Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Metal-Organic Coordination Architectures of 9,10-Bis(N-benzimidazoly)anthracene: Syntheses, Structures and Emission Properties ; loop_ _publ_author_name 'Xian-He Bu.' 'Tong-Liang Hu.' 'Lei Li.' 'Jian-Rong Li.' 'Duo-Zhi Wang.' ; Yong-Fei Zeng ; data_L _database_code_depnum_ccdc_archive 'CCDC 635086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 N4' _chemical_formula_weight 410.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 16.017(4) _cell_length_b 10.324(3) _cell_length_c 12.342(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.048(5) _cell_angle_gamma 90.00 _cell_volume 1979.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1266 _cell_measurement_theta_min 2.6050 _cell_measurement_theta_max 23.0369 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.982 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD area detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9867 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3494 _reflns_number_gt 1756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SHELXTL (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 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^)+(0.0467P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3494 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 N1 N 0.31516(14) 0.35365(19) 0.31549(18) 0.0364(6) Uani 1 1 d . . . C2 C 0.22287(16) -0.0198(2) 0.2095(2) 0.0305(7) Uani 1 1 d . . . C3 C 0.22534(17) 0.2129(2) 0.1742(2) 0.0325(7) Uani 1 1 d . . . C4 C 0.28219(17) 0.2265(2) 0.2792(2) 0.0331(7) Uani 1 1 d . . . C5 C 0.19291(17) 0.0864(2) 0.1398(2) 0.0310(7) Uani 1 1 d . . . N2 N 0.18999(14) -0.14722(19) 0.17528(18) 0.0334(6) Uani 1 1 d . . . C7 C 0.31090(17) 0.1213(2) 0.3503(2) 0.0306(7) Uani 1 1 d . . . C8 C 0.28133(16) -0.0063(2) 0.3131(2) 0.0307(7) Uani 1 1 d . . . C9 C 0.36773(18) 0.1348(3) 0.4584(2) 0.0411(8) Uani 1 1 d . . . H9A H 0.3854 0.2169 0.4853 0.049 Uiso 1 1 calc R . . N3 N 0.16522(16) -0.3337(2) 0.07836(19) 0.0456(7) Uani 1 1 d . . . C11 C 0.31375(17) -0.1139(3) 0.3833(2) 0.0378(7) Uani 1 1 d . . . H11A H 0.2964 -0.1973 0.3596 0.045 Uiso 1 1 calc R . . C12 C 0.11736(18) -0.3318(2) 0.1587(2) 0.0351(7) Uani 1 1 d . . . N4 N 0.31609(16) 0.5619(2) 0.3677(2) 0.0488(7) Uani 1 1 d . . . C14 C 0.13095(17) 0.0743(3) 0.0352(2) 0.0400(8) Uani 1 1 d . . . H14A H 0.1073 -0.0064 0.0125 0.048 Uiso 1 1 calc R . . C15 C 0.13249(17) -0.2174(2) 0.2207(2) 0.0310(7) Uani 1 1 d . . . C16 C 0.39626(18) 0.0295(3) 0.5222(2) 0.0470(8) Uani 1 1 d . . . H16A H 0.4339 0.0401 0.5920 0.056 Uiso 1 1 calc R . . C17 C 0.19915(18) 0.3194(3) 0.0995(2) 0.0418(8) Uani 1 1 d . . . H17A H 0.2219 0.4013 0.1193 0.050 Uiso 1 1 calc R . . C18 C 0.47182(19) 0.3353(3) 0.3112(2) 0.0396(7) Uani 1 1 d . . . H18A H 0.4714 0.2484 0.2913 0.047 Uiso 1 1 calc R . . C19 C 0.36937(18) -0.0960(3) 0.4837(2) 0.0460(8) Uani 1 1 d . . . H19A H 0.3902 -0.1674 0.5280 0.055 Uiso 1 1 calc R . . C20 C 0.10609(18) 0.1789(3) -0.0316(2) 0.0464(8) Uani 1 1 d . . . H20A H 0.0652 0.1692 -0.0989 0.056 Uiso 1 1 calc R . . C21 C 0.39885(18) 0.3967(2) 0.3254(2) 0.0326(7) Uani 1 1 d . . . C22 C 0.14182(19) 0.3022(3) 0.0005(3) 0.0484(8) Uani 1 1 d . . . H22A H 0.1256 0.3724 -0.0471 0.058 Uiso 1 1 calc R . . C23 C 0.09540(18) -0.1908(3) 0.3086(2) 0.0395(8) Uani 1 1 d . . . H23A H 0.1077 -0.1154 0.3506 0.047 Uiso 1 1 calc R . . C24 C 0.39826(19) 0.5274(2) 0.3576(2) 0.0365(7) Uani 1 1 d . . . C25 C 0.20598(19) -0.2229(3) 0.0914(2) 0.0422(8) Uani 1 1 d . . . H25A H 0.2427 -0.1976 0.0474 0.051 Uiso 1 1 calc R . . C26 C 0.27015(19) 0.4571(3) 0.3418(2) 0.0436(8) Uani 1 1 d . . . H26A H 0.2121 0.4528 0.3413 0.052 Uiso 1 1 calc R . . C27 C 0.4733(2) 0.6000(3) 0.3741(2) 0.0452(8) Uani 1 1 d . . . H27A H 0.4743 0.6868 0.3947 0.054 Uiso 1 1 calc R . . C28 C 0.06083(18) -0.4234(3) 0.1825(3) 0.0442(8) Uani 1 1 d . . . H28A H 0.0495 -0.5001 0.1422 0.053 Uiso 1 1 calc R . . C29 C 0.5461(2) 0.5392(3) 0.3590(2) 0.0490(9) Uani 1 1 d . . . H29A H 0.5971 0.5861 0.3698 0.059 Uiso 1 1 calc R . . C30 C 0.02214(19) -0.3962(3) 0.2683(3) 0.0493(9) Uani 1 1 d . . . H30A H -0.0165 -0.4555 0.2854 0.059 Uiso 1 1 calc R . . C31 C 0.5456(2) 0.4097(3) 0.3280(2) 0.0459(8) Uani 1 1 d . . . H31A H 0.5961 0.3722 0.3184 0.055 Uiso 1 1 calc R . . C32 C 0.03928(19) -0.2828(3) 0.3298(3) 0.0487(8) Uani 1 1 d . . . H32A H 0.0120 -0.2685 0.3873 0.058 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 N1 0.0333(15) 0.0253(13) 0.0502(16) -0.0048(11) 0.0092(12) -0.0022(11) C2 0.0314(17) 0.0228(15) 0.0369(17) -0.0029(13) 0.0079(14) -0.0019(12) C3 0.0297(17) 0.0319(16) 0.0364(17) 0.0028(13) 0.0086(14) 0.0007(13) C4 0.0315(17) 0.0232(15) 0.0444(18) -0.0042(13) 0.0088(15) -0.0018(13) C5 0.0294(17) 0.0312(16) 0.0323(17) -0.0009(13) 0.0072(13) 0.0021(13) N2 0.0395(15) 0.0249(13) 0.0368(14) -0.0052(11) 0.0112(12) -0.0030(11) C7 0.0331(17) 0.0263(16) 0.0316(17) -0.0037(13) 0.0063(14) -0.0014(13) C8 0.0306(17) 0.0262(15) 0.0348(17) -0.0012(13) 0.0069(14) -0.0017(12) C9 0.043(2) 0.0380(18) 0.0396(19) -0.0055(15) 0.0050(15) -0.0025(14) N3 0.0572(18) 0.0331(15) 0.0457(16) -0.0107(12) 0.0111(14) -0.0057(13) C11 0.0402(19) 0.0270(16) 0.0438(19) 0.0024(14) 0.0057(15) 0.0004(13) C12 0.0376(19) 0.0276(16) 0.0358(17) -0.0017(14) 0.0005(14) 0.0010(14) N4 0.0436(17) 0.0282(15) 0.0743(19) -0.0040(13) 0.0139(14) 0.0000(12) C14 0.0393(19) 0.0378(18) 0.0414(19) -0.0040(15) 0.0068(15) -0.0008(14) C15 0.0307(17) 0.0256(15) 0.0347(17) -0.0001(13) 0.0039(14) -0.0018(13) C16 0.044(2) 0.049(2) 0.0420(19) -0.0007(16) -0.0007(15) -0.0031(16) C17 0.0383(19) 0.0304(17) 0.056(2) 0.0071(15) 0.0106(16) 0.0010(14) C18 0.043(2) 0.0332(17) 0.0407(18) -0.0008(14) 0.0076(15) 0.0019(15) C19 0.044(2) 0.0428(19) 0.047(2) 0.0126(16) 0.0036(16) 0.0005(15) C20 0.044(2) 0.052(2) 0.0387(19) 0.0039(16) 0.0018(15) 0.0068(16) C21 0.0330(19) 0.0274(16) 0.0357(17) 0.0011(13) 0.0052(14) -0.0035(13) C22 0.045(2) 0.047(2) 0.050(2) 0.0116(16) 0.0064(17) 0.0067(16) C23 0.045(2) 0.0321(17) 0.0412(18) -0.0026(14) 0.0111(15) -0.0003(14) C24 0.041(2) 0.0263(16) 0.0412(18) 0.0002(13) 0.0075(15) -0.0032(14) C25 0.052(2) 0.0357(18) 0.0405(19) -0.0083(15) 0.0151(16) 0.0003(15) C26 0.0413(19) 0.0288(17) 0.062(2) -0.0036(15) 0.0154(16) 0.0017(15) C27 0.049(2) 0.0275(16) 0.057(2) 0.0006(14) 0.0096(17) -0.0089(15) C28 0.041(2) 0.0276(17) 0.058(2) -0.0021(15) -0.0004(17) -0.0060(14) C29 0.045(2) 0.044(2) 0.055(2) 0.0085(16) 0.0077(17) -0.0156(17) C30 0.041(2) 0.043(2) 0.063(2) 0.0104(17) 0.0102(18) -0.0109(15) C31 0.039(2) 0.049(2) 0.051(2) 0.0058(16) 0.0151(16) 0.0025(16) C32 0.051(2) 0.0459(19) 0.052(2) 0.0042(17) 0.0181(17) -0.0041(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C26 1.371(3) . ? N1 C21 1.389(3) . ? N1 C4 1.445(3) . ? C2 C8 1.397(3) . ? C2 C5 1.404(3) . ? C2 N2 1.441(3) . ? C3 C4 1.399(3) . ? C3 C17 1.430(3) . ? C3 C5 1.431(3) . ? C4 C7 1.402(3) . ? C5 C14 1.430(3) . ? N2 C25 1.370(3) . ? N2 C15 1.392(3) . ? C7 C9 1.427(3) . ? C7 C8 1.437(3) . ? C8 C11 1.426(3) . ? C9 C16 1.355(3) . ? N3 C25 1.308(3) . ? N3 C12 1.393(3) . ? C11 C19 1.352(4) . ? C12 C28 1.389(4) . ? C12 C15 1.396(3) . ? N4 C26 1.304(3) . ? N4 C24 1.398(3) . ? C14 C20 1.358(3) . ? C15 C23 1.385(3) . ? C16 C19 1.411(4) . ? C17 C22 1.350(4) . ? C18 C21 1.377(3) . ? C18 C31 1.382(4) . ? C20 C22 1.413(4) . ? C21 C24 1.408(3) . ? C23 C32 1.376(4) . ? C24 C27 1.389(4) . ? C27 C29 1.377(4) . ? C28 C30 1.380(4) . ? C29 C31 1.391(4) . ? C30 C32 1.386(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 N1 C21 106.4(2) . . ? C26 N1 C4 127.4(2) . . ? C21 N1 C4 126.2(2) . . ? C8 C2 C5 122.4(2) . . ? C8 C2 N2 118.4(2) . . ? C5 C2 N2 119.1(2) . . ? C4 C3 C17 122.9(3) . . ? C4 C3 C5 118.3(2) . . ? C17 C3 C5 118.8(3) . . ? C3 C4 C7 122.9(2) . . ? C3 C4 N1 119.0(2) . . ? C7 C4 N1 118.1(2) . . ? C2 C5 C14 122.9(2) . . ? C2 C5 C3 119.0(2) . . ? C14 C5 C3 118.0(2) . . ? C25 N2 C15 105.7(2) . . ? C25 N2 C2 128.3(2) . . ? C15 N2 C2 126.0(2) . . ? C4 C7 C9 123.2(2) . . ? C4 C7 C8 118.5(2) . . ? C9 C7 C8 118.3(2) . . ? C2 C8 C11 122.8(2) . . ? C2 C8 C7 118.7(2) . . ? C11 C8 C7 118.5(2) . . ? C16 C9 C7 120.9(3) . . ? C25 N3 C12 104.2(2) . . ? C19 C11 C8 120.8(3) . . ? C28 C12 N3 129.9(3) . . ? C28 C12 C15 119.7(3) . . ? N3 C12 C15 110.5(2) . . ? C26 N4 C24 104.7(2) . . ? C20 C14 C5 121.0(3) . . ? C23 C15 N2 131.6(2) . . ? C23 C15 C12 123.1(3) . . ? N2 C15 C12 105.3(2) . . ? C9 C16 C19 120.5(3) . . ? C22 C17 C3 120.7(3) . . ? C21 C18 C31 116.5(3) . . ? C11 C19 C16 120.9(3) . . ? C14 C20 C22 120.5(3) . . ? C18 C21 N1 132.3(2) . . ? C18 C21 C24 122.7(3) . . ? N1 C21 C24 105.0(2) . . ? C17 C22 C20 120.8(3) . . ? C32 C23 C15 115.9(3) . . ? C27 C24 N4 130.5(3) . . ? C27 C24 C21 119.6(3) . . ? N4 C24 C21 109.9(2) . . ? N3 C25 N2 114.4(3) . . ? N4 C26 N1 114.0(3) . . ? C29 C27 C24 117.7(3) . . ? C30 C28 C12 117.5(3) . . ? C27 C29 C31 121.8(3) . . ? C28 C30 C32 121.8(3) . . ? C18 C31 C29 121.5(3) . . ? C23 C32 C30 122.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.185 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.045 #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 635087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H20 Cl3 Cu I N4 O0.50' _chemical_formula_weight 729.28 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.177(2) _cell_length_b 11.855(2) _cell_length_c 13.009(3) _cell_angle_alpha 100.42(3) _cell_angle_beta 100.30(3) _cell_angle_gamma 115.33(3) _cell_volume 1336.