# 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_1 _database_code_depnum_ccdc_archive 'CCDC 908778' #TrackingRef 'M-Se-P-Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H19 Cr Fe O9 P Se' _chemical_formula_weight 597.11 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' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3001(8) _cell_length_b 18.7630(15) _cell_length_c 12.6710(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.187(2) _cell_angle_gamma 90.00 _cell_volume 2384.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9388 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.34 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6420 _exptl_absorpt_correction_T_max 0.8768 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27566 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.79 _reflns_number_total 6164 _reflns_number_gt 4715 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.3998P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6164 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3827(4) 0.1962(2) 0.4301(2) 0.0898(12) Uani 1 1 d . . . C2 C 0.3862(4) 0.1263(3) 0.4715(3) 0.0921(13) Uani 1 1 d . . . C3 C 0.2595(3) 0.11095(16) 0.4878(2) 0.0704(8) Uani 1 1 d . . . C4 C 0.1823(3) 0.17009(18) 0.4586(2) 0.0724(7) Uani 1 1 d . . . C5 C 0.2570(4) 0.22177(19) 0.4232(2) 0.0818(9) Uani 1 1 d . . . C6 C 0.5116(2) 0.20329(13) 0.65737(17) 0.0533(5) Uani 1 1 d . . . C7 C 0.3004(3) 0.28089(13) 0.6291(2) 0.0615(6) Uani 1 1 d . . . C8 C 0.4503(2) 0.03487(12) 0.74430(19) 0.0504(5) Uani 1 1 d . . . C9 C 0.4254(4) -0.04242(17) 0.7153(4) 0.0790(8) Uani 1 1 d . . . C10 C 0.5460(3) 0.0452(2) 0.8500(3) 0.0830(9) Uani 1 1 d . . . C11 C 0.2990(3) 0.19709(15) 0.92782(19) 0.0631(7) Uani 1 1 d . . . C12 C 0.2628(5) 0.2738(2) 0.9373(4) 0.0958(11) Uani 1 1 d . . . C13 C 0.4050(5) 0.1719(2) 1.0215(2) 0.0913(11) Uani 1 1 d . . . C14 C 0.1340(2) 0.01051(12) 0.87290(18) 0.0523(5) Uani 1 1 d . . . C15 C -0.1846(2) 0.04926(12) 0.6639(2) 0.0540(5) Uani 1 1 d . . . C16 C 0.0443(2) -0.01897(12) 0.66103(19) 0.0510(5) Uani 1 1 d . . . C17 C -0.0837(3) 0.08601(13) 0.8716(2) 0.0609(6) Uani 1 1 d . . . C18 C -0.1026(3) -0.05113(14) 0.8054(2) 0.0657(6) Uani 1 1 d . . . Cr1 Cr -0.02553(3) 0.030451(16) 0.76685(3) 0.04220(8) Uani 1 1 d . . . Fe1 Fe 0.34391(3) 0.196501(15) 0.58473(2) 0.04229(8) Uani 1 1 d . . . H1 H 0.436(3) 0.2231(17) 0.415(3) 0.084(10) Uiso 1 1 d . . . H2 H 0.432(3) 0.0999(18) 0.482(3) 0.082(12) Uiso 1 1 d . . . H3 H 0.230(4) 0.072(2) 0.513(3) 0.123(14) Uiso 1 1 d . . . H4 H 0.099(3) 0.1740(17) 0.465(2) 0.086(10) Uiso 1 1 d . . . H5 H 0.229(3) 0.2687(19) 0.401(3) 0.101(11) Uiso 1 1 d . . . H8 H 0.484(2) 0.0560(13) 0.693(2) 0.058(7) Uiso 1 1 d . . . H9A H 0.367(4) -0.049(2) 0.656(3) 0.127(16) Uiso 1 1 d . . . H9B H 0.399(4) -0.061(2) 0.783(4) 0.143(16) Uiso 1 1 d . . . H9C H 0.512(3) -0.0641(17) 0.714(2) 0.095(10) Uiso 1 1 d . . . H10A H 0.630(3) 0.0209(17) 0.849(3) 0.096(10) Uiso 1 1 d . . . H10B H 0.556(3) 0.0947(19) 0.869(3) 0.101(12) Uiso 1 1 d . . . H10C H 0.500(3) 0.0220(17) 0.902(3) 0.092(10) Uiso 1 1 d . . . H11 H 0.221(3) 0.1677(15) 0.920(2) 0.077(8) Uiso 1 1 d . . . H12A H 0.201(4) 0.288(2) 0.874(4) 0.120(15) Uiso 1 1 d . . . H12B H 0.351(4) 0.305(2) 0.939(3) 0.133(15) Uiso 1 1 d . . . H12C H 0.229(4) 0.277(2) 0.999(4) 0.128(14) Uiso 1 1 d . . . H13A H 0.376(4) 0.175(2) 1.082(3) 0.115(13) Uiso 1 1 d . . . H13B H 0.484(4) 0.2020(19) 1.029(3) 0.104(12) Uiso 1 1 d . . . H13C H 0.433(4) 0.122(2) 1.016(3) 0.135(15) Uiso 1 1 d . . . O1 O 0.62029(18) 0.20818(12) 0.70059(15) 0.0829(6) Uani 1 1 d . . . O2 O 0.2737(3) 0.33511(10) 0.6565(2) 0.0989(7) Uani 1 1 d . . . O3 O 0.31965(13) 0.06573(7) 0.74493(11) 0.0442(3) Uani 1 1 d . . . O4 O 0.35026(14) 0.19043(8) 0.82897(11) 0.0499(3) Uani 1 1 d . . . O5 O 0.2258(2) -0.00265(11) 0.93825(16) 0.0833(6) Uani 1 1 d . . . O6 O -0.28379(17) 0.05854(11) 0.60270(17) 0.0804(5) Uani 1 1 d . . . O7 O 0.08553(19) -0.04900(11) 0.59761(16) 0.0779(5) Uani 1 1 d . . . O8 O -0.1167(3) 0.11946(12) 0.93508(19) 0.0986(7) Uani 1 1 d . . . O9 O -0.1512(3) -0.10192(12) 0.8279(2) 0.1083(8) Uani 1 1 d . . . P1 P 0.27865(5) 0.14730(2) 0.72258(4) 0.03722(11) Uani 1 1 d . . . Se1 Se 0.062734(19) 0.148403(11) 0.703042(18) 0.04819(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.090(2) 0.144(3) 0.0395(13) -0.0005(16) 0.0230(14) -0.042(2) C2 0.094(3) 0.125(3) 0.0495(16) -0.0326(18) -0.0010(16) 0.044(3) C3 0.102(2) 0.0617(16) 0.0446(13) -0.0104(11) 0.0117(13) -0.0176(16) C4 0.0581(16) 0.095(2) 0.0569(15) -0.0125(14) -0.0021(12) -0.0093(15) C5 0.103(3) 0.082(2) 0.0485(14) 0.0185(13) -0.0095(14) -0.0084(18) C6 0.0522(12) 0.0653(14) 0.0441(11) -0.0046(10) 0.0145(9) -0.0138(10) C7 0.0744(16) 0.0508(13) 0.0636(15) 0.0087(11) 0.0248(12) -0.0062(12) C8 0.0392(10) 0.0602(13) 0.0535(12) 0.0144(10) 0.0143(9) 0.0095(9) C9 0.0700(19) 0.0651(18) 0.102(3) -0.0041(17) 0.0193(19) 0.0215(15) C10 0.0550(16) 0.108(3) 0.077(2) 0.0007(19) -0.0034(14) 0.0245(17) C11 0.0688(15) 0.0779(17) 0.0467(12) -0.0129(11) 0.0219(11) -0.0280(13) C12 0.098(3) 0.107(3) 0.090(3) -0.024(2) 0.036(2) 0.014(2) C13 0.128(3) 0.099(3) 0.0440(16) -0.0019(15) 0.0134(17) -0.006(2) C14 0.0578(13) 0.0490(12) 0.0502(12) 0.0086(9) 0.0122(10) -0.0065(10) C15 0.0434(12) 0.0535(12) 0.0665(14) -0.0062(10) 0.0157(10) -0.0007(9) C16 0.0415(10) 0.0509(12) 0.0577(13) -0.0054(10) 0.0051(9) -0.0030(9) C17 0.0724(15) 0.0522(13) 0.0651(15) 0.0007(11) 0.0305(12) -0.0018(11) C18 0.0645(15) 0.0558(14) 0.0807(18) 0.0005(12) 0.0249(13) -0.0117(12) Cr1 0.03947(16) 0.04018(17) 0.04832(18) -0.00034(13) 0.01288(13) -0.00356(13) Fe1 0.04464(15) 0.04432(16) 0.03758(15) 0.00408(11) 0.00866(11) -0.00589(12) O1 0.0521(10) 0.1224(17) 0.0703(12) -0.0172(11) 0.0059(8) -0.0219(11) O2 0.141(2) 0.0486(11) 0.1202(19) 0.0002(11) 0.0559(16) 0.0095(12) O3 0.0371(7) 0.0428(7) 0.0533(8) 0.0106(6) 0.0112(6) 0.0034(6) O4 0.0497(8) 0.0596(9) 0.0421(7) -0.0058(6) 0.0138(6) -0.0150(7) O5 0.0737(12) 0.1015(15) 0.0642(11) 0.0285(11) -0.0064(9) -0.0058(11) O6 0.0478(10) 0.0942(14) 0.0913(14) -0.0100(11) -0.0004(9) 0.0097(9) O7 0.0698(11) 0.0878(13) 0.0770(12) -0.0308(10) 0.0188(10) 0.0066(10) O8 0.142(2) 0.0788(13) 0.0931(15) -0.0136(12) 0.0644(15) 0.0106(14) O9 0.1231(19) 0.0722(14) 0.139(2) 0.0126(13) 0.0502(16) -0.0410(13) P1 0.0351(2) 0.0378(2) 0.0384(2) 0.00323(19) 0.00760(18) -0.00288(19) Se1 0.03548(11) 0.04391(12) 0.06441(14) 0.01279(9) 0.00983(9) 0.00179(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.364(5) . ? C1 C2 