Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 2003-08-24 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_contact_author_name 'Tomoyuki Mochida' _publ_contact_author_address ; Department of Chemistry, Faculty of Science, Toho University, Miyama, Funabashi, Chiba 274-8510, JAPAN ; _publ_contact_author_email mochida@chem.sci.toho-u.ac.jp _publ_contact_author_fax ' +81-47-472-4406' _publ_contact_author_phone ' +81-47-472-4406' _publ_section_title ; Metal complexes from 1,1'-di(pyrazinyl)ferrocene: coordination polymers and bridged diferrocenes ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Tomoyuki Mochida' 'Ryo Horikoshi' 'Kazuya Okazawa' #-----------END data_4 _database_code_depnum_ccdc_archive 'CCDC 212264' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C54 H42 Cu4 Fe3 I4 N12 ' _chemical_formula_moiety 'C54 H42 Cu4 Fe3 I4 N12 ' _chemical_formula_weight 1788.35 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 13.156(7) _cell_length_b 15.380(9) _cell_length_c 7.529(2) _cell_angle_alpha 93.94(3) _cell_angle_beta 101.77(3) _cell_angle_gamma 113.09(5) _cell_volume 1353.1(11) _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description orange _exptl_crystal_colour Plate _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856.00 _exptl_absorpt_coefficient_mu 4.656 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.394 _exptl_absorpt_correction_T_max 0.394 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6475 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0003 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0003 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.87 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6476 _reflns_number_gt 4227 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2191 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 4230 _refine_ls_number_parameters 371 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0103Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0034 _refine_diff_density_max -0.07 _refine_diff_density_min -0.07 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 146(20) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 I(1) I 0.58368(6) 0.47076(6) 0.78464(10) 0.0333(2) Uani 1.00 1 d . . . I(2) I 0.62526(8) 0.36089(6) 1.28843(11) 0.0379(2) Uani 1.00 1 d . . . Cu(1) Cu 0.40903(18) 0.49461(13) 0.6077(3) 0.0587(5) Uani 1.00 1 d . . . Cu(2) Cu 0.47841(14) 0.40224(12) 1.0526(2) 0.0428(4) Uani 1.00 1 d . . . Fe(1) Fe 0.23948(16) 0.01968(12) 0.3720(2) 0.0293(4) Uani 1.00 1 d . . . Fe(2) Fe 0.0000 0.5000 1.0000 0.032 Uani 1.00 2 d R . . N(1) N 0.2744(9) 0.3675(7) 0.5025(13) 0.036(2) Uani 1.00 1 d . . . N(2) N 0.0871(10) 0.1995(8) 0.3103(19) 0.048(3) Uani 1.00 1 d . . . N(3) N 0.3349(8) 0.2851(6) 0.9196(13) 0.031(2) Uani 1.00 1 d . . . N(4) N 0.1405(9) 0.1212(8) 0.7415(15) 0.038(2) Uani 1.00 1 d . . . N(5) N -0.3905(11) 0.2042(9) 0.8409(19) 0.053(3) Uani 1.00 1 d . . . N(6) N -0.1714(10) 0.2476(8) 1.0483(16) 0.046(3) Uani 1.00 1 d . . . C(1) C 0.1957(11) 0.2079(8) 0.3351(16) 0.034(3) Uani 1.00 1 d . . . C(2) C 0.2874(11) 0.2919(8) 0.4312(16) 0.034(3) Uani 1.00 1 d . . . C(3) C 0.1653(12) 0.3591(10) 0.4795(19) 0.041(3) Uani 1.00 1 d . . . C(4) C 0.0755(12) 0.2758(11) 0.385(2) 0.046(4) Uani 1.00 1 d . . . C(5) C 0.2149(11) 0.1271(8) 0.2523(15) 0.034(3) Uani 1.00 1 d . . . C(6) C 0.3185(13) 0.1250(9) 0.2314(18) 0.045(3) Uani 1.00 1 d . . . C(7) C 0.2918(16) 0.0343(11) 0.132(2) 0.053(4) Uani 1.00 1 d . . . C(8) C 0.1700(15) -0.0210(9) 0.0928(18) 0.048(3) Uani 1.00 1 d . . . C(9) C 0.1232(12) 0.0341(9) 0.1666(18) 0.043(3) Uani 1.00 1 d . . . C(10) C 0.2411(9) 0.1259(7) 0.7419(13) 0.027(2) Uani 1.00 1 d . . . C(11) C 0.3417(10) 0.2082(8) 0.8326(14) 0.030(2) Uani 1.00 1 d . . . C(12) C 0.2324(11) 0.2796(10) 0.9186(17) 0.037(3) Uani 1.00 1 d . . . C(13) C 0.1342(11) 0.1982(10) 0.8281(19) 0.043(3) Uani 1.00 1 d . . . C(14) C 0.2487(9) 0.0423(7) 0.6470(15) 0.027(2) Uani 1.00 1 d . . . C(15) C 0.3509(11) 0.0352(9) 0.6189(17) 0.036(3) Uani 1.00 1 d . . . C(16) C 0.3177(13) -0.0571(9) 0.5125(18) 0.043(3) Uani 1.00 1 d . . . C(17) C 0.1936(12) -0.1061(9) 0.4746(18) 0.040(3) Uani 1.00 1 d . . . C(18) C 0.1532(11) -0.0446(7) 0.5546(17) 0.035(3) Uani 1.00 1 d . . . C(19) C -0.1888(11) 0.2912(9) 0.9056(17) 0.037(3) Uani 1.00 1 d . . . C(20) C -0.3011(12) 0.2682(10) 0.799(2) 0.047(3) Uani 1.00 1 d . . . C(21) C -0.3727(14) 0.1643(10) 0.982(2) 0.053(4) Uani 1.00 1 d . . . C(22) C -0.2609(15) 0.1858(11) 1.089(2) 0.057(4) Uani 1.00 1 d . . . C(23) C -0.0862(12) 0.3633(8) 0.8621(17) 0.038(3) Uani 1.00 1 d . . . C(24) C 0.0289(11) 0.3798(10) 0.943(2) 0.043(3) Uani 1.00 1 d . . . C(25) C 0.1003(12) 0.4571(12) 0.8699(19) 0.048(4) Uani 1.00 1 d . . . C(26) C 0.0302(13) 0.4872(11) 0.7454(18) 0.048(4) Uani 1.00 1 d . . . C(27) C -0.0879(13) 0.4304(10) 0.7370(17) 0.045(3) Uani 1.00 1 d . . . H(2) H 0.3623 0.2955 0.4465 17.962 Uiso 1.00 1 c R . . H(3) H 0.1513 0.4109 0.5285 0.039 Uiso 1.00 1 c R . . H(4) H 0.0003 0.2719 0.3725 0.050 Uiso 1.00 1 c R . . H(6) H 0.3925 0.1756 0.2754 0.122 Uiso 1.00 1 c R . . H(7) H 0.3451 0.0130 0.0986 0.058 Uiso 1.00 1 c R . . H(8) H 0.1295 -0.0851 0.0293 0.091 Uiso 1.00 1 c R . . H(9) H 0.0446 0.0152 0.1607 0.044 Uiso 1.00 1 c R . . H(11) H 0.4145 0.2092 0.8324 0.075 Uiso 1.00 1 c R . . H(12) H 0.2250 0.3319 0.9804 0.001 Uiso 1.00 1 c R . . H(13) H 0.0614 0.1970 0.8278 0.070 Uiso 1.00 1 c R . . H(15) H 0.4266 0.0834 0.6620 0.036 Uiso 1.00 1 c R . . H(16) H 0.3669 -0.0814 0.4726 0.050 Uiso 1.00 1 c R . . H(17) H 0.1475 -0.1683 0.4049 0.126 Uiso 1.00 1 c R . . H(18) H 0.0754 -0.0588 0.5490 0.140 Uiso 1.00 1 c R . . H(20) H -0.3119 0.2991 0.6962 0.054 Uiso 1.00 1 c R . . H(21) H -0.4363 0.1191 1.0161 0.181 Uiso 1.00 1 c R . . H(22) H -0.2514 0.1545 1.1914 0.068 Uiso 1.00 1 c R . . H(24) H 0.0536 0.3459 1.0307 0.021 Uiso 1.00 1 c R . . H(25) H 0.1815 0.4844 0.9012 -0.003 Uiso 1.00 1 c R . . H(26) H 0.0574 0.5385 0.6798 0.070 Uiso 1.00 1 c R . . H(27) H -0.1528 0.4347 0.6626 0.011 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0452(5) 0.0373(4) 0.0233(4) 0.0203(3) 0.0141(3) 0.0076(2) I(2) 0.0525(5) 0.0384(4) 0.0288(4) 0.0254(3) 0.0100(3) 0.0044(3) Cu(1) 0.0558(12) 0.0408(9) 0.0678(13) 0.0218(9) -0.0055(10) -0.0129(9) Cu(2) 0.0429(9) 0.0411(9) 0.0360(8) 0.0122(7) 0.0060(7) -0.0036(7) Fe(1) 0.0421(10) 0.0235(7) 0.0204(7) 0.0111(7) 0.0092(6) 0.0041(5) Fe(2) 0.0347(13) 0.0382(13) 0.0228(11) 0.0141(10) 0.0088(9) 0.0072(9) N(1) 0.053(6) 0.026(4) 0.023(4) 0.014(4) 0.006(4) 0.003(3) N(2) 0.047(6) 0.032(5) 0.056(7) 0.012(5) 0.004(5) 0.004(5) N(3) 0.041(5) 0.024(4) 0.022(4) 0.003(4) 0.012(4) 0.006(3) N(4) 0.044(6) 0.043(6) 0.029(5) 0.018(5) 0.013(4) 0.003(4) N(5) 0.047(7) 0.054(7) 0.057(8) 0.021(6) 0.011(6) 0.009(6) N(6) 0.049(7) 0.050(6) 0.041(6) 0.023(5) 0.008(5) 0.018(5) C(1) 0.041(6) 0.033(6) 0.027(5) 0.013(5) 0.012(5) 0.010(4) C(2) 0.045(7) 0.034(6) 0.027(5) 0.019(5) 0.012(5) 0.012(4) C(3) 0.045(7) 0.051(7) 0.036(6) 0.027(6) 0.013(5) 0.014(5) C(4) 0.040(7) 0.053(8) 0.048(8) 0.019(6) 0.013(6) 0.011(6) C(5) 0.047(7) 0.032(6) 0.017(4) 0.010(5) 0.008(4) 0.003(4) C(6) 0.068(9) 0.029(6) 0.035(6) 0.009(6) 0.026(6) 0.010(5) C(7) 0.094(12) 0.054(8) 0.037(7) 0.046(8) 0.037(8) 0.019(6) C(8) 0.082(10) 0.023(5) 0.027(6) 0.011(6) 0.010(6) -0.001(4) C(9) 0.050(8) 0.032(6) 0.029(6) 0.004(5) -0.004(5) 0.007(5) C(10) 0.035(6) 0.017(4) 0.013(4) -0.003(4) 0.004(4) -0.001(3) C(11) 0.035(6) 0.036(6) 0.016(4) 0.014(5) 0.002(4) 0.004(4) C(12) 0.044(7) 0.048(7) 0.028(5) 0.028(6) 0.009(5) 0.001(5) C(13) 0.044(7) 0.054(8) 0.041(7) 0.025(6) 0.019(6) 0.005(6) C(14) 0.031(5) 0.026(5) 0.026(5) 0.009(4) 0.010(4) 0.009(4) C(15) 0.043(7) 0.040(6) 0.034(6) 0.025(5) 0.009(5) 0.008(5) C(16) 0.068(9) 0.036(6) 0.033(6) 0.030(6) 0.009(6) 0.010(5) C(17) 0.058(8) 0.032(6) 0.034(6) 0.017(5) 0.019(6) 0.018(5) C(18) 0.039(6) 0.015(4) 0.033(6) -0.006(4) 0.006(5) -0.001(4) C(19) 0.046(7) 0.043(7) 0.027(5) 0.027(5) 0.005(5) -0.002(5) C(20) 0.039(7) 0.048(8) 0.048(8) 0.018(6) 0.000(6) 0.003(6) C(21) 0.056(9) 0.030(6) 0.066(10) 0.010(6) 0.021(8) 0.004(6) C(22) 0.071(10) 0.046(8) 0.053(9) 0.026(7) 0.010(8) 0.014(7) C(23) 0.057(8) 0.028(5) 0.029(5) 0.016(5) 0.014(5) 0.004(4) C(24) 0.040(7) 0.049(7) 0.045(7) 0.021(6) 0.015(6) 0.012(6) C(25) 0.045(8) 0.070(10) 0.034(7) 0.026(7) 0.017(6) 0.003(6) C(26) 0.066(9) 0.048(8) 0.028(6) 0.017(7) 0.024(6) -0.002(5) C(27) 0.066(9) 0.046(7) 0.023(5) 0.019(6) 0.017(6) 0.014(5) #============================================================================== _computing_data_collection Unknown _computing_cell_refinement Unknown _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Cu(1) 2.582(2) ? . . I(2) Cu(2) 2.648(2) ? . . Cu(1) N(1) 2.021(8) ? . . Fe(1) C(5) 2.037(14) ? . . Fe(1) C(6) 2.046(14) ? . . Fe(1) C(7) 2.058(17) ? . . Fe(1) C(8) 2.057(12) ? . . Fe(1) C(9) 2.032(14) ? . . Fe(1) C(14) 2.047(11) ? . . Fe(1) C(15) 2.053(13) ? . . Fe(1) C(16) 2.062(17) ? . . Fe(1) C(17) 2.046(14) ? . . Fe(1) C(18) 2.025(13) ? . . Fe(2) C(23) 2.034(11) ? . . Fe(2) C(23) 2.034(11) ? . 56702 Fe(2) C(24) 2.062(18) ? . . Fe(2) C(24) 2.062(18) ? . 56702 Fe(2) C(25) 2.063(19) ? . . Fe(2) C(25) 2.063(19) ? . 56702 Fe(2) C(26) 2.047(15) ? . . Fe(2) C(26) 2.047(15) ? . 56702 Fe(2) C(27) 2.051(11) ? . . Fe(2) C(27) 2.051(11) ? . 56702 N(1) C(2) 1.333(19) ? . . N(1) C(3) 1.36(2) ? . . N(2) C(1) 1.36(2) ? . . N(2) C(4) 1.34(2) ? . . N(3) C(11) 1.356(18) ? . . N(3) C(12) 1.32(2) ? . . N(4) C(10) 1.296(19) ? . . N(4) C(13) 1.35(2) ? . . N(5) C(20) 1.318(19) ? . . N(5) C(21) 1.29(2) ? . . N(6) C(19) 1.334(19) ? . . N(6) C(22) 1.30(2) ? . . C(1) C(2) 1.394(14) ? . . C(1) C(5) 1.48(2) ? . . C(3) C(4) 1.373(16) ? . . C(5) C(6) 1.42(2) ? . . C(5) C(9) 1.456(15) ? . . C(6) C(7) 1.41(2) ? . . C(7) C(8) 1.44(2) ? . . C(8) C(9) 1.37(2) ? . . C(10) C(11) 1.421(12) ? . . C(10) C(14) 1.475(18) ? . . C(12) C(13) 1.398(16) ? . . C(14) C(15) 1.45(2) ? . . C(14) C(18) 1.431(13) ? . . C(15) C(16) 1.436(19) ? . . C(16) C(17) 1.46(2) ? . . C(17) C(18) 1.41(2) ? . . C(19) C(20) 1.42(2) ? . . C(19) C(23) 1.488(18) ? . . C(21) C(22) 1.42(2) ? . . C(23) C(24) 1.43(2) ? . . C(23) C(27) 1.45(2) ? . . C(24) C(25) 1.42(2) ? . . C(25) C(26) 1.41(2) ? . . C(26) C(27) 1.44(2) ? . . C(2) H(2) 0.948(15) ? . . C(3) H(3) 0.952(17) ? . . C(4) H(4) 0.951(17) ? . . C(6) H(6) 0.950(12) ? . . C(7) H(7) 0.95(2) ? . . C(8) H(8) 0.950(11) ? . . C(9) H(9) 0.948(15) ? . . C(11) H(11) 0.951(14) ? . . C(12) H(12) 0.950(16) ? . . C(13) H(13) 0.951(17) ? . . C(15) H(15) 0.951(11) ? . . C(16) H(16) 0.950(19) ? . . C(17) H(17) 0.951(11) ? . . C(18) H(18) 0.950(14) ? . . C(20) H(20) 0.95(2) ? . . C(21) H(21) 0.950(16) ? . . C(22) H(22) 0.95(2) ? . . C(24) H(24) 0.951(16) ? . . C(25) H(25) 0.951(14) ? . . C(26) H(26) 0.949(15) ? . . C(27) H(27) 0.950(17) ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) I(1) Cu(2) 91.81(7) ? . . . Cu(1) I(1) Cu(2) 61.45(6) ? . . 66702 Cu(2) I(1) Cu(2) 67.87(6) ? . . 66702 Cu(1) I(2) Cu(2) 62.79(6) ? 66702 . . I(1) Cu(1) I(2) 120.27(7) ? . . 66702 I(1) Cu(1) Cu(2) 61.50(6) ? . . 66702 I(1) Cu(1) N(1) 111.2(3) ? . . . I(2) Cu(1) Cu(2) 60.57(7) ? 66702 . 66702 I(2) Cu(1) N(1) 119.6(4) ? 66702 . . Cu(2) Cu(1) N(1) 135.8(3) ? 66702 . . I(1) Cu(2) I(1) 112.13(7) ? . . 66702 I(1) Cu(2) I(2) 105.75(7) ? . . . I(1) Cu(2) Cu(1) 114.02(7) ? . . 66702 I(1) Cu(2) N(3) 104.8(3) ? . . . I(1) Cu(2) I(2) 112.15(6) ? 66702 . . I(1) Cu(2) Cu(1) 57.05(6) ? 66702 . 66702 I(1) Cu(2) N(3) 108.5(3) ? 66702 . . I(2) Cu(2) Cu(1) 56.64(6) ? . . 66702 I(2) Cu(2) N(3) 113.3(3) ? . . . Cu(1) Cu(2) N(3) 141.2(3) ? 66702 . . C(5) Fe(1) C(6) 40.6(6) ? . . . C(5) Fe(1) C(7) 67.8(7) ? . . . C(5) Fe(1) C(8) 68.1(5) ? . . . C(5) Fe(1) C(9) 41.9(4) ? . . . C(5) Fe(1) C(14) 109.9(5) ? . . . C(5) Fe(1) C(15) 126.3(4) ? . . . C(5) Fe(1) C(16) 161.6(5) ? . . . C(5) Fe(1) C(17) 156.4(6) ? . . . C(5) Fe(1) C(18) 122.7(6) ? . . . C(6) Fe(1) C(7) 40.3(6) ? . . . C(6) Fe(1) C(8) 68.6(5) ? . . . C(6) Fe(1) C(9) 69.3(5) ? . . . C(6) Fe(1) C(14) 123.9(4) ? . . . C(6) Fe(1) C(15) 108.8(5) ? . . . C(6) Fe(1) C(16) 123.7(6) ? . . . C(6) Fe(1) C(17) 159.8(7) ? . . . C(6) Fe(1) C(18) 159.2(6) ? . . . C(7) Fe(1) C(8) 41.0(6) ? . . . C(7) Fe(1) C(9) 67.9(7) ? . . . C(7) Fe(1) C(14) 158.6(5) ? . . . C(7) Fe(1) C(15) 121.6(6) ? . . . C(7) Fe(1) C(16) 106.1(7) ? . . . C(7) Fe(1) C(17) 122.4(6) ? . . . C(7) Fe(1) C(18) 158.5(4) ? . . . C(8) Fe(1) C(9) 39.3(7) ? . . . C(8) Fe(1) C(14) 159.7(6) ? . . . C(8) Fe(1) C(15) 156.1(7) ? . . . C(8) Fe(1) C(16) 119.4(6) ? . . . C(8) Fe(1) C(17) 104.7(5) ? . . . C(8) Fe(1) C(18) 121.6(5) ? . . . C(9) Fe(1) C(14) 125.6(6) ? . . . C(9) Fe(1) C(15) 164.0(6) ? . . . C(9) Fe(1) C(16) 153.7(4) ? . . . C(9) Fe(1) C(17) 118.4(5) ? . . . C(9) Fe(1) C(18) 106.4(5) ? . . . C(14) Fe(1) C(15) 41.3(6) ? . . . C(14) Fe(1) C(16) 69.1(6) ? . . . C(14) Fe(1) C(17) 68.7(5) ? . . . C(14) Fe(1) C(18) 41.1(3) ? . . . C(15) Fe(1) C(16) 40.8(5) ? . . . C(15) Fe(1) C(17) 69.2(4) ? . . . C(15) Fe(1) C(18) 69.5(5) ? . . . C(16) Fe(1) C(17) 41.6(6) ? . . . C(16) Fe(1) C(18) 69.4(6) ? . . . C(17) Fe(1) C(18) 40.5(6) ? . . . C(23) Fe(2) C(23) 180.0(8) ? . . 56702 C(23) Fe(2) C(24) 40.7(5) ? . . . C(23) Fe(2) C(24) 139.3(5) ? . . 56702 C(23) Fe(2) C(25) 68.1(6) ? . . . C(23) Fe(2) C(25) 111.9(6) ? . . 56702 C(23) Fe(2) C(26) 68.2(5) ? . . . C(23) Fe(2) C(26) 111.8(5) ? . . 56702 C(23) Fe(2) C(27) 41.5(5) ? . . . C(23) Fe(2) C(27) 138.5(5) ? . . 56702 C(23) Fe(2) C(24) 139.3(5) ? 56702 . . C(23) Fe(2) C(24) 40.7(5) ? 56702 . 56702 C(23) Fe(2) C(25) 111.9(6) ? 56702 . . C(23) Fe(2) C(25) 68.1(6) ? 56702 . 56702 C(23) Fe(2) C(26) 111.8(5) ? 56702 . . C(23) Fe(2) C(26) 68.2(5) ? 56702 . 56702 C(23) Fe(2) C(27) 138.5(5) ? 56702 . . C(23) Fe(2) C(27) 41.5(5) ? 56702 . 56702 C(24) Fe(2) C(24) 180.0(8) ? . . 56702 C(24) Fe(2) C(25) 40.4(6) ? . . . C(24) Fe(2) C(25) 139.6(6) ? . . 56702 C(24) Fe(2) C(26) 67.9(6) ? . . . C(24) Fe(2) C(26) 112.1(6) ? . . 56702 C(24) Fe(2) C(27) 69.6(6) ? . . . C(24) Fe(2) C(27) 110.4(6) ? . . 56702 C(24) Fe(2) C(25) 139.6(6) ? 56702 . . C(24) Fe(2) C(25) 40.4(6) ? 56702 . 56702 C(24) Fe(2) C(26) 112.1(6) ? 56702 . . C(24) Fe(2) C(26) 67.9(6) ? 56702 . 56702 C(24) Fe(2) C(27) 110.4(6) ? 56702 . . C(24) Fe(2) C(27) 69.6(6) ? 56702 . 56702 C(25) Fe(2) C(25) 180.0(8) ? . . 56702 C(25) Fe(2) C(26) 40.1(7) ? . . . C(25) Fe(2) C(26) 139.9(7) ? . . 56702 C(25) Fe(2) C(27) 69.0(6) ? . . . C(25) Fe(2) C(27) 111.0(6) ? . . 56702 C(25) Fe(2) C(26) 139.9(7) ? 56702 . . C(25) Fe(2) C(26) 40.1(7) ? 56702 . 56702 C(25) Fe(2) C(27) 111.0(6) ? 56702 . . C(25) Fe(2) C(27) 69.0(6) ? 56702 . 56702 C(26) Fe(2) C(26) 180.0(9) ? . . 56702 C(26) Fe(2) C(27) 41.1(6) ? . . . C(26) Fe(2) C(27) 138.9(6) ? . . 56702 C(26) Fe(2) C(27) 138.9(6) ? 56702 . . C(26) Fe(2) C(27) 41.1(6) ? 56702 . 56702 C(27) Fe(2) C(27) 180.0(9) ? . . 56702 Cu(1) N(1) C(2) 121.7(9) ? . . . Cu(1) N(1) C(3) 121.0(9) ? . . . C(2) N(1) C(3) 116.7(10) ? . . . C(1) N(2) C(4) 115.7(10) ? . . . Cu(2) N(3) C(11) 120.8(8) ? . . . Cu(2) N(3) C(12) 121.7(9) ? . . . C(11) N(3) C(12) 117.5(9) ? . . . C(10) N(4) C(13) 117.6(9) ? . . . C(20) N(5) C(21) 118.0(14) ? . . . C(19) N(6) C(22) 117.4(13) ? . . . N(2) C(1) C(2) 120.6(14) ? . . . N(2) C(1) C(5) 118.6(9) ? . . . C(2) C(1) C(5) 120.8(13) ? . . . N(1) C(2) C(1) 122.9(13) ? . . . N(1) C(3) C(4) 119.9(15) ? . . . N(2) C(4) C(3) 124.1(15) ? . . . Fe(1) C(5) C(1) 128.8(8) ? . . . Fe(1) C(5) C(6) 70.0(8) ? . . . Fe(1) C(5) C(9) 68.8(8) ? . . . C(1) C(5) C(6) 128.9(10) ? . . . C(1) C(5) C(9) 123.5(13) ? . . . C(6) C(5) C(9) 107.6(13) ? . . . Fe(1) C(6) C(5) 69.4(8) ? . . . Fe(1) C(6) C(7) 70.3(8) ? . . . C(5) C(6) C(7) 107.7(12) ? . . . Fe(1) C(7) C(6) 69.4(9) ? . . . Fe(1) C(7) C(8) 69.5(9) ? . . . C(6) C(7) C(8) 108.2(18) ? . . . Fe(1) C(8) C(7) 69.5(8) ? . . . Fe(1) C(8) C(9) 69.4(7) ? . . . C(7) C(8) C(9) 108.3(12) ? . . . Fe(1) C(9) C(5) 69.2(7) ? . . . Fe(1) C(9) C(8) 71.4(9) ? . . . C(5) C(9) C(8) 108.2(13) ? . . . N(4) C(10) C(11) 121.5(12) ? . . . N(4) C(10) C(14) 118.0(8) ? . . . C(11) C(10) C(14) 120.5(12) ? . . . N(3) C(11) C(10) 120.6(12) ? . . . N(3) C(12) C(13) 121.2(14) ? . . . N(4) C(13) C(12) 121.5(15) ? . . . Fe(1) C(14) C(10) 124.1(8) ? . . . Fe(1) C(14) C(15) 69.5(7) ? . . . Fe(1) C(14) C(18) 68.6(7) ? . . . C(10) C(14) C(15) 127.0(9) ? . . . C(10) C(14) C(18) 125.1(12) ? . . . C(15) C(14) C(18) 107.8(11) ? . . . Fe(1) C(15) C(14) 69.1(7) ? . . . Fe(1) C(15) C(16) 69.9(7) ? . . . C(14) C(15) C(16) 108.0(10) ? . . . Fe(1) C(16) C(15) 69.2(9) ? . . . Fe(1) C(16) C(17) 68.6(9) ? . . . C(15) C(16) C(17) 107.0(15) ? . . . Fe(1) C(17) C(16) 69.8(8) ? . . . Fe(1) C(17) C(18) 68.9(7) ? . . . C(16) C(17) C(18) 108.4(10) ? . . . Fe(1) C(18) C(14) 70.3(7) ? . . . Fe(1) C(18) C(17) 70.5(8) ? . . . C(14) C(18) C(17) 108.8(12) ? . . . N(6) C(19) C(20) 120.8(12) ? . . . N(6) C(19) C(23) 117.2(12) ? . . . C(20) C(19) C(23) 122.0(13) ? . . . N(5) C(20) C(19) 120.6(15) ? . . . N(5) C(21) C(22) 122.0(15) ? . . . N(6) C(22) C(21) 121.1(16) ? . . . Fe(2) C(23) C(19) 123.6(11) ? . . . Fe(2) C(23) C(24) 70.7(7) ? . . . Fe(2) C(23) C(27) 69.9(6) ? . . . C(19) C(23) C(24) 125.3(13) ? . . . C(19) C(23) C(27) 125.1(14) ? . . . C(24) C(23) C(27) 109.5(12) ? . . . Fe(2) C(24) C(23) 68.6(9) ? . . . Fe(2) C(24) C(25) 69.8(10) ? . . . C(23) C(24) C(25) 107.2(13) ? . . . Fe(2) C(25) C(24) 69.8(10) ? . . . Fe(2) C(25) C(26) 69.4(10) ? . . . C(24) C(25) C(26) 108.3(13) ? . . . Fe(2) C(26) C(25) 70.6(9) ? . . . Fe(2) C(26) C(27) 69.6(8) ? . . . C(25) C(26) C(27) 110.0(13) ? . . . Fe(2) C(27) C(23) 68.6(6) ? . . . Fe(2) C(27) C(26) 69.3(7) ? . . . C(23) C(27) C(26) 104.9(14) ? . . . N(1) C(2) H(2) 118.6(10) ? . . . C(1) C(2) H(2) 118.5(14) ? . . . N(1) C(3) H(3) 120.0(10) ? . . . C(4) C(3) H(3) 120.0(16) ? . . . N(2) C(4) H(4) 117.9(12) ? . . . C(3) C(4) H(4) 118.0(17) ? . . . Fe(1) C(6) H(6) 126.1(11) ? . . . C(5) C(6) H(6) 126.2(15) ? . . . C(7) C(6) H(6) 126(2) ? . . . Fe(1) C(7) H(7) 125.8(14) ? . . . C(6) C(7) H(7) 125.8(15) ? . . . C(8) C(7) H(7) 126.0(15) ? . . . Fe(1) C(8) H(8) 125.8(11) ? . . . C(7) C(8) H(8) 126(2) ? . . . C(9) C(8) H(8) 126.0(17) ? . . . Fe(1) C(9) H(9) 125.9(11) ? . . . C(5) C(9) H(9) 125.9(16) ? . . . C(8) C(9) H(9) 125.9(12) ? . . . N(3) C(11) H(11) 119.7(9) ? . . . C(10) C(11) H(11) 119.7(13) ? . . . N(3) C(12) H(12) 119.4(10) ? . . . C(13) C(12) H(12) 119.4(15) ? . . . N(4) C(13) H(13) 119.2(11) ? . . . C(12) C(13) H(13) 119.2(16) ? . . . Fe(1) C(15) H(15) 126.0(11) ? . . . C(14) C(15) H(15) 126.0(14) ? . . . C(16) C(15) H(15) 126.0(17) ? . . . Fe(1) C(16) H(16) 126.5(11) ? . . . C(15) C(16) H(16) 126.6(13) ? . . . C(17) C(16) H(16) 126.4(12) ? . . . Fe(1) C(17) H(17) 125.7(11) ? . . . C(16) C(17) H(17) 125.9(17) ? . . . C(18) C(17) H(17) 125.7(15) ? . . . Fe(1) C(18) H(18) 125.6(10) ? . . . C(14) C(18) H(18) 125.6(13) ? . . . C(17) C(18) H(18) 125.6(10) ? . . . N(5) C(20) H(20) 119.7(16) ? . . . C(19) C(20) H(20) 119.7(15) ? . . . N(5) C(21) H(21) 119.1(16) ? . . . C(22) C(21) H(21) 118.9(17) ? . . . N(6) C(22) H(22) 119(2) ? . . . C(21) C(22) H(22) 119.5(19) ? . . . Fe(2) C(24) H(24) 126.5(12) ? . . . C(23) C(24) H(24) 126.5(13) ? . . . C(25) C(24) H(24) 126.3(14) ? . . . Fe(2) C(25) H(25) 125.9(12) ? . . . C(24) C(25) H(25) 125.7(17) ? . . . C(26) C(25) H(25) 125.9(16) ? . . . Fe(2) C(26) H(26) 125.0(13) ? . . . C(25) C(26) H(26) 124.7(15) ? . . . C(27) C(26) H(26) 125.3(17) ? . . . Fe(2) C(27) H(27) 127.6(14) ? . . . C(23) C(27) H(27) 127.6(14) ? . . . C(26) C(27) H(27) 127.5(14) ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cu(1) I(1) Cu(2) I(1) -58.06(7) ? . . . 66702 Cu(1) I(1) Cu(2) I(2) 179.42(6) ? . . . . Cu(1) I(1) Cu(2) N(3) 59.4(3) ? . . . . Cu(1) I(1) Cu(2) Cu(1) -120.57(10) ? . . . 66702 Cu(2) I(1) Cu(1) N(1) -68.2(3) ? . . . . Cu(2) I(1) Cu(1) I(2) 78.90(10) ? . . . 66702 Cu(2) I(1) Cu(1) Cu(2) 63.50(6) ? . . . 66702 Cu(1) I(1) Cu(2) I(1) 105.07(8) ? . . 66702 66702 Cu(1) I(1) Cu(2) I(2) -13.74(6) ? . . 66702 66702 Cu(1) I(1) Cu(2) N(3) -139.7(3) ? . . 66702 66702 Cu(2) I(1) Cu(1) N(1) -131.7(3) ? 66702 . . . Cu(2) I(1) Cu(1) I(2) 15.40(8) ? 66702 . . 66702 Cu(2) I(1) Cu(2) I(2) -118.81(7) ? . . 66702 66702 Cu(2) I(1) Cu(2) N(3) 115.2(3) ? . . 66702 66702 Cu(2) I(1) Cu(2) Cu(1) -105.07(7) ? . . 66702 . Cu(2) I(1) Cu(2) I(2) -122.52(6) ? 66702 . . . Cu(2) I(1) Cu(2) N(3) 117.5(3) ? 66702 . . . Cu(2) I(1) Cu(2) Cu(1) -62.50(9) ? 66702 . . 66702 Cu(1) I(2) Cu(2) I(1) 108.70(7) ? 66702 . . . Cu(1) I(2) Cu(2) I(1) -13.81(7) ? 66702 . . 66702 Cu(1) I(2) Cu(2) N(3) -137.1(3) ? 66702 . . . Cu(2) I(2) Cu(1) I(1) 15.55(8) ? . . 66702 66702 Cu(2) I(2) Cu(1) N(1) -128.8(3) ? . . 66702 66702 I(1) Cu(1) Cu(2) I(1) -101.69(9) ? . . 66702 66702 I(1) Cu(1) Cu(2) I(2) 164.73(7) ? . . 66702 66702 I(1) Cu(1) Cu(2) N(3) 78.3(6) ? . . 66702 66702 I(1) Cu(1) N(1) C(2) -38.7(10) ? . . . . I(1) Cu(1) N(1) C(3) 150.0(9) ? . . . . I(2) Cu(1) Cu(2) I(1) -164.73(7) ? 66702 . 66702 . I(2) Cu(1) Cu(2) I(1) 93.58(9) ? 66702 . 66702 66702 I(2) Cu(1) Cu(2) N(3) -86.4(6) ? 66702 . 66702 66702 I(2) Cu(1) N(1) C(2) 174.0(8) ? 66702 . . . I(2) Cu(1) N(1) C(3) 2.7(11) ? 66702 . . . Cu(2) Cu(1) N(1) C(2) -109.1(9) ? 66702 . . . Cu(2) Cu(1) N(1) C(3) 79.6(11) ? 66702 . . . N(1) Cu(1) Cu(2) I(1) 91.9(6) ? . . 66702 . N(1) Cu(1) Cu(2) I(1) -9.8(6) ? . . 66702 66702 N(1) Cu(1) Cu(2) I(2) -103.4(6) ? . . 66702 66702 N(1) Cu(1) Cu(2) N(3) 170.1(8) ? . . 66702 66702 I(1) Cu(2) N(3) C(11) 63.0(9) ? . . . . I(1) Cu(2) N(3) C(12) -118.9(9) ? . . . . I(1) Cu(2) N(3) C(11) -177.1(8) ? 66702 . . . I(1) Cu(2) N(3) C(12) 1.0(10) ? 66702 . . . I(2) Cu(2) N(3) C(11) -51.8(9) ? . . . . I(2) Cu(2) N(3) C(12) 126.3(9) ? . . . . Cu(1) Cu(2) N(3) C(11) -117.0(8) ? 66702 . . . Cu(1) Cu(2) N(3) C(12) 61.1(12) ? 66702 . . . C(5) Fe(1) C(6) C(7) -118.6(12) ? . . . . C(6) Fe(1) C(5) C(1) -124.4(13) ? . . . . C(6) Fe(1) C(5) C(9) 119.0(11) ? . . . . C(5) Fe(1) C(7) C(6) 38.1(9) ? . . . . C(5) Fe(1) C(7) C(8) -81.7(10) ? . . . . C(7) Fe(1) C(5) C(1) -162.2(12) ? . . . . C(7) Fe(1) C(5) C(6) -37.8(7) ? . . . . C(7) Fe(1) C(5) C(9) 81.2(9) ? . . . . C(5) Fe(1) C(8) C(7) 80.8(10) ? . . . . C(5) Fe(1) C(8) C(9) -39.2(8) ? . . . . C(8) Fe(1) C(5) C(1) 153.3(13) ? . . . . C(8) Fe(1) C(5) C(6) -82.3(8) ? . . . . C(8) Fe(1) C(5) C(9) 36.8(9) ? . . . . C(5) Fe(1) C(9) C(8) 118.7(12) ? . . . . C(9) Fe(1) C(5) C(1) 116.6(15) ? . . . . C(9) Fe(1) C(5) C(6) -119.0(11) ? . . . . C(5) Fe(1) C(14) C(10) -1.3(10) ? . . . . C(5) Fe(1) C(14) C(15) -122.9(7) ? . . . . C(5) Fe(1) C(14) C(18) 117.4(8) ? . . . . C(14) Fe(1) C(5) C(1) -5.0(12) ? . . . . C(14) Fe(1) C(5) C(6) 119.4(7) ? . . . . C(14) Fe(1) C(5) C(9) -121.6(8) ? . . . . C(5) Fe(1) C(15) C(14) 78.7(8) ? . . . . C(5) Fe(1) C(15) C(16) -161.9(9) ? . . . . C(15) Fe(1) C(5) C(1) -48.5(14) ? . . . . C(15) Fe(1) C(5) C(6) 75.9(9) ? . . . . C(15) Fe(1) C(5) C(9) -165.1(9) ? . . . . C(5) Fe(1) C(16) C(15) 52(2) ? . . . . C(5) Fe(1) C(16) C(17) 171.4(16) ? . . . . C(16) Fe(1) C(5) C(1) -89(2) ? . . . . C(16) Fe(1) C(5) C(6) 36(2) ? . . . . C(16) Fe(1) C(5) C(9) 154.8(17) ? . . . . C(5) Fe(1) C(17) C(16) -173.3(11) ? . . . . C(5) Fe(1) C(17) C(18) -53.1(14) ? . . . . C(17) Fe(1) C(5) C(1) 77.1(15) ? . . . . C(17) Fe(1) C(5) C(6) -158.5(12) ? . . . . C(17) Fe(1) C(5) C(9) -39.5(17) ? . . . . C(5) Fe(1) C(18) C(14) -83.0(9) ? . . . . C(5) Fe(1) C(18) C(17) 157.7(6) ? . . . . C(18) Fe(1) C(5) C(1) 39.0(12) ? . . . . C(18) Fe(1) C(5) C(6) 163.4(6) ? . . . . C(18) Fe(1) C(5) C(9) -77.6(9) ? . . . . C(6) Fe(1) C(7) C(8) -119.8(16) ? . . . . C(7) Fe(1) C(6) C(5) 118.6(12) ? . . . . C(6) Fe(1) C(8) C(7) 37.0(11) ? . . . . C(6) Fe(1) C(8) C(9) -83.0(9) ? . . . . C(8) Fe(1) C(6) C(5) 80.9(8) ? . . . . C(8) Fe(1) C(6) C(7) -37.7(11) ? . . . . C(6) Fe(1) C(9) C(5) -37.4(8) ? . . . . C(6) Fe(1) C(9) C(8) 81.3(9) ? . . . . C(9) Fe(1) C(6) C(5) 38.7(7) ? . . . . C(9) Fe(1) C(6) C(7) -79.9(11) ? . . . . C(6) Fe(1) C(14) C(10) 41.7(12) ? . . . . C(6) Fe(1) C(14) C(15) -79.8(10) ? . . . . C(6) Fe(1) C(14) C(18) 160.5(9) ? . . . . C(14) Fe(1) C(6) C(5) -81.0(8) ? . . . . C(14) Fe(1) C(6) C(7) 160.4(10) ? . . . . C(6) Fe(1) C(15) C(14) 120.4(8) ? . . . . C(6) Fe(1) C(15) C(16) -120.2(9) ? . . . . C(15) Fe(1) C(6) C(5) -124.4(7) ? . . . . C(15) Fe(1) C(6) C(7) 117.0(11) ? . . . . C(6) Fe(1) C(16) C(15) 79.7(10) ? . . . . C(6) Fe(1) C(16) C(17) -161.3(8) ? . . . . C(16) Fe(1) C(6) C(5) -167.2(6) ? . . . . C(16) Fe(1) C(6) C(7) 74.2(11) ? . . . . C(6) Fe(1) C(17) C(16) 50.3(16) ? . . . . C(6) Fe(1) C(17) C(18) 170.5(12) ? . . . . C(17) Fe(1) C(6) C(5) 154.9(13) ? . . . . C(17) Fe(1) C(6) C(7) 36.3(19) ? . . . . C(6) Fe(1) C(18) C(14) -51.4(19) ? . . . . C(6) Fe(1) C(18) C(17) -170.7(14) ? . . . . C(18) Fe(1) C(6) C(5) -42.7(17) ? . . . . C(18) Fe(1) C(6) C(7) -161.3(14) ? . . . . C(7) Fe(1) C(8) C(9) -120.0(12) ? . . . . C(8) Fe(1) C(7) C(6) 119.8(16) ? . . . . C(7) Fe(1) C(9) C(5) -80.8(9) ? . . . . C(7) Fe(1) C(9) C(8) 37.9(8) ? . . . . C(9) Fe(1) C(7) C(6) 83.5(11) ? . . . . C(9) Fe(1) C(7) C(8) -36.3(9) ? . . . . C(7) Fe(1) C(14) C(10) 78(2) ? . . . . C(7) Fe(1) C(14) C(15) -43(2) ? . . . . C(7) Fe(1) C(14) C(18) -162.9(18) ? . . . . C(14) Fe(1) C(7) C(6) -50(2) ? . . . . C(14) Fe(1) C(7) C(8) -169.7(16) ? . . . . C(7) Fe(1) C(15) C(14) 163.0(7) ? . . . . C(7) Fe(1) C(15) C(16) -77.6(10) ? . . . . C(15) Fe(1) C(7) C(6) -81.9(12) ? . . . . C(15) Fe(1) C(7) C(8) 158.3(9) ? . . . . C(7) Fe(1) C(16) C(15) 120.0(8) ? . . . . C(7) Fe(1) C(16) C(17) -121.0(8) ? . . . . C(16) Fe(1) C(7) C(6) -123.6(10) ? . . . . C(16) Fe(1) C(7) C(8) 116.6(10) ? . . . . C(7) Fe(1) C(17) C(16) 77.3(10) ? . . . . C(7) Fe(1) C(17) C(18) -162.6(8) ? . . . . C(17) Fe(1) C(7) C(6) -166.0(9) ? . . . . C(17) Fe(1) C(7) C(8) 74.2(12) ? . . . . C(7) Fe(1) C(18) C(14) 163.0(19) ? . . . . C(7) Fe(1) C(18) C(17) 44(2) ? . . . . C(18) Fe(1) C(7) C(6) 161.9(17) ? . . . . C(18) Fe(1) C(7) C(8) 42(2) ? . . . . C(8) Fe(1) C(9) C(5) -118.7(12) ? . . . . C(9) Fe(1) C(8) C(7) 120.0(12) ? . . . . C(8) Fe(1) C(14) C(10) -81.9(17) ? . . . . C(8) Fe(1) C(14) C(15) 156.6(15) ? . . . . C(8) Fe(1) C(14) C(18) 37(2) ? . . . . C(14) Fe(1) C(8) C(7) 169.2(15) ? . . . . C(14) Fe(1) C(8) C(9) 49.2(18) ? . . . . C(8) Fe(1) C(15) C(14) -160.1(11) ? . . . . C(8) Fe(1) C(15) C(16) -40.6(16) ? . . . . C(15) Fe(1) C(8) C(7) -51.3(16) ? . . . . C(15) Fe(1) C(8) C(9) -171.3(11) ? . . . . C(8) Fe(1) C(16) C(15) 162.4(8) ? . . . . C(8) Fe(1) C(16) C(17) -78.6(10) ? . . . . C(16) Fe(1) C(8) C(7) -80.6(11) ? . . . . C(16) Fe(1) C(8) C(9) 159.4(7) ? . . . . C(8) Fe(1) C(17) C(16) 118.0(9) ? . . . . C(8) Fe(1) C(17) C(18) -121.8(8) ? . . . . C(17) Fe(1) C(8) C(7) -122.9(11) ? . . . . C(17) Fe(1) C(8) C(9) 117.2(8) ? . . . . C(8) Fe(1) C(18) C(14) -165.9(9) ? . . . . C(8) Fe(1) C(18) C(17) 74.8(10) ? . . . . C(18) Fe(1) C(8) C(7) -163.3(10) ? . . . . C(18) Fe(1) C(8) C(9) 76.8(9) ? . . . . C(9) Fe(1) C(14) C(10) -45.8(10) ? . . . . C(9) Fe(1) C(14) C(15) -167.3(7) ? . . . . C(9) Fe(1) C(14) C(18) 72.9(9) ? . . . . C(14) Fe(1) C(9) C(5) 80.1(9) ? . . . . C(14) Fe(1) C(9) C(8) -161.1(7) ? . . . . C(9) Fe(1) C(15) C(14) 40(2) ? . . . . C(9) Fe(1) C(15) C(16) 159.6(18) ? . . . . C(15) Fe(1) C(9) C(5) 48(2) ? . . . . C(15) Fe(1) C(9) C(8) 167.2(17) ? . . . . C(9) Fe(1) C(16) C(15) -167.5(13) ? . . . . C(9) Fe(1) C(16) C(17) -48.5(18) ? . . . . C(16) Fe(1) C(9) C(5) -162.4(13) ? . . . . C(16) Fe(1) C(9) C(8) -43.7(17) ? . . . . C(9) Fe(1) C(17) C(16) 157.9(8) ? . . . . C(9) Fe(1) C(17) C(18) -82.0(8) ? . . . . C(17) Fe(1) C(9) C(5) 163.2(8) ? . . . . C(17) Fe(1) C(9) C(8) -78.1(10) ? . . . . C(9) Fe(1) C(18) C(14) -125.9(8) ? . . . . C(9) Fe(1) C(18) C(17) 114.8(8) ? . . . . C(18) Fe(1) C(9) C(5) 121.1(8) ? . . . . C(18) Fe(1) C(9) C(8) -120.2(8) ? . . . . C(14) Fe(1) C(15) C(16) 119.4(11) ? . . . . C(15) Fe(1) C(14) C(10) 121.5(11) ? . . . . C(15) Fe(1) C(14) C(18) -119.7(11) ? . . . . C(14) Fe(1) C(16) C(15) -38.0(8) ? . . . . C(14) Fe(1) C(16) C(17) 81.0(8) ? . . . . C(16) Fe(1) C(14) C(10) 159.1(10) ? . . . . C(16) Fe(1) C(14) C(15) 37.6(7) ? . . . . C(16) Fe(1) C(14) C(18) -82.2(8) ? . . . . C(14) Fe(1) C(17) C(16) -82.2(8) ? . . . . C(14) Fe(1) C(17) C(18) 38.0(7) ? . . . . C(17) Fe(1) C(14) C(10) -156.2(11) ? . . . . C(17) Fe(1) C(14) C(15) 82.3(8) ? . . . . C(17) Fe(1) C(14) C(18) -37.4(9) ? . . . . C(14) Fe(1) C(18) C(17) -119.3(11) ? . . . . C(18) Fe(1) C(14) C(10) -118.7(13) ? . . . . C(18) Fe(1) C(14) C(15) 119.7(11) ? . . . . C(15) Fe(1) C(16) C(17) 119.0(12) ? . . . . C(16) Fe(1) C(15) C(14) -119.4(11) ? . . . . C(15) Fe(1) C(17) C(16) -37.7(8) ? . . . . C(15) Fe(1) C(17) C(18) 82.4(8) ? . . . . C(17) Fe(1) C(15) C(14) -81.0(8) ? . . . . C(17) Fe(1) C(15) C(16) 38.4(9) ? . . . . C(15) Fe(1) C(18) C(14) 37.7(8) ? . . . . C(15) Fe(1) C(18) C(17) -81.6(8) ? . . . . C(18) Fe(1) C(15) C(14) -37.6(6) ? . . . . C(18) Fe(1) C(15) C(16) 81.8(9) ? . . . . C(16) Fe(1) C(17) C(18) 120.2(10) ? . . . . C(17) Fe(1) C(16) C(15) -119.0(12) ? . . . . C(16) Fe(1) C(18) C(14) 81.5(8) ? . . . . C(16) Fe(1) C(18) C(17) -37.8(7) ? . . . . C(18) Fe(1) C(16) C(15) -82.1(8) ? . . . . C(18) Fe(1) C(16) C(17) 36.9(7) ? . . . . C(17) Fe(1) C(18) C(14) 119.3(11) ? . . . . C(18) Fe(1) C(17) C(16) -120.2(10) ? . . . . C(23) Fe(2) C(24) C(25) 118.9 ? . . . . C(24) Fe(2) C(23) C(19) 120.2 ? . . . . C(24) Fe(2) C(23) C(27) -120.3 ? . . . . C(23) Fe(2) C(24) C(25) 61.1 ? . . 