# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. J F Corrigan' _publ_contact_author_email 'jfcorrig@uwo.ca; corrigan@uwo.ca' _publ_contact_author_address ;Dept of Chemistry The University of Western Ontario London ON N6A 5B7 Canada ; _publ_section_title ; Ferrocenylmethylselenolate Complex of Ag(I): Preparation of the Polyferrocenyl Cluster [Ag8(SeCH2Fc)8(PPh3)4] from the New Silylated Reagent FcCH2SeSiMe3 ; loop_ _publ_author_name J.Corrigan D.Fenske # Attachment 'Corrigan-New-J-Chem-2011.cif' data_05138 _database_code_depnum_ccdc_archive 'CCDC 814944' #TrackingRef 'Corrigan-New-J-Chem-2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Fe2 Se2' _chemical_formula_weight 556.02 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 15.3520(10) _cell_length_b 5.7588(3) _cell_length_c 22.802(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.678(3) _cell_angle_gamma 90.00 _cell_volume 1997.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 13275 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 50.06 _exptl_crystal_description yellow _exptl_crystal_colour needle _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 5.099 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5798 _exptl_absorpt_correction_T_max 0.9049 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi scans + omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6318 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.17 _reflns_number_total 3535 _reflns_number_gt 2006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3535 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 0.42522(6) 0.54675(16) 0.17587(5) 0.0289(3) Uani 1 1 d . . . Fe2 Fe 0.20696(6) 0.24926(16) -0.10352(4) 0.0283(3) Uani 1 1 d . . . Se1 Se 0.10997(5) 0.59230(12) 0.10582(4) 0.0344(2) Uani 1 1 d . . . Se2 Se 0.09451(5) 0.20035(12) 0.08686(3) 0.0319(2) Uani 1 1 d . . . C1 C 0.2919(4) 0.5371(11) 0.1616(3) 0.0264(17) Uani 1 1 d . . . C2 C 0.3206(4) 0.6643(11) 0.2146(3) 0.0269(18) Uani 1 1 d . . . H2A H 0.3067 0.8301 0.2225 0.032 Uiso 1 1 calc R . . C3 C 0.3733(4) 0.5128(13) 0.2536(3) 0.0349(19) Uani 1 1 d . . . H3A H 0.4035 0.5540 0.2938 0.042 Uiso 1 1 calc R . . C4 C 0.3763(5) 0.2941(13) 0.2256(3) 0.0369(19) Uani 1 1 d . . . H4A H 0.4092 0.1547 0.2428 0.044 Uiso 1 1 calc R . . C5 C 0.3274(4) 0.3078(11) 0.1688(3) 0.0279(18) Uani 1 1 d . . . H5A H 0.3184 0.1793 0.1391 0.034 Uiso 1 1 calc R . . C6 C 0.4666(5) 0.6896(18) 0.1034(4) 0.053(2) Uani 1 1 d . . . H6A H 0.4282 0.7423 0.0669 0.064 Uiso 1 1 calc R . . C7 C 0.4941(5) 0.8237(13) 0.1526(4) 0.047(2) Uani 1 1 d . . . H7A H 0.4785 0.9903 0.1579 0.057 Uiso 1 1 calc R . . C8 C 0.5463(5) 0.6886(16) 0.1937(4) 0.052(2) Uani 1 1 d . . . H8A H 0.5759 0.7399 0.2333 0.062 Uiso 1 1 calc R . . C9 C 0.5517(5) 0.4690(15) 0.1683(5) 0.059(3) Uani 1 1 d . . . H9A H 0.5854 0.3336 0.1871 0.071 Uiso 1 1 calc R . . C10 C 0.5032(6) 0.4710(16) 0.1129(5) 0.054(3) Uani 1 1 d . . . H10A H 0.4954 0.3374 0.0847 0.065 Uiso 1 1 calc R . . C11 C 0.2382(4) 0.6309(11) 0.1076(3) 0.0313(18) Uani 1 1 d . . . H11A H 0.2564 0.5526 0.0725 0.038 Uiso 1 1 calc R . . H11B H 0.2513 0.7984 0.1044 0.038 Uiso 1 1 calc R . . C12 C 0.1758(4) 0.2695(11) -0.0191(3) 0.0268(17) Uani 1 1 d . . . C13 C 0.2530(4) 0.1338(11) -0.0200(3) 0.0263(17) Uani 1 1 d . . . H13A H 0.2619 -0.0314 -0.0071 0.032 Uiso 1 1 calc R . . C14 C 0.3159(4) 0.2815(13) -0.0426(3) 0.0350(19) Uani 1 1 d . . . H14A H 0.3768 0.2352 -0.0487 0.042 Uiso 1 1 calc R . . C15 C 0.2779(5) 0.5001(12) -0.0559(3) 0.0351(19) Uani 1 1 d . . . H15A H 0.3070 0.6360 -0.0724 0.042 Uiso 1 1 calc R . . C16 C 0.1912(5) 0.4936(12) -0.0420(3) 0.0306(18) Uani 1 1 d . . . H16A H 0.1480 0.6246 -0.0469 0.037 Uiso 1 1 calc R . . C17 C 0.1023(5) 0.1031(13) -0.1559(3) 0.0367(19) Uani 1 1 d . . . H17A H 0.0456 0.0524 -0.1428 0.044 Uiso 1 1 calc R . . C18 C 0.1786(5) -0.0344(13) -0.1561(3) 0.041(2) Uani 1 1 d . . . H18A H 0.1853 -0.2001 -0.1432 0.049 Uiso 1 1 calc R . . C19 C 0.2440(5) 0.1030(13) -0.1779(3) 0.038(2) Uani 1 1 d . . . H19A H 0.3047 0.0514 -0.1832 0.046 Uiso 1 1 calc R . . C20 C 0.2077(5) 0.3253(13) -0.1911(3) 0.041(2) Uani 1 1 d . . . H20A H 0.2387 0.4594 -0.2070 0.049 Uiso 1 1 calc R . . C21 C 0.1210(5) 0.3270(13) -0.1776(3) 0.037(2) Uani 1 1 d . . . H21A H 0.0797 0.4620 -0.1822 0.045 Uiso 1 1 calc R . . C22 C 0.0931(4) 0.1856(11) -0.0002(3) 0.0301(18) Uani 1 1 d . . . H22C H 0.0829 0.0231 -0.0135 0.036 Uiso 1 1 calc R . . H22A H 0.0437 0.2807 -0.0195 0.036 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 0.0231(6) 0.0333(6) 0.0307(7) -0.0002(5) 0.0052(5) -0.0019(5) Fe2 0.0276(6) 0.0336(6) 0.0244(7) -0.0004(5) 0.0064(5) -0.0036(5) Se1 0.0264(5) 0.0380(5) 0.0377(5) -0.0056(4) -0.0002(4) 0.0031(3) Se2 0.0325(5) 0.0374(5) 0.0266(5) 0.0007(4) 0.0074(4) -0.0054(3) C1 0.022(4) 0.034(4) 0.023(5) 0.001(4) 0.004(3) -0.006(3) C2 0.012(4) 0.035(4) 0.033(5) -0.002(4) 0.002(4) -0.003(3) C3 0.024(4) 0.053(5) 0.027(5) -0.004(4) 0.002(4) 0.000(4) C4 0.034(5) 0.039(5) 0.038(5) 0.008(4) 0.005(4) -0.003(4) C5 0.027(4) 0.022(4) 0.034(5) -0.001(3) 0.000(4) -0.004(3) C6 0.031(5) 0.089(7) 0.042(6) 0.022(6) 0.012(5) -0.002(5) C7 0.043(6) 0.027(5) 0.077(8) 0.005(5) 0.029(5) -0.004(4) C8 0.036(5) 0.068(6) 0.051(6) -0.006(5) 0.006(5) -0.026(5) C9 0.036(6) 0.052(6) 0.098(9) 0.021(6) 0.036(6) 0.008(4) C10 0.044(6) 0.064(7) 0.060(7) -0.029(5) 0.030(5) -0.024(5) C11 0.032(4) 0.031(4) 0.030(5) -0.001(3) 0.001(4) 0.001(3) C12 0.031(4) 0.029(4) 0.020(4) -0.002(3) 0.002(3) 0.001(3) C13 0.023(4) 0.025(4) 0.030(5) 0.001(3) -0.001(3) 0.004(3) C14 0.024(4) 0.053(5) 0.029(5) -0.005(4) 0.009(4) -0.003(4) C15 0.041(5) 0.030(4) 0.035(5) 0.008(4) 0.006(4) -0.010(4) C16 0.034(5) 0.028(4) 0.032(5) -0.005(3) 0.010(4) -0.002(3) C17 0.036(5) 0.054(5) 0.020(5) 0.001(4) 0.002(4) -0.012(4) C18 0.051(6) 0.036(5) 0.034(5) -0.010(4) -0.003(4) 0.000(4) C19 0.043(5) 0.049(5) 0.024(5) -0.022(4) 0.015(4) -0.008(4) C20 0.054(6) 0.044(5) 0.023(5) 0.007(4) 0.004(4) -0.016(4) C21 0.039(5) 0.045(5) 0.026(5) -0.002(4) -0.002(4) 0.008(4) C22 0.025(4) 0.036(4) 0.029(5) -0.006(4) 0.004(4) 0.000(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 #Se2 C22 1.983(7) . ? #C1 C5 1.430(9) . ? Fe1 C8 2.021(7) . ? Fe1 C9 2.022(8) . ? Fe1 C6 2.022(8) . ? Fe1 C7 2.023(7) . ? Fe1 C5 2.027(6) . ? Fe1 C1 2.030(6) . ? Fe1 C10 2.035(8) . ? Fe1 C3 2.047(7) . ? Fe1 C4 2.048(7) . ? Fe1 C2 2.048(7) . ? Fe2 C16 2.025(7) . ? Fe2 C15 2.034(7) . ? Fe2 C14 2.035(7) . ? Fe2 C18 2.039(7) . ? Fe2 C19 2.041(7) . ? Fe2 C20 2.047(7) . ? Fe2 C12 2.047(7) . ? Fe2 C21 2.049(7) . ? Fe2 C17 2.051(7) . ? Fe2 C13 2.051(7) . ? Se1 C11 1.976(7) . ? Se1 Se2 2.3044(10) . ? C1 C2 1.430(9) . ? C1 C11 1.489(9) . ? C2 C3 1.419(9) . ? C3 C4 1.415(9) . ? C4 C5 1.410(9) . ? C6 C7 1.380(11) . ? C6 C10 1.384(11) . ? C7 C8 1.387(11) . ? C8 C9 1.397(11) . ? C9 C10 1.378(11) . ? C12 C13 1.422(8) . ? C12 C16 1.423(9) . ? C12 C22 1.477(9) . ? C13 C14 1.433(9) . ? C14 C15 1.404(9) . ? C15 C16 1.410(9) . ? C17 C18 1.415(9) . ? C17 C21 1.423(9) . ? C18 C19 1.420(9) . ? C19 C20 1.413(9) . ? C20 C21 1.407(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Fe1 C9 40.4(3) . . ? C8 Fe1 C6 67.6(3) . . ? C9 Fe1 C6 67.1(4) . . ? C8 Fe1 C7 40.1(3) . . ? C9 Fe1 C7 67.1(3) . . ? C6 Fe1 C7 39.9(3) . . ? C8 Fe1 C5 160.4(3) . . ? C9 Fe1 C5 123.5(3) . . ? C6 Fe1 C5 121.4(3) . . ? C7 Fe1 C5 157.2(4) . . ? C8 Fe1 C1 157.5(3) . . ? C9 Fe1 C1 160.0(4) . . ? C6 Fe1 C1 107.5(3) . . ? C7 Fe1 C1 122.0(3) . . ? C5 Fe1 C1 41.3(2) . . ? C8 Fe1 C10 67.4(3) . . ? C9 Fe1 C10 39.7(3) . . ? C6 Fe1 C10 39.9(3) . . ? C7 Fe1 C10 66.8(3) . . ? C5 Fe1 C10 107.3(3) . . ? C1 Fe1 C10 123.9(3) . . ? C8 Fe1 C3 108.6(3) . . ? C9 Fe1 C3 122.8(4) . . ? C6 Fe1 C3 161.3(4) . . ? C7 Fe1 C3 125.4(3) . . ? C5 Fe1 C3 68.5(3) . . ? C1 Fe1 C3 68.6(3) . . ? C10 Fe1 C3 157.5(4) . . ? C8 Fe1 C4 124.8(3) . . ? C9 Fe1 C4 108.5(3) . . ? C6 Fe1 C4 156.9(4) . . ? C7 Fe1 C4 161.5(4) . . ? C5 Fe1 C4 40.5(3) . . ? C1 Fe1 C4 68.4(3) . . ? C10 Fe1 C4 122.1(3) . . ? C3 Fe1 C4 40.4(3) . . ? C8 Fe1 C2 122.2(3) . . ? C9 Fe1 C2 158.0(4) . . ? C6 Fe1 C2 124.6(3) . . ? C7 Fe1 C2 108.7(3) . . ? C5 Fe1 C2 69.1(3) . . ? C1 Fe1 C2 41.1(2) . . ? C10 Fe1 C2 160.7(4) . . ? C3 Fe1 C2 40.5(3) . . ? C4 Fe1 C2 68.3(3) . . ? C16 Fe2 C15 40.7(3) . . ? C16 Fe2 C14 68.1(3) . . ? C15 Fe2 C14 40.4(3) . . ? C16 Fe2 C18 158.2(3) . . ? C15 Fe2 C18 160.1(3) . . ? C14 Fe2 C18 124.5(3) . . ? C16 Fe2 C19 159.2(3) . . ? C15 Fe2 C19 123.2(3) . . ? C14 Fe2 C19 108.1(3) . . ? C18 Fe2 C19 40.7(3) . . ? C16 Fe2 C20 123.0(3) . . ? C15 Fe2 C20 107.3(3) . . ? C14 Fe2 C20 122.4(3) . . ? C18 Fe2 C20 68.0(3) . . ? C19 Fe2 C20 40.4(3) . . ? C16 Fe2 C12 40.9(2) . . ? C15 Fe2 C12 68.5(3) . . ? C14 Fe2 C12 68.1(3) . . ? C18 Fe2 C12 