# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-05 at 12:46:59 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : sl85-a0 sl85-a0_ch2cl2-aac-abspack data_sl85-a0 _audit_creation_date 2010-08-05T12:46:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic data_publication_text _publ_requested_journal 'Chem. Commun.' _publ_contact_author_name 'Schollhammer, Philippe' _publ_contact_author_address ;Laboratoire de chimie, electrochimie moleculaire et chimie analytique (UMR 6521) Universite de Bretagne occidentale 6, avenue Victor Le Gorgeu CS 93837 F-29238 BREST cedex 3 FRANCE ; _publ_contact_author_email philippe.schollhammer@univ-brest.fr loop_ _publ_author_name 'Petillon, Francois Y.' 'Capon,Jean-Francois' 'Talarmin, Jean' 'Schollhammer, Philippe' 'Gloaguen, Frederic' 'Lounissi, Sondes' 'Matoussi, Fatma' _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C71 H70 Cl2 Fe4 N4 O8 P4 S4' _chemical_formula_moiety '2(C35 H34 Fe2 N2 O4 P2 S2), C H2 Cl2' _chemical_formula_weight 1653.73 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6550(7) _cell_length_b 12.7551(9) _cell_length_c 14.3432(10) _cell_angle_alpha 103.409(6) _cell_angle_beta 99.559(6) _cell_angle_gamma 99.746(6) _cell_volume 1825.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 4962 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 30.51 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description ; tip of blade, main axis [1 0 0], main faces {0 1 0}, {0 0 1} ; _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.03 0 1 0 0.015 0 0 1 0.03 0 0 -1 0.035 -1 0 1 0.05 1 0 0 0.06 -1 1 -1 0.045 -1 -1 1 0.05 0 1 -1 0.035 0 -1 1 0.045 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.111 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 0.955 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed X-ray tube' _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.3622 _diffrn_orient_matrix_ub_11 0.0041803657 _diffrn_orient_matrix_ub_12 -0.0314982644 _diffrn_orient_matrix_ub_13 0.0347330827 _diffrn_orient_matrix_ub_21 -0.0094035129 _diffrn_orient_matrix_ub_22 0.0447207814 _diffrn_orient_matrix_ub_23 0.036099453 _diffrn_orient_matrix_ub_31 -0.0683786769 _diffrn_orient_matrix_ub_32 -0.020903518 _diffrn_orient_matrix_ub_33 -0.0141132402 _diffrn_measurement_device 'Kappa-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method ; 4 stepped omega-scans over 115 deg. with kappa -79 deg. (chi -58.3 deg.), phi 0, 90, 180, 270 deg. step 1 deg., exposure time 150 s detector distance 50 mm detector angle 30 deg. ; _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_unetI/netI 0.1092 _diffrn_reflns_number 14161 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7431 _reflns_number_gt 4835 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1980-2002)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^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_number_reflns 7431 _refine_ls_number_parameters 435 _refine_ls_number_restraints 153 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.775 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3736(5) 0.8535(4) 0.3739(4) 0.0261(11) Uani 1 1 d U . . C2 C 0.5759(5) 0.6606(5) 0.1131(4) 0.0361(13) Uani 1 1 d U . . C3 C 0.6002(5) 0.8773(5) 0.1598(4) 0.0312(12) Uani 1 1 d U . . C4 C 0.6144(5) 0.7925(5) 0.3068(4) 0.0332(12) Uani 1 1 d U . . C5 C 0.2762(5) 0.5307(4) 0.1427(4) 0.0315(12) Uani 1 1 d U . . H5A H 0.3372 0.4938 0.1089 0.038 Uiso 1 1 calc R . . H5B H 0.2275 0.4769 0.1708 0.038 Uiso 1 1 calc R . . C6 C 0.1806(5) 0.5587(4) 0.0673(4) 0.0327(12) Uani 1 1 d U . . H6A H 0.1177 0.5933 0.1006 0.039 Uiso 1 1 calc R . . H6B H 0.1309 0.4891 0.0191 0.039 Uiso 1 1 calc R . . C7 C 0.2406(5) 0.6357(4) 0.0116(4) 0.0297(12) Uani 1 1 d U . . H7A H 0.1705 0.6447 -0.0387 0.036 Uiso 1 1 calc R . . H7B H 0.3022 0.6007 -0.023 0.036 Uiso 1 1 calc R . . C8 C 0.0738(4) 0.8915(4) 0.3592(4) 0.0203(10) Uani 1 1 d U . . H8A H -0.0164 0.8698 0.3677 0.024 Uiso 1 1 calc R . . H8B H 0.134 0.896 0.4212 0.024 Uiso 1 1 calc R . . C9 C 0.2261(4) 1.0498(4) 0.3394(3) 0.0210(10) Uani 1 1 d U . . H9A H 0.2848 1.051 0.401 0.025 Uiso 1 1 calc R . . H9B H 0.232 1.1269 0.3354 0.025 Uiso 1 1 calc R . . C10 C 0.0142(4) 1.0726(4) 0.3784(3) 0.0209(10) Uani 1 1 d U . . C11 C 0.0662(5) 1.1813(4) 0.4343(3) 0.0208(10) Uani 1 1 d U . . H11 H 0.158 1.2076 0.4536 0.025 Uiso 1 1 calc R . . C12 C -0.0152(5) 1.2509(4) 0.4618(4) 0.0255(11) Uani 1 1 d U . . H12 H 0.0214 1.325 0.4988 0.031 Uiso 1 1 calc R . . C13 C -0.1483(5) 1.2146(4) 0.4364(4) 0.0322(12) Uani 1 1 d U . . H13 H -0.2036 1.2631 0.4553 0.039 Uiso 1 1 calc R . . C14 C -0.2004(5) 1.1065(4) 0.3830(4) 0.0315(12) Uani 1 1 d U . . H14 H -0.2923 1.0805 0.3661 0.038 Uiso 1 1 calc R . . C15 C -0.1222(5) 1.0362(4) 0.3539(4) 0.0265(11) Uani 1 1 d U . . H15 H -0.1603 0.9623 0.3169 0.032 Uiso 1 1 calc R . . C16 C -0.0110(4) 0.8000(4) 0.1525(4) 0.0234(11) Uani 1 1 d U . . H16A H -0.066 0.7269 0.1151 0.028 Uiso 1 1 calc R . . H16B H -0.069 0.848 0.1768 0.028 Uiso 1 1 calc R . . C17 C 0.1370(4) 0.9594(4) 0.1320(4) 0.0242(11) Uani 1 1 d U . . H17A H 0.0803 1.0078 0.1582 0.029 Uiso 1 1 calc R . . H17B H 0.1708 0.9877 0.0803 0.029 Uiso 1 1 calc R . . C18 C -0.0034(5) 0.8195(4) -0.0127(4) 0.0241(11) Uani 1 1 d U . . C19 C 0.0730(5) 0.8301(4) -0.0822(4) 0.0304(12) Uani 1 1 d U . . H19 H 0.1638 0.8615 -0.0608 0.037 Uiso 1 1 calc R . . C20 C 0.0184(6) 0.7958(4) -0.1808(4) 0.0355(13) Uani 1 1 d U . . H20 H 0.0715 0.8024 -0.2271 0.043 Uiso 1 1 calc R . . C21 C -0.1141(6) 0.7515(4) -0.2127(4) 0.0378(13) Uani 1 1 d U . . H21 H -0.1514 0.7267 -0.281 0.045 Uiso 1 1 calc R . . C22 C -0.1915(6) 0.7431(4) -0.1466(4) 0.0327(12) Uani 1 1 d U . . H22 H -0.2826 0.714 -0.1692 0.039 Uiso 1 1 calc R . . C23 C -0.1373(5) 0.7772(4) -0.0462(4) 0.0266(11) Uani 1 1 d U . . H23 H -0.1916 0.7717 -0.0005 0.032 Uiso 1 1 calc R . . C24 C 0.0162(4) 0.6610(4) 0.2846(3) 0.0200(10) Uani 1 1 d U . . C25 C -0.1206(5) 0.6360(5) 0.2674(4) 0.0349(13) Uani 1 1 d U . . H25 H -0.1688 0.6829 0.2417 0.042 Uiso 1 1 calc R . . C26 C -0.1843(6) 0.5444(5) 0.2876(5) 0.0467(16) Uani 1 1 d U . . H26 H -0.2769 0.5281 0.2753 0.056 Uiso 1 1 calc R . . C27 C -0.1169(6) 0.4748(5) 0.3256(4) 0.0399(14) Uani 1 1 d U . . H27 H -0.1623 0.4111 0.3391 0.048 Uiso 1 1 calc R . . C28 C 0.0175(6) 0.4995(4) 0.3437(4) 0.0347(13) Uani 1 1 d U . . H28 H 0.0654 0.4535 0.3712 0.042 Uiso 1 1 calc R . . C29 C 0.0827(5) 0.5912(4) 0.3218(4) 0.0293(12) Uani 1 1 d U . . H29 H 0.1752 0.6062 0.3328 0.035 Uiso 1 1 calc R . . C30 C 0.4023(5) 1.0750(4) 0.2135(4) 0.0229(10) Uani 1 1 d U . . C31 C 0.4234(5) 1.0736(4) 0.1208(4) 0.0331(13) Uani 1 1 d U . . H31 H 0.3739 1.0156 0.0661 0.04 Uiso 1 1 calc R . . C32 C 0.5154(5) 1.1552(5) 0.1066(4) 0.0381(14) Uani 1 1 d U . . H32 H 0.5294 1.1524 0.0425 0.046 Uiso 1 1 calc R . . C33 C 0.5866(5) 1.2401(5) 0.1843(4) 0.0407(15) Uani 1 1 d U . . H33 H 0.6495 1.2963 0.1741 0.049 Uiso 1 1 calc R . . C34 C 0.5668(5) 1.2438(5) 0.2774(5) 0.0442(15) Uani 1 1 d U . . H34 H 0.6144 1.3036 0.3314 0.053 Uiso 1 1 calc R . . C35 C 0.4772(5) 1.1598(5) 0.2922(4) 0.0327(13) Uani 1 1 d U . . H35 H 0.467 1.1606 0.3569 0.039 Uiso 1 1 calc R . . N1 N 0.0921(4) 1.0006(3) 0.3400(3) 0.0230(9) Uani 1 1 d U . . N2 N 0.0582(4) 0.8476(3) 0.0878(3) 0.0222(9) Uani 1 1 d U . . O1 O 0.4184(4) 0.8795(3) 0.4568(3) 0.0387(9) Uani 1 1 d U . . O2 O 0.6211(4) 0.5976(4) 0.0662(3) 0.0589(13) Uani 1 1 d U . . O3 O 0.6606(4) 0.9487(4) 0.1393(3) 0.0467(11) Uani 1 1 d U . . O4 O 0.6787(4) 0.8117(4) 0.3845(3) 0.0524(12) Uani 1 1 d U . . P1 P 0.10358(12) 0.78404(10) 0.25906(9) 0.0188(3) Uani 1 1 d U . . P2 P 0.27738(12) 0.96884(10) 0.23299(9) 0.0199(3) Uani 1 1 d U . . S1 S 0.37188(12) 0.64749(10) 0.24355(9) 0.0242(3) Uani 1 1 d U . . S2 S 0.32720(11) 0.77258(10) 0.09000(9) 0.0211(3) Uani 1 1 d U . . Fe1 Fe 0.30771(6) 0.80764(5) 0.24695(5) 0.01856(18) Uani 1 1 d U . . Fe2 Fe 0.51123(6) 0.76102(6) 0.18804(5) 0.02277(19) Uani 1 1 d U . . C36 C 0.4914(17) 0.564(2) 0.4617(18) 0.135(8) Uiso 0.5 1 d PDU . . H36A H 0.4892 0.5433 0.3905 0.162 Uiso 0.5 1 calc PR . . H36B H 0.483 0.6419 0.4793 0.162 Uiso 0.5 1 calc PR . . Cl1 Cl 0.6324(14) 0.5616(10) 0.5155(11) 0.216(3) Uiso 0.5 1 d PDU . . Cl2 Cl 0.3605(14) 0.4904(11) 0.4777(11) 0.216(3) Uiso 0.5 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.025(3) 0.029(3) 0.008(2) 0.009(2) 0.005(2) C2 0.028(3) 0.043(3) 0.036(3) 0.004(3) 0.010(2) 0.009(3) C3 0.023(3) 0.039(3) 0.029(3) 0.011(3) 0.001(2) 0.004(2) C4 0.021(2) 0.041(3) 0.041(3) 0.014(3) 0.010(2) 0.009(2) C5 0.043(3) 0.018(2) 0.036(3) 0.007(2) 0.017(3) 0.006(2) C6 0.025(3) 0.026(3) 0.039(3) -0.001(3) 0.006(2) 0.000(2) C7 0.030(3) 0.030(3) 0.025(3) 0.000(2) 0.003(2) 0.009(2) C8 0.024(2) 0.016(2) 0.025(3) 0.009(2) 0.011(2) 0.006(2) C9 0.024(2) 0.018(2) 0.023(3) 0.007(2) 0.011(2) 0.004(2) C10 0.026(2) 0.023(2) 0.020(3) 0.010(2) 0.010(2) 0.011(2) C11 0.028(2) 0.020(2) 0.017(2) 0.008(2) 0.006(2) 0.004(2) C12 0.040(3) 0.017(2) 0.024(3) 0.009(2) 0.011(2) 0.010(2) C13 0.044(3) 0.034(3) 0.029(3) 0.011(2) 0.015(3) 0.023(3) C14 0.024(3) 0.037(3) 0.034(3) 0.007(3) 0.005(2) 0.011(2) C15 0.032(3) 0.020(3) 0.030(3) 0.006(2) 0.012(2) 0.005(2) C16 0.021(2) 0.025(3) 0.027(3) 0.013(2) 0.009(2) 0.003(2) C17 0.027(3) 0.023(3) 0.027(3) 0.013(2) 0.007(2) 0.006(2) C18 0.034(3) 0.019(3) 0.022(2) 0.009(2) 0.006(2) 