56702 56702 C(24) Fe(2) C(23) C(19) -59.8 ? 56702 . . . C(24) Fe(2) C(23) C(27) 59.7 ? 56702 . . . C(23) Fe(2) C(25) C(24) -38.0 ? . . . . C(23) Fe(2) C(25) C(26) 81.8 ? . . . . C(25) Fe(2) C(23) C(19) 157.9 ? . . . . C(25) Fe(2) C(23) C(24) 37.7 ? . . . . C(25) Fe(2) C(23) C(27) -82.6 ? . . . . C(23) Fe(2) C(25) C(24) -142.0 ? . . 56702 56702 C(23) Fe(2) C(25) C(26) 98.2 ? . . 56702 56702 C(25) Fe(2) C(23) C(19) -22.1 ? 56702 . . . C(25) Fe(2) C(23) C(24) -142.3 ? 56702 . . . C(25) Fe(2) C(23) C(27) 97.4 ? 56702 . . . C(23) Fe(2) C(26) C(25) -81.4 ? . . . . C(23) Fe(2) C(26) C(27) 39.8 ? . . . . C(26) Fe(2) C(23) C(19) -158.8 ? . . . . C(26) Fe(2) C(23) C(24) 81.0 ? . . . . C(26) Fe(2) C(23) C(27) -39.3 ? . . . . C(23) Fe(2) C(26) C(25) -98.6 ? . . 56702 56702 C(23) Fe(2) C(26) C(27) 140.2 ? . . 56702 56702 C(26) Fe(2) C(23) C(19) 21.2 ? 56702 . . . C(26) Fe(2) C(23) C(24) -99.0 ? 56702 . . . C(26) Fe(2) C(23) C(27) 140.7 ? 56702 . . . C(23) Fe(2) C(27) C(26) -116.4 ? . . . . C(27) Fe(2) C(23) C(19) -119.5 ? . . . . C(27) Fe(2) C(23) C(24) 120.3 ? . . . . C(23) Fe(2) C(27) C(26) -63.6 ? . . 56702 56702 C(27) Fe(2) C(23) C(19) 60.5 ? 56702 . . . C(27) Fe(2) C(23) C(24) -59.7 ? 56702 . . . C(23) Fe(2) C(24) C(25) -61.1 ? 56702 . . . C(24) Fe(2) C(23) C(19) 59.8 ? . . 56702 56702 C(24) Fe(2) C(23) C(27) -59.7 ? . . 56702 56702 C(23) Fe(2) C(24) C(25) -118.9 ? 56702 . 56702 56702 C(24) Fe(2) C(23) C(19) -120.2 ? 56702 . 56702 56702 C(24) Fe(2) C(23) C(27) 120.3 ? 56702 . 56702 56702 C(23) Fe(2) C(25) C(24) 142.0 ? 56702 . . . C(23) Fe(2) C(25) C(26) -98.2 ? 56702 . . . C(25) Fe(2) C(23) C(19) 22.1 ? . . 56702 56702 C(25) Fe(2) C(23) C(24) 142.3 ? . . 56702 56702 C(25) Fe(2) C(23) C(27) -97.4 ? . . 56702 56702 C(23) Fe(2) C(25) C(24) 38.0 ? 56702 . 56702 56702 C(23) Fe(2) C(25) C(26) -81.8 ? 56702 . 56702 56702 C(25) Fe(2) C(23) C(19) -157.9 ? 56702 . 56702 56702 C(25) Fe(2) C(23) C(24) -37.7 ? 56702 . 56702 56702 C(25) Fe(2) C(23) C(27) 82.6 ? 56702 . 56702 56702 C(23) Fe(2) C(26) C(25) 98.6 ? 56702 . . . C(23) Fe(2) C(26) C(27) -140.2 ? 56702 . . . C(26) Fe(2) C(23) C(19) -21.2 ? . . 56702 56702 C(26) Fe(2) C(23) C(24) 99.0 ? . . 56702 56702 C(26) Fe(2) C(23) C(27) -140.7 ? . . 56702 56702 C(23) Fe(2) C(26) C(25) 81.4 ? 56702 . 56702 56702 C(23) Fe(2) C(26) C(27) -39.8 ? 56702 . 56702 56702 C(26) Fe(2) C(23) C(19) 158.8 ? 56702 . 56702 56702 C(26) Fe(2) C(23) C(24) -81.0 ? 56702 . 56702 56702 C(26) Fe(2) C(23) C(27) 39.3 ? 56702 . 56702 56702 C(23) Fe(2) C(27) C(26) 63.6 ? 56702 . . . C(27) Fe(2) C(23) C(19) -60.5 ? . . 56702 56702 C(27) Fe(2) C(23) C(24) 59.7 ? . . 56702 56702 C(23) Fe(2) C(27) C(26) 116.4 ? 56702 . 56702 56702 C(27) Fe(2) C(23) C(19) 119.5 ? 56702 . 56702 56702 C(27) Fe(2) C(23) C(24) -120.3 ? 56702 . 56702 56702 C(24) Fe(2) C(25) C(26) 119.8 ? . . . . C(25) Fe(2) C(24) C(23) -118.9 ? . . . . C(24) Fe(2) C(25) C(26) 60.2 ? . . 56702 56702 C(25) Fe(2) C(24) C(23) 61.1 ? 56702 . . . C(24) Fe(2) C(26) C(25) -37.3 ? . . . . C(24) Fe(2) C(26) C(27) 83.8 ? . . . . C(26) Fe(2) C(24) C(23) -81.8 ? . . . . C(26) Fe(2) C(24) C(25) 37.1 ? . . . . C(24) Fe(2) C(26) C(25) -142.7 ? . . 56702 56702 C(24) Fe(2) C(26) C(27) 96.2 ? . . 56702 56702 C(26) Fe(2) C(24) C(23) 98.2 ? 56702 . . . C(26) Fe(2) C(24) C(25) -142.9 ? 56702 . . . C(24) Fe(2) C(27) C(23) 36.9 ? . . . . C(24) Fe(2) C(27) C(26) -79.4 ? . . . . C(27) Fe(2) C(24) C(23) -37.6 ? . . . . C(27) Fe(2) C(24) C(25) 81.3 ? . . . . C(24) Fe(2) C(27) C(23) 143.1 ? . . 56702 56702 C(24) Fe(2) C(27) C(26) -100.6 ? . . 56702 56702 C(27) Fe(2) C(24) C(23) 142.4 ? 56702 . . . C(27) Fe(2) C(24) C(25) -98.7 ? 56702 . . . C(24) Fe(2) C(25) C(26) -60.2 ? 56702 . . . C(25) Fe(2) C(24) C(23) -61.1 ? . . 56702 56702 C(24) Fe(2) C(25) C(26) -119.8 ? 56702 . 56702 56702 C(25) Fe(2) C(24) C(23) 118.9 ? 56702 . 56702 56702 C(24) Fe(2) C(26) C(25) 142.7 ? 56702 . . . C(24) Fe(2) C(26) C(27) -96.2 ? 56702 . . . C(26) Fe(2) C(24) C(23) -98.2 ? . . 56702 56702 C(26) Fe(2) C(24) C(25) 142.9 ? . . 56702 56702 C(24) Fe(2) C(26) C(25) 37.3 ? 56702 . 56702 56702 C(24) Fe(2) C(26) C(27) -83.8 ? 56702 . 56702 56702 C(26) Fe(2) C(24) C(23) 81.8 ? 56702 . 56702 56702 C(26) Fe(2) C(24) C(25) -37.1 ? 56702 . 56702 56702 C(24) Fe(2) C(27) C(23) -143.1 ? 56702 . . . C(24) Fe(2) C(27) C(26) 100.6 ? 56702 . . . C(27) Fe(2) C(24) C(23) -142.4 ? . . 56702 56702 C(27) Fe(2) C(24) C(25) 98.7 ? . . 56702 56702 C(24) Fe(2) C(27) C(23) -36.9 ? 56702 . 56702 56702 C(24) Fe(2) C(27) C(26) 79.4 ? 56702 . 56702 56702 C(27) Fe(2) C(24) C(23) 37.6 ? 56702 . 56702 56702 C(27) Fe(2) C(24) C(25) -81.3 ? 56702 . 56702 56702 C(25) Fe(2) C(26) C(27) 121.2 ? . . . . C(26) Fe(2) C(25) C(24) -119.8 ? . . . . C(25) Fe(2) C(26) C(27) 58.8 ? . . 56702 56702 C(26) Fe(2) C(25) C(24) 60.2 ? 56702 . . . C(25) Fe(2) C(27) C(23) 80.2 ? . . . . C(25) Fe(2) C(27) C(26) -36.2 ? . . . . C(27) Fe(2) C(25) C(24) -82.8 ? . . . . C(27) Fe(2) C(25) C(26) 37.0 ? . . . . C(25) Fe(2) C(27) C(23) 99.8 ? . . 56702 56702 C(25) Fe(2) C(27) C(26) -143.8 ? . . 56702 56702 C(27) Fe(2) C(25) C(24) 97.2 ? 56702 . . . C(27) Fe(2) C(25) C(26) -143.0 ? 56702 . . . C(25) Fe(2) C(26) C(27) -58.8 ? 56702 . . . C(26) Fe(2) C(25) C(24) -60.2 ? . . 56702 56702 C(25) Fe(2) C(26) C(27) -121.2 ? 56702 . 56702 56702 C(26) Fe(2) C(25) C(24) 119.8 ? 56702 . 56702 56702 C(25) Fe(2) C(27) C(23) -99.8 ? 56702 . . . C(25) Fe(2) C(27) C(26) 143.8 ? 56702 . . . C(27) Fe(2) C(25) C(24) -97.2 ? . . 56702 56702 C(27) Fe(2) C(25) C(26) 143.0 ? . . 56702 56702 C(25) Fe(2) C(27) C(23) -80.2 ? 56702 . 56702 56702 C(25) Fe(2) C(27) C(26) 36.2 ? 56702 . 56702 56702 C(27) Fe(2) C(25) C(24) 82.8 ? 56702 . 56702 56702 C(27) Fe(2) C(25) C(26) -37.0 ? 56702 . 56702 56702 C(26) Fe(2) C(27) C(23) 116.4 ? . . . . C(27) Fe(2) C(26) C(25) -121.2 ? . . . . C(26) Fe(2) C(27) C(23) 63.6 ? . . 56702 56702 C(27) Fe(2) C(26) C(25) 58.8 ? 56702 . . . C(26) Fe(2) C(27) C(23) -63.6 ? 56702 . . . C(27) Fe(2) C(26) C(25) -58.8 ? . . 56702 56702 C(26) Fe(2) C(27) C(23) -116.4 ? 56702 . 56702 56702 C(27) Fe(2) C(26) C(25) 121.2 ? 56702 . 56702 56702 Cu(1) N(1) C(2) C(1) -170.8(9) ? . . . . Cu(1) N(1) C(3) C(4) 171.2(11) ? . . . . C(2) N(1) C(3) C(4) -0.4(15) ? . . . . C(3) N(1) C(2) C(1) 0.8(18) ? . . . . C(1) N(2) C(4) C(3) 1(2) ? . . . . C(4) N(2) C(1) C(2) -0.8(17) ? . . . . C(4) N(2) C(1) C(5) -178.7(13) ? . . . . Cu(2) N(3) C(11) C(10) 179.1(8) ? . . . . Cu(2) N(3) C(12) C(13) -179.4(10) ? . . . . C(11) N(3) C(12) C(13) -1.2(19) ? . . . . C(12) N(3) C(11) C(10) 1.0(17) ? . . . . C(10) N(4) C(13) C(12) -1(2) ? . . . . C(13) N(4) C(10) C(11) 1.1(18) ? . . . . C(13) N(4) C(10) C(14) -179.8(8) ? . . . . C(20) N(5) C(21) C(22) -1(2) ? . . . . C(21) N(5) C(20) C(19) 1(2) ? . . . . C(19) N(6) C(22) C(21) 2(2) ? . . . . C(22) N(6) C(19) C(20) -2(2) ? . . . . C(22) N(6) C(19) C(23) 178.8(15) ? . . . . N(2) C(1) C(2) N(1) -0.2(16) ? . . . . N(2) C(1) C(5) Fe(1) -97.2(14) ? . . . . N(2) C(1) C(5) C(6) 167.9(13) ? . . . . N(2) C(1) C(5) C(9) -8.5(19) ? . . . . C(2) C(1) C(5) Fe(1) 84.9(15) ? . . . . C(2) C(1) C(5) C(6) -10(2) ? . . . . C(2) C(1) C(5) C(9) 173.6(12) ? . . . . C(5) C(1) C(2) N(1) 177.6(11) ? . . . . N(1) C(3) C(4) N(2) -0.6(19) ? . . . . Fe(1) C(5) C(6) C(7) 60.2(10) ? . . . . Fe(1) C(5) C(9) C(8) -61.0(10) ? . . . . C(1) C(5) C(6) Fe(1) 124.3(13) ? . . . . C(1) C(5) C(6) C(7) -175.5(13) ? . . . . C(1) C(5) C(9) Fe(1) -123.4(12) ? . . . . C(1) C(5) C(9) C(8) 175.6(12) ? . . . . C(6) C(5) C(9) Fe(1) 59.6(9) ? . . . . C(6) C(5) C(9) C(8) -1.5(15) ? . . . . C(9) C(5) C(6) Fe(1) -58.8(9) ? . . . . C(9) C(5) C(6) C(7) 1.4(15) ? . . . . Fe(1) C(6) C(7) C(8) 58.8(10) ? . . . . C(5) C(6) C(7) Fe(1) -59.6(9) ? . . . . C(5) C(6) C(7) C(8) -0.8(15) ? . . . . Fe(1) C(7) C(8) C(9) 58.6(10) ? . . . . C(6) C(7) C(8) Fe(1) -58.7(10) ? . . . . C(6) C(7) C(8) C(9) -0.1(14) ? . . . . Fe(1) C(8) C(9) C(5) 59.7(9) ? . . . . C(7) C(8) C(9) Fe(1) -58.7(10) ? . . . . C(7) C(8) C(9) C(5) 1.0(16) ? . . . . N(4) C(10) C(11) N(3) -1.0(17) ? . . . . N(4) C(10) C(14) Fe(1) 86.0(12) ? . . . . N(4) C(10) C(14) C(15) 174.9(12) ? . . . . N(4) C(10) C(14) C(18) -0.4(13) ? . . . . C(11) C(10) C(14) Fe(1) -94.8(11) ? . . . . C(11) C(10) C(14) C(15) -5.9(18) ? . . . . C(11) C(10) C(14) C(18) 178.8(11) ? . . . . C(14) C(10) C(11) N(3) 179.9(8) ? . . . . N(3) C(12) C(13) N(4) 1(2) ? . . . . Fe(1) C(14) C(15) C(16) -59.4(9) ? . . . . Fe(1) C(14) C(18) C(17) 60.3(9) ? . . . . C(10) C(14) C(15) Fe(1) -117.9(12) ? . . . . C(10) C(14) C(15) C(16) -177.2(11) ? . . . . C(10) C(14) C(18) Fe(1) 117.4(11) ? . . . . C(10) C(14) C(18) C(17) 177.6(11) ? . . . . C(15) C(14) C(18) Fe(1) -58.7(9) ? . . . . C(15) C(14) C(18) C(17) 1.6(14) ? . . . . C(18) C(14) C(15) Fe(1) 58.1(8) ? . . . . C(18) C(14) C(15) C(16) -1.3(14) ? . . . . Fe(1) C(15) C(16) C(17) -58.4(9) ? . . . . C(14) C(15) C(16) Fe(1) 58.9(9) ? . . . . C(14) C(15) C(16) C(17) 0.5(13) ? . . . . Fe(1) C(16) C(17) C(18) -58.3(9) ? . . . . C(15) C(16) C(17) Fe(1) 58.8(10) ? . . . . C(15) C(16) C(17) C(18) 0.5(13) ? . . . . Fe(1) C(17) C(18) C(14) -60.1(8) ? . . . . C(16) C(17) C(18) Fe(1) 58.8(9) ? . . . . C(16) C(17) C(18) C(14) -1.3(15) ? . . . . N(6) C(19) C(20) N(5) 1(2) ? . . . . N(6) C(19) C(23) Fe(2) -79.8 ? . . . . N(6) C(19) C(23) C(24) 9.3 ? . . . . N(6) C(19) C(23) C(27) -167.6 ? . . . . C(20) C(19) C(23) Fe(2) 101.1 ? . . . . C(20) C(19) C(23) C(24) -169.8 ? . . . . C(20) C(19) C(23) C(27) 13.3 ? . . . . C(23) C(19) C(20) N(5) -179.8(11) ? . . . . N(5) C(21) C(22) N(6) 0(2) ? . . . . Fe(2) C(23) C(24) C(25) -59.4 ? . . . . Fe(2) C(23) C(27) C(26) 60.2 ? . . . . C(19) C(23) C(24) Fe(2) -118.0 ? . . . . C(19) C(23) C(24) C(25) -177.4 ? . . . . C(19) C(23) C(27) Fe(2) 117.5 ? . . . . C(19) C(23) C(27) C(26) 177.7 ? . . . . C(24) C(23) C(27) Fe(2) -59.8 ? . . . . C(24) C(23) C(27) C(26) 0.4 ? . . . . C(27) C(23) C(24) Fe(2) 59.3 ? . . . . C(27) C(23) C(24) C(25) -0.1 ? . . . . Fe(2) C(24) C(25) C(26) -58.8 ? . . . . C(23) C(24) C(25) Fe(2) 58.6 ? . . . . C(23) C(24) C(25) C(26) -0.3 ? . . . . Fe(2) C(25) C(26) C(27) -58.6 ? . . . . C(24) C(25) C(26) Fe(2) 59.1 ? . . . . C(24) C(25) C(26) C(27) 0.5 ? . . . . Fe(2) C(26) C(27) C(23) -59.7 ? . . . . C(25) C(26) C(27) Fe(2) 59.2 ? . . . . C(25) C(26) C(27) C(23) -0.5 ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 I(1) Cu(1) 3.051(2) ? . 66602 I(1) Cu(2) 2.718(2) ? . . I(1) Cu(2) 2.705(2) ? . 66702 I(2) Cu(1) 2.539(2) ? . 66702 Cu(1) I(1) 3.051(2) ? . 66602 Cu(1) I(2) 2.539(2) ? . 66702 Cu(1) Cu(1) 3.113(3) ? . 66602 Cu(1) Cu(2) 2.703(2) ? . 66702 Cu(2) I(1) 2.718(2) ? . . Cu(2) I(1) 2.705(2) ? . 66702 Cu(2) Cu(1) 2.703(2) ? . 66702 Cu(2) N(3) 2.031(8) ? . . Cu(2) C(11) 2.963(10) ? . . Cu(2) C(12) 2.944(12) ? . . N(2) C(18) 3.527(18) ? . 55602 N(3) Cu(2) 2.031(8) ? . . N(3) C(6) 3.494(18) ? . 55601 N(4) C(9) 3.569(18) ? . 55601 N(4) C(9) 3.595(18) ? . 55602 N(5) C(11) 3.53(2) ? . 45501 N(5) C(15) 3.358(15) ? . 45501 N(6) C(4) 3.544(19) ? . 55601 N(6) C(8) 3.58(2) ? . 55602 C(1) C(12) 3.459(19) ? . 55401 C(4) N(6) 3.544(19) ? . 55401 C(5) C(12) 3.534(19) ? . 55401 C(5) C(13) 3.540(19) ? . 55401 C(6) N(3) 3.494(18) ? . 55401 C(6) C(11) 3.368(18) ? . 55401 C(7) C(10) 3.40(2) ? . 55401 C(7) C(11) 3.57(2) ? . 55401 C(7) C(14) 3.596(19) ? . 55401 C(7) C(22) 3.50(2) ? . 55602 C(8) N(6) 3.58(2) ? . 55602 C(8) C(22) 3.51(2) ? . 55602 C(9) N(4) 3.569(18) ? . 55401 C(9) N(4) 3.595(18) ? . 55602 C(9) C(9) 3.400(18) ? . 55502 C(10) C(7) 3.40(2) ? . 55601 C(11) Cu(2) 2.963(10) ? . . C(11) N(5) 3.53(2) ? . 65501 C(11) C(6) 3.368(18) ? . 55601 C(11) C(7) 3.57(2) ? . 55601 C(12) Cu(2) 2.944(12) ? . . C(12) C(1) 3.459(19) ? . 55601 C(12) C(5) 3.534(19) ? . 55601 C(13) C(5) 3.540(19) ? . 55601 C(14) C(7) 3.596(19) ? . 55601 C(15) N(5) 3.358(15) ? . 65501 C(18) N(2) 3.527(18) ? . 55602 C(22) C(7) 3.50(2) ? . 55602 C(22) C(8) 3.51(2) ? . 55602 I(1) H(20) 3.504(18) ? . 65501 I(1) H(25) 3.2771(7) ? . 66702 I(2) H(3) 3.5285(7) ? . 66702 I(2) H(6) 3.2407(8) ? . 55601 I(2) H(20) 3.316(16) ? . 65601 I(2) H(25) 3.3717(8) ? . 66702 I(2) H(27) 3.3697(7) ? . 65601 Cu(1) H(2) 3.5641(19) ? . 66602 Cu(2) H(11) 3.0105(17) ? . . Cu(2) H(12) 2.9892(18) ? . . N(2) H(8) 3.198(11) ? . 55502 N(2) H(13) 3.575(14) ? . 55401 N(2) H(18) 2.826(12) ? . 55602 N(2) H(24) 3.279(14) ? . 55401 N(3) H(6) 3.373(10) ? . 55601 N(4) H(9) 2.794(11) ? . 55602 N(4) H(18) 2.968(10) ? . 55602 N(5) H(11) 2.584(16) ? . 45501 N(5) H(15) 2.425(10) ? . 45501 N(5) H(16) 3.064(16) ? . 55602 N(6) H(4) 2.857(12) ? . 55601 N(6) H(8) 2.811(15) ? . 55602 C(1) H(12) 3.387(13) ? . 55401 C(2) H(12) 3.482(12) ? . 55401 C(3) H(24) 3.356(13) ? . 55401 C(3) H(25) 3.522(15) ? . . C(3) H(27) 3.468(17) ? . 56602 C(4) H(17) 3.503(16) ? . 55602 C(4) H(18) 3.279(15) ? . 55602 C(4) H(24) 2.951(16) ? . 55401 C(7) H(22) 3.45(2) ? . 55602 C(8) H(9) 3.106(17) ? . 55502 C(8) H(13) 3.384(15) ? . 55602 C(8) H(22) 3.46(2) ? . 55602 C(9) H(9) 2.781(12) ? . 55502 C(9) H(13) 3.438(12) ? . 55602 C(11) H(6) 3.376(11) ? . 55601 C(12) H(24) 3.140(17) ? . . C(12) H(25) 3.473(17) ? . . C(13) H(9) 3.221(13) ? . 55602 C(13) H(17) 3.596(15) ? . 55602 C(13) H(18) 3.405(12) ? . 55602 C(13) H(24) 3.269(18) ? . . C(14) H(7) 3.503(11) ? . 55601 C(14) H(22) 3.35(2) ? . 55702 C(15) H(21) 3.416(11) ? . 65501 C(15) H(22) 3.26(2) ? . 55702 C(16) H(22) 2.86(2) ? . 55702 C(17) H(4) 3.292(13) ? . 55602 C(17) H(13) 3.341(13) ? . 55602 C(17) H(22) 2.72(2) ? . 55702 C(18) H(4) 3.432(11) ? . 55602 C(18) H(13) 3.509(10) ? . 55602 C(18) H(22) 3.06(2) ? . 55702 C(19) H(8) 3.592(16) ? . 55602 C(19) H(17) 3.171(15) ? . 55602 C(20) H(11) 3.555(16) ? . 45501 C(20) H(15) 3.474(12) ? . 45501 C(20) H(16) 3.115(15) ? . 55602 C(20) H(17) 3.489(19) ? . 55602 C(21) H(7) 2.928(18) ? . 55602 C(21) H(11) 3.150(19) ? . 45501 C(21) H(15) 2.957(15) ? . 45501 C(21) H(16) 3.597(19) ? . 55602 C(22) H(4) 3.343(16) ? . 55601 C(22) H(7) 2.947(16) ? . 55602 C(22) H(8) 2.95(2) ? . 55602 C(23) H(17) 3.209(13) ? . 55602 C(24) H(12) 2.915(18) ? . . C(24) H(13) 3.099(17) ? . . C(25) H(3) 2.897(16) ? . . C(25) H(12) 3.04(2) ? . . C(26) H(3) 2.975(19) ? . . C(26) H(26) 3.114(13) ? . 56602 C(27) H(3) 3.498(16) ? . 56602 C(27) H(26) 3.287(14) ? . 56602 H(2) Cu(1) 3.5641(19) ? . 66602 H(3) I(2) 3.5285(7) ? . 66702 H(3) C(25) 2.897(16) ? . . H(3) C(26) 2.975(19) ? . . H(3) C(27) 3.498(16) ? . 56602 H(3) H(25) 2.841 ? . . H(3) H(26) 2.975 ? . . H(3) H(26) 3.270 ? . 56602 H(3) H(27) 2.855 ? . 56602 H(4) N(6) 2.857(12) ? . 55401 H(4) C(17) 3.292(13) ? . 55602 H(4) C(18) 3.432(10) ? . 55602 H(4) C(22) 3.343(16) ? . 55401 H(4) H(17) 2.897 ? . 55602 H(4) H(18) 3.167 ? . 55602 H(4) H(22) 3.035(15) ? . 55401 H(4) H(24) 2.987 ? . 55401 H(4) H(26) 3.317 ? . 56602 H(6) I(2) 3.2407(8) ? . 55401 H(6) N(3) 3.373(10) ? . 55401 H(6) C(11) 3.376(11) ? . 55401 H(6) H(11) 3.463 ? . 55401 H(6) H(21) 3.569 ? . 65401 H(7) C(14) 3.503(11) ? . 55401 H(7) C(21) 2.928(18) ? . 55602 H(7) C(22) 2.947(16) ? . 55602 H(7) H(21) 2.917 ? . 65401 H(7) H(21) 2.899 ? . 55602 H(7) H(22) 2.927(15) ? . 55602 H(8) N(2) 3.198(11) ? . 55502 H(8) N(6) 2.811(15) ? . 55602 H(8) C(19) 3.592(17) ? . 55602 H(8) C(22) 2.95(2) ? . 55602 H(8) H(9) 3.042 ? . 55502 H(8) H(13) 2.897 ? . 55602 H(8) H(22) 2.94(2) ? . 55602 H(9) N(4) 2.794(11) ? . 55602 H(9) C(8) 3.106(17) ? . 55502 H(9) C(9) 2.781(12) ? . 55502 H(9) C(13) 3.221(13) ? . 55602 H(9) H(8) 3.042 ? . 55502 H(9) H(9) 2.389 ? . 55502 H(9) H(13) 3.019 ? . 55602 H(9) H(18) 3.124 ? . 55602 H(11) Cu(2) 3.0105(17) ? . . H(11) N(5) 2.584(16) ? . 65501 H(11) C(20) 3.555(16) ? . 65501 H(11) C(21) 3.150(19) ? . 65501 H(11) H(6) 3.463 ? . 55601 H(11) H(21) 2.996 ? . 65501 H(12) Cu(2) 2.9892(18) ? . . H(12) C(1) 3.387(13) ? . 55601 H(12) C(2) 3.482(12) ? . 55601 H(12) C(24) 2.915(18) ? . . H(12) C(25) 3.04(2) ? . . H(12) H(24) 2.447 ? . . H(12) H(25) 2.699 ? . . H(13) N(2) 3.575(14) ? . 55601 H(13) C(8) 3.384(14) ? . 55602 H(13) C(9) 3.438(12) ? . 55602 H(13) C(17) 3.341(13) ? . 55602 H(13) C(18) 3.509(10) ? . 55602 H(13) C(24) 3.099(17) ? . . H(13) H(8) 2.897 ? . 55602 H(13) H(9) 3.019 ? . 55602 H(13) H(17) 2.792 ? . 55602 H(13) H(18) 3.145 ? . 55602 H(13) H(24) 2.713 ? . . H(15) N(5) 2.425(10) ? . 65501 H(15) C(20) 3.474(12) ? . 65501 H(15) C(21) 2.957(15) ? . 65501 H(15) H(16) 3.098 ? . 65602 H(15) H(21) 2.779 ? . 65501 H(16) N(5) 3.064(16) ? . 55602 H(16) C(20) 3.115(15) ? . 55602 H(16) C(21) 3.597(19) ? . 55602 H(16) H(15) 3.098 ? . 65602 H(16) H(16) 3.331 ? . 65602 H(16) H(20) 3.240(16) ? . 55602 H(16) H(22) 3.255(19) ? . 55702 H(17) C(4) 3.503(16) ? . 55602 H(17) C(13) 3.596(15) ? . 55602 H(17) C(19) 3.171(15) ? . 55602 H(17) C(20) 3.489(19) ? . 55602 H(17) C(23) 3.209(13) ? . 55602 H(17) H(4) 2.897 ? . 55602 H(17) H(13) 2.792 ? . 55602 H(17) H(22) 3.023(17) ? . 55702 H(18) N(2) 2.826(12) ? . 55602 H(18) N(4) 2.968(10) ? . 55602 H(18) C(4) 3.279(15) ? . 55602 H(18) C(13) 3.405(11) ? . 55602 H(18) H(4) 3.167 ? . 55602 H(18) H(9) 3.124 ? . 55602 H(18) H(13) 3.145 ? . 55602 H(18) H(18) 3.186 ? . 55602 H(18) H(22) 3.55(2) ? . 55702 H(20) I(1) 3.504(18) ? . 45501 H(20) I(2) 3.316(16) ? . 45401 H(20) H(16) 3.240(16) ? . 55602 H(21) C(15) 3.416(11) ? . 45501 H(21) H(6) 3.569 ? . 45601 H(21) H(7) 2.917 ? . 45601 H(21) H(7) 2.899 ? . 55602 H(21) H(11) 2.996 ? . 45501 H(21) H(15) 2.779 ? . 45501 H(21) H(21) 3.344 ? . 45702 H(22) C(7) 3.45(2) ? . 55602 H(22) C(8) 3.46(2) ? . 55602 H(22) C(14) 3.35(2) ? . 55702 H(22) C(15) 3.26(2) ? . 55702 H(22) C(16) 2.86(2) ? . 55702 H(22) C(17) 2.72(2) ? . 55702 H(22) C(18) 3.06(2) ? . 55702 H(22) H(4) 3.035(15) ? . 55601 H(22) H(7) 2.927(15) ? . 55602 H(22) H(8) 2.94(2) ? . 55602 H(22) H(16) 3.255(19) ? . 55702 H(22) H(17) 3.023(17) ? . 55702 H(22) H(18) 3.55(2) ? . 55702 H(24) N(2) 3.279(14) ? . 55601 H(24) C(3) 3.356(13) ? . 55601 H(24) C(4) 2.951(16) ? . 55601 H(24) C(12) 3.140(17) ? . . H(24) C(13) 3.269(18) ? . . H(24) H(4) 2.987 ? . 55601 H(24) H(12) 2.447 ? . . H(24) H(13) 2.713 ? . . H(25) I(1) 3.2771(7) ? . 66702 H(25) I(2) 3.3717(8) ? . 66702 H(25) C(3) 3.522(15) ? . . H(25) C(12) 3.473(17) ? . . H(25) H(3) 2.841 ? . . H(25) H(12) 2.699 ? . . H(26) C(26) 3.114(13) ? . 56602 H(26) C(27) 3.287(14) ? . 56602 H(26) H(3) 2.975 ? . . H(26) H(3) 3.270 ? . 56602 H(26) H(4) 3.317 ? . 56602 H(26) H(26) 2.739 ? . 56602 H(26) H(27) 3.075 ? . 56602 H(27) I(2) 3.3697(7) ? . 45401 H(27) C(3) 3.468(17) ? . 56602 H(27) H(3) 2.855 ? . 56602 H(27) H(26) 3.075 ? . 56602 #============================================================================== data_L1 _database_code_depnum_ccdc_archive 'CCDC 262865' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H14 Fe N4 ' _chemical_formula_moiety 'C18 H14 Fe N4 ' _chemical_formula_weight 342.18 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 #------------------------------------------------------------------------------ _cell_length_a 9.384(3) _cell_length_b 11.056(4) _cell_length_c 27.821(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2886.4(18) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7228 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(Numabs, HIGASHI, T., Rigaku Co.,1999)' _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.949 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 37482 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.8725 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.8725 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 23 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3294 _reflns_number_gt 2849 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1140 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2866 _refine_ls_number_parameters 222 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0022Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.66 _refine_diff_density_min -0.41 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.46062(3) 0.06930(3) 0.174760(10) 0.02902(10) Uani 1.00 1 d . . . N(1) N 0.7123(2) 0.0119(2) 0.01170(7) 0.0411(5) Uani 1.00 1 d . . . N(2) N 0.5426(2) 0.1986(2) 0.04895(7) 0.0396(5) Uani 1.00 1 d . . . N(3) N 0.9370(2) 0.1820(2) 0.09272(7) 0.0411(5) Uani 1.00 1 d . . . N(4) N 0.8416(2) -0.0250(2) 0.14021(6) 0.0340(4) Uani 1.00 1 d . . . C(1) C 0.5292(2) 0.0842(2) 0.06450(7) 0.0304(5) Uani 1.00 1 d . . . C(2) C 0.6152(2) -0.0081(2) 0.04550(7) 0.0346(5) Uani 1.00 1 d . . . C(3) C 0.7251(2) 0.1268(3) -0.00311(9) 0.0462(6) Uani 1.00 1 d . . . C(4) C 0.6420(3) 0.2173(2) 0.01491(8) 0.0459(6) Uani 1.00 1 d . . . C(5) C 0.4223(2) 0.0617(2) 0.10195(8) 0.0321(5) Uani 1.00 1 d . . . C(6) C 0.3882(2) -0.0509(2) 0.12432(8) 0.0378(6) Uani 1.00 1 d . . . C(7) C 0.2813(2) -0.0286(3) 0.15953(9) 0.0458(6) Uani 1.00 1 d . . . C(8) C 0.2501(2) 0.0973(3) 0.15925(9) 0.0466(7) Uani 1.00 1 d . . . C(9) C 0.3369(2) 0.1531(2) 0.12398(8) 0.0398(6) Uani 1.00 1 d . . . C(10) C 0.7865(2) 0.0842(2) 0.15023(7) 0.0275(5) Uani 1.00 1 d . . . C(11) C 0.8348(2) 0.1866(2) 0.12600(7) 0.0355(5) Uani 1.00 1 d . . . C(12) C 0.9892(3) 0.0733(2) 0.08315(9) 0.0400(6) Uani 1.00 1 d . . . C(13) C 0.9421(2) -0.0286(2) 0.10643(9) 0.0381(6) Uani 1.00 1 d . . . C(14) C 0.6745(2) 0.0897(2) 0.18712(7) 0.0311(5) Uani 1.00 1 d . . . C(15) C 0.6206(2) -0.0114(2) 0.21316(7) 0.0371(6) Uani 1.00 1 d . . . C(16) C 0.5121(3) 0.0301(3) 0.24447(8) 0.0448(7) Uani 1.00 1 d . . . C(17) C 0.4982(3) 0.1569(2) 0.23820(8) 0.0443(6) Uani 1.00 1 d . . . C(18) C 0.5982(2) 0.1949(2) 0.20270(8) 0.0371(5) Uani 1.00 1 d . . . H(1) H 0.4299 -0.1270 0.11691 0.0453 Uiso 1.00 1 c . . . H(2) H 0.2387 -0.0878 0.17970 0.0550 Uiso 1.00 1 c . . . H(3) H 0.1834 0.1367 0.17957 0.0558 Uiso 1.00 1 c . . . H(4) H 0.3381 0.2369 0.11634 0.0481 Uiso 1.00 1 c . . . H(5) H 0.6512 -0.0929 0.21000 0.0444 Uiso 1.00 1 c . . . H(6) H 0.4572 -0.0180 0.26583 0.0536 Uiso 1.00 1 c . . . H(7) H 0.4323 0.2075 0.25454 0.0533 Uiso 1.00 1 c . . . H(8) H 0.6115 0.2752 0.19145 0.0445 Uiso 1.00 1 c . . . H(9) H 0.6030 -0.0882 0.05711 0.0415 Uiso 1.00 1 c . . . H(10) H 0.6542 0.2970 0.00285 0.0550 Uiso 1.00 1 c . . . H(11) H 0.7945 0.1455 -0.02681 0.0555 Uiso 1.00 1 c . . . H(12) H 0.7936 0.2627 0.13368 0.0425 Uiso 1.00 1 c . . . H(13) H 1.0614 0.0661 0.05937 0.0479 Uiso 1.00 1 c . . . H(14) H 0.9830 -0.1045 0.09833 0.0461 Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0294(2) 0.0309(2) 0.0267(2) -0.00151(10) 0.00053(10) -0.00165(11) N(1) 0.0417(9) 0.0470(12) 0.0345(9) 0.0025(8) -0.0020(7) -0.0010(8) N(2) 0.0524(11) 0.0306(10) 0.0358(10) 0.0015(8) -0.0055(7) 0.0023(8) N(3) 0.0447(9) 0.0352(10) 0.0435(11) -0.0053(8) 0.0038(8) 0.0044(8) N(4) 0.0364(8) 0.0260(8) 0.0398(10) -0.0002(7) -0.0029(7) 0.0024(7) C(1) 0.0344(10) 0.0312(11) 0.0257(10) -0.0010(7) -0.0084(7) -0.0014(8) C(2) 0.0376(10) 0.0338(11) 0.0323(10) 0.0004(8) -0.0068(8) 0.0015(8) C(3) 0.0462(12) 0.059(2) 0.0336(11) -0.0080(11) 0.0019(10) 0.0055(10) C(4) 0.0603(13) 0.0402(13) 0.0371(12) -0.0087(10) -0.0052(10) 0.0077(10) C(5) 0.0321(9) 0.0352(11) 0.0290(10) -0.0010(7) -0.0061(8) -0.0015(8) C(6) 0.0391(10) 0.0350(11) 0.0392(12) -0.0071(8) -0.0033(9) -0.0047(9) C(7) 0.0372(11) 0.053(2) 0.0466(13) -0.0152(10) 0.0018(10) -0.0014(11) C(8) 0.0285(10) 0.063(2) 0.0481(13) 0.0036(10) -0.0001(10) -0.0035(12) C(9) 0.0351(10) 0.0451(13) 0.0394(12) 0.0080(9) -0.0047(8) -0.0028(9) C(10) 0.0267(9) 0.0266(10) 0.0293(9) -0.0009(7) -0.0064(7) 0.0003(7) C(11) 0.0389(10) 0.0268(10) 0.0407(11) -0.0011(8) 0.0003(8) 0.0019(9) C(12) 0.0358(10) 0.045(1) 0.0390(13) -0.0006(9) 0.0025(9) -0.0019(10) C(13) 0.0355(10) 0.0350(11) 0.0439(12) 0.0044(8) -0.0025(9) -0.0044(10) C(14) 0.0333(10) 0.0314(10) 0.0286(10) -0.0017(8) -0.0043(8) 0.0006(8) C(15) 0.0396(10) 0.0392(12) 0.0325(11) -0.0003(8) -0.0026(8) 0.0076(9) C(16) 0.0497(12) 0.059(2) 0.0260(11) -0.0022(12) 0.0009(9) 0.0066(11) C(17) 0.0500(11) 0.052(2) 0.0313(11) -0.0004(11) 0.0021(10) -0.0132(10) C(18) 0.0420(11) 0.0334(11) 0.0358(11) -0.0028(9) -0.0025(9) -0.0084(9) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) C(5) 2.059(2) yes . . Fe(1) C(6) 2.049(2) yes . . Fe(1) C(7) 2.045(2) yes . . Fe(1) C(8) 2.045(2) yes . . Fe(1) C(9) 2.050(2) yes . . Fe(1) C(14) 2.049(2) yes . . Fe(1) C(15) 2.047(2) yes . . Fe(1) C(16) 2.045(2) yes . . Fe(1) C(17) 2.044(2) yes . . Fe(1) C(18) 2.049(2) yes . . N(1) C(2) 1.328(3) yes . . N(1) C(3) 1.341(3) yes . . N(2) C(1) 1.343(3) yes . . N(2) C(4) 1.345(3) yes . . N(3) C(11) 1.334(3) yes . . N(3) C(12) 1.325(3) yes . . N(4) C(10) 1.342(3) yes . . N(4) C(13) 1.332(3) yes . . C(1) C(2) 1.404(3) yes . . C(1) C(5) 1.468(3) yes . . C(3) C(4) 1.364(4) yes . . C(5) C(6) 1.428(3) yes . . C(5) C(9) 1.428(3) yes . . C(6) C(7) 1.424(3) yes . . C(7) C(8) 1.422(4) yes . . C(8) C(9) 1.416(3) yes . . C(10) C(11) 1.394(3) yes . . C(10) C(14) 1.470(3) yes . . C(12) C(13) 1.373(3) yes . . C(14) C(15) 1.425(3) yes . . C(14) C(18) 1.433(3) yes . . C(15) C(16) 1.416(3) yes . . C(16) C(17) 1.419(4) yes . . C(17) C(18) 1.425(3) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(2) N(1) C(3) 115.9(2) yes . . . C(1) N(2) C(4) 115.9(2) yes . . . C(11) N(3) C(12) 116.1(2) yes . . . C(10) N(4) C(13) 116.5(2) yes . . . C(2) C(1) C(5) 122.5(2) yes . . . C(2) C(1) N(2) 120.6(2) yes . . . C(5) C(1) N(2) 116.9(2) yes . . . N(1) C(2) C(1) 122.7(2) yes . . . C(4) C(3) N(1) 122.1(2) yes . . . N(2) C(4) C(3) 122.8(2) yes . . . C(6) C(5) C(9) 107.7(2) yes . . . C(6) C(5) Fe(1) 69.3(1) yes . . . C(6) C(5) C(1) 127.6(2) yes . . . C(9) C(5) Fe(1) 69.3(1) yes . . . C(9) C(5) C(1) 124.7(2) yes . . . Fe(1) C(5) C(1) 124.9(1) yes . . . C(7) C(6) Fe(1) 69.5(1) yes . . . C(7) C(6) C(5) 107.9(2) yes . . . C(5) C(6) Fe(1) 70.0(1) yes . . . C(8) C(7) Fe(1) 69.7(1) yes . . . C(8) C(7) C(6) 108.1(2) yes . . . C(6) C(7) Fe(1) 69.8(1) yes . . . C(9) C(8) Fe(1) 70.0(1) yes . . . C(9) C(8) C(7) 108.2(2) yes . . . C(7) C(8) Fe(1) 69.6(1) yes . . . C(5) C(9) Fe(1) 70.0(1) yes . . . C(5) C(9) C(8) 108.1(2) yes . . . C(8) C(9) Fe(1) 69.6(1) yes . . . C(11) C(10) C(14) 122.4(2) yes . . . C(11) C(10) N(4) 120.3(2) yes . . . C(14) C(10) N(4) 117.2(2) yes . . . N(3) C(11) C(10) 122.6(2) yes . . . C(13) C(12) N(3) 122.0(2) yes . . . N(4) C(13) C(12) 122.4(2) yes . . . C(15) C(14) C(18) 107.8(2) yes . . . C(15) C(14) Fe(1) 69.6(1) yes . . . C(15) C(14) C(10) 125.2(2) yes . . . C(18) C(14) Fe(1) 69.5(1) yes . . . C(18) C(14) C(10) 127.0(2) yes . . . Fe(1) C(14) C(10) 125.4(1) yes . . . C(16) C(15) Fe(1) 69.7(1) yes . . . C(16) C(15) C(14) 108.3(2) yes . . . C(14) C(15) Fe(1) 69.7(1) yes . . . C(17) C(16) Fe(1) 69.7(1) yes . . . C(17) C(16) C(15) 108.1(2) yes . . . C(15) C(16) Fe(1) 69.8(1) yes . . . C(18) C(17) Fe(1) 69.8(1) yes . . . C(18) C(17) C(16) 108.4(2) yes . . . C(16) C(17) Fe(1) 69.7(1) yes . . . C(14) C(18) Fe(1) 69.5(1) yes . . . C(14) C(18) C(17) 107.5(2) yes . . . C(17) C(18) Fe(1) 69.5(1) yes . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Fe(1) C(1) 3.139(2) yes . 55501 Fe(1) C(5) 2.059(2) yes . 55501 Fe(1) C(6) 2.049(2) yes . 55501 Fe(1) C(7) 2.045(2) yes . 55501 Fe(1) C(8) 2.045(2) yes . 55501 Fe(1) C(9) 2.050(2) yes . 55501 Fe(1) C(10) 3.138(2) yes . 55501 Fe(1) C(14) 2.049(2) yes . 55501 Fe(1) C(15) 2.047(2) yes . 55501 Fe(1) C(16) 2.045(2) yes . 55501 Fe(1) C(17) 2.044(2) yes . 55501 Fe(1) C(18) 2.049(2) yes . 55501 N(1) N(2) 2.806(3) yes . 55501 N(1) C(1) 2.397(3) yes . 55501 N(1) C(1) 3.280(3) yes . 65505 N(1) C(2) 3.461(3) yes . 65505 N(1) C(4) 2.367(3) yes . 55501 N(1) C(4) 3.533(3) yes . 64502 N(1) C(5) 3.501(3) yes . 65505 N(1) C(12) 3.342(3) yes . 55501 N(1) C(13) 3.435(3) yes . 55501 N(2) N(1) 2.806(3) yes . 55501 N(2) C(2) 2.386(3) yes . 55501 N(2) C(3) 2.379(3) yes . 55501 N(2) C(5) 2.395(3) yes . 55501 N(2) C(9) 2.887(3) yes . 55501 N(2) C(11) 3.483(3) yes . 55501 N(2) C(13) 3.417(3) yes . 65502 N(3) N(4) 2.790(3) yes . 55501 N(3) C(3) 3.382(3) yes . 55501 N(3) C(4) 3.536(3) yes . 55501 N(3) C(6) 3.490(3) yes . 65502 N(3) C(8) 3.597(3) yes . 65501 N(3) C(10) 2.392(3) yes . 55501 N(3) C(13) 2.360(3) yes . 55501 N(4) N(3) 2.790(3) yes . 55501 N(4) C(2) 3.390(3) yes . 55501 N(4) C(11) 2.373(3) yes . 55501 N(4) C(12) 2.370(3) yes . 55501 N(4) C(14) 2.401(3) yes . 55501 N(4) C(15) 2.905(3) yes . 55501 N(4) C(18) 3.597(3) yes . 64502 C(1) Fe(1) 3.139(2) yes . 55501 C(1) N(1) 2.397(3) yes . 55501 C(1) N(1) 3.280(3) yes . 65505 C(1) C(2) 3.451(3) yes . 65505 C(1) C(3) 2.671(3) yes . 55501 C(1) C(4) 2.278(3) yes . 55501 C(1) C(6) 2.598(3) yes . 55501 C(1) C(9) 2.565(3) yes . 55501 C(1) C(10) 3.394(3) yes . 55501 C(1) C(11) 3.526(3) yes . 55501 C(2) N(1) 3.461(3) yes . 65505 C(2) N(2) 2.386(3) yes . 55501 C(2) N(4) 3.390(3) yes . 55501 C(2) C(1) 3.451(3) yes . 65505 C(2) C(2) 3.334(3) yes . 65505 C(2) C(3) 2.262(3) yes . 55501 C(2) C(4) 2.645(3) yes . 55501 C(2) C(5) 2.518(3) yes . 55501 C(2) C(6) 3.093(3) yes . 55501 C(2) C(10) 3.480(3) yes . 55501 C(2) C(13) 3.512(3) yes . 55501 C(3) N(2) 2.379(3) yes . 55501 C(3) N(3) 3.382(3) yes . 55501 C(3) C(1) 2.671(3) yes . 55501 C(3) C(2) 2.262(3) yes . 55501 C(3) C(12) 3.500(3) yes . 55501 C(4) N(1) 2.367(3) yes . 55501 C(4) N(1) 3.533(3) yes . 65502 C(4) N(3) 3.536(3) yes . 55501 C(4) C(1) 2.278(3) yes . 55501 C(4) C(2) 2.645(3) yes . 55501 C(4) C(11) 3.597(3) yes . 55501 C(5) Fe(1) 2.059(2) yes . 55501 C(5) N(1) 3.501(3) yes . 65505 C(5) N(2) 2.395(3) yes . 55501 C(5) C(2) 2.518(3) yes . 55501 C(5) C(7) 2.305(3) yes . 55501 C(5) C(8) 2.303(3) yes . 55501 C(5) C(14) 3.363(3) yes . 55501 C(5) C(18) 3.570(3) yes . 55501 C(6) Fe(1) 2.049(2) yes . 55501 C(6) N(3) 3.490(3) yes . 64502 C(6) C(1) 2.598(3) yes . 55501 C(6) C(2) 3.093(3) yes . 55501 C(6) C(8) 2.304(3) yes . 55501 C(6) C(9) 2.307(3) yes . 55501 C(6) C(14) 3.562(3) yes . 55501 C(6) C(15) 3.325(3) yes . 55501 C(7) Fe(1) 2.045(2) yes . 55501 C(7) C(5) 2.305(3) yes . 55501 C(7) C(9) 2.299(4) yes . 55501 C(7) C(15) 3.521(3) yes . 55501 C(7) C(16) 3.271(3) yes . 55501 C(8) Fe(1) 2.045(2) yes . 55501 C(8) C(5) 2.303(3) yes . 55501 C(8) C(6) 2.304(3) yes . 55501 C(8) C(16) 3.495(3) yes . 55501 C(8) C(17) 3.268(3) yes . 55501 C(9) Fe(1) 2.050(2) yes . 55501 C(9) N(2) 2.887(3) yes . 55501 C(9) C(1) 2.565(3) yes . 55501 C(9) C(6) 2.307(3) yes . 55501 C(9) C(7) 2.299(4) yes . 55501 C(9) C(17) 3.520(3) yes . 55501 C(9) C(18) 3.320(3) yes . 55501 C(10) Fe(1) 3.138(2) yes . 55501 C(10) N(3) 2.392(3) yes . 55501 C(10) C(1) 3.394(3) yes . 55501 C(10) C(2) 3.480(3) yes . 55501 C(10) C(12) 2.667(3) yes . 55501 C(10) C(13) 2.274(3) yes . 55501 C(10) C(15) 2.570(3) yes . 55501 C(10) C(18) 2.598(3) yes . 55501 C(11) N(2) 3.483(3) yes . 55501 C(11) N(4) 2.373(3) yes . 55501 C(11) C(1) 3.526(3) yes . 55501 C(11) C(4) 3.597(3) yes . 55501 C(11) C(12) 2.256(3) yes . 55501 C(11) C(13) 2.641(3) yes . 55501 C(11) C(14) 2.510(3) yes . 55501 C(11) C(18) 3.081(3) yes . 55501 C(12) N(1) 3.342(3) yes . 55501 C(12) N(4) 2.370(3) yes . 55501 C(12) C(3) 3.500(3) yes . 55501 C(12) C(8) 3.248(3) yes . 65501 C(12) C(9) 3.565(3) yes . 65501 C(12) C(10) 2.667(3) yes . 55501 C(12) C(11) 2.256(3) yes . 55501 C(13) N(1) 3.435(3) yes . 55501 C(13) N(2) 3.417(3) yes . 64502 C(13) N(3) 2.360(3) yes . 55501 C(13) C(2) 3.512(3) yes . 55501 C(13) C(7) 3.509(3) yes . 65501 C(13) C(8) 3.529(3) yes . 65501 C(13) C(10) 2.274(3) yes . 55501 C(13) C(11) 2.641(3) yes . 55501 C(14) Fe(1) 2.049(2) yes . 55501 C(14) N(4) 2.401(3) yes . 55501 C(14) C(5) 3.363(3) yes . 55501 C(14) C(6) 3.562(3) yes . 55501 C(14) C(11) 2.510(3) yes . 55501 C(14) C(16) 2.302(3) yes . 55501 C(14) C(17) 2.304(3) yes . 55501 C(15) Fe(1) 2.047(2) yes . 55501 C(15) N(4) 2.905(3) yes . 55501 C(15) C(6) 3.325(3) yes . 55501 C(15) C(7) 3.521(3) yes . 55501 C(15) C(10) 2.570(3) yes . 55501 C(15) C(17) 2.295(3) yes . 55501 C(15) C(18) 2.309(3) yes . 55501 C(16) Fe(1) 2.045(2) yes . 55501 C(16) C(7) 3.271(3) yes . 55501 C(16) C(8) 3.495(3) yes . 55501 C(16) C(8) 3.566(3) yes . 55508 C(16) C(14) 2.302(3) yes . 55501 C(16) C(18) 2.306(3) yes . 55501 C(17) Fe(1) 2.044(2) yes . 55501 C(17) C(8) 3.268(3) yes . 55501 C(17) C(9) 3.520(3) yes . 55501 C(17) C(14) 2.304(3) yes . 55501 C(17) C(15) 2.295(3) yes . 55501 C(18) Fe(1) 2.049(2) yes . 55501 C(18) N(4) 3.597(3) yes . 65502 C(18) C(5) 3.570(3) yes . 55501 C(18) C(9) 3.320(3) yes . 55501 C(18) C(10) 2.598(3) yes . 55501 C(18) C(11) 3.081(3) yes . 55501 C(18) C(15) 2.309(3) yes . 55501 C(18) C(16) 2.306(3) yes . 55501 #-----------END data_L2 _database_code_depnum_ccdc_archive 'CCDC 262866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,1'-(2-pyrimidyl)ferrocene ; _chemical_name_common 1,1'-(2-pyrimidyl)ferrocene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 Fe N4' _chemical_formula_weight 342.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.5306(19) _cell_length_b 5.9972(6) _cell_length_c 12.6084(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1476.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red-orange _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4272 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; SADABS; Sheldrick, 1996 ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10278 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2796 _reflns_number_gt 2599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.1340P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.276(19) _refine_ls_number_reflns 2796 _refine_ls_number_parameters 208 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.202845(13) 0.51712(4) 0.81202(5) 0.03342(10) Uani 1 1 d . . . C1 C 0.21667(13) 0.3794(4) 0.9589(2) 0.0393(5) Uani 1 1 d . . . C2 C 0.24971(12) 0.2475(4) 0.8798(2) 0.0451(6) Uani 1 1 d . . . C3 C 0.29831(12) 0.3838(6) 0.8279(3) 0.0565(9) Uani 1 1 d . . . C4 C 0.29555(13) 0.6005(7) 0.8743(3) 0.0600(9) Uani 1 1 d . . . C5 C 0.24505(14) 0.5990(5) 0.9540(3) 0.0500(6) Uani 1 1 d . . . C6 C 0.10043(12) 0.5340(4) 0.7752(2) 0.0356(5) Uani 1 1 d . . . C7 C 0.13680(12) 0.4024(4) 0.6991(2) 0.0397(5) Uani 1 1 d . . . C8 C 0.18726(16) 0.5401(5) 0.6519(3) 0.0453(6) Uani 1 1 d . . . C9 C 0.18341(13) 0.7555(4) 0.6990(2) 0.0438(6) Uani 1 1 d . . . C10 C 0.12992(12) 0.7522(4) 0.7756(2) 0.0393(5) Uani 1 1 d . . . C11 C 0.16262(13) 0.3019(4) 1.0302(2) 0.0380(5) Uani 1 1 d . . . C12 C 0.0879(2) 0.3720(6) 1.1619(3) 0.0708(10) Uani 1 1 d . . . C13 C 0.06183(16) 0.1607(6) 1.1552(3) 0.0637(8) Uani 1 1 d . . . C14 C 0.09252(19) 0.0238(5) 1.0836(3) 0.0595(8) Uani 1 1 d . . . C15 C 0.04430(12) 0.4569(4) 0.8423(2) 0.0361(5) Uani 1 1 d . . . C16 C -0.03617(18) 0.5325(5) 0.9651(3) 0.0603(9) Uani 1 1 d . . . C17 C -0.05937(14) 0.3178(6) 0.9627(3) 0.0573(7) Uani 1 1 d . . . C18 C -0.02644(15) 0.1777(5) 0.8938(3) 0.0543(7) Uani 1 1 d . . . N1 N 0.14308(12) 0.0904(4) 1.0201(2) 0.0507(5) Uani 1 1 d . . . N2 N 0.13798(16) 0.4481(4) 1.1007(2) 0.0597(7) Uani 1 1 d . . . N3 N 0.02483(11) 0.2437(3) 0.8319(2) 0.0469(5) Uani 1 1 d . . . N4 N 0.01556(12) 0.6068(4) 0.9069(2) 0.0529(6) Uani 1 1 d . . . H1 H 0.2408 0.0984 0.8650 0.054 Uiso 1 1 calc R . . H2 H 0.3271 0.3399 0.7730 0.068 Uiso 1 1 calc R . . H3 H 0.3225 0.7219 0.8552 0.072 Uiso 1 1 calc R . . H4 H 0.2324 0.7196 0.9960 0.060 Uiso 1 1 calc R . . H5 H 0.1287 0.2532 0.6833 0.048 Uiso 1 1 calc R . . H6 H 0.2178 0.4970 0.5991 0.054 Uiso 1 1 calc R . . H7 H 0.2110 0.8770 0.6826 0.053 Uiso 1 1 calc R . . H8 H 0.1165 0.8708 0.8183 0.047 Uiso 1 1 calc R . . H9 H 0.0695 0.4679 1.2123 0.085 Uiso 1 1 calc R . . H10 H 0.0254 0.1136 1.1971 0.076 Uiso 1 1 calc R . . H11 H 0.0775 -0.1230 1.0787 0.071 Uiso 1 1 calc R . . H12 H -0.0580 0.6326 1.0102 0.072 Uiso 1 1 calc R . . H13 H -0.0953 0.2696 1.0053 0.069 Uiso 1 1 calc R . . H14 H -0.0405 0.0298 0.8901 0.065 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 0.02991(15) 0.03652(16) 0.03383(17) 0.0016(2) 0.00197(17) 0.00300(9) C1 0.0393(11) 0.0412(12) 0.0373(13) 0.0029(10) -0.0090(10) 0.0027(9) C2 0.0408(12) 0.0490(14) 0.0455(14) 0.0045(11) 0.0005(11) 0.0135(10) C3 0.0342(12) 0.0739(18) 0.062(2) 0.0156(19) 0.0053(13) 0.0131(11) C4 0.0366(14) 0.072(2) 0.072(2) 0.0140(19) -0.0094(14) -0.0113(12) C5 0.0486(14) 0.0481(13) 0.0533(17) -0.0002(13) -0.0146(13) -0.0097(11) C6 0.0339(11) 0.0377(11) 0.0352(12) 0.0009(9) -0.0020(9) 0.0049(8) C7 0.0433(12) 0.0425(13) 0.0332(12) -0.0037(10) -0.0027(10) 0.0064(9) C8 0.0488(14) 0.0554(14) 0.0318(13) 0.0011(12) 0.0049(12) 0.0095(11) C9 0.0468(12) 0.0428(13) 0.0419(14) 0.0091(11) 0.0047(11) 0.0045(10) C10 0.0396(11) 0.0368(11) 0.0416(12) 0.0015(10) 0.0030(10) 0.0066(8) C11 0.0436(12) 0.0417(12) 0.0285(11) 0.0018(9) -0.0063(10) 0.0057(9) C12 0.088(2) 0.072(2) 0.053(2) 0.0036(17) 0.0260(19) 0.0177(18) C13 0.0580(17) 0.077(2) 0.056(2) 0.0192(17) 0.0090(16) 0.0035(15) C14 0.064(2) 0.0548(17) 0.060(2) 0.0120(15) -0.0031(17) -0.0095(13) C15 0.0288(10) 0.0422(11) 0.0372(13) 0.0001(9) -0.0039(9) 0.0041(8) C16 0.0558(17) 0.0639(18) 0.061(2) -0.0125(16) 0.0206(16) -0.0001(13) C17 0.0432(14) 0.0722(19) 0.0565(19) 0.0028(16) 0.0100(14) -0.0089(12) C18 0.0474(14) 0.0484(14) 0.067(2) 0.0022(14) 0.0031(14) -0.0063(11) N1 0.0583(13) 0.0453(12) 0.0486(14) 0.0006(11) 0.0045(12) -0.0042(10) N2 0.0828(19) 0.0489(13) 0.0475(15) -0.0027(12) 0.0178(15) 0.0042(12) N3 0.0431(10) 0.0425(10) 0.0551(15) -0.0035(10) 0.0020(11) -0.0002(8) N4 0.0519(12) 0.0482(12) 0.0586(15) -0.0105(12) 0.0148(12) -0.0035(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 Fe1 C5 2.031(3) . ? Fe1 C4 2.036(3) . ? Fe1 C3 2.039(2) . ? Fe1 C7 2.041(3) . ? Fe1 C2 2.045(2) . ? Fe1 C1 2.046(3) . ? Fe1 C8 2.046(3) . ? Fe1 C9 2.053(3) . ? Fe1 C10 2.056(2) . ? Fe1 C6 2.056(2) . ? C1 C2 1.427(4) . ? C1 C5 1.431(4) . ? C1 C11 1.462(4) . ? C3 C2 1.413(4) . ? C3 C4 1.426(6) . ? C4 C5 1.408(5) . ? C6 C10 1.430(3) . ? C6 C7 1.431(4) . ? C6 C15 1.460(4) . ? C7 C8 1.416(4) . ? C10 C9 1.422(3) . ? C13 C12 1.368(5) . ? C14 C13 1.360(6) . ? C17 C16 1.365(4) . ? C17 C18 1.369(5) . ? C9 C8 1.424(4) . ? N1 C11 1.331(4) . ? N1 C14 1.332(5) . ? N2 C12 1.326(4) . ? N2 C11 1.339(4) . ? N3 C18 1.330(4) . ? N3 C15 1.340(3) . ? N4 C16 1.326(4) . ? N4 C15 1.337(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 C5 Fe1 C4 40.51(15) . . ? C5 Fe1 C3 68.73(15) . . ? C4 Fe1 C3 40.98(18) . . ? C5 Fe1 C7 162.38(11) . . ? C4 Fe1 C7 156.06(15) . . ? C3 Fe1 C7 120.95(14) . . ? C5 Fe1 C2 68.99(12) . . ? C4 Fe1 C2 68.59(13) . . ? C3 Fe1 C2 40.49(12) . . ? C7 Fe1 C2 107.92(11) . . ? C5 Fe1 C1 41.09(11) . . ? C4 Fe1 C1 68.44(14) . . ? C3 Fe1 C1 68.41(14) . . ? C7 Fe1 C1 125.38(11) . . ? C2 Fe1 C1 40.85(11) . . ? C5 Fe1 C8 156.01(12) . . ? C4 Fe1 C8 119.76(14) . . ? C3 Fe1 C8 105.02(15) . . ? C7 Fe1 C8 40.55(12) . . ? C2 Fe1 C8 122.13(12) . . ? C1 Fe1 C8 160.04(11) . . ? C5 Fe1 C9 121.20(12) . . ? C4 Fe1 C9 105.13(14) . . ? C3 Fe1 C9 120.67(13) . . ? C7 Fe1 C9 68.52(11) . . ? C2 Fe1 C9 157.35(11) . . ? C1 Fe1 C9 158.99(11) . . ? C8 Fe1 C9 40.65(11) . . ? C5 Fe1 C10 108.20(12) . . ? C4 Fe1 C10 122.28(14) . . ? C3 Fe1 C10 157.58(12) . . ? C7 Fe1 C10 68.74(10) . . ? C2 Fe1 C10 161.02(11) . . ? C1 Fe1 C10 124.80(11) . . ? C8 Fe1 C10 68.30(11) . . ? C9 Fe1 C10 40.50(10) . . ? C5 Fe1 C6 125.61(12) . . ? C4 Fe1 C6 160.11(14) . . ? C3 Fe1 C6 158.63(13) . . ? C7 Fe1 C6 40.89(10) . . ? C2 Fe1 C6 124.66(10) . . ? C1 Fe1 C6 110.66(11) . . ? C8 Fe1 C6 68.22(12) . . ? C9 Fe1 C6 68.23(10) . . ? C10 Fe1 C6 40.70(9) . . ? C18 N3 C15 116.1(2) . . ? C2 C1 C5 107.7(3) . . ? C2 C1 C11 125.4(2) . . ? C5 C1 C11 126.8(3) . . ? C2 C1 Fe1 69.54(15) . . ? C5 C1 Fe1 68.89(16) . . ? C11 C1 Fe1 126.11(17) . . ? C12 N2 C11 115.2(3) . . ? C2 C3 C4 108.2(3) . . ? C2 C3 Fe1 69.99(13) . . ? C4 C3 Fe1 69.41(15) . . ? C10 C6 C7 107.9(2) . . ? C10 C6 C15 126.2(2) . . ? C7 C6 C15 125.9(2) . . ? C10 C6 Fe1 69.65(13) . . ? C7 C6 Fe1 69.00(13) . . ? C15 C6 Fe1 125.74(18) . . ? C9 C10 C6 107.8(2) . . ? C9 C10 Fe1 69.66(13) . . ? C6 C10 Fe1 69.65(13) . . ? C8 C7 C6 107.8(2) . . ? C8 C7 Fe1 69.90(17) . . ? C6 C7 Fe1 70.11(14) . . ? C16 C17 C18 115.9(3) . . ? C16 N4 C15 115.6(3) . . ? C10 C9 C8 108.0(2) . . ? C10 C9 Fe1 69.84(14) . . ? C8 C9 Fe1 69.39(16) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 Fe1 69.51(15) . . ? C1 C2 Fe1 69.61(14) . . ? N3 C18 C17 122.9(3) . . ? C11 N1 C14 116.2(3) . . ? N1 C14 C13 123.0(3) . . ? C5 C4 C3 108.3(3) . . ? C5 C4 Fe1 69.55(15) . . ? C3 C4 Fe1 69.61(17) . . ? C14 C13 C12 115.8(3) . . ? N1 C11 N2 125.8(3) . . ? N1 C11 C1 116.8(2) . . ? N2 C11 C1 117.4(2) . . ? N2 C12 C13 123.9(3) . . ? C4 C5 C1 107.9(3) . . ? C4 C5 Fe1 69.94(19) . . ? C1 C5 Fe1 70.02(15) . . ? N4 C16 C17 123.9(3) . . ? N4 C15 N3 125.6(2) . . ? N4 C15 C6 117.1(2) . . ? N3 C15 C6 117.3(2) . . ? C7 C8 C9 108.5(2) . . ? C7 C8 Fe1 69.55(16) . . ? C9 C8 Fe1 69.96(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.377 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.054 #-----------END data_1 _database_code_depnum_ccdc_archive 'CCDC 262867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H34 Cu2 Fe N4 O8' _chemical_formula_weight 953.70 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7964(9) _cell_length_b 13.3969(9) _cell_length_c 14.1537(10) _cell_angle_alpha 65.381(2) _cell_angle_beta 72.5220(10) _cell_angle_gamma 76.844(2) _cell_volume 2089.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7656 _exptl_absorpt_correction_T_max 0.7656 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; SADABS; Sheldrick, 1996 ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15734 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10274 _reflns_number_gt 7017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.4111P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10274 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.0977 _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 C1 C -0.0459(2) 1.1220(2) 0.1203(2) 0.0481(7) Uani 1 1 d . . . C2 C -0.0234(3) 1.2286(2) 0.1007(2) 0.0593(8) Uani 1 1 d . . . H2 H 0.0464 1.2506 0.0814 0.071 Uiso 1 1 calc R . . C3 C -0.1241(3) 1.2955(3) 0.1154(3) 0.0704(10) Uani 1 1 d . . . H3 H -0.1326 1.3693 0.1072 0.084 Uiso 1 1 calc R . . C4 C -0.2094(3) 1.2312(3) 0.1446(3) 0.0731(11) Uani 1 1 d . . . H4 H -0.2845 1.2552 0.1594 0.088 Uiso 1 1 calc R . . C5 C -0.1624(3) 1.1237(3) 0.1478(2) 0.0609(8) Uani 1 1 d . . . H5 H -0.2008 1.0650 0.1648 0.073 Uiso 1 1 calc R . . C6 C -0.0487(3) 1.0442(2) 0.3767(2) 0.0459(7) Uani 1 1 d . . . C7 C -0.0233(3) 1.1515(2) 0.3540(2) 0.0570(8) Uani 1 1 d . . . H7 H 0.0468 1.1732 0.3334 0.068 Uiso 1 1 calc R . . C8 C -0.1253(4) 1.2188(3) 0.3689(3) 0.0713(10) Uani 1 1 d . . . H8 H -0.1337 1.2927 0.3602 0.086 Uiso 1 1 calc R . . C9 C -0.2111(3) 1.1550(3) 0.3988(3) 0.0674(10) Uani 1 1 d . . . H9 H -0.2861 1.1795 0.4133 0.081 Uiso 1 1 calc R . . C10 C -0.1644(3) 1.0469(2) 0.4035(2) 0.0555(8) Uani 1 1 d . . . H10 H -0.2032 0.9883 0.4210 0.067 Uiso 1 1 calc R . . C11 C 0.0360(2) 1.0265(2) 0.1134(2) 0.0424(6) Uani 1 1 d . . . C12 C 0.0771(3) 0.8456(3) 0.1375(3) 0.0602(8) Uani 1 1 d . . . H12 H 0.0552 0.7765 0.1586 0.072 Uiso 1 1 calc R . . C13 C 0.1880(3) 0.8573(2) 0.1000(2) 0.0515(7) Uani 1 1 d . . . H13 H 0.2384 0.7961 0.0963 0.062 Uiso 1 1 calc R . . C14 C 0.1476(2) 1.0379(2) 0.0754(2) 0.0450(6) Uani 1 1 d . . . H14 H 0.1698 1.1072 0.0536 0.054 Uiso 1 1 calc R . . C15 C 0.0357(2) 0.9495(2) 0.3727(2) 0.0408(6) Uani 1 1 d . . . C16 C 0.2154(3) 0.8838(2) 0.3297(3) 0.0584(8) Uani 1 1 d . . . H16 H 0.2890 0.8958 0.2997 0.070 Uiso 1 1 calc R . . C17 C 0.1890(2) 0.7775(2) 0.3712(2) 0.0481(7) Uani 1 1 d . . . H17 H 0.2448 0.7195 0.3701 0.058 Uiso 1 1 calc R . . C18 C 0.0089(2) 0.8425(2) 0.4128(2) 0.0414(6) Uani 1 1 d . . . H18 H -0.0649 0.8306 0.4406 0.050 Uiso 1 1 calc R . . C19 C 0.5399(2) 0.9279(2) -0.1480(2) 0.0419(6) Uani 1 1 d . . . C20 C 0.5701(2) 0.8791(2) -0.2313(2) 0.0465(7) Uani 1 1 d . . . C21 C 0.4899(3) 0.8597(4) -0.2649(4) 0.1045(17) Uani 1 1 d . . . H21 H 0.4160 0.8779 -0.2362 0.125 Uiso 1 1 calc R . . C22 C 0.5176(4) 0.8135(5) -0.3406(5) 0.147(3) Uani 1 1 d . . . H22 H 0.4620 0.7995 -0.3617 0.176 Uiso 1 1 calc R . . C23 C 0.6244(5) 0.7881(4) -0.3851(4) 0.1047(16) Uani 1 1 d . . . H23 H 0.6424 0.7587 -0.4378 0.126 Uiso 1 1 calc R . . C24 C 0.7040(3) 0.8060(3) -0.3522(3) 0.0749(11) Uani 1 1 d . . . H24 H 0.7777 0.7861 -0.3801 0.090 Uiso 1 1 calc R . . C25 C 0.6771(3) 0.8540(3) -0.2770(3) 0.0580(8) Uani 1 1 d . . . H25 H 0.7331 0.8693 -0.2574 0.070 Uiso 1 1 calc R . . C26 C 0.5511(3) 0.8021(2) 0.1162(2) 0.0453(7) Uani 1 1 d . . . C27 C 0.5850(3) 0.6817(2) 0.1730(2) 0.0487(7) Uani 1 1 d . . . C28 C 0.5089(3) 0.6081(2) 0.2154(3) 0.0645(9) Uani 1 1 d . . . H28 H 0.4360 0.6331 0.2107 0.077 Uiso 1 1 calc R . . C29 C 0.5408(4) 0.4961(3) 0.2653(3) 0.0850(12) Uani 1 1 d . . . H29 H 0.4894 0.4458 0.2933 0.102 Uiso 1 1 calc R . . C30 C 0.6481(4) 0.4598(3) 0.2733(3) 0.0885(14) Uani 1 1 d . . . H30 H 0.6692 0.3848 0.3070 0.106 Uiso 1 1 calc R . . C31 C 0.7237(4) 0.5323(3) 0.2326(3) 0.0791(12) Uani 1 1 d . . . H31 H 0.7962 0.5069 0.2388 0.095 Uiso 1 1 calc R . . C32 C 0.6929(3) 0.6445(3) 0.1815(2) 0.0588(8) Uani 1 1 d . . . H32 H 0.7447 0.6943 0.1533 0.071 Uiso 1 1 calc R . . C33 C 0.0983(3) 0.4887(2) 0.3194(2) 0.0495(7) Uani 1 1 d . . . C34 C 0.1674(3) 0.4804(2) 0.2166(2) 0.0498(7) Uani 1 1 d . . . C35 C 0.1437(4) 0.4163(3) 0.1735(3) 0.0743(11) Uani 1 1 d . . . H35 H 0.0813 0.3793 0.2068 0.089 Uiso 1 1 calc R . . C36 C 0.2117(4) 0.4059(3) 0.0808(3) 0.0928(14) Uani 1 1 d . . . H36 H 0.1942 0.3626 0.0519 0.111 Uiso 1 1 calc R . . C37 C 0.3031(4) 0.4579(3) 0.0318(3) 0.0858(12) Uani 1 1 d . . . H37 H 0.3496 0.4489 -0.0294 0.103 Uiso 1 1 calc R . . C38 C 0.3270(4) 0.5240(4) 0.0728(3) 0.0889(13) Uani 1 1 d . . . H38 H 0.3894 0.5610 0.0389 0.107 Uiso 1 1 calc R . . C39 C 0.2583(3) 0.5357(3) 0.1645(3) 0.0721(10) Uani 1 1 d . . . H39 H 0.2741 0.5818 0.1913 0.086 Uiso 1 1 calc R . . C40 C 0.1761(3) 0.4020(2) 0.5595(2) 0.0478(7) Uani 1 1 d . . . C41 C 0.2792(3) 0.3344(2) 0.5884(2) 0.0493(7) Uani 1 1 d . . . C42 C 0.2778(3) 0.2242(3) 0.6549(3) 0.0650(9) Uani 1 1 d . . . H42 H 0.2115 0.1937 0.6841 0.078 Uiso 1 1 calc R . . C43 C 0.3739(4) 0.1592(3) 0.6784(3) 0.0838(12) Uani 1 1 d . . . H43 H 0.3721 0.0860 0.7257 0.101 Uiso 1 1 calc R . . C44 C 0.4707(4) 0.2026(4) 0.6323(4) 0.0876(13) Uani 1 1 d . . . H44 H 0.5360 0.1577 0.6450 0.105 Uiso 1 1 calc R . . C45 C 0.4740(3) 0.3119(4) 0.5669(3) 0.0769(11) Uani 1 1 d . . . H45 H 0.5410 0.3412 0.5371 0.092 Uiso 1 1 calc R . . C46 C 0.3776(3) 0.3784(3) 0.5455(3) 0.0613(8) Uani 1 1 d . . . H46 H 0.3794 0.4528 0.5021 0.074 Uiso 1 1 calc R . . Cu1 Cu 0.39714(3) 0.98062(2) 0.02406(3) 0.03869(9) Uani 1 1 d . . . Cu2 Cu 0.03991(3) 0.59222(2) 0.47346(3) 0.04373(10) Uani 1 1 d . . . Fe1 Fe -0.11319(4) 1.16040(3) 0.25291(3) 0.04788(12) Uani 1 1 d . . . N1 N 0.0007(2) 0.9289(2) 0.1449(2) 0.0545(6) Uani 1 1 d . . . N2 N 0.22428(19) 0.95394(18) 0.06885(17) 0.0430(5) Uani 1 1 d . . . N3 N 0.1402(2) 0.96972(19) 0.3306(2) 0.0544(6) Uani 1 1 d . . . N4 N 0.08489(19) 0.75678(17) 0.41298(17) 0.0406(5) Uani 1 1 d . . . O1 O 0.44173(16) 0.93074(17) -0.09617(17) 0.0537(5) Uani 1 1 d . . . O2 O 0.61643(16) 0.96204(16) -0.13521(15) 0.0486(5) Uani 1 1 d . . . O3 O 0.45154(18) 0.83201(15) 0.11449(17) 0.0570(5) Uani 1 1 d . . . O4 O 0.62646(17) 0.86462(15) 0.07181(15) 0.0505(5) Uani 1 1 d . . . O5 O 0.10877(19) 0.56954(16) 0.33858(16) 0.0598(6) Uani 1 1 d . . . O6 O 0.03667(19) 0.41513(16) 0.38053(16) 0.0576(5) Uani 1 1 d . . . O7 O 0.17074(18) 0.50505(16) 0.52518(18) 0.0586(5) Uani 1 1 d . . . O8 O 0.10055(18) 0.34974(16) 0.57024(18) 0.0601(6) 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 C1 0.0379(15) 0.0580(17) 0.0410(15) -0.0145(13) -0.0102(12) 0.0019(13) C2 0.0523(19) 0.0471(17) 0.0584(19) -0.0092(14) -0.0058(15) 0.0016(14) C3 0.073(3) 0.0529(19) 0.056(2) -0.0063(15) -0.0134(18) 0.0166(18) C4 0.049(2) 0.091(3) 0.061(2) -0.0228(19) -0.0208(17) 0.024(2) C5 0.0451(18) 0.081(2) 0.0561(19) -0.0261(17) -0.0174(15) 0.0026(16) C6 0.0615(19) 0.0324(13) 0.0410(15) -0.0112(11) -0.0149(14) -0.0012(13) C7 0.075(2) 0.0375(15) 0.064(2) -0.0177(14) -0.0310(18) -0.0010(15) C8 0.105(3) 0.0432(17) 0.067(2) -0.0248(16) -0.031(2) 0.0129(19) C9 0.071(2) 0.058(2) 0.0553(19) -0.0226(16) -0.0042(17) 0.0142(18) C10 0.0554(19) 0.0490(16) 0.0500(17) -0.0152(14) -0.0028(15) -0.0028(14) C11 0.0381(15) 0.0509(15) 0.0376(14) -0.0153(12) -0.0103(12) -0.0050(12) C12 0.061(2) 0.0522(18) 0.074(2) -0.0277(16) -0.0116(17) -0.0179(16) C13 0.0530(19) 0.0478(16) 0.0579(18) -0.0265(14) -0.0118(15) -0.0022(14) C14 0.0435(16) 0.0426(14) 0.0487(16) -0.0175(13) -0.0094(13) -0.0056(12) C15 0.0510(17) 0.0328(12) 0.0383(14) -0.0085(11) -0.0161(12) -0.0057(12) C16 0.0406(17) 0.0528(18) 0.066(2) -0.0044(15) -0.0121(15) -0.0113(14) C17 0.0442(17) 0.0418(15) 0.0480(16) -0.0099(12) -0.0110(13) 0.0013(13) C18 0.0428(15) 0.0383(13) 0.0413(14) -0.0143(12) -0.0052(12) -0.0090(12) C19 0.0477(17) 0.0341(13) 0.0427(14) -0.0160(11) -0.0093(13) -0.0014(12) C20 0.0478(17) 0.0448(15) 0.0534(16) -0.0278(13) -0.0066(14) -0.0058(13) C21 0.061(2) 0.155(4) 0.162(4) -0.132(4) -0.028(3) 0.009(3) C22 0.084(4) 0.231(7) 0.237(7) -0.201(6) -0.043(4) 0.003(4) C23 0.119(4) 0.128(4) 0.110(4) -0.095(3) -0.015(3) -0.013(3) C24 0.074(3) 0.079(2) 0.075(2) -0.049(2) 0.012(2) -0.016(2) C25 0.057(2) 0.066(2) 0.0586(19) -0.0341(16) -0.0016(15) -0.0152(16) C26 0.0554(19) 0.0370(14) 0.0384(14) -0.0160(12) -0.0083(13) 0.0044(13) C27 0.065(2) 0.0360(14) 0.0383(14) -0.0152(12) -0.0094(14) 0.0054(14) C28 0.077(2) 0.0417(16) 0.059(2) -0.0121(14) -0.0067(18) -0.0021(16) C29 0.109(4) 0.0437(19) 0.075(3) -0.0077(17) -0.005(2) -0.008(2) C30 0.130(4) 0.0411(19) 0.068(2) -0.0091(17) -0.023(3) 0.016(2) C31 0.096(3) 0.058(2) 0.072(2) -0.0248(19) -0.031(2) 0.028(2) C32 0.073(2) 0.0493(17) 0.0523(18) -0.0234(14) -0.0199(17) 0.0111(16) C33 0.0571(19) 0.0408(15) 0.0478(16) -0.0181(13) -0.0137(14) 0.0041(14) C34 0.0590(19) 0.0433(15) 0.0432(15) -0.0179(13) -0.0063(14) -0.0026(14) C35 0.102(3) 0.072(2) 0.055(2) -0.0327(18) 0.003(2) -0.034(2) C36 0.137(4) 0.093(3) 0.065(2) -0.051(2) 0.005(3) -0.041(3) C37 0.105(3) 0.091(3) 0.058(2) -0.042(2) 0.006(2) -0.010(3) C38 0.075(3) 0.114(3) 0.076(3) -0.045(3) 0.013(2) -0.030(2) C39 0.070(2) 0.086(3) 0.071(2) -0.046(2) -0.0015(19) -0.017(2) C40 0.0527(18) 0.0477(16) 0.0456(16) -0.0224(13) -0.0102(14) -0.0031(14) C41 0.0507(18) 0.0556(17) 0.0474(16) -0.0269(14) -0.0150(14) 0.0028(14) C42 0.072(2) 0.064(2) 0.060(2) -0.0179(17) -0.0276(18) -0.0021(18) C43 0.092(3) 0.074(3) 0.083(3) -0.017(2) -0.049(3) 0.011(2) C44 0.077(3) 0.103(3) 0.090(3) -0.042(3) -0.046(3) 0.021(3) C45 0.056(2) 0.108(3) 0.078(3) -0.046(2) -0.020(2) -0.002(2) C46 0.060(2) 0.072(2) 0.0575(19) -0.0315(17) -0.0148(17) -0.0045(18) Cu1 0.03587(18) 0.03517(17) 0.04356(18) -0.01710(14) -0.00594(14) -0.00131(13) Cu2 0.0510(2) 0.03219(17) 0.0478(2) -0.01783(14) -0.00685(16) -0.00511(14) Fe1 0.0480(3) 0.0405(2) 0.0471(2) -0.01317(18) -0.01167(19) 0.00439(18) N1 0.0454(15) 0.0582(15) 0.0618(16) -0.0248(13) -0.0090(12) -0.0101(12) N2 0.0409(13) 0.0436(12) 0.0446(12) -0.0192(10) -0.0087(10) -0.0015(10) N3 0.0502(15) 0.0392(12) 0.0629(16) -0.0026(11) -0.0183(13) -0.0102(11) N4 0.0452(13) 0.0342(11) 0.0411(12) -0.0147(9) -0.0063(10) -0.0060(10) O1 0.0413(12) 0.0631(13) 0.0680(13) -0.0421(11) -0.0063(10) -0.0014(10) O2 0.0491(12) 0.0572(12) 0.0461(11) -0.0282(9) -0.0008(9) -0.0154(10) O3 0.0519(13) 0.0345(10) 0.0710(14) -0.0086(9) -0.0162(11) 0.0010(9) O4 0.0496(12) 0.0401(10) 0.0515(12) -0.0107(9) -0.0129(10) 0.0028(9) O5 0.0806(16) 0.0464(11) 0.0518(12) -0.0263(10) 0.0011(11) -0.0130(11) O6 0.0718(15) 0.0515(12) 0.0489(12) -0.0253(10) 0.0024(11) -0.0152(11) O7 0.0560(13) 0.0453(12) 0.0770(15) -0.0244(11) -0.0192(11) -0.0024(10) O8 0.0594(14) 0.0454(11) 0.0793(15) -0.0213(11) -0.0247(12) -0.0057(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 C1 C2 1.417(4) . ? C1 C5 1.421(4) . ? C1 C11 1.476(4) . ? C1 Fe1 2.040(3) . ? C2 C3 1.406(4) . ? C2 Fe1 2.036(3) . ? C3 C4 1.402(5) . ? C3 Fe1 2.049(3) . ? C4 C5 1.416(5) . ? C4 Fe1 2.039(3) . ? C5 Fe1 2.041(3) . ? C6 C10 1.410(4) . ? C6 C7 1.429(4) . ? C6 C15 1.476(4) . ? C6 Fe1 2.046(3) . ? C7 C8 1.421(5) . ? C7 Fe1 2.042(3) . ? C8 C9 1.400(5) . ? C8 Fe1 2.048(3) . ? C9 C10 1.418(4) . ? C9 Fe1 2.050(3) . ? C10 Fe1 2.049(3) . ? C11 N1 1.333(4) . ? C11 C14 1.386(4) . ? C12 N1 1.323(4) . ? C12 C13 1.377(4) . ? C13 N2 1.328(4) . ? C14 N2 1.329(3) . ? C15 N3 1.330(4) . ? C15 C18 1.386(3) . ? C16 N3 1.324(4) . ? C16 C17 1.374(4) . ? C17 N4 1.327(4) . ? C18 N4 1.325(3) . ? C19 O1 1.251(3) . ? C19 O2 1.257(3) . ? C19 C20 1.491(4) . ? C20 C25 1.359(4) . ? C20 C21 1.365(5) . ? C21 C22 1.372(6) . ? C22 C23 1.353(6) . ? C23 C24 1.343(6) . ? C24 C25 1.383(4) . ? C26 O3 1.249(3) . ? C26 O4 1.262(3) . ? C26 C27 1.499(4) . ? C27 C28 1.369(5) . ? C27 C32 1.380(4) . ? C28 C29 1.389(4) . ? C29 C30 1.370(6) . ? C30 C31 1.355(6) . ? C31 C32 1.391(4) . ? C33 O6 1.255(4) . ? C33 O5 1.264(3) . ? C33 C34 1.494(4) . ? C34 C35 1.367(4) . ? C34 C39 1.367(5) . ? C35 C36 1.381(5) . ? C36 C37 1.347(6) . ? C37 C38 1.368(5) . ? C38 C39 1.380(5) . ? C40 O7 1.251(3) . ? C40 O8 1.257(4) . ? C40 C41 1.483(4) . ? C41 C46 1.372(5) . ? C41 C42 1.381(4) . ? C42 C43 1.377(5) . ? C43 C44 1.351(6) . ? C44 C45 1.370(6) . ? C45 C46 1.381(5) . ? Cu1 O4 1.9616(18) 2_675 ? Cu1 O1 1.9643(19) . ? Cu1 O3 1.9667(19) . ? Cu1 O2 1.9690(18) 2_675 ? Cu1 N2 2.180(2) . ? Cu1 Cu1 2.6295(7) 2_675 ? Cu2 O7 1.959(2) . ? Cu2 O8 1.962(2) 2_566 ? Cu2 O5 1.9657(19) . ? Cu2 O6 1.9745(19) 2_566 ? Cu2 N4 2.153(2) . ? Cu2 Cu2 2.6180(6) 2_566 ? O2 Cu1 1.9690(18) 2_675 ? O4 Cu1 1.9616(18) 2_675 ? O6 Cu2 1.9745(19) 2_566 ? O8 Cu2 1.962(2) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.4(3) . . ? C2 C1 C11 126.6(3) . . ? C5 C1 C11 126.0(3) . . ? C2 C1 Fe1 69.51(18) . . ? C5 C1 Fe1 69.66(17) . . ? C11 C1 Fe1 126.10(19) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe1 70.36(19) . . ? C1 C2 Fe1 69.81(17) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Fe1 69.6(2) . . ? C2 C3 Fe1 69.38(17) . . ? C3 C4 C5 108.8(3) . . ? C3 C4 Fe1 70.3(2) . . ? C5 C4 Fe1 69.77(18) . . ? C4 C5 C1 107.4(3) . . ? C4 C5 Fe1 69.6(2) . . ? C1 C5 Fe1 69.58(18) . . ? C10 C6 C7 108.2(3) . . ? C10 C6 C15 128.1(3) . . ? C7 C6 C15 123.6(3) . . ? C10 C6 Fe1 69.97(17) . . ? C7 C6 Fe1 69.40(16) . . ? C15 C6 Fe1 126.87(19) . . ? C8 C7 C6 107.0(3) . . ? C8 C7 Fe1 69.86(19) . . ? C6 C7 Fe1 69.67(16) . . ? C9 C8 C7 108.4(3) . . ? C9 C8 Fe1 70.1(2) . . ? C7 C8 Fe1 69.46(18) . . ? C8 C9 C10 108.5(3) . . ? C8 C9 Fe1 69.9(2) . . ? C10 C9 Fe1 69.71(17) . . ? C6 C10 C9 107.7(3) . . ? C6 C10 Fe1 69.75(17) . . ? C9 C10 Fe1 69.83(18) . . ? N1 C11 C14 120.6(3) . . ? N1 C11 C1 118.7(3) . . ? C14 C11 C1 120.7(3) . . ? N1 C12 C13 122.6(3) . . ? N2 C13 C12 121.4(3) . . ? N2 C14 C11 122.7(3) . . ? N3 C15 C18 120.5(3) . . ? N3 C15 C6 117.5(2) . . ? C18 C15 C6 122.0(3) . . ? N3 C16 C17 122.6(3) . . ? N4 C17 C16 120.7(3) . . ? N4 C18 C15 122.2(3) . . ? O1 C19 O2 125.5(2) . . ? O1 C19 C20 117.9(3) . . ? O2 C19 C20 116.6(3) . . ? C25 C20 C21 118.1(3) . . ? C25 C20 C19 121.5(3) . . ? C21 C20 C19 120.3(3) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 121.1(4) . . ? C24 C23 C22 119.1(4) . . ? C23 C24 C25 120.3(4) . . ? C20 C25 C24 120.9(3) . . ? O3 C26 O4 125.4(3) . . ? O3 C26 C27 117.8(3) . . ? O4 C26 C27 116.8(3) . . ? C28 C27 C32 119.8(3) . . ? C28 C27 C26 119.8(3) . . ? C32 C27 C26 120.4(3) . . ? C27 C28 C29 120.0(4) . . ? C30 C29 C28 119.8(4) . . ? C31 C30 C29 120.6(3) . . ? C30 C31 C32 120.0(4) . . ? C27 C32 C31 119.7(4) . . ? O6 C33 O5 125.2(3) . . ? O6 C33 C34 118.4(3) . . ? O5 C33 C34 116.4(3) . . ? C35 C34 C39 118.4(3) . . ? C35 C34 C33 121.6(3) . . ? C39 C34 C33 119.9(3) . . ? C34 C35 C36 120.6(4) . . ? C37 C36 C35 120.6(4) . . ? C36 C37 C38 119.6(4) . . ? C37 C38 C39 119.8(4) . . ? C34 C39 C38 120.9(3) . . ? O7 C40 O8 124.9(3) . . ? O7 C40 C41 118.8(3) . . ? O8 C40 C41 116.3(3) . . ? C46 C41 C42 119.2(3) . . ? C46 C41 C40 120.7(3) . . ? C42 C41 C40 120.0(3) . . ? C43 C42 C41 120.5(4) . . ? C44 C43 C42 119.5(4) . . ? C43 C44 C45 120.9(4) . . ? C44 C45 C46 119.8(4) . . ? C41 C46 C45 119.9(4) . . ? O4 Cu1 O1 91.54(9) 2_675 . ? O4 Cu1 O3 168.34(9) 2_675 . ? O1 Cu1 O3 88.46(9) . . ? O4 Cu1 O2 86.61(8) 2_675 2_675 ? O1 Cu1 O2 168.30(8) . 