122.7(3) . . ? C19 Fe2 C12 158.5(3) . . ? C20 Fe2 C12 159.7(3) . . ? C16 Fe2 C21 107.2(3) . . ? C15 Fe2 C21 121.7(3) . . ? C14 Fe2 C21 157.4(3) . . ? C18 Fe2 C21 68.1(3) . . ? C19 Fe2 C21 68.0(3) . . ? C20 Fe2 C21 40.2(3) . . ? C12 Fe2 C21 123.8(3) . . ? C16 Fe2 C17 122.1(3) . . ? C15 Fe2 C17 157.6(3) . . ? C14 Fe2 C17 160.7(3) . . ? C18 Fe2 C17 40.5(3) . . ? C19 Fe2 C17 68.3(3) . . ? C20 Fe2 C17 68.0(3) . . ? C12 Fe2 C17 107.9(3) . . ? C21 Fe2 C17 40.6(3) . . ? C16 Fe2 C13 68.9(3) . . ? C15 Fe2 C13 69.0(3) . . ? C14 Fe2 C13 41.0(2) . . ? C18 Fe2 C13 107.8(3) . . ? C19 Fe2 C13 122.5(3) . . ? C20 Fe2 C13 158.3(3) . . ? C12 Fe2 C13 40.6(2) . . ? C21 Fe2 C13 160.0(3) . . ? C17 Fe2 C13 123.6(3) . . ? C11 Se1 Se2 101.03(19) . . ? C22 Se2 Se1 102.51(19) . . ? C5 C1 C2 107.9(6) . . ? C5 C1 C11 126.1(6) . . ? C2 C1 C11 125.9(6) . . ? C5 C1 Fe1 69.3(4) . . ? C2 C1 Fe1 70.2(4) . . ? C11 C1 Fe1 123.9(5) . . ? C3 C2 C1 107.4(6) . . ? C3 C2 Fe1 69.7(4) . . ? C1 C2 Fe1 68.8(4) . . ? C4 C3 C2 108.4(6) . . ? C4 C3 Fe1 69.8(4) . . ? C2 C3 Fe1 69.8(4) . . ? C5 C4 C3 108.6(6) . . ? C5 C4 Fe1 69.0(4) . . ? C3 C4 Fe1 69.7(4) . . ? C4 C5 C1 107.7(6) . . ? C4 C5 Fe1 70.5(4) . . ? C1 C5 Fe1 69.4(4) . . ? C7 C6 C10 107.9(8) . . ? C7 C6 Fe1 70.1(5) . . ? C10 C6 Fe1 70.5(5) . . ? C6 C7 C8 108.7(7) . . ? C6 C7 Fe1 70.0(4) . . ? C8 C7 Fe1 69.8(4) . . ? C7 C8 C9 106.8(8) . . ? C7 C8 Fe1 70.0(4) . . ? C9 C8 Fe1 69.8(4) . . ? C10 C9 C8 108.5(8) . . ? C10 C9 Fe1 70.7(5) . . ? C8 C9 Fe1 69.7(4) . . ? C9 C10 C6 108.0(8) . . ? C9 C10 Fe1 69.6(5) . . ? C6 C10 Fe1 69.6(5) . . ? C1 C11 Se1 114.6(5) . . ? C13 C12 C16 108.3(6) . . ? C13 C12 C22 125.1(6) . . ? C16 C12 C22 126.5(6) . . ? C13 C12 Fe2 69.8(4) . . ? C16 C12 Fe2 68.7(4) . . ? C22 C12 Fe2 125.1(5) . . ? C12 C13 C14 106.3(6) . . ? C12 C13 Fe2 69.6(4) . . ? C14 C13 Fe2 68.9(4) . . ? C15 C14 C13 109.3(6) . . ? C15 C14 Fe2 69.8(4) . . ? C13 C14 Fe2 70.1(4) . . ? C14 C15 C16 107.8(6) . . ? C14 C15 Fe2 69.9(4) . . ? C16 C15 Fe2 69.3(4) . . ? C15 C16 C12 108.3(6) . . ? C15 C16 Fe2 70.0(4) . . ? C12 C16 Fe2 70.4(4) . . ? C18 C17 C21 107.5(7) . . ? C18 C17 Fe2 69.3(4) . . ? C21 C17 Fe2 69.6(4) . . ? C17 C18 C19 108.3(7) . . ? C17 C18 Fe2 70.2(4) . . ? C19 C18 Fe2 69.7(4) . . ? C20 C19 C18 107.6(7) . . ? C20 C19 Fe2 70.0(4) . . ? C18 C19 Fe2 69.5(4) . . ? C21 C20 C19 108.5(6) . . ? C21 C20 Fe2 70.0(4) . . ? C19 C20 Fe2 69.6(4) . . ? C20 C21 C17 108.1(6) . . ? C20 C21 Fe2 69.8(4) . . ? C17 C21 Fe2 69.7(4) . . ? C12 C22 Se2 112.6(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.599 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.150 data_cn321a _database_code_depnum_ccdc_archive 'CCDC 814945' #TrackingRef 'Corrigan-New-J-Chem-2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H62 Cl18 Fe2 N4 Se4 Zn2' _chemical_formula_weight 1819.34 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 17.346(4) _cell_length_b 42.440(9) _cell_length_c 12.596(3) _cell_angle_alpha 90.00 _cell_angle_beta 133.24(3) _cell_angle_gamma 90.00 _cell_volume 6755(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27315 _cell_measurement_theta_min 3.72 _cell_measurement_theta_max 31.74 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 4.023 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE STADI4 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27129 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 53 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 31.67 _reflns_number_total 14291 _reflns_number_gt 13069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE CRYSALIS ' _computing_cell_refinement 'STOE CRYSALIS ' _computing_data_reduction 'STOE CRYSALIS ' _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^)+(0.0861P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(8) _refine_ls_number_reflns 14291 _refine_ls_number_parameters 649 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1312 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 Se1 Se -0.20557(4) 0.702236(13) 0.34458(6) 0.01965(12) Uani 1 1 d . . . Se3 Se 0.11437(4) 0.698907(13) 0.70575(6) 0.01962(12) Uani 1 1 d . . . Se2 Se -0.00050(4) 0.554399(13) 0.71159(6) 0.02050(12) Uani 1 1 d . . . Se4 Se -0.06359(5) 0.549835(13) 0.33006(6) 0.02424(13) Uani 1 1 d . . . Zn1 Zn -0.04277(5) 0.728668(14) 0.53113(7) 0.01714(13) Uani 1 1 d . . . Zn2 Zn -0.03137(5) 0.524646(14) 0.52568(7) 0.01812(13) Uani 1 1 d . . . Fe2 Fe 0.07974(6) 0.647307(19) 0.32647(9) 0.01917(17) Uani 1 1 d . . . Fe1 Fe -0.30259(7) 0.622581(19) 0.51668(9) 0.01994(17) Uani 1 1 d . . . C1 C -0.3743(5) 0.64700(15) 0.3285(7) 0.0246(12) Uani 1 1 d . . . H1A H -0.3961 0.6382 0.2376 0.030 Uiso 1 1 calc R . . C2 C -0.4383(5) 0.64808(15) 0.3626(8) 0.0295(14) Uani 1 1 d . . . H2A H -0.5125 0.6402 0.2998 0.035 Uiso 1 1 calc R . . C3 C -0.3767(6) 0.66193(15) 0.5012(9) 0.0327(15) Uani 1 1 d . . . H3A H -0.4002 0.6655 0.5539 0.039 Uiso 1 1 calc R . . C4 C -0.2763(6) 0.67022(14) 0.5539(8) 0.0280(13) Uani 1 1 d . . . H4A H -0.2173 0.6805 0.6496 0.034 Uiso 1 1 calc R . . C5 C -0.2738(5) 0.66100(13) 0.4480(6) 0.0202(11) Uani 1 1 d . . . C6 C -0.1842(5) 0.66458(14) 0.4575(7) 0.0230(12) Uani 1 1 d . . . H6A H -0.1783 0.6455 0.4185 0.028 Uiso 1 1 calc R . . H6B H -0.1174 0.6670 0.5609 0.028 Uiso 1 1 calc R . . C7 C -0.1830(5) 0.59970(16) 0.7062(7) 0.0280(13) Uani 1 1 d . . . H7A H -0.1194 0.6098 0.7990 0.034 Uiso 1 1 calc R . . C8 C -0.2826(6) 0.59428(16) 0.6636(8) 0.0327(15) Uani 1 1 d . . . H8A H -0.3001 0.6000 0.7221 0.039 Uiso 1 1 calc R . . C9 C -0.3515(6) 0.57993(16) 0.5268(9) 0.0357(16) Uani 1 1 d . . . H9A H -0.4264 0.5737 0.4709 0.043 Uiso 1 1 calc R . . C10 C -0.2973(6) 0.57620(15) 0.4788(8) 0.0311(14) Uani 1 1 d . . . H10A H -0.3279 0.5670 0.3837 0.037 Uiso 1 1 calc R . . C11 C -0.1906(5) 0.58804(13) 0.5918(7) 0.0219(11) Uani 1 1 d . . . C12 C -0.1060(5) 0.58819(13) 0.5890(7) 0.0216(11) Uani 1 1 d . . . H12A H -0.0697 0.6089 0.6241 0.026 Uiso 1 1 calc R . . H12B H -0.1387 0.5854 0.4873 0.026 Uiso 1 1 calc R . . C13 C 0.1883(5) 0.67500(15) 0.5055(7) 0.0262(13) Uani 1 1 d . . . H13A H 0.2589 0.6679 0.5989 0.031 Uiso 1 1 calc R . . C14 C 0.0910(5) 0.67434(13) 0.4726(7) 0.0211(11) Uani 1 1 d . . . C15 C 0.0095(5) 0.68589(15) 0.3275(7) 0.0279(13) Uani 1 1 d . . . H15A H -0.0671 0.6880 0.2739 0.034 Uiso 1 1 calc R . . C16 C 0.0568(6) 0.69364(15) 0.2708(8) 0.0308(14) Uani 1 1 d . . . H16A H 0.0189 0.7022 0.1717 0.037 Uiso 1 1 calc R . . C17 C 0.1671(6) 0.68728(14) 0.3820(8) 0.0304(14) Uani 1 1 d . . . H17A H 0.2202 0.6903 0.3741 0.037 Uiso 1 1 calc R . . C18 C 0.0801(5) 0.66409(14) 0.5743(7) 0.0223(12) Uani 1 1 d . . . H18A H 0.1281 0.6461 0.6331 0.027 Uiso 1 1 calc R . . H18B H 0.0066 0.6569 0.5177 0.027 Uiso 1 1 calc R . . C19 C -0.0425(5) 0.61674(15) 0.1852(7) 0.0275(13) Uani 1 1 d . . . H19A H -0.1189 0.6208 0.1287 0.033 Uiso 1 1 calc R . . C20 C 0.0107(6) 0.62377(15) 0.1388(8) 0.0299(14) Uani 1 1 d . . . H20A H -0.0217 0.6335 0.0437 0.036 Uiso 1 1 calc R . . C21 C 0.1185(6) 0.61393(15) 0.2515(8) 0.0304(14) Uani 1 1 d . . . H21A H 0.1749 0.6160 0.2494 0.037 Uiso 1 1 calc R . . C22 C 0.1321(5) 0.60123(14) 0.3678(8) 0.0263(13) Uani 1 1 d . . . H22A H 0.1999 0.5930 0.4620 0.032 Uiso 1 1 calc R . . C23 C 0.0332(5) 0.60277(13) 0.3285(6) 0.0204(11) Uani 1 1 d . . . C24 C 0.0092(6) 0.59096(14) 0.4139(7) 0.0266(13) Uani 1 1 d . . . H24A H -0.0369 0.6061 0.4084 0.032 Uiso 1 1 calc R . . H24B H 0.0754 0.5884 0.5175 0.032 Uiso 1 1 calc R . . C25 C -0.0176(5) 0.79574(13) 0.5216(7) 0.0233(12) Uani 1 1 d . . . H25A H -0.0399 0.8150 0.4624 0.028 Uiso 1 1 calc R . . H25B H 0.0577 0.7982 0.6127 0.028 Uiso 1 1 calc R . . C26 C -0.0845(5) 0.79183(14) 0.5587(7) 0.0251(12) Uani 1 1 d . . . H26A H -0.0731 0.8101 0.6170 0.030 Uiso 1 1 calc R . . H26B H -0.1604 0.7913 0.4676 0.030 Uiso 1 1 calc R . . C27 C -0.1254(5) 0.77091(16) 0.2825(7) 0.0291(13) Uani 1 1 d . . . H27A H -0.1183 0.7891 0.2417 0.044 Uiso 1 1 calc R . . H27B H -0.1872 0.7739 0.2702 0.044 Uiso 1 1 calc R . . H27C H -0.1345 0.7517 0.2316 0.044 Uiso 1 1 calc R . . C28 C 0.0638(5) 0.76647(15) 0.4558(8) 0.0284(13) Uani 1 1 d . . . H28A H 0.0653 0.7852 0.4117 0.043 Uiso 1 1 calc R . . H28B H 0.0591 0.7475 0.4070 0.043 Uiso 1 1 calc R . . H28C H 0.1287 0.7656 0.5595 0.043 Uiso 1 1 calc R . . C29 C 0.0452(5) 0.76640(16) 0.7946(7) 0.0296(14) Uani 1 1 d . . . H29A H 0.0369 0.7820 0.8436 0.044 Uiso 1 1 calc R . . H29B H 0.0997 0.7736 0.7963 0.044 Uiso 1 1 calc R . . H29C H 0.0662 0.7461 0.8451 0.044 Uiso 1 1 calc R . . C30 C -0.1415(6) 0.75435(16) 0.6373(8) 0.0324(14) Uani 1 1 d . . . H30A H -0.1453 0.7704 0.6895 0.049 Uiso 1 1 calc R . . H30B H -0.1260 0.7338 0.6840 0.049 Uiso 1 1 calc R . . H30C H -0.2093 0.7533 0.5358 0.049 Uiso 1 1 calc R . . C31 C 0.0081(5) 0.45843(14) 