0.010(2) C19 0.036(3) 0.032(3) 0.033(3) 0.019(3) 0.014(2) 0.016(2) C20 0.059(3) 0.033(3) 0.029(3) 0.019(3) 0.019(3) 0.024(3) C21 0.069(4) 0.022(3) 0.025(3) 0.009(2) 0.003(3) 0.020(3) C22 0.045(3) 0.018(3) 0.033(3) 0.007(2) -0.002(2) 0.008(2) C23 0.033(3) 0.021(3) 0.028(3) 0.010(2) 0.007(2) 0.005(2) C24 0.028(2) 0.013(2) 0.017(2) 0.002(2) 0.009(2) -0.0003(19) C25 0.027(3) 0.038(3) 0.041(3) 0.021(3) 0.002(3) 0.000(2) C26 0.034(3) 0.046(4) 0.055(4) 0.024(3) 0.005(3) -0.012(3) C27 0.048(3) 0.025(3) 0.045(4) 0.014(3) 0.014(3) -0.010(3) C28 0.054(3) 0.020(3) 0.038(3) 0.014(3) 0.021(3) 0.010(3) C29 0.032(3) 0.028(3) 0.033(3) 0.009(2) 0.018(2) 0.007(2) C30 0.024(2) 0.016(2) 0.032(3) 0.008(2) 0.010(2) 0.0061(19) C31 0.034(3) 0.030(3) 0.036(3) 0.006(3) 0.016(3) 0.003(2) C32 0.038(3) 0.040(3) 0.039(3) 0.017(3) 0.015(3) 0.001(3) C33 0.028(3) 0.049(4) 0.046(3) 0.028(3) 0.007(3) -0.010(3) C34 0.030(3) 0.047(4) 0.046(3) 0.012(3) 0.001(3) -0.011(3) C35 0.025(3) 0.047(3) 0.026(3) 0.018(3) 0.003(2) -0.001(2) N1 0.020(2) 0.019(2) 0.033(2) 0.0066(19) 0.0114(18) 0.0066(17) N2 0.025(2) 0.025(2) 0.020(2) 0.0120(19) 0.0070(17) 0.0038(18) O1 0.041(2) 0.047(3) 0.024(2) 0.0044(19) 0.0025(18) 0.0097(19) O2 0.049(3) 0.063(3) 0.057(3) -0.011(3) 0.017(2) 0.027(2) O3 0.033(2) 0.051(3) 0.054(3) 0.027(2) 0.004(2) -0.009(2) O4 0.035(2) 0.075(3) 0.041(3) 0.019(2) -0.003(2) 0.004(2) P1 0.0202(6) 0.0173(6) 0.0210(7) 0.0071(5) 0.0071(5) 0.0042(5) P2 0.0207(6) 0.0189(6) 0.0238(7) 0.0090(6) 0.0094(5) 0.0051(5) S1 0.0270(6) 0.0206(6) 0.0290(7) 0.0085(6) 0.0102(6) 0.0093(5) S2 0.0221(6) 0.0224(6) 0.0201(6) 0.0045(5) 0.0075(5) 0.0067(5) Fe1 0.0203(3) 0.0174(4) 0.0204(4) 0.0061(3) 0.0082(3) 0.0056(3) Fe2 0.0205(4) 0.0244(4) 0.0248(4) 0.0059(3) 0.0081(3) 0.0063(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.153(6) . ? C1 Fe1 1.759(5) . ? C2 O2 1.148(6) . ? C2 Fe2 1.782(6) . ? C3 O3 1.149(6) . ? C3 Fe2 1.786(6) . ? C4 O4 1.154(6) . ? C4 Fe2 1.784(6) . ? C5 C6 1.507(7) . ? C5 S1 1.830(5) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.527(7) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 S2 1.834(5) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N1 1.468(6) . ? C8 P1 1.851(5) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 N1 1.461(6) . ? C9 P2 1.853(5) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.397(7) . ? C10 C15 1.406(7) . ? C10 N1 1.418(6) . ? C11 C12 1.381(6) . ? C11 H11 0.95 . ? C12 C13 1.373(7) . ? C12 H12 0.95 . ? C13 C14 1.380(7) . ? C13 H13 0.95 . ? C14 C15 1.366(7) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 N2 1.452(6) . ? C16 P1 1.864(5) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 N2 1.462(6) . ? C17 P2 1.868(5) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C23 1.396(7) . ? C18 C19 1.404(7) . ? C18 N2 1.416(6) . ? C19 C20 1.372(7) . ? C19 H19 0.95 . ? C20 C21 1.385(8) . ? C20 H20 0.95 . ? C21 C22 1.366(8) . ? C21 H21 0.95 . ? C22 C23 1.395(7) . ? C22 H22 0.95 . ? C23 H23 0.95 . ? C24 C29 1.374(7) . ? C24 C25 1.405(7) . ? C24 P1 1.830(5) . ? C25 C26 1.366(7) . ? C25 H25 0.95 . ? C26 C27 1.382(8) . ? C26 H26 0.95 . ? C27 C28 1.379(7) . ? C27 H27 0.95 . ? C28 C29 1.384(7) . ? C28 H28 0.95 . ? C29 H29 0.95 . ? C30 C31 1.381(7) . ? C30 C35 1.387(7) . ? C30 P2 1.836(5) . ? C31 C32 1.381(7) . ? C31 H31 0.95 . ? C32 C33 1.368(8) . ? C32 H32 0.95 . ? C33 C34 1.377(8) . ? C33 H33 0.95 . ? C34 C35 1.389(7) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? P1 Fe1 2.1862(13) . ? P2 Fe1 2.1833(14) . ? S1 Fe1 2.2540(14) . ? S1 Fe2 2.2660(14) . ? S2 Fe1 2.2428(14) . ? S2 Fe2 2.2633(14) . ? Fe1 Fe2 2.5655(9) . ? C36 Cl1 1.578(16) . ? C36 Cl2 1.626(16) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Fe1 177.2(5) . . ? O2 C2 Fe2 178.0(5) . . ? O3 C3 Fe2 176.7(5) . . ? O4 C4 Fe2 178.3(5) . . ? C6 C5 S1 115.7(4) . . ? C6 C5 H5A 108.4 . . ? S1 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? S1 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 115.4(4) . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 S2 113.9(4) . . ? C6 C7 H7A 108.8 . . ? S2 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? S2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 P1 112.6(3) . . ? N1 C8 H8A 109.1 . . ? P1 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? P1 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N1 C9 P2 109.8(3) . . ? N1 C9 H9A 109.7 . . ? P2 C9 H9A 109.7 . . ? N1 C9 H9B 109.7 . . ? P2 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C15 117.9(4) . . ? C11 C10 N1 122.9(4) . . ? C15 C10 N1 119.0(4) . . ? C12 C11 C10 120.3(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 121.1(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 118.9(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 121.3(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 120.4(5) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? N2 C16 P1 111.7(3) . . ? N2 C16 H16A 109.3 . . ? P1 C16 H16A 109.3 . . ? N2 C16 H16B 109.3 . . ? P1 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? N2 C17 P2 114.0(3) . . ? N2 C17 H17A 108.8 . . ? P2 C17 H17A 108.8 . . ? N2 C17 H17B 108.8 . . ? P2 C17 H17B 108.8 . . ? H17A C17 H17B 107.6 . . ? C23 C18 C19 118.3(5) . . ? C23 C18 N2 122.5(4) . . ? C19 C18 N2 119.2(4) . