# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Andrew J.P. White' _publ_contact_author_email a.white@imperial.ac.uk loop_ _publ_author_name J.Wilton-Ely K.Oliver G.Hogarth A.White data_2 _database_code_depnum_ccdc_archive 'CCDC 764405' #TrackingRef 'EJIC 01-10.cif' _audit_update_record ; 2011-02-03 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H74 Fe2 N2 Ni2 P4 S4, 2(F6 P), C H2 Cl2' _chemical_formula_sum 'C87 H76 Cl2 F12 Fe2 N2 Ni2 P6 S4' _chemical_formula_weight 1991.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 13.5263(2) _cell_length_b 17.6262(3) _cell_length_c 19.4449(4) _cell_angle_alpha 96.8975(15) _cell_angle_beta 97.5228(15) _cell_angle_gamma 107.7830(15) _cell_volume 4313.12(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 31764 _cell_measurement_theta_min 2.3216 _cell_measurement_theta_max 72.3376 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 6.276 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.310 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ? _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50144 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 72.59 _reflns_number_total 16955 _reflns_number_gt 14825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Two partial occupancy orientations were identified for the C12-, C55- and C62-based phenyl rings. SADI distance restraints were used for the C11-C12/C11-C12', P48-C55/P48-C55' and P61-C62/P61-C62' pairs of bonds. SIMU restraints were used for the equivalent adjacent atoms in each case, e.g. C14 with C14', and C67 with C67' etc. The two orientations of the phenyl ring in each case were constrained to be idealised hexagons, and for the C12/C12' rings, FLAT restraints were used to keep the six atoms of the phenyl rings coplanar with C11. Five partial occupancy orientations were identified for the included dichloromethane solvent molecule. A single SADI restraint was used for each of the ten C-Cl bonds, and another was used for the five Cl...Cl distances. A SIMU restraint was used for the five carbon atoms, and a separate one for the ten chlorine atoms. ; _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^)+(0.0717P)^2^+1.3400P] 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 16955 _refine_ls_number_parameters 1095 _refine_ls_number_restraints 225 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.141 _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 Ni1 Ni 0.81182(3) 0.56898(2) 0.33356(2) 0.02835(10) Uani 1 1 d . B . Ni2 Ni 0.85584(3) 0.88236(2) 0.15044(2) 0.02693(9) Uani 1 1 d . C . Fe1 Fe 0.52173(3) 0.38051(2) 0.30384(2) 0.03369(10) Uani 1 1 d . . . Fe2 Fe 0.61178(3) 0.98625(2) 0.14984(2) 0.03221(10) Uani 1 1 d . C . S1 S 0.87936(5) 0.69868(4) 0.38071(3) 0.03818(14) Uani 1 1 d . . . C2 C 0.97696(19) 0.70052(14) 0.33122(12) 0.0302(5) Uani 1 1 d . . . S3 S 0.93919(5) 0.61214(3) 0.27245(3) 0.03397(13) Uani 1 1 d . . . N4 N 1.06815(16) 0.75846(12) 0.33893(10) 0.0299(4) Uani 1 1 d . A . C5 C 1.14966(18) 0.74904(14) 0.29886(12) 0.0300(5) Uani 1 1 d . . . H5A H 1.1352 0.6908 0.2821 0.036 Uiso 1 1 calc R . . H5B H 1.2190 0.7698 0.3306 0.036 Uiso 1 1 calc R . . C6 C 1.15575(17) 0.79308(14) 0.23573(12) 0.0286(4) Uani 1 1 d . . . H6A H 1.1669 0.8509 0.2522 0.034 Uiso 1 1 calc R . . H6B H 1.2175 0.7896 0.2149 0.034 Uiso 1 1 calc R . . N7 N 1.06039(15) 0.76003(11) 0.18082(10) 0.0256(4) Uani 1 1 d . . . C8 C 0.99167(18) 0.79869(13) 0.17296(12) 0.0272(4) Uani 1 1 d . . . S9 S 1.00077(5) 0.88842(4) 0.22265(3) 0.03556(13) Uani 1 1 d . . . S10 S 0.87930(5) 0.76762(3) 0.11005(3) 0.03267(13) Uani 1 1 d . . . C11 C 1.0957(2) 0.83218(14) 0.39241(13) 0.0355(5) Uani 1 1 d D . . H11A H 1.0298 0.8411 0.4026 0.043 Uiso 0.831(9) 1 calc PR A 1 H11B H 1.1357 0.8792 0.3728 0.043 Uiso 0.831(9) 1 calc PR A 1 H11C H 1.0324 0.8400 0.4045 0.043 Uiso 0.169(9) 1 d PR A 2 H11D H 1.1335 0.8786 0.3740 0.043 Uiso 0.169(9) 1 d PR A 2 C12 C 1.1605(2) 0.82799(18) 0.46041(13) 0.0383(9) Uani 0.831(9) 1 d PGDU A 1 C13 C 1.1223(2) 0.76923(19) 0.5008(2) 0.0518(12) Uani 0.831(9) 1 d PGDU A 1 H13A H 1.0545 0.7297 0.4853 0.062 Uiso 0.831(9) 1 calc PR A 1 C14 C 1.1832(3) 0.76826(19) 0.56389(19) 0.0681(15) Uani 0.831(9) 1 d PGDU A 1 H14A H 1.1571 0.7281 0.5915 0.082 Uiso 0.831(9) 1 calc PR A 1 C15 C 1.2823(3) 0.8260(2) 0.58654(13) 0.0609(12) Uani 0.831(9) 1 d PGDU A 1 H15A H 1.3239 0.8254 0.6296 0.073 Uiso 0.831(9) 1 calc PR A 1 C16 C 1.3205(3) 0.8848(3) 0.54612(16) 0.0776(18) Uani 0.831(9) 1 d PGDU A 1 H16A H 1.3882 0.9243 0.5616 0.093 Uiso 0.831(9) 1 calc PR A 1 C17 C 1.2596(3) 0.8858(2) 0.48306(14) 0.0661(16) Uani 0.831(9) 1 d PGDU A 1 H17A H 1.2857 0.9259 0.4554 0.079 Uiso 0.831(9) 1 calc PR A 1 C12' C 1.1758(12) 0.8255(8) 0.4575(8) 0.039(4) Uiso 0.169(9) 1 d PGDU A 2 C13' C 1.1277(10) 0.7878(12) 0.5089(11) 0.039(4) Uiso 0.169(9) 1 d PGDU A 2 H13B H 1.0530 0.7673 0.5029 0.047 Uiso 0.169(9) 1 calc PR A 2 C14' C 1.1890(15) 0.7799(14) 0.5691(10) 0.060(5) Uiso 0.169(9) 1 d PGDU A 2 H14B H 1.1562 0.7541 0.6043 0.072 Uiso 0.169(9) 1 calc PR A 2 C15' C 1.2984(14) 0.8099(11) 0.5779(8) 0.063(5) Uiso 0.169(9) 1 d PGDU A 2 H15B H 1.3403 0.8046 0.6191 0.075 Uiso 0.169(9) 1 calc PR A 2 C16' C 1.3465(10) 0.8477(12) 0.5265(10) 0.067(4) Uiso 0.169(9) 1 d PGDU A 2 H16B H 1.4212 0.8681 0.5325 0.081 Uiso 0.169(9) 1 calc PR A 2 C17' C 1.2852(13) 0.8555(10) 0.4662(8) 0.054(4) Uiso 0.169(9) 1 d PGDU A 2 H17B H 1.3180 0.8813 0.4311 0.065 Uiso 0.169(9) 1 calc PR A 2 C18 C 1.04743(18) 0.68614(13) 0.13048(12) 0.0284(4) Uani 1 1 d . . . H18A H 0.9726 0.6513 0.1214 0.034 Uiso 1 1 calc R . . H18B H 1.0904 0.6556 0.1517 0.034 Uiso 1 1 calc R . . C19 C 1.0802(2) 0.70540(14) 0.06178(13) 0.0326(5) Uani 1 1 d . . . C20 C 1.1772(3) 0.7595(2) 0.05895(17) 0.0644(10) Uani 1 1 d . . . H20A H 1.2258 0.7850 0.1014 0.077 Uiso 1 1 calc R . . C21 C 1.2051(4) 0.7773(3) -0.00489(19) 0.0779(14) Uani 1 1 d . . . H21A H 1.2717 0.8156 -0.0059 0.093 Uiso 1 1 calc R . . C22 C 1.1367(3) 0.7397(2) -0.06650(17) 0.0577(9) Uani 1 1 d . . . H22A H 1.1558 0.7518 -0.1102 0.069 Uiso 1 1 calc R . . C23 C 1.0418(3) 0.6854(2) -0.06495(16) 0.0538(8) Uani 1 1 d . . . H23A H 0.9949 0.6586 -0.1077 0.065 Uiso 1 1 calc R . . C24 C 1.0129(2) 0.6687(2) -0.00096(15) 0.0466(6) Uani 1 1 d . . . H24A H 0.9454 0.6314 -0.0005 0.056 Uiso 1 1 calc R . . P25 P 0.77121(4) 0.44783(3) 0.26913(3) 0.02691(12) Uani 1 1 d . . . C26 C 0.76296(19) 0.46648(14) 0.17887(13) 0.0314(5) Uani 1 1 d . . . C27 C 0.7092(2) 0.51861(17) 0.15951(15) 0.0390(5) Uani 1 1 d . . . H27A H 0.6732 0.5394 0.1919 0.047 Uiso 1 1 calc R . . C28 C 0.7078(2) 0.54039(17) 0.09331(15) 0.0419(6) Uani 1 1 d . . . H28A H 0.6716 0.5766 0.0807 0.050 Uiso 1 1 calc R . . C29 C 0.7584(3) 0.50991(19) 0.04602(15) 0.0470(7) Uani 1 1 d . . . H29A H 0.7557 0.5237 0.0002 0.056 Uiso 1 1 calc R . . C30 C 0.8135(4) 0.4589(3) 0.06509(19) 0.0677(10) Uani 1 1 d . . . H30A H 0.8492 0.4381 0.0325 0.081 Uiso 1 1 calc R . . C31 C 0.8166(3) 0.4380(2) 0.13180(17) 0.0555(8) Uani 1 1 d . . . H31A H 0.8559 0.4041 0.1451 0.067 Uiso 1 1 calc R . . C32 C 0.86688(19) 0.39426(14) 0.28167(12) 0.0300(5) Uani 1 1 d . . . C33 C 0.8352(2) 0.31093(15) 0.25713(13) 0.0343(5) Uani 1 1 d . . . H33A H 0.7642 0.2827 0.2352 0.041 Uiso 1 1 calc R . . C34 C 0.9065(2) 0.26961(16) 0.26468(15) 0.0406(6) Uani 1 1 d . . . H34A H 0.8843 0.2131 0.2479 0.049 Uiso 1 1 calc R . . C35 C 1.0103(2) 0.30997(19) 0.29652(17) 0.0460(6) Uani 1 1 d . . . H35A H 1.0596 0.2815 0.3007 0.055 Uiso 1 1 calc R . . C36 C 1.0419(2) 0.39193(19) 0.3222(2) 0.0514(7) Uani 1 1 d . . . H36A H 1.1126 0.4195 0.3452 0.062 Uiso 1 1 calc R . . C37 C 0.9709(2) 0.43418(16) 0.31462(15) 0.0403(6) Uani 1 1 d . . . H37A H 0.9934 0.4906 0.3320 0.048 Uiso 1 1 calc R . . C38 C 0.65045(18) 0.36762(14) 0.26871(13) 0.0310(5) Uani 1 1 d . . . C39 C 0.5610(2) 0.33569(16) 0.21273(15) 0.0383(5) Uani 1 1 d . . . H39A H 0.5529 0.3543 0.1664 0.046 Uiso 1 1 calc R . . C40 C 0.4854(2) 0.27245(17) 0.23600(19) 0.0493(7) Uani 1 1 d . . . H40A H 0.4137 0.2402 0.2088 0.059 Uiso 1 1 calc R . . C41 C 0.5262(2) 0.26457(16) 0.3042(2) 0.0478(7) Uani 1 1 d . . . H41A H 0.4891 0.2256 0.3332 0.057 Uiso 1 1 calc R . . C42 C 0.6289(2) 0.32341(15) 0.32528(16) 0.0380(5) Uani 1 1 d . . . H42A H 0.6772 0.3319 0.3711 0.046 Uiso 1 1 calc R . . C43 C 0.5650(2) 0.48668(16) 0.37004(15) 0.0373(5) Uani 1 1 d . B . C44 C 0.4896(2) 0.42501(18) 0.39628(17) 0.0452(6) Uani 1 1 d . . . H44A H 0.5015 0.4062 0.4422 0.054 Uiso 1 1 calc R . . C45 C 0.3953(2) 0.3959(2) 0.3456(2) 0.0522(7) Uani 1 1 d . . . H45A H 0.3302 0.3515 0.3492 0.063 Uiso 1 1 calc R . . C46 C 0.4098(2) 0.43765(19) 0.28806(19) 0.0494(7) Uani 1 1 d . . . H46A H 0.3568 0.4281 0.2442 0.059 Uiso 1 1 calc R . . C47 C 0.5142(2) 0.49404(16) 0.30261(16) 0.0408(6) Uani 1 1 d . . . H47A H 0.5468 0.5318 0.2711 0.049 Uiso 1 1 calc R . . P48 P 0.70033(5) 0.54323(4) 0.40776(3) 0.03358(14) Uani 1 1 d D . . C49 C 0.7424(2) 0.48928(16) 0.47362(14) 0.0391(6) Uani 1 1 d . B . C50 C 0.8306(2) 0.46554(17) 0.46964(15) 0.0455(6) Uani 1 1 d . . . H50A H 0.8683 0.4772 0.4321 0.055 Uiso 1 1 calc R B . C51 C 0.8642(3) 0.4251(2) 0.51984(19) 0.0576(8) Uani 1 1 d . B . H51A H 0.9249 0.4093 0.5169 0.069 Uiso 1 1 calc R . . C52 C 0.8090(3) 0.4077(2) 0.57438(19) 0.0663(11) Uani 1 1 d . . . H52A H 0.8311 0.3790 0.6084 0.080 Uiso 1 1 calc R B . C53 C 0.7220(3) 0.4319(2) 0.57947(17) 0.0629(10) Uani 1 1 d . B . H53A H 0.6847 0.4200 0.6171 0.076 Uiso 1 1 calc R . . C54 C 0.6888(3) 0.47341(19) 0.53020(16) 0.0506(7) Uani 1 1 d . . . H54A H 0.6299 0.4911 0.5346 0.061 Uiso 1 1 calc R B . C55 C 0.6853(6) 0.6342(2) 0.4590(3) 0.0365(13) Uani 0.65(2) 1 d PGDU B 1 C56 C 0.7661(6) 0.6777(3) 0.5146(3) 0.0433(13) Uani 0.65(2) 1 d PGU B 1 H56A H 0.8242 0.6593 0.5264 0.052 Uiso 0.65(2) 1 calc PR B 1 C57 C 0.7620(8) 0.7482(2) 0.5528(3) 0.0515(18) Uani 0.65(2) 1 d PGU B 1 H57A H 0.8173 0.7780 0.5908 0.062 Uiso 0.65(2) 1 calc PR B 1 C58 C 0.6770(9) 0.7752(2) 0.5355(3) 0.058(2) Uani 0.65(2) 1 d PGU B 1 H58A H 0.6742 0.8234 0.5616 0.070 Uiso 0.65(2) 1 calc PR B 1 C59 C 0.5962(8) 0.7317(3) 0.4799(4) 0.0589(17) Uani 0.65(2) 1 d PGU B 1 H59A H 0.5381 0.7501 0.4680 0.071 Uiso 0.65(2) 1 calc PR B 1 C60 C 0.6003(6) 0.6612(3) 0.4416(3) 0.0460(13) Uani 0.65(2) 1 d PGU B 1 H60A H 0.5450 0.6314 0.4036 0.055 Uiso 0.65(2) 1 calc PR B 1 C55' C 0.7090(9) 0.6327(5) 0.4671(5) 0.039(2) Uiso 0.35(2) 1 d PGDU B 2 C56' C 0.7952(9) 0.6725(5) 0.5203(5) 0.042(2) Uiso 0.35(2) 1 d PGU B 2 H56B H 0.8502 0.6501 0.5294 0.051 Uiso 0.35(2) 1 calc PR B 2 C57' C 0.8008(10) 0.7451(5) 0.5603(4) 0.044(2) Uiso 0.35(2) 1 d PGU B 2 H57B H 0.8597 0.7723 0.5967 0.053 Uiso 0.35(2) 1 calc PR B 2 C58' C 0.7203(11) 0.7779(4) 0.5471(5) 0.052(3) Uiso 0.35(2) 1 d PGU B 2 H58B H 0.7242 0.8275 0.5744 0.063 Uiso 0.35(2) 1 calc PR B 2 C59' C 0.6341(10) 0.7380(6) 0.4938(6) 0.055(3) Uiso 0.35(2) 1 d PGU B 2 H59B H 0.5791 0.7604 0.4848 0.066 Uiso 0.35(2) 1 calc PR B 2 C60' C 0.6285(9) 0.6655(6) 0.4539(5) 0.046(2) Uiso 0.35(2) 1 d PGU B 2 H60B H 0.5696 0.6383 0.4175 0.055 Uiso 0.35(2) 1 calc PR B 2 P61 P 0.86409(5) 1.00077(3) 0.20945(3) 0.02952(12) Uani 1 1 d D . . C62 C 0.8579(5) 0.9871(3) 0.30039(14) 0.0367(11) Uani 0.698(15) 1 d PGDU C 1 C63 C 0.8098(5) 0.9102(3) 0.31445(19) 0.0451(11) Uani 0.698(15) 1 d PGU C 1 H63A H 0.7787 0.8660 0.2768 0.054 Uiso 0.698(15) 1 calc PR C 1 C64 C 0.8073(7) 0.8980(3) 0.3836(2) 0.0611(18) Uani 0.698(15) 1 d PGU C 1 H64A H 0.7744 0.8455 0.3932 0.073 Uiso 0.698(15) 1 calc PR C 1 C65 C 0.8528(8) 0.9627(4) 0.43868(16) 0.071(2) Uani 0.698(15) 1 d PGU C 1 H65A H 0.8511 0.9544 0.4859 0.085 Uiso 0.698(15) 1 calc PR C 1 C66 C 0.9009(7) 1.0396(4) 0.42462(16) 0.0680(18) Uani 0.698(15) 1 d PGU C 1 H66A H 0.9320 1.0839 0.4623 0.082 Uiso 0.698(15) 1 calc PR C 1 C67 C 0.9035(6) 1.0518(3) 0.3555(2) 0.0507(13) Uani 0.698(15) 1 d PGU C 1 H67A H 0.9363 1.1044 0.3459 0.061 Uiso 0.698(15) 1 calc PR C 1 C62' C 0.8823(10) 0.9974(7) 0.3047(4) 0.034(3) Uiso 0.302(15) 1 d PGDU C 2 C63' C 0.8461(10) 0.9228(6) 0.3260(5) 0.044(3) Uiso 0.302(15) 1 d PGU C 2 H63B H 0.8150 0.8750 0.2919 0.052 Uiso 0.302(15) 1 calc PR C 2 C64' C 0.8553(12) 0.9181(6) 0.3973(5) 0.064(4) Uiso 0.302(15) 1 d PGU C 2 H64B H 0.8305 0.8671 0.4119 0.077 Uiso 0.302(15) 1 calc PR C 2 C65' C 0.9007(11) 0.9880(7) 0.4472(4) 0.065(4) Uiso 0.302(15) 1 d PGU C 2 H65B H 0.9070 0.9847 0.4959 0.077 Uiso 0.302(15) 1 calc PR C 2 C66' C 0.9369(10) 1.0626(6) 0.4259(5) 0.054(3) Uiso 0.302(15) 1 d PGU C 2 H66B H 0.9680 1.1103 0.4600 0.064 Uiso 0.302(15) 1 calc PR C 2 C67' C 0.9277(10) 1.0673(6) 0.3546(6) 0.046(3) Uiso 0.302(15) 1 d PGU C 2 H67B H 0.9525 