0.5280(7) 0.0259(13) Uani 1 1 d . . . H31A H 0.0475 0.4389 0.5822 0.031 Uiso 1 1 calc R . . H31B H -0.0103 0.4579 0.4343 0.031 Uiso 1 1 calc R . . C32 C -0.0931(5) 0.45993(14) 0.4990(7) 0.0245(12) Uani 1 1 d . . . H32A H -0.1384 0.4416 0.4392 0.029 Uiso 1 1 calc R . . H32B H -0.0746 0.4588 0.5927 0.029 Uiso 1 1 calc R . . C35 C 0.1339(6) 0.48137(17) 0.7709(7) 0.0342(15) Uani 1 1 d . . . H35A H 0.1827 0.4636 0.8094 0.051 Uiso 1 1 calc R . . H35B H 0.0835 0.4770 0.7804 0.051 Uiso 1 1 calc R . . H35C H 0.1741 0.5005 0.8257 0.051 Uiso 1 1 calc R . . C36 C 0.1542(6) 0.49007(17) 0.6021(9) 0.0359(15) Uani 1 1 d . . . H36A H 0.2012 0.4717 0.6448 0.054 Uiso 1 1 calc R . . H36B H 0.1960 0.5091 0.6546 0.054 Uiso 1 1 calc R . . H36C H 0.1176 0.4920 0.4993 0.054 Uiso 1 1 calc R . . C34 C -0.2250(6) 0.49580(17) 0.4418(9) 0.0355(15) Uani 1 1 d . . . H34A H -0.2794 0.4794 0.3930 0.053 Uiso 1 1 calc R . . H34B H -0.2587 0.5164 0.3995 0.053 Uiso 1 1 calc R . . H34C H -0.1855 0.4959 0.5460 0.053 Uiso 1 1 calc R . . C33 C -0.2124(6) 0.48664(16) 0.2651(7) 0.0363(16) Uani 1 1 d . . . H33A H -0.2670 0.4704 0.2213 0.054 Uiso 1 1 calc R . . H33B H -0.1642 0.4808 0.2530 0.054 Uiso 1 1 calc R . . H33C H -0.2460 0.5069 0.2170 0.054 Uiso 1 1 calc R . . C37 C 0.7800(7) 0.91305(18) 0.4294(10) 0.0433(18) Uani 1 1 d . . . H37A H 0.7025 0.9142 0.3719 0.052 Uiso 1 1 calc R . . C42 C 0.8906(7) 0.1330(2) 0.5729(10) 0.048(2) Uani 1 1 d . . . H42A H 0.8135 0.1378 0.4920 0.058 Uiso 1 1 calc R . . C41 C 0.6440(7) 0.16326(16) 0.9943(8) 0.0368(16) Uani 1 1 d . . . H41A H 0.6558 0.1721 0.9329 0.044 Uiso 1 1 calc R . . C39 C 0.4739(6) 0.5240(2) 0.7186(9) 0.0417(17) Uani 1 1 d . . . H39A H 0.5135 0.5443 0.7647 0.050 Uiso 1 1 calc R . . C38 C 0.7379(7) 0.7344(2) 0.8695(10) 0.049(2) Uani 1 1 d . . . H38A H 0.7087 0.7473 0.9017 0.059 Uiso 1 1 calc R . . C40 C 0.6947(6) 0.40609(18) 0.5769(8) 0.0362(15) Uani 1 1 d . . . H40A H 0.7629 0.4166 0.6604 0.043 Uiso 1 1 calc R . . N3 N -0.1523(4) 0.48943(11) 0.4221(6) 0.0229(10) Uani 1 1 d . . . N4 N 0.0752(4) 0.48610(12) 0.6136(6) 0.0236(10) Uani 1 1 d . . . N1 N -0.0292(4) 0.76801(11) 0.4393(5) 0.0202(10) Uani 1 1 d . . . N2 N -0.0566(4) 0.76267(11) 0.6415(6) 0.0222(10) Uani 1 1 d . . . Cl12 Cl 0.67132(15) 0.41191(5) 0.4175(2) 0.0410(4) Uani 1 1 d . . . Cl11 Cl 0.59290(19) 0.42319(6) 0.5565(2) 0.0527(5) Uani 1 1 d . . . Cl10 Cl 0.70639(18) 0.36574(5) 0.6151(2) 0.0461(4) Uani 1 1 d . . . Cl1 Cl 0.8153(2) 0.87341(5) 0.4445(3) 0.0531(5) Uani 1 1 d . . . Cl15 Cl 0.5441(2) 0.18549(5) 0.9622(3) 0.0583(6) Uani 1 1 d . . . Cl18 Cl 0.91321(19) 0.11990(7) 0.7239(3) 0.0632(6) Uani 1 1 d . . . Cl7 Cl 0.53589(19) 0.49472(6) 0.8564(3) 0.0574(5) Uani 1 1 d . . . Cl4 Cl 0.8616(2) 0.75053(6) 0.9497(3) 0.0615(6) Uani 1 1 d . . . Cl2 Cl 0.8054(2) 0.93400(7) 0.3364(4) 0.0752(8) Uani 1 1 d . . . Cl3 Cl 0.8494(3) 0.92873(9) 0.6023(4) 0.0946(11) Uani 1 1 d . . . Cl13 Cl 0.76361(19) 0.16580(6) 1.1783(2) 0.0549(6) Uani 1 1 d . . . Cl14 Cl 0.60425(16) 0.12382(5) 0.9437(2) 0.0430(4) Uani 1 1 d . . . Cl16 Cl 0.9631(2) 0.16765(7) 0.6158(4) 0.0769(8) Uani 1 1 d . . . Cl17 Cl 0.9253(2) 0.10353(7) 0.5140(3) 0.0704(7) Uani 1 1 d . . . Cl8 Cl 0.34449(18) 0.52981(7) 0.6372(3) 0.0633(6) Uani 1 1 d . . . Cl9 Cl 0.4788(2) 0.51296(7) 0.5892(3) 0.0658(7) Uani 1 1 d . . . Cl5 Cl 0.6498(2) 0.73645(7) 0.6813(3) 0.0747(8) Uani 1 1 d . . . Cl6 Cl 0.7541(2) 0.69596(7) 0.9296(4) 0.0845(10) 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 Se1 0.0177(2) 0.0191(3) 0.0214(3) 0.0013(2) 0.0131(2) -0.0025(2) Se3 0.0196(3) 0.0225(3) 0.0176(2) 0.0002(2) 0.0130(2) 0.0032(2) Se2 0.0249(3) 0.0200(3) 0.0203(3) 0.0004(2) 0.0169(2) 0.0042(2) Se4 0.0376(3) 0.0184(3) 0.0242(3) -0.0011(2) 0.0241(3) -0.0053(2) Zn1 0.0173(3) 0.0156(3) 0.0211(3) -0.0005(3) 0.0141(2) -0.0007(2) Zn2 0.0254(3) 0.0144(3) 0.0220(3) -0.0002(3) 0.0191(3) -0.0004(3) Fe2 0.0248(4) 0.0168(4) 0.0253(4) -0.0034(3) 0.0208(4) -0.0040(3) Fe1 0.0237(4) 0.0165(4) 0.0287(4) 0.0031(3) 0.0215(4) 0.0019(3) C1 0.021(3) 0.027(3) 0.027(3) 0.008(2) 0.016(3) 0.004(2) C2 0.023(3) 0.028(3) 0.048(4) 0.017(3) 0.028(3) 0.009(2) C3 0.050(4) 0.019(3) 0.062(5) 0.006(3) 0.051(4) 0.007(3) C4 0.038(3) 0.018(3) 0.044(4) 0.001(3) 0.034(3) 0.001(2) C5 0.027(3) 0.014(3) 0.025(3) 0.003(2) 0.019(2) -0.001(2) C6 0.023(3) 0.019(3) 0.032(3) 0.006(2) 0.021(3) 0.004(2) C7 0.031(3) 0.032(3) 0.025(3) 0.007(2) 0.021(3) 0.009(3) C8 0.041(4) 0.033(3) 0.046(4) 0.015(3) 0.039(3) 0.013(3) C9 0.041(4) 0.021(3) 0.062(5) 0.010(3) 0.042(4) 0.004(3) C10 0.035(3) 0.019(3) 0.044(4) 0.004(3) 0.029(3) 0.003(2) C11 0.027(3) 0.017(3) 0.030(3) 0.004(2) 0.022(3) 0.005(2) C12 0.026(3) 0.018(3) 0.030(3) 0.000(2) 0.022(3) 0.003(2) C13 0.027(3) 0.026(3) 0.034(3) -0.010(3) 0.024(3) -0.005(2) C14 0.025(3) 0.013(3) 0.030(3) -0.006(2) 0.021(3) -0.003(2) C15 0.036(3) 0.026(3) 0.031(3) 0.002(3) 0.026(3) 0.004(3) C16 0.052(4) 0.021(3) 0.036(3) 0.002(3) 0.037(3) -0.001(3) C17 0.046(4) 0.018(3) 0.053(4) -0.014(3) 0.044(4) -0.015(3) C18 0.028(3) 0.021(3) 0.025(3) -0.002(2) 0.021(3) 0.003(2) C19 0.033(3) 0.029(3) 0.024(3) -0.005(2) 0.021(3) -0.011(3) C20 0.048(4) 0.025(3) 0.029(3) -0.008(2) 0.031(3) -0.013(3) C21 0.043(4) 0.022(3) 0.045(4) -0.015(3) 0.037(3) -0.011(3) C22 0.034(3) 0.013(3) 0.039(3) -0.006(2) 0.027(3) -0.004(2) C23 0.033(3) 0.014(3) 0.025(3) -0.003(2) 0.024(3) -0.005(2) C24 0.043(4) 0.023(3) 0.030(3) -0.002(2) 0.031(3) -0.008(3) C25 0.026(3) 0.012(2) 0.030(3) -0.005(2) 0.019(3) -0.005(2) C26 0.028(3) 0.019(3) 0.031(3) 0.002(2) 0.021(3) 0.004(2) C27 0.028(3) 0.029(3) 0.027(3) 0.003(2) 0.017(3) -0.002(2) C28 0.025(3) 0.030(3) 0.041(4) 0.003(3) 0.026(3) -0.002(2) C29 0.032(3) 0.027(3) 0.021(3) -0.004(2) 0.015(3) -0.003(3) C30 0.038(4) 0.030(3) 0.048(4) -0.010(3) 0.037(3) -0.008(3) C31 0.038(3) 0.015(3) 0.035(3) -0.002(2) 0.029(3) 0.002(2) C32 0.036(3) 0.014(3) 0.030(3) 0.001(2) 0.026(3) -0.002(2) C35 0.039(4) 0.036(4) 0.026(3) 0.005(3) 0.021(3) 0.003(3) C36 0.035(4) 0.035(4) 0.054(4) 0.001(3) 0.037(4) 0.003(3) C34 0.033(3) 0.027(3) 0.057(4) -0.007(3) 0.035(3) -0.008(3) C33 0.051(4) 0.022(3) 0.027(3) -0.001(3) 0.023(3) -0.004(3) C37 0.039(4) 0.039(4) 0.055(5) 0.011(4) 0.033(4) 0.008(3) C42 0.036(4) 0.058(5) 0.055(5) 0.003(4) 0.033(4) 0.010(4) C41 0.059(5) 0.030(4) 0.047(4) 0.001(3) 0.046(4) -0.005(3) C39 0.034(4) 0.048(4) 0.041(4) 0.000(3) 0.025(3) -0.005(3) C38 0.048(5) 0.054(5) 0.054(5) 0.002(4) 0.039(4) 0.016(4) C40 0.037(4) 0.039(4) 0.035(4) 0.001(3) 0.025(3) -0.001(3) N3 0.028(3) 0.014(2) 0.031(3) -0.001(2) 0.022(2) -0.0016(19) N4 0.031(3) 0.019(2) 0.029(3) 0.001(2) 0.024(2) 0.001(2) N1 0.019(2) 0.020(2) 0.022(2) 0.0021(18) 0.014(2) -0.0007(18) N2 0.026(3) 0.018(2) 0.028(3) -0.0014(19) 0.021(2) 0.0015(19) Cl12 0.0377(9) 0.0515(11) 0.0419(9) 0.0122(8) 0.0304(8) 0.0038(8) Cl11 0.0541(12) 0.0619(13) 0.0559(12) 0.0049(10) 0.0431(11) 0.0156(10) Cl10 0.0579(12) 0.0409(10) 0.0585(12) 0.0133(9) 0.0472(11) 0.0060(9) Cl1 0.0589(13) 0.0399(10) 0.0638(13) 0.0017(9) 0.0433(12) 0.0058(9) Cl15 0.0938(18) 0.0425(11) 0.0819(16) 0.0145(10) 0.0769(16) 0.0160(11) Cl18 0.0481(12) 0.0917(18) 0.0542(12) 0.0210(12) 0.0368(11) 0.0262(12) Cl7 0.0535(12) 0.0640(14) 0.0562(12) 0.0138(10) 0.0381(11) 0.0049(10) Cl4 0.0531(13) 0.0609(14) 0.0701(15) 0.0062(11) 0.0421(12) -0.0015(10) Cl2 0.0693(16) 0.0707(16) 0.114(2) 0.0410(16) 0.0740(18) 0.0200(13) Cl3 0.095(2) 0.085(2) 0.079(2) -0.0388(17) 0.0499(19) -0.0143(18) Cl13 0.0613(13) 0.0658(14) 0.0414(10) -0.0129(9) 0.0367(10) -0.0294(11) Cl14 0.0458(10) 0.0409(10) 0.0533(11) -0.0140(8) 0.0382(10) -0.0114(8) Cl16 0.0727(17) 0.0795(18) 0.113(2) -0.0274(17) 0.0772(19) -0.0257(14) Cl17 0.0665(16) 0.0788(17) 0.0691(15) -0.0027(13) 0.0478(14) 0.0251(13) Cl8 0.0384(10) 0.0976(19) 0.0542(12) -0.0034(12) 0.0319(10) 0.0094(11) Cl9 0.0653(15) 0.0956(19) 0.0609(14) 0.0017(13) 0.0527(13) 0.0088(13) Cl5 0.0727(17) 0.0720(16) 0.0430(12) 0.0010(11) 0.0255(12) 0.0208(14) Cl6 0.0622(16) 0.0709(17) 0.094(2) 0.0305(16) 0.0435(16) -0.0020(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 Se1 C6 1.998(6) . ? Se1 Zn1 2.3797(14) . ? Se3 C18 1.983(6) . ? Se3 Zn1 2.3767(13) . ? Se2 C12 1.979(6) . ? Se2 Zn2 2.3763(9) . ? Se4 C24 1.982(6) . ? Se4 Zn2 2.3748(10) . ? Zn1 N2 2.129(5) . ? Zn1 N1 2.134(5) . ? Zn2 N4 2.125(5) . ? Zn2 N3 2.141(5) . ? Fe2 C16 2.033(6) . ? Fe2 C20 2.035(6) . ? Fe2 C19 2.043(6) . ? Fe2 C15 2.047(6) . ? Fe2 C13 2.048(6) . ? Fe2 C17 2.052(6) . ? Fe2 C21 2.054(6) . ? Fe2 C14 2.061(6) . ? Fe2 C23 2.062(5) . ? Fe2 C22 2.067(6) . ? Fe1 C8 2.027(6) . ? Fe1 C3 2.034(6) . ? Fe1 C7 2.039(6) . ? Fe1 C9 2.040(7) . ? Fe1 C10 2.042(7) . ? Fe1 C1 2.049(6) . ? Fe1 C2 2.054(6) . ? Fe1 C4 2.055(6) . ? Fe1 C5 2.061(5) . ? Fe1 C11 2.073(6) . ? C1 C5 1.436(9) . ? C1 C2 