(7) . ? C3 H3 0.9300 . ? C4 C5 1.397(8) . ? C4 H4 0.9300 . ? C5 C6 1.374(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.490(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.521(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.380(5) . ? C11 C12 1.394(5) . ? C12 C13 1.393(5) . ? C13 C14 1.368(6) . ? C13 H13 0.9300 . ? C14 C15 1.381(7) . ? C14 H14 0.9300 . ? C15 C16 1.390(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.474(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.380(5) . ? C19 C20 1.398(5) . ? C20 C21 1.371(5) . ? C20 C25 1.504(5) . ? C21 C22 1.389(5) . ? C21 H21 0.9300 . ? C22 C23 1.362(6) . ? C22 H22 0.9300 . ? C23 C24 1.362(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.376(5) . ? C26 C31 1.391(5) . ? C27 C28 1.390(5) . ? C28 C29 1.369(6) . ? C28 H28 0.9300 . ? C29 C30 1.390(6) . ? C29 H29 0.9300 . ? C30 C31 1.383(6) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C33 C34 1.490(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.454(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.447(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? O3 C39 1.504(7) . ? O3 C41 1.542(8) . ? C40 C39 1.461(8) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.478(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 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 Pd1 N5 178.18(15) . . ? C7 Pd1 Cl2 87.38(10) . . ? N5 Pd1 Cl2 94.33(11) . . ? C7 Pd1 Cl1 89.10(10) . . ? N5 Pd1 Cl1 89.22(11) . . ? Cl2 Pd1 Cl1 175.78(4) . . ? C32 Pd2 N6 176.98(15) . . ? C32 Pd2 Cl3 88.20(10) . . ? N6 Pd2 Cl3 91.27(11) . . ? C32 Pd2 Cl4 87.91(10) . . ? N6 Pd2 Cl4 92.72(11) . . ? Cl3 Pd2 Cl4 175.66(5) . . ? C12 O1 C17 119.5(3) . . ? C19 O2 C18 118.9(3) . . ? C7 N1 C1 109.9(3) . . ? C7 N1 C10 125.6(3) . . ? C1 N1 C10 124.4(3) . . ? C7 N2 C2 110.5(3) . . ? C7 N2 C8 124.6(3) . . ? C2 N2 C8 124.8(3) . . ? C32 N3 C26 109.5(3) . . ? C32 N3 C25 125.2(3) . . ? C26 N3 C25 125.3(3) . . ? C32 N4 C27 109.8(3) . . ? C32 N4 C33 125.4(3) . . ? C27 N4 C33 124.8(3) . . ? C35 N5 Pd1 170.8(4) . . ? C37 N6 Pd2 168.7(4) . . ? N1 C1 C2 107.1(3) . . ? N1 C1 C6 131.8(4) . . ? C2 C1 C6 121.0(4) . . ? C3 C2 C1 122.6(4) . . ? C3 C2 N2 131.9(4) . . ? C1 C2 N2 105.5(3) . . ? C4 C3 C2 116.1(5) . . ? C4 C3 H3 121.9 . . ? C2 C3 H3 121.9 . . ? C3 C4 C5 122.1(5) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 122.1(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 115.9(4) . . ? C5 C6 H6 122.0 . . ? C1 C6 H6 122.0 . . ? N2 C7 N1 107.0(3) . . ? N2 C7 Pd1 125.6(2) . . ? N1 C7 Pd1 127.3(2) . . ? N2 C8 C9 111.7(3) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? 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 113.6(3) . . ? N1 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N1 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C16 C11 C12 119.7(3) . . ? C16 C11 C10 122.7(3) . . ? C12 C11 C10 117.6(3) . . ? O1 C12 C13 125.3(3) . . ? O1 C12 C11 115.1(3) . . ? C13 C12 C11 119.6(4) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.9(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 120.3(4) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? O1 C17 C18 106.7(3) . . ? O1 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O1 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? O2 C18 C17 107.3(3) . . ? O2 C18 H18A 110.3 . . ? C17 C18 H18A 110.3 . . ? O2 C18 H18B 110.3 . . ? C17 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? O2 C19 C24 125.1(3) . . ? O2 C19 C20 114.2(3) . . ? C24 C19 C20 120.7(3) . . ? C21 C20 C19 118.3(3) . . ? C21 C20 C25 123.8(3) . . ? C19 C20 C25 117.8(3) . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 119.6(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 121.1(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 119.5(4) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? N3 C25 C20 114.5(3) . . ? N3 C25 H25A 108.6 . . ? C20 C25 H25A 108.6 . . ? N3 C25 H25B 108.6 . . ? C20 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C27 C26 C31 121.7(3) . . ? C27 C26 N3 106.4(3) . . ? C31 C26 N3 131.8(3) . . ? C26 C27 C28 121.8(3) . . ? C26 C27 N4 106.7(3) . . ? C28 C27 N4 131.5(3) . . ? C29 C28 C27 116.8(4) . . ? C29 C28 H28 121.6 . . ? C27 C28 H28 121.6 . . ? C28 C29 C30 121.4(4) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C31 C30 C29 122.2(4) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C26 116.0(4) . . ? C30 C31 H31 122.0 . . ? C26 C31 H31 122.0 . . ? N4 C32 N3 107.7(3) . . ? N4 C32 Pd2 126.6(2) . . ? N3 C32 Pd2 125.8(2) . . ? N4 C33 C34 112.8(4) . . ? N4 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? N4 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? 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 . . ? N5 C35 C36 178.1(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 C38 179.6(6) . . ? 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 . . ? C39 O3 C41 117.9(8) . . ? 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 . . ? C42 C41 O3 106.0(9) . . ? C42 C41 H41A 110.5 . . ? O3 C41 H41A 110.5 . . ? C42 C41 H41B 110.5 . . ? O3 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? C40 C39 O3 113.6(9) . . ? C40 C39 H39A 108.9 . . ? O3 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? O3 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 Pd1 N5 C35 -49(5) . . . . ? Cl2 Pd1 N5 C35 152(2) . . . . ? Cl1 Pd1 N5 C35 -26(2) . . . . ? C32 Pd2 N6 C37 14(4) . . . . ? Cl3 Pd2 N6 C37 -66(2) . . . . ? Cl4 Pd2 N6 C37 116(2) . . . . ? C7 N1 C1 C2 0.2(4) . . . . ? C10 N1 C1 C2 -176.5(3) . . . . ? C7 N1 C1 C6 176.8(4) . . . . ? C10 N1 C1 C6 0.0(6) . . . . ? N1 C1 C2 C3 177.0(4) . . . . ? C6 C1 C2 C3 -0.1(6) . . . . ? N1 C1 C2 N2 -1.1(4) . . . . ? C6 C1 C2 N2 -178.1(3) . . . . ? C7 N2 C2 C3 -176.2(4) . . . . ? C8 N2 C2 C3 0.1(6) . . . . ? C7 N2 C2 C1 1.6(4) . . . . ? C8 N2 C2 C1 177.8(3) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? N2 C2 C3 C4 176.8(4) . . . . ? C2 C3 C4 C5 0.7(7) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C4 C5 C6 C1 -0.7(7) . . . . ? N1 C1 C6 C5 -175.4(4) . . . . ? C2 C1 C6 C5 0.7(6) . . . . ? C2 N2 C7 N1 -1.5(4) . . . . ? C8 N2 C7 N1 -177.7(3) . . . . ? C2 N2 C7 Pd1 176.6(2) . . . . ? C8 N2 C7 Pd1 0.3(5) . . . . ? C1 N1 C7 N2 0.8(4) . . . . ? C10 N1 C7 N2 177.5(3) . . . . ? C1 N1 C7 Pd1 -177.2(2) . . . . ? C10 N1 C7 Pd1 -0.6(5) . . . . ? N5 Pd1 C7 N2 -79(4) . . . . ? Cl2 Pd1 C7 N2 80.4(3) . . . . ? Cl1 Pd1 C7 N2 -101.9(3) . . . . ? N5 Pd1 C7 N1 99(4) . . . . ? Cl2 Pd1 C7 N1 -102.0(3) . . . . ? Cl1 Pd1 C7 N1 75.7(3) . . . . ? C7 N2 C8 C9 91.4(4) . . . . ? C2 N2 C8 C9 -84.3(5) . . . . ? C7 N1 C10 C11 110.0(4) . . . . ? C1 N1 C10 C11 -73.8(4) . . . . ? N1 C10 C11 C16 -28.3(5) . . . . ? N1 C10 C11 C12 152.8(3) . . . . ? C17 O1 C12 C13 5.6(6) . . . . ? C17 O1 C12 C11 -174.8(3) . . . . ? C16 C11 C12 O1 178.9(3) . . . . ? C10 C11 C12 O1 -2.2(5) . . . . ? C16 C11 C12 C13 -1.5(5) . . . . ? C10 C11 C12 C13 177.5(3) . . . . ? O1 C12 C13 C14 -178.4(4) . . . . ? C11 C12 C13 C14 1.9(6) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C16 0.1(8) . . . . ? C12 C11 C16 C15 0.3(6) . . . . ? C10 C11 C16 C15 -178.6(4) . . . . ? C14 C15 C16 C11 0.4(7) . . . . ? C12 O1 C17 C18 -179.9(3) . . . . ? C19 O2 C18 C17 159.0(3) . . . . ? O1 C17 C18 O2 -62.5(4) . . . . ? C18 