1.1183 0.3400 0.055 Uiso 0.302(15) 1 calc PR C 2 C68 C 0.98833(19) 1.08053(15) 0.20783(14) 0.0346(5) Uani 1 1 d . C . C69 C 1.0809(2) 1.08946(17) 0.25393(17) 0.0444(6) Uani 1 1 d . . . H69A H 1.0804 1.0544 0.2875 0.053 Uiso 1 1 calc R C . C70 C 1.1747(2) 1.1501(2) 0.2507(2) 0.0538(8) Uani 1 1 d . C . H70A H 1.2371 1.1565 0.2828 0.065 Uiso 1 1 calc R . . C71 C 1.1773(2) 1.2000(2) 0.2020(2) 0.0550(8) Uani 1 1 d . . . H71A H 1.2413 1.2410 0.2004 0.066 Uiso 1 1 calc R C . C72 C 1.0872(2) 1.1910(2) 0.15509(19) 0.0497(7) Uani 1 1 d . C . H72A H 1.0892 1.2255 0.1210 0.060 Uiso 1 1 calc R . . C73 C 0.9936(2) 1.13138(17) 0.15761(15) 0.0397(6) Uani 1 1 d . . . H73A H 0.9321 1.1251 0.1246 0.048 Uiso 1 1 calc R C . C74 C 0.76414(19) 1.04849(14) 0.19231(13) 0.0307(5) Uani 1 1 d . C . C75 C 0.6966(2) 1.06155(15) 0.24088(14) 0.0362(5) Uani 1 1 d . . . H75A H 0.6986 1.0476 0.2893 0.043 Uiso 1 1 calc R C . C76 C 0.6258(2) 1.09675(15) 0.20769(15) 0.0381(5) Uani 1 1 d . C . H76A H 0.5684 1.1107 0.2284 0.046 Uiso 1 1 calc R . . C77 C 0.6477(2) 1.10606(15) 0.13966(15) 0.0371(5) Uani 1 1 d . . . H77A H 0.6088 1.1281 0.1042 0.044 Uiso 1 1 calc R C . C78 C 0.73220(19) 1.07596(14) 0.12895(14) 0.0330(5) Uani 1 1 d . C . H78A H 0.7644 1.0751 0.0855 0.040 Uiso 1 1 calc R . . C79 C 0.60498(19) 0.87942(14) 0.09598(15) 0.0349(5) Uani 1 1 d . . . C80 C 0.5300(2) 0.91049(16) 0.05884(18) 0.0445(7) Uani 1 1 d . C . H80A H 0.5288 0.9238 0.0102 0.053 Uiso 1 1 calc R . . C81 C 0.4584(2) 0.91893(19) 0.1044(2) 0.0555(9) Uani 1 1 d . . . H81A H 0.3994 0.9411 0.0937 0.067 Uiso 1 1 calc R C . C82 C 0.4866(2) 0.89349(18) 0.1683(2) 0.0563(9) Uani 1 1 d . C . H82A H 0.4508 0.8947 0.2101 0.068 Uiso 1 1 calc R . . C83 C 0.5770(2) 0.86913(16) 0.16418(17) 0.0435(6) Uani 1 1 d . C . H83A H 0.6144 0.8486 0.2018 0.052 Uiso 1 1 calc R . . P84 P 0.71706(4) 0.85891(3) 0.06800(3) 0.02790(12) Uani 1 1 d . C . C85 C 0.75003(19) 0.91661(14) -0.00197(13) 0.0317(5) Uani 1 1 d . . . C86 C 0.8473(2) 0.97728(16) 0.00672(15) 0.0370(5) Uani 1 1 d . C . H86A H 0.8965 0.9884 0.0492 0.044 Uiso 1 1 calc R . . C87 C 0.8723(2) 1.02154(19) -0.04668(17) 0.0462(6) Uani 1 1 d . . . H87A H 0.9383 1.0633 -0.0405 0.055 Uiso 1 1 calc R C . C88 C 0.8009(3) 1.0047(2) -0.10912(17) 0.0488(7) Uani 1 1 d . C . H88A H 0.8181 1.0352 -0.1455 0.059 Uiso 1 1 calc R . . C89 C 0.7050(3) 0.94390(19) -0.11858(15) 0.0449(6) Uani 1 1 d . . . H89A H 0.6567 0.9324 -0.1616 0.054 Uiso 1 1 calc R C . C90 C 0.6792(2) 0.89953(17) -0.06538(14) 0.0387(5) Uani 1 1 d . C . H90A H 0.6133 0.8575 -0.0721 0.046 Uiso 1 1 calc R . . C91 C 0.6599(2) 0.75560(14) 0.01917(13) 0.0328(5) Uani 1 1 d . . . C92 C 0.7132(2) 0.72791(16) -0.02956(14) 0.0381(5) Uani 1 1 d . C . H92A H 0.7785 0.7627 -0.0370 0.046 Uiso 1 1 calc R . . C93 C 0.6714(3) 0.64958(18) -0.06757(15) 0.0464(7) Uani 1 1 d . . . H93A H 0.7086 0.6308 -0.1003 0.056 Uiso 1 1 calc R C . C94 C 0.5756(3) 0.59929(17) -0.05750(17) 0.0516(8) Uani 1 1 d . C . H94A H 0.5463 0.5461 -0.0839 0.062 Uiso 1 1 calc R . . C95 C 0.5222(3) 0.62632(18) -0.0089(2) 0.0531(8) Uani 1 1 d . . . H95A H 0.4567 0.5914 -0.0019 0.064 Uiso 1 1 calc R C . C96 C 0.5641(2) 0.70427(16) 0.02964(16) 0.0423(6) Uani 1 1 d . C . H96A H 0.5274 0.7224 0.0630 0.051 Uiso 1 1 calc R . . P10 P 0.21840(7) 0.53606(6) 0.17890(4) 0.05057(19) Uani 1 1 d . . . F11 F 0.1198(3) 0.5410(2) 0.2106(2) 0.1066(12) Uani 1 1 d . . . F12 F 0.1865(2) 0.44171(15) 0.18136(17) 0.0845(7) Uani 1 1 d . . . F13 F 0.2893(3) 0.55476(18) 0.25474(12) 0.0938(9) Uani 1 1 d . . . F14 F 0.25430(19) 0.63181(15) 0.17808(15) 0.0763(6) Uani 1 1 d . . . F15 F 0.1514(3) 0.5210(2) 0.10318(16) 0.1059(10) Uani 1 1 d . . . F16 F 0.3183(2) 0.53140(18) 0.14626(16) 0.0866(8) Uani 1 1 d . . . P20 P 0.36823(6) 1.01165(5) 0.32772(4) 0.04759(18) Uani 1 1 d . . . F21 F 0.24829(17) 0.99757(16) 0.33346(19) 0.0885(8) Uani 1 1 d . . . F22 F 0.3491(2) 0.92122(13) 0.34071(13) 0.0757(6) Uani 1 1 d . . . F23 F 0.4033(2) 1.0441(2) 0.40863(14) 0.0976(10) Uani 1 1 d . . . F24 F 0.3798(2) 1.09757(15) 0.3074(2) 0.1100(12) Uani 1 1 d . . . F25 F 0.33360(19) 0.97185(16) 0.24453(12) 0.0768(7) Uani 1 1 d . . . F26 F 0.48608(16) 1.02352(17) 0.32010(12) 0.0758(7) Uani 1 1 d . . . C100 C 0.4870(10) 0.6934(11) 0.2406(10) 0.064(3) Uiso 0.350(4) 1 d PDU D 1 H10A H 0.4664 0.7027 0.1924 0.077 Uiso 0.350(4) 1 calc PR D 1 H10B H 0.4431 0.6384 0.2450 0.077 Uiso 0.350(4) 1 calc PR D 1 Cl1 Cl 0.6228(2) 0.70167(17) 0.2559(2) 0.0521(7) Uiso 0.350(4) 1 d PDU D 1 Cl2 Cl 0.4667(4) 0.7663(3) 0.3032(2) 0.0776(11) Uiso 0.350(4) 1 d PDU D 1 C101 C 0.4975(12) 0.6967(13) 0.2505(11) 0.072(4) Uiso 0.321(4) 1 d PDU E 2 H10C H 0.4507 0.6950 0.2062 0.086 Uiso 0.321(4) 1 calc PR E 2 H10D H 0.4649 0.6470 0.2692 0.086 Uiso 0.321(4) 1 calc PR E 2 Cl3 Cl 0.6211(3) 0.6937(2) 0.2291(3) 0.0636(9) Uiso 0.321(4) 1 d PDU E 2 Cl4 Cl 0.4998(5) 0.7788(3) 0.3103(3) 0.0884(14) Uiso 0.321(4) 1 d PDU E 2 C102 C 0.4904(12) 0.8626(10) 0.4240(10) 0.045(4) Uiso 0.138(3) 1 d PDU F 3 H10E H 0.4515 0.9011 0.4165 0.054 Uiso 0.138(3) 1 calc PR F 3 H10F H 0.4993 0.8586 0.4746 0.054 Uiso 0.138(3) 1 calc PR F 3 Cl5 Cl 0.6136(7) 0.8988(6) 0.4004(6) 0.082(2) Uiso 0.138(3) 1 d PDU F 3 Cl6 Cl 0.4170(6) 0.7673(5) 0.3743(5) 0.076(2) Uiso 0.138(3) 1 d PDU F 3 C103 C 0.5407(16) 0.6786(12) 0.2321(12) 0.039(4) Uiso 0.100(3) 1 d PDU G 4 H10G H 0.4863 0.6664 0.2623 0.047 Uiso 0.100(3) 1 calc PR G 4 H10H H 0.5298 0.7213 0.2061 0.047 Uiso 0.100(3) 1 calc PR G 4 Cl7 Cl 0.5215(8) 0.5968(6) 0.1745(6) 0.073(3) Uiso 0.100(3) 1 d PDU G 4 Cl8 Cl 0.6586(11) 0.7153(8) 0.2836(8) 0.093(3) Uiso 0.100(3) 1 d PDU G 4 C104 C 0.463(2) 0.799(2) 0.3465(13) 0.068(5) Uiso 0.092(3) 1 d PDU H 5 H10I H 0.4157 0.8175 0.3147 0.081 Uiso 0.092(3) 1 calc PR H 5 H10J H 0.4741 0.7516 0.3193 0.081 Uiso 0.092(3) 1 calc PR H 5 Cl9 Cl 0.4011(8) 0.7673(6) 0.4150(6) 0.066(3) Uiso 0.092(3) 1 d PDU H 5 Cl10 Cl 0.5854(11) 0.8764(9) 0.3718(9) 0.083(3) Uiso 0.092(3) 1 d PDU H 5 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 Ni1 0.0319(2) 0.02330(18) 0.02640(19) 0.00417(14) 0.00975(15) 0.00215(15) Ni2 0.0300(2) 0.02414(18) 0.02647(19) 0.00146(14) 0.00314(15) 0.01037(15) Fe1 0.02884(19) 0.02841(19) 0.0431(2) 0.00872(16) 0.01035(16) 0.00560(15) Fe2 0.02780(19) 0.02490(18) 0.0430(2) 0.00095(15) 0.01110(15) 0.00701(14) S1 0.0423(3) 0.0268(3) 0.0393(3) -0.0001(2) 0.0182(3) 0.0000(2) C2 0.0340(12) 0.0261(10) 0.0270(11) 0.0081(8) 0.0052(9) 0.0035(9) S3 0.0374(3) 0.0254(3) 0.0331(3) 0.0013(2) 0.0144(2) -0.0003(2) N4 0.0324(10) 0.0279(9) 0.0232(9) 0.0049(7) 0.0027(7) 0.0017(8) C5 0.0265(11) 0.0319(11) 0.0287(11) 0.0095(9) 0.0024(8) 0.0049(9) C6 0.0228(10) 0.0334(11) 0.0267(11) 0.0090(9) 0.0021(8) 0.0046(9) N7 0.0275(9) 0.0255(9) 0.0230(8) 0.0053(7) 0.0034(7) 0.0075(7) C8 0.0294(11) 0.0259(10) 0.0247(10) 0.0057(8) 0.0037(8) 0.0066(8) S9 0.0388(3) 0.0302(3) 0.0342(3) -0.0045(2) -0.0047(2) 0.0146(2) S10 0.0334(3) 0.0284(3) 0.0336(3) -0.0035(2) -0.0043(2) 0.0139(2) C11 0.0430(13) 0.0274(11) 0.0270(11) 0.0024(9) 0.0054(10) -0.0006(10) C12 0.0414(18) 0.0422(18) 0.0235(14) -0.0012(11) 0.0050(13) 0.0055(14) C13 0.074(3) 0.031(2) 0.038(2) 0.0079(17) -0.0018(17) 0.0046(17) C14 0.108(4) 0.052(2) 0.041(2) 0.0124(19) -0.005(2) 0.025(2) C15 0.082(3) 0.076(3) 0.0273(17) -0.0105(17) -0.0103(17) 0.044(2) C16 0.052(2) 0.116(4) 0.042(2) 0.002(3) -0.0112(18) 0.007(3) C17 0.048(2) 0.093(3) 0.0342(18) 0.010(2) -0.0004(16) -0.008(2) C18 0.0315(11) 0.0261(10) 0.0292(11) 0.0055(8) 0.0059(9) 0.0113(9) C19 0.0443(13) 0.0277(11) 0.0290(11) 0.0057(9) 0.0091(10) 0.0148(10) C20 0.066(2) 0.065(2) 0.0333(15) -0.0003(14) 0.0121(14) -0.0182(17) C21 0.096(3) 0.066(2) 0.0408(17) 0.0018(16) 0.0271(18) -0.022(2) C22 0.099(3) 0.0440(16) 0.0337(14) 0.0089(12) 0.0235(16) 0.0224(17) C23 0.069(2) 0.069(2) 0.0302(14) 0.0049(13) 0.0052(13) 0.0342(17) C24 0.0443(15) 0.0628(18) 0.0343(14) 0.0045(12) 0.0051(11) 0.0219(14) P25 0.0282(3) 0.0229(2) 0.0269(3) 0.0046(2) 0.0056(2) 0.0039(2) C26 0.0349(12) 0.0258(11) 0.0285(11) 0.0034(8) 0.0039(9) 0.0037(9) C27 0.0379(13) 0.0417(13) 0.0381(13) 0.0094(11) 0.0055(10) 0.0134(11) C28 0.0395(13) 0.0428(14) 0.0404(14) 0.0136(11) 0.0000(11) 0.0093(11) C29 0.0560(17) 0.0498(16) 0.0348(14) 0.0163(12) 0.0080(12) 0.0135(13) C30 0.110(3) 0.082(2) 0.0398(16) 0.0243(16) 0.0332(18) 0.060(2) C31 0.091(2) 0.0598(19) 0.0397(15) 0.0195(14) 0.0268(16) 0.0480(18) C32 0.0318(11) 0.0302(11) 0.0270(11) 0.0063(9) 0.0075(9) 0.0072(9) C33 0.0367(12) 0.0283(11) 0.0346(12) 0.0032(9) 0.0051(10) 0.0073(10) C34 0.0486(15) 0.0317(12) 0.0418(14) 0.0053(10) 0.0093(11) 0.0133(11) C35 0.0452(15) 0.0460(15) 0.0525(16) 0.0082(12) 0.0077(12) 0.0233(13) C36 0.0360(14) 0.0459(16) 0.067(2) 0.0048(14) -0.0028(13) 0.0133(12) C37 0.0367(13) 0.0317(12) 0.0467(15) 0.0031(11) 0.0022(11) 0.0065(10) C38 0.0294(11) 0.0235(10) 0.0389(12) 0.0046(9) 0.0061(9) 0.0071(9) C39 0.0288(12) 0.0363(13) 0.0433(14) -0.0029(10) 0.0027(10) 0.0063(10) C40 0.0285(12) 0.0340(13) 0.073(2) -0.0062(13) 0.0076(13) -0.0007(10) C41 0.0378(14) 0.0271(12) 0.078(2) 0.0156(13) 0.0179(14) 0.0048(11) C42 0.0339(12) 0.0289(12) 0.0525(15) 0.0143(11) 0.0119(11) 0.0078(10) C43 0.0379(13) 0.0325(12) 0.0422(14) 0.0076(10) 0.0174(11) 0.0077(10) C44 0.0455(15) 0.0416(14) 0.0488(16) 0.0117(12) 0.0246(12) 0.0065(12) C45 0.0346(14) 0.0468(16) 0.074(2) 0.0050(15) 0.0230(14) 0.0077(12) C46 0.0379(14) 0.0449(15) 0.067(2) 0.0037(14) 0.0078(13) 0.0188(12) C47 0.0419(14) 0.0334(12) 0.0505(15) 0.0087(11) 0.0115(12) 0.0151(11) P48 0.0398(3) 0.0289(3) 0.0299(3) 0.0059(2) 0.0148(2) 0.0042(2) C49 0.0460(14) 0.0330(12) 0.0306(12) 0.0048(10) 0.0088(10) 0.0014(11) C50 0.0503(16) 0.0411(14) 0.0361(14) 0.0047(11) 0.0033(12) 0.0042(12) C51 0.061(2) 0.0487(17) 0.0515(18) 0.0099(14) -0.0083(15) 0.0087(15) C52 0.084(3) 0.0507(18) 0.0462(18) 0.0196(14) -0.0083(17) -0.0007(18) C53 0.077(2) 0.062(2) 0.0351(15) 0.0178(14) 0.0095(15) -0.0020(18) C54 0.0614(18) 0.0491(16) 0.0349(14) 0.0109(12) 0.0155(13) 0.0044(14) C55 0.044(3) 0.032(2) 0.030(2) 0.0063(15) 0.020(2) 0.0037(19) C56 0.051(3) 0.042(2) 0.038(2) 0.0044(18) 0.019(2) 0.013(2) C57 0.058(5) 0.052(3) 0.039(2) -0.0038(19) 0.012(3) 0.012(3) C58 0.080(6) 0.045(3) 0.053(3) 0.003(2) 0.025(3) 0.022(3) C59 0.073(5) 0.055(3) 0.062(3) 0.008(2) 0.028(3) 0.033(3) C60 0.054(3) 0.045(2) 0.045(3) 0.009(2) 0.019(3) 0.021(2) P61 0.0341(3) 0.0260(3) 0.0284(3) 0.0010(2) 0.0042(2) 0.0115(2) C62 0.044(3) 0.043(2) 0.0288(19) 0.0024(15) 0.0056(16) 0.023(2) C63 0.050(3) 0.054(2) 0.036(2) 0.0095(18) 0.012(2) 0.020(2) C64 0.087(5) 0.071(3) 0.045(3) 0.026(2) 0.026(3) 0.041(4) C65 0.117(6) 0.082(4) 0.033(2) 0.015(2) 0.022(3) 0.056(5) C66 0.111(6) 0.067(4) 0.030(2) -0.008(2) 0.009(3) 0.042(4) C67 0.073(4) 0.050(3) 0.033(2) -0.0027(19) 0.004(2) 0.032(3) C68 0.0314(12) 0.0295(11) 0.0405(13) -0.0046(10) 0.0032(10) 0.0119(9) C69 0.0424(14) 0.0352(13) 0.0493(16) -0.0037(11) -0.0069(12) 0.0140(11) C70 0.0312(13) 0.0482(16) 0.071(2) -0.0129(15) -0.0071(13) 0.0123(12) C71 0.0314(14) 0.0466(16) 0.083(2) -0.0002(16) 0.0136(14) 0.0093(12) C72 0.0353(14) 0.0500(16) 0.068(2) 0.0134(14) 0.0183(13) 0.0144(12) C73 0.0311(12) 0.0429(14) 0.0452(14) 0.0058(11) 0.0090(10) 0.0119(11) C74 0.0315(11) 0.0237(10) 0.0354(12) 0.0018(9) 0.0072(9) 0.0076(9) C75 0.0406(13) 0.0289(11) 0.0390(13) 0.0000(10) 0.0123(10) 0.0112(10) C76 0.0368(13) 0.0277(11) 0.0499(15) -0.0021(10) 0.0117(11) 0.0123(10) C77 0.0320(12) 0.0278(11) 0.0506(15) 0.0066(10) 0.0060(10) 0.0093(10) C78 0.0297(11) 0.0282(11) 0.0392(13) 0.0059(9) 0.0071(9) 0.0064(9) C79 0.0297(11) 0.0263(11) 0.0451(14) -0.0009(10) 0.0070(10) 0.0067(9) C80 0.0305(12) 0.0350(13) 0.0602(17) -0.0116(12) -0.0019(11) 0.0111(10) C81 0.0271(13) 0.0405(15) 0.091(3) -0.0127(16) 0.0099(14) 0.0088(11) C82 0.0419(15) 0.0328(14) 0.090(3) -0.0032(15) 0.0348(16) 0.0013(12) C83 0.0442(14) 0.0265(12) 0.0592(17) 0.0040(11) 0.0264(13) 0.0052(10) P84 0.0286(3) 0.0257(3) 0.0289(3) 0.0012(2) 0.0034(2) 0.0100(2) C85 0.0351(12) 0.0311(11) 0.0319(12) 0.0034(9) 0.0067(9) 0.0159(10) C86 0.0330(12) 0.0412(13) 0.0390(13) 0.0072(10) 0.0092(10) 0.0138(10) C87 0.0422(15) 0.0506(16) 0.0511(16) 0.0172(13) 0.0169(12) 0.0158(12) C88 0.0585(18) 0.0559(17) 0.0448(16) 0.0214(13) 0.0197(13) 0.0281(15) C89 0.0551(17) 0.0512(16) 0.0361(14) 0.0124(12) 0.0069(12) 0.0273(14) C90 0.0423(14) 0.0382(13) 0.0362(13) 0.0058(10) 0.0023(10) 0.0161(11) C91 0.0363(12) 0.0290(11) 0.0317(11) 0.0007(9) -0.0029(9) 0.0139(10) C92 0.0448(14) 0.0376(13) 0.0320(12) -0.0005(10) -0.0003(10) 0.0190(11) C93 0.0645(18) 0.0434(15) 0.0325(13) -0.0039(11) -0.0041(12) 0.0286(14) C94 0.0646(19) 0.0326(13) 0.0482(16) -0.0087(12) -0.0166(14) 