2_675 ? O3 Cu1 O2 91.02(9) . 2_675 ? O4 Cu1 N2 94.82(8) 2_675 . ? O1 Cu1 N2 96.65(8) . . ? O3 Cu1 N2 96.77(9) . . ? O2 Cu1 N2 95.02(8) 2_675 . ? O4 Cu1 Cu1 84.22(6) 2_675 2_675 ? O1 Cu1 Cu1 86.22(6) . 2_675 ? O3 Cu1 Cu1 84.14(7) . 2_675 ? O2 Cu1 Cu1 82.10(6) 2_675 2_675 ? N2 Cu1 Cu1 177.00(6) . 2_675 ? O7 Cu2 O8 168.40(8) . 2_566 ? O7 Cu2 O5 87.73(10) . . ? O8 Cu2 O5 90.48(10) 2_566 . ? O7 Cu2 O6 90.02(9) . 2_566 ? O8 Cu2 O6 89.49(10) 2_566 2_566 ? O5 Cu2 O6 168.64(8) . 2_566 ? O7 Cu2 N4 100.46(9) . . ? O8 Cu2 N4 91.10(9) 2_566 . ? O5 Cu2 N4 94.44(8) . . ? O6 Cu2 N4 96.92(8) 2_566 . ? O7 Cu2 Cu2 89.00(6) . 2_566 ? O8 Cu2 Cu2 79.41(6) 2_566 2_566 ? O5 Cu2 Cu2 82.79(6) . 2_566 ? O6 Cu2 Cu2 86.03(6) 2_566 2_566 ? N4 Cu2 Cu2 170.06(6) . 2_566 ? C2 Fe1 C4 67.64(14) . . ? C2 Fe1 C1 40.69(12) . . ? C4 Fe1 C1 68.19(13) . . ? C2 Fe1 C5 68.24(14) . . ? C4 Fe1 C5 40.61(13) . . ? C1 Fe1 C5 40.76(12) . . ? C2 Fe1 C7 107.63(14) . . ? C4 Fe1 C7 157.97(14) . . ? C1 Fe1 C7 123.25(13) . . ? C5 Fe1 C7 159.78(13) . . ? C2 Fe1 C6 124.33(13) . . ? C4 Fe1 C6 159.43(15) . . ? C1 Fe1 C6 108.86(11) . . ? C5 Fe1 C6 123.81(12) . . ? C7 Fe1 C6 40.93(11) . . ? C2 Fe1 C8 122.44(16) . . ? C4 Fe1 C8 122.18(14) . . ? C1 Fe1 C8 158.91(15) . . ? C5 Fe1 C8 158.42(15) . . ? C7 Fe1 C8 40.67(13) . . ? C6 Fe1 C8 68.11(12) . . ? C2 Fe1 C10 160.47(12) . . ? C4 Fe1 C10 123.25(15) . . ? C1 Fe1 C10 124.24(12) . . ? C5 Fe1 C10 108.44(14) . . ? C7 Fe1 C10 68.43(13) . . ? C6 Fe1 C10 40.27(12) . . ? C8 Fe1 C10 67.89(14) . . ? C2 Fe1 C3 40.25(12) . . ? C4 Fe1 C3 40.12(15) . . ? C1 Fe1 C3 68.22(13) . . ? C5 Fe1 C3 68.14(15) . . ? C7 Fe1 C3 122.38(15) . . ? C6 Fe1 C3 159.53(15) . . ? C8 Fe1 C3 106.91(15) . . ? C10 Fe1 C3 158.17(14) . . ? C2 Fe1 C9 157.58(13) . . ? C4 Fe1 C9 107.65(15) . . ? C1 Fe1 C9 160.08(14) . . ? C5 Fe1 C9 123.45(16) . . ? C7 Fe1 C9 68.02(15) . . ? C6 Fe1 C9 67.77(12) . . ? C8 Fe1 C9 39.96(15) . . ? C10 Fe1 C9 40.47(12) . . ? C3 Fe1 C9 122.02(13) . . ? C12 N1 C11 116.5(3) . . ? C13 N2 C14 116.1(2) . . ? C13 N2 Cu1 125.27(19) . . ? C14 N2 Cu1 118.32(18) . . ? C16 N3 C15 116.9(2) . . ? C18 N4 C17 117.1(2) . . ? C18 N4 Cu2 121.14(18) . . ? C17 N4 Cu2 121.77(18) . . ? C19 O1 Cu1 120.77(18) . . ? C19 O2 Cu1 125.27(18) . 2_675 ? C26 O3 Cu1 122.93(19) . . ? C26 O4 Cu1 122.85(18) . 2_675 ? C33 O5 Cu2 124.9(2) . . ? C33 O6 Cu2 120.74(18) . 2_566 ? C40 O7 Cu2 117.7(2) . . ? C40 O8 Cu2 128.71(19) . 2_566 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.584 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.065 #-----------END data_2 _database_code_depnum_ccdc_archive 'CCDC 262868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H116 Cu4 Fe2 N8 O16' _chemical_formula_weight 1859.71 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3978(9) _cell_length_b 22.6166(15) _cell_length_c 14.4661(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.918(2) _cell_angle_gamma 90.00 _cell_volume 4351.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.352 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5513 _exptl_absorpt_correction_T_max 0.7737 _exptl_absorpt_process_details 'SADABS;Sheldrick 1996' _exptl_special_details ; SADABS;Sheldrick,1996 ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32255 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.31 _reflns_number_total 10792 _reflns_number_gt 8615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+2.0271P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10792 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.62291(16) 0.01551(10) 0.52120(17) 0.0284(5) Uani 1 1 d . . . C2 C 0.62801(18) -0.01865(11) 0.6043(2) 0.0346(5) Uani 1 1 d . . . H2 H 0.6229 -0.0042 0.6637 0.042 Uiso 1 1 calc R . . C3 C 0.6422(2) -0.07847(12) 0.5804(2) 0.0438(7) Uani 1 1 d . . . H3 H 0.6472 -0.1102 0.6215 0.053 Uiso 1 1 calc R . . C4 C 0.64739(19) -0.08184(12) 0.4834(2) 0.0449(7) Uani 1 1 d . . . H4 H 0.6569 -0.1160 0.4499 0.054 Uiso 1 1 calc R . . C5 C 0.63566(18) -0.02418(12) 0.4468(2) 0.0369(6) Uani 1 1 d . . . H5 H 0.6361 -0.0138 0.3846 0.044 Uiso 1 1 calc R . . C6 C 0.87118(16) 0.03281(10) 0.54881(17) 0.0278(5) Uani 1 1 d . . . C7 C 0.87544(18) 0.00133(11) 0.63510(18) 0.0328(5) Uani 1 1 d . . . H7 H 0.8711 0.0179 0.6933 0.039 Uiso 1 1 calc R . . C8 C 0.88747(18) -0.05971(11) 0.6159(2) 0.0377(6) Uani 1 1 d . . . H8 H 0.8931 -0.0900 0.6596 0.045 Uiso 1 1 calc R . . C9 C 0.88941(18) -0.06648(11) 0.5190(2) 0.0363(6) Uani 1 1 d . . . H9 H 0.8959 -0.1021 0.4880 0.044 Uiso 1 1 calc R . . C10 C 0.87986(17) -0.00980(11) 0.47686(18) 0.0324(5) Uani 1 1 d . . . H10 H 0.8793 -0.0017 0.4138 0.039 Uiso 1 1 calc R . . C11 C 0.60807(16) 0.07966(10) 0.51184(16) 0.0281(5) Uani 1 1 d . . . C12 C 0.6050(3) 0.16244(13) 0.4230(2) 0.0489(7) Uani 1 1 d . . . H12 H 0.6160 0.1814 0.3681 0.059 Uiso 1 1 calc R . . C13 C 0.5711(2) 0.19554(12) 0.49346(19) 0.0405(6) Uani 1 1 d . . . H13 H 0.5582 0.2356 0.4842 0.049 Uiso 1 1 calc R . . C14 C 0.57643(17) 0.11320(10) 0.58388(16) 0.0275(5) Uani 1 1 d . . . H14 H 0.5689 0.0948 0.6401 0.033 Uiso 1 1 calc R . . C15 C 0.85912(16) 0.09678(10) 0.53712(16) 0.0270(5) Uani 1 1 d . . . C16 C 0.8158(2) 0.18597(12) 0.59319(19) 0.0396(6) Uani 1 1 d . . . H16 H 0.7904 0.2086 0.6387 0.048 Uiso 1 1 calc R . . C17 C 0.8414(2) 0.21370(11) 0.51428(19) 0.0377(6) Uani 1 1 d . . . H17 H 0.8348 0.2545 0.5089 0.045 Uiso 1 1 calc R . . C18 C 0.88241(17) 0.12497(11) 0.45616(17) 0.0295(5) Uani 1 1 d . . . H18 H 0.9034 0.1023 0.4084 0.035 Uiso 1 1 calc R . . C19 C 0.2837(2) 0.23428(12) 0.6809(2) 0.0389(6) Uani 1 1 d . . . C20 C 0.1758(2) 0.22797(16) 0.6361(2) 0.0532(8) Uani 1 1 d . . . H20A H 0.1564 0.2641 0.6026 0.064 Uiso 1 1 calc R . . H20B H 0.1728 0.1962 0.5908 0.064 Uiso 1 1 calc R . . C21 C 0.1003(3) 0.2156(2) 0.7027(3) 0.0750(12) Uani 1 1 d . . . C22 C 0.1084(7) 0.1767(6) 0.7745(6) 0.084(3) Uani 0.50 1 d P . . C23 C 0.1349(7) 0.1460(4) 0.7383(6) 0.0579(19) Uani 0.50 1 d P . . C24 C 0.1038(9) 0.1153(6) 0.7336(8) 0.088(3) Uani 0.50 1 d P . . C25 C 0.0569(6) 0.1203(4) 0.7997(6) 0.068(2) Uani 0.50 1 d P . . C26 C 0.0896(5) 0.0613(3) 0.8199(4) 0.1115(19) Uani 1 1 d . . . C27 C 0.4818(2) 0.34280(11) 0.67654(19) 0.0366(6) Uani 1 1 d . . . C28 C 0.4995(3) 0.40219(13) 0.6324(2) 0.0516(8) Uani 1 1 d . . . H28A H 0.4403 0.4129 0.5905 0.062 Uiso 1 1 calc R . . H28B H 0.5092 0.4320 0.6808 0.062 Uiso 1 1 calc R . . C29 C 0.5889(3) 0.40198(16) 0.5795(3) 0.0686(10) Uani 1 1 d . . . H29A H 0.5955 0.4407 0.5519 0.082 Uiso 1 1 calc R . . H29B H 0.5779 0.3734 0.5293 0.082 Uiso 1 1 calc R . . C30 C 0.6879(3) 0.38659(18) 0.6414(3) 0.0723(11) Uani 1 1 d . . . H30A H 0.7002 0.4163 0.6899 0.087 Uiso 1 1 calc R . . H30B H 0.6797 0.3488 0.6715 0.087 Uiso 1 1 calc R . . C31 C 0.7776(4) 0.3833(2) 0.5893(4) 0.0909(15) Uani 1 1 d . . . H31A H 0.7631 0.3561 0.5375 0.109 Uiso 1 1 calc R . . H31B H 0.7894 0.4220 0.5638 0.109 Uiso 1 1 calc R . . C32 C 0.8704(4) 0.3635(3) 0.6473(4) 0.1058(18) Uani 1 1 d . . . H32A H 0.8908 0.3930 0.6935 0.159 Uiso 1 1 calc R . . H32B H 0.9229 0.3577 0.6086 0.159 Uiso 1 1 calc R . . H32C H 0.8575 0.3270 0.6775 0.159 Uiso 1 1 calc R . . C33 C 0.6421(2) 0.25685(12) 0.83455(19) 0.0365(6) Uani 1 1 d . . . C34 C 0.7509(2) 0.26098(15) 0.8792(2) 0.0511(7) Uani 1 1 d . . . H34A H 0.7522 0.2740 0.9432 0.061 Uiso 1 1 calc R . . H34B H 0.7861 0.2902 0.8462 0.061 Uiso 1 1 calc R . . C35 C 0.8059(3) 0.2007(2) 0.8773(3) 0.0829(14) Uani 1 1 d . . . H35A H 0.8017 0.1867 0.8135 0.100 Uiso 1 1 calc R . . H35B H 0.8764 0.2060 0.9002 0.100 Uiso 1 1 calc R . . C36 C 0.7602(4) 0.1535(2) 0.9374(4) 0.0939(15) Uani 1 1 d . . . H36A H 0.7807 0.1629 1.0023 0.113 Uiso 1 1 calc R . . H36B H 0.6876 0.1573 0.9267 0.113 Uiso 1 1 calc R . . C37 C 0.7870(5) 0.0881(3) 0.9219(4) 0.116(2) Uani 1 1 d . . . H37A H 0.8591 0.0849 0.9208 0.139 Uiso 1 1 calc R . . H37B H 0.7696 0.0649 0.9739 0.139 Uiso 1 1 calc R . . C38 C 0.7373(5) 0.0642(3) 0.8382(4) 0.122(2) Uani 1 1 d . . . H38A H 0.6661 0.0702 0.8364 0.183 Uiso 1 1 calc R . . H38B H 0.7512 0.0227 0.8356 0.183 Uiso 1 1 calc R . . H38C H 0.7608 0.0837 0.7859 0.183 Uiso 1 1 calc R . . C39 C 0.4493(2) 0.14781(11) 0.83903(19) 0.0368(6) Uani 1 1 d . . . C40 C 0.4435(3) 0.08922(12) 0.8876(2) 0.0513(8) Uani 1 1 d . . . H40A H 0.3962 0.0928 0.9330 0.062 Uiso 1 1 calc R . . H40B H 0.5089 0.0806 0.9213 0.062 Uiso 1 1 calc R . . C41 C 0.4118(3) 0.03731(14) 0.8240(2) 0.0517(7) Uani 1 1 d . . . H41A H 0.3468 0.0458 0.7895 0.062 Uiso 1 1 calc R . . H41B H 0.4599 0.0327 0.7795 0.062 Uiso 1 1 calc R . . C42 C 0.4052(4) -0.01957(15) 0.8764(3) 0.0682(10) Uani 1 1 d . . . H42A H 0.3591 -0.0140 0.9224 0.082 Uiso 1 1 calc R . . H42B H 0.4709 -0.0282 0.9095 0.082 Uiso 1 1 calc R . . C43 C 0.3711(4) -0.0725(2) 0.8173(3) 0.0826(13) Uani 1 1 d . . . H43A H 0.4113 -0.0743 0.7659 0.099 Uiso 1 1 calc R . . H43B H 0.3859 -0.1077 0.8546 0.099 Uiso 1 1 calc R . . C44 C 0.2681(4) -0.0746(3) 0.7798(4) 0.1083(18) Uani 1 1 d . . . H44A H 0.2267 -0.0693 0.8289 0.162 Uiso 1 1 calc R . . H44B H 0.2536 -0.1123 0.7506 0.162 Uiso 1 1 calc R . . H44C H 0.2544 -0.0437 0.7345 0.162 Uiso 1 1 calc R . . Cu1 Cu 0.49484(2) 0.218575(12) 0.68612(2) 0.02947(9) Uani 1 1 d . . . Cu2 Cu 0.43113(2) 0.272588(13) 0.82778(2) 0.03131(9) Uani 1 1 d . . . Fe1 Fe 0.75762(2) -0.027689(14) 0.54393(2) 0.02600(9) Uani 1 1 d . . . N1 N 0.62247(18) 0.10450(10) 0.43066(15) 0.0407(5) Uani 1 1 d . . . N2 N 0.55665(15) 0.17075(9) 0.57451(14) 0.0296(4) Uani 1 1 d . . . N3 N 0.82603(16) 0.12767(10) 0.60643(15) 0.0349(5) Uani 1 1 d . . . N4 N 0.87530(15) 0.18333(9) 0.44585(15) 0.0320(4) Uani 1 1 d . . . O1 O 0.35100(15) 0.21109(9) 0.64014(14) 0.0443(5) Uani 1 1 d . . . O5 O 0.29780(14) 0.26267(9) 0.75585(14) 0.0449(5) Uani 1 1 d . . . O2 O 0.49518(16) 0.29714(8) 0.62975(13) 0.0424(4) Uani 1 1 d . . . O6 O 0.45512(15) 0.34401(8) 0.75652(13) 0.0404(4) Uani 1 1 d . . . O3 O 0.62860(14) 0.23529(9) 0.75428(14) 0.0433(5) Uani 1 1 d . . . O7 O 0.57425(15) 0.27469(9) 0.88014(14) 0.0436(5) Uani 1 1 d . . . O4 O 0.48422(16) 0.14731(8) 0.76228(14) 0.0441(5) Uani 1 1 d . . . O8 O 0.41995(17) 0.19234(8) 0.87884(14) 0.0453(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 C1 0.0202(10) 0.0302(11) 0.0355(12) -0.0052(10) 0.0056(9) 0.0015(8) C2 0.0283(12) 0.0310(12) 0.0470(15) 0.0009(11) 0.0147(10) -0.0018(9) C3 0.0316(13) 0.0264(12) 0.076(2) 0.0031(13) 0.0181(13) -0.0026(10) C4 0.0264(12) 0.0329(13) 0.075(2) -0.0179(14) 0.0037(12) -0.0027(10) C5 0.0249(11) 0.0410(14) 0.0440(15) -0.0161(12) 0.0007(10) 0.0027(10) C6 0.0210(10) 0.0292(11) 0.0332(12) 0.0038(9) 0.0031(8) -0.0029(8) C7 0.0285(12) 0.0355(12) 0.0332(12) 0.0060(10) -0.0013(9) -0.0037(10) C8 0.0277(12) 0.0329(12) 0.0513(16) 0.0112(12) -0.0011(10) 0.0011(10) C9 0.0243(11) 0.0327(12) 0.0525(16) -0.0019(11) 0.0067(10) 0.0057(9) C10 0.0225(11) 0.0393(13) 0.0367(13) 0.0001(11) 0.0082(9) 0.0015(10) C11 0.0220(10) 0.0315(11) 0.0308(12) -0.0026(9) 0.0034(8) 0.0029(9) C12 0.072(2) 0.0420(15) 0.0356(14) 0.0085(12) 0.0185(14) 0.0161(14) C13 0.0521(16) 0.0303(12) 0.0406(14) 0.0053(11) 0.0124(12) 0.0088(11) C14 0.0250(10) 0.0296(11) 0.0288(11) -0.0006(9) 0.0062(8) -0.0005(9) C15 0.0212(10) 0.0302(11) 0.0297(11) 0.0014(9) 0.0032(8) -0.0045(9) C16 0.0502(16) 0.0330(13) 0.0381(14) -0.0055(11) 0.0150(12) -0.0053(11) C17 0.0441(15) 0.0289(12) 0.0418(15) 0.0023(11) 0.0121(11) -0.0024(10) C18 0.0267(11) 0.0307(11) 0.0320(12) 0.0032(10) 0.0073(9) -0.0019(9) C19 0.0374(14) 0.0384(13) 0.0406(15) -0.0032(11) 0.0036(11) -0.0055(11) C20 0.0407(16) 0.068(2) 0.0488(18) -0.0069(15) -0.0032(13) -0.0057(14) C21 0.0429(19) 0.118(4) 0.064(2) -0.005(2) 0.0069(17) -0.018(2) C22 0.068(5) 0.124(8) 0.065(5) -0.030(6) 0.025(4) -0.033(5) C23 0.070(5) 0.050(4) 0.055(5) -0.012(4) 0.014(4) -0.013(4) C24 0.090(8) 0.095(8) 0.072(6) -0.020(6) -0.013(5) 0.004(6) C25 0.063(4) 0.082(6) 0.060(4) 0.007(4) 0.014(4) -0.017(4) C26 0.135(5) 0.088(4) 0.106(4) 0.000(3) -0.011(4) -0.004(3) C27 0.0401(14) 0.0285(12) 0.0401(14) 0.0001(11) -0.0003(11) 0.0013(10) C28 0.076(2) 0.0312(13) 0.0476(17) 0.0063(13) 0.0064(15) 0.0002(14) C29 0.104(3) 0.0442(18) 0.063(2) 0.0139(16) 0.029(2) -0.0063(19) C30 0.085(3) 0.063(2) 0.075(3) 0.002(2) 0.037(2) -0.017(2) C31 0.098(4) 0.078(3) 0.107(4) -0.004(3) 0.054(3) -0.009(3) C32 0.081(3) 0.129(5) 0.116(4) -0.025(4) 0.046(3) -0.023(3) C33 0.0385(14) 0.0339(13) 0.0366(14) 0.0001(11) 0.0022(11) -0.0051(11) C34 0.0403(16) 0.0613(19) 0.0498(18) -0.0032(15) -0.0022(13) -0.0118(14) C35 0.049(2) 0.131(4) 0.066(2) -0.028(3) -0.0066(18) 0.024(2) C36 0.113(4) 0.090(3) 0.077(3) 0.005(3) 0.007(3) 0.035(3) C37 0.120(5) 0.122(5) 0.100(4) -0.002(4) -0.013(3) 0.049(4) C38 0.145(6) 0.115(5) 0.108(5) -0.032(4) 0.021(4) 0.016(4) C39 0.0455(14) 0.0289(12) 0.0380(14) -0.0025(10) 0.0133(11) -0.0021(11) C40 0.087(2) 0.0312(13) 0.0405(16) 0.0014(12) 0.0275(15) -0.0013(14) C41 0.070(2) 0.0434(16) 0.0423(16) -0.0011(13) 0.0109(14) -0.0046(15) C42 0.102(3) 0.0483(19) 0.055(2) -0.0026(16) 0.015(2) -0.0224(19) C43 0.103(4) 0.069(3) 0.077(3) -0.018(2) 0.017(2) -0.030(2) C44 0.097(4) 0.111(4) 0.122(5) -0.030(4) 0.032(3) -0.033(3) Cu1 0.03472(17) 0.02482(15) 0.02989(16) -0.00385(11) 0.00805(12) 0.00021(11) Cu2 0.03554(17) 0.02739(15) 0.03181(17) -0.00689(11) 0.00742(12) 0.00140(12) Fe1 0.02088(16) 0.02296(16) 0.03450(19) -0.00025(13) 0.00474(12) 0.00015(12) N1 0.0520(14) 0.0411(12) 0.0308(11) 0.0015(9) 0.0123(10) 0.0110(10) N2 0.0295(10) 0.0274(9) 0.0327(10) -0.0025(8) 0.0072(8) 0.0009(8) N3 0.0410(12) 0.0343(11) 0.0307(11) -0.0009(9) 0.0093(9) -0.0064(9) N4 0.0305(10) 0.0308(10) 0.0361(11) 0.0063(9) 0.0091(8) -0.0015(8) O1 0.0396(10) 0.0480(11) 0.0453(11) -0.0167(9) 0.0054(8) -0.0027(9) O5 0.0354(10) 0.0529(12) 0.0467(11) -0.0148(9) 0.0059(8) -0.0003(9) O2 0.0606(13) 0.0303(9) 0.0374(10) 0.0006(8) 0.0107(9) -0.0010(9) O6 0.0516(11) 0.0284(9) 0.0418(11) -0.0021(8) 0.0082(8) 0.0011(8) O3 0.0357(10) 0.0561(12) 0.0379(10) -0.0083(9) 0.0044(8) -0.0003(9) O7 0.0398(11) 0.0501(11) 0.0399(11) -0.0112(9) 0.0009(8) 0.0028(8) O4 0.0662(13) 0.0293(9) 0.0416(11) 0.0027(8) 0.0267(9) 0.0048(9) O8 0.0661(13) 0.0301(9) 0.0437(11) -0.0039(8) 0.0232(10) 0.0020(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.423(4) . ? C1 C5 1.428(3) . ? C1 C11 1.468(3) . ? C1 Fe1 2.044(2) . ? C2 C3 1.415(4) . ? C2 Fe1 2.045(2) . ? C3 C4 1.414(5) . ? C3 Fe1 2.046(3) . ? C4 C5 1.410(4) . ? C4 Fe1 2.034(3) . ? C5 Fe1 2.025(3) . ? C6 C7 1.432(3) . ? C6 C10 1.433(3) . ? C6 C15 1.464(3) . ? C6 Fe1 2.041(2) . ? C7 C8 1.421(4) . ? C7 Fe1 2.040(2) . ? C8 C9 1.414(4) . ? C8 Fe1 2.049(2) . ? C9 C10 1.418(4) . ? C9 Fe1 2.043(2) . ? C10 Fe1 2.042(2) . ? C11 N1 1.337(3) . ? C11 C14 1.396(3) . ? C12 N1 1.333(4) . ? C12 C13 1.384(4) . ? C13 N2 1.335(3) . ? C14 N2 1.332(3) . ? C15 N3 1.340(3) . ? C15 C18 1.401(3) . ? C16 N3 1.337(3) . ? C16 C17 1.382(4) . ? C17 N4 1.329(3) . ? C18 N4 1.330(3) . ? C19 O1 1.250(3) . ? C19 O5 1.255(3) . ? C19 C20 1.518(4) . ? C20 C21 1.505(5) . ? C21 C22 1.354(12) . ? C21 C23 1.702(10) . ? C26 C25 1.423(10) . ? C26 C24 1.773(15) . ? C27 O6 1.252(3) . ? C27 O2 1.259(3) . ? C27 C28 1.518(4) . ? C28 C29 1.497(5) . ? C29 C30 1.549(6) . ? C30 C31 1.497(6) . ? C31 C32 1.482(7) . ? C33 O7 1.252(3) . ? C33 O3 1.252(3) . ? C33 C34 1.525(4) . ? C34 C35 1.553(6) . ? C35 C36 1.548(7) . ? C36 C37 1.545(7) . ? C37 C38 1.416(7) . ? C39 O8 1.247(3) . ? C39 O4 1.255(3) . ? C39 C40 1.506(4) . ? C40 C41 1.520(4) . ? C41 C42 1.500(5) . ? C42 C43 1.509(5) . ? C43 C44 1.421(7) . ? Cu1 O2 1.9553(19) . ? Cu1 O4 1.9671(18) . ? Cu1 O1 1.969(2) . ? Cu1 O3 1.9751(19) . ? Cu1 N2 2.187(2) . ? Cu1 Cu2 2.6157(4) . ? Cu2 O6 1.9636(19) . ? Cu2 O5 1.969(2) . ? Cu2 O8 1.9719(19) . ? Cu2 O7 1.975(2) . ? Cu2 N4 2.186(2) 4_566 ? N4 Cu2 2.186(2) 4_665 ? C23 C24 0.810(12) . ? C23 C22 0.964(12) . ? C23 C25 1.562(11) . ? C25 C24 1.211(14) . ? C25 C22 1.516(13) . ? C22 C24 1.510(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.3(2) . . ? C2 C1 C11 127.3(2) . . ? C5 C1 C11 125.4(2) . . ? C2 C1 Fe1 69.70(13) . . ? C5 C1 Fe1 68.73(13) . . ? C11 C1 Fe1 126.46(16) . . ? C3 C2 C1 107.9(2) . . ? C3 C2 Fe1 69.77(14) . . ? C1 C2 Fe1 69.57(13) . . ? C4 C3 C2 108.5(3) . . ? C4 C3 Fe1 69.26(15) . . ? C2 C3 Fe1 69.76(14) . . ? C5 C4 C3 107.9(2) . . ? C5 C4 Fe1 69.33(14) . . ? C3 C4 Fe1 70.18(15) . . ? C4 C5 C1 108.4(3) . . ? C4 C5 Fe1 70.02(16) . . ? C1 C5 Fe1 70.18(14) . . ? C7 C6 C10 107.5(2) . . ? C7 C6 C15 125.8(2) . . ? C10 C6 C15 126.7(2) . . ? C7 C6 Fe1 69.40(13) . . ? C10 C6 Fe1 69.49(13) . . ? C15 C6 Fe1 125.96(16) . . ? C8 C7 C6 107.8(2) . . ? C8 C7 Fe1 70.01(14) . . ? C6 C7 Fe1 69.50(13) . . ? C9 C8 C7 108.4(2) . . ? C9 C8 Fe1 69.54(14) . . ? C7 C8 Fe1 69.31(13) . . ? C8 C9 C10 108.4(2) . . ? C8 C9 Fe1 70.03(14) . . ? C10 C9 Fe1 69.66(13) . . ? C9 C10 C6 107.9(2) . . ? C9 C10 Fe1 69.70(14) . . ? C6 C10 Fe1 69.41(13) . . ? N1 C11 C14 121.1(2) . . ? N1 C11 C1 117.6(2) . . ? C14 C11 C1 121.2(2) . . ? N1 C12 C13 122.7(3) . . ? N2 C13 C12 121.0(2) . . ? N2 C14 C11 122.0(2) . . ? N3 C15 C18 121.0(2) . . ? N3 C15 C6 118.1(2) . . ? C18 C15 C6 120.9(2) . . ? N3 C16 C17 122.3(2) . . ? N4 C17 C16 121.5(2) . . ? N4 C18 C15 121.7(2) . . ? O1 C19 O5 125.4(3) . . ? O1 C19 C20 117.6(3) . . ? O5 C19 C20 117.0(3) . . ? C21 C20 C19 115.0(3) . . ? C22 C21 C20 127.9(5) . . ? C22 C21 C23 34.4(5) . . ? C20 C21 C23 100.8(4) . . ? C25 C26 C24 42.8(5) . . ? O6 C27 O2 126.1(2) . . ? O6 C27 C28 116.5(2) . . ? O2 C27 C28 117.4(3) . . ? C29 C28 C27 112.8(3) . . ? C28 C29 C30 112.7(3) . . ? C31 C30 C29 113.8(4) . . ? C32 C31 C30 113.5(4) . . ? O7 C33 O3 125.5(2) . . ? O7 C33 C34 118.3(2) . . ? O3 C33 C34 116.1(3) . . ? C33 C34 C35 111.7(3) . . ? C36 C35 C34 112.0(3) . . ? C37 C36 C35 117.6(5) . . ? C38 C37 C36 113.3(5) . . ? O8 C39 O4 126.0(3) . . ? O8 C39 C40 117.2(2) . . ? O4 C39 C40 116.8(2) . . ? C39 C40 C41 115.1(3) . . ? C42 C41 C40 112.7(3) . . ? C41 C42 C43 115.2(3) . . ? C44 C43 C42 117.2(5) . . ? O2 Cu1 O4 169.15(8) . . ? O2 Cu1 O1 89.35(9) . . ? O4 Cu1 O1 89.13(9) . . ? O2 Cu1 O3 89.24(9) . . ? O4 Cu1 O3 89.99(9) . . ? O1 Cu1 O3 167.82(8) . . ? O2 Cu1 N2 96.98(8) . . ? O4 Cu1 N2 93.88(7) . . ? O1 Cu1 N2 98.64(8) . . ? O3 Cu1 N2 93.54(8) . . ? O2 Cu1 Cu2 85.39(6) . . ? O4 Cu1 Cu2 83.77(5) . . ? O1 Cu1 Cu2 84.63(6) . . ? O3 Cu1 Cu2 83.20(6) . . ? N2 Cu1 Cu2 175.96(6) . . ? O6 Cu2 O5 90.67(9) . . ? O6 Cu2 O8 168.09(8) . . ? O5 Cu2 O8 89.32(9) . . ? O6 Cu2 O7 88.21(9) . . ? O5 Cu2 O7 169.21(8) . . ? O8 Cu2 O7 89.58(9) . . ? O6 Cu2 N4 97.36(8) . 4_566 ? O5 Cu2 N4 95.21(8) . 4_566 ? O8 Cu2 N4 94.51(8) . 4_566 ? O7 Cu2 N4 95.58(8) . 4_566 ? O6 Cu2 Cu1 83.30(6) . . ? O5 Cu2 Cu1 83.90(6) . . ? O8 Cu2 Cu1 84.85(6) . . ? O7 Cu2 Cu1 85.32(6) . . ? N4 Cu2 Cu1 178.90(6) 4_566 . ? C5 Fe1 C4 40.65(11) . . ? C5 Fe1 C7 158.96(10) . . ? C4 Fe1 C7 159.62(12) . . ? C5 Fe1 C6 122.25(11) . . ? C4 Fe1 C6 156.68(12) . . ? C7 Fe1 C6 41.09(9) . . ? C5 Fe1 C10 106.78(11) . . ? C4 Fe1 C10 119.82(12) . . ? C7 Fe1 C10 68.96(10) . . ? C6 Fe1 C10 41.10(10) . . ? C5 Fe1 C9 122.45(11) . . ? C4 Fe1 C9 105.29(11) . . ? C7 Fe1 C9 68.55(11) . . ? C6 Fe1 C9 68.74(10) . . ? C10 Fe1 C9 40.64(10) . . ? C5 Fe1 C1 41.09(9) . . ? C4 Fe1 C1 68.73(10) . . ? C7 Fe1 C1 123.36(10) . . ? C6 Fe1 C1 108.98(9) . . ? C10 Fe1 C1 124.89(10) . . ? C9 Fe1 C1 160.45(11) . . ? C5 Fe1 C2 68.70(11) . . ? C4 Fe1 C2 68.53(11) . . ? C7 Fe1 C2 108.82(11) . . ? C6 Fe1 C2 125.86(10) . . ? C10 Fe1 C2 162.47(10) . . ? C9 Fe1 C2 156.18(11) . . ? C1 Fe1 C2 40.73(10) . . ? C5 Fe1 C3 68.22(12) . . ? C4 Fe1 C3 40.57(13) . . ? C7 Fe1 C3 124.35(12) . . ? C6 Fe1 C3 161.98(12) . . ? C10 Fe1 C3 155.24(11) . . ? C9 Fe1 C3 120.06(11) . . ? C1 Fe1 C3 68.25(10) . . ? C2 Fe1 C3 40.47(10) . . ? C5 Fe1 C8 158.66(11) . . ? C4 Fe1 C8 122.27(11) . . ? C7 Fe1 C8 40.68(10) . . ? C6 Fe1 C8 68.63(10) . . ? C10 Fe1 C8 68.34(10) . . ? C9 Fe1 C8 40.43(11) . . ? C1 Fe1 C8 158.44(11) . . ? C2 Fe1 C8 122.08(11) . . ? C3 Fe1 C8 107.02(11) . . ? C12 N1 C11 116.3(2) . . ? C14 N2 C13 116.9(2) . . ? C14 N2 Cu1 119.77(16) . . ? C13 N2 Cu1 123.26(17) . . ? C16 N3 C15 116.4(2) . . ? C17 N4 C18 117.1(2) . . ? C17 N4 Cu2 121.73(16) . 4_665 ? C18 N4 Cu2 120.89(17) . 