# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jt298 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N O P S' _chemical_formula_sum 'C26 H26 Fe N O P S' _chemical_formula_weight 487.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.3665(2) _cell_length_b 24.8131(6) _cell_length_c 11.1353(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.1350(10) _cell_angle_gamma 90.00 _cell_volume 2282.36(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.7080 _exptl_absorpt_correction_T_max 0.8772 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39428 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5253 _reflns_number_gt 4635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0404P)^2^+1.8600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5253 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Fe Fe 0.48126(3) 0.381028(10) 0.78445(2) 0.01913(8) Uani 1 1 d . . . S S -0.00712(7) 0.24358(2) 0.69914(8) 0.0540(2) Uani 1 1 d . . . P P 0.40516(5) 0.518903(18) 0.78995(4) 0.01754(10) Uani 1 1 d . . . O O 0.3914(2) 0.25008(6) 0.98775(14) 0.0382(4) Uani 1 1 d . . . N N 0.3846(2) 0.23766(6) 0.78554(16) 0.0274(3) Uani 1 1 d . . . H1N H 0.4023 0.2512 0.7180 0.033 Uiso 1 1 d R . . C1 C 0.5347(2) 0.31263(7) 0.88500(17) 0.0245(4) Uani 1 1 d . . . C2 C 0.5391(2) 0.35810(8) 0.96376(17) 0.0260(4) Uani 1 1 d . . . H2 H 0.4747 0.3629 1.0260 0.031 Uiso 1 1 calc R . . C3 C 0.6559(2) 0.39497(8) 0.93336(18) 0.0286(4) Uani 1 1 d . . . H3 H 0.6831 0.4287 0.9714 0.034 Uiso 1 1 calc R . . C4 C 0.7250(2) 0.37258(8) 0.8363(2) 0.0311(4) Uani 1 1 d . . . H4 H 0.8069 0.3888 0.7984 0.037 Uiso 1 1 calc R . . C5 C 0.6510(2) 0.32188(8) 0.80538(19) 0.0289(4) Uani 1 1 d . . . H5 H 0.6743 0.2983 0.7432 0.035 Uiso 1 1 calc R . . C6 C 0.3780(2) 0.45259(7) 0.72252(15) 0.0190(3) Uani 1 1 d . . . C7 C 0.4545(2) 0.42687(7) 0.63132(16) 0.0249(4) Uani 1 1 d . . . H7 H 0.5397 0.4415 0.5944 0.030 Uiso 1 1 calc R . . C8 C 0.3810(3) 0.37565(8) 0.60573(18) 0.0324(5) Uani 1 1 d . . . H8 H 0.4087 0.3503 0.5485 0.039 Uiso 1 1 calc R . . C9 C 0.2600(3) 0.36882(8) 0.67959(19) 0.0316(5) Uani 1 1 d . . . H9 H 0.1924 0.3381 0.6806 0.038 Uiso 1 1 calc R . . C10 C 0.2570(2) 0.41585(7) 0.75226(17) 0.0243(4) Uani 1 1 d . . . H10 H 0.1872 0.4219 0.8104 0.029 Uiso 1 1 calc R . . C11 C 0.4298(2) 0.26451(7) 0.89073(18) 0.0272(4) Uani 1 1 d . . . C12 C 0.31265(19) 0.56175(7) 0.66323(15) 0.0181(3) Uani 1 1 d . . . C13 C 0.3308(2) 0.61758(7) 0.67576(19) 0.0273(4) Uani 1 1 d . . . H13 H 0.3948 0.6320 0.7465 0.033 Uiso 1 1 calc R . . C14 C 0.2563(2) 0.65208(8) 0.5859(2) 0.0326(5) Uani 1 1 d . . . H14 H 0.2717 0.6899 0.5946 0.039 Uiso 1 1 calc R . . C15 C 0.1596(2) 0.63158(8) 0.48351(19) 0.0306(4) Uani 1 1 d . . . H15 H 0.1080 0.6553 0.4224 0.037 Uiso 1 1 calc R . . C16 C 0.1386(2) 0.57639(8) 0.47077(17) 0.0263(4) Uani 1 1 d . . . H16 H 0.0721 0.5622 0.4008 0.032 Uiso 1 1 calc R . . C17 C 0.2147(2) 0.54166(7) 0.56032(16) 0.0214(4) Uani 1 1 d . . . H17 H 0.1995 0.5039 0.5510 0.026 Uiso 1 1 calc R . . C18 C 0.6206(2) 0.53378(6) 0.79366(15) 0.0170(3) Uani 1 1 d . . . C19 C 0.7155(2) 0.53917(7) 0.90741(16) 0.0222(4) Uani 1 1 d . . . H19 H 0.6675 0.5352 0.9787 0.027 Uiso 1 1 calc R . . C20 C 0.8803(2) 0.55041(8) 0.91779(18) 0.0288(4) Uani 1 1 d . . . H20 H 0.9443 0.5540 0.9959 0.035 Uiso 1 1 calc R . . C21 C 0.9503(2) 0.55632(8) 0.8143(2) 0.0296(4) Uani 1 1 d . . . H21 H 1.0630 0.5633 0.8212 0.035 Uiso 1 1 calc R . . C22 C 0.8564(2) 0.55205(8) 0.70059(19) 0.0278(4) Uani 1 1 d . . . H22 H 0.9046 0.5567 0.6296 0.033 Uiso 1 1 calc R . . C23 C 0.6921(2) 0.54101(7) 0.68976(16) 0.0216(4) Uani 1 1 d . . . H23 H 0.6281 0.5384 0.6115 0.026 Uiso 1 1 calc R . . C24 C 0.2843(2) 0.18950(7) 0.7796(2) 0.0297(4) Uani 1 1 d . . . H24A H 0.3374 0.1630 0.8396 0.036 Uiso 1 1 calc R . . H24B H 0.2782 0.1733 0.6978 0.036 Uiso 1 1 calc R . . C26 C -0.0264(4) 0.20427(13) 0.5617(3) 0.0783(11) Uani 1 1 d . . . H26A H 0.0805 0.1995 0.5379 0.118 Uiso 1 1 calc R . . H26B H -0.0978 0.2230 0.4967 0.118 Uiso 1 1 calc R . . H26C H -0.0724 0.1689 0.5758 0.118 Uiso 1 1 calc R . . C25 C 0.1136(3) 0.19941(9) 0.8043(2) 0.0378(5) Uani 1 1 d . . . H25A H 0.1202 0.2147 0.8871 0.045 Uiso 1 1 calc R . . H25B H 0.0574 0.1643 0.8037 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.02035(13) 0.01541(13) 0.02023(14) 0.00190(9) -0.00109(9) -0.00058(9) S 0.0287(3) 0.0260(3) 0.1033(6) 0.0112(3) -0.0016(3) 0.0025(2) P 0.0168(2) 0.0171(2) 0.0189(2) 0.00089(16) 0.00317(16) -0.00056(16) O 0.0522(10) 0.0277(8) 0.0340(8) 0.0069(6) 0.0050(7) -0.0077(7) N 0.0295(8) 0.0189(8) 0.0330(9) 0.0038(6) 0.0021(7) -0.0004(6) C1 0.0246(9) 0.0191(8) 0.0275(9) 0.0056(7) -0.0030(7) 0.0044(7) C2 0.0304(10) 0.0231(9) 0.0218(9) 0.0052(7) -0.0041(7) 0.0015(8) C3 0.0293(10) 0.0241(9) 0.0282(10) 0.0032(7) -0.0087(8) -0.0021(8) C4 0.0197(9) 0.0322(11) 0.0394(11) 0.0058(9) -0.0015(8) -0.0015(8) C5 0.0226(9) 0.0262(10) 0.0371(11) 0.0001(8) 0.0016(8) 0.0055(8) C6 0.0201(8) 0.0172(8) 0.0185(8) 0.0034(6) -0.0005(6) 0.0005(6) C7 0.0344(10) 0.0208(9) 0.0189(8) 0.0016(7) 0.0030(7) 0.0022(8) C8 0.0475(12) 0.0223(9) 0.0230(9) -0.0035(7) -0.0084(8) 0.0035(9) C9 0.0316(10) 0.0196(9) 0.0372(11) 0.0041(8) -0.0145(8) -0.0055(8) C10 0.0195(8) 0.0216(9) 0.0294(9) 0.0072(7) -0.0032(7) -0.0021(7) C11 0.0275(9) 0.0182(9) 0.0341(10) 0.0053(7) -0.0003(8) 0.0047(7) C12 0.0148(7) 0.0188(8) 0.0220(8) 0.0029(6) 0.0072(6) 0.0026(6) C13 0.0258(9) 0.0211(9) 0.0330(10) -0.0002(7) -0.0013(8) 0.0011(7) C14 0.0311(10) 0.0186(9) 0.0466(12) 0.0066(8) 0.0016(9) 0.0029(8) C15 0.0255(9) 0.0306(10) 0.0354(11) 0.0128(8) 0.0037(8) 0.0091(8) C16 0.0218(9) 0.0328(10) 0.0235(9) 0.0039(8) 0.0012(7) 0.0030(8) C17 0.0195(8) 0.0223(9) 0.0228(9) 0.0015(7) 0.0048(7) 0.0015(7) C18 0.0179(8) 0.0130(7) 0.0201(8) 0.0010(6) 0.0035(6) 0.0007(6) C19 0.0232(9) 0.0237(9) 0.0198(8) 0.0030(7) 0.0034(7) -0.0012(7) C20 0.0232(9) 0.0324(10) 0.0279(10) 0.0006(8) -0.0047(7) -0.0002(8) C21 0.0159(8) 0.0294(10) 0.0438(12) -0.0037(9) 0.0060(8) -0.0005(7) C22 0.0272(9) 0.0274(10) 0.0323(10) -0.0027(8) 0.0159(8) -0.0014(8) C23 0.0241(9) 0.0209(8) 0.0204(8) -0.0005(7) 0.0055(7) -0.0024(7) C24 0.0320(10) 0.0167(9) 0.0383(11) 0.0012(8) -0.0008(8) 0.0006(8) C26 0.079(2) 0.0571(18) 0.081(2) 0.0200(17) -0.0424(19) -0.0113(17) C25 0.0353(11) 0.0245(10) 0.0540(14) -0.0002(9) 0.0088(10) -0.0033(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C5 2.0299(19) . ? Fe C7 2.0323(18) . ? Fe C8 2.037(2) . ? Fe C4 2.040(2) . ? Fe C1 2.0432(18) . ? Fe C10 2.0447(18) . ? Fe C6 2.0458(17) . ? Fe C9 2.0481(19) . ? Fe C3 2.0579(19) . ? Fe C2 2.0585(18) . ? S C25 1.793(2) . ? S C26 1.800(4) . ? P C6 1.8080(18) . ? P C18 1.8340(17) . ? P C12 1.8367(17) . ? O C11 1.228(2) . ? N C11 1.348(3) . ? N C24 1.456(2) . ? N H1N 0.8577 . ? C1 C2 1.426(3) . ? C1 C5 1.435(3) . ? C1 C11 1.489(3) . ? C2 C3 1.418(3) . ? C2 H2 0.9500 . ? C3 C4 1.417(3) . ? C3 H3 0.9500 . ? C4 C5 1.420(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.433(3) . ? C6 C10 1.439(2) . ? C7 C8 1.421(3) . ? C7 H7 0.9500 . ? C8 C9 1.412(3) . ? C8 H8 0.9500 . ? C9 C10 1.423(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C17 1.391(2) . ? C12 C13 1.398(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.386(3) . ? C14 H14 0.9500 . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.390(2) . ? C18 C23 1.396(2) . ? C19 C20 1.393(3) . ? C19 H19 0.9500 . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.388(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.517(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe C7 118.87(8) . . ? C5 Fe C8 103.69(8) . . ? C7 Fe C8 40.87(8) . . ? C5 Fe C4 40.84(8) . . ? C7 Fe C4 105.48(8) . . ? C8 Fe C4 120.51(9) . . ? C5 Fe C1 41.26(8) . . ? C7 Fe C1 155.51(8) . . ? C8 Fe C1 120.08(8) . . ? C4 Fe C1 68.74(8) . . ? C5 Fe C10 158.65(8) . . ? C7 Fe C10 68.95(8) . . ? C8 Fe C10 68.45(9) . . ? C4 Fe C10 160.24(8) . . ? C1 Fe C10 124.19(8) . . ? C5 Fe C6 156.42(8) . . ? C7 Fe C6 41.16(7) . . ? C8 Fe C6 68.98(7) . . ? C4 Fe C6 122.29(8) . . ? C1 Fe C6 161.73(8) . . ? C10 Fe C6 41.21(7) . . ? C5 Fe C9 120.73(8) . . ? C7 Fe C9 68.62(8) . . ? C8 Fe C9 40.44(9) . . ? C4 Fe C9 156.70(9) . . ? C1 Fe C9 106.79(8) . . ? C10 Fe C9 40.68(8) . . ? C6 Fe C9 68.97(7) . . ? C5 Fe C3 68.57(8) . . ? C7 Fe C3 123.46(8) . . ? C8 Fe C3 158.04(9) . . ? C4 Fe C3 40.46(9) . . ? C1 Fe C3 68.43(8) . . ? C10 Fe C3 125.77(8) . . ? C6 Fe C3 109.48(7) . . ? C9 Fe C3 161.09(9) . . ? C5 Fe C2 68.69(8) . . ? C7 Fe C2 161.10(8) . . ? C8 Fe C2 157.84(8) . . ? C4 Fe C2 68.07(8) . . ? C1 Fe C2 40.68(7) . . ? C10 Fe C2 110.76(8) . . ? C6 Fe C2 126.04(7) . . ? C9 Fe C2 124.33(9) . . ? C3 Fe C2 40.31(8) . . ? C25 S C26 100.90(13) . . ? C6 P C18 104.53(8) . . ? C6 P C12 101.42(8) . . ? C18 P C12 101.16(8) . . ? C11 N C24 121.68(17) . . ? C11 N H1N 120.3 . . ? C24 N H1N 117.4 . . ? C2 C1 C5 107.45(17) . . ? C2 C1 C11 124.45(18) . . ? C5 C1 C11 128.07(18) . . ? C2 C1 Fe 70.24(10) . . ? C5 C1 Fe 68.87(10) . . ? C11 C1 Fe 127.60(13) . . ? C3 C2 C1 108.34(18) . . ? C3 C2 Fe 69.82(11) . . ? C1 C2 Fe 69.08(10) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe C2 H2 126.8 . . ? C4 C3 C2 108.00(18) . . ? C4 C3 Fe 69.09(11) . . ? C2 C3 Fe 69.87(11) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe C3 H3 126.6 . . ? C3 C4 C5 108.52(18) . . ? C3 C4 Fe 70.45(11) . . ? C5 C4 Fe 69.20(11) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Fe C4 H4 126.2 . . ? C4 C5 C1 107.68(18) . . ? C4 C5 Fe 69.96(11) . . ? C1 C5 Fe 