1.439(9) . ? C2 C3 1.407(11) . ? C3 C4 1.419(10) . ? C4 C5 1.420(9) . ? C5 C6 1.483(8) . ? C7 C8 1.434(10) . ? C7 C11 1.441(9) . ? C8 C9 1.395(12) . ? C9 C10 1.433(10) . ? C10 C11 1.447(10) . ? C11 C12 1.493(8) . ? C13 C17 1.430(10) . ? C13 C14 1.436(8) . ? C14 C15 1.428(9) . ? C14 C18 1.483(8) . ? C15 C16 1.447(9) . ? C16 C17 1.423(11) . ? C19 C20 1.422(9) . ? C19 C23 1.444(9) . ? C20 C21 1.431(11) . ? C21 C22 1.421(10) . ? C22 C23 1.425(9) . ? C23 C24 1.482(8) . ? C25 N1 1.488(7) . ? C25 C26 1.529(9) . ? C26 N2 1.470(8) . ? C27 N1 1.478(8) . ? C28 N1 1.480(8) . ? C29 N2 1.482(8) . ? C30 N2 1.479(8) . ? C31 N4 1.475(8) . ? C31 C32 1.530(9) . ? C32 N3 1.482(8) . ? C35 N4 1.496(8) . ? C36 N4 1.483(8) . ? C34 N3 1.468(8) . ? C33 N3 1.479(8) . ? C37 Cl3 1.745(10) . ? C37 Cl2 1.751(9) . ? C37 Cl1 1.756(8) . ? C42 Cl18 1.749(9) . ? C42 Cl17 1.759(9) . ? C42 Cl16 1.761(10) . ? C41 Cl14 1.755(7) . ? C41 Cl15 1.759(8) . ? C41 Cl13 1.760(9) . ? C39 Cl8 1.731(8) . ? C39 Cl9 1.755(8) . ? C39 Cl7 1.778(8) . ? C38 Cl5 1.732(9) . ? C38 Cl6 1.740(10) . ? C38 Cl4 1.767(10) . ? C40 Cl10 1.752(8) . ? C40 Cl11 1.757(8) . ? C40 Cl12 1.773(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 C6 Se1 Zn1 99.09(19) . . ? C18 Se3 Zn1 97.20(18) . . ? C12 Se2 Zn2 98.77(18) . . ? C24 Se4 Zn2 103.43(17) . . ? N2 Zn1 N1 85.8(2) . . ? N2 Zn1 Se3 109.08(15) . . ? N1 Zn1 Se3 115.77(14) . . ? N2 Zn1 Se1 112.08(15) . . ? N1 Zn1 Se1 109.31(14) . . ? Se3 Zn1 Se1 119.74(4) . . ? N4 Zn2 N3 85.39(19) . . ? N4 Zn2 Se4 112.92(14) . . ? N3 Zn2 Se4 104.24(15) . . ? N4 Zn2 Se2 111.56(15) . . ? N3 Zn2 Se2 115.88(14) . . ? Se4 Zn2 Se2 121.15(3) . . ? C16 Fe2 C20 104.7(3) . . ? C16 Fe2 C19 118.2(3) . . ? C20 Fe2 C19 40.8(3) . . ? C16 Fe2 C15 41.5(3) . . ? C20 Fe2 C15 121.4(3) . . ? C19 Fe2 C15 104.3(3) . . ? C16 Fe2 C13 68.9(3) . . ? C20 Fe2 C13 157.9(3) . . ? C19 Fe2 C13 161.1(3) . . ? C15 Fe2 C13 68.7(3) . . ? C16 Fe2 C17 40.8(3) . . ? C20 Fe2 C17 120.7(3) . . ? C19 Fe2 C17 154.8(3) . . ? C15 Fe2 C17 68.9(3) . . ? C13 Fe2 C17 40.8(3) . . ? C16 Fe2 C21 123.8(3) . . ? C20 Fe2 C21 41.0(3) . . ? C19 Fe2 C21 68.5(3) . . ? C15 Fe2 C21 159.8(3) . . ? C13 Fe2 C21 123.9(3) . . ? C17 Fe2 C21 109.2(3) . . ? C16 Fe2 C14 69.3(2) . . ? C20 Fe2 C14 158.6(3) . . ? C19 Fe2 C14 122.6(2) . . ? C15 Fe2 C14 40.7(2) . . ? C13 Fe2 C14 40.9(2) . . ? C17 Fe2 C14 68.9(2) . . ? C21 Fe2 C14 159.0(3) . . ? C16 Fe2 C23 154.8(3) . . ? C20 Fe2 C23 68.9(2) . . ? C19 Fe2 C23 41.2(2) . . ? C15 Fe2 C23 119.6(3) . . ? C13 Fe2 C23 125.8(3) . . ? C17 Fe2 C23 163.2(3) . . ? C21 Fe2 C23 68.2(2) . . ? C14 Fe2 C23 107.3(2) . . ? C16 Fe2 C22 161.8(3) . . ? C20 Fe2 C22 68.6(3) . . ? C19 Fe2 C22 68.5(3) . . ? C15 Fe2 C22 156.4(3) . . ? C13 Fe2 C22 110.6(3) . . ? C17 Fe2 C22 127.0(3) . . ? C21 Fe2 C22 40.3(3) . . ? C14 Fe2 C22 123.1(3) . . ? C23 Fe2 C22 40.4(2) . . ? C8 Fe1 C3 106.0(3) . . ? C8 Fe1 C7 41.3(3) . . ? C3 Fe1 C7 124.9(3) . . ? C8 Fe1 C9 40.1(3) . . ? C3 Fe1 C9 118.2(3) . . ? C7 Fe1 C9 68.7(3) . . ? C8 Fe1 C10 68.6(3) . . ? C3 Fe1 C10 153.6(3) . . ? C7 Fe1 C10 69.0(3) . . ? C9 Fe1 C10 41.1(3) . . ? C8 Fe1 C1 160.8(3) . . ? C3 Fe1 C1 68.4(3) . . ? C7 Fe1 C1 156.8(3) . . ? C9 Fe1 C1 124.9(3) . . ? C10 Fe1 C1 107.8(3) . . ? C8 Fe1 C2 122.9(3) . . ? C3 Fe1 C2 40.3(3) . . ? C7 Fe1 C2 160.9(3) . . ? C9 Fe1 C2 105.7(3) . . ? C10 Fe1 C2 119.5(3) . . ? C1 Fe1 C2 41.1(2) . . ? C8 Fe1 C4 120.1(3) . . ? C3 Fe1 C4 40.6(3) . . ? C7 Fe1 C4 108.2(3) . . ? C9 Fe1 C4 153.6(3) . . ? C10 Fe1 C4 164.4(3) . . ? C1 Fe1 C4 68.3(3) . . ? C2 Fe1 C4 68.2(3) . . ? C8 Fe1 C5 155.9(3) . . ? C3 Fe1 C5 68.2(2) . . ? C7 Fe1 C5 121.6(3) . . ? C9 Fe1 C5 163.5(3) . . ? C10 Fe1 C5 127.0(3) . . ? C1 Fe1 C5 40.9(2) . . ? C2 Fe1 C5 68.7(2) . . ? C4 Fe1 C5 40.4(2) . . ? C8 Fe1 C11 69.1(2) . . ? C3 Fe1 C11 163.2(3) . . ? C7 Fe1 C11 41.0(2) . . ? C9 Fe1 C11 69.1(3) . . ? C10 Fe1 C11 41.2(3) . . ? C1 Fe1 C11 121.5(2) . . ? C2 Fe1 C11 155.9(3) . . ? C4 Fe1 C11 126.8(3) . . ? C5 Fe1 C11 109.3(2) . . ? C5 C1 C2 107.7(6) . . ? C5 C1 Fe1 70.0(3) . . ? C2 C1 Fe1 69.6(3) . . ? C3 C2 C1 107.4(6) . . ? C3 C2 Fe1 69.1(4) . . ? C1 C2 Fe1 69.3(3) . . ? C2 C3 C4 109.2(6) . . ? C2 C3 Fe1 70.6(4) . . ? C4 C3 Fe1 70.5(4) . . ? C3 C4 C5 108.1(6) . . ? C3 C4 Fe1 68.9(4) . . ? C5 C4 Fe1 70.1(3) . . ? C4 C5 C1 107.6(5) . . ? C4 C5 C6 126.9(6) . . ? C1 C5 C6 125.5(5) . . ? C4 C5 Fe1 69.6(3) . . ? C1 C5 Fe1 69.1(3) . . ? C6 C5 Fe1 126.1(4) . . ? C5 C6 Se1 110.6(4) . . ? C8 C7 C11 108.0(6) . . ? C8 C7 Fe1 68.9(4) . . ? C11 C7 Fe1 70.7(3) . . ? C9 C8 C7 109.0(6) . . ? C9 C8 Fe1 70.4(4) . . ? C7 C8 Fe1 69.8(4) . . ? C8 C9 C10 108.4(6) . . ? C8 C9 Fe1 69.5(4) . . ? C10 C9 Fe1 69.5(4) . . ? C9 C10 C11 108.2(6) . . ? C9 C10 Fe1 69.4(4) . . ? C11 C10 Fe1 70.6(4) . . ? C7 C11 C10 106.4(5) . . ? C7 C11 C12 127.2(6) . . ? C10 C11 C12 126.4(6) . . ? C7 C11 Fe1 68.2(3) . . ? C10 C11 Fe1 68.3(3) . . ? C12 C11 Fe1 128.0(4) . . ? C11 C12 Se2 112.2(4) . . ? C17 C13 C14 108.5(6) . . ? C17 C13 Fe2 69.8(4) . . ? C14 C13 Fe2 70.0(3) . . ? C15 C14 C13 107.5(6) . . ? C15 C14 C18 127.3(5) . . ? C13 C14 C18 125.2(6) . . ? C15 C14 Fe2 69.1(3) . . ? C13 C14 Fe2 69.1(3) . . ? C18 C14 Fe2 128.2(4) . . ? C14 C15 C16 108.1(6) . . ? C14 C15 Fe2 70.2(3) . . ? C16 C15 Fe2 68.7(4) . . ? C17 C16 C15 107.9(6) . . ? C17 C16 Fe2 70.3(4) . . ? C15 C16 Fe2 69.7(4) . . ? C16 C17 C13 108.0(5) . . ? C16 C17 Fe2 68.9(4) . . ? C13 C17 Fe2 69.4(3) . . ? C14 C18 Se3 111.1(4) . . ? C20 C19 C23 108.0(6) . . ? C20 C19 Fe2 69.3(4) . . ? C23 C19 Fe2 70.1(3) . . ? C19 C20 C21 107.8(6) . . ? C19 C20 Fe2 69.9(4) . . ? C21 C20 Fe2 70.2(4) . . ? C22 C21 C20 108.3(6) . . ? C22 C21 Fe2 70.3(3) . . ? C20 C21 Fe2 68.8(4) . . ? C21 C22 C23 108.3(6) . . ? C21 C22 Fe2 69.4(4) . . ? C23 C22 Fe2 69.6(3) . . ? C22 C23 C19 107.5(5) . . ? C22 C23 C24 127.1(6) . . ? C19 C23 C24 125.4(6) . . ? C22 C23 Fe2 70.0(3) . . ? C19 C23 Fe2 68.7(3) . . ? C24 C23 Fe2 128.7(4) . . ? C23 C24 Se4 107.7(4) . . ? N1 C25 C26 111.0(5) . . ? N2 C26 C25 111.0(5) . . ? N4 C31 C32 110.1(5) . . ? N3 C32 C31 111.1(5) . . ? Cl3 C37 Cl2 111.5(5) . . ? Cl3 C37 Cl1 109.8(5) . . ? Cl2 C37 Cl1 109.3(5) . . ? Cl18 C42 Cl17 110.2(5) . . ? Cl18 C42 Cl16 110.6(5) . . ? Cl17 C42 Cl16 110.1(5) . . ? Cl14 C41 Cl15 110.4(4) . . ? Cl14 C41 Cl13 110.6(4) . . ? Cl15 C41 Cl13 110.9(4) . . ? Cl8 C39 Cl9 110.9(4) . . ? Cl8 C39 Cl7 110.4(4) . . ? Cl9 C39 Cl7 109.7(5) . . ? Cl5 C38 Cl6 111.7(5) . . ? Cl5 C38 Cl4 110.5(5) . . ? Cl6 C38 Cl4 110.0(5) . . ? Cl10 C40 Cl11 111.1(4) . . ? Cl10 C40 Cl12 109.9(4) . . ? Cl11 C40 Cl12 110.5(4) . . ? C34 N3 C33 109.9(6) . . ? C34 N3 C32 109.6(5) . . ? C33 N3 C32 110.2(5) . . ? C34 N3 Zn2 111.4(4) . . ? C33 N3 Zn2 111.7(4) . . ? C32 N3 Zn2 103.9(4) . . ? C31 N4 C36 109.8(5) . . ? C31 N4 C35 110.0(5) . . ? C36 N4 C35 107.9(6) . . ? C31 N4 Zn2 105.2(4) . . ? C36 N4 Zn2 113.2(4) . . ? C35 N4 Zn2 110.7(4) . . ? C27 N1 C28 108.4(5) . . ? C27 N1 C25 110.8(5) . . ? C28 N1 C25 108.9(5) . . ? C27 N1 Zn1 110.2(4) . . ? C28 N1 Zn1 113.8(4) . . ? C25 N1 Zn1 104.7(4) . . ? C26 N2 C30 109.9(5) . . ? C26 N2 C29 110.7(5) . . ? C30 N2 C29 110.0(5) . . ? C26 N2 Zn1 103.7(4) . . ? C30 N2 Zn1 111.7(4) . . ? C29 N2 Zn1 110.8(4) . . ? _diffrn_measured_fraction_theta_max 0.700 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.484 _refine_diff_density_min -2.298 _refine_diff_density_rms 0.402 data_08030b _database_code_depnum_ccdc_archive 'CCDC 814946' #TrackingRef 'Corrigan-New-J-Chem-2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C169 H157 Ag8 Cl27 Fe8 P4 Se8' _chemical_formula_weight 5210.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.8840(6) _cell_length_b 44.2400(7) _cell_length_c 22.0150(5) _cell_angle_alpha 90.00 _cell_angle_beta 130.4630(10) _cell_angle_gamma 90.00 _cell_volume 22144.