O2 C19 C24 16.9(5) . . . . ? C18 O2 C19 C20 -164.5(3) . . . . ? O2 C19 C20 C21 -178.7(3) . . . . ? C24 C19 C20 C21 0.0(5) . . . . ? O2 C19 C20 C25 0.5(4) . . . . ? C24 C19 C20 C25 179.1(3) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C25 C20 C21 C22 -179.6(3) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C19 -0.2(6) . . . . ? O2 C19 C24 C23 178.9(3) . . . . ? C20 C19 C24 C23 0.4(5) . . . . ? C32 N3 C25 C20 111.7(4) . . . . ? C26 N3 C25 C20 -70.3(4) . . . . ? C21 C20 C25 N3 -18.3(5) . . . . ? C19 C20 C25 N3 162.6(3) . . . . ? C32 N3 C26 C27 -0.2(4) . . . . ? C25 N3 C26 C27 -178.5(3) . . . . ? C32 N3 C26 C31 177.4(3) . . . . ? C25 N3 C26 C31 -0.9(6) . . . . ? C31 C26 C27 C28 0.9(5) . . . . ? N3 C26 C27 C28 178.8(3) . . . . ? C31 C26 C27 N4 -177.9(3) . . . . ? N3 C26 C27 N4 0.0(4) . . . . ? C32 N4 C27 C26 0.2(4) . . . . ? C33 N4 C27 C26 -177.5(3) . . . . ? C32 N4 C27 C28 -178.4(4) . . . . ? C33 N4 C27 C28 3.9(6) . . . . ? C26 C27 C28 C29 0.4(5) . . . . ? N4 C27 C28 C29 178.8(4) . . . . ? C27 C28 C29 C30 -1.8(6) . . . . ? C28 C29 C30 C31 2.0(6) . . . . ? C29 C30 C31 C26 -0.7(6) . . . . ? C27 C26 C31 C30 -0.7(5) . . . . ? N3 C26 C31 C30 -178.0(3) . . . . ? C27 N4 C32 N3 -0.4(4) . . . . ? C33 N4 C32 N3 177.4(3) . . . . ? C27 N4 C32 Pd2 -179.8(2) . . . . ? C33 N4 C32 Pd2 -2.0(5) . . . . ? C26 N3 C32 N4 0.4(4) . . . . ? C25 N3 C32 N4 178.7(3) . . . . ? C26 N3 C32 Pd2 179.8(2) . . . . ? C25 N3 C32 Pd2 -1.9(5) . . . . ? N6 Pd2 C32 N4 -169(3) . . . . ? Cl3 Pd2 C32 N4 -88.8(3) . . . . ? Cl4 Pd2 C32 N4 89.3(3) . . . . ? N6 Pd2 C32 N3 12(3) . . . . ? Cl3 Pd2 C32 N3 91.9(3) . . . . ? Cl4 Pd2 C32 N3 -90.0(3) . . . . ? C32 N4 C33 C34 -103.2(4) . . . . ? C27 N4 C33 C34 74.2(5) . . . . ? Pd1 N5 C35 C36 -19(17) . . . . ? Pd2 N6 C37 C38 -67(100) . . . . ? C39 O3 C41 C42 -171.9(9) . . . . ? C41 O3 C39 C40 -174.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.813 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.063 # Attachment '- complex 3.cif' data_90401a _database_code_depnum_ccdc_archive 'CCDC 818680' #TrackingRef '- complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 Ag2 Cl2 N4 O2' _chemical_formula_weight 873.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.3332(5) _cell_length_b 13.3581(6) _cell_length_c 13.9474(7) _cell_angle_alpha 67.4780(10) _cell_angle_beta 76.8630(10) _cell_angle_gamma 71.0840(10) _cell_volume 1832.24(15) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5120 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.882 _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 9196 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6471 _reflns_number_gt 5074 _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^)+(0.1158P)^2^+9.9571P] 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 6401 _refine_ls_number_parameters 438 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.2152 _refine_ls_wR_factor_gt 0.1993 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 1.0000 0.5000 0.0602(3) Uani 1 2 d S . . Ag2 Ag 0.63889(5) 0.80587(5) 0.67610(5) 0.0447(2) Uani 1 1 d . . . Ag3 Ag 1.0000 0.0000 1.0000 0.0956(5) Uani 1 2 d S . . Cl1 Cl 0.42438(17) 1.10738(13) 0.61513(14) 0.0403(4) Uani 1 1 d . . . Cl2 Cl 0.9477(3) 0.1451(2) 0.8435(3) 0.0891(9) Uani 1 1 d . . . O1 O 0.8831(5) 0.5900(4) 0.7201(4) 0.0445(12) Uani 1 1 d . . . O2 O 0.6703(5) 0.5088(4) 0.7448(4) 0.0466(12) Uani 1 1 d . . . N1 N 0.8500(6) 0.9040(5) 0.6824(5) 0.0457(15) Uani 1 1 d . . . N2 N 0.9167(6) 0.8054(5) 0.5796(5) 0.0410(14) Uani 1 1 d . . . N3 N 0.4208(5) 0.6938(5) 0.7074(5) 0.0380(13) Uani 1 1 d . . . N4 N 0.3865(6) 0.7871(5) 0.8124(5) 0.0467(15) Uani 1 1 d . . . C1 C 0.9744(7) 0.9059(6) 0.6460(7) 0.0459(18) Uani 1 1 d . . . C2 C 1.0166(7) 0.8437(6) 0.5803(6) 0.0441(17) Uani 1 1 d . . . C3 C 1.1357(7) 0.8321(7) 0.5247(7) 0.053(2) Uani 1 1 d . . . H3 H 1.1632 0.7914 0.4790 0.063 Uiso 1 1 calc R . . C4 C 1.2118(8) 0.8868(7) 0.5428(8) 0.059(2) Uani 1 1 d . . . H4 H 1.2927 0.8815 0.5080 0.071 Uiso 1 1 calc R . . C5 C 1.1706(8) 0.9481(7) 0.6105(8) 0.058(2) Uani 1 1 d . . . H5 H 1.2246 0.9825 0.6197 0.070 Uiso 1 1 calc R . . C6 C 1.0516(8) 0.9594(7) 0.6645(8) 0.056(2) Uani 1 1 d . . . H6 H 1.0238 1.0000 0.7103 0.067 Uiso 1 1 calc R . . C7 C 0.8136(7) 0.8432(6) 0.6419(6) 0.0439(17) Uani 1 1 d . . . C8 C 0.7702(8) 0.9597(7) 0.7552(7) 0.056(2) Uani 1 1 d . . . H8A H 0.6830 0.9726 0.7476 0.067 Uiso 1 1 calc R . . H8B H 0.7860 1.0324 0.7366 0.067 Uiso 1 1 calc R . . C9 C 0.7902(9) 0.8950(8) 0.8669(8) 0.062(2) Uani 1 1 d . . . H9A H 0.8752 0.8882 0.8759 0.074 Uiso 1 1 calc R . . H9B H 0.7821 0.8199 0.8838 0.074 Uiso 1 1 calc R . . C10 C 0.6986(11) 0.9486(11) 0.9432(9) 0.082(3) Uani 1 1 d . . . H10A H 0.6133 0.9584 0.9327 0.098 Uiso 1 1 calc R . . H10B H 0.7094 1.0222 0.9291 0.098 Uiso 1 1 calc R . . C11 C 0.7189(16) 0.8761(14) 1.0580(10) 0.112(5) Uani 1 1 d . . . H11A H 0.7351 0.7982 1.0665 0.168 Uiso 1 1 calc R . . H11B H 0.6449 0.8971 1.1032 0.168 Uiso 1 1 calc R . . H11C H 0.7892 0.8879 1.0757 0.168 Uiso 1 1 calc R . . C12 C 0.9214(7) 0.7334(7) 0.5226(6) 0.0458(18) Uani 1 1 d . . . H12A H 0.9474 0.7692 0.4493 0.055 Uiso 1 1 calc R . . H12B H 0.8375 0.7261 0.5281 0.055 Uiso 1 1 calc R . . C13 C 1.0082(7) 0.6187(7) 0.5596(6) 0.0424(17) Uani 1 1 d . . . C14 C 0.9850(7) 0.5452(6) 0.6602(6) 0.0412(16) Uani 1 1 d . . . C15 C 1.0624(7) 0.4364(7) 0.6943(7) 0.0505(19) Uani 1 1 d . . . H15 H 1.0477 0.3891 0.7624 0.061 Uiso 1 1 calc R . . C16 C 1.1607(8) 0.3990(8) 0.6269(8) 0.060(2) Uani 1 1 d . . . H16 H 1.2111 0.3258 0.6489 0.072 Uiso 1 1 calc R . . C17 C 1.1848(8) 0.4710(8) 0.5255(8) 0.060(2) Uani 1 1 d . . . H17 H 1.2514 0.4463 0.4799 0.072 Uiso 1 1 calc R . . C18 C 1.1086(8) 0.5791(8) 0.4939(7) 0.055(2) Uani 1 1 d . . . H18 H 1.1251 0.6269 0.4264 0.065 Uiso 1 1 calc R . . C19 C 0.8358(8) 0.5188(7) 0.8165(6) 0.0475(18) Uani 1 1 d . . . H19A H 0.7732 0.5648 0.8534 0.057 Uiso 1 1 calc R . . H19B H 0.9038 0.4755 0.8593 0.057 Uiso 1 1 calc R . . C20 C 0.7778(7) 0.4394(7) 0.8018(7) 0.0493(19) Uani 1 1 d . . . H20A H 0.8380 0.3947 0.7624 0.059 Uiso 1 1 calc R . . H20B H 0.7512 0.3892 0.8690 0.059 Uiso 1 1 calc R . . C21 C 0.6109(7) 0.4534(6) 0.7157(6) 0.0412(16) Uani 1 1 d . . . C22 C 0.5119(7) 0.5214(6) 0.6555(6) 0.0415(16) Uani 1 1 d . . . C23 C 0.4484(8) 0.4689(7) 0.6244(7) 0.052(2) Uani 1 1 d . . . H23 H 0.3823 0.5129 0.5849 0.062 Uiso 1 1 calc R . . C24 C 0.4786(9) 0.3539(8) 0.6495(8) 0.059(2) Uani 1 1 d . . . H24 H 0.4335 0.3210 0.6278 0.071 Uiso 1 1 calc R . . C25 C 0.5753(9) 0.2899(7) 0.7064(8) 0.058(2) Uani 1 1 d . . . H25 H 0.5968 0.2124 0.7231 0.070 Uiso 1 1 calc R . . C26 C 0.6432(8) 0.3369(7) 0.7406(7) 0.0510(19) Uani 1 1 d . . . H26 H 0.7093 0.2914 0.7797 0.061 Uiso 1 1 calc R . . C27 C 0.4807(7) 0.6475(6) 0.6221(6) 0.0422(16) Uani 1 1 d . . . H27A H 0.5573 0.6708 0.5913 0.051 Uiso 1 1 calc R . . H27B H 0.4249 0.6795 0.5682 0.051 Uiso 1 1 calc R . . C28 C 0.3082(7) 0.6801(6) 0.7670(6) 0.0414(16) Uani 1 1 d . . . C29 C 0.2868(7) 0.7386(6) 0.8358(6) 0.0442(17) Uani 1 1 d . . . C30 C 0.1805(8) 0.7424(8) 0.9094(7) 0.056(2) Uani 1 1 d . . . H30 H 0.1661 0.7804 0.9564 0.068 Uiso 1 1 calc R . . C31 C 0.0963(8) 0.6853(9) 0.9083(8) 0.068(3) Uani 1 1 d . . . H31 H 0.0244 0.6849 