1.409(6) . ? C1 Fe1 2.086(3) . ? C1 H1 0.81(3) . ? C2 C3 1.398(5) . ? C2 Fe1 2.066(3) . ? C2 H2 0.67(3) . ? C3 C4 1.366(4) . ? C3 Fe1 2.086(3) . ? C3 H3 0.88(4) . ? C4 C5 1.375(4) . ? C4 Fe1 2.087(3) . ? C4 H4 0.88(3) . ? C5 Fe1 2.092(3) . ? C5 H5 0.95(3) . ? C6 O1 1.132(3) . ? C6 Fe1 1.767(2) . ? C7 O2 1.129(3) . ? C7 Fe1 1.772(3) . ? C8 O3 1.467(2) . ? C8 C10 1.483(4) . ? C8 C9 1.504(4) . ? C8 H8 0.90(3) . ? C9 H9A 0.86(4) . ? C9 H9B 1.02(4) . ? C9 H9C 0.98(4) . ? C10 H10A 0.98(3) . ? C10 H10B 0.96(3) . ? C10 H10C 1.00(3) . ? C11 O4 1.471(3) . ? C11 C13 1.495(5) . ? C11 C12 1.499(5) . ? C11 H11 0.96(3) . ? C12 H12A 0.94(4) . ? C12 H12B 1.07(4) . ? C12 H12C 0.92(4) . ? C13 H13A 0.88(4) . ? C13 H13B 0.98(4) . ? C13 H13C 0.99(4) . ? C14 O5 1.133(3) . ? C14 Cr1 1.908(2) . ? C15 O6 1.146(3) . ? C15 Cr1 1.880(2) . ? C16 O7 1.140(3) . ? C16 Cr1 1.901(2) . ? C17 O8 1.132(3) . ? C17 Cr1 1.890(3) . ? C18 O9 1.142(3) . ? C18 Cr1 1.841(2) . ? Cr1 Se1 2.5910(4) . ? Fe1 P1 2.2116(6) . ? O3 P1 1.5957(14) . ? O4 P1 1.6008(14) . ? P1 Se1 2.1810(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.2(3) . . ? C5 C1 Fe1 71.17(17) . . ? C2 C1 Fe1 69.37(17) . . ? C5 C1 H1 117(2) . . ? C2 C1 H1 135(2) . . ? Fe1 C1 H1 121(2) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 Fe1 71.14(17) . . ? C1 C2 Fe1 70.96(19) . . ? C3 C2 H2 117(3) . . ? C1 C2 H2 136(3) . . ? Fe1 C2 H2 125(3) . . ? C4 C3 C2 107.3(3) . . ? C4 C3 Fe1 70.92(16) . . ? C2 C3 Fe1 69.52(18) . . ? C4 C3 H3 123(3) . . ? C2 C3 H3 130(3) . . ? Fe1 C3 H3 124(3) . . ? C3 C4 C5 109.1(3) . . ? C3 C4 Fe1 70.87(16) . . ? C5 C4 Fe1 70.98(16) . . ? C3 C4 H4 124(2) . . ? C5 C4 H4 127(2) . . ? Fe1 C4 H4 122(2) . . ? C1 C5 C4 108.9(3) . . ? C1 C5 Fe1 70.71(16) . . ? C4 C5 Fe1 70.59(15) . . ? C1 C5 H5 125(2) . . ? C4 C5 H5 126(2) . . ? Fe1 C5 H5 122(2) . . ? O1 C6 Fe1 177.6(2) . . ? O2 C7 Fe1 179.1(2) . . ? O3 C8 C10 111.4(2) . . ? O3 C8 C9 106.0(2) . . ? C10 C8 C9 112.8(3) . . ? O3 C8 H8 109.4(16) . . ? C10 C8 H8 108.4(16) . . ? C9 C8 H8 108.7(15) . . ? C8 C9 H9A 113(3) . . ? C8 C9 H9B 101(2) . . ? H9A C9 H9B 116(4) . . ? C8 C9 H9C 107.4(19) . . ? H9A C9 H9C 112(3) . . ? H9B C9 H9C 107(3) . . ? C8 C10 H10A 109.3(19) . . ? C8 C10 H10B 111(2) . . ? H10A C10 H10B 114(3) . . ? C8 C10 H10C 103.0(18) . . ? H10A C10 H10C 111(3) . . ? H10B C10 H10C 107(3) . . ? O4 C11 C13 108.1(3) . . ? O4 C11 C12 107.1(2) . . ? C13 C11 C12 113.0(3) . . ? O4 C11 H11 108.2(17) . . ? C13 C11 H11 110.2(17) . . ? C12 C11 H11 110.1(17) . . ? C11 C12 H12A 109(2) . . ? C11 C12 H12B 107(2) . . ? H12A C12 H12B 106(3) . . ? C11 C12 H12C 106(3) . . ? H12A C12 H12C 114(4) . . ? H12B C12 H12C 115(3) . . ? C11 C13 H13A 109(3) . . ? C11 C13 H13B 110(2) . . ? H13A C13 H13B 109(3) . . ? C11 C13 H13C 115(2) . . ? H13A C13 H13C 107(3) . . ? H13B C13 H13C 108(3) . . ? O5 C14 Cr1 177.3(2) . . ? O6 C15 Cr1 177.4(2) . . ? O7 C16 Cr1 179.5(2) . . ? O8 C17 Cr1 179.0(3) . . ? O9 C18 Cr1 179.1(3) . . ? C18 Cr1 C15 88.84(11) . . ? C18 Cr1 C17 92.70(11) . . ? C15 Cr1 C17 91.02(11) . . ? C18 Cr1 C16 92.14(11) . . ? C15 Cr1 C16 90.73(10) . . ? C17 Cr1 C16 174.89(10) . . ? C18 Cr1 C14 90.24(11) . . ? C15 Cr1 C14 178.93(10) . . ? C17 Cr1 C14 88.48(11) . . ? C16 Cr1 C14 89.85(10) . . ? C18 Cr1 Se1 175.06(9) . . ? C15 Cr1 Se1 86.31(7) . . ? C17 Cr1 Se1 86.45(7) . . ? C16 Cr1 Se1 88.88(7) . . ? C14 Cr1 Se1 94.60(6) . . ? C6 Fe1 C7 93.33(12) . . ? C6 Fe1 C2 94.12(13) . . ? C7 Fe1 C2 154.00(15) . . ? C6 Fe1 C1 96.64(12) . . ? C7 Fe1 C1 114.65(15) . . ? C2 Fe1 C1 39.67(16) . . ? C6 Fe1 C3 126.07(12) . . ? C7 Fe1 C3 140.59(13) . . ? C2 Fe1 C3 39.34(15) . . ? C1 Fe1 C3 65.71(14) . . ? C6 Fe1 C4 158.46(12) . . ? C7 Fe1 C4 103.88(13) . . ? C2 Fe1 C4 64.83(14) . . ? C1 Fe1 C4 64.57(13) . . ? C3 Fe1 C4 38.21(12) . . ? C6 Fe1 C5 129.97(13) . . ? C7 Fe1 C5 91.44(13) . . ? C2 Fe1 C5 64.93(15) . . ? C1 Fe1 C5 38.12(14) . . ? C3 Fe1 C5 64.60(12) . . ? C4 Fe1 C5 38.43(12) . . ? C6 Fe1 P1 93.20(7) . . ? C7 Fe1 P1 88.74(8) . . ? C2 Fe1 P1 115.63(14) . . ? C1 Fe1 P1 153.89(12) . . ? C3 Fe1 P1 89.00(8) . . ? C4 Fe1 P1 99.93(9) . . ? C5 Fe1 P1 136.71(10) . . ? C8 O3 P1 125.71(13) . . ? C11 O4 P1 125.01(13) . . ? O3 P1 O4 106.44(8) . . ? O3 P1 Se1 104.53(5) . . ? O4 P1 Se1 110.66(6) . . ? O3 P1 Fe1 115.13(6) . . ? O4 P1 Fe1 106.82(6) . . ? Se1 P1 Fe1 113.09(2) . . ? P1 Se1 Cr1 112.194(16) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.79 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.444 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.053 data_2 _database_code_depnum_ccdc_archive 'CCDC 908779' #TrackingRef 'M-Se-P-Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H19 Fe O9 P Se W' _chemical_formula_weight 728.96 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' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3498(6) _cell_length_b 18.9176(10) _cell_length_c 12.7083(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.344(2) _cell_angle_gamma 90.00 _cell_volume 2421.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7549 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 6.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2648 _exptl_absorpt_correction_T_max 0.5149 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18814 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6013 _reflns_number_gt 5077 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6013 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1165(5) 0.1960(3) 1.0701(3) 0.0957(18) Uani 1 1 d . . . C2 C 0.1157(5) 0.1260(3) 1.0288(3) 0.0904(16) Uani 1 1 d . . . C3 C 0.2421(4) 0.11328(19) 1.0138(3) 0.0672(9) Uani 1 1 d . . . C4 C 0.3169(3) 0.1721(2) 1.0424(3) 0.0698(9) Uani 1 1 d . . . C5 C 0.2421(5) 0.2233(2) 1.0765(3) 0.0822(11) Uani 1 1 d . . . C6 C -0.0114(3) 0.20308(16) 0.8427(2) 0.0528(7) Uani 1 1 d . . . C7 C 0.1970(3) 0.28021(17) 0.8698(3) 0.0621(8) Uani 1 1 d . . . C8 C 0.0523(3) 0.03486(16) 0.7600(2) 0.0519(7) Uani 1 1 d . . . C9 C 0.0791(4) -0.0422(2) 0.7877(4) 0.0761(10) Uani 1 1 d . . . C10 C -0.0450(4) 0.0449(3) 0.6546(3) 0.0788(11) Uani 1 1 d . . . C11 C 0.1971(3) 0.19388(19) 0.5724(2) 0.0643(9) Uani 1 1 d . . . C12 C 0.2381(6) 0.2690(3) 0.5609(5) 0.0980(14) Uani 1 1 d . . . C13 C 0.0885(5) 0.1699(3) 0.4796(3) 0.0877(12) Uani 1 1 d . . . C14 C 0.3543(3) 0.00631(16) 0.6227(2) 0.0524(6) Uani 1 1 d . . . C15 C 0.6963(3) 0.04824(16) 0.8427(2) 0.0534(7) Uani 1 1 d . . . C16 C 0.4539(3) -0.02474(14) 0.8471(3) 0.0520(7) Uani 1 1 d . . . C17 C 0.5857(3) 0.08666(17) 0.6202(3) 0.0616(7) Uani 1 1 d . . . C18 C 