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120 . . ? C21 C20 H20 120 . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.2(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.1(5) . . ? C22 C23 H23 120 . . ? C18 C23 H23 120 . . ? C29 C24 C25 118.3(4) . . ? C29 C24 P1 120.9(4) . . ? C25 C24 P1 120.8(4) . . ? C26 C25 C24 120.1(5) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 121.3(5) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 118.9(5) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C29 120.1(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 121.2(5) . . ? C24 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C35 118.2(5) . . ? C31 C30 P2 121.4(4) . . ? C35 C30 P2 120.4(4) . . ? C32 C31 C30 120.9(5) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 120.5(5) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 119.7(5) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 119.8(6) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C30 C35 C34 120.7(5) . . ? C30 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C10 N1 C9 117.5(4) . . ? C10 N1 C8 117.3(4) . . ? C9 N1 C8 115.0(4) . . ? C18 N2 C16 117.5(4) . . ? C18 N2 C17 117.9(4) . . ? C16 N2 C17 115.1(4) . . ? C24 P1 C8 99.4(2) . . ? C24 P1 C16 103.1(2) . . ? C8 P1 C16 100.1(2) . . ? C24 P1 Fe1 123.07(16) . . ? C8 P1 Fe1 113.12(16) . . ? C16 P1 Fe1 114.78(15) . . ? C30 P2 C9 100.8(2) . . ? C30 P2 C17 101.5(2) . . ? C9 P2 C17 100.5(2) . . ? C30 P2 Fe1 124.07(15) . . ? C9 P2 Fe1 113.70(16) . . ? C17 P2 Fe1 113.07(16) . . ? C5 S1 Fe1 114.19(18) . . ? C5 S1 Fe2 110.65(18) . . ? Fe1 S1 Fe2 69.17(4) . . ? C7 S2 Fe1 115.60(17) . . ? C7 S2 Fe2 110.66(17) . . ? Fe1 S2 Fe2 69.41(4) . . ? C1 Fe1 P2 94.81(17) . . ? C1 Fe1 P1 95.88(16) . . ? P2 Fe1 P1 82.41(5) . . ? C1 Fe1 S2 152.19(16) . . ? P2 Fe1 S2 86.42(5) . . ? P1 Fe1 S2 111.79(5) . . ? C1 Fe1 S1 89.42(17) . . ? P2 Fe1 S1 167.95(5) . . ? P1 Fe1 S1 108.42(5) . . ? S2 Fe1 S1 84.61(5) . . ? C1 Fe1 Fe2 98.92(16) . . ? P2 Fe1 Fe2 112.46(4) . . ? P1 Fe1 Fe2 157.87(5) . . ? S2 Fe1 Fe2 55.67(4) . . ? S1 Fe1 Fe2 55.64(4) . . ? C2 Fe2 C4 104.4(3) . . ? C2 Fe2 C3 95.6(3) . . ? C4 Fe2 C3 92.4(2) . . ? C2 Fe2 S2 104.95(18) . . ? C4 Fe2 S2 150.15(17) . . ? C3 Fe2 S2 90.23(17) . . ? C2 Fe2 S1 99.39(19) . . ? C4 Fe2 S1 85.96(17) . . ? C3 Fe2 S1 164.83(18) . . ? S2 Fe2 S1 83.87(5) . . ? C2 Fe2 Fe1 145.95(18) . . ? C4 Fe2 Fe1 96.58(17) . . ? C3 Fe2 Fe1 110.18(17) . . ? S2 Fe2 Fe1 54.92(4) . . ? S1 Fe2 Fe1 55.20(4) . . ? Cl1 C36 Cl2 122.2(18) . . ? Cl1 C36 H36A 106.8 . . ? Cl2 C36 H36A 106.8 . . ? Cl1 C36 H36B 106.8 . . ? Cl2 C36 H36B 106.8 . . ? H36A C36 H36B 106.6 . . ? #----------------------------------------------------------------------------# # END # #----------------------------------------------------------------------------# #####################END OF 1########################################## #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-05 at 17:14:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : sl95-a0 sl95-a0_ data_sl95-a0 _audit_creation_date 2010-08-05T17:14:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_compound_source ? _chemical_formula_moiety 'C36 H34 Fe2 N2 O5 P2 S3, C H2 Cl2' _chemical_formula_sum 'C37 H36 Cl2 Fe2 N2 O5 P2 S3' _chemical_formula_weight 929.4 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.7119(8) _cell_length_b 12.2358(5) _cell_length_c 19.4661(10) _cell_angle_alpha 90 _cell_angle_beta 94.263(5) _cell_angle_gamma 90 _cell_volume 3969.