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3483 _cell_measurement_theta_min 1.6621 _cell_measurement_theta_max 27.8286 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 2.303 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6819 _exptl_absorpt_correction_T_max 0.8024 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12577 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6234 _reflns_number_gt 4830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+1.5689P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0127(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6234 _refine_ls_number_parameters 367 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Cu1 Cu -0.06746(8) -0.09287(7) 0.40396(5) 0.0263(2) Uani 1 1 d . . . I1 I 0.13114(4) 0.15029(4) 0.42107(3) 0.03227(18) Uani 1 1 d . . . N1 N 0.0157(6) -0.2082(5) 0.3338(4) 0.0311(11) Uani 1 1 d . . . N2 N 0.0553(5) -0.3343(5) 0.2066(3) 0.0252(10) Uani 1 1 d . . . N3 N -0.2556(5) -0.1383(5) 0.2810(3) 0.0230(9) Uani 1 1 d . . . N4 N -0.3977(5) -0.1226(4) 0.1371(3) 0.0203(9) Uani 1 1 d . . . C1 C -0.0388(7) -0.2879(6) 0.2351(5) 0.0309(13) Uani 1 1 d . . . H1A H -0.1327 -0.3107 0.1886 0.037 Uiso 1 1 calc R . . C2 C 0.1554(7) -0.2025(7) 0.3756(5) 0.0343(14) Uani 1 1 d . . . C3 C 0.2615(9) -0.1336(9) 0.4759(5) 0.055(2) Uani 1 1 d . . . H3A H 0.2469 -0.0792 0.5285 0.067 Uiso 1 1 calc R . . C4 C 0.3903(9) -0.1482(11) 0.4954(5) 0.070(3) Uani 1 1 d . . . H4A H 0.4617 -0.1057 0.5637 0.083 Uiso 1 1 calc R . . C5 C 0.4165(8) -0.2257(8) 0.4146(5) 0.048(2) Uani 1 1 d . . . H5A H 0.5060 -0.2312 0.4298 0.058 Uiso 1 1 calc R . . C6 C 0.3133(6) -0.2926(6) 0.3148(5) 0.0294(13) Uani 1 1 d . . . H6A H 0.3301 -0.3439 0.2611 0.035 Uiso 1 1 calc R . . C7 C 0.1831(6) -0.2812(6) 0.2968(4) 0.0259(12) Uani 1 1 d . . . C8 C 0.0281(6) -0.4189(6) 0.1017(4) 0.0232(11) Uani 1 1 d . . . C9 C 0.0108(6) -0.5438(5) 0.0946(4) 0.0234(11) Uani 1 1 d . . . C10 C 0.0227(6) -0.5919(6) 0.1873(5) 0.0302(12) Uani 1 1 d . . . H10A H 0.0410 -0.5390 0.2560 0.036 Uiso 1 1 calc R . . C11 C 0.0077(7) -0.7136(6) 0.1769(5) 0.0350(14) Uani 1 1 d . . . H11A H 0.0183 -0.7424 0.2383 0.042 Uiso 1 1 calc R . . C12 C -0.0236(7) -0.7953(6) 0.0734(5) 0.0349(14) Uani 1 1 d . . . H12A H -0.0361 -0.8790 0.0672 0.042 Uiso 1 1 calc R . . C13 C -0.0364(6) -0.7564(6) -0.0181(5) 0.0301(13) Uani 1 1 d . . . H13A H -0.0567 -0.8130 -0.0854 0.036 Uiso 1 1 calc R . . C14 C -0.0186(6) -0.6284(6) -0.0114(4) 0.0241(11) Uani 1 1 d . . . C15 C -0.2753(6) -0.0582(6) 0.2280(4) 0.0235(11) Uani 1 1 d . . . H15A H -0.2128 0.0316 0.2504 0.028 Uiso 1 1 calc R . . C16 C -0.3738(6) -0.2627(5) 0.2220(4) 0.0215(10) Uani 1 1 d . . . C17 C -0.4087(7) -0.3815(6) 0.2416(5) 0.0282(12) Uani 1 1 d . . . H17A H -0.3513 -0.3879 0.3023 0.034 Uiso 1 1 calc R . . C18 C -0.5321(7) -0.4904(6) 0.1673(5) 0.0346(14) Uani 1 1 d . . . H18A H -0.5580 -0.5717 0.1783 0.042 Uiso 1 1 calc R . . C19 C -0.6196(7) -0.4816(6) 0.0758(5) 0.0308(13) Uani 1 1 d . . . H19A H -0.7015 -0.5573 0.0274 0.037 Uiso 1 1 calc R . . C20 C -0.5874(6) -0.3641(6) 0.0556(5) 0.0291(12) Uani 1 1 d . . . H20A H -0.6456 -0.3581 -0.0049 0.035 Uiso 1 1 calc R . . C21 C -0.4632(6) -0.2546(5) 0.1308(4) 0.0228(11) Uani 1 1 d . . . C22 C -0.4511(6) -0.0618(5) 0.0660(4) 0.0221(11) Uani 1 1 d . . . C23 C -0.5399(6) -0.0063(5) 0.0992(4) 0.0213(10) Uani 1 1 d . . . C24 C -0.4172(6) 0.0125(6) -0.1972(4) 0.0273(12) Uani 1 1 d . . . H24A H -0.4468 0.0556 -0.2417 0.033 Uiso 1 1 calc R . . C25 C -0.3320(6) -0.0453(7) -0.2260(5) 0.0310(13) Uani 1 1 d . . . H25A H -0.3042 -0.0405 -0.2900 0.037 Uiso 1 1 calc R . . C26 C -0.2865(6) -0.1116(6) -0.1604(4) 0.0295(13) Uani 1 1 d . . . H26A H -0.2301 -0.1509 -0.1819 0.035 Uiso 1 1 calc R . . C27 C -0.3245(6) -0.1189(6) -0.0647(4) 0.0256(11) Uani 1 1 d . . . H27A H -0.2936 -0.1630 -0.0219 0.031 Uiso 1 1 calc R . . C28 C -0.4113(6) -0.0590(5) -0.0309(4) 0.0223(11) Uani 1 1 d . . . C29 C 0.2742(12) -0.3845(11) 0.5850(9) 0.210(13) Uani 1 1 d D . . Cl3 Cl 0.4386(9) -0.4014(8) 0.5833(6) 0.224(4) Uani 1 1 d D A . Cl2 Cl 0.288(3) -0.378(2) 0.7248(13) 0.252(15) Uani 0.402(13) 1 d PD A 1 Cl1 Cl 0.085(3) -0.485(7) 0.499(5) 0.54(4) Uiso 0.402(13) 1 d PD . 1 Cl1' Cl 0.1393(9) -0.5513(5) 0.5479(7) 0.153(5) Uani 0.598(13) 1 d PD A 2 Cl2' Cl 0.2939(7) -0.3198(12) 0.7236(5) 0.138(4) Uani 0.598(13) 1 d PD A 2 O1 O -0.067(2) -0.653(2) 0.4282(14) 0.120(8) Uani 0.50 1 d P B 3 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 Cu1 0.0293(4) 0.0443(4) 0.0144(3) 0.0054(3) 0.0046(3) 0.0273(3) I1 0.0324(2) 0.0521(3) 0.0207(2) 0.01306(17) 0.01041(16) 0.0254(2) N1 0.032(2) 0.051(3) 0.019(2) 0.002(2) 0.0069(19) 0.030(2) N2 0.024(2) 0.038(3) 0.017(2) 0.0013(19) 0.0059(18) 0.021(2) N3 0.027(2) 0.034(3) 0.017(2) 0.0071(18) 0.0043(18) 0.023(2) N4 0.022(2) 0.028(2) 0.015(2) 0.0070(17) 0.0014(16) 0.0158(18) C1 0.025(3) 0.049(4) 0.022(3) 0.001(2) 0.003(2) 0.026(3) C2 0.039(3) 0.058(4) 0.021(3) 0.009(3) 0.008(2) 0.037(3) C3 0.061(5) 0.095(6) 0.016(3) -0.011(3) -0.005(3) 0.059(5) C4 0.061(5) 0.133(9) 0.019(3) -0.016(4) -0.013(3) 0.074(6) C5 0.045(4) 0.081(6) 0.030(3) 0.000(3) -0.002(3) 0.051(4) C6 0.030(3) 0.045(4) 0.023(3) 0.006(2) 0.010(2) 0.027(3) C7 0.025(3) 0.038(3) 0.020(3) 0.007(2) 0.007(2) 0.019(2) C8 0.019(2) 0.037(3) 0.017(2) 0.001(2) 0.0032(19) 0.019(2) C9 0.018(2) 0.029(3) 0.021(3) 0.001(2) 0.003(2) 0.013(2) C10 0.029(3) 0.038(3) 0.024(3) 0.011(2) 0.007(2) 0.015(3) C11 0.031(3) 0.036(3) 0.034(3) 0.010(3) 0.004(3) 0.015(3) C12 0.031(3) 0.032(3) 0.043(3) 0.011(3) 0.003(3) 0.019(3) C13 0.025(3) 0.032(3) 0.031(3) 0.005(2) 0.000(2) 0.017(2) C14 0.020(2) 0.031(3) 0.022(3) 0.003(2) 0.001(2) 0.017(2) C15 0.018(2) 0.031(3) 0.019(2) 0.001(2) 0.000(2) 0.014(2) C16 0.019(2) 0.034(3) 0.015(2) 0.004(2) 0.0061(19) 0.016(2) C17 0.030(3) 0.037(3) 0.029(3) 0.011(2) 0.012(2) 0.024(3) C18 0.034(3) 0.036(3) 0.044(4) 0.014(3) 0.022(3) 0.021(3) C19 0.025(3) 0.032(3) 0.036(3) 0.005(2) 0.009(2) 0.016(2) C20 0.025(3) 0.039(3) 0.026(3) 0.004(2) 0.008(2) 0.019(2) C21 0.023(2) 0.032(3) 0.019(2) 0.007(2) 0.008(2) 0.018(2) C22 0.024(2) 0.028(3) 0.015(2) 0.003(2) 0.000(2) 0.017(2) C23 0.021(2) 0.033(3) 0.015(2) 0.007(2) 0.0061(19) 0.017(2) C24 0.026(3) 0.044(3) 0.018(3) 0.013(2) 0.009(2) 0.021(3) C25 0.026(3) 0.054(4) 0.021(3) 0.010(3) 0.009(2) 0.025(3) C26 0.026(3) 0.044(3) 0.020(3) 0.000(2) 0.005(2) 0.023(3) C27 0.023(2) 0.037(3) 0.021(3) 0.007(2) 0.004(2) 0.019(2) C28 0.020(2) 0.030(3) 0.017(2) 0.004(2) 0.0023(19) 0.014(2) C29 0.142(17) 0.33(4) 0.108(14) 0.008(18) 0.028(13) 0.10(2) Cl3 0.298(9) 0.338(10) 0.253(7) 0.204(7) 0.191(7) 0.252(9) Cl2 0.189(19) 0.21(2) 0.44(4) 0.12(2) 0.09(2) 0.157(19) Cl1' 0.153(6) 0.057(3) 0.178(7) 0.004(3) -0.078(5) 0.049(4) Cl2' 0.056(3) 0.171(9) 0.108(5) -0.028(4) 0.037(3) 0.007(4) O1 0.202(19) 0.21(2) 0.130(13) 0.152(15) 0.146(14) 0.186(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.056(4) . ? Cu1 N1 2.058(5) . ? Cu1 I1 2.6029(10) 2_556 ? Cu1 I1 2.6580(14) . ? Cu1 Cu1 2.6782(19) 2_556 ? I1 Cu1 2.6029(10) 2_556 ? N1 C1 1.307(7) . ? N1 C2 1.397(7) . ? N2 C1 1.364(7) . ? N2 C7 1.397(7) . ? N2 C8 1.441(7) . ? N3 C15 1.329(7) . ? N3 C16 1.397(7) . ? N4 C15 1.366(6) . ? N4 C21 1.394(7) . ? N4 C22 1.437(7) . ? C1 H1A 0.9300 . ? C2 C3 1.374(8) . ? C2 C7 1.408(8) . ? C3 C4 1.380(9) . ? C3 H3A 0.9300 . ? C4 C5 1.407(9) . ? C4 H4A 0.9300 . ? C5 C6 1.358(8) . ? C5 H5A 0.9300 . ? C6 C7 1.372(7) . ? C6 H6A 0.9300 . ? C8 C14 1.395(8) 2_545 ? C8 C9 1.399(8) . ? C9 C10 1.431(8) . ? C9 C14 1.446(7) . ? C10 C11 1.364(9) . ? C10 H10A 0.9300 . ? C11 C12 1.401(9) . ? C11 H11A 0.9300 . ? C12 C13 1.357(9) . ? C12 H12A 0.9300 . ? C13 C14 1.434(8) . ? C13 H13A 0.9300 . ? C14 C8 1.395(8) 2_545 ? C15 H15A 0.9300 . ? C16 C17 1.382(8) . ? C16 C21 1.405(7) . ? C17 C18 1.380(8) . ? C17 H17A 0.9300 . ? C18 C19 1.402(9) . ? C18 H18A 0.9300 . ? C19 C20 1.375(9) . ? C19 H19A 0.9300 . ? C20 C21 1.391(8) . ? C20 H20A 0.9300 . ? C22 C28 1.394(7) . ? C22 C23 1.408(7) . ? C23 C24 1.422(7) 2_455 ? C23 C28 1.433(7) 2_455 ? C24 C25 1.376(8) . ? C24 C23 1.422(7) 2_455 ? C24 H24A 0.9300 . ? C25 C26 1.405(9) . ? C25 H25A 0.9300 . ? C26 C27 1.374(8) . ? C26 H26A 0.9300 . ? C27 C28 1.429(7) . ? C27 H27A 0.9300 . ? C28 C23 1.433(7) 2_455 ? C29 Cl2' 1.765(9) . ? C29 Cl1' 1.767(10) . ? C29 Cl3 1.772(9) . ? C29 Cl1 1.776(10) . ? C29 Cl2 1.783(10) . ? Cl1 Cl1 1.62(9) 2_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N1 102.33(18) . . ? N3 Cu1 I1 113.39(14) . 2_556 ? N1 Cu1 I1 109.94(15) . 2_556 ? N3 Cu1 I1 105.28(15) . . ? N1 Cu1 I1 105.58(17) . . ? I1 Cu1 I1 118.81(4) 2_556 . ? N3 Cu1 Cu1 130.34(13) . 2_556 ? N1 Cu1 Cu1 126.74(14) . 2_556 ? I1 Cu1 Cu1 60.42(4) 2_556 2_556 ? I1 Cu1 Cu1 58.39(4) . 2_556 ? Cu1 I1 Cu1 61.19(4) 2_556 . ? C1 N1 C2 105.0(5) . . ? C1 N1 Cu1 127.6(4) . . ? C2 N1 Cu1 126.7(4) . . ? C1 N2 C7 107.0(4) . . ? C1 N2 C8 125.8(4) . . ? C7 N2 C8 127.2(4) . . ? C15 N3 C16 105.5(4) . . ? C15 N3 Cu1 126.4(4) . . ? C16 N3 Cu1 127.0(4) . . ? C15 N4 C21 107.2(4) . . ? C15 N4 C22 125.2(5) . . ? C21 N4 C22 127.4(4) . . ? N1 C1 N2 113.6(5) . . ? N1 C1 H1A 123.2 . . ? N2 C1 H1A 123.2 . . ? C3 C2 N1 130.1(6) . . ? C3 C2 C7 119.7(5) . . ? N1 C2 C7 110.1(5) . . ? C2 C3 C4 117.4(6) . . ? C2 C3 H3A 121.3 . . ? C4 C3 H3A 121.3 . . ? C3 C4 C5 121.7(6) . . ? C3 C4 H4A 119.1 . . ? C5 C4 H4A 119.1 . . ? C6 C5 C4 121.2(6) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 117.0(5) . . ? C5 C6 H6A 121.5 . . ? C7 C6 H6A 121.5 . . ? C6 C7 N2 132.8(5) . . ? C6 C7 C2 122.9(5) . . ? N2 C7 C2 104.3(5) . . ? C14 C8 C9 123.2(5) 2_545 . ? C14 C8 N2 117.8(5) 2_545 . ? C9 C8 N2 119.1(5) . . ? C8 C9 C10 123.3(5) . . ? C8 C9 C14 118.5(5) . . ? C10 C9 C14 118.2(5) . . ? C11 C10 C9 121.3(6) . . ? C11 C10 H10A 119.3 . . ? C9 C10 H10A 119.3 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C13 C12 C11 122.1(6) . . ? C13 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C8 C14 C13 123.5(5) 2_545 . ? C8 C14 C9 118.3(5) 2_545 . ? C13 C14 C9 118.2(5) . . ? N3 C15 N4 112.4(5) . . ? N3 C15 H15A 123.8 . . ? N4 C15 H15A 123.8 . . ? C17 C16 N3 129.9(5) . . ? C17 C16 C21 120.6(5) . . ? N3 C16 C21 109.5(5) . . ? C18 C17 C16 117.3(5) . . ? C18 C17 H17A 121.4 . . ? C16 C17 H17A 121.4 . . ? C17 C18 C19 121.7(6) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C18 121.8(6) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C21 116.3(5) . . ? C19 C20 H20A 121.9 . . ? C21 C20 H20A 121.9 . . ? C20 C21 N4 132.3(5) . . ? C20 C21 C16 122.3(5) . . ? N4 C21 C16 105.3(4) . . ? C28 C22 C23 123.3(5) . . ? C28 C22 N4 118.9(5) . . ? C23 C22 N4 117.8(5) . . ? C22 C23 C24 122.8(5) . 