4_665 ? C19 O1 Cu1 122.48(18) . . ? C19 O5 Cu2 123.20(18) . . ? C27 O2 Cu1 120.89(18) . . ? C27 O6 Cu2 123.39(17) . . ? C33 O3 Cu1 123.94(18) . . ? C33 O7 Cu2 121.52(18) . . ? C39 O4 Cu1 123.21(17) . . ? C39 O8 Cu2 121.86(18) . . ? C24 C23 C22 116.5(16) . . ? C24 C23 C25 49.9(11) . . ? C22 C23 C25 69.2(9) . . ? C24 C23 C21 130.6(13) . . ? C22 C23 C21 52.6(8) . . ? C25 C23 C21 109.9(7) . . ? C24 C25 C26 84.2(9) . . ? C24 C25 C22 66.2(7) . . ? C26 C25 C22 134.5(8) . . ? C24 C25 C23 30.7(6) . . ? C26 C25 C23 104.9(7) . . ? C22 C25 C23 36.4(4) . . ? C23 C22 C21 92.9(9) . . ? C23 C22 C24 28.7(8) . . ? C21 C22 C24 107.5(8) . . ? C23 C22 C25 74.4(9) . . ? C21 C22 C25 137.2(8) . . ? C24 C22 C25 47.2(6) . . ? C23 C24 C25 99.4(13) . . ? C23 C24 C22 34.8(9) . . ? C25 C24 C22 66.7(7) . . ? C23 C24 C26 129.0(13) . . ? C25 C24 C26 53.0(7) . . ? C22 C24 C26 111.1(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.078 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.084 #-----------END data_3 _database_code_depnum_ccdc_archive 'CCDC 262869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Pz2CuOAc _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H77 Cu6 Fe2 N11 O26' _chemical_formula_weight 1933.39 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' Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6142(6) _cell_length_b 11.3799(6) _cell_length_c 17.5157(9) _cell_angle_alpha 96.2600(10) _cell_angle_beta 101.2480(10) _cell_angle_gamma 106.5040(10) _cell_volume 1958.90(18) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.038 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4961 _exptl_absorpt_correction_T_max 0.4961 _exptl_absorpt_process_details 'SADABS;Sheldrick 1996' _exptl_special_details ; SADABS;Sheldrick,1996 ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14752 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.33 _reflns_number_total 9645 _reflns_number_gt 7847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.1106P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9645 _refine_ls_number_parameters 512 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.6076(2) 0.7179(2) 0.28210(13) 0.0386(5) Uani 1 1 d . . . C2 C 0.6659(3) 0.8147(3) 0.24183(15) 0.0479(6) Uani 1 1 d . . . H2 H 0.6234 0.8341 0.1954 0.057 Uiso 1 1 calc R . . C3 C 0.8019(3) 0.8762(3) 0.28627(17) 0.0559(7) Uani 1 1 d . . . H3 H 0.8638 0.9425 0.2734 0.067 Uiso 1 1 calc R . . C4 C 0.8263(3) 0.8196(3) 0.35276(18) 0.0543(7) Uani 1 1 d . . . H4 H 0.9069 0.8423 0.3912 0.065 Uiso 1 1 calc R . . C5 C 0.7078(2) 0.7225(2) 0.35134(15) 0.0449(6) Uani 1 1 d . . . H5 H 0.6968 0.6706 0.3887 0.054 Uiso 1 1 calc R . . C6 C 0.5005(2) 0.9205(2) 0.38409(14) 0.0385(5) Uani 1 1 d . . . C7 C 0.5651(3) 1.0153(2) 0.34384(18) 0.0494(6) Uani 1 1 d . . . H7 H 0.5254 1.0351 0.2968 0.059 Uiso 1 1 calc R . . C8 C 0.6990(3) 1.0730(3) 0.3881(2) 0.0620(8) Uani 1 1 d . . . H8 H 0.7631 1.1374 0.3751 0.074 Uiso 1 1 calc R . . C9 C 0.7199(3) 1.0171(3) 0.45501(19) 0.0597(8) Uani 1 1 d . . . H9 H 0.7998 1.0386 0.4940 0.072 Uiso 1 1 calc R . . C10 C 0.5978(3) 0.9215(3) 0.45314(15) 0.0469(6) Uani 1 1 d . . . H10 H 0.5842 0.8695 0.4902 0.056 Uiso 1 1 calc R . . C11 C 0.4689(2) 0.6342(2) 0.26040(13) 0.0343(4) Uani 1 1 d . . . C12 C 0.3013(3) 0.4917(2) 0.29495(14) 0.0434(5) Uani 1 1 d . . . H12 H 0.2707 0.4413 0.3302 0.052 Uiso 1 1 calc R . . C13 C 0.2114(3) 0.4892(2) 0.22592(15) 0.0437(5) Uani 1 1 d . . . H13 H 0.1219 0.4392 0.2165 0.052 Uiso 1 1 calc R . . C14 C 0.3794(2) 0.6292(2) 0.18922(13) 0.0375(5) Uani 1 1 d . . . H14 H 0.4103 0.6770 0.1529 0.045 Uiso 1 1 calc R . . C15 C 0.3592(2) 0.8414(2) 0.35864(13) 0.0332(4) Uani 1 1 d . . . C16 C 0.1565(3) 0.7809(3) 0.26787(15) 0.0481(6) Uani 1 1 d . . . H16 H 0.1037 0.7864 0.2202 0.058 Uiso 1 1 calc R . . C17 C 0.0984(2) 0.7020(2) 0.31402(14) 0.0416(5) Uani 1 1 d . . . H17 H 0.0074 0.6555 0.2969 0.050 Uiso 1 1 calc R . . C18 C 0.2983(2) 0.7609(2) 0.40516(13) 0.0359(5) Uani 1 1 d . . . H18 H 0.3499 0.7561 0.4535 0.043 Uiso 1 1 calc R . . C19 C 0.0639(2) 0.3135(2) 0.44756(16) 0.0449(5) Uani 1 1 d . . . C20 C 0.0945(4) 0.1991(3) 0.4157(2) 0.0702(9) Uani 1 1 d . . . H20A H 0.1657 0.1864 0.4537 0.105 Uiso 1 1 calc R . . H20B H 0.1226 0.2099 0.3674 0.105 Uiso 1 1 calc R . . H20C H 0.0149 0.1281 0.4058 0.105 Uiso 1 1 calc R . . C21 C -0.2138(2) 0.4247(2) 0.39054(15) 0.0411(5) Uani 1 1 d . . . C22 C -0.3397(3) 0.3755(3) 0.32573(17) 0.0544(7) Uani 1 1 d . . . H22A H -0.4123 0.3281 0.3460 0.082 Uiso 1 1 calc R . . H22B H -0.3248 0.3230 0.2839 0.082 Uiso 1 1 calc R . . H22C H -0.3630 0.4437 0.3057 0.082 Uiso 1 1 calc R . . C23 C 0.1743(3) 0.5239(3) -0.08217(17) 0.0494(6) Uani 1 1 d . . . C24 C 0.2747(4) 0.5342(4) -0.1323(2) 0.0772(10) Uani 1 1 d . . . H24A H 0.2284 0.5179 -0.1870 0.116 Uiso 1 1 calc R . . H24B H 0.3218 0.4747 -0.1227 0.116 Uiso 1 1 calc R . . H24C H 0.3384 0.6166 -0.1192 0.116 Uiso 1 1 calc R . . C25 C 0.0094(2) 0.7271(2) 0.00627(14) 0.0397(5) Uani 1 1 d . . . C26 C 0.0073(3) 0.8593(2) 0.01169(18) 0.0555(7) Uani 1 1 d . . . H26A H 0.0734 0.9050 -0.0136 0.083 Uiso 1 1 calc R . . H26B H 0.0282 0.8972 0.0663 0.083 Uiso 1 1 calc R . . H26C H -0.0808 0.8601 -0.0141 0.083 Uiso 1 1 calc R . . C27 C 0.5801(3) 0.8117(3) 0.00835(18) 0.0531(6) Uani 1 1 d . . . C28 C 0.6290(4) 0.7003(3) 0.0153(3) 0.0849(11) Uani 1 1 d . . . H28A H 0.7063 0.7213 0.0591 0.127 Uiso 1 1 calc R . . H28B H 0.6536 0.6762 -0.0325 0.127 Uiso 1 1 calc R . . H28C H 0.5582 0.6325 0.0238 0.127 Uiso 1 1 calc R . . C29 C 0.7010(3) 1.1216(2) 0.11242(16) 0.0489(6) Uani 1 1 d . . . C30 C 0.8258(3) 1.1871(3) 0.1757(2) 0.0668(8) Uani 1 1 d . . . H30A H 0.8015 1.2038 0.2248 0.100 Uiso 1 1 calc R . . H30B H 0.8727 1.2642 0.1618 0.100 Uiso 1 1 calc R . . H30C H 0.8835 1.1356 0.1811 0.100 Uiso 1 1 calc R . . C31 C 0.3061(6) 0.1909(5) 0.2078(4) 0.149(3) Uani 1 1 d . . . H31A H 0.3499 0.1447 0.1789 0.223 Uiso 1 1 calc R . . H31B H 0.3623 0.2258 0.2599 0.223 Uiso 1 1 calc R . . H31C H 0.2916 0.2567 0.1808 0.223 Uiso 1 1 calc R . . C32 C 0.1841(6) 0.1132(5) 0.2131(3) 0.0970(14) Uani 1 1 d . . . C33 C 0.5754(9) 0.6954(10) 0.5629(7) 0.101(3) Uani 0.50 1 d P . . C34 C 0.5284(6) 0.5684(7) 0.5184(4) 0.170(5) Uani 0.50 1 d P . . Cu1 Cu 0.06386(3) 0.56343(3) 0.453122(16) 0.03699(8) Uani 1 1 d . . . Cu2 Cu 0.09830(3) 0.53129(2) 0.063610(16) 0.03625(8) Uani 1 1 d . . . Cu3 Cu 0.43272(3) 0.96983(3) 0.053059(18) 0.04277(9) Uani 1 1 d . . . Fe1 Fe 0.66684(3) 0.88747(3) 0.35397(2) 0.03615(9) Uani 1 1 d . . . N1 N 0.4291(2) 0.56250(19) 0.31327(11) 0.0403(4) Uani 1 1 d . . . N2 N 0.2505(2) 0.55727(18) 0.17224(11) 0.0391(4) Uani 1 1 d . . . N3 N 0.2868(2) 0.8502(2) 0.28919(12) 0.0425(4) Uani 1 1 d . . . N4 N 0.16892(19) 0.69052(18) 0.38265(11) 0.0366(4) Uani 1 1 d . . . N5 N 0.0786(6) 0.0459(6) 0.2141(4) 0.163(2) Uani 1 1 d . . . N6 N 0.5284(6) 0.5684(7) 0.5184(4) 0.170(5) Uani 0.50 1 d P . . O1 O 0.1054(2) 0.41036(19) 0.41976(13) 0.0597(5) Uani 1 1 d . . . O2 O -0.00254(19) 0.30402(17) 0.49930(11) 0.0496(4) Uani 1 1 d . . . O3 O -0.11104(19) 0.49520(19) 0.37507(11) 0.0527(5) Uani 1 1 d . . . O4 O -0.21934(18) 0.39149(19) 0.45595(11) 0.0530(5) Uani 1 1 d . . . O5 O 0.21887(19) 0.54605(19) -0.00851(12) 0.0534(4) Uani 1 1 d . . . O6 O 0.0511(2) 0.49334(19) -0.11722(11) 0.0531(4) Uani 1 1 d . . . O7 O 0.09316(18) 0.70244(14) 0.05959(10) 0.0446(4) Uani 1 1 d . . . O8 O -0.07235(19) 0.64910(15) -0.05029(11) 0.0502(4) Uani 1 1 d . . . O9 O 0.5060(2) 0.83025(18) 0.05249(12) 0.0536(5) Uani 1 1 d . . . O10 O 0.6186(3) 0.8795(2) -0.04048(14) 0.0694(6) Uani 1 1 d . . . O11 O 0.5950(2) 1.0705(2) 0.13305(12) 0.0619(5) Uani 1 1 d . . . O12 O 0.7099(2) 1.1209(2) 0.04165(12) 0.0579(5) Uani 1 1 d . . . O13 O 0.31141(18) 0.90398(18) 0.13462(10) 0.0490(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 C1 0.0333(11) 0.0435(13) 0.0375(11) 0.0049(9) 0.0057(9) 0.0122(9) C2 0.0426(13) 0.0609(16) 0.0408(12) 0.0145(11) 0.0136(11) 0.0127(12) C3 0.0396(14) 0.0691(19) 0.0586(16) 0.0098(14) 0.0237(12) 0.0087(13) C4 0.0308(12) 0.0641(18) 0.0621(17) 0.0004(13) 0.0035(11) 0.0146(12) C5 0.0380(12) 0.0442(13) 0.0506(14) 0.0092(11) 0.0012(11) 0.0157(10) C6 0.0333(11) 0.0324(11) 0.0480(13) 0.0058(9) 0.0121(10) 0.0065(9) C7 0.0364(12) 0.0334(12) 0.0769(18) 0.0157(12) 0.0145(12) 0.0054(10) C8 0.0399(14) 0.0326(13) 0.104(3) 0.0067(14) 0.0170(15) -0.0006(11) C9 0.0400(14) 0.0540(17) 0.0662(18) -0.0169(14) 0.0003(13) 0.0041(12) C10 0.0403(13) 0.0506(14) 0.0426(13) -0.0019(11) 0.0084(10) 0.0080(11) C11 0.0365(11) 0.0304(10) 0.0346(10) 0.0033(8) 0.0045(9) 0.0118(9) C12 0.0461(13) 0.0417(13) 0.0398(12) 0.0140(10) 0.0085(10) 0.0086(10) C13 0.0406(12) 0.0369(12) 0.0479(13) 0.0090(10) 0.0046(10) 0.0066(10) C14 0.0425(12) 0.0334(11) 0.0353(11) 0.0082(9) 0.0055(9) 0.0115(9) C15 0.0331(11) 0.0312(10) 0.0366(11) 0.0067(8) 0.0123(9) 0.0089(8) C16 0.0387(13) 0.0603(16) 0.0412(12) 0.0213(11) 0.0072(10) 0.0063(11) C17 0.0297(11) 0.0495(14) 0.0422(12) 0.0135(10) 0.0100(9) 0.0039(9) C18 0.0353(11) 0.0384(12) 0.0346(11) 0.0101(9) 0.0108(9) 0.0095(9) C19 0.0377(12) 0.0442(13) 0.0519(14) 0.0079(11) 0.0119(11) 0.0108(10) C20 0.075(2) 0.0557(18) 0.088(2) 0.0072(16) 0.0325(19) 0.0252(16) C21 0.0359(12) 0.0389(12) 0.0457(13) 0.0094(10) 0.0071(10) 0.0086(9) C22 0.0407(14) 0.0625(17) 0.0516(15) 0.0107(13) 0.0022(12) 0.0085(12) C23 0.0550(16) 0.0445(14) 0.0598(16) 0.0260(12) 0.0221(13) 0.0209(12) C24 0.069(2) 0.105(3) 0.082(2) 0.047(2) 0.0396(19) 0.040(2) C25 0.0442(13) 0.0280(11) 0.0459(13) 0.0083(9) 0.0089(10) 0.0101(9) C26 0.0608(17) 0.0304(12) 0.0715(18) 0.0088(12) 0.0036(14) 0.0167(11) C27 0.0577(16) 0.0439(14) 0.0612(16) 0.0155(12) 0.0098(14) 0.0221(13) C28 0.099(3) 0.068(2) 0.115(3) 0.038(2) 0.035(2) 0.053(2) C29 0.0533(15) 0.0410(13) 0.0535(15) 0.0179(11) 0.0126(12) 0.0128(11) C30 0.0604(19) 0.069(2) 0.0650(19) 0.0162(16) 0.0041(16) 0.0157(15) C31 0.112(4) 0.103(4) 0.210(7) -0.050(4) 0.059(5) 0.015(3) C32 0.108(4) 0.113(4) 0.086(3) 0.004(3) 0.027(3) 0.062(3) C33 0.068(5) 0.109(7) 0.137(9) 0.066(7) 0.037(5) 0.021(5) C34 0.091(5) 0.296(12) 0.175(7) 0.186(10) 0.057(5) 0.071(6) Cu1 0.03150(15) 0.04058(16) 0.03970(15) 0.01667(12) 0.01350(11) 0.00558(11) Cu2 0.03803(15) 0.02836(14) 0.03741(15) 0.00767(11) -0.00077(11) 0.00856(11) Cu3 0.04708(18) 0.04386(17) 0.04564(17) 0.02142(13) 0.02167(13) 0.01481(13) Fe1 0.02821(16) 0.03456(17) 0.04244(18) 0.00853(13) 0.00748(13) 0.00474(12) N1 0.0414(11) 0.0418(11) 0.0347(9) 0.0103(8) 0.0036(8) 0.0107(9) N2 0.0412(10) 0.0347(10) 0.0364(10) 0.0069(8) -0.0003(8) 0.0103(8) N3 0.0374(10) 0.0465(11) 0.0423(10) 0.0183(9) 0.0125(8) 0.0051(8) N4 0.0348(10) 0.0381(10) 0.0383(10) 0.0119(8) 0.0150(8) 0.0075(8) N5 0.145(5) 0.173(6) 0.226(7) 0.068(5) 0.099(5) 0.083(4) N6 0.091(5) 0.296(12) 0.175(7) 0.186(10) 0.057(5) 0.071(6) O1 0.0691(13) 0.0534(12) 0.0735(13) 0.0237(10) 0.0438(11) 0.0227(10) O2 0.0520(11) 0.0436(10) 0.0585(11) 0.0164(8) 0.0237(9) 0.0135(8) O3 0.0426(10) 0.0597(11) 0.0450(10) 0.0159(8) 0.0081(8) -0.0017(8) O4 0.0361(9) 0.0643(12) 0.0518(10) 0.0261(9) 0.0054(8) 0.0026(8) O5 0.0439(10) 0.0597(12) 0.0591(11) 0.0166(9) 0.0125(9) 0.0176(9) O6 0.0516(11) 0.0600(12) 0.0506(10) 0.0187(9) 0.0135(9) 0.0175(9) O7 0.0531(10) 0.0259(8) 0.0471(9) 0.0070(7) -0.0002(8) 0.0082(7) O8 0.0577(11) 0.0304(8) 0.0539(10) 0.0056(7) -0.0065(9) 0.0145(8) O9 0.0609(12) 0.0497(11) 0.0630(12) 0.0284(9) 0.0234(10) 0.0244(9) O10 0.0924(17) 0.0603(13) 0.0866(16) 0.0345(12) 0.0508(14) 0.0442(12) O11 0.0616(13) 0.0627(13) 0.0526(11) 0.0124(10) 0.0188(10) 0.0017(10) O12 0.0487(11) 0.0691(13) 0.0542(11) 0.0219(10) 0.0137(9) 0.0109(10) O13 0.0463(10) 0.0531(11) 0.0403(9) 0.0127(8) 0.0161(8) -0.0014(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 N6 N6 1.516(17) 2_666 ? N6 C34 1.516(17) 2_666 ? C1 C2 1.431(3) . ? C1 C5 1.434(3) . ? C1 C11 1.457(3) . ? C1 Fe1 2.044(2) . ? C2 C3 1.431(4) . ? C2 Fe1 2.044(3) . ? C3 C4 1.407(4) . ? C3 Fe1 2.053(3) . ? C4 C5 1.413(4) . ? C4 Fe1 2.053(3) . ? C5 Fe1 2.042(3) . ? C6 C10 1.426(4) . ? C6 C7 1.437(3) . ? C6 C15 1.464(3) . ? C6 Fe1 2.058(2) . ? C7 C8 1.407(4) . ? C7 Fe1 2.047(3) . ? C8 C9 1.404(5) . ? C8 Fe1 2.041(3) . ? C9 C10 1.428(4) . ? C9 Fe1 2.048(3) . ? C10 Fe1 2.053(3) . ? C11 N1 1.350(3) . ? C11 C14 1.397(3) . ? C12 N1 1.320(3) . ? C12 C13 1.378(3) . ? C13 N2 1.336(3) . ? C14 N2 1.335(3) . ? C15 N3 1.337(3) . ? C15 C18 1.397(3) . ? C16 N3 1.337(3) . ? C16 C17 1.371(3) . ? C17 N4 1.327(3) . ? C18 N4 1.334(3) . ? C19 O2 1.248(3) . ? C19 O1 1.254(3) . ? C19 C20 1.505(4) . ? C21 O4 1.252(3) . ? C21 O3 1.254(3) . ? C21 C22 1.494(3) . ? C23 O5 1.255(3) . ? C23 O6 1.260(3) . ? C23 C24 1.496(4) . ? C25 O8 1.248(3) . ? C25 O7 1.272(3) . ? C25 C26 1.503(3) . ? C27 O9 1.247(3) . ? C27 O10 1.263(3) . ? C27 C28 1.508(4) . ? C29 O11 1.252(3) . ? C29 O12 1.261(3) . ? C29 C30 1.491(4) . ? C31 C32 1.372(7) . ? C32 N5 1.168(7) . ? Cu1 O4 1.9592(18) 2_566 ? Cu1 O3 1.9692(18) . ? Cu1 O1 1.971(2) . ? Cu1 O2 1.9720(18) 2_566 ? Cu1 N4 2.2065(18) . ? Cu1 Cu1 2.6254(5) 2_566 ? Cu2 O5 1.954(2) . ? Cu2 O6 1.9650(19) 2_565 ? Cu2 O7 1.9724(16) . ? Cu2 O8 1.9732(16) 2_565 ? Cu2 N2 2.1736(18) . ? Cu2 Cu2 2.6121(5) 2_565 ? Cu3 O9 1.9570(19) . ? Cu3 O11 1.957(2) . ? Cu3 O10 1.962(2) 2_675 ? Cu3 O12 1.967(2) 2_675 ? Cu3 O13 2.1593(16) . ? Cu3 Cu3 2.5929(6) 2_675 ? O2 Cu1 1.9720(18) 2_566 ? O4 Cu1 1.9592(18) 2_566 ? O6 Cu2 1.9650(19) 2_565 ? O8 Cu2 1.9732(16) 2_565 ? O10 Cu3 1.962(2) 2_675 ? O12 Cu3 1.967(2) 2_675 ? 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 N6 N6 C34 0.0(5) 2_666 2_666 ? C2 C1 C5 107.7(2) . . ? C2 C1 C11 126.8(2) . . ? C5 C1 C11 125.4(2) . . ? C2 C1 Fe1 69.51(15) . . ? C5 C1 Fe1 69.39(14) . . ? C11 C1 Fe1 123.55(16) . . ? C1 C2 C3 107.2(2) . . ? C1 C2 Fe1 69.51(13) . . ? C3 C2 Fe1 69.88(15) . . ? C4 C3 C2 108.5(2) . . ? C4 C3 Fe1 69.97(15) . . ? C2 C3 Fe1 69.22(15) . . ? C3 C4 C5 108.6(2) . . ? C3 C4 Fe1 69.95(16) . . ? C5 C4 Fe1 69.42(14) . . ? C4 C5 C1 107.9(2) . . ? C4 C5 Fe1 70.23(15) . . ? C1 C5 Fe1 69.51(14) . . ? C10 C6 C7 107.4(2) . . ? C10 C6 C15 127.4(2) . . ? C7 C6 C15 125.2(2) . . ? C10 C6 Fe1 69.52(14) . . ? C7 C6 Fe1 69.08(14) . . ? C15 C6 Fe1 127.98(16) . . ? C8 C7 C6 108.0(3) . . ? C8 C7 Fe1 69.64(16) . . ? C6 C7 Fe1 69.93(14) . . ? C9 C8 C7 108.7(3) . . ? C9 C8 Fe1 70.19(17) . . ? C7 C8 Fe1 70.08(15) . . ? C8 C9 C10 108.4(3) . . ? C8 C9 Fe1 69.65(17) . . ? C10 C9 Fe1 69.82(15) . . ? C6 C10 C9 107.5(2) . . ? C6 C10 Fe1 69.89(14) . . ? C9 C10 Fe1 69.43(16) . . ? N1 C11 C14 120.9(2) . . ? N1 C11 C1 116.86(19) . . ? C14 C11 C1 122.2(2) . . ? N1 C12 C13 122.9(2) . . ? N2 C13 C12 121.2(2) . . ? N2 C14 C11 121.5(2) . . ? N3 C15 C18 119.9(2) . . ? N3 C15 C6 117.8(2) . . ? C18 C15 C6 122.3(2) . . ? N3 C16 C17 122.1(2) . . ? N4 C17 C16 121.5(2) . . ? N4 C18 C15 122.3(2) . . ? O2 C19 O1 124.9(2) . . ? O2 C19 C20 117.2(2) . . ? O1 C19 C20 117.9(2) . . ? O4 C21 O3 125.2(2) . . ? O4 C21 C22 117.2(2) . . ? O3 C21 C22 117.6(2) . . ? O5 C23 O6 125.0(3) . . ? O5 C23 C24 117.6(3) . . ? O6 C23 C24 117.4(3) . . ? O8 C25 O7 124.6(2) . . ? O8 C25 C26 117.4(2) . . ? O7 C25 C26 118.0(2) . . ? O9 C27 O10 125.3(3) . . ? O9 C27 C28 116.9(3) . . ? O10 C27 C28 117.8(3) . . ? O11 C29 O12 124.5(3) . . ? O11 C29 C30 118.0(3) . . ? O12 C29 C30 117.6(3) . . ? N5 C32 C31 177.1(7) . . ? O4 Cu1 O3 168.20(7) 2_566 . ? O4 Cu1 O1 89.38(9) 2_566 . ? O3 Cu1 O1 88.40(9) . . ? O4 Cu1 O2 89.41(9) 2_566 2_566 ? O3 Cu1 O2 90.39(9) . 2_566 ? O1 Cu1 O2 168.14(7) . 2_566 ? O4 Cu1 N4 94.72(7) 2_566 . ? O3 Cu1 N4 97.08(7) . . ? O1 Cu1 N4 101.21(7) . . ? O2 Cu1 N4 90.65(7) 2_566 . ? O4 Cu1 Cu1 83.71(5) 2_566 2_566 ? O3 Cu1 Cu1 84.57(5) . 2_566 ? O1 Cu1 Cu1 85.65(6) . 2_566 ? O2 Cu1 Cu1 82.48(5) 2_566 2_566 ? N4 Cu1 Cu1 172.96(5) . 2_566 ? O5 Cu2 O6 168.84(8) . 2_565 ? O5 Cu2 O7 91.27(8) . . ? O6 Cu2 O7 88.01(8) 2_565 . ? O5 Cu2 O8 88.98(9) . 2_565 ? O6 Cu2 O8 89.60(9) 2_565 2_565 ? O7 Cu2 O8 168.87(7) . 2_565 ? O5 Cu2 N2 97.33(8) . . ? O6 Cu2 N2 93.71(8) 2_565 . ? O7 Cu2 N2 102.05(7) . . ? O8 Cu2 N2 88.95(7) 2_565 . ? O5 Cu2 Cu2 85.87(6) . 2_565 ? O6 Cu2 Cu2 82.98(6) 2_565 2_565 ? O7 Cu2 Cu2 85.07(5) . 2_565 ? O8 Cu2 Cu2 83.85(5) 2_565 2_565 ? N2 Cu2 Cu2 172.08(5) . 2_565 ? O9 Cu3 O11 89.02(9) . . ? O9 Cu3 O10 169.30(8) . 2_675 ? O11 Cu3 O10 89.36(10) . 2_675 ? O9 Cu3 O12 90.25(9) . 2_675 ? O11 Cu3 O12 169.18(8) . 2_675 ? O10 Cu3 O12 89.37(10) 2_675 2_675 ? O9 Cu3 O13 92.90(8) . . ? O11 Cu3 O13 96.55(8) . . ? O10 Cu3 O13 97.80(8) 2_675 . ? O12 Cu3 O13 94.27(7) 2_675 . ? O9 Cu3 Cu3 84.40(6) . 2_675 ? O11 Cu3 Cu3 87.69(6) . 2_675 ? O10 Cu3 Cu3 84.96(6) 2_675 2_675 ? O12 Cu3 Cu3 81.49(6) 2_675 2_675 ? O13 Cu3 Cu3 174.94(5) . 2_675 ? C8 Fe1 C5 156.99(11) . . ? C8 Fe1 C1 159.37(12) . . ? C5 Fe1 C1 41.10(9) . . ? C8 Fe1 C2 121.82(13) . . ? C5 Fe1 C2 68.96(11) . . ? C1 Fe1 C2 40.99(10) . . ? C8 Fe1 C7 40.28(11) . . ? C5 Fe1 C7 161.92(10) . . ? C1 Fe1 C7 124.39(10) . . ? C2 Fe1 C7 106.87(12) . . ? C8 Fe1 C9 40.16(13) . . ? C5 Fe1 C9 122.75(12) . . ? C1 Fe1 C9 159.71(12) . . ? C2 Fe1 C9 157.65(12) . . ? C7 Fe1 C9 67.82(12) . . ? C8 Fe1 C3 105.83(13) . . ? C5 Fe1 C3 68.01(12) . . ? C1 Fe1 C3 68.45(11) . . ? C2 Fe1 C3 40.90(11) . . ? C7 Fe1 C3 121.11(12) . . ? C9 Fe1 C3 121.70(12) . . ? C8 Fe1 C4 120.81(12) . . ? C5 Fe1 C4 40.35(11) . . ? C1 Fe1 C4 68.38(10) . . ? C2 Fe1 C4 68.43(11) . . ? C7 Fe1 C4 156.11(11) . . ? C9 Fe1 C4 107.12(12) . . ? C3 Fe1 C4 40.08(12) . . ? C8 Fe1 C10 68.27(13) . . ? C5 Fe1 C10 108.95(11) . . ? C1 Fe1 C10 124.13(10) . . ? C2 Fe1 C10 159.66(10) . . ? C7 Fe1 C10 68.48(12) . . ? C9 Fe1 C10 40.75(11) . . ? C3 Fe1 C10 158.67(11) . . ? C4 Fe1 C10 123.93(12) . . ? C8 Fe1 C6 68.31(10) . . ? C5 Fe1 C6 125.45(10) . . ? C1 Fe1 C6 109.25(9) . . ? C2 Fe1 C6 123.03(10) . . ? C7 Fe1 C6 40.99(10) . . ? C9 Fe1 C6 68.18(10) . . ? C3 Fe1 C6 158.24(11) . . ? C4 Fe1 C6 160.99(11) . . ? C10 Fe1 C6 40.58(10) . . ? C12 N1 C11 116.4(2) . . ? C14 N2 C13 117.0(2) . . ? C14 N2 Cu2 127.02(16) . . ? C13 N2 Cu2 115.90(16) . . ? C15 N3 C16 117.3(2) . . ? C17 N4 C18 116.86(19) . . ? C17 N4 Cu1 118.39(15) . . ? C18 N4 Cu1 124.71(15) . . ? C19 O1 Cu1 121.54(17) . . ? C19 O2 Cu1 125.36(17) . 2_566 ? C21 O3 Cu1 122.43(16) . . ? C21 O4 Cu1 123.98(16) . 2_566 ? C23 O5 Cu2 121.74(18) . . ? C23 O6 Cu2 124.41(18) . 2_565 ? C25 O7 Cu2 122.19(15) . . ? C25 O8 Cu2 124.10(15) . 2_565 ? C27 O9 Cu3 123.31(17) . . ? C27 O10 Cu3 122.00(19) . 2_675 ? C29 O11 Cu3 119.81(18) . . ? C29 O12 Cu3 126.35(18) . 2_675 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.678 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.081 #-----------END data_5a _database_code_depnum_ccdc_archive 'CCDC 262870' _audit_creation_method SHELXL-97 #------------------------------------------------------- _chemical_name_systematic ; Fc(Pyz)2AgClO4 ; _chemical_name_common Fc(Pyz)2AgClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Ag2 Cl2 Fe2 N8 O8' _chemical_formula_weight 1255.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 7.9070(7) _cell_length_b 12.3062(10) _cell_length_c 12.9616(11) _cell_angle_alpha 75.626(2) _cell_angle_beta 74.130(2) _cell_angle_gamma 87.774(2) _cell_volume 1174.61(17) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6994 _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; SADABS; Sheldrick, 1996 ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8881 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5788 _reflns_number_gt 2796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5788 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _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 0.34591(5) 0.97191(3) 0.94630(4) 0.06763(17) Uani 1 1 d . . . C1 C 1.1251(5) 0.7316(4) 0.8859(4) 0.0448(11) Uani 1 1 d . . . C2 C 1.2023(6) 0.6277(4) 0.8757(4) 0.0501(12) Uani 1 1 d . . . H2 H 1.1760 0.5599 0.9290 0.060 Uiso 1 1 calc R . . C3 C 1.3258(6) 0.6444(4) 0.7710(4) 0.0569(13) Uani 1 1 d . . . H3 H 1.3954 0.5896 0.7439 0.068 Uiso 1 1 calc R . . C4 C 1.3259(6) 0.7571(4) 0.7147(4) 0.0614(13) Uani 1 1 d . . . H4 H 1.3955 0.7898 0.6439 0.074 Uiso 1 1 calc R . . C5 C 1.2022(6) 0.8130(4) 0.7837(4) 0.0545(12) Uani 1 1 d . . . H5 H 1.1756 0.8885 0.7662 0.065 Uiso 1 1 calc R . . C6 C 0.8150(6) 0.6737(4) 0.7731(4) 0.0477(11) Uani 1 1 d . . . C7 C 0.8956(6) 0.5682(4) 0.7666(4) 0.0541(12) Uani 1 1 d . . . H7 H 0.8694 0.5011 0.8209 0.065 Uiso 1 1 calc R . . C8 C 1.0207(6) 0.5848(5) 0.6639(4) 0.0647(14) Uani 1 1 d . . . H8 H 1.0913 0.5297 0.6381 0.078 Uiso 1 1 calc R . . C9 C 1.0233(7) 0.6980(5) 0.6055(4) 0.0673(15) Uani 1 1 d . . . H9 H 1.0953 0.7303 0.5353 0.081 Uiso 1 1 calc R . . C10 C 0.8970(7) 0.7538(4) 0.6725(4) 0.0627(14) Uani 1 1 d . . . H10 H 0.8717 0.8294 0.6544 0.075 Uiso 1 1 calc R . . C11 C 0.9918(6) 0.7512(4) 0.9819(4) 0.0444(11) Uani 1 1 d . . . C12 C 0.8299(6) 0.6877(4) 1.1595(4) 0.0583(13) Uani 1 1 d . . . H12 H 0.8005 0.6316 1.2250 0.070 Uiso 1 1 calc R . . C13 C 0.6801(6) 0.6948(4) 0.8666(4) 0.0481(11) Uani 1 1 d . . . C14 C 0.5987(6) 0.7966(4) 0.8634(4) 0.0535(12) Uani 1 1 d . . . H14 H 0.6334 0.8545 0.7996 0.064 Uiso 1 1 calc R . . C15 C 0.4251(6) 0.7285(4) 1.0383(4) 0.0581(13) Uani 1 1 d . . . H15 H 0.3349 0.7363 1.0992 0.070 Uiso 1 1 calc R . . C16 C 0.5088(6) 0.6289(4) 1.0410(4) 0.0602(13) Uani 1 1 d . . . H16 H 0.4747 0.5715 1.1053 0.072 Uiso 1 1 calc R . . C17 C 0.7451(6) 0.7871(4) 1.1553(4) 0.0613(13) Uani 1 1 d . . . H17 H 0.659 0.7964 1.2174 0.074 Uiso 1 1 calc R . . C18 C 0.9089(6) 0.8523(4) 0.9785(4) 0.0465(11) Uani 1 1 d . . . H18 H 0.9419 0.9096 0.9141 0.056 Uiso 1 1 calc R . . C19 C 0.6384(14) 0.9488(6) 0.4448(8) 0.103(2) Uani 1 1 d . . . H19 H 0.7319 0.9124 0.4078 0.124 Uiso 1 1 calc R . . C20 C 0.479(2) 0.9484(6) 0.4251(6) 0.104(3) Uani 1 1 d . . . H20 H 0.4639 0.9139 0.3718 0.125 Uiso 1 1 calc R . . C21 C 0.3415(12) 0.9972(8) 0.4816(10) 0.108(3) Uani 1 1 d . . . H21 H 0.2316 0.9933 0.4693 0.129 Uiso 1 1 calc R . . C22 C 0.605(2) 0.569(4) 0.518(3) 0.175(11) Uani 1 1 d . . . H22 H 0.6804 0.6174 0.5304 0.210 Uiso 1 1 calc R . . C23 C 0.498(5) 0.6080(10) 0.457(2) 0.186(12) Uani 1 1 d . . . H23 H 0.4964 0.6848 0.4267 0.223 Uiso 1 1 calc R . . C24 C 0.394(3) 0.541(4) 0.4387(9) 0.173(9) Uani 1 1 d . . . H24 H 0.3187 0.5697 0.3951 0.207 Uiso 1 1 calc R . . Cl1 Cl 0.16743(18) 0.88250(11) 1.24854(11) 0.0649(4) Uani 1 1 d . . . Fe1 Fe 1.08021(8) 0.68600(5) 0.75320(5) 0.04739(19) Uani 1 1 d . . . N1 N 0.9532(5) 0.6683(3) 1.0732(3) 0.0524(10) Uani 1 1 d . . . N2 N 0.7832(5) 0.8708(3) 1.0641(3) 0.0507(10) Uani 1 1 d . . . N3 N 0.6357(5) 0.6095(3) 0.9574(3) 0.0549(10) Uani 1 1 d . . . N4 N 0.4714(5) 0.8144(3) 0.9495(4) 0.0573(10) Uani 1 1 d . . . O1 O 0.3480(6) 0.9153(5) 1.2015(5) 0.147(2) Uani 1 1 d . . . O2 O 0.1570(10) 0.7780(4) 1.3119(4) 0.182(3) Uani 1 1 d . . . O3 O 0.1003(6) 0.8849(4) 1.1571(4) 0.1018(14) Uani 1 1 d . . . O4 O 0.0890(6) 0.9590(5) 1.3073(4) 0.1312(19) 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 0.0624(3) 0.0591(3) 0.0889(3) -0.0301(2) -0.0255(2) 0.0253(2) C1 0.041(3) 0.044(3) 0.047(3) -0.005(2) -0.013(2) 0.003(2) C2 0.050(3) 0.050(3) 0.049(3) -0.006(2) -0.017(2) 0.014(2) C3 0.041(3) 0.072(4) 0.057(3) -0.017(3) -0.013(2) 0.019(2) C4 0.046(3) 0.071(4) 0.057(3) -0.009(3) -0.003(2) 0.004(3) C5 0.053(3) 0.046(3) 0.062(3) -0.008(2) -0.016(2) 0.004(2) C6 0.049(3) 0.050(3) 0.050(3) -0.018(2) -0.020(2) 0.009(2) C7 0.049(3) 0.053(3) 0.063(3) -0.021(3) -0.015(2) 0.008(2) C8 0.063(3) 0.077(4) 0.066(4) -0.036(3) -0.025(3) 0.022(3) C9 0.072(4) 0.088(4) 0.045(3) -0.018(3) -0.022(3) 0.024(3) C10 0.072(4) 0.065(3) 0.058(3) -0.016(3) -0.031(3) 0.020(3) C11 0.046(3) 0.039(3) 0.049(3) -0.008(2) -0.016(2) -0.001(2) C12 0.067(4) 0.051(3) 0.048(3) -0.004(2) -0.010(3) 0.007(3) C13 0.043(3) 0.047(3) 0.062(3) -0.019(3) -0.022(2) 0.012(2) C14 0.052(3) 0.050(3) 0.063(3) -0.019(3) -0.019(2) 0.007(2) C15 0.049(3) 0.058(3) 0.072(4) -0.030(3) -0.011(3) 0.003(3) C16 0.054(3) 0.054(3) 0.074(4) -0.023(3) -0.012(3) -0.002(2) C17 0.054(3) 0.067(4) 0.063(4) -0.025(3) -0.009(3) 0.008(3) C18 0.052(3) 0.041(3) 0.045(3) -0.005(2) -0.017(2) 0.006(2) C19 0.105(7) 0.058(4) 0.112(7) 0.005(4) 0.004(5) 0.003(4) C20 0.176(9) 0.066(5) 0.072(5) -0.004(4) -0.044(6) -0.024(6) C21 0.107(7) 0.069(5) 0.150(8) 0.020(5) -0.080(7) -0.026(5) C22 0.104(10) 0.26(3) 0.168(17) -0.14(2) 0.031(8) -0.019(10) C23 0.23(2) 0.083(6) 0.156(17) -0.028(9) 0.098(16) 0.001(12) C24 0.161(16) 0.246(17) 0.068(6) -0.016(11) 0.003(7) 0.121(17) Cl1 0.0717(9) 0.0652(9) 0.0621(9) -0.0185(7) -0.0241(7) 0.0137(7) Fe1 0.0482(4) 0.0477(4) 0.0437(4) -0.0089(3) -0.0116(3) 0.0104(3) N1 0.059(3) 0.043(2) 0.051(3) -0.007(2) -0.012(2) 0.0075(18) N2 0.051(2) 0.047(2) 0.058(3) -0.017(2) -0.016(2) 0.0092(18) N3 0.051(2) 0.048(2) 0.068(3) -0.022(2) -0.015(2) 0.0107(19) N4 0.046(2) 0.054(3) 0.081(3) -0.029(2) -0.022(2) 0.009(2) O1 0.077(3) 0.223(6) 0.161(5) -0.113(5) -0.006(3) -0.013(4) O2 0.326(9) 0.089(4) 0.106(4) 0.028(3) -0.068(5) 0.023(5) O3 0.123(4) 0.099(3) 0.108(3) -0.028(3) -0.070(3) 0.006(3) O4 0.101(4) 0.164(5) 0.167(5) -0.118(4) -0.036(3) 0.050(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 N4 2.140(4) . ? Ag1 N2 2.145(4) . ? Ag1 Ag1 3.2890(9) 2_677 ? C1 C2 1.416(6) . ? C1 C5 1.441(6) . ? C1 C11 1.459(6) . ? C1 Fe1 2.056(4) . ? C2 C3 1.411(6) . ? C2 Fe1 2.046(4) . ? C3 C4 1.397(6) . ? C3 Fe1 2.048(4) . ? C4 C5 1.416(6) . ? C4 Fe1 2.043(5) . ? C5 Fe1 2.040(5) . ? C6 C10 1.428(6) . ? C6 C7 1.435(6) . ? C6 C13 1.449(6) . ? C6 Fe1 2.048(4) . ? C7 C8 1.398(6) . ? C7 Fe1 2.040(5) . ? C8 C9 1.408(7) . ? C8 Fe1 2.042(5) . ? C9 C10 1.410(6) . ? C9 Fe1 2.053(5) . ? C10 Fe1 2.046(5) . ? C11 N1 1.327(5) . ? C11 C18 1.379(6) 2_677 ? C12 N1 1.333(5) . ? C12 C17 1.368(6) 2_677 ? C13 N3 1.341(6) . ? C13 C14 1.383(6) . ? C14 N4 1.340(6) . ? C15 N4 1.332(6) . ? C15 C16 1.368(6) . ? C16 N3 1.324(6) . ? C17 N2 1.332(6) . ? C17 C12 1.368(6) 2_677 ? C18 N2 1.332(5) . ? C18 C11 1.379(6) 2_677 ? C19 C21 1.336(10) 2_676 ? C19 C20 1.355(10) . ? C20 C21 1.344(11) . ? C21 C19 1.336(10) 2_676 ? C22 C23 1.314(19) . ? C22 C24 1.331(18) 2_666 ? C23 C24 1.289(19) . ? C24 C22 1.331(18) 2_666 ? Cl1 O2 1.335(5) . ? Cl1 O4 1.379(4) . ? Cl1 O3 1.418(4) . ? Cl1 O1 1.421(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 N4 Ag1 N2 177.17(15) . . ? N4 Ag1 Ag1 84.12(10) . 2_677 ? N2 Ag1 Ag1 98.26(10) . 2_677 ? C2 C1 C5 107.0(4) . . ? C2 C1 C11 126.0(4) . . ? C5 C1 C11 127.0(4) . . ? C2 C1 Fe1 69.4(2) . . ? C5 C1 Fe1 68.8(3) . . ? C11 C1 Fe1 126.4(3) . . ? C3 C2 C1 108.4(4) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 Fe1 70.2(3) . . ? C4 C3 C2 108.6(4) . . ? C4 C3 Fe1 69.8(3) . . ? C2 C3 Fe1 69.8(3) . . ? C3 C4 C5 108.5(4) . . ? C3 C4 Fe1 70.2(3) . . ? C5 C4 Fe1 69.6(3) . . ? C4 C5 C1 107.5(4) . . ? C4 C5 Fe1 69.8(3) . . ? C1 C5 Fe1 70.0(3) . . ? C10 C6 C7 107.2(4) . . ? C10 C6 C13 126.9(4) . . ? C7 C6 C13 125.9(4) . . ? C10 C6 Fe1 69.5(3) . . ? C7 C6 Fe1 69.1(2) . . ? C13 C6 Fe1 124.8(3) . . ? C8 C7 C6 107.5(4) . . ? C8 C7 Fe1 70.1(3) . . ? C6 C7 Fe1 69.8(3) . . ? C7 C8 C9 109.4(4) . . ? C7 C8 Fe1 69.9(3) . . ? C9 C8 Fe1 70.3(3) . . ? C8 C9 C10 107.8(5) . . ? C8 C9 Fe1 69.5(3) . . ? C10 C9 Fe1 69.6(3) . . ? C9 C10 C6 108.1(4) . . ? C9 C10 Fe1 70.1(3) . . ? C6 C10 Fe1 69.7(3) . . ? N1 C11 C18 120.9(4) . 2_677 ? N1 C11 C1 117.6(4) . . ? C18 C11 C1 121.5(4) 2_677 . ? N1 C12 C17 122.4(5) . 2_677 ? N3 C13 C14 120.9(4) . . ? N3 C13 C6 116.6(4) . . ? C14 C13 C6 122.5(4) . . ? N4 C14 C13 122.0(5) . . ? N4 C15 C16 120.7(5) . . ? N3 C16 C15 123.7(5) . . ? N2 C17 C12 121.4(4) . 2_677 ? N2 C18 C11 122.4(4) . 2_677 ? C21 C19 C20 118.5(7) 2_676 . ? C21 C20 C19 120.9(7) . . ? C19 C21 C20 120.5(7) 2_676 . ? C23 C22 C24 119.4(15) . 2_666 ? C24 C23 C22 120.7(15) . . ? C23 C24 C22 119.9(14) . 2_666 ? O2 Cl1 O4 112.8(4) . . ? O2 Cl1 O3 110.0(4) . . ? O4 Cl1 O3 112.4(3) . . ? O2 Cl1 O1 108.4(4) . . ? O4 Cl1 O1 107.6(3) . . ? O3 Cl1 O1 105.2(3) . . ? C5 Fe1 C7 160.96(18) . . ? C5 Fe1 C8 157.9(2) . . ? C7 Fe1 C8 40.05(18) . . ? C5 Fe1 C4 40.57(18) . . ? C7 Fe1 C4 157.15(19) . . ? C8 Fe1 C4 121.6(2) . . ? C5 Fe1 C10 108.4(2) . . ? C7 Fe1 C10 68.7(2) . . ? C8 Fe1 C10 67.7(2) . . ? C4 Fe1 C10 122.4(2) . . ? C5 Fe1 C2 68.38(18) . . ? C7 Fe1 C2 108.09(19) . . ? C8 Fe1 C2 122.2(2) . . ? C4 Fe1 C2 67.81(19) . . ? C10 Fe1 C2 161.67(19) . . ? C5 Fe1 C3 67.87(19) . . ? C7 Fe1 C3 122.39(19) . . ? C8 Fe1 C3 106.62(19) . . ? C4 Fe1 C3 39.93(18) . . ? C10 Fe1 C3 156.9(2) . . ? C2 Fe1 C3 40.33(17) . . ? C5 Fe1 C6 124.45(18) . . ? C7 Fe1 C6 41.08(17) . . ? C8 Fe1 C6 67.88(18) . . ? C4 Fe1 C6 159.49(19) . . ? C10 Fe1 C6 40.83(18) . . ? C2 Fe1 C6 124.94(19) . . ? C3 Fe1 C6 159.97(19) . . ? C5 Fe1 C9 122.7(2) . . ? C7 Fe1 C9 68.1(2) . . ? C8 Fe1 C9 40.2(2) . . ? C4 Fe1 C9 106.4(2) . . ? C10 Fe1 C9 40.25(18) . . ? C2 Fe1 C9 156.90(19) . . ? C3 Fe1 C9 121.0(2) . . ? C6 Fe1 C9 68.13(19) . . ? C5 Fe1 C1 41.18(17) . . ? C7 Fe1 C1 124.05(18) . . ? C8 Fe1 C1 158.7(2) . . ? C4 Fe1 C1 68.40(18) . . ? C10 Fe1 C1 125.39(19) . . ? C2 Fe1 C1 40.38(16) . . ? C3 Fe1 C1 67.92(18) . . ? C6 Fe1 C1 109.76(17) . . ? C9 Fe1 C1 160.5(2) . . ? C11 N1 C12 116.6(4) . . ? C17 N2 C18 116.2(4) . . ? C17 N2 Ag1 122.7(3) . . ? C18 N2 Ag1 121.1(3) . . ? C16 N3 C13 116.0(4) . . ? C15 N4 C14 116.7(4) . . ? C15 N4 Ag1 120.9(3) . . ? C14 N4 Ag1 122.4(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.466 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.080 #-----------END data_5b _database_code_depnum_ccdc_archive 'CCDC 262871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PzClO4Cl _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Ag2 Cl2 Fe2 N8 O8' _chemical_formula_weight 1099.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1873(15) _cell_length_b 14.2776(15) _cell_length_c 20.081(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.238(2) _cell_angle_gamma 90.00 _cell_volume 3975.