69.87(10) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe C5 H5 125.6 . . ? C7 C6 C10 106.90(16) . . ? C7 C6 P 131.18(14) . . ? C10 C6 P 121.83(14) . . ? C7 C6 Fe 68.92(10) . . ? C10 C6 Fe 69.36(10) . . ? P C6 Fe 129.16(9) . . ? C8 C7 C6 108.20(17) . . ? C8 C7 Fe 69.76(11) . . ? C6 C7 Fe 69.93(10) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.0 . . ? C9 C8 C7 108.54(18) . . ? C9 C8 Fe 70.18(11) . . ? C7 C8 Fe 69.37(11) . . ? C9 C8 H8 125.7 . . ? C7 C8 H8 125.7 . . ? Fe C8 H8 126.3 . . ? C8 C9 C10 108.17(17) . . ? C8 C9 Fe 69.37(11) . . ? C10 C9 Fe 69.53(10) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 126.8 . . ? C9 C10 C6 108.18(18) . . ? C9 C10 Fe 69.79(11) . . ? C6 C10 Fe 69.44(10) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe C10 H10 126.4 . . ? O C11 N 122.90(19) . . ? O C11 C1 120.65(19) . . ? N C11 C1 116.43(17) . . ? C17 C12 C13 118.53(16) . . ? C17 C12 P 123.15(13) . . ? C13 C12 P 118.10(14) . . ? C14 C13 C12 120.67(18) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.26(18) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.68(18) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.14(18) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 120.70(17) . . ? C12 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C23 119.03(16) . . ? C19 C18 P 117.18(13) . . ? C23 C18 P 123.78(13) . . ? C18 C19 C20 120.60(17) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 119.83(18) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.04(17) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 120.34(18) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 120.13(17) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? N C24 C25 114.28(16) . . ? N C24 H24A 108.7 . . ? C25 C24 H24A 108.7 . . ? N C24 H24B 108.7 . . ? C25 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? S C26 H26A 109.5 . . ? S C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C25 S 115.45(16) . . ? C24 C25 H25A 108.4 . . ? S C25 H25A 108.4 . . ? C24 C25 H25B 108.4 . . ? S C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.193 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.061 _database_code_depnum_ccdc_archive 'CCDC 962382' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jt290_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Fe N O2 P S' _chemical_formula_sum 'C26 H26 Fe N O2 P S' _chemical_formula_weight 503.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5814(4) _cell_length_b 11.0866(4) _cell_length_c 11.8118(4) _cell_angle_alpha 69.9620(10) _cell_angle_beta 64.8300(10) _cell_angle_gamma 81.9310(10) _cell_volume 1178.16(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7912 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.02 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.873 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16356 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5129 _reflns_number_gt 4407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0731P)^2^+0.5620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5129 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.88460(3) 0.92539(3) 0.36474(3) 0.01613(11) Uani 1 1 d . . . S S 0.43263(6) 0.81124(6) 0.31777(7) 0.03096(16) Uani 1 1 d . . . P P 0.67681(5) 0.72036(5) 0.65204(5) 0.01646(13) Uani 1 1 d . . . O O 0.81042(18) 0.82444(16) 0.09895(15) 0.0278(4) Uani 1 1 d . . . O1P O 0.67127(16) 0.62958(14) 0.58523(15) 0.0220(3) Uani 1 1 d . . . N N 0.73129(18) 0.68307(17) 0.30736(18) 0.0206(4) Uani 1 1 d . . . H1N H 0.7265 0.6717 0.3859 0.025 Uiso 1 1 d R . . C1 C 0.9183(2) 0.8275(2) 0.2369(2) 0.0197(4) Uani 1 1 d . . . C2 C 0.9874(2) 0.9497(2) 0.1674(2) 0.0233(5) Uani 1 1 d . . . H2 H 0.9714 1.0159 0.0986 0.028 Uiso 1 1 calc R . . C3 C 1.0838(2) 0.9538(2) 0.2201(2) 0.0266(5) Uani 1 1 d . . . H3 H 1.1440 1.0239 0.1919 0.032 Uiso 1 1 calc R . . C4 C 1.0762(2) 0.8369(2) 0.3214(2) 0.0257(5) Uani 1 1 d . . . H4 H 1.1298 0.8151 0.3728 0.031 Uiso 1 1 calc R . . C5 C 0.9740(2) 0.7579(2) 0.3325(2) 0.0206(4) Uani 1 1 d . . . H5 H 0.9473 0.6738 0.3926 0.025 Uiso 1 1 calc R . . C6 C 0.7254(2) 0.8810(2) 0.5457(2) 0.0163(4) Uani 1 1 d . . . C7 C 0.6745(2) 0.9506(2) 0.4466(2) 0.0186(4) Uani 1 1 d . . . H7 H 0.6073 0.9204 0.4288 0.022 Uiso 1 1 calc R . . C8 C 0.7420(2) 1.0724(2) 0.3796(2) 0.0214(4) Uani 1 1 d . . . H8 H 0.7276 1.1380 0.3094 0.026 Uiso 1 1 calc R . . C9 C 0.8348(2) 1.0794(2) 0.4358(2) 0.0199(4) Uani 1 1 d . . . H9 H 0.8934 1.1503 0.4090 0.024 Uiso 1 1 calc R . . C10 C 0.8253(2) 0.9624(2) 0.5386(2) 0.0177(4) Uani 1 1 d . . . H10 H 0.8757 0.9417 0.5929 0.021 Uiso 1 1 calc R . . C11 C 0.8135(2) 0.7804(2) 0.2088(2) 0.0196(4) Uani 1 1 d . . . C12 C 0.5116(2) 0.7325(2) 0.7833(2) 0.0189(4) Uani 1 1 d . . . C13 C 0.4620(2) 0.8492(2) 0.8055(2) 0.0227(5) Uani 1 1 d . . . H13 H 0.5161 0.9252 0.7509 0.027 Uiso 1 1 calc R . . C14 C 0.3331(2) 0.8547(2) 0.9078(2) 0.0272(5) Uani 1 1 d . . . H14 H 0.2993 0.9345 0.9223 0.033 Uiso 1 1 calc R . . C15 C 0.2549(3) 0.7444(3) 0.9877(2) 0.0326(6) Uani 1 1 d . . . H15 H 0.1675 0.7482 1.0577 0.039 Uiso 1 1 calc R . . C16 C 0.3034(3) 0.6282(3) 0.9661(3) 0.0362(6) Uani 1 1 d . . . H16 H 0.2488 0.5526 1.0212 0.043 Uiso 1 1 calc R . . C17 C 0.4314(3) 0.6211(2) 0.8646(2) 0.0295(5) Uani 1 1 d . . . H17 H 0.4642 0.5411 0.8505 0.035 Uiso 1 1 calc R . . C18 C 0.8024(2) 0.6723(2) 0.7256(2) 0.0186(4) Uani 1 1 d . . . C19 C 0.9088(2) 0.5881(2) 0.6819(2) 0.0259(5) Uani 1 1 d . . . H19 H 0.9108 0.5530 0.6183 0.031 Uiso 1 1 calc R . . C20 C 1.0113(3) 0.5553(2) 0.7304(3) 0.0311(5) Uani 1 1 d . . . H20 H 1.0837 0.4983 0.6997 0.037 Uiso 1 1 calc R . . C21 C 1.0082(3) 0.6061(2) 0.8246(2) 0.0290(5) Uani 1 1 d . . . H21 H 1.0794 0.5847 0.8570 0.035 Uiso 1 1 calc R . . C22 C 0.9013(3) 0.6877(2) 0.8710(2) 0.0271(5) Uani 1 1 d . . . H22 H 0.8984 0.7213 0.9360 0.033 Uiso 1 1 calc R . . C23 C 0.7988(2) 0.7201(2) 0.8222(2) 0.0221(4) Uani 1 1 d . . . H23 H 0.7252 0.7753 0.8548 0.027 Uiso 1 1 calc R . . C24 C 0.6333(2) 0.6178(2) 0.2917(2) 0.0241(5) Uani 1 1 d . . . H24A H 0.6488 0.5241 0.3211 0.029 Uiso 1 1 calc R . . H24B H 0.6519 0.6442 0.1970 0.029 Uiso 1 1 calc R . . C25 C 0.4819(2) 0.6456(2) 0.3685(2) 0.0271(5) Uani 1 1 d . . . H25A H 0.4639 0.6193 0.4631 0.032 Uiso 1 1 calc R . . H25B H 0.4215 0.5922 0.3593 0.032 Uiso 1 1 calc R . . C26 C 0.4594(4) 0.8319(3) 0.1513(3) 0.0508(8) Uani 1 1 d . . . H26A H 0.5595 0.8285 0.0975 0.076 Uiso 1 1 calc R . . H26B H 0.4223 0.9152 0.1150 0.076 Uiso 1 1 calc R . . H26C H 0.4109 0.7631 0.1508 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.01605(17) 0.01833(17) 0.01475(16) -0.00742(12) -0.00417(12) -0.00333(12) S 0.0263(3) 0.0302(3) 0.0411(4) -0.0159(3) -0.0152(3) 0.0027(2) P 0.0180(3) 0.0162(3) 0.0156(3) -0.0061(2) -0.0053(2) -0.0030(2) O 0.0357(9) 0.0326(9) 0.0184(8) -0.0081(7) -0.0117(7) -0.0072(7) O1P 0.0286(8) 0.0195(7) 0.0197(7) -0.0087(6) -0.0076(6) -0.0055(6) N 0.0218(9) 0.0235(9) 0.0200(9) -0.0092(8) -0.0094(7) -0.0020(7) C1 0.0183(10) 0.0240(11) 0.0166(10) -0.0099(9) -0.0033(8) -0.0024(8) C2 0.0243(11) 0.0262(11) 0.0160(10) -0.0095(9) -0.0009(8) -0.0068(9) C3 0.0186(11) 0.0342(13) 0.0258(12) -0.0176(10) 0.0008(9) -0.0078(9) C4 0.0166(10) 0.0369(13) 0.0310(12) -0.0223(11) -0.0076(9) 0.0009(9) C5 0.0167(10) 0.0248(11) 0.0221(10) -0.0127(9) -0.0057(8) 0.0019(8) C6 0.0151(10) 0.0182(10) 0.0154(9) -0.0077(8) -0.0031(8) -0.0027(8) C7 0.0165(10) 0.0219(10) 0.0180(10) -0.0090(8) -0.0055(8) 0.0004(8) C8 0.0242(11) 0.0197(10) 0.0181(10) -0.0054(8) -0.0070(9) 0.0009(9) C9 0.0243(11) 0.0167(10) 0.0183(10) -0.0084(8) -0.0051(8) -0.0033(8) C10 0.0180(10) 0.0209(10) 0.0164(10) -0.0092(8) -0.0054(8) -0.0027(8) C11 0.0209(10) 0.0207(10) 0.0190(10) -0.0112(9) -0.0060(8) 0.0007(8) C12 0.0181(10) 0.0219(10) 0.0161(10) -0.0052(8) -0.0056(8) -0.0044(8) C13 0.0225(11) 0.0236(11) 0.0216(11) -0.0068(9) -0.0080(9) -0.0022(9) C14 0.0251(12) 0.0341(13) 0.0232(11) -0.0136(10) -0.0084(9) 0.0045(10) C15 0.0224(12) 0.0462(15) 0.0230(12) -0.0123(11) -0.0016(10) -0.0023(11) C16 0.0293(13) 0.0350(14) 0.0300(13) -0.0038(11) 0.0003(11) -0.0137(11) C17 0.0302(13) 0.0220(11) 0.0276(12) -0.0064(10) -0.0029(10) -0.0067(10) C18 0.0215(10) 0.0165(10) 0.0173(10) -0.0036(8) -0.0079(8) -0.0028(8) C19 0.0309(12) 0.0251(11) 0.0250(11) -0.0119(10) -0.0121(10) 0.0033(10) C20 0.0304(13) 0.0299(13) 0.0345(13) -0.0123(11) -0.0153(11) 0.0080(10) C21 0.0284(12) 0.0288(12) 0.0311(13) -0.0035(10) -0.0172(10) -0.0019(10) C22 0.0342(13) 0.0276(12) 0.0230(11) -0.0073(10) -0.0137(10) -0.0048(10) C23 0.0263(11) 0.0191(10) 0.0203(10) -0.0075(9) -0.0075(9) -0.0011(9) C24 0.0283(12) 0.0206(11) 0.0294(12) -0.0100(9) -0.0144(10) -0.0040(9) C25 0.0283(12) 0.0254(11) 0.0290(12) -0.0071(10) -0.0112(10) -0.0094(9) C26 0.0523(19) 0.060(2) 0.0437(17) -0.0083(15) -0.0305(15) 0.0059(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C6 2.025(2) . ? Fe C7 2.034(2) . ? Fe C1 2.035(2) . ? Fe C5 2.043(2) . ? Fe C2 2.045(2) . ? Fe C10 2.047(2) . ? Fe C3 2.053(2) . ? Fe C4 2.058(2) . ? Fe C8 2.061(2) . ? Fe C9 2.061(2) . ? S C26 1.798(3) . ? S C25 1.802(3) . ? P O1P 1.4964(15) . ? P C6 1.786(2) . ? P C12 1.803(2) . ? P C18 1.809(2) . ? O C11 1.233(3) . ? N C11 1.348(3) . ? N C24 1.449(3) . ? N H1N 0.8726 . ? C1 C2 1.431(3) . ? C1 C5 1.435(3) . ? C1 C11 1.486(3) . ? C2 C3 1.414(3) . ? C2 H2 0.9500 . ? C3 C4 1.415(4) . ? C3 H3 0.9500 . ? C4 C5 1.421(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.434(3) . ? C6 C10 1.443(3) . ? C7 C8 1.421(3) . ? C7 H7 0.9500 . ? C8 C9 1.421(3) . ? C8 H8 0.9500 . ? C9 C10 1.421(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C13 1.393(3) . ? C12 C17 1.399(3) . ? C13 C14 1.396(3) . ? C13 H13 0.9500 . ? C14 C15 1.378(4) . ? C14 H14 0.9500 . ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 C17 1.389(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.394(3) . ? C18 C23 1.399(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.397(4) . ? C20 H20 0.9500 . ? C21 C22 1.387(4) . ? C21 H21 0.9500 . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.517(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Fe C7 41.38(8) . . ? C6 Fe C1 122.22(8) . . ? C7 Fe C1 105.87(9) . . ? C6 Fe C5 108.08(9) . . ? C7 Fe C5 123.21(9) . . ? C1 Fe C5 41.21(9) . . ? C6 Fe C2 157.92(9) . . ? C7 Fe C2 120.65(9) . . ? C1 Fe C2 41.07(8) . . ? C5 Fe C2 68.91(9) . . ? C6 Fe C10 41.49(8) . . ? C7 Fe C10 69.26(8) . . ? C1 Fe C10 160.07(9) . . ? C5 Fe C10 124.23(9) . . ? C2 Fe C10 158.15(9) . . ? C6 Fe C3 160.55(10) . . ? C7 Fe C3 156.93(10) . . ? C1 Fe C3 68.30(9) . . ? C5 Fe C3 68.01(9) . . ? C2 Fe C3 40.37(9) . . ? C10 Fe C3 123.69(9) . . ? C6 Fe C4 124.44(9) . . ? C7 Fe C4 160.46(10) . . ? C1 Fe C4 68.71(9) . . ? C5 Fe C4 40.54(9) . . ? C2 Fe C4 68.39(10) . . ? C10 Fe C4 109.08(9) . . ? C3 Fe C4 40.27(10) . . ? C6 Fe C8 68.91(8) . . ? C7 Fe C8 40.61(8) . . ? C1 Fe C8 121.24(9) . . ? C5 Fe C8 158.70(9) . . ? C2 Fe C8 105.55(9) . . ? C10 Fe C8 68.38(9) . . ? C3 Fe C8 121.87(9) . . ? C4 Fe C8 158.33(9) . . ? C6 Fe C9 68.89(8) . . ? C7 Fe C9 68.43(8) . . ? C1 Fe C9 157.36(9) . . ? C5 Fe C9 160.03(9) . . ? C2 Fe C9 121.52(9) . . ? C10 Fe C9 40.48(8) . . ? C3 Fe C9 107.89(9) . . ? C4 Fe C9 123.76(9) . . ? C8 Fe C9 40.34(9) . . ? C26 S C25 100.44(14) . . ? O1P P C6 114.52(9) . . ? O1P P C12 112.55(9) . . ? C6 P C12 105.71(10) . . ? O1P P C18 112.46(10) . . ? C6 P C18 104.76(10) . . ? C12 P C18 106.11(10) . . ? C11 N C24 122.44(18) . . ? C11 N H1N 116.3 . . ? C24 N H1N 120.0 . . ? C2 C1 C5 107.59(19) . . ? C2 C1 C11 125.5(2) . . ? C5 C1 C11 126.87(19) . . ? C2 C1 Fe 69.84(12) . . ? C5 C1 Fe 69.69(12) . . ? C11 C1 Fe 128.22(15) . . ? C3 C2 C1 107.5(2) . . ? C3 C2 Fe 70.11(13) . . ? C1 C2 Fe 69.09(12) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? Fe C2 H2 126.1 . . ? C2 C3 C4 109.2(2) . . ? C2 C3 Fe 69.52(12) . . ? C4 C3 Fe 70.08(13) . . ? C2 C3 H3 125.4 . . ? C4 C3 H3 125.4 . . ? Fe C3 H3 126.6 . . ? C3 C4 C5 107.7(2) . . ? C3 C4 Fe 69.65(13) . . ? C5 C4 Fe 69.14(12) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Fe C4 H4 126.6 . . ? C4 C5 C1 108.0(2) . . ? C4 C5 Fe 70.32(13) . . ? C1 C5 Fe 69.10(12) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 126.1 . . ? C7 C6 C10 107.46(18) . . ? C7 C6 P 125.11(16) . . ? C10 C6 P 127.38(16) . . ? C7 C6 Fe 69.67(12) . . ? C10 C6 Fe 70.08(11) . . ? P C6 Fe 123.58(11) . . ? C8 C7 C6 108.08(19) . . ? C8 C7 Fe 70.68(12) . . ? C6 C7 Fe 68.95(12) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe C7 H7 126.0 . . ? C9 C8 C7 108.24(19) . . ? C9 C8 Fe 69.86(12) . . ? C7 C8 Fe 68.70(12) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Fe C8 H8 127.1 . . ? C8 C9 C10 108.60(18) . . ? C8 C9 Fe 69.81(12) . . ? C10 C9 Fe 69.22(11) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe C9 H9 126.9 . . ? C9 C10 C6 107.62(18) . . ? C9 C10 Fe 70.30(11) . . ? C6 C10 Fe 68.43(11) . . ? C9 C10 H10 126.2 . . ? C6 C10 H10 126.2 . . ? Fe C10 H10 126.6 . . ? O C11 N 123.8(2) . . ? O C11 C1 120.6(2) . . ? N C11 C1 115.48(18) . . ? C13 C12 C17 119.4(2) . . ? C13 C12 P 121.96(16) . . ? C17 C12 P 118.61(17) . . ? C12 C13 C14 120.2(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 120.6(2) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 119.7(2) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? C19 C18 C23 118.8(2) . . ? C19 C18 P 119.11(16) . . ? C23 C18 P 122.02(17) . . ? C20 C19 C18 120.6(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.9(2) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 120.0(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.7(2) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? N C24 C25 113.29(18) . . ? N C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C24 C25 S 114.57(17) . . ? C24 C25 H25A 108.6 . . ? S C25 H25A 108.6 . . ? C24 C25 H25B 108.6 . . ? S C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? S C26 H26A 109.5 . . ? S C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.109 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.092 _database_code_depnum_ccdc_archive 'CCDC 962383' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jt295 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl2 Fe N O P Pd S, 0.5 (H2 O)' _chemical_formula_sum 'C26 H27 Cl2 Fe N O1.50 P Pd S' _chemical_formula_weight 673.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4362(3) _cell_length_b 10.7177(3) _cell_length_c 14.0579(4) _cell_angle_alpha 109.4160(10) _cell_angle_beta 107.2910(10) _cell_angle_gamma 90.3020(10) _cell_volume 1271.70(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 27.60 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 1.656 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4855 _exptl_absorpt_correction_T_max 0.7892 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19504 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5815 _reflns_number_gt 5447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0170P)^2^+0.9858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5815 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0459 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Pd Pd 0.357002(13) 0.227544(11) 0.255984(9) 0.01227(4) Uani 1 1 d . . . Fe Fe -0.07750(2) 0.38110(2) 0.222985(18) 0.01310(5) Uani 1 1 d . . . Cl1 Cl 0.24409(5) 0.01626(4) 0.15105(3) 0.02033(9) Uani 1 1 d . . . Cl2 Cl 0.47341(5) 0.43600(4) 0.36481(3) 0.01827(8) Uani 1 1 d . . . S S 0.48443(5) 0.12130(4) 0.37768(3) 0.01677(8) Uani 1 1 d . . . P P 0.22637(4) 0.30628(4) 0.12905(3) 0.01243(8) Uani 1 1 d . . . O O -0.00081(15) 0.18945(13) 0.41811(11) 0.0273(3) Uani 1 1 d . . . N N 0.22262(16) 0.30443(14) 0.45619(11) 0.0180(3) Uani 1 1 d . . . H1N H 0.2677 0.3740 0.4584 0.022 Uiso 1 1 d R . . C1 C -0.00053(18) 0.38671(16) 0.37660(13) 0.0159(3) Uani 1 1 d . . . C2 C -0.15802(19) 0.39257(18) 0.34485(13) 0.0197(3) Uani 1 1 d . . . H2 H -0.2318 0.3303 0.3430 0.024 Uiso 1 1 calc R . . C3 C -0.1852(2) 0.50747(18) 0.31656(14) 0.0223(4) Uani 1 1 d . . . H3 H -0.2804 0.5357 0.2927 0.027 Uiso 1 1 calc R . . C4 C -0.0458(2) 0.57316(17) 0.32990(14) 0.0214(4) Uani 1 1 d . . . H4 H -0.0316 0.6529 0.3166 0.026 Uiso 1 1 calc R . . C5 C 0.0687(2) 0.49876(16) 0.36666(13) 0.0178(3) Uani 1 1 d . . . H5 H 0.1728 0.5198 0.3819 0.021 Uiso 1 1 calc R . . C6 C 0.03149(18) 0.30191(16) 0.11506(12) 0.0147(3) Uani 1 1 d . . . C7 C -0.05106(18) 0.19808(16) 0.12690(13) 0.0178(3) Uani 1 1 d . . . H7 H -0.0104 0.1281 0.1497 0.021 Uiso 1 1 calc R . . C8 C -0.2035(2) 0.21859(18) 0.09868(14) 0.0227(4) Uani 1 1 d . . . H8 H -0.2830 0.1642 0.0991 0.027 Uiso 1 1 calc R . . C9 C -0.21822(19) 0.33344(19) 0.06976(14) 0.0228(4) Uani 1 1 d . . . H9 H -0.3090 0.3694 0.0478 0.027 Uiso 1 1 calc R . . C10 C -0.07441(19) 0.38576(18) 0.07913(13) 0.0191(3) Uani 1 1 d . . . H10 H -0.0519 0.4625 0.0643 0.023 Uiso 1 1 calc R . . C11 C 0.07239(19) 0.28428(16) 0.41703(13) 0.0173(3) Uani 1 1 d . . . C12 C 0.23491(18) 0.20771(15) -0.00193(13) 0.0156(3) Uani 1 1 d . . . C13 C 0.1135(2) 0.18751(19) -0.09257(14) 0.0247(4) Uani 1 1 d . . . H13 H 0.0241 0.2249 -0.0867 0.030 Uiso 1 1 calc R . . C14 C 0.1230(2) 0.1125(2) -0.19209(16) 0.0338(5) Uani 1 1 d . . . H14 H 0.0397 0.0980 -0.2541 0.041 Uiso 1 1 calc R . . C15 C 0.2537(2) 0.05899(19) -0.20073(16) 0.0314(4) Uani 1 1 d . . . H15 H 0.2599 0.0082 -0.2688 0.038 Uiso 1 1 calc R . . C16 C 0.3752(2) 0.07901(17) -0.11099(16) 0.0255(4) Uani 1 1 d . . . H16 H 0.4651 0.0430 -0.1174 0.031 Uiso 1 1 calc R . . C17 C 0.3654(2) 0.15206(17) -0.01138(15) 0.0203(3) Uani 1 1 d . . . H17 H 0.4480 0.1641 0.0505 0.024 Uiso 1 1 calc R . . C18 C 0.29484(18) 0.47509(16) 0.14877(13) 0.0150(3) Uani 1 1 d . . . C19 C 0.2320(2) 0.58583(16) 0.19810(14) 0.0193(3) Uani 1 1 d . . . H19 H 0.1448 0.5740 0.2161 0.023 Uiso 1 1 calc R . . C20 C 0.2968(2) 0.71336(17) 0.22089(15) 0.0231(4) Uani 1 1 d . . . H20 H 0.2517 0.7883 0.2525 0.028 Uiso 1 1 calc R . . C21 C 0.4264(2) 0.73228(17) 0.19803(14) 0.0230(4) Uani 1 1 d . . . H21 H 0.4716 0.8198 0.2154 0.028 Uiso 1 1 calc R . . C22 C 0.4900(2) 0.62254(18) 0.14959(15) 0.0223(4) Uani 1 1 d . . . H22 H 0.5791 0.6349 0.1338 0.027 Uiso 1 1 calc R . . C23 C 0.42385(19) 0.49493(17) 0.12418(14) 0.0191(3) Uani 1 1 d . . . H23 H 0.4668 0.4203 0.0897 0.023 Uiso 1 1 calc R . . C24 C 0.3077(2) 0.22458(17) 0.51303(14) 0.0203(3) Uani 1 1 d . . . H24A H 0.2487 0.1990 0.5527 0.024 Uiso 1 1 calc R . . H24B H 0.4004 0.2795 0.5657 0.024 Uiso 1 1 calc R . . C25 C 0.34924(19) 0.09889(16) 0.44161(14) 0.0200(3) Uani 1 1 d . . . H25A H 0.2566 0.0488 0.3853 0.024 Uiso 1 1 calc R . . H25B H 0.3893 0.0427 0.4846 0.024 Uiso 1 1 calc R . . C26 C 0.6344(2) 0.22937(17) 0.48828(14) 0.0221(4) Uani 1 1 d . . . H26A H 0.6034 0.3185 0.5129 0.033 Uiso 1 1 calc R . . H26B H 0.7225 0.2347 0.4659 0.033 Uiso 1 1 calc R . . H26C H 0.6589 0.1937 0.5463 0.033 Uiso 1 1 calc R . . O1W O 0.0695(4) 0.9412(3) 0.4546(3) 0.0465(8) Uani 0.50 1 d P . . H1W H 0.0398 1.0227 0.4535 0.071(19) Uiso 0.50 1 d PR . . H2W H 0.0389 0.9143 0.5005 0.059(17) Uiso 0.50 1 d PR . . 