2_455 ? C22 C23 C28 118.2(5) . 2_455 ? C24 C23 C28 119.1(5) 2_455 2_455 ? C25 C24 C23 120.0(5) . 2_455 ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 2_455 . ? C24 C25 C26 121.1(5) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C27 C26 C25 120.7(5) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 120.1(5) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C22 C28 C27 122.5(5) . . ? C22 C28 C23 118.5(5) . 2_455 ? C27 C28 C23 119.0(5) . 2_455 ? Cl2' C29 Cl1' 106.2(8) . . ? Cl2' C29 Cl3 106.0(7) . . ? Cl1' C29 Cl3 98.7(8) . . ? Cl2' C29 Cl1 116(2) . . ? Cl1' C29 Cl1 44(3) . . ? Cl3 C29 Cl1 129(3) . . ? Cl2' C29 Cl2 21.6(8) . . ? Cl1' C29 Cl2 89.0(11) . . ? Cl3 C29 Cl2 96.3(9) . . ? Cl1 C29 Cl2 112(2) . . ? Cl1 Cl1 C29 138(6) 2_546 . ? 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 N3 Cu1 I1 Cu1 128.30(13) . . . 2_556 ? N1 Cu1 I1 Cu1 -123.88(14) . . . 2_556 ? I1 Cu1 I1 Cu1 0.0 2_556 . . 2_556 ? N3 Cu1 N1 C1 0.9(6) . . . . ? I1 Cu1 N1 C1 121.7(6) 2_556 . . . ? I1 Cu1 N1 C1 -109.0(6) . . . . ? Cu1 Cu1 N1 C1 -170.9(5) 2_556 . . . ? N3 Cu1 N1 C2 169.9(5) . . . . ? I1 Cu1 N1 C2 -69.3(6) 2_556 . . . ? I1 Cu1 N1 C2 60.0(6) . . . . ? Cu1 Cu1 N1 C2 -1.9(6) 2_556 . . . ? N1 Cu1 N3 C15 -114.7(5) . . . . ? I1 Cu1 N3 C15 127.0(4) 2_556 . . . ? I1 Cu1 N3 C15 -4.5(5) . . . . ? Cu1 Cu1 N3 C15 56.8(5) 2_556 . . . ? N1 Cu1 N3 C16 51.9(5) . . . . ? I1 Cu1 N3 C16 -66.5(4) 2_556 . . . ? I1 Cu1 N3 C16 162.0(4) . . . . ? Cu1 Cu1 N3 C16 -136.7(4) 2_556 . . . ? C2 N1 C1 N2 -1.2(8) . . . . ? Cu1 N1 C1 N2 169.7(4) . . . . ? C7 N2 C1 N1 1.1(8) . . . . ? C8 N2 C1 N1 -177.1(6) . . . . ? C1 N1 C2 C3 179.8(9) . . . . ? Cu1 N1 C2 C3 8.8(12) . . . . ? C1 N1 C2 C7 0.8(8) . . . . ? Cu1 N1 C2 C7 -170.2(4) . . . . ? N1 C2 C3 C4 179.2(9) . . . . ? C7 C2 C3 C4 -1.8(13) . . . . ? C2 C3 C4 C5 2.9(16) . . . . ? C3 C4 C5 C6 -2.0(16) . . . . ? C4 C5 C6 C7 -0.1(12) . . . . ? C5 C6 C7 N2 180.0(7) . . . . ? C5 C6 C7 C2 1.1(10) . . . . ? C1 N2 C7 C6 -179.5(7) . . . . ? C8 N2 C7 C6 -1.3(11) . . . . ? C1 N2 C7 C2 -0.5(7) . . . . ? C8 N2 C7 C2 177.7(6) . . . . ? C3 C2 C7 C6 -0.2(11) . . . . ? N1 C2 C7 C6 179.0(6) . . . . ? C3 C2 C7 N2 -179.3(7) . . . . ? N1 C2 C7 N2 -0.2(7) . . . . ? C1 N2 C8 C14 62.9(8) . . . 2_545 ? C7 N2 C8 C14 -114.9(6) . . . 2_545 ? C1 N2 C8 C9 -116.4(7) . . . . ? C7 N2 C8 C9 65.8(8) . . . . ? C14 C8 C9 C10 179.1(5) 2_545 . . . ? N2 C8 C9 C10 -1.7(8) . . . . ? C14 C8 C9 C14 -0.2(9) 2_545 . . . ? N2 C8 C9 C14 179.1(5) . . . . ? C8 C9 C10 C11 -178.8(6) . . . . ? C14 C9 C10 C11 0.4(8) . . . . ? C9 C10 C11 C12 -1.6(9) . . . . ? C10 C11 C12 C13 1.6(10) . . . . ? C11 C12 C13 C14 -0.4(9) . . . . ? C12 C13 C14 C8 179.1(5) . . . 2_545 ? C12 C13 C14 C9 -0.8(8) . . . . ? C8 C9 C14 C8 0.2(8) . . . 2_545 ? C10 C9 C14 C8 -179.1(5) . . . 2_545 ? C8 C9 C14 C13 -179.9(5) . . . . ? C10 C9 C14 C13 0.8(7) . . . . ? C16 N3 C15 N4 -1.0(6) . . . . ? Cu1 N3 C15 N4 167.9(3) . . . . ? C21 N4 C15 N3 0.4(6) . . . . ? C22 N4 C15 N3 177.3(5) . . . . ? C15 N3 C16 C17 -179.1(5) . . . . ? Cu1 N3 C16 C17 12.1(8) . . . . ? C15 N3 C16 C21 1.2(6) . . . . ? Cu1 N3 C16 C21 -167.6(4) . . . . ? N3 C16 C17 C18 -178.7(5) . . . . ? C21 C16 C17 C18 1.1(8) . . . . ? C16 C17 C18 C19 -0.3(8) . . . . ? C17 C18 C19 C20 -0.4(9) . . . . ? C18 C19 C20 C21 0.2(8) . . . . ? C19 C20 C21 N4 179.8(6) . . . . ? C19 C20 C21 C16 0.6(8) . . . . ? C15 N4 C21 C20 -179.0(6) . . . . ? C22 N4 C21 C20 4.2(9) . . . . ? C15 N4 C21 C16 0.3(6) . . . . ? C22 N4 C21 C16 -176.5(5) . . . . ? C17 C16 C21 C20 -1.3(8) . . . . ? N3 C16 C21 C20 178.5(5) . . . . ? C17 C16 C21 N4 179.3(5) . . . . ? N3 C16 C21 N4 -0.9(6) . . . . ? C15 N4 C22 C28 99.3(6) . . . . ? C21 N4 C22 C28 -84.5(7) . . . . ? C15 N4 C22 C23 -79.9(7) . . . . ? C21 N4 C22 C23 96.4(6) . . . . ? C28 C22 C23 C24 178.5(5) . . . 2_455 ? N4 C22 C23 C24 -2.4(8) . . . 2_455 ? C28 C22 C23 C28 -1.5(9) . . . 2_455 ? N4 C22 C23 C28 177.6(5) . . . 2_455 ? C23 C24 C25 C26 0.3(9) 2_455 . . . ? C24 C25 C26 C27 -0.8(9) . . . . ? C25 C26 C27 C28 0.1(9) . . . . ? C23 C22 C28 C27 -178.3(5) . . . . ? N4 C22 C28 C27 2.6(8) . . . . ? C23 C22 C28 C23 1.5(9) . . . 2_455 ? N4 C22 C28 C23 -177.6(5) . . . 2_455 ? C26 C27 C28 C22 -179.1(5) . . . . ? C26 C27 C28 C23 1.2(8) . . . 2_455 ? Cl2' C29 Cl1 Cl1 17(13) . . . 2_546 ? Cl1' C29 Cl1 Cl1 104(13) . . . 2_546 ? Cl3 C29 Cl1 Cl1 160(10) . . . 2_546 ? Cl2 C29 Cl1 Cl1 41(13) . . . 2_546 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.566 _refine_diff_density_min -1.775 _refine_diff_density_rms 0.172 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 635088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H56 Cd N10 O10' _chemical_formula_weight 1237.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.163(10) _cell_length_b 15.442(9) _cell_length_c 12.133(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.534(8) _cell_angle_gamma 90.00 _cell_volume 2948(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3896 _cell_measurement_theta_min 2.5038 _cell_measurement_theta_max 26.3300 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9251 _exptl_absorpt_correction_T_max 0.9331 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7487 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2712 _reflns_number_gt 2379 _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^)+(0.1011P)^2^+1.8919P] 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 2712 _refine_ls_number_parameters 211 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.5000 0.0403(2) Uani 1 4 d S . . N1 N 0.02847(18) 0.11249(18) 0.6433(2) 0.0409(7) Uani 1 1 d . . . N2 N 0.10348(18) 0.19299(19) 0.8030(2) 0.0432(7) Uani 1 1 d . . . N3 N 0.1916(4) 0.0000 0.5150(5) 0.0608(13) Uani 1 2 d S . . C1 C 0.1007(2) 0.1213(2) 0.7360(3) 0.0421(8) Uani 1 1 d . . . H1A H 0.1456 0.0825 0.7544 0.050 Uiso 1 1 calc R . . C2 C -0.0210(2) 0.1834(2) 0.6465(3) 0.0410(8) Uani 1 1 d . . . C3 C -0.1025(2) 0.2095(3) 0.5673(4) 0.0537(10) Uani 1 1 d . . . H3A H -0.1340 0.1766 0.5000 0.064 Uiso 1 1 calc R . . C4 C -0.1340(3) 0.2851(3) 0.5924(5) 0.0765(14) Uani 1 1 d . . . H4A H -0.1873 0.3044 0.5401 0.092 Uiso 1 1 calc R . . C5 C -0.0877(3) 0.3339(4) 0.6952(5) 0.0937(19) Uani 1 1 d . . . H5A H -0.1117 0.3840 0.7106 0.112 Uiso 1 1 calc R . . C6 C -0.0070(3) 0.3093(3) 0.7744(5) 0.0797(16) Uani 1 1 d . . . H6A H 0.0239 0.3417 0.8426 0.096 Uiso 1 1 calc R . . C7 C 0.0249(2) 0.2342(2) 0.7469(3) 0.0476(9) Uani 1 1 d . . . C8 C 0.1773(2) 0.2230(2) 0.9039(3) 0.0396(8) Uani 1 1 d . . . C9 C 0.1883(2) 0.1961(2) 1.0190(3) 0.0421(8) Uani 1 1 d . . . C10 C 0.2651(2) 0.2231(2) 1.1191(3) 0.0415(8) Uani 1 1 d . . . C11 C 0.2784(3) 0.1928(3) 1.2365(3) 0.0583(10) Uani 1 1 d . . . H11A H 0.3276 0.2087 1.3018 0.070 Uiso 1 1 calc R . . C12 C 0.2206(3) 0.1415(4) 1.2538(4) 0.0745(13) Uani 1 1 d . . . H12A H 0.2313 0.1208 1.3332 0.089 Uiso 1 1 d R . . C13 C 0.1443(3) 0.1174(4) 1.1566(4) 0.0739(13) Uani 1 1 d . . . H13A H 0.1045 0.0834 1.1708 0.089 Uiso 1 1 calc R . . C14 C 0.1290(3) 0.1434(3) 1.0435(4) 0.0598(11) Uani 1 1 d . . . H14A H 0.0789 0.1266 0.9806 0.072 Uiso 1 1 calc R . . C15 C 0.3527(9) 0.0000 0.9176(11) 0.39(3) Uani 1 2 d S . . H15A H 0.3851 0.0513 0.9168 0.463 Uiso 0.50 1 d PR . . C16 C 0.3306(11) 0.0000 1.0247(15) 0.199(8) Uani 1 2 d S . . H16A H 0.3824 0.0000 1.0958 0.299 Uiso 1 2 d SR . . H16B H 0.2982 0.0508 1.0241 0.299 Uiso 0.50 1 d PR . . O1 O 0.1498(3) 0.0000 0.5766(4) 0.0787(13) Uani 1 2 d S . . O2 O 0.2682(3) 0.0000 0.5502(7) 0.133(3) Uani 1 2 d S . . O3 O 0.1485(4) 0.0000 0.4022(5) 0.0997(17) Uani 1 2 d S . . O4 O 0.2743(5) 0.0000 0.8224(8) 0.155(3) Uani 1 2 d S . . H4B H 0.2808 0.0000 0.7590 0.233 Uiso 1 2 calc SR . . C17 C -0.0714(10) 0.5322(13) 0.379(2) 0.185(11) Uani 0.50 1 d PD . . H17A H -0.1121 0.5676 0.3184 0.222 Uiso 0.50 1 d PR . . H17B H -0.0991 0.5120 0.4294 0.222 Uiso 0.50 1 d PR . . C18 C 0.0000 0.6101(10) 0.5000 0.174(6) Uani 1 2 d S . . H18A H -0.0243 0.6552 0.5306 0.261 Uiso 0.50 1 d PR . . H18B H 0.0408 0.5784 0.5659 0.261 Uiso 0.50 1 d PR . . H18C H 0.0276 0.6351 0.4526 0.261 Uiso 0.50 1 d PR . . O5 O -0.051(3) 0.5000 0.484(5) 0.67(5) Uani 1 2 d SD . . H5B H -0.0984 0.4754 0.4460 1.001 Uiso 0.50 1 d 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 Cd1 0.0499(3) 0.0315(3) 0.0213(3) 0.000 -0.0049(2) 0.000 N1 0.0424(15) 0.0384(16) 0.0292(14) -0.0060(11) 0.0010(11) -0.0014(12) N2 0.0390(15) 0.0422(16) 0.0333(14) -0.0101(12) -0.0013(12) -0.0005(12) N3 0.082(4) 0.041(3) 0.078(4) 0.000 0.051(3) 0.000 C1 0.0417(18) 0.0394(18) 0.0309(16) -0.0071(14) -0.0004(14) 0.0033(15) C2 0.0410(18) 0.0367(18) 0.0355(17) -0.0042(13) 0.0048(14) -0.0032(14) C3 0.042(2) 0.051(2) 0.050(2) -0.0059(17) -0.0011(16) -0.0021(17) C4 0.047(2) 0.068(3) 