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8341 _exptl_absorpt_correction_T_max 0.8954 _exptl_absorpt_process_details 'SADABS;Sheldrick 1996' _exptl_special_details ; SADABS;Sheldrick,1996 ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28132 _diffrn_reflns_av_R_equivalents 0.2182 _diffrn_reflns_av_sigmaI/netI 0.2974 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9878 _reflns_number_gt 2773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9878 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3094 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.3289 _refine_ls_wR_factor_gt 0.2471 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 1.12805(15) 0.77902(14) 0.38405(11) 0.0379(6) Uani 1 1 d . . . Fe2 Fe 0.88138(15) -0.05227(15) 0.14707(10) 0.0349(5) Uani 1 1 d . . . Ag1 Ag 0.87945(10) 0.38121(10) 0.24354(7) 0.0649(5) Uani 1 1 d . . . Ag2 Ag 1.10873(11) 0.38196(10) 0.21375(8) 0.0700(5) Uani 1 1 d . . . Cl1 Cl 1.1697(6) 0.1425(5) 0.3641(4) 0.106(2) Uani 1 1 d . . . Cl2 Cl 0.8432(7) 0.5998(5) 0.1339(4) 0.131(3) Uani 1 1 d . . . C1 C 1.0194(11) 0.6950(11) 0.3981(7) 0.040(4) Uani 1 1 d . . . C2 C 1.0557(12) 0.7461(13) 0.4573(9) 0.059(5) Uani 1 1 d . . . H2 H 1.0832 0.7219 0.5000 0.071 Uiso 1 1 calc R . . C3 C 1.0422(13) 0.8443(13) 0.4395(11) 0.064(5) Uani 1 1 d . . . H3 H 1.0592 0.8934 0.4700 0.077 Uiso 1 1 calc R . . C4 C 1.0003(13) 0.8556(12) 0.3707(11) 0.065(6) Uani 1 1 d . . . H4 H 0.9847 0.9111 0.3467 0.078 Uiso 1 1 calc R . . C5 C 0.9870(11) 0.7616(11) 0.3455(8) 0.048(4) Uani 1 1 d . . . H5 H 0.9606 0.7461 0.3004 0.057 Uiso 1 1 calc R . . C6 C 1.2415(10) 0.6997(11) 0.3647(7) 0.034(4) Uani 1 1 d . . . C7 C 1.2719(10) 0.7547(11) 0.4252(9) 0.047(4) Uani 1 1 d . . . H7 H 1.2972 0.7321 0.4687 0.056 Uiso 1 1 calc R . . C8 C 1.2557(11) 0.8521(12) 0.4059(9) 0.051(5) Uani 1 1 d . . . H8 H 1.2691 0.9033 0.4351 0.061 Uiso 1 1 calc R . . C9 C 1.2178(11) 0.8557(11) 0.3381(10) 0.049(5) Uani 1 1 d . . . H9 H 1.2015 0.9107 0.3136 0.059 Uiso 1 1 calc R . . C10 C 1.2061(11) 0.7641(11) 0.3093(8) 0.041(4) Uani 1 1 d . . . H10 H 1.1807 0.7487 0.2640 0.049 Uiso 1 1 calc R . . C11 C 1.0166(10) 0.5933(10) 0.3926(7) 0.035(4) Uani 1 1 d . . . C12 C 0.9700(10) 0.5445(10) 0.3355(7) 0.036(4) Uani 1 1 d . . . H12 H 0.9393 0.5797 0.2983 0.044 Uiso 1 1 calc R . . C13 C 1.0111(12) 0.4097(12) 0.3838(9) 0.053(5) Uani 1 1 d . . . H13 H 1.0117 0.3445 0.3834 0.063 Uiso 1 1 calc R . . C14 C 1.0590(12) 0.4532(12) 0.4421(8) 0.050(4) Uani 1 1 d . . . H14 H 1.0882 0.4172 0.4794 0.060 Uiso 1 1 calc R . . C15 C 1.2415(10) 0.6003(10) 0.3616(8) 0.037(4) Uani 1 1 d . . . C16 C 1.1923(10) 0.5513(11) 0.3049(7) 0.038(4) Uani 1 1 d . . . H16 H 1.1582 0.5851 0.2680 0.046 Uiso 1 1 calc R . . C17 C 1.2425(13) 0.4122(11) 0.3520(10) 0.052(5) Uani 1 1 d . . . H17 H 1.2457 0.3472 0.3512 0.063 Uiso 1 1 calc R . . C18 C 1.2937(12) 0.4619(11) 0.4100(9) 0.053(5) Uani 1 1 d . . . H18 H 1.3302 0.4279 0.4459 0.063 Uiso 1 1 calc R . . C19 C 0.9877(10) 0.0283(10) 0.1201(7) 0.036(4) Uani 1 1 d . . . C20 C 0.9563(10) -0.0448(10) 0.0706(8) 0.041(4) Uani 1 1 d . . . H20 H 0.9301 -0.0366 0.0244 0.050 Uiso 1 1 calc R . . C21 C 0.9734(12) -0.1325(11) 0.1062(9) 0.051(5) Uani 1 1 d . . . H21 H 0.9597 -0.1915 0.0869 0.062 Uiso 1 1 calc R . . C22 C 1.0156(12) -0.1138(13) 0.1770(9) 0.059(5) Uani 1 1 d . . . H22 H 1.0349 -0.1587 0.2106 0.070 Uiso 1 1 calc R . . C23 C 1.0224(11) -0.0184(11) 0.1861(9) 0.048(4) Uani 1 1 d . . . H23 H 1.0453 0.0118 0.2274 0.058 Uiso 1 1 calc R . . C24 C 0.7639(10) 0.0288(10) 0.1499(8) 0.039(4) Uani 1 1 d . . . C25 C 0.7391(11) -0.0438(11) 0.1017(8) 0.044(4) Uani 1 1 d . . . H25 H 0.7136 -0.0364 0.0554 0.053 Uiso 1 1 calc R . . C26 C 0.7604(11) -0.1316(11) 0.1370(9) 0.048(4) Uani 1 1 d . . . H26 H 0.7524 -0.1907 0.1172 0.057 Uiso 1 1 calc R . . C27 C 0.7950(11) -0.1128(12) 0.2058(10) 0.052(5) Uani 1 1 d . . . H27 H 0.8115 -0.1575 0.2400 0.062 Uiso 1 1 calc R . . C28 C 0.8010(11) -0.0138(12) 0.2154(8) 0.047(4) Uani 1 1 d . . . H28 H 0.8245 0.0174 0.2562 0.056 Uiso 1 1 calc R . . C29 C 0.9848(10) 0.1273(10) 0.1051(8) 0.037(4) Uani 1 1 d . . . C30 C 1.0276(11) 0.1950(12) 0.1537(7) 0.043(4) Uani 1 1 d . . . H30 H 1.0584 0.1743 0.1967 0.052 Uiso 1 1 calc R . . C31 C 0.9812(12) 0.3112(13) 0.0788(10) 0.054(5) Uani 1 1 d . . . H31 H 0.9780 0.3742 0.0668 0.065 Uiso 1 1 calc R . . C32 C 0.9409(12) 0.2467(11) 0.0337(8) 0.047(4) Uani 1 1 d . . . H32 H 0.9108 0.2685 -0.0092 0.057 Uiso 1 1 calc R . . C33 C 0.7568(10) 0.1299(10) 0.1348(7) 0.035(4) Uani 1 1 d . . . C34 C 0.8028(10) 0.1946(11) 0.1843(8) 0.041(4) Uani 1 1 d . . . H34 H 0.8345 0.1736 0.2270 0.049 Uiso 1 1 calc R . . C35 C 0.7483(12) 0.3116(11) 0.1072(9) 0.049(4) Uani 1 1 d . . . H35 H 0.7441 0.3746 0.0954 0.058 Uiso 1 1 calc R . . C36 C 0.7030(11) 0.2489(11) 0.0624(9) 0.051(5) Uani 1 1 d . . . H36 H 0.6667 0.2704 0.0212 0.061 Uiso 1 1 calc R . . N1 N 1.0642(9) 0.5434(9) 0.4460(6) 0.047(3) Uani 1 1 d . . . N2 N 0.9650(9) 0.4519(9) 0.3290(6) 0.044(3) Uani 1 1 d . . . N3 N 1.2919(8) 0.5517(9) 0.4150(6) 0.042(3) Uani 1 1 d . . . N4 N 1.1918(9) 0.4562(10) 0.3008(7) 0.047(3) Uani 1 1 d . . . N5 N 0.9389(9) 0.1560(9) 0.0432(6) 0.045(3) Uani 1 1 d . . . N6 N 1.0263(10) 0.2854(9) 0.1414(8) 0.053(4) Uani 1 1 d . . . N7 N 0.7073(9) 0.1568(9) 0.0740(6) 0.042(3) Uani 1 1 d . . . N8 N 0.8006(10) 0.2866(9) 0.1697(7) 0.047(3) Uani 1 1 d . . . O1 O 1.256(2) 0.136(3) 0.413(2) 0.315(10) Uani 1 1 d . . . O2 O 1.189(2) 0.100(3) 0.309(2) 0.315(10) Uani 1 1 d . . . O3 O 1.119(2) 0.211(3) 0.363(2) 0.315(10) Uani 1 1 d . . . O4 O 1.083(2) 0.082(3) 0.363(2) 0.315(10) Uani 1 1 d . . . O5 O 0.883(2) 0.5091(18) 0.1511(12) 0.230(7) Uani 1 1 d . . . O6 O 0.842(2) 0.6456(17) 0.1914(13) 0.230(7) Uani 1 1 d . . . O7 O 0.755(3) 0.6198(18) 0.0868(13) 0.230(7) Uani 1 1 d . . . O8 O 0.900(2) 0.6302(17) 0.0859(13) 0.230(7) 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 Fe1 0.0403(14) 0.0333(13) 0.0415(13) -0.0040(10) 0.0118(10) -0.0035(10) Fe2 0.0353(13) 0.0367(13) 0.0336(12) 0.0039(10) 0.0096(9) 0.0001(10) Ag1 0.0609(10) 0.0606(10) 0.0715(10) -0.0277(8) 0.0104(8) -0.0147(7) Ag2 0.0651(11) 0.0634(10) 0.0810(11) -0.0335(8) 0.0146(8) -0.0167(8) Cl2 0.233(9) 0.081(5) 0.084(5) 0.023(4) 0.046(5) 0.026(5) Cl1 0.118(6) 0.094(5) 0.110(5) -0.026(4) 0.031(4) 0.005(4) C1 0.050(11) 0.036(10) 0.034(9) -0.002(7) 0.011(8) -0.004(7) C2 0.058(13) 0.076(15) 0.050(11) -0.023(10) 0.027(9) -0.021(10) C3 0.059(13) 0.053(13) 0.087(16) -0.028(11) 0.031(11) -0.004(9) C4 0.059(13) 0.037(12) 0.101(17) -0.011(10) 0.024(12) 0.005(8) C5 0.047(11) 0.047(11) 0.050(10) 0.007(9) 0.009(8) 0.013(8) C6 0.025(8) 0.043(10) 0.032(9) -0.008(7) -0.002(6) -0.007(6) C7 0.024(9) 0.045(11) 0.076(12) -0.006(9) 0.021(8) -0.004(7) C8 0.044(11) 0.052(12) 0.059(12) -0.013(9) 0.015(9) 0.005(8) C9 0.046(11) 0.029(10) 0.080(14) 0.013(8) 0.031(10) 0.008(7) C10 0.043(10) 0.044(10) 0.039(9) 0.007(8) 0.016(7) 0.003(7) C11 0.034(9) 0.036(10) 0.038(9) 0.001(7) 0.011(7) -0.004(7) C12 0.049(10) 0.031(9) 0.030(8) -0.007(7) 0.010(7) -0.008(7) C13 0.044(11) 0.042(11) 0.074(13) 0.026(10) 0.018(10) 0.010(8) C14 0.058(12) 0.054(12) 0.035(10) 0.011(9) 0.002(8) 0.001(9) C15 0.037(9) 0.037(10) 0.041(9) -0.003(7) 0.015(7) 0.002(7) C16 0.030(9) 0.046(10) 0.034(9) -0.005(8) -0.003(7) -0.002(7) C17 0.057(12) 0.024(10) 0.085(14) -0.011(9) 0.035(11) 0.004(8) C18 0.057(12) 0.030(10) 0.071(13) 0.006(9) 0.014(9) 0.004(8) C19 0.045(10) 0.037(10) 0.030(8) -0.002(7) 0.016(7) -0.004(7) C20 0.040(10) 0.040(10) 0.040(9) 0.009(8) -0.001(7) -0.003(7) C21 0.053(11) 0.030(10) 0.076(13) -0.001(8) 0.025(10) 0.004(7) C22 0.065(13) 0.054(12) 0.064(12) 0.026(10) 0.028(10) -0.001(9) C23 0.033(10) 0.044(11) 0.064(12) 0.009(9) 0.004(8) 0.002(7) C24 0.038(10) 0.039(10) 0.047(10) 0.002(8) 0.024(7) -0.006(7) C25 0.047(10) 0.040(10) 0.043(10) -0.014(8) 0.005(8) -0.003(7) C26 0.040(10) 0.036(11) 0.068(12) -0.003(8) 0.014(9) 0.002(7) C27 0.034(10) 0.042(10) 0.081(14) 0.026(10) 0.017(9) 0.001(8) C28 0.037(10) 0.070(13) 0.034(9) 0.009(8) 0.006(7) 0.001(8) C29 0.036(9) 0.037(10) 0.042(9) -0.011(8) 0.017(7) -0.009(7) C30 0.040(10) 0.062(12) 0.030(9) -0.003(8) 0.013(7) 0.001(8) C31 0.051(12) 0.056(13) 0.062(12) 0.021(11) 0.026(10) 0.013(9) C32 0.064(12) 0.041(11) 0.036(9) 0.000(8) 0.011(8) -0.003(8) C33 0.027(8) 0.043(10) 0.037(9) -0.006(7) 0.014(7) 0.002(7) C34 0.041(10) 0.046(11) 0.035(9) -0.008(8) 0.005(7) 0.003(7) C35 0.057(12) 0.036(10) 0.056(12) -0.007(9) 0.020(9) -0.004(8) C36 0.048(11) 0.033(10) 0.062(11) 0.004(8) -0.012(9) 0.000(7) N1 0.066(10) 0.030(8) 0.043(8) 0.007(6) 0.005(7) -0.009(7) N2 0.051(9) 0.030(8) 0.048(8) -0.005(7) 0.008(7) -0.012(6) N3 0.035(8) 0.044(9) 0.043(8) -0.005(7) -0.002(6) 0.008(6) N4 0.045(9) 0.045(9) 0.051(9) -0.011(7) 0.008(7) 0.002(7) N5 0.054(9) 0.040(8) 0.034(8) 0.000(6) -0.003(6) -0.010(6) N6 0.049(9) 0.027(8) 0.088(12) -0.006(8) 0.028(8) -0.009(6) N7 0.040(8) 0.039(8) 0.042(8) 0.003(6) -0.003(6) 0.006(6) N8 0.061(10) 0.042(9) 0.042(8) -0.008(7) 0.021(7) 0.002(7) O1 0.162(15) 0.35(3) 0.42(3) -0.12(2) 0.038(15) 0.014(15) O2 0.162(15) 0.35(3) 0.42(3) -0.12(2) 0.038(15) 0.014(15) O3 0.162(15) 0.35(3) 0.42(3) -0.12(2) 0.038(15) 0.014(15) O4 0.162(15) 0.35(3) 0.42(3) -0.12(2) 0.038(15) 0.014(15) O5 0.37(2) 0.152(11) 0.139(9) 0.007(8) -0.011(13) 0.047(13) O6 0.37(2) 0.152(11) 0.139(9) 0.007(8) -0.011(13) 0.047(13) O7 0.37(2) 0.152(11) 0.139(9) 0.007(8) -0.011(13) 0.047(13) O8 0.37(2) 0.152(11) 0.139(9) 0.007(8) -0.011(13) 0.047(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 Cl1 1.40(4) . ? Cl2 O6 1.33(3) . ? Cl2 O5 1.42(2) . ? Cl2 O7 1.43(3) . ? Cl2 O8 1.45(3) . ? Cl1 O3 1.22(4) . ? Cl1 O2 1.34(4) . ? Cl1 O4 1.50(4) . ? Ag1 N2 2.134(12) . ? Ag1 N8 2.139(13) . ? Ag2 N6 2.159(14) . ? Ag2 N4 2.167(12) . ? C1 C2 1.40(2) . ? C1 C5 1.42(2) . ? C1 C11 1.46(2) . ? C1 Fe1 2.020(15) . ? C2 C3 1.45(2) . ? C2 Fe1 2.020(16) . ? C3 C4 1.39(3) . ? C3 Fe1 2.041(17) . ? C4 C5 1.43(2) . ? C4 Fe1 2.084(17) . ? C5 Fe1 2.002(16) . ? C6 C15 1.42(2) . ? C6 C7 1.43(2) . ? C6 C10 1.449(19) . ? C6 Fe1 2.071(15) . ? C7 C8 1.45(2) . ? C7 Fe1 2.062(15) . ? C8 C9 1.36(2) . ? C8 Fe1 2.055(17) . ? C9 C10 1.43(2) . ? C9 Fe1 2.042(15) . ? C10 Fe1 2.057(15) . ? C11 N1 1.345(17) . ? C11 C12 1.384(18) . ? C12 N2 1.329(17) . ? C13 N2 1.303(18) . ? C13 C14 1.37(2) . ? C14 N1 1.291(19) . ? C15 N3 1.349(18) . ? C15 C16 1.392(19) . ? C16 N4 1.360(18) . ? C17 N4 1.29(2) . ? C17 C18 1.42(2) . ? C18 N3 1.287(18) . ? C19 C29 1.44(2) . ? C19 C20 1.445(19) . ? C19 C23 1.47(2) . ? C19 Fe2 2.059(14) . ? C20 C21 1.44(2) . ? C20 Fe2 2.048(15) . ? C21 C22 1.45(2) . ? C21 Fe2 2.037(16) . ? C22 C23 1.38(2) . ? C22 Fe2 2.067(18) . ? C23 Fe2 2.046(15) . ? C24 C25 1.41(2) . ? C24 C28 1.44(2) . ? C24 C33 1.47(2) . ? C24 Fe2 2.039(15) . ? C25 C26 1.44(2) . ? C25 Fe2 2.034(15) . ? C26 C27 1.39(2) . ? C26 Fe2 2.030(16) . ? C27 C28 1.43(2) . ? C27 Fe2 2.062(15) . ? C28 Fe2 2.036(16) . ? C29 N5 1.339(18) . ? C29 C30 1.42(2) . ? C30 N6 1.314(19) . ? C31 C32 1.33(2) . ? C31 N6 1.33(2) . ? C32 N5 1.310(18) . ? C33 N7 1.329(17) . ? C33 C34 1.411(19) . ? C34 N8 1.344(18) . ? C35 C36 1.33(2) . ? C35 N8 1.362(19) . ? C36 N7 1.334(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 O6 Cl2 O5 108.2(15) . . ? O6 Cl2 O7 107.8(18) . . ? O5 Cl2 O7 126.1(17) . . ? O6 Cl2 O8 122.7(19) . . ? O5 Cl2 O8 100.7(17) . . ? O7 Cl2 O8 92.1(16) . . ? O3 Cl1 O2 125(3) . . ? O3 Cl1 O1 119(2) . . ? O2 Cl1 O1 104(2) . . ? O3 Cl1 O4 89(2) . . ? O2 Cl1 O4 92(2) . . ? O1 Cl1 O4 125(2) . . ? N2 Ag1 N8 168.9(5) . . ? N6 Ag2 N4 168.5(6) . . ? C2 C1 C5 106.6(14) . . ? C2 C1 C11 125.8(15) . . ? C5 C1 C11 127.7(14) . . ? C2 C1 Fe1 69.8(9) . . ? C5 C1 Fe1 68.6(9) . . ? C11 C1 Fe1 126.2(11) . . ? C1 C2 C3 106.8(16) . . ? C1 C2 Fe1 69.7(9) . . ? C3 C2 Fe1 69.9(10) . . ? C4 C3 C2 111.3(16) . . ? C4 C3 Fe1 71.9(11) . . ? C2 C3 Fe1 68.3(9) . . ? C3 C4 C5 103.8(16) . . ? C3 C4 Fe1 68.6(10) . . ? C5 C4 Fe1 66.4(9) . . ? C1 C5 C4 111.5(15) . . ? C1 C5 Fe1 69.9(9) . . ? C4 C5 Fe1 72.6(10) . . ? C15 C6 C7 125.6(14) . . ? C15 C6 C10 127.1(13) . . ? C7 C6 C10 107.3(13) . . ? C15 C6 Fe1 124.1(10) . . ? C7 C6 Fe1 69.4(8) . . ? C10 C6 Fe1 68.9(8) . . ? C6 C7 C8 107.3(15) . . ? C6 C7 Fe1 70.0(9) . . ? C8 C7 Fe1 69.2(9) . . ? C9 C8 C7 108.1(15) . . ? C9 C8 Fe1 70.1(10) . . ? C7 C8 Fe1 69.6(9) . . ? C8 C9 C10 111.2(14) . . ? C8 C9 Fe1 71.2(10) . . ? C10 C9 Fe1 70.2(8) . . ? C9 C10 C6 106.1(13) . . ? C9 C10 Fe1 69.1(9) . . ? C6 C10 Fe1 70.0(8) . . ? N1 C11 C12 117.7(13) . . ? N1 C11 C1 117.8(13) . . ? C12 C11 C1 124.5(14) . . ? N2 C12 C11 126.1(14) . . ? N2 C13 C14 125.5(16) . . ? N1 C14 C13 121.1(15) . . ? N3 C15 C16 118.9(14) . . ? N3 C15 C6 118.9(13) . . ? C16 C15 C6 122.2(14) . . ? N4 C16 C15 123.1(14) . . ? N4 C17 C18 120.8(15) . . ? N3 C18 C17 123.0(16) . . ? C29 C19 C20 124.9(13) . . ? C29 C19 C23 128.3(13) . . ? C20 C19 C23 106.8(13) . . ? C29 C19 Fe2 127.7(10) . . ? C20 C19 Fe2 69.0(8) . . ? C23 C19 Fe2 68.6(8) . . ? C21 C20 C19 106.9(13) . . ? C21 C20 Fe2 69.0(9) . . ? C19 C20 Fe2 69.8(8) . . ? C20 C21 C22 108.6(14) . . ? C20 C21 Fe2 69.8(9) . . ? C22 C21 Fe2 70.5(10) . . ? C23 C22 C21 108.5(15) . . ? C23 C22 Fe2 69.6(10) . . ? C21 C22 Fe2 68.2(9) . . ? C22 C23 C19 109.1(15) . . ? C22 C23 Fe2 71.3(10) . . ? C19 C23 Fe2 69.4(8) . . ? C25 C24 C28 107.7(14) . . ? C25 C24 C33 125.6(14) . . ? C28 C24 C33 126.6(14) . . ? C25 C24 Fe2 69.5(9) . . ? C28 C24 Fe2 69.1(9) . . ? C33 C24 Fe2 124.8(9) . . ? C24 C25 C26 107.8(14) . . ? C24 C25 Fe2 69.9(8) . . ? C26 C25 Fe2 69.1(9) . . ? C27 C26 C25 108.3(14) . . ? C27 C26 Fe2 71.4(9) . . ? C25 C26 Fe2 69.4(9) . . ? C26 C27 C28 108.9(14) . . ? C26 C27 Fe2 68.9(10) . . ? C28 C27 Fe2 68.6(9) . . ? C27 C28 C24 107.1(14) . . ? C27 C28 Fe2 70.6(9) . . ? C24 C28 Fe2 69.4(8) . . ? N5 C29 C30 118.9(14) . . ? N5 C29 C19 118.7(13) . . ? C30 C29 C19 122.4(14) . . ? N6 C30 C29 123.7(15) . . ? C32 C31 N6 120.0(16) . . ? N5 C32 C31 127.1(16) . . ? N7 C33 C34 122.2(14) . . ? N7 C33 C24 118.2(13) . . ? C34 C33 C24 119.6(13) . . ? N8 C34 C33 119.9(14) . . ? C36 C35 N8 122.4(16) . . ? C35 C36 N7 123.1(15) . . ? C5 Fe1 C1 41.5(6) . . ? C5 Fe1 C2 68.4(7) . . ? C1 Fe1 C2 40.5(6) . . ? C5 Fe1 C3 66.7(7) . . ? C1 Fe1 C3 68.5(7) . . ? C2 Fe1 C3 41.8(7) . . ? C5 Fe1 C9 124.0(7) . . ? C1 Fe1 C9 161.6(7) . . ? C2 Fe1 C9 156.3(7) . . ? C3 Fe1 C9 120.2(7) . . ? C5 Fe1 C8 155.4(7) . . ? C1 Fe1 C8 159.3(7) . . ? C2 Fe1 C8 121.5(7) . . ? C3 Fe1 C8 104.6(7) . . ? C9 Fe1 C8 38.6(6) . . ? C5 Fe1 C10 110.7(6) . . ? C1 Fe1 C10 125.8(6) . . ? C2 Fe1 C10 160.6(7) . . ? C3 Fe1 C10 157.1(7) . . ? C9 Fe1 C10 40.7(6) . . ? C8 Fe1 C10 67.8(6) . . ? C5 Fe1 C7 163.2(6) . . ? C1 Fe1 C7 124.3(6) . . ? C2 Fe1 C7 106.4(7) . . ? C3 Fe1 C7 120.9(8) . . ? C9 Fe1 C7 67.2(7) . . ? C8 Fe1 C7 41.2(6) . . ? C10 Fe1 C7 68.6(6) . . ? C5 Fe1 C6 127.8(6) . . ? C1 Fe1 C6 110.4(6) . . ? C2 Fe1 C6 123.0(7) . . ? C3 Fe1 C6 158.3(7) . . ? C9 Fe1 C6 67.9(6) . . ? C8 Fe1 C6 68.4(6) . . ? C10 Fe1 C6 41.1(5) . . ? C7 Fe1 C6 40.6(5) . . ? C5 Fe1 C4 41.0(6) . . ? C1 Fe1 C4 70.2(7) . . ? C2 Fe1 C4 69.7(8) . . ? C3 Fe1 C4 39.4(7) . . ? C9 Fe1 C4 105.6(7) . . ? C8 Fe1 C4 117.7(7) . . ? C10 Fe1 C4 123.2(8) . . ? C7 Fe1 C4 154.1(7) . . ? C6 Fe1 C4 162.1(7) . . ? C26 Fe2 C25 41.5(6) . . ? C26 Fe2 C28 68.6(7) . . ? C25 Fe2 C28 69.0(6) . . ? C26 Fe2 C21 104.3(6) . . ? C25 Fe2 C21 120.9(7) . . ? C28 Fe2 C21 157.2(7) . . ? C26 Fe2 C24 69.0(6) . . ? C25 Fe2 C24 40.5(6) . . ? C28 Fe2 C24 41.5(6) . . ? C21 Fe2 C24 158.1(7) . . ? C26 Fe2 C23 155.1(7) . . ? C25 Fe2 C23 162.6(6) . . ? C28 Fe2 C23 108.7(7) . . ? C21 Fe2 C23 68.2(7) . . ? C24 Fe2 C23 126.4(6) . . ? C26 Fe2 C20 121.1(7) . . ? C25 Fe2 C20 106.5(6) . . ? C28 Fe2 C20 160.9(6) . . ? C21 Fe2 C20 41.2(6) . . ? C24 Fe2 C20 123.3(6) . . ? C23 Fe2 C20 69.8(6) . . ? C26 Fe2 C19 159.5(7) . . ? C25 Fe2 C19 124.2(6) . . ? C28 Fe2 C19 124.9(6) . . ? C21 Fe2 C19 68.9(6) . . ? C24 Fe2 C19 109.8(6) . . ? C23 Fe2 C19 42.0(6) . . ? C20 Fe2 C19 41.2(5) . . ? C26 Fe2 C27 39.7(6) . . ? C25 Fe2 C27 68.1(6) . . ? C28 Fe2 C27 40.8(6) . . ? C21 Fe2 C27 120.3(7) . . ? C24 Fe2 C27 68.5(6) . . ? C23 Fe2 C27 122.1(7) . . ? C20 Fe2 C27 156.5(7) . . ? C19 Fe2 C27 160.4(7) . . ? C26 Fe2 C22 119.9(7) . . ? C25 Fe2 C22 157.0(7) . . ? C28 Fe2 C22 122.1(7) . . ? C21 Fe2 C22 41.2(6) . . ? C24 Fe2 C22 160.2(7) . . ? C23 Fe2 C22 39.1(6) . . ? C20 Fe2 C22 69.3(6) . . ? C19 Fe2 C22 68.4(6) . . ? C27 Fe2 C22 106.2(6) . . ? C14 N1 C11 117.9(13) . . ? C13 N2 C12 111.7(14) . . ? C13 N2 Ag1 124.0(11) . . ? C12 N2 Ag1 124.0(11) . . ? C18 N3 C15 117.8(14) . . ? C17 N4 C16 116.4(13) . . ? C17 N4 Ag2 121.5(12) . . ? C16 N4 Ag2 122.1(10) . . ? C32 N5 C29 114.7(13) . . ? C30 N6 C31 115.7(15) . . ? C30 N6 Ag2 121.1(12) . . ? C31 N6 Ag2 122.7(12) . . ? C33 N7 C36 116.1(13) . . ? C34 N8 C35 116.1(13) . . ? C34 N8 Ag1 118.7(10) . . ? C35 N8 Ag1 125.1(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.971 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.210 #-----------END data_6a _database_code_depnum_ccdc_archive 'CCDC 262872' _audit_creation_method SHELXL-97 #------------------------------------------------------- _chemical_name_systematic ; Fc(Pyz)2AgNO3 ; _chemical_name_common Fc(Pyz)2AgNO3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 Ag2 Fe2 N10 O6' _chemical_formula_weight 1102.23 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1428(12) _cell_length_b 10.4419(16) _cell_length_c 12.6662(19) _cell_angle_alpha 69.139(3) _cell_angle_beta 84.507(3) _cell_angle_gamma 85.800(3) _cell_volume 1000.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 1.738 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5432 _exptl_absorpt_correction_T_max 0.9337 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; SADABS; Sheldrick, 1996 ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7466 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4928 _reflns_number_gt 3587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4928 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.008 _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 1.14383(4) 0.07047(3) 0.03547(2) 0.05824(13) Uani 1 1 d . . . Fe1 Fe 0.43731(6) 0.27690(5) 0.26779(4) 0.04324(14) Uani 1 1 d . . . C1 C 0.3754(4) 0.1167(4) 0.2224(3) 0.0429(7) Uani 1 1 d . . . C2 C 0.2768(4) 0.1210(4) 0.3200(3) 0.0495(8) Uani 1 1 d . . . C3 C 0.1889(4) 0.2491(4) 0.2918(4) 0.0548(9) Uani 1 1 d . . . C4 C 0.2344(5) 0.3250(4) 0.1767(4) 0.0558(9) Uani 1 1 d . . . C5 C 0.3491(4) 0.2465(4) 0.1332(3) 0.0482(8) Uani 1 1 d . . . C6 C 0.6809(4) 0.2593(4) 0.3021(3) 0.0452(8) Uani 1 1 d . . . C7 C 0.5756(5) 0.2573(4) 0.3990(3) 0.0534(9) Uani 1 1 d . . . C8 C 0.4810(5) 0.3824(4) 0.3700(4) 0.0597(10) Uani 1 1 d . . . C9 C 0.5250(5) 0.4607(4) 0.2553(4) 0.0610(11) Uani 1 1 d . . . C10 C 0.6478(4) 0.3845(4) 0.2126(4) 0.0517(9) Uani 1 1 d . . . C11 C 0.4829(4) 0.0018(3) 0.2152(3) 0.0419(7) Uani 1 1 d . . . C12 C 0.5831(4) 0.0107(3) 0.1181(3) 0.0427(7) Uani 1 1 d . . . C13 C 0.6826(5) -0.2081(4) 0.2011(4) 0.0561(9) Uani 1 1 d . . . C14 C 0.5807(6) -0.2179(4) 0.2965(4) 0.0614(10) Uani 1 1 d . . . C15 C 0.7938(4) 0.1468(4) 0.2956(3) 0.0427(7) Uani 1 1 d . . . C16 C 0.8857(4) 0.1533(4) 0.1956(3) 0.0447(8) Uani 1 1 d . . . C17 C 0.9966(5) -0.0594(4) 0.2795(3) 0.0559(9) Uani 1 1 d . . . C18 C 0.9094(6) -0.0651(4) 0.3793(4) 0.0657(11) Uani 1 1 d . . . C19 C 0.9582(8) 0.4424(6) 0.6120(4) 0.0899(17) Uani 1 1 d . . . C20 C 0.9131(7) 0.4738(6) 0.4254(5) 0.0854(17) Uani 1 1 d . . . C21 C 0.8723(6) 0.4161(5) 0.5378(6) 0.0852(16) Uani 1 1 d . . . N1 N 0.4816(4) -0.1139(3) 0.3054(3) 0.0547(8) Uani 1 1 d . . . N2 N 0.6842(4) -0.0933(3) 0.1111(2) 0.0473(7) Uani 1 1 d . . . N3 N 0.8083(4) 0.0357(4) 0.3889(3) 0.0578(8) Uani 1 1 d . . . N4 N 0.9863(4) 0.0508(3) 0.1873(3) 0.0471(7) Uani 1 1 d . . . N5 N 0.8037(5) 0.2729(4) -0.0893(3) 0.0652(9) Uani 1 1 d . . . O1 O 0.7426(6) 0.2022(4) -0.1355(3) 0.1090(14) Uani 1 1 d . . . O2 O 0.9498(5) 0.2801(6) -0.0931(4) 0.137(2) Uani 1 1 d . . . O3 O 0.7087(4) 0.3334(3) -0.0410(3) 0.0795(9) Uani 1 1 d . . . H1 H 0.2718 0.0515 0.3905 0.047(10) Uiso 1 1 d R . . H2 H 0.1138 0.2775 0.3401 0.067(13) Uiso 1 1 d R . . H3 H 0.1948 0.4132 0.1364 0.082(15) Uiso 1 1 d R . . H4 H 0.3992 0.2735 0.0600 0.068(13) Uiso 1 1 d R . . H5 H 0.5705 0.1870 0.4692 0.060(12) Uiso 1 1 d R . . H6 H 0.4026 0.4085 0.4177 0.069(13) Uiso 1 1 d R . . H7 H 0.4811 0.5473 0.2149 0.17(3) Uiso 1 1 d R . . H8 H 0.6977 0.4115 0.1393 0.079(15) Uiso 1 1 d R . . H9 H 0.5799 0.0921 0.0561 0.036(8) Uiso 1 1 d R . . H10 H 0.7518 -0.2829 0.2000 0.059(11) Uiso 1 1 d R . . H11 H 0.5807 -0.3005 0.3573 0.074 Uiso 1 1 calc R . . H12 H 0.8751 0.2324 0.1323 0.043(10) Uiso 1 1 d R . . H13 H 1.0642 -0.1338 0.2769 0.053(10) Uiso 1 1 d R . . H14 H 0.9212 -0.1439 0.4427 0.080(15) Uiso 1 1 d R . . H15 H 0.9296 0.4032 0.6893 0.108 Uiso 1 1 calc R . . H16 H 0.8528 0.4559 0.3738 0.102 Uiso 1 1 calc R . . H17 H 0.7843 0.3581 0.5635 0.102 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 0.05137(19) 0.0761(2) 0.05047(19) -0.02915(16) 0.01147(13) -0.00747(15) Fe1 0.0434(3) 0.0445(3) 0.0453(3) -0.0197(2) -0.0058(2) -0.0008(2) C1 0.0432(17) 0.0474(19) 0.0402(17) -0.0177(15) -0.0008(14) -0.0074(14) C2 0.0461(19) 0.052(2) 0.051(2) -0.0202(18) 0.0062(16) -0.0076(16) C3 0.0411(19) 0.062(2) 0.067(3) -0.031(2) -0.0009(18) 0.0000(17) C4 0.049(2) 0.054(2) 0.069(3) -0.025(2) -0.0201(19) 0.0049(17) C5 0.049(2) 0.052(2) 0.0439(19) -0.0142(16) -0.0092(16) -0.0082(16) C6 0.0491(19) 0.049(2) 0.0426(18) -0.0210(16) -0.0088(15) -0.0040(15) C7 0.050(2) 0.068(2) 0.049(2) -0.0288(19) -0.0085(16) 0.0087(18) C8 0.057(2) 0.071(3) 0.067(3) -0.044(2) -0.012(2) 0.011(2) C9 0.063(2) 0.049(2) 0.081(3) -0.031(2) -0.023(2) 0.0000(19) C10 0.049(2) 0.048(2) 0.062(2) -0.0212(18) -0.0083(18) -0.0082(16) C11 0.0474(18) 0.0433(18) 0.0388(17) -0.0183(15) 0.0009(14) -0.0116(14) C12 0.0461(18) 0.0459(19) 0.0372(17) -0.0155(15) 0.0015(14) -0.0093(14) C13 0.064(2) 0.045(2) 0.061(2) -0.0239(19) 0.0060(19) -0.0020(18) C14 0.082(3) 0.045(2) 0.053(2) -0.0147(18) 0.009(2) -0.0024(19) C15 0.0404(17) 0.051(2) 0.0403(17) -0.0196(15) -0.0035(14) -0.0037(14) C16 0.0430(17) 0.051(2) 0.0408(18) -0.0148(16) -0.0050(14) -0.0076(15) C17 0.056(2) 0.051(2) 0.058(2) -0.0190(19) 0.0047(18) 0.0033(17) C18 0.073(3) 0.059(2) 0.050(2) -0.006(2) 0.0108(19) 0.009(2) C19 0.114(5) 0.085(4) 0.058(3) -0.018(3) 0.014(3) 0.015(4) C20 0.099(4) 0.079(3) 0.098(4) -0.050(3) -0.051(3) 0.029(3) C21 0.058(3) 0.063(3) 0.133(5) -0.034(3) 0.003(3) -0.005(2) N1 0.072(2) 0.0468(17) 0.0415(16) -0.0135(14) 0.0095(15) -0.0049(15) N2 0.0487(16) 0.0532(18) 0.0435(16) -0.0220(14) 0.0033(13) -0.0083(13) N3 0.0590(19) 0.063(2) 0.0460(17) -0.0163(16) 0.0064(15) 0.0041(16) N4 0.0443(16) 0.0559(18) 0.0442(16) -0.0215(14) 0.0008(12) -0.0063(13) N5 0.077(3) 0.065(2) 0.0389(17) -0.0028(16) 0.0019(17) 0.0061(19) O1 0.160(4) 0.098(3) 0.076(2) -0.042(2) 0.017(2) -0.023(3) O2 0.064(2) 0.214(5) 0.078(3) 0.014(3) -0.002(2) 0.007(3) O3 0.096(2) 0.069(2) 0.069(2) -0.0228(17) -0.0022(18) 0.0133(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 C19 C21 1.336(8) . ? C19 C20 1.354(8) 2_766 ? C20 C21 1.352(8) . ? C20 C19 1.354(8) 2_766 ? Ag1 N4 2.161(3) . ? Ag1 N2 2.168(3) 2_755 ? Ag1 O2 2.718(4) . ? Ag1 Ag1 3.2109(7) 2_755 ? O2 N5 1.193(5) . ? O3 N5 1.219(5) . ? O1 N5 1.246(6) . ? C1 C2 1.421(5) . ? C1 C5 1.439(5) . ? C1 C11 1.457(5) . ? C1 Fe1 2.060(3) . ? C2 C3 1.413(5) . ? C2 Fe1 2.043(4) . ? C3 C4 1.417(6) . ? C3 Fe1 2.043(4) . ? C4 C5 1.399(5) . ? C4 Fe1 2.036(4) . ? C5 Fe1 2.044(4) . ? C6 C10 1.420(5) . ? C6 C7 1.423(5) . ? C6 C15 1.459(5) . ? C6 Fe1 2.052(3) . ? C7 C8 1.414(5) . ? C7 Fe1 2.038(4) . ? C8 C9 1.417(6) . ? C8 Fe1 2.044(4) . ? C9 C10 1.419(6) . ? C9 Fe1 2.045(4) . ? C10 Fe1 2.045(4) . ? C11 N1 1.335(4) . ? C11 C12 1.387(5) . ? C12 N2 1.337(4) . ? C13 N2 1.328(5) . ? C13 C14 1.375(6) . ? C14 N1 1.336(5) . ? C15 N3 1.337(5) . ? C15 C16 1.389(5) . ? C16 N4 1.328(5) . ? C17 N4 1.320(5) . ? C17 C18 1.373(5) . ? C18 N3 1.321(5) . ? N2 Ag1 2.168(3) 2_755 ? 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 C21 C19 C20 119.9(5) . 2_766 ? C21 C20 C19 120.0(5) . 2_766 ? C19 C21 C20 120.1(5) . . ? N4 Ag1 N2 175.99(11) . 2_755 ? N4 Ag1 O2 92.04(12) . . ? N2 Ag1 O2 89.93(12) 2_755 . ? N4 Ag1 Ag1 85.95(8) . 2_755 ? N2 Ag1 Ag1 97.95(8) 2_755 2_755 ? O2 Ag1 Ag1 74.09(13) . 2_755 ? N5 O2 Ag1 121.9(4) . . ? O2 N5 O3 122.1(5) . . ? O2 N5 O1 120.4(5) . . ? O3 N5 O1 117.4(5) . . ? C2 C1 C5 107.2(3) . . ? C2 C1 C11 125.9(3) . . ? C5 C1 C11 126.9(3) . . ? C2 C1 Fe1 69.1(2) . . ? C5 C1 Fe1 68.85(19) . . ? C11 C1 Fe1 127.2(2) . . ? C3 C2 C1 108.5(3) . . ? C3 C2 Fe1 69.8(2) . . ? C1 C2 Fe1 70.4(2) . . ? C2 C3 C4 107.5(3) . . ? C2 C3 Fe1 69.8(2) . . ? C4 C3 Fe1 69.4(2) . . ? C5 C4 C3 109.2(3) . . ? C5 C4 Fe1 70.2(2) . . ? C3 C4 Fe1 69.9(2) . . ? C4 C5 C1 107.6(3) . . ? C4 C5 Fe1 69.6(2) . . ? C1 C5 Fe1 70.09(19) . . ? C10 C6 C7 108.1(3) . . ? C10 C6 C15 126.8(3) . . ? C7 C6 C15 125.0(3) . . ? C10 C6 Fe1 69.4(2) . . ? C7 C6 Fe1 69.1(2) . . ? C15 C6 Fe1 123.8(2) . . ? C8 C7 C6 107.8(4) . . ? C8 C7 Fe1 70.0(2) . . ? C6 C7 Fe1 70.2(2) . . ? C7 C8 C9 108.2(4) . . ? C7 C8 Fe1 69.5(2) . . ? C9 C8 Fe1 69.8(2) . . ? C8 C9 C10 108.3(4) . . ? C8 C9 Fe1 69.7(2) . . ? C10 C9 Fe1 69.7(2) . . ? C9 C10 C6 107.6(4) . . ? C9 C10 Fe1 69.7(2) . . ? C6 C10 Fe1 70.0(2) . . ? N1 C11 C12 120.6(3) . . ? N1 C11 C1 117.8(3) . . ? C12 C11 C1 121.7(3) . . ? N2 C12 C11 122.2(3) . . ? N2 C13 C14 120.8(3) . . ? N1 C14 C13 122.9(4) . . ? N3 C15 C16 120.0(3) . . ? N3 C15 C6 118.4(3) . . ? C16 C15 C6 121.6(3) . . ? N4 C16 C15 122.5(3) . . ? N4 C17 C18 121.0(4) . . ? N3 C18 C17 123.0(4) . . ? C4 Fe1 C7 157.05(16) . . ? C4 Fe1 C3 40.64(17) . . ? C7 Fe1 C3 121.74(16) . . ? C4 Fe1 C2 68.05(16) . . ? C7 Fe1 C2 108.23(17) . . ? C3 Fe1 C2 40.47(15) . . ? C4 Fe1 C5 40.12(15) . . ? C7 Fe1 C5 161.68(15) . . ? C3 Fe1 C5 68.34(15) . . ? C2 Fe1 C5 68.57(15) . . ? C4 Fe1 C8 120.54(16) . . ? C7 Fe1 C8 40.53(15) . . ? C3 Fe1 C8 104.87(16) . . ? C2 Fe1 C8 121.46(17) . . ? C5 Fe1 C8 156.86(16) . . ? C4 Fe1 C10 121.88(17) . . ? C7 Fe1 C10 68.65(16) . . ? C3 Fe1 C10 156.43(16) . . ? C2 Fe1 C10 162.15(15) . . ? C5 Fe1 C10 108.54(16) . . ? C8 Fe1 C10 68.38(16) . . ? C4 Fe1 C9 105.47(17) . . ? C7 Fe1 C9 68.31(17) . . ? C3 Fe1 C9 119.76(16) . . ? C2 Fe1 C9 156.19(17) . . ? C5 Fe1 C9 122.14(17) . . ? C8 Fe1 C9 40.54(17) . . ? C10 Fe1 C9 40.59(16) . . ? C4 Fe1 C6 159.37(16) . . ? C7 Fe1 C6 40.73(14) . . ? C3 Fe1 C6 159.75(15) . . ? C2 Fe1 C6 125.74(15) . . ? C5 Fe1 C6 125.48(14) . . ? C8 Fe1 C6 68.07(15) . . ? C10 Fe1 C6 40.57(14) . . ? C9 Fe1 C6 68.01(15) . . ? C4 Fe1 C1 68.00(15) . . ? C7 Fe1 C1 124.88(16) . . ? C3 Fe1 C1 68.19(14) . . ? C2 Fe1 C1 40.52(14) . . ? C5 Fe1 C1 41.05(14) . . ? C8 Fe1 C1 158.89(16) . . ? C10 Fe1 C1 125.81(15) . . ? C9 Fe1 C1 160.32(17) . . ? C6 Fe1 C1 111.21(14) . . ? C11 N1 C14 116.6(3) . . ? C13 N2 C12 117.0(3) . . ? C13 N2 Ag1 121.4(2) . 2_755 ? C12 N2 Ag1 121.4(2) . 2_755 ? C18 N3 C15 116.7(3) . . ? C17 N4 C16 116.8(3) . . ? C17 N4 Ag1 121.2(2) . . ? C16 N4 Ag1 121.7(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.055 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.108 #-----------END data_6b _database_code_depnum_ccdc_archive 'CCDC 262873' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H33 Ag2 Cl Fe1 N10 O6' _chemical_formula_weight 1136.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.7418(10) _cell_length_b 13.2726(7) _cell_length_c 14.9841(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.0440(10) _cell_angle_gamma 90.00 _cell_volume 4084.