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 5372 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 22.8 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description ; fragment of planar crystal, main faces {1 0 0} ; _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.02 0 1 1 0.13 1 0 0 0.02 0 0 1 0.13 0 -1 0 0.135 0 1 0 0.155 0 -1 -1 0.16 0 -3 -1 0.14 0 0 -1 0.13 15 0 -22 0.105 16 3 18 0.095 _exptl_crystal_recrystallization_method 'Slow evaporation of dichloromethane solution' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) 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_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.955 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed X-ray tube' _diffrn_ambient_temperature 170(2) _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.3622 _diffrn_orient_matrix_ub_11 0.0424386577 _diffrn_orient_matrix_ub_12 0.0023602207 _diffrn_orient_matrix_ub_13 0.0051478118 _diffrn_orient_matrix_ub_21 -0.0028658433 _diffrn_orient_matrix_ub_22 0.0003490606 _diffrn_orient_matrix_ub_23 0.0361704545 _diffrn_orient_matrix_ub_31 0.001679204 _diffrn_orient_matrix_ub_32 -0.0579113045 _diffrn_orient_matrix_ub_33 0.0004220773 _diffrn_measurement_device 'Kappa-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method ; 4 stepped omega-scans over 115 deg. with kappa -79 deg. (chi -58.3 deg.), phi 0, 90, 180, 270 deg. step 1 deg., exposure time 60 s detector distance 50 mm detector angle 30 deg. ; _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_unetI/netI 0.0943 _diffrn_reflns_number 29973 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 8080 _reflns_number_gt 4527 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1980-2002)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^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_number_reflns 8080 _refine_ls_number_parameters 426 _refine_ls_number_restraints 163 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.668 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' N N 0.0061 0.0033 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2030(2) 0.4552(3) 0.3147(2) 0.0314(10) Uani 1 1 d U . . C2 C 0.1536(2) 0.3708(4) 0.1968(2) 0.0340(10) Uani 1 1 d U . . C3 C -0.0238(3) 0.6929(4) 0.1499(3) 0.0489(13) Uani 1 1 d U . . C4 C 0.0182(3) 0.4918(4) 0.1015(3) 0.0527(13) Uani 1 1 d U . . C5 C 0.1098(3) 0.6562(4) 0.0826(3) 0.0474(12) Uani 1 1 d U . . C6 C 0.0994(3) 0.7434(4) 0.2991(3) 0.0477(12) Uani 1 1 d U . . H6A H 0.1375 0.7928 0.3251 0.057 Uiso 1 1 calc R . . H6B H 0.0534 0.7883 0.2807 0.057 Uiso 1 1 calc R . . C7 C 0.0692(3) 0.6609(4) 0.3485(2) 0.0481(12) Uani 1 1 d U . . H7A H 0.0486 0.7003 0.388 0.058 Uiso 1 1 calc R . . H7B H 0.1148 0.6151 0.3666 0.058 Uiso 1 1 calc R . . C8 C 0.0037(3) 0.5872(4) 0.3171(2) 0.0468(12) Uani 1 1 d U . . H8A H -0.0423 0.6333 0.3002 0.056 Uiso 1 1 calc R . . H8B H -0.0147 0.5394 0.3538 0.056 Uiso 1 1 calc R . . C10 C 0.29312(15) 0.5356(2) 0.09993(12) 0.0261(9) Uani 1 1 d GDU . . C11 C 0.24705(16) 0.4640(2) 0.05881(14) 0.0341(10) Uani 1 1 d GDU . . H11 H 0.2118 0.4145 0.079 0.041 Uiso 1 1 calc R . . C12 C 0.25228(17) 0.4642(2) -0.01173(14) 0.0421(12) Uani 1 1 d GU . . H12 H 0.2206 0.415 -0.04 0.051 Uiso 1 1 calc R . . C13 C 0.30358(17) 0.5362(2) -0.04115(13) 0.0406(11) Uani 1 1 d GU . . H13 H 0.3072 0.5364 -0.0896 0.049 Uiso 1 1 calc R . . C14 C 0.34966(16) 0.6078(2) -0.00002(14) 0.0367(11) Uani 1 1 d GU . . H14 H 0.3849 0.6573 -0.0202 0.044 Uiso 1 1 calc R . . C15 C 0.34443(15) 0.6076(2) 0.07051(13) 0.0294(10) Uani 1 1 d GU . . H15 H 0.3761 0.6568 0.0988 0.035 Uiso 1 1 calc R . . C20A C 0.63249(17) 0.5100(3) 0.25652(19) 0.020(3) Uiso 0.5 1 d PGDU A 1 C21A C 0.6946(2) 0.4516(3) 0.2884(2) 0.032(3) Uiso 0.5 1 d PGDU A 1 H21A H 0.6838 0.3931 0.3184 0.038 Uiso 0.5 1 calc PR A 1 C22A C 0.77217(19) 0.4776(3) 0.2769(2) 0.040(3) Uiso 0.5 1 d PGU A 1 H22A H 0.8152 0.4371 0.299 0.049 Uiso 0.5 1 calc PR A 1 C23A C 0.78768(16) 0.5619(3) 0.2336(2) 0.037(3) Uiso 0.5 1 d PGU A 1 H23A H 0.8415 0.5799 0.2256 0.044 Uiso 0.5 1 calc PR A 1 C24A C 0.72559(17) 0.6202(3) 0.20170(18) 0.033(3) Uiso 0.5 1 d PGU A 1 H24A H 0.7363 0.6787 0.1716 0.04 Uiso 0.5 1 calc PR A 1 C25A C 0.64800(17) 0.5943(3) 0.21318(17) 0.037(3) Uiso 0.5 1 d PGU A 1 H25A H 0.6049 0.6348 0.1911 0.044 Uiso 0.5 1 calc PR A 1 C20B C 0.62990(16) 0.5225(3) 0.24610(18) 0.024(3) Uiso 0.5 1 d PGDU A 2 C21B C 0.69561(17) 0.4622(2) 0.27332(19) 0.029(3) Uiso 0.5 1 d PGDU A 2 H21B H 0.6876 0.4009 0.302 0.035 Uiso 0.5 1 calc PR A 2 C22B C 0.77303(17) 0.4918(3) 0.2584(2) 0.031(2) Uiso 0.5 1 d PGU A 2 H22B H 0.8178 0.4507 0.277 0.037 Uiso 0.5 1 calc PR A 2 C23B C 0.78475(17) 0.5818(3) 0.2163(2) 0.036(3) Uiso 0.5 1 d PGU A 2 H23B H 0.8375 0.6019 0.2062 0.043 Uiso 0.5 1 calc PR A 2 C24B C 0.7190(2) 0.6421(3) 0.18910(19) 0.025(2) Uiso 0.5 1 d PGU A 2 H24B H 0.727 0.7033 0.1604 0.03 Uiso 0.5 1 calc PR A 2 C25B C 0.64162(19) 0.6125(3) 0.20399(18) 0.021(3) Uiso 0.5 1 d PGU A 2 H25B H 0.5969 0.6536 0.1854 0.025 Uiso 0.5 1 calc PR A 2 C31 C 0.3503(2) 0.6338(3) 0.23405(19) 0.0274(9) Uani 1 1 d U A . H31A H 0.3868 0.6597 0.1997 0.033 Uiso 1 1 calc R . . H31B H 0.3147 0.6955 0.2442 0.033 Uiso 1 1 calc R . . C32 C 0.4840(2) 0.6063(3) 0.2918(2) 0.0257(9) Uani 1 1 d U A . H32A