# om030200u.cif data_OM030200U _publ_contact_author ; Dr Ulrich Fl\"orke Anorganische und Analytische Chemie Universit\"at-GH Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; _publ_contact_author_email uf@chemie.uni-paderborn.de _publ_contact_author_fax '+49 5251 60 3423' _publ_contact_author_phone '+49 5251 60 2496' _publ_contact_letter ; Please find below 6 data set(s) in CIF format as supplementary crystallographic data in connection with submission of our manuscript entitled "see below" for publication in Organometallics. Thank you very much! ; _publ_section_title ; Chalcogen centered spirocyclic mixed metal carbonyl complexes: Synthesis and molecular structures of (CO)~8~(\m-PCy~2~)Re~2~(\m~4~-E)Fe~2~(\m-ER)(CO)~6~ and ((CO)~8~(\m-PCy~2~)Re~2~(\m~4~-E)Fe~2~(CO)~6~)~2~(\m~4~-E~2~) (E = S, Se, Te; R = org. residue) ; loop_ _publ_author_name _publ_author_address 'Klose, Stefanie' ;Department Chemie Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Fl\"orke, Ulrich' ;Department Chemie Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Mathur, Pradeep' ;Chemistry Department Indian Institute of Technology Bombay, Powai Bombay 400 076, India ; 'Egold, Hans' ;Department Chemie Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H25 Fe2 O14 P Re2 S2' _chemical_formula_weight 1152.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Re' 'Re' -1.0185 7.2310 '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)/c 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 9.766(5) _cell_length_b 17.954(2) _cell_length_c 20.300(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.73(3) _cell_angle_gamma 90.00 _cell_volume 3551.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 7.639 _cell_measurement_theta_max 20.226 _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'none' _exptl_crystal_density_diffrn 2.156 _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 7.820 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 10188 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8166 _reflns_number_gt 4655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0071P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000003(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8166 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 Re1 Re -0.91882(4) 0.37414(2) 0.382136(17) 0.01966(10) Uani 1 1 d . . . Re2 Re -0.56153(4) 0.37736(2) 0.306299(17) 0.01891(10) Uani 1 1 d . . . Fe1 Fe -0.69680(16) 0.17101(8) 0.39109(7) 0.0262(4) Uani 1 1 d . . . Fe2 Fe -0.58797(15) 0.25387(8) 0.48121(6) 0.0255(3) Uani 1 1 d . . . S1 S -0.6974(3) 0.30011(13) 0.38671(11) 0.0196(5) Uani 1 1 d . . . S2 S -0.4717(3) 0.19842(14) 0.40233(12) 0.0283(6) Uani 1 1 d . . . P1 P -0.7960(3) 0.43638(13) 0.29167(11) 0.0179(6) Uani 1 1 d . . . O1 O -0.7912(9) 0.4740(4) 0.4972(3) 0.055(2) Uani 1 1 d . . . C1 C -0.8356(10) 0.4398(5) 0.4542(5) 0.027(2) Uani 1 1 d . . . O2 O -1.1710(7) 0.4748(4) 0.3565(3) 0.039(2) Uani 1 1 d . . . C2 C -1.0788(10) 0.4376(5) 0.3678(4) 0.026(2) Uani 1 1 d . . . O3 O -1.0079(8) 0.2543(4) 0.2768(3) 0.045(2) Uani 1 1 d . . . C3 C -0.9805(10) 0.2976(6) 0.3149(5) 0.029(3) Uani 1 1 d . . . O4 O -1.0897(8) 0.2923(4) 0.4836(3) 0.055(2) Uani 1 1 d . . . C4 C -1.0209(10) 0.3204(6) 0.4477(5) 0.027(2) Uani 1 1 d . . . C5 C -0.4739(10) 0.4382(6) 0.2433(5) 0.030(3) Uani 1 1 d . . . O5 O -0.4191(8) 0.4715(4) 0.2051(3) 0.042(2) Uani 1 1 d . . . O6 O -0.6386(8) 0.2646(4) 0.1932(3) 0.042(2) Uani 1 1 d . . . C6 C -0.6132(10) 0.3051(5) 0.2347(5) 0.027(2) Uani 1 1 d . . . O7 O -0.2700(7) 0.3114(4) 0.3302(4) 0.046(2) Uani 1 1 d . . . C7 C -0.3807(10) 0.3309(5) 0.3243(5) 0.027(2) Uani 1 1 d . . . O8 O -0.4895(8) 0.4951(4) 0.4179(4) 0.048(2) Uani 1 1 d . . . C8 C -0.5171(10) 0.4534(5) 0.3780(5) 0.027(2) Uani 1 1 d . . . O9 O -0.9826(8) 0.1551(4) 0.4208(4) 0.055(2) Uani 1 1 d . . . C9 C -0.8696(11) 0.1644(6) 0.4097(6) 0.041(3) Uani 1 1 d . . . O10 O -0.7416(10) 0.1211(5) 0.2530(3) 0.075(3) Uani 1 1 d . . . C10 C -0.7202(12) 0.1421(5) 0.3051(5) 0.040(3) Uani 1 1 d . . . O11 O -0.6432(8) 0.0243(4) 0.4496(4) 0.052(2) Uani 1 1 d . . . C11 C -0.6650(11) 0.0820(6) 0.4258(5) 0.033(3) Uani 1 1 d . . . O12 O -0.5029(8) 0.1427(4) 0.5806(3) 0.056(2) Uani 1 1 d . . . C12 C -0.5359(11) 0.1858(5) 0.5409(5) 0.034(3) Uani 1 1 d . . . O13 O -0.3807(8) 0.3703(4) 0.5101(4) 0.055(2) Uani 1 1 d . . . C13 C -0.4649(11) 0.3269(6) 0.5002(5) 0.036(3) Uani 1 1 d . . . O14 O -0.8052(8) 0.3013(5) 0.5645(3) 0.062(3) Uani 1 1 d . . . C14 C -0.7221(11) 0.2836(6) 0.5306(5) 0.037(3) Uani 1 1 d . . . C21 C -0.8825(8) 0.4129(5) 0.2094(4) 0.018(2) Uani 1 1 d . . . H21A H -0.8749 0.3582 0.2047 0.021 Uiso 1 1 calc R . . C22 C -0.8115(9) 0.4468(5) 0.1505(4) 0.022(2) Uani 1 1 d . . . H22A H -0.8196 0.5012 0.1518 0.027 Uiso 1 1 calc R . . H22B H -0.7137 0.4341 0.1544 0.027 Uiso 1 1 calc R . . C23 C -0.8754(10) 0.4180(6) 0.0844(4) 0.038(3) Uani 1 1 d . . . H23A H -0.8309 0.4421 0.0481 0.046 Uiso 1 1 calc R . . H23B H -0.8601 0.3642 0.0812 0.046 Uiso 1 1 calc R . . C24 C -1.0292(11) 0.4341(6) 0.0779(4) 0.041(3) Uani 1 1 d . . . H24A H -1.0442 0.4880 0.0763 0.049 Uiso 1 1 calc R . . H24B H -1.0691 0.4126 0.0366 0.049 Uiso 1 1 calc R . . C25 C -1.0995(9) 0.4018(6) 0.1352(4) 0.035(3) Uani 1 1 d . . . H25A H -1.0908 0.3474 0.1345 0.042 Uiso 1 1 calc R . . H25B H -1.1975 0.4141 0.1304 0.042 Uiso 1 1 calc R . . C26 C -1.0391(9) 0.4312(5) 0.2008(4) 0.026(2) Uani 1 1 d . . . H26A H -1.0865 0.4085 0.2368 0.031 Uiso 1 1 calc R . . H26B H -1.0524 0.4852 0.2027 0.031 Uiso 1 1 calc R . . C31 C -0.7985(10) 0.5408(5) 0.2917(4) 0.026(2) Uani 1 1 d . . . H31A H -0.8766 0.5551 0.2608 0.031 Uiso 1 1 calc R . . C32 C -0.6704(11) 0.5754(5) 0.2635(5) 0.029(3) Uani 1 1 d . . . H32A H -0.5898 0.5650 0.2933 0.035 Uiso 1 1 calc R . . H32B H -0.6556 0.5528 0.2206 0.035 Uiso 1 1 calc R . . C33 C -0.6870(11) 0.6593(5) 0.2551(5) 0.032(3) Uani 1 1 d . . . H33A H -0.6036 0.6802 0.2382 0.038 Uiso 1 1 calc R . . H33B H -0.7638 0.6697 0.2230 0.038 Uiso 1 1 calc R . . C34 C -0.7135(11) 0.6960(5) 0.3205(4) 0.039(3) Uani 1 1 d . . . H34A H -0.7284 0.7495 0.3134 0.047 Uiso 1 1 calc R . . H34B H -0.6324 0.6900 0.3511 0.047 Uiso 1 1 calc R . . C35 C -0.8377(12) 0.6628(5) 0.3513(5) 0.035(3) Uani 1 1 d . . . H35A H -0.9209 0.6756 0.3241 0.042 Uiso 1 1 calc R . . H35B H -0.8455 0.6844 0.3952 0.042 Uiso 1 1 calc R . . C36 C -0.8262(11) 0.5772(5) 0.3573(4) 0.028(3) Uani 1 1 d . . . H36A H -0.7517 0.5647 0.3901 0.033 Uiso 1 1 calc R . . H36B H -0.9117 0.5573 0.3729 0.033 Uiso 1 1 calc R . . C41 C -0.3565(10) 0.1233(6) 0.4318(4) 0.048(3) Uani 1 1 d . . . H41A H -0.3110 0.1025 0.3949 0.072 Uiso 1 1 calc R . . H41B H -0.4091 0.0846 0.4520 0.072 Uiso 1 1 calc R . . H41C H -0.2883 0.1429 0.4641 0.072 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 Re1 0.0160(2) 0.0229(2) 0.0202(2) -0.0003(2) 0.00269(17) 0.0002(2) Re2 0.0143(2) 0.01851(19) 0.0241(2) -0.0009(2) 0.00300(17) -0.0006(2) Fe1 0.0313(9) 0.0198(7) 0.0276(8) 0.0033(6) 0.0016(7) -0.0011(7) Fe2 0.0267(8) 0.0276(8) 0.0221(7) 0.0013(7) 0.0005(7) 0.0040(7) S1 0.0183(13) 0.0207(12) 0.0201(12) 0.0001(10) 0.0026(11) 0.0019(11) S2 0.0266(15) 0.0310(14) 0.0273(14) 0.0035(12) 0.0029(12) 0.0085(13) P1 0.0151(13) 0.0184(13) 0.0204(13) -0.0016(11) 0.0022(11) 0.0030(12) O1 0.079(7) 0.055(5) 0.029(4) -0.018(4) -0.016(5) -0.018(5) C1 0.025(6) 0.022(5) 0.032(6) 0.008(5) -0.007(5) -0.008(5) O2 0.029(4) 0.042(5) 0.046(5) -0.002(4) 0.002(4) 0.018(4) C2 0.017(5) 0.032(6) 0.028(6) -0.005(5) 0.005(5) -0.003(5) O3 0.043(5) 0.047(5) 0.045(5) -0.023(4) -0.005(4) -0.005(4) C3 0.015(6) 0.036(6) 0.035(6) 0.018(5) 0.004(5) 0.012(5) O4 0.051(6) 0.068(6) 0.048(5) 0.017(5) 0.029(4) -0.003(5) C4 0.016(6) 0.039(6) 0.027(6) 0.008(5) 0.004(5) 0.007(5) C5 0.018(6) 0.030(6) 0.044(7) -0.018(5) 0.009(5) 0.007(5) O5 0.050(5) 0.032(4) 0.047(5) 0.011(4) 0.021(4) -0.009(4) O6 0.054(5) 0.036(4) 0.035(4) -0.014(4) 0.005(4) -0.013(4) C6 0.022(6) 0.026(6) 0.034(6) -0.006(5) 0.007(5) -0.008(5) O7 0.007(4) 0.027(4) 0.103(7) 0.000(4) 0.000(4) -0.001(3) C7 0.025(6) 0.020(5) 0.036(6) -0.003(5) 0.003(5) -0.011(5) O8 0.048(5) 0.035(5) 0.060(5) -0.019(4) -0.007(5) 0.002(4) C8 0.020(6) 0.026(6) 0.035(6) 0.000(5) -0.001(5) 0.001(5) O9 0.036(5) 0.040(5) 0.091(7) 0.015(5) 0.019(5) -0.002(4) C9 0.030(7) 0.033(7) 0.058(8) 0.015(6) 0.001(6) -0.003(6) O10 0.132(9) 0.057(5) 0.035(4) -0.009(5) -0.012(5) -0.009(7) C10 0.050(8) 0.028(7) 0.042(6) 0.008(5) 0.004(6) 0.004(6) O11 0.061(6) 0.032(4) 0.063(5) 0.019(4) -0.007(5) 0.002(5) C11 0.030(6) 0.032(6) 0.037(6) -0.016(5) -0.004(5) 0.000(6) O12 0.074(6) 0.057(6) 0.037(4) 0.022(4) -0.001(4) 0.022(5) C12 0.038(7) 0.035(6) 0.028(6) 0.008(5) 0.007(5) 0.011(6) O13 0.049(5) 0.054(5) 0.060(5) -0.013(5) -0.015(4) -0.003(6) C13 0.039(7) 0.042(7) 0.025(6) 0.008(5) -0.011(6) -0.006(6) O14 0.057(6) 0.094(7) 0.038(5) 0.004(5) 0.013(5) 0.031(6) C14 0.043(7) 0.047(7) 0.020(5) 0.017(5) 0.008(5) 0.018(6) C21 0.018(5) 0.025(5) 0.010(4) 0.005(4) 0.002(4) 0.005(4) C22 0.021(5) 0.031(5) 0.014(4) 0.004(4) -0.001(4) -0.010(5) C23 0.032(7) 0.064(8) 0.018(5) -0.010(5) 0.003(5) 0.000(6) C24 0.044(8) 0.057(8) 0.019(5) -0.009(5) -0.011(5) 0.002(7) C25 0.022(6) 0.054(7) 0.027(6) -0.003(5) -0.006(5) 0.000(6) C26 0.031(6) 0.030(6) 0.016(5) 0.000(4) 0.000(5) 0.006(5) C31 0.037(6) 0.014(5) 0.026(5) -0.003(4) 0.000(5) 0.001(5) C32 0.042(7) 0.020(5) 0.025(6) 0.002(5) 0.002(5) -0.005(5) C33 0.039(7) 0.023(6) 0.034(6) 0.010(5) 0.002(6) 0.002(5) C34 0.057(8) 0.025(6) 0.034(6) 0.006(5) -0.006(6) 0.001(6) C35 0.060(9) 0.024(6) 0.024(6) -0.002(5) 0.017(6) 0.018(6) C36 0.030(6) 0.023(5) 0.030(6) 0.000(5) -0.004(5) 0.005(5) C41 0.056(8) 0.043(6) 0.046(6) 0.019(6) 0.008(6) 0.034(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 Re1 C2 1.941(10) . ? Re1 C4 1.968(10) . ? Re1 C3 2.002(11) . ? Re1 C1 2.010(9) . ? Re1 P1 2.519(2) . ? Re1 S1 2.535(3) . ? Re2 C5 1.925(11) . ? Re2 C7 1.966(10) . ? Re2 C6 1.989(10) . ? Re2 C8 2.023(10) . ? Re2 P1 2.523(3) . ? Re2 S1 2.575(2) . ? Fe1 C9 1.758(11) . ? Fe1 C11 1.765(10) . ? Fe1 C10 1.822(11) . ? Fe1 S2 2.250(3) . ? Fe1 S1 2.320(3) . ? Fe1 Fe2 2.537(2) . ? Fe2 C12 1.771(10) . ? Fe2 C14 1.782(11) . ? Fe2 C13 1.803(11) . ? Fe2 S2 2.254(3) . ? Fe2 S1 2.290(3) . ? S2 C41 1.832(9) . ? P1 C21 1.870(8) . ? P1 C31 1.874(9) . ? O1 C1 1.130(10) . ? O2 C2 1.132(10) . ? O3 C3 1.117(11) . ? O4 C4 1.139(10) . ? C5 O5 1.140(11) . ? O6 C6 1.129(10) . ? O7 C7 1.135(10) . ? O8 C8 1.122(10) . ? O9 C9 1.152(12) . ? O10 C10 1.129(11) . ? O11 C11 1.158(11) . ? O12 C12 1.150(10) . ? O13 C13 1.142(11) . ? O14 C14 1.143(11) . ? C21 C22 1.545(10) . ? C21 C26 1.563(11) . ? C22 C23 1.534(10) . ? C23 C24 1.527(13) . ? C24 C25 1.504(12) . ? C25 C26 1.517(10) . ? C31 C36 1.523(11) . ? C31 C32 1.541(13) . ? C32 C33 1.522(11) . ? C33 C34 1.518(12) . ? C34 C35 1.522(13) . ? C35 C36 1.545(11) . ? 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 C2 Re1 C4 87.2(4) . . ? C2 Re1 C3 95.6(4) . . ? C4 Re1 C3 88.9(4) . . ? C2 Re1 C1 92.8(4) . . ? C4 Re1 C1 89.6(4) . . ? C3 Re1 C1 171.4(4) . . ? C2 Re1 P1 92.7(3) . . ? C4 Re1 P1 175.7(3) . . ? C3 Re1 P1 86.8(3) . . ? C1 Re1 P1 94.7(3) . . ? C2 Re1 S1 171.9(3) . . ? C4 Re1 S1 100.7(3) . . ? C3 Re1 S1 83.3(3) . . ? C1 Re1 S1 88.7(3) . . ? P1 Re1 S1 79.26(8) . . ? C5 Re2 C7 86.1(4) . . ? C5 Re2 C6 89.3(4) . . ? C7 Re2 C6 92.4(4) . . ? C5 Re2 C8 90.7(4) . . ? C7 Re2 C8 90.3(4) . . ? C6 Re2 C8 177.4(4) . . ? C5 Re2 P1 97.0(3) . . ? C7 Re2 P1 176.0(3) . . ? C6 Re2 P1 90.2(3) . . ? C8 Re2 P1 87.2(3) . . ? C5 Re2 S1 175.4(3) . . ? C7 Re2 S1 98.5(3) . . ? C6 Re2 S1 89.7(3) . . ? C8 Re2 S1 90.1(3) . . ? P1 Re2 S1 78.45(8) . . ? C9 Fe1 C11 90.0(5) . . ? C9 Fe1 C10 97.2(5) . . ? C11 Fe1 C10 97.6(4) . . ? C9 Fe1 S2 159.8(4) . . ? C11 Fe1 S2 90.7(4) . . ? C10 Fe1 S2 102.7(4) . . ? C9 Fe1 S1 94.3(4) . . ? C11 Fe1 S1 156.9(3) . . ? C10 Fe1 S1 104.4(3) . . ? S2 Fe1 S1 77.60(10) . . ? C9 Fe1 Fe2 104.3(4) . . ? C11 Fe1 Fe2 100.9(3) . . ? C10 Fe1 Fe2 151.5(3) . . ? S2 Fe1 Fe2 55.79(8) . . ? S1 Fe1 Fe2 56.05(7) . . ? C12 Fe2 C14 90.6(4) . . ? C12 Fe2 C13 101.4(5) . . ? C14 Fe2 C13 99.5(5) . . ? C12 Fe2 S2 92.6(3) . . ? C14 Fe2 S2 162.6(4) . . ? C13 Fe2 S2 96.5(4) . . ? C12 Fe2 S1 157.0(3) . . ? C14 Fe2 S1 92.4(3) . . ? C13 Fe2 S1 100.6(3) . . ? S2 Fe2 S1 78.12(10) . . ? C12 Fe2 Fe1 100.2(3) . . ? C14 Fe2 Fe1 107.0(4) . . ? C13 Fe2 Fe1 145.4(3) . . ? S2 Fe2 Fe1 55.64(8) . . ? S1 Fe2 Fe1 57.17(7) . . ? Fe2 S1 Fe1 66.78(8) . . ? Fe2 S1 Re1 124.83(10) . . ? Fe1 S1 Re1 121.68(11) . . ? Fe2 S1 Re2 119.66(11) . . ? Fe1 S1 Re2 124.23(11) . . ? Re1 S1 Re2 99.66(8) . . ? C41 S2 Fe1 116.6(4) . . ? C41 S2 Fe2 114.9(3) . . ? Fe1 S2 Fe2 68.56(9) . . ? C21 P1 C31 102.7(4) . . ? C21 P1 Re1 110.0(3) . . ? C31 P1 Re1 115.9(3) . . ? C21 P1 Re2 111.4(3) . . ? C31 P1 Re2 115.6(3) . . ? Re1 P1 Re2 101.51(9) . . ? O1 C1 Re1 176.3(9) . . ? O2 C2 Re1 176.8(9) . . ? O3 C3 Re1 176.3(9) . . ? O4 C4 Re1 174.2(9) . . ? O5 C5 Re2 177.0(9) . . ? O6 C6 Re2 177.7(9) . . ? O7 C7 Re2 171.2(9) . . ? O8 C8 Re2 178.5(9) . . ? O9 C9 Fe1 175.4(11) . . ? O10 C10 Fe1 175.4(11) . . ? O11 C11 Fe1 178.7(9) . . ? O12 C12 Fe2 178.5(9) . . ? O13 C13 Fe2 175.3(11) . . ? O14 C14 Fe2 177.1(9) . . ? C22 C21 C26 108.4(7) . . ? C22 C21 P1 113.7(6) . . ? C26 C21 P1 115.7(6) . . ? C23 C22 C21 111.5(7) . . ? C24 C23 C22 110.7(8) . . ? C25 C24 C23 110.9(8) . . ? C24 C25 C26 111.9(8) . . ? C25 C26 C21 110.3(7) . . ? C36 C31 C32 110.2(8) . . ? C36 C31 P1 115.7(6) . . ? C32 C31 P1 113.1(7) . . ? C33 C32 C31 111.0(9) . . ? C34 C33 C32 110.8(8) . . ? C33 C34 C35 112.0(9) . . ? C34 C35 C36 111.5(9) . . ? C31 C36 C35 112.0(8) . . ? 