0.0192(13) C95 0.0460(16) 0.0325(13) 0.067(2) -0.0011(13) -0.0075(14) 0.0040(12) C96 0.0393(14) 0.0326(13) 0.0501(16) 0.0000(11) 0.0021(11) 0.0098(11) P10 0.0581(4) 0.0698(5) 0.0400(4) 0.0133(3) 0.0117(3) 0.0414(4) F11 0.111(2) 0.120(2) 0.152(3) 0.074(2) 0.088(2) 0.082(2) F12 0.0768(15) 0.0677(14) 0.116(2) 0.0164(14) 0.0099(14) 0.0358(12) F13 0.151(3) 0.0947(18) 0.0456(12) 0.0047(11) -0.0127(14) 0.0696(18) F14 0.0698(13) 0.0771(14) 0.1005(18) 0.0364(13) 0.0171(12) 0.0415(12) F15 0.0948(19) 0.142(3) 0.0688(16) 0.0249(17) -0.0212(14) 0.0338(19) F16 0.0733(15) 0.1037(19) 0.0939(18) -0.0049(15) 0.0332(13) 0.0454(14) P20 0.0369(3) 0.0442(4) 0.0557(4) 0.0174(3) 0.0070(3) 0.0020(3) F21 0.0405(11) 0.0731(15) 0.144(3) 0.0148(15) 0.0269(13) 0.0040(10) F22 0.0960(17) 0.0537(12) 0.0689(14) 0.0174(10) 0.0106(12) 0.0114(11) F23 0.0710(15) 0.120(2) 0.0638(14) -0.0312(14) 0.0146(12) -0.0065(14) F24 0.0824(17) 0.0496(13) 0.189(4) 0.0488(17) 0.0089(19) 0.0042(12) F25 0.0678(13) 0.0926(16) 0.0545(12) 0.0231(11) -0.0019(10) 0.0052(12) F26 0.0430(10) 0.1136(19) 0.0596(12) 0.0084(12) 0.0100(9) 0.0114(11) _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 Ni1 P48 2.2070(7) . ? Ni1 P25 2.2119(7) . ? Ni1 S1 2.2143(7) . ? Ni1 S3 2.2162(7) . ? Ni2 P84 2.2007(7) . ? Ni2 S10 2.2100(7) . ? Ni2 P61 2.2213(7) . ? Ni2 S9 2.2230(7) . ? Fe1 C43 2.014(3) . ? Fe1 C38 2.016(2) . ? Fe1 C44 2.027(3) . ? Fe1 C42 2.030(3) . ? Fe1 C47 2.037(3) . ? Fe1 C39 2.052(3) . ? Fe1 C45 2.062(3) . ? Fe1 C41 2.064(3) . ? Fe1 C40 2.065(3) . ? Fe1 C46 2.070(3) . ? Fe2 C79 2.012(2) . ? Fe2 C78 2.018(2) . ? Fe2 C74 2.022(2) . ? Fe2 C83 2.035(3) . ? Fe2 C80 2.038(3) . ? Fe2 C75 2.046(3) . ? Fe2 C77 2.058(2) . ? Fe2 C81 2.063(3) . ? Fe2 C82 2.069(3) . ? Fe2 C76 2.071(2) . ? S1 C2 1.727(3) . ? C2 N4 1.316(3) . ? C2 S3 1.711(2) . ? N4 C5 1.468(3) . ? N4 C11 1.479(3) . ? C5 C6 1.527(3) . ? C6 N7 1.475(3) . ? N7 C8 1.314(3) . ? N7 C18 1.481(3) . ? C8 S9 1.713(2) . ? C8 S10 1.718(2) . ? C11 C12 1.510(3) . ? C11 C12' 1.594(11) . ? C12 C13 1.3900 . ? C12 C17 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C12' C13' 1.3900 . ? C12' C17' 1.3900 . ? C13' C14' 1.3900 . ? C14' C15' 1.3900 . ? C15' C16' 1.3900 . ? C16' C17' 1.3900 . ? C18 C19 1.506(3) . ? C19 C24 1.377(4) . ? C19 C20 1.379(4) . ? C20 C21 1.387(5) . ? C21 C22 1.369(6) . ? C22 C23 1.353(5) . ? C23 C24 1.390(5) . ? P25 C38 1.803(2) . ? P25 C26 1.820(2) . ? P25 C32 1.829(3) . ? C26 C31 1.379(4) . ? C26 C27 1.391(4) . ? C27 C28 1.386(4) . ? C28 C29 1.369(5) . ? C29 C30 1.385(5) . ? C30 C31 1.389(5) . ? C32 C37 1.392(4) . ? C32 C33 1.401(3) . ? C33 C34 1.379(4) . ? C34 C35 1.384(4) . ? C35 C36 1.383(5) . ? C36 C37 1.387(4) . ? C38 C42 1.433(4) . ? C38 C39 1.435(4) . ? C39 C40 1.428(4) . ? C40 C41 1.407(5) . ? C41 C42 1.429(4) . ? C43 C47 1.438(4) . ? C43 C44 1.441(4) . ? C43 P48 1.800(3) . ? C44 C45 1.417(5) . ? C45 C46 1.415(5) . ? C46 C47 1.426(4) . ? P48 C55' 1.802(7) . ? P48 C49 1.816(3) . ? P48 C55 1.864(3) . ? C49 C50 1.389(5) . ? C49 C54 1.405(4) . ? C50 C51 1.384(5) . ? C51 C52 1.386(6) . ? C52 C53 1.380(7) . ? C53 C54 1.382(5) . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C55' C56' 1.3900 . ? C55' C60' 1.3900 . ? C56' C57' 1.3900 . ? C57' C58' 1.3900 . ? C58' C59' 1.3900 . ? C59' C60' 1.3900 . ? P61 C74 1.814(2) . ? P61 C62 1.822(2) . ? P61 C68 1.839(3) . ? P61 C62' 1.846(7) . ? C62 C63 1.3900 . ? C62 C67 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C62' C63' 1.3900 . ? C62' C67' 1.3900 . ? C63' C64' 1.3900 . ? C64' C65' 1.3900 . ? C65' C66' 1.3900 . ? C66' C67' 1.3900 . ? C68 C69 1.396(4) . ? C68 C73 1.397(4) . ? C69 C70 1.401(5) . ? C70 C71 1.366(6) . ? C71 C72 1.377(5) . ? C72 C73 1.388(4) . ? C74 C78 1.439(4) . ? C74 C75 1.443(4) . ? C75 C76 1.420(4) . ? C76 C77 1.411(4) . ? C77 C78 1.427(4) . ? C79 C83 1.443(4) . ? C79 C80 1.447(4) . ? C79 P84 1.797(3) . ? C80 C81 1.423(5) . ? C81 C82 1.416(6) . ? C82 C83 1.424(4) . ? P84 C85 1.816(3) . ? P84 C91 1.830(2) . ? C85 C86 1.394(4) . ? C85 C90 1.398(4) . ? C86 C87 1.388(4) . ? C87 C88 1.388(5) . ? C88 C89 1.381(5) . ? C89 C90 1.388(4) . ? C91 C92 1.391(4) . ? C91 C96 1.392(4) . ? C92 C93 1.393(4) . ? C93 C94 1.382(5) . ? C94 C95 1.386(5) . ? C95 C96 1.392(4) . ? P10 F11 1.562(3) . ? P10 F15 1.571(3) . ? P10 F16 1.586(2) . ? P10 F13 1.589(2) . ? P10 F12 1.594(3) . ? P10 F14 1.610(3) . ? P20 F23 1.565(3) . ? P20 F26 1.572(2) . ? P20 F24 1.577(3) . ? P20 F21 1.586(2) . ? P20 F22 1.592(2) . ? P20 F25 1.630(3) . ? C100 Cl2 1.771(11) . ? C100 Cl1 1.779(11) . ? C101 Cl4 1.733(12) . ? C101 Cl3 1.790(12) . ? C102 Cl5 1.736(13) . ? C102 Cl6 1.756(13) . ? C103 Cl7 1.645(14) . ? C103 Cl8 1.662(15) . ? C104 Cl9 1.723(16) . ? C104 Cl10 1.760(16) . ? 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 P48 Ni1 P25 100.76(3) . . ? P48 Ni1 S1 92.94(3) . . ? P25 Ni1 S1 166.29(3) . . ? P48 Ni1 S3 170.59(3) . . ? P25 Ni1 S3 87.94(2) . . ? S1 Ni1 S3 78.41(2) . . ? P84 Ni2 S10 92.06(2) . . ? P84 Ni2 P61 101.05(3) . . ? S10 Ni2 P61 166.89(3) . . ? P84 Ni2 S9 170.11(3) . . ? S10 Ni2 S9 78.27(2) . . ? P61 Ni2 S9 88.63(2) . . ? C43 Fe1 C38 108.55(10) . . ? C43 Fe1 C44 41.76(11) . . ? C38 Fe1 C44 136.11(12) . . ? C43 Fe1 C42 109.44(12) . . ? C38 Fe1 C42 41.48(10) . . ? C44 Fe1 C42 108.28(13) . . ? C43 Fe1 C47 41.57(12) . . ? C38 Fe1 C47 111.81(11) . . ? C44 Fe1 C47 69.40(12) . . ? C42 Fe1 C47 140.28(11) . . ? C43 Fe1 C39 137.43(10) . . ? C38 Fe1 C39 41.29(10) . . ? C44 Fe1 C39 177.34(12) . . ? C42 Fe1 C39 69.32(11) . . ? C47 Fe1 C39 111.61(12) . . ? C43 Fe1 C45 69.10(12) . . ? C38 Fe1 C45 176.64(13) . . ? C44 Fe1 C45 40.56(14) . . ? C42 Fe1 C45 136.45(13) . . ? C47 Fe1 C45 68.21(12) . . ? C39 Fe1 C45 142.03(13) . . ? C43 Fe1 C41 139.19(13) . . ? C38 Fe1 C41 68.97(10) . . ? C44 Fe1 C41 110.68(13) . . ? C42 Fe1 C41 40.84(11) . . ? C47 Fe1 C41 178.87(12) . . ? C39 Fe1 C41 68.37(13) . . ? C45 Fe1 C41 111.07(13) . . ? C43 Fe1 C40 177.07(11) . . ? C38 Fe1 C40 68.56(10) . . ? C44 Fe1 C40 140.08(12) . . ? C42 Fe1 C40 68.15(12) . . ? C47 Fe1 C40 139.44(14) . . ? C39 Fe1 C40 40.57(12) . . ? C45 Fe1 C40 113.76(12) . . ? C41 Fe1 C40 39.86(15) . . ? C43 Fe1 C46 69.21(12) . . ? C38 Fe1 C46 141.96(12) . . ? C44 Fe1 C46 68.42(14) . . ? C42 Fe1 C46 176.40(13) . . ? C47 Fe1 C46 40.63(12) . . ? C39 Fe1 C46 114.01(13) . . ? C45 Fe1 C46 40.04(15) . . ? C41 Fe1 C46 138.27(12) . . ? C40 Fe1 C46 113.30(13) . . ? C79 Fe2 C78 110.10(11) . . ? C79 Fe2 C74 108.45(10) . . ? C78 Fe2 C74 41.73(10) . . ? C79 Fe2 C83 41.78(12) . . ? C78 Fe2 C83 139.61(11) . . ? C74 Fe2 C83 109.94(12) . . ? C79 Fe2 C80 41.85(11) . . ? C78 Fe2 C80 109.99(12) . . ? C74 Fe2 C80 137.36(11) . . ? C83 Fe2 C80 69.81(13) . . ? C79 Fe2 C75 137.14(11) . . ? C78 Fe2 C75 69.51(10) . . ? C74 Fe2 C75 41.56(10) . . ? C83 Fe2 C75 109.81(12) . . ? C80 Fe2 C75 178.80(11) . . ? C79 Fe2 C77 140.41(12) . . ? C78 Fe2 C77 40.97(10) . . ? C74 Fe2 C77 69.14(10) . . ? C83 Fe2 C77 177.70(12) . . ? C80 Fe2 C77 112.35(12) . . ? C75 Fe2 C77 68.05(11) . . ? C79 Fe2 C81 69.11(11) . . ? C78 Fe2 C81 138.46(14) . . ? C74 Fe2 C81 177.55(11) . . ? C83 Fe2 C81 68.45(14) . . ? C80 Fe2 C81 40.60(13) . . ? C75 Fe2 C81 140.45(13) . . ? C77 Fe2 C81 112.54(13) . . ? C79 Fe2 C82 69.09(11) . . ? C78 Fe2 C82 178.42(14) . . ? C74 Fe2 C82 139.69(14) . . ? C83 Fe2 C82 40.59(13) . . ? C80 Fe2 C82 68.48(15) . . ? C75 Fe2 C82 112.03(14) . . ? C77 Fe2 C82 138.93(12) . . ? C81 Fe2 C82 40.08(17) . . ? C79 Fe2 C76 177.32(11) . . ? C78 Fe2 C76 68.64(10) . . ? C74 Fe2 C76 68.99(10) . . ? C83 Fe2 C76 137.80(12) . . ? C80 Fe2 C76 140.65(12) . . ? C75 Fe2 C76 40.35(11) . . ? C77 Fe2 C76 39.97(12) . . ? C81 Fe2 C76 113.45(11) . . ? C82 Fe2 C76 112.23(12) . . ? C2 S1 Ni1 85.27(8) . . ? N4 C2 S3 124.75(19) . . ? N4 C2 S1 126.12(19) . . ? S3 C2 S1 109.07(13) . . ? C2 S3 Ni1 85.59(8) . . ? C2 N4 C5 121.0(2) . . ? C2 N4 C11 121.3(2) . . ? C5 N4 C11 117.55(19) . . ? N4 C5 C6 113.53(19) . . ? N7 C6 C5 113.30(18) . . ? C8 N7 C6 120.71(19) . . ? C8 N7 C18 120.05(18) . . ? C6 N7 C18 119.04(18) . . ? N7 C8 S9 125.57(17) . . ? N7 C8 S10 125.12(17) . . ? S9 C8 S10 109.31(13) . . ? C8 S9 Ni2 85.99(8) . . ? C8 S10 Ni2 86.29(8) . . ? N4 C11 C12 113.3(2) . . ? N4 C11 C12' 108.7(4) . . ? C13 C12 C17 120.0 . . ? C13 C12 C11 121.6(2) . . ? C17 C12 C11 118.4(2) . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C16 C17 C12 120.0 . . ? C13' C12' C17' 120.0 . . ? C13' C12' C11 114.4(12) . . ? C17' C12' C11 125.6(12) . . ? C14' C13' C12' 120.0 . . ? C13' C14' C15' 120.0 . . ? C16' C15' C14' 120.0 . . ? C15' C16' C17' 120.0 . . ? C16' C17' C12' 120.0 . . ? N7 C18 C19 112.10(18) . . ? C24 C19 C20 117.7(3) . . ? C24 C19 C18 120.3(2) . . ? C20 C19 C18 122.0(2) . . ? C19 C20 C21 121.0(3) . . ? C22 C21 C20 120.0(3) . . ? C23 C22 C21 119.9(3) . . ? C22 C23 C24 120.2(3) . . ? C19 C24 C23 121.2(3) . . ? C38 P25 C26 104.58(11) . . ? C38 P25 C32 100.47(11) . . ? C26 P25 C32 106.64(11) . . ? C38 P25 Ni1 122.47(8) . . ? C26 P25 Ni1 104.32(8) . . ? C32 P25 Ni1 116.99(8) . . ? C31 C26 C27 119.1(2) . . ? C31 C26 P25 122.7(2) . . ? C27 C26 P25 117.9(2) . . ? C28 C27 C26 120.5(3) . . ? C29 C28 C27 120.2(3) . . ? C28 C29 C30 119.8(3) . . ? C29 C30 C31 120.2(3) . . ? C26 C31 C30 120.2(3) . . ? C37 C32 C33 118.9(2) . . ? C37 C32 P25 121.75(19) . . ? C33 C32 P25 119.37(18) . . ? C34 C33 C32 120.4(2) . . ? C33 C34 C35 120.4(3) . . ? C36 C35 C34 119.7(3) . . ? C35 C36 C37 120.4(3) . . ? C36 C37 C32 120.2(3) . . ? C42 C38 C39 108.1(2) . . ? C42 C38 P25 124.83(19) . . ? C39 C38 P25 127.1(2) . . ? C42 C38 Fe1 69.77(15) . . ? C39 C38 Fe1 70.69(15) . . ? P25 C38 Fe1 126.05(13) . . ? C40 C39 C38 106.9(3) . . ? C40 C39 Fe1 70.21(18) . . ? C38 C39 Fe1 68.02(15) . . ? C41 C40 C39 109.3(2) . . ? C41 C40 Fe1 70.02(18) . . ? C39 C40 Fe1 69.22(16) . . ? C40 C41 C42 108.0(3) . . ? C40 C41 Fe1 70.13(17) . . ? C42 C41 Fe1 68.31(15) . . ? C41 C42 C38 107.7(3) . . ? C41 C42 Fe1 70.84(16) . . ? C38 C42 Fe1 68.75(14) . . ? C47 C43 C44 107.0(2) . . ? C47 C43 P48 123.5(2) . . ? C44 C43 P48 129.5(2) . . ? C47 C43 Fe1 70.07(15) . . ? C44 C43 Fe1 69.61(16) . . ? P48 C43 Fe1 122.97(14) . . ? C45 C44 C43 108.0(3) . . ? C45 C44 Fe1 71.02(18) . . ? C43 C44 Fe1 68.63(16) . . ? C46 C45 C44 108.9(3) . . ? C46 C45 Fe1 70.32(17) . . ? C44 C45 Fe1 68.42(16) . . ? C45 C46 C47 108.0(3) . . ? C45 C46 Fe1 69.64(18) . . ? C47 C46 Fe1 68.43(16) . . ? C46 C47 C43 108.2(3) . . ? C46 C47 Fe1 70.94(16) . . ? C43 C47 Fe1 68.36(15) . . ? C43 P48 C55' 110.8(4) . . ? C43 P48 C49 107.06(12) . . ? C55' P48 C49 97.2(4) . . ? C43 P48 C55 101.0(2) . . ? C49 P48 C55 105.0(2) . . ? C43 P48 Ni1 116.54(9) . . ? C55' P48 Ni1 112.3(4) . . ? C49 P48 Ni1 111.10(10) . . ? C55 P48 Ni1 115.01(15) . . ? C50 C49 C54 119.2(3) . . ? C50 C49 P48 119.9(2) . . ? C54 C49 P48 120.9(3) . . ? C51 C50 C49 120.6(3) . . ? C50 C51 C52 119.8(4) . . ? C53 C52 C51 120.2(3) . . ? C52 C53 C54 120.4(3) . . ? C53 C54 C49 119.8(4) . . ? C56 C55 C60 120.0 . . ? C56 C55 P48 117.2(2) . . ? C60 C55 P48 122.8(2) . . ? C57 C56 C55 120.0 . . ? C56 C57 C58 120.0 . . ? C59 C58 C57 120.0 . . ? C60 C59 C58 120.0 . . ? C59 C60 C55 120.0 . . ? C56' C55' C60' 120.0 . . ? C56' C55' P48 123.0(5) . . ? C60' C55' P48 116.7(5) . . ? C55' C56' C57' 120.0 . . ? C58' C57' C56' 120.0 . . ? C57' C58' C59' 120.0 . . ? C58' C59' C60' 120.0 . . ? C59' C60' C55' 120.0 . . ? C74 P61 C62 101.09(19) . . ? C74 P61 C68 103.93(11) . . ? C62 P61 C68 108.5(2) . . ? C74 P61 C62' 106.3(4) . . ? C68 P61 C62' 98.8(4) . . ? C74 P61 Ni2 123.62(8) . . ? C62 P61 Ni2 106.59(14) . . ? C68 P61 Ni2 111.97(8) . . ? C62' P61 Ni2 109.3(4) . . ? C63 C62 C67 120.0 . . ? C63 C62 P61 119.1(2) . . ? C67 C62 P61 120.9(2) . . ? C62 C63 C64 120.0 . . ? C63 C64 C65 120.0 . . ? C64 C65 C66 120.0 . . ? C67 C66 C65 120.0 . . ? C66 C67 C62 120.0 . . ? C63' C62' C67' 120.0 . . ? C63' C62' P61 118.3(6) . . ? C67' C62' P61 121.7(6) . . ? C64' C63' C62' 120.0 . . ? C63' C64' C65' 120.0 . . ? C64' C65' C66' 120.0 . . ? C67' C66' C65' 120.0 . . ? C66' C67' C62' 120.0 . . ? C69 C68 C73 118.1(3) . . ? C69 C68 P61 121.4(2) . . ? C73 C68 P61 120.48(19) . . ? C68 C69 C70 120.0(3) . . ? C71 C70 C69 120.8(3) . . ? C70 C71 C72 120.0(3) . . ? C71 C72 C73 120.0(3) . . ? C72 C73 C68 121.1(3) . . ? C78 C74 C75 107.0(2) . . ? C78 C74 P61 128.36(19) . . ? C75 C74 P61 124.58(19) . . ? C78 C74 Fe2 68.99(13) . . ? C75 C74 Fe2 70.10(14) . . ? P61 C74 Fe2 123.39(12) . . ? C76 C75 C74 108.1(2) . . ? C76 C75 Fe2 70.78(15) . . ? C74 C75 Fe2 68.34(14) . . ? C77 C76 C75 108.4(2) . . ? C77 C76 Fe2 69.52(14) . . ? C75 C76 Fe2 68.88(14) . . ? C76 C77 C78 108.7(2) . . ? C76 