0.9563 0.082 Uiso 1 1 calc R . . C32 C 0.1171(9) 0.6309(9) 0.8390(8) 0.068(3) Uani 1 1 d . . . H32 H 0.0580 0.5956 0.8404 0.082 Uiso 1 1 calc R . . C33 C 0.2218(8) 0.6259(8) 0.7669(7) 0.056(2) Uani 1 1 d . . . H33 H 0.2346 0.5880 0.7201 0.068 Uiso 1 1 calc R . . C34 C 0.4690(7) 0.7585(6) 0.7341(6) 0.0420(17) Uani 1 1 d . . . C35 C 0.4031(9) 0.8502(7) 0.8689(7) 0.057(2) Uani 1 1 d . . . H35A H 0.3241 0.9042 0.8788 0.068 Uiso 1 1 calc R . . H35B H 0.4643 0.8917 0.8281 0.068 Uiso 1 1 calc R . . C36 C 0.4471(11) 0.7753(9) 0.9752(9) 0.073(3) Uani 1 1 d . . . H36A H 0.4602 0.8217 1.0089 0.088 Uiso 1 1 calc R . . H36B H 0.3814 0.7406 1.0186 0.088 Uiso 1 1 calc R . . C37 C 0.5650(13) 0.6856(11) 0.9694(12) 0.099(4) Uani 1 1 d D . . H37A H 0.5515 0.6438 0.9311 0.119 Uiso 1 1 calc R . . H37B H 0.6297 0.7225 0.9273 0.119 Uiso 1 1 calc R . . C38 C 0.616(2) 0.6052(18) 1.0634(14) 0.181(9) Uani 1 1 d DU . . H38A H 0.7054 0.5903 1.0530 0.271 Uiso 1 1 calc R . . H38B H 0.5925 0.5367 1.0802 0.271 Uiso 1 1 calc R . . H38C H 0.5825 0.6347 1.1197 0.271 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0559(6) 0.0504(5) 0.0745(7) -0.0176(5) -0.0131(5) -0.0148(4) Ag2 0.0389(3) 0.0434(4) 0.0519(4) -0.0137(3) -0.0001(2) -0.0174(2) Ag3 0.0829(9) 0.0661(8) 0.1457(13) -0.0502(8) -0.0400(9) 0.0059(6) Cl1 0.0522(10) 0.0268(8) 0.0487(10) -0.0189(7) 0.0033(8) -0.0178(7) Cl2 0.099(2) 0.0520(14) 0.117(2) -0.0339(15) -0.0469(18) 0.0086(14) O1 0.039(3) 0.042(3) 0.044(3) -0.010(2) 0.005(2) -0.010(2) O2 0.041(3) 0.041(3) 0.058(3) -0.012(2) -0.018(2) -0.007(2) N1 0.047(4) 0.029(3) 0.060(4) -0.011(3) -0.010(3) -0.012(3) N2 0.039(3) 0.036(3) 0.044(3) -0.006(3) -0.002(3) -0.015(3) N3 0.032(3) 0.035(3) 0.043(3) -0.013(3) -0.001(2) -0.006(2) N4 0.048(4) 0.041(3) 0.051(4) -0.019(3) 0.006(3) -0.015(3) C1 0.041(4) 0.031(4) 0.059(5) -0.002(3) -0.013(3) -0.012(3) C2 0.044(4) 0.035(4) 0.048(4) 0.000(3) -0.012(3) -0.017(3) C3 0.041(4) 0.048(5) 0.059(5) -0.001(4) -0.007(4) -0.017(4) C4 0.037(4) 0.049(5) 0.070(6) 0.013(4) -0.013(4) -0.018(4) C5 0.046(5) 0.048(5) 0.076(6) 0.001(4) -0.021(4) -0.023(4) C6 0.059(5) 0.038(4) 0.073(6) -0.009(4) -0.024(4) -0.015(4) C7 0.046(4) 0.036(4) 0.045(4) -0.002(3) -0.009(3) -0.015(3) C8 0.048(5) 0.045(5) 0.079(6) -0.029(4) -0.006(4) -0.009(4) C9 0.058(5) 0.058(5) 0.072(6) -0.029(5) -0.004(4) -0.012(4) C10 0.077(7) 0.093(8) 0.095(9) -0.058(7) 0.007(6) -0.028(6) C11 0.145(14) 0.131(13) 0.084(9) -0.063(9) 0.006(9) -0.048(11) C12 0.042(4) 0.052(5) 0.043(4) -0.012(4) 0.001(3) -0.021(4) C13 0.040(4) 0.051(4) 0.044(4) -0.019(4) -0.002(3) -0.019(3) C14 0.034(4) 0.045(4) 0.048(4) -0.019(3) -0.003(3) -0.012(3) C15 0.042(4) 0.047(4) 0.061(5) -0.014(4) -0.009(4) -0.012(4) C16 0.039(4) 0.057(5) 0.086(7) -0.029(5) -0.009(4) -0.008(4) C17 0.040(4) 0.072(6) 0.079(7) -0.042(5) 0.005(4) -0.018(4) C18 0.048(5) 0.069(6) 0.056(5) -0.029(4) 0.007(4) -0.027(4) C19 0.044(4) 0.057(5) 0.040(4) -0.010(4) -0.006(3) -0.018(4) C20 0.039(4) 0.049(4) 0.050(5) 0.000(4) -0.012(3) -0.013(3) C21 0.037(4) 0.042(4) 0.041(4) -0.014(3) 0.000(3) -0.009(3) C22 0.036(4) 0.042(4) 0.048(4) -0.019(3) -0.002(3) -0.010(3) C23 0.047(4) 0.056(5) 0.063(5) -0.031(4) -0.013(4) -0.010(4) C24 0.059(5) 0.060(5) 0.071(6) -0.032(5) -0.008(4) -0.020(4) C25 0.058(5) 0.042(4) 0.079(6) -0.026(4) -0.001(5) -0.016(4) C26 0.047(4) 0.041(4) 0.059(5) -0.014(4) -0.007(4) -0.006(3) C27 0.040(4) 0.043(4) 0.042(4) -0.017(3) -0.007(3) -0.005(3) C28 0.036(4) 0.037(4) 0.045(4) -0.008(3) -0.005(3) -0.009(3) C29 0.037(4) 0.041(4) 0.044(4) -0.009(3) 0.001(3) -0.005(3) C30 0.045(5) 0.057(5) 0.050(5) -0.012(4) 0.002(4) -0.004(4) C31 0.028(4) 0.086(7) 0.068(6) -0.014(5) 0.003(4) -0.007(4) C32 0.044(5) 0.086(7) 0.067(6) -0.013(5) 0.000(4) -0.028(5) C33 0.041(4) 0.069(6) 0.060(5) -0.016(4) -0.010(4) -0.021(4) C34 0.038(4) 0.034(4) 0.048(4) -0.010(3) 0.001(3) -0.009(3) C35 0.063(5) 0.051(5) 0.061(5) -0.029(4) 0.007(4) -0.017(4) C36 0.078(7) 0.075(7) 0.080(7) -0.038(6) -0.009(5) -0.024(6) C37 0.086(8) 0.074(8) 0.141(12) -0.044(8) -0.044(8) 0.005(6) C38 0.180(10) 0.180(10) 0.178(10) -0.060(6) -0.020(5) -0.043(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 Ag1 Cl1 2.3900(16) . ? Ag1 Cl1 2.3900(16) 2_676 ? Ag1 Ag2 3.0767(6) 2_676 ? Ag1 Ag2 3.0767(6) . ? Ag2 C7 2.104(8) . ? Ag2 C34 2.110(7) . ? Ag3 Cl2 2.340(3) . ? Ag3 Cl2 2.340(3) 2_757 ? O1 C14 1.372(9) . ? O1 C19 1.422(9) . ? O2 C21 1.359(9) . ? O2 C20 1.456(9) . ? N1 C7 1.350(10) . ? N1 C1 1.391(10) . ? N1 C8 1.460(11) . ? N2 C7 1.366(10) . ? N2 C2 1.389(10) . ? N2 C12 1.447(10) . ? N3 C34 1.353(10) . ? N3 C28 1.380(9) . ? N3 C27 1.477(9) . ? N4 C34 1.355(10) . ? N4 C29 1.394(10) . ? N4 C35 1.431(11) . ? C1 C2 1.374(12) . ? C1 C6 1.411(11) . ? C2 C3 1.389(11) . ? C3 C4 1.410(13) . ? C3 H3 0.9300 . ? C4 C5 1.388(14) . ? C4 H4 0.9300 . ? C5 C6 1.379(13) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.492(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.524(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.546(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.493(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.386(11) . ? C13 C14 1.395(11) . ? C14 C15 1.394(11) . ? C15 C16 1.378(12) . ? C15 H15 0.9300 . ? C16 C17 1.397(14) . ? C16 H16 0.9300 . ? C17 C18 1.380(13) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.510(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.396(11) . ? C21 C22 1.404(11) . ? C22 C23 1.378(11) . ? C22 C27 1.505(10) . ? C23 C24 1.379(12) . ? C23 H23 0.9300 . ? C24 C25 1.353(14) . ? C24 H24 0.9300 . ? C25 C26 1.386(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.392(11) . ? C28 C33 1.395(11) . ? C29 C30 1.395(11) . ? C30 C31 1.408(14) . ? C30 H30 0.9300 . ? C31 C32 1.357(15) . ? C31 H31 0.9300 . ? C32 C33 1.371(13) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C35 C36 1.525(14) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.488(16) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.436(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 Cl1 Ag1 Cl1 180.0 . 2_676 ? Cl1 Ag1 Ag2 91.39(5) . 2_676 ? Cl1 Ag1 Ag2 88.61(5) 2_676 2_676 ? Cl1 Ag1 Ag2 88.61(5) . . ? Cl1 Ag1 Ag2 91.39(5) 2_676 . ? Ag2 Ag1 Ag2 179.998(1) 2_676 . ? C7 Ag2 C34 171.4(3) . . ? C7 Ag2 Ag1 100.0(2) . . ? C34 Ag2 Ag1 87.4(2) . . ? Cl2 Ag3 Cl2 179.999(2) . 2_757 ? C14 O1 C19 120.0(6) . . ? C21 O2 C20 115.9(6) . . ? C7 N1 C1 111.0(7) . . ? C7 N1 C8 124.7(7) . . ? C1 N1 C8 124.2(7) . . ? C7 N2 C2 110.7(7) . . ? C7 N2 C12 124.5(6) . . ? C2 N2 C12 124.8(6) . . ? C34 N3 C28 111.7(6) . . ? C34 N3 C27 123.4(6) . . ? C28 N3 C27 124.9(6) . . ? C34 N4 C29 110.1(6) . . ? C34 N4 C35 125.3(7) . . ? C29 N4 C35 124.4(7) . . ? C2 C1 N1 106.5(7) . . ? C2 C1 C6 121.9(8) . . ? N1 C1 C6 131.5(8) . . ? C1 C2 N2 106.3(7) . . ? C1 C2 C3 122.8(7) . . ? N2 C2 C3 130.8(8) . . ? C2 C3 C4 114.9(9) . . ? C2 C3 H3 122.5 . . ? C4 C3 H3 122.5 . . ? C5 C4 C3 122.6(8) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C6 C5 C4 121.6(8) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 116.1(9) . . ? C5 C6 H6 121.9 . . ? C1 C6 H6 121.9 . . ? N1 C7 N2 105.4(6) . . ? N1 C7 Ag2 127.0(6) . . ? N2 C7 Ag2 127.5(6) . . ? N1 C8 C9 113.9(7) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 113.6(9) . . ? 