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 C9 Fe1 Fe2 C12 90.0(5) . . . . ? C11 Fe1 Fe2 C12 -2.8(5) . . . . ? C10 Fe1 Fe2 C12 -132.3(8) . . . . ? S2 Fe1 Fe2 C12 -86.2(4) . . . . ? S1 Fe1 Fe2 C12 175.5(4) . . . . ? C9 Fe1 Fe2 C14 -3.9(5) . . . . ? C11 Fe1 Fe2 C14 -96.6(5) . . . . ? C10 Fe1 Fe2 C14 133.9(8) . . . . ? S2 Fe1 Fe2 C14 180.0(3) . . . . ? S1 Fe1 Fe2 C14 81.7(3) . . . . ? C9 Fe1 Fe2 C13 -142.3(7) . . . . ? C11 Fe1 Fe2 C13 125.0(7) . . . . ? C10 Fe1 Fe2 C13 -4.5(10) . . . . ? S2 Fe1 Fe2 C13 41.6(6) . . . . ? S1 Fe1 Fe2 C13 -56.7(6) . . . . ? C9 Fe1 Fe2 S2 176.1(4) . . . . ? C11 Fe1 Fe2 S2 83.4(4) . . . . ? C10 Fe1 Fe2 S2 -46.1(7) . . . . ? S1 Fe1 Fe2 S2 -98.31(12) . . . . ? C9 Fe1 Fe2 S1 -85.6(4) . . . . ? C11 Fe1 Fe2 S1 -178.3(4) . . . . ? C10 Fe1 Fe2 S1 52.2(7) . . . . ? S2 Fe1 Fe2 S1 98.31(12) . . . . ? C12 Fe2 S1 Fe1 -11.3(9) . . . . ? C14 Fe2 S1 Fe1 -108.7(4) . . . . ? C13 Fe2 S1 Fe1 151.1(4) . . . . ? S2 Fe2 S1 Fe1 56.59(9) . . . . ? C12 Fe2 S1 Re1 102.1(9) . . . . ? C14 Fe2 S1 Re1 4.7(4) . . . . ? C13 Fe2 S1 Re1 -95.5(4) . . . . ? S2 Fe2 S1 Re1 170.02(14) . . . . ? Fe1 Fe2 S1 Re1 113.44(14) . . . . ? C12 Fe2 S1 Re2 -128.7(9) . . . . ? C14 Fe2 S1 Re2 133.9(4) . . . . ? C13 Fe2 S1 Re2 33.7(4) . . . . ? S2 Fe2 S1 Re2 -60.81(12) . . . . ? Fe1 Fe2 S1 Re2 -117.40(13) . . . . ? C9 Fe1 S1 Fe2 104.3(4) . . . . ? C11 Fe1 S1 Fe2 4.2(9) . . . . ? C10 Fe1 S1 Fe2 -157.1(4) . . . . ? S2 Fe1 S1 Fe2 -56.92(9) . . . . ? C9 Fe1 S1 Re1 -13.4(4) . . . . ? C11 Fe1 S1 Re1 -113.6(9) . . . . ? C10 Fe1 S1 Re1 85.2(4) . . . . ? S2 Fe1 S1 Re1 -174.67(12) . . . . ? Fe2 Fe1 S1 Re1 -117.75(13) . . . . ? C9 Fe1 S1 Re2 -144.6(4) . . . . ? C11 Fe1 S1 Re2 115.3(9) . . . . ? C10 Fe1 S1 Re2 -46.0(4) . . . . ? S2 Fe1 S1 Re2 54.14(13) . . . . ? Fe2 Fe1 S1 Re2 111.06(14) . . . . ? C2 Re1 S1 Fe2 150.3(19) . . . . ? C4 Re1 S1 Fe2 -39.5(3) . . . . ? C3 Re1 S1 Fe2 -127.1(3) . . . . ? C1 Re1 S1 Fe2 49.9(3) . . . . ? P1 Re1 S1 Fe2 144.87(13) . . . . ? C2 Re1 S1 Fe1 -127.5(19) . . . . ? C4 Re1 S1 Fe1 42.7(3) . . . . ? C3 Re1 S1 Fe1 -44.9(3) . . . . ? C1 Re1 S1 Fe1 132.1(3) . . . . ? P1 Re1 S1 Fe1 -132.88(13) . . . . ? C2 Re1 S1 Re2 13(2) . . . . ? C4 Re1 S1 Re2 -176.4(3) . . . . ? C3 Re1 S1 Re2 96.0(3) . . . . ? C1 Re1 S1 Re2 -87.0(3) . . . . ? P1 Re1 S1 Re2 7.98(8) . . . . ? C5 Re2 S1 Fe2 -161(3) . . . . ? C7 Re2 S1 Fe2 29.6(3) . . . . ? C6 Re2 S1 Fe2 122.0(3) . . . . ? C8 Re2 S1 Fe2 -60.6(3) . . . . ? P1 Re2 S1 Fe2 -147.79(12) . . . . ? C5 Re2 S1 Fe1 119(3) . . . . ? C7 Re2 S1 Fe1 -51.1(3) . . . . ? C6 Re2 S1 Fe1 41.3(3) . . . . ? C8 Re2 S1 Fe1 -141.4(3) . . . . ? P1 Re2 S1 Fe1 131.49(14) . . . . ? C5 Re2 S1 Re1 -21(3) . . . . ? C7 Re2 S1 Re1 169.4(3) . . . . ? C6 Re2 S1 Re1 -98.2(3) . . . . ? C8 Re2 S1 Re1 79.2(3) . . . . ? P1 Re2 S1 Re1 -7.99(8) . . . . ? C9 Fe1 S2 C41 97.1(11) . . . . ? C11 Fe1 S2 C41 5.3(5) . . . . ? C10 Fe1 S2 C41 -92.7(5) . . . . ? S1 Fe1 S2 C41 165.2(4) . . . . ? Fe2 Fe1 S2 C41 108.0(3) . . . . ? C9 Fe1 S2 Fe2 -10.9(10) . . . . ? C11 Fe1 S2 Fe2 -102.7(3) . . . . ? C10 Fe1 S2 Fe2 159.4(3) . . . . ? S1 Fe1 S2 Fe2 57.19(8) . . . . ? C12 Fe2 S2 C41 -9.8(5) . . . . ? C14 Fe2 S2 C41 -110.3(11) . . . . ? C13 Fe2 S2 C41 92.0(5) . . . . ? S1 Fe2 S2 C41 -168.5(4) . . . . ? Fe1 Fe2 S2 C41 -110.3(4) . . . . ? C12 Fe2 S2 Fe1 100.5(3) . . . . ? C14 Fe2 S2 Fe1 0.0(11) . . . . ? C13 Fe2 S2 Fe1 -157.7(3) . . . . ? S1 Fe2 S2 Fe1 -58.17(9) . . . . ? C2 Re1 P1 C21 -69.4(4) . . . . ? C4 Re1 P1 C21 19(4) . . . . ? C3 Re1 P1 C21 26.0(4) . . . . ? C1 Re1 P1 C21 -162.4(4) . . . . ? S1 Re1 P1 C21 109.8(3) . . . . ? C2 Re1 P1 C31 46.5(5) . . . . ? C4 Re1 P1 C31 135(4) . . . . ? C3 Re1 P1 C31 142.0(5) . . . . ? C1 Re1 P1 C31 -46.5(5) . . . . ? S1 Re1 P1 C31 -134.2(4) . . . . ? C2 Re1 P1 Re2 172.6(3) . . . . ? C4 Re1 P1 Re2 -99(4) . . . . ? C3 Re1 P1 Re2 -92.0(3) . . . . ? C1 Re1 P1 Re2 79.6(3) . . . . ? S1 Re1 P1 Re2 -8.20(8) . . . . ? C5 Re2 P1 C21 70.0(4) . . . . ? C7 Re2 P1 C21 -149(4) . . . . ? C6 Re2 P1 C21 -19.3(4) . . . . ? C8 Re2 P1 C21 160.4(4) . . . . ? S1 Re2 P1 C21 -108.9(3) . . . . ? C5 Re2 P1 C31 -46.7(4) . . . . ? C7 Re2 P1 C31 95(4) . . . . ? C6 Re2 P1 C31 -136.0(4) . . . . ? C8 Re2 P1 C31 43.6(4) . . . . ? S1 Re2 P1 C31 134.3(3) . . . . ? C5 Re2 P1 Re1 -172.9(3) . . . . ? C7 Re2 P1 Re1 -32(4) . . . . ? C6 Re2 P1 Re1 97.8(3) . . . . ? C8 Re2 P1 Re1 -82.6(3) . . . . ? S1 Re2 P1 Re1 8.09(8) . . . . ? C2 Re1 C1 O1 101(15) . . . . ? C4 Re1 C1 O1 14(15) . . . . ? C3 Re1 C1 O1 -66(16) . . . . ? P1 Re1 C1 O1 -166(15) . . . . ? S1 Re1 C1 O1 -87(15) . . . . ? C4 Re1 C2 O2 -143(15) . . . . ? C3 Re1 C2 O2 -55(15) . . . . ? C1 Re1 C2 O2 127(15) . . . . ? P1 Re1 C2 O2 32(15) . . . . ? S1 Re1 C2 O2 27(17) . . . . ? C2 Re1 C3 O3 147(14) . . . . ? C4 Re1 C3 O3 -126(14) . . . . ? C1 Re1 C3 O3 -46(15) . . . . ? P1 Re1 C3 O3 54(14) . . . . ? S1 Re1 C3 O3 -25(14) . . . . ? C2 Re1 C4 O4 13(9) . . . . ? C3 Re1 C4 O4 -82(9) . . . . ? C1 Re1 C4 O4 106(9) . . . . ? P1 Re1 C4 O4 -76(11) . . . . ? S1 Re1 C4 O4 -165(9) . . . . ? C7 Re2 C5 O5 43(18) . . . . ? C6 Re2 C5 O5 -50(18) . . . . ? C8 Re2 C5 O5 133(18) . . . . ? P1 Re2 C5 O5 -140(18) . . . . ? S1 Re2 C5 O5 -127(16) . . . . ? C5 Re2 C6 O6 34(24) . . . . ? C7 Re2 C6 O6 -52(24) . . . . ? C8 Re2 C6 O6 123(23) . . . . ? P1 Re2 C6 O6 131(24) . . . . ? S1 Re2 C6 O6 -150(24) . . . . ? C5 Re2 C7 O7 12(6) . . . . ? C6 Re2 C7 O7 101(6) . . . . ? C8 Re2 C7 O7 -78(6) . . . . ? P1 Re2 C7 O7 -129(5) . . . . ? S1 Re2 C7 O7 -169(6) . . . . ? C5 Re2 C8 O8 -71(34) . . . . ? C7 Re2 C8 O8 15(34) . . . . ? C6 Re2 C8 O8 -160(30) . . . . ? P1 Re2 C8 O8 -168(34) . . . . ? S1 Re2 C8 O8 113(34) . . . . ? C11 Fe1 C9 O9 -39(14) . . . . ? C10 Fe1 C9 O9 59(14) . . . . ? S2 Fe1 C9 O9 -131(13) . . . . ? S1 Fe1 C9 O9 164(14) . . . . ? Fe2 Fe1 C9 O9 -140(14) . . . . ? C9 Fe1 C10 O10 -34(14) . . . . ? C11 Fe1 C10 O10 57(14) . . . . ? S2 Fe1 C10 O10 150(13) . . . . ? S1 Fe1 C10 O10 -130(13) . . . . ? Fe2 Fe1 C10 O10 -173(13) . . . . ? C9 Fe1 C11 O11 -98(50) . . . . ? C10 Fe1 C11 O11 165(50) . . . . ? S2 Fe1 C11 O11 62(50) . . . . ? S1 Fe1 C11 O11 3(51) . . . . ? Fe2 Fe1 C11 O11 6(50) . . . . ? C14 Fe2 C12 O12 -35(42) . . . . ? C13 Fe2 C12 O12 65(42) . . . . ? S2 Fe2 C12 O12 162(42) . . . . ? S1 Fe2 C12 O12 -133(41) . . . . ? Fe1 Fe2 C12 O12 -142(42) . . . . ? C12 Fe2 C13 O13 78(12) . . . . ? C14 Fe2 C13 O13 170(12) . . . . ? S2 Fe2 C13 O13 -16(12) . . . . ? S1 Fe2 C13 O13 -95(12) . . . . ? Fe1 Fe2 C13 O13 -50(12) . . . . ? C12 Fe2 C14 O14 20(23) . . . . ? C13 Fe2 C14 O14 -82(23) . . . . ? S2 Fe2 C14 O14 121(22) . . . . ? S1 Fe2 C14 O14 177(100) . . . . ? Fe1 Fe2 C14 O14 121(23) . . . . ? C31 P1 C21 C22 57.8(7) . . . . ? Re1 P1 C21 C22 -178.3(5) . . . . ? Re2 P1 C21 C22 -66.5(7) . . . . ? C31 P1 C21 C26 -68.7(7) . . . . ? Re1 P1 C21 C26 55.2(7) . . . . ? Re2 P1 C21 C26 167.0(6) . . . . ? C26 C21 C22 C23 -56.9(10) . . . . ? P1 C21 C22 C23 172.9(6) . . . . ? C21 C22 C23 C24 56.7(11) . . . . ? C22 C23 C24 C25 -55.7(12) . . . . ? C23 C24 C25 C26 57.4(12) . . . . ? C24 C25 C26 C21 -58.5(11) . . . . ? C22 C21 C26 C25 57.1(10) . . . . ? P1 C21 C26 C25 -173.7(6) . . . . ? C21 P1 C31 C36 141.3(7) . . . . ? Re1 P1 C31 C36 21.4(9) . . . . ? Re2 P1 C31 C36 -97.2(7) . . . . ? C21 P1 C31 C32 -90.2(7) . . . . ? Re1 P1 C31 C32 149.8(6) . . . . ? Re2 P1 C31 C32 31.3(8) . . . . ? C36 C31 C32 C33 -57.2(11) . . . . ? P1 C31 C32 C33 171.6(7) . . . . ? C31 C32 C33 C34 57.8(12) . . . . ? C32 C33 C34 C35 -56.0(12) . . . . ? C33 C34 C35 C36 53.3(12) . . . . ? C32 C31 C36 C35 54.6(12) . . . . ? P1 C31 C36 C35 -175.5(8) . . . . ? C34 C35 C36 C31 -53.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.920 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.232 #===END data_3b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H25 Fe2 O14 P Re2 Se2' _chemical_formula_sum 'C27 H25 Fe2 O14 P Re2 Se2' _chemical_formula_weight 1246.46 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' 'Re' 'Re' -1.0185 7.2310 '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)/c 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 9.857(3) _cell_length_b 18.234(3) _cell_length_c 20.473(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.25(2) _cell_angle_gamma 90.00 _cell_volume 3673.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 7.159 _cell_measurement_theta_max 14.905 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 9.428 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.596 _exptl_absorpt_process_details 'face indexed, XPREP (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 10487 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8427 _reflns_number_gt 5329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00038(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8427 _refine_ls_number_parameters 435 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.987 _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 Re1 Re 0.42598(3) 0.37879(2) 0.119368(15) 0.03406(10) Uani 1 1 d . . . Re2 Re 0.06476(3) 0.382512(19) 0.198520(15) 0.03273(10) Uani 1 1 d . . . Se1 Se 0.19827(8) 0.30360(5) 0.11382(4) 0.0340(2) Uani 1 1 d . . . Se2 Se -0.04010(11) 0.19965(6) 0.09752(5) 0.0566(3) Uani 1 1 d . . . Fe1 Fe 0.19387(14) 0.17147(7) 0.10679(6) 0.0437(3) Uani 1 1 d . . . Fe2 Fe 0.08683(13) 0.25499(7) 0.01638(6) 0.0443(3) Uani 1 1 d . . . P1 P 0.2995(2) 0.44069(12) 0.20826(10) 0.0330(5) Uani 1 1 d . . . O1 O 0.6767(7) 0.4785(4) 0.1435(3) 0.069(2) Uani 1 1 d . . . C1 C 0.5819(9) 0.4400(5) 0.1337(4) 0.043(2) Uani 1 1 d U . . O2 O 0.3021(9) 0.4764(4) 0.0051(3) 0.088(3) Uani 1 1 d . . . C2 C 0.3465(10) 0.4430(5) 0.0473(5) 0.052(3) Uani 1 1 d U . . O3 O 0.5087(8) 0.2581(4) 0.2223(3) 0.074(2) Uani 1 1 d . . . C3 C 0.4842(9) 0.3034(6) 0.1866(5) 0.049(2) Uani 1 1 d U . . O4 O 0.5944(8) 0.2992(4) 0.0198(4) 0.087(3) Uani 1 1 d . . . C4 C 0.5270(10) 0.3265(6) 0.0559(5) 0.054(3) Uani 1 1 d U . . O5 O -0.0150(8) 0.4955(4) 0.0866(3) 0.082(3) Uani 1 1 d . . . C5 C 0.0156(8) 0.4538(5) 0.1260(5) 0.045(2) Uani 1 1 d U . . O6 O -0.2243(7) 0.3167(4) 0.1816(4) 0.074(2) Uani 1 1 d . . . C6 C -0.1151(9) 0.3373(5) 0.1846(5) 0.045(2) Uani 1 1 d U . . O7 O -0.0688(7) 0.4769(4) 0.3015(3) 0.076(2) Uani 1 1 d . . . C7 C -0.0157(9) 0.4428(5) 0.2632(5) 0.047(2) Uani 1 1 d U . . O8 O 0.1500(8) 0.2679(4) 0.3066(3) 0.074(2) Uani 1 1 d . . . C8 C 0.1207(9) 0.3094(5) 0.2676(4) 0.040(2) Uani 1 1 d U . . O9 O 0.4753(8) 0.1606(4) 0.0757(5) 0.099(3) Uani 1 1 d . . . C9 C 0.3647(11) 0.1665(6) 0.0868(6) 0.064(3) Uani 1 1 d U . . O10 O 0.1429(8) 0.0284(4) 0.0466(4) 0.083(2) Uani 1 1 d . . . C10 C 0.1631(11) 0.0836(6) 0.0703(5) 0.062(3) Uani 1 1 d U . . O11 O 0.2323(11) 0.1218(5) 0.2425(4) 0.115(4) Uani 1 1 d . . . C11 C 0.2155(12) 0.1424(5) 0.1907(5) 0.065(3) Uani 1 1 d U . . O12 O 0.3099(9) 0.3001(6) -0.0611(3) 0.105(3) Uani 1 1 d . . . C12 C 0.2246(12) 0.2821(6) -0.0304(5) 0.065(3) Uani 1 1 d U . . O13 O -0.1071(9) 0.3723(5) -0.0137(4) 0.096(3) Uani 1 1 d . . . C13 C -0.0303(12) 0.3263(6) -0.0040(5) 0.063(3) Uani 1 1 d U . . O14 O -0.0001(9) 0.1467(5) -0.0812(4) 0.098(3) Uani 1 1 d . . . C14 C 0.0336(11) 0.1885(6) -0.0431(5) 0.064(3) Uani 1 1 d U . . C21 C 0.3849(8) 0.4187(5) 0.2901(4) 0.040(2) Uani 1 1 d U . . H21 H 0.3794 0.3653 0.2947 0.048 Uiso 1 1 calc R . . C22 C 0.5362(8) 0.4378(6) 0.2971(4) 0.051(2) Uani 1 1 d U . . H22A H 0.5472 0.4906 0.2944 0.061 Uiso 1 1 calc R . . H22B H 0.5825 0.4158 0.2614 0.061 Uiso 1 1 calc R . . C23 C 0.6014(10) 0.4099(6) 0.3632(4) 0.068(3) Uani 1 1 d U . . H23A H 0.5983 0.3567 0.3643 0.081 Uiso 1 1 calc R . . H23B H 0.6959 0.4249 0.3676 0.081 Uiso 1 1 calc R . . C24 C 0.5257(11) 0.4408(7) 0.4196(4) 0.075(3) Uani 1 1 d U . . H24A H 0.5643 0.4205 0.4603 0.090 Uiso 1 1 calc R . . H24B H 0.5384 0.4936 0.4212 0.090 Uiso 1 1 calc R . . C25 C 0.3769(10) 