Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew D. Burrows' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email A.D.BURROWS@BATH.AC.UK _publ_section_title ; The stepwise formation of mixed-metal coordination networks using complexes of 3-cyanoacetylacetonate ; loop_ _publ_author_name A.D.Burrows 'Kevin Cassar' M.Mahon 'John E Warren' # Attachment 'b702074k.cif' data_compound_2_h06kc2 _database_code_depnum_ccdc_archive 'CCDC 636527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Cu6 N6 O18' _chemical_formula_weight 1312.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6030(1) _cell_length_b 10.6410(2) _cell_length_c 14.7610(3) _cell_angle_alpha 102.936(1) _cell_angle_beta 100.006(1) _cell_angle_gamma 104.594(1) _cell_volume 1235.97(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17677 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _diffrn_measurement_method CCD _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 2.613 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 00.77 _exptl_absorpt_correction_T_max 00.84 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32325 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.62 _diffrn_reflns_theta_max 30.08 _reflns_number_total 7172 _reflns_number_gt 5097 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0495P)^2^+0.0758P] 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 0.0140(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7172 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Cu1 Cu 0.56988(3) 0.51048(3) 0.602018(18) 0.02098(9) Uani 1 1 d . . . O1 O 0.7680(2) 0.48357(16) 0.66652(11) 0.0239(3) Uani 1 1 d . . . N1 N 0.7934(3) 0.4517(3) 0.98198(16) 0.0405(6) Uani 1 1 d . . . C1 C 0.9677(3) 0.4525(3) 0.78349(18) 0.0309(5) Uani 1 1 d . . . H1A H 1.0309 0.4609 0.7348 0.046 Uiso 1 1 calc R . . H1B H 0.9518 0.3625 0.7935 0.046 Uiso 1 1 calc R . . H1C H 1.0286 0.5217 0.8438 0.046 Uiso 1 1 calc R . . Cu2 Cu 0.47683(3) 0.77389(3) 0.576952(18) 0.02201(9) Uani 1 1 d . . . O2 O 0.4712(2) 0.50383(18) 0.70915(12) 0.0287(4) Uani 1 1 d . . . N2 N 0.8820(3) 0.8380(3) 1.17903(17) 0.0438(6) Uani 1 1 d . . . C2 C 0.8019(3) 0.4712(2) 0.75039(16) 0.0226(4) Uani 1 1 d . . . Cu3 Cu 0.61955(3) 0.80809(3) 0.781103(18) 0.02297(9) Uani 1 1 d . . . O3 O 0.37927(18) 0.53214(16) 0.52255(11) 0.0211(3) Uani 1 1 d . . . N3 N 0.3008(3) 0.9380(2) 0.23019(15) 0.0348(5) Uani 1 1 d . . . C3 C 0.6933(3) 0.4728(2) 0.81230(16) 0.0238(5) Uani 1 1 d . . . O4 O 0.67087(18) 0.75480(16) 0.65743(11) 0.0226(3) Uani 1 1 d . . . C4 C 0.5335(3) 0.4885(2) 0.78880(16) 0.0237(5) Uani 1 1 d . . . O5 O 0.4166(2) 0.78827(19) 0.69619(11) 0.0287(4) Uani 1 1 d . . . C5 C 0.4268(3) 0.4879(3) 0.85834(17) 0.0315(5) Uani 1 1 d . . . H5A H 0.3659 0.5535 0.8536 0.047 Uiso 1 1 calc R . . H5B H 0.4963 0.5124 0.9235 0.047 Uiso 1 1 calc R . . H5C H 0.3481 0.3973 0.8436 0.047 Uiso 1 1 calc R . . O6 O 0.8316(2) 0.81327(17) 0.85157(11) 0.0268(4) Uani 1 1 d . . . C6 C 0.7494(3) 0.4608(3) 0.90617(17) 0.0304(5) Uani 1 1 d . . . O7 O 0.5363(2) 0.83329(18) 0.89384(11) 0.0281(4) Uani 1 1 d . . . C7 C 0.2155(3) 0.4883(3) 0.53609(17) 0.0286(5) Uani 1 1 d . . . H7A H 0.1863 0.3921 0.5330 0.043 Uiso 1 1 calc R . . H7B H 0.1366 0.5022 0.4856 0.043 Uiso 1 1 calc R . . H7C H 0.2114 0.5408 0.5989 0.043 Uiso 1 1 calc R . . O8 O 0.5787(2) 0.79313(17) 0.47198(11) 0.0268(4) Uani 1 1 d . . . C8 C 1.0457(3) 0.8122(3) 0.97508(18) 0.0305(5) Uani 1 1 d . . . H8A H 1.0384 0.7242 0.9872 0.046 Uiso 1 1 calc R . . H8B H 1.1019 0.8845 1.0346 0.046 Uiso 1 1 calc R . . H8C H 1.1086 0.8230 0.9265 0.046 Uiso 1 1 calc R . . O9 O 0.2825(2) 0.80866(17) 0.51497(11) 0.0251(3) Uani 1 1 d . . . C9 C 0.8746(3) 0.8194(2) 0.93980(16) 0.0242(5) Uani 1 1 d . . . C10 C 0.7710(3) 0.8298(2) 1.00336(16) 0.0240(5) Uani 1 1 d . . . C11 C 0.6077(3) 0.8373(2) 0.97805(16) 0.0243(5) Uani 1 1 d . . . C12 C 0.5097(3) 0.8515(3) 1.05154(17) 0.0326(6) Uani 1 1 d . . . H12A H 0.5551 0.9427 1.0961 0.049 Uiso 1 1 calc R . . H12B H 0.5156 0.7845 1.0870 0.049 Uiso 1 1 calc R . . H12C H 0.3940 0.8366 1.0199 0.049 Uiso 1 1 calc R . . C13 C 0.8341(3) 0.8347(3) 1.10085(17) 0.0298(5) Uani 1 1 d . . . C14 C 0.2671(3) 0.7977(3) 0.71993(18) 0.0305(5) Uani 1 1 d . . . H14A H 0.2290 0.7291 0.7524 0.046 Uiso 1 1 calc R . . H14B H 0.1829 0.7827 0.6613 0.046 Uiso 1 1 calc R . . H14C H 0.2855 0.8879 0.7626 0.046 Uiso 1 1 calc R . . C15 C 0.8390(3) 0.8046(2) 0.65182(17) 0.0266(5) Uani 1 1 d . . . H15A H 0.8892 0.8968 0.6944 0.040 Uiso 1 1 calc R . . H15B H 0.8413 0.8051 0.5858 0.040 Uiso 1 1 calc R . . H15C H 0.9016 0.7458 0.6715 0.040 Uiso 1 1 calc R . . C16 C 0.6425(3) 0.8544(3) 0.33644(18) 0.0316(5) Uani 1 1 d . . . H16A H 0.7125 0.9489 0.3571 0.047 Uiso 1 1 calc R . . H16B H 0.5777 0.8330 0.2704 0.047 Uiso 1 1 calc R . . H16C H 0.7125 0.7949 0.3396 0.047 Uiso 1 1 calc R . . C17 C 0.5282(3) 0.8337(2) 0.40065(16) 0.0232(4) Uani 1 1 d . . . C18 C 0.3726(3) 0.8584(2) 0.38096(16) 0.0234(5) Uani 1 1 d . . . C19 C 0.2577(3) 0.8427(2) 0.43866(16) 0.0226(4) Uani 1 1 d . . . C20 C 0.0947(3) 0.8691(3) 0.41088(18) 0.0295(5) Uani 1 1 d . . . H20A H 0.0125 0.8158 0.4370 0.044 Uiso 1 1 calc R . . H20B H 0.0570 0.8431 0.3409 0.044 Uiso 1 1 calc R . . H20C H 0.1085 0.9655 0.4367 0.044 Uiso 1 1 calc R . . C21 C 0.3314(3) 0.9019(2) 0.29670(17) 0.0268(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01915(14) 0.03263(16) 0.01524(14) 0.01013(11) 0.00515(10) 0.01124(12) O1 0.0228(8) 0.0348(9) 0.0169(8) 0.0095(6) 0.0039(6) 0.0125(7) N1 0.0361(12) 0.0621(16) 0.0294(12) 0.0202(11) 0.0086(10) 0.0185(11) C1 0.0275(12) 0.0435(14) 0.0235(12) 0.0107(10) 0.0033(10) 0.0150(11) Cu2 0.01950(15) 0.03369(16) 0.01675(14) 0.00973(11) 0.00539(10) 0.01185(12) O2 0.0259(8) 0.0487(10) 0.0212(8) 0.0179(7) 0.0094(7) 0.0184(8) N2 0.0365(13) 0.0657(16) 0.0292(12) 0.0199(11) 0.0043(10) 0.0121(12) C2 0.0238(11) 0.0260(11) 0.0184(10) 0.0069(8) 0.0017(8) 0.0099(9) Cu3 0.02125(15) 0.03402(17) 0.01587(14) 0.00781(11) 0.00402(11) 0.01185(12) O3 0.0160(7) 0.0334(8) 0.0167(7) 0.0094(6) 0.0054(6) 0.0095(6) N3 0.0366(12) 0.0471(13) 0.0301(11) 0.0209(10) 0.0119(9) 0.0177(10) C3 0.0251(11) 0.0295(11) 0.0179(10) 0.0080(9) 0.0040(9) 0.0097(9) O4 0.0168(7) 0.0350(9) 0.0176(7) 0.0088(6) 0.0043(6) 0.0092(7) C4 0.0274(12) 0.0265(11) 0.0179(10) 0.0088(9) 0.0057(9) 0.0073(9) O5 0.0212(8) 0.0520(11) 0.0171(8) 0.0103(7) 0.0071(6) 0.0162(8) C5 0.0315(13) 0.0468(15) 0.0227(12) 0.0148(11) 0.0108(10) 0.0161(11) O6 0.0249(8) 0.0394(9) 0.0190(8) 0.0099(7) 0.0048(6) 0.0137(7) C6 0.0282(12) 0.0393(13) 0.0249(12) 0.0107(10) 0.0064(10) 0.0111(11) O7 0.0277(8) 0.0414(9) 0.0204(8) 0.0106(7) 0.0063(7) 0.0176(8) C7 0.0188(11) 0.0441(14) 0.0222(11) 0.0089(10) 0.0076(9) 0.0068(10) O8 0.0255(8) 0.0416(9) 0.0203(8) 0.0138(7) 0.0084(7) 0.0160(7) C8 0.0269(12) 0.0398(13) 0.0263(12) 0.0118(10) 0.0038(10) 0.0123(11) O9 0.0229(8) 0.0367(9) 0.0206(8) 0.0119(7) 0.0066(6) 0.0132(7) C9 0.0255(11) 0.0242(11) 0.0222(11) 0.0078(9) 0.0017(9) 0.0081(9) C10 0.0259(11) 0.0272(11) 0.0198(11) 0.0080(9) 0.0047(9) 0.0091(9) C11 0.0288(12) 0.0247(10) 0.0199(11) 0.0071(9) 0.0058(9) 0.0082(9) C12 0.0347(13) 0.0469(15) 0.0207(12) 0.0112(11) 0.0096(10) 0.0167(12) C13 0.0267(12) 0.0391(13) 0.0242(12) 0.0110(10) 0.0033(10) 0.0108(11) C14 0.0228(11) 0.0483(15) 0.0253(12) 0.0120(11) 0.0086(9) 0.0162(11) C15 0.0197(11) 0.0357(12) 0.0262(12) 0.0113(10) 0.0074(9) 0.0080(10) C16 0.0276(12) 0.0465(15) 0.0258(12) 0.0156(11) 0.0114(10) 0.0122(11) C17 0.0234(11) 0.0271(11) 0.0191(11) 0.0056(9) 0.0059(9) 0.0075(9) C18 0.0245(11) 0.0267(11) 0.0197(11) 0.0076(9) 0.0032(9) 0.0094(9) C19 0.0234(11) 0.0236(10) 0.0209(11) 0.0068(9) 0.0030(9) 0.0084(9) C20 0.0250(12) 0.0445(14) 0.0266(12) 0.0161(11) 0.0085(10) 0.0170(11) C21 0.0263(12) 0.0303(12) 0.0271(12) 0.0093(10) 0.0080(10) 0.0117(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9232(15) . ? Cu1 O2 1.9269(16) . ? Cu1 O3 1.9394(15) . ? Cu1 O3 1.9453(16) 2_666 ? Cu1 O4 2.4178(17) . ? Cu1 Cu1 2.9786(5) 2_666 ? O1 C2 1.265(3) . ? N1 C6 1.151(3) . ? C1 C2 1.503(3) . ? Cu2 O5 1.9042(16) . ? Cu2 O9 1.9235(16) . ? Cu2 O8 1.9325(16) . ? Cu2 O4 1.9567(15) . ? Cu2 O3 2.3916(17) . ? Cu2 Cu3 2.9528(4) . ? O2 C4 1.268(3) . ? N2 C13 1.146(3) . ? C2 C3 1.416(3) . ? Cu3 O5 1.8973(16) . ? Cu3 O7 1.9146(17) . ? Cu3 O6 1.9173(16) . ? Cu3 O4 1.9472(16) . ? O3 C7 1.432(3) . ? O3 Cu1 1.9453(16) 2_666 ? N3 C21 1.145(3) . ? C3 C4 1.419(3) . ? C3 C6 1.431(3) . ? O4 C15 1.434(3) . ? C4 C5 1.491(3) . ? O5 C14 1.412(3) . ? O6 C9 1.273(3) . ? O7 C11 1.274(3) . ? O8 C17 1.274(3) . ? C8 C9 1.501(3) . ? O9 C19 1.258(3) . ? C9 C10 1.408(3) . ? C10 C11 1.417(3) . ? C10 C13 1.431(3) . ? C11 C12 1.489(3) . ? C16 C17 1.490(3) . ? C17 C18 1.423(3) . ? C18 C19 1.416(3) . ? C18 C21 1.440(3) . ? C19 C20 1.504(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 92.53(7) . . ? O1 Cu1 O3 172.90(6) . . ? O2 Cu1 O3 94.32(7) . . ? O1 Cu1 O3 93.03(6) . 2_666 ? O2 Cu1 O3 163.62(8) . 2_666 ? O3 Cu1 O3 79.88(7) . 2_666 ? O1 Cu1 O4 95.26(6) . . ? O2 Cu1 O4 91.01(7) . . ? O3 Cu1 O4 86.46(6) . . ? O3 Cu1 O4 103.80(6) 2_666 . ? O1 Cu1 Cu1 132.89(5) . 2_666 ? O2 Cu1 Cu1 132.51(5) . 2_666 ? O3 Cu1 Cu1 40.01(5) . 2_666 ? O3 Cu1 Cu1 39.86(4) 2_666 2_666 ? O4 Cu1 Cu1 96.63(4) . 2_666 ? C2 O1 Cu1 127.53(15) . . ? O5 Cu2 O9 94.08(7) . . ? O5 Cu2 O8 167.47(8) . . ? O9 Cu2 O8 91.66(7) . . ? O5 Cu2 O4 78.55(7) . . ? O9 Cu2 O4 171.57(7) . . ? O8 Cu2 O4 94.81(6) . . ? O5 Cu2 O3 95.67(7) . . ? O9 Cu2 O3 98.08(6) . . ? O8 Cu2 O3 94.54(6) . . ? O4 Cu2 O3 86.81(6) . . ? O5 Cu2 Cu3 38.95(5) . . ? O9 Cu2 Cu3 131.19(5) . . ? O8 Cu2 Cu3 131.79(5) . . ? O4 Cu2 Cu3 40.74(5) . . ? O3 Cu2 Cu3 98.98(4) . . ? C4 O2 Cu1 127.67(16) . . ? O1 C2 C3 124.0(2) . . ? O1 C2 C1 116.4(2) . . ? C3 C2 C1 119.6(2) . . ? O5 Cu3 O7 94.88(7) . . ? O5 Cu3 O6 171.91(7) . . ? O7 Cu3 O6 92.42(7) . . ? O5 Cu3 O4 78.95(7) . . ? O7 Cu3 O4 170.08(7) . . ? O6 Cu3 O4 93.33(7) . . ? O5 Cu3 Cu2 39.12(5) . . ? O7 Cu3 Cu2 133.89(5) . . ? O6 Cu3 Cu2 133.69(5) . . ? O4 Cu3 Cu2 40.97(4) . . ? C7 O3 Cu1 122.57(13) . . ? C7 O3 Cu1 123.04(13) . 