C77 Fe2 70.51(15) . . ? C78 C77 Fe2 68.03(14) . . ? C77 C78 C74 107.8(2) . . ? C77 C78 Fe2 71.00(14) . . ? C74 C78 Fe2 69.28(14) . . ? C83 C79 C80 107.5(2) . . ? C83 C79 P84 123.5(2) . . ? C80 C79 P84 128.9(2) . . ? C83 C79 Fe2 69.97(15) . . ? C80 C79 Fe2 70.07(15) . . ? P84 C79 Fe2 123.71(13) . . ? C81 C80 C79 107.3(3) . . ? C81 C80 Fe2 70.62(18) . . ? C79 C80 Fe2 68.08(15) . . ? C82 C81 C80 109.0(3) . . ? C82 C81 Fe2 70.19(18) . . ? C80 C81 Fe2 68.77(15) . . ? C81 C82 C83 108.5(3) . . ? C81 C82 Fe2 69.73(18) . . ? C83 C82 Fe2 68.41(15) . . ? C82 C83 C79 107.7(3) . . ? C82 C83 Fe2 71.00(17) . . ? C79 C83 Fe2 68.25(15) . . ? C79 P84 C85 106.67(12) . . ? C79 P84 C91 102.91(11) . . ? C85 P84 C91 101.81(11) . . ? C79 P84 Ni2 116.30(9) . . ? C85 P84 Ni2 111.27(8) . . ? C91 P84 Ni2 116.41(8) . . ? C86 C85 C90 119.5(2) . . ? C86 C85 P84 120.08(19) . . ? C90 C85 P84 120.4(2) . . ? C87 C86 C85 120.1(3) . . ? C86 C87 C88 120.0(3) . . ? C89 C88 C87 120.4(3) . . ? C88 C89 C90 120.1(3) . . ? C89 C90 C85 120.1(3) . . ? C92 C91 C96 119.4(2) . . ? C92 C91 P84 119.4(2) . . ? C96 C91 P84 121.3(2) . . ? C91 C92 C93 120.6(3) . . ? C94 C93 C92 119.7(3) . . ? C93 C94 C95 120.0(3) . . ? C94 C95 C96 120.4(3) . . ? C95 C96 C91 119.9(3) . . ? F11 P10 F15 88.9(2) . . ? F11 P10 F16 179.56(18) . . ? F15 P10 F16 90.71(18) . . ? F11 P10 F13 92.2(2) . . ? F15 P10 F13 177.6(2) . . ? F16 P10 F13 88.19(17) . . ? F11 P10 F12 90.90(16) . . ? F15 P10 F12 92.37(18) . . ? F16 P10 F12 89.37(15) . . ? F13 P10 F12 89.79(15) . . ? F11 P10 F14 90.09(15) . . ? F15 P10 F14 89.28(17) . . ? F16 P10 F14 89.66(15) . . ? F13 P10 F14 88.54(15) . . ? F12 P10 F14 178.09(14) . . ? F23 P20 F26 90.33(14) . . ? F23 P20 F24 94.5(2) . . ? F26 P20 F24 90.00(16) . . ? F23 P20 F21 91.17(17) . . ? F26 P20 F21 178.29(17) . . ? F24 P20 F21 90.70(16) . . ? F23 P20 F22 90.93(17) . . ? F26 P20 F22 91.90(15) . . ? F24 P20 F22 174.27(18) . . ? F21 P20 F22 87.27(15) . . ? F23 P20 F25 175.80(19) . . ? F26 P20 F25 88.33(13) . . ? F24 P20 F25 89.51(18) . . ? F21 P20 F25 90.11(16) . . ? F22 P20 F25 85.14(13) . . ? Cl2 C100 Cl1 108.7(7) . . ? Cl4 C101 Cl3 117.2(9) . . ? Cl5 C102 Cl6 111.1(10) . . ? Cl7 C103 Cl8 115.7(13) . . ? Cl9 C104 Cl10 115.0(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 72.59 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.977 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.067 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 764406' #TrackingRef 'EJIC 01-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H74 Fe2 N2 P4 Pd2 S4, 2(F6 P), C H2 Cl2, C2 H6 O' _chemical_formula_sum 'C89 H82 Cl2 F12 Fe2 N2 O P6 Pd2 S4' _chemical_formula_weight 2133.03 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' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 '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' 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 13.8220(2) _cell_length_b 17.8518(3) _cell_length_c 19.3592(3) _cell_angle_alpha 98.2051(14) _cell_angle_beta 96.9952(14) _cell_angle_gamma 108.4619(17) _cell_volume 4413.11(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 23455 _cell_measurement_theta_min 2.9672 _cell_measurement_theta_max 32.5423 _exptl_crystal_description blocks _exptl_crystal_colour Orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2156 _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.873 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ? _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46924 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 32.64 _reflns_number_total 28689 _reflns_number_gt 19906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Two partial occupancy orientations were identified for both the C19- and C26-based phenyl rings. SADI distance restraints were used for the C18-C19/C18-C19' and P25-C26/P25-C26' pairs of bonds. SIMU restraints were used for the equivalent adjacent atoms in each case, e.g. C21 with C21', and C30 with C30' etc. The two orientations of the phenyl ring in each case were constrained to be idealised hexagons. Two partial occupancy orientations were identified for the P20-based PF6 anion. SADI restraints were used for all of the P-F and cis F...F distances, and a SIMU restraint was used for adjacent fluorine atoms Three partial occupancy orientations were identified for both the dichloromethane and ethanol solvent molecules. A single SADI restraint was used for each of the six C-Cl bonds, and another was used for the three Cl...Cl distances. A SIMU restraint was used for the three carbon atoms, and two separate ones for the two pairs of three proximal chlorine atoms. Separate SADI restraints were used the three O-C, three C-C and three O...C distances. Separate SIMU restraints were used the three proximal oxygen, C(methylene) and C(methyl) atoms. The O-H protons of the three ethanol orientations could not be located, and so the atom list for the asymmetric unit is low by one hydrogen atom. ; _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^)+(0.0612P)^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 28689 _refine_ls_number_parameters 1151 _refine_ls_number_restraints 550 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.818358(14) 0.572245(10) 0.336958(9) 0.02073(4) Uani 1 1 d . . . Pd2 Pd 0.859858(14) 0.882338(10) 0.150657(9) 0.01994(4) Uani 1 1 d . . . Fe1 Fe 0.52662(3) 0.38561(2) 0.30906(2) 0.02799(8) Uani 1 1 d . . . Fe2 Fe 0.61847(3) 0.98336(2) 0.15500(2) 0.02533(8) Uani 1 1 d . . . S1 S 0.89961(5) 0.70935(4) 0.38815(4) 0.02930(14) Uani 1 1 d . . . C2 C 0.98807(19) 0.70758(14) 0.33264(12) 0.0221(5) Uani 1 1 d . . . S3 S 0.94679(5) 0.61997(4) 0.27038(3) 0.02642(13) Uani 1 1 d . . . N4 N 1.07818(16) 0.76432(12) 0.33867(10) 0.0212(4) Uani 1 1 d . B . C5 C 1.15571(18) 0.75242(14) 0.29638(12) 0.0217(5) Uani 1 1 d . . . H5A H 1.1393 0.6940 0.2796 0.026 Uiso 1 1 calc R D . H5B H 1.2249 0.7734 0.3272 0.026 Uiso 1 1 calc R . . C6 C 1.16028(19) 0.79378(14) 0.23248(12) 0.0225(5) Uani 1 1 d . . . H6A H 1.1724 0.8516 0.2490 0.027 Uiso 1 1 calc R . . H6B H 1.2199 0.7895 0.2105 0.027 Uiso 1 1 calc R . . N7 N 1.06549(15) 0.75952(12) 0.17844(10) 0.0203(4) Uani 1 1 d . . . C8 C 0.99714(19) 0.79693(14) 0.17141(12) 0.0219(5) Uani 1 1 d . D . S9 S 1.00999(5) 0.88684(4) 0.22453(3) 0.02788(13) Uani 1 1 d . D . S10 S 0.88742(5) 0.76301(4) 0.10813(3) 0.02712(13) Uani 1 1 d . D . C11 C 1.1105(2) 0.83859(14) 0.39258(13) 0.0260(5) Uani 1 1 d . . . H11A H 1.0482 0.8481 0.4064 0.031 Uiso 1 1 calc R A 1 H11B H 1.1481 0.8846 0.3718 0.031 Uiso 1 1 calc R A 1 C12 C 1.1796(2) 0.83497(17) 0.45811(13) 0.0300(6) Uani 1 1 d . B 1 C13 C 1.1527(3) 0.7715(2) 0.49246(17) 0.0482(8) Uani 1 1 d . B 1 H13A H 1.0910 0.7271 0.4737 0.058 Uiso 1 1 calc R B 1 C14 C 1.2151(3) 0.7716(2) 0.55486(18) 0.0589(10) Uani 1 1 d . B 1 H14A H 1.1951 0.7276 0.5787 0.071 Uiso 1 1 calc R B 1 C15 C 1.3045(3) 0.8342(3) 0.58159(17) 0.0581(10) Uani 1 1 d . B 1 H15A H 1.3488 0.8330 0.6226 0.070 Uiso 1 1 calc R B 1 C16 C 1.3299(3) 0.8989(3) 0.54896(18) 0.0597(10) Uani 1 1 d . B 1 H16A H 1.3909 0.9437 0.5686 0.072 Uiso 1 1 calc R B 1 C17 C 1.2679(3) 0.9002(2) 0.48777(16) 0.0460(8) Uani 1 1 d . B 1 H17A H 1.2861 0.9459 0.4660 0.055 Uiso 1 1 calc R B 1 C18 C 1.0518(2) 0.68574(14) 0.12691(12) 0.0237(5) Uani 1 1 d D C . H18A H 0.9791 0.6492 0.1200 0.028 Uiso 0.845(7) 1 calc PR C 1 H18B H 1.0971 0.6577 0.1464 0.028 Uiso 0.845(7) 1 calc PR C 1 H18C H 0.9795 0.6543 0.1141 0.028 Uiso 0.155(7) 1 d PR C 2 H18D H 1.0873 0.6541 0.1481 0.028 Uiso 0.155(7) 1 d PR C 2 C19 C 1.0773(2) 0.70363(16) 0.05669(10) 0.0300(8) Uani 0.845(7) 1 d PGDU C 1 C20 C 1.1673(3) 0.76534(17) 0.05369(11) 0.0574(15) Uani 0.845(7) 1 d PGU C 1 H20A H 1.2126 0.7964 0.0962 0.069 Uiso 0.845(7) 1 calc PR C 1 C21 C 1.1909(3) 0.78162(16) -0.01156(15) 0.0671(16) Uani 0.845(7) 1 d PGU C 1 H21A H 1.2524 0.8238 -0.0136 0.081 Uiso 0.845(7) 1 calc PR C 1 C22 C 1.1245(3) 0.73620(18) -0.07381(11) 0.0534(13) Uani 0.845(7) 1 d PGU C 1 H22A H 1.1407 0.7473 -0.1184 0.064 Uiso 0.845(7) 1 calc PR C 1 C23 C 1.0345(3) 0.6745(2) -0.07081(11) 0.0534(13) Uani 0.845(7) 1 d PGU C 1 H23A H 0.9892 0.6434 -0.1134 0.064 Uiso 0.845(7) 1 calc PR C 1 C24 C 1.0109(2) 0.6582(2) -0.00556(14) 0.0459(11) Uani 0.845(7) 1 d PGU C 1 H24A H 0.9494 0.6160 -0.0035 0.055 Uiso 0.845(7) 1 calc PR C 1 C19' C 1.1028(14) 0.7035(11) 0.0613(8) 0.029(4) Uiso 0.155(7) 1 d PGDU C 2 C20' C 1.2085(13) 0.7391(12) 0.0632(7) 0.051(4) Uiso 0.155(7) 1 d PGU C 2 H20B H 1.2557 0.7506 0.1065 0.061 Uiso 0.155(7) 1 calc PR C 2 C21' C 1.2451(11) 0.7577(12) 0.0018(9) 0.063(5) Uiso 0.155(7) 1 d PGU C 2 H21B H 1.3174 0.7820 0.0031 0.076 Uiso 0.155(7) 1 calc PR C 2 C22' C 1.1760(15) 0.7408(11) -0.0615(7) 0.054(5) Uiso 0.155(7) 1 d PGU C 2 H22B H 1.2011 0.7535 -0.1035 0.064 Uiso 0.155(7) 1 calc PR C 2 C23' C 1.0703(13) 0.7053(12) -0.0634(8) 0.044(5) Uiso 0.155(7) 1 d PGU C 2 H23B H 1.0231 0.6937 -0.1067 0.053 Uiso 0.155(7) 1 calc PR C 2 C24' C 1.0337(11) 0.6866(12) -0.0020(10) 0.044(5) Uiso 0.155(7) 1 d PGU C 2 H24B H 0.9614 0.6624 -0.0034 0.053 Uiso 0.155(7) 1 calc PR C 2 P25 P 0.76867(5) 0.44586(4) 0.26749(3) 0.02101(12) Uani 1 1 d D D . C26 C 0.7631(4) 0.4651(3) 0.17834(17) 0.0232(14) Uani 0.649(13) 1 d PGDU D 1 C27 C 0.7044(4) 0.5115(4) 0.1588(3) 0.0314(12) Uani 0.649(13) 1 d PGU D 1 H27A H 0.6640 0.5277 0.1903 0.038 Uiso 0.649(13) 1 calc PR D 1 C28 C 0.7048(4) 0.5344(3) 0.0931(3) 0.0393(16) Uani 0.649(13) 1 d PGU D 1 H28A H 0.6647 0.5661 0.0797 0.047 Uiso 0.649(13) 1 calc PR D 1 C29 C 0.7639(5) 0.5107(3) 0.0469(2) 0.0458(15) Uani 0.649(13) 1 d PGU D 1 H29A H 0.7642 0.5263 0.0020 0.055 Uiso 0.649(13) 1 calc PR D 1 C30 C 0.8227(6) 0.4643(4) 0.0665(2) 0.0550(19) Uani 0.649(13) 1 d PGU D 1 H30A H 0.8631 0.4481 0.0350 0.066 Uiso 0.649(13) 1 calc PR D 1 C31 C 0.8223(6) 0.4414(4) 0.1322(2) 0.0441(16) Uani 0.649(13) 1 d PGU D 1 H31A H 0.8624 0.4097 0.1456 0.053 Uiso 0.649(13) 1 calc PR D 1 C26' C 0.7523(8) 0.4601(6) 0.1747(4) 0.029(3) Uiso 0.351(13) 1 d PGDU D 2 C27' C 0.7235(10) 0.5248(6) 0.1600(5) 0.027(2) Uiso 0.351(13) 1 d PGU D 2 H27B H 0.7057 0.5571 0.1962 0.032 Uiso 0.351(13) 1 calc PR D 2 C28' C 0.7208(10) 0.5422(6) 0.0922(6) 0.033(3) Uiso 0.351(13) 1 d PGU D 2 H28B H 0.7010 0.5864 0.0821 0.040 Uiso 0.351(13) 1 calc PR D 2 C29' C 0.7469(9) 0.4949(7) 0.0391(4) 0.049(3) Uiso 0.351(13) 1 d PGU D 2 H29B H 0.7450 0.5068 -0.0072 0.059 Uiso 0.351(13) 1 calc PR D 2 C30' C 0.7757(9) 0.4302(7) 0.0539(4) 0.048(3) Uiso 0.351(13) 1 d PGU D 2 H30B H 0.7935 0.3979 0.0177 0.058 Uiso 0.351(13) 1 calc PR D 2 C31' C 0.7784(9) 0.4128(6) 0.1217(4) 0.045(3) Uiso 0.351(13) 1 d PGU D 2 H31B H 0.7981 0.3686 0.1318 0.054 Uiso 0.351(13) 1 calc PR D 2 C32 C 0.8613(2) 0.39283(14) 0.27843(13) 0.0241(5) Uani 1 1 d . D 1 C33 C 0.8271(2) 0.30900(16) 0.26193(15) 0.0319(6) Uani 1 1 d . D 1 H33A H 0.7555 0.2796 0.2456 0.038 Uiso 1 1 calc R D 1 C34 C 0.8970(2) 0.26833(17) 0.26926(16) 0.0379(7) Uani 1 1 d . D 1 H34A H 0.8730 0.2112 0.2583 0.046 Uiso 1 1 calc R D 1 C35 C 1.0008(3) 0.31018(19) 0.29233(16) 0.0404(7) Uani 1 1 d . D 1 H35A H 1.0488 0.2823 0.2963 0.048 Uiso 1 1 calc R D 1 C36 C 1.0346(3) 0.3924(2) 0.3095(2) 0.0629(11) Uani 1 1 d . D 1 H36A H 1.1062 0.4215 0.3261 0.075 Uiso 1 1 calc R D 1 C37 C 0.9649(2) 0.43392(18) 0.3029(2) 0.0489(9) Uani 1 1 d . D 1 H37A H 0.9893 0.4910 0.3154 0.059 Uiso 1 1 calc R D 1 C38 C 0.64902(19) 0.36934(14) 0.26947(13) 0.0247(5) Uani 1 1 d . D 1 C39 C 0.5582(2) 0.33745(17) 0.21553(15) 0.0338(6) Uani 1 1 d . D 1 H39A H 0.5487 0.3551 0.1692 0.041 Uiso 1 1 calc R D 1 C40 C 0.4829(2) 0.27632(17) 0.24020(18) 0.0423(7) Uani 1 1 d . D 1 H40A H 0.4110 0.2446 0.2143 0.051 Uiso 1 1 calc R D 1 C41 C 0.5261(2) 0.27007(17) 0.30835(19) 0.0417(7) Uani 1 1 d . D 1 H41A H 0.4904 0.2330 0.3386 0.050 Uiso 1 1 calc R D 1 C42 C 0.6283(2) 0.32750(15) 0.32718(16) 0.0307(6) Uani 1 1 d . D 1 H42A H 0.6774 0.3367 0.3725 0.037 Uiso 1 1 calc R D 1 C43 C 0.5742(2) 0.49157(16) 0.37780(14) 0.0293(5) Uani 1 1 d . D 1 C44 C 0.4981(2) 0.43070(18) 0.40360(17) 0.0407(7) Uani 1 1 d . D 1 H44A H 0.5089 0.4117 0.4491 0.049 Uiso 1 1 calc R D 1 C45 C 0.4060(3) 0.4030(2) 0.3530(2) 0.0488(8) Uani 1 1 d . D 1 H45A H 0.3407 0.3597 0.3560 0.059 Uiso 1 1 calc R D 1 C46 C 0.4219(3) 0.4443(2) 0.2962(2) 0.0487(8) Uani 1 1 d . D 1 H46A H 0.3699 0.4355 0.2525 0.058 Uiso 1 1 calc R D 1 C47 C 0.5255(2) 0.49914(17) 0.31097(16) 0.0339(6) Uani 1 1 d . D 1 H47A H 0.5586 0.5362 0.2799 0.041 Uiso 1 1 calc R D 1 P48 P 0.70748(5) 0.54538(4) 0.41627(3) 0.02511(13) Uani 1 1 d . D 1 C49 C 0.7484(2) 0.49141(16) 0.48021(13) 0.0299(5) Uani 1 1 d . D 1 C50 C 