0.4244(6) 0.4139(4) 0.068(3) Uani 1 1 d U . . H25A H 0.3325 0.4484 0.4492 0.081 Uiso 1 1 calc R . . H25B H 0.3629 0.3720 0.4178 0.081 Uiso 1 1 calc R . . C26 C 0.3146(9) 0.4510(6) 0.3486(4) 0.053(2) Uani 1 1 d U . . H26A H 0.3206 0.5041 0.3469 0.064 Uiso 1 1 calc R . . H26B H 0.2192 0.4378 0.3451 0.064 Uiso 1 1 calc R . . C31 C 0.3007(10) 0.5438(4) 0.2064(4) 0.050(2) Uani 1 1 d U . . H31 H 0.3769 0.5573 0.2368 0.059 Uiso 1 1 calc R . . C32 C 0.1779(10) 0.5799(5) 0.2349(5) 0.051(2) Uani 1 1 d U . . H32A H 0.0974 0.5688 0.2072 0.061 Uiso 1 1 calc R . . H32B H 0.1652 0.5593 0.2779 0.061 Uiso 1 1 calc R . . C33 C 0.1926(13) 0.6623(5) 0.2410(5) 0.079(3) Uani 1 1 d U . . H33A H 0.1093 0.6826 0.2566 0.095 Uiso 1 1 calc R . . H33B H 0.2655 0.6734 0.2733 0.095 Uiso 1 1 calc R . . C34 C 0.2219(13) 0.6983(6) 0.1781(5) 0.080(3) Uani 1 1 d U . . H34A H 0.2393 0.7500 0.1854 0.096 Uiso 1 1 calc R . . H34B H 0.1436 0.6937 0.1475 0.096 Uiso 1 1 calc R . . C35 C 0.3470(12) 0.6623(5) 0.1485(5) 0.070(3) Uani 1 1 d U . . H35A H 0.3572 0.6816 0.1049 0.084 Uiso 1 1 calc R . . H35B H 0.4282 0.6747 0.1752 0.084 Uiso 1 1 calc R . . C36 C 0.3324(12) 0.5787(5) 0.1450(5) 0.064(3) Uani 1 1 d U . . H36A H 0.2611 0.5667 0.1120 0.077 Uiso 1 1 calc R . . H36B H 0.4165 0.5581 0.1307 0.077 Uiso 1 1 calc R . . C41 C -0.1538(10) 0.1192(6) 0.0633(5) 0.081(4) Uani 1 1 d U . . H41A H -0.1502 0.1171 0.0166 0.121 Uiso 1 1 calc R . . H41B H -0.2459 0.1271 0.0745 0.121 Uiso 1 1 calc R . . H41C H -0.1212 0.0738 0.0820 0.121 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 Re1 0.02967(18) 0.0419(2) 0.03091(17) -0.00021(16) 0.00473(14) -0.00085(18) Re2 0.02749(18) 0.03276(18) 0.03822(19) 0.00181(16) 0.00420(14) 0.00109(17) Se1 0.0329(5) 0.0372(5) 0.0318(4) -0.0023(4) 0.0012(4) -0.0019(4) Se2 0.0550(6) 0.0586(6) 0.0568(6) -0.0075(5) 0.0081(5) -0.0119(6) Fe1 0.0507(8) 0.0368(7) 0.0435(7) -0.0046(6) 0.0018(6) 0.0001(7) Fe2 0.0485(8) 0.0511(8) 0.0329(6) -0.0037(6) -0.0017(6) -0.0094(7) P1 0.0314(12) 0.0357(12) 0.0320(11) -0.0004(10) 0.0031(10) -0.0022(10) O1 0.051(4) 0.079(5) 0.077(5) 0.006(4) -0.003(4) -0.020(4) C1 0.041(5) 0.052(6) 0.037(5) -0.001(4) 0.009(4) 0.008(5) O2 0.128(7) 0.081(6) 0.053(4) 0.024(4) -0.016(5) 0.018(6) C2 0.053(6) 0.058(6) 0.046(6) -0.001(5) 0.012(5) 0.002(5) O3 0.068(5) 0.071(5) 0.081(5) 0.029(4) -0.011(4) 0.017(4) C3 0.029(5) 0.061(7) 0.057(6) -0.010(5) 0.002(5) 0.000(5) O4 0.086(6) 0.099(6) 0.081(5) -0.016(5) 0.042(5) 0.007(5) C4 0.043(6) 0.067(7) 0.053(6) -0.008(5) 0.018(5) 0.000(5) O5 0.087(6) 0.075(5) 0.078(5) 0.039(4) -0.035(5) -0.008(5) C5 0.024(5) 0.049(6) 0.061(6) -0.003(5) -0.003(4) -0.001(4) O6 0.036(4) 0.047(4) 0.140(7) 0.011(4) 0.009(4) 0.002(4) C6 0.030(5) 0.029(5) 0.077(7) 0.006(4) 0.005(5) 0.006(4) O7 0.085(6) 0.059(5) 0.088(5) -0.003(4) 0.047(5) 0.016(4) C7 0.030(5) 0.043(5) 0.070(6) -0.004(5) 0.014(5) 0.001(4) O8 0.098(6) 0.067(5) 0.058(4) 0.022(4) 0.000(4) 0.010(5) C8 0.035(5) 0.051(6) 0.036(5) 0.000(4) 0.007(4) 0.010(5) O9 0.055(5) 0.079(6) 0.168(9) -0.033(6) 0.034(6) 0.006(5) C9 0.052(7) 0.056(7) 0.084(8) -0.022(6) 0.003(6) 0.007(6) O10 0.099(6) 0.052(5) 0.100(6) -0.033(4) 0.016(5) -0.020(5) C10 0.077(8) 0.049(6) 0.061(7) -0.002(5) 0.011(6) 0.002(6) O11 0.201(11) 0.079(6) 0.063(5) 0.008(5) -0.025(6) 0.009(7) C11 0.091(9) 0.045(6) 0.059(6) -0.015(5) -0.009(6) 0.005(6) O12 0.104(7) 0.163(9) 0.052(5) -0.012(5) 0.025(5) -0.049(7) C12 0.080(8) 0.079(8) 0.036(5) -0.005(5) 0.005(5) -0.025(7) O13 0.101(7) 0.085(6) 0.098(6) 0.013(5) -0.033(6) 0.011(6) C13 0.072(8) 0.063(7) 0.052(6) 0.006(5) -0.025(6) -0.002(6) O14 0.126(8) 0.104(7) 0.063(5) -0.033(5) 0.003(5) -0.056(6) C14 0.066(7) 0.083(8) 0.044(6) -0.013(6) 0.005(5) -0.020(7) C21 0.038(4) 0.051(5) 0.030(4) -0.003(4) -0.002(4) 0.000(4) C22 0.038(5) 0.079(7) 0.034(4) -0.008(5) -0.006(4) -0.008(5) C23 0.046(5) 0.108(9) 0.047(5) 0.000(6) -0.012(4) -0.003(6) C24 0.080(6) 0.111(9) 0.032(5) -0.003(6) -0.014(5) -0.003(7) C25 0.076(6) 0.096(8) 0.031(4) 0.008(5) 0.008(5) -0.002(7) C26 0.046(5) 0.079(7) 0.035(4) -0.004(5) 0.007(4) 0.002(5) C31 0.060(6) 0.035(5) 0.056(5) 0.004(4) 0.022(5) 0.003(5) C32 0.051(6) 0.040(5) 0.062(6) -0.003(4) 0.013(5) 0.005(5) C33 0.113(10) 0.041(5) 0.087(7) -0.008(5) 0.031(7) 0.009(6) C34 0.127(10) 0.053(6) 0.058(6) 0.010(5) 0.001(6) 0.023(7) C35 0.106(9) 0.041(5) 0.063(6) 0.006(5) 0.014(6) -0.020(6) C36 0.092(8) 0.042(5) 0.061(6) 0.010(5) 0.023(6) 0.003(6) C41 0.064(7) 0.083(8) 0.095(9) -0.035(7) 0.010(6) -0.042(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 Re1 C1 1.909(10) . ? Re1 C4 1.932(9) . ? Re1 C3 2.006(10) . ? Re1 C2 2.007(10) . ? Re1 P1 2.529(2) . ? Re1 Se1 2.6270(11) . ? Re2 C7 1.926(9) . ? Re2 C6 1.962(9) . ? Re2 C8 1.999(9) . ? Re2 C5 2.012(10) . ? Re2 P1 2.543(2) . ? Re2 Se1 2.6585(10) . ? Se1 Fe2 2.3924(15) . ? Se1 Fe1 2.4139(15) . ? Se2 C41 1.952(9) . ? Se2 Fe1 2.3599(19) . ? Se2 Fe2 2.3620(17) . ? Fe1 C9 1.757(11) . ? Fe1 C10 1.786(11) . ? Fe1 C11 1.800(11) . ? Fe1 Fe2 2.5762(18) . ? Fe2 C13 1.773(12) . ? Fe2 C12 1.775(11) . ? Fe2 C14 1.776(10) . ? P1 C21 1.875(8) . ? P1 C31 1.880(8) . ? O1 C1 1.177(10) . ? O2 C2 1.124(10) . ? O3 C3 1.119(10) . ? O4 C4 1.137(10) . ? O5 C5 1.137(10) . ? O6 C6 1.138(10) . ? O7 C7 1.150(10) . ? O8 C8 1.125(9) . ? O9 C9 1.132(11) . ? O10 C10 1.129(11) . ? O11 C11 1.127(11) . ? O12 C12 1.127(11) . ? O13 C13 1.139(12) . ? O14 C14 1.128(10) . ? C21 C22 1.531(11) . ? C21 C26 1.535(10) . ? C21 H21 0.9800 . ? C22 C23 1.551(11) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.519(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.494(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.520(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C31 C36 1.459(11) . ? C31 C32 1.524(11) . ? C31 H31 0.9800 . ? C32 C33 1.514(12) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.489(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.549(14) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.534(12) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? 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 C1 Re1 C4 87.2(4) . . ? C1 Re1 C3 95.6(4) . . ? C4 Re1 C3 89.2(4) . . ? C1 Re1 C2 92.8(4) . . ? C4 Re1 C2 89.3(4) . . ? C3 Re1 C2 171.3(4) . . ? C1 Re1 P1 93.1(3) . . ? C4 Re1 P1 176.0(3) . . ? C3 Re1 P1 86.9(3) . . ? C2 Re1 P1 94.6(3) . . ? C1 Re1 Se1 172.0(2) . . ? C4 Re1 Se1 100.7(3) . . ? C3 Re1 Se1 83.3(3) . . ? C2 Re1 Se1 88.6(3) . . ? P1 Re1 Se1 78.99(6) . . ? C7 Re2 C6 86.3(4) . . ? C7 Re2 C8 90.1(4) . . ? C6 Re2 C8 91.9(4) . . ? C7 Re2 C5 92.8(4) . . ? C6 Re2 C5 89.2(3) . . ? C8 Re2 C5 177.0(3) . . ? C7 Re2 P1 96.7(3) . . ? C6 Re2 P1 176.2(3) . . ? C8 Re2 P1 90.5(3) . . ? C5 Re2 P1 88.2(2) . . ? C7 Re2 Se1 174.6(3) . . ? C6 Re2 Se1 98.9(3) . . ? C8 Re2 Se1 88.5(2) . . ? C5 Re2 Se1 88.6(3) . . ? P1 Re2 Se1 78.18(5) . . ? Fe2 Se1 Fe1 64.82(5) . . ? Fe2 Se1 Re1 125.46(5) . . ? Fe1 Se1 Re1 122.41(5) . . ? Fe2 Se1 Re2 121.57(5) . . ? Fe1 Se1 Re2 124.83(5) . . ? Re1 Se1 Re2 98.20(3) . . ? C41 Se2 Fe1 113.8(3) . . ? C41 Se2 Fe2 112.7(3) . . ? Fe1 Se2 Fe2 66.13(6) . . ? C9 Fe1 C10 89.9(5) . . ? C9 Fe1 C11 98.3(5) . . ? C10 Fe1 C11 98.2(4) . . ? C9 Fe1 Se2 159.6(4) . . ? C10 Fe1 Se2 91.1(4) . . ? C11 Fe1 Se2 101.7(4) . . ? C9 Fe1 Se1 93.0(3) . . ? C10 Fe1 Se1 157.2(3) . . ? C11 Fe1 Se1 103.7(3) . . ? Se2 Fe1 Se1 78.56(5) . . ? C9 Fe1 Fe2 102.8(4) . . ? C10 Fe1 Fe2 100.2(3) . . ? C11 Fe1 Fe2 151.9(3) . . ? Se2 Fe1 Fe2 56.97(5) . . ? Se1 Fe1 Fe2 57.19(4) . . ? C13 Fe2 C12 100.2(5) . . ? C13 Fe2 C14 100.2(5) . . ? C12 Fe2 C14 91.5(5) . . ? C13 Fe2 Se2 96.6(4) . . ? C12 Fe2 Se2 161.8(4) . . ? C14 Fe2 Se2 92.4(3) . . ? C13 Fe2 Se1 100.7(3) . . ? C12 Fe2 Se1 91.0(3) . . ? C14 Fe2 Se1 158.2(4) . . ? Se2 Fe2 Se1 78.95(5) . . ? C13 Fe2 Fe1 146.8(4) . . ? C12 Fe2 Fe1 104.9(4) . . ? C14 Fe2 Fe1 100.5(4) . . ? Se2 Fe2 Fe1 56.90(5) . . ? Se1 Fe2 Fe1 57.99(5) . . ? C21 P1 C31 103.3(4) . . ? C21 P1 Re1 109.4(3) . . ? C31 P1 Re1 115.3(3) . . ? C21 P1 Re2 110.0(3) . . ? C31 P1 Re2 115.0(3) . . ? Re1 P1 Re2 103.94(8) . . ? O1 C1 Re1 178.6(8) . . ? O2 C2 Re1 176.9(9) . . ? O3 C3 Re1 174.6(9) . . ? O4 C4 Re1 174.8(9) . . ? O5 C5 Re2 177.3(9) . . ? O6 C6 Re2 172.1(9) . . ? O7 C7 Re2 177.0(8) . . ? O8 C8 Re2 178.9(9) . . ? O9 C9 Fe1 176.9(12) . . ? O10 C10 Fe1 179.2(11) . . ? O11 C11 Fe1 177.1(11) . . ? O12 C12 Fe2 178.3(12) . . ? O13 C13 Fe2 176.4(11) . . ? O14 C14 Fe2 179.5(10) . . ? C22 C21 C26 108.6(7) . . ? C22 C21 P1 114.9(6) . . ? C26 C21 P1 114.5(6) . . ? C22 C21 H21 106.0 . . ? C26 C21 H21 106.0 . . ? P1 C21 H21 106.0 . . ? C21 C22 C23 111.1(7) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 110.1(8) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 112.9(9) . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 110.5(8) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C21 112.7(8) . . ? C25 C26 H26A 109.0 . . ? C21 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? C21 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C36 C31 C32 110.8(8) . . ? C36 C31 P1 117.1(6) . . ? C32 C31 P1 114.7(6) . . ? C36 C31 H31 104.1 . . ? C32 C31 H31 104.1 . . ? P1 C31 H31 104.1 . . ? C33 C32 C31 112.7(8) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 112.8(9) . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? C32 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 C35 110.5(9) . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 111.4(9) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 114.6(8) . . ? C31 C36 H36A 108.6 . . ? C35 C36 H36A 108.6 . . ? C31 C36 H36B 108.6 . . ? C35 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? Se2 C41 H41A 109.5 . . ? Se2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Se2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 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 C1 Re1 Se1 Fe2 150.6(19) . . . . ? C4 Re1 Se1 Fe2 -39.1(3) . . . . ? C3 Re1 Se1 Fe2 -127.0(3) . . . . ? C2 Re1 Se1 Fe2 49.9(3) . . . . ? P1 Re1 Se1 Fe2 144.91(8) . . . . ? C1 Re1 Se1 Fe1 -128.9(19) . . . . ? C4 Re1 Se1 Fe1 41.3(3) . . . . ? C3 Re1 Se1 Fe1 -46.6(3) . . . . ? C2 Re1 Se1 Fe1 130.4(3) . . . . ? P1 Re1 Se1 Fe1 -134.67(7) . . . . ? C1 Re1 Se1 Re2 11.9(19) . . . . ? C4 Re1 Se1 Re2 -177.9(3) . . . . ? C3 Re1 Se1 Re2 94.2(3) . . . . ? C2 Re1 Se1 Re2 -88.8(3) . . . . ? P1 Re1 Se1 Re2 6.14(5) . . . . ? C7 Re2 Se1 Fe2 -163(3) . . . . ? C6 Re2 Se1 Fe2 30.4(3) . . . . ? C8 Re2 Se1 Fe2 122.0(3) . . . . ? C5 Re2 Se1 Fe2 -58.6(2) . . . . ? P1 Re2 Se1 Fe2 -147.07(7) . . . . ? C7 Re2 Se1 Fe1 117(3) . . . . ? C6 Re2 Se1 Fe1 -49.2(3) . . . . ? C8 Re2 Se1 Fe1 42.5(3) . . . . ? C5 Re2 Se1 Fe1 -138.2(2) . . . . ? P1 Re2 Se1 Fe1 133.34(7) . . . . ? C7 Re2 Se1 Re1 -22(3) . . . . ? C6 Re2 Se1 Re1 171.3(3) . . . . ? C8 Re2 Se1 Re1 -97.0(3) . . . . ? C5 Re2 Se1 Re1 82.3(2) . . . . ? P1 Re2 Se1 Re1 -6.12(5) . . . . ? C41 Se2 Fe1 C9 96.7(10) . . . . ? Fe2 Se2 Fe1 C9 -8.7(10) . . . . ? C41 Se2 Fe1 C10 3.9(5) . . . . ? Fe2 Se2 Fe1 C10 -101.4(3) . . . . ? C41 Se2 Fe1 C11 -94.7(5) . . . . ? Fe2 Se2 Fe1 C11 159.9(3) . . . . ? C41 Se2 Fe1 Se1 163.5(4) . . . . ? Fe2 Se2 Fe1 Se1 58.13(5) . . . . ? C41 Se2 Fe1 Fe2 105.4(4) . . . . ? Fe2 Se1 Fe1 C9 103.4(4) . . . . ? Re1 Se1 Fe1 C9 -14.1(4) . . . . ? Re2 Se1 Fe1 C9 -144.4(4) . . . . ? Fe2 Se1 Fe1 C10 6.6(9) . . . . ? Re1 Se1 Fe1 C10 -110.9(9) . . . . ? Re2 Se1 Fe1 C10 118.8(9) . . . . ? Fe2 Se1 Fe1 C11 -157.4(4) . . . . ? Re1 Se1 Fe1 C11 85.2(4) . . . . ? Re2 Se1 Fe1 C11 -45.2(4) . . . . ? Fe2 Se1 Fe1 Se2 -57.91(5) . . . . ? Re1 Se1 Fe1 Se2 -175.36(4) . . . . ? Re2 Se1 Fe1 Se2 54.28(6) . . . . ? Re1 Se1 Fe1 Fe2 -117.45(6) . . . . ? Re2 Se1 Fe1 Fe2 112.19(6) . . . . ? C41 Se2 Fe2 C13 94.4(5) . . . . ? Fe1 Se2 Fe2 C13 -158.5(3) . . . . ? C41 Se2 Fe2 C12 -108.4(11) . . . . ? Fe1 Se2 Fe2 C12 -1.3(11) . . . . ? C41 Se2 Fe2 C14 -6.2(5) . . . . ? Fe1 Se2 Fe2 C14 100.9(4) . . . . ? C41 Se2 Fe2 Se1 -165.9(4) . . . . ? Fe1 Se2 Fe2 Se1 -58.84(5) . . . . ? C41 Se2 Fe2 Fe1 -107.1(4) . . . . ? Fe1 Se1 Fe2 C13 152.4(4) . . . . ? Re1 Se1 Fe2 C13 -94.5(4) . . . . ? Re2 Se1 Fe2 C13 35.5(4) . . . . ? Fe1 Se1 Fe2 C12 -107.0(4) . . . . ? Re1 Se1 Fe2 C12 6.1(4) . . . . ? Re2 Se1 Fe2 C12 136.1(4) . . . . ? Fe1 Se1 Fe2 C14 -10.6(9) . . . . ? Re1 Se1 Fe2 C14 102.5(9) . . . . ? Re2 Se1 Fe2 C14 -127.4(9) . . . . ? Fe1 Se1 Fe2 Se2 57.71(5) . . . . ? Re1 Se1 Fe2 Se2 170.80(5) . . . . ? Re2 Se1 Fe2 Se2 -59.16(6) . . . . ? Re1 Se1 Fe2 Fe1 113.09(6) . . . . ? Re2 Se1 Fe2 Fe1 -116.87(6) . . . . ? C9 Fe1 Fe2 C13 -141.5(7) . . . . ? C10 Fe1 Fe2 C13 126.3(7) . . . . ? C11 Fe1 Fe2 C13 -3.8(10) . . . . ? Se2 Fe1 Fe2 C13 41.6(6) . . . . ? Se1 Fe1 Fe2 C13 -56.3(6) . . . . ? C9 Fe1 Fe2 C12 -3.5(5) . . . . ? C10 Fe1 Fe2 C12 -95.8(5) . . . . ? C11 Fe1 Fe2 C12 