0.6072(3) -0.05762(18) 0.6917(3) 0.0663(8) Uani 1 1 d . . . Fe3 Fe 0.15502(3) 0.196616(19) 0.91555(3) 0.04207(8) Uani 1 1 d . . . H1 H 0.065(5) 0.218(2) 1.080(4) 0.107(17) Uiso 1 1 d . . . H2 H 0.060(5) 0.101(3) 1.032(4) 0.14(2) Uiso 1 1 d . . . H3 H 0.279(4) 0.072(2) 0.990(3) 0.093(12) Uiso 1 1 d . . . H4 H 0.406(4) 0.174(2) 1.028(3) 0.101(13) Uiso 1 1 d . . . H5 H 0.276(4) 0.272(2) 1.102(3) 0.093(12) Uiso 1 1 d . . . H8 H 0.023(2) 0.0599(14) 0.820(2) 0.043(7) Uiso 1 1 d . . . H9A H 0.001(4) -0.069(2) 0.792(3) 0.107(14) Uiso 1 1 d . . . H9B H 0.112(4) -0.061(2) 0.727(3) 0.100(14) Uiso 1 1 d . . . H9C H 0.147(4) -0.0447(18) 0.865(3) 0.088(12) Uiso 1 1 d . . . H10A H -0.007(4) 0.0243(18) 0.601(3) 0.086(13) Uiso 1 1 d . . . H10B H -0.127(4) 0.0212(19) 0.662(3) 0.095(13) Uiso 1 1 d . . . H10C H -0.061(3) 0.0948(18) 0.637(2) 0.062(10) Uiso 1 1 d . . . H11 H 0.271(3) 0.1641(16) 0.580(2) 0.061(9) Uiso 1 1 d . . . H12A H 0.297(5) 0.287(3) 0.624(4) 0.13(2) Uiso 1 1 d . . . H12B H 0.285(4) 0.273(2) 0.498(4) 0.114(14) Uiso 1 1 d . . . H12C H 0.153(5) 0.300(2) 0.557(3) 0.105(14) Uiso 1 1 d . . . H13A H 0.067(4) 0.121(3) 0.491(3) 0.116(17) Uiso 1 1 d . . . H13B H 0.112(4) 0.179(2) 0.414(4) 0.112(15) Uiso 1 1 d . . . H13C H -0.007(5) 0.198(2) 0.472(4) 0.120(15) Uiso 1 1 d . . . O1 O -0.1205(2) 0.20665(15) 0.79968(19) 0.0811(7) Uani 1 1 d . . . O2 O 0.2242(3) 0.33371(13) 0.8410(2) 0.0947(9) Uani 1 1 d . . . O3 O 0.18113(15) 0.06602(9) 0.75740(14) 0.0433(4) Uani 1 1 d . . . O4 O 0.14796(17) 0.18917(10) 0.67211(14) 0.0495(4) Uani 1 1 d . . . O5 O 0.2606(2) -0.00675(15) 0.5597(2) 0.0847(7) Uani 1 1 d . . . O6 O 0.7951(2) 0.05841(14) 0.9037(2) 0.0810(7) Uani 1 1 d . . . O7 O 0.4132(2) -0.05409(14) 0.9106(2) 0.0785(7) Uani 1 1 d . . . O8 O 0.6174(3) 0.12040(15) 0.5561(2) 0.1016(9) Uani 1 1 d . . . O9 O 0.6553(3) -0.10818(15) 0.6674(3) 0.1127(10) Uani 1 1 d . . . P1 P 0.21979(6) 0.14739(3) 0.77867(5) 0.03717(13) Uani 1 1 d . . . Se1 Se 0.43445(2) 0.150270(14) 0.79885(2) 0.04862(7) Uani 1 1 d . . . W1 W 0.525724(9) 0.028242(5) 0.733341(8) 0.04048(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.091(3) 0.161(5) 0.0387(17) 0.011(2) 0.0223(19) 0.056(3) C2 0.092(3) 0.125(4) 0.0458(19) 0.030(2) -0.0015(19) -0.041(3) C3 0.092(3) 0.060(2) 0.0453(16) 0.0085(15) 0.0078(16) 0.0115(19) C4 0.0564(19) 0.091(3) 0.0538(18) 0.0071(17) -0.0043(15) 0.0088(18) C5 0.103(3) 0.083(3) 0.0482(19) -0.0140(18) -0.0088(19) 0.010(2) C6 0.0526(15) 0.0648(18) 0.0421(14) 0.0032(13) 0.0134(12) 0.0152(13) C7 0.078(2) 0.0519(19) 0.0606(18) -0.0101(15) 0.0256(16) 0.0065(15) C8 0.0398(13) 0.0623(19) 0.0550(16) -0.0132(14) 0.0140(12) -0.0130(12) C9 0.071(2) 0.069(2) 0.090(3) 0.001(2) 0.021(2) -0.0251(18) C10 0.0521(19) 0.105(3) 0.071(2) 0.000(2) -0.0014(17) -0.020(2) C11 0.0657(19) 0.084(2) 0.0472(16) 0.0134(15) 0.0222(14) 0.0282(17) C12 0.092(3) 0.118(4) 0.094(3) 0.028(3) 0.042(3) -0.016(3) C13 0.118(4) 0.096(3) 0.046(2) 0.004(2) 0.013(2) 0.010(3) C14 0.0562(16) 0.0518(16) 0.0489(15) -0.0106(13) 0.0115(13) 0.0060(13) C15 0.0426(14) 0.0547(16) 0.0653(18) 0.0060(14) 0.0176(13) 0.0009(12) C16 0.0425(14) 0.0503(17) 0.0602(17) 0.0093(13) 0.0057(12) 0.0014(11) C17 0.0748(19) 0.0544(18) 0.0617(18) -0.0023(15) 0.0285(16) 0.0028(15) C18 0.0656(19) 0.0560(19) 0.082(2) -0.0004(16) 0.0264(17) 0.0146(15) Fe3 0.04474(19) 0.0449(2) 0.03624(18) -0.00385(15) 0.00861(14) 0.00690(15) O1 0.0516(13) 0.120(2) 0.0684(14) 0.0161(14) 0.0063(11) 0.0227(12) O2 0.138(2) 0.0469(14) 0.113(2) -0.0001(13) 0.0559(19) -0.0108(14) O3 0.0352(8) 0.0424(10) 0.0533(10) -0.0106(8) 0.0125(7) -0.0028(7) O4 0.0483(10) 0.0619(12) 0.0396(9) 0.0054(8) 0.0131(8) 0.0154(8) O5 0.0715(15) 0.1035(19) 0.0675(15) -0.0343(14) -0.0078(12) 0.0066(14) O6 0.0460(12) 0.1021(18) 0.0868(17) 0.0085(14) -0.0011(11) -0.0135(12) O7 0.0682(14) 0.0939(17) 0.0742(16) 0.0345(13) 0.0184(12) -0.0086(12) O8 0.162(3) 0.0771(17) 0.0857(18) 0.0121(15) 0.0695(19) -0.0160(17) O9 0.127(2) 0.0751(19) 0.145(3) -0.0160(18) 0.050(2) 0.0425(17) P1 0.0352(3) 0.0383(3) 0.0376(3) -0.0038(2) 0.0076(2) 0.0034(2) Se1 0.03513(12) 0.04394(15) 0.06592(17) -0.01388(12) 0.00987(12) -0.00201(10) W1 0.03756(6) 0.03989(6) 0.04523(7) 0.00017(4) 0.01210(4) 0.00335(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.383(7) . ? C1 C2 1.424(7) . ? C1 Fe3 2.093(4) . ? C1 H1 0.72(5) . ? C2 C3 1.386(6) . ? C2 Fe3 2.072(4) . ? C2 H2 0.75(5) . ? C3 C4 1.356(5) . ? C3 Fe3 2.083(3) . ? C3 H3 0.95(4) . ? C4 C5 1.371(5) . ? C4 Fe3 2.092(3) . ? C4 H4 0.98(4) . ? C5 Fe3 2.098(3) . ? C5 H5 1.01(4) . ? C6 O1 1.137(3) . ? C6 Fe3 1.762(3) . ? C7 O2 1.133(4) . ? C7 Fe3 1.773(4) . ? C8 O3 1.465(3) . ? C8 C10 1.490(5) . ? C8 C9 1.511(5) . ? C8 H8 1.00(3) . ? C9 H9A 0.96(4) . ? C9 H9B 0.97(4) . ? C9 H9C 1.07(4) . ? C10 H10A 0.95(4) . ? C10 H10B 0.98(4) . ? C10 H10C 0.98(3) . ? C11 O4 1.473(3) . ? C11 C13 1.500(5) . ? C11 C12 1.501(6) . ? C11 H11 0.94(3) . ? C12 H12A 0.95(5) . ? C12 H12B 1.02(5) . ? C12 H12C 1.04(4) . ? C13 H13A 0.97(5) . ? C13 H13B 0.94(5) . ? C13 H13C 1.10(5) . ? C14 O5 1.134(3) . ? C14 W1 2.036(3) . ? C15 O6 1.148(3) . ? C15 W1 2.015(3) . ? C16 O7 1.138(4) . ? C16 W1 2.035(3) . ? C17 O8 1.141(4) . ? C17 W1 2.021(3) . ? C18 O9 1.153(4) . ? C18 W1 1.959(3) . ? Fe3 P1 2.2092(7) . ? O3 P1 1.5977(17) . ? O4 P1 1.5958(18) . ? P1 Se1 2.1775(6) . ? Se1 W1 2.6977(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.1(4) . . ? C5 C1 Fe3 70.9(2) . . ? C2 C1 Fe3 69.2(2) . . ? C5 C1 H1 120(4) . . ? C2 C1 H1 133(4) . . ? Fe3 C1 H1 118(4) . . ? C3 C2 C1 106.7(4) . . ? C3 C2 Fe3 70.9(2) . . ? C1 C2 Fe3 70.8(2) . . ? C3 C2 H2 131(4) . . ? C1 C2 H2 120(4) . . ? Fe3 C2 H2 136(4) . . ? C4 C3 C2 108.6(4) . . ? C4 C3 Fe3 71.39(19) . . ? C2 C3 Fe3 70.1(2) . . ? C4 C3 H3 121(2) . . ? C2 C3 H3 130(2) . . ? Fe3 C3 H3 125(2) . . ? C3 C4 C5 109.6(4) . . ? C3 C4 Fe3 70.69(19) . . ? C5 C4 Fe3 71.15(19) . . ? C3 C4 H4 119(2) . . ? C5 C4 H4 131(2) . . ? Fe3 C4 H4 118(2) . . ? C4 C5 C1 108.0(4) . . ? C4 C5 Fe3 70.64(19) . . ? C1 C5 Fe3 70.5(2) . . ? C4 C5 H5 124(2) . . ? C1 C5 H5 128(2) . . ? Fe3 C5 H5 125(2) . . ? O1 C6 Fe3 177.0(3) . . ? O2 C7 Fe3 179.7(4) . . ? O3 C8 C10 111.0(3) . . ? O3 C8 C9 105.9(3) . . ? C10 C8 C9 112.4(3) . . ? O3 C8 H8 105.4(15) . . ? C10 C8 H8 111.2(15) . . ? C9 C8 H8 110.5(15) . . ? C8 C9 H9A 114(3) . . ? C8 C9 H9B 104(2) . . ? H9A C9 H9B 108(4) . . ? C8 C9 H9C 107.6(19) . . ? H9A C9 H9C 108(3) . . ? H9B C9 H9C 116(3) . . ? C8 C10 H10A 107(2) . . ? C8 C10 H10B 106(2) . . ? H10A C10 H10B 113(3) . . ? C8 C10 H10C 112.0(18) . . ? H10A