2_666 ? Cu1 O3 Cu1 100.12(7) . 2_666 ? C7 O3 Cu2 108.26(14) . . ? Cu1 O3 Cu2 93.99(6) . . ? Cu1 O3 Cu2 103.88(7) 2_666 . ? C2 C3 C4 124.7(2) . . ? C2 C3 C6 118.0(2) . . ? C4 C3 C6 117.3(2) . . ? C15 O4 Cu3 117.95(13) . . ? C15 O4 Cu2 125.81(13) . . ? Cu3 O4 Cu2 98.29(7) . . ? C15 O4 Cu1 111.32(13) . . ? Cu3 O4 Cu1 106.91(7) . . ? Cu2 O4 Cu1 92.74(6) . . ? O2 C4 C3 123.6(2) . . ? O2 C4 C5 115.4(2) . . ? C3 C4 C5 121.1(2) . . ? C14 O5 Cu3 127.54(14) . . ? C14 O5 Cu2 130.19(14) . . ? Cu3 O5 Cu2 101.93(8) . . ? C9 O6 Cu3 127.58(16) . . ? N1 C6 C3 179.3(3) . . ? C11 O7 Cu3 127.75(16) . . ? C17 O8 Cu2 127.77(15) . . ? C19 O9 Cu2 128.34(15) . . ? O6 C9 C10 123.9(2) . . ? O6 C9 C8 116.4(2) . . ? C10 C9 C8 119.7(2) . . ? C9 C10 C11 124.6(2) . . ? C9 C10 C13 118.3(2) . . ? C11 C10 C13 117.1(2) . . ? O7 C11 C10 123.5(2) . . ? O7 C11 C12 116.2(2) . . ? C10 C11 C12 120.3(2) . . ? N2 C13 C10 178.8(3) . . ? O8 C17 C18 123.4(2) . . ? O8 C17 C16 116.1(2) . . ? C18 C17 C16 120.5(2) . . ? C19 C18 C17 124.1(2) . . ? C19 C18 C21 118.8(2) . . ? C17 C18 C21 117.1(2) . . ? O9 C19 C18 124.1(2) . . ? O9 C19 C20 115.7(2) . . ? C18 C19 C20 120.13(19) . . ? N3 C21 C18 179.0(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.913 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.095 #===END data_compound_3_h05kc2 _database_code_depnum_ccdc_archive 'CCDC 636528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H18 Fe N3 O6' _chemical_formula_weight 428.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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 P21/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 15.3320(2) _cell_length_b 13.0220(2) _cell_length_c 21.3520(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.265(1) _cell_angle_gamma 90.00 _cell_volume 3916.36(11) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 37230 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71520 _diffrn_reflns_av_R_equivalents 0.1389 _diffrn_reflns_av_sigmaI/netI 0.1470 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11424 _reflns_number_gt 5305 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0660P)^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 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11424 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1643 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 Fe1 Fe -0.19144(3) 0.80255(4) 0.45489(2) 0.02630(14) Uani 1 1 d . . . O1 O -0.24658(15) 0.66858(17) 0.41369(11) 0.0322(5) Uani 1 1 d . . . N1 N -0.0465(2) 0.4125(2) 0.38706(15) 0.0479(8) Uani 1 1 d . . . C1 C -0.2746(2) 0.5011(3) 0.36812(18) 0.0408(9) Uani 1 1 d . . . H1A H -0.2646 0.4468 0.4021 0.061 Uiso 1 1 calc R . . H1B H -0.2612 0.4741 0.3300 0.061 Uiso 1 1 calc R . . H1C H -0.3407 0.5246 0.3513 0.061 Uiso 1 1 calc R . . Fe2 Fe 0.32875(3) 0.80196(3) 0.49195(2) 0.02467(13) Uani 1 1 d . . . O2 O -0.06681(15) 0.74652(17) 0.46325(11) 0.0309(5) Uani 1 1 d . . . N2 N -0.4816(2) 1.0286(3) 0.22500(16) 0.0495(8) Uani 1 1 d . . . C2 C -0.2096(2) 0.5893(3) 0.40015(16) 0.0303(8) Uani 1 1 d . . . O3 O -0.32179(14) 0.85516(17) 0.43147(10) 0.0287(5) Uani 1 1 d . . . N3 N 0.0364(2) 0.9243(3) 0.74193(17) 0.0538(9) Uani 1 1 d . . . C3 C -0.1116(2) 0.5819(2) 0.41448(16) 0.0289(7) Uani 1 1 d . . . O4 O -0.19870(15) 0.86623(17) 0.36796(11) 0.0305(5) Uani 1 1 d . . . N4 N 0.3315(2) 0.7399(3) 0.76686(17) 0.0563(9) Uani 1 1 d . . . C4 C -0.0454(2) 0.6628(3) 0.44259(16) 0.0282(7) Uani 1 1 d . . . O5 O -0.12638(15) 0.92965(16) 0.50300(11) 0.0292(5) Uani 1 1 d . . . N5 N 0.4177(3) 0.4010(3) 0.39851(16) 0.0542(9) Uani 1 1 d . . . C5 C 0.0545(2) 0.6507(3) 0.44840(19) 0.0416(9) Uani 1 1 d . . . H5A H 0.0903 0.7135 0.4676 0.062 Uiso 1 1 calc R . . H5B H 0.0544 0.6382 0.4031 0.062 Uiso 1 1 calc R . . H5C H 0.0842 0.5925 0.4783 0.062 Uiso 1 1 calc R . . O6 O -0.18066(15) 0.75532(16) 0.54652(11) 0.0301(5) Uani 1 1 d . . . N6 N 0.2223(3) 1.0946(3) 0.26030(16) 0.0616(10) Uani 1 1 d . . . C6 C -0.0755(2) 0.4879(3) 0.39823(16) 0.0347(8) Uani 1 1 d . . . O7 O 0.23910(15) 0.83470(16) 0.53597(10) 0.0286(5) Uani 1 1 d . . . C7 C -0.4758(2) 0.9268(3) 0.37746(16) 0.0312(8) Uani 1 1 d . . . H7A H -0.4872 0.8861 0.4121 0.047 Uiso 1 1 calc R . . H7B H -0.5237 0.9099 0.3322 0.047 Uiso 1 1 calc R . . H7C H -0.4797 1.0001 0.3866 0.047 Uiso 1 1 calc R . . O8 O 0.42781(14) 0.80315(16) 0.58644(10) 0.0278(5) Uani 1 1 d . . . C8 C -0.3782(2) 0.9029(2) 0.37977(16) 0.0279(7) Uani 1 1 d . . . O9 O 0.28949(15) 0.65566(17) 0.49081(11) 0.0316(5) Uani 1 1 d . . . C9 C -0.3529(2) 0.9343(2) 0.32547(15) 0.0268(7) Uani 1 1 d . . . O10 O 0.42715(15) 0.75100(16) 0.46063(10) 0.0281(5) Uani 1 1 d . . . C10 C -0.2651(2) 0.9135(3) 0.32204(16) 0.0294(8) Uani 1 1 d . . . O11 O 0.22608(15) 0.81156(17) 0.39916(11) 0.0316(5) Uani 1 1 d . . . C11 C -0.2471(2) 0.9453(3) 0.26066(16) 0.0406(9) Uani 1 1 d . . . H11A H -0.1786 0.9467 0.2722 0.061 Uiso 1 1 calc R . . H11B H -0.2738 1.0138 0.2460 0.061 Uiso 1 1 calc R . . H11C H -0.2773 0.8960 0.2237 0.061 Uiso 1 1 calc R . . O12 O 0.36019(14) 0.94514(16) 0.47751(10) 0.0278(5) Uani 1 1 d . . . C12 C -0.4239(3) 0.9865(3) 0.26973(18) 0.0347(8) Uani 1 1 d . . . C13 C -0.1236(3) 0.7188(3) 0.66365(17) 0.0385(9) Uani 1 1 d . . . H13A H -0.1879 0.6957 0.6559 0.058 Uiso 1 1 calc R . . H13B H -0.0974 0.7581 0.7062 0.058 Uiso 1 1 calc R . . H13C H -0.0832 0.6590 0.6669 0.058 Uiso 1 1 calc R . . C14 C -0.1271(2) 0.7851(2) 0.60569(17) 0.0306(8) Uani 1 1 d . . . C15 C -0.0739(2) 0.8769(2) 0.61783(15) 0.0261(7) Uani 1 1 d . . . C16 C -0.0793(2) 0.9476(2) 0.56580(17) 0.0267(7) Uani 1 1 d . . . C17 C -0.0311(2) 1.0500(2) 0.58220(17) 0.0329(8) Uani 1 1 d . . . H17A H 0.0237 1.0500 0.5695 0.049 Uiso 1 1 calc R . . H17B H -0.0097 1.0633 0.6312 0.049 Uiso 1 1 calc R . . H17C H -0.0758 1.1037 0.5567 0.049 Uiso 1 1 calc R . . C18 C -0.0125(3) 0.9031(3) 0.6871(2) 0.0377(9) Uani 1 1 d . . . C19 C 0.1578(2) 0.8311(3) 0.60954(17) 0.0367(9) Uani 1 1 d . . . H19A H 0.1238 0.8921 0.5852 0.055 Uiso 1 1 calc R . . H19B H 0.1751 0.8400 0.6586 0.055 Uiso 1 1 calc R . . H19C H 0.1169 0.7706 0.5936 0.055 Uiso 1 1 calc R . . C20 C 0.2460(2) 0.8165(2) 0.59622(16) 0.0265(7) Uani 1 1 d . . . C21 C 0.3327(2) 0.7845(2) 0.64926(15) 0.0260(7) Uani 1 1 d . . . C22 C 0.4203(2) 0.7824(2) 0.64218(16) 0.0261(7) Uani 1 1 d . . . C23 C 0.5110(2) 0.7578(3) 0.70113(16) 0.0369(8) Uani 1 1 d . . . H23A H 0.5361 0.6924 0.6927 0.055 Uiso 1 1 calc R . . H23B H 0.4989 0.7524 0.7428 0.055 Uiso 1 1 calc R . . H23C H 0.5573 0.8125 0.7066 0.055 Uiso 1 1 calc R . . C24 C 0.3314(2) 0.7600(3) 0.71441(19) 0.0374(8) Uani 1 1 d . . . C25 C 0.2459(3) 0.4864(3) 0.45141(19) 0.0440(9) Uani 1 1 d . . . H25A H 0.2096 0.4919 0.4801 0.066 Uiso 1 1 calc R . . H25B H 0.2850 0.4242 0.4636 0.066 Uiso 1 1 calc R . . H25C H 0.2020 0.4827 0.4034 0.066 Uiso 1 1 calc R . . C26 C 0.3089(2) 0.5790(2) 0.46227(16) 0.0294(8) Uani 1 1 d . . . C27 C 0.3839(2) 0.5770(2) 0.44008(15) 0.0282(7) Uani 1 1 d . . . C28 C 0.4422(2) 0.6622(3) 0.44250(15) 0.0285(7) Uani 1 1 d . . . C29 C 0.5240(2) 0.6519(3) 0.42173(17) 0.0379(9) Uani 1 1 d . . . H29A H 0.5038 0.6710 0.3737 0.057 Uiso 1 1 calc R . . H29B H 0.5463 0.5806 0.4280 0.057 Uiso 1 1 calc R . . H29C H 0.5756 0.6973 0.4499 0.057 Uiso 1 1 calc R . . C30 C 0.4037(3) 0.4810(3) 0.41655(17) 0.0373(9) Uani 1 1 d . . . C31 C 0.2117(2) 0.8772(3) 0.35173(16) 0.0288(8) Uani 1 1 d . . . C32 C 0.2625(2) 0.9693(2) 0.36142(15) 0.0272(7) Uani 1 1 d . . . C33 C 0.3325(2) 1.0013(2) 0.42435(16) 0.0269(7) Uani 1 1 d . . . C34 C 0.3776(2) 1.1049(2) 0.43221(16) 0.0317(8) Uani 1 1 d . . . H34A H 0.3494 1.1510 0.4554 0.048 Uiso 1 1 calc R . . H34B H 0.3669 1.1328 0.3871 0.048 Uiso 1 1 calc R . . H34C H 0.4459 1.0989 0.4593 0.048 Uiso 1 1 calc R . . C35 C 0.2397(3) 1.0389(3) 0.30493(19) 0.0415(9) Uani 1 1 d . . . C36 C 0.1353(2) 0.8508(3) 0.28398(16) 0.0406(9) Uani 1 1 d . . . H36A H 0.1033 0.7876 0.2882 0.061 Uiso 1 1 calc R . . H36B H 0.1636 0.8404 0.2505 0.061 Uiso 1 1 calc R . . H36C H 0.0891 0.9069 0.2689 0.061 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 Fe1 0.0224(3) 0.0252(3) 0.0312(3) -0.0007(2) 0.0105(2) -0.0017(2) O1 0.0226(12) 0.0324(14) 0.0418(14) -0.0074(10) 0.0130(11) -0.0063(10) N1 0.055(2) 0.0358(19) 0.048(2) -0.0079(15) 0.0157(17) 0.0067(16) C1 0.041(2) 0.032(2) 0.049(2) -0.0131(17) 0.0173(19) -0.0099(17) Fe2 0.0248(3) 0.0236(3) 0.0264(3) -0.0013(2) 0.0110(2) -0.0018(2) O2 0.0223(12) 0.0268(13) 0.0413(14) -0.0030(11) 0.0103(10) -0.0023(10) N2 0.046(2) 0.056(2) 0.045(2) 0.0102(17) 0.0162(17) 0.0097(18) C2 0.035(2) 0.0266(19) 0.0275(18) -0.0007(15) 0.0102(15) -0.0062(16) O3 0.0251(12) 0.0312(13) 0.0318(13) 0.0025(10) 0.0135(10) 0.0017(10) N3 0.059(2) 0.052(2) 0.041(2) -0.0028(17) 0.0099(17) -0.0125(18) C3 0.0282(18) 0.0265(19) 0.0314(19) 0.0000(15) 0.0113(15) 0.0005(15) O4 0.0243(12) 0.0361(14) 0.0320(13) 0.0024(11) 0.0119(10) 0.0002(11) N4 0.048(2) 0.085(3) 0.040(2) 0.0154(19) 0.0223(17) 0.0029(19) C4 0.0246(18) 0.0295(19) 0.0288(18) 0.0031(14) 0.0086(14) 0.0038(15) O5 0.0306(13) 0.0260(13) 0.0303(13) -0.0011(10) 0.0114(10) -0.0046(10) N5 0.077(3) 0.039(2) 0.045(2) -0.0043(16) 0.0228(18) 0.0114(19) C5 0.029(2) 0.041(2) 0.057(2) -0.0051(19) 0.0192(18) -0.0013(17) O6 0.0311(13) 0.0274(13) 0.0311(13) 0.0020(10) 0.0115(11) -0.0058(11) N6 0.084(3) 0.056(2) 0.037(2) 0.0085(18) 0.0153(19) 0.000(2) C6 0.033(2) 0.038(2) 0.030(2) -0.0012(16) 0.0097(16) -0.0009(17) O7 0.0281(12) 0.0320(13) 0.0270(13) -0.0001(10) 0.0124(10) 0.0021(10) C7 0.0245(18) 0.036(2) 0.0338(19) -0.0029(15) 0.0122(15) 0.0039(15) O8 0.0248(12) 0.0314(13) 0.0275(12) 0.0018(10) 0.0108(10) 0.0017(10) C8 0.0267(18) 0.0245(18) 0.0303(19) -0.0057(15) 0.0088(15) -0.0045(14) O9 0.0309(13) 0.0237(13) 