134.1(8) . . . . ? Se2 Fe1 Fe2 C12 179.6(3) . . . . ? Se1 Fe1 Fe2 C12 81.7(3) . . . . ? C9 Fe1 Fe2 C14 90.8(5) . . . . ? C10 Fe1 Fe2 C14 -1.4(5) . . . . ? C11 Fe1 Fe2 C14 -131.5(8) . . . . ? Se2 Fe1 Fe2 C14 -86.1(3) . . . . ? Se1 Fe1 Fe2 C14 176.0(4) . . . . ? C9 Fe1 Fe2 Se2 176.9(3) . . . . ? C10 Fe1 Fe2 Se2 84.7(4) . . . . ? C11 Fe1 Fe2 Se2 -45.5(8) . . . . ? Se1 Fe1 Fe2 Se2 -97.92(6) . . . . ? C9 Fe1 Fe2 Se1 -85.2(3) . . . . ? C10 Fe1 Fe2 Se1 -177.4(4) . . . . ? C11 Fe1 Fe2 Se1 52.4(8) . . . . ? Se2 Fe1 Fe2 Se1 97.92(6) . . . . ? C1 Re1 P1 C21 -68.4(4) . . . . ? C4 Re1 P1 C21 25(4) . . . . ? C3 Re1 P1 C21 27.1(4) . . . . ? C2 Re1 P1 C21 -161.4(4) . . . . ? Se1 Re1 P1 C21 110.9(3) . . . . ? C1 Re1 P1 C31 47.5(4) . . . . ? C4 Re1 P1 C31 141(4) . . . . ? C3 Re1 P1 C31 142.9(4) . . . . ? C2 Re1 P1 C31 -45.6(5) . . . . ? Se1 Re1 P1 C31 -133.3(4) . . . . ? C1 Re1 P1 Re2 174.2(3) . . . . ? C4 Re1 P1 Re2 -92(4) . . . . ? C3 Re1 P1 Re2 -90.3(3) . . . . ? C2 Re1 P1 Re2 81.1(3) . . . . ? Se1 Re1 P1 Re2 -6.55(6) . . . . ? C7 Re2 P1 C21 68.0(4) . . . . ? C6 Re2 P1 C21 -151(4) . . . . ? C8 Re2 P1 C21 -22.2(4) . . . . ? C5 Re2 P1 C21 160.5(4) . . . . ? Se1 Re2 P1 C21 -110.5(3) . . . . ? C7 Re2 P1 C31 -48.0(4) . . . . ? C6 Re2 P1 C31 93(4) . . . . ? C8 Re2 P1 C31 -138.2(4) . . . . ? C5 Re2 P1 C31 44.5(4) . . . . ? Se1 Re2 P1 C31 133.5(3) . . . . ? C7 Re2 P1 Re1 -175.0(3) . . . . ? C6 Re2 P1 Re1 -34(4) . . . . ? C8 Re2 P1 Re1 94.8(2) . . . . ? C5 Re2 P1 Re1 -82.4(3) . . . . ? Se1 Re2 P1 Re1 6.49(6) . . . . ? C4 Re1 C1 O1 178(100) . . . . ? C3 Re1 C1 O1 -93(39) . . . . ? C2 Re1 C1 O1 89(39) . . . . ? P1 Re1 C1 O1 -6(39) . . . . ? Se1 Re1 C1 O1 -11(41) . . . . ? C1 Re1 C2 O2 121(18) . . . . ? C4 Re1 C2 O2 34(18) . . . . ? C3 Re1 C2 O2 -46(19) . . . . ? P1 Re1 C2 O2 -145(18) . . . . ? Se1 Re1 C2 O2 -66(18) . . . . ? C1 Re1 C3 O3 -170(9) . . . . ? C4 Re1 C3 O3 -83(10) . . . . ? C2 Re1 C3 O3 -3(11) . . . . ? P1 Re1 C3 O3 97(10) . . . . ? Se1 Re1 C3 O3 18(9) . . . . ? C1 Re1 C4 O4 2(11) . . . . ? C3 Re1 C4 O4 -94(11) . . . . ? C2 Re1 C4 O4 95(11) . . . . ? P1 Re1 C4 O4 -92(12) . . . . ? Se1 Re1 C4 O4 -177(11) . . . . ? C7 Re2 C5 O5 -8(17) . . . . ? C6 Re2 C5 O5 79(17) . . . . ? C8 Re2 C5 O5 -170(15) . . . . ? P1 Re2 C5 O5 -104(17) . . . . ? Se1 Re2 C5 O5 178(100) . . . . ? C7 Re2 C6 O6 4(6) . . . . ? C8 Re2 C6 O6 94(6) . . . . ? C5 Re2 C6 O6 -89(6) . . . . ? P1 Re2 C6 O6 -137(5) . . . . ? Se1 Re2 C6 O6 -178(6) . . . . ? C6 Re2 C7 O7 7(17) . . . . ? C8 Re2 C7 O7 -85(17) . . . . ? C5 Re2 C7 O7 96(17) . . . . ? P1 Re2 C7 O7 -176(100) . . . . ? Se1 Re2 C7 O7 -160(15) . . . . ? C7 Re2 C8 O8 66(41) . . . . ? C6 Re2 C8 O8 -21(41) . . . . ? C5 Re2 C8 O8 -132(39) . . . . ? P1 Re2 C8 O8 162(41) . . . . ? Se1 Re2 C8 O8 -119(41) . . . . ? C10 Fe1 C9 O9 -63(21) . . . . ? C11 Fe1 C9 O9 35(21) . . . . ? Se2 Fe1 C9 O9 -156(20) . . . . ? Se1 Fe1 C9 O9 139(21) . . . . ? Fe2 Fe1 C9 O9 -164(21) . . . . ? C9 Fe1 C10 O10 -102(89) . . . . ? C11 Fe1 C10 O10 159(89) . . . . ? Se2 Fe1 C10 O10 57(89) . . . . ? Se1 Fe1 C10 O10 -5(90) . . . . ? Fe2 Fe1 C10 O10 1(89) . . . . ? C9 Fe1 C11 O11 -48(24) . . . . ? C10 Fe1 C11 O11 43(24) . . . . ? Se2 Fe1 C11 O11 136(24) . . . . ? Se1 Fe1 C11 O11 -143(24) . . . . ? Fe2 Fe1 C11 O11 173(23) . . . . ? C13 Fe2 C12 O12 -28(39) . . . . ? C14 Fe2 C12 O12 72(39) . . . . ? Se2 Fe2 C12 O12 175(100) . . . . ? Se1 Fe2 C12 O12 -129(39) . . . . ? Fe1 Fe2 C12 O12 174(100) . . . . ? C12 Fe2 C13 O13 -138(17) . . . . ? C14 Fe2 C13 O13 129(17) . . . . ? Se2 Fe2 C13 O13 35(17) . . . . ? Se1 Fe2 C13 O13 -45(17) . . . . ? Fe1 Fe2 C13 O13 1(17) . . . . ? C13 Fe2 C14 O14 52(100) . . . . ? C12 Fe2 C14 O14 -49(100) . . . . ? Se2 Fe2 C14 O14 149(100) . . . . ? Se1 Fe2 C14 O14 -145(100) . . . . ? Fe1 Fe2 C14 O14 -155(100) . . . . ? C31 P1 C21 C22 -68.1(7) . . . . ? Re1 P1 C21 C22 55.2(7) . . . . ? Re2 P1 C21 C22 168.8(6) . . . . ? C31 P1 C21 C26 58.7(7) . . . . ? Re1 P1 C21 C26 -178.0(6) . . . . ? Re2 P1 C21 C26 -64.5(7) . . . . ? C26 C21 C22 C23 56.6(11) . . . . ? P1 C21 C22 C23 -173.7(7) . . . . ? C21 C22 C23 C24 -56.2(12) . . . . ? C22 C23 C24 C25 55.3(13) . . . . ? C23 C24 C25 C26 -55.0(14) . . . . ? C24 C25 C26 C21 56.1(12) . . . . ? C22 C21 C26 C25 -57.0(11) . . . . ? P1 C21 C26 C25 173.1(7) . . . . ? C21 P1 C31 C36 138.8(8) . . . . ? Re1 P1 C31 C36 19.5(9) . . . . ? Re2 P1 C31 C36 -101.5(8) . . . . ? C21 P1 C31 C32 -88.7(8) . . . . ? Re1 P1 C31 C32 152.0(6) . . . . ? Re2 P1 C31 C32 31.1(8) . . . . ? C36 C31 C32 C33 -52.6(12) . . . . ? P1 C31 C32 C33 172.0(7) . . . . ? C31 C32 C33 C34 54.8(13) . . . . ? C32 C33 C34 C35 -53.6(14) . . . . ? C33 C34 C35 C36 51.3(13) . . . . ? C32 C31 C36 C35 52.1(13) . . . . ? P1 C31 C36 C35 -173.7(8) . . . . ? C34 C35 C36 C31 -52.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.914 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.174 #===END data_3c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H25 Fe2 O14 P Re2 Te2' _chemical_formula_sum 'C27 H25 Fe2 O14 P Re2 Te2' _chemical_formula_weight 1343.74 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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2896(4) _cell_length_b 13.0401(6) _cell_length_c 15.9914(8) _cell_angle_alpha 68.577(1) _cell_angle_beta 87.538(1) _cell_angle_gamma 89.335(1) _cell_volume 1801.63(14) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6279 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.16 _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.477 _exptl_crystal_density_method none _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 9.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.1204 _exptl_absorpt_correction_T_max 0.7103 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 196 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 10231 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7365 _reflns_number_gt 6759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00013(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7365 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Te1 Te -0.23408(3) 0.73591(2) 0.176391(18) 0.01634(6) Uani 1 1 d . . . Te2 Te -0.37760(3) 0.75946(2) -0.01767(2) 0.02685(8) Uani 1 1 d . . . Re1 Re -0.434847(17) 0.874018(12) 0.214901(11) 0.01491(5) Uani 1 1 d . . . Re2 Re -0.090710(17) 0.684334(12) 0.336081(11) 0.01533(5) Uani 1 1 d . . . Fe1 Fe -0.11661(7) 0.74325(5) 0.02769(4) 0.02355(14) Uani 1 1 d . . . Fe2 Fe -0.30981(7) 0.58976(5) 0.11535(4) 0.02108(14) Uani 1 1 d . . . P1 P -0.26307(11) 0.83414(8) 0.34323(7) 0.0140(2) Uani 1 1 d . . . O1 O -0.2586(4) 1.0862(3) 0.1037(2) 0.0350(8) Uani 1 1 d . . . C1 C -0.3187(5) 1.0081(4) 0.1441(3) 0.0236(9) Uani 1 1 d . . . O2 O -0.6284(4) 1.0109(3) 0.2936(3) 0.0367(9) Uani 1 1 d . . . C2 C -0.5569(5) 0.9596(3) 0.2640(3) 0.0226(9) Uani 1 1 d . . . O3 O -0.6140(4) 0.6590(3) 0.3147(2) 0.0357(8) Uani 1 1 d . . . C3 C -0.5474(5) 0.7366(4) 0.2804(3) 0.0225(9) Uani 1 1 d . . . O4 O -0.6434(4) 0.9278(3) 0.0588(2) 0.0350(8) Uani 1 1 d . . . C4 C -0.5620(5) 0.9042(3) 0.1150(3) 0.0221(9) Uani 1 1 d . . . O5 O 0.0645(4) 0.6482(3) 0.5101(2) 0.0363(8) Uani 1 1 d . . . C5 C 0.0023(5) 0.6620(3) 0.4466(3) 0.0221(9) Uani 1 1 d . . . O6 O 0.1149(4) 0.5045(3) 0.3158(3) 0.0369(8) Uani 1 1 d . . . C6 C 0.0370(5) 0.5702(3) 0.3204(3) 0.0241(9) Uani 1 1 d . . . O7 O 0.1475(4) 0.8588(3) 0.2372(2) 0.0337(8) Uani 1 1 d . . . C7 C 0.0590(5) 0.7973(3) 0.2714(3) 0.0215(9) Uani 1 1 d . . . O8 O -0.3329(4) 0.5124(3) 0.4333(3) 0.0403(9) Uani 1 1 d . . . C8 C -0.2456(5) 0.5742(3) 0.3984(3) 0.0217(9) Uani 1 1 d . . . O9 O -0.0443(4) 0.9728(3) -0.0808(3) 0.0549(11) Uani 1 1 d . . . C9 C -0.0724(5) 0.8847(4) -0.0374(4) 0.0349(12) Uani 1 1 d . . . O10 O -0.0343(5) 0.6342(4) -0.0975(3) 0.0636(13) Uani 1 1 d . . . C10 C -0.0686(6) 0.6777(4) -0.0491(3) 0.0381(12) Uani 1 1 d . . . O11 O 0.1586(4) 0.6902(3) 0.1158(3) 0.0519(11) Uani 1 1 d . . . C11 C 0.0502(6) 0.7075(4) 0.0825(3) 0.0346(12) Uani 1 1 d . . . O12 O -0.1508(4) 0.4291(3) 0.2580(3) 0.0455(10) Uani 1 1 d . . . C12 C -0.2113(5) 0.4932(3) 0.2009(3) 0.0280(10) Uani 1 1 d . . . O13 O -0.6049(4) 0.5274(3) 0.1899(2) 0.0379(8) Uani 1 1 d . . . C13 C -0.4891(5) 0.5530(3) 0.1620(3) 0.0254(10) Uani 1 1 d . . . O14 O -0.2928(5) 0.4498(3) 0.0089(3) 0.0537(11) Uani 1 1 d . . . C14 C -0.2983(6) 0.5062(4) 0.0489(3) 0.0318(11) Uani 1 1 d . . . C21 C -0.3568(4) 0.8086(3) 0.4555(3) 0.0176(8) Uani 1 1 d . . . H21 H -0.3730 0.8829 0.4590 0.021 Uiso 1 1 calc R . . C22 C -0.2669(5) 0.7446(4) 0.5360(3) 0.0229(9) Uani 1 1 d . . . H22A H -0.2505 0.6691 0.5369 0.027 Uiso 1 1 calc R . . H22B H -0.1718 0.7810 0.5290 0.027 Uiso 1 1 calc R . . C23 C -0.3396(5) 0.7380(4) 0.6251(3) 0.0285(10) Uani 1 1 d . . . H23A H -0.3460 0.8128 0.6274 0.034 Uiso 1 1 calc R . . H23B H -0.2805 0.6922 0.6752 0.034 Uiso 1 1 calc R . . C24 C -0.4907(5) 0.6882(4) 0.6369(3) 0.0310(11) Uani 1 1 d . . . H24A H -0.4835 0.6099 0.6431 0.037 Uiso 1 1 calc R . . H24B H -0.5385 0.6910 0.6925 0.037 Uiso 1 1 calc R . . C25 C -0.5808(5) 0.7503(4) 0.5570(3) 0.0254(10) Uani 1 1 d . . . H25A H -0.5973 0.8263 0.5551 0.030 Uiso 1 1 calc R . . H25B H -0.6757 0.7137 0.5644 0.030 Uiso 1 1 calc R . . C26 C -0.5064(4) 0.7549(3) 0.4681(3) 0.0211(9) Uani 1 1 d . . . H26A H -0.5664 0.7976 0.4174 0.025 Uiso 1 1 calc R . . H26B H -0.4965 0.6792 0.4680 0.025 Uiso 1 1 calc R . . C31 C -0.1599(4) 0.9638(3) 0.3240(3) 0.0160(8) Uani 1 1 d . . . H31 H -0.1109 0.9834 0.2633 0.019 Uiso 1 1 calc R . . C32 C -0.0390(5) 0.9562(3) 0.3889(3) 0.0215(9) Uani 1 1 d . . . H32A H -0.0815 0.9446 0.4495 0.026 Uiso 1 1 calc R . . H32B H 0.0236 0.8926 0.3934 0.026 Uiso 1 1 calc R . . C33 C 0.0505(5) 1.0615(3) 0.3552(3) 0.0277(10) Uani 1 1 d . . . H33A H 0.0964 1.0710 0.2958 0.033 Uiso 1 1 calc R . . H33B H 0.1279 1.0554 0.3974 0.033 Uiso 1 1 calc R . . C34 C -0.0416(5) 1.1623(4) 0.3468(4) 0.0365(13) Uani 1 1 d . . . H34A H -0.0800 1.1568 0.4070 0.044 Uiso 1 1 calc R . . H34B H 0.0183 1.2298 0.3215 0.044 Uiso 1 1 calc R . . C35 C -0.1657(5) 1.1693(3) 0.2859(4) 0.0299(11) Uani 1 1 d . . . H35A H -0.2289 1.2316 0.2842 0.036 Uiso 1 1 calc R . . H35B H -0.1270 1.1835 0.2240 0.036 Uiso 1 1 calc R . . C36 C -0.2535(5) 1.0634(3) 0.3187(3) 0.0222(9) Uani 1 1 d . . . H36A H -0.3322 1.0700 0.2773 0.027 Uiso 1 1 calc R . . H36B H -0.2977 1.0519 0.3789 0.027 Uiso 1 1 calc R . . C41 C -0.3872(7) 0.7146(5) -0.1339(3) 0.0516(16) Uani 1 1 d . . . H41A H -0.3319 0.6471 -0.1241 0.077 Uiso 1 1 calc R . . H41B H -0.3463 0.7742 -0.1866 0.077 Uiso 1 1 calc R . . H41C H -0.4878 0.7021 -0.1438 0.077 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 Te1 0.01745(14) 0.01795(13) 0.01524(14) -0.00803(11) -0.00076(10) 0.00174(10) Te2 0.03627(19) 0.02577(15) 0.01938(15) -0.00870(12) -0.00684(13) 0.00190(12) Re1 0.01331(9) 0.01751(8) 0.01431(9) -0.00618(7) -0.00170(6) 0.00127(6) Re2 0.01431(9) 0.01467(8) 0.01645(9) -0.00495(7) -0.00152(6) 0.00151(6) Fe1 0.0279(4) 0.0232(3) 0.0185(3) -0.0071(3) 0.0047(3) 0.0022(3) Fe2 0.0281(4) 0.0186(3) 0.0186(3) -0.0091(3) -0.0012(3) -0.0005(2) P1 0.0150(5) 0.0143(5) 0.0128(5) -0.0051(4) -0.0005(4) 0.0002(4) O1 0.036(2) 0.0359(19) 0.0249(18) -0.0010(15) -0.0021(15) -0.0134(16) C1 0.023(2) 0.028(2) 0.019(2) -0.0065(19) -0.0060(18) 0.0006(18) O2 0.0264(19) 0.0367(19) 0.054(2) -0.0259(18) 0.0050(17) 0.0058(15) C2 0.020(2) 0.022(2) 0.024(2) -0.0061(19) -0.0017(18) -0.0006(17) O3 0.036(2) 0.0345(19) 0.036(2) -0.0130(16) 0.0035(16) -0.0124(16) C3 0.019(2) 0.031(2) 0.023(2) -0.016(2) -0.0047(18) 0.0010(18) O4 0.0270(19) 0.054(2) 0.0252(18) -0.0148(17) -0.0110(15) 0.0043(16) C4 0.019(2) 0.027(2) 0.022(2) -0.0117(19) 0.0033(18) -0.0021(17) O5 0.032(2) 0.050(2) 0.0240(19) -0.0090(17) -0.0107(15) 0.0063(16) C5 0.023(2) 0.022(2) 0.021(2) -0.0081(19) 0.0030(19) -0.0008(17) O6 0.0253(19) 0.0317(18) 0.055(2) -0.0178(17) 0.0030(17) 0.0082(14) C6 0.022(2) 0.021(2) 0.028(2) -0.0070(19) -0.0004(19) -0.0040(17) O7 0.0232(18) 0.0365(19) 0.036(2) -0.0081(16) 0.0062(15) -0.0063(15) C7 0.018(2) 0.022(2) 0.024(2) -0.0086(19) -0.0015(18) 0.0033(17) O8 0.038(2) 0.0252(18) 0.051(2) -0.0073(17) 0.0072(18) -0.0105(15) C8 0.020(2) 0.019(2) 0.026(2) -0.0079(19) -0.0033(19) 0.0050(17) O9 0.047(3) 0.033(2) 0.063(3) 0.008(2) 0.007(2) -0.0017(18) C9 0.024(3) 0.039(3) 0.037(3) -0.008(2) 0.003(2) 0.001(2) O10 0.074(3) 0.075(3) 0.059(3) -0.048(3) 0.027(2) -0.008(2) C10 0.042(3) 0.040(3) 0.031(3) -0.014(2) 0.015(2) -0.007(2) O11 0.030(2) 0.075(3) 0.044(2) -0.015(2) -0.0071(19) 0.021(2) C11 0.044(3) 0.037(3) 0.022(3) -0.011(2) 0.009(2) 0.007(2) O12 0.062(3) 0.0213(17) 0.052(3) -0.0094(17) -0.030(2) 0.0065(17) C12 0.035(3) 0.018(2) 0.035(3) -0.015(2) -0.003(2) -0.0047(18) O13 0.037(2) 0.039(2) 0.035(2) -0.0105(17) 