C10 H10C 108(3) . . ? H10B C10 H10C 111(3) . . ? O4 C11 C13 108.3(3) . . ? O4 C11 C12 107.6(3) . . ? C13 C11 C12 112.8(4) . . ? O4 C11 H11 108.1(18) . . ? C13 C11 H11 110.3(18) . . ? C12 C11 H11 109.6(19) . . ? C11 C12 H12A 114(3) . . ? C11 C12 H12B 110(3) . . ? H12A C12 H12B 108(4) . . ? C11 C12 H12C 106(2) . . ? H12A C12 H12C 102(4) . . ? H12B C12 H12C 118(3) . . ? C11 C13 H13A 109(3) . . ? C11 C13 H13B 110(3) . . ? H13A C13 H13B 116(4) . . ? C11 C13 H13C 115(2) . . ? H13A C13 H13C 103(4) . . ? H13B C13 H13C 105(3) . . ? O5 C14 W1 178.4(3) . . ? O6 C15 W1 178.3(3) . . ? O7 C16 W1 179.6(3) . . ? O8 C17 W1 178.7(3) . . ? O9 C18 W1 179.8(4) . . ? C6 Fe3 C7 92.83(15) . . ? C6 Fe3 C2 94.87(16) . . ? C7 Fe3 C2 154.84(18) . . ? C6 Fe3 C3 127.09(15) . . ? C7 Fe3 C3 140.07(16) . . ? C2 Fe3 C3 38.98(17) . . ? C6 Fe3 C4 158.86(15) . . ? C7 Fe3 C4 103.73(16) . . ? C2 Fe3 C4 64.68(16) . . ? C3 Fe3 C4 37.92(14) . . ? C6 Fe3 C1 96.83(16) . . ? C7 Fe3 C1 115.3(2) . . ? C2 Fe3 C1 40.0(2) . . ? C3 Fe3 C1 65.35(17) . . ? C4 Fe3 C1 64.36(17) . . ? C6 Fe3 C5 130.07(16) . . ? C7 Fe3 C5 91.31(17) . . ? C2 Fe3 C5 65.57(18) . . ? C3 Fe3 C5 64.42(15) . . ? C4 Fe3 C5 38.21(15) . . ? C1 Fe3 C5 38.54(19) . . ? C6 Fe3 P1 93.04(9) . . ? C7 Fe3 P1 88.63(10) . . ? C2 Fe3 P1 114.78(17) . . ? C3 Fe3 P1 89.13(11) . . ? C4 Fe3 P1 100.30(11) . . ? C1 Fe3 P1 153.49(16) . . ? C5 Fe3 P1 136.81(13) . . ? C8 O3 P1 125.28(16) . . ? C11 O4 P1 125.03(16) . . ? O4 P1 O3 106.51(10) . . ? O4 P1 Se1 110.51(7) . . ? O3 P1 Se1 104.65(6) . . ? O4 P1 Fe3 107.02(7) . . ? O3 P1 Fe3 115.45(7) . . ? Se1 P1 Fe3 112.55(3) . . ? P1 Se1 W1 111.262(19) . . ? C18 W1 C15 88.77(13) . . ? C18 W1 C17 92.23(13) . . ? C15 W1 C17 91.36(12) . . ? C18 W1 C16 91.97(13) . . ? C15 W1 C16 90.48(11) . . ? C17 W1 C16 175.44(11) . . ? C18 W1 C14 90.30(13) . . ? C15 W1 C14 179.03(11) . . ? C17 W1 C14 88.97(13) . . ? C16 W1 C14 89.26(12) . . ? C18 W1 Se1 175.13(10) . . ? C15 W1 Se1 86.56(8) . . ? C17 W1 Se1 86.47(9) . . ? C16 W1 Se1 89.48(8) . . ? C14 W1 Se1 94.37(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.544 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.072 data_3 _database_code_depnum_ccdc_archive 'CCDC 908780' #TrackingRef 'M-Se-P-Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 Cl Fe O4 P Pd0.50 Se' _chemical_formula_weight 493.71 _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' 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' 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' Se Se -0.0929 2.2259 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0946(10) _cell_length_b 8.5615(6) _cell_length_c 15.8903(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.242(2) _cell_angle_gamma 90.00 _cell_volume 1900.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2335 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 20.23 _exptl_crystal_description plane _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 3.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5495 _exptl_absorpt_correction_T_max 0.9351 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20348 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4752 _reflns_number_gt 2455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4752 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 0.0000 0.5000 0.0000 0.0507(2) Uani 1 2 d S . . Se1 Se 0.01916(6) 0.57551(8) 0.15295(5) 0.0738(3) Uani 1 1 d . . . Fe1 Fe 0.04819(6) 0.14733(9) 0.23753(6) 0.0547(3) Uani 1 1 d . . . Cl1 Cl 0.09620(14) 0.7121(2) 0.00834(12) 0.0786(5) Uani 1 1 d . . . P1 P -0.01412(11) 0.38378(17) 0.22796(10) 0.0490(4) Uani 1 1 d . . . O1 O -0.1256(3) 0.3605(5) 0.1996(3) 0.0610(11) Uani 1 1 d . . . O2 O 0.0128(3) 0.4573(5) 0.3272(3) 0.0676(12) Uani 1 1 d . . . O3 O 0.0075(4) 0.0942(7) 0.4008(4) 0.1038(19) Uani 1 1 d . . . O4 O -0.1282(4) 0.0021(6) 0.1196(4) 0.0925(16) Uani 1 1 d . . . C1 C 0.0216(5) 0.1155(8) 0.3360(5) 0.0682(18) Uani 1 1 d . . . C2 C -0.0612(5) 0.0652(7) 0.1636(5) 0.0631(17) Uani 1 1 d . . . C3 C 0.1419(7) -0.0280(10) 0.2349(10) 0.115(4) Uani 1 1 d . . . H3 H 0.1320 -0.1402 0.2400 0.139 Uiso 1 1 calc R . . C4 C 0.1147(6) 0.0543(17) 0.1558(8) 0.115(4) Uani 1 1 d . . . H4 H 0.0817 0.0107 0.0948 0.138 Uiso 1 1 calc R . . C5 C 0.1414(7) 0.2032(13) 0.1743(9) 0.104(3) Uani 1 1 d . . . H5 H 0.1326 0.2866 0.1296 0.125 Uiso 1 1 calc R . . C6 C 0.1885(5) 0.2169(10) 0.2694(8) 0.094(3) Uani 1 1 d . . . H6 H 0.2197 0.3101 0.3035 0.113 Uiso 1 1 calc R . . C7 C 0.1881(5) 0.0674(15) 0.3039(7) 0.106(3) Uani 1 1 d . . . H7 H 0.2174 0.0373 0.3681 0.128 Uiso 1 1 calc R . . C8 C -0.1916(5) 0.4927(9) 0.1875(6) 0.086(2) Uani 1 1 d . . . H8 H -0.1565 0.5913 0.1953 0.103 Uiso 1 1 calc R . . C9 C -0.2641(8) 0.4812(16) 0.0929(8) 0.181(6) Uani 1 1 d . . . H9A H -0.2329 0.4907 0.0505 0.272 Uiso 1 1 calc R . . H9B H -0.3103 0.5634 0.0825 0.272 Uiso 1 1 calc R . . H9C H -0.2959 0.3819 0.0847 0.272 Uiso 1 1 calc R . . C10 C -0.2344(7) 0.4803(14) 0.2554(8) 0.134(4) Uani 1 1 d . . . H10A H -0.2699 0.3845 0.2465 0.201 Uiso 1 1 calc R . . H10B H -0.2767 0.5670 0.2493 0.201 Uiso 1 1 calc R . . H10C H -0.1849 0.4811 0.3151 0.201 Uiso 1 1 calc R . . C11 C 0.0922(7) 0.5571(12) 0.3775(5) 0.115(3) Uani 1 1 d . . . H11 H 0.1317 0.5750 0.3417 0.138 Uiso 1 1 calc R . . C12 C 0.0615(12) 0.7027(13) 0.3993(9) 0.227(9) Uani 1 1 d . . . H12A H 0.0194 0.7522 0.3445 0.340 Uiso 1 1 calc R . . H12B H 0.1161 0.7683 0.4286 0.340 Uiso 1 1 calc R . . H12C H 0.0282 0.6861 0.4394 0.340 Uiso 1 1 calc R . . C13 C 0.1497(9) 0.4651(17) 0.4631(7) 0.200(7) Uani 1 1 d . . . H13A H 0.2129 0.5087 0.4902 0.300 Uiso 1 1 calc R . . H13B H 0.1542 0.3579 0.4473 0.300 Uiso 1 1 calc R . . H13C H 0.1184 0.4708 0.5055 0.300 Uiso 1 1 calc R . . _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 0.0657(4) 0.0434(3) 0.0392(4) 0.0016(3) 0.0155(3) -0.0042(3) Se1 0.1263(7) 0.0489(4) 0.0503(4) -0.0074(3) 0.0381(4) -0.0231(4) Fe1 0.0447(5) 0.0480(5) 0.0665(6) -0.0025(4) 0.0157(4) -0.0009(4) Cl1 0.1050(14) 0.0706(10) 0.0582(10) -0.0075(8) 0.0286(10) -0.0348(10) P1 0.0576(9) 0.0425(7) 0.0467(9) -0.0002(6) 0.0195(7) -0.0001(7) O1 0.052(2) 0.063(2) 0.064(3) 0.001(2) 0.017(2) 0.014(2) O2 0.091(3) 0.059(3) 0.047(2) -0.005(2) 0.021(2) -0.010(2) O3 0.117(5) 0.112(5) 0.093(4) 0.025(4) 0.051(4) 0.002(4) O4 0.067(3) 0.088(4) 0.102(4) 0.000(3) 0.009(3) -0.027(3) C1 0.060(4) 0.063(4) 0.078(5) 0.009(4) 0.023(4) 0.001(3) C2 0.054(4) 0.052(3) 0.075(5) 0.003(3) 0.016(3) -0.005(3) C3 0.062(6) 0.073(6) 0.218(14) -0.039(8) 0.062(8) -0.003(4) C4 0.071(6) 