0.083(3) -0.012(2) -0.008(2) 0.014(2) C5 0.067(3) 0.073(3) 0.108(4) -0.035(3) 0.000(3) 0.021(3) C6 0.061(3) 0.071(3) 0.078(3) -0.039(3) -0.003(2) 0.010(2) C7 0.0382(18) 0.046(2) 0.0433(19) -0.0095(16) 0.0003(15) -0.0001(16) C8 0.0354(17) 0.0400(18) 0.0303(16) -0.0110(13) -0.0007(13) -0.0009(14) C9 0.0406(18) 0.043(2) 0.0344(17) -0.0077(14) 0.0065(14) -0.0019(15) C10 0.0463(19) 0.0421(19) 0.0283(15) -0.0065(13) 0.0068(14) 0.0009(15) C11 0.061(2) 0.070(3) 0.0326(18) -0.0017(17) 0.0077(17) -0.006(2) C12 0.090(3) 0.090(4) 0.041(2) 0.008(2) 0.024(2) -0.012(3) C13 0.075(3) 0.083(3) 0.063(3) 0.002(2) 0.027(2) -0.027(3) C14 0.052(2) 0.068(3) 0.049(2) -0.0071(19) 0.0105(18) -0.017(2) C15 0.096(9) 0.98(8) 0.049(6) 0.000 -0.007(6) 0.000 C16 0.229(18) 0.113(10) 0.181(15) 0.000 0.003(13) 0.000 O1 0.079(3) 0.102(4) 0.061(3) 0.000 0.034(2) 0.000 O2 0.044(3) 0.147(6) 0.191(8) 0.000 0.030(4) 0.000 O3 0.135(5) 0.087(4) 0.079(4) 0.000 0.044(4) 0.000 O4 0.116(6) 0.195(9) 0.139(7) 0.000 0.034(5) 0.000 C17 0.101(10) 0.152(18) 0.224(18) 0.151(16) -0.018(10) 0.014(9) C18 0.239(18) 0.124(11) 0.163(13) 0.000 0.085(13) 0.000 O5 0.76(10) 0.28(3) 1.31(14) 0.000 0.78(12) 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 Cd1 O1 2.359(5) . ? Cd1 O1 2.359(5) 5_556 ? Cd1 N1 2.366(3) . ? Cd1 N1 2.366(3) 5_556 ? Cd1 N1 2.366(3) 6 ? Cd1 N1 2.366(3) 2_556 ? N1 C1 1.306(4) . ? N1 C2 1.395(4) . ? N2 C1 1.363(4) . ? N2 C7 1.398(4) . ? N2 C8 1.443(4) . ? N3 O2 1.209(7) . ? N3 O1 1.225(6) . ? N3 O3 1.270(8) . ? C1 H1A 0.9300 . ? C2 C7 1.398(5) . ? C2 C3 1.403(5) . ? C3 C4 1.371(6) . ? C3 H3A 0.9300 . ? C4 C5 1.401(7) . ? C4 H4A 0.9300 . ? C5 C6 1.387(7) . ? C5 H5A 0.9300 . ? C6 C7 1.379(6) . ? C6 H6A 0.9300 . ? C8 C9 1.396(5) . ? C8 C10 1.403(5) 7_557 ? C9 C14 1.423(5) . ? C9 C10 1.453(4) . ? C10 C8 1.403(5) 7_557 ? C10 C11 1.427(5) . ? C11 C12 1.351(6) . ? C11 H11A 0.9300 . ? C12 C13 1.418(6) . ? C12 H12A 0.9602 . ? C13 C14 1.352(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O4 1.380(13) . ? C15 C16 1.49(2) . ? C15 H15A 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9599 . ? O4 H4B 0.8200 . ? C17 C17 1.00(4) 6_565 ? C17 O5 1.28(4) . ? C17 C18 1.91(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9601 . ? C17 H5B 1.3923 . ? C18 O5 1.89(2) . ? C18 O5 1.89(2) 5_566 ? C18 C17 1.91(3) 2_556 ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? O5 C17 1.28(4) 6_565 ? O5 O5 1.63(7) 5_566 ? O5 C18 1.89(2) 5_566 ? O5 H17B 0.8491 . ? O5 H5B 0.8501 . ? 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 O1 Cd1 O1 180.00(9) . 5_556 ? O1 Cd1 N1 80.66(10) . . ? O1 Cd1 N1 99.34(10) 5_556 . ? O1 Cd1 N1 99.34(10) . 5_556 ? O1 Cd1 N1 80.66(10) 5_556 5_556 ? N1 Cd1 N1 180.0 . 5_556 ? O1 Cd1 N1 80.66(10) . 6 ? O1 Cd1 N1 99.34(10) 5_556 6 ? N1 Cd1 N1 94.45(14) . 6 ? N1 Cd1 N1 85.55(14) 5_556 6 ? O1 Cd1 N1 99.34(10) . 2_556 ? O1 Cd1 N1 80.66(10) 5_556 2_556 ? N1 Cd1 N1 85.55(14) . 2_556 ? N1 Cd1 N1 94.45(14) 5_556 2_556 ? N1 Cd1 N1 180.0 6 2_556 ? C1 N1 C2 105.8(3) . . ? C1 N1 Cd1 123.7(2) . . ? C2 N1 Cd1 130.3(2) . . ? C1 N2 C7 106.4(3) . . ? C1 N2 C8 125.3(3) . . ? C7 N2 C8 128.1(3) . . ? O2 N3 O1 127.2(7) . . ? O2 N3 O3 117.6(6) . . ? O1 N3 O3 115.2(6) . . ? N1 C1 N2 113.2(3) . . ? N1 C1 H1A 123.4 . . ? N2 C1 H1A 123.4 . . ? N1 C2 C7 109.1(3) . . ? N1 C2 C3 131.1(3) . . ? C7 C2 C3 119.7(3) . . ? C4 C3 C2 117.8(4) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 121.1 . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C7 C6 C5 116.4(4) . . ? C7 C6 H6A 121.8 . . ? C5 C6 H6A 121.8 . . ? C6 C7 N2 131.6(3) . . ? C6 C7 C2 122.9(3) . . ? N2 C7 C2 105.5(3) . . ? C9 C8 C10 123.5(3) . 7_557 ? C9 C8 N2 118.4(3) . . ? C10 C8 N2 118.1(3) 7_557 . ? C8 C9 C14 123.9(3) . . ? C8 C9 C10 117.7(3) . . ? C14 C9 C10 118.4(3) . . ? C8 C10 C11 123.2(3) 7_557 . ? C8 C10 C9 118.7(3) 7_557 . ? C11 C10 C9 118.1(3) . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C13 121.1(4) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.4 . . ? C14 C13 C12 120.5(4) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C9 121.1(4) . . ? C13 C14 H14A 119.4 . . ? C9 C14 H14A 119.4 . . ? O4 C15 C16 103.2(13) . . ? O4 C15 H15A 111.2 . . ? C16 C15 H15A 110.8 . . ? C15 C16 H16A 108.5 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 109.5 . . ? N3 O1 Cd1 124.9(4) . . ? C15 O4 H4B 109.5 . . ? C17 C17 O5 67.1(13) 6_565 . ? C17 C17 C18 129.0(5) 6_565 . ? O5 C17 C18 69.2(15) . . ? C17 C17 H17A 124.7 6_565 . ? O5 C17 H17A 144.6 . . ? C18 C17 H17A 106.2 . . ? C17 C17 H17B 71.0 6_565 . ? O5 C17 H17B 41.7 . . ? C18 C17 H17B 92.8 . . ? H17A C17 H17B 106.3 . . ? C17 C17 H5B 50.9 6_565 . ? O5 C17 H5B 36.8 . . ? C18 C17 H5B 102.3 . . ? H17A C17 H5B 119.8 . . ? H17B C17 H5B 20.7 . . ? O5 C18 O5 51(2) . 5_566 ? O5 C18 C17 39.3(15) . . ? O5 C18 C17 68.9(16) 5_566 . ? O5 C18 C17 68.9(16) . 2_556 ? O5 C18 C17 39.3(15) 5_566 2_556 ? C17 C18 C17 102.1(10) . 2_556 ? O5 C18 H18A 116.0 . . ? O5 C18 H18A 150.5 5_566 . ? C17 C18 H18A 120.5 . . ? C17 C18 H18A 113.9 2_556 . ? O5 C18 H18B 77.3 . . ? O5 C18 H18B 45.7 5_566 . ? C17 C18 H18B 110.4 . . ? C17 C18 H18B 8.5 2_556 . ? H18A C18 H18B 109.5 . . ? O5 C18 H18C 128.4 . . ? O5 C18 H18C 96.0 5_566 . ? C17 C18 H18C 96.5 . . ? C17 C18 H18C 113.2 2_556 . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 O5 C17 46(3) . 6_565 ? C17 O5 O5 94(3) . 5_566 ? C17 O5 O5 94(3) 6_565 5_566 ? C17 O5 C18 71.5(12) . . ? C17 O5 C18 113(2) 6_565 . ? O5 O5 C18 64.3(10) 5_566 . ? C17 O5 C18 113(2) . 5_566 ? C17 O5 C18 71.5(12) 6_565 5_566 ? O5 O5 C18 64.3(10) 5_566 5_566 ? C18 O5 C18 129(2) . 5_566 ? C17 O5 H17B 48.7 . . ? C17 O5 H17B 60.7 6_565 . ? O5 O5 H17B 143.1 5_566 . ? C18 O5 H17B 98.6 . . ? C18 O5 H17B 122.9 5_566 . ? C17 O5 H5B 79.0 . . ? C17 O5 H5B 57.3 6_565 . ? O5 O5 H5B 146.3 5_566 . ? C18 O5 H5B 139.8 . . ? C18 O5 H5B 87.5 5_566 . ? H17B O5 H5B 41.3 . . ? 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 O1 Cd1 N1 C1 -22.3(3) . . . . ? O1 Cd1 N1 C1 157.7(3) 5_556 . . . ? N1 Cd1 N1 C1 152(100) 5_556 . . . ? N1 Cd1 N1 C1 57.4(3) 6 . . . ? N1 Cd1 N1 C1 -122.6(3) 2_556 . . . ? O1 Cd1 N1 C2 153.5(3) . . . . ? O1 Cd1 N1 C2 -26.5(3) 5_556 . . . ? N1 Cd1 N1 C2 -32(100) 5_556 . . . ? N1 Cd1 N1 C2 -126.7(3) 6 . . . ? N1 Cd1 N1 C2 53.3(3) 2_556 . . . ? C2 N1 C1 N2 0.6(4) . . . . ? Cd1 N1 C1 N2 177.3(2) . . . . ? C7 N2 C1 N1 -0.2(4) . . . . ? C8 N2 C1 N1 -174.3(3) . . . . ? C1 N1 C2 C7 -0.8(4) . . . . ? Cd1 N1 C2 C7 -177.2(2) . . . . ? C1 N1 C2 C3 177.0(4) . . . . ? Cd1 N1 C2 C3 0.6(6) . . . . ? N1 C2 C3 C4 -177.7(4) . . . . ? C7 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 -1.6(8) . . . . ? C3 C4 C5 C6 1.8(10) . . . . ? C4 C5 C6 C7 -0.2(10) . . . . ? C5 C6 C7 N2 177.3(5) . . . . ? C5 C6 C7 C2 -1.5(8) . . . . ? C1 N2 C7 C6 -179.3(5) . . . . ? C8 N2 C7 C6 -5.4(7) . . . . ? C1 N2 C7 C2 -0.4(4) . . . . ? C8 N2 C7 C2 173.6(3) . . . . ? N1 C2 C7 C6 179.8(4) . . . . ? C3 C2 C7 C6 1.7(6) . . . . ? N1 C2 C7 N2 0.7(4) . . . . ? C3 C2 C7 N2 -177.4(3) . . . . ? C1 N2 C8 C9 -93.1(4) . . . . ? C7 N2 C8 C9 94.0(4) . . . . ? C1 N2 C8 C10 86.1(4) . . . 7_557 ? C7 N2 C8 C10 -86.8(4) . . . 7_557 ? C10 C8 C9 C14 178.1(4) 7_557 . . . ? N2 C8 C9 C14 -2.7(5) . . . . ? C10 C8 C9 C10 -2.4(6) 7_557 . . . ? N2 C8 C9 C10 176.8(3) . . . . ? C8 C9 C10 C8 2.2(5) . . . 7_557 ? C14 C9 C10 C8 -178.2(4) . . . 7_557 ? C8 C9 C10 C11 -177.5(3) . . . . ? C14 C9 C10 C11 2.1(5) . . . . ? C8 C10 C11 C12 179.5(4) 7_557 . . . ? C9 C10 C11 C12 -0.8(6) . . . . ? C10 C11 C12 C13 -1.1(8) . . . . ? C11 C12 C13 C14 1.9(9) . . . . ? C12 C13 C14 C9 -0.6(8) . . . . ? C8 C9 C14 C13 178.1(4) . . . . ? C10 C9 C14 C13 -1.4(6) . . . . ? O2 N3 O1 Cd1 180.000(2) . . . . ? O3 N3 O1 Cd1 0.000(1) . . . . ? O1 Cd1 O1 N3 180.0(4) 5_556 . . . ? N1 Cd1 O1 N3 -131.94(7) . . . . ? N1 Cd1 O1 N3 48.06(7) 5_556 . . . ? N1 Cd1 O1 N3 131.94(7) 6 . . . ? N1 Cd1 O1 N3 -48.06(7) 2_556 . . . ? C17 C17 C18 O5 -32.6(14) 6_565 . . . ? C17 C17 C18 O5 21.5(11) 6_565 . . 5_566 ? O5 C17 C18 O5 54(2) . . . 5_566 ? C17 C17 C18 C17 0.000(6) 6_565 . . 2_556 ? O5 C17 C18 C17 32.6(14) . . . 2_556 ? C18 C17 O5 C17 -152.9(12) . . . 6_565 ? C17 C17 O5 O5 91.9(13) 6_565 . . 5_566 ? C18 C17 O5 O5 -61.1(15) . . . 5_566 ? C17 C17 O5 C18 152.9(12) 6_565 . . . ? C17 C17 O5 C18 27.9(12) 6_565 . . 5_566 ? C18 C17 O5 C18 -125(2) . . . 5_566 ? O5 C18 O5 C17 -105(3) 5_566 . . . ? C17 C18 O5 C17 -145.6(14) 2_556 . . . ? O5 C18 O5 C17 -84(3) 5_566 . . 6_565 ? C17 C18 O5 C17 20.7(17) . . . 6_565 ? C17 C18 O5 C17 -125(2) 2_556 . . 6_565 ? C17 C18 O5 O5 105(3) . . . 5_566 ? C17 C18 O5 O5 -41(3) 2_556 . . 5_566 ? O5 C18 O5 C18 0.000(1) 5_566 . . 5_566 ? C17 C18 O5 C18 105(3) . . . 5_566 ? C17 C18 O5 C18 -41(3) 2_556 . . 5_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.904 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.082 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 635089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H21 Ag B Cl9 F4 N4 O0' _chemical_formula_weight 963.25 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.302(2) _cell_length_b 25.713(7) _cell_length_c 9.153(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.842(5) _cell_angle_gamma 90.00 _cell_volume 1905.