0.0006(17) -0.0034(16) C13 0.034(3) 0.023(2) 0.020(2) -0.0094(19) -0.004(2) -0.0014(19) O14 0.078(3) 0.049(2) 0.051(3) -0.038(2) -0.005(2) 0.002(2) C14 0.043(3) 0.027(2) 0.027(3) -0.012(2) 0.000(2) -0.001(2) C21 0.019(2) 0.020(2) 0.013(2) -0.0048(17) 0.0038(16) -0.0044(15) C22 0.022(2) 0.031(2) 0.016(2) -0.0087(19) -0.0013(17) -0.0009(18) C23 0.032(3) 0.043(3) 0.014(2) -0.013(2) -0.0010(19) -0.005(2) C24 0.037(3) 0.040(3) 0.016(2) -0.009(2) 0.006(2) -0.006(2) C25 0.016(2) 0.037(3) 0.021(2) -0.008(2) 0.0035(18) -0.0029(18) C26 0.019(2) 0.027(2) 0.016(2) -0.0074(18) 0.0001(17) 0.0010(17) C31 0.017(2) 0.0102(17) 0.019(2) -0.0040(16) 0.0026(16) -0.0034(14) C32 0.023(2) 0.025(2) 0.020(2) -0.0120(19) -0.0054(18) 0.0016(17) C33 0.021(2) 0.029(2) 0.039(3) -0.018(2) -0.007(2) -0.0022(18) C34 0.028(3) 0.030(3) 0.061(4) -0.026(3) -0.006(3) -0.003(2) C35 0.027(3) 0.018(2) 0.046(3) -0.011(2) -0.004(2) -0.0010(18) C36 0.021(2) 0.019(2) 0.028(2) -0.0113(19) 0.0001(19) 0.0002(17) C41 0.093(5) 0.046(3) 0.021(3) -0.016(3) -0.010(3) -0.002(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 Te1 Fe1 2.5432(7) . ? Te1 Fe2 2.5552(6) . ? Te1 Re1 2.7811(3) . ? Te1 Re2 2.7864(3) . ? Te2 C41 2.147(5) . ? Te2 Fe2 2.5422(7) . ? Te2 Fe1 2.5448(7) . ? Re1 C2 1.919(4) . ? Re1 C4 1.948(5) . ? Re1 C3 1.995(5) . ? Re1 C1 1.999(5) . ? Re1 P1 2.5516(10) . ? Re2 C5 1.925(5) . ? Re2 C6 1.973(4) . ? Re2 C7 1.997(4) . ? Re2 C8 2.001(4) . ? Re2 P1 2.5432(10) . ? Fe1 C10 1.774(5) . ? Fe1 C11 1.786(6) . ? Fe1 C9 1.798(5) . ? Fe1 Fe2 2.6476(9) . ? Fe2 C12 1.766(5) . ? Fe2 C14 1.778(5) . ? Fe2 C13 1.792(5) . ? P1 C31 1.872(4) . ? P1 C21 1.879(4) . ? O1 C1 1.126(5) . ? O2 C2 1.143(5) . ? O3 C3 1.135(5) . ? O4 C4 1.151(5) . ? O5 C5 1.145(5) . ? O6 C6 1.136(5) . ? O7 C7 1.129(5) . ? O8 C8 1.125(5) . ? O9 C9 1.131(6) . ? O10 C10 1.148(6) . ? O11 C11 1.140(6) . ? O12 C12 1.150(5) . ? O13 C13 1.152(6) . ? O14 C14 1.137(5) . ? C21 C22 1.531(6) . ? C21 C26 1.536(6) . ? C22 C23 1.524(6) . ? C23 C24 1.529(7) . ? C24 C25 1.520(6) . ? C25 C26 1.534(6) . ? C31 C36 1.532(5) . ? C31 C32 1.539(6) . ? C32 C33 1.521(6) . ? C33 C34 1.527(6) . ? C34 C35 1.522(6) . ? C35 C36 1.519(6) . ? 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 Fe1 Te1 Fe2 62.57(2) . . ? Fe1 Te1 Re1 130.889(17) . . ? Fe2 Te1 Re1 121.434(18) . . ? Fe1 Te1 Re2 124.692(18) . . ? Fe2 Te1 Re2 122.664(17) . . ? Re1 Te1 Re2 95.339(9) . . ? C41 Te2 Fe2 108.45(15) . . ? C41 Te2 Fe1 107.74(18) . . ? Fe2 Te2 Fe1 62.73(2) . . ? C2 Re1 C4 89.99(18) . . ? C2 Re1 C3 92.32(18) . . ? C4 Re1 C3 88.65(18) . . ? C2 Re1 C1 90.58(18) . . ? C4 Re1 C1 89.94(18) . . ? C3 Re1 C1 176.78(17) . . ? C2 Re1 P1 91.27(13) . . ? C4 Re1 P1 178.56(13) . . ? C3 Re1 P1 91.99(12) . . ? C1 Re1 P1 89.35(12) . . ? C2 Re1 Te1 168.78(13) . . ? C4 Re1 Te1 100.93(12) . . ? C3 Re1 Te1 85.44(12) . . ? C1 Re1 Te1 91.99(13) . . ? P1 Re1 Te1 77.85(2) . . ? C5 Re2 C6 87.86(18) . . ? C5 Re2 C7 88.75(18) . . ? C6 Re2 C7 88.95(17) . . ? C5 Re2 C8 92.67(18) . . ? C6 Re2 C8 92.29(17) . . ? C7 Re2 C8 178.15(16) . . ? C5 Re2 P1 96.95(12) . . ? C6 Re2 P1 175.17(13) . . ? C7 Re2 P1 90.69(12) . . ? C8 Re2 P1 87.96(11) . . ? C5 Re2 Te1 174.54(12) . . ? C6 Re2 Te1 97.29(13) . . ? C7 Re2 Te1 89.54(12) . . ? C8 Re2 Te1 88.94(12) . . ? P1 Re2 Te1 77.89(2) . . ? C10 Fe1 C11 92.4(2) . . ? C10 Fe1 C9 101.8(2) . . ? C11 Fe1 C9 97.0(2) . . ? C10 Fe1 Te1 150.06(17) . . ? C11 Fe1 Te1 88.42(15) . . ? C9 Fe1 Te1 107.77(17) . . ? C10 Fe1 Te2 91.28(19) . . ? C11 Fe1 Te2 166.74(16) . . ? C9 Fe1 Te2 94.71(16) . . ? Te1 Fe1 Te2 82.04(2) . . ? C10 Fe1 Fe2 92.69(17) . . ? C11 Fe1 Fe2 108.50(17) . . ? C9 Fe1 Fe2 150.09(16) . . ? Te1 Fe1 Fe2 58.94(2) . . ? Te2 Fe1 Fe2 58.59(2) . . ? C12 Fe2 C14 91.6(2) . . ? C12 Fe2 C13 99.7(2) . . ? C14 Fe2 C13 98.3(2) . . ? C12 Fe2 Te2 162.32(15) . . ? C14 Fe2 Te2 92.53(16) . . ? C13 Fe2 Te2 96.67(14) . . ? C12 Fe2 Te1 87.78(13) . . ? C14 Fe2 Te1 157.62(17) . . ? C13 Fe2 Te1 103.87(13) . . ? Te2 Fe2 Te1 81.860(19) . . ? C12 Fe2 Fe1 103.66(15) . . ? C14 Fe2 Fe1 100.11(17) . . ? C13 Fe2 Fe1 149.65(14) . . ? Te2 Fe2 Fe1 58.69(2) . . ? Te1 Fe2 Fe1 58.491(19) . . ? C31 P1 C21 102.10(18) . . ? C31 P1 Re2 109.66(13) . . ? C21 P1 Re2 115.75(13) . . ? C31 P1 Re1 107.47(13) . . ? C21 P1 Re1 113.66(13) . . ? Re2 P1 Re1 107.78(4) . . ? O1 C1 Re1 177.0(4) . . ? O2 C2 Re1 179.3(4) . . ? O3 C3 Re1 177.4(4) . . ? O4 C4 Re1 174.2(4) . . ? O5 C5 Re2 176.3(4) . . ? O6 C6 Re2 175.8(4) . . ? O7 C7 Re2 177.3(4) . . ? O8 C8 Re2 179.9(5) . . ? O9 C9 Fe1 177.8(5) . . ? O10 C10 Fe1 178.2(5) . . ? O11 C11 Fe1 176.6(5) . . ? O12 C12 Fe2 178.0(5) . . ? O13 C13 Fe2 177.5(4) . . ? O14 C14 Fe2 177.6(5) . . ? C22 C21 C26 109.1(3) . . ? C22 C21 P1 114.2(3) . . ? C26 C21 P1 115.0(3) . . ? C23 C22 C21 112.4(4) . . ? C22 C23 C24 111.2(4) . . ? C25 C24 C23 110.9(4) . . ? C24 C25 C26 111.5(4) . . ? C25 C26 C21 110.8(3) . . ? C36 C31 C32 107.9(3) . . ? C36 C31 P1 114.6(3) . . ? C32 C31 P1 116.6(3) . . ? C33 C32 C31 110.2(3) . . ? C32 C33 C34 111.6(4) . . ? C35 C34 C33 109.8(4) . . ? C36 C35 C34 111.2(4) . . ? C35 C36 C31 111.5(4) . . ? 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 Fe1 Te1 Re1 C2 -153.4(7) . . . . ? Fe2 Te1 Re1 C2 127.2(7) . . . . ? Re2 Te1 Re1 C2 -6.6(7) . . . . ? Fe1 Te1 Re1 C4 40.03(13) . . . . ? Fe2 Te1 Re1 C4 -39.32(13) . . . . ? Re2 Te1 Re1 C4 -173.14(13) . . . . ? Fe1 Te1 Re1 C3 127.77(12) . . . . ? Fe2 Te1 Re1 C3 48.42(12) . . . . ? Re2 Te1 Re1 C3 -85.40(12) . . . . ? Fe1 Te1 Re1 C1 -50.30(13) . . . . ? Fe2 Te1 Re1 C1 -129.64(12) . . . . ? Re2 Te1 Re1 C1 96.53(12) . . . . ? Fe1 Te1 Re1 P1 -139.20(3) . . . . ? Fe2 Te1 Re1 P1 141.45(3) . . . . ? Re2 Te1 Re1 P1 7.63(2) . . . . ? Fe1 Te1 Re2 C5 123.0(14) . . . . ? Fe2 Te1 Re2 C5 -159.8(14) . . . . ? Re1 Te1 Re2 C5 -26.8(14) . . . . ? Fe1 Te1 Re2 C6 -37.54(13) . . . . ? Fe2 Te1 Re2 C6 39.65(13) . . . . ? Re1 Te1 Re2 C6 172.66(13) . . . . ? Fe1 Te1 Re2 C7 51.34(12) . . . . ? Fe2 Te1 Re2 C7 128.53(12) . . . . ? Re1 Te1 Re2 C7 -98.46(11) . . . . ? Fe1 Te1 Re2 C8 -129.71(11) . . . . ? Fe2 Te1 Re2 C8 -52.52(11) . . . . ? Re1 Te1 Re2 C8 80.49(11) . . . . ? Fe1 Te1 Re2 P1 142.15(3) . . . . ? Fe2 Te1 Re2 P1 -140.66(3) . . . . ? Re1 Te1 Re2 P1 -7.66(2) . . . . ? Fe2 Te1 Fe1 C10 -20.6(4) . . . . ? Re1 Te1 Fe1 C10 -129.8(4) . . . . ? Re2 Te1 Fe1 C10 91.7(4) . . . . ? Fe2 Te1 Fe1 C11 -112.77(16) . . . . ? Re1 Te1 Fe1 C11 138.09(16) . . . . ? Re2 Te1 Fe1 C11 -0.42(16) . . . . ? Fe2 Te1 Fe1 C9 150.41(17) . . . . ? Re1 Te1 Fe1 C9 41.27(18) . . . . ? Re2 Te1 Fe1 C9 -97.24(17) . . . . ? Fe2 Te1 Fe1 Te2 57.98(2) . . . . ? Re1 Te1 Fe1 Te2 -51.16(3) . . . . ? Re2 Te1 Fe1 Te2 170.333(13) . . . . ? Re1 Te1 Fe1 Fe2 -109.14(2) . . . . ? Re2 Te1 Fe1 Fe2 112.35(2) . . . . ? C41 Te2 Fe1 C10 -9.7(2) . . . . ? Fe2 Te2 Fe1 C10 92.37(17) . . . . ? C41 Te2 Fe1 C11 -115.9(7) . . . . ? Fe2 Te2 Fe1 C11 -13.9(7) . . . . ? C41 Te2 Fe1 C9 92.3(2) . . . . ? Fe2 Te2 Fe1 C9 -165.65(17) . . . . ? C41 Te2 Fe1 Te1 -160.38(16) . . . . ? Fe2 Te2 Fe1 Te1 -58.325(19) . . . . ? C41 Te2 Fe1 Fe2 -102.06(16) . . . . ? C41 Te2 Fe2 C12 104.1(5) . . . . ? Fe1 Te2 Fe2 C12 3.2(5) . . . . ? C41 Te2 Fe2 C14 0.6(3) . . . . ? Fe1 Te2 Fe2 C14 -100.30(17) . . . . ? C41 Te2 Fe2 C13 -98.0(2) . . . . ? Fe1 Te2 Fe2 C13 161.05(14) . . . . ? C41 Te2 Fe2 Te1 158.85(19) . . . . ? Fe1 Te2 Fe2 Te1 57.93(2) . . . . ? C41 Te2 Fe2 Fe1 100.9(2) . . . . ? Fe1 Te1 Fe2 C12 107.52(16) . . . . ? Re1 Te1 Fe2 C12 -129.31(16) . . . . ? Re2 Te1 Fe2 C12 -7.89(16) . . . . ? Fe1 Te1 Fe2 C14 18.6(4) . . . . ? Re1 Te1 Fe2 C14 141.7(4) . . . . ? Re2 Te1 Fe2 C14 -96.8(4) . . . . ? Fe1 Te1 Fe2 C13 -153.03(15) . . . . ? Re1 Te1 Fe2 C13 -29.86(15) . . . . ? Re2 Te1 Fe2 C13 91.57(15) . . . . ? Fe1 Te1 Fe2 Te2 -58.12(2) . . . . ? Re1 Te1 Fe2 Te2 65.05(2) . . . . ? Re2 Te1 Fe2 Te2 -173.523(14) . . . . ? Re1 Te1 Fe2 Fe1 123.17(2) . . . . ? Re2 Te1 Fe2 Fe1 -115.40(2) . . . . ? C10 Fe1 Fe2 C12 91.1(2) . . . . ? C11 Fe1 Fe2 C12 -2.3(2) . . . . ? C9 Fe1 Fe2 C12 -149.3(4) . . . . ? Te1 Fe1 Fe2 C12 -78.71(15) . . . . ? Te2 Fe1 Fe2 C12 -179.00(15) . . . . ? C10 Fe1 Fe2 C14 -3.1(2) . . . . ? C11 Fe1 Fe2 C14 -96.5(2) . . . . ? C9 Fe1 Fe2 C14 116.5(4) . . . . ? Te1 Fe1 Fe2 C14 -172.92(16) . . . . ? Te2 Fe1 Fe2 C14 86.79(16) . . . . ? C10 Fe1 Fe2 C13 -129.5(3) . . . . ? C11 Fe1 Fe2 C13 137.0(3) . . . . ? C9 Fe1 Fe2 C13 -10.0(5) . . . . ? Te1 Fe1 Fe2 C13 60.6(3) . . . . ? Te2 Fe1 Fe2 C13 -39.7(3) . . . . ? C10 Fe1 Fe2 Te2 -89.86(18) . . . . ? C11 Fe1 Fe2 Te2 176.67(16) . . . . ? C9 Fe1 Fe2 Te2 29.7(4) . . . . ? Te1 Fe1 Fe2 Te2 100.28(2) . . . . ? C10 Fe1 Fe2 Te1 169.86(18) . . . . ? C11 Fe1 Fe2 Te1 76.39(16) . . . . ? C9 Fe1 Fe2 Te1 -70.6(4) . . . . ? Te2 Fe1 Fe2 Te1 -100.28(2) . . . . ? C5 Re2 P1 C31 70.23(19) . . . . ? C6 Re2 P1 C31 -104.3(15) . . . . ? C7 Re2 P1 C31 -18.59(18) . . . . ? C8 Re2 P1 C31 162.68(19) . . . . ? Te1 Re2 P1 C31 -107.97(14) . . . . ? C5 Re2 P1 C21 -44.57(19) . . . . ? C6 Re2 P1 C21 140.9(15) . . . . ? C7 Re2 P1 C21 -133.39(19) . . . . ? C8 Re2 P1 C21 47.88(19) . . . . ? Te1 Re2 P1 C21 137.23(14) . . . . ? C5 Re2 P1 Re1 -173.07(13) . . . . ? C6 Re2 P1 Re1 12.4(15) . . . . ? C7 Re2 P1 Re1 98.11(13) . . . . ? C8 Re2 P1 Re1 -80.62(13) . . . . ? Te1 Re2 P1 Re1 8.73(3) . . . . ? C2 Re1 P1 C31 -73.37(19) . . . . ? C4 Re1 P1 C31 78(5) . . . . ? C3 Re1 P1 C31 -165.73(18) . . . . ? C1 Re1 P1 C31 17.20(18) . . . . ? Te1 Re1 P1 C31 109.37(13) . . . . ? C2 Re1 P1 C21 38.83(19) . . . . ? C4 Re1 P1 C21 -170(5) . . . . ? C3 Re1 P1 C21 -53.53(18) . . . . ? C1 Re1 P1 C21 129.39(19) . . . . ? Te1 Re1 P1 C21 -138.43(14) . . . . ? C2 Re1 P1 Re2 168.51(13) . . . . ? C4 Re1 P1 Re2 -41(5) . . . . ? C3 Re1 P1 Re2 76.15(12) . . . . ? C1 Re1 P1 Re2 -100.92(13) . . . . ? Te1 Re1 P1 Re2 -8.75(3) . . . . ? C2 Re1 C1 O1 -37(8) . . . . ? C4 Re1 C1 O1 53(8) . . . . ? C3 Re1 C1 O1 118(7) . . . . ? P1 Re1 C1 O1 -128(8) . . . . ? Te1 Re1 C1 O1 154(8) . . . . ? C4 Re1 C2 O2 -144(39) . . . . ? C3 Re1 C2 O2 127(39) . . . . ? C1 Re1 C2 O2 -54(39) . . . . ? P1 Re1 C2 O2 35(39) . . . . ? Te1 Re1 C2 O2 49(39) . . . . ? C2 Re1 C3 O3 100(9) . . . . ? C4 Re1 C3 O3 10(9) . . . . ? C1 Re1 C3 O3 -54(10) . . . . ? P1 Re1 C3 O3 -169(9) . . . . ? Te1 Re1 C3 O3 -91(9) . . . . ? C2 Re1 C4 O4 5(4) . . . . ? C3 Re1 C4 O4 98(4) . . . . ? C1 Re1 C4 O4 -85(4) . . . . ? P1 Re1 C4 O4 -146(4) . . . . ? Te1 Re1 C4 O4 -177(4) . . . . ? C6 Re2 C5 O5 39(6) . . . . ? C7 Re2 C5 O5 -50(6) . . . . ? C8 Re2 C5 O5 131(6) . . . . ? P1 Re2 C5 O5 -140(6) . . . . ? Te1 Re2 C5 O5 -121(5) . . . . ? C5 Re2 C6 O6 -7(5) . . . . ? C7 Re2 C6 O6 82(5) . . . . ? C8 Re2 C6 O6 -100(5) . . . . ? P1 Re2 C6 O6 167(4) . . . . ? Te1 Re2 C6 O6 171(5) . . . . ? C5 Re2 C7 O7 34(8) . . . . ? C6 Re2 C7 O7 -54(8) . . . . ? C8 Re2 C7 O7 174(7) . . . . ? P1 Re2 C7 O7 131(8) . . . . ? Te1 Re2 C7 O7 -151(8) . . . . ? C5 Re2 C8 O8 145(100) . . . . ? C6 Re2 C8 O8 -127(100) . . . . ? C7 Re2 C8 O8 5(100) . . . . ? P1 Re2 C8 O8 48(100) . . . . ? Te1 Re2 C8 O8 -30(100) . . . . ? C10 Fe1 C9 O9 15(12) . . . . ? C11 Fe1 C9 O9 109(12) . . . . ? Te1 Fe1 C9 O9 -160(12) . . . . ? Te2 Fe1 C9 O9 -77(12) . . . . ? Fe2 Fe1 C9 O9 -102(12) . . . . ? C11 Fe1 C10 O10 7(16) . . . . ? C9 Fe1 C10 O10 104(16) . . . . ? Te1 Fe1 C10 O10 -84(16) . . . . ? Te2 Fe1 C10 O10 -161(16) . . . . ? Fe2 Fe1 C10 O10 -102(16) . . . . ? C10 Fe1 C11 O11 111(7) . . . . ? C9 Fe1 C11 O11 8(7) . . . . ? Te1 Fe1 C11 O11 -99(7) . . . . ? Te2 Fe1 C11 O11 -143(7) . . . . ? Fe2 Fe1 C11 O11 -156(7) . . . . ? C14 Fe2 C12 O12 -96(12) . . . . ? C13 Fe2 C12 O12 3(12) . . . . ? Te2 Fe2 C12 O12 161(11) . . . . ? Te1 Fe2 C12 O12 107(12) . . . . ? Fe1 Fe2 C12 O12 163(12) . . . . ? C12 Fe2 C13 O13 -100(10) . . . . ? C14 Fe2 C13 O13 -7(10) . . . . ? Te2 Fe2 C13 O13 86(10) . . . . ? Te1 Fe2 C13 O13 169(10) . . . . ? Fe1 Fe2 C13 O13 120(10) . . . . ? C12 Fe2 C14 O14 53(12) . . . . ? C13 Fe2 C14 O14 -47(12) . . . . ? Te2 Fe2 C14 O14 -144(12) . . . . ? Te1 Fe2 C14 O14 141(11) . . . . ? Fe1 Fe2 C14 O14 157(12) . . . . ? C31 P1 C21 C22 -86.0(3) . . . . ? Re2 P1 C21 C22 33.0(3) . . . . ? Re1 P1 C21 C22 158.6(2) . . . . ? C31 P1 C21 C26 146.7(3) . . . . ? Re2 P1 C21 C26 -94.3(3) . . . . ? Re1 P1 C21 C26 31.3(3) . . . . ? C26 C21 C22 C23 -56.7(4) . . . . ? P1 C21 C22 C23 173.0(3) . . . . ? C21 C22 C23 C24 55.7(5) . . . . ? C22 C23 C24 C25 -54.1(5) . . . . ? C23 C24 C25 C26 55.4(5) . . . . ? C24 C25 C26 C21 -57.5(5) . . . . ? C22 C21 C26 C25 56.9(4) . . . . ? P1 C21 C26 C25 -173.2(3) . . . . ? C21 P1 C31 C36 -61.7(3) . . . . ? Re2 P1 C31 C36 175.0(3) . . . . ? Re1 P1 C31 C36 58.1(3) . . . . ? C21 P1 C31 C32 65.7(3) . . . . ? Re2 P1 C31 C32 -57.6(3) . . . . ? Re1 P1 C31 C32 -174.5(3) . . . . ? C36 C31 C32 C33 -59.1(5) . . . . ? P1 C31 C32 C33 170.3(3) . . . . ? C31 C32 C33 C34 59.1(5) . . . . ? C32 C33 C34 C35 -56.1(6) . . . . ? C33 C34 C35 C36 55.0(6) . . . . ? C34 C35 C36 C31 -58.1(5) . . . . ? C32 C31 C36 C35 59.0(5) . . . . ? P1 C31 C36 C35 -169.