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 88895 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10184 _exptl_absorpt_coefficient_mu 2.906 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2745 _exptl_absorpt_correction_T_max 0.5303 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Nonius KappaCCD' _diffrn_measurement_method '\w scans + omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83259 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -57 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 25385 _reflns_number_gt 13578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.1657P)^2^+38.3641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25385 _refine_ls_number_parameters 994 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.1537 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2922 _refine_ls_wR_factor_gt 0.2319 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 0.61410(3) 0.075270(16) 0.44104(5) 0.0488(2) Uani 1 1 d . . . Ag2 Ag 0.51341(3) 0.113127(15) 0.18021(4) 0.0448(2) Uani 1 1 d . . . Ag3 Ag 0.59369(3) 0.171687(16) 0.22575(5) 0.0457(2) Uani 1 1 d . . . Ag4 Ag 0.58766(3) 0.134607(15) 0.34345(4) 0.0433(2) Uani 1 1 d . . . Se1 Se 0.59109(4) 0.07837(2) 0.30328(6) 0.0434(2) Uani 1 1 d . . . Se2 Se 0.46421(4) 0.08548(2) 0.04460(6) 0.0479(3) Uani 1 1 d . . . Se3 Se 0.67661(4) 0.16503(2) 0.37864(6) 0.0439(2) Uani 1 1 d . . . Se4 Se 0.52003(4) 0.170258(19) 0.35201(6) 0.0412(2) Uani 1 1 d . . . P1 P 0.71418(12) 0.05687(6) 0.55212(18) 0.0523(7) Uani 1 1 d . . . P2 P 0.61413(13) 0.18755(6) 0.13752(17) 0.0505(7) Uani 1 1 d . . . Fe1 Fe 0.74541(7) 0.07231(3) 0.28499(10) 0.0538(4) Uani 1 1 d . . . Fe2 Fe 0.50470(6) -0.02046(3) 0.12807(8) 0.0477(4) Uani 1 1 d . . . Fe3 Fe 0.62386(6) 0.27038(3) 0.37375(9) 0.0468(4) Uani 1 1 d . . . Fe4 Fe 0.66845(7) 0.16721(3) 0.64241(9) 0.0554(4) Uani 1 1 d . . . C1 C 0.6785(4) 0.0651(2) 0.2862(6) 0.044(2) Uani 1 1 d . . . C2 C 0.7191(6) 0.0404(2) 0.3240(8) 0.065(3) Uani 1 1 d . . . H2A H 0.7402 0.0340 0.3776 0.078 Uiso 1 1 calc R . . C3 C 0.7226(7) 0.0272(3) 0.2694(11) 0.082(4) Uani 1 1 d . . . H3A H 0.7469 0.0107 0.2791 0.098 Uiso 1 1 calc R . . C4 C 0.6833(7) 0.0432(4) 0.1974(10) 0.091(5) Uani 1 1 d . . . H4A H 0.6760 0.0388 0.1494 0.109 Uiso 1 1 calc R . . C5 C 0.6558(5) 0.0671(3) 0.2066(7) 0.060(3) Uani 1 1 d . . . H5A H 0.6280 0.0813 0.1674 0.073 Uiso 1 1 calc R . . C6 C 0.7900(5) 0.1092(3) 0.3545(8) 0.068(3) Uani 1 1 d . . . H6A H 0.7831 0.1197 0.3853 0.082 Uiso 1 1 calc R . . C7 C 0.8267(5) 0.0857(3) 0.3796(8) 0.076(4) Uani 1 1 d . . . H7A H 0.8503 0.0770 0.4314 0.092 Uiso 1 1 calc R . . C8 C 0.8248(5) 0.0758(3) 0.3158(10) 0.074(4) Uani 1 1 d . . . H8A H 0.8459 0.0594 0.3174 0.089 Uiso 1 1 calc R . . C9 C 0.7868(7) 0.0946(3) 0.2522(10) 0.083(4) Uani 1 1 d . . . H9A H 0.7776 0.0938 0.2021 0.100 Uiso 1 1 calc R . . C10 C 0.7635(6) 0.1155(3) 0.2748(9) 0.071(4) Uani 1 1 d . . . H10A H 0.7353 0.1308 0.2420 0.085 Uiso 1 1 calc R . . C11 C 0.6663(5) 0.0868(3) 0.3254(7) 0.059(3) Uani 1 1 d . . . H11A H 0.6645 0.1075 0.3067 0.071 Uiso 1 1 calc R . . H11B H 0.6992 0.0862 0.3838 0.071 Uiso 1 1 calc R . . C12 C 0.4725(5) 0.0210(2) 0.0769(6) 0.052(3) Uani 1 1 d . . . C13 C 0.4583(5) 0.0136(3) 0.1272(7) 0.058(3) Uani 1 1 d . . . H13A H 0.4701 0.0246 0.1726 0.069 Uiso 1 1 calc R . . C14 C 0.4232(6) -0.0135(3) 0.0953(8) 0.074(4) Uani 1 1 d . . . H14A H 0.4075 -0.0236 0.1159 0.089 Uiso 1 1 calc R . . C15 C 0.4167(5) -0.0217(2) 0.0325(7) 0.055(3) Uani 1 1 d . . . H15A H 0.3956 -0.0391 0.0011 0.066 Uiso 1 1 calc R . . C16 C 0.4458(4) -0.0010(2) 0.0175(6) 0.048(2) Uani 1 1 d . . . H16A H 0.4467 -0.0021 -0.0249 0.057 Uiso 1 1 calc R . . C17 C 0.5914(5) -0.0200(3) 0.1806(7) 0.065(3) Uani 1 1 d . . . H17A H 0.6099 -0.0048 0.1732 0.078 Uiso 1 1 calc R . . C18 C 0.5857(5) -0.0199(2) 0.2389(6) 0.056(3) Uani 1 1 d . . . H18A H 0.5996 -0.0046 0.2778 0.067 Uiso 1 1 calc R . . C19 C 0.5565(5) -0.0459(3) 0.2305(6) 0.062(3) Uani 1 1 d . . . H19A H 0.5472 -0.0513 0.2630 0.075 Uiso 1 1 calc R . . C20 C 0.5427(5) -0.0626(3) 0.1674(7) 0.063(3) Uani 1 1 d . . . H20A H 0.5223 -0.0813 0.1486 0.076 Uiso 1 1 calc R . . C21 C 0.5652(5) -0.0463(3) 0.1352(7) 0.060(3) Uani 1 1 d . . . H21A H 0.5626 -0.0523 0.0916 0.072 Uiso 1 1 calc R . . C22 C 0.5097(4) 0.0465(2) 0.0899(7) 0.059(3) Uani 1 1 d . . . H22A H 0.5267 0.0418 0.0645 0.071 Uiso 1 1 calc R . . H22B H 0.5426 0.0490 0.1479 0.071 Uiso 1 1 calc R . . C23 C 0.6502(4) 0.2292(2) 0.3636(6) 0.043(2) Uani 1 1 d . . . C24 C 0.5925(5) 0.2363(2) 0.2931(6) 0.054(3) Uani 1 1 d . . . H24A H 0.5584 0.2245 0.2708 0.065 Uiso 1 1 calc R . . C25 C 0.5941(5) 0.2641(2) 0.2609(7) 0.055(3) Uani 1 1 d . . . H25A H 0.5617 0.2742 0.2142 0.066 Uiso 1 1 calc R . . C26 C 0.6542(5) 0.2735(2) 0.3131(7) 0.059(3) Uani 1 1 d . . . H26A H 0.6689 0.2912 0.3068 0.071 Uiso 1 1 calc R . . C27 C 0.6878(4) 0.2525(2) 0.3749(6) 0.049(2) Uani 1 1 d . . . H27A H 0.7290 0.2537 0.4177 0.059 Uiso 1 1 calc R . . C28 C 0.6393(5) 0.2705(2) 0.4779(7) 0.056(3) Uani 1 1 d . . . H28A H 0.6632 0.2563 0.5199 0.068 Uiso 1 1 calc R . . C29 C 0.5807(5) 0.2674(3) 0.4161(7) 0.065(3) Uani 1 1 d . . . H29A H 0.5567 0.2510 0.4078 0.079 Uiso 1 1 calc R . . C30 C 0.5612(5) 0.2938(2) 0.3648(7) 0.054(3) Uani 1 1 d . . . H30A H 0.5226 0.2979 0.3166 0.065 Uiso 1 1 calc R . . C31 C 0.6109(5) 0.3117(2) 0.4011(7) 0.059(3) Uani 1 1 d . . . H31A H 0.6116 0.3307 0.3814 0.070 Uiso 1 1 calc R . . C32 C 0.6593(5) 0.2979(2) 0.4701(7) 0.060(3) Uani 1 1 d . . . H32A H 0.6984 0.3054 0.5055 0.072 Uiso 1 1 calc R . . C33 C 0.6657(5) 0.2031(2) 0.4158(6) 0.051(3) Uani 1 1 d . . . H33A H 0.6342 0.2000 0.4185 0.061 Uiso 1 1 calc R . . H33B H 0.7025 0.2076 0.4704 0.061 Uiso 1 1 calc R . . C34 C 0.6158(4) 0.1743(2) 0.5221(6) 0.043(2) Uani 1 1 d . . . C35 C 0.6624(5) 0.1538(3) 0.5490(7) 0.059(3) Uani 1 1 d . . . H35A H 0.6569 0.1336 0.5305 0.071 Uiso 1 1 calc R . . C36 C 0.7180(6) 0.1676(3) 0.6071(8) 0.070(3) Uani 1 1 d . . . H36A H 0.7556 0.1589 0.6335 0.084 Uiso 1 1 calc R . . C37 C 0.7052(5) 0.1984(3) 0.6177(7) 0.059(3) Uani 1 1 d . . . H37A H 0.7332 0.2132 0.6540 0.070 Uiso 1 1 calc R . . C38 C 0.6439(5) 0.2017(2) 0.5643(6) 0.055(3) Uani 1 1 d . . . H38A H 0.6239 0.2198 0.5572 0.066 Uiso 1 1 calc R . . C39 C 0.6511(7) 0.1303(3) 0.6809(8) 0.082(4) Uani 1 1 d . . . H39A H 0.6390 0.1109 0.6567 0.099 Uiso 1 1 calc R . . C40 C 0.7104(7) 0.1391(3) 0.7404(8) 0.089(5) Uani 1 1 d . . . H40A H 0.7441 0.1270 0.7622 0.107 Uiso 1 1 calc R . . C41 C 0.7105(8) 0.1695(4) 0.7616(8) 0.101(6) Uani 1 1 d . . . H41A H 0.7436 0.1817 0.8001 0.122 Uiso 1 1 calc R . . C42 C 0.6528(9) 0.1770(4) 0.7147(10) 0.099(5) Uani 1 1 d . . . H42A H 0.6401 0.1964 0.7166 0.118 Uiso 1 1 calc R . . C43 C 0.6125(7) 0.1537(3) 0.6622(8) 0.080(4) Uani 1 1 d . . . H43A H 0.5707 0.1540 0.6247 0.096 Uiso 1 1 calc R . . C44 C 0.5537(4) 0.1683(2) 0.4658(6) 0.048(2) Uani 1 1 d . . . H44A H 0.5332 0.1832 0.4738 0.057 Uiso 1 1 calc R . . H44B H 0.5463 0.1479 0.4764 0.057 Uiso 1 1 calc R . . C45 C 0.7731(4) 0.0738(2) 0.5585(6) 0.050(2) Uani 1 1 d . . . C46 C 0.8231(5) 0.0582(3) 0.5848(8) 0.067(3) Uani 1 1 d . . . H46A H 0.8283 0.0378 0.6012 0.080 Uiso 1 1 calc R . . C47 C 0.8655(5) 0.0724(3) 0.5872(9) 0.072(4) Uani 1 1 d . . . H47A H 0.8989 0.0614 0.6030 0.086 Uiso 1 1 calc R . . C48 C 0.8596(5) 0.1016(3) 0.5673(7) 0.067(3) Uani 1 1 d . . . H48A H 0.8895 0.1113 0.5707 0.080 Uiso 1 1 calc R . . C49 C 0.8084(5) 0.1187(3) 0.5408(7) 0.069(4) Uani 1 1 d . . . H49A H 0.8044 0.1394 0.5266 0.083 Uiso 1 1 calc R . . C50 C 0.7662(4) 0.1046(2) 0.5366(6) 0.056(3) Uani 1 1 d . . . H50A H 0.7321 0.1153 0.5189 0.068 Uiso 1 1 calc R . . C51 C 0.7234(4) 0.0168(2) 0.5442(7) 0.054(3) Uani 1 1 d . . . C52 C 0.7063(5) 0.0068(2) 0.4711(7) 0.058(3) Uani 1 1 d . . . H52A H 0.6896 0.0206 0.4283 0.069 Uiso 1 1 calc R . . C53 C 0.7139(5) -0.0234(3) 0.4614(8) 0.072(4) Uani 1 1 d . . . H53A H 0.7025 -0.0303 0.4122 0.086 Uiso 1 1 calc R . . C54 C 0.7387(6) -0.0437(3) 0.5255(11) 0.095(5) Uani 1 1 d . . . H54A H 0.7463 -0.0641 0.5208 0.114 Uiso 1 1 calc R . . C55 C 0.7523(6) -0.0337(3) 0.5966(10) 0.087(4) Uani 1 1 d . . . H55A H 0.7661 -0.0477 0.6384 0.104 Uiso 1 1 calc R . . C56 C 0.7454(5) -0.0034(3) 0.6055(8) 0.067(3) Uani 1 1 d . . . H56A H 0.7558 0.0034 0.6542 0.081 Uiso 1 1 calc R . . C57 C 0.7394(5) 0.0602(2) 0.6533(7) 0.059(3) Uani 1 1 d . . . C58 C 0.7003(5) 0.0544(2) 0.6654(7) 0.057(3) Uani 1 1 d . . . H58A H 0.6606 0.0497 0.6210 0.069 Uiso 1 1 calc R . . C59 C 0.7178(5) 0.0553(3) 0.7408(7) 0.068(3) Uani 1 1 d . . . H59A H 0.6911 0.0508 0.7491 0.082 Uiso 1 1 calc R . . C60 C 0.7763(6) 0.0631(3) 0.8046(7) 0.077(4) Uani 1 1 d . . . H60A H 0.7894 0.0634 0.8571 0.092 Uiso 1 1 calc R . . C61 C 0.8159(6) 0.0705(4) 0.7932(9) 0.098(5) Uani 1 1 d . . . H61A H 0.8551 0.0763 0.8372 0.118 Uiso 1 1 calc R . . C62 C 0.7979(6) 0.0692(3) 0.7200(8) 0.081(4) Uani 1 1 d . . . H62A H 0.8245 0.0743 0.7119 0.098 Uiso 1 1 calc R . . C63 C 0.6822(5) 0.2085(2) 0.1882(7) 0.057(3) Uani 1 1 d . . . C64 C 0.7280(5) 0.2030(3) 0.2666(7) 0.062(3) Uani 1 1 d . . . H64A H 0.7234 0.1886 0.2943 0.074 Uiso 1 1 calc R . . C65 C 0.7802(6) 0.2176(4) 0.3063(9) 0.087(5) Uani 1 1 d . . . H65A H 0.8120 0.2128 0.3606 0.105 Uiso 1 1 calc R . . C66 C 0.7871(7) 0.2393(4) 0.2682(10) 0.093(5) Uani 1 1 d . . . H66A H 0.8237 0.2495 0.2958 0.112 Uiso 1 1 calc R . . C67 C 0.7424(7) 0.2458(3) 0.1929(10) 0.093(5) Uani 1 1 d . . . H67A H 0.7463 0.2614 0.1669 0.111 Uiso 1 1 calc R . . C68 C 0.6910(5) 0.2305(3) 0.1521(8) 0.067(3) Uani 1 1 d . . . H68A H 0.6602 0.2349 0.0972 0.081 Uiso 1 1 calc R . . C69 C 0.5594(4) 0.2117(2) 0.0537(7) 0.051(3) Uani 1 1 d . . . C70 C 0.5369(6) 0.2360(3) 0.0663(8) 0.064(3) Uani 1 