0.8346(2) 0.46873(17) 0.47496(15) 0.0349(6) Uani 1 1 d . D 1 H50A H 0.8702 0.4791 0.4365 0.042 Uiso 1 1 calc R D 1 C51 C 0.8691(3) 0.4312(2) 0.52529(17) 0.0464(8) Uani 1 1 d . D 1 H51A H 0.9289 0.4165 0.5218 0.056 Uiso 1 1 calc R D 1 C52 C 0.8169(3) 0.4149(2) 0.58066(17) 0.0522(9) Uani 1 1 d . D 1 H52A H 0.8399 0.3880 0.6147 0.063 Uiso 1 1 calc R D 1 C53 C 0.7324(3) 0.4373(2) 0.58680(17) 0.0529(9) Uani 1 1 d . D 1 H53A H 0.6970 0.4262 0.6253 0.064 Uiso 1 1 calc R D 1 C54 C 0.6976(3) 0.47607(18) 0.53736(15) 0.0400(7) Uani 1 1 d . D 1 H54A H 0.6392 0.4922 0.5423 0.048 Uiso 1 1 calc R D 1 C55 C 0.7071(2) 0.63641(16) 0.47261(14) 0.0333(6) Uani 1 1 d . D 1 C56 C 0.7924(3) 0.67909(18) 0.52636(16) 0.0434(7) Uani 1 1 d . D 1 H56A H 0.8475 0.6586 0.5348 0.052 Uiso 1 1 calc R D 1 C57 C 0.7973(3) 0.7503(2) 0.56712(18) 0.0552(10) Uani 1 1 d . D 1 H57A H 0.8556 0.7790 0.6034 0.066 Uiso 1 1 calc R D 1 C58 C 0.7169(4) 0.7802(2) 0.55511(19) 0.0642(12) Uani 1 1 d . D 1 H58A H 0.7201 0.8295 0.5831 0.077 Uiso 1 1 calc R D 1 C59 C 0.6343(4) 0.7394(2) 0.5037(2) 0.0616(11) Uani 1 1 d . D 1 H59A H 0.5792 0.7600 0.4962 0.074 Uiso 1 1 calc R D 1 C60 C 0.6282(3) 0.66682(19) 0.46104(17) 0.0437(8) Uani 1 1 d . D 1 H60A H 0.5700 0.6391 0.4245 0.052 Uiso 1 1 calc R D 1 P61 P 0.86944(5) 1.00652(4) 0.21120(3) 0.02135(12) Uani 1 1 d . E 1 C62 C 0.8789(2) 1.00410(17) 0.30488(13) 0.0285(5) Uani 1 1 d . E 1 C63 C 0.8434(3) 0.93029(19) 0.32635(16) 0.0401(7) Uani 1 1 d . E 1 H63A H 0.8151 0.8820 0.2918 0.048 Uiso 1 1 calc R E 1 C64 C 0.8493(3) 0.9270(3) 0.39837(19) 0.0559(10) Uani 1 1 d . E 1 H64A H 0.8244 0.8768 0.4131 0.067 Uiso 1 1 calc R E 1 C65 C 0.8925(3) 0.9987(3) 0.44839(17) 0.0566(10) Uani 1 1 d . E 1 H65A H 0.8972 0.9974 0.4975 0.068 Uiso 1 1 calc R E 1 C66 C 0.9281(3) 1.0711(2) 0.42688(16) 0.0486(8) Uani 1 1 d . E 1 H66A H 0.9576 1.1195 0.4613 0.058 Uiso 1 1 calc R E 1 C67 C 0.9214(2) 1.07414(18) 0.35601(14) 0.0352(6) Uani 1 1 d . E 1 H67A H 0.9460 1.1246 0.3419 0.042 Uiso 1 1 calc R E 1 C68 C 0.98931(19) 1.08494(14) 0.20494(13) 0.0240(5) Uani 1 1 d . E 1 C69 C 1.0827(2) 1.09343(16) 0.24687(15) 0.0311(6) Uani 1 1 d . E 1 H69A H 1.0836 1.0591 0.2800 0.037 Uiso 1 1 calc R E 1 C70 C 1.1745(2) 1.15106(19) 0.24118(17) 0.0391(7) Uani 1 1 d . E 1 H70A H 1.2376 1.1561 0.2703 0.047 Uiso 1 1 calc R E 1 C71 C 1.1741(2) 1.2011(2) 0.19318(19) 0.0447(8) Uani 1 1 d . E 1 H71A H 1.2367 1.2413 0.1897 0.054 Uiso 1 1 calc R E 1 C72 C 1.0823(2) 1.1925(2) 0.15013(18) 0.0432(7) Uani 1 1 d . E 1 H72A H 1.0821 1.2265 0.1166 0.052 Uiso 1 1 calc R E 1 C73 C 0.9906(2) 1.13454(17) 0.15562(15) 0.0324(6) Uani 1 1 d . E 1 H73A H 0.9280 1.1287 0.1254 0.039 Uiso 1 1 calc R E 1 C74 C 0.76896(19) 1.04965(14) 0.19480(13) 0.0233(5) Uani 1 1 d . E 1 C75 C 0.7043(2) 1.06392(15) 0.24431(14) 0.0276(5) Uani 1 1 d . E 1 H75A H 0.7089 1.0531 0.2937 0.033 Uiso 1 1 calc R E 1 C76 C 0.6316(2) 1.09477(16) 0.21094(15) 0.0316(6) Uani 1 1 d . E 1 H76A H 0.5758 1.1086 0.2325 0.038 Uiso 1 1 calc R E 1 C77 C 0.6502(2) 1.10038(16) 0.14079(15) 0.0314(6) Uani 1 1 d . E 1 H77A H 0.6101 1.1192 0.1046 0.038 Uiso 1 1 calc R E 1 C78 C 0.7339(2) 1.07200(15) 0.13036(14) 0.0266(5) Uani 1 1 d . E 1 H78A H 0.7637 1.0688 0.0859 0.032 Uiso 1 1 calc R E 1 C79 C 0.6087(2) 0.87590(15) 0.09997(14) 0.0269(5) Uani 1 1 d . E 1 C80 C 0.5310(2) 0.90351(17) 0.06612(17) 0.0366(7) Uani 1 1 d . E 1 H80A H 0.5238 0.9141 0.0167 0.044 Uiso 1 1 calc R E 1 C81 C 0.4661(2) 0.91298(19) 0.11692(19) 0.0455(8) Uani 1 1 d . E 1 H81A H 0.4068 0.9334 0.1093 0.055 Uiso 1 1 calc R E 1 C82 C 0.5016(2) 0.89160(18) 0.18005(19) 0.0432(8) Uani 1 1 d . E 1 H82A H 0.4719 0.8940 0.2245 0.052 Uiso 1 1 calc R E 1 C83 C 0.5893(2) 0.86870(16) 0.17023(15) 0.0329(6) Uani 1 1 d . E 1 H83A H 0.6308 0.8510 0.2064 0.039 Uiso 1 1 calc R E 1 P84 P 0.71583(5) 0.85659(4) 0.06647(3) 0.02189(12) Uani 1 1 d . E 1 C85 C 0.7458(2) 0.91386(15) -0.00318(13) 0.0248(5) Uani 1 1 d . E 1 C86 C 0.8422(2) 0.97230(17) 0.00413(14) 0.0308(6) Uani 1 1 d . E 1 H86A H 0.8924 0.9824 0.0456 0.037 Uiso 1 1 calc R E 1 C87 C 0.8658(3) 1.01631(19) -0.04893(16) 0.0406(7) Uani 1 1 d . E 1 H87A H 0.9318 1.0566 -0.0439 0.049 Uiso 1 1 calc R E 1 C88 C 0.7918(3) 1.0008(2) -0.10969(16) 0.0430(7) Uani 1 1 d . E 1 H88A H 0.8072 1.0309 -0.1461 0.052 Uiso 1 1 calc R E 1 C89 C 0.6965(3) 0.94212(19) -0.11720(15) 0.0392(7) Uani 1 1 d . E 1 H89A H 0.6466 0.9317 -0.1588 0.047 Uiso 1 1 calc R E 1 C90 C 0.6732(2) 0.89852(17) -0.06502(14) 0.0320(6) Uani 1 1 d . E 1 H90A H 0.6074 0.8577 -0.0709 0.038 Uiso 1 1 calc R E 1 C91 C 0.6597(2) 0.75389(15) 0.01757(13) 0.0282(5) Uani 1 1 d . E 1 C92 C 0.7135(2) 0.72525(17) -0.03106(14) 0.0352(6) Uani 1 1 d . E 1 H92A H 0.7784 0.7598 -0.0378 0.042 Uiso 1 1 calc R E 1 C93 C 0.6726(3) 0.64667(19) -0.06940(16) 0.0455(8) Uani 1 1 d . E 1 H93A H 0.7088 0.6278 -0.1027 0.055 Uiso 1 1 calc R E 1 C94 C 0.5793(3) 0.5964(2) -0.05871(18) 0.0539(10) Uani 1 1 d . E 1 H94A H 0.5513 0.5425 -0.0845 0.065 Uiso 1 1 calc R E 1 C95 C 0.5263(3) 0.6236(2) -0.0109(2) 0.0605(10) Uani 1 1 d . E 1 H95A H 0.4617 0.5886 -0.0042 0.073 Uiso 1 1 calc R E 1 C96 C 0.5664(2) 0.70181(18) 0.02751(18) 0.0434(7) Uani 1 1 d . E 1 H96A H 0.5296 0.7198 0.0609 0.052 Uiso 1 1 calc R E 1 P10 P 0.23228(9) 0.54796(7) 0.18267(5) 0.0561(3) Uani 1 1 d . F 1 F11 F 0.1518(3) 0.55805(18) 0.22912(16) 0.1006(10) Uani 1 1 d . F 1 F12 F 0.2033(3) 0.45630(18) 0.1868(2) 0.1103(11) Uani 1 1 d . F 1 F13 F 0.3205(2) 0.57141(18) 0.25196(12) 0.0894(9) Uani 1 1 d . F 1 F14 F 0.2654(2) 0.64265(17) 0.18162(16) 0.0893(8) Uani 1 1 d . F 1 F15 F 0.1516(2) 0.5302(2) 0.11303(14) 0.1053(11) Uani 1 1 d . F 1 F16 F 0.3174(2) 0.5402(2) 0.13734(14) 0.1001(10) Uani 1 1 d . F 1 P20 P 0.36610(7) 1.01709(6) 0.32259(7) 0.0322(2) Uani 0.892(3) 1 d PD G 1 F21 F 0.24824(18) 1.00837(15) 0.32507(18) 0.0737(9) Uani 0.892(3) 1 d PDU G 1 F22 F 0.3417(2) 0.93006(13) 0.34355(13) 0.0540(6) Uani 0.892(3) 1 d PDU G 1 F23 F 0.3981(2) 1.05984(17) 0.40340(12) 0.0659(8) Uani 0.892(3) 1 d PDU G 1 F24 F 0.3850(2) 1.10017(13) 0.29796(15) 0.0801(9) Uani 0.892(3) 1 d PDU G 1 F25 F 0.33392(18) 0.97166(13) 0.24130(10) 0.0541(6) Uani 0.892(3) 1 d PDU G 1 F26 F 0.48139(17) 1.02203(19) 0.31962(13) 0.0611(8) Uani 0.892(3) 1 d PDU G 1 P20' P 0.3711(8) 1.0350(6) 0.3480(6) 0.052(4) Uiso 0.108(3) 1 d PD G 2 F21' F 0.2676(10) 1.0178(9) 0.3793(9) 0.056(4) Uiso 0.108(3) 1 d PDU G 2 F22' F 0.3402(14) 0.9418(8) 0.3140(9) 0.066(5) Uiso 0.108(3) 1 d PDU G 2 F23' F 0.4294(12) 1.0198(10) 0.4165(7) 0.059(5) Uiso 0.108(3) 1 d PDU G 2 F24' F 0.4057(13) 1.1268(7) 0.3801(9) 0.079(5) Uiso 0.108(3) 1 d PDU G 2 F25' F 0.3112(14) 1.0472(12) 0.2768(8) 0.091(5) Uiso 0.108(3) 1 d PDU G 2 F26' F 0.4738(12) 1.0535(11) 0.3126(10) 0.062(6) Uiso 0.108(3) 1 d PDU G 2 C100 C 0.5072(6) 0.7797(5) 0.3189(4) 0.059(2) Uiso 0.449(3) 1 d PD H 1 H10A H 0.4785 0.7843 0.2709 0.071 Uiso 0.449(3) 1 calc PR H 1 H10B H 0.5436 0.7400 0.3154 0.071 Uiso 0.449(3) 1 calc PR H 1 Cl1 Cl 0.5835(4) 0.8711(3) 0.3698(3) 0.1211(16) Uiso 0.449(3) 1 d PDU H 1 Cl2 Cl 0.4162(3) 0.7597(2) 0.3716(3) 0.1130(12) Uiso 0.449(3) 1 d PDU H 1 C101 C 0.4906(5) 0.8591(4) 0.4223(4) 0.0294(16) Uiso 0.417(4) 1 d PDU I 2 H10C H 0.4507 0.8901 0.4014 0.035 Uiso 0.417(4) 1 calc PR I 2 H10D H 0.5047 0.8785 0.4743 0.035 Uiso 0.417(4) 1 calc PR I 2 Cl3 Cl 0.6068(3) 0.8873(2) 0.3954(2) 0.0757(11) Uiso 0.417(4) 1 d PDU I 2 Cl4 Cl 0.4069(2) 0.75918(18) 0.4067(2) 0.0683(9) Uiso 0.417(4) 1 d PDU I 2 C102 C 0.4720(13) 0.8565(10) 0.4339(13) 0.028(4) Uiso 0.134(3) 1 d PDU J 3 H10E H 0.4480 0.8611 0.3849 0.033 Uiso 0.134(3) 1 calc PR J 3 H10F H 0.4498 0.8944 0.4654 0.033 Uiso 0.134(3) 1 calc PR J 3 Cl5 Cl 0.5968(11) 0.8943(9) 0.4467(10) 0.146(3) Uiso 0.134(3) 1 d PDU J 3 Cl6 Cl 0.4005(10) 0.7651(7) 0.4425(9) 0.111(3) Uiso 0.134(3) 1 d PDU J 3 O110 O 0.6529(6) 0.7101(3) 0.2588(4) 0.0727(19) Uani 0.541(4) 1 d PDU K 4 C111 C 0.5486(6) 0.6783(4) 0.2387(4) 0.0514(17) Uani 0.541(4) 1 d PDU K 4 H11C H 0.5209 0.7165 0.2178 0.062 Uiso 0.541(4) 1 calc PR K 4 H11D H 0.5147 0.6642 0.2795 0.062 Uiso 0.541(4) 1 calc PR K 4 C112 C 0.5311(5) 0.6017(4) 0.1825(3) 0.0380(14) Uani 0.541(4) 1 d PDU K 4 H11E H 0.4566 0.5743 0.1655 0.057 Uiso 0.541(4) 1 calc PR K 4 H11F H 0.5606 0.5655 0.2040 0.057 Uiso 0.541(4) 1 calc PR K 4 H11G H 0.5650 0.6171 0.1426 0.057 Uiso 0.541(4) 1 calc PR K 4 O115 O 0.6665(7) 0.7133(5) 0.2926(5) 0.050(2) Uiso 0.318(6) 1 d PDU L 5 C116 C 0.6480(11) 0.6981(9) 0.2223(6) 0.056(4) Uiso 0.318(6) 1 d PDU L 5 H11H H 0.7036 0.6810 0.2048 0.068 Uiso 0.318(6) 1 calc PR L 5 H11I H 0.6491 0.7479 0.2051 0.068 Uiso 0.318(6) 1 calc PR L 5 C117 C 0.5407(12) 0.6306(10) 0.1915(9) 0.066(4) Uiso 0.318(6) 1 d PDU L 5 H11J H 0.5327 0.6174 0.1397 0.099 Uiso 0.318(6) 1 calc PR L 5 H11K H 0.4850 0.6498 0.2042 0.099 Uiso 0.318(6) 1 calc PR L 5 H11L H 0.5374 0.5825 0.2113 0.099 Uiso 0.318(6) 1 calc PR L 5 O120 O 0.516(2) 0.7081(17) 0.2649(12) 0.100(10) Uiso 0.141(6) 1 d PD M 6 C122 C 0.5469(13) 0.6510(10) 0.1603(8) 0.022(4) Uiso 0.141(6) 1 d PDU M 6 H12A H 0.5978 0.6367 0.1351 0.033 Uiso 0.141(6) 1 calc PR M 6 H12B H 0.5210 0.6875 0.1364 0.033 Uiso 0.141(6) 1 calc PR M 6 H12C H 0.4890 0.6022 0.1605 0.033 Uiso 0.141(6) 1 calc PR M 6 C121 C 0.601(2) 0.695(2) 0.2401(12) 0.047(5) Uiso 0.141(6) 1 d PDU M 6 H12D H 0.6266 0.6592 0.2665 0.056 Uiso 0.141(6) 1 calc PR M 6 H12E H 0.6578 0.7456 0.2422 0.056 Uiso 0.141(6) 1 calc PR M 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02271(9) 0.01735(8) 0.02014(9) 0.00325(6) 0.00711(7) 0.00303(6) Pd2 0.02191(9) 0.01861(9) 0.01920(9) 0.00111(6) 0.00170(7) 0.00854(7) Fe1 0.02189(19) 0.02247(18) 0.0384(2) 0.00629(15) 0.00855(16) 0.00447(14) Fe2 0.02183(18) 0.02284(18) 0.03101(19) 0.00163(14) 0.00755(14) 0.00767(14) S1 0.0318(4) 0.0206(3) 0.0309(3) -0.0013(2) 0.0144(3) 0.0020(2) C2 0.0269(13) 0.0200(11) 0.0194(11) 0.0054(8) 0.0052(9) 0.0068(9) S3 0.0298(3) 0.0196(3) 0.0241(3) -0.0003(2) 0.0113(2) 0.0001(2) N4 0.0223(10) 0.0198(10) 0.0185(9) 0.0026(7) 0.0031(8) 0.0038(7) C5 0.0187(11) 0.0246(12) 0.0219(11) 0.0057(9) 0.0017(9) 0.0077(9) C6 0.0196(12) 0.0242(12) 0.0225(11) 0.0064(9) 0.0032(9) 0.0054(9) N7 0.0224(10) 0.0200(9) 0.0173(9) 0.0015(7) 0.0012(7) 0.0075(8) C8 0.0224(12) 0.0203(11) 0.0211(11) 0.0026(8) 0.0023(9) 0.0058(9) S9 0.0302(3) 0.0231(3) 0.0270(3) -0.0047(2) -0.0057(2) 0.0125(2) S10 0.0277(3) 0.0237(3) 0.0272(3) -0.0048(2) -0.0052(2) 0.0129(2) C11 0.0287(13) 0.0212(12) 0.0214(12) -0.0003(9) 0.0018(10) 0.0019(9) C12 0.0306(14) 0.0370(15) 0.0193(12) -0.0007(10) 0.0021(10) 0.0105(11) C13 0.057(2) 0.0354(17) 0.0435(18) 0.0091(13) -0.0090(15) 0.0097(15) C14 0.085(3) 0.049(2) 0.0415(19) 0.0139(16) -0.0100(19) 0.027(2) C15 0.069(3) 0.072(3) 0.0289(16) -0.0061(16) -0.0161(16) 0.035(2) C16 0.046(2) 0.077(3) 0.0364(18) -0.0069(17) -0.0119(16) 0.0089(19) C17 0.0383(18) 0.053(2) 0.0322(16) 0.0041(13) -0.0003(13) -0.0003(14) C18 0.0299(13) 0.0236(12) 0.0208(11) 0.0047(9) 0.0054(9) 0.0131(10) C19 0.047(2) 0.0322(17) 0.0215(15) 0.0065(12) 0.0098(15) 0.0267(17) C20 0.080(3) 0.046(2) 0.0291(19) 0.0051(16) 0.018(2) -0.005(2) C21 0.103(4) 0.054(3) 0.041(2) 0.0192(19) 0.034(3) 0.011(3) C22 0.095(4) 0.058(3) 0.0306(19) 0.0188(17) 0.024(2) 0.050(3) C23 0.070(3) 0.076(4) 0.0237(17) 0.0012(19) 0.0010(19) 0.043(3) C24 0.045(2) 0.069(3) 0.0269(18) 0.0000(18) 0.0011(16) 0.029(2) P25 0.0225(3) 0.0175(3) 0.0218(3) 0.0038(2) 0.0044(2) 0.0048(2) C26 0.029(3) 0.019(2) 0.018(2) 0.0010(13) 0.0016(15) 0.0041(16) C27 0.026(3) 0.035(3) 0.026(2) 0.0040(18) -0.0018(19) 0.004(2) C28 0.033(3) 0.040(3) 0.035(3) 0.014(2) -0.010(2) 0.002(2) C29 0.061(4) 0.058(4) 0.023(2) 0.019(2) 0.006(2) 0.022(3) C30 0.086(5) 0.063(4) 0.034(3) 0.013(3) 0.028(3) 0.042(4) C31 0.073(5) 0.045(3) 0.033(2) 0.014(2) 0.021(3) 0.038(3) C32 0.0274(13) 0.0222(12) 0.0241(12) 0.0054(9) 0.0061(10) 0.0092(10) C33 0.0299(14) 0.0245(13) 0.0392(15) 0.0031(11) 0.0037(11) 0.0085(11) C34 0.0429(18) 0.0252(14) 0.0471(17) 0.0055(12) 0.0081(14) 0.0141(12) C35 0.0393(18) 0.0415(17) 0.0472(18) 0.0076(13) 0.0043(14) 0.0249(14) C36 0.0271(17) 0.039(2) 0.112(3) 0.003(2) -0.0055(19) 0.0092(14) C37 0.0300(16) 0.0237(15) 0.087(3) 0.0036(15) 0.0020(16) 0.0070(12) C38 0.0212(12) 0.0178(11) 0.0317(13) 0.0028(9) 0.0031(10) 0.0034(9) C39 0.0271(14) 0.0311(14) 0.0367(15) -0.0030(11) 0.0011(11) 0.0069(11) C40 0.0230(14) 0.0286(15) 0.064(2) -0.0066(13) 0.0042(14) 0.0019(11) C41 0.0351(17) 0.0203(13) 0.069(2) 0.0118(13) 0.0161(15) 0.0044(11) C42 0.0269(14) 0.0239(13) 0.0443(16) 0.0139(11) 0.0094(12) 0.0084(10) C43 0.0264(14) 0.0275(13) 0.0347(14) 0.0050(10) 0.0135(11) 0.0076(10) C44 0.0355(17) 0.0367(16) 0.0475(18) 