0.169(11) 0.096(7) -0.060(8) 0.021(5) 0.015(7) C5 0.084(6) 0.118(8) 0.142(10) 0.054(7) 0.079(7) 0.044(6) C6 0.056(5) 0.081(6) 0.158(10) -0.035(6) 0.054(6) -0.019(4) C7 0.046(4) 0.151(9) 0.114(8) 0.036(7) 0.020(5) 0.023(5) C8 0.076(5) 0.077(5) 0.105(6) 0.008(5) 0.036(5) 0.033(4) C9 0.149(10) 0.258(15) 0.103(8) 0.006(9) 0.010(7) 0.133(11) C10 0.109(8) 0.174(10) 0.137(9) -0.014(8) 0.066(7) 0.050(7) C11 0.133(8) 0.153(9) 0.055(5) -0.016(5) 0.032(5) -0.068(7) C12 0.33(2) 0.085(7) 0.175(14) -0.066(9) -0.002(13) -0.011(11) C13 0.191(14) 0.224(15) 0.098(9) -0.039(10) -0.044(9) 0.031(12) _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. ; _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 Cl1 2.2973(16) . ? Pd Cl1 2.2973(16) 3_565 ? Pd Se1 2.4241(7) 3_565 ? Pd Se1 2.4242(7) . ? Se1 P1 2.1956(16) . ? Fe1 C2 1.770(7) . ? Fe1 C1 1.777(8) . ? Fe1 C6 2.070(7) . ? Fe1 C5 2.071(8) . ? Fe1 C3 2.074(8) . ? Fe1 C4 2.078(9) . ? Fe1 C7 2.087(7) . ? Fe1 P1 2.2130(16) . ? P1 O1 1.582(4) . ? P1 O2 1.601(4) . ? O1 C8 1.471(7) . ? O2 C11 1.442(9) . ? O3 C1 1.141(8) . ? O4 C2 1.126(7) . ? C3 C7 1.333(13) . ? C3 C4 1.362(14) . ? C4 C5 1.335(13) . ? C5 C6 1.411(13) . ? C6 C7 1.393(12) . ? C8 C10 1.456(11) . ? C8 C9 1.491(13) . ? C11 C12 1.417(15) . ? C11 C13 1.526(13) . ? _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 Cl1 Pd Cl1 180.0 . 3_565 ? Cl1 Pd Se1 95.83(5) . 3_565 ? Cl1 Pd Se1 84.17(5) 3_565 3_565 ? Cl1 Pd Se1 84.17(5) . . ? Cl1 Pd Se1 95.83(5) 3_565 . ? Se1 Pd Se1 180.0 3_565 . ? P1 Se1 Pd 112.33(5) . . ? C2 Fe1 C1 93.4(3) . . ? C2 Fe1 C6 152.6(4) . . ? C1 Fe1 C6 112.3(4) . . ? C2 Fe1 C5 113.8(5) . . ? C1 Fe1 C5 152.1(4) . . ? C6 Fe1 C5 39.9(4) . . ? C2 Fe1 C3 99.9(4) . . ? C1 Fe1 C3 106.8(4) . . ? C6 Fe1 C3 64.6(3) . . ? C5 Fe1 C3 64.1(4) . . ? C2 Fe1 C4 89.1(4) . . ? C1 Fe1 C4 144.6(5) . . ? C6 Fe1 C4 64.6(3) . . ? C5 Fe1 C4 37.6(4) . . ? C3 Fe1 C4 38.3(4) . . ? C2 Fe1 C7 135.8(4) . . ? C1 Fe1 C7 91.6(3) . . ? C6 Fe1 C7 39.2(3) . . ? C5 Fe1 C7 65.0(4) . . ? C3 Fe1 C7 37.4(4) . . ? C4 Fe1 C7 63.5(4) . . ? C2 Fe1 P1 93.0(2) . . ? C1 Fe1 P1 88.2(2) . . ? C6 Fe1 P1 97.0(3) . . ? C5 Fe1 P1 96.0(3) . . ? C3 Fe1 P1 159.4(3) . . ? C4 Fe1 P1 126.9(4) . . ? C7 Fe1 P1 131.1(4) . . ? O1 P1 O2 100.1(2) . . ? O1 P1 Se1 112.16(17) . . ? O2 P1 Se1 102.46(16) . . ? O1 P1 Fe1 106.45(16) . . ? O2 P1 Fe1 110.41(18) . . ? Se1 P1 Fe1 122.86(8) . . ? C8 O1 P1 122.3(4) . . ? C11 O2 P1 128.9(5) . . ? O3 C1 Fe1 177.9(7) . . ? O4 C2 Fe1 174.6(6) . . ? C7 C3 C4 108.9(9) . . ? C7 C3 Fe1 71.9(5) . . ? C4 C3 Fe1 71.0(5) . . ? C5 C4 C3 109.3(9) . . ? C5 C4 Fe1 70.9(5) . . ? C3 C4 Fe1 70.7(6) . . ? C4 C5 C6 107.6(9) . . ? C4 C5 Fe1 71.5(6) . . ? C6 C5 Fe1 70.0(4) . . ? C7 C6 C5 105.7(8) . . ? C7 C6 Fe1 71.1(4) . . ? C5 C6 Fe1 70.1(4) . . ? C3 C7 C6 108.5(9) . . ? C3 C7 Fe1 70.8(5) . . ? C6 C7 Fe1 69.7(4) . . ? C10 C8 O1 108.4(7) . . ? C10 C8 C9 112.3(9) . . ? O1 C8 C9 106.5(7) . . ? C12 C11 O2 112.2(10) . . ? C12 C11 C13 111.4(10) . . ? O2 C11 C13 105.2(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.426 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.114 data_4 _database_code_depnum_ccdc_archive 'CCDC 908781' #TrackingRef 'M-Se-P-Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Cl2 Fe2 O8 P2 Pt Se2' _chemical_formula_weight 1076.11 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' 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' 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' Se Se -0.0929 2.2259 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.149(2) _cell_length_b 8.5423(12) _cell_length_c 15.876(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.924(3) _cell_angle_gamma 90.00 _cell_volume 1905.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2482 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 19.61 _exptl_crystal_description plane _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 6.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3526 _exptl_absorpt_correction_T_max 0.5054 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28089 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.42 _reflns_number_total 4766 _reflns_number_gt 2291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4766 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1473 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6411(10) -0.020(2) 0.7257(13) 0.123(3) Uani 1 1 d . . . H1 H 0.6304 -0.1323 0.7311 0.148 Uiso 1 1 calc R . . C2 C 0.6118(10) 0.056(2) 0.6460(14) 0.123(3) Uani 1 1 d . . . H2 H 0.5818 0.0131 0.5845 0.148 Uiso 1 1 calc R . . C3 C 0.6436(9) 0.220(2) 0.6746(12) 0.123(3) Uani 1 1 d . . . H3 H 0.6376 0.3095 0.6344 0.148 Uiso 1 1 calc R . . C4 C 0.6879(9) 0.219(2) 0.7672(13) 0.123(3) Uani 1 1 d . . . H4 H 0.7182 0.3089 0.8050 0.148 Uiso 1 1 calc R . . C5 C 0.6864(10) 0.072(2) 0.7971(14) 0.123(3) Uani 1 1 d . . . H5 H 0.7147 0.0374 0.8605 0.148 Uiso 1 1 calc R . . C6 C 0.4372(8) 0.0679(14) 0.6568(9) 0.078(3) Uani 1 1 d . . . C7 C 0.5218(8) 0.1156(15) 0.8297(9) 0.086(4) Uani 1 1 d . . . C8 C 0.3046(9) 0.4880(15) 0.6878(10) 0.095(4) Uani 1 1 d . . . H8 H 0.3389 0.5877 0.6966 0.115 Uiso 1 1 calc R . . C9 C 0.2323(15) 0.485(3) 0.5965(14) 0.226(15) Uani 1 1 d . . . H9A H 0.2621 0.4676 0.5534 0.339 Uiso 1 1 calc R . . H9B H 0.1993 0.5835 0.5838 0.339 Uiso 1 1 calc R . . H9C H 0.1879 0.4024 0.5919 0.339 Uiso 1 1 calc R . . C10 C 0.2662(14) 0.469(3) 0.7634(17) 0.165(9) Uani 1 1 d . . . H10A H 0.2049 0.5176 0.7457 0.248 Uiso 1 1 calc R . . H10B H 0.3092 0.5167 0.8179 0.248 Uiso 1 1 calc R . . H10C H 0.2603 0.3592 0.7742 0.248 Uiso 1 1 calc R . . C11 C 0.5932(12) 0.548(2) 0.8754(9) 0.114(5) Uani 1 1 d . . . H11 H 0.6321 0.5665 0.8390 0.137 Uiso 1 1 calc R . . C12 C 0.6472(15) 0.447(3) 0.9562(12) 0.192(11) Uani 1 1 d . . . H12A H 0.7136 0.4729 0.9777 0.287 Uiso 1 1 calc R . . H12B H 0.6388 0.3388 0.9387 0.287 Uiso 1 1 calc R . . H12C H 0.6236 0.4650 1.0037 0.287 Uiso 1 1 calc R . . C13 C 0.5639(17) 0.692(2) 0.8997(16) 0.234(15) Uani 1 1 d . . . H13A H 0.5150 0.7366 0.8476 0.351 Uiso 1 1 calc R . . H13B H 0.6172 0.7620 0.9213 0.351 Uiso 1 1 calc R . . H13C H 0.5395 0.6748 0.9467 0.351 Uiso 1 1 calc R . . Cl1 Cl 0.3941(3) 0.3001(4) 0.4876(2) 0.1012(11) Uani 1 1 d . . . Fe1 Fe 0.54649(10) 0.15167(17) 0.73111(11) 0.0677(4) Uani 1 1 d . . . O1 O 0.3708(6) 0.0017(10) 0.6144(7) 0.109(3) Uani 1 1 d . . . O2 O 0.5085(8) 0.0922(14) 0.8951(8) 0.127(4) Uani 1 1 d . . . O3 O 0.3731(4) 0.3593(8) 0.6999(5) 0.0728(19) Uani 1 1 d . . . O4 O 0.5102(6) 0.4594(8) 0.8238(5) 0.078(2) Uani 1 