1 d . . . H70A H 0.5508 0.2397 0.1185 0.077 Uiso 1 1 calc R . . C71 C 0.4961(6) 0.2544(3) 0.0065(9) 0.073(4) Uani 1 1 d . . . H71A H 0.4819 0.2708 0.0176 0.087 Uiso 1 1 calc R . . C72 C 0.4751(6) 0.2503(3) -0.0674(9) 0.078(4) Uani 1 1 d . . . H72A H 0.4459 0.2636 -0.1086 0.093 Uiso 1 1 calc R . . C73 C 0.4958(6) 0.2263(3) -0.0851(8) 0.084(4) Uani 1 1 d . . . H73A H 0.4816 0.2234 -0.1377 0.101 Uiso 1 1 calc R . . C74 C 0.5365(6) 0.2071(3) -0.0252(7) 0.068(3) Uani 1 1 d . . . H74A H 0.5498 0.1904 -0.0368 0.082 Uiso 1 1 calc R . . C75 C 0.6199(5) 0.1567(2) 0.0880(6) 0.053(3) Uani 1 1 d . . . C76 C 0.6626(6) 0.1547(3) 0.0805(8) 0.071(4) Uani 1 1 d . . . H76A H 0.6912 0.1702 0.1021 0.085 Uiso 1 1 calc R . . C77 C 0.6640(6) 0.1303(3) 0.0419(9) 0.077(4) Uani 1 1 d . . . H77A H 0.6924 0.1298 0.0352 0.093 Uiso 1 1 calc R . . C78 C 0.6253(7) 0.1074(3) 0.0139(8) 0.077(4) Uani 1 1 d . . . H78A H 0.6272 0.0907 -0.0116 0.093 Uiso 1 1 calc R . . C79 C 0.5818(6) 0.1076(3) 0.0218(7) 0.068(3) Uani 1 1 d . . . H79A H 0.5541 0.0917 0.0015 0.081 Uiso 1 1 calc R . . C80 C 0.5813(5) 0.1321(2) 0.0602(6) 0.054(3) Uani 1 1 d . . . H80A H 0.5537 0.1324 0.0681 0.064 Uiso 1 1 calc R . . C1S C 0.8979(13) 0.1750(5) 0.9482(15) 0.28(3) Uani 1 1 d D . . Cl1 Cl 0.8819(12) 0.1924(6) 0.9985(14) 0.548(18) Uani 1 1 d D . . Cl2 Cl 0.8699(7) 0.1398(4) 0.9313(13) 0.417(11) Uani 1 1 d D . . Cl3 Cl 0.8757(8) 0.1901(4) 0.8644(10) 0.395(9) Uani 1 1 d D . . C2S C 0.8936(16) -0.0169(6) 0.467(3) 0.19(2) Uiso 0.50 1 d PD . . Cl4 Cl 0.9148(12) 0.0183(7) 0.4775(17) 0.338(14) Uiso 0.50 1 d PD . . Cl5 Cl 0.9321(9) -0.0485(5) 0.5149(12) 0.235(8) Uiso 0.50 1 d PD . . Cl6 Cl 0.8506(6) -0.0073(3) 0.4875(8) 0.158(4) Uiso 0.50 1 d PD . . C3S C 0.7029(7) -0.1270(3) 0.3792(10) 0.167(11) Uani 1 1 d D . . Cl7 Cl 0.7713(5) -0.1130(3) 0.4544(7) 0.273(5) Uani 1 1 d D . . Cl8 Cl 0.6932(6) -0.15931(19) 0.4106(6) 0.267(6) Uani 1 1 d D . . Cl9 Cl 0.6542(4) -0.10005(17) 0.3510(4) 0.225(4) Uani 1 1 d D . . C4S C 0.9164(7) 0.1433(3) 0.4110(9) 0.120(7) Uani 1 1 d D . . Cl10 Cl 0.9312(8) 0.1663(2) 0.3675(10) 0.407(11) Uani 1 1 d D . . Cl11 Cl 0.9155(3) 0.16233(13) 0.4768(4) 0.151(2) Uani 1 1 d D . . Cl12 Cl 0.9684(3) 0.1166(2) 0.4520(8) 0.331(9) Uani 1 1 d D . . C5S C 0.9378(13) 0.1133(6) 0.769(2) 0.18(2) Uiso 0.50 1 d PD . . Cl13 Cl 0.8990(9) 0.1370(5) 0.7766(13) 0.237(8) Uiso 0.50 1 d PD . . Cl14 Cl 0.9892(8) 0.1298(4) 0.7712(12) 0.211(7) Uiso 0.50 1 d PD . . Cl15 Cl 0.9658(7) 0.0840(4) 0.8315(10) 0.190(6) Uiso 0.50 1 d PD . . C6S C 0.4800 0.1556 -0.2617 0.250 Uiso 0.50 1 d P A -1 Cl16 Cl 0.5085 0.1494 -0.3092 0.217(7) Uiso 0.50 1 d P A -1 Cl17 Cl 0.5225 0.1424 -0.1690 0.170(5) Uiso 0.50 1 d P A -1 Cl18 Cl 0.4696 0.1942 -0.2773 0.264(10) Uiso 0.50 1 d P A -1 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 0.0501(4) 0.0406(4) 0.0473(5) 0.0022(3) 0.0279(4) -0.0019(3) Ag2 0.0534(4) 0.0338(4) 0.0417(4) -0.0016(3) 0.0284(4) 0.0026(3) Ag3 0.0544(4) 0.0409(4) 0.0401(4) -0.0032(3) 0.0299(4) -0.0033(3) Ag4 0.0511(4) 0.0344(4) 0.0421(4) -0.0031(3) 0.0291(4) -0.0028(3) Se1 0.0460(5) 0.0334(5) 0.0441(6) -0.0007(4) 0.0263(5) 0.0004(4) Se2 0.0538(6) 0.0397(5) 0.0455(6) -0.0090(4) 0.0301(5) -0.0013(4) Se3 0.0488(5) 0.0385(5) 0.0406(5) -0.0055(4) 0.0272(5) -0.0074(4) Se4 0.0507(5) 0.0331(4) 0.0387(5) 0.0000(4) 0.0285(5) -0.0001(4) P1 0.0472(14) 0.0486(15) 0.0488(16) 0.0080(12) 0.0257(13) 0.0009(11) P2 0.0620(16) 0.0476(14) 0.0446(16) -0.0056(11) 0.0357(14) -0.0087(12) Fe1 0.0571(9) 0.0516(9) 0.0545(10) -0.0134(7) 0.0371(8) -0.0082(7) Fe2 0.0521(8) 0.0461(8) 0.0379(8) -0.0010(6) 0.0261(7) 0.0043(6) Fe3 0.0502(8) 0.0379(7) 0.0486(9) -0.0082(6) 0.0304(7) -0.0084(6) Fe4 0.0621(9) 0.0491(8) 0.0385(8) -0.0012(6) 0.0253(8) -0.0022(7) C1 0.041(5) 0.045(5) 0.040(6) -0.004(4) 0.024(5) 0.000(4) C2 0.088(8) 0.052(6) 0.081(9) -0.004(6) 0.067(8) -0.002(6) C3 0.101(10) 0.049(7) 0.127(14) -0.018(8) 0.088(11) -0.013(7) C4 0.099(10) 0.099(11) 0.090(11) -0.060(9) 0.068(10) -0.063(9) C5 0.057(6) 0.079(8) 0.043(6) -0.011(6) 0.031(6) -0.006(6) C6 0.064(7) 0.070(8) 0.063(8) -0.029(6) 0.038(7) -0.020(6) C7 0.060(7) 0.098(10) 0.050(8) 0.004(7) 0.026(6) -0.013(7) C8 0.056(7) 0.072(8) 0.099(11) -0.022(8) 0.052(8) -0.006(6) C9 0.095(10) 0.092(10) 0.102(12) -0.033(9) 0.081(10) -0.029(8) C10 0.071(8) 0.051(7) 0.080(10) -0.014(6) 0.045(7) -0.018(6) C11 0.068(7) 0.058(6) 0.060(7) -0.019(5) 0.046(6) -0.012(5) C12 0.062(6) 0.040(5) 0.046(6) -0.005(4) 0.032(5) 0.002(5) C13 0.076(7) 0.060(7) 0.049(6) 0.002(5) 0.046(6) 0.020(6) C14 0.076(8) 0.090(9) 0.072(9) 0.035(7) 0.055(8) 0.021(7) C15 0.053(6) 0.049(6) 0.049(7) 0.010(5) 0.027(5) 0.003(5) C16 0.059(6) 0.042(5) 0.030(5) 0.000(4) 0.023(5) 0.007(4) C17 0.060(7) 0.065(7) 0.054(7) 0.014(6) 0.030(6) 0.006(6) C18 0.061(6) 0.054(6) 0.034(6) -0.008(4) 0.022(5) 0.012(5) C19 0.071(7) 0.064(7) 0.037(6) 0.013(5) 0.028(6) 0.014(6) C20 0.057(6) 0.052(6) 0.053(7) -0.006(5) 0.023(6) 0.009(5) C21 0.063(7) 0.062(7) 0.059(7) -0.005(6) 0.041(6) 0.017(5) C22 0.049(6) 0.051(6) 0.060(7) -0.015(5) 0.027(6) -0.003(5) C23 0.051(5) 0.040(5) 0.040(5) -0.004(4) 0.031(5) -0.003(4) C24 0.055(6) 0.050(6) 0.050(7) -0.015(5) 0.031(5) -0.006(5) C25 0.063(7) 0.054(6) 0.046(6) 0.006(5) 0.035(6) 0.019(5) C26 0.084(8) 0.052(6) 0.068(8) 0.009(5) 0.061(7) 0.002(6) C27 0.052(6) 0.045(5) 0.054(6) -0.004(5) 0.036(5) -0.011(4) C28 0.072(7) 0.049(6) 0.068(8) -0.017(5) 0.054(7) -0.010(5) C29 0.054(6) 0.072(8) 0.061(8) -0.021(6) 0.034(6) -0.013(6) C30 0.054(6) 0.052(6) 0.057(7) -0.010(5) 0.037(6) -0.003(5) C31 0.074(7) 0.039(5) 0.052(7) -0.009(5) 0.036(6) -0.001(5) C32 0.065(7) 0.043(6) 0.053(7) -0.013(5) 0.030(6) -0.007(5) C33 0.063(6) 0.038(5) 0.052(6) -0.009(4) 0.037(6) -0.010(4) C34 0.048(5) 0.039(5) 0.043(6) -0.007(4) 0.031(5) -0.001(4) C35 0.056(6) 0.061(7) 0.046(7) -0.009(5) 0.027(6) 0.006(5) C36 0.065(7) 0.071(8) 0.065(8) -0.014(6) 0.038(7) -0.008(6) C37 0.072(7) 0.057(6) 0.059(7) -0.013(5) 0.048(6) -0.014(5) C38 0.059(6) 0.042(5) 0.047(6) 0.004(4) 0.027(5) -0.003(5) C39 0.112(11) 0.055(7) 0.063(9) 0.000(6) 0.049(9) -0.024(7) C40 0.120(12) 0.066(8) 0.042(7) 0.022(6) 0.035(8) 0.012(8) C41 0.121(14) 0.109(13) 0.040(8) 0.009(8) 0.037(9) -0.023(10) C42 0.157(17) 0.086(10) 0.073(11) 0.009(9) 0.084(12) -0.001(11) C43 0.112(11) 0.072(8) 0.062(9) 0.010(7) 0.059(9) -0.010(8) C44 0.054(6) 0.043(5) 0.043(6) -0.003(4) 0.031(5) -0.006(4) C45 0.045(5) 0.050(6) 0.039(6) -0.004(4) 0.021(5) -0.008(4) C46 0.046(6) 0.056(7) 0.080(9) 0.015(6) 0.033(6) 0.006(5) C47 0.056(7) 0.056(7) 0.108(11) 0.001(7) 0.056(8) -0.001(5) C48 0.056(7) 0.082(9) 0.066(8) -0.016(6) 0.040(7) -0.028(6) C49 0.067(7) 0.049(6) 0.058(8) 0.003(5) 0.026(6) -0.017(6) C50 0.043(5) 0.044(5) 0.053(7) -0.001(5) 0.019(5) -0.008(4) C51 0.043(5) 0.045(5) 0.059(7) 0.011(5) 0.026(5) 0.001(4) C52 0.055(6) 0.050(6) 0.057(7) 0.013(5) 0.031(6) 0.004(5) C53 0.060(7) 0.065(8) 0.080(9) 0.000(7) 0.041(7) -0.008(6) C54 0.066(8) 0.058(8) 0.124(15) 0.018(9) 0.045(9) 0.003(6) C55 0.099(11) 0.061(8) 0.083(11) 0.017(7) 0.051(9) 0.007(7) C56 0.067(7) 0.058(7) 0.071(9) 0.007(6) 0.042(7) 0.004(6) C57 0.054(6) 0.054(6) 0.054(7) 0.014(5) 0.029(6) 0.013(5) C58 0.047(6) 0.057(6) 0.049(7) 0.005(5) 0.023(5) 0.000(5) C59 0.070(8) 0.068(7) 0.054(8) 0.005(6) 0.035(7) -0.004(6) C60 0.072(8) 0.088(9) 0.034(6) 0.007(6) 0.018(6) -0.003(7) C61 0.060(8) 0.166(16) 0.048(8) -0.001(9) 0.026(7) -0.015(9) C62 0.069(8) 0.116(11) 0.046(7) -0.006(7) 0.031(7) -0.026(7) C63 0.074(7) 0.055(6) 0.056(7) -0.015(5) 0.048(6) -0.018(5) C64 0.070(7) 0.075(8) 0.054(7) -0.015(6) 0.046(7) -0.026(6) C65 0.083(9) 0.111(12) 0.063(9) -0.051(8) 0.045(8) -0.038(8) C66 0.098(11) 0.095(11) 0.087(12) -0.052(9) 0.061(10) -0.053(9) C67 0.102(11) 0.071(9) 0.096(12) -0.015(8) 0.060(10) -0.035(8) C68 0.069(7) 0.065(7) 0.075(9) -0.003(6) 0.050(7) -0.013(6) C69 0.053(6) 0.045(5) 0.056(7) -0.005(5) 0.036(5) -0.010(4) C70 0.090(9) 0.056(7) 0.062(8) -0.004(6) 0.056(7) -0.003(6) C71 0.103(10) 0.046(6) 0.086(10) 0.002(6) 0.069(9) 0.005(6) C72 0.075(8) 0.073(9) 0.080(10) 0.035(7) 0.048(8) 0.018(7) C73 0.092(10) 0.085(9) 0.050(8) 0.013(7) 0.035(7) 0.007(8) C74 0.083(8) 0.073(8) 0.056(8) -0.007(6) 0.048(7) 0.001(6) C75 0.076(7) 0.046(5) 0.049(6) -0.012(5) 0.047(6) -0.017(5) C76 0.107(10) 0.062(7) 0.074(9) -0.007(6) 0.072(9) -0.021(7) C77 0.094(10) 0.081(9) 0.093(11) -0.010(8) 0.076(9) -0.008(8) C78 0.122(11) 0.058(7) 0.077(9) -0.019(6) 0.075(9) -0.010(7) C79 0.086(9) 0.060(7) 0.055(7) -0.007(6) 0.044(7) 0.000(6) C80 0.059(6) 0.054(6) 0.050(6) -0.005(5) 0.036(6) -0.006(5) C1S 0.23(3) 0.29(4) 0.24(4) 0.13(4) 0.11(3) -0.09(3) Cl1 0.66(4) 0.56(4) 0.42(3) -0.15(3) 0.35(3) -0.01(3) Cl2 0.300(16) 0.41(2) 0.54(3) 0.15(2) 0.274(19) 0.050(15) Cl3 0.44(2) 0.327(17) 