0.0064(13) 0.0231(14) 0.0039(12) C45 0.0320(17) 0.0418(18) 0.070(2) 0.0019(16) 0.0250(16) 0.0075(13) C46 0.0309(17) 0.0420(18) 0.072(2) -0.0021(16) 0.0023(16) 0.0193(14) C47 0.0308(15) 0.0277(14) 0.0461(17) 0.0056(11) 0.0070(12) 0.0146(11) P48 0.0277(3) 0.0226(3) 0.0246(3) 0.0049(2) 0.0108(3) 0.0054(2) C49 0.0351(15) 0.0273(13) 0.0241(12) 0.0059(10) 0.0070(11) 0.0051(11) C50 0.0386(17) 0.0316(15) 0.0316(14) 0.0073(11) 0.0065(12) 0.0075(12) C51 0.049(2) 0.0429(18) 0.0453(19) 0.0124(14) -0.0021(15) 0.0147(15) C52 0.071(3) 0.0440(19) 0.0372(18) 0.0176(14) -0.0013(17) 0.0127(18) C53 0.076(3) 0.047(2) 0.0310(16) 0.0166(14) 0.0144(17) 0.0092(18) C54 0.052(2) 0.0378(16) 0.0296(15) 0.0093(12) 0.0167(13) 0.0094(14) C55 0.0457(18) 0.0289(14) 0.0273(13) 0.0079(10) 0.0194(12) 0.0097(12) C56 0.054(2) 0.0344(16) 0.0349(16) 0.0001(12) 0.0147(14) 0.0064(14) C57 0.077(3) 0.0367(18) 0.0426(19) -0.0048(14) 0.0203(18) 0.0082(17) C58 0.114(4) 0.0352(19) 0.045(2) -0.0012(15) 0.027(2) 0.027(2) C59 0.096(3) 0.053(2) 0.053(2) 0.0085(18) 0.023(2) 0.046(2) C60 0.061(2) 0.0401(17) 0.0390(17) 0.0087(13) 0.0184(15) 0.0255(16) P61 0.0239(3) 0.0201(3) 0.0204(3) 0.0017(2) 0.0040(2) 0.0088(2) C62 0.0325(15) 0.0375(15) 0.0208(12) 0.0040(10) 0.0064(10) 0.0193(11) C63 0.053(2) 0.0416(17) 0.0319(15) 0.0101(12) 0.0162(14) 0.0192(14) C64 0.073(3) 0.072(3) 0.045(2) 0.0318(18) 0.0281(19) 0.040(2) C65 0.069(3) 0.098(3) 0.0243(15) 0.0149(17) 0.0163(16) 0.053(2) C66 0.055(2) 0.066(2) 0.0276(15) -0.0033(14) 0.0021(14) 0.0315(18) C67 0.0402(17) 0.0398(16) 0.0263(13) -0.0023(11) 0.0033(12) 0.0192(13) C68 0.0230(12) 0.0203(11) 0.0283(12) -0.0008(9) 0.0049(10) 0.0090(9) C69 0.0300(15) 0.0284(13) 0.0337(14) 0.0019(10) 0.0029(11) 0.0109(11) C70 0.0269(15) 0.0425(17) 0.0467(18) 0.0047(13) 0.0042(13) 0.0126(12) C71 0.0242(15) 0.0445(18) 0.066(2) 0.0160(16) 0.0161(15) 0.0076(13) C72 0.0306(16) 0.0491(19) 0.058(2) 0.0254(15) 0.0159(14) 0.0150(14) C73 0.0257(14) 0.0358(15) 0.0400(15) 0.0140(12) 0.0099(11) 0.0121(11) C74 0.0260(13) 0.0164(11) 0.0266(12) 0.0022(9) 0.0053(10) 0.0066(9) C75 0.0304(14) 0.0244(12) 0.0285(13) 0.0011(10) 0.0071(10) 0.0109(10) C76 0.0277(14) 0.0246(13) 0.0426(16) -0.0023(11) 0.0088(12) 0.0116(10) C77 0.0296(14) 0.0274(13) 0.0395(15) 0.0075(11) 0.0043(11) 0.0134(11) C78 0.0266(13) 0.0242(12) 0.0286(13) 0.0067(9) 0.0055(10) 0.0073(10) C79 0.0226(13) 0.0213(12) 0.0344(14) 0.0007(10) 0.0040(10) 0.0064(9) C80 0.0259(14) 0.0325(15) 0.0464(17) -0.0059(12) -0.0020(12) 0.0120(11) C81 0.0219(14) 0.0353(16) 0.073(2) -0.0075(15) 0.0085(14) 0.0084(12) C82 0.0341(17) 0.0301(15) 0.060(2) 0.0000(13) 0.0243(15) 0.0015(12) C83 0.0324(15) 0.0221(13) 0.0418(16) 0.0035(11) 0.0147(12) 0.0042(10) P84 0.0219(3) 0.0213(3) 0.0216(3) 0.0012(2) 0.0016(2) 0.0083(2) C85 0.0298(14) 0.0253(12) 0.0217(11) 0.0018(9) 0.0048(10) 0.0135(10) C86 0.0295(14) 0.0378(15) 0.0291(13) 0.0085(11) 0.0075(11) 0.0151(11) C87 0.0387(18) 0.0442(18) 0.0425(17) 0.0161(14) 0.0159(14) 0.0125(14) C88 0.055(2) 0.0516(19) 0.0345(16) 0.0208(14) 0.0166(14) 0.0265(16) C89 0.0488(19) 0.0441(17) 0.0269(14) 0.0078(12) -0.0003(13) 0.0211(15) C90 0.0337(15) 0.0336(14) 0.0285(13) 0.0034(11) -0.0004(11) 0.0144(12) C91 0.0302(14) 0.0245(12) 0.0264(13) -0.0005(9) -0.0056(10) 0.0110(10) C92 0.0444(18) 0.0338(15) 0.0265(13) -0.0019(11) 0.0003(12) 0.0176(13) C93 0.066(2) 0.0363(17) 0.0339(16) -0.0087(12) -0.0083(15) 0.0291(16) C94 0.070(3) 0.0282(16) 0.050(2) -0.0113(13) -0.0216(18) 0.0184(16) C95 0.047(2) 0.0279(17) 0.089(3) -0.0041(17) -0.009(2) 0.0028(15) C96 0.0360(17) 0.0283(15) 0.058(2) -0.0020(13) 0.0039(14) 0.0061(12) P10 0.0729(7) 0.0789(7) 0.0396(5) 0.0097(4) 0.0096(4) 0.0584(6) F11 0.126(3) 0.102(2) 0.119(2) 0.0372(18) 0.074(2) 0.075(2) F12 0.109(2) 0.0678(18) 0.174(3) 0.0279(19) 0.027(2) 0.0551(18) F13 0.121(2) 0.114(2) 0.0449(13) 0.0117(13) -0.0079(14) 0.0659(19) F14 0.086(2) 0.088(2) 0.118(2) 0.0412(17) 0.0191(17) 0.0544(17) F15 0.100(2) 0.145(3) 0.0722(18) -0.0055(17) -0.0250(16) 0.069(2) F16 0.100(2) 0.148(3) 0.0732(18) -0.0094(17) 0.0219(16) 0.082(2) P20 0.0243(4) 0.0316(5) 0.0350(6) 0.0115(4) -0.0004(4) 0.0014(3) F21 0.0307(13) 0.0626(17) 0.122(3) 0.0071(16) 0.0126(14) 0.0122(11) F22 0.0732(17) 0.0450(13) 0.0456(13) 0.0253(10) 0.0076(12) 0.0165(11) F23 0.0598(16) 0.0787(19) 0.0421(13) -0.0139(12) 0.0053(12) 0.0127(13) F24 0.097(2) 0.0270(12) 0.092(2) 0.0233(12) -0.0126(16) -0.0053(12) F25 0.0567(15) 0.0500(13) 0.0358(11) 0.0132(9) -0.0102(10) -0.0046(10) F26 0.0286(12) 0.090(2) 0.0519(15) -0.0012(13) 0.0040(10) 0.0102(12) O110 0.103(5) 0.026(2) 0.073(5) 0.016(3) -0.025(4) 0.011(3) C111 0.062(5) 0.027(3) 0.059(4) 0.014(3) 0.005(3) 0.007(3) C112 0.053(3) 0.022(3) 0.035(3) -0.006(2) 0.005(2) 0.013(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 Pd1 P48 2.2923(6) . ? Pd1 P25 2.3018(6) . ? Pd1 S3 2.3348(6) . ? Pd1 S1 2.3516(6) . ? Pd2 P84 2.2906(7) . ? Pd2 P61 2.3110(6) . ? Pd2 S10 2.3347(6) . ? Pd2 S9 2.3445(7) . ? Fe1 C43 2.015(3) . ? Fe1 C42 2.020(3) . ? Fe1 C38 2.024(2) . ? Fe1 C47 2.027(3) . ? Fe1 C44 2.027(3) . ? Fe1 C39 2.048(3) . ? Fe1 C45 2.049(3) . ? Fe1 C46 2.050(3) . ? Fe1 C41 2.058(3) . ? Fe1 C40 2.065(3) . ? Fe2 C79 2.012(2) . ? Fe2 C78 2.020(3) . ? Fe2 C74 2.028(3) . ? Fe2 C83 2.029(3) . ? Fe2 C80 2.038(3) . ? Fe2 C75 2.043(3) . ? Fe2 C81 2.059(3) . ? Fe2 C77 2.060(3) . ? Fe2 C82 2.066(3) . ? Fe2 C76 2.066(2) . ? S1 C2 1.728(2) . ? C2 N4 1.313(3) . ? C2 S3 1.719(2) . ? N4 C11 1.471(3) . ? N4 C5 1.474(3) . ? C5 C6 1.526(3) . ? C6 N7 1.470(3) . ? N7 C8 1.323(3) . ? N7 C18 1.479(3) . ? C8 S10 1.709(2) . ? C8 S9 1.723(2) . ? C11 C12 1.514(4) . ? C12 C13 1.368(4) . ? C12 C17 1.383(4) . ? C13 C14 1.396(4) . ? C14 C15 1.359(6) . ? C15 C16 1.364(6) . ? C16 C17 1.382(5) . ? C18 C19 1.498(3) . ? C18 C19' 1.550(11) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C19' C20' 1.3900 . ? C19' C24' 1.3900 . ? C20' C21' 1.3900 . ? C21' C22' 1.3900 . ? C22' C23' 1.3900 . ? C23' C24' 1.3900 . ? P25 C38 1.790(3) . ? P25 C26 1.804(3) . ? P25 C32 1.827(2) . ? P25 C26' 1.846(7) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C26' C27' 1.3900 . ? C26' C31' 1.3900 . ? C27' C28' 1.3900 . ? C28' C29' 1.3900 . ? C29' C30' 1.3900 . ? C30' C31' 1.3900 . ? C32 C37 1.373(4) . ? C32 C33 1.394(3) . ? C33 C34 1.386(4) . ? C34 C35 1.373(4) . ? C35 C36 1.369(5) . ? C36 C37 1.393(4) . ? C38 C39 1.432(4) . ? C38 C42 1.438(4) . ? C39 C40 1.433(4) . ? C40 C41 1.415(5) . ? C41 C42 1.425(4) . ? C43 C47 1.429(4) . ? C43 C44 1.448(4) . ? C43 P48 1.792(3) . ? C44 C45 1.409(5) . ? C45 C46 1.410(5) . ? C46 C47 1.422(4) . ? P48 C49 1.816(3) . ? P48 C55 1.825(3) . ? C49 C50 1.384(4) . ? C49 C54 1.395(4) . ? C50 C51 1.379(4) . ? C51 C52 1.378(5) . ? C52 C53 1.361(5) . ? C53 C54 1.383(4) . ? C55 C60 1.372(4) . ? C55 C56 1.400(4) . ? C56 C57 1.375(4) . ? C57 C58 1.386(6) . ? C58 C59 1.347(6) . ? C59 C60 1.406(4) . ? P61 C74 1.806(2) . ? P61 C62 1.810(3) . ? P61 C68 1.830(3) . ? C62 C67 1.389(4) . ? C62 C63 1.395(4) . ? C63 C64 1.397(4) . ? C64 C65 1.398(6) . ? C65 C66 1.373(5) . ? C66 C67 1.374(4) . ? C68 C73 1.390(4) . ? C68 C69 1.391(4) . ? C69 C70 1.385(4) . ? C70 C71 1.379(4) . ? C71 C72 1.382(4) . ? C72 C73 1.387(4) . ? C74 C75 1.437(3) . ? C74 C78 1.438(3) . ? C75 C76 1.423(4) . ? C76 C77 1.424(4) . ? C77 C78 1.426(4) . ? C79 C83 1.434(4) . ? C79 C80 1.442(4) . ? C79 P84 1.796(3) . ? C80 C81 1.437(4) . ? C81 C82 1.409(5) . ? C82 C83 1.421(4) . ? P84 C91 1.812(3) . ? P84 C85 1.815(3) . ? C85 C86 1.384(4) . ? C85 C90 1.398(4) . ? C86 C87 1.389(4) . ? C87 C88 1.393(4) . ? C88 C89 1.374(5) . ? C89 C90 1.369(4) . ? C91 C96 1.385(4) . ? C91 C92 1.405(4) . ? C92 C93 1.392(4) . ? C93 C94 1.378(5) . ? C94 C95 1.375(5) . ? C95 C96 1.386(4) . ? P10 F11 1.550(3) . ? P10 F15 1.565(3) . ? P10 F12 1.573(3) . ? P10 F16 1.579(3) . ? P10 F13 1.606(3) . ? P10 F14 1.609(3) . ? P20 F24 1.575(2) . ? P20 F26 1.576(2) . ? P20 F23 1.582(2) . ? P20 F21 1.594(2) . ? P20 F25 1.603(2) . ? P20 F22 1.604(2) . ? P20' F24' 1.563(11) . ? P20' F23' 1.571(11) . ? P20' F21' 1.579(11) . ? P20' F25' 1.598(11) . ? P20' F22' 1.598(11) . ? P20' F26' 1.611(11) . ? C100 Cl2 1.698(8) . ? C100 Cl1 1.715(9) . ? C101 Cl3 1.695(7) . ? C101 Cl4 1.751(7) . ? C102 Cl5 1.614(14) . ? C102 Cl6 1.662(13) . ? O110 C111 1.355(9) . ? C111 C112 1.553(8) . ? O115 C116 1.325(13) . ? C116 C117 1.566(14) . ? O120 C121 1.395(19) . ? C122 C121 1.598(17) . ? 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 P48 Pd1 P25 99.27(2) . . ? P48 Pd1 S3 170.12(2) . . ? P25 Pd1 S3 90.25(2) . . ? P48 Pd1 S1 95.41(2) . . ? P25 Pd1 S1 165.31(2) . . ? S3 Pd1 S1 75.07(2) . . ? P84 Pd2 P61 99.49(2) . . ? P84 Pd2 S10 94.27(2) . . ? P61 Pd2 S10 166.19(2) . . ? P84 Pd2 S9 169.19(2) . . ? P61 Pd2 S9 91.23(2) . . ? S10 Pd2 S9 74.98(2) . . ? C43 Fe1 C42 109.36(12) . . ? C43 Fe1 C38 109.47(10) . . ? C42 Fe1 C38 41.67(10) . . ? C43 Fe1 C47 41.39(11) . . ? C42 Fe1 C47 139.64(11) . . ? C38 Fe1 C47 111.69(11) . . ? C43 Fe1 C44 41.98(11) . . ? C42 Fe1 C44 108.52(13) . . ? C38 Fe1 C44 137.41(12) . . ? C47 Fe1 C44 69.58(12) . . ? C43 Fe1 C39 138.78(11) . . ? C42 Fe1 C39 69.31(12) . . ? C38 Fe1 C39 41.16(10) . . ? C47 Fe1 C39 112.34(12) . . ? C44 Fe1 C39 177.77(13) . . ? C43 Fe1 C45 69.14(12) . . ? C42 Fe1 C45 136.80(13) . . ? C38 Fe1 C45 177.80(13) . . ? C47 Fe1 C45 68.52(13) . . ? C44 Fe1 C45 40.43(13) . . ? C39 Fe1 C45 140.97(13) . . ? C43 Fe1 C46 69.15(12) . . ? C42 Fe1 C46 176.86(13) . . ? C38 Fe1 C46 141.25(13) . . ? C47 Fe1 C46 40.82(12) . . ? C44 Fe1 C46 68.48(15) . . ? C39 Fe1 C46 113.68(14) . . ? C45 Fe1 C46 40.23(14) . . ? C43 Fe1 C41 138.20(13) . . ? C42 Fe1 C41 40.88(11) . . ? C38 Fe1 C41 69.23(11) . . ? C47 Fe1 C41 179.03(13) . . ? C44 Fe1 C41 109.56(13) . . ? C39 Fe1 C41 68.54(13) . . ? C45 Fe1 C41 110.55(13) . . ? C46 Fe1 C41 138.59(13) . . ? C43 Fe1 C40 177.83(12) . . ? C42 Fe1 C40 68.47(12) . . ? C38 Fe1 C40 68.90(11) . . ? C47 Fe1 C40 140.30(13) . . ? C44 Fe1 C40 138.35(13) . . ? C39 Fe1 C40 40.77(12) . . ? C45 Fe1 C40 112.44(13) . . ? C46 Fe1 C40 113.02(13) . . ? C41 Fe1 C40 40.14(13) . . ? C79 Fe2 C78 110.11(10) . . ? C79 Fe2 C74 109.84(10) . . ? C78 Fe2 C74 41.62(10) . . ? C79 Fe2 C83 41.55(11) . . ? C78 Fe2 C83 138.60(11) . . ? C74 Fe2 C83 109.85(11) . . ? C79 Fe2 C80 41.70(10) . . ? C78 Fe2 C80 111.09(12) . . ? C74 Fe2 C80 139.39(11) . . ? C83 Fe2 C80 69.49(12) . . ? C79 Fe2 C75 139.02(10) . . ? C78 Fe2 C75 69.23(11) . . ? C74 Fe2 C75 41.34(10) . . ? C83 Fe2 C75 110.81(11) . . ? C80 Fe2 C75 179.17(11) . . ? C79 Fe2 C81 69.24(11) . . ? C78 Fe2 C81 140.41(13) . . ? C74 Fe2 C81 177.86(13) . . ? C83 Fe2 C81 68.14(13) . . ? C80 Fe2 C81 41.06(12) . . ? C75 Fe2 C81 138.23(12) . . ? C79 Fe2 C77 138.87(11) . . ? C78 Fe2 C77 40.91(10) . . ? C74 Fe2 C77 69.29(10) . . ? C83 Fe2 C77 179.09(12) . . ? C80 Fe2 C77 111.34(12) . . ? C75 Fe2 C77 68.36(11) . . ? C81 Fe2 C77 112.71(13) . . ? C79 Fe2 C82 69.22(11) . . ? C78 Fe2 C82 179.18(11) . . ? C74 Fe2 C82 138.00(13) . . ? C83 Fe2 C82 40.58(12) . . ? C80 Fe2 C82 68.76(13) . . ? C75 Fe2 C82 110.93(12) . . ? C81 Fe2 C82 39.96(14) . . ? C77 Fe2 C82 139.91(12) . . ? C79 Fe2 C76 178.77(11) . . ? C78 Fe2 C76 68.70(11) . . ? C74 Fe2 C76 69.10(10) . . ? C83 Fe2 C76 139.19(11) . . ? C80 Fe2 C76 138.78(11) . . ? C75 Fe2 C76 40.51(10) . . ? C81 Fe2 C76 111.84(11) . . ? C77 Fe2 C76 40.37(11) . . ? C82 Fe2 C76 111.96(11) . . ? C2 S1 Pd1 85.39(8) . . ? N4 C2 S3 123.48(18) . . ? N4 C2 S1 124.58(18) . . ? S3 C2 S1 111.88(14) . . ? C2 S3 Pd1 86.13(8) . . ? C2 N4 C11 121.8(2) . . ? C2 N4 C5 120.9(2) . . ? C11 N4 C5 116.9(2) . . ? N4 C5 C6 113.40(19) . . ? N7 C6 C5 113.4(2) . . ? C8 N7 C6 121.32(19) . . ? C8 N7 C18 119.6(2) . . ? C6 N7 C18 118.78(19) . . ? N7 C8 S10 124.26(18) . . ? N7 C8 S9 123.58(18) . . ? S10 C8 S9 112.15(13) . . ? C8 S9 Pd2 86.04(8) . . ? C8 S10 Pd2 86.67(8) . . ? N4 C11 C12 112.5(2) . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C11 121.7(3) . . ? C17 C12 C11 119.5(3) . . ? C12 C13 C14 120.5(3) . . ? C15 C14 C13 120.3(4) . . ? C14 C15 C16 119.4(3) . . ? C15 C16 C17 120.8(4) . . ? C16 C17 C12 120.2(3) . . ? N7 C18 C19 112.2(2) . . ? N7 C18 C19' 112.9(7) . . ? C20 C19 C24 120.0 . . ? C20 C19 C18 120.1(2) . . ? C24 C19 C18 119.9(2) . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ? C20' C19' C24' 120.0 . . ? C20' C19' C18 124.8(11) . . ? C24' C19' C18 115.0(11) . . ? C21' C20' C19' 120.0 . . ? C20' C21' C22' 120.0 . . ? C23' C22' C21' 120.0 . . ? C22' C23' C24' 120.0 . . ? C23' C24' C19' 120.0 . . ? C38 P25 C26 107.06(19) . . ? C38 P25 C32 101.90(11) . . ? C26 P25 C32 106.25(18) . . ? C38 P25 C26' 102.6(3) . . ? C32 P25 C26' 108.1(3) . . ? C38 P25 Pd1 121.79(8) . . ? C26 P25 Pd1 103.55(15) . . ? C32 P25 Pd1 115.26(8) . . ? C26' P25 Pd1 106.0(3) . . ? C27 C26 C31 120.0 . . ? C27 C26 P25 117.5(3) . . ? C31 C26 P25 122.2(3) . . ? C26 C27 C28 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C26 120.0 . . ? C27' C26' C31' 120.0 . . ? C27' C26' P25 118.5(6) . . ? C31' C26' P25 121.2(6) . . ? C26' C27' C28' 120.0 . . ? C27' C28' C29' 120.0 . . ? C30' C29' C28' 120.0 . . ? C31' C30' C29' 120.0 . . ? C30' C31' C26' 120.0 . . ? C37 C32 C33 118.7(2) . . ? C37 C32 P25 121.3(2) . . ? C33 C32 P25 120.0(2) . . ? C34 C33 C32 120.4(3) . . ? C35 C34 C33 120.4(3) . . ? C36 C35 C34 119.5(3) . . ? C35 C36 C37 120.6(3) . . ? C32 C37 C36 120.4(3) . . ? C39 C38 C42 107.4(2) . . ? C39 C38 P25 127.7(2) . . ? C42 C38 P25 124.8(2) . . ? C39 C38 Fe1 70.30(15) . . ? C42 C38 Fe1 69.01(15) . . ? P25 C38 Fe1 126.62(13) . . ? C38 C39 C40 107.7(3) . . ? C38 C39 Fe1 68.54(15) . . ? C40 C39 Fe1 70.26(17) . . ? C41 C40 C39 108.6(3) . . ? C41 C40 Fe1 69.69(17) . . ? C39 C40 Fe1 68.97(16) . . ? C40 C41 C42 108.1(3) . . ? C40 C41 Fe1 70.17(17) . . ? C42 C41 Fe1 68.11(15) . . ? C41 C42 C38 108.2(3) . . ? C41 C42 Fe1 71.01(16) . . ? C38 C42 Fe1 69.33(14) . . ? C47 C43 C44 107.0(3) . . ? C47 C43 P48 124.1(2) . . ? C44 C43 P48 128.8(2) . . ? C47 C43 Fe1 69.73(15) . . ? C44 C43 Fe1 69.45(16) . . ? P48 C43 Fe1 123.16(13) . . ? C45 C44 C43 107.7(3) . . ? C45 C44 Fe1 70.61(18) . . ? C43 C44 Fe1 68.58(15) . . ? C44 C45 C46 109.0(3) . . ? C44 C45 Fe1 68.96(17) . . ? C46 C45 Fe1 69.94(17) . . ? C45 C46 C47 108.2(3) . . ? C45 C46 Fe1 69.83(19) . . ? C47 C46 Fe1 68.70(16) . . ? C46 C47 C43 108.1(3) . . ? C46 C47 Fe1 70.47(17) . . ? C43 C47 Fe1 68.87(15) . . ? C43 P48 C49 108.51(13) . . ? C43 P48 C55 105.07(13) . . ? C49 P48 C55 102.61(12) . . ? C43 P48 Pd1 115.35(9) . . ? C49 P48 Pd1 111.63(9) . . ? C55 P48 Pd1 112.71(9) . . ? C50 C49 C54 118.9(3) . . ? C50 C49 P48 120.1(2) . . ? C54 C49 P48 120.9(2) . . ? C51 C50 C49 120.4(3) . . ? C52 C51 C50 120.0(3) . . ? C53 C52 C51 120.3(3) . . ? C52 C53 C54 120.4(3) . . ? C53 C54 C49 119.9(3) . . ? C60 C55 C56 119.0(3) . . ? C60 C55 P48 121.8(2) . . ? C56 C55 P48 119.1(2) . . ? C57 C56 C55 120.7(3) . . ? C56 C57 C58 119.8(4) . . ? C59 C58 C57 120.0(3) . . ? C58 C59 C60 121.2(4) . . ? C55 C60 C59 119.4(3) . . ? C74 P61 C62 102.93(11) . . ? C74 P61 C68 104.95(11) . . ? C62 P61 C68 104.43(13) . . ? C74 P61 Pd2 122.92(8) . . ? C62 P61 Pd2 108.72(9) . . ? C68 P61 Pd2 111.19(7) . . ? C67 C62 C63 119.2(3) . . ? C67 C62 P61 121.4(2) . . ? C63 C62 P61 119.4(2) . . ? C62 C63 C64 120.4(3) . . ? C63 C64 C65 118.9(3) . . ? C66 C65 C64 120.4(3) . . ? C65 C66 C67 120.6(3) . . ? C66 C67 C62 120.6(3) . . ? C73 C68 C69 118.2(2) . . ? C73 C68 P61 121.0(2) . . ? C69 C68 P61 120.6(2) . . ? C70 C69 C68 121.2(3) . . ? C71 C70 C69 119.9(3) . . ? C70 C71 C72 119.7(3) . . ? C71 C72 C73 120.4(3) . . ? C72 C73 C68 120.6(3) . . ? C75 C74 C78 106.8(2) . . ? C75 C74 P61 125.21(19) . . ? C78 C74 P61 127.90(18) . . ? C75 C74 Fe2 69.92(15) . . ? C78 C74 Fe2 68.89(14) . . ? P61 C74 Fe2 123.65(12) . . ? C76 C75 C74 108.6(2) . . ? C76 C75 Fe2 70.62(15) . . ? C74 C75 Fe2 68.74(14) . . ? C75 C76 C77 108.2(2) . . ? C75 C76 Fe2 68.87(14) . . ? C77 C76 Fe2 69.59(14) . . ? C76 C77 C78 108.0(2) . . ? C76 C77 Fe2 70.04(15) . . ? C78 C77 Fe2 68.00(14) . . ? C77 C78 C74 108.5(2) . . ? C77 C78 Fe2 71.08(15) . . ? C74 C78 Fe2 69.49(14) . . ? C83 C79 C80 107.4(2) . . ? C83 C79 P84 123.4(2) . . ? C80 C79 P84 129.2(2) . . ? C83 C79 Fe2 69.85(14) . . ? C80 C79 Fe2 70.11(15) . . ? P84 C79 Fe2 123.36(14) . . ? C81 C80 C79 106.9(3) . . ? C81 C80 Fe2 70.24(17) . . ? C79 C80 Fe2 68.19(15) . . ? C82 C81 C80 109.0(3) . . ? C82 C81 Fe2 70.29(18) . . ? C80 C81 Fe2 68.70(16) . . ? C81 C82 C83 108.1(3) . . ? C81 C82 Fe2 69.75(18) . . ? C83 C82 Fe2 68.31(16) . . ? C82 C83 C79 108.5(3) . . ? C82 C83 Fe2 71.11(17) . . ? C79 C83 Fe2 68.60(15) . . ? C79 P84 C91 103.61(12) . . ? C79 P84 C85 107.95(12) . . ? C91 P84 C85 102.67(12) . . ? C79 P84 Pd2 114.72(9) . . ? C91 P84 Pd2 115.52(8) . . ? C85 P84 Pd2 111.34(9) . . ? C86 C85 C90 119.4(2) . . ? C86 C85 P84 119.85(19) . . ? C90 C85 P84 120.7(2) . . ? C85 C86 C87 120.2(3) . . ? C86 C87 C88 119.4(3) . . ? C89 C88 C87 120.3(3) . . ? C90 C89 C88 120.4(3) . . ? C89 C90 C85 120.3(3) . . ? C96 C91 C92 118.6(3) . . ? C96 C91 P84 122.3(2) . . ? C92 C91 P84 119.1(2) . . ? C93 C92 C91 120.5(3) . . ? C94 C93 C92 119.6(3) . . ? C95 C94 C93 120.3(3) . . ? C94 C95 C96 120.5(4) . . ? C91 C96 C95 120.4(3) . . ? F11 P10 F15 91.49(18) . . ? F11 P10 F12 91.59(18) . . ? F15 P10 F12 92.9(2) . . ? F11 P10 F16 177.9(2) . . ? F15 P10 F16 90.17(16) . . ? F12 P10 F16 89.55(17) . . ? F11 P10 F13 90.84(17) . . ? F15 P10 F13 175.9(2) . . ? F12 P10 F13 90.45(17) . . ? F16 P10 F13 87.43(15) . . ? F11 P10 F14 88.24(15) . . ? F15 P10 F14 89.55(17) . . ? F12 P10 F14 177.53(19) . . ? F16 P10 F14 90.55(17) . . ? F13 P10 F14 87.10(16) . . ? F24 P20 F26 91.59(17) . . ? F24 P20 F23 91.67(16) . . ? F26 P20 F23 90.68(14) . . ? F24 P20 F21 90.41(16) . . ? F26 P20 F21 177.77(16) . . ? F23 P20 F21 90.26(16) . . ? F24 P20 F25 89.79(14) . . ? F26 P20 F25 88.92(14) . . ? F23 P20 F25 178.50(15) . . ? F21 P20 F25 90.09(15) . . ? F24 P20 F22 176.61(16) . . ? F26 P20 F22 90.07(16) . . ? F23 P20 F22 91.27(15) . . ? F21 P20 F22 87.89(14) . . ? F25 P20 F22 87.29(13) . . ? F24' P20' F23' 90.9(7) . . ? F24' P20' F21' 91.5(7) . . ? F23' P20' F21' 91.3(7) . . ? F24' P20' F25' 91.2(7) . . ? F23' P20' F25' 177.8(9) . . ? F21' P20' F25' 89.1(7) . . ? F24' P20' F22' 177.6(9) . . ? F23' P20' F22' 88.9(7) . . ? F21' P20' F22' 90.9(7) . . ? F25' P20' F22' 88.9(7) . . ? F24' P20' F26' 88.4(7) . . ? F23' P20' F26' 91.5(7) . . ? F21' P20' F26' 177.2(9) . . ? F25' P20' F26' 88.1(7) . . ? F22' P20' F26' 89.2(7) . . ? Cl2 C100 Cl1 96.0(5) . . ? Cl3 C101 Cl4 123.4(4) . . ? Cl5 C102 Cl6 127.3(14) . . ? O110 C111 C112 104.2(6) . . ? O115 C116 C117 111.8(12) . . ? O120 C121 C122 99.3(15) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.157 _refine_diff_density_min -1.675 _refine_diff_density_rms 0.092 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 764407' #TrackingRef 'EJIC 01-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H48 Au2 N2 P2 S4, 2(C H2 Cl2), 0.5(C2 H6 O)' _chemical_formula_sum 'C57 H55 Au2 Cl4 N2 O0.50 P2 S4' _chemical_formula_weight 1501.94 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' 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 9.0346(3) _cell_length_b 12.1805(3) _cell_length_c 14.0257(4) _cell_angle_alpha 93.738(2) _cell_angle_beta 105.979(3) _cell_angle_gamma 102.402(3) _cell_volume 1436.45(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used 8716 _cell_measurement_theta_min 3.0413 _cell_measurement_theta_max 32.6893 _exptl_crystal_description plates _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 735 _exptl_absorpt_coefficient_mu 5.528 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.331 _exptl_absorpt_correction_T_max 0.685 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ? _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16291 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 32.75 _reflns_number_total 9388 _reflns_number_gt 7186 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Two partial occupancy orientations were identified for the dichloromethane solvent molecule. A single SADI restraint was used for each of the four C-Cl bonds, and another was used for the two Cl...Cl distances. A SIMU restraint was used for the two carbon atoms, and two separate ones for the two pairs of proximal chlorine atoms. The O-H proton of the 25% occupancy ethanol molecule could not be located, and so the atom list for the asymmetric unit is low by H0.25. ; _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^)+(0.0382P)^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 9388 _refine_ls_number_parameters 341 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.034 _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 Au1 Au 0.446864(18) 0.912377(13) 0.340038(13) 0.02586(5) Uani 1 1 d . . . S1 S 0.62133(11) 0.85520(7) 0.47189(7) 0.02345(19) Uani 1 1 d . . . C2 C 0.5523(4) 0.7090(3) 0.4350(3) 0.0224(7) Uani 1 1 d . . . S3 S 0.40196(13) 0.65382(9) 0.32894(8) 0.0332(2) Uani 1 1 d . . . N4 N 0.6251(4) 0.6425(2) 0.4946(2) 0.0234(7) Uani 1 1 d . . . C5 C 0.5664(5) 0.5179(3) 0.4752(3) 0.0274(8) Uani 1 1 d . . . H5A H 0.6543 0.4817 0.5030 0.033 Uiso 1 1 calc R . . H5B H 0.5245 0.4930 0.4022 0.033 Uiso 1 1 calc R . . C6 C 0.7563(4) 0.6877(3) 0.5862(3) 0.0238(8) Uani 1 1 d . . . H6A H 0.7615 0.6287 0.6316 0.029 Uiso 1 1 calc R . . H6B H 0.7340 0.7531 0.6205 0.029 Uiso 1 1 calc R . . C7 C 0.9161(4) 0.7251(3) 0.5682(3) 0.0239(8) Uani 1 1 d . . . C8 C 1.0178(5) 0.8266(4) 0.6186(4) 0.0344(10) Uani 1 1 d . . . H8A H 0.9856 0.8728 0.6625 0.041 Uiso 1 1 calc R . . C9 C 1.1679(5) 0.8614(4) 0.6053(4) 0.0436(12) Uani 1 1 d . . . H9A H 1.2375 0.9310 0.6405 0.052 Uiso 1 1 calc R . . C10 C 1.2154(5) 0.7961(4) 0.5417(4) 0.0404(11) Uani 1 1 d . . . H10A H 1.3172 0.8200 0.5326 0.049 Uiso 1 1 calc R . . C11 C 1.1157(5) 0.6973(4) 0.4922(4) 0.0415(11) Uani 1 1 d . . . H11A H 1.1491 0.6516 0.4486 0.050 Uiso 1 1 calc R . . C12 C 0.9632(5) 0.6601(4) 0.5035(4) 0.0352(10) Uani 1 1 d . . . H12A H 0.8939 0.5910 0.4670 0.042 Uiso 1 1 calc R . . P13 P 0.27302(12) 0.96086(8) 0.21122(8) 0.0242(2) Uani 1 1 d . . . C14 C 0.2857(5) 0.9041(4) 0.0913(3) 0.0292(8) Uani 1 1 d . . . C15 C 0.2943(7) 0.7918(4) 0.0783(4) 0.0503(13) Uani 1 1 d . . . H15A H 0.3004 0.7481 0.1322 0.060 Uiso 1 1 calc R . . C16 C 0.2940(9) 0.7440(5) -0.0152(5) 0.073(2) Uani 1 1 d . . . H16A H 0.2941 0.6661 -0.0253 0.088 Uiso 1 1 calc R . . C17 C 0.2935(6) 0.8066(5) -0.0918(4) 0.0490(13) Uani 1 1 d . . . H17A H 0.2965 0.7736 -0.1542 0.059 Uiso 1 1 calc R . . C18 C 0.2886(6) 0.9180(5) -0.0779(4) 0.0451(12) Uani 1 1 d . . . H18A H 0.2880 0.9623 -0.1312 0.054 Uiso 1 1 calc R . . C19 C 0.2843(5) 0.9668(4) 0.0133(3) 0.0355(10) Uani 1 1 d . . . H19A H 0.2805 1.0441 0.0218 0.043 Uiso 1 1 calc R . . C20 C 0.0707(5) 0.9003(3) 0.2128(3) 0.0270(8) Uani 1 1 d . . . C21 C -0.0518(5) 0.8518(4) 0.1265(3) 0.0353(10) Uani 1 1 d . . . H21A H -0.0319 0.8479 0.0635 0.042 Uiso 1 1 calc R . . C22 C -0.2041(5) 0.8090(4) 0.1330(4) 0.0408(11) Uani 1 1 d . . . H22A H -0.2888 0.7763 0.0743 0.049 Uiso 1 1 calc R . . C23 C -0.2318(6) 0.8143(4) 0.2257(4) 0.0452(12) Uani 1 1 d . . . H23A H -0.3358 0.7862 0.2302 0.054 Uiso 1 1 calc R . . C24 C -0.1104(6) 0.8594(4) 0.3097(4) 0.0437(12) Uani 1 1 d . . . H24A H -0.1302 0.8615 0.3728 0.052 Uiso 1 1 calc R . . C25 C 0.0415(5) 0.9025(4) 0.3050(3) 0.0344(9) Uani 1 1 d . . . H25A H 0.1256 0.9334 0.3645 0.041 Uiso 1 1 calc R . . C26 C 0.2860(5) 1.1109(3) 0.2042(3) 0.0263(8) Uani 1 1 d . . . C27 C 0.1525(5) 1.1503(4) 0.1589(3) 0.0329(9) Uani 1 1 d . . . H27A H 0.0508 1.0991 0.1357 0.040 Uiso 1 1 calc R . . C28 C 0.1690(6) 1.2640(4) 0.1480(4) 0.0415(11) Uani 1 1 d . . . H28A H 0.0787 1.2909 0.1165 0.050 Uiso 1 1 calc R . . C29 C 0.3180(7) 1.3390(4) 0.1832(4) 0.0484(14) Uani 1 1 d . . . H29A H 0.3293 1.4171 0.1759 0.058 Uiso 1 1 calc R . . C30 C 0.4468(6) 1.3009(4) 0.2279(4) 0.0424(12) Uani 1 1 d . . . H30A H 0.5479 1.3529 0.2514 0.051 Uiso 1 1 calc R . . C31 C 0.4343(5) 1.1869(4) 0.2401(3) 0.0343(9) Uani 1 1 d . . . H31A H 0.5255 1.1615 0.2725 0.041 Uiso 1 1 calc R . . C40 C 0.9654(9) 0.5816(5) 0.2206(5) 0.0544(17) Uani 0.875(4) 1 d PDU A 1 H40A H 0.8743 0.6169 0.2111 0.065 Uiso 0.875(4) 1 calc PR A 1 H40B H 1.0607 0.6367 0.2648 0.065 Uiso 0.875(4) 1 calc PR A 1 Cl1 Cl 0.9944(4) 0.55108(19) 0.10656(18) 0.0856(8) Uani 0.875(4) 1 d PDU A 1 Cl2 Cl 0.9286(2) 0.45868(13) 0.27756(14) 0.0640(6) Uani 0.875(4) 1 d PDU A 1 C40' C 0.961(4) 0.527(5) 0.207(2) 0.062(6) Uiso 0.125(4) 1 d PDU A 2 H40C H 1.0435 0.5926 0.2485 0.075 Uiso 0.125(4) 1 calc PR A 2 H40D H 1.0051 0.4597 0.2088 0.075 Uiso 0.125(4) 1 calc PR A 2 Cl1' Cl 0.898(3) 0.5557(17) 0.0849(13) 0.089(4) Uiso 0.125(4) 1 d PDU A 2 Cl2' Cl 0.795(2) 0.5028(16) 0.2503(14) 0.103(4) Uiso 0.125(4) 1 d PDU A 2 O50 O 0.576(4) 0.550(2) 0.162(2) 0.134(10) Uiso 0.25 1 d P B -1 C51 C 0.469(5) 0.572(3) 0.076(3) 0.111(12) Uiso 0.25 1 d P B -1 H51A H 0.4938 0.6517 0.0631 0.133 Uiso 0.25 1 calc PR B -1 H51B H 0.3563 0.5466 0.0745 0.133 Uiso 0.25 1 calc PR B -1 C52 C 0.522(9) 0.488(7) 0.008(6) 0.132(15) Uiso 0.25 1 d P B -1 H52A H 0.4578 0.4823 -0.0622 0.198 Uiso 0.25 1 calc PR B -1 H52B H 0.5060 0.4128 0.0297 0.198 Uiso 0.25 1 calc PR B -1 H52C H 0.6341 0.5171 0.0133 0.198 Uiso 0.25 1 calc