1 d . . . P1 P 0.48303(18) 0.3857(3) 0.72468(16) 0.0575(6) Uani 1 1 d . . . Pt Pt 0.5000 0.5000 0.5000 0.0646(2) Uani 1 2 d S . . Se1 Se 0.51040(11) 0.58231(15) 0.64903(7) 0.0898(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.073(4) 0.145(7) 0.159(7) 0.005(6) 0.052(5) 0.022(4) C2 0.073(4) 0.145(7) 0.159(7) 0.005(6) 0.052(5) 0.022(4) C3 0.073(4) 0.145(7) 0.159(7) 0.005(6) 0.052(5) 0.022(4) C4 0.073(4) 0.145(7) 0.159(7) 0.005(6) 0.052(5) 0.022(4) C5 0.073(4) 0.145(7) 0.159(7) 0.005(6) 0.052(5) 0.022(4) C6 0.060(7) 0.067(7) 0.106(9) -0.002(7) 0.029(6) -0.008(6) C7 0.077(8) 0.086(9) 0.089(9) 0.021(7) 0.024(7) -0.005(6) C8 0.081(8) 0.089(9) 0.107(10) 0.002(7) 0.024(8) 0.032(7) C9 0.19(2) 0.33(3) 0.106(14) 0.008(16) -0.001(13) 0.19(2) C10 0.125(14) 0.20(2) 0.20(2) 0.010(16) 0.099(15) 0.061(13) C11 0.124(12) 0.145(14) 0.071(9) -0.010(9) 0.033(9) -0.030(10) C12 0.173(19) 0.23(2) 0.097(13) -0.027(15) -0.030(12) 0.060(18) C13 0.25(3) 0.111(15) 0.22(3) -0.063(17) -0.05(2) 0.040(18) Cl1 0.133(3) 0.099(2) 0.0719(18) -0.0140(16) 0.0377(19) -0.051(2) Fe1 0.0504(8) 0.0627(9) 0.0828(10) -0.0038(8) 0.0166(7) -0.0018(6) O1 0.066(5) 0.107(7) 0.132(8) -0.017(6) 0.010(5) -0.029(5) O2 0.131(8) 0.140(9) 0.108(8) 0.054(7) 0.041(7) 0.014(7) O3 0.056(4) 0.074(5) 0.083(5) 0.001(4) 0.019(4) 0.015(3) O4 0.101(6) 0.071(5) 0.060(4) 0.000(3) 0.029(4) -0.011(4) P1 0.0612(15) 0.0542(15) 0.0534(14) 0.0015(11) 0.0173(12) -0.0014(12) Pt 0.0876(4) 0.0564(3) 0.0439(3) 0.0024(3) 0.0176(3) -0.0088(3) Se1 0.1550(12) 0.0615(7) 0.0561(6) -0.0066(5) 0.0432(7) -0.0255(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.34(2) . ? C1 C2 1.34(2) . ? C1 Fe1 2.076(15) . ? C1 H1 0.9800 . ? C2 C3 1.50(2) . ? C2 Fe1 2.114(17) . ? C2 H2 0.9800 . ? C3 C4 1.37(2) . ? C3 Fe1 2.071(16) . ? C3 H3 0.9800 . ? C4 C5 1.35(2) . ? C4 Fe1 2.080(15) . ? C4 H4 0.9800 . ? C5 Fe1 2.097(15) . ? C5 H5 0.9800 . ? C6 O1 1.131(13) . ? C6 Fe1 1.785(12) . ? C7 O2 1.146(15) . ? C7 Fe1 1.767(14) . ? C8 C9 1.45(2) . ? C8 O3 1.475(12) . ? C8 C10 1.53(2) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.41(2) . ? C11 O4 1.434(16) . ? C11 C12 1.51(2) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Cl1 Pt 2.301(3) . ? Fe1 P1 2.204(3) . ? O3 P1 1.577(7) . ? O4 P1 1.600(8) . ? P1 Se1 2.192(3) . ? Pt Cl1 2.301(3) 3_666 ? Pt Se1 2.4163(12) 3_666 ? Pt Se1 2.4164(12) . ? 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 C1 C2 114(2) . . ? C5 C1 Fe1 72.2(10) . . ? C2 C1 Fe1 72.9(10) . . ? C5 C1 H1 123.2 . . ? C2 C1 H1 123.2 . . ? Fe1 C1 H1 123.2 . . ? C1 C2 C3 102.2(19) . . ? C1 C2 Fe1 69.8(11) . . ? C3 C2 Fe1 67.5(9) . . ? C1 C2 H2 128.8 . . ? C3 C2 H2 128.8 . . ? Fe1 C2 H2 128.8 . . ? C4 C3 C2 107.0(19) . . ? C4 C3 Fe1 71.1(10) . . ? C2 C3 Fe1 70.6(10) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? Fe1 C3 H3 126.4 . . ? C5 C4 C3 109(2) . . ? C5 C4 Fe1 71.9(10) . . ? C3 C4 Fe1 70.4(9) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe1 C4 H4 125.7 . . ? C1 C5 C4 109(2) . . ? C1 C5 Fe1 70.4(10) . . ? C4 C5 Fe1 70.5(9) . . ? C1 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? Fe1 C5 H5 125.7 . . ? O1 C6 Fe1 173.3(12) . . ? O2 C7 Fe1 178.1(12) . . ? C9 C8 O3 110.4(12) . . ? C9 C8 C10 114.6(17) . . ? O3 C8 C10 105.8(12) . . ? C9 C8 H8 108.6 . . ? O3 C8 H8 108.6 . . ? C10 C8 H8 108.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 O4 108.5(16) . . ? C13 C11 C12 113.1(17) . . ? O4 C11 C12 105.4(15) . . ? C13 C11 H11 109.9 . . ? O4 C11 H11 109.9 . . ? C12 C11 H11 109.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 Fe1 C6 93.7(6) . . ? C7 Fe1 C3 148.4(6) . . ? C6 Fe1 C3 117.4(6) . . ? C7 Fe1 C1 106.9(7) . . ? C6 Fe1 C1 100.0(6) . . ? C3 Fe1 C1 64.4(7) . . ? C7 Fe1 C4 109.9(6) . . ? C6 Fe1 C4 153.9(7) . . ? C3 Fe1 C4 38.5(6) . . ? C1 Fe1 C4 63.3(7) . . ? C7 Fe1 C5 90.5(7) . . ? C6 Fe1 C5 135.6(7) . . ? C3 Fe1 C5 63.8(7) . . ? C1 Fe1 C5 37.4(6) . . ? C4 Fe1 C5 37.6(6) . . ? C7 Fe1 C2 143.4(7) . . ? C6 Fe1 C2 87.8(6) . . ? C3 Fe1 C2 41.9(6) . . ? C1 Fe1 C2 37.3(6) . . ? C4 Fe1 C2 66.6(7) . . ? C5 Fe1 C2 64.3(7) . . ? C7 Fe1 P1 88.1(4) . . ? C6 Fe1 P1 93.0(4) . . ? C3 Fe1 P1 95.4(5) . . ? C1 Fe1 P1 159.3(5) . . ? C4 Fe1 P1 98.6(5) . . ? C5 Fe1 P1 131.3(5) . . ? C2 Fe1 P1 128.5(5) . . ? C8 O3 P1 123.5(7) . . ? C11 O4 P1 128.2(8) . . ? O3 P1 O4 99.3(4) . . ? O3 P1 Se1 111.8(3) . . ? O4 P1 Se1 101.9(3) . . ? O3 P1 Fe1 106.4(3) . . ? O4 P1 Fe1 111.4(3) . . ? Se1 P1 Fe1 123.48(14) . . ? Cl1 Pt Cl1 180.00(15) . 3_666 ? Cl1 Pt Se1 84.93(8) . 3_666 ? Cl1 Pt Se1 95.07(8) 3_666 3_666 ? Cl1 Pt Se1 95.07(8) . . ? Cl1 Pt Se1 84.93(8) 3_666 . ? Se1 Pt Se1 180.0 3_666 . ? P1 Se1 Pt 110.92(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.674 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.186 data_5 _database_code_depnum_ccdc_archive 'CCDC 908782' #TrackingRef 'M-Se-P-Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Au4 Cl4 Fe2 O8 P2 Se2' _chemical_formula_weight 1739.79 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' 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' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.659(6) _cell_length_b 12.657(9) _cell_length_c 18.066(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.327(17) _cell_angle_gamma 90.00 _cell_volume 2179(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6352 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 16.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1332 _exptl_absorpt_correction_T_max 0.1964 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16477 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.23 _reflns_number_total 5359 _reflns_number_gt 4316 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+4.8210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5359 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0596 _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 Au1 Au 1.01135(2) 0.464126(17) 0.124824(13) 0.04320(7) Uani 1 1 d . . . Au2 Au 1.02080(3) 0.31781(2) -0.039001(13) 0.05005(8) Uani 1 1 d . . . C1 C 0.6788(7) 0.1747(4) -0.0694(3) 0.0454(13) Uani 1 1 d . . . H1 H 0.7815 0.1707 -0.0608 0.054 Uiso 1 1 calc R . . C2 C 0.6175(10) 0.0657(5) -0.0710(4) 0.075(2) Uani 1 1 d . . . H2A H 0.6621 0.0267 -0.0281 0.112 Uiso 1 1 calc R . . H2B H 0.6325 0.0301 -0.1159 0.112 Uiso 1 1 calc R . . H2C H 0.5186 0.0704 -0.0699 0.112 Uiso 1 1 calc R . . C3 C 0.6269(9) 0.2375(6) -0.1418(4) 0.074(2) Uani 1 1 d . . . H3A H 0.5274 0.2477 -0.1468 0.111 Uiso 1 1 calc R . . H3B H 0.6482 0.1989 -0.1843 0.111 Uiso 1 1 calc R . . H3C H 