0.0445(14) -0.0006(11) 0.0196(11) -0.0020(10) C9 0.0267(18) 0.0263(18) 0.0236(17) -0.0006(14) 0.0058(14) -0.0019(14) O10 0.0289(13) 0.0263(13) 0.0332(13) -0.0026(10) 0.0167(10) -0.0024(10) C10 0.0283(19) 0.033(2) 0.0274(18) -0.0078(15) 0.0117(15) -0.0083(16) O11 0.0316(13) 0.0342(14) 0.0268(12) -0.0033(11) 0.0092(10) -0.0068(11) C11 0.032(2) 0.060(3) 0.0290(19) 0.0019(17) 0.0105(16) -0.0016(18) O12 0.0290(13) 0.0245(13) 0.0275(12) -0.0014(10) 0.0084(10) -0.0032(10) C12 0.039(2) 0.033(2) 0.036(2) -0.0015(17) 0.0193(18) 0.0010(17) C13 0.050(2) 0.032(2) 0.032(2) 0.0045(15) 0.0140(18) -0.0069(17) C14 0.0278(19) 0.029(2) 0.037(2) 0.0039(15) 0.0157(17) 0.0055(15) C15 0.0248(17) 0.0252(18) 0.0281(18) 0.0006(14) 0.0101(14) -0.0006(14) C16 0.0195(17) 0.0245(18) 0.040(2) -0.0028(15) 0.0161(16) 0.0004(14) C17 0.034(2) 0.0274(19) 0.040(2) -0.0009(15) 0.0176(16) -0.0052(15) C18 0.040(2) 0.030(2) 0.045(2) 0.0019(17) 0.0176(19) -0.0022(17) C19 0.030(2) 0.045(2) 0.039(2) -0.0062(16) 0.0178(17) -0.0001(16) C20 0.0298(18) 0.0185(17) 0.0334(19) -0.0067(14) 0.0149(15) -0.0027(14) C21 0.0286(18) 0.0259(19) 0.0250(17) -0.0003(13) 0.0123(15) -0.0008(14) C22 0.0310(19) 0.0163(17) 0.0297(18) -0.0030(13) 0.0106(15) -0.0011(13) C23 0.035(2) 0.041(2) 0.033(2) 0.0037(16) 0.0114(17) 0.0110(17) C24 0.033(2) 0.041(2) 0.039(2) 0.0006(17) 0.0140(17) -0.0010(17) C25 0.044(2) 0.029(2) 0.061(3) -0.0028(18) 0.023(2) -0.0053(18) C26 0.0292(19) 0.0217(18) 0.0326(19) 0.0064(15) 0.0072(15) 0.0011(15) C27 0.0330(19) 0.0214(18) 0.0275(18) -0.0047(14) 0.0088(15) 0.0008(15) C28 0.0288(19) 0.0318(19) 0.0212(17) 0.0008(14) 0.0058(14) 0.0015(15) C29 0.038(2) 0.039(2) 0.043(2) -0.0024(17) 0.0232(18) 0.0023(17) C30 0.040(2) 0.037(2) 0.030(2) -0.0008(17) 0.0087(17) -0.0043(18) C31 0.0242(18) 0.036(2) 0.0268(18) -0.0046(16) 0.0112(14) 0.0066(15) C32 0.0325(19) 0.0285(19) 0.0216(17) 0.0009(14) 0.0118(15) 0.0032(15) C33 0.0292(18) 0.0264(18) 0.0312(19) 0.0005(15) 0.0184(15) 0.0043(14) C34 0.034(2) 0.0309(19) 0.0315(19) 0.0001(15) 0.0146(16) -0.0050(16) C35 0.046(2) 0.041(2) 0.034(2) -0.0028(18) 0.0118(18) 0.0007(19) C36 0.037(2) 0.045(2) 0.033(2) -0.0016(17) 0.0060(17) -0.0027(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 Fe1 O3 1.981(2) . ? Fe1 O1 1.986(2) . ? Fe1 O2 1.987(2) . ? Fe1 O6 1.994(2) . ? Fe1 O5 1.995(2) . ? Fe1 O4 1.995(2) . ? O1 C2 1.266(4) . ? N1 C6 1.141(4) . ? C1 C2 1.498(4) . ? Fe2 O12 1.980(2) . ? Fe2 O11 1.989(2) . ? Fe2 O8 1.989(2) . ? Fe2 O10 1.990(2) . ? Fe2 O7 1.994(2) . ? Fe2 O9 1.995(2) . ? O2 C4 1.267(4) . ? N2 C12 1.153(4) . ? C2 C3 1.413(4) . ? O3 C8 1.264(4) . ? N3 C18 1.147(4) . ? C3 C4 1.420(4) . ? C3 C6 1.442(5) . ? O4 C10 1.260(4) . ? N4 C24 1.150(4) . ? C4 C5 1.495(4) . ? O5 C16 1.268(4) . ? N5 C30 1.160(4) . ? O6 C14 1.266(4) . ? N6 C35 1.142(4) . ? O7 C20 1.270(4) . ? C7 C8 1.509(4) . ? O8 C22 1.269(3) . ? C8 C9 1.421(4) . ? O9 C26 1.265(4) . ? C9 C10 1.403(4) . ? C9 C12 1.429(5) . ? O10 C28 1.269(4) . ? C10 C11 1.499(4) . ? O11 C31 1.276(4) . ? O12 C33 1.274(3) . ? C13 C14 1.493(4) . ? C14 C15 1.412(4) . ? C15 C16 1.419(4) . ? C15 C18 1.445(5) . ? C16 C17 1.498(4) . ? C19 C20 1.500(4) . ? C20 C21 1.426(4) . ? C21 C22 1.410(4) . ? C21 C24 1.435(5) . ? C22 C23 1.495(4) . ? C25 C26 1.505(4) . ? C26 C27 1.407(4) . ? C27 C28 1.413(4) . ? C27 C30 1.424(5) . ? C28 C29 1.492(4) . ? C31 C32 1.400(4) . ? C31 C36 1.498(4) . ? C32 C33 1.411(4) . ? C32 C35 1.437(5) . ? C33 C34 1.495(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 O3 Fe1 O1 88.94(9) . . ? O3 Fe1 O2 171.29(9) . . ? O1 Fe1 O2 86.75(9) . . ? O3 Fe1 O6 92.22(9) . . ? O1 Fe1 O6 91.12(9) . . ? O2 Fe1 O6 95.42(9) . . ? O3 Fe1 O5 95.31(9) . . ? O1 Fe1 O5 174.60(9) . . ? O2 Fe1 O5 89.47(9) . . ? O6 Fe1 O5 85.41(9) . . ? O3 Fe1 O4 86.64(9) . . ? O1 Fe1 O4 95.48(9) . . ? O2 Fe1 O4 86.24(9) . . ? O6 Fe1 O4 173.29(9) . . ? O5 Fe1 O4 88.11(9) . . ? C2 O1 Fe1 131.8(2) . . ? O12 Fe2 O11 86.06(9) . . ? O12 Fe2 O8 90.88(9) . . ? O11 Fe2 O8 175.38(9) . . ? O12 Fe2 O10 89.90(9) . . ? O11 Fe2 O10 95.34(9) . . ? O8 Fe2 O10 88.10(9) . . ? O12 Fe2 O7 97.33(9) . . ? O11 Fe2 O7 91.97(9) . . ? O8 Fe2 O7 84.98(8) . . ? O10 Fe2 O7 170.05(9) . . ? O12 Fe2 O9 171.11(9) . . ? O11 Fe2 O9 86.08(9) . . ? O8 Fe2 O9 97.21(9) . . ? O10 Fe2 O9 86.71(9) . . ? O7 Fe2 O9 87.08(9) . . ? C4 O2 Fe1 131.1(2) . . ? O1 C2 C3 122.7(3) . . ? O1 C2 C1 116.9(3) . . ? C3 C2 C1 120.4(3) . . ? C8 O3 Fe1 131.7(2) . . ? C2 C3 C4 124.2(3) . . ? C2 C3 C6 118.8(3) . . ? C4 C3 C6 117.0(3) . . ? C10 O4 Fe1 131.2(2) . . ? O2 C4 C3 123.0(3) . . ? O2 C4 C5 117.4(3) . . ? C3 C4 C5 119.6(3) . . ? C16 O5 Fe1 131.1(2) . . ? C14 O6 Fe1 130.9(2) . . ? N1 C6 C3 178.2(4) . . ? C20 O7 Fe2 129.8(2) . . ? C22 O8 Fe2 129.4(2) . . ? O3 C8 C9 122.7(3) . . ? O3 C8 C7 117.2(3) . . ? C9 C8 C7 120.1(3) . . ? C26 O9 Fe2 129.2(2) . . ? C10 C9 C8 124.4(3) . . ? C10 C9 C12 118.7(3) . . ? C8 C9 C12 116.9(3) . . ? C28 O10 Fe2 131.3(2) . . ? O4 C10 C9 123.4(3) . . ? O4 C10 C11 116.4(3) . . ? C9 C10 C11 120.2(3) . . ? C31 O11 Fe2 130.8(2) . . ? C33 O12 Fe2 131.6(2) . . ? N2 C12 C9 179.5(4) . . ? O6 C14 C15 122.9(3) . . ? O6 C14 C13 116.5(3) . . ? C15 C14 C13 120.6(3) . . ? C14 C15 C16 123.6(3) . . ? C14 C15 C18 118.9(3) . . ? C16 C15 C18 117.5(3) . . ? O5 C16 C15 122.8(3) . . ? O5 C16 C17 115.7(3) . . ? C15 C16 C17 121.6(3) . . ? N3 C18 C15 179.7(4) . . ? O7 C20 C21 122.5(3) . . ? O7 C20 C19 116.6(3) . . ? C21 C20 C19 120.9(3) . . ? C22 C21 C20 123.3(3) . . ? C22 C21 C24 118.6(3) . . ? C20 C21 C24 118.0(3) . . ? O8 C22 C21 122.6(3) . . ? O8 C22 C23 115.9(3) . . ? C21 C22 C23 121.4(3) . . ? N4 C24 C21 179.1(4) . . ? O9 C26 C27 123.8(3) . . ? O9 C26 C25 116.6(3) . . ? C27 C26 C25 119.6(3) . . ? C26 C27 C28 124.2(3) . . ? C26 C27 C30 116.9(3) . . ? C28 C27 C30 118.9(3) . . ? O10 C28 C27 122.6(3) . . ? O10 C28 C29 116.6(3) . . ? C27 C28 C29 120.8(3) . . ? N5 C30 C27 177.4(4) . . ? O11 C31 C32 123.0(3) . . ? O11 C31 C36 115.9(3) . . ? C32 C31 C36 121.1(3) . . ? C31 C32 C33 124.3(3) . . ? C31 C32 C35 118.7(3) . . ? C33 C32 C35 117.0(3) . . ? O12 C33 C32 122.6(3) . . ? O12 C33 C34 116.2(3) . . ? C32 C33 C34 121.1(3) . . ? N6 C35 C32 179.4(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.472 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.110 #===END data_compound_5_bath148 _database_code_depnum_ccdc_archive 'CCDC 636529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Ag Cu N3 O7' _chemical_formula_weight 481.66 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7735(2) _cell_length_b 8.4210(2) _cell_length_c 13.4553(4) _cell_angle_alpha 91.187(1) _cell_angle_beta 97.692(1) _cell_angle_gamma 117.238(1) _cell_volume 772.71(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6217 _cell_measurement_theta_min 2.819 _cell_measurement_theta_max 30.089 _exptl_crystal_description block _exptl_crystal_colour aqua _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 474 _exptl_absorpt_coefficient_mu 2.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4985 _exptl_absorpt_correction_T_max 0.8675 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6751 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2 SMX' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10 _diffrn_reflns_number 9381 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 30.88 _reflns_number_total 5002 _reflns_number_gt 4564 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0338P)^2^+0.2267P] 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 5002 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.430933(17) 0.404463(15) 0.184302(8) 0.02552(4) Uani 1 1 d . . . Cu1 Cu 0.60223(2) 0.06009(2) 0.331557(11) 0.01462(4) Uani 1 1 d . . . O1 O 0.79450(14) -0.00568(13) 0.29581(7) 0.01817(17) Uani 1 1 d . . . O2 O 0.40378(14) -0.10335(14) 0.22460(7) 0.01964(18) Uani 1 1 d . . . O3 O 0.78331(14) 0.18379(13) 0.45440(7) 0.01783(17) Uani 1 1 d . . . O4 O 0.39796(14) 0.10172(13) 0.37657(7) 0.01778(17) Uani 1 1 d . . . O5 O 0.67110(18) 0.29547(18) 0.24275(10) 0.0339(3) Uani 1 1 d . . . O6 O 0.93869(18) 0.34088(18) 0.18698(10) 0.0331(3) Uani 1 1 d . . . O7 O 0.80572(18) 0.51470(15) 0.15274(9) 0.0294(2) Uani 1 1 d . . . N1 N 0.64976(19) -0.2675(2) -0.03695(10) 0.0271(3) Uani 1 1 d . . . N2 N 0.57405(19) 0.45739(18) 0.68360(9) 0.0234(2) Uani 1 1 d . . . N3 N 0.80926(18) 0.38395(16) 0.19294(9) 0.0213(2) Uani 1 1 d . . . C1 C 0.9834(2) -0.0479(2) 0.18445(11) 0.0222(3) Uani 1 1 d . . . H1A H 1.0830 -0.0012 0.2452 0.033 Uiso 1 1 calc R . . H1B H 1.0265 0.0343 0.1320 0.033 Uiso 1 1 calc R . . H1C H 0.9646 -0.1662 0.1604 0.033 Uiso 1 1 calc R . . C2 C 0.79382(18) -0.06383(17) 0.20857(9) 0.0159(2) Uani 1 1 d . . . C3 C 0.62275(19) -0.14365(17) 0.13327(9) 0.0167(2) Uani 1 1 d . . . C4 C 0.43398(19) -0.16689(17) 0.14714(9) 0.0170(2) Uani 1 1 d . . . C5 C 0.2602(2) -0.2692(2) 0.06654(11) 0.0259(3) Uani 1 1 d . . . H5A H 0.1405 -0.3213 0.0969 0.039 Uiso 1 1 calc R . . H5B H 0.2749 -0.3654 0.0327 0.039 Uiso 1 1 calc R . . H5C H 0.2515 -0.1879 0.0174 0.039 Uiso 1 1 calc R . . C6 C 0.6391(2) -0.21161(19) 0.04005(10) 0.0199(2) Uani 1 1 d . . . C7 C 0.9235(2) 0.3527(2) 0.61275(10) 0.0244(3) Uani 1 1 d . . . H7A H 1.0298 0.3253 0.6025 0.037 Uiso 1 1 calc R . . H7B H 0.8771 0.3077 0.6757 0.037 Uiso 1 1 calc R . . H7C H 0.9717 0.4828 0.6165 0.037 Uiso 1 1 calc R . . C8 C 0.75764(18) 0.26425(17) 0.52635(9) 0.0163(2) Uani 1 1 d . . . C9 C 0.58091(19) 0.27513(17) 0.52990(9) 0.0159(2) Uani 1 1 d . . . C10 C 0.40866(18) 0.19141(17) 0.45532(9) 0.0153(2) Uani 1 1 d . . . C11 C 0.2286(2) 0.20438(19) 0.47205(10) 0.0199(2) Uani 1 1 d . . . H11A H 0.1347 0.1656 0.4092 0.030 Uiso 1 1 calc R . . H11B H 0.2643 0.3289 0.4937 0.030 Uiso 1 1 calc R . . H11C H 0.1689 0.1272 0.5242 0.030 Uiso 1 1 calc R . . C12 C 0.5756(2) 0.37451(18) 0.61495(10) 0.0180(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03436(7) 0.03085(7) 0.01363(6) -0.00875(4) 0.00239(4) 0.01792(5) Cu1 0.01526(7) 