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1738 _cell_measurement_theta_min 2.4159 _cell_measurement_theta_max 25.0341 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8117 _exptl_absorpt_correction_T_max 0.8300 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 8979 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3408 _reflns_number_gt 1759 _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^)+(0.1684P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.029(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3408 _refine_ls_number_parameters 236 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2899 _refine_ls_wR_factor_gt 0.2454 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 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 0.69071(16) 0.2500 0.32902(13) 0.0654(6) Uani 1 2 d S . . N1 N 0.6713(10) 0.1671(3) 0.3136(8) 0.055(2) Uani 1 1 d . . . N2 N 0.6130(9) 0.0870(2) 0.3616(8) 0.0420(17) Uani 1 1 d . . . C2 C 0.6874(12) 0.1368(3) 0.1938(10) 0.050(2) Uani 1 1 d . . . C7 C 0.6498(11) 0.0868(3) 0.2231(9) 0.044(2) Uani 1 1 d . . . C9 C 0.3915(11) 0.0286(3) 0.3881(9) 0.040(2) Uani 1 1 d . . . C1 C 0.6319(12) 0.1360(3) 0.4117(11) 0.052(2) Uani 1 1 d . . . H1A H 0.6184 0.1465 0.5055 0.063 Uiso 1 1 calc R . . C8 C 0.5556(11) 0.0423(3) 0.4335(9) 0.040(2) Uani 1 1 d . . . C5 C 0.6900(13) 0.0593(4) -0.0140(11) 0.062(3) Uani 1 1 d . . . H5A H 0.6929 0.0336 -0.0850 0.074 Uiso 1 1 calc R . . C6 C 0.6495(11) 0.0453(3) 0.1176(10) 0.049(2) Uani 1 1 d . . . H6A H 0.6235 0.0112 0.1375 0.059 Uiso 1 1 calc R . . C10 C 0.2752(12) 0.0575(4) 0.2760(10) 0.052(2) Uani 1 1 d . . . H10A H 0.3102 0.0868 0.2323 0.063 Uiso 1 1 calc R . . C12 C 0.6671(11) 0.0161(3) 0.5460(10) 0.043(2) Uani 1 1 d . . . C13 C 0.8369(12) 0.0301(3) 0.5953(11) 0.053(2) Uani 1 1 d . . . H13A H 0.8766 0.0594 0.5548 0.064 Uiso 1 1 calc R . . C14 C 0.9398(13) 0.0021(4) 0.6983(12) 0.065(3) Uani 1 1 d . . . H14A H 1.0503 0.0117 0.7265 0.078 Uiso 1 1 calc R . . C4 C 0.7272(15) 0.1104(5) -0.0466(12) 0.074(3) Uani 1 1 d . . . H4A H 0.7538 0.1176 -0.1380 0.088 Uiso 1 1 calc R . . C11 C 0.1156(13) 0.0420(4) 0.2345(12) 0.064(3) Uani 1 1 d . . . H11A H 0.0419 0.0605 0.1614 0.076 Uiso 1 1 calc R . . Cl3 Cl 0.2651(8) 0.1064(2) 0.6215(6) 0.154(2) Uani 1 1 d . . . C17 C 0.2291(18) 0.1470(6) 0.7570(14) 0.095(4) Uani 1 1 d . . . H17A H 0.3157 0.1737 0.7777 0.114 Uiso 1 1 calc R . . Cl2 Cl 0.2368(7) 0.10977(19) 0.9201(5) 0.1370(17) Uani 1 1 d . . . Cl1 Cl 0.0351(7) 0.1774(2) 0.7151(7) 0.159(2) Uani 1 1 d . . . C3 C 0.7254(14) 0.1517(4) 0.0564(11) 0.064(3) Uani 1 1 d . . . H3A H 0.7475 0.1860 0.0350 0.076 Uiso 1 1 calc R . . Cl4 Cl 0.3243(12) 0.2500 0.0932(11) 0.182(3) Uani 1 2 d S . . Cl5 Cl 0.1265(15) 0.1957(3) 0.2590(12) 0.264(5) Uani 1 1 d . . . C18 C 0.213(4) 0.2500 0.240(5) 0.186(15) Uani 1 2 d S . . H18A H 0.3038 0.2500 0.3293 0.223 Uiso 1 2 calc SR . . B1 B 0.533(4) 0.2500 0.669(3) 0.27(4) Uani 1 2 d SD . . F1 F 0.606(3) 0.2035(5) 0.6791(17) 0.274(10) Uani 1 1 d D . . F2 F 0.485(2) 0.2500 0.8035(19) 0.174(6) Uani 1 2 d SD . . F3 F 0.686(5) 0.2500 0.756(6) 0.55(5) Uani 1 2 d SD . . 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 0.0879(11) 0.0260(6) 0.0865(10) 0.000 0.0286(7) 0.000 N1 0.078(6) 0.028(4) 0.062(5) -0.004(3) 0.020(4) -0.003(3) N2 0.057(5) 0.025(3) 0.050(4) 0.000(3) 0.026(4) -0.005(3) C2 0.066(6) 0.030(4) 0.055(6) -0.002(4) 0.017(5) -0.007(4) C7 0.053(6) 0.033(4) 0.049(5) 0.003(4) 0.020(4) 0.004(4) C9 0.047(6) 0.033(4) 0.042(5) -0.004(4) 0.014(4) 0.002(4) C1 0.067(7) 0.029(4) 0.063(6) 0.001(4) 0.020(5) -0.007(4) C8 0.054(6) 0.025(4) 0.048(5) 0.001(3) 0.023(4) -0.006(3) C5 0.067(7) 0.068(7) 0.055(6) -0.012(5) 0.023(5) -0.002(5) C6 0.050(6) 0.039(5) 0.059(6) -0.013(4) 0.012(5) -0.002(4) C10 0.054(6) 0.044(5) 0.062(6) 0.004(4) 0.020(5) -0.005(4) C12 0.048(6) 0.037(4) 0.048(5) -0.004(4) 0.018(4) -0.007(4) C13 0.052(6) 0.044(5) 0.065(6) 0.009(4) 0.015(5) -0.001(4) C14 0.043(6) 0.068(7) 0.082(7) 0.004(6) 0.007(5) -0.004(5) C4 0.086(9) 0.082(8) 0.056(7) 0.000(6) 0.021(6) -0.009(6) C11 0.052(7) 0.066(6) 0.070(7) 0.012(5) 0.005(5) 0.016(5) Cl3 0.210(6) 0.135(4) 0.149(4) -0.064(3) 0.113(4) -0.053(3) C17 0.106(11) 0.100(10) 0.092(9) -0.011(7) 0.048(8) -0.018(8) Cl2 0.171(5) 0.133(4) 0.104(3) 0.014(3) 0.025(3) -0.003(3) Cl1 0.139(4) 0.124(4) 0.202(5) 0.014(3) 0.010(4) 0.030(3) C3 0.088(8) 0.050(6) 0.056(6) 0.011(5) 0.024(6) -0.007(5) Cl4 0.153(8) 0.173(8) 0.207(8) 0.000 0.013(6) 0.000 Cl5 0.363(13) 0.130(6) 0.330(11) -0.009(6) 0.143(9) -0.081(7) C18 0.14(3) 0.12(2) 0.34(5) 0.000 0.14(3) 0.000 B1 0.34(7) 0.09(3) 0.50(9) 0.000 0.39(8) 0.000 F1 0.50(3) 0.133(10) 0.220(14) -0.065(10) 0.149(17) 0.083(16) F2 0.186(17) 0.181(16) 0.182(15) 0.000 0.098(13) 0.000 F3 0.65(10) 0.11(2) 1.08(14) 0.000 0.57(10) 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 N1 2.140(7) . ? Ag1 N1 2.140(7) 4_565 ? N1 C1 1.297(11) . ? N1 C2 1.376(11) . ? N2 C1 1.337(10) . ? N2 C7 1.368(10) . ? N2 C8 1.456(9) . ? C2 C7 1.365(11) . ? C2 C3 1.415(12) . ? C7 C6 1.438(11) . ? C9 C8 1.378(12) . ? C9 C12 1.432(11) 3_656 ? C9 C10 1.449(12) . ? C1 H1A 0.9300 . ? C8 C12 1.396(12) . ? C5 C6 1.369(13) . ? C5 C4 1.398(14) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C10 C11 1.355(13) . ? C10 H10A 0.9300 . ? C12 C13 1.428(13) . ? C12 C9 1.432(11) 3_656 ? C13 C14 1.335(13) . ? C13 H13A 0.9300 . ? C14 C11 1.415(14) 3_656 ? C14 H14A 0.9300 . ? C4 C3 1.422(14) . ? C4 H4A 0.9300 . ? C11 C14 1.415(14) 3_656 ? C11 H11A 0.9300 . ? Cl3 C17 1.698(13) . ? C17 Cl1 1.754(15) . ? C17 Cl2 1.763(14) . ? C17 H17A 0.9800 . ? C3 H3A 0.9300 . ? Cl4 C18 1.80(3) . ? Cl5 C18 1.596(14) . ? C18 Cl5 1.596(14) 4_565 ? C18 H18A 0.9800 . ? B1 F1 1.336(16) . ? B1 F1 1.336(16) 4_565 ? B1 F3 1.34(2) . ? B1 F2 1.377(18) . ? F1 F3 1.47(3) . ? F3 F1 1.47(3) 4_565 ? 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 N1 Ag1 N1 169.9(4) . 4_565 ? C1 N1 C2 106.7(7) . . ? C1 N1 Ag1 126.6(6) . . ? C2 N1 Ag1 126.6(6) . . ? C1 N2 C7 106.8(7) . . ? C1 N2 C8 127.9(7) . . ? C7 N2 C8 125.3(6) . . ? C7 C2 N1 108.0(8) . . ? C7 C2 C3 122.4(8) . . ? N1 C2 C3 129.5(8) . . ? C2 C7 N2 106.6(7) . . ? C2 C7 C6 122.2(8) . . ? N2 C7 C6 131.2(7) . . ? C8 C9 C12 119.0(7) . 3_656 ? C8 C9 C10 122.7(7) . . ? C12 C9 C10 118.4(8) 3_656 . ? N1 C1 N2 111.8(8) . . ? N1 C1 H1A 124.1 . . ? N2 C1 H1A 124.1 . . ? C9 C8 C12 123.2(7) . . ? C9 C8 N2 117.9(7) . . ? C12 C8 N2 119.0(7) . . ? C6 C5 C4 123.0(9) . . ? C6 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? C5 C6 C7 115.6(8) . . ? C5 C6 H6A 122.2 . . ? C7 C6 H6A 122.2 . . ? C11 C10 C9 120.3(8) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C8 C12 C13 123.9(8) . . ? C8 C12 C9 117.8(7) . 3_656 ? C13 C12 C9 118.3(8) . 3_656 ? C14 C13 C12 121.2(9) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C11 121.5(10) . 3_656 ? C13 C14 H14A 119.3 . . ? C11 C14 H14A 119.3 3_656 . ? C5 C4 C3 121.7(10) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C10 C11 C14 120.4(9) . 3_656 ? C10 C11 H11A 119.8 . . ? C14 C11 H11A 119.8 3_656 . ? Cl3 C17 Cl1 114.6(8) . . ? Cl3 C17 Cl2 107.8(8) . . ? Cl1 C17 Cl2 106.6(7) . . ? Cl3 C17 H17A 109.3 . . ? Cl1 C17 H17A 109.3 . . ? Cl2 C17 H17A 109.3 . . ? C2 C3 C4 115.1(9) . . ? C2 C3 H3A 122.4 . . ? C4 C3 H3A 122.4 . . ? Cl5 C18 Cl5 122.1(18) . 4_565 ? Cl5 C18 Cl4 113.5(14) . . ? Cl5 C18 Cl4 113.5(14) 4_565 . ? Cl5 C18 H18A 101.1 . . ? Cl5 C18 H18A 101.1 4_565 . ? Cl4 C18 H18A 101.1 . . ? F1 B1 F1 127(3) . 4_565 ? F1 B1 F3 66.6(18) . . ? F1 B1 F3 66.6(18) 4_565 . ? F1 B1 F2 98.8(15) . . ? F1 B1 F2 98.8(15) 4_565 . ? F3 B1 F2 84(3) . . ? B1 F1 F3 56.9(9) . . ? B1 F3 F1 56.5(14) . . ? B1 F3 F1 56.5(14) . 4_565 ? F1 F3 F1 109(3) . 4_565 ? 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 N1 Ag1 N1 C1 -109(2) 4_565 . . . ? N1 Ag1 N1 C2 66(3) 4_565 . . . ? C1 N1 C2 C7 2.2(11) . . . . ? Ag1 N1 C2 C7 -173.9(6) . . . . ? C1 N1 C2 C3 178.5(11) . . . . ? Ag1 N1 C2 C3 2.4(15) . . . . ? N1 C2 C7 N2 -0.7(10) . . . . ? C3 C2 C7 N2 -177.3(9) . . . . ? N1 C2 C7 C6 178.0(8) . . . . ? C3 C2 C7 C6 1.4(15) . . . . ? C1 N2 C7 C2 -1.0(10) . . . . ? C8 N2 C7 C2 175.8(8) . . . . ? C1 N2 C7 C6 -179.6(10) . . . . ? C8 N2 C7 C6 -2.7(15) . . . . ? C2 N1 C1 N2 -3.0(11) . . . . ? Ag1 N1 C1 N2 173.2(6) . . . . ? C7 N2 C1 N1 2.5(11) . . . . ? C8 N2 C1 N1 -174.2(8) . . . . ? C12 C9 C8 C12 -2.9(13) 3_656 . . . ? C10 C9 C8 C12 177.1(8) . . . . ? C12 C9 C8 N2 178.3(7) 3_656 . . . ? C10 C9 C8 N2 -1.7(12) . . . . ? C1 N2 C8 C9 97.5(11) . . . . ? C7 N2 C8 C9 -78.7(10) . . . . ? C1 N2 C8 C12 -81.4(11) . . . . ? C7 N2 C8 C12 102.4(10) . . . . ? C4 C5 C6 C7 -0.9(15) . . . . ? C2 C7 C6 C5 0.2(13) . . . . ? N2 C7 C6 C5 178.6(9) . . . . ? C8 C9 C10 C11 179.4(8) . . . . ? C12 C9 C10 C11 -0.6(13) 3_656 . . . ? C9 C8 C12 C13 -179.4(8) . . . . ? N2 C8 C12 C13 -0.6(12) . . . . ? C9 C8 C12 C9 2.9(13) . . . 3_656 ? N2 C8 C12 C9 -178.3(7) . . . 3_656 ? C8 C12 C13 C14 -176.7(9) . . . . ? C9 C12 C13 C14 1.0(14) 3_656 . . . ? C12 C13 C14 C11 -1.4(16) . . . 3_656 ? C6 C5 C4 C3 0.0(18) . . . . ? C9 C10 C11 C14 0.9(15) . . . 3_656 ? C7 C2 C3 C4 -2.2(15) . . . . ? N1 C2 C3 C4 -178.0(10) . . . . ? C5 C4 C3 C2 1.5(16) . . . . ? F1 B1 F1 F3 29(4) 4_565 . . . ? F2 B1 F1 F3 -79(3) . . . . ? F1 B1 F3 F1 -155(3) 4_565 . . . ? F2 B1 F3 F1 102.5(15) . . . . ? F1 B1 F3 F1 155(3) . . . 4_565 ? F2 B1 F3 F1 -102.5(15) . . . 4_565 ? B1 F1 F3 F1 -22(2) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.975 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.171 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 635090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Ag Cl6 N5 O3' _chemical_formula_weight 819.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 23.438(5) _cell_length_b 16.481(3) _cell_length_c 7.9237(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.64(3) _cell_angle_gamma 90.00 _cell_volume 3054.