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 0.979 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.147 #===END data_4a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Fe4 O28 P2 Re4 S4, 0.5 C H2 Cl2' _chemical_formula_sum 'C52.50 H45 Cl Fe4 O28 P2 Re4 S4' _chemical_formula_weight 2317.71 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' '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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.793(3) _cell_length_b 15.605(5) _cell_length_c 32.027(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.01(1) _cell_angle_gamma 90.00 _cell_volume 7231(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.847 _cell_measurement_theta_max 14.771 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'none' _exptl_crystal_density_diffrn 2.129 _exptl_crystal_F_000 4396 _exptl_absorpt_coefficient_mu 7.718 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.357 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 4 _diffrn_reflns_number 17654 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.1648 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15065 _reflns_number_gt 6901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0468P)^2^] 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 15065 _refine_ls_number_parameters 868 _refine_ls_number_restraints 1213 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.895 _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 Re1 Re 0.51681(4) 1.14024(4) 0.30248(2) 0.02825(15) Uani 1 1 d U A . Re2 Re 0.61477(4) 1.27570(4) 0.40522(2) 0.03155(16) Uani 1 1 d U . . Re3 Re 0.90363(4) 1.30391(4) 0.13206(2) 0.02894(15) Uani 1 1 d U . . Re4 Re 0.96907(4) 1.08190(4) 0.08856(2) 0.03021(16) Uani 1 1 d U . . Fe1 Fe 0.70547(13) 1.31896(13) 0.28456(7) 0.0296(5) Uani 1 1 d U . . Fe2 Fe 0.80764(13) 1.21267(14) 0.33132(7) 0.0302(5) Uani 1 1 d U . . Fe3 Fe 0.75052(14) 1.09747(14) 0.16233(8) 0.0354(6) Uani 1 1 d U . . Fe4 Fe 0.90563(14) 1.07737(14) 0.21000(7) 0.0321(5) Uani 1 1 d U . . S1 S 0.6542(2) 1.2356(2) 0.33386(13) 0.0281(8) Uani 1 1 d U . . S2 S 0.7343(2) 1.1835(2) 0.26443(13) 0.0297(8) Uani 1 1 d U . . S3 S 0.8127(2) 1.1889(2) 0.21587(13) 0.0305(8) Uani 1 1 d U . . S4 S 0.8835(2) 1.1419(2) 0.14337(13) 0.0307(8) Uani 1 1 d U . . P1 P 0.5102(2) 1.1491(3) 0.38053(14) 0.0300(9) Uani 1 1 d U . . P2 P 1.0266(2) 1.2342(3) 0.09927(13) 0.0277(8) Uani 1 1 d U . . O1 O 0.3439(7) 1.0312(7) 0.2718(4) 0.055(3) Uani 1 1 d U . . C1 C 0.4095(10) 1.0701(10) 0.2850(5) 0.037(3) Uani 1 1 d U . . O2 O 0.5248(7) 1.1397(8) 0.2066(4) 0.050(3) Uani 1 1 d U . . C2 C 0.5273(10) 1.1408(11) 0.2429(5) 0.039(3) Uani 1 1 d U . . O3 O 0.6488(7) 0.9821(7) 0.3187(4) 0.054(3) Uani 1 1 d U . . C3 C 0.5985(10) 1.0388(10) 0.3143(6) 0.037(3) Uani 1 1 d U . . O41 O 0.3826(16) 1.2972(15) 0.291(2) 0.052(10) Uani 0.50 1 d PDU A 1 O42 O 0.416(2) 1.3155(13) 0.2871(19) 0.061(13) Uani 0.50 1 d PDU A 2 C4 C 0.4407(11) 1.2445(10) 0.2951(5) 0.043(4) Uani 1 1 d DU . . O5 O 0.4640(8) 1.4124(8) 0.3671(4) 0.058(3) Uani 1 1 d U . . C5 C 0.5160(10) 1.3603(10) 0.3794(5) 0.036(3) Uani 1 1 d U . . O6 O 0.7760(7) 1.1583(8) 0.4490(4) 0.055(3) Uani 1 1 d U . . C6 C 0.7168(10) 1.1990(11) 0.4322(5) 0.041(3) Uani 1 1 d U . . O7 O 0.5629(9) 1.2892(9) 0.4930(4) 0.067(4) Uani 1 1 d U . . C7 C 0.5791(10) 1.2854(11) 0.4590(6) 0.045(4) Uani 1 1 d U . . O8 O 0.7390(8) 1.4343(8) 0.4284(4) 0.065(4) Uani 1 1 d U . . C8 C 0.6950(11) 1.3752(12) 0.4190(6) 0.047(4) Uani 1 1 d U . . O9 O 0.6674(8) 1.4682(7) 0.3321(4) 0.060(4) Uani 1 1 d U . . C9 C 0.6877(11) 1.4098(10) 0.3142(6) 0.039(4) Uani 1 1 d U . . O10 O 0.8557(7) 1.4033(7) 0.2537(4) 0.047(3) Uani 1 1 d U . . C10 C 0.7988(9) 1.3688(9) 0.2653(5) 0.029(3) Uani 1 1 d U . . O11 O 0.5497(8) 1.3535(8) 0.2122(5) 0.073(4) Uani 1 1 d U . . C11 C 0.6093(10) 1.3400(10) 0.2419(6) 0.044(4) Uani 1 1 d U . . O12 O 0.8805(7) 1.3398(8) 0.3964(4) 0.060(4) Uani 1 1 d U . . C12 C 0.8465(9) 1.2915(10) 0.3720(5) 0.031(3) Uani 1 1 d U . . O13 O 0.9896(7) 1.2163(8) 0.3096(4) 0.060(4) Uani 1 1 d U . . C13 C 0.9168(10) 1.2154(11) 0.3177(5) 0.040(4) Uani 1 1 d U . . O14 O 0.8341(8) 1.0510(7) 0.3794(4) 0.055(3) Uani 1 1 d U . . C14 C 0.8247(10) 1.1103(10) 0.3591(5) 0.036(3) Uani 1 1 d U . . O15 O 0.7661(8) 1.3147(9) 0.0448(4) 0.066(4) Uani 1 1 d U . . C15 C 0.8182(10) 1.3055(11) 0.0749(6) 0.041(3) Uani 1 1 d U . . O16 O 0.7339(7) 1.3743(8) 0.1629(3) 0.048(3) Uani 1 1 d U . . C16 C 0.7988(9) 1.3465(9) 0.1541(5) 0.031(3) Uani 1 1 d U . . O17 O 1.0240(8) 1.3114(8) 0.2250(4) 0.054(3) Uani 1 1 d U . . C17 C 0.9830(10) 1.3064(10) 0.1926(5) 0.033(3) Uani 1 1 d U . . O18 O 0.9618(8) 1.4903(7) 0.1218(5) 0.059(4) Uani 1 1 d U . . C18 C 0.9399(11) 1.4201(10) 0.1237(5) 0.038(3) Uani 1 1 d U . . O19 O 1.0896(7) 1.0461(8) 0.0235(4) 0.057(3) Uani 1 1 d U . . C19 C 1.0448(10) 1.0590(11) 0.0507(5) 0.037(3) Uani 1 1 d U . . O20 O 0.9026(8) 0.8938(7) 0.0749(4) 0.060(4) Uani 1 1 d U . . C20 C 0.9239(10) 0.9655(10) 0.0814(5) 0.035(3) Uani 1 1 d U . . O21 O 0.7985(8) 1.1289(9) 0.0187(5) 0.073(4) Uani 1 1 d U . . C21 C 0.8638(11) 1.1177(10) 0.0449(6) 0.040(3) Uani 1 1 d U . . O22 O 1.1253(8) 1.0144(8) 0.1621(4) 0.055(3) Uani 1 1 d U . . C22 C 1.0698(10) 1.0406(9) 0.1353(5) 0.034(3) Uani 1 1 d U . . O23 O 0.7216(8) 0.9643(9) 0.0969(5) 0.079(5) Uani 1 1 d U . . C23 C 0.7349(10) 1.0165(12) 0.1230(6) 0.050(4) Uani 1 1 d U . . O24 O 0.6051(9) 1.2110(10) 0.1172(5) 0.089(5) Uani 1 1 d U . . C24 C 0.6625(11) 1.1656(13) 0.1342(6) 0.058(5) Uani 1 1 d U . . O25 O 0.6567(8) 0.9930(8) 0.2156(4) 0.058(3) Uani 1 1 d U . . C25 C 0.6914(11) 1.0342(11) 0.1960(6) 0.047(4) Uani 1 1 d U . . O26 O 0.9343(9) 0.9088(7) 0.1761(4) 0.057(3) Uani 1 1 d U . . C26 C 0.9227(12) 0.9748(11) 0.1882(6) 0.045(4) Uani 1 1 d U . . O27 O 0.8700(9) 0.9940(8) 0.2868(4) 0.062(4) Uani 1 1 d U . . C27 C 0.8851(10) 1.0278(11) 0.2577(6) 0.041(4) Uani 1 1 d U . . O28 O 1.0997(7) 1.1223(8) 0.2458(4) 0.058(4) Uani 1 1 d U . . C28 C 1.0254(11) 1.1081(11) 0.2334(5) 0.039(4) Uani 1 1 d U . . C31 C 0.5605(11) 1.0511(10) 0.4087(5) 0.039(3) Uani 1 1 d U . . H31 H 0.6234 1.0466 0.4029 0.047 Uiso 1 1 calc R . . C32 C 0.5737(10) 1.0521(10) 0.4565(5) 0.038(3) Uani 1 1 d U . . H32A H 0.5130 1.0516 0.4643 0.046 Uiso 1 1 calc R . . H32B H 0.6051 1.1052 0.4676 0.046 Uiso 1 1 calc R . . C33 C 0.6294(11) 0.9766(10) 0.4773(6) 0.048(4) Uani 1 1 d U . . H33A H 0.6924 0.9809 0.4724 0.057 Uiso 1 1 calc R . . H33B H 0.6330 0.9790 0.5082 0.057 Uiso 1 1 calc R . . C34 C 0.5885(13) 0.8918(11) 0.4605(6) 0.059(5) Uani 1 1 d U . . H34A H 0.6312 0.8456 0.4722 0.070 Uiso 1 1 calc R . . H34B H 0.5305 0.8824 0.4701 0.070 Uiso 1 1 calc R . . C35 C 0.5704(12) 0.8889(10) 0.4131(6) 0.054(4) Uani 1 1 d U . . H35A H 0.5384 0.8353 0.4032 0.065 Uiso 1 1 calc R . . H35B H 0.6294 0.8892 0.4038 0.065 Uiso 1 1 calc R . . C36 C 0.5117(10) 0.9647(9) 0.3927(5) 0.040(3) Uani 1 1 d U . . H36A H 0.4508 0.9625 0.4002 0.048 Uiso 1 1 calc R . . H36B H 0.5028 0.9613 0.3616 0.048 Uiso 1 1 calc R . . C41 C 0.3925(10) 1.1525(11) 0.3936(7) 0.054(4) Uani 1 1 d U . . H41 H 0.3989 1.1143 0.4188 0.065 Uiso 1 1 calc R . . C42 C 0.3203(12) 1.1114(16) 0.3623(9) 0.113(8) Uani 1 1 d U . . H42A H 0.3410 1.0540 0.3562 0.136 Uiso 1 1 calc R . . H42B H 0.3101 1.1445 0.3357 0.136 Uiso 1 1 calc R . . C43 C 0.2245(13) 1.1035(18) 0.3778(10) 0.133(9) Uani 1 1 d U . . H43A H 0.1772 1.0775 0.3554 0.160 Uiso 1 1 calc R . . H43B H 0.2323 1.0676 0.4034 0.160 Uiso 1 1 calc R . . C44 C 0.1952(12) 1.1948(17) 0.3877(9) 0.105(7) Uani 1 1 d U . . H44A H 0.1915 1.2325 0.3630 0.126 Uiso 1 1 calc R . . H44B H 0.1351 1.1942 0.3961 0.126 Uiso 1 1 calc R . . C45 C 0.2650(13) 1.2212(18) 0.4216(9) 0.114(8) Uani 1 1 d U . . H45A H 0.2700 1.1804 0.4452 0.137 Uiso 1 1 calc R . . H45B H 0.2492 1.2773 0.4317 0.137 Uiso 1 1 calc R . . C46 C 0.3601(13) 1.2272(16) 0.4076(9) 0.116(8) Uani 1 1 d U . . H46A H 0.3545 1.2698 0.3847 0.139 Uiso 1 1 calc R . . H46B H 0.4063 1.2485 0.4318 0.139 Uiso 1 1 calc R . . C51 C 1.1395(9) 1.2329(9) 0.1395(5) 0.025(3) Uani 1 1 d U . . H51 H 1.1292 1.1973 0.1637 0.030 Uiso 1 1 calc R . . C52 C 1.1751(9) 1.3208(8) 0.1588(5) 0.028(3) Uani 1 1 d U . . H52A H 1.1992 1.3548 0.1378 0.034 Uiso 1 1 calc R . . H52B H 1.1248 1.3529 0.1672 0.034 Uiso 1 1 calc R . . C53 C 1.2502(9) 1.3034(10) 0.1971(5) 0.037(4) Uani 1 1 d U . . H53A H 1.2708 1.3574 0.2117 0.044 Uiso 1 1 calc R . . H53B H 1.2265 1.2664 0.2171 0.044 Uiso 1 1 calc R . . C54 C 1.3300(10) 1.2605(10) 0.1836(5) 0.042(4) Uani 1 1 d U . . H54A H 1.3790 1.2497 0.2088 0.050 Uiso 1 1 calc R . . H54B H 1.3549 1.2986 0.1644 0.050 Uiso 1 1 calc R . . C55 C 1.3013(10) 1.1776(10) 0.1613(5) 0.041(4) Uani 1 1 d U . . H55A H 1.2831 1.1372 0.1815 0.049 Uiso 1 1 calc R . . H55B H 1.3538 1.1529 0.1513 0.049 Uiso 1 1 calc R . . C56 C 1.2197(9) 1.1904(10) 0.1230(5) 0.040(4) Uani 1 1 d U . . H56A H 1.1998 1.1350 0.1098 0.048 Uiso 1 1 calc R . . H56B H 1.2386 1.2269 0.1015 0.048 Uiso 1 1 calc R . . C61 C 1.0542(9) 1.2840(9) 0.0501(4) 0.029(3) Uani 1 1 d U . . H61 H 1.1133 1.2575 0.0471 0.035 Uiso 1 1 calc R . . C62 C 1.0731(11) 1.3786(10) 0.0529(5) 0.043(4) Uani 1 1 d U . . H62A H 1.1168 1.3911 0.0797 0.052 Uiso 1 1 calc R . . H62B H 1.0155 1.4092 0.0533 0.052 Uiso 1 1 calc R . . C63 C 1.1124(13) 1.4105(12) 0.0159(6) 0.064(5) Uani 1 1 d U . . H63A H 1.1731 1.3843 0.0171 0.077 Uiso 1 1 calc R . . H63B H 1.1210 1.4727 0.0183 0.077 Uiso 1 1 calc R . . C64 C 1.0491(13) 1.3893(12) -0.0268(6) 0.059(5) Uani 1 1 d U . . H64A H 0.9920 1.4228 -0.0301 0.071 Uiso 1 1 calc R . . H64B H 1.0797 1.4042 -0.0501 0.071 Uiso 1 1 calc R . . C65 C 1.0265(13) 1.2956(12) -0.0286(6) 0.058(5) Uani 1 1 d U . . H65A H 1.0825 1.2631 -0.0299 0.070 Uiso 1 1 calc R . . H65B H 0.9809 1.2839 -0.0548 0.070 Uiso 1 1 calc R . . C66 C 0.9886(12) 1.2644(12) 0.0095(5) 0.052(4) Uani 1 1 d U . . H66A H 0.9292 1.2923 0.0094 0.062 Uiso 1 1 calc R . . H66B H 0.9781 1.2024 0.0072 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.661(2) 1.620(2) 0.4786(11) 0.295(14) Uiso 0.50 1 d PDU . . Cl2 Cl 0.555(2) 1.528(2) 0.4629(11) 0.283(13) Uiso 0.50 1 d PDU . . C100 C 0.582(4) 1.606(3) 0.437(2) 0.149(19) Uiso 0.50 1 d PDU . . H10A H 0.5354 1.6520 0.4316 0.179 Uiso 0.50 1 calc PR . . H10B H 0.6038 1.5908 0.4113 0.179 Uiso 0.50 1 calc 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 Re1 0.0231(3) 0.0254(3) 0.0353(4) -0.0014(3) 0.0038(3) -0.0003(3) Re2 0.0288(3) 0.0316(4) 0.0347(4) -0.0051(3) 0.0077(3) -0.0011(3) Re3 0.0286(3) 0.0274(3) 0.0322(4) 0.0015(3) 0.0093(3) 0.0017(3) Re4 0.0284(3) 0.0283(3) 0.0345(4) -0.0051(3) 0.0079(3) -0.0031(3) Fe1 0.0278(11) 0.0251(11) 0.0361(13) 0.0043(10) 0.0071(10) 0.0002(9) Fe2 0.0228(10) 0.0336(13) 0.0334(13) 0.0019(11) 0.0042(9) 0.0011(9) Fe3 0.0321(12) 0.0354(13) 0.0397(14) -0.0046(12) 0.0095(10) -0.0034(10) Fe4 0.0338(11) 0.0277(12) 0.0351(13) 0.0030(11) 0.0082(10) 0.0022(10) S1 0.0229(17) 0.0245(19) 0.038(2) 0.0011(17) 0.0077(16) 0.0010(15) S2 0.0291(19) 0.029(2) 0.032(2) 0.0001(18) 0.0096(16) -0.0010(16) S3 0.0303(19) 0.030(2) 0.032(2) -0.0007(18) 0.0082(16) 0.0000(16) S4 0.0305(19) 0.0257(19) 0.037(2) -0.0020(18) 0.0084(16) -0.0021(16) P1 0.0260(19) 0.029(2) 0.037(2) -0.0028(19) 0.0120(17) -0.0007(17) P2 0.0233(18) 0.031(2) 0.029(2) 0.0020(18) 0.0056(16) -0.0022(16) O1 0.043(6) 0.046(8) 0.073(10) -0.012(7) 0.004(6) -0.019(5) C1 0.038(7) 0.031(8) 0.041(8) -0.009(7) 0.008(6) -0.006(5) O2 0.042(6) 0.071(9) 0.036(5) 0.011(7) 0.005(6) 0.005(6) C2 0.029(8) 0.051(10) 0.035(5) -0.003(7) 0.002(6) -0.005(7) O3 0.056(7) 0.040(7) 0.066(9) 0.009(7) 0.017(7) 0.019(5) C3 0.044(8) 0.022(6) 0.053(10) 0.004(6) 0.024(7) 0.002(5) O41 0.027(15) 0.026(12) 0.09(2) -0.022(17) -0.021(19) -0.001(10) O42 0.06(2) 0.027(11) 0.07(2) -0.022(16) -0.05(2) 0.013(14) C4 0.045(7) 0.030(6) 0.041(8) -0.011(7) -0.019(7) 0.010(6) O5 0.067(8) 0.048(8) 0.053(8) -0.003(7) 0.004(6) 0.020(6) C5 0.036(7) 0.029(6) 0.046(9) -0.007(7) 0.015(6) -0.001(5) O6 0.041(6) 0.079(9) 0.042(8) -0.002(7) 0.004(5) 0.014(6) C6 0.035(7) 0.051(9) 0.033(7) -0.009(8) 0.001(6) -0.003(6) O7 0.090(9) 0.073(10) 0.044(7) -0.014(8) 0.030(7) 0.010(8) C7 0.035(8) 0.055(11) 0.048(7) -0.007(7) 0.017(7) -0.006(7) O8 0.069(8) 0.055(8) 0.069(10) -0.018(8) 0.008(7) -0.025(6) C8 0.039(8) 0.051(8) 0.051(11) -0.012(7) 0.012(7) -0.012(6) O9 0.072(8) 0.039(7) 0.080(10) -0.006(7) 0.044(8) 0.008(6) C9 0.048(9) 0.027(6) 0.052(10) 0.010(6) 0.030(7) 0.006(6) O10 0.052(7) 0.046(7) 0.049(8) 0.003(6) 0.026(6) -0.015(6) C10 0.033(6) 0.031(7) 