0.01924(8) 0.00943(7) -0.00592(5) -0.00038(5) 0.00898(6) O1 0.0192(4) 0.0253(4) 0.0113(4) -0.0068(3) -0.0014(3) 0.0128(4) O2 0.0173(4) 0.0265(5) 0.0143(4) -0.0090(3) -0.0001(3) 0.0105(4) O3 0.0172(4) 0.0237(4) 0.0119(4) -0.0070(3) -0.0001(3) 0.0099(3) O4 0.0171(4) 0.0228(4) 0.0131(4) -0.0071(3) -0.0004(3) 0.0100(3) O5 0.0305(6) 0.0392(6) 0.0391(7) 0.0202(5) 0.0141(5) 0.0193(5) O6 0.0315(6) 0.0374(6) 0.0354(6) 0.0012(5) 0.0082(5) 0.0197(5) O7 0.0340(6) 0.0228(5) 0.0299(6) 0.0052(4) 0.0065(5) 0.0114(4) N1 0.0247(6) 0.0379(7) 0.0162(5) -0.0108(5) 0.0017(4) 0.0133(5) N2 0.0276(6) 0.0278(6) 0.0162(5) -0.0065(4) 0.0023(4) 0.0146(5) N3 0.0232(5) 0.0213(5) 0.0146(5) -0.0036(4) -0.0011(4) 0.0076(4) C1 0.0179(5) 0.0291(7) 0.0196(6) -0.0074(5) 0.0014(5) 0.0119(5) C2 0.0178(5) 0.0174(5) 0.0131(5) -0.0036(4) 0.0012(4) 0.0093(4) C3 0.0176(5) 0.0209(6) 0.0104(5) -0.0060(4) 0.0005(4) 0.0087(4) C4 0.0181(5) 0.0198(5) 0.0118(5) -0.0047(4) -0.0002(4) 0.0086(4) C5 0.0184(6) 0.0352(8) 0.0187(6) -0.0134(5) -0.0041(5) 0.0104(5) C6 0.0186(5) 0.0249(6) 0.0136(5) -0.0049(4) 0.0015(4) 0.0086(5) C7 0.0184(6) 0.0346(7) 0.0154(6) -0.0121(5) -0.0032(5) 0.0104(5) C8 0.0168(5) 0.0183(5) 0.0117(5) -0.0042(4) 0.0011(4) 0.0070(4) C9 0.0183(5) 0.0181(5) 0.0109(5) -0.0053(4) 0.0013(4) 0.0088(4) C10 0.0169(5) 0.0162(5) 0.0132(5) -0.0022(4) 0.0026(4) 0.0081(4) C11 0.0182(5) 0.0254(6) 0.0184(6) -0.0041(5) 0.0031(4) 0.0124(5) C12 0.0201(5) 0.0197(6) 0.0137(5) -0.0033(4) 0.0019(4) 0.0093(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 Ag1 N2 2.1185(12) 2_666 ? Ag1 N1 2.1366(12) 2_655 ? Ag1 O5 2.4802(13) . ? Cu1 O1 1.9264(10) . ? Cu1 O2 1.9301(9) . ? Cu1 O3 1.9396(9) . ? Cu1 O4 1.9415(9) . ? Cu1 O5 2.2229(12) . ? O1 C2 1.2609(14) . ? O2 C4 1.2590(15) . ? O3 C8 1.2588(14) . ? O4 C10 1.2593(14) . ? O5 N3 1.2801(17) . ? O6 N3 1.2267(18) . ? O7 N3 1.2466(17) . ? N1 C6 1.1576(17) . ? N1 Ag1 2.1366(12) 2_655 ? N2 C12 1.1508(17) . ? N2 Ag1 2.1185(12) 2_666 ? C1 C2 1.4975(18) . ? C2 C3 1.4282(17) . ? C3 C6 1.4129(18) . ? C3 C4 1.4277(18) . ? C4 C5 1.4992(18) . ? C7 C8 1.5006(18) . ? C8 C9 1.4250(18) . ? C9 C12 1.4200(19) . ? C9 C10 1.4296(18) . ? C10 C11 1.4986(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 161.76(5) 2_666 2_655 ? N2 Ag1 O5 102.95(5) 2_666 . ? N1 Ag1 O5 94.40(5) 2_655 . ? O1 Cu1 O2 92.19(4) . . ? O1 Cu1 O3 87.46(4) . . ? O2 Cu1 O3 168.70(5) . . ? O1 Cu1 O4 173.23(4) . . ? O2 Cu1 O4 87.10(4) . . ? O3 Cu1 O4 91.91(4) . . ? O1 Cu1 O5 98.92(5) . . ? O2 Cu1 O5 92.89(5) . . ? O3 Cu1 O5 98.33(5) . . ? O4 Cu1 O5 87.85(5) . . ? C2 O1 Cu1 124.56(9) . . ? C4 O2 Cu1 126.01(9) . . ? C8 O3 Cu1 127.95(9) . . ? C10 O4 Cu1 128.18(9) . . ? N3 O5 Cu1 133.58(10) . . ? N3 O5 Ag1 101.59(9) . . ? Cu1 O5 Ag1 123.48(5) . . ? C6 N1 Ag1 161.43(12) . 2_655 ? C12 N2 Ag1 176.19(12) . 2_666 ? O6 N3 O7 122.65(13) . . ? O6 N3 O5 120.51(13) . . ? O7 N3 O5 116.84(13) . . ? O1 C2 C3 123.33(12) . . ? O1 C2 C1 117.41(11) . . ? C3 C2 C1 119.26(11) . . ? C6 C3 C4 117.59(11) . . ? C6 C3 C2 117.82(11) . . ? C4 C3 C2 124.53(11) . . ? O2 C4 C3 123.25(11) . . ? O2 C4 C5 116.80(12) . . ? C3 C4 C5 119.95(11) . . ? N1 C6 C3 178.95(15) . . ? O3 C8 C9 123.64(11) . . ? O3 C8 C7 117.56(12) . . ? C9 C8 C7 118.80(11) . . ? C12 C9 C8 117.16(12) . . ? C12 C9 C10 117.90(12) . . ? C8 C9 C10 124.93(11) . . ? O4 C10 C9 123.18(12) . . ? O4 C10 C11 117.61(11) . . ? C9 C10 C11 119.18(11) . . ? N2 C12 C9 178.88(16) . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 30.88 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 0.496 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.070 #===END data_compound_6_h06kc3 _database_code_depnum_ccdc_archive 'CCDC 636530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H18 Ag Fe N4 O9' _chemical_formula_weight 598.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 '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' C C 0.0033 0.0016 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0460(1) _cell_length_b 11.3220(1) _cell_length_c 15.0110(1) _cell_angle_alpha 90.00 _cell_angle_beta 116.650(1) _cell_angle_gamma 90.00 _cell_volume 2133.57(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.657 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.73 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54883 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.61 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6128 _reflns_number_gt 5597 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0389P)^2^+1.0704P] 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 0.0087(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6128 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.283054(10) 0.165392(12) -0.218096(9) 0.03020(6) Uani 1 1 d . . . Fe1 Fe 0.206588(16) 0.120428(18) 0.296714(15) 0.01850(6) Uani 1 1 d . . . O1 O 0.09552(8) 0.23756(9) 0.22342(8) 0.0227(2) Uani 1 1 d . . . O2 O 0.10224(8) -0.00237(9) 0.21594(8) 0.0229(2) Uani 1 1 d . . . O3 O 0.16790(9) 0.12348(10) 0.40796(8) 0.0229(2) Uani 1 1 d . . . O4 O 0.30855(9) -0.00785(10) 0.37239(8) 0.0247(2) Uani 1 1 d . . . O5 O 0.30706(9) 0.25396(10) 0.36090(8) 0.0234(2) Uani 1 1 d . . . O6 O 0.26769(9) 0.11562(10) 0.19938(8) 0.0227(2) Uani 1 1 d . . . O7 O -0.12438(15) 0.33713(16) -0.15402(16) 0.0570(4) Uani 1 1 d . . . O8 O -0.1568(2) 0.46848(15) -0.26974(17) 0.0677(6) Uani 1 1 d . . . O9 O -0.23051(16) 0.29599(16) -0.30785(14) 0.0526(4) Uani 1 1 d . . . N1 N -0.21858(15) 0.12206(15) -0.05140(13) 0.0443(4) Uani 1 1 d . . . N2 N 0.36203(13) -0.11042(15) 0.69371(12) 0.0347(3) Uani 1 1 d . . . N3 N 0.53630(12) 0.38150(14) 0.22805(12) 0.0309(3) Uani 1 1 d . . . N4 N -0.16967(16) 0.36858(16) -0.24361(17) 0.0445(4) Uani 1 1 d . . . C1 C -0.05849(13) 0.33803(13) 0.11174(13) 0.0253(3) Uani 1 1 d . . . H1A H -0.1164 0.3395 0.1312 0.038 Uiso 1 1 calc R . . H1B H -0.0885 0.3405 0.0389 0.038 Uiso 1 1 calc R . . H1C H -0.0122 0.4067 0.1403 0.038 Uiso 1 1 calc R . . C2 C 0.00482(11) 0.22753(12) 0.14955(10) 0.0196(2) Uani 1 1 d . . . C3 C -0.03777(12) 0.11734(13) 0.10461(11) 0.0217(3) Uani 1 1 d . . . C4 C 0.01053(12) 0.00693(13) 0.14291(10) 0.0206(3) Uani 1 1 d . . . C5 C -0.04786(13) -0.10557(14) 0.09917(13) 0.0276(3) Uani 1 1 d . . . H5A H 0.0031 -0.1709 0.1168 0.041 Uiso 1 1 calc R . . H5B H -0.0860 -0.0981 0.0265 0.041 Uiso 1 1 calc R . . H5C H -0.0990 -0.1213 0.1256 0.041 Uiso 1 1 calc R . . C6 C -0.13879(14) 0.11859(14) 0.01952(13) 0.0296(3) Uani 1 1 d . . . C7 C 0.15097(14) 0.09649(15) 0.55489(12) 0.0275(3) Uani 1 1 d . . . H7A H 0.1609 0.1799 0.5743 0.041 Uiso 1 1 calc R . . H7B H 0.1820 0.0470 0.6147 0.041 Uiso 1 1 calc R . . H7C H 0.0747 0.0794 0.5177 0.041 Uiso 1 1 calc R . . C8 C 0.20479(12) 0.07082(12) 0.49071(11) 0.0205(3) Uani 1 1 d . . . C9 C 0.29090(11) -0.01033(13) 0.52161(11) 0.0213(3) Uani 1 1 d . . . C10 C 0.33679(11) -0.04799(14) 0.45958(11) 0.0225(3) Uani 1 1 d . . . C11 C 0.42106(16) -0.14146(19) 0.49509(14) 0.0361(4) Uani 1 1 d . . . H11A H 0.3890 -0.2178 0.4968 0.054 Uiso 1 1 calc R . . H11B H 0.4757 -0.1215 0.5621 0.054 Uiso 1 1 calc R . . H11C H 0.4536 -0.1463 0.4495 0.054 Uiso 1 1 calc R . . C12 C 0.32908(13) -0.06510(14) 0.61736(12) 0.0256(3) Uani 1 1 d . . . C13 C 0.42217(15) 0.41691(15) 0.39494(13) 0.0307(3) Uani 1 1 d . . . H13A H 0.3885 0.4875 0.3555 0.046 Uiso 1 1 calc R . . H13B H 0.4980 0.4162 0.4112 0.046 Uiso 1 1 calc R . . H13C H 0.4144 0.4179 0.4566 0.046 Uiso 1 1 calc R . . C14 C 0.36977(12) 0.30912(13) 0.33617(10) 0.0214(3) Uani 1 1 d . . . C15 C 0.39166(11) 0.27197(13) 0.25671(10) 0.0211(3) Uani 1 1 d . . . C16 C 0.34010(11) 0.17535(13) 0.19255(11) 0.0200(3) Uani 1 1 d . . . C17 C 0.36907(14) 0.14292(15) 0.11133(12) 0.0267(3) Uani 1 1 d . . . H17A H 0.3409 0.0643 0.0857 0.040 Uiso 1 1 calc R . . H17B H 0.4468 0.1424 0.1377 0.040 Uiso 1 1 calc R . . H17C H 0.3385 0.2008 0.0573 0.040 Uiso 1 1 calc R . . C18 C 0.47147(12) 0.33356(13) 0.24105(12) 0.0239(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02703(8) 0.03315(9) 0.02924(8) -0.00168(4) 0.01157(6) -0.00242(4) Fe1 0.01770(10) 0.01876(11) 0.01921(10) 0.00153(7) 0.00841(8) 0.00052(7) O1 0.0215(5) 0.0187(5) 0.0241(5) 0.0010(4) 0.0069(4) 0.0008(4) O2 0.0210(5) 0.0185(5) 0.0276(5) 0.0011(4) 0.0094(4) -0.0001(4) O3 0.0239(5) 0.0235(5) 0.0251(5) 0.0036(4) 0.0145(4) 0.0039(4) O4 0.0239(5) 0.0293(5) 0.0225(5) 0.0051(4) 0.0117(4) 0.0081(4) O5 0.0254(5) 0.0259(5) 0.0209(5) -0.0029(4) 0.0122(4) -0.0057(4) O6 0.0242(5) 0.0240(5) 0.0220(5) -0.0029(4) 0.0123(4) -0.0038(4) O7 0.0500(10) 0.0512(10) 0.0672(12) -0.0022(8) 0.0240(9) 0.0142(7) O8 0.1115(17) 0.0381(8) 0.0944(15) -0.0115(9) 0.0825(14) -0.0203(10) O9 0.0741(11) 0.0437(8) 0.0607(9) -0.0184(7) 0.0488(9) -0.0180(8) N1 0.0428(9) 0.0314(8) 0.0342(8) 0.0025(6) -0.0043(7) -0.0044(7) N2 0.0363(8) 0.0390(8) 0.0282(7) 0.0061(6) 0.0140(6) 0.0015(6) N3 0.0265(7) 0.0338(7) 0.0352(7) 0.0011(6) 0.0163(6) -0.0021(5) N4 0.0545(11) 0.0340(8) 0.0683(12) -0.0120(8) 0.0483(10) -0.0061(8) C1 0.0259(7) 0.0209(7) 0.0291(7) 0.0038(5) 0.0123(6) 0.0052(5) C2 0.0208(6) 0.0200(6) 0.0207(6) 0.0030(5) 0.0117(5) 0.0018(5) C3 0.0215(6) 0.0217(7) 0.0200(6) 0.0010(5) 0.0077(5) -0.0003(5) C4 0.0235(6) 0.0198(6) 0.0214(6) 0.0000(5) 0.0126(5) -0.0012(5) C5 0.0288(7) 0.0209(7) 0.0309(8) -0.0036(6) 0.0114(6) -0.0047(6) C6 0.0313(8) 0.0235(7) 0.0265(7) 0.0022(6) 0.0064(6) -0.0019(6) C7 0.0321(8) 0.0285(7) 0.0288(7) 0.0001(6) 0.0197(6) 0.0012(6) C8 0.0217(6) 0.0184(6) 0.0230(6) -0.0017(5) 0.0116(5) -0.0047(5) C9 0.0203(6) 0.0227(6) 0.0203(6) 0.0015(5) 0.0085(5) -0.0015(5) C10 0.0195(6) 0.0247(7) 0.0218(6) 0.0018(5) 0.0079(5) 0.0014(5) C11 0.0332(9) 0.0448(10) 0.0308(8) 0.0121(7) 0.0146(7) 0.0197(8) C12 0.0261(7) 0.0274(7) 0.0241(7) 0.0000(6) 0.0120(6) -0.0013(6) C13 0.0387(9) 0.0297(8) 0.0256(7) -0.0066(6) 0.0161(7) -0.0121(7) C14 0.0207(6) 0.0235(6) 0.0180(6) 0.0003(5) 0.0071(5) -0.0017(5) C15 0.0186(6) 0.0244(7) 0.0198(6) 0.0010(5) 0.0082(5) -0.0008(5) C16 0.0186(6) 0.0218(6) 0.0190(6) 0.0024(5) 0.0079(5) 0.0031(5) C17 0.0296(8) 0.0302(7) 0.0244(7) -0.0040(6) 0.0159(6) -0.0014(6) C18 0.0216(7) 0.0265(7) 0.0230(7) 0.0015(5) 0.0095(6) 0.0006(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 2.2998(18) . ? Ag1 O9 2.3320(17) . ? Ag1 N3 2.3523(15) 4_465 ? Fe1 O1 1.9655(11) . ? Fe1 O3 1.9747(11) . ? Fe1 O2 1.9892(11) . ? Fe1 O5 1.9964(11) . ? Fe1 O4 1.9979(11) . ? Fe1 O6 1.9998(11) . ? O1 C2 1.2642(18) . ? O2 C4 1.2670(18) . ? O3 C8 1.2608(18) . ? O4 C10 1.2694(18) . ? O5 C14 1.2638(18) . ? O6 C16 1.2632(18) . ? O7 N4 1.254(3) . ? O8 N4 1.237(3) . ? O9 N4 1.264(3) . ? N1 C6 1.149(2) . ? N2 C12 1.147(2) . ? N3 C18 1.149(2) . ? N3 Ag1 2.3523(15) 4_666 ? C1 C2 1.4917(19) . ? C2 C3 1.417(2) . ? C3 C4 1.416(2) . ? C3 C6 1.421(2) . ? C4 C5 1.498(2) . ? C7 C8 1.496(2) . ? C8 C9 1.421(2) . ? C9 C10 1.415(2) . ? C9 C12 1.431(2) . ? C10 C11 1.496(2) . ? C13 C14 1.492(2) . ? C14 C15 1.422(2) . ? C15 C16 1.422(2) . ? C15 C18 1.426(2) . ? C16 C17 1.494(2) . ? 