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4898 _cell_measurement_theta_min 1.5114 _cell_measurement_theta_max 28.6817 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7912 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Molybdenum _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19930 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.67 _reflns_number_total 3945 _reflns_number_gt 3425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.1381P)^2^+11.7687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0077(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3945 _refine_ls_number_parameters 233 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.2012 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.07457(3) 0.2500 0.0291(2) Uani 1 2 d S . . N1 N 0.41054(14) 0.1055(2) 0.2472(4) 0.0228(7) Uani 1 1 d . . . N2 N 0.32857(14) 0.1613(2) 0.3177(4) 0.0207(7) Uani 1 1 d . . . C1 C 0.38349(17) 0.1405(3) 0.3684(5) 0.0231(8) Uani 1 1 d . . . H1A H 0.3999 0.1500 0.4765 0.028 Uiso 1 1 calc R . . C2 C 0.37181(16) 0.1031(2) 0.1067(5) 0.0210(7) Uani 1 1 d . . . C3 C 0.3787(2) 0.0730(2) -0.0551(6) 0.0243(8) Uani 1 1 d . . . H3A H 0.4129 0.0496 -0.0839 0.029 Uiso 1 1 calc R . . C4 C 0.3323(2) 0.0798(2) -0.1707(6) 0.0276(9) Uani 1 1 d . . . H4A H 0.3353 0.0606 -0.2801 0.033 Uiso 1 1 calc R . . C5 C 0.28050(19) 0.1151(3) -0.1266(5) 0.0276(8) Uani 1 1 d . . . H5A H 0.2502 0.1184 -0.2079 0.033 Uiso 1 1 calc R . . C6 C 0.27341(18) 0.1450(3) 0.0335(5) 0.0243(8) Uani 1 1 d . . . H6A H 0.2392 0.1684 0.0623 0.029 Uiso 1 1 calc R . . C7 C 0.32016(16) 0.1381(2) 0.1492(5) 0.0206(7) Uani 1 1 d . . . C8 C 0.1789(2) 0.0484(3) 0.4699(7) 0.0376(11) Uani 1 1 d . . . H8A H 0.1721 -0.0059 0.4442 0.045 Uiso 1 1 calc R . . C9 C 0.2272(2) 0.0842(3) 0.4198(6) 0.0281(9) Uani 1 1 d . . . H9A H 0.2530 0.0540 0.3614 0.034 Uiso 1 1 calc R . . C10 C 0.23890(16) 0.1676(2) 0.4557(5) 0.0221(8) Uani 1 1 d . . . C11 C 0.28885(16) 0.2055(3) 0.4122(5) 0.0213(8) Uani 1 1 d . . . C12 C 0.30188(16) 0.2870(2) 0.4533(5) 0.0224(8) Uani 1 1 d . . . C13 C 0.35148(18) 0.3271(3) 0.4021(6) 0.0300(9) Uani 1 1 d . . . H13A H 0.3778 0.2985 0.3424 0.036 Uiso 1 1 calc R . . C14 C 0.3612(2) 0.4076(3) 0.4393(7) 0.0375(11) Uani 1 1 d . . . H14A H 0.3939 0.4332 0.4050 0.045 Uiso 1 1 calc R . . C15 C 0.0461(3) 0.1733(5) 0.0616(13) 0.066(5) Uani 0.50 1 d PD A 1 H15A H 0.0293 0.2156 0.1301 0.079 Uiso 1 1 calc R A 1 C15' C 0.0623(6) 0.1349(10) -0.0012(19) 0.35(4) Uani 0.50 1 d PD A 2 Cl1 Cl 0.11817(15) 0.1928(3) 0.0927(7) 0.1546(17) Uani 1 1 d D . . Cl2 Cl 0.0184(2) 0.1961(8) -0.1380(11) 0.403(8) Uani 1 1 d D . . Cl3 Cl 0.0254(4) 0.0866(3) 0.1579(17) 0.245(5) Uani 0.80 1 d PD . 1 Cl3' Cl 0.0466(7) 0.0772(5) -0.0438(16) 0.087(4) Uani 0.20 1 d PD A 2 N3 N 0.5000 -0.1184(4) 0.2500 0.108(6) Uani 1 2 d SD . . O1 O 0.5227(2) -0.0730(4) 0.3708(7) 0.079(2) Uani 1 1 d D B . O2 O 0.5000 -0.1990(7) 0.2500 0.21(2) Uani 0.50 2 d SPD B 1 O2' O 0.5202(9) -0.1856(6) 0.331(3) 0.036(4) Uani 0.25 1 d PD . 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 0.0126(3) 0.0308(3) 0.0448(4) 0.000 0.00808(18) 0.000 N1 0.0147(15) 0.0247(17) 0.0298(17) 0.0004(13) 0.0068(12) 0.0037(12) N2 0.0167(15) 0.0253(16) 0.0207(15) -0.0005(12) 0.0058(11) 0.0067(12) C1 0.0162(17) 0.0267(19) 0.0265(18) -0.0006(15) 0.0028(14) 0.0050(14) C2 0.0184(17) 0.0199(18) 0.0254(17) 0.0026(14) 0.0083(14) 0.0037(14) C3 0.026(2) 0.0188(18) 0.030(2) 0.0011(14) 0.0155(16) 0.0020(13) C4 0.036(2) 0.024(2) 0.0229(18) -0.0019(14) 0.0092(17) -0.0007(16) C5 0.031(2) 0.027(2) 0.0253(19) 0.0000(15) 0.0007(16) 0.0021(16) C6 0.0230(18) 0.0250(19) 0.0255(18) 0.0010(15) 0.0063(14) 0.0063(15) C7 0.0191(17) 0.0232(18) 0.0201(16) 0.0003(13) 0.0075(13) 0.0051(14) C8 0.032(2) 0.028(2) 0.053(3) -0.006(2) 0.015(2) -0.0008(19) C9 0.024(2) 0.026(2) 0.035(2) -0.0050(16) 0.0102(17) 0.0045(15) C10 0.0176(17) 0.0258(19) 0.0232(17) -0.0004(14) 0.0035(13) 0.0051(14) C11 0.0173(17) 0.028(2) 0.0190(16) -0.0026(14) 0.0037(13) 0.0081(14) C12 0.0165(17) 0.027(2) 0.0240(17) -0.0018(14) 0.0047(13) 0.0042(14) C13 0.0201(19) 0.032(2) 0.039(2) -0.0032(17) 0.0099(16) 0.0020(16) C14 0.027(2) 0.032(2) 0.055(3) -0.006(2) 0.018(2) -0.0012(19) C15 0.010(4) 0.060(8) 0.130(14) -0.029(9) 0.021(6) 0.004(4) C15' 0.28(6) 0.36(7) 0.39(7) 0.34(7) -0.04(5) -0.16(6) Cl1 0.083(2) 0.139(3) 0.241(5) 0.037(3) 0.010(3) -0.023(2) Cl2 0.077(3) 0.79(3) 0.342(12) 0.101(14) 0.032(4) 0.021(8) Cl3 0.144(6) 0.105(4) 0.500(17) 0.045(6) 0.123(8) -0.002(3) Cl3' 0.139(12) 0.036(4) 0.087(7) -0.007(4) 0.019(7) 0.044(5) N3 0.084(7) 0.014(3) 0.241(16) 0.000 0.131(10) 0.000 O1 0.035(3) 0.139(6) 0.064(3) 0.055(3) 0.007(2) 0.011(3) O2 0.21(5) 0.067(16) 0.37(7) 0.000 0.22(4) 0.000 O2' 0.036(8) 0.011(5) 0.057(9) -0.003(6) -0.016(7) -0.011(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 N1 2.157(3) 2_655 ? Ag1 N1 2.157(3) . ? N1 C1 1.317(5) . ? N1 C2 1.392(5) . ? N2 C1 1.368(5) . ? N2 C7 1.391(5) . ? N2 C11 1.430(5) . ? C1 H1A 0.9300 . ? C2 C3 1.394(6) . ? C2 C7 1.401(5) . ? C3 C4 1.381(7) . ? C3 H3A 0.9300 . ? C4 C5 1.410(6) . ? C4 H4A 0.9300 . ? C5 C6 1.381(6) . ? C5 H5A 0.9300 . ? C6 C7 1.388(6) . ? C6 H6A 0.9300 . ? C8 C9 1.357(7) . ? C8 C14 1.419(7) 7_556 ? C8 H8A 0.9300 . ? C9 C10 1.426(6) . ? C9 H9A 0.9300 . ? C10 C11 1.389(6) . ? C10 C12 1.442(5) 7_556 ? C11 C12 1.412(6) . ? C12 C13 1.419(6) . ? C12 C10 1.442(5) 7_556 ? C13 C14 1.375(7) . ? C13 H13A 0.9300 . ? C14 C8 1.419(7) 7_556 ? C14 H14A 0.9300 . ? C15 Cl3 1.706(8) . ? C15 Cl2 1.714(9) . ? C15 Cl1 1.721(7) . ? C15 H15A 0.9800 . ? C15' Cl3' 1.066(19) . ? C15' Cl1 1.749(10) . ? C15' Cl2 1.765(10) . ? Cl2 Cl2 1.923(17) 2_554 ? Cl2 Cl3' 2.185(15) . ? Cl3 Cl3 1.943(18) 2 ? N3 O1 1.301(6) . ? N3 O1 1.301(6) 2_655 ? N3 O2 1.329(10) . ? N3 O2' 1.352(9) . ? N3 O2' 1.352(9) 2_655 ? O2' O2' 1.55(3) 2_655 ? 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 N1 Ag1 N1 152.65(19) 2_655 . ? C1 N1 C2 106.0(3) . . ? C1 N1 Ag1 127.5(3) . . ? C2 N1 Ag1 125.8(3) . . ? C1 N2 C7 106.6(3) . . ? C1 N2 C11 127.3(3) . . ? C7 N2 C11 125.8(3) . . ? N1 C1 N2 112.5(4) . . ? N1 C1 H1A 123.7 . . ? N2 C1 H1A 123.7 . . ? N1 C2 C3 129.7(4) . . ? N1 C2 C7 109.0(3) . . ? C3 C2 C7 121.3(4) . . ? C4 C3 C2 116.6(4) . . ? C4 C3 H3A 121.7 . . ? C2 C3 H3A 121.7 . . ? C3 C4 C5 121.6(4) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C6 C5 C4 122.0(4) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C7 116.2(4) . . ? C5 C6 H6A 121.9 . . ? C7 C6 H6A 121.9 . . ? C6 C7 N2 132.0(3) . . ? C6 C7 C2 122.2(4) . . ? N2 C7 C2 105.8(3) . . ? C9 C8 C14 121.2(5) . 7_556 ? C9 C8 H8A 119.4 . . ? C14 C8 H8A 119.4 7_556 . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 122.5(4) . . ? C11 C10 C12 119.1(4) . 7_556 ? C9 C10 C12 118.3(4) . 7_556 ? C10 C11 C12 122.9(3) . . ? C10 C11 N2 119.2(4) . . ? C12 C11 N2 117.8(3) . . ? C11 C12 C13 123.1(4) . . ? C11 C12 C10 117.9(3) . 7_556 ? C13 C12 C10 118.9(4) . 7_556 ? C14 C13 C12 121.0(4) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C8 119.7(5) . 7_556 ? C13 C14 H14A 120.2 . . ? C8 C14 H14A 120.2 7_556 . ? Cl3 C15 Cl2 119.7(8) . . ? Cl3 C15 Cl1 113.4(6) . . ? Cl2 C15 Cl1 113.7(5) . . ? Cl3 C15 H15A 102.3 . . ? Cl2 C15 H15A 102.3 . . ? Cl1 C15 H15A 102.3 . . ? Cl3' C15' Cl1 148.9(17) . . ? Cl3' C15' Cl2 98.0(11) . . ? Cl1 C15' Cl2 109.9(8) . . ? C15 Cl1 C15' 30.2(8) . . ? C15 Cl2 C15' 30.1(8) . . ? C15 Cl2 Cl2 166.8(6) . 2_554 ? C15' Cl2 Cl2 141.0(8) . 2_554 ? C15 Cl2 Cl3' 53.0(5) . . ? C15' Cl2 Cl3' 28.9(6) . . ? Cl2 Cl2 Cl3' 115.1(4) 2_554 . ? C15 Cl3 Cl3 122.8(4) . 2 ? C15' Cl3' Cl2 53.1(8) . . ? O1 N3 O1 109.8(6) . 2_655 ? O1 N3 O2 125.1(3) . . ? O1 N3 O2 125.1(3) 2_655 . ? O1 N3 O2' 90.4(7) . . ? O1 N3 O2' 159.4(9) 2_655 . ? O2 N3 O2' 35.0(6) . . ? O1 N3 O2' 159.4(9) . 2_655 ? O1 N3 O2' 90.4(7) 2_655 2_655 ? O2 N3 O2' 35.0(6) . 2_655 ? O2' N3 O2' 70.0(12) . 2_655 ? N3 O2' O2' 55.0(6) . 2_655 ? 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 N1 Ag1 N1 C1 -67.6(4) 2_655 . . . ? N1 Ag1 N1 C2 102.3(3) 2_655 . . . ? C2 N1 C1 N2 0.4(5) . . . . ? Ag1 N1 C1 N2 171.9(3) . . . . ? C7 N2 C1 N1 -0.5(5) . . . . ? C11 N2 C1 N1 -174.9(4) . . . . ? C1 N1 C2 C3 179.4(4) . . . . ? Ag1 N1 C2 C3 7.8(6) . . . . ? C1 N1 C2 C7 -0.1(5) . . . . ? Ag1 N1 C2 C7 -171.7(3) . . . . ? N1 C2 C3 C4 -179.3(4) . . . . ? C7 C2 C3 C4 0.2(6) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C4 C5 C6 C7 -0.2(6) . . . . ? C5 C6 C7 N2 179.6(4) . . . . ? C5 C6 C7 C2 0.2(6) . . . . ? C1 N2 C7 C6 -179.1(4) . . . . ? C11 N2 C7 C6 -4.7(7) . . . . ? C1 N2 C7 C2 0.4(4) . . . . ? C11 N2 C7 C2 174.9(4) . . . . ? N1 C2 C7 C6 179.4(4) . . . . ? C3 C2 C7 C6 -0.2(6) . . . . ? N1 C2 C7 N2 -0.2(4) . . . . ? C3 C2 C7 N2 -179.7(4) . . . . ? C14 C8 C9 C10 -0.6(8) 7_556 . . . ? C8 C9 C10 C11 177.5(5) . . . . ? C8 C9 C10 C12 0.0(7) . . . 7_556 ? C9 C10 C11 C12 -177.3(4) . . . . ? C12 C10 C11 C12 0.1(6) 7_556 . . . ? C9 C10 C11 N2 4.4(6) . . . . ? C12 C10 C11 N2 -178.2(3) 7_556 . . . ? C1 N2 C11 C10 -116.6(5) . . . . ? C7 N2 C11 C10 70.1(5) . . . . ? C1 N2 C11 C12 65.0(5) . . . . ? C7 N2 C11 C12 -108.3(4) . . . . ? C10 C11 C12 C13 -176.8(4) . . . . ? N2 C11 C12 C13 1.5(6) . . . . ? C10 C11 C12 C10 -0.1(6) . . . 7_556 ? N2 C11 C12 C10 178.2(3) . . . 7_556 ? C11 C12 C13 C14 177.3(5) . . . . ? C10 C12 C13 C14 0.6(7) 7_556 . . . ? C12 C13 C14 C8 -0.1(8) . . . 7_556 ? Cl3 C15 Cl1 C15' 70.8(8) . . . . ? Cl2 C15 Cl1 C15' -70.3(9) . . . . ? Cl3' C15' Cl1 C15 -145(3) . . . . ? Cl2 C15' Cl1 C15 62.9(11) . . . . ? Cl3 C15 Cl2 C15' -69.1(8) . . . . ? Cl1 C15 Cl2 C15' 69.4(9) . . . . ? Cl3 C15 Cl2 Cl2 -14(3) . . . 2_554 ? Cl1 C15 Cl2 Cl2 125(3) . . . 2_554 ? Cl3 C15 Cl2 Cl3' -41.6(7) . . . . ? Cl1 C15 Cl2 Cl3' 96.9(8) . . . . ? Cl3' C15' Cl2 C15 130.2(16) . . . . ? Cl1 C15' Cl2 C15 -63.8(11) . . . . ? Cl3' C15' Cl2 Cl2 -32.5(19) . . . 