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 . . ? C9 C10 C11 111.8(11) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? 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 114.3(7) . . ? N2 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? N2 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C18 C13 C14 118.0(8) . . ? C18 C13 C12 121.6(7) . . ? C14 C13 C12 120.3(7) . . ? O1 C14 C15 124.5(7) . . ? O1 C14 C13 114.6(7) . . ? C15 C14 C13 120.9(7) . . ? C16 C15 C14 119.8(8) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.1(9) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.2(8) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C13 122.0(9) . . ? C17 C18 H18 119.0 . . ? C13 C18 H18 119.0 . . ? O1 C19 C20 112.6(6) . . ? O1 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? O1 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? O2 C20 C19 106.6(6) . . ? O2 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? O2 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? O2 C21 C26 124.4(7) . . ? O2 C21 C22 115.6(6) . . ? C26 C21 C22 120.0(7) . . ? C23 C22 C21 117.7(7) . . ? C23 C22 C27 121.4(7) . . ? C21 C22 C27 120.9(7) . . ? C22 C23 C24 122.8(8) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 118.6(8) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 121.8(8) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C21 119.1(8) . . ? C25 C26 H26 120.4 . . ? C21 C26 H26 120.4 . . ? N3 C27 C22 114.4(6) . . ? N3 C27 H27A 108.7 . . ? C22 C27 H27A 108.7 . . ? N3 C27 H27B 108.7 . . ? C22 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? N3 C28 C29 105.5(6) . . ? N3 C28 C33 133.4(8) . . ? C29 C28 C33 121.0(7) . . ? C28 C29 N4 106.7(6) . . ? C28 C29 C30 121.5(8) . . ? N4 C29 C30 131.8(8) . . ? C29 C30 C31 115.9(9) . . ? C29 C30 H30 122.0 . . ? C31 C30 H30 122.0 . . ? C32 C31 C30 121.8(8) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C33 122.7(9) . . ? C31 C32 H32 118.6 . . ? C33 C32 H32 118.6 . . ? C32 C33 C28 117.0(9) . . ? C32 C33 H33 121.5 . . ? C28 C33 H33 121.5 . . ? N3 C34 N4 106.0(6) . . ? N3 C34 Ag2 130.0(5) . . ? N4 C34 Ag2 124.0(6) . . ? N4 C35 C36 112.2(7) . . ? N4 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? N4 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C37 C36 C35 113.6(9) . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C36 120.3(15) . . ? C38 C37 H37A 107.3 . . ? C36 C37 H37A 107.3 . . ? C38 C37 H37B 107.3 . . ? C36 C37 H37B 107.3 . . ? H37A C37 H37B 106.9 . . ? 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 Cl1 Ag1 Ag2 C7 -91.5(2) . . . . ? Cl1 Ag1 Ag2 C7 88.5(2) 2_676 . . . ? Ag2 Ag1 Ag2 C7 -25(24) 2_676 . . . ? Cl1 Ag1 Ag2 C34 84.0(2) . . . . ? Cl1 Ag1 Ag2 C34 -96.0(2) 2_676 . . . ? Ag2 Ag1 Ag2 C34 150(24) 2_676 . . . ? C7 N1 C1 C2 0.0(9) . . . . ? C8 N1 C1 C2 179.6(7) . . . . ? C7 N1 C1 C6 178.6(8) . . . . ? C8 N1 C1 C6 -1.9(13) . . . . ? N1 C1 C2 N2 -0.5(8) . . . . ? C6 C1 C2 N2 -179.2(7) . . . . ? N1 C1 C2 C3 176.4(7) . . . . ? C6 C1 C2 C3 -2.3(12) . . . . ? C7 N2 C2 C1 0.8(8) . . . . ? C12 N2 C2 C1 -178.1(7) . . . . ? C7 N2 C2 C3 -175.7(8) . . . . ? C12 N2 C2 C3 5.4(13) . . . . ? C1 C2 C3 C4 1.6(12) . . . . ? N2 C2 C3 C4 177.6(7) . . . . ? C2 C3 C4 C5 -0.4(12) . . . . ? C3 C4 C5 C6 -0.1(13) . . . . ? C4 C5 C6 C1 -0.5(12) . . . . ? C2 C1 C6 C5 1.7(12) . . . . ? N1 C1 C6 C5 -176.7(8) . . . . ? C1 N1 C7 N2 0.4(8) . . . . ? C8 N1 C7 N2 -179.1(7) . . . . ? C1 N1 C7 Ag2 176.7(5) . . . . ? C8 N1 C7 Ag2 -2.9(11) . . . . ? C2 N2 C7 N1 -0.7(8) . . . . ? C12 N2 C7 N1 178.1(6) . . . . ? C2 N2 C7 Ag2 -176.9(5) . . . . ? C12 N2 C7 Ag2 1.9(11) . . . . ? C34 Ag2 C7 N1 -55(2) . . . . ? Ag1 Ag2 C7 N1 93.5(6) . . . . ? C34 Ag2 C7 N2 120.3(18) . . . . ? Ag1 Ag2 C7 N2 -91.1(6) . . . . ? C7 N1 C8 C9 98.5(9) . . . . ? C1 N1 C8 C9 -81.0(10) . . . . ? N1 C8 C9 C10 -174.8(8) . . . . ? C8 C9 C10 C11 177.4(10) . . . . ? C7 N2 C12 C13 -113.5(8) . . . . ? C2 N2 C12 C13 65.2(9) . . . . ? N2 C12 C13 C18 -120.2(8) . . . . ? N2 C12 C13 C14 64.1(9) . . . . ? C19 O1 C14 C15 -12.1(11) . . . . ? C19 O1 C14 C13 168.7(6) . . . . ? C18 C13 C14 O1 -179.2(7) . . . . ? C12 C13 C14 O1 -3.3(10) . . . . ? C18 C13 C14 C15 1.5(11) . . . . ? C12 C13 C14 C15 177.4(7) . . . . ? O1 C14 C15 C16 178.5(7) . . . . ? C13 C14 C15 C16 -2.3(12) . . . . ? C14 C15 C16 C17 1.7(13) . . . . ? C15 C16 C17 C18 -0.4(13) . . . . ? C16 C17 C18 C13 -0.3(13) . . . . ? C14 C13 C18 C17 -0.3(12) . . . . ? C12 C13 C18 C17 -176.1(8) . . . . ? C14 O1 C19 C20 -67.6(9) . . . . ? C21 O2 C20 C19 174.6(6) . . . . ? O1 C19 C20 O2 -63.5(8) . . . . ? C20 O2 C21 C26 2.9(10) . . . . ? C20 O2 C21 C22 -176.4(7) . . . . ? O2 C21 C22 C23 -179.7(7) . . . . ? C26 C21 C22 C23 1.0(11) . . . . ? O2 C21 C22 C27 3.1(10) . . . . ? C26 C21 C22 C27 -176.2(7) . . . . ? C21 C22 C23 C24 -0.4(12) . . . . ? C27 C22 C23 C24 176.8(8) . . . . ? C22 C23 C24 C25 -0.5(14) . . . . ? C23 C24 C25 C26 0.7(14) . . . . ? C24 C25 C26 C21 0.0(14) . . . . ? O2 C21 C26 C25 179.9(7) . . . . ? C22 C21 C26 C25 -0.8(12) . . . . ? C34 N3 C27 C22 122.1(8) . . . . ? C28 N3 C27 C22 -60.1(9) . . . . ? C23 C22 C27 N3 110.8(8) . . . . ? C21 C22 C27 N3 -72.1(9) . . . . ? C34 N3 C28 C29 -1.0(8) . . . . ? C27 N3 C28 C29 -179.0(6) . . . . ? C34 N3 C28 C33 177.2(9) . . . . ? C27 N3 C28 C33 -0.8(13) . . . . ? N3 C28 C29 N4 1.5(8) . . . . ? C33 C28 C29 N4 -177.0(7) . . . . ? N3 C28 C29 C30 -179.5(7) . . . . ? C33 C28 C29 C30 2.0(12) . . . . ? C34 N4 C29 C28 -1.5(9) . . . . ? C35 N4 C29 C28 -176.9(8) . . . . ? C34 N4 C29 C30 179.6(9) . . . . ? C35 N4 C29 C30 4.2(14) . . . . ? C28 C29 C30 C31 -1.0(12) . . . . ? N4 C29 C30 C31 177.8(8) . . . . ? C29 C30 C31 C32 -0.6(14) . . . . ? C30 C31 C32 C33 1.2(16) . . . . ? C31 C32 C33 C28 -0.2(15) . . . . ? N3 C28 C33 C32 -179.4(9) . . . . ? C29 C28 C33 C32 -1.4(13) . . . . ? C28 N3 C34 N4 0.1(8) . . . . ? C27 N3 C34 N4 178.1(6) . . . . ? C28 N3 C34 Ag2 178.0(5) . . . . ? C27 N3 C34 Ag2 -4.0(11) . . . . ? C29 N4 C34 N3 0.9(9) . . . . ? C35 N4 C34 N3 176.2(7) . . . . ? C29 N4 C34 Ag2 -177.2(5) . . . . ? C35 N4 C34 Ag2 -1.8(11) . . . . ? C7 Ag2 C34 N3 -125.9(18) . . . . ? Ag1 Ag2 C34 N3 85.0(7) . . . . ? C7 Ag2 C34 N4 52(2) . . . . ? Ag1 Ag2 C34 N4 -97.5(6) . . . . ? C34 N4 C35 C36 -100.7(10) . . . . ? C29 N4 C35 C36 74.0(11) . . . . ? N4 C35 C36 C37 56.2(12) . . . . ? C35 C36 C37 C38 -177.3(15) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.273 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.157 # Attachment '- complex 4.cif' data_090916a _database_code_depnum_ccdc_archive 'CCDC 818681' #TrackingRef '- complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H40 Ag2 Cl2 N4 O2' _chemical_formula_weight 859.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8829(11) _cell_length_b 19.1733(18) _cell_length_c 17.7442(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.147(2) _cell_angle_gamma 90.00 _cell_volume 3605.