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 O9 133.76(6) . . ? N1 Ag1 N3 99.41(6) . 4_465 ? O9 Ag1 N3 121.11(6) . 4_465 ? O1 Fe1 O3 90.64(5) . . ? O1 Fe1 O2 87.00(4) . . ? O3 Fe1 O2 96.93(5) . . ? O1 Fe1 O5 88.34(5) . . ? O3 Fe1 O5 88.95(4) . . ? O2 Fe1 O5 172.52(5) . . ? O1 Fe1 O4 174.47(5) . . ? O3 Fe1 O4 86.04(4) . . ? O2 Fe1 O4 89.01(5) . . ? O5 Fe1 O4 96.02(5) . . ? O1 Fe1 O6 95.88(5) . . ? O3 Fe1 O6 171.66(5) . . ? O2 Fe1 O6 88.62(5) . . ? O5 Fe1 O6 86.05(4) . . ? O4 Fe1 O6 87.85(5) . . ? C2 O1 Fe1 131.68(10) . . ? C4 O2 Fe1 130.88(10) . . ? C8 O3 Fe1 132.65(10) . . ? C10 O4 Fe1 131.24(10) . . ? C14 O5 Fe1 131.87(10) . . ? C16 O6 Fe1 132.05(10) . . ? N4 O9 Ag1 104.63(14) . . ? C6 N1 Ag1 139.44(18) . . ? C18 N3 Ag1 130.52(13) . 4_666 ? O8 N4 O7 121.6(2) . . ? O8 N4 O9 119.9(2) . . ? O7 N4 O9 118.5(2) . . ? O1 C2 C3 122.74(13) . . ? O1 C2 C1 116.91(13) . . ? C3 C2 C1 120.33(13) . . ? C4 C3 C2 124.13(13) . . ? C4 C3 C6 118.51(13) . . ? C2 C3 C6 117.22(13) . . ? O2 C4 C3 122.74(13) . . ? O2 C4 C5 116.94(13) . . ? C3 C4 C5 120.30(13) . . ? N1 C6 C3 177.2(2) . . ? O3 C8 C9 122.75(13) . . ? O3 C8 C7 116.07(13) . . ? C9 C8 C7 121.17(13) . . ? C10 C9 C8 123.53(13) . . ? C10 C9 C12 117.02(13) . . ? C8 C9 C12 119.26(13) . . ? O4 C10 C9 123.14(13) . . ? O4 C10 C11 116.86(14) . . ? C9 C10 C11 119.98(14) . . ? N2 C12 C9 178.03(18) . . ? O5 C14 C15 122.79(13) . . ? O5 C14 C13 117.03(13) . . ? C15 C14 C13 120.18(13) . . ? C16 C15 C14 124.01(13) . . ? C16 C15 C18 117.61(13) . . ? C14 C15 C18 118.37(13) . . ? O6 C16 C15 122.73(13) . . ? O6 C16 C17 117.30(13) . . ? C15 C16 C17 119.95(13) . . ? N3 C18 C15 178.89(17) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.565 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.071 #===END data_compound_7_k06kc4 _database_code_depnum_ccdc_archive 'CCDC 636531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H36 Ag2 Fe2 N6 O17' _chemical_formula_weight 1068.08 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.2710(2) _cell_length_b 12.5520(2) _cell_length_c 18.9510(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.217(1) _cell_angle_gamma 90.00 _cell_volume 3829.83(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 95063 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.809 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74741 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 30.05 _reflns_number_total 11179 _reflns_number_gt 6904 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0691P)^2^+8.9381P] 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 11179 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.28241(3) 0.31856(4) -0.07906(3) 0.05420(14) Uani 1 1 d . . . Ag2 Ag 0.72061(2) 0.33396(3) 0.26718(2) 0.04238(12) Uani 1 1 d . . . Fe1 Fe 0.15893(4) 0.27201(5) 0.27486(4) 0.03019(15) Uani 1 1 d . . . Fe2 Fe 0.32956(4) 0.28592(5) 0.40384(3) 0.02974(15) Uani 1 1 d . . . O1 O 0.1070(2) 0.3516(3) 0.17712(19) 0.0386(8) Uani 1 1 d . . . O2 O 0.1994(2) 0.1715(3) 0.21392(19) 0.0415(8) Uani 1 1 d . . . O3 O 0.0616(2) 0.1779(3) 0.26118(19) 0.0371(7) Uani 1 1 d . . . O4 O 0.10124(19) 0.3782(3) 0.31889(18) 0.0355(7) Uani 1 1 d . . . O5 O 0.3937(2) 0.1926(3) 0.35755(19) 0.0346(7) Uani 1 1 d . . . O6 O 0.42338(19) 0.3895(3) 0.42173(17) 0.0361(7) Uani 1 1 d . . . O7 O 0.29041(19) 0.3868(3) 0.46701(16) 0.0334(7) Uani 1 1 d . . . O8 O 0.3794(2) 0.2019(3) 0.50044(18) 0.0353(7) Uani 1 1 d . . . O9 O 0.26286(19) 0.3558(2) 0.30751(17) 0.0314(7) Uani 1 1 d . . . O10 O 0.2274(2) 0.2029(3) 0.36933(17) 0.0339(7) Uani 1 1 d . . . O11 O 0.1771(2) 0.3917(3) -0.2030(2) 0.0535(10) Uani 1 1 d . . . O12 O 0.1874(2) 0.5144(3) -0.2784(2) 0.0533(10) Uani 1 1 d . . . O13 O 0.2871(2) 0.4881(3) -0.1707(2) 0.0553(10) Uani 1 1 d . . . O14 O 0.3555(3) 0.4074(4) 0.0417(3) 0.0754(13) Uani 1 1 d . . . O15 O 0.4099(4) 0.3552(6) 0.1578(3) 0.105(2) Uani 1 1 d . . . O16 O 0.3701(4) 0.2410(5) 0.0661(4) 0.111(2) Uani 1 1 d . . . O17 O 0.1129(4) 0.2673(5) 0.5019(3) 0.0950(18) Uani 1 1 d . . . N1 N 0.1835(4) 0.2686(6) -0.0297(3) 0.0782(18) Uani 1 1 d . . . N2 N -0.1262(3) 0.2644(4) 0.3800(2) 0.0467(11) Uani 1 1 d . . . N3 N 0.6129(3) 0.3415(3) 0.2994(3) 0.0404(10) Uani 1 1 d . . . N4 N 0.2713(3) 0.2544(4) 0.6916(2) 0.0412(10) Uani 1 1 d . . . N5 N 0.2172(2) 0.4645(3) -0.2179(3) 0.0378(9) Uani 1 1 d . . . N6 N 0.3774(4) 0.3363(5) 0.0885(4) 0.0705(16) Uani 1 1 d . . . C1 C 0.0783(4) 0.4275(5) 0.0565(3) 0.0585(15) Uani 1 1 d . . . H1A H 0.0241 0.4016 0.0226 0.088 Uiso 1 1 calc R . . H1B H 0.1134 0.4429 0.0271 0.088 Uiso 1 1 calc R . . H1C H 0.0708 0.4927 0.0818 0.088 Uiso 1 1 calc R . . C2 C 0.1188(3) 0.3447(4) 0.1143(3) 0.0404(11) Uani 1 1 d . . . C3 C 0.1659(3) 0.2631(4) 0.0989(3) 0.0412(11) Uani 1 1 d . . . C4 C 0.2062(3) 0.1807(4) 0.1505(3) 0.0407(11) Uani 1 1 d . . . C5 C 0.2576(5) 0.0999(5) 0.1289(4) 0.071(2) Uani 1 1 d . . . H5A H 0.2817 0.0497 0.1708 0.107 Uiso 1 1 calc R . . H5B H 0.3023 0.1361 0.1179 0.107 Uiso 1 1 calc R . . H5C H 0.2225 0.0610 0.0838 0.107 Uiso 1 1 calc R . . C6 C 0.1755(4) 0.2653(5) 0.0274(3) 0.0521(14) Uani 1 1 d . . . C7 C -0.0424(3) 0.0817(4) 0.2869(3) 0.0478(13) Uani 1 1 d . . . H7A H -0.0791 0.0700 0.2343 0.072 Uiso 1 1 calc R . . H7B H -0.0759 0.0893 0.3188 0.072 Uiso 1 1 calc R . . H7C H -0.0048 0.0208 0.3044 0.072 Uiso 1 1 calc R . . C8 C 0.0073(3) 0.1809(4) 0.2918(3) 0.0349(10) Uani 1 1 d . . . C9 C -0.0070(3) 0.2728(4) 0.3288(2) 0.0319(9) Uani 1 1 d . . . C10 C 0.0404(3) 0.3679(4) 0.3398(2) 0.0328(10) Uani 1 1 d . . . C11 C 0.0184(3) 0.4619(4) 0.3776(3) 0.0390(11) Uani 1 1 d . . . H11A H 0.0602 0.5179 0.3851 0.058 Uiso 1 1 calc R . . H11B H 0.0168 0.4402 0.4267 0.058 Uiso 1 1 calc R . . H11C H -0.0363 0.4892 0.3456 0.058 Uiso 1 1 calc R . . C12 C -0.0730(3) 0.2689(4) 0.3575(3) 0.0362(10) Uani 1 1 d . . . C13 C 0.4749(4) 0.1325(4) 0.2882(3) 0.0486(14) Uani 1 1 d . . . H13A H 0.4480 0.0646 0.2908 0.073 Uiso 1 1 calc R . . H13B H 0.5353 0.1229 0.3079 0.073 Uiso 1 1 calc R . . H13C H 0.4565 0.1564 0.2355 0.073 Uiso 1 1 calc R . . C14 C 0.4521(3) 0.2137(4) 0.3344(3) 0.0323(10) Uani 1 1 d . . . C15 C 0.4949(3) 0.3128(4) 0.3497(3) 0.0308(9) Uani 1 1 d . . . C16 C 0.4792(3) 0.3951(4) 0.3928(2) 0.0334(10) Uani 1 1 d . . . C17 C 0.5273(4) 0.4986(5) 0.4061(3) 0.0507(14) Uani 1 1 d . . . H17A H 0.4950 0.5521 0.3696 0.076 Uiso 1 1 calc R . . H17B H 0.5804 0.4869 0.3997 0.076 Uiso 1 1 calc R . . H17C H 0.5375 0.5238 0.4576 0.076 Uiso 1 1 calc R . . C18 C 0.5604(3) 0.3289(4) 0.3215(3) 0.0353(10) Uani 1 1 d . . . C19 C 0.2374(3) 0.4593(4) 0.5550(3) 0.0428(12) Uani 1 1 d . . . H19A H 0.2588 0.5288 0.5471 0.064 Uiso 1 1 calc R . . H19B H 0.2475 0.4498 0.6090 0.064 Uiso 1 1 calc R . . H19C H 0.1776 0.4558 0.5260 0.064 Uiso 1 1 calc R . . C20 C 0.2806(3) 0.3732(4) 0.5292(2) 0.0310(9) Uani 1 1 d . . . C21 C 0.3100(3) 0.2803(4) 0.5740(2) 0.0313(9) Uani 1 1 d . . . C22 C 0.3589(3) 0.1997(4) 0.5587(3) 0.0333(10) Uani 1 1 d . . . C23 C 0.3888(4) 0.1086(5) 0.6112(3) 0.0477(13) Uani 1 1 d . . . H23A H 0.4456 0.0905 0.6157 0.072 Uiso 1 1 calc R . . H23B H 0.3525 0.0471 0.5916 0.072 Uiso 1 1 calc R . . H23C H 0.3882 0.1281 0.6611 0.072 Uiso 1 1 calc R . . C24 C 0.2882(3) 0.2667(4) 0.6395(3) 0.0341(10) Uani 1 1 d . . . C25 C 0.0571(5) 0.1162(7) 0.5304(5) 0.093(3) Uani 1 1 d . . . H25A H 0.0825 0.0839 0.4969 0.140 Uiso 1 1 calc R . . H25B H -0.0034 0.1086 0.5079 0.140 Uiso 1 1 calc R . . H25C H 0.0778 0.0802 0.5797 0.140 Uiso 1 1 calc R . . C26 C 0.0782(4) 0.2262(7) 0.5404(4) 0.0679(18) Uani 1 1 d . . . C27 C 0.0594(6) 0.2885(9) 0.5974(7) 0.123(4) Uani 1 1 d . . . H27A H 0.0778 0.2494 0.6454 0.185 Uiso 1 1 calc R . . H27B H -0.0006 0.3009 0.5804 0.185 Uiso 1 1 calc R . . H27C H 0.0884 0.3571 0.6046 0.185 Uiso 1 1 calc R . . C28 C 0.2914(3) 0.4140(5) 0.2565(3) 0.0453(12) Uani 1 1 d . . . H28A H 0.3363 0.4624 0.2854 0.068 Uiso 1 1 calc R . . H28B H 0.2454 0.4554 0.2215 0.068 Uiso 1 1 calc R . . H28C H 0.3122 0.3641 0.2277 0.068 Uiso 1 1 calc R . . C29 C 0.2087(5) 0.1060(6) 0.4005(4) 0.0711(19) Uani 1 1 d . . . H29A H 0.2591 0.0625 0.4209 0.107 Uiso 1 1 calc R . . H29B H 0.1659 0.0662 0.3607 0.107 Uiso 1 1 calc R . . H29C H 0.1883 0.1233 0.4412 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0505(3) 0.0743(3) 0.0495(3) -0.0056(2) 0.0322(2) 0.0035(2) Ag2 0.0440(2) 0.0481(2) 0.0500(2) -0.00604(18) 0.03489(19) -0.00453(17) Fe1 0.0339(3) 0.0314(3) 0.0302(3) -0.0003(3) 0.0176(3) -0.0014(3) Fe2 0.0305(3) 0.0375(4) 0.0275(3) -0.0007(3) 0.0181(3) -0.0032(3) O1 0.0408(18) 0.0419(19) 0.0357(18) 0.0047(15) 0.0172(15) 0.0044(15) O2 0.060(2) 0.0343(18) 0.0372(18) 0.0017(14) 0.0259(17) 0.0027(16) O3 0.0363(17) 0.0391(19) 0.0396(18) -0.0075(14) 0.0182(15) -0.0036(14) O4 0.0364(17) 0.0326(17) 0.0441(19) -0.0046(14) 0.0227(15) -0.0048(14) O5 0.0351(17) 0.0355(17) 0.0425(18) -0.0018(14) 0.0254(15) -0.0038(13) O6 0.0365(17) 0.048(2) 