2_554 ? Cl1 C15' Cl2 Cl2 133.5(9) . . . 2_554 ? Cl1 C15' Cl2 Cl3' 166(2) . . . . ? Cl2 C15 Cl3 Cl3 -106.8(13) . . . 2 ? Cl1 C15 Cl3 Cl3 114.6(11) . . . 2 ? Cl1 C15' Cl3' Cl2 -154(3) . . . . ? C15 Cl2 Cl3' C15' -28.6(13) . . . . ? Cl2 Cl2 Cl3' C15' 158.1(15) 2_554 . . . ? O1 N3 O2' O2' 173.7(16) . . . 2_655 ? O1 N3 O2' O2' -18(4) 2_655 . . 2_655 ? O2 N3 O2' O2' 0.000(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.67 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.665 _refine_diff_density_min -1.350 _refine_diff_density_rms 0.180 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 635091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H38 Cl8 Mn N8' _chemical_formula_weight 1185.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _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 9.0079(16) _cell_length_b 12.129(2) _cell_length_c 14.031(2) _cell_angle_alpha 110.672(2) _cell_angle_beta 100.713(3) _cell_angle_gamma 98.948(3) _cell_volume 1367.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1916 _cell_measurement_theta_min 2.3707 _cell_measurement_theta_max 23.9990 _exptl_crystal_description BLOCK _exptl_crystal_colour PINK _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 603 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min 0.7912 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% NONE _diffrn_reflns_number 7028 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4796 _reflns_number_gt 3152 _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^)+(0.0736P)^2^+1.5242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4796 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Mn1 Mn 0.5000 1.5000 1.0000 0.0319(3) Uani 1 2 d S . . Cl1 Cl 0.70002(13) 1.42154(9) 0.90918(8) 0.0403(3) Uani 1 1 d . . . Cl2' Cl 0.7129(8) 1.1225(4) 0.6167(3) 0.1381(18) Uani 0.55 1 d P . . Cl2 Cl 0.6389(6) 1.1957(8) 0.5711(5) 0.158(3) Uani 0.45 1 d P . . Cl3 Cl 0.7419(10) 1.3504(7) 0.6042(4) 0.177(3) Uani 0.55 1 d P . . Cl3' Cl 0.8761(16) 1.3919(9) 0.6347(7) 0.280(8) Uani 0.45 1 d P . . Cl4 Cl 1.0000(5) 1.2826(6) 0.6975(6) 0.168(2) Uani 0.60 1 d P . . Cl4' Cl 0.9211(14) 1.1673(11) 0.6454(6) 0.191(5) Uani 0.40 1 d P . . N1 N 0.3322(4) 1.3136(3) 0.9245(3) 0.0363(8) Uani 1 1 d . . . N2 N 0.1753(4) 1.1556(3) 0.9311(2) 0.0349(8) Uani 1 1 d . . . N5 N 0.4078(4) 1.5494(3) 0.8490(2) 0.0366(8) Uani 1 1 d . . . N6 N 0.4075(4) 1.5493(3) 0.6894(2) 0.0388(9) Uani 1 1 d . . . C1 C 0.2510(5) 1.2749(3) 0.9801(3) 0.0405(11) Uani 1 1 d . . . H1A H 0.2458 1.3244 1.0467 0.049 Uiso 1 1 calc R . . C2 C 0.3066(5) 1.2122(3) 0.8305(3) 0.0305(9) Uani 1 1 d . . . C3 C 0.3595(5) 1.1978(4) 0.7408(3) 0.0384(10) Uani 1 1 d . . . H3A H 0.4243 1.2624 0.7362 0.046 Uiso 1 1 calc R . . C4 C 0.3134(6) 1.0861(4) 0.6598(3) 0.0529(13) Uani 1 1 d . . . H4A H 0.3469 1.0752 0.5990 0.063 Uiso 1 1 calc R . . C5 C 0.2170(6) 0.9872(4) 0.6655(4) 0.0607(15) Uani 1 1 d . . . H5A H 0.1888 0.9122 0.6090 0.073 Uiso 1 1 calc R . . C6 C 0.1635(6) 0.9998(4) 0.7535(3) 0.0498(12) Uani 1 1 d . . . H6A H 0.0999 0.9350 0.7585 0.060 Uiso 1 1 calc R . . C7 C 0.2093(5) 1.1133(3) 0.8338(3) 0.0325(9) Uani 1 1 d . . . C8 C 0.0861(5) 1.0801(3) 0.9697(3) 0.0315(9) Uani 1 1 d . . . C9 C -0.0751(5) 1.0618(3) 0.9434(3) 0.0314(9) Uani 1 1 d . . . C10 C -0.1548(5) 1.1234(4) 0.8894(3) 0.0423(11) Uani 1 1 d . . . H10A H -0.0982 1.1798 0.8707 0.051 Uiso 1 1 calc R . . C11 C -0.3114(6) 1.1013(5) 0.8647(4) 0.0542(13) Uani 1 1 d . . . H11A H -0.3614 1.1431 0.8298 0.065 Uiso 1 1 calc R . . C12 C -0.3998(6) 1.0157(5) 0.8912(4) 0.0554(13) Uani 1 1 d . . . H12A H -0.5078 1.0001 0.8717 0.066 Uiso 1 1 calc R . . C13 C -0.3306(5) 0.9555(4) 0.9446(3) 0.0433(11) Uani 1 1 d . . . H13A H -0.3912 0.9001 0.9623 0.052 Uiso 1 1 calc R . . C14 C 0.1653(5) 1.0231(3) 1.0262(3) 0.0306(9) Uani 1 1 d . . . C15 C 0.4754(5) 1.5237(4) 0.7717(3) 0.0376(10) Uani 1 1 d . . . H15A H 0.5620 1.4909 0.7729 0.045 Uiso 1 1 calc R . . C16 C 0.2832(5) 1.5943(4) 0.8151(3) 0.0407(11) Uani 1 1 d . . . C17 C 0.1714(7) 1.6367(5) 0.8639(4) 0.0613(15) Uani 1 1 d . . . H17A H 0.1713 1.6395 0.9310 0.074 Uiso 1 1 calc R . . C18 C 0.0607(8) 1.6744(6) 0.8098(4) 0.0807(19) Uani 1 1 d . . . H18A H -0.0158 1.7028 0.8411 0.097 Uiso 1 1 calc R . . C19 C 0.0596(8) 1.6714(6) 0.7093(4) 0.0775(18) Uani 1 1 d . . . H19A H -0.0184 1.6965 0.6748 0.093 Uiso 1 1 calc R . . C20 C 0.1710(7) 1.6321(5) 0.6602(4) 0.0604(14) Uani 1 1 d . . . H20A H 0.1723 1.6314 0.5939 0.072 Uiso 1 1 calc R . . C21 C 0.2811(5) 1.5937(4) 0.7150(3) 0.0406(11) Uani 1 1 d . . . C22 C 0.4530(5) 1.5248(4) 0.5927(3) 0.0361(10) Uani 1 1 d . . . C23 C 0.5579(5) 1.6168(4) 0.5840(3) 0.0368(10) Uani 1 1 d . . . C24 C 0.6171(6) 1.7351(4) 0.6649(3) 0.0512(12) Uani 1 1 d . . . H24A H 0.5863 1.7539 0.7273 0.061 Uiso 1 1 calc R . . C25 C 0.7177(6) 1.8211(4) 0.6522(4) 0.0586(14) Uani 1 1 d . . . H25A H 0.7549 1.8980 0.7060 0.070 Uiso 1 1 calc R . . C26 C 0.7664(6) 1.7954(4) 0.5590(4) 0.0571(13) Uani 1 1 d . . . H26A H 0.8355 1.8556 0.5519 0.068 Uiso 1 1 calc R . . C27 C 0.7140(5) 1.6840(4) 0.4793(3) 0.0449(11) Uani 1 1 d . . . H27A H 0.7480 1.6684 0.4183 0.054 Uiso 1 1 calc R . . C28 C 0.3925(5) 1.4092(4) 0.5117(3) 0.0363(10) Uani 1 1 d . . . C29 C 0.8096(7) 1.2743(6) 0.6713(5) 0.0774(17) 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 Mn1 0.0425(6) 0.0254(5) 0.0266(5) 0.0108(4) 0.0129(4) -0.0010(4) Cl1 0.0497(7) 0.0418(6) 0.0334(5) 0.0170(5) 0.0148(5) 0.0122(5) Cl2' 0.176(5) 0.118(3) 0.083(3) 0.012(2) 0.044(3) -0.016(3) Cl2 0.079(4) 0.207(7) 0.154(6) 0.035(5) 0.048(4) 0.003(4) Cl3 0.265(8) 0.242(7) 0.123(4) 0.124(5) 0.069(5) 0.189(7) Cl3' 0.402(16) 0.192(8) 0.153(7) 0.096(6) -0.012(9) -0.151(10) Cl4 0.070(2) 0.221(6) 0.269(7) 0.152(6) 0.054(3) 0.049(3) Cl4' 0.262(12) 0.287(11) 0.123(5) 0.119(7) 0.082(7) 0.209(10) N1 0.045(2) 0.0284(18) 0.0340(18) 0.0113(15) 0.0182(16) -0.0031(15) N2 0.045(2) 0.0265(17) 0.0306(17) 0.0108(14) 0.0146(16) -0.0045(15) N5 0.049(2) 0.040(2) 0.0252(17) 0.0144(15) 0.0152(16) 0.0128(17) N6 0.053(2) 0.046(2) 0.0251(17) 0.0199(15) 0.0127(16) 0.0157(18) C1 0.053(3) 0.027(2) 0.035(2) 0.0076(18) 0.020(2) -0.005(2) C2 0.031(2) 0.029(2) 0.029(2) 0.0118(17) 0.0061(17) 0.0023(17) C3 0.039(3) 0.043(2) 0.033(2) 0.0182(19) 0.0108(19) -0.001(2) C4 0.060(3) 0.056(3) 0.033(2) 0.008(2) 0.022(2) -0.002(2) C5 0.077(4) 0.044(3) 0.040(3) -0.004(2) 0.023(3) -0.005(3) C6 0.057(3) 0.036(2) 0.045(3) 0.007(2) 0.019(2) -0.007(2) C7 0.035(2) 0.030(2) 0.031(2) 0.0113(17) 0.0105(18) 0.0017(18) C8 0.041(3) 0.0233(19) 0.029(2) 0.0103(16) 0.0145(18) -0.0013(17) C9 0.042(3) 0.024(2) 0.027(2) 0.0082(16) 0.0105(18) 0.0063(18) C10 0.053(3) 0.037(2) 0.041(2) 0.019(2) 0.013(2) 0.010(2) C11 0.060(3) 0.059(3) 0.050(3) 0.027(2) 0.011(3) 0.026(3) C12 0.037(3) 0.074(4) 0.053(3) 0.021(3) 0.013(2) 0.017(3) C13 0.035(3) 0.051(3) 0.042(2) 0.016(2) 0.016(2) 0.003(2) C14 0.034(2) 0.027(2) 0.029(2) 0.0087(16) 0.0125(17) 0.0038(17) C15 0.045(3) 0.044(2) 0.029(2) 0.0200(18) 0.0076(19) 0.013(2) C16 0.056(3) 0.041(2) 0.030(2) 0.0165(19) 0.014(2) 0.019(2) C17 0.080(4) 0.084(4) 0.037(3) 0.028(3) 0.026(3) 0.044(3) C18 0.094(5) 0.115(5) 0.062(4) 0.041(4) 0.038(3) 0.069(4) C19 0.096(5) 0.106(5) 0.057(3) 0.042(3) 0.026(3) 0.065(4) C20 0.085(4) 0.074(4) 0.038(3) 0.031(3) 0.019(3) 0.037(3) C21 0.057(3) 0.041(2) 0.030(2) 0.0177(19) 0.013(2) 0.017(2) C22 0.047(3) 0.045(2) 0.0221(19) 0.0189(18) 0.0098(18) 0.011(2) C23 0.048(3) 0.038(2) 0.025(2) 0.0143(18) 0.0072(19) 0.010(2) C24 0.068(3) 0.046(3) 0.036(2) 0.012(2) 0.013(2) 0.013(3) C25 0.069(4) 0.043(3) 0.048(3) 0.008(2) 0.009(3) 0.003(3) C26 0.060(3) 0.049(3) 0.062(3) 0.029(3) 0.010(3) -0.001(2) C27 0.055(3) 0.046(3) 0.037(2) 0.021(2) 0.016(2) 0.007(2) C28 0.046(3) 0.039(2) 0.028(2) 0.0197(18) 0.0074(19) 0.008(2) C29 0.075(4) 0.085(4) 0.081(4) 0.038(4) 0.022(3) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N1 2.274(3) 2_687 ? Mn1 N1 2.274(3) . ? Mn1 N5 2.436(3) 2_687 ? Mn1 N5 2.436(3) . ? Mn1 Cl1 2.5113(11) 2_687 ? Mn1 Cl1 2.5113(11) . ? Cl2' Cl2 1.439(9) . ? Cl2' C29 1.731(8) . ? Cl2' Cl4' 1.795(13) . ? Cl2 C29 1.745(9) . ? Cl2 Cl3 1.811(10) . ? Cl3 Cl3' 1.169(12) . ? Cl3 C29 1.638(7) . ? Cl3' C29 1.739(9) . ? Cl3' Cl4 2.168(15) . ? Cl4 Cl4' 1.331(12) . ? Cl4 C29 1.666(8) . ? Cl4' C29 1.742(9) . ? N1 C1 1.315(5) . ? N1 C2 1.399(5) . ? N2 C1 1.359(5) . ? N2 C7 1.389(5) . ? N2 C8 1.435(5) . ? N5 C15 1.308(5) . ? N5 C16 1.399(5) . ? N6 C15 1.362(5) . ? N6 C21 1.386(6) . ? N6 C22 1.434(5) . ? C1 H1A 0.9300 . ? C2 C7 1.391(5) . ? C2 C3 1.392(5) . ? C3 C4 1.365(6) . ? C3 H3A 0.9300 . ? C4 C5 1.403(6) . ? C4 H4A 0.9300 . ? C5 C6 1.376(6) . ? C5 H5A 0.9300 . ? C6 C7 1.375(6) . ? C6 H6A 0.9300 . ? C8 C9 1.392(6) . ? C8 C14 1.395(5) . ? C9 C10 1.419(6) . ? C9 C14 1.442(5) 2_577 ? C10 C11 1.348(7) . ? C10 H10A 0.9300 . ? C11 C12 1.405(7) . ? C11 H11A 0.9300 . ? C12 C13 1.356(6) . ? C12 H12A 0.9300 . ? C13 C14 1.424(6) 2_577 ? C13 H13A 0.9300 . ? C14 C13 1.424(6) 2_577 ? C14 C9 1.442(5) 2_577 ? C15 H15A 0.9300 . ? C16 C17 1.384(7) . ? C16 C21 1.398(5) . ? C17 C18 1.373(7) . ? C17 H17A 0.9300 . ? C18 C19 1.396(7) . ? C18 H18A 0.9300 . ? C19 C20 1.372(8) . ? C19 H19A 0.9300 . ? C20 C21 1.380(6) . ? C20 H20A 0.9300 . ? C22 C28 1.401(6) . ? C22 C23 1.401(6) . ? C23 C24 1.421(6) . ? C23 C28 1.440(6) 2_686 ? C24 C25 1.355(7) . ? C24 H24A 0.9300 . ? C25 C26 1.402(7) . ? C25 H25A 0.9300 . ? C26 C27 1.355(6) . ? C26 H26A 0.9300 . ? C27 C28 1.422(6) 2_686 ? C27 H27A 0.9300 . ? C28 C27 1.422(6) 2_686 ? C28 C23 1.440(6) 2_686 ? 