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 Pd 0.01265(6) 0.01057(6) 0.01277(6) 0.00369(5) 0.00330(5) 0.00154(4) Fe 0.01230(11) 0.01564(11) 0.01181(11) 0.00436(9) 0.00494(9) 0.00327(8) Cl1 0.0217(2) 0.01214(17) 0.0217(2) 0.00307(15) 0.00232(17) 0.00009(15) Cl2 0.0204(2) 0.01334(17) 0.01679(19) 0.00377(15) 0.00151(16) -0.00102(14) S 0.0179(2) 0.01422(18) 0.0171(2) 0.00591(16) 0.00334(16) 0.00382(15) P 0.01254(19) 0.01259(18) 0.01276(19) 0.00441(15) 0.00487(16) 0.00232(15) O 0.0256(7) 0.0257(7) 0.0313(7) 0.0155(6) 0.0040(6) -0.0028(5) N 0.0188(7) 0.0175(7) 0.0202(7) 0.0090(6) 0.0070(6) 0.0033(5) C1 0.0181(8) 0.0185(8) 0.0106(7) 0.0034(6) 0.0057(6) 0.0028(6) C2 0.0197(9) 0.0262(9) 0.0163(8) 0.0071(7) 0.0105(7) 0.0055(7) C3 0.0239(9) 0.0280(9) 0.0177(8) 0.0072(7) 0.0110(7) 0.0135(7) C4 0.0298(10) 0.0165(8) 0.0184(9) 0.0045(7) 0.0100(8) 0.0076(7) C5 0.0212(9) 0.0159(8) 0.0139(8) 0.0025(6) 0.0051(7) 0.0018(6) C6 0.0132(8) 0.0185(8) 0.0113(7) 0.0030(6) 0.0048(6) 0.0029(6) C7 0.0164(8) 0.0159(8) 0.0179(8) 0.0009(6) 0.0063(7) 0.0003(6) C8 0.0153(8) 0.0249(9) 0.0201(9) -0.0015(7) 0.0049(7) -0.0038(7) C9 0.0141(8) 0.0364(10) 0.0138(8) 0.0050(7) 0.0027(7) 0.0071(7) C10 0.0194(8) 0.0275(9) 0.0136(8) 0.0094(7) 0.0070(7) 0.0075(7) C11 0.0210(8) 0.0187(8) 0.0108(8) 0.0031(6) 0.0054(7) 0.0023(6) C12 0.0184(8) 0.0133(7) 0.0158(8) 0.0037(6) 0.0082(7) 0.0006(6) C13 0.0206(9) 0.0327(10) 0.0189(9) 0.0051(8) 0.0079(7) 0.0027(7) C14 0.0312(11) 0.0451(12) 0.0173(9) 0.0018(9) 0.0069(8) -0.0029(9) C15 0.0443(12) 0.0267(10) 0.0232(10) -0.0007(8) 0.0214(9) -0.0015(9) C16 0.0324(10) 0.0193(8) 0.0347(11) 0.0097(8) 0.0242(9) 0.0070(7) C17 0.0206(9) 0.0192(8) 0.0259(9) 0.0100(7) 0.0118(7) 0.0049(7) C18 0.0170(8) 0.0153(7) 0.0139(8) 0.0075(6) 0.0037(6) 0.0021(6) C19 0.0228(9) 0.0189(8) 0.0197(9) 0.0082(7) 0.0099(7) 0.0041(7) C20 0.0326(10) 0.0163(8) 0.0230(9) 0.0077(7) 0.0115(8) 0.0054(7) C21 0.0282(10) 0.0177(8) 0.0215(9) 0.0090(7) 0.0036(8) -0.0028(7) C22 0.0185(9) 0.0257(9) 0.0253(9) 0.0132(8) 0.0060(7) -0.0010(7) C23 0.0177(8) 0.0197(8) 0.0206(9) 0.0075(7) 0.0067(7) 0.0034(6) C24 0.0207(9) 0.0234(8) 0.0189(8) 0.0105(7) 0.0057(7) 0.0053(7) C25 0.0208(9) 0.0178(8) 0.0250(9) 0.0117(7) 0.0076(7) 0.0035(7) C26 0.0196(9) 0.0226(9) 0.0211(9) 0.0094(7) 0.0004(7) 0.0004(7) O1W 0.061(2) 0.0429(18) 0.060(2) 0.0360(17) 0.0335(19) 0.0156(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd P 2.2628(4) . ? Pd Cl2 2.2894(4) . ? Pd Cl1 2.2932(4) . ? Pd S 2.3991(4) . ? Fe C6 2.0397(15) . ? Fe C2 2.0402(16) . ? Fe C1 2.0434(16) . ? Fe C7 2.0441(16) . ? Fe C10 2.0482(16) . ? Fe C5 2.0505(17) . ? Fe C8 2.0543(17) . ? Fe C3 2.0545(17) . ? Fe C9 2.0555(17) . ? Fe C4 2.0628(17) . ? S C26 1.7997(18) . ? S C25 1.8206(17) . ? P C6 1.7890(16) . ? P C12 1.8190(16) . ? P C18 1.8209(16) . ? O C11 1.233(2) . ? N C11 1.346(2) . ? N C24 1.448(2) . ? N H1N 0.8437 . ? C1 C2 1.427(2) . ? C1 C5 1.430(2) . ? C1 C11 1.481(2) . ? C2 C3 1.417(2) . ? C2 H2 0.9500 . ? C3 C4 1.420(3) . ? C3 H3 0.9500 . ? C4 C5 1.422(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.437(2) . ? C6 C10 1.440(2) . ? C7 C8 1.413(2) . ? C7 H7 0.9500 . ? C8 C9 1.415(3) . ? C8 H8 0.9500 . ? C9 C10 1.418(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C13 1.389(2) . ? C12 C17 1.393(2) . ? C13 C14 1.393(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.382(3) . ? C15 H15 0.9500 . ? C16 C17 1.390(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.394(2) . ? C18 C19 1.395(2) . ? C19 C20 1.389(2) . ? C19 H19 0.9500 . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 C23 1.386(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.522(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O1W H1W 0.9221 . ? O1W H2W 0.9050 . ? 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 P Pd Cl2 91.656(15) . . ? P Pd Cl1 90.113(15) . . ? Cl2 Pd Cl1 178.227(15) . . ? P Pd S 174.033(15) . . ? Cl2 Pd S 94.285(15) . . ? Cl1 Pd S 83.947(15) . . ? C6 Fe C2 156.29(7) . . ? C6 Fe C1 123.01(6) . . ? C2 Fe C1 40.91(7) . . ? C6 Fe C7 41.19(6) . . ? C2 Fe C7 118.85(7) . . ? C1 Fe C7 107.84(7) . . ? C6 Fe C10 41.24(6) . . ? C2 Fe C10 158.87(7) . . ? C1 Fe C10 159.52(7) . . ? C7 Fe C10 68.91(7) . . ? C6 Fe C5 111.11(7) . . ? C2 Fe C5 68.63(7) . . ? C1 Fe C5 40.89(6) . . ? C7 Fe C5 127.61(7) . . ? C10 Fe C5 124.13(7) . . ? C6 Fe C8 68.47(7) . . ? C2 Fe C8 104.32(7) . . ? C1 Fe C8 123.37(7) . . ? C7 Fe C8 40.33(7) . . ? C10 Fe C8 68.07(7) . . ? C5 Fe C8 162.30(7) . . ? C6 Fe C3 163.01(7) . . ? C2 Fe C3 40.50(7) . . ? C1 Fe C3 68.35(7) . . ? C7 Fe C3 152.90(7) . . ? C10 Fe C3 124.04(7) . . ? C5 Fe C3 68.11(7) . . ? C8 Fe C3 117.75(7) . . ? C6 Fe C9 68.64(7) . . ? C2 Fe C9 121.27(7) . . ? C1 Fe C9 158.85(7) . . ? C7 Fe C9 68.21(7) . . ? C10 Fe C9 40.42(7) . . ? C5 Fe C9 157.28(7) . . ? C8 Fe C9 40.27(7) . . ? C3 Fe C9 105.21(7) . . ? C6 Fe C4 128.03(7) . . ? C2 Fe C4 68.21(7) . . ? C1 Fe C4 68.36(7) . . ? C7 Fe C4 165.38(7) . . ? C10 Fe C4 109.39(7) . . ? C5 Fe C4 40.44(7) . . ? C8 Fe C4 153.71(7) . . ? C3 Fe C4 40.34(7) . . ? C9 Fe C4 120.58(7) . . ? C26 S C25 102.10(9) . . ? C26 S Pd 113.16(6) . . ? C25 S Pd 104.25(6) . . ? C6 P C12 105.07(8) . . ? C6 P C18 107.83(7) . . ? C12 P C18 104.24(7) . . ? C6 P Pd 112.76(5) . . ? C12 P Pd 112.06(5) . . ? C18 P Pd 114.13(5) . . ? C11 N C24 121.89(14) . . ? C11 N H1N 119.2 . . ? C24 N H1N 117.9 . . ? C2 C1 C5 107.61(15) . . ? C2 C1 C11 124.16(15) . . ? C5 C1 C11 128.17(15) . . ? C2 C1 Fe 69.42(9) . . ? C5 C1 Fe 69.82(9) . . ? C11 C1 Fe 128.36(11) . . ? C3 C2 C1 108.04(15) . . ? C3 C2 Fe 70.29(9) . . ? C1 C2 Fe 69.66(9) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe C2 H2 125.6 . . ? C2 C3 C4 108.38(15) . . ? C2 C3 Fe 69.21(9) . . ? C4 C3 Fe 70.15(10) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Fe C3 H3 126.4 . . ? C3 C4 C5 108.01(15) . . ? C3 C4 Fe 69.52(10) . . ? C5 C4 Fe 69.31(9) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe C4 H4 126.7 . . ? C4 C5 C1 107.97(15) . . ? C4 C5 Fe 70.25(10) . . ? C1 C5 Fe 69.29(9) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 126.0 . . ? C7 C6 C10 107.21(14) . . ? C7 C6 P 123.43(12) . . ? C10 C6 P 128.97(13) . . ? C7 C6 Fe 69.57(9) . . ? C10 C6 Fe 69.70(9) . . ? P C6 Fe 131.32(9) . . ? C8 C7 C6 107.86(15) . . ? C8 C7 Fe 70.22(10) . . ? C6 C7 Fe 69.24(9) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe C7 H7 126.0 . . ? C7 C8 C9 108.77(15) . . ? C7 C8 Fe 69.45(10) . . ? C9 C8 Fe 69.91(10) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? Fe C8 H8 126.6 . . ? C8 C9 C10 108.33(15) . . ? C8 C9 Fe 69.82(10) . . ? C10 C9 Fe 69.51(10) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Fe C9 H9 126.4 . . ? C9 C10 C6 107.82(15) . . ? C9 C10 Fe 70.07(10) . . ? C6 C10 Fe 69.06(9) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 126.3 . . ? O C11 N 122.45(16) . . ? O C11 C1 121.73(16) . . ? N C11 C1 115.77(14) . . ? C13 C12 C17 119.57(16) . . ? C13 C12 P 120.97(13) . . ? C17 C12 P 119.46(13) . . ? C12 C13 C14 119.97(18) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.01(19) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.41(18) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.74(17) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 120.28(17) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C23 C18 C19 118.93(15) . . ? C23 C18 P 118.67(12) . . ? C19 C18 P 122.04(12) . . ? C20 C19 C18 120.10(16) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.63(16) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.52(16) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.15(16) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.64(16) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? N C24 C25 113.86(14) . . ? N C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? N C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C24 C25 S 116.82(12) . . ? C24 C25 H25A 108.1 . . ? S C25 H25A 108.1 . . ? C24 C25 H25B 108.1 . . ? S C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? S C26 H26A 109.5 . . ? S C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H1W O1W H2W 112.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.354 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 962384' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jt296 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl2 Fe N O P Pt S' _chemical_formula_sum 'C26 H26 Cl2 Fe N O P Pt S' _chemical_formula_weight 753.