0.0305(16) -0.0099(14) 0.0206(14) -0.0101(15) O7 0.0405(17) 0.0395(18) 0.0278(16) 0.0013(13) 0.0213(14) 0.0019(14) O8 0.0367(17) 0.0434(19) 0.0332(17) 0.0041(14) 0.0213(14) 0.0033(14) O9 0.0353(17) 0.0364(17) 0.0291(16) 0.0035(13) 0.0194(13) -0.0020(13) O10 0.0386(17) 0.0369(18) 0.0309(16) 0.0040(13) 0.0180(14) -0.0041(14) O11 0.051(2) 0.045(2) 0.078(3) 0.003(2) 0.039(2) -0.0076(18) O12 0.047(2) 0.052(2) 0.054(2) 0.0063(19) 0.0101(18) -0.0077(18) O13 0.045(2) 0.052(2) 0.062(3) 0.003(2) 0.0105(19) 0.0009(18) O14 0.094(4) 0.069(3) 0.062(3) 0.010(3) 0.026(3) -0.006(3) O15 0.101(4) 0.156(6) 0.061(3) -0.003(4) 0.031(3) 0.008(4) O16 0.113(5) 0.062(4) 0.147(6) 0.002(4) 0.034(4) -0.007(3) O17 0.090(4) 0.107(5) 0.076(4) 0.005(3) 0.014(3) -0.025(3) N1 0.072(4) 0.133(6) 0.039(3) -0.007(3) 0.031(3) -0.017(4) N2 0.052(3) 0.051(3) 0.045(2) -0.005(2) 0.027(2) -0.013(2) N3 0.040(2) 0.036(2) 0.057(3) 0.0036(19) 0.031(2) 0.0000(17) N4 0.045(2) 0.048(3) 0.039(2) 0.0080(19) 0.0262(19) 0.0028(19) N5 0.033(2) 0.033(2) 0.053(3) -0.0015(19) 0.023(2) 0.0007(17) N6 0.076(4) 0.080(5) 0.062(4) -0.014(3) 0.032(3) -0.015(3) C1 0.059(4) 0.069(4) 0.045(3) 0.017(3) 0.015(3) 0.003(3) C2 0.039(3) 0.050(3) 0.035(3) 0.002(2) 0.016(2) -0.003(2) C3 0.049(3) 0.049(3) 0.031(2) -0.004(2) 0.022(2) -0.009(2) C4 0.056(3) 0.037(3) 0.038(3) -0.005(2) 0.028(2) -0.004(2) C5 0.125(6) 0.045(3) 0.076(4) 0.003(3) 0.074(5) 0.017(4) C6 0.049(3) 0.072(4) 0.039(3) -0.005(3) 0.021(3) -0.009(3) C7 0.048(3) 0.044(3) 0.060(3) -0.009(3) 0.029(3) -0.015(2) C8 0.031(2) 0.042(3) 0.032(2) 0.000(2) 0.0110(19) -0.005(2) C9 0.032(2) 0.038(3) 0.030(2) 0.0000(19) 0.0156(18) -0.0047(19) C10 0.033(2) 0.037(2) 0.029(2) 0.0030(19) 0.0127(19) 0.0006(19) C11 0.040(3) 0.037(3) 0.045(3) -0.009(2) 0.022(2) -0.001(2) C12 0.037(2) 0.039(3) 0.035(2) 0.000(2) 0.017(2) -0.005(2) C13 0.058(3) 0.033(3) 0.076(4) -0.003(3) 0.049(3) 0.001(2) C14 0.031(2) 0.038(3) 0.033(2) 0.0034(19) 0.0170(19) 0.0047(19) C15 0.027(2) 0.038(3) 0.032(2) 0.0054(19) 0.0173(18) 0.0043(18) C16 0.030(2) 0.045(3) 0.029(2) -0.004(2) 0.0152(18) -0.008(2) C17 0.055(3) 0.056(3) 0.055(3) -0.022(3) 0.038(3) -0.024(3) C18 0.035(2) 0.036(3) 0.042(3) 0.002(2) 0.023(2) 0.004(2) C19 0.056(3) 0.042(3) 0.041(3) 0.001(2) 0.031(2) 0.005(2) C20 0.030(2) 0.039(2) 0.028(2) 0.0002(19) 0.0161(18) -0.0054(19) C21 0.032(2) 0.041(3) 0.025(2) -0.0023(19) 0.0155(18) -0.0078(19) C22 0.034(2) 0.038(3) 0.031(2) 0.0028(19) 0.0153(19) -0.0032(19) C23 0.053(3) 0.053(3) 0.044(3) 0.012(3) 0.026(3) 0.009(3) C24 0.032(2) 0.042(3) 0.031(2) 0.001(2) 0.0146(19) -0.002(2) C25 0.080(5) 0.087(6) 0.111(7) 0.005(5) 0.033(5) 0.013(5) C26 0.047(4) 0.093(6) 0.055(4) 0.001(4) 0.009(3) -0.006(4) C27 0.080(6) 0.141(9) 0.153(10) -0.064(8) 0.049(6) 0.007(6) C28 0.049(3) 0.054(3) 0.037(3) 0.006(2) 0.020(2) -0.011(2) C29 0.070(4) 0.062(4) 0.085(5) 0.015(4) 0.032(4) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.251(4) 4_665 ? Ag1 N1 2.311(5) . ? Ag1 O14 2.446(5) . ? Ag1 O11 2.564(4) . ? Ag1 Ag2 3.3232(6) 4_565 ? Ag2 N3 2.160(4) . ? Ag2 N4 2.227(4) 4_665 ? Ag2 O12 2.439(4) 3_665 ? Ag2 Ag1 3.3232(6) 4_666 ? Fe1 O10 1.955(3) . ? Fe1 O9 1.977(3) . ? Fe1 O3 1.993(3) . ? Fe1 O2 1.999(3) . ? Fe1 O1 2.008(3) . ? Fe1 O4 2.017(3) . ? Fe2 O10 1.947(3) . ? Fe2 O9 1.976(3) . ? Fe2 O6 2.008(3) . ? Fe2 O8 2.016(3) . ? Fe2 O5 2.017(3) . ? Fe2 O7 2.020(3) . ? O1 C2 1.282(6) . ? O2 C4 1.254(6) . ? O3 C8 1.270(5) . ? O4 C10 1.257(5) . ? O5 C14 1.264(5) . ? O6 C16 1.272(5) . ? O7 C20 1.261(5) . ? O8 C22 1.276(5) . ? O9 C28 1.435(5) . ? O10 C29 1.439(7) . ? O11 N5 1.239(5) . ? O12 N5 1.242(5) . ? O12 Ag2 2.439(4) 3_665 ? O13 N5 1.250(5) . ? O14 N6 1.217(7) . ? O15 N6 1.251(8) . ? O16 N6 1.261(8) . ? O17 C26 1.213(8) . ? N1 C6 1.140(7) . ? N2 C12 1.146(6) . ? N2 Ag1 2.251(4) 4_566 ? N3 C18 1.139(6) . ? N4 C24 1.136(6) . ? N4 Ag2 2.226(4) 4_566 ? C1 C2 1.488(8) . ? C2 C3 1.403(7) . ? C3 C4 1.420(7) . ? C3 C6 1.423(7) . ? C4 C5 1.501(7) . ? C7 C8 1.497(7) . ? C8 C9 1.416(7) . ? C9 C10 1.419(7) . ? C9 C12 1.431(6) . ? C10 C11 1.499(6) . ? C13 C14 1.488(7) . ? C14 C15 1.423(7) . ? C15 C16 1.405(6) . ? C15 C18 1.428(6) . ? C16 C17 1.512(7) . ? C19 C20 1.493(6) . ? C20 C21 1.423(7) . ? C21 C22 1.414(7) . ? C21 C24 1.432(6) . ? C22 C23 1.481(7) . ? C25 C26 1.423(12) . ? C26 C27 1.463(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 136.7(2) 4_665 . ? N2 Ag1 O14 110.16(18) 4_665 . ? N1 Ag1 O14 87.24(19) . . ? N2 Ag1 O11 101.71(14) 4_665 . ? N1 Ag1 O11 94.87(17) . . ? O14 Ag1 O11 130.44(15) . . ? N2 Ag1 Ag2 58.24(12) 4_665 4_565 ? N1 Ag1 Ag2 98.56(15) . 4_565 ? O14 Ag1 Ag2 167.45(13) . 4_565 ? O11 Ag1 Ag2 60.46(9) . 4_565 ? N3 Ag2 N4 141.57(16) . 4_665 ? N3 Ag2 O12 122.79(15) . 3_665 ? N4 Ag2 O12 92.84(15) 4_665 3_665 ? N3 Ag2 Ag1 79.25(12) . 4_666 ? N4 Ag2 Ag1 101.60(12) 4_665 4_666 ? O12 Ag2 Ag1 112.39(9) 3_665 4_666 ? O10 Fe1 O9 76.69(13) . . ? O10 Fe1 O3 93.32(14) . . ? O9 Fe1 O3 169.61(13) . . ? O10 Fe1 O2 91.55(14) . . ? O9 Fe1 O2 92.81(14) . . ? O3 Fe1 O2 90.30(14) . . ? O10 Fe1 O1 170.30(13) . . ? O9 Fe1 O1 94.37(13) . . ? O3 Fe1 O1 95.78(14) . . ? O2 Fe1 O1 85.08(14) . . ? O10 Fe1 O4 98.05(14) . . ? O9 Fe1 O4 92.71(13) . . ? O3 Fe1 O4 85.77(13) . . ? O2 Fe1 O4 169.81(15) . . ? O1 Fe1 O4 85.97(14) . . ? O10 Fe2 O9 76.87(13) . . ? O10 Fe2 O6 168.77(14) . . ? O9 Fe2 O6 91.93(13) . . ? O10 Fe2 O8 93.57(13) . . ? O9 Fe2 O8 170.22(13) . . ? O6 Fe2 O8 97.59(14) . . ? O10 Fe2 O5 96.69(13) . . ? O9 Fe2 O5 94.83(13) . . ? O6 Fe2 O5 85.02(13) . . ? O8 Fe2 O5 88.28(13) . . ? O10 Fe2 O7 94.45(13) . . ? O9 Fe2 O7 93.51(12) . . ? O6 Fe2 O7 85.22(13) . . ? O8 Fe2 O7 85.07(13) . . ? O5 Fe2 O7 167.36(14) . . ? C2 O1 Fe1 130.9(3) . . ? C4 O2 Fe1 132.0(3) . . ? C8 O3 Fe1 130.6(3) . . ? C10 O4 Fe1 131.0(3) . . ? C14 O5 Fe2 131.4(3) . . ? C16 O6 Fe2 130.9(3) . . ? C20 O7 Fe2 131.0(3) . . ? C22 O8 Fe2 129.5(3) . . ? C28 O9 Fe2 128.4(3) . . ? C28 O9 Fe1 123.7(3) . . ? Fe2 O9 Fe1 102.29(13) . . ? C29 O10 Fe2 128.7(4) . . ? C29 O10 Fe1 126.9(4) . . ? Fe2 O10 Fe1 104.13(14) . . ? N5 O11 Ag1 101.8(3) . . ? N5 O12 Ag2 105.9(3) . 3_665 ? N6 O14 Ag1 105.5(4) . . ? C6 N1 Ag1 139.0(5) . . ? C12 N2 Ag1 155.2(4) . 4_566 ? C18 N3 Ag2 168.4(4) . . ? C24 N4 Ag2 155.6(4) . 4_566 ? O11 N5 O12 120.3(4) . . ? O11 N5 O13 119.0(4) . . ? O12 N5 O13 120.7(4) . . ? O14 N6 O15 122.0(7) . . ? O14 N6 O16 118.9(6) . . ? O15 N6 O16 119.0(8) . . ? O1 C2 C3 122.8(5) . . ? O1 C2 C1 116.4(5) . . ? C3 C2 C1 120.7(5) . . ? C2 C3 C4 124.3(4) . . ? C2 C3 C6 117.3(5) . . ? C4 C3 C6 118.3(5) . . ? O2 C4 C3 122.4(5) . . ? O2 C4 C5 118.0(5) . . ? C3 C4 C5 119.6(5) . . ? N1 C6 C3 179.0(7) . . ? O3 C8 C9 122.7(4) . . ? O3 C8 C7 116.7(4) . . ? C9 C8 C7 120.6(4) . . ? C8 C9 C10 124.3(4) . . ? C8 C9 C12 117.8(4) . . ? C10 C9 C12 117.9(4) . . ? O4 C10 C9 122.9(4) . . ? O4 C10 C11 117.0(4) . . ? C9 C10 C11 120.0(4) . . ? N2 C12 C9 179.0(6) . . ? O5 C14 C15 122.3(4) . . ? O5 C14 C13 118.4(4) . . ? C15 C14 C13 119.2(4) . . ? C16 C15 C14 124.4(4) . . ? C16 C15 C18 117.3(4) . . ? C14 C15 C18 118.2(4) . . ? O6 C16 C15 123.1(4) . . ? O6 C16 C17 115.6(4) . . ? C15 C16 C17 121.3(4) . . ? N3 C18 C15 179.6(6) . . ? O7 C20 C21 122.0(4) . . ? O7 C20 C19 117.4(4) . . ? C21 C20 C19 120.6(4) . . ? C22 C21 C20 125.0(4) . . ? C22 C21 C24 117.2(4) . . ? C20 C21 C24 117.8(4) . . ? O8 C22 C21 122.4(4) . . ? O8 C22 C23 117.4(4) . . ? C21 C22 C23 120.2(4) . . ? N4 C24 C21 179.0(6) . . ? O17 C26 C25 119.5(8) . . ? O17 C26 C27 120.4(8) . . ? C25 C26 C27 120.1(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.572 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.125 #===END data_compound_8_bath175 _database_code_depnum_ccdc_archive 'CCDC 636532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Ag Fe2 N5 O13' _chemical_formula_weight 840.12 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1107(5) _cell_length_b 11.3532(5) _cell_length_c 13.0922(6) _cell_angle_alpha 99.941(1) _cell_angle_beta 93.406(1) _cell_angle_gamma 96.678(1) _cell_volume 1610.30(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3341 _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 31.11 _exptl_crystal_description block _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9121 _exptl_absorpt_correction_T_max 0.9401 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8460 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2 SMX' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12013 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 33.07 _reflns_number_total 6591 _reflns_number_gt 5503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0514P)^2^+0.7435P] 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 6591 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.95868(3) 0.80047(3) 0.29235(2) 0.02676(10) Uani 1 1 d . . . Fe1 Fe 1.71490(4) 1.32946(4) 0.20873(4) 0.01842(13) Uani 1 1 d . . . O1 O 1.7437(2) 1.4507(2) 0.11508(18) 0.0212(5) Uani 1 1 d . . . N1 N 1.9230(3) 1.3327(3) -0.2001(3) 0.0345(8) Uani 1 1 d . . . C1 C 1.8205(4) 1.5621(3) -0.0078(3) 0.0257(8) Uani 1 1 d . . . H1A H 1.7474 1.5757 -0.0475 0.039 Uiso 1 1 calc R . . H1B H 1.8878 1.5577 -0.0529 0.039 Uiso 1 1 calc R . . H1C H 1.8421 1.6287 0.0512 0.039 Uiso 1 1 calc R . . Fe2 Fe 1.45821(4) 1.38175(4) 0.25984(4) 0.01805(13) Uani 1 1 d . . . O2 O 1.7675(2) 1.2129(2) 0.0941(2) 0.0243(6) Uani 1 1 d . . . N2 N 2.0644(3) 1.2348(3) 0.5408(2) 0.0278(7) Uani 1 1 d . . . C2 C 1.7964(3) 1.4460(3) 0.0316(3) 0.0193(7) Uani 1 1 d . . . O3 O 1.8853(2) 1.3974(2) 0.2712(2) 0.0254(6) Uani 1 1 d . . . N3 N 1.3983(4) 1.9002(3) 0.2819(3) 0.0524(11) Uani 1 1 d . . . C3 C 1.8278(3) 1.3371(3) -0.0253(3) 0.0198(7) Uani 1 1 d . . . O4 O 1.7335(2) 1.1997(2) 0.29427(19) 0.0228(6) Uani 1 1 d . . . N4 N 1.0924(3) 0.9829(3) 0.3330(3) 0.0307(8) Uani 1 1 d . . . C4 C 1.8071(3) 1.2232(3) 0.0078(3) 0.0213(8) Uani 1 1 d . . . O5 O 1.4602(2) 1.4971(2) 0.16018(19) 0.0212(5) Uani 1 1 d . . . N5 N 