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5923 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.78 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.718 _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 18333 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6363 _reflns_number_gt 4625 _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^)+(0.0372P)^2^+3.6459P] 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 6363 _refine_ls_number_parameters 453 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.017 _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 0.60054(3) 0.032298(17) 0.093951(18) 0.06757(12) Uani 1 1 d . . . Ag2 Ag 1.32934(4) 0.008023(19) 0.38732(3) 0.09007(15) Uani 1 1 d . . . Cl1 Cl 0.64920(12) -0.06883(6) 0.03063(7) 0.0826(3) Uani 1 1 d . . . Cl2 Cl 1.39767(18) -0.08648(8) 0.47006(9) 0.1178(5) Uani 1 1 d . . . O1 O 0.8372(2) 0.25437(14) 0.14434(14) 0.0616(7) Uani 1 1 d . . . O2 O 1.0522(2) 0.23794(14) 0.34501(14) 0.0595(7) Uani 1 1 d . . . N1 N 0.5972(3) 0.10556(18) 0.24947(17) 0.0570(8) Uani 1 1 d . . . N2 N 0.5981(3) 0.18210(16) 0.16047(16) 0.0504(7) Uani 1 1 d . . . N3 N 1.2854(3) 0.15827(16) 0.32852(18) 0.0551(8) Uani 1 1 d . A . N4 N 1.2798(3) 0.0897(2) 0.2311(2) 0.0800(12) Uani 1 1 d D . . C1 C 0.8309(5) 0.0169(4) 0.2898(3) 0.117(2) Uani 1 1 d . . . H1A H 0.8109 -0.0186 0.2508 0.176 Uiso 1 1 calc R . . H1B H 0.9107 0.0065 0.3240 0.176 Uiso 1 1 calc R . . H1C H 0.8358 0.0613 0.2656 0.176 Uiso 1 1 calc R . . C2 C 0.7302(4) 0.0193(3) 0.3350(3) 0.0831(14) Uani 1 1 d . . . H2A H 0.7249 -0.0262 0.3579 0.100 Uiso 1 1 calc R . . H2B H 0.7553 0.0525 0.3769 0.100 Uiso 1 1 calc R . . C3 C 0.6020(4) 0.0390(2) 0.2890(2) 0.0701(12) Uani 1 1 d . . . H3A H 0.5724 0.0029 0.2509 0.084 Uiso 1 1 calc R . . H3B H 0.5445 0.0406 0.3235 0.084 Uiso 1 1 calc R . . C4 C 0.6023(3) 0.1708(2) 0.2851(2) 0.0585(10) Uani 1 1 d . . . C5 C 0.6073(4) 0.1900(3) 0.3618(2) 0.0763(14) Uani 1 1 d . . . H5 H 0.6059 0.1573 0.4003 0.092 Uiso 1 1 calc R . . C6 C 0.6143(4) 0.2609(4) 0.3765(3) 0.0895(17) Uani 1 1 d . . . H6 H 0.6185 0.2762 0.4268 0.107 Uiso 1 1 calc R . . C7 C 0.6155(4) 0.3098(3) 0.3199(3) 0.0876(15) Uani 1 1 d . . . H7 H 0.6208 0.3568 0.3329 0.105 Uiso 1 1 calc R . . C8 C 0.6091(4) 0.2906(2) 0.2442(3) 0.0699(12) Uani 1 1 d . . . H8 H 0.6090 0.3236 0.2058 0.084 Uiso 1 1 calc R . . C9 C 0.6027(3) 0.2196(2) 0.2282(2) 0.0552(9) Uani 1 1 d . . . C10 C 0.5946(3) 0.1132(2) 0.1731(2) 0.0538(9) Uani 1 1 d . . . C11 C 0.5932(3) 0.2128(2) 0.0840(2) 0.0565(9) Uani 1 1 d . . . H11A H 0.5947 0.2632 0.0886 0.068 Uiso 1 1 calc R . . H11B H 0.5142 0.1998 0.0492 0.068 Uiso 1 1 calc R . . C12 C 0.7002(3) 0.18996(19) 0.0498(2) 0.0516(9) Uani 1 1 d . . . C13 C 0.8237(3) 0.2118(2) 0.0816(2) 0.0520(9) Uani 1 1 d . . . C14 C 0.9210(4) 0.1904(2) 0.0481(2) 0.0669(11) Uani 1 1 d . . . H14 H 1.0030 0.2058 0.0681 0.080 Uiso 1 1 calc R . . C15 C 0.8958(5) 0.1464(2) -0.0145(3) 0.0779(13) Uani 1 1 d . . . H15 H 0.9618 0.1307 -0.0354 0.093 Uiso 1 1 calc R . . C16 C 0.7749(5) 0.1253(2) -0.0468(3) 0.0780(13) Uani 1 1 d . . . H16 H 0.7583 0.0967 -0.0903 0.094 Uiso 1 1 calc R . . C17 C 0.6786(4) 0.1471(2) -0.0141(2) 0.0655(11) Uani 1 1 d . . . H17 H 0.5967 0.1324 -0.0356 0.079 Uiso 1 1 calc R . . C18 C 0.9618(4) 0.2808(2) 0.1777(2) 0.0659(11) Uani 1 1 d . . . H18A H 0.9895 0.3116 0.1415 0.079 Uiso 1 1 calc R . . H18B H 1.0215 0.2427 0.1903 0.079 Uiso 1 1 calc R . . C19 C 0.9536(4) 0.3201(2) 0.2501(2) 0.0700(12) Uani 1 1 d . . . H19A H 1.0303 0.3471 0.2673 0.084 Uiso 1 1 calc R . . H19B H 0.8837 0.3527 0.2375 0.084 Uiso 1 1 calc R . . C20 C 0.9359(4) 0.2746(2) 0.3156(2) 0.0641(11) Uani 1 1 d . . . H20A H 0.9144 0.3028 0.3561 0.077 Uiso 1 1 calc R . . H20B H 0.8679 0.2416 0.2974 0.077 Uiso 1 1 calc R . . C21 C 1.0544(3) 0.1908(2) 0.4028(2) 0.0528(9) Uani 1 1 d . . . C22 C 0.9498(4) 0.1726(2) 0.4312(2) 0.0655(11) Uani 1 1 d . . . H22 H 0.8724 0.1938 0.4115 0.079 Uiso 1 1 calc R . . C23 C 0.9608(4) 0.1230(3) 0.4886(3) 0.0753(12) Uani 1 1 d . . . H23 H 0.8899 0.1099 0.5061 0.090 Uiso 1 1 calc R . . C24 C 1.0744(5) 0.0927(2) 0.5200(3) 0.0794(13) Uani 1 1 d . . . H24 H 1.0812 0.0594 0.5588 0.095 Uiso 1 1 calc R . . C25 C 1.1793(4) 0.1122(2) 0.4933(2) 0.0685(11) Uani 1 1 d . . . H25 H 1.2570 0.0921 0.5152 0.082 Uiso 1 1 calc R . . C26 C 1.1717(3) 0.16082(19) 0.4349(2) 0.0529(9) Uani 1 1 d . . . C27 C 1.2874(3) 0.1822(2) 0.4072(2) 0.0559(9) Uani 1 1 d . . . H27A H 1.2941 0.2326 0.4088 0.067 Uiso 1 1 calc R . . H27B H 1.3616 0.1634 0.4422 0.067 Uiso 1 1 calc R . . C28 C 1.2817(3) 0.2009(2) 0.2648(2) 0.0548(9) Uani 1 1 d . . . C29 C 1.2841(4) 0.2728(2) 0.2568(2) 0.0659(11) Uani 1 1 d . A . H29 H 1.2873 0.3024 0.2987 0.079 Uiso 1 1 calc R . . C30 C 1.2815(4) 0.2982(3) 0.1839(3) 0.0842(14) Uani 1 1 d . . . H30 H 1.2826 0.3462 0.1767 0.101 Uiso 1 1 calc R A . C31 C 1.2772(4) 0.2553(4) 0.1217(3) 0.0975(18) Uani 1 1 d . A . H31 H 1.2753 0.2750 0.0735 0.117 Uiso 1 1 calc R . . C32 C 1.2758(4) 0.1838(4) 0.1281(3) 0.0915(17) Uani 1 1 d . . . H32 H 1.2736 0.1547 0.0859 0.110 Uiso 1 1 calc R A . C33 C 1.2779(4) 0.1574(3) 0.2024(3) 0.0705(12) Uani 1 1 d . A . C34 C 1.2865(4) 0.0904(2) 0.3088(3) 0.0693(12) Uani 1 1 d . A . C35 C 1.2678(7) 0.0365(5) 0.1689(5) 0.062(3) Uani 0.537(11) 1 d PD A 1 H35A H 1.2919 -0.0088 0.1919 0.074 Uiso 0.537(11) 1 calc PR A 1 H35B H 1.3247 0.0480 0.1359 0.074 Uiso 0.537(11) 1 calc PR A 1 C36 C 1.1328(8) 0.0331(5) 0.1202(5) 0.075(3) Uani 0.537(11) 1 d PD A 1 H36A H 1.1116 0.0776 0.0946 0.090 Uiso 0.537(11) 1 calc PR A 1 H36B H 1.1284 -0.0022 0.0805 0.090 Uiso 0.537(11) 1 calc PR A 1 C37 C 1.0351(10) 0.0161(13) 0.1671(10) 0.133(8) Uani 0.537(11) 1 d PD A 1 H37A H 0.9526 0.0148 0.1333 0.200 Uiso 0.537(11) 1 calc PR A 1 H37B H 1.0372 0.0513 0.2058 0.200 Uiso 0.537(11) 1 calc PR A 1 H37C H 1.0540 -0.0285 0.1917 0.200 Uiso 0.537(11) 1 calc PR A 1 C35' C 1.2646(9) 0.0148(5) 0.2031(8) 0.068(4) Uani 0.463(11) 1 d PD A 2 H35C H 1.3227 -0.0140 0.2397 0.082 Uiso 0.463(11) 1 calc PR A 2 H35D H 1.2894 0.0121 0.1540 0.082 Uiso 0.463(11) 1 calc PR A 2 C36' C 1.1313(10) -0.0165(5) 0.1923(6) 0.084(4) Uani 0.463(11) 1 d PD A 2 H36C H 1.1335 -0.0645 0.1755 0.101 Uiso 0.463(11) 1 calc PR A 2 H36D H 1.1084 -0.0169 0.2420 0.101 Uiso 0.463(11) 1 calc PR A 2 C37' C 1.0297(12) 0.0223(10) 0.1344(10) 0.097(7) Uani 0.463(11) 1 d PD A 2 H37D H 0.9494 0.0005 0.1318 0.146 Uiso 0.463(11) 1 calc PR A 2 H37E H 1.0491 0.0210 0.0843 0.146 Uiso 0.463(11) 1 calc PR A 2 H37F H 1.0264 0.0699 0.1506 0.146 Uiso 0.463(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 Ag1 0.0745(2) 0.0681(2) 0.0605(2) -0.00657(15) 0.01616(15) -0.01107(16) Ag2 0.0894(3) 0.0617(2) 0.1318(4) 0.0000(2) 0.0514(3) 0.00493(19) Cl1 0.0840(8) 0.0805(8) 0.0779(8) -0.0164(6) 0.0074(6) -0.0001(6) Cl2 0.1509(14) 0.0841(9) 0.1195(12) 0.0063(8) 0.0331(10) -0.0091(9) O1 0.0407(14) 0.0834(19) 0.0549(16) 0.0013(14) -0.0010(11) -0.0008(13) O2 0.0410(14) 0.0763(18) 0.0557(16) 0.0025(14) -0.0008(11) 0.0078(12) N1 0.0429(17) 0.077(2) 0.0513(19) 0.0076(17) 0.0106(14) 0.0029(15) N2 0.0384(16) 0.063(2) 0.0488(18) 0.0015(15) 0.0071(13) 0.0021(14) N3 0.0416(17) 0.060(2) 0.063(2) -0.0059(16) 0.0102(14) 0.0019(14) N4 0.050(2) 0.099(3) 0.090(3) -0.043(2) 0.0137(19) 0.006(2) C1 0.083(4) 0.169(6) 0.106(4) 0.042(4) 0.036(3) 0.049(4) C2 0.070(3) 0.101(4) 0.077(3) 0.025(3) 0.013(2) 0.014(3) C3 0.061(3) 0.091(3) 0.060(3) 0.016(2) 0.016(2) -0.003(2) C4 0.0338(19) 0.089(3) 0.052(2) -0.004(2) 0.0078(16) 0.0077(19) C5 0.040(2) 0.133(4) 0.055(3) -0.001(3) 0.0084(18) 0.017(3) C6 0.057(3) 0.139(5) 0.069(3) -0.039(3) 0.007(2) 0.025(3) C7 