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 N1 Mn1 N1 180.000(1) 2_687 . ? N1 Mn1 N5 92.39(12) 2_687 2_687 ? N1 Mn1 N5 87.61(12) . 2_687 ? N1 Mn1 N5 87.61(12) 2_687 . ? N1 Mn1 N5 92.39(12) . . ? N5 Mn1 N5 180.000(1) 2_687 . ? N1 Mn1 Cl1 91.89(9) 2_687 2_687 ? N1 Mn1 Cl1 88.11(9) . 2_687 ? N5 Mn1 Cl1 86.14(8) 2_687 2_687 ? N5 Mn1 Cl1 93.86(8) . 2_687 ? N1 Mn1 Cl1 88.11(9) 2_687 . ? N1 Mn1 Cl1 91.89(9) . . ? N5 Mn1 Cl1 93.86(8) 2_687 . ? N5 Mn1 Cl1 86.14(8) . . ? Cl1 Mn1 Cl1 180.000(1) 2_687 . ? Cl2 Cl2' C29 66.1(4) . . ? Cl2 Cl2' Cl4' 111.8(5) . . ? C29 Cl2' Cl4' 59.2(4) . . ? Cl2' Cl2 C29 65.0(4) . . ? Cl2' Cl2 Cl3 119.0(5) . . ? C29 Cl2 Cl3 54.8(3) . . ? Cl3' Cl3 C29 74.5(6) . . ? Cl3' Cl3 Cl2 127.8(8) . . ? C29 Cl3 Cl2 60.5(4) . . ? Cl3 Cl3' C29 65.2(5) . . ? Cl3 Cl3' Cl4 112.7(6) . . ? C29 Cl3' Cl4 49.0(4) . . ? Cl4' Cl4 C29 70.1(5) . . ? Cl4' Cl4 Cl3' 107.6(5) . . ? C29 Cl4 Cl3' 52.0(4) . . ? Cl4 Cl4' C29 64.0(4) . . ? Cl4 Cl4' Cl2' 122.2(6) . . ? C29 Cl4' Cl2' 58.6(4) . . ? C1 N1 C2 104.6(3) . . ? C1 N1 Mn1 120.0(3) . . ? C2 N1 Mn1 134.5(2) . . ? C1 N2 C7 106.4(3) . . ? C1 N2 C8 129.5(3) . . ? C7 N2 C8 124.0(3) . . ? C15 N5 C16 104.5(3) . . ? C15 N5 Mn1 119.7(3) . . ? C16 N5 Mn1 135.6(3) . . ? C15 N6 C21 106.3(3) . . ? C15 N6 C22 125.6(4) . . ? C21 N6 C22 127.9(3) . . ? N1 C1 N2 113.6(3) . . ? N1 C1 H1A 123.2 . . ? N2 C1 H1A 123.2 . . ? C7 C2 C3 119.1(4) . . ? C7 C2 N1 109.7(3) . . ? C3 C2 N1 131.2(3) . . ? C4 C3 C2 117.9(4) . . ? C4 C3 H3A 121.0 . . ? C2 C3 H3A 121.0 . . ? C3 C4 C5 122.0(4) . . ? C3 C4 H4A 119.0 . . ? C5 C4 H4A 119.0 . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C7 C6 C5 116.4(4) . . ? C7 C6 H6A 121.8 . . ? C5 C6 H6A 121.8 . . ? C6 C7 N2 130.6(4) . . ? C6 C7 C2 123.7(4) . . ? N2 C7 C2 105.7(3) . . ? C9 C8 C14 123.5(3) . . ? C9 C8 N2 118.4(4) . . ? C14 C8 N2 118.0(4) . . ? C8 C9 C10 123.3(4) . . ? C8 C9 C14 118.2(4) . 2_577 ? C10 C9 C14 118.4(4) . 2_577 ? C11 C10 C9 121.0(4) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 120.2(4) . 2_577 ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 2_577 . ? C8 C14 C13 123.3(4) . 2_577 ? C8 C14 C9 118.2(4) . 2_577 ? C13 C14 C9 118.4(4) 2_577 2_577 ? N5 C15 N6 114.0(4) . . ? N5 C15 H15A 123.0 . . ? N6 C15 H15A 123.0 . . ? C17 C16 C21 119.4(4) . . ? C17 C16 N5 130.9(4) . . ? C21 C16 N5 109.7(4) . . ? C18 C17 C16 117.7(4) . . ? C18 C17 H17A 121.1 . . ? C16 C17 H17A 121.1 . . ? C17 C18 C19 121.9(5) . . ? C17 C18 H18A 119.0 . . ? C19 C18 H18A 119.0 . . ? C20 C19 C18 121.4(5) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C21 116.1(4) . . ? C19 C20 H20A 121.9 . . ? C21 C20 H20A 121.9 . . ? C20 C21 N6 131.1(4) . . ? C20 C21 C16 123.4(4) . . ? N6 C21 C16 105.5(4) . . ? C28 C22 C23 122.9(4) . . ? C28 C22 N6 118.5(4) . . ? C23 C22 N6 118.6(4) . . ? C22 C23 C24 123.2(4) . . ? C22 C23 C28 118.6(4) . 2_686 ? C24 C23 C28 118.2(4) . 2_686 ? C25 C24 C23 120.9(4) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C27 C26 C25 120.9(5) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 120.6(4) . 2_686 ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 2_686 . ? C22 C28 C27 122.8(4) . 2_686 ? C22 C28 C23 118.5(4) . 2_686 ? C27 C28 C23 118.7(4) 2_686 2_686 ? Cl3 C29 Cl4 118.0(5) . . ? Cl3 C29 Cl2' 112.8(5) . . ? Cl4 C29 Cl2' 107.9(5) . . ? Cl3 C29 Cl3' 40.3(5) . . ? Cl4 C29 Cl3' 79.0(6) . . ? Cl2' C29 Cl3' 140.9(5) . . ? Cl3 C29 Cl4' 132.1(5) . . ? Cl4 C29 Cl4' 45.9(4) . . ? Cl2' C29 Cl4' 62.2(5) . . ? Cl3' C29 Cl4' 110.9(8) . . ? Cl3 C29 Cl2 64.6(5) . . ? Cl4 C29 Cl2 140.5(5) . . ? Cl2' C29 Cl2 48.9(4) . . ? Cl3' C29 Cl2 101.1(6) . . ? Cl4' C29 Cl2 100.7(6) . . ? 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 Cl4' Cl2' Cl2 C29 -38.7(5) . . . . ? C29 Cl2' Cl2 Cl3 10.1(4) . . . . ? Cl4' Cl2' Cl2 Cl3 -28.6(7) . . . . ? Cl2' Cl2 Cl3 Cl3' 23.1(11) . . . . ? C29 Cl2 Cl3 Cl3' 34.3(9) . . . . ? Cl2' Cl2 Cl3 C29 -11.2(5) . . . . ? Cl2 Cl3 Cl3' C29 -30.6(8) . . . . ? C29 Cl3 Cl3' Cl4 12.3(6) . . . . ? Cl2 Cl3 Cl3' Cl4 -18.3(13) . . . . ? Cl3 Cl3' Cl4 Cl4' 30.5(12) . . . . ? C29 Cl3' Cl4 Cl4' 45.3(6) . . . . ? Cl3 Cl3' Cl4 C29 -14.8(8) . . . . ? Cl3' Cl4 Cl4' C29 -36.6(5) . . . . ? C29 Cl4 Cl4' Cl2' -6.9(6) . . . . ? Cl3' Cl4 Cl4' Cl2' -43.5(9) . . . . ? Cl2 Cl2' Cl4' Cl4 48.9(8) . . . . ? C29 Cl2' Cl4' Cl4 7.3(6) . . . . ? Cl2 Cl2' Cl4' C29 41.7(5) . . . . ? N1 Mn1 N1 C1 172(100) 2_687 . . . ? N5 Mn1 N1 C1 45.7(3) 2_687 . . . ? N5 Mn1 N1 C1 -134.3(3) . . . . ? Cl1 Mn1 N1 C1 -40.5(3) 2_687 . . . ? Cl1 Mn1 N1 C1 139.5(3) . . . . ? N1 Mn1 N1 C2 5(100) 2_687 . . . ? N5 Mn1 N1 C2 -121.6(4) 2_687 . . . ? N5 Mn1 N1 C2 58.4(4) . . . . ? Cl1 Mn1 N1 C2 152.2(4) 2_687 . . . ? Cl1 Mn1 N1 C2 -27.8(4) . . . . ? N1 Mn1 N5 C15 89.3(3) 2_687 . . . ? N1 Mn1 N5 C15 -90.7(3) . . . . ? N5 Mn1 N5 C15 60(100) 2_687 . . . ? Cl1 Mn1 N5 C15 -179.0(3) 2_687 . . . ? Cl1 Mn1 N5 C15 1.0(3) . . . . ? N1 Mn1 N5 C16 -96.9(4) 2_687 . . . ? N1 Mn1 N5 C16 83.1(4) . . . . ? N5 Mn1 N5 C16 -126(100) 2_687 . . . ? Cl1 Mn1 N5 C16 -5.2(4) 2_687 . . . ? Cl1 Mn1 N5 C16 174.8(4) . . . . ? C2 N1 C1 N2 0.8(5) . . . . ? Mn1 N1 C1 N2 -169.9(3) . . . . ? C7 N2 C1 N1 -0.7(5) . . . . ? C8 N2 C1 N1 174.9(4) . . . . ? C1 N1 C2 C7 -0.5(5) . . . . ? Mn1 N1 C2 C7 168.1(3) . . . . ? C1 N1 C2 C3 178.8(5) . . . . ? Mn1 N1 C2 C3 -12.6(7) . . . . ? C7 C2 C3 C4 -0.3(6) . . . . ? N1 C2 C3 C4 -179.6(4) . . . . ? C2 C3 C4 C5 -0.7(8) . . . . ? C3 C4 C5 C6 0.7(9) . . . . ? C4 C5 C6 C7 0.2(8) . . . . ? C5 C6 C7 N2 179.5(5) . . . . ? C5 C6 C7 C2 -1.2(7) . . . . ? C1 N2 C7 C6 179.7(5) . . . . ? C8 N2 C7 C6 3.8(7) . . . . ? C1 N2 C7 C2 0.3(5) . . . . ? C8 N2 C7 C2 -175.6(4) . . . . ? C3 C2 C7 C6 1.2(7) . . . . ? N1 C2 C7 C6 -179.3(4) . . . . ? C3 C2 C7 N2 -179.3(4) . . . . ? N1 C2 C7 N2 0.1(5) . . . . ? C1 N2 C8 C9 97.6(5) . . . . ? C7 N2 C8 C9 -87.5(5) . . . . ? C1 N2 C8 C14 -86.4(5) . . . . ? C7 N2 C8 C14 88.5(5) . . . . ? C14 C8 C9 C10 177.6(4) . . . . ? N2 C8 C9 C10 -6.6(6) . . . . ? C14 C8 C9 C14 -1.6(6) . . . 2_577 ? N2 C8 C9 C14 174.2(3) . . . 2_577 ? C8 C9 C10 C11 179.3(4) . . . . ? C14 C9 C10 C11 -1.5(6) 2_577 . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C10 C11 C12 C13 1.8(8) . . . . ? C11 C12 C13 C14 -0.9(7) . . . 2_577 ? C9 C8 C14 C13 -178.4(4) . . . 2_577 ? N2 C8 C14 C13 5.8(6) . . . 2_577 ? C9 C8 C14 C9 1.6(6) . . . 2_577 ? N2 C8 C14 C9 -174.2(3) . . . 2_577 ? C16 N5 C15 N6 0.9(5) . . . . ? Mn1 N5 C15 N6 176.4(3) . . . . ? C21 N6 C15 N5 -1.4(5) . . . . ? C22 N6 C15 N5 -176.8(4) . . . . ? C15 N5 C16 C17 -179.5(5) . . . . ? Mn1 N5 C16 C17 6.1(8) . . . . ? C15 N5 C16 C21 0.0(5) . . . . ? Mn1 N5 C16 C21 -174.4(3) . . . . ? C21 C16 C17 C18 1.2(8) . . . . ? N5 C16 C17 C18 -179.3(5) . . . . ? C16 C17 C18 C19 -0.3(10) . . . . ? C17 C18 C19 C20 -1.0(11) . . . . ? C18 C19 C20 C21 1.4(9) . . . . ? C19 C20 C21 N6 -180.0(5) . . . . ? C19 C20 C21 C16 -0.5(8) . . . . ? C15 N6 C21 C20 -179.2(5) . . . . ? C22 N6 C21 C20 -3.9(8) . . . . ? C15 N6 C21 C16 1.3(5) . . . . ? C22 N6 C21 C16 176.5(4) . . . . ? C17 C16 C21 C20 -0.9(7) . . . . ? N5 C16 C21 C20 179.6(4) . . . . ? C17 C16 C21 N6 178.8(4) . . . . ? N5 C16 C21 N6 -0.8(5) . . . . ? C15 N6 C22 C28 85.0(5) . . . . ? C21 N6 C22 C28 -89.5(5) . . . . ? C15 N6 C22 C23 -94.0(5) . . . . ? C21 N6 C22 C23 91.6(5) . . . . ? C28 C22 C23 C24 178.5(4) . . . . ? N6 C22 C23 C24 -2.6(7) . . . . ? C28 C22 C23 C28 -0.9(7) . . . 2_686 ? N6 C22 C23 C28 178.0(4) . . . 2_686 ? C22 C23 C24 C25 -179.6(5) . . . . ? C28 C23 C24 C25 -0.2(7) 2_686 . . . ? C23 C24 C25 C26 -0.1(8) . . . . ? C24 C25 C26 C27 0.0(8) . . . . ? C25 C26 C27 C28 0.4(8) . . . 2_686 ? C23 C22 C28 C27 -180.0(4) . . . 2_686 ? N6 C22 C28 C27 1.1(6) . . . 2_686 ? C23 C22 C28 C23 0.9(7) . . . 2_686 ? N6 C22 C28 C23 -178.0(4) . . . 2_686 ? Cl3' Cl3 C29 Cl4 -16.8(10) . . . . ? Cl2 Cl3 C29 Cl4 135.7(6) . . . . ? Cl3' Cl3 C29 Cl2' -143.7(9) . . . . ? Cl2 Cl3 C29 Cl2' 8.8(4) . . . . ? Cl2 Cl3 C29 Cl3' 152.5(9) . . . . ? Cl3' Cl3 C29 Cl4' -71.2(12) . . . . ? Cl2 Cl3 C29 Cl4' 81.3(9) . . . . ? Cl3' Cl3 C29 Cl2 -152.5(9) . . . . ? Cl4' Cl4 C29 Cl3 -122.8(6) . . . . ? Cl3' Cl4 C29 Cl3 11.0(6) . . . . ? Cl4' Cl4 C29 Cl2' 6.3(6) . . . . ? Cl3' Cl4 C29 Cl2' 140.2(6) . . . . ? Cl4' Cl4 C29 Cl3' -133.8(6) . . . . ? Cl3' Cl4 C29 Cl4' 133.8(6) . . . . ? Cl4' Cl4 C29 Cl2 -39.6(9) . . . . ? Cl3' Cl4 C29 Cl2 94.2(9) . . . . ? Cl2 Cl2' C29 Cl3 -10.6(5) . . . . ? Cl4' Cl2' C29 Cl3 126.9(6) . . . . ? Cl2 Cl2' C29 Cl4 -142.6(5) . . . . ? Cl4' Cl2' C29 Cl4 -5.1(4) . . . . ? Cl2 Cl2' C29 Cl3' -48.0(12) . . . . ? Cl4' Cl2' C29 Cl3' 89.5(12) . . . . ? Cl2 Cl2' C29 Cl4' -137.5(5) . . . . ? Cl4' Cl2' C29 Cl2 137.5(5) . . . . ? Cl4 Cl3' C29 Cl3 -164.9(8) . . . . ? Cl3 Cl3' C29 Cl4 164.9(8) . . . . ? Cl3 Cl3' C29 Cl2' 60.0(14) . . . . ? Cl4 Cl3' C29 Cl2' -104.9(10) . . . . ? Cl3 Cl3' C29 Cl4' 131.2(8) . . . . ? Cl4 Cl3' C29 Cl4' -33.7(5) . . . . ? Cl3 Cl3' C29 Cl2 25.2(8) . . . . ? Cl4 Cl3' C29 Cl2 -139.8(5) . . . . ? Cl4 Cl4' C29 Cl3 90.3(9) . . . . ? Cl2' Cl4' C29 Cl3 -96.5(9) . . . . ? Cl2' Cl4' C29 Cl4 173.2(6) . . . . ? Cl4 Cl4' C29 Cl2' -173.2(6) . . . . ? Cl4 Cl4' C29 Cl3' 49.3(6) . . . . ? Cl2' Cl4' C29 Cl3' -137.5(6) . . . . ? Cl4 Cl4' C29 Cl2 155.6(6) . . . . ? Cl2' Cl4' C29 Cl2 -31.2(4) . . . . ? Cl2' Cl2 C29 Cl3 169.2(5) . . . . ? Cl2' Cl2 C29 Cl4 65.3(8) . . . . ? Cl3 Cl2 C29 Cl4 -103.9(9) . . . . ? Cl3 Cl2 C29 Cl2' -169.2(5) . . . . ? Cl2' Cl2 C29 Cl3' 151.4(7) . . . . ? Cl3 Cl2 C29 Cl3' -17.7(6) . . . . ? Cl2' Cl2 C29 Cl4' 37.5(5) . . . . ? Cl3 Cl2 C29 Cl4' -131.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.004 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.068 #===END