PR B -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 Au1 0.02104(7) 0.02857(8) 0.02866(9) 0.00618(6) 0.00654(5) 0.00781(5) S1 0.0197(4) 0.0197(4) 0.0285(5) 0.0035(4) 0.0045(4) 0.0029(3) C2 0.0194(17) 0.0199(16) 0.028(2) 0.0019(15) 0.0101(15) 0.0019(14) S3 0.0278(5) 0.0285(5) 0.0335(6) 0.0014(4) -0.0008(4) 0.0000(4) N4 0.0178(15) 0.0212(14) 0.0299(18) 0.0054(13) 0.0075(13) 0.0007(12) C5 0.026(2) 0.0196(17) 0.037(2) 0.0038(16) 0.0129(17) 0.0035(15) C6 0.0255(18) 0.0244(17) 0.024(2) 0.0069(15) 0.0097(15) 0.0072(15) C7 0.0178(17) 0.0286(18) 0.025(2) 0.0078(15) 0.0054(14) 0.0053(15) C8 0.024(2) 0.032(2) 0.044(3) -0.0001(19) 0.0115(18) 0.0015(17) C9 0.023(2) 0.047(3) 0.055(3) 0.006(2) 0.011(2) -0.003(2) C10 0.0179(19) 0.060(3) 0.045(3) 0.014(2) 0.0114(18) 0.008(2) C11 0.030(2) 0.065(3) 0.038(3) 0.007(2) 0.0169(19) 0.020(2) C12 0.027(2) 0.041(2) 0.038(3) -0.001(2) 0.0122(18) 0.0066(19) P13 0.0229(5) 0.0277(5) 0.0230(5) 0.0031(4) 0.0073(4) 0.0080(4) C14 0.0213(18) 0.037(2) 0.029(2) -0.0023(17) 0.0100(15) 0.0063(16) C15 0.067(4) 0.036(2) 0.052(3) -0.002(2) 0.030(3) 0.008(2) C16 0.095(5) 0.036(3) 0.082(5) -0.010(3) 0.037(4) -0.008(3) C17 0.047(3) 0.063(3) 0.036(3) -0.012(2) 0.024(2) 0.002(3) C18 0.042(3) 0.064(3) 0.033(3) -0.002(2) 0.018(2) 0.012(2) C19 0.039(2) 0.044(2) 0.028(2) 0.0027(19) 0.0144(18) 0.015(2) C20 0.028(2) 0.0265(18) 0.029(2) 0.0059(16) 0.0105(16) 0.0080(16) C21 0.031(2) 0.040(2) 0.032(2) 0.0072(19) 0.0074(18) 0.0045(19) C22 0.024(2) 0.047(3) 0.046(3) 0.009(2) 0.0051(19) 0.0023(19) C23 0.029(2) 0.047(3) 0.065(4) 0.016(3) 0.023(2) 0.008(2) C24 0.050(3) 0.050(3) 0.048(3) 0.015(2) 0.034(2) 0.022(2) C25 0.037(2) 0.040(2) 0.033(2) 0.0082(19) 0.0160(19) 0.0146(19) C26 0.030(2) 0.0309(19) 0.0205(19) 0.0030(16) 0.0092(15) 0.0100(16) C27 0.035(2) 0.033(2) 0.029(2) -0.0002(17) 0.0046(17) 0.0126(18) C28 0.057(3) 0.039(2) 0.033(3) 0.007(2) 0.009(2) 0.026(2) C29 0.079(4) 0.031(2) 0.048(3) 0.010(2) 0.036(3) 0.017(3) C30 0.045(3) 0.032(2) 0.054(3) -0.001(2) 0.030(2) 0.001(2) C31 0.029(2) 0.039(2) 0.036(2) 0.0031(19) 0.0147(18) 0.0063(18) C40 0.063(4) 0.034(3) 0.064(4) 0.006(3) 0.015(3) 0.011(3) Cl1 0.111(2) 0.0693(12) 0.0746(15) -0.0020(11) 0.0431(15) 0.0014(14) Cl2 0.0794(13) 0.0451(8) 0.0637(11) 0.0090(7) 0.0182(9) 0.0107(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 Au1 P13 2.2483(10) . ? Au1 S1 2.3290(10) . ? Au1 S3 3.0756(10) . ? S1 C2 1.747(4) . ? C2 N4 1.343(5) . ? C2 S3 1.695(4) . ? N4 C6 1.465(5) . ? N4 C5 1.476(5) . ? C5 C5 1.545(8) 2_666 ? C6 C7 1.513(5) . ? C7 C12 1.377(6) . ? C7 C8 1.383(6) . ? C8 C9 1.399(6) . ? C9 C10 1.370(7) . ? C10 C11 1.351(7) . ? C11 C12 1.411(6) . ? P13 C26 1.817(4) . ? P13 C14 1.819(4) . ? P13 C20 1.826(4) . ? C14 C19 1.373(6) . ? C14 C15 1.390(6) . ? C15 C16 1.398(8) . ? C16 C17 1.357(8) . ? C17 C18 1.370(8) . ? C18 C19 1.389(7) . ? C20 C21 1.387(6) . ? C20 C25 1.388(6) . ? C21 C22 1.394(6) . ? C22 C23 1.389(7) . ? C23 C24 1.356(8) . ? C24 C25 1.382(7) . ? C26 C31 1.393(6) . ? C26 C27 1.398(6) . ? C27 C28 1.385(6) . ? C28 C29 1.392(7) . ? C29 C30 1.353(8) . ? C30 C31 1.394(6) . ? C40 Cl1 1.720(7) . ? C40 Cl2 1.755(6) . ? C40' Cl1' 1.726(17) . ? C40' Cl2' 1.741(17) . ? O50 C51 1.40(5) . ? C51 C52 1.59(9) . ? 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 P13 Au1 S1 177.86(3) . . ? P13 Au1 S3 111.96(3) . . ? S1 Au1 S3 65.96(3) . . ? C2 S1 Au1 97.67(14) . . ? N4 C2 S3 121.6(3) . . ? N4 C2 S1 116.6(3) . . ? S3 C2 S1 121.8(2) . . ? C2 S3 Au1 74.60(13) . . ? C2 N4 C6 122.9(3) . . ? C2 N4 C5 120.8(3) . . ? C6 N4 C5 116.1(3) . . ? N4 C5 C5 108.9(4) . 2_666 ? N4 C6 C7 113.8(3) . . ? C12 C7 C8 119.3(4) . . ? C12 C7 C6 121.5(4) . . ? C8 C7 C6 119.2(4) . . ? C7 C8 C9 120.2(4) . . ? C10 C9 C8 120.5(4) . . ? C11 C10 C9 119.2(4) . . ? C10 C11 C12 121.6(5) . . ? C7 C12 C11 119.1(4) . . ? C26 P13 C14 105.04(19) . . ? C26 P13 C20 105.52(18) . . ? C14 P13 C20 106.03(19) . . ? C26 P13 Au1 117.87(14) . . ? C14 P13 Au1 111.76(14) . . ? C20 P13 Au1 109.81(13) . . ? C19 C14 C15 119.1(4) . . ? C19 C14 P13 122.8(3) . . ? C15 C14 P13 118.1(4) . . ? C14 C15 C16 119.3(5) . . ? C17 C16 C15 121.3(6) . . ? C16 C17 C18 119.2(5) . . ? C17 C18 C19 120.7(5) . . ? C14 C19 C18 120.4(5) . . ? C21 C20 C25 119.8(4) . . ? C21 C20 P13 122.6(3) . . ? C25 C20 P13 117.6(3) . . ? C20 C21 C22 119.6(4) . . ? C23 C22 C21 119.8(5) . . ? C24 C23 C22 120.1(4) . . ? C23 C24 C25 121.1(5) . . ? C24 C25 C20 119.6(5) . . ? C31 C26 C27 119.7(4) . . ? C31 C26 P13 118.7(3) . . ? C27 C26 P13 121.5(3) . . ? C28 C27 C26 119.9(4) . . ? C27 C28 C29 119.9(5) . . ? C30 C29 C28 120.2(4) . . ? C29 C30 C31 121.4(5) . . ? C26 C31 C30 119.0(4) . . ? Cl1 C40 Cl2 111.2(4) . . ? Cl1' C40' Cl2' 107.2(15) . . ? O50 C51 C52 90(4) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.746 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.146 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 764408' #TrackingRef 'EJIC 01-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 Au2 N2 P2 S4' _chemical_formula_sum 'C24 H36 Au2 N2 P2 S4' _chemical_formula_weight 936.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 6.41819(12) _cell_length_b 23.1984(4) _cell_length_c 10.39421(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.3353(16) _cell_angle_gamma 90.00 _cell_volume 1543.18(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 9180 _cell_measurement_theta_min 3.1774 _cell_measurement_theta_max 32.6472 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 9.887 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.163 _exptl_absorpt_correction_T_max 0.562 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ? _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16525 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 32.71 _reflns_number_total 5174 _reflns_number_gt 4032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Two partial occupancy orientations were identified for the AuPMe3 unit. Separate SADI restraints were used for the two Au-P bonds, for the six P-C bonds, for the six C...C distances, and for the six Au...C distances. Separate SIMU restraints were used for the two gold atoms, the two phosphorus atoms, and each pair of proximal carbon atoms. ; _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^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00060(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5174 _refine_ls_number_parameters 176 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0340 _refine_ls_wR_factor_gt 0.0332 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.003 _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 Au1 Au 0.389171(13) 0.708061(3) 0.795649(8) 0.02609(3) Uani 0.9578(4) 1 d PDU A 1 Au1' Au 0.1771(3) 0.69292(9) 0.7128(2) 0.0336(7) Uiso 0.0422(4) 1 d PDU A 2 S1 S 0.65090(8) 0.64130(2) 0.76559(5) 0.02596(11) Uani 1 1 d . . . C2 C 0.5055(3) 0.59126(8) 0.67134(18) 0.0194(4) Uani 1 1 d . A . S3 S 0.26025(7) 0.60655(2) 0.60950(5) 0.02719(11) Uani 1 1 d . . . N4 N 0.5972(2) 0.54033(6) 0.64845(16) 0.0204(3) Uani 1 1 d . . . C5 C 0.8105(3) 0.52520(8) 0.6945(2) 0.0236(4) Uani 1 1 d . A . H5A H 0.8850 0.5607 0.7244 0.028 Uiso 1 1 calc R . . H5B H 0.8832 0.5094 0.6216 0.028 Uiso 1 1 calc R . . C6 C 0.8238(3) 0.48183(8) 0.80281(19) 0.0211(4) Uani 1 1 d . . . C7 C 0.6570(3) 0.46826(9) 0.8743(2) 0.0272(4) Uani 1 1 d . A . H7A H 0.5247 0.4856 0.8533 0.033 Uiso 1 1 calc R . . C8 C 0.6810(3) 0.42980(9) 0.9757(2) 0.0315(5) Uani 1 1 d . . . H8A H 0.5650 0.4209 1.0238 0.038 Uiso 1 1 calc R A . C9 C 0.8710(3) 0.40423(9) 1.0078(2) 0.0326(5) Uani 1 1 d . A . H9A H 0.8868 0.3780 1.0780 0.039 Uiso 1 1 calc R . . C10 C 1.0381(3) 0.41700(10) 0.9372(2) 0.0379(6) Uani 1 1 d . . . H10A H 1.1700 0.3995 0.9587 0.045 Uiso 1 1 calc R A . C11 C 1.0149(3) 0.45496(9) 0.8357(2) 0.0309(5) Uani 1 1 d . A . H11A H 1.1310 0.4630 0.7870 0.037 Uiso 1 1 calc R . . C12 C 0.4872(3) 0.49535(8) 0.57165(18) 0.0229(4) Uani 1 1 d . . . H12A H 0.3369 0.4961 0.5872 0.027 Uiso 1 1 calc R . . H12B H 0.5438 0.4571 0.5983 0.027 Uiso 1 1 calc R . . P13 P 0.15469(12) 0.77585(3) 0.83832(7) 0.03040(15) Uani 0.9578(4) 1 d PDU A 1 C14 C -0.0115(5) 0.79649(14) 0.6985(3) 0.0657(9) Uani 0.9578(4) 1 d PDU A 1 H14A H -0.1103 0.8260 0.7228 0.099 Uiso 0.9578(4) 1 calc PR A 1 H14B H -0.0887 0.7627 0.6642 0.099 Uiso 0.9578(4) 1 calc PR A 1 H14C H 0.0743 0.8120 0.6324 0.099 Uiso 0.9578(4) 1 calc PR A 1 C15 C 0.2706(4) 0.84194(10) 0.9007(3) 0.0506(7) Uani 0.9578(4) 1 d PDU A 1 H15A H 0.1600 0.8695 0.9171 0.076 Uiso 0.9578(4) 1 calc PR A 1 H15B H 0.3600 0.8582 0.8376 0.076 Uiso 0.9578(4) 1 calc PR A 1 H15C H 0.3546 0.8340 0.9814 0.076 Uiso 0.9578(4) 1 calc PR A 1 C16 C -0.0230(5) 0.75493(12) 0.9559(3) 0.0395(6) Uani 0.9578(4) 1 d PDU A 1 H16A H -0.1199 0.7867 0.9690 0.059 Uiso 0.9578(4) 1 calc PR A 1 H16B H 0.0562 0.7459 1.0377 0.059 Uiso 0.9578(4) 1 calc PR A 1 H16C H -0.1020 0.7209 0.9250 0.059 Uiso 0.9578(4) 1 calc PR A 1 P13' P 0.071(2) 0.7708(6) 0.8187(16) 0.029(4) Uiso 0.0422(4) 1 d PDU A 2 C14' C -0.120(7) 0.8138(15) 0.727(4) 0.064(6) Uiso 0.0422(4) 1 d PDU A 2 H14D H -0.1587 0.8468 0.7791 0.096 Uiso 0.0422(4) 1 calc PR A 2 H14E H -0.2441 0.7904 0.7038 0.096 Uiso 0.0422(4) 1 calc PR A 2 H14F H -0.0609 0.8276 0.6486 0.096 Uiso 0.0422(4) 1 calc PR A 2 C15' C 0.276(5) 0.8197(15) 0.872(5) 0.050(6) Uiso 0.0422(4) 1 d PDU A 2 H15D H 0.2171 0.8522 0.9167 0.076 Uiso 0.0422(4) 1 calc PR A 2 H15E H 0.3447 0.8339 0.7968 0.076 Uiso 0.0422(4) 1 calc PR A 2 H15F H 0.3785 0.7996 0.9303 0.076 Uiso 0.0422(4) 1 calc PR A 2 C16' C -0.052(10) 0.7526(15) 0.964(4) 0.037(6) Uiso 0.0422(4) 1 d PDU A 2 H16D H -0.0959 0.7880 1.0062 0.056 Uiso 0.0422(4) 1 calc PR A 2 H16E H 0.0474 0.7316 1.0233 0.056 Uiso 0.0422(4) 1 calc PR A 2 H16F H -0.1747 0.7283 0.9426 0.056 Uiso 0.0422(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03524(5) 0.01938(4) 0.02414(4) -0.00144(3) 0.00557(3) 0.00368(4) S1 0.0269(3) 0.0225(3) 0.0280(3) -0.0046(2) -0.0013(2) -0.00041(19) C2 0.0208(9) 0.0185(9) 0.0194(9) 0.0030(7) 0.0048(8) -0.0019(7) S3 0.0203(2) 0.0258(3) 0.0353(3) -0.0005(2) 0.0008(2) 0.00086(19) N4 0.0220(8) 0.0166(8) 0.0225(8) 0.0016(6) 0.0022(7) -0.0009(6) C5 0.0207(9) 0.0203(10) 0.0306(11) 0.0032(8) 0.0069(9) 0.0020(7) C6 0.0225(9) 0.0169(9) 0.0242(10) -0.0023(7) 0.0033(9) 0.0004(7) C7 0.0241(10) 0.0280(11) 0.0302(11) 0.0029(8) 0.0062(9) 0.0025(8) C8 0.0334(12) 0.0322(12) 0.0298(12) 0.0041(9) 0.0075(10) -0.0039(9) C9 0.0442(13) 0.0274(12) 0.0254(11) 0.0048(9) -0.0029(10) 0.0002(9) C10 0.0310(12) 0.0436(14) 0.0380(13) 0.0076(11) -0.0050(11) 0.0095(10) C11 0.0214(10) 0.0378(13) 0.0337(12) 0.0040(10) 0.0034(10) 0.0038(9) C12 0.0294(10) 0.0164(9) 0.0235(10) -0.0002(7) 0.0060(9) -0.0044(8) P13 0.0390(4) 0.0234(3) 0.0285(3) -0.0043(2) 0.0007(3) 0.0082(3) C14 0.070(2) 0.071(2) 0.0533(19) 0.0089(16) -0.0127(17) 0.0269(17) C15 0.0640(17) 0.0254(14) 0.065(2) -0.0118(13) 0.0207(16) -0.0007(12) C16 0.0343(15) 0.0396(14) 0.0451(15) -0.0132(12) 0.0070(12) 0.0017(11) _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 Au1 P13 2.2440(6) . ? Au1 S1 2.3233(5) . ? Au1 S3 3.1196(5) . ? Au1' P13' 2.248(13) . ? Au1' S3 2.353(2) . ? S1 C2 1.7436(19) . ? C2 N4 1.349(2) . ? C2 S3 1.6922(19) . ? N4 C5 1.459(2) . ? N4 C12 1.463(2) . ? C5 C6 1.507(3) . ? C6 C7 1.384(3) . ? C6 C11 1.395(3) . ? C7 C8 1.381(3) . ? C8 C9 1.374(3) . ? C9 C10 1.377(3) . ? C10 C11 1.374(3) . ? C12 C12 1.526(4) 3_666 ? P13 C16 1.800(3) . ? P13 C14 1.801(3) . ? P13 C15 1.803(3) . ? P13' C15' 1.792(13) . ? P13' C14' 1.795(13) . ? P13' C16' 1.811(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 P13 Au1 S1 175.07(2) . . ? P13' Au1' S3 174.4(4) . . ? C2 S1 Au1 99.07(6) . . ? N4 C2 S3 121.49(14) . . ? N4 C2 S1 117.39(14) . . ? S3 C2 S1 121.12(11) . . ? C2 S3 Au1' 103.99(9) . . ? C2 S3 Au1 74.17(6) . . ? C2 N4 C5 124.33(16) . . ? C2 N4 C12 121.46(16) . . ? C5 N4 C12 114.20(15) . . ? N4 C5 C6 113.85(15) . . ? C7 C6 C11 117.92(19) . . ? C7 C6 C5 123.38(17) . . ? C11 C6 C5 118.68(17) . . ? C8 C7 C6 120.71(19) . . ? C9 C8 C7 120.6(2) . . ? C8 C9 C10 119.4(2) . . ? C11 C10 C9 120.2(2) . . ? C10 C11 C6 121.1(2) . . ? N4 C12 C12 110.41(18) . 3_666 ? C16 P13 C14 104.64(17) . . ? C16 P13 C15 104.49(12) . . ? C14 P13 C15 105.49(15) . . ? C16 P13 Au1 114.46(9) . . ? C14 P13 Au1 113.07(11) . . ? C15 P13 Au1 113.73(10) . . ? C15' P13' C14' 105.5(10) . . ? C15' P13' C16' 104.3(10) . . ? C14' P13' C16' 104.4(10) . . ? C15' P13' Au1' 114.6(9) . . ? C14' P13' Au1' 114.0(9) . . ? C16' P13' Au1' 112.9(9) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.973 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.089 #===END