H 0.5099 0.6293 0.3368 0.031 Uiso 1 1 calc R . . H32B H 0.4968 0.6622 0.2575 0.031 Uiso 1 1 calc R . . C33 C 0.36785(16) 0.61719(19) 0.36411(13) 0.0270(9) Uani 1 1 d GU A . C34 C 0.41229(17) 0.5776(2) 0.42088(14) 0.0404(12) Uani 1 1 d GU . . H34 H 0.4628 0.544 0.4157 0.049 Uiso 1 1 calc R . . C35 C 0.38388(19) 0.5865(2) 0.48520(14) 0.0485(13) Uani 1 1 d GU . . H35 H 0.4147 0.559 0.5244 0.058 Uiso 1 1 calc R . . C36 C 0.31103(19) 0.6349(2) 0.49275(14) 0.0494(13) Uani 1 1 d GU . . H36 H 0.2914 0.6411 0.5371 0.059 Uiso 1 1 calc R . . C37 C 0.26660(17) 0.6745(3) 0.43598(16) 0.0537(14) Uani 1 1 d GU . . H37 H 0.2161 0.7081 0.4411 0.064 Uiso 1 1 calc R . . C38 C 0.29501(16) 0.6656(2) 0.37165(14) 0.0412(11) Uani 1 1 d GU . . H38 H 0.2642 0.6931 0.3325 0.049 Uiso 1 1 calc R . . C41 C 0.3508(2) 0.3979(3) 0.2148(2) 0.0257(9) Uani 1 1 d U A . H41A H 0.3731 0.4051 0.2632 0.031 Uiso 1 1 calc R . . H41B H 0.315 0.3333 0.2128 0.031 Uiso 1 1 calc R . . C42 C 0.4874(2) 0.4436(3) 0.17983(19) 0.0262(9) Uani 1 1 d U A . H42A H 0.4739 0.5133 0.156 0.031 Uiso 1 1 calc R . . H42B H 0.5301 0.4081 0.1551 0.031 Uiso 1 1 calc R . . C43 C 0.40266(16) 0.3173(2) 0.10875(13) 0.0275(9) Uani 1 1 d GU A . C44 C 0.34920(16) 0.2305(2) 0.10438(15) 0.0374(11) Uani 1 1 d GU . . H44 H 0.3208 0.2114 0.1431 0.045 Uiso 1 1 calc R . . C45 C 0.33713(18) 0.1716(2) 0.04356(16) 0.0478(13) Uani 1 1 d GU . . H45 H 0.3005 0.1122 0.0407 0.057 Uiso 1 1 calc R . . C46 C 0.37852(19) 0.1995(2) -0.01288(15) 0.0531(14) Uani 1 1 d GU . . H46 H 0.3703 0.1593 -0.0545 0.064 Uiso 1 1 calc R . . C47 C 0.43200(18) 0.2863(3) -0.00851(14) 0.0447(12) Uani 1 1 d GU . . H47 H 0.4604 0.3055 -0.0472 0.054 Uiso 1 1 calc R . . C48 C 0.44406(16) 0.3452(2) 0.05231(14) 0.0336(10) Uani 1 1 d GU . . H48 H 0.4807 0.4047 0.0552 0.04 Uiso 1 1 calc R . . O1 O 0.22655(19) 0.4149(2) 0.36619(16) 0.0477(9) Uani 1 1 d U . . O2 O 0.14578(19) 0.2840(3) 0.17499(17) 0.0509(9) Uani 1 1 d U . . O3 O -0.0765(2) 0.7516(3) 0.1494(2) 0.0797(13) Uani 1 1 d U . . O4 O -0.0066(3) 0.4212(3) 0.0679(2) 0.0878(14) Uani 1 1 d U . . O5 O 0.1398(2) 0.6947(3) 0.0382(2) 0.0717(12) Uani 1 1 d U . . P1 P 0.28700(6) 0.52051(8) 0.19445(5) 0.0243(3) Uani 1 1 d DU . . P2 P 0.52918(6) 0.47578(8) 0.26749(5) 0.0257(3) Uani 1 1 d DU . . S1 S 0.14929(6) 0.68601(9) 0.22610(6) 0.0355(3) Uani 1 1 d U . . S2 S 0.03166(6) 0.50078(9) 0.24611(6) 0.0350(3) Uani 1 1 d U . . S3 S 0.52219(7) 0.35645(9) 0.33343(5) 0.0324(3) Uani 1 1 d U A . Fe1 Fe 0.16471(3) 0.50253(5) 0.23293(3) 0.02771(16) Uani 1 1 d U . . Fe2 Fe 0.05883(4) 0.60044(5) 0.15314(3) 0.03504(18) Uani 1 1 d U . . N1 N 0.39816(18) 0.6056(2) 0.29671(16) 0.0244(7) Uani 1 1 d U . . N2 N 0.41700(18) 0.3741(2) 0.17314(16) 0.0258(8) Uani 1 1 d U . . C50A C 0.8938(15) 0.5633(10) 0.5055(10) 0.149(5) Uiso 0.5 1 d PDU B 1 H50A H 0.9378 0.558 0.5422 0.178 Uiso 0.5 1 calc PR B 1 H50B H 0.843 0.5597 0.5286 0.178 Uiso 0.5 1 calc PR B 1 Cl1A Cl 0.8987(3) 0.6886(4) 0.4721(3) 0.126(2) Uani 0.5 1 d PDU B 1 Cl2A Cl 0.8978(4) 0.4519(6) 0.4588(4) 0.125(2) Uani 0.5 1 d PDU B 1 C50B C 0.8742(13) 0.5932(17) 0.5001(11) 0.149(5) Uiso 0.5 1 d PDU C 2 H50C H 0.8263 0.6408 0.5002 0.178 Uiso 0.5 1 calc PR C 2 H50D H 0.8789 0.5545 0.5448 0.178 Uiso 0.5 1 calc PR C 2 Cl1B Cl 0.9505(9) 0.6709(14) 0.4978(5) 0.465(12) Uani 0.5 1 d PDU C 2 Cl2B Cl 0.8559(5) 0.5009(10) 0.4397(6) 0.253(6) Uani 0.5 1 d PDU C 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 C1 0.024(2) 0.026(2) 0.045(3) -0.001(2) 0.0093(19) -0.0026(19) C2 0.028(2) 0.032(2) 0.042(3) 0.005(2) 0.002(2) -0.002(2) C3 0.032(3) 0.055(3) 0.058(3) 0.016(3) -0.003(2) 0.003(2) C4 0.068(4) 0.048(3) 0.040(3) 0.010(2) -0.010(2) -0.006(3) C5 0.036(3) 0.051(3) 0.053(3) 0.017(3) -0.004(2) 0.006(2) C6 0.038(3) 0.038(3) 0.067(3) -0.010(2) 0.005(2) 0.018(2) C7 0.033(3) 0.058(3) 0.054(3) -0.015(3) 0.007(2) 0.011(2) C8 0.038(3) 0.057(3) 0.047(3) 0.000(3) 0.013(2) 0.009(2) C10 0.022(2) 0.027(2) 0.029(2) -0.0016(18) -0.0014(17) 0.0053(18) C11 0.033(3) 0.036(3) 0.033(2) 0.001(2) -0.0013(19) 0.001(2) C12 0.050(3) 0.044(3) 0.031(3) -0.011(2) -0.004(2) -0.001(2) C13 0.053(3) 0.043(3) 0.025(2) -0.005(2) 0.003(2) 0.011(2) C14 0.039(3) 0.036(3) 0.036(3) 0.004(2) 0.009(2) 0.006(2) C15 0.024(2) 0.033(2) 0.031(2) -0.005(2) 0.0002(18) 0.0029(19) C31 0.023(2) 0.028(2) 0.031(2) 0.0008(19) 0.0014(17) -0.0006(18) C32 0.024(2) 0.023(2) 0.029(2) -0.0052(18) -0.0026(17) 0.0003(18) C33 0.032(2) 0.021(2) 0.028(2) -0.0072(18) 0.0030(18) -0.0005(18) C34 0.053(3) 0.036(3) 0.032(3) -0.003(2) 0.003(2) 0.015(2) C35 0.084(4) 0.030(3) 0.030(3) -0.004(2) -0.003(2) 0.004(3) C36 0.068(4) 0.046(3) 0.036(3) -0.016(2) 0.017(2) -0.019(3) C37 0.035(3) 0.078(4) 