0.020(7) 0.001(6) -0.002(5) -0.003(6) O11 0.060(8) 0.055(8) 0.087(11) 0.023(8) -0.024(6) -0.010(7) C11 0.032(7) 0.035(8) 0.060(9) 0.023(7) -0.001(6) -0.005(6) O12 0.038(7) 0.067(9) 0.067(9) -0.017(7) -0.008(6) -0.002(6) C12 0.014(6) 0.039(8) 0.039(7) 0.000(6) 0.005(5) -0.007(6) O13 0.026(5) 0.074(9) 0.079(10) -0.022(8) 0.006(6) -0.006(6) C13 0.025(5) 0.054(10) 0.039(9) -0.002(8) 0.003(5) 0.000(6) O14 0.067(8) 0.031(6) 0.064(9) 0.014(6) 0.009(7) 0.018(6) C14 0.029(7) 0.041(7) 0.032(8) 0.002(6) -0.005(6) 0.006(6) O15 0.045(7) 0.097(11) 0.049(7) 0.002(8) -0.005(5) 0.012(7) C15 0.031(7) 0.052(9) 0.039(6) 0.005(7) 0.004(5) 0.011(7) O16 0.045(6) 0.067(8) 0.033(7) 0.004(6) 0.008(5) 0.028(6) C16 0.029(6) 0.030(7) 0.029(8) -0.002(7) -0.004(5) 0.008(6) O17 0.061(8) 0.057(8) 0.040(6) 0.002(7) 0.002(5) -0.009(7) C17 0.033(7) 0.029(7) 0.039(6) 0.003(6) 0.009(5) -0.006(6) O18 0.062(8) 0.028(5) 0.095(11) 0.016(7) 0.034(7) 0.008(6) C18 0.046(9) 0.034(5) 0.038(9) 0.000(7) 0.014(7) 0.006(6) O19 0.047(7) 0.067(9) 0.063(9) -0.011(8) 0.023(6) -0.002(7) C19 0.027(7) 0.045(8) 0.037(8) 0.002(7) 0.004(6) 0.002(6) O20 0.060(8) 0.035(6) 0.086(11) -0.002(7) 0.018(7) -0.010(6) C20 0.039(8) 0.039(6) 0.028(9) -0.005(6) 0.006(6) -0.010(6) O21 0.037(7) 0.089(10) 0.085(11) -0.006(9) -0.009(6) 0.014(7) C21 0.036(7) 0.036(8) 0.048(7) -0.002(7) 0.008(5) 0.003(6) O22 0.065(8) 0.054(8) 0.040(7) 0.017(7) 0.000(5) 0.002(6) C22 0.041(7) 0.022(7) 0.038(7) -0.004(6) 0.007(5) -0.001(6) O23 0.062(8) 0.078(10) 0.104(12) -0.051(8) 0.029(8) -0.018(8) C23 0.030(8) 0.058(10) 0.061(10) -0.022(8) 0.010(7) -0.007(6) O24 0.069(9) 0.089(11) 0.096(13) 0.000(10) -0.009(8) 0.029(7) C24 0.033(7) 0.072(11) 0.065(11) 0.002(8) -0.002(6) 0.010(7) O25 0.065(8) 0.053(8) 0.056(9) -0.003(7) 0.015(6) -0.020(6) C25 0.044(7) 0.038(9) 0.064(11) -0.012(7) 0.022(8) -0.018(7) O26 0.089(9) 0.037(6) 0.046(8) -0.008(6) 0.016(7) 0.003(7) C26 0.062(9) 0.032(6) 0.044(10) 0.012(6) 0.016(8) 0.016(6) O27 0.095(10) 0.041(8) 0.058(8) 0.010(7) 0.033(8) 0.004(7) C27 0.042(8) 0.042(9) 0.040(7) 0.004(6) 0.012(6) 0.001(7) O28 0.032(5) 0.071(9) 0.065(9) 0.004(8) 0.000(6) 0.001(6) C28 0.038(5) 0.052(10) 0.028(8) 0.010(8) 0.007(5) 0.005(6) C31 0.048(8) 0.029(5) 0.043(7) 0.004(6) 0.015(7) 0.005(6) C32 0.042(8) 0.035(7) 0.043(7) 0.011(6) 0.021(7) 0.002(7) C33 0.060(10) 0.046(9) 0.039(8) 0.013(7) 0.013(8) 0.007(7) C34 0.076(12) 0.041(7) 0.062(9) 0.031(9) 0.021(9) 0.012(8) C35 0.070(11) 0.021(7) 0.067(10) -0.001(8) 0.006(10) 0.009(7) C36 0.052(9) 0.030(6) 0.042(8) 0.002(6) 0.019(7) 0.008(6) C41 0.031(6) 0.049(10) 0.089(12) -0.024(10) 0.027(7) -0.011(6) C42 0.043(8) 0.135(17) 0.162(19) -0.076(14) 0.024(10) -0.028(10) C43 0.033(9) 0.156(18) 0.21(2) -0.052(17) 0.027(12) -0.014(11) C44 0.026(8) 0.144(17) 0.144(19) 0.015(16) 0.017(10) 0.021(11) C45 0.042(10) 0.161(18) 0.15(2) -0.051(15) 0.044(10) 0.009(12) C46 0.041(9) 0.130(16) 0.19(2) -0.088(14) 0.046(11) -0.006(10) C51 0.029(5) 0.022(7) 0.027(7) -0.004(6) 0.010(5) -0.004(5) C52 0.024(6) 0.018(7) 0.037(8) -0.006(6) -0.004(5) -0.003(5) C53 0.037(7) 0.037(9) 0.030(8) -0.017(7) -0.007(6) 0.000(6) C54 0.034(7) 0.047(9) 0.038(9) -0.001(7) -0.009(6) 0.011(7) C55 0.040(7) 0.043(9) 0.041(9) -0.003(7) 0.012(6) 0.013(7) C56 0.033(6) 0.031(8) 0.054(10) -0.010(7) 0.006(6) 0.006(6) C61 0.028(7) 0.037(7) 0.024(5) -0.012(6) 0.009(5) -0.011(6) C62 0.063(10) 0.036(7) 0.027(7) 0.005(6) 0.001(7) -0.008(7) C63 0.097(13) 0.050(10) 0.050(9) 0.010(9) 0.029(8) -0.017(9) C64 0.078(12) 0.067(10) 0.040(7) 0.014(9) 0.032(8) -0.002(10) C65 0.080(12) 0.060(10) 0.032(7) 0.015(9) 0.005(8) 0.003(9) C66 0.071(11) 0.056(10) 0.022(6) -0.004(7) -0.002(7) -0.018(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 Re1 C1 1.913(15) . ? Re1 C2 1.945(17) . ? Re1 C4 1.965(15) . ? Re1 C3 1.979(15) . ? Re1 P1 2.526(4) . ? Re1 S1 2.551(4) . ? Re2 C7 1.908(17) . ? Re2 C8 1.949(17) . ? Re2 C6 1.978(17) . ? Re2 C5 2.016(16) . ? Re2 P1 2.532(4) . ? Re2 S1 2.552(4) . ? Re3 C18 1.926(17) . ? Re3 C16 1.949(14) . ? Re3 C15 1.997(17) . ? Re3 C17 2.047(17) . ? Re3 P2 2.528(4) . ? Re3 S4 2.580(4) . ? Re4 C19 1.848(16) . ? Re4 C20 1.933(16) . ? Re4 C21 1.946(17) . ? Re4 C22 1.987(16) . ? Re4 P2 2.524(4) . ? Re4 S4 2.547(4) . ? Fe1 C9 1.755(17) . ? Fe1 C11 1.785(16) . ? Fe1 C10 1.803(15) . ? Fe1 S2 2.276(4) . ? Fe1 S1 2.293(4) . ? Fe1 Fe2 2.517(3) . ? Fe2 C13 1.759(15) . ? Fe2 C12 1.797(16) . ? Fe2 C14 1.820(16) . ? Fe2 S2 2.237(5) . ? Fe2 S1 2.315(4) . ? Fe3 C23 1.766(18) . ? Fe3 C24 1.774(18) . ? Fe3 C25 1.814(17) . ? Fe3 S3 2.273(5) . ? Fe3 S4 2.284(4) . ? Fe3 Fe4 2.497(3) . ? Fe4 C26 1.785(17) . ? Fe4 C27 1.794(17) . ? Fe4 C28 1.839(16) . ? Fe4 S3 2.250(4) . ? Fe4 S4 2.320(5) . ? S2 S3 2.127(5) . ? P1 C31 1.851(16) . ? P1 C41 1.875(14) . ? P2 C61 1.877(14) . ? P2 C51 1.886(14) . ? O1 C1 1.148(16) . ? O2 C2 1.158(18) . ? O3 C3 1.146(16) . ? O41 C4 1.18(2) . ? O42 C4 1.18(2) . ? O5 C5 1.132(17) . ? O6 C6 1.124(17) . ? O7 C7 1.165(19) . ? O8 C8 1.133(18) . ? O9 C9 1.150(17) . ? O10 C10 1.124(15) . ? O11 C11 1.174(18) . ? O12 C12 1.127(17) . ? O13 C13 1.158(16) . ? O14 C14 1.124(17) . ? O15 C15 1.110(18) . ? O16 C16 1.141(15) . ? O17 C17 1.091(18) . ? O18 C18 1.146(17) . ? O19 C19 1.216(17) . ? O20 C20 1.169(17) . ? O21 C21 1.153(18) . ? O22 C22 1.134(17) . ? O23 C23 1.155(19) . ? O24 C24 1.152(19) . ? O25 C25 1.099(18) . ? O26 C26 1.126(18) . ? O27 C27 1.131(18) . ? O28 C28 1.111(16) . ? C31 C32 1.50(2) . ? C31 C36 1.56(2) . ? C32 C33 1.51(2) . ? C33 C34 1.51(2) . ? C34 C35 1.49(2) . ? C35 C36 1.53(2) . ? C41 C46 1.37(2) . ? C41 C42 1.45(2) . ? C42 C43 1.60(3) . ? C43 C44 1.54(3) . ? C44 C45 1.39(3) . ? C45 C46 1.57(2) . ? C51 C56 1.545(18) . ? C51 C52 1.551(17) . ? C52 C53 1.497(18) . ? C53 C54 1.497(19) . ? C54 C55 1.50(2) . ? C55 C56 1.55(2) . ? C61 C66 1.48(2) . ? C61 C62 1.500(19) . ? C62 C63 1.51(2) . ? C63 C64 1.52(2) . ? C64 C65 1.50(2) . ? C65 C66 1.52(2) . ? Cl1 C100 1.60(5) . ? Cl1 Cl2 2.11(4) . ? Cl2 C100 1.57(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 C1 Re1 C2 87.0(7) . . ? C1 Re1 C4 91.1(7) . . ? C2 Re1 C4 92.3(7) . . ? C1 Re1 C3 92.0(6) . . ? C2 Re1 C3 91.2(7) . . ? C4 Re1 C3 175.5(7) . . ? C1 Re1 P1 96.9(5) . . ? C2 Re1 P1 175.9(5) . . ? C4 Re1 P1 86.2(5) . . ? C3 Re1 P1 90.1(5) . . ? C1 Re1 S1 173.5(5) . . ? C2 Re1 S1 99.4(5) . . ? C4 Re1 S1 87.4(5) . . ? C3 Re1 S1 89.2(5) . . ? P1 Re1 S1 76.70(12) . . ? C7 Re2 C8 90.1(7) . . ? C7 Re2 C6 89.1(7) . . ? C8 Re2 C6 90.5(7) . . ? C7 Re2 C5 90.3(7) . . ? C8 Re2 C5 85.8(7) . . ? C6 Re2 C5 176.3(7) . . ? C7 Re2 P1 94.5(5) . . ? C8 Re2 P1 175.0(5) . . ? C6 Re2 P1 91.5(5) . . ? C5 Re2 P1 92.3(4) . . ? C7 Re2 S1 170.1(5) . . ? C8 Re2 S1 99.0(5) . . ? C6 Re2 S1 86.9(5) . . ? C5 Re2 S1 94.3(5) . . ? P1 Re2 S1 76.57(12) . . ? C18 Re3 C16 89.7(6) . . ? C18 Re3 C15 90.2(7) . . ? C16 Re3 C15 85.9(6) . . ? C18 Re3 C17 89.5(7) . . ? C16 Re3 C17 89.6(6) . . ? C15 Re3 C17 175.5(6) . . ? C18 Re3 P2 95.9(5) . . ? C16 Re3 P2 173.0(4) . . ? C15 Re3 P2 89.8(5) . . ? C17 Re3 P2 94.6(4) . . ? C18 Re3 S4 170.4(5) . . ? C16 Re3 S4 99.2(4) . . ? C15 Re3 S4 94.1(5) . . ? C17 Re3 S4 86.9(4) . . ? P2 Re3 S4 75.57(12) . . ? C19 Re4 C20 89.0(7) . . ? C19 Re4 C21 95.0(7) . . ? C20 Re4 C21 88.8(7) . . ? C19 Re4 C22 88.2(6) . . ? C20 Re4 C22 88.4(6) . . ? C21 Re4 C22 175.6(6) . . ? C19 Re4 P2 92.2(5) . . ? C20 Re4 P2 178.8(5) . . ? C21 Re4 P2 91.4(5) . . ? C22 Re4 P2 91.4(4) . . ? C19 Re4 S4 168.2(5) . . ? C20 Re4 S4 102.6(5) . . ? C21 Re4 S4 87.3(5) . . ? C22 Re4 S4 90.1(5) . . ? P2 Re4 S4 76.23(12) . . ? C9 Fe1 C11 94.6(8) . . ? C9 Fe1 C10 92.8(7) . . ? C11 Fe1 C10 101.8(7) . . ? C9 Fe1 S2 163.9(5) . . ? C11 Fe1 S2 96.9(6) . . ? C10 Fe1 S2 95.8(5) . . ? C9 Fe1 S1 88.7(5) . . ? C11 Fe1 S1 107.8(5) . . ? C10 Fe1 S1 150.2(5) . . ? S2 Fe1 S1 77.08(15) . . ? C9 Fe1 Fe2 110.4(6) . . ? C11 Fe1 Fe2 149.3(5) . . ? C10 Fe1 Fe2 94.6(5) . . ? S2 Fe1 Fe2 55.37(12) . . ? S1 Fe1 Fe2 57.31(11) . . ? C13 Fe2 C12 89.5(7) . . ? C13 Fe2 C14 95.8(7) . . ? C12 Fe2 C14 104.8(7) . . ? C13 Fe2 S2 93.1(5) . . ? C12 Fe2 S2 148.4(5) . . ? C14 Fe2 S2 106.2(5) . . ? C13 Fe2 S1 164.2(6) . . ? C12 Fe2 S1 92.1(4) . . ? C14 Fe2 S1 98.9(5) . . ? S2 Fe2 S1 77.39(15) . . ? C13 Fe2 Fe1 107.7(5) . . ? C12 Fe2 Fe1 92.4(5) . . ? C14 Fe2 Fe1 150.9(5) . . ? S2 Fe2 Fe1 56.82(12) . . ? S1 Fe2 Fe1 56.47(12) . . ? C23 Fe3 C24 95.4(9) . . ? C23 Fe3 C25 91.5(8) . . ? C24 Fe3 C25 103.5(8) . . ? C23 Fe3 S3 163.7(5) . . ? C24 Fe3 S3 98.3(7) . . ? C25 Fe3 S3 93.6(6) . . ? C23 Fe3 S4 91.1(5) . . ? C24 Fe3 S4 105.4(6) . . ? C25 Fe3 S4 150.6(6) . . ? S3 Fe3 S4 76.94(15) . . ? C23 Fe3 Fe4 108.3(6) . . ? C24 Fe3 Fe4 150.4(6) . . ? C25 Fe3 Fe4 93.6(6) . . ? S3 Fe3 Fe4 56.03(12) . . ? S4 Fe3 Fe4 57.87(12) . . ? C26 Fe4 C27 90.5(8) . . ? C26 Fe4 C28 101.0(8) . . ? C27 Fe4 C28 94.8(7) . . ? C26 Fe4 S3 149.9(6) . . ? C27 Fe4 S3 92.7(5) . . ? C28 Fe4 S3 108.5(5) . . ? C26 Fe4 S4 92.0(6) . . ? C27 Fe4 S4 162.5(5) . . ? C28 Fe4 S4 101.7(5) . . ? S3 Fe4 S4 76.65(15) . . ? C26 Fe4 Fe3 93.5(6) . . ? C27 Fe4 Fe3 106.1(5) . . ? C28 Fe4 Fe3 154.4(5) . . ? S3 Fe4 Fe3 56.94(12) . . ? S4 Fe4 Fe3 56.44(11) . . ? Fe1 S1 Fe2 66.22(12) . . ? Fe1 S1 Re1 114.21(17) . . ? Fe2 S1 Re1 127.07(17) . . ? Fe1 S1 Re2 130.35(17) . . ? Fe2 S1 Re2 118.56(17) . . ? Re1 S1 Re2 100.59(12) . . ? S3 S2 Fe2 117.6(2) . . ? S3 S2 Fe1 109.5(2) . . ? Fe2 S2 Fe1 67.81(14) . . ? S2 S3 Fe4 117.8(2) . . ? S2 S3 Fe3 109.27(19) . . ? Fe4 S3 Fe3 67.03(14) . . ? Fe3 S4 Fe4 65.69(13) . . ? Fe3 S4 Re4 130.60(17) . . ? Fe4 S4 Re4 118.62(16) . . ? Fe3 S4 Re3 117.77(16) . . ? Fe4 S4 Re3 123.79(17) . . ? Re4 S4 Re3 100.08(13) . . ? C31 P1 C41 102.2(8) . . ? C31 P1 Re1 110.0(5) . . ? C41 P1 Re1 116.9(6) . . ? C31 P1 Re2 109.6(5) . . ? C41 P1 Re2 116.3(6) . . ? Re1 P1 Re2 101.82(14) . . ? C61 P2 C51 105.2(6) . . ? C61 P2 Re4 113.7(5) . . ? C51 P2 Re4 108.0(5) . . ? C61 P2 Re3 118.1(5) . . ? C51 P2 Re3 109.4(5) . . ? Re4 P2 Re3 102.13(13) . . ? O1 C1 Re1 175.1(15) . . ? O2 C2 Re1 173.6(13) . . ? O3 C3 Re1 174.9(14) . . ? O41 C4 O42 30(3) . . ? O41 C4 Re1 168(2) . . ? O42 C4 Re1 161(3) . . ? O5 C5 Re2 174.6(15) . . ? O6 C6 Re2 176.7(15) . . ? O7 C7 Re2 175.6(16) . . ? O8 C8 Re2 176.6(16) . . ? O9 C9 Fe1 173.6(16) . . ? O10 C10 Fe1 177.0(14) . . ? O11 C11 Fe1 175.9(17) . . ? O12 C12 Fe2 172.2(13) . . ? O13 C13 Fe2 178.4(16) . . ? O14 C14 Fe2 173.8(15) . . ? O15 C15 Re3 171.6(16) . . ? O16 C16 Re3 173.1(13) . . ? O17 C17 Re3 176.8(16) . . ? O18 C18 Re3 175.0(16) . . ? O19 C19 Re4 175.2(14) . . ? O20 C20 Re4 174.0(15) . . ? O21 C21 Re4 172.0(15) . . ? O22 C22 Re4 177.3(14) . . ? O23 C23 Fe3 177.6(16) . . ? O24 C24 Fe3 177.9(19) . . ? O25 C25 Fe3 177.1(16) . . ? O26 C26 Fe4 177.1(16) . . ? O27 C27 Fe4 177.1(17) . . ? O28 C28 Fe4 175.0(16) . . ? C32 C31 C36 107.2(13) . . ? C32 C31 P1 116.2(11) . . ? C36 C31 P1 116.2(11) . . ? C31 C32 C33 112.6(13) . . ? C34 C33 C32 112.7(14) . . ? C35 C34 C33 111.4(14) . . ? C34 C35 C36 112.2(15) . . ? C35 C36 C31 110.2(13) . . ? C46 C41 C42 110.1(18) . . ? C46 C41 P1 120.1(13) . . ? C42 C41 P1 114.6(14) . . ? C41 C42 C43 113(2) . . ? C44 C43 C42 107(2) . . ? C45 C44 C43 104(2) . . ? C44 C45 C46 111(2) . . ? C41 C46 C45 116(2) . . ? C56 C51 C52 107.2(11) . . ? C56 C51 P2 113.8(10) . . ? C52 C51 P2 116.3(9) . . ? C53 C52 C51 107.3(11) . . ? C54 C53 C52 109.9(13) . . ? C53 C54 C55 111.2(13) . . ? C54 C55 C56 111.4(13) . . ? C55 C56 C51 108.1(13) . . ? C66 C61 C62 109.6(14) . . ? C66 C61 P2 115.6(10) . . ? C62 C61 P2 115.3(11) . . ? C61 C62 C63 112.1(15) . . ? C62 C63 C64 111.5(15) . . ? C65 C64 C63 109.7(16) . . ? C64 C65 C66 113.4(16) . . ? C61 C66 C65 110.6(14) . . ? C100 Cl1 Cl2 47.5(19) . . ? C100 Cl2 Cl1 48.7(19) . . ? Cl2 C100 Cl1 84(4) . . ? 