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7438(2) _cell_length_b 10.5637(2) _cell_length_c 14.1431(3) _cell_angle_alpha 91.9530(10) _cell_angle_beta 90.0810(10) _cell_angle_gamma 99.9570(10) _cell_volume 1285.89(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9983 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.51 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 6.370 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2686 _exptl_absorpt_correction_T_max 0.4289 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21895 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5907 _reflns_number_gt 5621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0114P)^2^+0.9259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5907 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0151 _refine_ls_wR_factor_ref 0.0322 _refine_ls_wR_factor_gt 0.0317 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Pt Pt 0.384693(9) 0.239179(7) 0.389209(5) 0.01514(3) Uani 1 1 d . . . Fe Fe 0.23277(3) 0.44644(3) 0.15021(2) 0.01583(6) Uani 1 1 d . . . Cl1 Cl 0.45585(7) 0.29391(6) 0.54807(4) 0.03038(12) Uani 1 1 d . . . Cl2 Cl 0.14453(6) 0.29301(5) 0.42315(4) 0.02612(11) Uani 1 1 d . . . S S 0.63233(6) 0.21013(5) 0.35784(4) 0.02150(11) Uani 1 1 d . . . P P 0.29634(6) 0.15623(5) 0.24731(3) 0.01435(10) Uani 1 1 d . . . O O 0.67501(19) 0.48953(15) 0.14007(11) 0.0302(4) Uani 1 1 d . . . N N 0.6316(2) 0.49348(17) 0.29836(13) 0.0219(4) Uani 1 1 d . . . H1N H 0.5777 0.5280 0.3457 0.026 Uiso 1 1 d R . . C1 C 0.4416(2) 0.55239(18) 0.19433(15) 0.0190(4) Uani 1 1 d . . . C2 C 0.3234(3) 0.56246(19) 0.26315(16) 0.0219(4) Uani 1 1 d . . . H2 H 0.3248 0.5380 0.3271 0.026 Uiso 1 1 calc R . . C3 C 0.2047(3) 0.6150(2) 0.21920(18) 0.0286(5) Uani 1 1 d . . . H3 H 0.1128 0.6328 0.2486 0.034 Uiso 1 1 calc R . . C4 C 0.2463(3) 0.6368(2) 0.12383(18) 0.0316(6) Uani 1 1 d . . . H4 H 0.1869 0.6718 0.0783 0.038 Uiso 1 1 calc R . . C5 C 0.3906(3) 0.5977(2) 0.10739(16) 0.0273(5) Uani 1 1 d . . . H5 H 0.4444 0.6008 0.0490 0.033 Uiso 1 1 calc R . . C6 C 0.2064(2) 0.25245(18) 0.16773(14) 0.0161(4) Uani 1 1 d . . . C7 C 0.0646(2) 0.29772(19) 0.18867(15) 0.0198(4) Uani 1 1 d . . . H7 H 0.0116 0.2903 0.2474 0.024 Uiso 1 1 calc R . . C8 C 0.0163(3) 0.35545(19) 0.10723(15) 0.0220(4) Uani 1 1 d . . . H8 H -0.0743 0.3932 0.1020 0.026 Uiso 1 1 calc R . . C9 C 0.1266(3) 0.34699(19) 0.03505(15) 0.0218(5) Uani 1 1 d . . . H9 H 0.1232 0.3789 -0.0268 0.026 Uiso 1 1 calc R . . C10 C 0.2430(3) 0.28277(18) 0.07093(14) 0.0192(4) Uani 1 1 d . . . H10 H 0.3301 0.2632 0.0370 0.023 Uiso 1 1 calc R . . C11 C 0.5923(2) 0.50894(18) 0.20777(15) 0.0196(4) Uani 1 1 d . . . C12 C 0.1416(2) 0.01868(18) 0.26103(15) 0.0178(4) Uani 1 1 d . . . C13 C 0.0667(3) -0.0431(2) 0.18085(16) 0.0245(5) Uani 1 1 d . . . H13 H 0.0990 -0.0148 0.1198 0.029 Uiso 1 1 calc R . . C14 C -0.0542(3) -0.1452(2) 0.18943(18) 0.0299(5) Uani 1 1 d . . . H14 H -0.1040 -0.1874 0.1344 0.036 Uiso 1 1 calc R . . C15 C -0.1024(3) -0.1858(2) 0.27809(19) 0.0329(6) Uani 1 1 d . . . H15 H -0.1874 -0.2544 0.2839 0.040 Uiso 1 1 calc R . . C16 C -0.0285(3) -0.1277(2) 0.35752(19) 0.0348(6) Uani 1 1 d . . . H16 H -0.0611 -0.1571 0.4182 0.042 Uiso 1 1 calc R . . C17 C 0.0944(3) -0.0255(2) 0.34970(16) 0.0256(5) Uani 1 1 d . . . H17 H 0.1461 0.0141 0.4050 0.031 Uiso 1 1 calc R . . C18 C 0.4411(2) 0.09273(18) 0.17735(13) 0.0164(4) Uani 1 1 d . . . C19 C 0.5513(2) 0.17529(19) 0.12707(14) 0.0204(4) Uani 1 1 d . . . H19 H 0.5466 0.2644 0.1263 0.024 Uiso 1 1 calc R . . C20 C 0.6677(3) 0.1275(2) 0.07812(15) 0.0235(5) Uani 1 1 d . . . H20 H 0.7409 0.1836 0.0426 0.028 Uiso 1 1 calc R . . C21 C 0.6775(3) -0.0018(2) 0.08090(16) 0.0252(5) Uani 1 1 d . . . H21 H 0.7566 -0.0346 0.0468 0.030 Uiso 1 1 calc R . . C22 C 0.5720(3) -0.0830(2) 0.13339(17) 0.0274(5) Uani 1 1 d . . . H22 H 0.5807 -0.1712 0.1367 0.033 Uiso 1 1 calc R . . C23 C 0.4542(3) -0.03710(19) 0.18110(15) 0.0210(4) Uani 1 1 d . . . H23 H 0.3818 -0.0938 0.2166 0.025 Uiso 1 1 calc R . . C24 C 0.7775(3) 0.4582(2) 0.32532(18) 0.0291(5) Uani 1 1 d . . . H24A H 0.8485 0.5358 0.3497 0.035 Uiso 1 1 calc R . . H24B H 0.8258 0.4243 0.2688 0.035 Uiso 1 1 calc R . . C25 C 0.7574(2) 0.3572(2) 0.40071(16) 0.0248(5) Uani 1 1 d . . . H25A H 0.7114 0.3914 0.4580 0.030 Uiso 1 1 calc R . . H25B H 0.8603 0.3377 0.4183 0.030 Uiso 1 1 calc R . . C26 C 0.6844(3) 0.0993(2) 0.44155(19) 0.0349(6) Uani 1 1 d . . . H26A H 0.7944 0.0933 0.4344 0.052 Uiso 1 1 calc R . . H26B H 0.6209 0.0142 0.4297 0.052 Uiso 1 1 calc R . . H26C H 0.6661 0.1301 0.5060 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01413(4) 0.01782(4) 0.01367(4) -0.00020(3) 0.00045(3) 0.00346(3) Fe 0.01911(15) 0.01322(12) 0.01478(14) 0.00155(10) -0.00225(11) 0.00156(11) Cl1 0.0274(3) 0.0446(3) 0.0183(3) -0.0096(2) -0.0026(2) 0.0057(3) Cl2 0.0203(3) 0.0394(3) 0.0215(3) 0.0043(2) 0.0053(2) 0.0125(2) S 0.0175(3) 0.0269(3) 0.0213(3) -0.0013(2) -0.0010(2) 0.0075(2) P 0.0148(3) 0.0143(2) 0.0136(2) 0.00201(18) 0.00098(19) 0.00146(19) O 0.0267(9) 0.0354(9) 0.0274(9) -0.0016(7) 0.0097(7) 0.0028(7) N 0.0165(9) 0.0259(9) 0.0248(10) 0.0012(7) 0.0029(7) 0.0075(7) C1 0.0215(11) 0.0138(9) 0.0203(10) -0.0001(8) -0.0016(8) -0.0006(8) C2 0.0234(12) 0.0186(10) 0.0233(11) -0.0068(8) -0.0034(9) 0.0042(9) C3 0.0263(13) 0.0176(10) 0.0422(14) -0.0090(9) -0.0066(11) 0.0067(9) C4 0.0359(14) 0.0141(10) 0.0437(15) 0.0073(9) -0.0153(11) 0.0006(9) C5 0.0342(13) 0.0193(10) 0.0246(12) 0.0071(9) -0.0036(10) -0.0070(9) C6 0.0187(10) 0.0132(8) 0.0157(10) 0.0016(7) -0.0015(8) 0.0006(8) C7 0.0187(11) 0.0194(9) 0.0208(10) 0.0031(8) -0.0002(8) 0.0016(8) C8 0.0195(11) 0.0203(10) 0.0255(11) 0.0023(8) -0.0066(9) 0.0017(8) C9 0.0298(12) 0.0189(9) 0.0158(10) 0.0009(8) -0.0073(9) 0.0010(9) C10 0.0248(11) 0.0174(9) 0.0146(10) -0.0011(8) -0.0003(8) 0.0016(8) C11 0.0185(11) 0.0145(9) 0.0238(11) -0.0015(8) 0.0024(9) -0.0027(8) C12 0.0151(10) 0.0159(9) 0.0225(10) 0.0042(8) 0.0003(8) 0.0022(8) C13 0.0249(12) 0.0224(10) 0.0256(12) 0.0027(9) -0.0014(9) 0.0017(9) C14 0.0260(13) 0.0204(10) 0.0418(14) -0.0014(10) -0.0085(11) 0.0003(9) C15 0.0215(12) 0.0192(10) 0.0565(17) 0.0089(11) 0.0052(12) -0.0025(9) C16 0.0379(15) 0.0265(11) 0.0389(14) 0.0132(11) 0.0143(12) 0.0004(11) C17 0.0276(12) 0.0234(10) 0.0247(11) 0.0074(9) 0.0027(10) 0.0001(9) C18 0.0177(10) 0.0186(9) 0.0127(9) -0.0009(7) -0.0004(8) 0.0027(8) C19 0.0227(11) 0.0185(9) 0.0195(10) 0.0015(8) 0.0012(9) 0.0022(8) C20 0.0191(11) 0.0292(11) 0.0213(11) 0.0025(9) 0.0037(9) 0.0017(9) C21 0.0177(11) 0.0307(11) 0.0277(12) -0.0052(9) 0.0040(9) 0.0068(9) C22 0.0255(12) 0.0181(10) 0.0390(14) -0.0027(9) 0.0010(10) 0.0056(9) C23 0.0195(11) 0.0170(9) 0.0258(11) 0.0016(8) 0.0024(9) 0.0011(8) C24 0.0176(12) 0.0320(12) 0.0382(14) 0.0075(10) 0.0028(10) 0.0045(9) C25 0.0128(11) 0.0323(12) 0.0293(12) 0.0024(9) -0.0035(9) 0.0036(9) C26 0.0299(14) 0.0333(13) 0.0450(15) 0.0118(11) -0.0022(12) 0.0137(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 Pt P 2.2437(5) . ? Pt S 2.2810(5) . ? Pt Cl2 2.3154(5) . ? Pt Cl1 2.3564(5) . ? Fe C5 2.032(2) . ? Fe C9 2.040(2) . ? Fe C4 2.041(2) . ? Fe C10 2.044(2) . ? Fe C6 2.0458(18) . ? Fe C7 2.047(2) . ? Fe C8 2.050(2) . ? Fe C2 2.051(2) . ? Fe C3 2.054(2) . ? Fe C1 2.054(2) . ? S C26 1.805(2) . ? S C25 1.823(2) . ? P C6 1.809(2) . ? P C18 1.812(2) . ? P C12 1.822(2) . ? O C11 1.234(3) . ? N C11 1.349(3) . ? N C24 1.444(3) . ? N H1N 0.9204 . ? C1 C5 1.432(3) . ? C1 C2 1.435(3) . ? C1 C11 1.482(3) . ? C2 C3 1.412(3) . ? C2 H2 0.9500 . ? C3 C4 1.413(4) . ? C3 H3 0.9500 . ? C4 C5 1.411(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.432(3) . ? C6 C10 1.440(3) . ? C7 C8 1.419(3) . ? C7 H7 0.9500 . ? C8 C9 1.417(3) . ? C8 H8 0.9500 . ? C9 C10 1.419(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C17 1.391(3) . ? C12 C13 1.393(3) . ? C13 C14 1.382(3) . ? C13 H13 0.9500 . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.367(4) . ? C15 H15 0.9500 . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.396(3) . ? C18 C23 1.399(3) . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 C21 1.385(3) . ? C20 H20 0.9500 . ? C21 C22 1.382(3) . ? C21 H21 0.9500 . ? C22 C23 1.380(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.523(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 P Pt S 92.857(19) . . ? P Pt Cl2 90.372(19) . . ? S Pt Cl2 173.57(2) . . ? P Pt Cl1 170.476(19) . . ? S Pt Cl1 89.84(2) . . ? Cl2 Pt Cl1 87.87(2) . . ? C5 Fe C9 109.69(9) . . ? C5 Fe C4 40.55(10) . . ? C9 Fe C4 106.35(9) . . ? C5 Fe C10 111.82(9) . . ? C9 Fe C10 40.68(8) . . ? C4 Fe C10 135.76(9) . . ? C5 Fe C6 141.33(9) . . ? C9 Fe C6 69.11(8) . . ? C4 Fe C6 175.31(9) . . ? C10 Fe C6 41.25(7) . . ? C5 Fe C7 176.75(9) . . ? C9 Fe C7 68.35(8) . . ? C4 Fe C7 136.91(9) . . ? C10 Fe C7 68.55(8) . . ? C6 Fe C7 40.96(8) . . ? C5 Fe C8 136.35(9) . . ? C9 Fe C8 40.53(9) . . ? C4 Fe C8 107.00(9) . . ? C10 Fe C8 68.32(9) . . ? C6 Fe C8 68.86(8) . . ? C7 Fe C8 40.52(8) . . ? C5 Fe C2 68.78(9) . . ? C9 Fe C2 173.22(9) . . ? C4 Fe C2 68.02(9) . . ? C10 Fe C2 146.08(9) . . ? C6 Fe C2 116.42(8) . . ? C7 Fe C2 112.84(9) . . ? C8 Fe C2 136.16(9) . . ? C5 Fe C3 68.35(10) . . ? C9 Fe C3 133.00(9) . . ? C4 Fe C3 40.39(10) . . ? C10 Fe C3 173.66(9) . . ? C6 Fe C3 142.07(9) . . ? C7 Fe C3 110.90(9) . . ? C8 Fe C3 106.95(9) . . ? C2 Fe C3 40.23(9) . . ? C5 Fe C1 41.04(8) . . ? C9 Fe C1 141.67(9) . . ? C4 Fe C1 68.33(9) . . ? C10 Fe C1 116.31(9) . . ? C6 Fe C1 115.90(8) . . ? C7 Fe C1 141.97(8) . . ? C8 Fe C1 174.91(8) . . ? C2 Fe C1 40.93(8) . . ? C3 Fe C1 68.26(9) . . ? C26 S C25 99.54(11) . . ? C26 S Pt 108.02(9) . . ? C25 S Pt 105.73(8) . . ? C6 P C18 105.37(9) . . ? C6 P C12 101.48(9) . . ? C18 P C12 104.30(9) . . ? C6 P Pt 119.94(7) . . ? C18 P Pt 113.55(7) . . ? C12 P Pt 110.52(7) . . ? C11 N C24 123.07(19) . . ? C11 N H1N 118.3 . . ? C24 N H1N 116.4 . . ? C5 C1 C2 107.1(2) . . ? C5 C1 C11 124.6(2) . . ? C2 C1 C11 128.29(19) . . ? C5 C1 Fe 68.67(12) . . ? C2 C1 Fe 69.45(12) . . ? C11 C1 Fe 128.65(14) . . ? C3 C2 C1 108.1(2) . . ? C3 C2 Fe 69.97(13) . . ? C1 C2 Fe 69.62(12) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe C2 H2 126.0 . . ? C2 C3 C4 108.2(2) . . ? C2 C3 Fe 69.81(12) . . ? C4 C3 Fe 69.31(13) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Fe C3 H3 126.6 . . ? C5 C4 C3 108.7(2) . . ? C5 C4 Fe 69.40(12) . . ? C3 C4 Fe 70.30(12) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe C4 H4 126.2 . . ? C4 C5 C1 107.9(2) . . ? C4 C5 Fe 70.05(13) . . ? C1 C5 Fe 70.30(11) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 125.2 . . ? C7 C6 C10 106.64(17) . . ? C7 C6 P 123.19(15) . . ? C10 C6 P 129.60(16) . . ? C7 C6 Fe 69.55(11) . . ? C10 C6 Fe 69.29(11) . . ? P C6 Fe 132.63(11) . . ? C8 C7 C6 108.68(19) . . ? C8 C7 Fe 69.89(12) . . ? C6 C7 Fe 69.49(11) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? Fe C7 H7 126.5 . . ? C9 C8 C7 108.10(19) . . ? C9 C8 Fe 69.32(12) . . ? C7 C8 Fe 69.60(12) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Fe C8 H8 126.7 . . ? C8 C9 C10 108.32(18) . . ? C8 C9 Fe 70.15(12) . . ? C10 C9 Fe 69.81(12) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Fe C9 H9 125.8 . . ? C9 C10 C6 108.25(19) . . ? C9 C10 Fe 69.51(12) . . ? C6 C10 Fe 69.46(11) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe C10 H10 126.7 . . ? O C11 N 123.1(2) . . ? O C11 C1 121.6(2) . . ? N C11 C1 115.32(18) . . ? C17 C12 C13 118.89(19) . . ? C17 C12 P 121.78(17) . . ? C13 C12 P 119.32(15) . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.4(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.2(2) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 120.1(2) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C23 119.02(19) . . ? C19 C18 P 120.27(15) . . ? C23 C18 P 120.37(15) . . ? C20 C19 C18 120.18(19) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 119.8(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C18 120.20(19) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? N C24 C25 112.21(18) . . ? N C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 S 110.87(16) . . ? C24 C25 H25A 109.5 . . ? S C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? S C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? S C26 H26A 109.5 . . ? S C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.570 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 962385' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_jt296_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl2 Fe N O P Pt S, 0.5 (C4 H8 O2)' _chemical_formula_sum 'C28 H30 Cl2 Fe N O2 P Pt S' _chemical_formula_weight 797.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3969(12) _cell_length_b 10.9050(13) _cell_length_c 15.3844(18) _cell_angle_alpha 95.995(4) _cell_angle_beta 102.319(4) _cell_angle_gamma 113.710(4) _cell_volume 1377.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.54 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 5.953 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.296 _exptl_absorpt_correction_T_max 0.588 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20413 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6309 _reflns_number_gt 5977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0147P)^2^+0.6334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6309 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0164 _refine_ls_wR_factor_ref 0.0347 _refine_ls_wR_factor_gt 0.0342 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Pt Pt 0.261904(9) 0.163670(8) 0.321994(5) 0.01252(3) Uani 1 1 d . . . Fe Fe -0.26687(3) -0.00174(3) 0.22163(2) 0.01421(7) Uani 1 1 d . . . Cl1 Cl 0.25806(6) 0.18491(5) 0.47203(3) 0.01911(11) Uani 1 1 d . . . Cl2 Cl 0.26828(6) 0.15719(5) 0.17273(3) 0.01965(11) Uani 1 1 d . . . S S 0.45333(6) 0.39657(5) 0.37221(4) 0.01858(12) Uani 1 1 d . . . P P 0.07997(6) -0.05861(5) 0.29198(4) 0.01218(11) Uani 1 1 d . . . O O -0.0954(2) 0.39771(18) 0.30768(13) 0.0354(4) Uani 1 1 d . . . N N 0.0908(2) 0.36241(18) 0.24999(13) 0.0216(4) Uani 1 1 d . . . H1N H 0.1097 0.3063 0.2137 0.026 Uiso 1 1 d R . . C1 C -0.1872(3) 0.1930(2) 0.19795(15) 0.0187(5) Uani 1 1 d . . . C2 C -0.3547(3) 0.1382(2) 0.19454(16) 0.0225(5) Uani 1 1 d . . . H2 H -0.4011 0.1759 0.2324 0.027 Uiso 1 1 calc R . . C3 C -0.4398(3) 0.0177(2) 0.12481(16) 0.0256(5) Uani 1 1 d . . . H3 H -0.5530 -0.0393 0.1080 0.031 Uiso 1 1 calc R . . C4 C -0.3267(3) -0.0031(2) 0.08445(15) 0.0245(5) Uani 1 1 d . . . H4 H -0.3510 -0.0760 0.0358 0.029 Uiso 1 1 calc R . . C5 C -0.1707(3) 0.1044(2) 0.12953(14) 0.0193(5) Uani 1 1 d . . . H5 H -0.0724 0.1155 0.1165 0.023 Uiso 1 1 calc R . . C6 C -0.1202(2) -0.0782(2) 0.28963(14) 0.0139(4) Uani 1 1 d . . . C7 C -0.1518(3) 0.0067(2) 0.35263(14) 0.0170(4) Uani 1 1 d . . . H7 H -0.0729 0.0869 0.3958 0.020 Uiso 1 1 calc R . . C8 C -0.3216(3) -0.0496(2) 0.33951(15) 0.0210(5) Uani 1 1 d . . . H8 H -0.3763 -0.0137 0.3723 0.025 Uiso 1 1 calc R . . C9 C -0.3958(3) -0.1691(2) 0.26870(16) 0.0209(5) Uani 1 1 d . . . H9 H -0.5087 -0.2266 0.2461 0.025 Uiso 1 1 calc R . . C10 C -0.2734(2) -0.1881(2) 0.23746(15) 0.0168(4) Uani 1 1 d . . . H10 H -0.2894 -0.2603 0.1906 0.020 Uiso 1 1 calc R . . C11 C -0.0615(3) 0.3252(2) 0.25823(16) 0.0208(5) Uani 1 1 d . . . C12 C 0.1281(2) -0.1489(2) 0.37869(14) 0.0139(4) Uani 1 1 d . . . C13 C 0.0075(3) -0.2439(2) 0.40798(15) 0.0188(5) Uani 1 1 d . . . H13 H -0.1023 -0.2615 0.3838 0.023 Uiso 1 1 calc R . . C14 C 0.0480(3) -0.3130(2) 0.47287(16) 0.0248(5) Uani 1 1 d . . . H14 H -0.0343 -0.3776 0.4931 0.030 Uiso 1 1 calc R . . C15 C 0.2077(3) -0.2883(2) 0.50801(15) 0.0246(5) Uani 1 1 d . . . H15 H 0.2348 -0.3354 0.5526 0.030 Uiso 1 1 calc R . . C16 C 0.3287(3) -0.1943(2) 0.47810(15) 0.0227(5) Uani 1 1 d . . . H16 H 0.4381 -0.1788 0.5010 0.027 Uiso 1 1 calc R . . C17 C 0.2886(3) -0.1236(2) 0.41474(15) 0.0182(5) Uani 1 1 d . . . H17 H 0.3715 -0.0572 0.3958 0.022 Uiso 1 1 calc R . . C18 C 0.0590(2) -0.1645(2) 0.18625(14) 0.0156(4) Uani 1 1 d . . . C19 C -0.0405(3) -0.1679(2) 0.10343(15) 0.0196(5) Uani 1 1 d . . . H19 H -0.1014 -0.1162 0.1022 0.024 Uiso 1 1 calc R . . C20 C -0.0513(3) -0.2457(2) 0.02321(16) 0.0245(5) Uani 1 1 d . . . H20 H -0.1222 -0.2495 -0.0323 0.029 Uiso 1 1 calc R . . C21 C 0.0400(3) -0.3176(3) 0.02317(17) 0.0297(6) Uani 1 1 d . . . H21 H 0.0333 -0.3698 -0.0323 0.036 Uiso 1 1 calc R . . C22 C 0.1420(3) -0.3138(3) 0.10449(17) 0.0320(6) Uani 1 1 d . . . H22 H 0.2061 -0.3625 0.1047 0.038 Uiso 1 1 calc R . . C23 C 0.1499(3) -0.2387(2) 0.18527(16) 0.0241(5) Uani 1 1 d . . . H23 H 0.2183 -0.2378 0.2408 0.029 Uiso 1 1 calc R . . C24 C 0.2235(3) 0.4941(2) 0.29724(17) 0.0248(5) Uani 1 1 d . . . H24A H 0.1779 0.5581 0.3129 0.030 Uiso 1 1 calc R . . H24B H 0.2883 0.5307 0.2550 0.030 Uiso 1 1 calc R . . C25 C 0.3359(3) 0.4922(2) 0.38356(16) 0.0223(5) Uani 1 1 d . . . H25A H 0.2700 0.4545 0.4251 0.027 Uiso 1 1 calc R . . H25B H 0.4126 0.5883 0.4136 0.027 Uiso 1 1 calc R . . C26 C 0.5522(3) 0.4680(2) 0.28885(17) 0.0283(6) Uani 1 1 d . . . H26A H 0.4716 0.4409 0.2296 0.042 Uiso 1 1 calc R . . H26B H 0.6326 0.4339 0.2839 0.042 Uiso 1 1 calc R . . H26C H 0.6062 0.5682 0.3077 0.042 Uiso 1 1 calc R . . O1S O 0.5901(4) 0.4535(4) -0.0817(2) 0.0335(8) Uani 0.50 1 d P . . O2S O 0.5189(6) 0.5375(4) 0.0328(3) 0.0363(9) Uani 0.50 1 d P . . C1S C 0.6221(10) 0.3771(8) 0.0577(5) 0.0454(18) Uani 0.50 1 d P . . H11S H 0.5261 0.2959 0.0583 0.068 Uiso 0.50 1 d PR . . H12S H 0.6725 0.4362 0.1188 0.068 Uiso 0.50 1 d PR . . H13S H 0.6996 0.3485 0.0392 0.068 Uiso 0.50 1 d PR . . C2S C 0.5768(7) 0.4583(5) -0.0057(4) 0.0281(12) Uani 0.50 1 d P . . C3S C 0.4736(8) 0.6244(6) -0.0209(5) 0.0406(14) Uani 0.50 1 d P . . H31S H 0.5522 0.6593 -0.0565 0.049 Uiso 0.50 1 d PR . . H32S H 0.4821 0.7041 0.0208 0.049 Uiso 0.50 1 d PR . . C4S C 0.3085(8) 0.5550(7) -0.0830(5) 0.0376(15) Uani 0.50 1 d P . . H41S H 0.3141 0.5251 -0.1440 0.056 Uiso 0.50 1 d PR . . H42S H 0.2582 0.6182 -0.0853 0.056 Uiso 0.50 1 d PR . . H43S H 0.2437 0.4750 -0.0614 0.056 Uiso 0.50 1 d PR . . 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 Pt 0.01054(4) 0.01215(4) 0.01431(4) 0.00467(3) 0.00252(3) 0.00443(3) Fe 0.01057(14) 0.01429(14) 0.01711(15) 0.00540(12) 0.00116(12) 0.00564(11) Cl1 0.0190(3) 0.0202(2) 0.0154(2) 0.0035(2) 0.0040(2) 0.0063(2) Cl2 0.0186(3) 0.0229(3) 0.0172(3) 0.0077(2) 0.0063(2) 0.0074(2) S 0.0147(3) 0.0141(2) 0.0220(3) 0.0052(2) 0.0009(2) 0.0032(2) P 0.0109(2) 0.0117(2) 0.0140(3) 0.0041(2) 0.0024(2) 0.0052(2) O 0.0339(10) 0.0255(9) 0.0451(11) -0.0005(8) 0.0171(9) 0.0102(8) N 0.0174(9) 0.0174(9) 0.0272(10) 0.0030(8) 0.0010(8) 0.0079(8) C1 0.0190(11) 0.0163(10) 0.0222(11) 0.0096(9) 0.0040(9) 0.0087(9) C2 0.0186(11) 0.0235(11) 0.0312(13) 0.0132(10) 0.0062(10) 0.0134(9) C3 0.0151(11) 0.0282(12) 0.0298(13) 0.0115(10) -0.0052(10) 0.0102(10) C4 0.0266(13) 0.0236(12) 0.0181(11) 0.0068(9) -0.0026(10) 0.0097(10) C5 0.0211(11) 0.0203(11) 0.0175(11) 0.0099(9) 0.0049(9) 0.0090(9) C6 0.0108(10) 0.0152(10) 0.0163(10) 0.0070(8) 0.0014(8) 0.0066(8) C7 0.0170(11) 0.0186(10) 0.0150(10) 0.0053(8) 0.0025(9) 0.0080(9) C8 0.0197(11) 0.0277(12) 0.0222(12) 0.0102(10) 0.0092(10) 0.0140(10) C9 0.0133(10) 0.0198(11) 0.0301(13) 0.0128(10) 0.0065(9) 0.0056(9) C10 0.0141(10) 0.0138(10) 0.0213(11) 0.0058(8) 0.0017(9) 0.0060(8) C11 0.0219(12) 0.0174(10) 0.0241(12) 0.0102(9) 0.0049(10) 0.0090(9) C12 0.0165(10) 0.0124(9) 0.0134(10) 0.0022(8) 0.0027(8) 0.0079(8) C13 0.0163(11) 0.0198(11) 0.0215(11) 0.0062(9) 0.0065(9) 0.0080(9) C14 0.0331(13) 0.0201(11) 0.0258(12) 0.0121(10) 0.0132(11) 0.0121(10) C15 0.0372(14) 0.0240(12) 0.0182(11) 0.0069(9) 0.0029(10) 0.0205(11) C16 0.0214(12) 0.0219(11) 0.0225(12) -0.0016(9) -0.0041(10) 0.0138(9) C17 0.0156(10) 0.0157(10) 0.0206(11) 0.0019(9) 0.0034(9) 0.0055(8) C18 0.0149(10) 0.0146(10) 0.0162(10) 0.0039(8) 0.0046(9) 0.0051(8) C19 0.0199(11) 0.0225(11) 0.0209(11) 0.0069(9) 0.0060(9) 0.0128(9) C20 0.0249(12) 0.0301(13) 0.0172(11) 0.0056(10) 0.0029(10) 0.0121(10) C21 0.0386(15) 0.0320(13) 0.0194(12) -0.0011(10) 0.0065(11) 0.0185(12) C22 0.0430(16) 0.0373(14) 0.0271(13) 0.0019(11) 