0.063(3) 0.102(4) 0.092(4) -0.034(3) 0.006(3) 0.020(3) C8 0.047(2) 0.081(3) 0.079(3) -0.011(2) 0.008(2) 0.012(2) C9 0.0337(19) 0.077(3) 0.053(2) -0.006(2) 0.0067(16) 0.0067(17) C10 0.0373(19) 0.072(3) 0.051(2) 0.0040(18) 0.0070(16) -0.0015(17) C11 0.047(2) 0.068(2) 0.050(2) 0.0086(18) 0.0008(17) 0.0000(18) C12 0.049(2) 0.057(2) 0.048(2) 0.0089(17) 0.0081(17) 0.0022(17) C13 0.047(2) 0.063(2) 0.044(2) 0.0094(18) 0.0065(16) 0.0039(17) C14 0.051(2) 0.084(3) 0.067(3) 0.014(2) 0.015(2) 0.002(2) C15 0.084(3) 0.080(3) 0.081(3) 0.006(3) 0.041(3) 0.012(3) C16 0.092(4) 0.074(3) 0.073(3) -0.011(2) 0.030(3) -0.007(3) C17 0.069(3) 0.067(3) 0.061(3) 0.007(2) 0.016(2) -0.010(2) C18 0.047(2) 0.080(3) 0.065(3) 0.011(2) -0.0004(19) -0.006(2) C19 0.054(3) 0.063(3) 0.082(3) 0.002(2) -0.010(2) 0.0018(19) C20 0.048(2) 0.076(3) 0.061(2) -0.007(2) -0.0053(18) 0.011(2) C21 0.043(2) 0.063(2) 0.048(2) -0.0073(18) 0.0022(16) 0.0004(17) C22 0.048(2) 0.085(3) 0.061(3) -0.009(2) 0.0054(19) 0.001(2) C23 0.067(3) 0.089(3) 0.071(3) -0.004(3) 0.018(2) -0.014(2) C24 0.078(3) 0.079(3) 0.082(3) 0.015(2) 0.017(3) 0.003(3) C25 0.062(3) 0.073(3) 0.067(3) 0.007(2) 0.008(2) 0.010(2) C26 0.046(2) 0.057(2) 0.053(2) -0.0073(18) 0.0054(17) 0.0022(17) C27 0.045(2) 0.066(2) 0.052(2) -0.0036(18) 0.0016(17) 0.0050(18) C28 0.035(2) 0.073(3) 0.055(2) -0.008(2) 0.0076(16) 0.0029(17) C29 0.047(2) 0.080(3) 0.068(3) 0.001(2) 0.0059(19) -0.001(2) C30 0.057(3) 0.111(4) 0.084(4) 0.022(3) 0.014(2) 0.000(3) C31 0.050(3) 0.169(6) 0.074(4) 0.025(4) 0.015(2) 0.013(3) C32 0.040(2) 0.171(6) 0.061(3) -0.023(3) 0.008(2) 0.014(3) C33 0.036(2) 0.100(4) 0.072(3) -0.019(3) 0.0056(19) 0.010(2) C34 0.042(2) 0.065(3) 0.104(4) -0.016(2) 0.021(2) 0.0041(19) C35 0.065(5) 0.067(6) 0.057(6) -0.011(5) 0.022(5) 0.004(4) C36 0.065(6) 0.067(5) 0.090(7) -0.020(5) 0.011(5) -0.001(4) C37 0.055(9) 0.22(2) 0.123(16) -0.012(13) 0.013(8) -0.051(10) C35' 0.069(7) 0.091(9) 0.055(7) -0.023(6) 0.032(6) 0.006(6) C36' 0.087(9) 0.077(7) 0.089(8) -0.015(6) 0.026(7) -0.006(6) C37' 0.121(16) 0.084(9) 0.081(11) 0.004(8) 0.011(9) 0.008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C10 2.103(4) . ? Ag1 Cl1 2.3608(12) . ? Ag2 C34 2.087(5) . ? Ag2 Cl2 2.3441(16) . ? O1 C13 1.362(4) . ? O1 C18 1.443(4) . ? O2 C21 1.362(4) . ? O2 C20 1.438(4) . ? N1 C10 1.357(4) . ? N1 C4 1.396(5) . ? N1 C3 1.452(5) . ? N2 C10 1.343(5) . ? N2 C9 1.392(5) . ? N2 C11 1.469(4) . ? N3 C34 1.349(5) . ? N3 C28 1.387(5) . ? N3 C27 1.465(5) . ? N4 C34 1.364(6) . ? N4 C33 1.393(6) . ? N4 C35 1.485(7) . ? N4 C35' 1.515(8) . ? C1 C2 1.498(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.496(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.377(5) . ? C4 C5 1.399(6) . ? C5 C6 1.382(7) . ? C5 H5 0.9300 . ? C6 C7 1.377(7) . ? C6 H6 0.9300 . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C8 C9 1.390(6) . ? C8 H8 0.9300 . ? C11 C12 1.495(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.377(5) . ? C12 C13 1.398(5) . ? C13 C14 1.388(5) . ? C14 C15 1.373(6) . ? C14 H14 0.9300 . ? C15 C16 1.371(7) . ? C15 H15 0.9300 . ? C16 C17 1.374(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.509(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.502(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.391(5) . ? C21 C26 1.398(5) . ? C22 C23 1.378(6) . ? C22 H22 0.9300 . ? C23 C24 1.364(6) . ? C23 H23 0.9300 . ? C24 C25 1.383(6) . ? C24 H24 0.9300 . ? C25 C26 1.382(5) . ? C25 H25 0.9300 . ? C26 C27 1.509(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C33 1.381(5) . ? C28 C29 1.387(6) . ? C29 C30 1.377(6) . ? C29 H29 0.9300 . ? C30 C31 1.370(8) . ? C30 H30 0.9300 . ? C31 C32 1.375(8) . ? C31 H31 0.9300 . ? C32 C33 1.407(7) . ? C32 H32 0.9300 . ? C35 C36 1.527(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.526(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C35' C36' 1.540(9) . ? C35' H35C 0.9700 . ? C35' H35D 0.9700 . ? C36' C37' 1.522(9) . ? C36' H36C 0.9700 . ? C36' H36D 0.9700 . ? C37' H37D 0.9600 . ? C37' H37E 0.9600 . ? C37' H37F 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 C10 Ag1 Cl1 165.42(10) . . ? C34 Ag2 Cl2 173.56(12) . . ? C13 O1 C18 117.6(3) . . ? C21 O2 C20 117.4(3) . . ? C10 N1 C4 110.2(3) . . ? C10 N1 C3 124.6(4) . . ? C4 N1 C3 125.1(3) . . ? C10 N2 C9 111.2(3) . . ? C10 N2 C11 123.5(3) . . ? C9 N2 C11 125.3(3) . . ? C34 N3 C28 110.9(3) . . ? C34 N3 C27 123.4(4) . . ? C28 N3 C27 125.7(3) . . ? C34 N4 C33 110.7(3) . . ? C34 N4 C35 137.1(6) . . ? C33 N4 C35 112.1(6) . . ? C34 N4 C35' 108.5(6) . . ? C33 N4 C35' 140.5(6) . . ? C35 N4 C35' 28.6(4) . . ? 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 115.0(4) . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N1 C3 C2 114.3(4) . . ? N1 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C9 C4 N1 106.5(3) . . ? C9 C4 C5 121.8(4) . . ? N1 C4 C5 131.7(4) . . ? C6 C5 C4 115.6(5) . . ? C6 C5 H5 122.2 . . ? C4 C5 H5 122.2 . . ? C7 C6 C5 122.7(5) . . ? C7 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C6 C7 C8 121.5(5) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C9 116.7(5) . . ? C7 C8 H8 121.7 . . ? C9 C8 H8 121.7 . . ? C4 C9 C8 121.7(4) . . ? C4 C9 N2 106.0(4) . . ? C8 C9 N2 132.3(4) . . ? N2 C10 N1 106.1(3) . . ? N2 C10 Ag1 127.4(3) . . ? N1 C10 Ag1 126.2(3) . . ? N2 C11 C12 112.9(3) . . ? N2 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C17 C12 C13 118.6(4) . . ? C17 C12 C11 120.4(3) . . ? C13 C12 C11 121.0(3) . . ? O1 C13 C14 125.2(3) . . ? O1 C13 C12 115.1(3) . . ? C14 C13 C12 119.8(4) . . ? C15 C14 C13 119.8(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.1(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C12 121.7(4) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? O1 C18 C19 107.1(3) . . ? O1 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? O1 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C20 C19 C18 114.3(4) . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? C18 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? O2 C20 C19 107.9(3) . . ? O2 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O2 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O2 C21 C22 124.3(3) . . ? O2 C21 C26 116.0(3) . . ? C22 C21 C26 119.7(4) . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 121.7(4) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C21 118.5(4) . . ? C25 C26 C27 121.0(3) . . ? C21 C26 C27 120.5(3) . . ? N3 C27 C26 113.2(3) . . ? N3 C27 H27A 108.9 . . ? C26 C27 H27A 108.9 . . ? N3 C27 H27B 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.8 . . ? C33 C28 N3 106.8(4) . . ? C33 C28 C29 121.1(4) . . ? N3 C28 C29 132.2(4) . . ? C30 C29 C28 116.8(4) . . ? C30 C29 H29 121.6 . . ? C28 C29 H29 121.6 . . ? C31 C30 C29 122.3(5) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 C32 122.0(5) . . ? C30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C31 C32 C33 116.0(5) . . ? C31 C32 H32 122.0 . . ? C33 C32 H32 122.0 . . ? C28 C33 N4 105.9(4) . . ? C28 C33 C32 121.7(5) . . ? N4 C33 C32 132.4(5) . . ? N3 C34 N4 105.7(4) . . ? N3 C34 Ag2 124.8(3) . . ? N4 C34 Ag2 128.3(3) . . ? N4 C35 C36 111.1(6) . . ? N4 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N4 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C37 C36 C35 113.6(7) . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C35' C36' 116.0(7) . . ? N4 C35' H35C 108.3 . . ? C36' C35' H35C 108.3 . . ? N4 C35' H35D 108.3 . . ? C36' C35' H35D 108.3 . . ? H35C C35' H35D 107.4 . . ? C37' C36' C35' 114.4(8) . . ? C37' C36' H36C 108.7 . . ? C35' C36' H36C 108.7 . . ? C37' C36' H36D 108.7 . . ? C35' C36' H36D 108.7 . . ? H36C C36' H36D 107.6 . . ? C36' C37' H37D 109.5 . . ? C36' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C36' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 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 C10 N1 C3 C2 101.0(5) . . . . ? C4 N1 C3 C2 -75.0(5) . . . . ? C1 C2 C3 N1 -56.6(6) . . . . ? C10 N1 C4 C9 0.0(4) . . . . ? C3 N1 C4 C9 176.5(3) . . . . ? C10 N1 C4 C5 -179.5(4) . . . . ? C3 N1 C4 C5 -3.1(6) . . . . ? C9 C4 C5 C6 -0.9(6) . . . . ? N1 C4 C5 C6 178.6(4) . . . . ? C4 C5 C6 C7 0.5(6) . . . . ? C5 C6 C7 C8 0.3(7) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? N1 C4 C9 C8 -179.1(3) . . . . ? C5 C4 C9 C8 0.6(6) . . . . ? N1 C4 C9 N2 -0.2(4) . . . . ? C5 C4 C9 N2 179.5(3) . . . . ? C7 C8 C9 C4 0.2(6) . . . . ? C7 C8 C9 N2 -178.4(4) . . . . ? C10 N2 C9 C4 0.2(4) . . . . ? C11 N2 C9 C4 178.2(3) . . . . ? C10 N2 C9 C8 179.0(4) . . . . ? C11 N2 C9 C8 -3.1(6) . . . . ? C9 N2 C10 N1 -0.2(4) . . . . ? C11 N2 C10 N1 -178.2(3) . . . . ? C9 N2 C10 Ag1 -175.1(2) . . . . ? C11 N2 C10 Ag1 6.9(5) . . . . ? C4 N1 C10 N2 0.1(4) . . . . ? C3 N1 C10 N2 -176.4(3) . . . . ? C4 N1 C10 Ag1 175.1(2) . . . . ? C3 N1 C10 Ag1 -1.4(5) . . . . ? Cl1 Ag1 C10 N2 127.8(4) . . . . ? Cl1 Ag1 C10 N1 -46.1(6) . . . . ? C10 N2 C11 C12 -60.3(4) . . . . ? C9 N2 C11 C12 122.0(4) . . . . ? N2 C11 C12 C17 111.3(4) . . . . ? N2 C11 C12 C13 -69.0(5) . . . . ? C18 O1 C13 C14 1.6(5) . . . . ? C18 O1 C13 C12 -177.6(3) . . . . ? C17 C12 C13 O1 179.6(3) . . . . ? C11 C12 C13 O1 -0.1(5) . . . . ? C17 C12 C13 C14 0.5(5) . . . . ? C11 C12 C13 C14 -179.3(3) . . . . ? O1 C13 C14 C15 179.1(4) . . . . ? C12 C13 C14 C15 -1.8(6) . . . . ? C13 C14 C15 C16 2.7(7) . . . . ? C14 C15 C16 C17 -2.1(7) . . . . ? C15 C16 C17 C12 0.7(7) . . . . ? C13 C12 C17 C16 0.1(6) . . . . ? C11 C12 C17 C16 179.8(4) . . . . ? C13 O1 C18 C19 -174.5(3) . . . . ? O1 C18 C19 C20 71.1(4) . . . . ? C21 O2 C20 C19 -176.9(3) . . . . ? C18 C19 C20 O2 71.2(4) . . . . ? C20 O2 C21 C22 4.6(5) . . . . ? C20 O2 C21 C26 -174.4(3) . . . . ? O2 C21 C22 C23 178.3(4) . . . . ? C26 C21 C22 C23 -2.7(6) . . . . ? C21 C22 C23 C24 2.1(7) . . . . ? C22 C23 C24 C25 -0.3(7) . . . . ? C23 C24 C25 C26 -0.9(7) . . . . ? C24 C25 C26 C21 0.3(6) . . . . ? C24 C25 C26 C27 179.2(4) . . . . ? O2 C21 C26 C25 -179.4(3) . . . . ? C22 C21 C26 C25 1.5(5) . . . . ? O2 C21 C26 C27 1.6(5) . . . . ? C22 C21 C26 C27 -177.4(3) . . . . ? C34 N3 C27 C26 -64.0(4) . . . . ? C28 N3 C27 C26 115.7(4) . . . . ? C25 C26 C27 N3 111.3(4) . . . . ? C21 C26 C27 N3 -69.8(4) . . . . ? C34 N3 C28 C33 1.2(4) . . . . ? C27 N3 C28 C33 -178.6(3) . . . . ? C34 N3 C28 C29 -177.2(4) . . . . ? C27 N3 C28 C29 3.1(6) . . . . ? C33 C28 C29 C30 0.5(6) . . . . ? N3 C28 C29 C30 178.7(4) . . . . ? C28 C29 C30 C31 -0.3(6) . . . . ? C29 C30 C31 C32 -0.2(7) . . . . ? C30 C31 C32 C33 0.5(7) . . . . ? N3 C28 C33 N4 -0.1(4) . . . . ? C29 C28 C33 N4 178.4(3) . . . . ? N3 C28 C33 C32 -178.8(3) . . . . ? C29 C28 C33 C32 -0.2(6) . . . . ? C34 N4 C33 C28 -0.9(4) . . . . ? C35 N4 C33 C28 176.4(4) . . . . ? C35' N4 C33 C28 171.4(7) . . . . ? C34 N4 C33 C32 177.6(4) . . . . ? C35 N4 C33 C32 -5.2(7) . . . . ? C35' N4 C33 C32 -10.1(10) . . . . ? C31 C32 C33 C28 -0.3(6) . . . . ? C31 C32 C33 N4 -178.5(4) . . . . ? C28 N3 C34 N4 -1.7(4) . . . . ? C27 N3 C34 N4 178.0(3) . . . . ? C28 N3 C34 Ag2 166.6(3) . . . . ? C27 N3 C34 Ag2 -13.7(5) . . . . ? C33 N4 C34 N3 1.6(4) . . . . ? C35 N4 C34 N3 -174.7(6) . . . . ? C35' N4 C34 N3 -173.2(5) . . . . ? C33 N4 C34 Ag2 -166.1(3) . . . . ? C35 N4 C34 Ag2 17.6(8) . . . . ? C35' N4 C34 Ag2 19.1(6) . . . . ? Cl2 Ag2 C34 N3 -113.7(11) . . . . ? Cl2 Ag2 C34 N4 51.8(14) . . . . ? C34 N4 C35 C36 102.0(8) . . . . ? C33 N4 C35 C36 -74.3(8) . . . . ? C35' N4 C35 C36 99.1(14) . . . . ? N4 C35 C36 C37 -58.3(14) . . . . ? C34 N4 C35' C36' 78.0(10) . . . . ? C33 N4 C35' C36' -94.4(11) . . . . ? C35 N4 C35' C36' -104.1(16) . . . . ? N4 C35' C36' C37' 59.6(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.002 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.057 data_complex _database_code_depnum_ccdc_archive 'CCDC 818682' #TrackingRef '- complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H44 Ag2 Cl2 N4 O2' _chemical_formula_weight 887.42 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' Cl Cl 0.1484 0.1585 '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 10.9386(5) _cell_length_b 21.6466(11) _cell_length_c 16.7369(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.3440(10) _cell_angle_gamma 90.00 _cell_volume 3821.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6300 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.805 _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 9526 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3369 _reflns_number_gt 2910 _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^)+(0.1390P)^2^+35.0215P] 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 3348 _refine_ls_number_parameters 223 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.2289 _refine_ls_wR_factor_gt 0.2216 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.63098(6) 0.02752(3) 0.10892(4) 0.0625(3) Uani 1 1 d . . . Cl1 Cl 0.62174(15) -0.07368(7) 0.04633(10) 0.0474(4) Uani 1 1 d U . . O1 O 0.8859(5) 0.2297(3) 0.1454(3) 0.0587(13) Uani 1 1 d . . . N1 N 0.6605(5) 0.1054(3) 0.2679(4) 0.0484(13) Uani 1 1 d . . . N2 N 0.6539(5) 0.1663(3) 0.1645(3) 0.0454(12) Uani 1 1 d . . . C1 C 0.6650(6) 0.1658(3) 0.2984(4) 0.0482(16) Uani 1 1 d . . . C2 C 0.6616(6) 0.2038(3) 0.2316(4) 0.0470(15) Uani 1 1 d . . . C3 C 0.6638(7) 0.2681(4) 0.2401(5) 0.0567(18) Uani 1 1 d . . . H3 H 0.6603 0.2942 0.1954 0.068 Uiso 1 1 calc R . . C4 C 0.6712(8) 0.2911(4) 0.3187(6) 0.067(2) Uani 1 1 d . . . H4 H 0.6745 0.3336 0.3271 0.081 Uiso 1 1 calc R . . C5 C 0.6740(8) 0.2518(4) 0.3853(5) 0.063(2) Uani 1 1 d . . . H5 H 0.6784 0.2688 0.4370 0.075 Uiso 1 1 calc R . . C6 C 0.6702(7) 0.1894(4) 0.3766(5) 0.0559(18) Uani 1 1 d . . . H6 H 0.6712 0.1635 0.4211 0.067 Uiso 1 1 calc R . . C7 C 0.6526(6) 0.1051(3) 0.1868(4) 0.0495(16) Uani 1 1 d . . . C8 C 0.6710(7) 0.0513(4) 0.3204(5) 0.0564(17) Uani 1 1 d . . . H8A H 0.6459 0.0151 0.2858 0.068 Uiso 1 1 calc R . . H8B H 0.6129 0.0555 0.3550 0.068 Uiso 1 1 calc R . . C9 C 0.8050(8) 0.0416(4) 0.3758(5) 0.0588(18) Uani 1 1 d . . . H9A H 0.8340 0.0796 0.4055 0.071 Uiso 1 1 calc R . . H9B H 0.8030 0.0099 0.4163 0.071 Uiso 1 1 calc R . . C10 C 0.8986(9) 0.0228(5) 0.3273(6) 0.076(3) Uani 1 1 d . . . H10A H 0.8681 -0.0145 0.2963 0.091 Uiso 1 1 calc R . . H10B H 0.9020 0.0551 0.2878 0.091 Uiso 1 1 calc R . . C11 C 1.0315(9) 0.0113(5) 0.3817(7) 0.080(3) Uani 1 1 d . . . H11A H 1.0653 0.0490 0.4090 0.120 Uiso 1 1 calc R . . H11B H 1.0847 -0.0028 0.3480 0.120 Uiso 1 1 calc R . . H11C H 1.0287 -0.0195 0.4224 0.120 Uiso 1 1 calc R . . C12 C 0.6411(7) 0.1868(4) 0.0791(4) 0.0508(16) Uani 1 1 d . . . H12A H 0.6314 0.2314 0.0772 0.061 Uiso 1 1 calc R . . H12B H 0.5639 0.1693 0.0439 0.061 Uiso 1 1 calc R . . C13 C 0.7492(7) 0.1702(3) 0.0435(4) 0.0505(16) Uani 1 1 d . . . C14 C 0.8713(7) 0.1936(3) 0.0767(4) 0.0501(16) Uani 1 1 d . . . C15 C 0.9675(8) 0.1802(4) 0.0395(5) 0.062(2) Uani 1 1 d . . . H15 H 1.0493 0.1946 0.0628 0.075 Uiso 1 1 calc R . . C16 C 0.9414(10) 0.1457(4) -0.0318(6) 0.072(2) Uani 1 1 d . . . H16 H 1.0056 0.1378 -0.0573 0.086 Uiso 1 1 calc R . . C17 C 0.8220(10) 0.1226(4) -0.0660(5) 0.071(2) Uani 1 1 d . . . H17 H 0.8060 0.0985 -0.1137 0.085 Uiso 1 1 calc R . . C18 C 0.7251(9) 0.1354(4) -0.0286(5) 0.0607(19) Uani 1 1 d . . . H18 H 0.6437 0.1206 -0.0521 0.073 Uiso 1 1 calc R . . C19 C 1.0061(7) 0.2601(4) 0.1763(5) 0.063(2) Uani 1 1 d . . . H19A H 1.0229 0.2871 0.1342 0.075 Uiso 1 1 calc R . . H19B H 1.0736 0.2298 0.1914 0.075 Uiso 1 1 calc R . . C20 C 1.0000 0.2967(6) 0.2500 0.068(3) Uani 1 2 d S . . H20A H 0.9260 0.3232 0.2348 0.082 Uiso 0.50 1 calc PR . . H20B H 1.0740 0.3232 0.2652 0.082 Uiso 0.50 1 calc PR . . 