0.049(3) -0.035(3) 0.008(2) -0.005(3) C38 0.030(3) 0.053(3) 0.040(3) -0.014(2) 0.000(2) -0.001(2) C41 0.019(2) 0.025(2) 0.033(2) -0.0032(19) -0.0013(17) -0.0024(18) C42 0.022(2) 0.029(2) 0.027(2) -0.0001(18) 0.0013(17) 0.0014(18) C43 0.025(2) 0.024(2) 0.033(2) -0.0067(19) -0.0049(18) 0.0060(18) C44 0.037(3) 0.030(2) 0.044(3) -0.008(2) -0.006(2) 0.000(2) C45 0.042(3) 0.037(3) 0.062(3) -0.020(2) -0.013(2) 0.000(2) C46 0.060(4) 0.048(3) 0.048(3) -0.027(3) -0.017(3) 0.011(3) C47 0.045(3) 0.054(3) 0.035(3) -0.011(2) 0.002(2) 0.009(2) C48 0.034(3) 0.036(3) 0.031(2) -0.010(2) -0.0035(19) 0.003(2) O1 0.054(2) 0.046(2) 0.042(2) 0.0144(17) -0.0058(16) -0.0004(17) O2 0.055(2) 0.0334(18) 0.065(2) -0.0065(17) 0.0087(17) -0.0097(17) O3 0.052(3) 0.084(3) 0.103(3) 0.019(2) 0.005(2) 0.034(2) O4 0.132(4) 0.072(3) 0.055(3) 0.000(2) -0.022(2) -0.033(3) O5 0.053(2) 0.089(3) 0.075(3) 0.042(2) 0.017(2) 0.006(2) P1 0.0208(6) 0.0229(6) 0.0290(6) -0.0011(5) 0.0012(4) -0.0001(5) P2 0.0224(6) 0.0261(6) 0.0279(6) -0.0028(5) -0.0019(4) 0.0011(5) S1 0.0273(6) 0.0265(6) 0.0524(8) 0.0008(5) 0.0018(5) 0.0029(5) S2 0.0240(6) 0.0370(6) 0.0444(7) 0.0058(6) 0.0048(5) -0.0013(5) S3 0.0365(7) 0.0285(6) 0.0319(6) 0.0018(5) -0.0006(5) 0.0038(5) Fe1 0.0222(3) 0.0257(3) 0.0352(4) 0.0012(3) 0.0020(3) -0.0003(3) Fe2 0.0268(4) 0.0350(4) 0.0430(4) 0.0079(3) -0.0001(3) 0.0006(3) N1 0.0233(18) 0.0235(18) 0.0264(18) -0.0033(15) 0.0015(14) -0.0003(15) N2 0.0204(18) 0.0249(19) 0.0322(19) -0.0030(15) 0.0024(14) -0.0005(14) Cl1A 0.131(4) 0.160(4) 0.094(4) 0.070(3) 0.059(3) 0.087(4) Cl2A 0.098(5) 0.151(4) 0.130(4) 0.035(4) 0.030(4) -0.047(4) Cl1B 0.50(2) 0.73(3) 0.189(10) -0.228(13) 0.190(11) -0.441(19) Cl2B 0.169(9) 0.338(14) 0.269(13) -0.089(10) 0.135(8) -0.118(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.158(5) . ? C1 Fe1 1.770(5) . ? C2 O2 1.148(5) . ? C2 Fe1 1.763(5) . ? C3 O3 1.135(5) . ? C3 Fe2 1.783(5) . ? C4 O4 1.144(5) . ? C4 Fe2 1.771(6) . ? C5 O5 1.133(5) . ? C5 Fe2 1.803(5) . ? C6 C7 1.506(6) . ? C6 S1 1.841(5) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.512(6) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 S2 1.828(4) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C10 C11 1.3823 . ? C10 C15 1.3824 . ? C10 P1 1.860(3) . ? C11 C12 1.3823 . ? C11 H11 0.95 . ? C12 C13 1.3823 . ? C12 H12 0.95 . ? C13 C14 1.3824 . ? C13 H13 0.95 . ? C14 C15 1.3823 . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C20A C21A 1.369 . ? C20A C25A 1.369 . ? C20A P2 1.805(3) . ? C21A C22A 1.369 . ? C21A H21A 0.95 . ? C22A C23A 1.369 . ? C22A H22A 0.95 . ? C23A C24A 1.369 . ? C23A H23A 0.95 . ? C24A C25A 1.369 . ? C24A H24A 0.95 . ? C25A H25A 0.95 . ? C20B C21B 1.395 . ? C20B C25B 1.395 . ? C20B P2 1.854(3) . ? C21B C22B 1.395 . ? C21B H21B 0.95 . ? C22B C23B 1.395 . ? C22B H22B 0.95 . ? C23B C24B 1.395 . ? C23B H23B 0.95 . ? C24B C25B 1.395 . ? C24B H24B 0.95 . ? C25B H25B 0.95 . ? C31 N1 1.449(5) . ? C31 P1 1.875(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 N1 1.445(5) . ? C32 P2 1.843(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C38 1.3716 . ? C33 C34 1.3732 . ? C33 N1 1.448(4) . ? C34 C35 1.3759 . ? C34 H34 0.95 . ? C35 C36 1.3718 . ? C35 H35 0.95 . ? C36 C37 1.3730 . ? C36 H36 0.95 . ? C37 C38 1.3760 . ? C37 H37 0.95 . ? C38 H38 0.95 . ? C41 N2 1.450(5) . ? C41 P1 1.865(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 N2 1.449(5) . ? C42 P2 1.838(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C48 1.3840 . ? C43 C44 1.3863 . ? C43 N2 1.437(4) . ? C44 C45 1.3879 . ? C44 H44 0.95 . ? C45 C46 1.3837 . ? C45 H45 0.95 . ? C46 C47 1.3865 . ? C46 H46 0.95 . ? C47 C48 1.3880 . ? C47 H47 0.95 . ? C48 H48 0.95 . ? P1 Fe1 2.2392(12) . ? P2 S3 1.9533(15) . ? S1 Fe2 2.2537(13) . ? S1 Fe1 2.2625(12) . ? S2 Fe2 2.2562(12) . ? S2 Fe1 2.2571(12) . ? Fe1 Fe2 2.5632(8) . ? C50A Cl2A 1.642(12) . ? C50A Cl1A 1.670(13) . ? C50A H50A 0.99 . ? C50A H50B 0.99 . ? C50B Cl1B 1.593(14) . ? C50B Cl2B 1.643(12) . ? C50B H50C 0.99 . ? C50B H50D 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Fe1 173.9(4) . . ? O2 C2 Fe1 178.0(4) . . ? O3 C3 Fe2 178.4(5) . . ? O4 C4 Fe2 178.7(6) . . ? O5 C5 Fe2 177.3(5) . . ? C7 C6 S1 115.4(3) . . ? C7 C6 H6A 108.4 . . ? S1 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? S1 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 114.1(4) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 S2 115.7(3) . . ? C7 C8 H8A 108.4 . . ? S2 C8 H8A 108.4 . . ? C7 C8 H8B 108.4 . . ? S2 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C11 C10 C15 120 . . ? C11 C10 P1 116.15(15) . . ? C15 C10 P1 123.68(15) . . ? C12 C11 C10 120 . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C11 C12 C13 120 . . ? C11 C12 H12 120 . . ? C13 C12 H12 120 . . ? C12 C13 C14 120 . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C15 C14 C13 120 . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C14 C15 C10 120 . . ? C14 C15 H15 120 . . ? C10 C15 H15 120 . . ? C21A C20A C25A 120 . . ? C21A C20A P2 121.66(19) . . ? C25A C20A P2 118.30(19) . . ? C22A C21A C20A 120 . . ? C22A C21A H21A 120 . . ? C20A C21A H21A 120 . . ? C21A C22A C23A 120 . . ? C21A C22A H22A 120 . . ? C23A C22A H22A 120 . . ? C22A C23A C24A 120 . . ? C22A C23A H23A 120 . . ? C24A C23A H23A 120 . . ? C25A C24A C23A 120 . . ? C25A C24A H24A 120 . . ? C23A C24A H24A 120 . . ? C24A C25A C20A 120 . . ? C24A C25A H25A 120 . . ? C20A C25A H25A 120 . . ? C21B C20B C25B 120 . . ? C21B C20B P2 116.97(18) . . ? C25B C20B P2 123.02(19) . . ? C22B C21B C20B 120 . . ? C22B C21B H21B 120 . . ? C20B C21B H21B 120 . . ? C21B C22B C23B 120 . . ? C21B C22B H22B 120 . . ? C23B C22B H22B 120 . . ? C24B C23B C22B 120 . . ? C24B C23B H23B 120 . . ? C22B C23B H23B 120 . . ? C25B C24B C23B 120 . . ? C25B C24B H24B 120 . . ? C23B C24B H24B 120 . . ? C24B C25B C20B 120 . . ? C24B C25B H25B 120 . . ? C20B C25B H25B 120 . . ? N1 C31 P1 115.4(3) . . ? N1 C31 H31A 108.4 . . ? P1 C31 H31A 108.4 . . ? N1 C31 H31B 108.4 . . ? P1 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? N1 C32 P2 116.1(3) . . ? N1 C32 H32A 108.3 . . ? P2 C32 H32A 108.3 . . ? N1 C32 H32B 108.3 . . ? P2 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C38 C33 C34 119.8 . . ? C38 C33 N1 120.8(2) . . ? C34 C33 N1 119.4(2) . . ? C33 C34 C35 120.1 . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120 . . ? C36 C35 H35 120 . . ? C34 C35 H35 120 . . ? C35 C36 C37 119.8 . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.1 . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C33 C38 C37 120 . . ? C33 C38 H38 120 . . ? C37 C38 H38 120 . . ? N2 C41 P1 119.4(3) . . ? N2 C41 H41A 107.5 . . ? P1 C41 H41A 107.5 . . ? N2 C41 H41B 107.5 . . ? P1 C41 H41B 107.5 . . ? H41A C41 H41B 107 . . ? N2 C42 P2 117.3(3) . . ? N2 C42 H42A 108 . . ? P2 C42 H42A 108 . . ? N2 C42 H42B 108 . . ? P2 C42 H42B 108 . . ? H42A C42 H42B 107.2 . . ? C48 C43 C44 119.9 . . ? C48 C43 N2 120.8(2) . . ? C44 C43 N2 119.2(2) . . ? C43 C44 C45 120.2 . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120 . . ? C46 C45 H45 120 . . ? C44 C45 H45 120 . . ? C45 C46 C47 119.9 . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C48 120.1 . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C43 C48 C47 120 . . ? C43 C48 H48 120 . . ? C47 C48 H48 120 . . ? C10 P1 C41 102.59(15) . . ? C10 P1 C31 105.21(15) . . ? C41 P1 C31 102.17(17) . . ? C10 P1 Fe1 117.36(9) . . ? C41 P1 Fe1 111.78(13) . . ? C31 P1 Fe1 115.88(13) . . ? C20A P2 C42 103.92(17) . . ? C20A P2 C32 104.07(16) . . ? C42 P2 C32 106.81(18) . . ? C20A P2 C20B 7.9 . . ? C42 P2 C20B 98.41(16) . . ? C32 P2 C20B 100.73(16) . . ? C20A P2 S3 110.83(14) . . ? C42 P2 S3 114.37(14) . . ? C32 P2 S3 115.70(14) . . ? C20B P2 S3 118.54(13) . . ? C6 S1 Fe2 110.05(16) . . ? C6 S1 Fe1 112.93(16) . . ? Fe2 S1 Fe1 69.16(4) . . ? C8 S2 Fe2 111.81(16) . . ? C8 S2 Fe1 112.91(15) . . ? Fe2 S2 Fe1 69.21(4) . . ? C2 Fe1 C1 94.60(19) . . ? C2 Fe1 P1 91.58(14) . . ? C1 Fe1 P1 93.15(13) . . ? C2 Fe1 S2 87.80(14) . . ? C1 Fe1 S2 100.86(13) . . ? P1 Fe1 S2 165.98(5) . . ? C2 Fe1 S1 151.10(14) . . ? C1 Fe1 S1 114.21(13) . . ? P1 Fe1 S1 89.18(4) . . ? S2 Fe1 S1 84.68(4) . . ? C2 Fe1 Fe2 97.93(14) . . ? C1 Fe1 Fe2 152.37(13) . . ? P1 Fe1 Fe2 110.94(4) . . ? S2 Fe1 Fe2 55.38(3) . . ? S1 Fe1 Fe2 55.26(3) . . ? C4 Fe2 C3 101.1(2) . . ? C4 Fe2 C5 91.9(2) . . ? C3 Fe2 C5 98.1(2) . . ? C4 Fe2 S1 156.51(17) . . ? C3 Fe2 S1 102.08(17) . . ? C5 Fe2 S1 88.38(16) . . ? C4 Fe2 S2 87.62(16) . . ? C3 Fe2 S2 99.79(16) . . ? C5 Fe2 S2 161.84(15) . . ? S1 Fe2 S2 84.90(5) . . ? C4 Fe2 Fe1 102.21(16) . . ? C3 Fe2 Fe1 144.72(16) . . ? C5 Fe2 Fe1 107.14(15) . . ? S1 Fe2 Fe1 55.58(3) . . ? S2 Fe2 Fe1 55.41(3) . . ? C32 N1 C33 118.4(3) . . ? C32 N1 C31 115.5(3) . . ? C33 N1 C31 122.1(3) . . ? C43 N2 C42 116.3(3) . . ? C43 N2 C41 120.0(3) . . ? C42 N2 C41 118.7(3) . . ? Cl2A C50A Cl1A 122.7(11) . . ? Cl2A C50A H50A 106.6 . . ? Cl1A C50A H50A 106.6 . . ? Cl2A C50A H50B 106.6 . . ? Cl1A C50A H50B 106.6 . . ? H50A C50A H50B 106.6 . . ? Cl1B C50B Cl2B 119.8(13) . . ? Cl1B C50B H50C 107.4 . . ? Cl2B C50B H50C 107.4 . . ? Cl1B C50B H50D 107.4 . . ? Cl2B C50B H50D 107.4 . . ? H50C C50B H50D 106.9 . . ? #----------------------------------------------------------------------------# # END # #----------------------------------------------------------------------------#