0.0077(12) 0.0309(13) C23 0.0281(13) 0.0274(12) 0.0196(11) 0.0030(10) 0.0013(10) 0.0180(10) C24 0.0200(12) 0.0153(10) 0.0335(13) 0.0061(10) -0.0002(10) 0.0057(9) C25 0.0226(12) 0.0146(10) 0.0259(12) 0.0007(9) 0.0024(10) 0.0073(9) C26 0.0232(12) 0.0222(12) 0.0377(14) 0.0131(11) 0.0125(11) 0.0045(10) O1S 0.033(2) 0.042(2) 0.0253(19) 0.0038(16) 0.0082(16) 0.0178(17) O2S 0.038(2) 0.037(2) 0.039(2) 0.0091(17) 0.011(2) 0.021(2) C1S 0.040(5) 0.041(4) 0.050(4) 0.017(4) 0.004(4) 0.016(3) C2S 0.025(3) 0.027(3) 0.024(3) 0.004(2) 0.003(2) 0.005(2) C3S 0.045(4) 0.031(3) 0.057(4) 0.019(3) 0.020(3) 0.023(3) C4S 0.045(4) 0.038(4) 0.049(4) 0.024(3) 0.031(4) 0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt P 2.2602(6) . ? Pt Cl2 2.3043(6) . ? Pt Cl1 2.3050(6) . ? Pt S 2.3677(6) . ? Fe C6 2.045(2) . ? Fe C2 2.045(2) . ? Fe C7 2.047(2) . ? Fe C9 2.048(2) . ? Fe C10 2.050(2) . ? Fe C1 2.050(2) . ? Fe C8 2.051(2) . ? Fe C5 2.052(2) . ? Fe C3 2.053(2) . ? Fe C4 2.062(2) . ? S C26 1.803(2) . ? S C25 1.818(2) . ? P C6 1.797(2) . ? P C18 1.818(2) . ? P C12 1.824(2) . ? O C11 1.219(3) . ? N C11 1.360(3) . ? N C24 1.449(3) . ? N H1N 0.8808 . ? C1 C2 1.428(3) . ? C1 C5 1.429(3) . ? C1 C11 1.489(3) . ? C2 C3 1.418(3) . ? C2 H2 0.9500 . ? C3 C4 1.418(4) . ? C3 H3 0.9500 . ? C4 C5 1.421(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.429(3) . ? C6 C10 1.439(3) . ? C7 C8 1.419(3) . ? C7 H7 0.9500 . ? C8 C9 1.421(3) . ? C8 H8 0.9500 . ? C9 C10 1.415(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C13 1.389(3) . ? C12 C17 1.391(3) . ? C13 C14 1.392(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 C17 1.386(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.395(3) . ? C18 C19 1.398(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.376(4) . ? C20 H20 0.9500 . ? C21 C22 1.390(3) . ? C21 H21 0.9500 . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.518(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O1S C2S 1.200(6) . ? O2S C2S 1.342(7) . ? O2S C3S 1.449(7) . ? C1S C2S 1.491(9) . ? C1S H11S 0.9800 . ? C1S H12S 0.9800 . ? C1S H13S 0.9800 . ? C3S C4S 1.471(9) . ? C3S H31S 0.9900 . ? C3S H32S 0.9900 . ? C4S H41S 0.9800 . ? C4S H42S 0.9800 . ? C4S H43S 0.9800 . ? 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 P Pt Cl2 93.05(2) . . ? P Pt Cl1 90.084(19) . . ? Cl2 Pt Cl1 176.227(19) . . ? P Pt S 173.044(19) . . ? Cl2 Pt S 93.89(2) . . ? Cl1 Pt S 82.999(19) . . ? C6 Fe C2 157.55(9) . . ? C6 Fe C7 40.88(9) . . ? C2 Fe C7 119.96(9) . . ? C6 Fe C9 68.50(8) . . ? C2 Fe C9 120.48(9) . . ? C7 Fe C9 68.28(9) . . ? C6 Fe C10 41.15(8) . . ? C2 Fe C10 157.70(9) . . ? C7 Fe C10 68.78(9) . . ? C9 Fe C10 40.41(9) . . ? C6 Fe C1 124.43(8) . . ? C2 Fe C1 40.80(9) . . ? C7 Fe C1 108.94(9) . . ? C9 Fe C1 158.34(10) . . ? C10 Fe C1 160.50(9) . . ? C6 Fe C8 68.52(9) . . ? C2 Fe C8 104.11(10) . . ? C7 Fe C8 40.51(8) . . ? C9 Fe C8 40.57(9) . . ? C10 Fe C8 68.39(9) . . ? C1 Fe C8 123.31(9) . . ? C6 Fe C5 112.05(9) . . ? C2 Fe C5 68.35(9) . . ? C7 Fe C5 128.25(9) . . ? C9 Fe C5 157.03(9) . . ? C10 Fe C5 124.49(9) . . ? C1 Fe C5 40.78(9) . . ? C8 Fe C5 162.36(9) . . ? C6 Fe C3 161.87(9) . . ? C2 Fe C3 40.51(9) . . ? C7 Fe C3 153.45(10) . . ? C9 Fe C3 104.04(9) . . ? C10 Fe C3 122.69(9) . . ? C1 Fe C3 68.39(9) . . ? C8 Fe C3 117.26(10) . . ? C5 Fe C3 68.06(9) . . ? C6 Fe C4 127.86(10) . . ? C2 Fe C4 68.05(10) . . ? C7 Fe C4 165.36(9) . . ? C9 Fe C4 119.83(9) . . ? C10 Fe C4 108.72(9) . . ? C1 Fe C4 68.30(9) . . ? C8 Fe C4 153.30(9) . . ? C5 Fe C4 40.41(9) . . ? C3 Fe C4 40.32(10) . . ? C26 S C25 102.16(12) . . ? C26 S Pt 114.40(9) . . ? C25 S Pt 105.59(7) . . ? C6 P C18 106.15(10) . . ? C6 P C12 104.65(9) . . ? C18 P C12 103.66(10) . . ? C6 P Pt 112.46(7) . . ? C18 P Pt 116.30(7) . . ? C12 P Pt 112.57(7) . . ? C11 N C24 122.1(2) . . ? C11 N H1N 119.6 . . ? C24 N H1N 118.4 . . ? C2 C1 C5 107.3(2) . . ? C2 C1 C11 123.8(2) . . ? C5 C1 C11 128.7(2) . . ? C2 C1 Fe 69.40(12) . . ? C5 C1 Fe 69.68(12) . . ? C11 C1 Fe 129.87(15) . . ? C3 C2 C1 108.2(2) . . ? C3 C2 Fe 70.04(13) . . ? C1 C2 Fe 69.80(13) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe C2 H2 125.9 . . ? C4 C3 C2 108.2(2) . . ? C4 C3 Fe 70.18(13) . . ? C2 C3 Fe 69.46(12) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 126.0 . . ? C3 C4 C5 108.0(2) . . ? C3 C4 Fe 69.49(13) . . ? C5 C4 Fe 69.44(12) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe C4 H4 126.7 . . ? C4 C5 C1 108.2(2) . . ? C4 C5 Fe 70.15(13) . . ? C1 C5 Fe 69.54(12) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 126.0 . . ? C7 C6 C10 107.56(18) . . ? C7 C6 P 123.38(15) . . ? C10 C6 P 128.42(17) . . ? C7 C6 Fe 69.64(12) . . ? C10 C6 Fe 69.61(12) . . ? P C6 Fe 133.16(11) . . ? C8 C7 C6 108.12(19) . . ? C8 C7 Fe 69.89(12) . . ? C6 C7 Fe 69.48(11) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.3 . . ? C7 C8 C9 108.0(2) . . ? C7 C8 Fe 69.60(12) . . ? C9 C8 Fe 69.60(13) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe C8 H8 126.4 . . ? C10 C9 C8 108.68(19) . . ? C10 C9 Fe 69.88(12) . . ? C8 C9 Fe 69.83(12) . . ? C10 C9 H9 125.7 . . ? C8 C9 H9 125.7 . . ? Fe C9 H9 126.2 . . ? C9 C10 C6 107.6(2) . . ? C9 C10 Fe 69.71(12) . . ? C6 C10 Fe 69.24(12) . . ? C9 C10 H10 126.2 . . ? C6 C10 H10 126.2 . . ? Fe C10 H10 126.4 . . ? O C11 N 122.7(2) . . ? O C11 C1 121.9(2) . . ? N C11 C1 115.3(2) . . ? C13 C12 C17 119.62(19) . . ? C13 C12 P 121.32(16) . . ? C17 C12 P 119.05(15) . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.0(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 119.6(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C12 120.5(2) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 118.2(2) . . ? C23 C18 P 120.32(16) . . ? C19 C18 P 121.40(17) . . ? C20 C19 C18 120.7(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.5(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.8(2) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.8(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 121.0(2) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? N C24 C25 115.30(18) . . ? N C24 H24A 108.4 . . ? C25 C24 H24A 108.4 . . ? N C24 H24B 108.4 . . ? C25 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? C24 C25 S 117.57(17) . . ? C24 C25 H25A 107.9 . . ? S C25 H25A 107.9 . . ? C24 C25 H25B 107.9 . . ? S C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? S C26 H26A 109.5 . . ? S C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2S O2S C3S 117.2(4) . . ? C2S C1S H11S 110.7 . . ? C2S C1S H12S 107.6 . . ? H11S C1S H12S 109.5 . . ? C2S C1S H13S 110.1 . . ? H11S C1S H13S 109.5 . . ? H12S C1S H13S 109.5 . . ? O1S C2S O2S 124.1(6) . . ? O1S C2S C1S 124.3(6) . . ? O2S C2S C1S 111.5(5) . . ? O2S C3S C4S 113.9(5) . . ? O2S C3S H31S 108.3 . . ? C4S C3S H31S 109.5 . . ? O2S C3S H32S 108.8 . . ? C4S C3S H32S 108.5 . . ? H31S C3S H32S 107.8 . . ? C3S C4S H41S 108.9 . . ? C3S C4S H42S 109.9 . . ? H41S C4S H42S 109.5 . . ? C3S C4S H43S 109.6 . . ? H41S C4S H43S 109.5 . . ? H42S C4S H43S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Pt S C26 -9.88(10) . . . . ? Cl1 Pt S C26 172.26(10) . . . . ? Cl2 Pt S C25 101.63(8) . . . . ? Cl1 Pt S C25 -76.23(8) . . . . ? Cl2 Pt P C6 -104.41(7) . . . . ? Cl1 Pt P C6 73.49(7) . . . . ? Cl2 Pt P C18 18.28(8) . . . . ? Cl1 Pt P C18 -163.82(8) . . . . ? Cl2 Pt P C12 137.67(8) . . . . ? Cl1 Pt P C12 -44.42(8) . . . . ? C6 Fe C1 C2 -157.02(14) . . . . ? C7 Fe C1 C2 -114.23(14) . . . . ? C9 Fe C1 C2 -35.5(3) . . . . ? C10 Fe C1 C2 166.0(2) . . . . ? C8 Fe C1 C2 -71.65(16) . . . . ? C5 Fe C1 C2 118.59(19) . . . . ? C3 Fe C1 C2 37.57(14) . . . . ? C4 Fe C1 C2 81.10(15) . . . . ? C6 Fe C1 C5 84.39(15) . . . . ? C2 Fe C1 C5 -118.59(19) . . . . ? C7 Fe C1 C5 127.17(13) . . . . ? C9 Fe C1 C5 -154.1(2) . . . . ? C10 Fe C1 C5 47.4(3) . . . . ? C8 Fe C1 C5 169.75(13) . . . . ? C3 Fe C1 C5 -81.02(14) . . . . ? C4 Fe C1 C5 -37.49(13) . . . . ? C6 Fe C1 C11 -39.6(3) . . . . ? C2 Fe C1 C11 117.4(3) . . . . ? C7 Fe C1 C11 3.2(2) . . . . ? C9 Fe C1 C11 81.9(3) . . . . ? C10 Fe C1 C11 -76.6(4) . . . . ? C8 Fe C1 C11 45.8(3) . . . . ? C5 Fe C1 C11 -124.0(3) . . . . ? C3 Fe C1 C11 155.0(2) . . . . ? C4 Fe C1 C11 -161.5(2) . . . . ? C5 C1 C2 C3 -0.1(2) . . . . ? C11 C1 C2 C3 175.36(19) . . . . ? Fe C1 C2 C3 -59.72(15) . . . . ? C5 C1 C2 Fe 59.61(14) . . . . ? C11 C1 C2 Fe -124.9(2) . . . . ? C6 Fe C2 C3 176.7(2) . . . . ? C7 Fe C2 C3 -156.19(14) . . . . ? C9 Fe C2 C3 -75.19(17) . . . . ? C10 Fe C2 C3 -48.5(3) . . . . ? C1 Fe C2 C3 119.2(2) . . . . ? C8 Fe C2 C3 -115.65(15) . . . . ? C5 Fe C2 C3 81.13(15) . . . . ? C4 Fe C2 C3 37.46(14) . . . . ? C6 Fe C2 C1 57.5(3) . . . . ? C7 Fe C2 C1 84.58(15) . . . . ? C9 Fe C2 C1 165.58(13) . . . . ? C10 Fe C2 C1 -167.7(2) . . . . ? C8 Fe C2 C1 125.12(14) . . . . ? C5 Fe C2 C1 -38.10(13) . . . . ? C3 Fe C2 C1 -119.2(2) . . . . ? C4 Fe C2 C1 -81.77(15) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? Fe C2 C3 C4 -59.70(15) . . . . ? C1 C2 C3 Fe 59.57(15) . . . . ? C6 Fe C3 C4 -56.6(3) . . . . ? C2 Fe C3 C4 119.34(19) . . . . ? C7 Fe C3 C4 170.82(17) . . . . ? C9 Fe C3 C4 -119.85(14) . . . . ? C10 Fe C3 C4 -80.39(15) . . . . ? C1 Fe C3 C4 81.50(14) . . . . ? C8 Fe C3 C4 -161.09(13) . . . . ? C5 Fe C3 C4 37.43(13) . . . . ? C6 Fe C3 C2 -176.0(2) . . . . ? C7 Fe C3 C2 51.5(3) . . . . ? C9 Fe C3 C2 120.81(14) . . . . ? C10 Fe C3 C2 160.27(13) . . . . ? C1 Fe C3 C2 -37.83(14) . . . . ? C8 Fe C3 C2 79.57(16) . . . . ? C5 Fe C3 C2 -81.90(15) . . . . ? C4 Fe C3 C2 -119.34(19) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? Fe C3 C4 C5 -58.93(15) . . . . ? C2 C3 C4 Fe 59.25(15) . . . . ? C6 Fe C4 C3 160.78(13) . . . . ? C2 Fe C4 C3 -37.62(13) . . . . ? C7 Fe C4 C3 -163.6(3) . . . . ? C9 Fe C4 C3 75.91(16) . . . . ? C10 Fe C4 C3 118.82(14) . . . . ? C1 Fe C4 C3 -81.73(14) . . . . ? C8 Fe C4 C3 39.9(3) . . . . ? C5 Fe C4 C3 -119.6(2) . . . . ? C6 Fe C4 C5 -79.66(17) . . . . ? C2 Fe C4 C5 81.94(15) . . . . ? C7 Fe C4 C5 -44.1(4) . . . . ? C9 Fe C4 C5 -164.53(14) . . . . ? C10 Fe C4 C5 -121.62(14) . . . . ? C1 Fe C4 C5 37.83(14) . . . . ? C8 Fe C4 C5 159.4(2) . . . . ? C3 Fe C4 C5 119.6(2) . . . . ? C3 C4 C5 C1 -0.4(2) . . . . ? Fe C4 C5 C1 -59.35(14) . . . . ? C3 C4 C5 Fe 58.96(15) . . . . ? C2 C1 C5 C4 0.3(2) . . . . ? C11 C1 C5 C4 -174.9(2) . . . . ? Fe C1 C5 C4 59.74(15) . . . . ? C2 C1 C5 Fe -59.43(14) . . . . ? C11 C1 C5 Fe 125.4(2) . . . . ? C6 Fe C5 C4 123.07(15) . . . . ? C2 Fe C5 C4 -81.14(15) . . . . ? C7 Fe C5 C4 167.07(14) . . . . ? C9 Fe C5 C4 36.4(3) . . . . ? C10 Fe C5 C4 78.09(17) . . . . ? C1 Fe C5 C4 -119.3(2) . . . . ? C8 Fe C5 C4 -148.6(3) . . . . ? C3 Fe C5 C4 -37.36(15) . . . . ? C6 Fe C5 C1 -117.67(13) . . . . ? C2 Fe C5 C1 38.12(13) . . . . ? C7 Fe C5 C1 -73.67(16) . . . . ? C9 Fe C5 C1 155.6(2) . . . . ? C10 Fe C5 C1 -162.65(12) . . . . ? C8 Fe C5 C1 -29.4(4) . . . . ? C3 Fe C5 C1 81.90(14) . . . . ? C4 Fe C5 C1 119.3(2) . . . . ? C18 P C6 C7 -168.52(16) . . . . ? C12 P C6 C7 82.22(18) . . . . ? Pt P C6 C7 -40.29(18) . . . . ? C18 P C6 C10 21.9(2) . . . . ? C12 P C6 C10 -87.4(2) . . . . ? Pt P C6 C10 150.09(16) . . . . ? C18 P C6 Fe -75.85(17) . . . . ? C12 P C6 Fe 174.89(14) . . . . ? Pt P C6 Fe 52.39(17) . . . . ? C2 Fe C6 C7 37.1(3) . . . . ? C9 Fe C6 C7 -81.22(13) . . . . ? C10 Fe C6 C7 -118.77(17) . . . . ? C1 Fe C6 C7 79.01(14) . . . . ? C8 Fe C6 C7 -37.46(12) . . . . ? C5 Fe C6 C7 123.54(12) . . . . ? C3 Fe C6 C7 -149.8(3) . . . . ? C4 Fe C6 C7 167.01(12) . . . . ? C2 Fe C6 C10 155.9(2) . . . . ? C7 Fe C6 C10 118.77(17) . . . . ? C9 Fe C6 C10 37.55(13) . . . . ? C1 Fe C6 C10 -162.23(13) . . . . ? C8 Fe C6 C10 81.30(14) . . . . ? C5 Fe C6 C10 -117.70(13) . . . . ? C3 Fe C6 C10 -31.0(3) . . . . ? C4 Fe C6 C10 -74.22(15) . . . . ? C2 Fe C6 P -80.1(3) . . . . ? C7 Fe C6 P -117.2(2) . . . . ? C9 Fe C6 P 161.62(19) . . . . ? C10 Fe C6 P 124.1(2) . . . . ? C1 Fe C6 P -38.2(2) . . . . ? C8 Fe C6 P -154.63(18) . . . . ? C5 Fe C6 P 6.38(19) . . . . ? C3 Fe C6 P 93.0(3) . . . . ? C4 Fe C6 P 49.8(2) . . . . ? C10 C6 C7 C8 -0.1(2) . . . . ? P C6 C7 C8 -171.59(15) . . . . ? Fe C6 C7 C8 59.42(14) . . . . ? C10 C6 C7 Fe -59.52(13) . . . . ? P C6 C7 Fe 128.99(15) . . . . ? C6 Fe C7 C8 -119.39(18) . . . . ? C2 Fe C7 C8 76.03(15) . . . . ? C9 Fe C7 C8 -37.58(14) . . . . ? C10 Fe C7 C8 -81.16(14) . . . . ? C1 Fe C7 C8 119.48(14) . . . . ? C5 Fe C7 C8 160.99(14) . . . . ? C3 Fe C7 C8 40.1(3) . . . . ? C4 Fe C7 C8 -164.0(3) . . . . ? C2 Fe C7 C6 -164.58(12) . . . . ? C9 Fe C7 C6 81.80(13) . . . . ? C10 Fe C7 C6 38.23(11) . . . . ? C1 Fe C7 C6 -121.13(12) . . . . ? C8 Fe C7 C6 119.39(18) . . . . ? C5 Fe C7 C6 -79.63(15) . . . . ? C3 Fe C7 C6 159.50(18) . . . . ? C4 Fe C7 C6 -44.6(4) . . . . ? C6 C7 C8 C9 0.0(2) . . . . ? Fe C7 C8 C9 59.18(15) . . . . ? C6 C7 C8 Fe -59.16(14) . . . . ? C6 Fe C8 C7 37.80(13) . . . . ? C2 Fe C8 C7 -119.90(14) . . . . ? C9 Fe C8 C7 119.40(19) . . . . ? C10 Fe C8 C7 82.20(14) . . . . ? C1 Fe C8 C7 -80.14(16) . . . . ? C5 Fe C8 C7 -57.6(4) . . . . ? C3 Fe C8 C7 -161.10(13) . . . . ? C4 Fe C8 C7 171.1(2) . . . . ? C6 Fe C8 C9 -81.61(14) . . . . ? C2 Fe C8 C9 120.70(14) . . . . ? C7 Fe C8 C9 -119.40(19) . . . . ? C10 Fe C8 C9 -37.21(13) . . . . ? C1 Fe C8 C9 160.46(13) . . . . ? C5 Fe C8 C9 -177.0(3) . . . . ? C3 Fe C8 C9 79.50(15) . . . . ? C4 Fe C8 C9 51.7(3) . . . . ? C7 C8 C9 C10 0.1(2) . . . . ? Fe C8 C9 C10 59.26(15) . . . . ? C7 C8 C9 Fe -59.18(15) . . . . ? C6 Fe C9 C10 -38.22(13) . . . . ? C2 Fe C9 C10 164.75(13) . . . . ? C7 Fe C9 C10 -82.34(14) . . . . ? C1 Fe C9 C10 -169.1(2) . . . . ? C8 Fe C9 C10 -119.87(19) . . . . ? C5 Fe C9 C10 57.8(3) . . . . ? C3 Fe C9 C10 124.41(14) . . . . ? C4 Fe C9 C10 84.10(15) . . . . ? C6 Fe C9 C8 81.66(14) . . . . ? C2 Fe C9 C8 -75.38(16) . . . . ? C7 Fe C9 C8 37.53(13) . . . . ? C10 Fe C9 C8 119.87(19) . . . . ? C1 Fe C9 C8 -49.2(3) . . . . ? C5 Fe C9 C8 177.7(2) . . . . ? C3 Fe C9 C8 -115.72(14) . . . . ? C4 Fe C9 C8 -156.03(14) . . . . ? C8 C9 C10 C6 -0.1(2) . . . . ? Fe C9 C10 C6 59.09(14) . . . . ? C8 C9 C10 Fe -59.23(15) . . . . ? C7 C6 C10 C9 0.2(2) . . . . ? P C6 C10 C9 171.08(15) . . . . ? Fe C6 C10 C9 -59.39(14) . . . . ? C7 C6 C10 Fe 59.54(14) . . . . ? P C6 C10 Fe -129.54(17) . . . . ? C6 Fe C10 C9 119.00(19) . . . . ? C2 Fe C10 C9 -36.7(3) . . . . ? C7 Fe C10 C9 81.01(14) . . . . ? C1 Fe C10 C9 167.9(2) . . . . ? C8 Fe C10 C9 37.35(13) . . . . ? C5 Fe C10 C9 -156.38(13) . . . . ? C3 Fe C10 C9 -71.99(16) . . . . ? C4 Fe C10 C9 -114.34(14) . . . . ? C2 Fe C10 C6 -155.7(2) . . . . ? C7 Fe C10 C6 -37.99(12) . . . . ? C9 Fe C10 C6 -119.00(19) . . . . ? C1 Fe C10 C6 48.9(3) . . . . ? C8 Fe C10 C6 -81.65(14) . . . . ? C5 Fe C10 C6 84.62(15) . . . . ? C3 Fe C10 C6 169.01(13) . . . . ? C4 Fe C10 C6 126.66(13) . . . . ? C24 N C11 O -2.2(3) . . . . ? C24 N C11 C1 173.92(18) . . . . ? C2 C1 C11 O -2.0(3) . . . . ? C5 C1 C11 O 172.5(2) . . . . ? Fe C1 C11 O -92.4(3) . . . . ? C2 C1 C11 N -178.15(19) . . . . ? C5 C1 C11 N -3.7(3) . . . . ? Fe C1 C11 N 91.4(2) . . . . ? C6 P C12 C13 18.1(2) . . . . ? C18 P C12 C13 -92.94(19) . . . . ? Pt P C12 C13 140.55(16) . . . . ? C6 P C12 C17 -163.07(17) . . . . ? C18 P C12 C17 85.88(18) . . . . ? Pt P C12 C17 -40.63(19) . . . . ? C17 C12 C13 C14 -0.1(3) . . . . ? P C12 C13 C14 178.66(17) . . . . ? C12 C13 C14 C15 -0.3(4) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? C14 C15 C16 C17 1.6(4) . . . . ? C15 C16 C17 C12 -2.1(3) . . . . ? C13 C12 C17 C16 1.4(3) . . . . ? P C12 C17 C16 -177.47(17) . . . . ? C6 P C18 C23 -141.36(18) . . . . ? C12 P C18 C23 -31.4(2) . . . . ? Pt P C18 C23 92.71(18) . . . . ? C6 P C18 C19 42.38(19) . . . . ? C12 P C18 C19 152.33(17) . . . . ? Pt P C18 C19 -83.55(18) . . . . ? C23 C18 C19 C20 1.7(3) . . . . ? P C18 C19 C20 177.99(17) . . . . ? C18 C19 C20 C21 -2.1(3) . . . . ? C19 C20 C21 C22 0.9(4) . . . . ? C20 C21 C22 C23 0.7(4) . . . . ? C21 C22 C23 C18 -1.2(4) . . . . ? C19 C18 C23 C22 0.0(3) . . . . ? P C18 C23 C22 -176.38(19) . . . . ? C11 N C24 C25 99.9(3) . . . . ? N C24 C25 S 64.7(3) . . . . ? C26 S C25 C24 53.44(19) . . . . ? Pt S C25 C24 -66.48(17) . . . . ? O2S O1S C2S C3S 93.0(9) 2_665 . . 2_665 ? O2S O1S C2S O2S -39.2(6) 2_665 . . . ? O2S O1S C2S C1S 140.7(8) 2_665 . . . ? O2S O1S C2S C4S 175.1(9) 2_665 . . 2_665 ? O2S O1S C2S C2S -21.5(3) 2_665 . . 2_665 ? C2S O2S C2S O2S 0.000(2) 2_665 . . 2_665 ? O1S O2S C2S O2S 80.9(10) 2_665 . . 2_665 ? C3S O2S C2S O2S -50.9(6) . . . 2_665 ? C3S O2S C2S O2S 92.7(7) 2_665 . . 2_665 ? C2S O2S C2S C3S -92.7(7) 2_665 . . 2_665 ? O2S O2S C2S C3S -92.7(7) 2_665 . . 2_665 ? O1S O2S C2S C3S -11.8(13) 2_665 . . 2_665 ? C3S O2S C2S C3S -143.6(4) . . . 2_665 ? C2S O2S C2S O1S 49.5(7) 2_665 . . . ? O2S O2S C2S O1S 49.5(7) 2_665 . . . ? O1S O2S C2S O1S 130.4(7) 2_665 . . . ? C3S O2S C2S O1S -1.4(9) . . . . ? C3S O2S C2S O1S 142.1(10) 2_665 . . . ? C2S O2S C2S C1S -130.5(7) 2_665 . . . ? O2S O2S C2S C1S -130.5(7) 2_665 . . . ? O1S O2S C2S C1S -49.5(12) 2_665 . . . ? C3S O2S C2S C1S 178.6(5) . . . . ? C3S O2S C2S C1S -37.8(5) 2_665 . . . ? C2S O2S C2S C4S -157.2(7) 2_665 . . 2_665 ? O2S O2S C2S C4S -157.2(7) 2_665 . . 2_665 ? O1S O2S C2S C4S -76.3(10) 2_665 . . 2_665 ? C3S O2S C2S C4S 151.9(5) . . . 2_665 ? C3S O2S C2S C4S -64.6(5) 2_665 . . 2_665 ? O2S O2S C2S C2S 0.000(1) 2_665 . . 2_665 ? O1S O2S C2S C2S 80.9(10) 2_665 . . 2_665 ? C3S O2S C2S C2S -50.9(6) . . . 2_665 ? C3S O2S C2S C2S 92.7(7) 2_665 . . 2_665 ? C4S C1S C2S O2S -133.8(11) 2_665 . . 2_665 ? C3S C1S C2S O2S 12.9(11) 2_665 . . 2_665 ? C4S C1S C2S C3S -146.7(15) 2_665 . . 2_665 ? C4S C1S C2S O1S 108.7(10) 2_665 . . . ? C3S C1S C2S O1S -104.7(10) 2_665 . . . ? C4S C1S C2S O2S -71.4(11) 2_665 . . . ? C3S C1S C2S O2S 75.3(9) 2_665 . . . ? C3S C1S C2S C4S 146.7(15) 2_665 . . 2_665 ? C4S C1S C2S C2S -92.0(11) 2_665 . . 2_665 ? C3S C1S C2S C2S 54.7(9) 2_665 . . 2_665 ? C2S O2S C3S C1S -13.6(12) 2_665 . . 2_665 ? O2S O2S C3S C1S 66.8(13) 2_665 . . 2_665 ? C2S O2S C3S C1S 98.8(13) . . . 2_665 ? O1S O2S C3S C1S -57.4(13) 2_665 . . 2_665 ? C3S O2S C3S C1S 66.8(13) 2_665 . . 2_665 ? O2S O2S C3S C2S 80.3(7) 2_665 . . 2_665 ? C2S O2S C3S C2S 112.4(7) . . . 2_665 ? O1S O2S C3S C2S -43.9(6) 2_665 . . 2_665 ? C3S O2S C3S C2S 80.3(7) 2_665 . . 2_665 ? C2S O2S C3S C4S -27.8(7) 2_665 . . . ? O2S O2S C3S C4S 52.6(7) 2_665 . . . ? C2S O2S C3S C4S 84.6(7) . . . . ? O1S O2S C3S C4S -71.7(5) 2_665 . . . ? C3S O2S C3S C4S 52.6(7) 2_665 . . . ? C2S O2S C3S O2S -80.3(7) 2_665 . . 2_665 ? C2S O2S C3S O2S 32.1(4) . . . 2_665 ? O1S O2S C3S O2S -124.2(6) 2_665 . . 2_665 ? C3S O2S C3S O2S 0.000(1) 2_665 . . 2_665 ? C2S C3S C4S C1S 140.8(16) 2_665 . . 2_665 ? O2S C3S C4S C1S 158.4(15) . . . 2_665 ? O2S C3S C4S C1S -171.7(15) 2_665 . . 2_665 ? C1S C3S C4S C2S -140.8(16) 2_665 . . 2_665 ? O2S C3S C4S C2S 17.6(4) . . . 2_665 ? O2S C3S C4S C2S 47.5(4) 2_665 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.763 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.081 #===END _database_code_depnum_ccdc_archive 'CCDC 962386'