0.36(2) -0.067(15) 0.234(19) -0.131(17) C3S 0.32(4) 0.102(14) 0.117(17) 0.014(12) 0.16(2) 0.020(19) Cl7 0.226(10) 0.320(14) 0.257(12) -0.028(10) 0.150(9) 0.079(9) Cl8 0.512(18) 0.181(7) 0.233(9) 0.060(7) 0.297(12) 0.098(9) Cl9 0.243(8) 0.162(6) 0.131(5) -0.005(4) 0.060(5) 0.107(6) C4S 0.121(14) 0.111(13) 0.18(2) -0.024(13) 0.118(15) -0.025(11) Cl10 0.82(3) 0.254(11) 0.57(2) -0.221(14) 0.64(3) -0.289(16) Cl11 0.168(5) 0.125(4) 0.175(6) -0.071(4) 0.117(5) -0.052(4) Cl12 0.128(5) 0.303(12) 0.447(17) -0.241(12) 0.136(8) -0.040(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.469(3) . ? Ag1 Se2 2.5963(14) 2_655 ? Ag1 Se1 2.6423(14) . ? Ag1 Ag4 3.1508(10) . ? Ag1 Ag2 3.3539(10) 2_655 ? Ag2 Se2 2.6217(12) . ? Ag2 Se1 2.6327(12) . ? Ag2 Se4 2.6401(11) 2_655 ? Ag2 Ag4 2.8733(11) 2_655 ? Ag2 Ag4 2.8968(10) . ? Ag2 Ag3 3.2171(10) . ? Ag2 Ag1 3.3539(10) 2_655 ? Ag3 P2 2.486(3) . ? Ag3 Se3 2.5943(12) . ? Ag3 Se4 2.6330(12) 2_655 ? Ag3 Ag4 3.1690(11) . ? Ag4 Se3 2.6086(12) . ? Ag4 Se1 2.6645(11) . ? Ag4 Se4 2.6650(12) . ? Ag4 Ag2 2.8733(11) 2_655 ? Se1 C11 2.001(11) . ? Se2 C22 2.014(10) . ? Se2 Ag1 2.5963(14) 2_655 ? Se3 C33 1.987(9) . ? Se4 C44 2.007(10) . ? Se4 Ag3 2.6330(12) 2_655 ? Se4 Ag2 2.6401(11) 2_655 ? P1 C51 1.820(11) . ? P1 C45 1.833(11) . ? P1 C57 1.836(13) . ? P2 C63 1.815(11) . ? P2 C69 1.818(11) . ? P2 C75 1.824(11) . ? Fe1 C8 2.006(12) . ? Fe1 C7 2.006(12) . ? Fe1 C6 2.033(11) . ? Fe1 C10 2.037(12) . ? Fe1 C1 2.043(10) . ? Fe1 C4 2.044(11) . ? Fe1 C9 2.044(14) . ? Fe1 C5 2.051(11) . ? Fe1 C2 2.056(12) . ? Fe1 C3 2.062(12) . ? Fe2 C18 2.036(10) . ? Fe2 C12 2.037(10) . ? Fe2 C13 2.039(10) . ? Fe2 C17 2.039(12) . ? Fe2 C15 2.040(10) . ? Fe2 C16 2.051(9) . ? Fe2 C19 2.052(10) . ? Fe2 C21 2.056(10) . ? Fe2 C20 2.058(11) . ? Fe2 C14 2.065(12) . ? Fe3 C28 2.024(12) . ? Fe3 C29 2.028(13) . ? Fe3 C30 2.034(10) . ? Fe3 C24 2.037(10) . ? Fe3 C31 2.040(10) . ? Fe3 C25 2.043(11) . ? Fe3 C32 2.047(11) . ? Fe3 C26 2.048(11) . ? Fe3 C27 2.051(10) . ? Fe3 C23 2.055(9) . ? Fe4 C42 1.976(16) . ? Fe4 C35 2.032(12) . ? Fe4 C34 2.044(10) . ? Fe4 C37 2.044(11) . ? Fe4 C38 2.047(10) . ? Fe4 C41 2.049(14) . ? Fe4 C39 2.056(12) . ? Fe4 C40 2.064(11) . ? Fe4 C43 2.071(15) . ? Fe4 C36 2.072(14) . ? C1 C5 1.411(15) . ? C1 C2 1.430(15) . ? C1 C11 1.488(14) . ? C2 C3 1.401(18) . ? C3 C4 1.40(2) . ? C4 C5 1.433(19) . ? C6 C7 1.341(18) . ? C6 C10 1.408(18) . ? C7 C8 1.437(19) . ? C8 C9 1.37(2) . ? C9 C10 1.426(18) . ? C12 C16 1.393(13) . ? C12 C13 1.455(15) . ? C12 C22 1.477(15) . ? C13 C14 1.438(18) . ? C14 C15 1.317(16) . ? C15 C16 1.443(15) . ? C17 C21 1.394(16) . ? C17 C18 1.401(16) . ? C18 C19 1.378(16) . ? C19 C20 1.381(16) . ? C20 C21 1.444(17) . ? C23 C24 1.416(14) . ? C23 C27 1.423(13) . ? C23 C33 1.476(13) . ? C24 C25 1.438(15) . ? C25 C26 1.427(16) . ? C26 C27 1.396(15) . ? C28 C29 1.357(15) . ? C28 C32 1.410(15) . ? C29 C30 1.458(16) . ? C30 C31 1.390(14) . ? C31 C32 1.387(15) . ? C34 C38 1.426(13) . ? C34 C35 1.427(14) . ? C34 C44 1.436(13) . ? C35 C36 1.419(16) . ? C36 C37 1.472(16) . ? C37 C38 1.401(15) . ? C39 C43 1.40(2) . ? C39 C40 1.413(19) . ? C40 C41 1.42(2) . ? C41 C42 1.36(2) . ? C42 C43 1.43(2) . ? C45 C46 1.385(14) . ? C45 C50 1.415(14) . ? C46 C47 1.382(15) . ? C47 C48 1.338(16) . ? C48 C49 1.448(17) . ? C49 C50 1.354(15) . ? C51 C56 1.379(15) . ? C51 C52 1.407(16) . ? C52 C53 1.395(16) . ? C53 C54 1.410(19) . ? C54 C55 1.41(2) . ? C55 C56 1.390(17) . ? C57 C58 1.380(16) . ? C57 C62 1.427(16) . ? C58 C59 1.380(16) . ? C59 C60 1.398(16) . ? C60 C61 1.399(19) . ? C61 C62 1.329(18) . ? C63 C64 1.358(16) . ? C63 C68 1.385(16) . ? C64 C65 1.357(16) . ? C65 C66 1.38(2) . ? C66 C67 1.32(2) . ? C67 C68 1.353(17) . ? C69 C70 1.388(15) . ? C69 C74 1.408(15) . ? C70 C71 1.342(17) . ? C71 C72 1.321(18) . ? C72 C73 1.407(19) . ? C73 C74 1.361(17) . ? C75 C76 1.393(16) . ? C75 C80 1.401(14) . ? C76 C77 1.392(17) . ? C77 C78 1.351(17) . ? C78 C79 1.420(18) . ? C79 C80 1.379(15) . ? C1S Cl3 1.643(14) . ? C1S Cl1 1.657(15) . ? C1S Cl2 1.690(14) . ? C2S Cl4 1.642(15) . ? C2S Cl6 1.672(15) . ? C2S Cl5 1.678(15) . ? Cl4 Cl6 2.36(3) . ? C3S Cl9 1.659(13) . ? C3S Cl8 1.692(12) . ? C3S Cl7 1.706(13) . ? C4S Cl10 1.642(12) . ? C4S Cl12 1.676(12) . ? C4S Cl11 1.691(12) . ? C5S Cl13 1.655(15) . ? C5S Cl14 1.670(15) . ? C5S Cl15 1.670(15) . ? Cl14 Cl14 1.44(3) 2_756 ? C6S Cl17 1.6596 . ? C6S Cl18 1.7302 . ? C6S Cl16 1.7462 . ? 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 P1 Ag1 Se2 123.02(9) . 2_655 ? P1 Ag1 Se1 113.56(8) . . ? Se2 Ag1 Se1 123.16(4) 2_655 . ? P1 Ag1 Ag4 123.82(7) . . ? Se2 Ag1 Ag4 95.23(3) 2_655 . ? Se1 Ag1 Ag4 53.90(3) . . ? P1 Ag1 Ag2 166.74(8) . 2_655 ? Se2 Ag1 Ag2 50.34(3) 2_655 2_655 ? Se1 Ag1 Ag2 75.27(3) . 2_655 ? Ag4 Ag1 Ag2 52.31(2) . 2_655 ? Se2 Ag2 Se1 111.58(4) . . ? Se2 Ag2 Se4 107.81(4) . 2_655 ? Se1 Ag2 Se4 139.72(4) . 2_655 ? Se2 Ag2 Ag4 101.60(4) . 2_655 ? Se1 Ag2 Ag4 120.05(4) . 2_655 ? Se4 Ag2 Ag4 57.63(3) 2_655 2_655 ? Se2 Ag2 Ag4 167.89(4) . . ? Se1 Ag2 Ag4 57.38(3) . . ? Se4 Ag2 Ag4 82.58(3) 2_655 . ? Ag4 Ag2 Ag4 89.15(3) 2_655 . ? Se2 Ag2 Ag3 118.97(4) . . ? Se1 Ag2 Ag3 99.70(3) . . ? Se4 Ag2 Ag3 52.30(3) 2_655 . ? Ag4 Ag2 Ag3 105.89(3) 2_655 . ? Ag4 Ag2 Ag3 62.18(2) . . ? Se2 Ag2 Ag1 49.67(3) . 2_655 ? Se1 Ag2 Ag1 108.36(3) . 2_655 ? Se4 Ag2 Ag1 103.16(3) 2_655 2_655 ? Ag4 Ag2 Ag1 60.21(2) 2_655 2_655 ? Ag4 Ag2 Ag1 135.32(3) . 2_655 ? Ag3 Ag2 Ag1 151.94(3) . 2_655 ? P2 Ag3 Se3 122.25(8) . . ? P2 Ag3 Se4 111.51(8) . 2_655 ? Se3 Ag3 Se4 125.73(5) . 2_655 ? P2 Ag3 Ag4 163.38(7) . . ? Se3 Ag3 Ag4 52.68(3) . . ? Se4 Ag3 Ag4 77.58(3) 2_655 . ? P2 Ag3 Ag2 119.70(7) . . ? Se3 Ag3 Ag2 101.78(3) . . ? Se4 Ag3 Ag2 52.50(3) 2_655 . ? Ag4 Ag3 Ag2 53.95(2) . . ? Se3 Ag4 Se1 109.21(4) . . ? Se3 Ag4 Se4 110.31(4) . . ? Se1 Ag4 Se4 140.38(4) . . ? Se3 Ag4 Ag2 166.71(4) . 2_655 ? Se1 Ag4 Ag2 83.88(3) . 2_655 ? Se4 Ag4 Ag2 56.79(3) . 2_655 ? Se3 Ag4 Ag2 110.50(4) . . ? Se1 Ag4 Ag2 56.32(3) . . ? Se4 Ag4 Ag2 106.04(3) . . ? Ag2 Ag4 Ag2 78.34(3) 2_655 . ? Se3 Ag4 Ag1 118.10(4) . . ? Se1 Ag4 Ag1 53.25(3) . . ? Se4 Ag4 Ag1 108.12(4) . . ? Ag2 Ag4 Ag1 67.48(2) 2_655 . ? Ag2 Ag4 Ag1 102.94(3) . . ? Se3 Ag4 Ag3 52.27(3) . . ? Se1 Ag4 Ag3 100.21(4) . . ? Se4 Ag4 Ag3 101.51(3) . . ? Ag2 Ag4 Ag3 129.33(3) 2_655 . ? Ag2 Ag4 Ag3 63.88(2) . . ? Ag1 Ag4 Ag3 150.07(3) . . ? C11 Se1 Ag2 104.0(4) . . ? C11 Se1 Ag1 108.4(3) . . ? Ag2 Se1 Ag1 127.62(4) . . ? C11 Se1 Ag4 91.3(3) . . ? Ag2 Se1 Ag4 66.30(3) . . ? Ag1 Se1 Ag4 72.84(3) . . ? C22 Se2 Ag1 99.4(3) . 2_655 ? C22 Se2 Ag2 97.8(3) . . ? Ag1 Se2 Ag2 79.99(4) 2_655 . ? C33 Se3 Ag3 99.4(3) . . ? C33 Se3 Ag4 98.7(3) . . ? Ag3 Se3 Ag4 75.05(3) . . ? C44 Se4 Ag3 101.7(3) . 2_655 ? C44 Se4 Ag2 95.1(3) . 2_655 ? Ag3 Se4 Ag2 75.19(3) 2_655 2_655 ? C44 Se4 Ag4 105.9(3) . . ? Ag3 Se4 Ag4 133.34(4) 2_655 . ? Ag2 Se4 Ag4 65.59(3) 2_655 . ? C51 P1 C45 102.0(5) . . ? C51 P1 C57 103.1(5) . . ? C45 P1 C57 104.9(5) . . ? C51 P1 Ag1 112.8(3) . . ? C45 P1 Ag1 115.3(3) . . ? C57 P1 Ag1 117.0(4) . . ? C63 P2 C69 103.6(5) . . ? C63 P2 C75 104.4(5) . . ? C69 P2 C75 101.9(5) . . ? C63 P2 Ag3 114.1(4) . . ? C69 P2 Ag3 116.3(4) . . ? C75 P2 Ag3 114.9(3) . . ? C8 Fe1 C7 42.0(5) . . ? C8 Fe1 C6 68.2(5) . . ? C7 Fe1 C6 38.8(5) . . ? C8 Fe1 C10 67.9(5) . . ? C7 Fe1 C10 66.9(5) . . ? C6 Fe1 C10 40.5(5) . . ? C8 Fe1 C1 163.9(6) . . ? C7 Fe1 C1 124.7(5) . . ? C6 Fe1 C1 106.6(5) . . ? C10 Fe1 C1 118.8(5) . . ? C8 Fe1 C4 121.2(6) . . ? C7 Fe1 C4 155.8(7) . . ? C6 Fe1 C4 165.1(7) . . ? C10 Fe1 C4 129.1(7) . . ? C1 Fe1 C4 67.4(5) . . ? C8 Fe1 C9 39.5(6) . . ? C7 Fe1 C9 67.7(6) . . ? C6 Fe1 C9 68.1(5) . . ? C10 Fe1 C9 40.9(5) . . ? C1 Fe1 C9 154.4(6) . . ? C4 Fe1 C9 110.9(6) . . ? C8 Fe1 C5 154.9(6) . . ? C7 Fe1 C5 161.3(6) . . ? C6 Fe1 C5 125.7(5) . . ? C10 Fe1 C5 108.0(5) . . ? C1 Fe1 C5 40.3(4) . . ? C4 Fe1 C5 41.0(5) . . ? C9 Fe1 C5 121.1(6) . . ? C8 Fe1 C2 127.0(6) . . ? C7 Fe1 C2 107.7(6) . . ? C6 Fe1 C2 118.6(5) . . ? C10 Fe1 C2 153.0(5) . . ? C1 Fe1 C2 40.8(4) . . ? C4 Fe1 C2 66.6(6) . . ? C9 Fe1 C2 164.1(6) . . ? C5 Fe1 C2 68.2(5) . . ? C8 Fe1 C3 108.8(5) . . ? C7 Fe1 C3 120.4(6) . . ? C6 Fe1 C3 152.3(7) . . ? C10 Fe1 C3 166.1(6) . . ? C1 Fe1 C3 68.3(5) . . ? C4 Fe1 C3 40.0(6) . . ? C9 Fe1 C3 128.1(6) . . ? C5 Fe1 C3 69.0(5) . . ? C2 Fe1 C3 39.8(5) . . ? C18 Fe2 C12 114.9(4) . . ? C18 Fe2 C13 105.9(4) . . ? C12 Fe2 C13 41.8(4) . . ? C18 Fe2 C17 40.2(5) . . ? C12 Fe2 C17 106.0(5) . . ? C13 Fe2 C17 127.2(5) . . ? C18 Fe2 C15 165.9(5) . . ? C12 Fe2 C15 67.9(4) . . ? C13 Fe2 C15 66.2(5) . . ? C17 Fe2 C15 153.8(5) . . ? C18 Fe2 C16 148.7(5) . . ? C12 Fe2 C16 39.8(4) . . ? C13 Fe2 C16 67.9(4) . . ? C17 Fe2 C16 117.7(5) . . ? C15 Fe2 C16 41.3(4) . . ? C18 Fe2 C19 39.4(4) . . ? C12 Fe2 C19 148.1(4) . . ? C13 Fe2 C19 116.0(5) . . ? C17 