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 0.0611(5) 0.0621(5) 0.0676(5) -0.0139(3) 0.0227(3) -0.0082(3) Cl1 0.0493(9) 0.0398(8) 0.0494(9) -0.0196(6) 0.0065(7) -0.0046(6) O1 0.046(3) 0.071(3) 0.055(3) -0.003(2) 0.007(2) -0.002(2) N1 0.041(3) 0.054(3) 0.050(3) 0.001(3) 0.011(2) 0.000(2) N2 0.039(3) 0.053(3) 0.042(3) 0.000(2) 0.007(2) 0.000(2) C1 0.033(3) 0.059(4) 0.051(4) 0.003(3) 0.008(3) 0.005(3) C2 0.035(3) 0.059(4) 0.046(3) 0.001(3) 0.009(3) 0.006(3) C3 0.057(4) 0.054(4) 0.056(4) 0.002(3) 0.010(3) 0.006(3) C4 0.064(5) 0.065(5) 0.070(5) -0.014(4) 0.010(4) 0.012(4) C5 0.057(4) 0.075(5) 0.052(4) -0.012(4) 0.007(3) 0.015(4) C6 0.045(4) 0.074(5) 0.049(4) 0.002(3) 0.013(3) 0.009(3) C7 0.039(3) 0.057(4) 0.051(4) -0.002(3) 0.008(3) -0.002(3) C8 0.056(4) 0.054(4) 0.063(5) 0.008(3) 0.023(3) -0.003(3) C9 0.062(5) 0.055(4) 0.060(4) 0.009(3) 0.016(4) 0.008(4) C10 0.061(5) 0.113(8) 0.059(5) 0.017(5) 0.022(4) 0.010(5) C11 0.061(5) 0.093(7) 0.088(7) 0.010(5) 0.021(5) 0.012(5) C12 0.044(3) 0.061(4) 0.045(4) 0.005(3) 0.006(3) 0.006(3) C13 0.059(4) 0.048(4) 0.044(4) 0.009(3) 0.014(3) 0.007(3) C14 0.047(4) 0.051(4) 0.050(4) 0.007(3) 0.010(3) 0.004(3) C15 0.059(5) 0.062(5) 0.069(5) 0.012(4) 0.025(4) 0.003(4) C16 0.083(6) 0.067(5) 0.080(6) 0.012(5) 0.047(5) 0.011(5) C17 0.106(7) 0.059(5) 0.055(5) 0.004(4) 0.035(5) 0.008(5) C18 0.079(5) 0.055(4) 0.049(4) 0.003(3) 0.017(4) 0.000(4) C19 0.047(4) 0.070(5) 0.065(5) 0.005(4) 0.003(3) -0.007(4) C20 0.058(6) 0.060(7) 0.076(8) 0.000 -0.002(6) 0.000 _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 2.100(7) . ? Ag1 Cl1 2.4187(15) . ? O1 C14 1.364(9) . ? O1 C19 1.439(9) . ? N1 C7 1.337(9) . ? N1 C1 1.398(10) . ? N1 C8 1.452(10) . ? N2 C2 1.370(9) . ? N2 C7 1.377(9) . ? N2 C12 1.467(9) . ? C1 C2 1.381(10) . ? C1 C6 1.393(11) . ? C2 C3 1.400(11) . ? C3 C4 1.388(12) . ? C3 H3 0.9300 . ? C4 C5 1.397(13) . ? C4 H4 0.9300 . ? C5 C6 1.358(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.527(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.520(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.518(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.503(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.386(10) . ? C13 C14 1.399(11) . ? C14 C15 1.387(11) . ? C15 C16 1.373(13) . ? C15 H15 0.9300 . ? C16 C17 1.374(14) . ? C16 H16 0.9300 . ? C17 C18 1.395(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.481(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C19 1.481(11) 2_755 ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? 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 Cl1 167.9(2) . . ? C14 O1 C19 117.2(6) . . ? C7 N1 C1 111.2(6) . . ? C7 N1 C8 125.8(6) . . ? C1 N1 C8 122.9(6) . . ? C2 N2 C7 110.5(6) . . ? C2 N2 C12 126.0(6) . . ? C7 N2 C12 123.4(6) . . ? C2 C1 C6 121.9(7) . . ? C2 C1 N1 105.7(6) . . ? C6 C1 N1 132.5(7) . . ? N2 C2 C1 107.1(6) . . ? N2 C2 C3 132.0(7) . . ? C1 C2 C3 121.0(7) . . ? C4 C3 C2 116.6(8) . . ? C4 C3 H3 121.7 . . ? C2 C3 H3 121.7 . . ? C3 C4 C5 121.5(8) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 121.8(8) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 117.3(8) . . ? C5 C6 H6 121.3 . . ? C1 C6 H6 121.3 . . ? N1 C7 N2 105.5(6) . . ? N1 C7 Ag1 126.9(5) . . ? N2 C7 Ag1 127.5(5) . . ? N1 C8 C9 112.8(6) . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 112.8(7) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 113.5(8) . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? 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 115.6(6) . . ? N2 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? N2 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C18 C13 C14 119.0(7) . . ? C18 C13 C12 119.1(7) . . ? C14 C13 C12 121.6(7) . . ? O1 C14 C15 124.3(7) . . ? O1 C14 C13 115.4(6) . . ? C15 C14 C13 120.2(7) . . ? C16 C15 C14 119.7(8) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.1(8) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.4(8) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 120.4(8) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? O1 C19 C20 107.8(6) . . ? O1 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? O1 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.5 . . ? C19 C20 C19 115.5(11) . 2_755 ? C19 C20 H20A 108.4 . . ? C19 C20 H20A 108.4 2_755 . ? C19 C20 H20B 108.4 . . ? C19 C20 H20B 108.4 2_755 . ? H20A C20 H20B 107.5 . . ? 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 -0.9(7) . . . . ? C8 N1 C1 C2 175.6(6) . . . . ? C7 N1 C1 C6 178.2(7) . . . . ? C8 N1 C1 C6 -5.3(11) . . . . ? C7 N2 C2 C1 -0.2(7) . . . . ? C12 N2 C2 C1 176.5(6) . . . . ? C7 N2 C2 C3 -178.8(7) . . . . ? C12 N2 C2 C3 -2.2(12) . . . . ? C6 C1 C2 N2 -178.6(6) . . . . ? N1 C1 C2 N2 0.7(7) . . . . ? C6 C1 C2 C3 0.2(10) . . . . ? N1 C1 C2 C3 179.5(6) . . . . ? N2 C2 C3 C4 179.4(7) . . . . ? C1 C2 C3 C4 0.9(11) . . . . ? C2 C3 C4 C5 -1.2(12) . . . . ? C3 C4 C5 C6 0.4(13) . . . . ? C4 C5 C6 C1 0.7(12) . . . . ? C2 C1 C6 C5 -1.0(10) . . . . ? N1 C1 C6 C5 179.9(7) . . . . ? C1 N1 C7 N2 0.8(7) . . . . ? C8 N1 C7 N2 -175.6(6) . . . . ? C1 N1 C7 Ag1 -175.6(5) . . . . ? C8 N1 C7 Ag1 8.0(10) . . . . ? C2 N2 C7 N1 -0.4(7) . . . . ? C12 N2 C7 N1 -177.1(5) . . . . ? C2 N2 C7 Ag1 176.0(5) . . . . ? C12 N2 C7 Ag1 -0.8(9) . . . . ? Cl1 Ag1 C7 N1 -18.8(14) . . . . ? Cl1 Ag1 C7 N2 165.6(5) . . . . ? C7 N1 C8 C9 104.0(8) . . . . ? C1 N1 C8 C9 -71.9(9) . . . . ? N1 C8 C9 C10 -69.3(9) . . . . ? C8 C9 C10 C11 -178.4(8) . . . . ? C2 N2 C12 C13 116.8(7) . . . . ? C7 N2 C12 C13 -66.9(9) . . . . ? N2 C12 C13 C18 122.2(7) . . . . ? N2 C12 C13 C14 -63.8(9) . . . . ? C19 O1 C14 C15 5.8(10) . . . . ? C19 O1 C14 C13 -173.5(6) . . . . ? C18 C13 C14 O1 177.0(6) . . . . ? C12 C13 C14 O1 3.0(10) . . . . ? C18 C13 C14 C15 -2.3(10) . . . . ? C12 C13 C14 C15 -176.3(7) . . . . ? O1 C14 C15 C16 -176.9(7) . . . . ? C13 C14 C15 C16 2.3(11) . . . . ? C14 C15 C16 C17 -1.8(13) . . . . ? C15 C16 C17 C18 1.3(13) . . . . ? C14 C13 C18 C17 1.8(11) . . . . ? C12 C13 C18 C17 175.9(7) . . . . ? C16 C17 C18 C13 -1.3(12) . . . . ? C14 O1 C19 C20 179.7(7) . . . . ? O1 C19 C20 C19 68.6(5) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.616 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.150