0.6730 0.3049 -0.1392 0.111 Uiso 1 1 calc R . . C4 C 0.9530(7) 0.1661(5) 0.1433(4) 0.0638(19) Uani 1 1 d . . . H4 H 0.9879 0.2362 0.1601 0.077 Uiso 1 1 calc R . . C5 C 1.0636(11) 0.1081(11) 0.1072(6) 0.137(5) Uani 1 1 d . . . H5A H 1.0357 0.0358 0.0982 0.206 Uiso 1 1 calc R . . H5B H 1.1521 0.1105 0.1402 0.206 Uiso 1 1 calc R . . H5C H 1.0726 0.1414 0.0604 0.206 Uiso 1 1 calc R . . C6 C 0.9165(10) 0.1052(7) 0.2078(4) 0.086(3) Uani 1 1 d . . . H6A H 0.8482 0.1436 0.2302 0.129 Uiso 1 1 calc R . . H6B H 0.9993 0.0947 0.2443 0.129 Uiso 1 1 calc R . . H6C H 0.8784 0.0378 0.1906 0.129 Uiso 1 1 calc R . . C7 C 0.7366(7) 0.3684(5) 0.2153(3) 0.0472(14) Uani 1 1 d . . . C8 C 0.5685(8) 0.4554(6) 0.1062(4) 0.0634(19) Uani 1 1 d . . . C9 C 0.4500(11) 0.3011(8) 0.2186(6) 0.097(3) Uani 1 1 d . . . H9 H 0.4405 0.3446 0.2624 0.116 Uiso 1 1 calc R . . C10 C 0.5351(10) 0.2127(8) 0.2196(5) 0.086(3) Uani 1 1 d . . . H10 H 0.5941 0.1818 0.2635 0.103 Uiso 1 1 calc R . . C11 C 0.5162(9) 0.1740(7) 0.1461(6) 0.083(3) Uani 1 1 d . . . H11 H 0.5612 0.1107 0.1296 0.100 Uiso 1 1 calc R . . C12 C 0.4200(8) 0.2386(8) 0.0999(5) 0.083(3) Uani 1 1 d . . . H12 H 0.3839 0.2283 0.0465 0.100 Uiso 1 1 calc R . . C13 C 0.3781(9) 0.3167(8) 0.1475(6) 0.092(3) Uani 1 1 d . . . H13 H 0.3093 0.3727 0.1323 0.111 Uiso 1 1 calc R . . Cl1 Cl 1.17390(19) 0.51703(15) 0.22441(9) 0.0634(4) Uani 1 1 d . . . Cl2 Cl 1.1871(2) 0.2262(2) -0.08971(12) 0.0922(7) Uani 1 1 d . . . Fe1 Fe 0.59572(8) 0.32700(7) 0.14627(5) 0.04291(19) Uani 1 1 d . . . O1 O 0.6304(4) 0.2321(3) -0.0074(2) 0.0444(9) Uani 1 1 d . . . O2 O 0.8290(4) 0.1768(3) 0.0847(2) 0.0458(9) Uani 1 1 d . . . O3 O 0.8238(5) 0.3968(4) 0.2621(3) 0.0702(14) Uani 1 1 d . . . O4 O 0.5478(8) 0.5381(5) 0.0819(4) 0.102(2) Uani 1 1 d . . . P1 P 0.72671(14) 0.27412(10) 0.06498(8) 0.0337(3) Uani 1 1 d . . . Se1 Se 0.84783(6) 0.40837(4) 0.01857(3) 0.04448(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.04621(13) 0.04023(12) 0.04448(13) -0.00162(9) 0.01135(10) -0.00789(9) Au2 0.05150(14) 0.05966(15) 0.03988(13) 0.00194(10) 0.01004(10) -0.00865(11) C1 0.052(3) 0.044(3) 0.040(3) -0.014(2) 0.009(3) -0.008(3) C2 0.103(6) 0.053(4) 0.075(5) -0.021(4) 0.032(5) -0.019(4) C3 0.097(6) 0.079(5) 0.044(4) -0.002(4) 0.004(4) -0.009(5) C4 0.056(4) 0.045(3) 0.084(5) 0.020(3) -0.007(4) 0.001(3) C5 0.084(7) 0.221(14) 0.118(8) 0.098(9) 0.048(6) 0.081(8) C6 0.103(7) 0.090(6) 0.065(5) 0.026(5) 0.014(5) 0.015(5) C7 0.050(3) 0.052(3) 0.042(3) -0.005(3) 0.016(3) -0.007(3) C8 0.072(5) 0.061(4) 0.057(4) -0.007(3) 0.009(4) 0.024(4) C9 0.096(7) 0.118(8) 0.094(7) -0.051(6) 0.071(6) -0.041(6) C10 0.099(7) 0.094(6) 0.072(6) -0.006(5) 0.036(5) -0.053(6) C11 0.074(5) 0.072(5) 0.115(7) -0.035(5) 0.049(5) -0.046(4) C12 0.046(4) 0.146(8) 0.059(5) -0.032(5) 0.010(4) -0.041(5) C13 0.050(4) 0.122(8) 0.112(8) -0.019(6) 0.031(5) 0.003(5) Cl1 0.0685(11) 0.0719(11) 0.0464(9) -0.0088(8) -0.0008(8) -0.0086(8) Cl2 0.0851(15) 0.130(2) 0.0643(12) -0.0105(12) 0.0206(11) 0.0261(14) Fe1 0.0382(4) 0.0485(5) 0.0434(5) -0.0120(4) 0.0108(3) -0.0047(3) O1 0.040(2) 0.051(2) 0.041(2) -0.0129(18) 0.0034(17) -0.0057(17) O2 0.048(2) 0.043(2) 0.043(2) 0.0027(17) -0.0001(18) 0.0060(17) O3 0.061(3) 0.093(4) 0.057(3) -0.009(3) 0.009(2) -0.018(3) O4 0.134(6) 0.075(4) 0.096(5) 0.009(3) 0.013(4) 0.050(4) P1 0.0342(6) 0.0326(6) 0.0345(7) -0.0036(5) 0.0061(5) -0.0034(5) Se1 0.0490(3) 0.0406(3) 0.0436(3) 0.0049(2) 0.0067(3) -0.0095(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Cl1 2.2880(18) . ? Au1 Se1 2.3864(11) . ? Au1 Au2 3.1563(17) 3_765 ? Au2 Cl2 2.289(2) . ? Au2 Se1 2.3979(12) . ? Au2 Au1 3.1564(17) 3_765 ? C1 O1 1.473(7) . ? C1 C2 1.500(8) . ? C1 C3 1.543(9) . ? C4 O2 1.470(7) . ? C4 C6 1.487(10) . ? C4 C5 1.527(12) . ? C7 O3 1.149(7) . ? C7 Fe1 1.770(6) . ? C8 O4 1.141(8) . ? C8 Fe1 1.781(8) . ? C9 C13 1.372(13) . ? C9 C10 1.387(14) . ? C9 Fe1 2.096(8) . ? C10 C11 1.399(12) . ? C10 Fe1 2.107(8) . ? C11 C12 1.407(13) . ? C11 Fe1 2.084(7) . ? C12 C13 1.412(12) . ? C12 Fe1 2.091(7) . ? C13 Fe1 2.110(8) . ? Fe1 P1 2.1926(18) . ? O1 P1 1.570(4) . ? O2 P1 1.583(4) . ? P1 Se1 2.2971(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Au1 Se1 178.12(5) . . ? Cl1 Au1 Au2 97.51(6) . 3_765 ? Se1 Au1 Au2 82.18(3) . 3_765 ? Cl2 Au2 Se1 177.50(7) . . ? Cl2 Au2 Au1 105.42(7) . 3_765 ? Se1 Au2 Au1 77.00(3) . 3_765 ? O1 C1 C2 107.2(5) . . ? O1 C1 C3 106.9(5) . . ? C2 C1 C3 112.6(6) . . ? O2 C4 C6 110.1(6) . . ? O2 C4 C5 106.3(7) . . ? C6 C4 C5 110.9(6) . . ? O3 C7 Fe1 177.0(6) . . ? O4 C8 Fe1 177.8(8) . . ? C13 C9 C10 109.6(8) . . ? C13 C9 Fe1 71.5(5) . . ? C10 C9 Fe1 71.2(5) . . ? C9 C10 C11 106.6(9) . . ? C9 C10 Fe1 70.3(5) . . ? C11 C10 Fe1 69.6(5) . . ? C10 C11 C12 109.3(9) . . ? C10 C11 Fe1 71.4(4) . . ? C12 C11 Fe1 70.6(5) . . ? C11 C12 C13 105.8(8) . . ? C11 C12 Fe1 70.0(4) . . ? C13 C12 Fe1 71.1(5) . . ? C9 C13 C12 108.6(9) . . ? C9 C13 Fe1 70.4(5) . . ? C12 C13 Fe1 69.6(4) . . ? C7 Fe1 C8 93.6(3) . . ? C7 Fe1 C11 121.2(4) . . ? C8 Fe1 C11 144.8(4) . . ? C7 Fe1 C12 157.3(3) . . ? C8 Fe1 C12 105.6(4) . . ? C11 Fe1 C12 39.4(4) . . ? C7 Fe1 C9 97.1(4) . . ? C8 Fe1 C9 109.0(4) . . ? C11 Fe1 C9 64.6(3) . . ? C12 Fe1 C9 65.4(3) . . ? C7 Fe1 C10 91.2(3) . . ? C8 Fe1 C10 147.6(4) . . ? C11 Fe1 C10 39.0(3) . . ? C12 Fe1 C10 66.1(4) . . ? C9 Fe1 C10 38.5(4) . . ? C7 Fe1 C13 131.6(4) . . ? C8 Fe1 C13 88.8(4) . . ? C11 Fe1 C13 64.8(4) . . ? C12 Fe1 C13 39.3(3) . . ? C9 Fe1 C13 38.1(4) . . ? C10 Fe1 C13 64.6(4) . . ? C7 Fe1 P1 95.8(2) . . ? C8 Fe1 P1 94.0(2) . . ? C11 Fe1 P1 88.1(2) . . ? C12 Fe1 P1 95.0(2) . . ? C9 Fe1 P1 152.7(3) . . ? C10 Fe1 P1 117.4(3) . . ? C13 Fe1 P1 132.3(3) . . ? C1 O1 P1 125.6(4) . . ? C4 O2 P1 129.7(4) . . ? O1 P1 O2 100.8(2) . . ? O1 P1 Fe1 109.45(16) . . ? O2 P1 Fe1 119.61(17) . . ? O1 P1 Se1 102.41(16) . . ? O2 P1 Se1 108.74(17) . . ? Fe1 P1 Se1 113.70(7) . . ? P1 Se1 Au1 103.59(5) . . ? P1 Se1 Au2 103.68(6) . . ? Au1 Se1 Au2 94.21(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.441 _refine_diff_density_min -1.319 _refine_diff_density_rms 0.132 data_6 _database_code_depnum_ccdc_archive 'CCDC 908783' #TrackingRef 'M-Se-P-Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 Au Fe I O4 P Se' _chemical_formula_weight 728.93 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' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.3544(4) _cell_length_b 13.0141(4) _cell_length_c 23.5321(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4089.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.45 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 11.