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5379 _exptl_absorpt_correction_T_max 0.7185 _exptl_absorpt_process_details 'SADABS;Sheldrick 1996' _exptl_special_details ; SADABS;Sheldrick,1996 ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15015 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.34 _reflns_number_total 7337 _reflns_number_gt 6807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+0.6300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(2) _refine_ls_number_reflns 7337 _refine_ls_number_parameters 527 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.95001(2) 0.28800(4) 0.55678(3) 0.06637(15) Uani 1 1 d . . . Ag2 Ag 0.86409(2) 0.30291(3) 0.72290(3) 0.05713(12) Uani 1 1 d . . . C1 C 0.8416(2) 0.6589(3) 0.4436(3) 0.0388(9) Uani 1 1 d . . . C2 C 0.8856(2) 0.7174(4) 0.5044(4) 0.0487(11) Uani 1 1 d . . . H2 H 0.9184 0.6923 0.5471 0.058 Uiso 1 1 calc R . . C3 C 0.8704(3) 0.8213(5) 0.4883(5) 0.0610(15) Uani 1 1 d . . . H3 H 0.8921 0.8757 0.5180 0.073 Uiso 1 1 calc R . . C4 C 0.8163(3) 0.8270(4) 0.4189(5) 0.0593(15) Uani 1 1 d . . . H4 H 0.7965 0.8861 0.3956 0.071 Uiso 1 1 calc R . . C5 C 0.7973(3) 0.7270(4) 0.3904(4) 0.0479(11) Uani 1 1 d . . . H5 H 0.7630 0.7093 0.3463 0.057 Uiso 1 1 calc R . . C6 C 0.7415(3) 0.6577(4) 0.6046(4) 0.0457(11) Uani 1 1 d . . . C7 C 0.7878(3) 0.7185(4) 0.6580(4) 0.0539(13) Uani 1 1 d . . . H7 H 0.8227 0.6965 0.6992 0.065 Uiso 1 1 calc R . . C8 C 0.7704(4) 0.8198(5) 0.6361(5) 0.0663(19) Uani 1 1 d . . . H8 H 0.7917 0.8763 0.6626 0.080 Uiso 1 1 calc R . . C9 C 0.7184(4) 0.8217(5) 0.5711(6) 0.070(2) Uani 1 1 d . . . H9 H 0.6987 0.8797 0.5451 0.084 Uiso 1 1 calc R . . C10 C 0.6981(3) 0.7208(4) 0.5482(5) 0.0592(15) Uani 1 1 d . . . H10 H 0.6637 0.7007 0.5054 0.071 Uiso 1 1 calc R . . C11 C 0.8377(2) 0.5501(4) 0.4359(3) 0.0384(9) Uani 1 1 d . . . C12 C 0.7861(3) 0.4103(4) 0.3713(4) 0.0514(11) Uani 1 1 d . . . H12 H 0.7521 0.3812 0.3329 0.062 Uiso 1 1 calc R . . C13 C 0.8335(3) 0.3484(4) 0.4191(4) 0.0553(12) Uani 1 1 d . . . H13 H 0.8309 0.2790 0.4105 0.066 Uiso 1 1 calc R . . C14 C 0.8842(2) 0.4863(4) 0.4844(3) 0.0422(9) Uani 1 1 d . . . H14 H 0.9179 0.5149 0.5237 0.051 Uiso 1 1 calc R . . C15 C 0.7389(2) 0.5456(3) 0.6011(3) 0.0393(9) Uani 1 1 d . . . C16 C 0.6887(3) 0.4035(5) 0.5473(4) 0.0565(12) Uani 1 1 d . . . H16 H 0.6545 0.3711 0.5120 0.068 Uiso 1 1 calc R . . C17 C 0.7370(3) 0.3452(4) 0.5953(4) 0.0531(12) Uani 1 1 d . . . H17 H 0.7352 0.2754 0.5899 0.064 Uiso 1 1 calc R . . C18 C 0.7860(2) 0.4886(4) 0.6521(3) 0.0436(10) Uani 1 1 d . . . H18 H 0.8191 0.5207 0.6899 0.052 Uiso 1 1 calc R . . C19 C 0.9921(2) -0.0407(4) 0.8691(3) 0.0402(9) Uani 1 1 d . . . C20 C 0.9492(3) -0.1103(4) 0.8168(4) 0.0506(11) Uani 1 1 d . . . H20 H 0.9135 -0.0933 0.7749 0.061 Uiso 1 1 calc R . . C21 C 0.9706(3) -0.2087(4) 0.8400(5) 0.0535(13) Uani 1 1 d . . . H21 H 0.9513 -0.2679 0.8162 0.064 Uiso 1 1 calc R . . C22 C 1.0271(3) -0.2022(4) 0.9063(4) 0.0518(12) Uani 1 1 d . . . H22 H 1.0511 -0.2563 0.9326 0.062 Uiso 1 1 calc R . . C23 C 1.0403(3) -0.0987(4) 0.9253(3) 0.0443(10) Uani 1 1 d . . . H23 H 1.0740 -0.0732 0.9666 0.053 Uiso 1 1 calc R . . C24 C 1.0889(2) -0.0427(3) 0.7075(3) 0.0395(9) Uani 1 1 d . . . C25 C 1.0470(3) -0.1115(4) 0.6582(3) 0.0473(10) Uani 1 1 d . . . H25 H 1.0120 -0.0951 0.6148 0.057 Uiso 1 1 calc R . . C26 C 1.0672(4) -0.2116(4) 0.6859(5) 0.0555(13) Uani 1 1 d . . . H26 H 1.0476 -0.2714 0.6641 0.067 Uiso 1 1 calc R . . C27 C 1.1216(3) -0.2023(4) 0.7517(5) 0.0549(14) Uani 1 1 d . . . H27 H 1.1448 -0.2553 0.7814 0.066 Uiso 1 1 calc R . . C28 C 1.1357(2) -0.0977(4) 0.7656(4) 0.0454(10) Uani 1 1 d . . . H28 H 1.1696 -0.0707 0.8056 0.054 Uiso 1 1 calc R . . C29 C 0.9891(2) 0.0685(4) 0.8668(3) 0.0379(8) Uani 1 1 d . . . C30 C 1.0318(3) 0.2202(4) 0.9165(4) 0.0513(11) Uani 1 1 d . . . H30 H 1.0620 0.2579 0.9543 0.062 Uiso 1 1 calc R . . C31 C 0.9870(3) 0.2699(4) 0.8583(4) 0.0493(11) Uani 1 1 d . . . H31 H 0.9883 0.3399 0.8557 0.059 Uiso 1 1 calc R . . C32 C 0.9420(2) 0.1195(4) 0.8096(3) 0.0417(9) Uani 1 1 d . . . H32 H 0.9101 0.0826 0.7738 0.050 Uiso 1 1 calc R . . C33 C 1.0866(2) 0.0679(3) 0.7011(3) 0.0368(8) Uani 1 1 d . . . C34 C 1.1290(3) 0.2219(4) 0.7399(4) 0.0528(12) Uani 1 1 d . . . H34 H 1.1618 0.2610 0.7713 0.063 Uiso 1 1 calc R . . C35 C 1.0795(3) 0.2691(4) 0.6874(4) 0.0489(11) Uani 1 1 d . . . H35 H 1.0782 0.3391 0.6850 0.059 Uiso 1 1 calc R . . C36 C 1.0367(2) 0.1163(4) 0.6447(3) 0.0439(10) Uani 1 1 d . . . H36 H 1.0052 0.0776 0.6100 0.053 Uiso 1 1 calc R . . C37 C 0.6554(3) 0.0251(5) 0.3823(4) 0.1104(14) Uani 1 1 d G . . C38 C 0.5938(4) -0.0182(5) 0.3751(4) 0.1104(14) Uani 1 1 d G . . H38 H 0.5762 -0.0498 0.3218 0.132 Uiso 1 1 calc R . . C39 C 0.5586(3) -0.0141(5) 0.4474(5) 0.1104(14) Uani 1 1 d G . . H39 H 0.5175 -0.0431 0.4426 0.132 Uiso 1 1 calc R . . C40 C 0.5850(3) 0.0332(5) 0.5270(4) 0.1104(14) Uani 1 1 d G . . H40 H 0.5615 0.0359 0.5754 0.132 Uiso 1 1 calc R . . C41 C 0.6465(4) 0.0764(4) 0.5342(4) 0.1104(14) Uani 1 1 d G . . H41 H 0.6642 0.1081 0.5874 0.132 Uiso 1 1 calc R . . C42 C 0.6817(3) 0.0724(5) 0.4619(5) 0.1104(14) Uani 1 1 d G . . H42 H 0.7229 0.1014 0.4667 0.132 Uiso 1 1 calc R . . Cl1 Cl 0.6974(3) 0.0190(4) 0.2941(4) 0.194(2) Uani 1 1 d . . . Fe2 Fe 1.04364(3) -0.12939(4) 0.79198(4) 0.03605(13) Uani 1 1 d . . . Fe1 Fe 0.79202(3) 0.74523(5) 0.52590(5) 0.04296(16) Uani 1 1 d . . . N1 N 0.7887(2) 0.5101(4) 0.3799(3) 0.0485(9) Uani 1 1 d . . . N2 N 0.8818(2) 0.3861(3) 0.4761(3) 0.0473(9) Uani 1 1 d . . . N3 N 0.6890(2) 0.5032(4) 0.5492(3) 0.0504(10) Uani 1 1 d . . . N4 N 0.7850(2) 0.3873(3) 0.6483(3) 0.0436(8) Uani 1 1 d . . . N5 N 1.0350(2) 0.1195(3) 0.9226(3) 0.0472(9) Uani 1 1 d . . . N6 N 0.9407(2) 0.2199(3) 0.8041(3) 0.0428(8) Uani 1 1 d . . . N7 N 1.1326(2) 0.1219(3) 0.7487(3) 0.0466(9) Uani 1 1 d . . . N8 N 1.0331(2) 0.2158(3) 0.6394(3) 0.0495(10) Uani 1 1 d . . . N9 N 0.8527(3) 0.0949(5) 0.5952(5) 0.0785(17) Uani 1 1 d . . . N10 N 0.9542(2) 0.5150(3) 0.7185(3) 0.0486(9) Uani 1 1 d . . . O1 O 0.8833(4) 0.0213(6) 0.6145(6) 0.117(2) Uani 1 1 d . . . O2 O 0.8525(6) 0.1641(9) 0.5554(9) 0.196(6) Uani 1 1 d . . . O3 O 0.8086(5) 0.1019(10) 0.6479(8) 0.161(4) Uani 1 1 d . . . O4 O 0.9281(3) 0.5049(6) 0.7843(4) 0.097(2) Uani 1 1 d . . . O5 O 0.9704(4) 0.4344(5) 0.6851(5) 0.112(2) Uani 1 1 d . . . O6 O 0.9593(5) 0.5959(5) 0.6859(5) 0.132(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 0.0608(3) 0.0661(3) 0.0700(3) 0.0211(2) 0.0012(2) 0.0218(2) Ag2 0.0585(2) 0.0522(2) 0.0576(2) 0.00724(17) -0.00280(17) 0.01674(18) C1 0.040(2) 0.040(2) 0.038(2) 0.0027(16) 0.0088(17) 0.0083(17) C2 0.036(2) 0.055(3) 0.057(3) -0.001(2) 0.013(2) -0.001(2) C3 0.066(4) 0.047(3) 0.077(4) -0.004(3) 0.032(3) -0.014(3) C4 0.068(4) 0.042(3) 0.074(4) 0.015(2) 0.033(3) 0.013(3) C5 0.050(3) 0.048(3) 0.047(3) 0.009(2) 0.011(2) 0.010(2) C6 0.046(3) 0.042(2) 0.053(3) 0.0036(19) 0.019(2) 0.0066(19) C7 0.067(3) 0.046(3) 0.054(3) -0.006(2) 0.026(3) -0.002(2) C8 0.080(5) 0.046(3) 0.081(4) -0.012(3) 0.043(4) 0.002(3) C9 0.071(4) 0.039(3) 0.112(6) 0.011(3) 0.051(4) 0.014(3) C10 0.046(3) 0.051(3) 0.087(4) 0.017(3) 0.031(3) 0.008(2) C11 0.037(2) 0.047(2) 0.0328(19) -0.0002(16) 0.0101(16) 0.0071(17) C12 0.051(3) 0.051(3) 0.050(3) -0.007(2) 0.000(2) 0.002(2) C13 0.062(3) 0.051(3) 0.053(3) -0.003(2) 0.011(2) 0.001(2) C14 0.039(2) 0.045(2) 0.041(2) -0.0022(18) 0.0018(17) 0.0072(18) C15 0.040(2) 0.038(2) 0.042(2) 0.0048(16) 0.0131(18) 0.0002(17) C16 0.043(3) 0.052(3) 0.071(3) 0.000(2) -0.002(2) -0.008(2) C17 0.054(3) 0.042(3) 0.064(3) 0.001(2) 0.011(2) -0.002(2) C18 0.037(2) 0.051(3) 0.042(2) -0.0011(18) 0.0003(17) -0.0009(19) C19 0.042(2) 0.041(2) 0.039(2) -0.0021(16) 0.0073(17) -0.0003(17) C20 0.038(2) 0.054(3) 0.060(3) -0.006(2) 0.008(2) -0.011(2) C21 0.059(3) 0.039(2) 0.067(3) -0.002(2) 0.024(3) -0.011(2) C22 0.064(3) 0.040(2) 0.054(3) 0.011(2) 0.015(2) 0.004(2) C23 0.057(3) 0.042(2) 0.033(2) 0.0072(17) 0.0036(19) 0.003(2) C24 0.040(2) 0.037(2) 0.043(2) 0.0028(16) 0.0093(18) -0.0008(16) C25 0.058(3) 0.048(2) 0.036(2) -0.0046(18) 0.0063(19) -0.002(2) C26 0.067(3) 0.042(2) 0.060(3) -0.014(2) 0.015(3) -0.007(2) C27 0.054(3) 0.031(2) 0.082(4) 0.005(2) 0.018(3) 0.0057(19) C28 0.038(2) 0.040(2) 0.058(3) 0.0017(19) 0.0040(19) -0.0017(18) C29 0.040(2) 0.041(2) 0.0342(19) -0.0037(15) 0.0088(16) -0.0001(16) C30 0.047(3) 0.048(3) 0.057(3) -0.007(2) 0.000(2) -0.001(2) C31 0.053(3) 0.041(2) 0.055(3) -0.0017(19) 0.012(2) 0.004(2) C32 0.042(2) 0.041(2) 0.043(2) -0.0046(17) 0.0082(18) 0.0001(18) C33 0.037(2) 0.039(2) 0.036(2) -0.0019(15) 0.0120(16) -0.0014(16) C34 0.051(3) 0.041(2) 0.065(3) 0.001(2) 0.006(2) -0.004(2) C35 0.057(3) 0.033(2) 0.058(3) 0.002(2) 0.014(2) 0.006(2) C36 0.046(2) 0.044(2) 0.042(2) 0.0044(18) 0.0102(19) 0.0049(19) C37 0.120(3) 0.067(2) 0.139(4) 0.024(2) 0.001(3) 0.020(2) C38 0.120(3) 0.067(2) 0.139(4) 0.024(2) 0.001(3) 0.020(2) C39 0.120(3) 0.067(2) 0.139(4) 0.024(2) 0.001(3) 0.020(2) C40 0.120(3) 0.067(2) 0.139(4) 0.024(2) 0.001(3) 0.020(2) C41 0.120(3) 0.067(2) 0.139(4) 0.024(2) 0.001(3) 0.020(2) C42 0.120(3) 0.067(2) 0.139(4) 0.024(2) 0.001(3) 0.020(2) Cl1 0.220(5) 0.200(5) 0.180(4) 0.096(4) 0.089(4) 0.096(4) Fe2 0.0371(3) 0.0315(3) 0.0391(3) -0.0012(2) 0.0036(2) -0.0023(2) Fe1 0.0415(3) 0.0349(3) 0.0556(4) 0.0033(3) 0.0179(3) 0.0022(2) N1 0.043(2) 0.058(2) 0.044(2) -0.0030(18) 0.0009(16) 0.0060(18) N2 0.050(2) 0.048(2) 0.045(2) 0.0040(16) 0.0074(17) 0.0069(18) N3 0.0386(19) 0.052(2) 0.059(2) 0.0096(19) 0.0018(17) 0.0031(17) N4 0.0406(19) 0.043(2) 0.046(2) 0.0043(15) 0.0039(16) 0.0047(16) N5 0.045(2) 0.045(2) 0.048(2) -0.0057(16) -0.0052(17) 0.0030(16) N6 0.046(2) 0.044(2) 0.0396(19) -0.0013(15) 0.0082(16) 0.0066(16) N7 0.040(2) 0.044(2) 0.054(2) 0.0040(17) 0.0014(17) 0.0038(16) N8 0.052(2) 0.053(2) 0.044(2) 0.0110(17) 0.0109(18) 0.0142(19) N9 0.081(4) 0.050(3) 0.092(4) -0.004(3) -0.029(3) -0.004(3) N10 0.0404(19) 0.047(2) 0.057(2) -0.0052(18) -0.0003(18) -0.0019(16) O1 0.127(6) 0.084(4) 0.124(5) -0.032(4) -0.035(4) 0.017(4) O2 0.229(13) 0.140(8) 0.193(11) 0.089(8) -0.061(9) -0.075(9) O3 0.136(8) 0.204(12) 0.139(8) -0.032(8) 0.006(7) 0.016(7) O4 0.075(3) 0.161(6) 0.057(3) -0.003(3) 0.012(2) 0.012(4) O5 0.131(5) 0.077(4) 0.122(5) -0.032(4) -0.005(4) 0.040(4) O6 0.222(9) 0.055(3) 0.109(5) 0.019(3) -0.016(5) -0.047(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 2.164(4) . ? Ag1 N8 2.196(5) . ? Ag1 Ag2 3.2639(6) . ? Ag2 N6 2.163(4) . ? Ag2 N4 2.164(4) . ? C1 C2 1.425(8) . ? C1 C5 1.446(7) . ? C1 C11 1.450(7) . ? C1 Fe1 2.061(4) . ? C2 C3 1.427(8) . ? C2 Fe1 2.044(5) . ? C3 C4 1.421(11) . ? C3 Fe1 2.058(5) . ? C4 C5 1.433(9) . ? C4 Fe1 2.057(5) . ? C5 Fe1 2.062(5) . ? C6 C7 1.414(9) . ? C6 C10 1.418(9) . ? C6 C15 1.489(7) . ? C6 Fe1 2.045(5) . ? C7 C8 1.419(9) . ? C7 Fe1 2.024(6) . ? C8 C9 1.350(12) . ? C8 Fe1 2.029(6) . ? C9 C10 1.432(10) . ? C9 Fe1 2.028(5) . ? C10 Fe1 2.048(5) . ? C11 N1 1.334(7) . ? C11 C14 1.407(7) . ? C12 N1 1.331(7) . ? C12 C13 1.399(9) . ? C13 N2 1.321(8) . ? C14 N2 1.336(7) . ? C15 N3 1.330(7) . ? C15 C18 1.380(7) . ? C16 N3 1.323(8) . ? C16 C17 1.384(9) . ? C17 N4 1.309(7) . ? C18 N4 1.345(7) . ? C19 C23 1.436(7) . ? C19 C20 1.438(7) . ? C19 C29 1.451(7) . ? C19 Fe2 2.052(4) . ? C20 C21 1.407(9) . ? C20 Fe2 2.060(5) . ? C21 C22 1.429(10) . ? C21 Fe2 2.056(5) . ? C22 C23 1.422(7) . ? C22 Fe2 2.038(5) . ? C23 Fe2 2.049(5) . ? C24 C25 1.398(7) . ? C24 C28 1.412(7) . ? C24 C33 1.472(6) . ? C24 Fe2 2.035(4) . ? C25 C26 1.436(8) . ? C25 Fe2 2.029(5) . ? C26 C27 1.398(10) . ? C26 Fe2 2.042(5) . ? C27 C28 1.427(7) . ? C27 Fe2 2.047(5) . ? C28 Fe2 2.047(5) . ? C29 N5 1.357(6) . ? C29 C32 1.383(7) . ? C30 N5 1.340(7) . ? C30 C31 1.355(8) . ? C31 N6 1.343(8) . ? C32 N6 1.335(6) . ? C33 N7 1.320(6) . ? C33 C36 1.398(7) . ? C34 N7 1.335(7) . ? C34 C35 1.356(9) . ? C35 N8 1.323(8) . ? C36 N8 1.324(7) . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 Cl1 1.684(7) . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? N9 O2 1.095(11) . ? N9 O1 1.180(9) . ? N9 O3 1.291(13) . ? N10 O6 1.190(7) . ? N10 O4 1.196(7) . ? N10 O5 1.248(7) . ? 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 N8 167.94(18) . . ? N2 Ag1 Ag2 90.33(11) . . ? N8 Ag1 Ag2 93.76(11) . . ? N6 Ag2 N4 176.83(15) . . ? N6 Ag2 Ag1 87.81(10) . . ? N4 Ag2 Ag1 95.32(11) . . ? C2 C1 C5 108.2(5) . . ? C2 C1 C11 128.1(5) . . ? C5 C1 C11 123.7(5) . . ? C2 C1 Fe1 69.1(3) . . ? C5 C1 Fe1 69.5(3) . . ? C11 C1 Fe1 125.0(3) . . ? C1 C2 C3 108.2(5) . . ? C1 C2 Fe1 70.3(3) . . ? C3 C2 Fe1 70.2(3) . . ? C4 C3 C2 107.9(6) . . ? C4 C3 Fe1 69.7(3) . . ? C2 C3 Fe1 69.1(3) . . ? C3 C4 C5 109.0(5) . . ? C3 C4 Fe1 69.8(3) . . ? C5 C4 Fe1 69.8(3) . . ? C4 C5 C1 106.7(5) . . ? C4 C5 Fe1 69.5(3) . . ? C1 C5 Fe1 69.4(3) . . ? C7 C6 C10 109.0(5) . . ? C7 C6 C15 127.5(5) . . ? C10 C6 C15 123.5(6) . . ? C7 C6 Fe1 68.9(3) . . ? C10 C6 Fe1 69.8(3) . . ? C15 C6 Fe1 124.5(3) . . ? C6 C7 C8 106.2(6) . . ? C6 C7 Fe1 70.5(3) . . ? C8 C7 Fe1 69.7(4) . . ? C9 C8 C7 109.7(6) . . ? C9 C8 Fe1 70.5(4) . . ? C7 C8 Fe1 69.4(3) . . ? C8 C9 C10 109.5(6) . . ? C8 C9 Fe1 70.6(4) . . ? C10 C9 Fe1 70.2(3) . . ? C6 C10 C9 105.6(7) . . ? C6 C10 Fe1 69.6(3) . . ? C9 C10 Fe1 68.7(3) . . ? N1 C11 C14 119.4(5) . . ? N1 C11 C1 118.4(4) . . ? C14 C11 C1 122.1(4) . . ? N1 C12 C13 121.3(5) . . ? N2 C13 C12 121.5(5) . . ? N2 C14 C11 122.5(5) . . ? N3 C15 C18 121.6(4) . . ? N3 C15 C6 117.7(5) . . ? C18 C15 C6 120.6(5) . . ? N3 C16 C17 123.2(6) . . ? N4 C17 C16 120.6(5) . . ? N4 C18 C15 121.3(4) . . ? C23 C19 C20 107.5(5) . . ? C23 C19 C29 125.0(4) . . ? C20 C19 C29 127.4(5) . . ? C23 C19 Fe2 69.4(3) . . ? C20 C19 Fe2 69.8(3) . . ? C29 C19 Fe2 125.7(3) . . ? C21 C20 C19 108.2(5) . . ? C21 C20 Fe2 69.9(3) . . ? C19 C20 Fe2 69.2(3) . . ? C20 C21 C22 108.4(5) . . ? C20 C21 Fe2 70.2(3) . . ? C22 C21 Fe2 68.9(3) . . ? C23 C22 C21 108.3(5) . . ? C23 C22 Fe2 70.1(3) . . ? C21 C22 Fe2 70.3(3) . . ? C22 C23 C19 107.6(5) . . ? C22 C23 Fe2 69.2(3) . . ? C19 C23 Fe2 69.6(2) . . ? C25 C24 C28 108.1(4) . . ? C25 C24 C33 127.2(4) . . ? C28 C24 C33 124.7(4) . . ? C25 C24 Fe2 69.7(3) . . ? C28 C24 Fe2 70.2(3) . . ? C33 C24 Fe2 126.2(3) . . ? C24 C25 C26 108.5(5) . . ? C24 C25 Fe2 70.1(3) . . ? C26 C25 Fe2 69.8(3) . . ? C27 C26 C25 107.2(5) . . ? C27 C26 Fe2 70.2(3) . . ? C25 C26 Fe2 68.8(3) . . ? C26 C27 C28 108.5(5) . . ? C26 C27 Fe2 69.8(3) . . ? C28 C27 Fe2 69.6(3) . . ? C24 C28 C27 107.7(5) . . ? C24 C28 Fe2 69.3(2) . . ? C27 C28 Fe2 69.6(3) . . ? N5 C29 C32 120.8(4) . . ? N5 C29 C19 117.4(4) . . ? C32 C29 C19 121.8(4) . . ? N5 C30 C31 123.6(5) . . ? N6 C31 C30 121.1(5) . . ? N6 C32 C29 122.1(5) . . ? N7 C33 C36 119.7(4) . . ? N7 C33 C24 119.4(4) . . ? C36 C33 C24 120.8(4) . . ? N7 C34 C35 123.0(5) . . ? N8 C35 C34 120.2(5) . . ? N8 C36 C33 121.7(5) . . ? C38 C37 C42 120.0 . . ? C38 C37 Cl1 119.3(5) . . ? C42 C37 Cl1 120.7(5) . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C41 C42 C37 120.0 . . ? C25 Fe2 C24 40.2(2) . . ? C25 Fe2 C22 156.8(2) . . ? C24 Fe2 C22 159.7(2) . . ? C25 Fe2 C26 41.3(2) . . ? C24 Fe2 C26 68.7(2) . . ? C22 Fe2 C26 119.2(2) . . ? C25 Fe2 C28 67.8(2) . . ? C24 Fe2 C28 40.49(19) . . ? C22 Fe2 C28 122.1(2) . . ? C26 Fe2 C28 68.2(2) . . ? C25 Fe2 C27 68.0(3) . . ? C24 Fe2 C27 68.35(19) . . ? C22 Fe2 C27 104.9(2) . . ? C26 Fe2 C27 40.0(3) . . ? C28 Fe2 C27 40.8(2) . . ? C25 Fe2 C23 161.79(19) . . ? C24 Fe2 C23 125.1(2) . . ? C22 Fe2 C23 40.7(2) . . ? C26 Fe2 C23 155.4(2) . . ? C28 Fe2 C23 107.9(2) . . ? C27 Fe2 C23 121.2(3) . . ? C25 Fe2 C19 125.6(2) . . ? C24 Fe2 C19 110.36(18) . . ? C22 Fe2 C19 68.6(2) . . ? C26 Fe2 C19 160.9(3) . . ? C28 Fe2 C19 124.4(2) . . ? C27 Fe2 C19 158.8(2) . . ? C23 Fe2 C19 40.99(19) . . ? C25 Fe2 C21 122.3(3) . . ? C24 Fe2 C21 159.1(3) . . ? C22 Fe2 C21 40.8(3) . . ? C26 Fe2 C21 105.5(2) . . ? C28 Fe2 C21 157.8(2) . . ? C27 Fe2 C21 120.9(2) . . ? C23 Fe2 C21 68.5(2) . . ? C19 Fe2 C21 68.2(2) . . ? C25 Fe2 C20 109.2(2) . . ? C24 Fe2 C20 125.2(2) . . ? C22 Fe2 C20 68.3(3) . . ? C26 Fe2 C20 122.9(3) . . ? C28 Fe2 C20 161.1(2) . . ? C27 Fe2 C20 157.2(2) . . ? C23 Fe2 C20 68.7(2) . . ? C19 Fe2 C20 40.9(2) . . ? C21 Fe2 C20 40.0(2) . . ? C7 Fe1 C9 67.9(3) . . ? C7 Fe1 C8 41.0(3) . . ? C9 Fe1 C8 38.9(3) . . ? C7 Fe1 C2 107.1(3) . . ? C9 Fe1 C2 156.8(3) . . ? C8 Fe1 C2 122.6(3) . . ? C7 Fe1 C6 40.7(2) . . ? C9 Fe1 C6 67.8(2) . . ? C8 Fe1 C6 67.6(2) . . ? C2 Fe1 C6 124.2(2) . . ? C7 Fe1 C10 68.9(3) . . ? C9 Fe1 C10 41.1(3) . . ? C8 Fe1 C10 67.7(3) . . ? C2 Fe1 C10 160.5(2) . . ? C6 Fe1 C10 40.5(2) . . ? C7 Fe1 C4 154.6(3) . . ? C9 Fe1 C4 105.9(3) . . ? C8 Fe1 C4 118.9(2) . . ? C2 Fe1 C4 68.3(2) . . ? C6 Fe1 C4 161.9(3) . . ? C10 Fe1 C4 123.6(3) . . ? C7 Fe1 C3 119.8(3) . . ? C9 Fe1 C3 120.4(2) . . ? C8 Fe1 C3 104.8(3) . . ? C2 Fe1 C3 40.7(2) . . ? C6 Fe1 C3 157.6(3) . . ? C10 Fe1 C3 158.2(3) . . ? C4 Fe1 C3 40.4(3) . . ? C7 Fe1 C1 125.5(2) . . ? C9 Fe1 C1 160.1(3) . . ? C8 Fe1 C1 160.8(3) . . ? C2 Fe1 C1 40.6(2) . . ? C6 Fe1 C1 111.61(18) . . ? C10 Fe1 C1 125.1(2) . . ? C4 Fe1 C1 68.2(2) . . ? C3 Fe1 C1 68.3(2) . . ? C7 Fe1 C5 163.2(2) . . ? C9 Fe1 C5 122.2(3) . . ? C8 Fe1 C5 155.0(3) . . ? C2 Fe1 C5 69.0(2) . . ? C6 Fe1 C5 127.1(2) . . ? C10 Fe1 C5 108.9(3) . . ? C4 Fe1 C5 40.7(2) . . ? C3 Fe1 C5 68.6(3) . . ? C1 Fe1 C5 41.07(19) . . ? C12 N1 C11 118.3(5) . . ? C13 N2 C14 116.9(5) . . ? C13 N2 Ag1 120.7(4) . . ? C14 N2 Ag1 122.3(4) . . ? C16 N3 C15 115.9(5) . . ? C17 N4 C18 117.3(4) . . ? C17 N4 Ag2 123.3(4) . . ? C18 N4 Ag2 119.3(3) . . ? C30 N5 C29 115.6(4) . . ? C32 N6 C31 116.8(5) . . ? C32 N6 Ag2 123.3(4) . . ? C31 N6 Ag2 119.7(3) . . ? C33 N7 C34 117.4(5) . . ? C35 N8 C36 118.0(5) . . ? C35 N8 Ag1 121.8(3) . . ? C36 N8 Ag1 120.2(4) . . ? O2 N9 O1 142.0(13) . . ? O2 N9 O3 108.9(12) . . ? O1 N9 O3 108.3(9) . . ? O6 N10 O4 121.1(7) . . ? O6 N10 O5 124.3(7) . . ? O4 N10 O5 114.4(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.444 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.098 #-----------END data_6c _database_code_depnum_ccdc_archive 'CCDC 262874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H36 Ag2 Fe2 N10 O6' _chemical_formula_weight 1116.26 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 Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.5823(11) _cell_length_b 13.2444(7) _cell_length_c 14.9704(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.6120(10) _cell_angle_gamma 90.00 _cell_volume 4045.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6262 _exptl_absorpt_correction_T_max 0.8467 _exptl_absorpt_process_details 'SADABS;Sheldrick 1996' _exptl_special_details ; SADABS;Sheldrick,1996 ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14930 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.34 _reflns_number_total 8601 _reflns_number_gt 7951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+2.7756P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.519(19) _refine_ls_number_reflns 8601 _refine_ls_number_parameters 527 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.041 _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 -0.028041(17) 0.19501(3) 0.60409(2) 0.04074(10) Uani 1 1 d . . . Ag2 Ag 0.056725(19) 0.21123(3) 0.43827(3) 0.04911(12) Uani 1 1 d . . . C1 C -0.1522(2) -0.1587(3) 0.4838(3) 0.0334(9) Uani 1 1 d . . . C2 C -0.1069(3) -0.2215(4) 0.5376(3) 0.0381(10) Uani 1 1 d . . . H2 H -0.0725 -0.1998 0.5799 0.046 Uiso 1 1 calc R . . C3 C -0.1231(3) -0.3222(4) 0.5158(4) 0.0497(14) Uani 1 1 d . . . H3 H -0.1016 -0.3786 0.5420 0.060 Uiso 1 1 calc R . . C4 C -0.1776(3) -0.3240(4) 0.4475(5) 0.0517(15) Uani 1 1 d . . . H4 H -0.1976 -0.3814 0.4208 0.062 Uiso 1 1 calc R . . C5 C -0.1964(2) -0.2223(4) 0.4269(4) 0.0430(12) Uani 1 1 d . . . H5A H -0.2309 -0.2011 0.3845 0.052 Uiso 1 1 calc R . . C6 C -0.05159(19) -0.1604(3) 0.3236(3) 0.0294(9) Uani 1 1 d . . . C7 C -0.0079(2) -0.2191(4) 0.3837(3) 0.0351(10) Uani 1 1 d . . . H7 H 0.0251 -0.1941 0.4263 0.042 Uiso 1 1 calc R . . C8 C -0.0233(3) -0.3236(4) 0.3676(4) 0.0428(11) Uani 1 1 d . . . H8 H -0.0021 -0.3785 0.3972 0.051 Uiso 1 1 calc R . . C9 C -0.0775(3) -0.3276(4) 0.2973(4) 0.0428(12) Uani 1 1 d . . . H9 H -0.0974 -0.3863 0.2731 0.051 Uiso 1 1 calc R . . C10 C -0.0961(2) -0.2287(4) 0.2703(3) 0.0362(10) Uani 1 1 d . . . H10 H -0.1304 -0.2106 0.2265 0.043 Uiso 1 1 calc R . . C11 C -0.1543(2) -0.0483(3) 0.4815(3) 0.0291(8) Uani 1 1 d . . . C12 C -0.2038(2) 0.0968(4) 0.4263(4) 0.0384(10) Uani 1 1 d . . . H12 H -0.2376 0.1300 0.3906 0.046 Uiso 1 1 calc R . . C13 C -0.1551(2) 0.1536(4) 0.4754(4) 0.0394(11) Uani 1 1 d . . . H13 H -0.1563 0.2237 0.4710 0.047 Uiso 1 1 calc R . . C14 C -0.1067(2) 0.0095(3) 0.5319(3) 0.0303(9) Uani 1 1 d . . . H14 H -0.0735 -0.0230 0.5694 0.036 Uiso 1 1 calc R . . C15 C -0.05476(19) -0.0507(3) 0.3154(3) 0.0281(8) Uani 1 1 d . . . C16 C -0.1063(2) 0.0894(4) 0.2513(3) 0.0386(10) Uani 1 1 d . . . H16 H -0.1397 0.1189 0.2119 0.046 Uiso 1 1 calc R . . C17 C -0.0603(2) 0.1507(4) 0.2999(3) 0.0381(10) Uani 1 1 d . . . H17 H -0.0636 0.2204 0.2926 0.046 Uiso 1 1 calc R . . C18 C -0.0086(2) 0.0117(3) 0.3647(3) 0.0303(9) Uani 1 1 d . . . H18 H 0.0250 -0.0173 0.4040 0.036 Uiso 1 1 calc R . . C19 C 0.1964(2) 0.5431(3) 0.5865(3) 0.0302(9) Uani 1 1 d . . . C20 C 0.1532(2) 0.6135(4) 0.5370(3) 0.0369(10) Uani 1 1 d . . . H20 H 0.1181 0.5976 0.4936 0.044 Uiso 1 1 calc R . . C21 C 0.1735(3) 0.7129(3) 0.5659(4) 0.0407(11) Uani 1 1 d . . . H21 H 0.1539 0.7730 0.5449 0.049 Uiso 1 1 calc R . . C22 C 0.2289(3) 0.7032(3) 0.6320(4) 0.0424(12) Uani 1 1 d . . . H22 H 0.2519 0.7564 0.6617 0.051 Uiso 1 1 calc R . . C23 C 0.2436(2) 0.5992(3) 0.6458(3) 0.0340(9) Uani 1 1 d . . . H23 H 0.2776 0.5724 0.6860 0.041 Uiso 1 1 calc R . . C24 C 0.0994(2) 0.5416(3) 0.7509(3) 0.0310(9) Uani 1 1 d . . . C25 C 0.0555(2) 0.6095(4) 0.6976(4) 0.0369(10) Uani 1 1 d . . . H25 H 0.0197 0.5915 0.6559 0.044 Uiso 1 1 calc R . . C26 C 0.0769(2) 0.7091(3) 0.7205(4) 0.0374(10) Uani 1 1 d . . . H26 H 0.0578 0.7683 0.6962 0.045 Uiso 1 1 calc R . . C27 C 0.1330(3) 0.7029(4) 0.7873(4) 0.0390(11) Uani 1 1 d . . . H27 H 0.1565 0.7572 0.8145 0.047 Uiso 1 1 calc R . . C28 C 0.1466(2) 0.5996(3) 0.8051(3) 0.0344(9) Uani 1 1 d . . . H28 H 0.1809 0.5742 0.8457 0.041 Uiso 1 1 calc R . . C29 C 0.19349(19) 0.4329(3) 0.5803(3) 0.0281(8) Uani 1 1 d . . . C30 C 0.2353(2) 0.2792(4) 0.6218(4) 0.0385(10) Uani 1 1 d . . . H30 H 0.2677 0.2398 0.6541 0.046 Uiso 1 1 calc R . . C31 C 0.1854(2) 0.2314(3) 0.5693(3) 0.0364(10) Uani 1 1 d . . . H31 H 0.1838 0.1612 0.5685 0.044 Uiso 1 1 calc R . . C32 C 0.1431(2) 0.3847(4) 0.5242(3) 0.0337(9) Uani 1 1 d . . . H32 H 0.1117 0.4236 0.4895 0.040 Uiso 1 1 calc R . . C33 C 0.0968(2) 0.4306(3) 0.7479(3) 0.0269(8) Uani 1 1 d . . . C34 C 0.1401(2) 0.2804(4) 0.7969(4) 0.0384(10) Uani 1 1 d . . . H34 H 0.1705 0.2432 0.8351 0.046 Uiso 1 1 calc R . . C35 C 0.0958(2) 0.2287(4) 0.7383(3) 0.0369(10) Uani 1 1 d . . . H35 H 0.0981 0.1587 0.7351 0.044 Uiso 1 1 calc R . . C36 C 0.0494(2) 0.3793(3) 0.6910(3) 0.0303(9) Uani 1 1 d . . . H36 H 0.0170 0.4160 0.6559 0.036 Uiso 1 1 calc R . . C37 C 0.7687(4) 0.4777(5) 0.2444(5) 0.137(3) Uani 1 1 d GD . . C38 C 0.7071(4) 0.5210(4) 0.2432(5) 0.137(3) Uani 1 1 d G . . H38 H 0.6876 0.5547 0.1921 0.165 Uiso 1 1 calc R . . C39 C 0.6744(3) 0.5138(4) 0.3186(6) 0.137(3) Uani 1 1 d G . . H39 H 0.6332 0.5427 0.3178 0.165 Uiso 1 1 calc R . . C40 C 0.7034(4) 0.4634(5) 0.3950(5) 0.137(3) Uani 1 1 d G . . H40 H 0.6816 0.4585 0.4454 0.165 Uiso 1 1 calc R . . C41 C 0.7651(4) 0.4201(4) 0.3962(5) 0.137(3) Uani 1 1 d G . . H41 H 0.7845 0.3863 0.4473 0.165 Uiso 1 1 calc R . . C42 C 0.7977(3) 0.4273(4) 0.3208(6) 0.137(3) Uani 1 1 d G . . H42 H 0.8389 0.3983 0.3216 0.165 Uiso 1 1 calc R . . C43 C 0.8072(11) 0.4784(13) 0.1790(12) 0.270(13) Uani 1 1 d D . . Fe1 Fe -0.10177(3) -0.24695(4) 0.40490(4) 0.03115(14) Uani 1 1 d . . . Fe2 Fe 0.15025(3) 0.62994(4) 0.67239(4) 0.02714(12) Uani 1 1 d . . . N1 N -0.20412(18) -0.0041(3) 0.4283(3) 0.0370(9) Uani 1 1 d . . . N2 N -0.10691(18) 0.1100(3) 0.5283(3) 0.0323(8) Uani 1 1 d . . . N3 N -0.10426(18) -0.0110(3) 0.2590(3) 0.0344(8) Uani 1 1 d . . . N4 N -0.01142(19) 0.1126(3) 0.3570(3) 0.0367(8) Uani 1 1 d . . . N5 N 0.24014(18) 0.3791(3) 0.6295(3) 0.0357(8) Uani 1 1 d . . . N6 N 0.13908(19) 0.2840(3) 0.5193(3) 0.0350(8) Uani 1 1 d . . . N7 N 0.14263(18) 0.3801(3) 0.8031(3) 0.0354(8) Uani 1 1 d . . . N8 N 0.04901(18) 0.2789(3) 0.6850(3) 0.0325(8) Uani 1 1 d . . . N9 N -0.0412(3) 0.4038(4) 0.4810(4) 0.0575(14) Uani 1 1 d . . . N10 N 0.06128(19) -0.0153(3) 0.5950(3) 0.0378(9) Uani 1 1 d . . . O1 O -0.0380(4) 0.3385(7) 0.4318(6) 0.159(4) Uani 1 1 d . . . O2 O -0.0837(3) 0.3897(6) 0.5353(5) 0.111(2) Uani 1 1 d . . . O3 O -0.0086(3) 0.4787(4) 0.4963(4) 0.0826(16) Uani 1 1 d . . . O4 O 0.0339(2) -0.0023(5) 0.6631(3) 0.0773(15) Uani 1 1 d . . . O5 O 0.0818(3) 0.0605(4) 0.5615(4) 0.0912(19) Uani 1 1 d . . . O6 O 0.0640(4) -0.0980(4) 0.5642(4) 0.103(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 0.04178(19) 0.03617(17) 0.0421(2) -0.00483(15) -0.00229(15) -0.01117(15) Ag2 0.0436(2) 0.0482(2) 0.0539(3) -0.01694(18) 0.00044(18) -0.01485(17) C1 0.032(2) 0.030(2) 0.040(3) -0.0049(17) 0.0139(18) -0.0040(17) C2 0.044(3) 0.035(2) 0.038(3) 0.0043(19) 0.016(2) 0.0012(19) C3 0.061(4) 0.038(3) 0.057(3) 0.012(2) 0.030(3) 0.000(2) C4 0.052(3) 0.031(2) 0.080(4) -0.008(2) 0.039(3) -0.010(2) C5 0.029(2) 0.040(3) 0.064(3) -0.017(2) 0.019(2) -0.0068(18) C6 0.0234(19) 0.036(2) 0.031(2) -0.0019(16) 0.0085(16) -0.0050(16) C7 0.029(2) 0.038(2) 0.040(3) 0.0018(19) 0.0110(19) 0.0046(17) C8 0.041(3) 0.035(2) 0.057(3) 0.004(2) 0.026(2) 0.006(2) C9 0.045(3) 0.030(2) 0.058(3) -0.012(2) 0.026(2) -0.011(2) C10 0.035(2) 0.037(2) 0.037(2) -0.0081(19) 0.0069(19) -0.0070(18) C11 0.0284(19) 0.032(2) 0.029(2) -0.0039(15) 0.0111(16) -0.0022(16) C12 0.029(2) 0.036(2) 0.048(3) 0.002(2) -0.0022(19) 0.0058(17) C13 0.036(2) 0.030(2) 0.053(3) -0.001(2) 0.009(2) 0.0018(18) C14 0.0290(19) 0.032(2) 0.030(2) 0.0005(16) 0.0024(17) -0.0015(16) C15 0.0251(19) 0.031(2) 0.030(2) -0.0008(16) 0.0066(16) -0.0016(15) C16 0.040(2) 0.033(2) 0.040(3) 0.0049(18) -0.001(2) -0.0011(18) C17 0.041(2) 0.033(2) 0.041(3) 0.0031(19) 0.006(2) -0.0005(19) C18 0.030(2) 0.029(2) 0.031(2) 0.0041(16) 0.0018(17) -0.0013(16) C19 0.031(2) 0.028(2) 0.032(2) -0.0021(16) 0.0049(17) -0.0008(16) C20 0.043(2) 0.038(2) 0.029(2) 0.0027(18) 0.0046(19) 0.005(2) C21 0.044(3) 0.030(2) 0.050(3) 0.011(2) 0.014(2) 0.0049(19) C22 0.040(3) 0.026(2) 0.063(4) -0.002(2) 0.017(2) -0.0044(18) C23 0.026(2) 0.031(2) 0.045(3) -0.0017(18) 0.0016(18) -0.0007(16) C24 0.029(2) 0.032(2) 0.032(2) -0.0016(16) 0.0043(17) 0.0016(16) C25 0.027(2) 0.039(3) 0.045(3) 0.000(2) 0.0073(19) 0.0023(18) C26 0.035(2) 0.029(2) 0.049(3) 0.0009(19) 0.012(2) 0.0052(18) C27 0.044(3) 0.036(3) 0.038(3) -0.0102(19) 0.007(2) 0.0011(19) C28 0.039(2) 0.034(2) 0.030(2) -0.0046(17) 0.0011(18) -0.0005(18) C29 0.027(2) 0.0265(19) 0.032(2) -0.0017(16) 0.0083(16) 0.0014(15) C30 0.034(2) 0.031(2) 0.052(3) 0.0015(19) 0.008(2) 0.0022(17) C31 0.037(2) 0.029(2) 0.045(3) -0.0028(19) 0.010(2) -0.0057(18) C32 0.031(2) 0.037(2) 0.033(2) -0.0002(17) 0.0043(18) 0.0012(17) C33 0.0296(19) 0.029(2) 0.0238(19) 0.0026(15) 0.0078(15) -0.0031(15) C34 0.034(2) 0.036(2) 0.044(3) 0.0058(19) -0.002(2) 0.0012(18) C35 0.039(2) 0.030(2) 0.041(3) 0.0017(18) 0.005(2) -0.0019(17) C36 0.032(2) 0.031(2) 0.029(2) 0.0005(16) 0.0065(16) 0.0012(16) C37 0.136(4) 0.058(2) 0.196(6) -0.028(3) -0.059(4) -0.022(2) C38 0.136(4) 0.058(2) 0.196(6) -0.028(3) -0.059(4) -0.022(2) C39 0.136(4) 0.058(2) 0.196(6) -0.028(3) -0.059(4) -0.022(2) C40 0.136(4) 0.058(2) 0.196(6) -0.028(3) -0.059(4) -0.022(2) C41 0.136(4) 0.058(2) 0.196(6) -0.028(3) -0.059(4) -0.022(2) C42 0.136(4) 0.058(2) 0.196(6) -0.028(3) -0.059(4) -0.022(2) C43 0.40(2) 0.226(15) 0.243(17) -0.192(14) 0.250(18) -0.249(17) Fe1 0.0297(3) 0.0249(3) 0.0408(4) -0.0017(2) 0.0119(2) -0.0018(2) Fe2 0.0271(3) 0.0230(3) 0.0311(3) 0.0000(2) 0.0027(2) 0.0020(2) N1 0.0272(17) 0.035(2) 0.048(2) -0.0092(17) 0.0016(16) -0.0027(15) N2 0.0326(18) 0.0292(18) 0.035(2) -0.0032(14) 0.0051(15) -0.0025(14) N3 0.0307(17) 0.037(2) 0.034(2) 0.0026(15) -0.0030(15) -0.0050(15) N4 0.0372(19) 0.037(2) 0.036(2) -0.0026(15) 0.0038(16) -0.0090(16) N5 0.0324(19) 0.0307(19) 0.043(2) -0.0034(15) 0.0022(16) -0.0013(15) N6 0.0352(19) 0.036(2) 0.035(2) -0.0090(15) 0.0083(16) -0.0088(15) N7 0.0344(19) 0.0337(19) 0.036(2) 0.0048(15) -0.0031(16) -0.0041(15) N8 0.0330(19) 0.035(2) 0.0297(19) 0.0024(15) 0.0065(15) -0.0041(15) N9 0.058(3) 0.038(2) 0.069(3) -0.001(2) -0.022(3) 0.011(2) N10 0.0369(19) 0.032(2) 0.041(2) 0.0037(16) -0.0079(17) 0.0010(15) O1 0.156(7) 0.142(6) 0.152(7) -0.099(6) -0.072(6) 0.088(6) O2 0.077(4) 0.148(6) 0.104(5) 0.028(4) -0.005(4) -0.019(4) O3 0.086(3) 0.049(3) 0.104(4) 0.022(3) -0.021(3) -0.012(2) O4 0.057(3) 0.128(4) 0.048(3) 0.003(3) 0.011(2) -0.002(3) O5 0.115(4) 0.080(4) 0.074(3) 0.023(3) -0.009(3) -0.054(3) O6 0.178(6) 0.045(3) 0.077(4) -0.013(2) -0.022(4) 0.046(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 2.168(4) . ? Ag1 N8 2.170(4) . ? Ag1 Ag2 3.2249(6) . ? Ag2 N4 2.168(4) . ? Ag2 N6 2.174(4) . ? Ag2 O1 2.569(6) . ? C1 C2 1.418(7) . ? C1 C5 1.435(7) . ? C1 C11 1.463(6) . ? C1 Fe1 2.039(5) . ? C2 C3 1.403(7) . ? C2 Fe1 2.032(5) . ? C3 C4 1.413(9) . ? C3 Fe1 2.034(6) . ? C4 C5 1.425(8) . ? C4 Fe1 2.036(5) . ? C5 Fe1 2.044(5) . ? C6 C7 1.417(6) . ? C6 C10 1.448(6) . ? C6 C15 1.459(6) . ? C6 Fe1 2.048(4) . ? C7 C8 1.433(7) . ? C7 Fe1 2.033(5) . ? C8 C9 1.429(8) . ? C8 Fe1 2.047(5) . ? C9 C10 1.408(7) . ? C9 Fe1 2.049(5) . ? C10 Fe1 2.048(5) . ? C11 N1 1.346(6) . ? C11 C14 1.386(6) . ? C12 N1 1.336(6) . ? C12 C13 1.385(7) . ? C13 N2 1.317(6) . ? C14 N2 1.333(6) . ? C15 N3 1.342(5) . ? C15 C18 1.395(6) . ? C16 N3 1.335(6) . ? C16 C17 1.380(7) . ? C17 N4 1.330(6) . ? C18 N4 1.342(6) . ? C19 C20 1.427(6) . ? C19 C23 1.434(6) . ? C19 C29 1.462(6) . ? C19 Fe2 2.051(4) . ? C20 C21 1.431(7) . ? C20 Fe2 2.048(5) . ? C21 C22 1.412(8) . ? C21 Fe2 2.045(5) . ? C22 C23 1.420(6) . ? C22 Fe2 2.045(5) . ? C23 Fe2 2.054(4) . ? C24 C28 1.409(6) . ? C24 C25 1.439(6) . ? C24 C33 1.472(6) . ? C24 Fe2 2.042(5) . ? C25 C26 1.420(7) . ? C25 Fe2 2.053(5) . ? C26 C27 1.425(8) . ? C26 Fe2 2.046(5) . ? C27 C28 1.415(7) . ? C27 Fe2 2.045(5) . ? C28 Fe2 2.039(5) . ? C29 N5 1.337(6) . ? C29 C32 1.399(6) . ? C30 N5 1.330(6) . ? C30 C31 1.364(7) . ? C31 N6 1.329(6) . ? C32 N6 1.338(6) . ? C33 N7 1.346(5) . ? C33 C36 1.385(6) . ? C34 N7 1.325(6) . ? C34 C35 1.363(7) . ? C35 N8 1.342(6) . ? C36 N8 1.334(6) . ? N9 O1 1.144(7) . ? N9 O3 1.202(6) . ? N9 O2 1.284(9) . ? N10 O6 1.193(6) . ? N10 O5 1.223(6) . ? N10 O4 1.240(7) . ? C42 C41 1.3900 . ? C42 C37 1.3900 . ? C41 C40 1.3900 . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C43 1.339(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 N8 177.58(15) . . ? N2 Ag1 Ag2 94.34(10) . . ? N8 Ag1 Ag2 88.05(10) . . ? N4 Ag2 N6 168.09(15) . . ? N4 Ag2 O1 86.72(19) . . ? N6 Ag2 O1 105.18(19) . . ? N4 Ag2 Ag1 90.94(11) . . ? N6 Ag2 Ag1 93.53(11) . . ? O1 Ag2 Ag1 65.7(3) . . ? C2 C1 C5 108.2(4) . . ? C2 C1 C11 127.9(4) . . ? C5 C1 C11 123.9(5) . . ? C2 C1 Fe1 69.3(3) . . ? C5 C1 Fe1 69.6(3) . . ? C11 C1 Fe1 125.1(3) . . ? C3 C2 C1 107.8(5) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 Fe1 69.9(3) . . ? C2 C3 C4 109.1(5) . . ? C2 C3 Fe1 69.8(3) . . ? C4 C3 Fe1 69.8(3) . . ? C3 C4 C5 107.9(5) . . ? C3 C4 Fe1 69.6(3) . . ? C5 C4 Fe1 69.9(3) . . ? C4 C5 C1 107.0(5) . . ? C4 C5 Fe1 69.3(3) . . ? C1 C5 Fe1 69.2(3) . . ? C7 C6 C10 108.0(4) . . ? C7 C6 C15 128.1(4) . . ? C10 C6 C15 123.9(4) . . ? C7 C6 Fe1 69.1(3) . . ? C10 C6 Fe1 69.3(3) . . ? C15 C6 Fe1 125.9(3) . . ? C6 C7 C8 108.4(4) . . ? C6 C7 Fe1 70.3(2) . . ? C8 C7 Fe1 70.0(3) . . ? C9 C8 C7 107.0(4) . . ? C9 C8 Fe1 69.7(3) . . ? C7 C8 Fe1 68.9(3) . . ? C10 C9 C8 109.4(4) . . ? C10 C9 Fe1 69.9(3) . . ? C8 C9 Fe1 69.5(3) . . ? C9 C10 C6 107.1(4) . . ? C9 C10 Fe1 69.9(3) . . ? C6 C10 Fe1 69.3(3) . . ? N1 C11 C14 120.7(4) . . ? N1 C11 C1 117.9(4) . . ? C14 C11 C1 121.4(4) . . ? N1 C12 C13 122.5(4) . . ? N2 C13 C12 121.0(4) . . ? N2 C14 C11 122.1(4) . . ? N3 C15 C18 120.5(4) . . ? N3 C15 C6 117.7(4) . . ? C18 C15 C6 121.8(4) . . ? N3 C16 C17 121.9(4) . . ? N4 C17 C16 121.6(4) . . ? N4 C18 C15 121.7(4) . . ? C20 C19 C23 107.9(4) . . ? C20 C19 C29 126.9(4) . . ? C23 C19 C29 125.1(4) . . ? C20 C19 Fe2 69.5(3) . . ? C23 C19 Fe2 69.7(3) . . ? C29 C19 Fe2 125.5(3) . . ? C19 C20 C21 107.9(4) . . ? C19 C20 Fe2 69.7(3) . . ? C21 C20 Fe2 69.4(3) . . ? C22 C21 C20 107.7(4) . . ? C22 C21 Fe2 69.8(3) . . ? C20 C21 Fe2 69.7(3) . . ? C21 C22 C23 109.1(4) . . ? C21 C22 Fe2 69.8(3) . . ? C23 C22 Fe2 70.1(3) . . ? C22 C23 C19 107.3(4) . . ? C22 C23 Fe2 69.4(3) . . ? C19 C23 Fe2 69.4(2) . . ? C28 C24 C25 108.3(4) . . ? C28 C24 C33 125.5(4) . . ? C25 C24 C33 126.2(4) . . ? C28 C24 Fe2 69.7(3) . . ? C25 C24 Fe2 69.8(3) . . ? C33 C24 Fe2 125.1(3) . . ? C26 C25 C24 107.1(4) . . ? C26 C25 Fe2 69.4(3) . . ? C24 C25 Fe2 69.0(2) . . ? C25 C26 C27 108.2(4) . . ? C25 C26 Fe2 70.0(3) . . ? C27 C26 Fe2 69.6(3) . . ? C28 C27 C26 108.1(4) . . ? C28 C27 Fe2 69.5(3) . . ? C26 C27 Fe2 69.6(3) . . ? C24 C28 C27 108.3(4) . . ? C24 C28 Fe2 69.9(3) . . ? C27 C28 Fe2 70.0(3) . . ? N5 C29 C32 120.6(4) . . ? N5 C29 C19 118.5(4) . . ? C32 C29 C19 121.0(4) . . ? N5 C30 C31 123.6(4) . . ? N6 C31 C30 120.8(4) . . ? N6 C32 C29 121.6(4) . . ? N7 C33 C36 120.9(4) . . ? N7 C33 C24 117.2(4) . . ? C36 C33 C24 121.8(4) . . ? N7 C34 C35 124.3(4) . . ? N8 C35 C34 120.0(4) . . ? N8 C36 C33 121.8(4) . . ? C2 Fe1 C7 107.2(2) . . ? C2 Fe1 C3 40.4(2) . . ? C7 Fe1 C3 122.0(2) . . ? C2 Fe1 C4 68.6(2) . . ? C7 Fe1 C4 157.4(2) . . ? C3 Fe1 C4 40.6(3) . . ? C2 Fe1 C1 40.8(2) . . ? C7 Fe1 C1 123.60(19) . . ? C3 Fe1 C1 68.1(2) . . ? C4 Fe1 C1 68.7(2) . . ? C2 Fe1 C5 69.1(2) . . ? C7 Fe1 C5 160.35(18) . . ? C3 Fe1 C5 68.5(2) . . ? C4 Fe1 C5 40.9(2) . . ? C1 Fe1 C5 41.13(19) . . ? C2 Fe1 C8 119.6(2) . . ? C7 Fe1 C8 41.13(19) . . ? C3 Fe1 C8 104.1(2) . . ? C4 Fe1 C8 120.1(2) . . ? C1 Fe1 C8 157.3(2) . . ? C5 Fe1 C8 157.8(2) . . ? C2 Fe1 C10 163.66(18) . . ? C7 Fe1 C10 69.21(19) . . ? C3 Fe1 C10 155.2(2) . . ? C4 Fe1 C10 120.9(2) . . ? C1 Fe1 C10 127.0(2) . . ? C5 Fe1 C10 108.6(2) . . ? C8 Fe1 C10 68.9(2) . . ? C2 Fe1 C6 125.72(18) . . ? C7 Fe1 C6 40.63(18) . . ? C3 Fe1 C6 160.0(2) . . ? C4 Fe1 C6 159.1(2) . . ? C1 Fe1 C6 111.02(18) . . ? C5 Fe1 C6 124.9(2) . . ? C8 Fe1 C6 68.72(19) . . ? C10 Fe1 C6 41.41(17) . . ? C2 Fe1 C9 154.8(2) . . ? C7 Fe1 C9 68.6(2) . . ? C3 Fe1 C9 119.2(2) . . ? C4 Fe1 C9 105.2(2) . . ? C1 Fe1 C9 161.7(2) . . ? C5 Fe1 C9 123.1(2) . . ? C8 Fe1 C9 40.8(2) . . ? C10 Fe1 C9 40.2(2) . . ? C6 Fe1 C9 68.24(18) . . ? C28 Fe2 C24 40.40(17) . . ? C28 Fe2 C21 155.3(2) . . ? C24 Fe2 C21 161.3(2) . . ? C28 Fe2 C22 121.0(2) . . ? C24 Fe2 C22 158.1(2) . . ? C21 Fe2 C22 40.4(2) . . ? C28 Fe2 C27 40.55(19) . . ? C24 Fe2 C27 68.11(19) . . ? C21 Fe2 C27 119.2(2) . . ? C22 Fe2 C27 104.9(2) . . ? C28 Fe2 C26 68.5(2) . . ? C24 Fe2 C26 68.45(18) . . ? C21 Fe2 C26 105.0(2) . . ? C22 Fe2 C26 120.69(18) . . ? C27 Fe2 C26 40.8(2) . . ? C28 Fe2 C20 162.49(18) . . ? C24 Fe2 C20 126.37(19) . . ? C21 Fe2 C20 40.9(2) . . ? C22 Fe2 C20 68.2(2) . . ? C27 Fe2 C20 156.1(2) . . ? C26 Fe2 C20 121.6(2) . . ? C28 Fe2 C19 125.48(18) . . ? C24 Fe2 C19 110.79(17) . . ? C21 Fe2 C19 68.67(19) . . ? C22 Fe2 C19 68.28(19) . . ? C27 Fe2 C19 159.94(19) . . ? C26 Fe2 C19 159.00(19) . . ? C20 Fe2 C19 40.74(17) . . ? C28 Fe2 C25 68.7(2) . . ? C24 Fe2 C25 41.13(18) . . ? C21 Fe2 C25 122.7(2) . . ? C22 Fe2 C25 157.7(2) . . ? C27 Fe2 C25 68.4(2) . . ? C26 Fe2 C25 40.5(2) . . ? C20 Fe2 C25 108.7(2) . . ? C19 Fe2 C25 124.88(19) . . ? C28 Fe2 C23 107.79(19) . . ? C24 Fe2 C23 124.18(18) . . ? C21 Fe2 C23 68.5(2) . . ? C22 Fe2 C23 40.52(18) . . ? C27 Fe2 C23 121.9(2) . . ? C26 Fe2 C23 157.29(19) . . ? C20 Fe2 C23 68.7(2) . . ? C19 Fe2 C23 40.89(17) . . ? C25 Fe2 C23 160.97(18) . . ? C12 N1 C11 116.3(4) . . ? C13 N2 C14 117.4(4) . . ? C13 N2 Ag1 122.6(3) . . ? C14 N2 Ag1 120.0(3) . . ? C16 N3 C15 117.3(4) . . ? C17 N4 C18 117.0(4) . . ? C17 N4 Ag2 120.7(3) . . ? C18 N4 Ag2 122.3(3) . . ? C30 N5 C29 116.3(4) . . ? C31 N6 C32 117.2(4) . . ? C31 N6 Ag2 122.0(3) . . ? C32 N6 Ag2 120.7(3) . . ? C34 N7 C33 115.7(4) . . ? C36 N8 C35 117.2(4) . . ? C36 N8 Ag1 123.1(3) . . ? C35 N8 Ag1 119.5(3) . . ? O1 N9 O3 131.9(9) . . ? O1 N9 O2 113.6(9) . . ? O3 N9 O2 114.1(6) . . ? O6 N10 O5 124.0(6) . . ? O6 N10 O4 119.6(6) . . ? O5 N10 O4 116.3(5) . . ? N9 O1 Ag2 125.4(5) . . ? C41 C42 C37 120.0 . . ? C42 C41 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C38 C37 120.0 . . ? C43 C37 C38 128.0(14) . . ? C43 C37 C42 112.0(14) . . ? C38 C37 C42 120.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.867 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.088 #-----------END data_7 _database_code_depnum_ccdc_archive 'CCDC 262875' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Ag2 F12 Fe2 N8 P2' _chemical_formula_weight 1190.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.176(4) _cell_length_b 14.414(4) _cell_length_c 20.314(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.132(5) _cell_angle_gamma 90.00 _cell_volume 4042.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.833 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6093 _exptl_absorpt_correction_T_max 0.9303 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; SADABS; Sheldrick, 1996 ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25749 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.1831 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.46 _reflns_number_total 10100 _reflns_number_gt 4096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10100 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2028 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2209 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.60304(7) 0.12160(5) 0.21027(5) 0.0560(3) Uani 1 1 d . . . Ag2 Ag 0.37941(7) 0.12041(6) 0.24664(5) 0.0589(3) Uani 1 1 d . . . C1 C 0.7393(6) -0.1993(6) 0.3587(5) 0.031(2) Uani 1 1 d . . . C2 C 0.7729(7) -0.2509(6) 0.4180(5) 0.040(2) Uani 1 1 d . . . H2 H 0.8001 -0.2263 0.4604 0.048 Uiso 1 1 calc R . . C3 C 0.7587(7) -0.3471(7) 0.4029(6) 0.046(3) Uani 1 1 d . . . H3 H 0.7750 -0.3953 0.4338 0.056 Uiso 1 1 calc R . . C4 C 0.7154(7) -0.3578(6) 0.3325(6) 0.048(3) Uani 1 1 d . . . H4 H 0.6986 -0.4130 0.3090 0.058 Uiso 1 1 calc R . . C5 C 0.7034(7) -0.2652(6) 0.3058(5) 0.042(2) Uani 1 1 d . . . H5 H 0.6764 -0.2502 0.2610 0.050 Uiso 1 1 calc R . . C6 C 0.5186(7) -0.1951(6) 0.3934(5) 0.034(2) Uani 1 1 d . . . C7 C 0.5562(7) -0.2488(6) 0.4524(5) 0.042(2) Uani 1 1 d . . . H7 H 0.5850 -0.2262 0.4951 0.050 Uiso 1 1 calc R . . C8 C 0.5417(8) -0.3423(7) 0.4339(6) 0.053(3) Uani 1 1 d . . . H8 H 0.5578 -0.3920 0.4635 0.064 Uiso 1 1 calc R . . C9 C 0.4991(8) -0.3506(7) 0.3639(7) 0.055(3) Uani 1 1 d . . . H9 H 0.4841 -0.4053 0.3395 0.066 Uiso 1 1 calc R . . C10 C 0.4840(7) -0.2585(6) 0.3384(6) 0.046(3) Uani 1 1 d . . . H10 H 0.4565 -0.2421 0.2939 0.055 Uiso 1 1 calc R . . C11 C 0.7383(7) -0.0990(6) 0.3534(5) 0.031(2) Uani 1 1 d . . . C12 C 0.6890(7) -0.0522(6) 0.2979(5) 0.036(2) Uani 1 1 d . . . H12 H 0.6548 -0.0864 0.2614 0.043 Uiso 1 1 calc R . . C13 C 0.7372(8) 0.0868(6) 0.3461(6) 0.047(3) Uani 1 1 d . . . H13 H 0.7390 0.1513 0.3446 0.057 Uiso 1 1 calc R . . C14 C 0.7851(7) 0.0426(6) 0.4014(6) 0.047(3) Uani 1 1 d . . . H14 H 0.8179 0.0780 0.4378 0.057 Uiso 1 1 calc R . . C15 C 0.5170(6) -0.0925(6) 0.3905(5) 0.033(2) Uani 1 1 d . . . C16 C 0.4665(7) -0.0460(6) 0.3342(5) 0.034(2) Uani 1 1 d . . . H16 H 0.4328 -0.0803 0.2976 0.041 Uiso 1 1 calc R . . C17 C 0.5074(7) 0.0914(6) 0.3844(5) 0.042(3) Uani 1 1 d . . . H17 H 0.5039 0.1559 0.3846 0.050 Uiso 1 1 calc R . . C18 C 0.5590(7) 0.0459(6) 0.4418(5) 0.046(3) Uani 1 1 d . . . H18 H 0.5906 0.0811 0.4787 0.055 Uiso 1 1 calc R . . C19 C 0.2624(7) 0.4704(6) 0.1512(5) 0.036(2) Uani 1 1 d . . . C20 C 0.2318(7) 0.5410(6) 0.1013(5) 0.036(2) Uani 1 1 d . . . H20 H 0.2008 0.5317 0.0563 0.043 Uiso 1 1 calc R . . C21 C 0.2577(8) 0.6286(7) 0.1336(6) 0.051(3) Uani 1 1 d . . . H21 H 0.2486 0.6864 0.1127 0.061 Uiso 1 1 calc R . . C22 C 0.3000(8) 0.6122(7) 0.2035(7) 0.057(3) Uani 1 1 d . . . H22 H 0.3204 0.6578 0.2360 0.069 Uiso 1 1 calc R . . C23 C 0.3059(7) 0.5164(6) 0.2152(5) 0.038(2) Uani 1 1 d . . . H23 H 0.3325 0.4874 0.2561 0.046 Uiso 1 1 calc R . . C24 C 0.4836(7) 0.4714(6) 0.1141(5) 0.035(2) Uani 1 1 d . . . C25 C 0.4511(6) 0.5434(6) 0.0660(5) 0.031(2) Uani 1 1 d . . . H25 H 0.4240 0.5355 0.0202 0.037 Uiso 1 1 calc R . . C26 C 0.4677(7) 0.6291(6) 0.1009(6) 0.042(3) Uani 1 1 d . . . H26 H 0.4513 0.6874 0.0821 0.050 Uiso 1 1 calc R . . C27 C 0.5122(8) 0.6118(6) 0.1677(6) 0.045(3) Uani 1 1 d . . . H27 H 0.5319 0.6571 0.2005 0.054 Uiso 1 1 calc R . . C28 C 0.5234(7) 0.5174(6) 0.1788(5) 0.036(2) Uani 1 1 d . . . H28 H 0.5510 0.4886 0.2196 0.043 Uiso 1 1 calc R . . C29 C 0.2560(6) 0.3706(6) 0.1383(4) 0.028(2) Uani 1 1 d . . . C30 C 0.3025(7) 0.3047(6) 0.1841(5) 0.039(2) Uani 1 1 d . . . H30 H 0.3384 0.3255 0.2256 0.047 Uiso 1 1 calc R . . C31 C 0.2477(7) 0.1859(6) 0.1135(6) 0.044(3) Uani 1 1 d . . . H31 H 0.2435 0.1227 0.1039 0.052 Uiso 1 1 calc R . . C32 C 0.1991(8) 0.2499(7) 0.0646(6) 0.049(3) Uani 1 1 d . . . H32 H 0.1642 0.2288 0.0229 0.059 Uiso 1 1 calc R . . C33 C 0.4801(6) 0.3722(6) 0.1007(5) 0.031(2) Uani 1 1 d . . . C34 C 0.5257(7) 0.3068(6) 0.1490(5) 0.038(2) Uani 1 1 d . . . H34 H 0.5595 0.3274 0.1911 0.045 Uiso 1 1 calc R . . C35 C 0.4757(7) 0.1877(6) 0.0741(5) 0.042(3) Uani 1 1 d . . . H35 H 0.4736 0.1247 0.0638 0.051 Uiso 1 1 calc R . . C36 C 0.4315(8) 0.2512(7) 0.0259(5) 0.051(3) Uani 1 1 d . . . H36 H 0.4003 0.2295 -0.0165 0.062 Uiso 1 1 calc R . . F1 F 0.6954(12) 0.2935(8) 0.3989(6) 0.201(7) Uani 1 1 d . . . F2 F 0.6719(9) 0.3974(9) 0.3122(6) 0.169(5) Uani 1 1 d . . . F3 F 0.6502(11) 0.4372(6) 0.4122(6) 0.171(5) Uani 1 1 d . . . F4 F 0.5546(10) 0.3181(8) 0.4122(5) 0.160(5) Uani 1 1 d . . . F5 F 0.5836(12) 0.2756(6) 0.3108(5) 0.186(6) Uani 1 1 d . . . F6 F 0.5271(11) 0.4155(8) 0.3237(6) 0.185(6) Uani 1 1 d . . . F7 F 0.4534(13) 0.8720(10) 0.0801(8) 0.222(8) Uani 1 1 d . . . F8 F 0.4634(10) 0.9782(7) 0.1678(7) 0.184(5) Uani 1 1 d . . . F9 F 0.4185(13) 0.8366(7) 0.1778(5) 0.228(8) Uani 1 1 d . . . F10 F 0.3082(12) 0.8421(7) 0.0832(6) 0.195(7) Uani 1 1 d . . . F11 F 0.3591(12) 0.9851(6) 0.0709(6) 0.205(7) Uani 1 1 d . . . F12 F 0.3208(10) 0.9483(11) 0.1680(8) 0.214(7) Uani 1 1 d . . . Fe1 Fe 0.62859(10) -0.27850(8) 0.37909(7) 0.0348(4) Uani 1 1 d . . . Fe2 Fe 0.37983(9) 0.55076(8) 0.14350(7) 0.0320(3) Uani 1 1 d . . . N1 N 0.7884(6) -0.0536(5) 0.4075(4) 0.041(2) Uani 1 1 d . . . N2 N 0.6872(6) 0.0405(5) 0.2933(4) 0.041(2) Uani 1 1 d . . . N3 N 0.5649(6) -0.0479(5) 0.4460(4) 0.040(2) Uani 1 1 d . . . N4 N 0.4641(6) 0.0467(5) 0.3305(4) 0.043(2) Uani 1 1 d . . . N5 N 0.2034(6) 0.3418(5) 0.0784(4) 0.0374(19) Uani 1 1 d . . . N6 N 0.2992(6) 0.2147(5) 0.1729(4) 0.039(2) Uani 1 1 d . . . N7 N 0.4316(6) 0.3441(5) 0.0378(4) 0.039(2) Uani 1 1 d . . . N8 N 0.5219(6) 0.2169(5) 0.1360(4) 0.040(2) Uani 1 1 d . . . P1 P 0.6186(5) 0.3566(2) 0.3632(2) 0.1083(19) Uani 1 1 d . . . P2 P 0.3907(4) 0.9099(2) 0.1241(2) 0.0953(15) 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 0.0650(6) 0.0337(4) 0.0655(6) 0.0206(4) 0.0070(5) 0.0109(4) Ag2 0.0658(6) 0.0370(4) 0.0708(7) 0.0242(4) 0.0092(5) 0.0124(4) C1 0.036(6) 0.018(4) 0.038(6) -0.002(4) 0.007(4) 0.007(4) C2 0.044(6) 0.032(5) 0.043(6) 0.009(5) 0.004(5) 0.009(4) C3 0.037(6) 0.035(5) 0.067(8) 0.008(5) 0.012(6) 0.004(5) C4 0.042(7) 0.018(5) 0.089(10) -0.003(5) 0.023(6) 0.004(4) C5 0.039(6) 0.036(5) 0.051(7) -0.002(5) 0.010(5) -0.005(4) C6 0.045(6) 0.021(4) 0.038(6) 0.002(4) 0.014(5) -0.001(4) C7 0.042(7) 0.032(5) 0.051(7) 0.005(5) 0.011(5) 0.003(4) C8 0.055(7) 0.034(5) 0.077(9) 0.028(6) 0.029(7) 0.007(5) C9 0.064(8) 0.026(5) 0.078(9) -0.004(5) 0.025(7) 0.000(5) C10 0.047(7) 0.032(5) 0.060(8) -0.009(5) 0.016(5) -0.008(5) C11 0.041(6) 0.020(5) 0.034(6) 0.001(4) 0.014(4) -0.005(4) C12 0.039(6) 0.026(5) 0.044(6) 0.002(4) 0.010(5) -0.008(4) C13 0.063(8) 0.017(4) 0.065(8) -0.001(5) 0.023(6) -0.002(5) C14 0.053(7) 0.025(5) 0.060(8) -0.006(5) 0.007(6) -0.017(5) C15 0.025(5) 0.025(5) 0.049(7) -0.001(4) 0.012(5) -0.001(4) C16 0.046(6) 0.021(4) 0.034(6) -0.003(4) 0.009(4) -0.004(4) C17 0.046(7) 0.025(5) 0.055(7) 0.003(5) 0.014(5) 0.003(4) C18 0.059(7) 0.029(5) 0.050(7) -0.014(5) 0.011(5) -0.004(5) C19 0.032(6) 0.033(5) 0.043(6) -0.004(4) 0.006(4) 0.005(4) C20 0.039(6) 0.019(4) 0.048(6) -0.007(4) 0.006(5) -0.002(4) C21 0.057(7) 0.031(6) 0.067(9) -0.005(5) 0.019(6) 0.006(5) C22 0.053(7) 0.040(6) 0.092(10) -0.023(6) 0.042(7) -0.015(5) C23 0.044(6) 0.032(5) 0.037(6) -0.001(4) 0.006(5) 0.007(4) C24 0.036(6) 0.026(5) 0.043(6) 0.008(4) 0.012(5) -0.004(4) C25 0.033(5) 0.029(5) 0.031(5) 0.005(4) 0.011(4) 0.001(4) C26 0.045(6) 0.022(5) 0.062(8) 0.001(5) 0.019(5) -0.008(4) C27 0.064(7) 0.024(5) 0.051(7) -0.009(5) 0.021(6) -0.004(5) C28 0.037(6) 0.034(5) 0.036(6) 0.001(4) 0.006(4) 0.003(4) C29 0.032(5) 0.023(4) 0.030(5) 0.003(4) 0.007(4) -0.001(4) C30 0.048(7) 0.029(5) 0.041(6) 0.014(4) 0.010(5) -0.004(4) C31 0.045(7) 0.022(5) 0.064(8) -0.010(5) 0.013(6) 0.004(4) C32 0.069(8) 0.034(6) 0.047(7) -0.007(5) 0.019(6) -0.004(5) C33 0.036(6) 0.023(4) 0.037(6) 0.006(4) 0.015(4) 0.002(4) C34 0.036(6) 0.038(5) 0.039(6) 0.009(5) 0.007(5) 0.012(4) C35 0.052(7) 0.024(5) 0.052(7) -0.004(5) 0.015(5) 0.008(4) C36 0.081(9) 0.036(6) 0.035(7) 0.007(5) 0.010(6) 0.002(5) F1 0.318(18) 0.153(10) 0.108(9) -0.008(8) -0.004(10) 0.136(12) F2 0.159(11) 0.218(13) 0.141(10) 0.046(9) 0.058(8) -0.017(9) F3 0.313(16) 0.065(6) 0.137(10) -0.053(6) 0.059(10) -0.049(8) F4 0.262(15) 0.126(9) 0.092(8) -0.005(7) 0.042(8) -0.053(9) F5 0.40(2) 0.081(7) 0.069(7) -0.010(5) 0.027(9) -0.005(9) F6 0.292(17) 0.148(10) 0.118(10) 0.064(8) 0.054(10) 0.110(11) F7 0.31(2) 0.191(14) 0.201(15) -0.014(11) 0.140(15) 0.092(13) F8 0.223(14) 0.106(8) 0.193(13) -0.036(8) -0.014(10) -0.061(9) F9 0.50(3) 0.084(7) 0.058(7) 0.009(6) -0.032(10) 0.032(11) F10 0.35(2) 0.097(8) 0.118(9) -0.015(7) 0.006(11) -0.087(10) F11 0.42(2) 0.047(5) 0.112(9) 0.007(5) -0.015(11) -0.003(8) F12 0.190(14) 0.244(17) 0.229(16) -0.083(14) 0.090(12) -0.034(12) Fe1 0.0414(9) 0.0171(6) 0.0461(9) 0.0048(6) 0.0101(7) 0.0030(6) Fe2 0.0364(8) 0.0197(6) 0.0393(8) -0.0028(6) 0.0074(6) -0.0011(6) N1 0.054(6) 0.023(4) 0.042(5) 0.003(4) 0.005(4) -0.003(4) N2 0.042(5) 0.035(4) 0.047(6) 0.006(4) 0.009(4) -0.001(4) N3 0.046(5) 0.028(4) 0.043(5) -0.009(4) 0.004(4) 0.008(4) N4 0.044(5) 0.028(4) 0.057(6) 0.001(4) 0.013(4) 0.006(4) N5 0.042(5) 0.027(4) 0.040(5) -0.001(4) 0.002(4) 0.000(4) N6 0.040(5) 0.028(4) 0.050(6) 0.015(4) 0.013(4) 0.004(4) N7 0.056(6) 0.028(4) 0.031(5) 0.001(4) 0.005(4) 0.000(4) N8 0.051(6) 0.023(4) 0.049(6) 0.009(4) 0.016(4) 0.011(4) P1 0.246(6) 0.0260(16) 0.053(3) 0.0061(16) 0.034(3) 0.011(2) P2 0.196(5) 0.0300(16) 0.058(3) -0.0069(17) 0.026(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N8 2.168(8) . ? Ag1 N2 2.173(8) . ? Ag2 N4 2.131(8) . ? Ag2 N6 2.148(8) . ? C1 C2 1.405(12) . ? C1 C5 1.438(13) . ? C1 C11 1.449(11) . ? C1 Fe1 2.058(9) . ? C2 C3 1.424(13) . ? C2 Fe1 2.058(10) . ? C3 C4 1.430(15) . ? C3 Fe1 2.051(10) . ? C4 C5 1.436(13) . ? C4 Fe1 2.060(10) . ? C5 Fe1 2.023(10) . ? C6 C7 1.425(13) . ? C6 C10 1.441(13) . ? C6 C15 1.479(12) . ? C6 Fe1 2.041(9) . ? C7 C8 1.401(13) . ? C7 Fe1 2.036(10) . ? C8 C9 1.418(15) . ? C8 Fe1 2.056(10) . ? C9 C10 1.424(13) . ? C9 Fe1 2.071(11) . ? C10 Fe1 2.049(11) . ? C11 N1 1.336(11) . ? C11 C12 1.362(12) . ? C12 N2 1.339(11) . ? C13 N2 1.324(13) . ? C13 C14 1.335(14) . ? C14 N1 1.393(11) . ? C15 N3 1.340(12) . ? C15 C16 1.377(13) . ? C16 N4 1.339(11) . ? C17 N4 1.298(12) . ? C17 C18 1.393(14) . ? C18 N3 1.356(11) . ? C19 C20 1.433(13) . ? C19 C29 1.461(12) . ? C19 C23 1.466(13) . ? C19 Fe2 2.064(9) . ? C20 C21 1.432(13) . ? C20 Fe2 2.084(9) . ? C21 C22 1.429(16) . ? C21 Fe2 2.035(10) . ? C22 C23 1.401(13) . ? C22 Fe2 2.044(10) . ? C23 Fe2 2.040(9) . ? C24 C25 1.428(12) . ? C24 C33 1.454(12) . ? C24 C28 1.467(13) . ? C24 Fe2 2.056(9) . ? C25 C26 1.418(12) . ? C25 Fe2 2.057(8) . ? C26 C27 1.383(14) . ? C26 Fe2 2.016(9) . ? C27 C28 1.381(12) . ? C27 Fe2 2.030(10) . ? C28 Fe2 2.056(9) . ? C29 N5 1.341(11) . ? C29 C30 1.388(12) . ? C30 N6 1.315(11) . ? C31 N6 1.326(12) . ? C31 C32 1.415(14) . ? C32 N5 1.351(11) . ? C33 N7 1.367(12) . ? C33 C34 1.407(12) . ? C34 N8 1.321(11) . ? C35 N8 1.346(12) . ? C35 C36 1.382(13) . ? C36 N7 1.361(12) . ? F1 P1 1.476(11) . ? F2 P1 1.531(11) . ? F3 P1 1.529(9) . ? F4 P1 1.591(12) . ? F5 P1 1.583(10) . ? F6 P1 1.606(12) . ? F7 P2 1.500(12) . ? F8 P2 1.550(11) . ? F9 P2 1.505(10) . ? F10 P2 1.604(12) . ? F11 P2 1.524(10) . ? F12 P2 1.576(13) . ? 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 N8 Ag1 N2 172.9(3) . . ? N4 Ag2 N6 170.4(3) . . ? C2 C1 C5 106.5(8) . . ? C2 C1 C11 126.0(9) . . ? C5 C1 C11 127.5(9) . . ? C2 C1 Fe1 70.0(5) . . ? C5 C1 Fe1 68.1(5) . . ? C11 C1 Fe1 125.0(6) . . ? C1 C2 C3 109.0(9) . . ? C1 C2 Fe1 70.0(6) . . ? C3 C2 Fe1 69.5(6) . . ? C2 C3 C4 109.2(9) . . ? C2 C3 Fe1 70.0(6) . . ? C4 C3 Fe1 70.0(6) . . ? C3 C4 C5 105.3(9) . . ? C3 C4 Fe1 69.3(6) . . ? C5 C4 Fe1 68.0(5) . . ? C4 C5 C1 109.9(9) . . ? C4 C5 Fe1 70.8(6) . . ? C1 C5 Fe1 70.7(5) . . ? C7 C6 C10 107.7(8) . . ? C7 C6 C15 125.1(9) . . ? C10 C6 C15 127.2(9) . . ? C7 C6 Fe1 69.3(5) . . ? C10 C6 Fe1 69.7(5) . . ? C15 C6 Fe1 126.0(6) . . ? C8 C7 C6 107.0(10) . . ? C8 C7 Fe1 70.7(6) . . ? C6 C7 Fe1 69.7(5) . . ? C7 C8 C9 110.7(9) . . ? C7 C8 Fe1 69.2(6) . . ? C9 C8 Fe1 70.5(6) . . ? C8 C9 C10 106.3(9) . . ? C8 C9 Fe1 69.3(6) . . ? C10 C9 Fe1 69.0(6) . . ? C9 C10 C6 108.2(10) . . ? C9 C10 Fe1 70.6(6) . . ? C6 C10 Fe1 69.1(6) . . ? N1 C11 C12 121.0(8) . . ? N1 C11 C1 115.6(8) . . ? C12 C11 C1 123.3(9) . . ? N2 C12 C11 123.4(9) . . ? N2 C13 C14 121.2(9) . . ? C13 C14 N1 123.4(10) . . ? N3 C15 C16 122.2(8) . . ? N3 C15 C6 116.5(9) . . ? C16 C15 C6 121.3(9) . . ? N4 C16 C15 122.3(9) . . ? N4 C17 C18 122.0(9) . . ? N3 C18 C17 122.3(9) . . ? C20 C19 C29 125.2(9) . . ? C20 C19 C23 107.7(8) . . ? C29 C19 C23 127.0(9) . . ? C20 C19 Fe2 70.5(5) . . ? C29 C19 Fe2 123.9(6) . . ? C23 C19 Fe2 68.2(5) . . ? C21 C20 C19 107.3(9) . . ? C21 C20 Fe2 67.8(6) . . ? C19 C20 Fe2 69.0(5) . . ? C22 C21 C20 108.4(9) . . ? C22 C21 Fe2 69.8(6) . . ? C20 C21 Fe2 71.5(5) . . ? C23 C22 C21 109.1(10) . . ? C23 C22 Fe2 69.8(6) . . ? C21 C22 Fe2 69.2(6) . . ? C22 C23 C19 107.4(10) . . ? C22 C23 Fe2 70.1(6) . . ? C19 C23 Fe2 69.9(5) . . ? C25 C24 C33 126.5(9) . . ? C25 C24 C28 106.5(8) . . ? C33 C24 C28 127.0(8) . . ? C25 C24 Fe2 69.7(5) . . ? C33 C24 Fe2 127.2(6) . . ? C28 C24 Fe2 69.1(5) . . ? C26 C25 C24 107.4(8) . . ? C26 C25 Fe2 68.1(5) . . ? C24 C25 Fe2 69.7(5) . . ? C27 C26 C25 108.7(8) . . ? C27 C26 Fe2 70.5(6) . . ? C25 C26 Fe2 71.2(5) . . ? C26 C27 C28 110.4(9) . . ? C26 C27 Fe2 69.5(6) . . ? C28 C27 Fe2 71.3(6) . . ? C27 C28 C24 106.9(9) . . ? C27 C28 Fe2 69.2(6) . . ? C24 C28 Fe2 69.1(5) . . ? N5 C29 C30 118.6(8) . . ? N5 C29 C19 117.8(8) . . ? C30 C29 C19 123.6(9) . . ? N6 C30 C29 124.5(10) . . ? N6 C31 C32 120.9(9) . . ? N5 C32 C31 120.1(10) . . ? N7 C33 C34 120.4(8) . . ? N7 C33 C24 117.0(8) . . ? C34 C33 C24 122.5(9) . . ? N8 C34 C33 121.8(10) . . ? N8 C35 C36 120.0(9) . . ? N7 C36 C35 123.0(10) . . ? C5 Fe1 C7 162.4(4) . . ? C5 Fe1 C6 126.4(4) . . ? C7 Fe1 C6 40.9(4) . . ? C5 Fe1 C3 68.0(4) . . ? C7 Fe1 C3 120.3(4) . . ? C6 Fe1 C3 157.7(4) . . ? C5 Fe1 C10 109.5(4) . . ? C7 Fe1 C10 69.0(4) . . ? C6 Fe1 C10 41.2(4) . . ? C3 Fe1 C10 157.9(4) . . ? C5 Fe1 C8 156.9(4) . . ? C7 Fe1 C8 40.0(4) . . ? C6 Fe1 C8 67.4(4) . . ? C3 Fe1 C8 105.9(4) . . ? C10 Fe1 C8 67.3(4) . . ? C5 Fe1 C2 67.9(4) . . ? C7 Fe1 C2 107.5(4) . . ? C6 Fe1 C2 123.8(4) . . ? C3 Fe1 C2 40.6(4) . . ? C10 Fe1 C2 160.7(4) . . ? C8 Fe1 C2 123.0(4) . . ? C5 Fe1 C4 41.2(4) . . ? C7 Fe1 C4 154.8(4) . . ? C6 Fe1 C4 161.3(4) . . ? C3 Fe1 C4 40.7(4) . . ? C10 Fe1 C4 122.7(4) . . ? C8 Fe1 C4 119.6(4) . . ? C2 Fe1 C4 68.8(4) . . ? C5 Fe1 C1 41.2(3) . . ? C7 Fe1 C1 124.4(4) . . ? C6 Fe1 C1 110.1(3) . . ? C3 Fe1 C1 68.2(4) . . ? C10 Fe1 C1 125.4(4) . . ? C8 Fe1 C1 159.3(5) . . ? C2 Fe1 C1 39.9(3) . . ? C4 Fe1 C1 69.7(3) . . ? C5 Fe1 C9 122.2(5) . . ? C7 Fe1 C9 68.7(4) . . ? C6 Fe1 C9 68.7(4) . . ? C3 Fe1 C9 120.8(4) . . ? C10 Fe1 C9 40.4(4) . . ? C8 Fe1 C9 40.2(4) . . ? C2 Fe1 C9 157.6(4) . . ? C4 Fe1 C9 104.8(4) . . ? C1 Fe1 C9 159.9(4) . . ? C26 Fe2 C27 40.0(4) . . ? C26 Fe2 C21 104.1(4) . . ? C27 Fe2 C21 120.3(4) . . ? C26 Fe2 C23 155.5(4) . . ? C27 Fe2 C23 122.0(4) . . ? C21 Fe2 C23 68.9(4) . . ? C26 Fe2 C22 119.5(4) . . ? C27 Fe2 C22 106.0(4) . . ? C21 Fe2 C22 41.0(4) . . ? C23 Fe2 C22 40.1(4) . . ? C26 Fe2 C25 40.7(3) . . ? C27 Fe2 C25 67.6(4) . . ? C21 Fe2 C25 120.5(4) . . ? C23 Fe2 C25 162.8(3) . . ? C22 Fe2 C25 155.9(4) . . ? C26 Fe2 C28 67.8(4) . . ? C27 Fe2 C28 39.5(4) . . ? C21 Fe2 C28 156.4(4) . . ? C23 Fe2 C28 108.8(4) . . ? C22 Fe2 C28 122.1(5) . . ? C25 Fe2 C28 68.6(4) . . ? C26 Fe2 C24 68.6(3) . . ? C27 Fe2 C24 68.1(4) . . ? C21 Fe2 C24 158.0(4) . . ? C23 Fe2 C24 126.2(4) . . ? C22 Fe2 C24 160.7(5) . . ? C25 Fe2 C24 40.6(3) . . ? C28 Fe2 C24 41.8(4) . . ? C26 Fe2 C19 159.2(4) . . ? C27 Fe2 C19 160.5(4) . . ? C21 Fe2 C19 68.5(4) . . ? C23 Fe2 C19 41.9(4) . . ? C22 Fe2 C19 68.5(4) . . ? C25 Fe2 C19 125.0(4) . . ? C28 Fe2 C19 126.5(4) . . ? C24 Fe2 C19 110.6(3) . . ? C26 Fe2 C20 121.6(4) . . ? C27 Fe2 C20 156.7(4) . . ? C21 Fe2 C20 40.7(4) . . ? C23 Fe2 C20 69.2(4) . . ? C22 Fe2 C20 68.4(4) . . ? C25 Fe2 C20 107.8(4) . . ? C28 Fe2 C20 162.3(3) . . ? C24 Fe2 C20 124.3(4) . . ? C19 Fe2 C20 40.4(3) . . ? C11 N1 C14 114.4(8) . . ? C13 N2 C12 116.6(9) . . ? C13 N2 Ag1 117.1(7) . . ? C12 N2 Ag1 126.1(7) . . ? C15 N3 C18 114.5(9) . . ? C17 N4 C16 116.6(9) . . ? C17 N4 Ag2 119.9(7) . . ? C16 N4 Ag2 123.1(7) . . ? C29 N5 C32 118.7(8) . . ? C30 N6 C31 117.2(8) . . ? C30 N6 Ag2 120.7(7) . . ? C31 N6 Ag2 122.0(6) . . ? C36 N7 C33 115.9(8) . . ? C34 N8 C35 118.9(8) . . ? C34 N8 Ag1 119.4(7) . . ? C35 N8 Ag1 121.3(6) . . ? F1 P1 F2 98.4(9) . . ? F1 P1 F3 94.3(8) . . ? F2 P1 F3 91.9(7) . . ? F1 P1 F5 87.6(7) . . ? F2 P1 F5 87.4(7) . . ? F3 P1 F5 178.0(8) . . ? F1 P1 F4 86.6(8) . . ? F2 P1 F4 174.8(8) . . ? F3 P1 F4 89.0(6) . . ? F5 P1 F4 91.5(7) . . ? F1 P1 F6 173.6(9) . . ? F2 P1 F6 85.7(7) . . ? F3 P1 F6 90.5(7) . . ? F5 P1 F6 87.6(7) . . ? F4 P1 F6 89.2(8) . . ? F7 P2 F9 94.8(9) . . ? F7 P2 F11 87.4(8) . . ? F9 P2 F11 177.7(10) . . ? F7 P2 F8 99.6(10) . . ? F9 P2 F8 90.0(7) . . ? F11 P2 F8 90.2(7) . . ? F7 P2 F12 177.5(10) . . ? F9 P2 F12 86.1(9) . . ? F11 P2 F12 91.7(9) . . ? F8 P2 F12 82.8(7) . . ? F7 P2 F10 86.0(8) . . ? F9 P2 F10 89.3(7) . . ? F11 P2 F10 90.2(7) . . ? F8 P2 F10 174.5(9) . . ? F12 P2 F10 91.7(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.563 _refine_diff_density_min -1.515 _refine_diff_density_rms 0.157 #-----------END