0.7879(3) 0.8688(3) 0.1415(3) 0.0339(8) Uani 1 1 d . . . C5 C 1.8310(4) 1.1102(3) -0.0617(3) 0.0329(10) Uani 1 1 d . . . H5A H 1.8119 1.0411 -0.0272 0.049 Uiso 1 1 calc R . . H5B H 1.9168 1.1171 -0.0762 0.049 Uiso 1 1 calc R . . H5C H 1.7799 1.0986 -0.1272 0.049 Uiso 1 1 calc R . . O6 O 1.3904(2) 1.5096(2) 0.3570(2) 0.0246(6) Uani 1 1 d . . . C6 C 1.8806(3) 1.3380(3) -0.1219(3) 0.0244(8) Uani 1 1 d . . . O7 O 1.2921(2) 1.3054(2) 0.19774(19) 0.0210(5) Uani 1 1 d . . . C7 C 2.0715(3) 1.4515(3) 0.3734(3) 0.0253(8) Uani 1 1 d . . . H7A H 2.0769 1.5173 0.3336 0.038 Uiso 1 1 calc R . . H7B H 2.1394 1.4047 0.3596 0.038 Uiso 1 1 calc R . . H7C H 2.0751 1.4850 0.4478 0.038 Uiso 1 1 calc R . . O8 O 1.4304(2) 1.2792(2) 0.36986(19) 0.0233(6) Uani 1 1 d . . . C8 C 1.9534(3) 1.3708(3) 0.3412(3) 0.0196(7) Uani 1 1 d . . . O9 O 1.6325(2) 1.4373(2) 0.30797(18) 0.0199(5) Uani 1 1 d . . . C9 C 1.9238(3) 1.2677(3) 0.3884(3) 0.0189(7) Uani 1 1 d . . . O10 O 1.5431(2) 1.2658(2) 0.17152(18) 0.0203(5) Uani 1 1 d . . . C10 C 1.8163(3) 1.1836(3) 0.3583(3) 0.0193(7) Uani 1 1 d . . . O11 O 0.7625(3) 0.8098(3) 0.2128(2) 0.0464(8) Uani 1 1 d . . . C11 C 1.7982(4) 1.0706(3) 0.4027(3) 0.0266(8) Uani 1 1 d . . . H11A H 1.7148 1.0309 0.3837 0.040 Uiso 1 1 calc R . . H11B H 1.8126 1.0905 0.4787 0.040 Uiso 1 1 calc R . . H11C H 1.8555 1.0161 0.3749 0.040 Uiso 1 1 calc R . . O12 O 0.8961(3) 0.9038(4) 0.1348(3) 0.0687(12) Uani 1 1 d . . . C12 C 2.0034(3) 1.2492(3) 0.4716(3) 0.0224(8) Uani 1 1 d . . . O13 O 0.7103(3) 0.8890(3) 0.0792(3) 0.0618(11) Uani 1 1 d . . . C13 C 1.4913(3) 1.6740(3) 0.0885(3) 0.0252(8) Uani 1 1 d . . . H13A H 1.5770 1.7083 0.1023 0.038 Uiso 1 1 calc R . . H13B H 1.4411 1.7389 0.0849 0.038 Uiso 1 1 calc R . . H13C H 1.4801 1.6172 0.0222 0.038 Uiso 1 1 calc R . . C14 C 1.4542(3) 1.6094(3) 0.1741(3) 0.0196(7) Uani 1 1 d . . . C15 C 1.4145(3) 1.6733(3) 0.2668(3) 0.0227(8) Uani 1 1 d . . . C16 C 1.3793(3) 1.6184(3) 0.3508(3) 0.0237(8) Uani 1 1 d . . . C17 C 1.3246(4) 1.6888(4) 0.4406(3) 0.0329(9) Uani 1 1 d . . . H17A H 1.2431 1.7040 0.4178 0.049 Uiso 1 1 calc R . . H17B H 1.3761 1.7658 0.4655 0.049 Uiso 1 1 calc R . . H17C H 1.3189 1.6424 0.4971 0.049 Uiso 1 1 calc R . . C18 C 1.4052(4) 1.7985(4) 0.2737(3) 0.0341(10) Uani 1 1 d . . . C19 C 1.1043(3) 1.1843(3) 0.1473(3) 0.0233(8) Uani 1 1 d . . . H19A H 1.0579 1.2531 0.1515 0.035 Uiso 1 1 calc R . . H19B H 1.0554 1.1168 0.1690 0.035 Uiso 1 1 calc R . . H19C H 1.1245 1.1600 0.0755 0.035 Uiso 1 1 calc R . . C20 C 1.2192(3) 1.2196(3) 0.2176(3) 0.0175(7) Uani 1 1 d . . . C21 C 1.2418(3) 1.1621(3) 0.3041(3) 0.0199(7) Uani 1 1 d . . . C22 C 1.3462(3) 1.1978(3) 0.3775(3) 0.0211(8) Uani 1 1 d . . . C23 C 1.3554(4) 1.1371(3) 0.4701(3) 0.0287(9) Uani 1 1 d . . . H23A H 1.3665 1.0525 0.4471 0.043 Uiso 1 1 calc R . . H23B H 1.2807 1.1412 0.5060 0.043 Uiso 1 1 calc R . . H23C H 1.4250 1.1778 0.5176 0.043 Uiso 1 1 calc R . . C24 C 1.1581(3) 1.0630(3) 0.3195(3) 0.0218(8) Uani 1 1 d . . . C25 C 1.6831(4) 1.5555(3) 0.3602(3) 0.0315(9) Uani 1 1 d . . . H25A H 1.7703 1.5567 0.3780 0.047 Uiso 1 1 calc R . . H25B H 1.6424 1.5771 0.4239 0.047 Uiso 1 1 calc R . . H25C H 1.6713 1.6137 0.3144 0.047 Uiso 1 1 calc R . . C26 C 1.4986(4) 1.1412(3) 0.1287(3) 0.0300(9) Uani 1 1 d . . . H26A H 1.4694 1.1003 0.1843 0.045 Uiso 1 1 calc R . . H26B H 1.5646 1.1013 0.0972 0.045 Uiso 1 1 calc R . . H26C H 1.4318 1.1376 0.0755 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02925(18) 0.02904(18) 0.02250(16) 0.00821(12) 0.00205(12) 0.00055(12) Fe1 0.0191(3) 0.0175(3) 0.0197(3) 0.0067(2) 0.0035(2) 0.0006(2) O1 0.0257(14) 0.0196(13) 0.0203(13) 0.0075(10) 0.0056(10) 0.0036(10) N1 0.046(2) 0.0295(19) 0.031(2) 0.0104(15) 0.0123(17) 0.0057(16) C1 0.033(2) 0.0191(19) 0.026(2) 0.0082(15) 0.0072(16) 0.0009(16) Fe2 0.0189(3) 0.0158(3) 0.0195(3) 0.0052(2) 0.0032(2) -0.00161(19) O2 0.0312(15) 0.0175(13) 0.0277(14) 0.0096(11) 0.0122(11) 0.0048(11) N2 0.0336(19) 0.0282(18) 0.0216(17) 0.0088(14) -0.0006(14) -0.0008(14) C2 0.0147(17) 0.0202(18) 0.0247(19) 0.0112(15) -0.0022(14) 0.0003(14) O3 0.0211(13) 0.0257(14) 0.0309(15) 0.0133(12) 0.0000(11) -0.0027(11) N3 0.075(3) 0.028(2) 0.056(3) 0.0038(19) 0.011(2) 0.016(2) C3 0.0206(18) 0.0184(18) 0.0212(18) 0.0064(14) 0.0040(14) 0.0005(14) O4 0.0231(13) 0.0197(13) 0.0267(14) 0.0109(11) 0.0014(11) -0.0021(10) N4 0.0353(19) 0.0248(18) 0.0303(19) 0.0083(14) 0.0021(15) -0.0072(15) C4 0.0182(18) 0.0194(18) 0.028(2) 0.0058(15) 0.0028(15) 0.0046(14) O5 0.0251(13) 0.0170(12) 0.0221(13) 0.0057(10) 0.0043(10) 0.0007(10) N5 0.034(2) 0.0309(19) 0.034(2) 0.0111(16) -0.0102(16) -0.0054(15) C5 0.045(3) 0.0186(19) 0.038(2) 0.0056(17) 0.017(2) 0.0065(18) O6 0.0266(14) 0.0226(14) 0.0251(14) 0.0047(11) 0.0093(11) 0.0010(11) C6 0.028(2) 0.0186(18) 0.028(2) 0.0068(15) 0.0042(16) 0.0026(15) O7 0.0199(13) 0.0214(13) 0.0226(13) 0.0096(10) 0.0009(10) -0.0011(10) C7 0.0237(19) 0.024(2) 0.028(2) 0.0069(16) 0.0059(16) -0.0011(15) O8 0.0213(13) 0.0225(13) 0.0256(14) 0.0097(11) -0.0003(11) -0.0059(10) C8 0.0208(18) 0.0186(18) 0.0199(18) 0.0033(14) 0.0083(14) 0.0016(14) O9 0.0218(13) 0.0156(12) 0.0197(13) -0.0002(10) 0.0015(10) -0.0027(10) C9 0.0226(18) 0.0185(17) 0.0161(17) 0.0038(14) 0.0052(14) 0.0026(14) O10 0.0225(13) 0.0160(12) 0.0207(13) 0.0009(10) 0.0019(10) -0.0012(10) C10 0.0260(19) 0.0154(17) 0.0183(18) 0.0044(14) 0.0096(15) 0.0048(14) O11 0.0471(19) 0.0458(19) 0.047(2) 0.0234(16) -0.0113(15) -0.0074(15) C11 0.034(2) 0.0199(19) 0.029(2) 0.0126(16) 0.0043(17) 0.0011(16) O12 0.033(2) 0.115(4) 0.063(3) 0.041(2) 0.0014(17) -0.006(2) C12 0.029(2) 0.0171(18) 0.0214(19) 0.0038(15) 0.0092(16) -0.0019(15) O13 0.047(2) 0.067(2) 0.073(3) 0.048(2) -0.0285(19) -0.0190(18) C13 0.025(2) 0.0237(19) 0.027(2) 0.0087(16) 0.0016(16) -0.0003(15) C14 0.0128(17) 0.0213(18) 0.0245(19) 0.0065(15) -0.0024(14) 0.0001(14) C15 0.0204(19) 0.0212(18) 0.026(2) 0.0030(15) 0.0019(15) 0.0048(14) C16 0.0187(18) 0.026(2) 0.026(2) 0.0008(16) 0.0044(15) 0.0019(15) C17 0.029(2) 0.037(2) 0.030(2) -0.0023(18) 0.0088(17) 0.0029(18) C18 0.041(3) 0.027(2) 0.035(2) 0.0044(18) 0.0077(19) 0.0094(18) C19 0.0220(19) 0.0226(19) 0.0239(19) 0.0039(15) -0.0003(15) -0.0013(15) C20 0.0182(17) 0.0142(16) 0.0195(18) 0.0000(13) 0.0043(14) 0.0019(13) C21 0.0210(18) 0.0158(17) 0.0215(18) 0.0017(14) 0.0026(14) -0.0016(14) C22 0.0251(19) 0.0159(17) 0.0233(19) 0.0054(14) 0.0052(15) 0.0029(14) C23 0.033(2) 0.025(2) 0.028(2) 0.0106(16) -0.0008(17) -0.0070(17) C24 0.0242(19) 0.0192(18) 0.0208(19) 0.0025(15) -0.0010(15) 0.0016(15) C25 0.027(2) 0.023(2) 0.038(2) -0.0049(17) 0.0000(18) -0.0043(16) C26 0.029(2) 0.021(2) 0.037(2) 0.0011(17) 0.0034(18) -0.0001(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.312(3) 2_876 ? Ag1 N1 2.344(4) 2_875 ? Ag1 N4 2.364(3) . ? Ag1 O11 2.381(3) . ? Fe1 O10 1.962(2) . ? Fe1 O9 1.969(2) . ? Fe1 O2 1.986(2) . ? Fe1 O1 2.007(2) . ? Fe1 O4 2.020(2) . ? Fe1 O3 2.027(3) . ? O1 C2 1.266(4) . ? N1 C6 1.148(5) . ? N1 Ag1 2.344(4) 2_875 ? C1 C2 1.497(5) . ? Fe2 O10 1.963(2) . ? Fe2 O9 1.995(2) . ? Fe2 O5 2.001(2) . ? Fe2 O6 2.006(3) . ? Fe2 O7 2.006(2) . ? Fe2 O8 2.018(2) . ? O2 C4 1.257(4) . ? N2 C12 1.144(5) . ? N2 Ag1 2.312(3) 2_876 ? C2 C3 1.420(5) . ? O3 C8 1.253(4) . ? N3 C18 1.152(5) . ? C3 C6 1.427(5) . ? C3 C4 1.431(5) . ? O4 C10 1.257(4) . ? N4 C24 1.143(5) . ? C4 C5 1.500(5) . ? O5 C14 1.267(4) . ? N5 O13 1.220(4) . ? N5 O12 1.235(5) . ? N5 O11 1.266(4) . ? O6 C16 1.272(4) . ? O7 C20 1.266(4) . ? C7 C8 1.503(5) . ? O8 C22 1.258(4) . ? C8 C9 1.430(5) . ? O9 C25 1.431(4) . ? C9 C12 1.422(5) . ? C9 C10 1.430(5) . ? O10 C26 1.446(4) . ? C10 C11 1.495(5) . ? C13 C14 1.494(5) . ? C14 C15 1.425(5) . ? C15 C16 1.408(5) . ? C15 C18 1.425(5) . ? C16 C17 1.505(5) . ? C19 C20 1.501(5) . ? C20 C21 1.425(5) . ? C21 C24 1.424(5) . ? C21 C22 1.434(5) . ? C22 C23 1.497(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 112.31(12) 2_876 2_875 ? N2 Ag1 N4 98.90(11) 2_876 . ? N1 Ag1 N4 102.92(12) 2_875 . ? N2 Ag1 O11 108.00(11) 2_876 . ? N1 Ag1 O11 116.55(12) 2_875 . ? N4 Ag1 O11 116.86(11) . . ? O10 Fe1 O9 77.91(10) . . ? O10 Fe1 O2 91.81(10) . . ? O9 Fe1 O2 169.25(11) . . ? O10 Fe1 O1 102.37(10) . . ? O9 Fe1 O1 93.50(10) . . ? O2 Fe1 O1 85.57(10) . . ? O10 Fe1 O4 90.54(10) . . ? O9 Fe1 O4 98.48(10) . . ? O2 Fe1 O4 84.61(10) . . ? O1 Fe1 O4 164.01(10) . . ? O10 Fe1 O3 170.79(10) . . ? O9 Fe1 O3 95.19(10) . . ? O2 Fe1 O3 95.36(11) . . ? O1 Fe1 O3 83.98(10) . . ? O4 Fe1 O3 84.41(10) . . ? C2 O1 Fe1 131.2(2) . . ? C6 N1 Ag1 134.1(3) . 2_875 ? O10 Fe2 O9 77.26(10) . . ? O10 Fe2 O5 94.30(10) . . ? O9 Fe2 O5 91.45(10) . . ? O10 Fe2 O6 173.41(10) . . ? O9 Fe2 O6 96.15(10) . . ? O5 Fe2 O6 85.51(10) . . ? O10 Fe2 O7 94.18(10) . . ? O9 Fe2 O7 171.42(10) . . ? O5 Fe2 O7 89.79(10) . . ? O6 Fe2 O7 92.42(10) . . ? O10 Fe2 O8 95.08(10) . . ? O9 Fe2 O8 94.61(10) . . ? O5 Fe2 O8 169.76(10) . . ? O6 Fe2 O8 85.64(10) . . ? O7 Fe2 O8 85.44(10) . . ? C4 O2 Fe1 133.2(2) . . ? C12 N2 Ag1 137.4(3) . 