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1447 _exptl_absorpt_correction_T_max 0.2831 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35454 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3594 _reflns_number_gt 3009 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+9.3712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3594 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.070900(16) 0.945246(16) 0.330287(9) 0.05259(8) Uani 1 1 d . . . Fe3 Fe 0.05518(5) 0.74801(6) 0.46591(3) 0.04460(17) Uani 1 1 d . . . I1 I 0.05466(3) 1.13436(3) 0.35353(2) 0.07537(14) Uani 1 1 d . . . Se1 Se 0.09656(5) 0.76927(4) 0.30582(3) 0.06300(17) Uani 1 1 d . . . P5 P 0.02048(9) 0.69961(9) 0.37895(5) 0.0390(3) Uani 1 1 d . . . O1 O -0.0916(3) 0.9130(3) 0.4621(2) 0.0775(12) Uani 1 1 d . . . O2 O -0.0874(3) 0.5953(3) 0.50568(18) 0.0728(12) Uani 1 1 d . . . O3 O -0.0969(2) 0.7082(3) 0.37092(14) 0.0535(9) Uani 1 1 d . . . O4 O 0.0475(3) 0.5809(2) 0.37624(14) 0.0513(9) Uani 1 1 d . . . C1 C 0.2064(5) 0.7363(10) 0.4476(4) 0.112(4) Uani 1 1 d . . . H1 H 0.2352 0.7149 0.4111 0.135 Uiso 1 1 calc R . . C2 C 0.1827(6) 0.6719(6) 0.4927(5) 0.109(3) Uani 1 1 d . . . H2 H 0.1925 0.5974 0.4942 0.130 Uiso 1 1 calc R . . C3 C 0.1484(5) 0.7350(6) 0.5369(3) 0.0782(19) Uani 1 1 d . . . H3 H 0.1282 0.7122 0.5749 0.094 Uiso 1 1 calc R . . C4 C 0.1505(5) 0.8335(5) 0.5179(3) 0.0728(18) Uani 1 1 d . . . H4 H 0.1309 0.8939 0.5401 0.087 Uiso 1 1 calc R . . C5 C 0.1846(5) 0.8353(7) 0.4632(3) 0.090(2) Uani 1 1 d . . . H5 H 0.1952 0.8969 0.4400 0.108 Uiso 1 1 calc R . . C6 C -0.0339(4) 0.8484(4) 0.4627(2) 0.0539(13) Uani 1 1 d . . . C7 C -0.0321(4) 0.6562(4) 0.4901(2) 0.0522(13) Uani 1 1 d . . . C8 C -0.1544(4) 0.7201(5) 0.3184(2) 0.0644(16) Uani 1 1 d . . . H8 H -0.1097 0.7171 0.2854 0.077 Uiso 1 1 calc R . . C9 C -0.2041(5) 0.8243(6) 0.3218(3) 0.092(2) Uani 1 1 d . . . H9A H -0.2459 0.8271 0.3550 0.138 Uiso 1 1 calc R . . H9B H -0.2441 0.8352 0.2885 0.138 Uiso 1 1 calc R . . H9C H -0.1537 0.8767 0.3242 0.138 Uiso 1 1 calc R . . C10 C -0.2288(6) 0.6347(6) 0.3159(3) 0.107(3) Uani 1 1 d . . . H10A H -0.2657 0.6322 0.3509 0.161 Uiso 1 1 calc R . . H10B H -0.1944 0.5707 0.3102 0.161 Uiso 1 1 calc R . . H10C H -0.2741 0.6463 0.2849 0.161 Uiso 1 1 calc R . . C11 C 0.0442(5) 0.5143(4) 0.3273(2) 0.0567(14) Uani 1 1 d . . . H11 H 0.0190 0.5521 0.2943 0.068 Uiso 1 1 calc R . . C12 C -0.0255(6) 0.4282(5) 0.3418(3) 0.092(2) Uani 1 1 d . . . H12A H 0.0023 0.3885 0.3724 0.138 Uiso 1 1 calc R . . H12B H -0.0344 0.3849 0.3091 0.138 Uiso 1 1 calc R . . H12C H -0.0891 0.4558 0.3532 0.138 Uiso 1 1 calc R . . C13 C 0.1472(7) 0.4768(7) 0.3160(4) 0.128(3) Uani 1 1 d . . . H13A H 0.1904 0.5342 0.3086 0.192 Uiso 1 1 calc R . . H13B H 0.1466 0.4321 0.2835 0.192 Uiso 1 1 calc R . . H13C H 0.1714 0.4398 0.3485 0.192 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 Au1 0.05556(14) 0.04845(13) 0.05377(14) 0.00452(10) 0.00443(10) -0.00494(9) Fe3 0.0395(4) 0.0498(4) 0.0445(4) -0.0106(3) -0.0018(3) 0.0024(3) I1 0.0841(3) 0.0508(2) 0.0913(3) -0.0033(2) 0.0037(2) 0.0013(2) Se1 0.0770(4) 0.0528(3) 0.0592(3) -0.0017(3) 0.0303(3) -0.0061(3) P5 0.0392(7) 0.0382(7) 0.0395(6) -0.0012(5) 0.0020(5) 0.0008(5) O1 0.074(3) 0.061(3) 0.098(3) -0.006(2) 0.015(2) 0.023(2) O2 0.068(3) 0.074(3) 0.076(3) 0.016(2) 0.008(2) -0.009(2) O3 0.0399(19) 0.079(3) 0.0416(19) 0.0076(18) -0.0017(15) 0.0012(17) O4 0.073(2) 0.0395(18) 0.0410(19) -0.0049(15) -0.0018(17) 0.0042(16) C1 0.033(4) 0.207(11) 0.097(6) -0.076(7) -0.004(4) 0.007(5) C2 0.058(5) 0.077(5) 0.191(10) -0.033(6) -0.064(6) 0.023(4) C3 0.062(4) 0.103(6) 0.070(4) 0.010(4) -0.027(3) -0.008(4) C4 0.070(4) 0.070(4) 0.078(5) -0.020(4) -0.026(3) -0.001(3) C5 0.058(4) 0.130(7) 0.081(5) 0.018(5) -0.017(4) -0.035(4) C6 0.053(3) 0.055(3) 0.054(3) -0.008(3) 0.009(3) -0.002(3) C7 0.054(3) 0.058(3) 0.044(3) -0.002(3) -0.004(2) 0.010(3) C8 0.054(3) 0.098(5) 0.042(3) 0.003(3) -0.008(2) 0.015(3) C9 0.069(4) 0.116(6) 0.092(5) 0.036(4) -0.001(4) 0.029(4) C10 0.084(6) 0.111(6) 0.126(7) -0.019(5) -0.054(5) 0.004(5) C11 0.082(4) 0.046(3) 0.042(3) -0.010(2) -0.006(3) 0.008(3) C12 0.112(6) 0.052(4) 0.111(6) -0.006(4) -0.027(5) -0.014(4) C13 0.115(7) 0.118(7) 0.151(8) -0.021(6) 0.050(6) 0.042(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Se1 2.3862(6) . ? Au1 I1 2.5305(5) . ? Fe3 C7 1.764(6) . ? Fe3 C6 1.768(6) . ? Fe3 C2 2.068(6) . ? Fe3 C5 2.069(7) . ? Fe3 C1 2.071(7) . ? Fe3 C4 2.087(6) . ? Fe3 C3 2.090(6) . ? Fe3 P5 2.1905(14) . ? Se1 P5 2.1944(13) . ? P5 O3 1.583(3) . ? P5 O4 1.588(3) . ? O1 C6 1.140(6) . ? O2 C7 1.143(6) . ? O3 C8 1.464(6) . ? O4 C11 1.442(6) . ? C1 C5 1.371(12) . ? C1 C2 1.389(12) . ? C2 C3 1.402(11) . ? C3 C4 1.358(9) . ? C4 C5 1.366(9) . ? C8 C10 1.491(9) . ? C8 C9 1.512(9) . ? C11 C13 1.484(10) . ? C11 C12 1.497(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se1 Au1 I1 176.31(2) . . ? C7 Fe3 C6 94.0(2) . . ? C7 Fe3 C2 97.0(3) . . ? C6 Fe3 C2 157.0(3) . . ? C7 Fe3 C5 159.0(3) . . ? C6 Fe3 C5 98.9(3) . . ? C2 Fe3 C5 65.5(3) . . ? C7 Fe3 C1 131.5(4) . . ? C6 Fe3 C1 134.5(4) . . ? C2 Fe3 C1 39.2(3) . . ? C5 Fe3 C1 38.7(3) . . ? C7 Fe3 C4 125.0(3) . . ? C6 Fe3 C4 92.4(3) . . ? C2 Fe3 C4 64.8(3) . . ? C5 Fe3 C4 38.4(3) . . ? C1 Fe3 C4 64.3(3) . . ? C7 Fe3 C3 94.6(3) . . ? C6 Fe3 C3 119.7(3) . . ? C2 Fe3 C3 39.4(3) . . ? C5 Fe3 C3 64.7(3) . . ? C1 Fe3 C3 65.2(3) . . ? C4 Fe3 C3 37.9(2) . . ? C7 Fe3 P5 88.14(17) . . ? C6 Fe3 P5 91.71(18) . . ? C2 Fe3 P5 108.7(3) . . ? C5 Fe3 P5 107.8(2) . . ? C1 Fe3 P5 89.5(2) . . ? C4 Fe3 P5 146.1(2) . . ? C3 Fe3 P5 148.1(2) . . ? P5 Se1 Au1 98.09(4) . . ? O3 P5 O4 106.8(2) . . ? O3 P5 Fe3 107.50(14) . . ? O4 P5 Fe3 105.63(13) . . ? O3 P5 Se1 109.61(14) . . ? O4 P5 Se1 105.39(14) . . ? Fe3 P5 Se1 121.06(6) . . ? C8 O3 P5 128.9(3) . . ? C11 O4 P5 127.6(3) . . ? C5 C1 C2 108.2(7) . . ? C5 C1 Fe3 70.6(4) . . ? C2 C1 Fe3 70.3(4) . . ? C1 C2 C3 106.8(7) . . ? C1 C2 Fe3 70.5(4) . . ? C3 C2 Fe3 71.2(4) . . ? C4 C3 C2 107.5(7) . . ? C4 C3 Fe3 70.9(4) . . ? C2 C3 Fe3 69.4(4) . . ? C3 C4 C5 109.5(7) . . ? C3 C4 Fe3 71.2(4) . . ? C5 C4 Fe3 70.1(4) . . ? C4 C5 C1 107.9(8) . . ? C4 C5 Fe3 71.5(4) . . ? C1 C5 Fe3 70.7(4) . . ? O1 C6 Fe3 178.2(5) . . ? O2 C7 Fe3 178.7(5) . . ? O3 C8 C10 107.7(5) . . ? O3 C8 C9 106.2(5) . . ? C10 C8 C9 112.2(6) . . ? O4 C11 C13 108.3(6) . . ? O4 C11 C12 106.6(5) . . ? C13 C11 C12 111.8(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.095 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.088