Fe2 C19 66.9(5) . . ? C15 Fe2 C19 131.8(5) . . ? C16 Fe2 C19 171.3(4) . . ? C18 Fe2 C21 67.2(4) . . ? C12 Fe2 C21 128.3(5) . . ? C13 Fe2 C21 165.9(5) . . ? C17 Fe2 C21 39.8(5) . . ? C15 Fe2 C21 123.0(5) . . ? C16 Fe2 C21 111.0(5) . . ? C19 Fe2 C21 67.2(5) . . ? C18 Fe2 C20 66.7(4) . . ? C12 Fe2 C20 168.9(5) . . ? C13 Fe2 C20 149.3(5) . . ? C17 Fe2 C20 67.5(5) . . ? C15 Fe2 C20 113.5(4) . . ? C16 Fe2 C20 133.9(4) . . ? C19 Fe2 C20 39.3(4) . . ? C21 Fe2 C20 41.1(5) . . ? C18 Fe2 C14 129.1(5) . . ? C12 Fe2 C14 69.2(5) . . ? C13 Fe2 C14 41.0(5) . . ? C17 Fe2 C14 166.5(6) . . ? C15 Fe2 C14 37.4(5) . . ? C16 Fe2 C14 67.3(5) . . ? C19 Fe2 C14 110.1(5) . . ? C21 Fe2 C14 152.7(5) . . ? C20 Fe2 C14 119.2(5) . . ? C28 Fe3 C29 39.1(4) . . ? C28 Fe3 C30 68.1(5) . . ? C29 Fe3 C30 42.1(5) . . ? C28 Fe3 C24 128.8(4) . . ? C29 Fe3 C24 106.4(5) . . ? C30 Fe3 C24 114.8(4) . . ? C28 Fe3 C31 67.1(5) . . ? C29 Fe3 C31 67.9(5) . . ? C30 Fe3 C31 39.9(4) . . ? C24 Fe3 C31 148.6(4) . . ? C28 Fe3 C25 167.8(4) . . ? C29 Fe3 C25 130.2(5) . . ? C30 Fe3 C25 107.8(4) . . ? C24 Fe3 C25 41.3(4) . . ? C31 Fe3 C25 117.7(4) . . ? C28 Fe3 C32 40.5(4) . . ? C29 Fe3 C32 67.5(5) . . ? C30 Fe3 C32 67.8(4) . . ? C24 Fe3 C32 168.5(5) . . ? C31 Fe3 C32 39.7(4) . . ? C25 Fe3 C32 150.0(5) . . ? C28 Fe3 C26 150.1(5) . . ? C29 Fe3 C26 170.7(5) . . ? C30 Fe3 C26 132.2(5) . . ? C24 Fe3 C26 68.3(5) . . ? C31 Fe3 C26 112.4(5) . . ? C25 Fe3 C26 40.8(4) . . ? C32 Fe3 C26 119.1(5) . . ? C28 Fe3 C27 117.4(5) . . ? C29 Fe3 C27 146.5(5) . . ? C30 Fe3 C27 171.2(4) . . ? C24 Fe3 C27 67.9(4) . . ? C31 Fe3 C27 134.0(4) . . ? C25 Fe3 C27 68.3(4) . . ? C32 Fe3 C27 111.4(4) . . ? C26 Fe3 C27 39.8(4) . . ? C28 Fe3 C23 107.7(4) . . ? C29 Fe3 C23 113.3(4) . . ? C30 Fe3 C23 146.6(4) . . ? C24 Fe3 C23 40.5(4) . . ? C31 Fe3 C23 170.8(4) . . ? C25 Fe3 C23 69.0(4) . . ? C32 Fe3 C23 131.6(4) . . ? C26 Fe3 C23 68.0(4) . . ? C27 Fe3 C23 40.6(4) . . ? C42 Fe4 C35 165.1(7) . . ? C42 Fe4 C34 128.7(6) . . ? C35 Fe4 C34 41.0(4) . . ? C42 Fe4 C37 121.0(6) . . ? C35 Fe4 C37 68.8(5) . . ? C34 Fe4 C37 69.3(4) . . ? C42 Fe4 C38 111.8(6) . . ? C35 Fe4 C38 67.6(5) . . ? C34 Fe4 C38 40.8(4) . . ? C37 Fe4 C38 40.0(4) . . ? C42 Fe4 C41 39.3(7) . . ? C35 Fe4 C41 152.7(7) . . ? C34 Fe4 C41 165.7(6) . . ? C37 Fe4 C41 108.6(6) . . ? C38 Fe4 C41 128.9(6) . . ? C42 Fe4 C39 65.6(6) . . ? C35 Fe4 C39 107.7(5) . . ? C34 Fe4 C39 117.9(5) . . ? C37 Fe4 C39 165.6(6) . . ? C38 Fe4 C39 152.9(5) . . ? C41 Fe4 C39 67.6(6) . . ? C42 Fe4 C40 65.8(7) . . ? C35 Fe4 C40 118.5(6) . . ? C34 Fe4 C40 151.7(5) . . ? C37 Fe4 C40 128.1(6) . . ? C38 Fe4 C40 166.1(5) . . ? C41 Fe4 C40 40.4(6) . . ? C39 Fe4 C40 40.1(6) . . ? C42 Fe4 C43 41.3(6) . . ? C35 Fe4 C43 125.1(5) . . ? C34 Fe4 C43 105.6(5) . . ? C37 Fe4 C43 153.8(5) . . ? C38 Fe4 C43 119.6(5) . . ? C41 Fe4 C43 69.6(6) . . ? C39 Fe4 C43 39.6(5) . . ? C40 Fe4 C43 68.4(6) . . ? C42 Fe4 C36 154.3(7) . . ? C35 Fe4 C36 40.4(4) . . ? C34 Fe4 C36 69.5(4) . . ? C37 Fe4 C36 41.9(4) . . ? C38 Fe4 C36 68.4(5) . . ? C41 Fe4 C36 119.1(7) . . ? C39 Fe4 C36 126.5(6) . . ? C40 Fe4 C36 107.5(6) . . ? C43 Fe4 C36 162.3(5) . . ? C5 C1 C2 108.3(10) . . ? C5 C1 C11 125.3(10) . . ? C2 C1 C11 126.2(10) . . ? C5 C1 Fe1 70.1(6) . . ? C2 C1 Fe1 70.1(6) . . ? C11 C1 Fe1 121.1(7) . . ? C3 C2 C1 109.0(12) . . ? C3 C2 Fe1 70.4(7) . . ? C1 C2 Fe1 69.1(6) . . ? C2 C3 C4 106.6(12) . . ? C2 C3 Fe1 69.9(7) . . ? C4 C3 Fe1 69.3(7) . . ? C3 C4 C5 110.3(13) . . ? C3 C4 Fe1 70.7(8) . . ? C5 C4 Fe1 69.8(7) . . ? C1 C5 C4 105.8(11) . . ? C1 C5 Fe1 69.5(6) . . ? C4 C5 Fe1 69.2(7) . . ? C7 C6 C10 108.4(12) . . ? C7 C6 Fe1 69.6(7) . . ? C10 C6 Fe1 69.9(6) . . ? C6 C7 C8 109.3(12) . . ? C6 C7 Fe1 71.7(7) . . ? C8 C7 Fe1 69.0(7) . . ? C9 C8 C7 107.2(12) . . ? C9 C8 Fe1 71.8(7) . . ? C7 C8 Fe1 69.0(7) . . ? C8 C9 C10 107.8(14) . . ? C8 C9 Fe1 68.8(8) . . ? C10 C9 Fe1 69.3(7) . . ? C6 C10 C9 107.4(13) . . ? C6 C10 Fe1 69.6(7) . . ? C9 C10 Fe1 69.8(7) . . ? C1 C11 Se1 113.4(7) . . ? C16 C12 C13 106.7(10) . . ? C16 C12 C22 127.9(11) . . ? C13 C12 C22 125.4(10) . . ? C16 C12 Fe2 70.6(6) . . ? C13 C12 Fe2 69.2(6) . . ? C22 C12 Fe2 123.6(7) . . ? C14 C13 C12 107.2(10) . . ? C14 C13 Fe2 70.5(7) . . ? C12 C13 Fe2 69.0(6) . . ? C15 C14 C13 107.9(11) . . ? C15 C14 Fe2 70.2(7) . . ? C13 C14 Fe2 68.5(7) . . ? C14 C15 C16 111.4(11) . . ? C14 C15 Fe2 72.3(7) . . ? C16 C15 Fe2 69.8(6) . . ? C12 C16 C15 106.8(10) . . ? C12 C16 Fe2 69.5(6) . . ? C15 C16 Fe2 68.9(6) . . ? C21 C17 C18 108.3(11) . . ? C21 C17 Fe2 70.7(7) . . ? C18 C17 Fe2 69.8(7) . . ? C19 C18 C17 108.5(10) . . ? C19 C18 Fe2 70.9(6) . . ? C17 C18 Fe2 70.0(6) . . ? C18 C19 C20 109.3(11) . . ? C18 C19 Fe2 69.7(6) . . ? C20 C19 Fe2 70.6(7) . . ? C19 C20 C21 107.3(11) . . ? C19 C20 Fe2 70.1(6) . . ? C21 C20 Fe2 69.4(6) . . ? C17 C21 C20 106.7(11) . . ? C17 C21 Fe2 69.4(6) . . ? C20 C21 Fe2 69.5(6) . . ? C12 C22 Se2 112.1(7) . . ? C24 C23 C27 107.0(9) . . ? C24 C23 C33 124.7(9) . . ? C27 C23 C33 128.3(9) . . ? C24 C23 Fe3 69.1(5) . . ? C27 C23 Fe3 69.6(6) . . ? C33 C23 Fe3 124.0(7) . . ? C23 C24 C25 108.9(9) . . ? C23 C24 Fe3 70.4(5) . . ? C25 C24 Fe3 69.6(6) . . ? C26 C25 C24 106.2(9) . . ? C26 C25 Fe3 69.8(6) . . ? C24 C25 Fe3 69.1(6) . . ? C27 C26 C25 108.9(9) . . ? C27 C26 Fe3 70.2(6) . . ? C25 C26 Fe3 69.4(6) . . ? C26 C27 C23 109.0(9) . . ? C26 C27 Fe3 70.0(6) . . ? C23 C27 Fe3 69.9(5) . . ? C29 C28 C32 109.8(11) . . ? C29 C28 Fe3 70.6(8) . . ? C32 C28 Fe3 70.6(7) . . ? C28 C29 C30 107.6(10) . . ? C28 C29 Fe3 70.3(7) . . ? C30 C29 Fe3 69.2(7) . . ? C31 C30 C29 105.8(10) . . ? C31 C30 Fe3 70.3(6) . . ? C29 C30 Fe3 68.7(6) . . ? C32 C31 C30 110.0(10) . . ? C32 C31 Fe3 70.4(6) . . ? C30 C31 Fe3 69.8(6) . . ? C31 C32 C28 106.9(10) . . ? C31 C32 Fe3 69.9(6) . . ? C28 C32 Fe3 68.9(6) . . ? C23 C33 Se3 113.3(7) . . ? C38 C34 C35 105.4(9) . . ? C38 C34 C44 127.2(9) . . ? C35 C34 C44 127.4(9) . . ? C38 C34 Fe4 69.7(6) . . ? C35 C34 Fe4 69.1(6) . . ? C44 C34 Fe4 124.6(7) . . ? C36 C35 C34 111.0(10) . . ? C36 C35 Fe4 71.3(7) . . ? C34 C35 Fe4 70.0(6) . . ? C35 C36 C37 105.5(10) . . ? C35 C36 Fe4 68.3(7) . . ? C37 C36 Fe4 68.0(7) . . ? C38 C37 C36 107.3(10) . . ? C38 C37 Fe4 70.1(6) . . ? C36 C37 Fe4 70.1(7) . . ? C37 C38 C34 110.7(9) . . ? C37 C38 Fe4 69.9(6) . . ? C34 C38 Fe4 69.5(6) . . ? C43 C39 C40 111.5(12) . . ? C43 C39 Fe4 70.8(7) . . ? C40 C39 Fe4 70.2(7) . . ? C39 C40 C41 107.5(14) . . ? C39 C40 Fe4 69.6(7) . . ? C41 C40 Fe4 69.2(7) . . ? C42 C41 C40 104.5(15) . . ? C42 C41 Fe4 67.4(9) . . ? C40 C41 Fe4 70.4(8) . . ? C41 C42 C43 115.3(16) . . ? C41 C42 Fe4 73.3(10) . . ? C43 C42 Fe4 72.9(9) . . ? C39 C43 C42 101.2(14) . . ? C39 C43 Fe4 69.6(8) . . ? C42 C43 Fe4 65.8(9) . . ? C34 C44 Se4 112.9(7) . . ? C46 C45 C50 120.0(10) . . ? C46 C45 P1 123.6(8) . . ? C50 C45 P1 116.5(8) . . ? C47 C46 C45 120.3(10) . . ? C48 C47 C46 120.1(11) . . ? C47 C48 C49 121.0(10) . . ? C50 C49 C48 118.8(10) . . ? C49 C50 C45 119.8(10) . . ? C56 C51 C52 120.2(11) . . ? C56 C51 P1 122.9(10) . . ? C52 C51 P1 116.9(8) . . ? C53 C52 C51 120.2(11) . . ? C52 C53 C54 119.2(14) . . ? C53 C54 C55 119.8(14) . . ? C56 C55 C54 119.8(13) . . ? C51 C56 C55 120.5(14) . . ? C58 C57 C62 118.5(12) . . ? C58 C57 P1 119.1(9) . . ? C62 C57 P1 122.4(10) . . ? C57 C58 C59 121.3(11) . . ? C58 C59 C60 117.8(13) . . ? C59 C60 C61 121.9(13) . . ? C62 C61 C60 118.8(13) . . ? C61 C62 C57 121.5(13) . . ? C64 C63 C68 116.4(11) . . ? C64 C63 P2 119.6(9) . . ? C68 C63 P2 124.1(10) . . ? C63 C64 C65 121.5(12) . . ? C64 C65 C66 120.2(14) . . ? C67 C66 C65 119.1(14) . . ? C66 C67 C68 120.8(15) . . ? C67 C68 C63 121.8(14) . . ? C70 C69 C74 116.5(11) . . ? C70 C69 P2 119.1(9) . . ? C74 C69 P2 124.4(9) . . ? C71 C70 C69 121.6(12) . . ? C72 C71 C70 121.9(12) . . ? C71 C72 C73 120.0(12) . . ? C74 C73 C72 118.7(13) . . ? C73 C74 C69 121.3(12) . . ? C76 C75 C80 117.1(10) . . ? C76 C75 P2 124.5(8) . . ? C80 C75 P2 118.2(8) . . ? C77 C76 C75 121.0(11) . . ? C78 C77 C76 120.3(12) . . ? C77 C78 C79 121.3(12) . . ? C80 C79 C78 117.1(12) . . ? C79 C80 C75 123.0(11) . . ? Cl3 C1S Cl1 119(2) . . ? Cl3 C1S Cl2 110.2(16) . . ? Cl1 C1S Cl2 105.2(16) . . ? Cl4 C2S Cl6 90.7(16) . . ? Cl4 C2S Cl5 131(3) . . ? Cl6 C2S Cl5 112.0(18) . . ? C2S Cl4 Cl6 45.2(9) . . ? C2S Cl6 Cl4 44.1(9) . . ? Cl9 C3S Cl8 114.7(10) . . ? Cl9 C3S Cl7 107.9(9) . . ? Cl8 C3S Cl7 109.0(11) . . ? Cl10 C4S Cl12 104.0(11) . . ? Cl10 C4S Cl11 110.7(9) . . ? Cl12 C4S Cl11 114.5(10) . . ? Cl13 C5S Cl14 114.3(18) . . ? Cl13 C5S Cl15 114.6(19) . . ? Cl14 C5S Cl15 110.8(16) . . ? Cl14 Cl14 C5S 140(2) 2_756 . ? Cl17 C6S Cl18 119.1 . . ? Cl17 C6S Cl16 113.544(3) . . ? Cl18 C6S Cl16 97.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.902 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.218