2_876 ? O1 C2 C3 122.9(3) . . ? O1 C2 C1 116.4(3) . . ? C3 C2 C1 120.7(3) . . ? C8 O3 Fe1 132.9(2) . . ? C2 C3 C6 119.6(3) . . ? C2 C3 C4 123.6(3) . . ? C6 C3 C4 116.8(3) . . ? C10 O4 Fe1 133.1(2) . . ? C24 N4 Ag1 158.4(3) . . ? O2 C4 C3 122.3(3) . . ? O2 C4 C5 117.4(3) . . ? C3 C4 C5 120.3(3) . . ? C14 O5 Fe2 131.5(2) . . ? O13 N5 O12 119.9(4) . . ? O13 N5 O11 122.4(4) . . ? O12 N5 O11 117.6(3) . . ? C16 O6 Fe2 130.8(2) . . ? N1 C6 C3 176.7(4) . . ? C20 O7 Fe2 132.9(2) . . ? C22 O8 Fe2 131.5(2) . . ? O3 C8 C9 122.8(3) . . ? O3 C8 C7 117.0(3) . . ? C9 C8 C7 120.2(3) . . ? C25 O9 Fe1 125.3(2) . . ? C25 O9 Fe2 126.6(2) . . ? Fe1 O9 Fe2 101.46(10) . . ? C12 C9 C8 118.6(3) . . ? C12 C9 C10 118.0(3) . . ? C8 C9 C10 123.4(3) . . ? C26 O10 Fe1 124.7(2) . . ? C26 O10 Fe2 127.1(2) . . ? Fe1 O10 Fe2 102.87(11) . . ? O4 C10 C9 122.7(3) . . ? O4 C10 C11 117.0(3) . . ? C9 C10 C11 120.3(3) . . ? N5 O11 Ag1 102.0(2) . . ? N2 C12 C9 177.7(4) . . ? O5 C14 C15 122.4(3) . . ? O5 C14 C13 117.1(3) . . ? C15 C14 C13 120.5(3) . . ? C16 C15 C14 123.5(3) . . ? C16 C15 C18 118.0(3) . . ? C14 C15 C18 118.5(3) . . ? O6 C16 C15 124.0(3) . . ? O6 C16 C17 115.8(3) . . ? C15 C16 C17 120.3(3) . . ? N3 C18 C15 178.3(5) . . ? O7 C20 C21 122.3(3) . . ? O7 C20 C19 116.3(3) . . ? C21 C20 C19 121.3(3) . . ? C24 C21 C20 119.3(3) . . ? C24 C21 C22 117.1(3) . . ? C20 C21 C22 123.5(3) . . ? O8 C22 C21 123.7(3) . . ? O8 C22 C23 117.5(3) . . ? C21 C22 C23 118.7(3) . . ? N4 C24 C21 178.8(4) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 33.07 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 1.042 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.103 #===END data_compound_9_bath177 _database_code_depnum_ccdc_archive 'CCDC 636533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H31.80 Ag Fe2 N4 O11.40' _chemical_formula_weight 802.32 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 7.6634(5) _cell_length_b 9.6825(7) _cell_length_c 27.1105(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2011.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3195 _cell_measurement_theta_min 4.13 _cell_measurement_theta_max 31.51 _exptl_crystal_description Irregular _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8460 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2 SMX' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13713 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 33.11 _reflns_number_total 2234 _reflns_number_gt 1594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1541P)^2^+2.5464P] 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 0.004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2234 _refine_ls_number_parameters 118 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.2420 _refine_ls_wR_factor_gt 0.2246 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -1.0000 -1.0000 0.2500 0.0488(4) Uani 1 4 d S . . Fe1 Fe -0.5000 -0.5000 0.05635(3) 0.0438(4) Uani 1 2 d S . . O1 O -0.7347(4) -0.5886(4) 0.06437(12) 0.0551(9) Uani 1 1 d . . . N1 N -0.8345(8) -0.8713(7) 0.2016(3) 0.114(3) Uani 1 1 d . . . C1 C -0.9830(6) -0.6906(8) 0.0981(4) 0.090(2) Uani 1 1 d . . . H1A H -1.0380 -0.6298 0.1225 0.136 Uiso 1 1 calc R . . H1B H -1.0060 -0.7871 0.1069 0.136 Uiso 1 1 calc R . . H1C H -1.0311 -0.6713 0.0654 0.136 Uiso 1 1 calc R . . C7A C -0.601(3) -0.2399(16) 0.0000 0.108(7) Uani 0.64 2 d SPD A 1 H7A1 H -0.6382 -0.2100 0.0329 0.162 Uiso 0.16 1 calc PR A 1 H7A2 H -0.6921 -0.2162 -0.0240 0.162 Uiso 0.16 1 calc PR A 1 H7A3 H -0.4924 -0.1934 -0.0089 0.162 Uiso 0.16 1 calc PR A 1 C7B C -0.730(4) -0.303(4) 0.0000 0.090(10) Uani 0.36 2 d SPD A 2 H7B1 H -0.7415 -0.2568 0.0319 0.135 Uiso 0.09 1 calc PR A 2 H7B2 H -0.8319 -0.3621 -0.0057 0.135 Uiso 0.09 1 calc PR A 2 H7B3 H -0.7219 -0.2339 -0.0263 0.135 Uiso 0.09 1 calc PR A 2 O2 O -0.4177(4) -0.6372(4) 0.10719(12) 0.0583(10) Uani 1 1 d . . . C2 C -0.7920(5) -0.6659(6) 0.0977(2) 0.0562(13) Uani 1 1 d . . . O3 O -0.5748(5) -0.3865(5) 0.0000 0.0502(12) Uani 1 2 d SD . . C3 C -0.6844(7) -0.7246(6) 0.1348(2) 0.0643(15) Uani 1 1 d . . . C4 C -0.5032(6) -0.7107(7) 0.1365(2) 0.0593(14) Uani 1 1 d . . . C5 C -0.3931(9) -0.7899(9) 0.1734(3) 0.097(3) Uani 1 1 d . . . H5A H -0.4647 -0.8146 0.2020 0.145 Uiso 1 1 calc R . . H5B H -0.2952 -0.7321 0.1841 0.145 Uiso 1 1 calc R . . H5C H -0.3481 -0.8741 0.1579 0.145 Uiso 1 1 calc R . . C6 C -0.7671(9) -0.8076(8) 0.1709(3) 0.089(2) Uani 1 1 d . . . OH2 O -0.5000 0.0000 0.0771(12) 0.069(8) Uiso 0.20 2 d SP B 2 OH1 O -0.184(3) -0.5000 0.2500 0.068(5) Uiso 0.30 2 d SP C 1 OS1 O -0.317(4) -0.121(3) 0.0000 0.077(8) Uiso 0.20 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0275(5) 0.0671(6) 0.0519(6) 0.000 0.000 0.000 Fe1 0.0223(6) 0.0747(8) 0.0344(6) 0.000 0.000 0.0040(4) O1 0.0199(14) 0.090(2) 0.0557(19) -0.0046(19) -0.0041(13) 0.0027(15) N1 0.075(4) 0.112(5) 0.154(6) 0.049(5) 0.056(4) 0.001(4) C1 0.025(2) 0.090(5) 0.156(7) 0.001(5) 0.004(3) -0.005(3) C7A 0.15(2) 0.090(13) 0.090(12) 0.000 0.000 0.052(14) C7B 0.076(17) 0.14(3) 0.054(13) 0.000 0.000 0.056(19) O2 0.0223(14) 0.105(3) 0.0478(18) 0.0201(18) -0.0031(13) -0.0006(16) C2 0.0206(19) 0.072(3) 0.076(3) -0.004(3) 0.010(2) -0.002(2) O3 0.033(2) 0.076(3) 0.041(2) 0.000 0.000 0.015(2) C3 0.039(3) 0.084(4) 0.070(3) 0.009(3) 0.021(2) -0.001(3) C4 0.041(3) 0.088(4) 0.049(3) 0.014(3) 0.008(2) 0.005(2) C5 0.056(4) 0.145(6) 0.090(5) 0.062(5) 0.000(3) -0.003(4) C6 0.051(3) 0.105(5) 0.112(5) 0.025(5) 0.034(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.210(6) 4_355 ? Ag1 N1 2.210(6) 3_535 ? Ag1 N1 2.210(6) 2_335 ? Ag1 N1 2.210(6) . ? Fe1 O3 1.967(3) 5_445 ? Fe1 O3 1.967(3) . ? Fe1 O1 2.004(3) . ? Fe1 O1 2.004(3) 2_445 ? Fe1 O2 2.016(3) 2_445 ? Fe1 O2 2.016(3) . ? O1 C2 1.253(6) . ? N1 C6 1.157(9) . ? C1 C2 1.483(6) . ? C7A O3 1.434(15) . ? C7B O3 1.436(18) . ? O2 C4 1.253(7) . ? C2 C3 1.418(8) . ? O3 Fe1 1.967(3) 5_445 ? C3 C4 1.396(7) . ? C3 C6 1.417(9) . ? C4 C5 1.517(8) . ? 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 107.1(5) 4_355 3_535 ? N1 Ag1 N1 110.0(4) 4_355 2_335 ? N1 Ag1 N1 111.4(4) 3_535 2_335 ? N1 Ag1 N1 111.4(4) 4_355 . ? N1 Ag1 N1 110.0(4) 3_535 . ? N1 Ag1 N1 107.1(5) 2_335 . ? O3 Fe1 O3 78.1(2) 5_445 . ? O3 Fe1 O1 96.14(17) 5_445 . ? O3 Fe1 O1 93.53(16) . . ? O3 Fe1 O1 93.53(16) 5_445 2_445 ? O3 Fe1 O1 96.14(17) . 2_445 ? O1 Fe1 O1 167.5(2) . 2_445 ? O3 Fe1 O2 172.05(16) 5_445 2_445 ? O3 Fe1 O2 94.11(15) . 2_445 ? O1 Fe1 O2 85.81(14) . 2_445 ? O1 Fe1 O2 85.69(14) 2_445 2_445 ? O3 Fe1 O2 94.11(15) 5_445 . ? O3 Fe1 O2 172.05(16) . . ? O1 Fe1 O2 85.69(14) . . ? O1 Fe1 O2 85.81(14) 2_445 . ? O2 Fe1 O2 93.7(2) 2_445 . ? C2 O1 Fe1 130.4(3) . . ? C6 N1 Ag1 169.6(8) . . ? C4 O2 Fe1 130.1(3) . . ? O1 C2 C3 123.1(4) . . ? O1 C2 C1 116.6(5) . . ? C3 C2 C1 120.2(6) . . ? C7A O3 C7B 47.6(17) . . ? C7A O3 Fe1 126.5(3) . 5_445 ? C7B O3 Fe1 123.7(7) . 5_445 ? C7A O3 Fe1 126.5(3) . . ? C7B O3 Fe1 123.7(7) . . ? Fe1 O3 Fe1 101.9(2) 5_445 . ? C4 C3 C6 118.4(6) . . ? C4 C3 C2 124.3(5) . . ? C6 C3 C2 117.2(5) . . ? O2 C4 C3 123.6(5) . . ? O2 C4 C5 114.5(4) . . ? C3 C4 C5 121.9(5) . . ? N1 C6 C3 177.5(9) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 33.11 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.190 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.146 #===END data_compound_10_bath151h _database_code_depnum_ccdc_archive 'CCDC 636534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Ag N O2' _chemical_formula_weight 231.99 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 3.7884(2) _cell_length_b 13.4634(6) _cell_length_c 12.8252(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.679(1) _cell_angle_gamma 90.00 _cell_volume 652.80(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3033 _cell_measurement_theta_min 2.875 _cell_measurement_theta_max 30.10 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 3.013 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6751 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8153 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 30.93 _reflns_number_total 2238 _reflns_number_gt 1811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2238 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.10971(5) 0.625515(13) 0.927849(14) 0.02566(7) Uani 1 1 d . . . O1 O -0.4414(4) 0.81102(12) 1.30817(13) 0.0213(3) Uani 1 1 d . . . O2 O 0.0105(5) 0.76063(12) 1.02061(13) 0.0223(3) Uani 1 1 d . . . N1 N -0.1822(6) 0.52735(15) 1.11613(16) 0.0253(4) Uani 1 1 d . . . C1 C -0.4006(5) 0.72603(15) 1.27203(16) 0.0164(4) Uani 1 1 d . . . C2 C -0.2495(6) 0.70858(15) 1.17376(16) 0.0162(4) Uani 1 1 d . . . C3 C -0.1264(6) 0.78262(16) 1.10410(17) 0.0171(4) Uani 1 1 d . . . C4 C -0.5032(6) 0.63631(16) 1.33435(18) 0.0201(4) Uani 1 1 d . . . H4A H -0.6459 0.6576 1.3914 0.030 Uiso 1 1 calc R . . H4B H -0.2892 0.6029 1.3634 0.030 Uiso 1 1 calc R . . H4C H -0.6411 0.5903 1.2886 0.030 Uiso 1 1 calc R . . C5 C -0.1636(6) 0.89077(16) 1.12817(19) 0.0221(4) Uani 1 1 d . . . H5A H -0.0707 0.9303 1.0719 0.033 Uiso 1 1 calc R . . H5B H -0.0305 0.9061 1.1943 0.033 Uiso 1 1 calc R . . H5C H -0.4139 0.9067 1.1341 0.033 Uiso 1 1 calc R . . C6 C -0.2137(6) 0.60867(17) 1.14176(17) 0.0191(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04157(13) 0.01510(9) 0.02162(10) -0.00145(6) 0.01220(7) 0.00293(7) O1 0.0275(8) 0.0167(7) 0.0209(8) -0.0052(6) 0.0108(6) 0.0000(6) O2 0.0335(9) 0.0167(7) 0.0179(7) 0.0005(6) 0.0105(6) 0.0020(6) N1 0.0395(12) 0.0174(9) 0.0204(10) -0.0020(7) 0.0121(8) -0.0006(8) C1 0.0185(10) 0.0155(9) 0.0156(9) -0.0010(7) 0.0048(7) 0.0008(7) C2 0.0210(10) 0.0143(9) 0.0138(9) -0.0007(7) 0.0047(7) 0.0014(7) C3 0.0192(10) 0.0156(9) 0.0167(9) 0.0009(8) 0.0033(7) 0.0028(7) C4 0.0245(11) 0.0180(10) 0.0186(10) 0.0017(8) 0.0059(8) 0.0002(8) C5 0.0301(11) 0.0136(10) 0.0234(11) 0.0001(8) 0.0082(9) -0.0007(8) C6 0.0246(11) 0.0197(10) 0.0135(9) 0.0006(7) 0.0058(8) -0.0008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.156(2) 3_567 ? Ag1 O2 2.2187(16) . ? Ag1 O1 2.5126(15) 4_675 ? O1 C1 1.248(2) . ? O1 Ag1 2.5126(15) 4_476 ? O2 C3 1.255(3) . ? N1 C6 1.152(3) . ? N1 Ag1 2.156(2) 3_567 ? C1 C2 1.437(3) . ? C1 C4 1.513(3) . ? C2 C6 1.415(3) . ? C2 C3 1.436(3) . ? C3 C5 1.497(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 O2 162.10(7) 3_567 . ? N1 Ag1 O1 93.57(6) 3_567 4_675 ? O2 Ag1 O1 101.15(6) . 4_675 ? C1 O1 Ag1 130.06(14) . 4_476 ? C3 O2 Ag1 138.12(15) . . ? C6 N1 Ag1 178.1(2) . 3_567 ? O1 C1 C2 122.8(2) . . ? O1 C1 C4 119.59(19) . . ? C2 C1 C4 117.60(18) . . ? C6 C2 C1 117.43(19) . . ? C6 C2 C3 115.99(19) . . ? C1 C2 C3 126.57(19) . . ? O2 C3 C2 122.38(19) . . ? O2 C3 C5 117.1(2) . . ? C2 C3 C5 120.54(19) . . ? N1 C6 C2 179.5(3) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 30.93 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.111 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.116 #===END