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 C9 Fe1 Fe2 C13 -106.7(8) . . . . ? C11 Fe1 Fe2 C13 110.5(13) . . . . ? C10 Fe1 Fe2 C13 -12.0(7) . . . . ? S2 Fe1 Fe2 C13 81.9(6) . . . . ? S1 Fe1 Fe2 C13 178.8(6) . . . . ? C9 Fe1 Fe2 C12 -16.5(7) . . . . ? C11 Fe1 Fe2 C12 -159.2(12) . . . . ? C10 Fe1 Fe2 C12 78.3(6) . . . . ? S2 Fe1 Fe2 C12 172.1(5) . . . . ? S1 Fe1 Fe2 C12 -90.9(4) . . . . ? C9 Fe1 Fe2 C14 110.6(12) . . . . ? C11 Fe1 Fe2 C14 -32.2(16) . . . . ? C10 Fe1 Fe2 C14 -154.7(12) . . . . ? S2 Fe1 Fe2 C14 -60.8(11) . . . . ? S1 Fe1 Fe2 C14 36.1(11) . . . . ? C9 Fe1 Fe2 S2 171.4(5) . . . . ? C11 Fe1 Fe2 S2 28.6(11) . . . . ? C10 Fe1 Fe2 S2 -93.9(5) . . . . ? S1 Fe1 Fe2 S2 96.91(17) . . . . ? C9 Fe1 Fe2 S1 74.5(5) . . . . ? C11 Fe1 Fe2 S1 -68.3(11) . . . . ? C10 Fe1 Fe2 S1 169.2(5) . . . . ? S2 Fe1 Fe2 S1 -96.91(17) . . . . ? C23 Fe3 Fe4 C26 -10.6(8) . . . . ? C24 Fe3 Fe4 C26 -151.9(14) . . . . ? C25 Fe3 Fe4 C26 82.2(8) . . . . ? S3 Fe3 Fe4 C26 174.1(6) . . . . ? S4 Fe3 Fe4 C26 -90.0(6) . . . . ? C23 Fe3 Fe4 C27 -102.2(9) . . . . ? C24 Fe3 Fe4 C27 116.5(14) . . . . ? C25 Fe3 Fe4 C27 -9.3(8) . . . . ? S3 Fe3 Fe4 C27 82.6(6) . . . . ? S4 Fe3 Fe4 C27 178.4(6) . . . . ? C23 Fe3 Fe4 C28 114.1(14) . . . . ? C24 Fe3 Fe4 C28 -27.3(18) . . . . ? C25 Fe3 Fe4 C28 -153.1(13) . . . . ? S3 Fe3 Fe4 C28 -61.2(12) . . . . ? S4 Fe3 Fe4 C28 34.6(12) . . . . ? C23 Fe3 Fe4 S3 175.3(7) . . . . ? C24 Fe3 Fe4 S3 33.9(13) . . . . ? C25 Fe3 Fe4 S3 -91.9(6) . . . . ? S4 Fe3 Fe4 S3 95.81(18) . . . . ? C23 Fe3 Fe4 S4 79.4(7) . . . . ? C24 Fe3 Fe4 S4 -61.9(13) . . . . ? C25 Fe3 Fe4 S4 172.3(6) . . . . ? S3 Fe3 Fe4 S4 -95.81(18) . . . . ? C9 Fe1 S1 Fe2 -115.4(6) . . . . ? C11 Fe1 S1 Fe2 150.2(6) . . . . ? C10 Fe1 S1 Fe2 -22.1(10) . . . . ? S2 Fe1 S1 Fe2 56.94(13) . . . . ? C9 Fe1 S1 Re1 123.0(6) . . . . ? C11 Fe1 S1 Re1 28.6(6) . . . . ? C10 Fe1 S1 Re1 -143.7(10) . . . . ? S2 Fe1 S1 Re1 -64.67(16) . . . . ? Fe2 Fe1 S1 Re1 -121.60(18) . . . . ? C9 Fe1 S1 Re2 -7.3(6) . . . . ? C11 Fe1 S1 Re2 -101.7(6) . . . . ? C10 Fe1 S1 Re2 86.1(10) . . . . ? S2 Fe1 S1 Re2 165.1(2) . . . . ? Fe2 Fe1 S1 Re2 108.1(2) . . . . ? C13 Fe2 S1 Fe1 -4(2) . . . . ? C12 Fe2 S1 Fe1 91.5(5) . . . . ? C14 Fe2 S1 Fe1 -163.1(5) . . . . ? S2 Fe2 S1 Fe1 -58.37(14) . . . . ? C13 Fe2 S1 Re1 99(2) . . . . ? C12 Fe2 S1 Re1 -165.3(5) . . . . ? C14 Fe2 S1 Re1 -59.9(5) . . . . ? S2 Fe2 S1 Re1 44.9(2) . . . . ? Fe1 Fe2 S1 Re1 103.2(2) . . . . ? C13 Fe2 S1 Re2 -129(2) . . . . ? C12 Fe2 S1 Re2 -33.0(5) . . . . ? C14 Fe2 S1 Re2 72.4(5) . . . . ? S2 Fe2 S1 Re2 177.18(19) . . . . ? Fe1 Fe2 S1 Re2 -124.5(2) . . . . ? C1 Re1 S1 Fe1 -149(4) . . . . ? C2 Re1 S1 Fe1 19.1(5) . . . . ? C4 Re1 S1 Fe1 -72.7(6) . . . . ? C3 Re1 S1 Fe1 110.2(5) . . . . ? P1 Re1 S1 Fe1 -159.47(18) . . . . ? C1 Re1 S1 Fe2 133(4) . . . . ? C2 Re1 S1 Fe2 -58.5(5) . . . . ? C4 Re1 S1 Fe2 -150.4(6) . . . . ? C3 Re1 S1 Fe2 32.6(5) . . . . ? P1 Re1 S1 Fe2 122.9(2) . . . . ? C1 Re1 S1 Re2 -5(4) . . . . ? C2 Re1 S1 Re2 162.9(5) . . . . ? C4 Re1 S1 Re2 71.0(5) . . . . ? C3 Re1 S1 Re2 -106.0(5) . . . . ? P1 Re1 S1 Re2 -15.73(12) . . . . ? C7 Re2 S1 Fe1 177(3) . . . . ? C8 Re2 S1 Fe1 -27.1(6) . . . . ? C6 Re2 S1 Fe1 -117.1(5) . . . . ? C5 Re2 S1 Fe1 59.3(5) . . . . ? P1 Re2 S1 Fe1 150.6(2) . . . . ? C7 Re2 S1 Fe2 -101(3) . . . . ? C8 Re2 S1 Fe2 54.9(6) . . . . ? C6 Re2 S1 Fe2 -35.2(5) . . . . ? C5 Re2 S1 Fe2 141.3(4) . . . . ? P1 Re2 S1 Fe2 -127.4(2) . . . . ? C7 Re2 S1 Re1 42(3) . . . . ? C8 Re2 S1 Re1 -162.0(5) . . . . ? C6 Re2 S1 Re1 108.0(5) . . . . ? C5 Re2 S1 Re1 -75.6(4) . . . . ? P1 Re2 S1 Re1 15.70(12) . . . . ? C13 Fe2 S2 S3 -8.1(6) . . . . ? C12 Fe2 S2 S3 86.1(8) . . . . ? C14 Fe2 S2 S3 -105.1(5) . . . . ? S1 Fe2 S2 S3 159.1(2) . . . . ? Fe1 Fe2 S2 S3 101.2(2) . . . . ? C13 Fe2 S2 Fe1 -109.2(6) . . . . ? C12 Fe2 S2 Fe1 -15.1(8) . . . . ? C14 Fe2 S2 Fe1 153.8(5) . . . . ? S1 Fe2 S2 Fe1 57.99(12) . . . . ? C9 Fe1 S2 S3 -143.1(19) . . . . ? C11 Fe1 S2 S3 81.5(6) . . . . ? C10 Fe1 S2 S3 -21.1(5) . . . . ? S1 Fe1 S2 S3 -171.7(2) . . . . ? Fe2 Fe1 S2 S3 -112.7(2) . . . . ? C9 Fe1 S2 Fe2 -30.4(19) . . . . ? C11 Fe1 S2 Fe2 -165.8(5) . . . . ? C10 Fe1 S2 Fe2 91.6(4) . . . . ? S1 Fe1 S2 Fe2 -59.00(13) . . . . ? Fe2 S2 S3 Fe4 78.1(3) . . . . ? Fe1 S2 S3 Fe4 152.63(18) . . . . ? Fe2 S2 S3 Fe3 151.68(19) . . . . ? Fe1 S2 S3 Fe3 -133.82(18) . . . . ? C26 Fe4 S3 S2 88.8(11) . . . . ? C27 Fe4 S3 S2 -7.0(6) . . . . ? C28 Fe4 S3 S2 -103.1(6) . . . . ? S4 Fe4 S3 S2 158.9(2) . . . . ? Fe3 Fe4 S3 S2 100.5(2) . . . . ? C26 Fe4 S3 Fe3 -11.7(11) . . . . ? C27 Fe4 S3 Fe3 -107.5(5) . . . . ? C28 Fe4 S3 Fe3 156.5(5) . . . . ? S4 Fe4 S3 Fe3 58.44(13) . . . . ? C23 Fe3 S3 S2 -129(2) . . . . ? C24 Fe3 S3 S2 83.4(7) . . . . ? C25 Fe3 S3 S2 -20.9(6) . . . . ? S4 Fe3 S3 S2 -172.7(2) . . . . ? Fe4 Fe3 S3 S2 -112.8(2) . . . . ? C23 Fe3 S3 Fe4 -16(2) . . . . ? C24 Fe3 S3 Fe4 -163.8(6) . . . . ? C25 Fe3 S3 Fe4 91.9(6) . . . . ? S4 Fe3 S3 Fe4 -59.86(13) . . . . ? C23 Fe3 S4 Fe4 -111.0(6) . . . . ? C24 Fe3 S4 Fe4 153.1(7) . . . . ? C25 Fe3 S4 Fe4 -15.9(11) . . . . ? S3 Fe3 S4 Fe4 57.89(14) . . . . ? C23 Fe3 S4 Re4 -3.2(7) . . . . ? C24 Fe3 S4 Re4 -99.1(7) . . . . ? C25 Fe3 S4 Re4 91.9(12) . . . . ? S3 Fe3 S4 Re4 165.6(2) . . . . ? Fe4 Fe3 S4 Re4 107.8(2) . . . . ? C23 Fe3 S4 Re3 132.2(6) . . . . ? C24 Fe3 S4 Re3 36.2(7) . . . . ? C25 Fe3 S4 Re3 -132.7(11) . . . . ? S3 Fe3 S4 Re3 -58.97(19) . . . . ? Fe4 Fe3 S4 Re3 -116.9(2) . . . . ? C26 Fe4 S4 Fe3 92.9(6) . . . . ? C27 Fe4 S4 Fe3 -5.1(19) . . . . ? C28 Fe4 S4 Fe3 -165.5(5) . . . . ? S3 Fe4 S4 Fe3 -58.97(13) . . . . ? C26 Fe4 S4 Re4 -31.7(6) . . . . ? C27 Fe4 S4 Re4 -129.7(19) . . . . ? C28 Fe4 S4 Re4 70.0(6) . . . . ? S3 Fe4 S4 Re4 176.49(19) . . . . ? Fe3 Fe4 S4 Re4 -124.5(2) . . . . ? C26 Fe4 S4 Re3 -158.9(6) . . . . ? C27 Fe4 S4 Re3 103.1(19) . . . . ? C28 Fe4 S4 Re3 -57.2(6) . . . . ? S3 Fe4 S4 Re3 49.27(18) . . . . ? Fe3 Fe4 S4 Re3 108.24(19) . . . . ? C19 Re4 S4 Fe3 169(2) . . . . ? C20 Re4 S4 Fe3 -21.1(5) . . . . ? C21 Re4 S4 Fe3 67.1(5) . . . . ? C22 Re4 S4 Fe3 -109.4(5) . . . . ? P2 Re4 S4 Fe3 159.2(3) . . . . ? C19 Re4 S4 Fe4 -110(2) . . . . ? C20 Re4 S4 Fe4 60.3(5) . . . . ? C21 Re4 S4 Fe4 148.5(5) . . . . ? C22 Re4 S4 Fe4 -28.0(5) . . . . ? P2 Re4 S4 Fe4 -119.40(19) . . . . ? C19 Re4 S4 Re3 28(2) . . . . ? C20 Re4 S4 Re3 -161.9(5) . . . . ? C21 Re4 S4 Re3 -73.8(5) . . . . ? C22 Re4 S4 Re3 109.7(4) . . . . ? P2 Re4 S4 Re3 18.36(12) . . . . ? C18 Re3 S4 Fe3 167(3) . . . . ? C16 Re3 S4 Fe3 9.7(5) . . . . ? C15 Re3 S4 Fe3 -76.8(5) . . . . ? C17 Re3 S4 Fe3 98.8(4) . . . . ? P2 Re3 S4 Fe3 -165.6(2) . . . . ? C18 Re3 S4 Fe4 89(3) . . . . ? C16 Re3 S4 Fe4 -68.4(5) . . . . ? C15 Re3 S4 Fe4 -154.8(5) . . . . ? C17 Re3 S4 Fe4 20.8(4) . . . . ? P2 Re3 S4 Fe4 116.4(2) . . . . ? C18 Re3 S4 Re4 -46(3) . . . . ? C16 Re3 S4 Re4 156.9(4) . . . . ? C15 Re3 S4 Re4 70.4(5) . . . . ? C17 Re3 S4 Re4 -114.0(4) . . . . ? P2 Re3 S4 Re4 -18.38(12) . . . . ? C1 Re1 P1 C31 81.0(7) . . . . ? C2 Re1 P1 C31 -120(7) . . . . ? C4 Re1 P1 C31 171.6(7) . . . . ? C3 Re1 P1 C31 -11.1(7) . . . . ? S1 Re1 P1 C31 -100.2(6) . . . . ? C1 Re1 P1 C41 -35.0(8) . . . . ? C2 Re1 P1 C41 124(7) . . . . ? C4 Re1 P1 C41 55.6(8) . . . . ? C3 Re1 P1 C41 -127.0(8) . . . . ? S1 Re1 P1 C41 143.8(7) . . . . ? C1 Re1 P1 Re2 -162.9(5) . . . . ? C2 Re1 P1 Re2 -4(7) . . . . ? C4 Re1 P1 Re2 -72.3(5) . . . . ? C3 Re1 P1 Re2 105.1(4) . . . . ? S1 Re1 P1 Re2 15.93(12) . . . . ? C7 Re2 P1 C31 -75.1(8) . . . . ? C8 Re2 P1 C31 128(6) . . . . ? C6 Re2 P1 C31 14.1(7) . . . . ? C5 Re2 P1 C31 -165.6(7) . . . . ? S1 Re2 P1 C31 100.5(6) . . . . ? C7 Re2 P1 C41 40.2(9) . . . . ? C8 Re2 P1 C41 -117(6) . . . . ? C6 Re2 P1 C41 129.4(9) . . . . ? C5 Re2 P1 C41 -50.3(9) . . . . ? S1 Re2 P1 C41 -144.2(8) . . . . ? C7 Re2 P1 Re1 168.4(5) . . . . ? C8 Re2 P1 Re1 11(6) . . . . ? C6 Re2 P1 Re1 -102.4(5) . . . . ? C5 Re2 P1 Re1 77.9(5) . . . . ? S1 Re2 P1 Re1 -15.93(12) . . . . ? C19 Re4 P2 C61 34.6(7) . . . . ? C20 Re4 P2 C61 -161(25) . . . . ? C21 Re4 P2 C61 -60.5(7) . . . . ? C22 Re4 P2 C61 122.9(7) . . . . ? S4 Re4 P2 C61 -147.3(5) . . . . ? C19 Re4 P2 C51 -81.7(7) . . . . ? C20 Re4 P2 C51 83(25) . . . . ? C21 Re4 P2 C51 -176.8(7) . . . . ? C22 Re4 P2 C51 6.6(6) . . . . ? S4 Re4 P2 C51 96.4(5) . . . . ? C19 Re4 P2 Re3 163.0(5) . . . . ? C20 Re4 P2 Re3 -32(25) . . . . ? C21 Re4 P2 Re3 67.9(5) . . . . ? C22 Re4 P2 Re3 -108.7(5) . . . . ? S4 Re4 P2 Re3 -18.89(13) . . . . ? C18 Re3 P2 C61 -40.1(7) . . . . ? C16 Re3 P2 C61 102(4) . . . . ? C15 Re3 P2 C61 50.0(7) . . . . ? C17 Re3 P2 C61 -130.2(6) . . . . ? S4 Re3 P2 C61 144.3(5) . . . . ? C18 Re3 P2 C51 80.1(7) . . . . ? C16 Re3 P2 C51 -138(4) . . . . ? C15 Re3 P2 C51 170.2(7) . . . . ? C17 Re3 P2 C51 -10.0(6) . . . . ? S4 Re3 P2 C51 -95.6(5) . . . . ? C18 Re3 P2 Re4 -165.7(5) . . . . ? C16 Re3 P2 Re4 -23(4) . . . . ? C15 Re3 P2 Re4 -75.6(5) . . . . ? C17 Re3 P2 Re4 104.3(4) . . . . ? S4 Re3 P2 Re4 18.70(13) . . . . ? C2 Re1 C1 O1 -33(17) . . . . ? C4 Re1 C1 O1 60(17) . . . . ? C3 Re1 C1 O1 -124(17) . . . . ? P1 Re1 C1 O1 146(17) . . . . ? S1 Re1 C1 O1 136(15) . . . . ? C1 Re1 C2 O2 25(15) . . . . ? C4 Re1 C2 O2 -66(15) . . . . ? C3 Re1 C2 O2 117(15) . . . . ? P1 Re1 C2 O2 -134(12) . . . . ? S1 Re1 C2 O2 -153(15) . . . . ? C1 Re1 C3 O3 114(18) . . . . ? C2 Re1 C3 O3 27(18) . . . . ? C4 Re1 C3 O3 -113(19) . . . . ? P1 Re1 C3 O3 -149(18) . . . . ? S1 Re1 C3 O3 -72(18) . . . . ? C1 Re1 C4 O41 15(17) . . . . ? C2 Re1 C4 O41 102(17) . . . . ? C3 Re1 C4 O41 -118(18) . . . . ? P1 Re1 C4 O41 -82(17) . . . . ? S1 Re1 C4 O41 -159(17) . . . . ? C1 Re1 C4 O42 -144(9) . . . . ? C2 Re1 C4 O42 -57(9) . . . . ? C3 Re1 C4 O42 83(13) . . . . ? P1 Re1 C4 O42 119(9) . . . . ? S1 Re1 C4 O42 42(9) . . . . ? C7 Re2 C5 O5 62(16) . . . . ? C8 Re2 C5 O5 -28(16) . . . . ? C6 Re2 C5 O5 -18(23) . . . . ? P1 Re2 C5 O5 157(16) . . . . ? S1 Re2 C5 O5 -127(16) . . . . ? C7 Re2 C6 O6 -50(28) . . . . ? C8 Re2 C6 O6 40(28) . . . . ? C5 Re2 C6 O6 30(35) . . . . ? P1 Re2 C6 O6 -145(28) . . . . ? S1 Re2 C6 O6 139(28) . . . . ? C8 Re2 C7 O7 -76(22) . . . . ? C6 Re2 C7 O7 15(22) . . . . ? C5 Re2 C7 O7 -162(22) . . . . ? P1 Re2 C7 O7 106(22) . . . . ? S1 Re2 C7 O7 81(22) . . . . ? C7 Re2 C8 O8 -25(31) . . . . ? C6 Re2 C8 O8 -114(31) . . . . ? C5 Re2 C8 O8 65(31) . . . . ? P1 Re2 C8 O8 132(28) . . . . ? S1 Re2 C8 O8 159(31) . . . . ? C11 Fe1 C9 O9 33(13) . . . . ? C10 Fe1 C9 O9 136(13) . . . . ? S2 Fe1 C9 O9 -102(13) . . . . ? S1 Fe1 C9 O9 -74(13) . . . . ? Fe2 Fe1 C9 O9 -129(13) . . . . ? C9 Fe1 C10 O10 -16(26) . . . . ? C11 Fe1 C10 O10 79(26) . . . . ? S2 Fe1 C10 O10 177(100) . . . . ? S1 Fe1 C10 O10 -109(26) . . . . ? Fe2 Fe1 C10 O10 -127(26) . . . . ? C9 Fe1 C11 O11 126(21) . . . . ? C10 Fe1 C11 O11 32(22) . . . . ? S2 Fe1 C11 O11 -65(21) . . . . ? S1 Fe1 C11 O11 -144(21) . . . . ? Fe2 Fe1 C11 O11 -89(21) . . . . ? C13 Fe2 C12 O12 -7(11) . . . . ? C14 Fe2 C12 O12 89(11) . . . . ? S2 Fe2 C12 O12 -102(11) . . . . ? S1 Fe2 C12 O12 -171(11) . . . . ? Fe1 Fe2 C12 O12 -115(11) . . . . ? C12 Fe2 C13 O13 70(64) . . . . ? C14 Fe2 C13 O13 -35(64) . . . . ? S2 Fe2 C13 O13 -141(64) . . . . ? S1 Fe2 C13 O13 166(62) . . . . ? Fe1 Fe2 C13 O13 163(64) . . . . ? C13 Fe2 C14 O14 120(13) . . . . ? C12 Fe2 C14 O14 28(13) . . . . ? S2 Fe2 C14 O14 -146(13) . . . . ? S1 Fe2 C14 O14 -66(13) . . . . ? Fe1 Fe2 C14 O14 -96(13) . . . . ? C18 Re3 C15 O15 -55(11) . . . . ? C16 Re3 C15 O15 34(11) . . . . ? C17 Re3 C15 O15 31(18) . . . . ? P2 Re3 C15 O15 -151(11) . . . . ? S4 Re3 C15 O15 133(11) . . . . ? C18 Re3 C16 O16 68(11) . . . . ? C15 Re3 C16 O16 -22(11) . . . . ? C17 Re3 C16 O16 158(11) . . . . ? P2 Re3 C16 O16 -75(13) . . . . ? S4 Re3 C16 O16 -116(11) . . . . ? C18 Re3 C17 O17 38(26) . . . . ? C16 Re3 C17 O17 -52(26) . . . . ? C15 Re3 C17 O17 -48(30) . . . . ? P2 Re3 C17 O17 134(26) . . . . ? S4 Re3 C17 O17 -151(26) . . . . ? C16 Re3 C18 O18 57(16) . . . . ? C15 Re3 C18 O18 143(16) . . . . ? C17 Re3 C18 O18 -33(16) . . . . ? P2 Re3 C18 O18 -127(16) . . . . ? S4 Re3 C18 O18 -101(16) . . . . ? C20 Re4 C19 O19 93(18) . . . . ? C21 Re4 C19 O19 4(18) . . . . ? C22 Re4 C19 O19 -179(100) . . . . ? P2 Re4 C19 O19 -88(18) . . . . ? S4 Re4 C19 O19 -97(18) . . . . ? C19 Re4 C20 O20 7(15) . . . . ? C21 Re4 C20 O20 102(15) . . . . ? C22 Re4 C20 O20 -81(15) . . . . ? P2 Re4 C20 O20 -158(15) . . . . ? S4 Re4 C20 O20 -171(15) . . . . ? C19 Re4 C21 O21 89(11) . . . . ? C20 Re4 C21 O21 0(11) . . . . ? C22 Re4 C21 O21 -50(17) . . . . ? P2 Re4 C21 O21 -179(100) . . . . ? S4 Re4 C21 O21 -103(11) . . . . ? C19 Re4 C22 O22 -111(33) . . . . ? C20 Re4 C22 O22 -22(33) . . . . ? C21 Re4 C22 O22 28(38) . . . . ? P2 Re4 C22 O22 157(33) . . . . ? S4 Re4 C22 O22 81(33) . . . . ? C24 Fe3 C23 O23 -30(45) . . . . ? C25 Fe3 C23 O23 73(45) . . . . ? S3 Fe3 C23 O23 -178(100) . . . . ? S4 Fe3 C23 O23 -136(45) . . . . ? Fe4 Fe3 C23 O23 168(45) . . . . ? C23 Fe3 C24 O24 155(53) . . . . ? C25 Fe3 C24 O24 62(53) . . . . ? S3 Fe3 C24 O24 -34(53) . . . . ? S4 Fe3 C24 O24 -112(53) . . . . ? Fe4 Fe3 C24 O24 -61(54) . . . . ? C23 Fe3 C25 O25 27(37) . . . . ? C24 Fe3 C25 O25 123(37) . . . . ? S3 Fe3 C25 O25 -138(37) . . . . ? S4 Fe3 C25 O25 -68(38) . . . . ? Fe4 Fe3 C25 O25 -81(37) . . . . ? C27 Fe4 C26 O26 -21(33) . . . . ? C28 Fe4 C26 O26 74(33) . . . . ? S3 Fe4 C26 O26 -117(33) . . . . ? S4 Fe4 C26 O26 177(100) . . . . ? Fe3 Fe4 C26 O26 -127(33) . . . . ? C26 Fe4 C27 O27 -42(32) . . . . ? C28 Fe4 C27 O27 -143(32) . . . . ? S3 Fe4 C27 O27 108(32) . . . . ? S4 Fe4 C27 O27 56(33) . . . . ? Fe3 Fe4 C27 O27 52(32) . . . . ? C26 Fe4 C28 O28 17(18) . . . . ? C27 Fe4 C28 O28 109(18) . . . . ? S3 Fe4 C28 O28 -157(18) . . . . ? S4 Fe4 C28 O28 -77(18) . . . . ? Fe3 Fe4 C28 O28 -106(18) . . . . ? C41 P1 C31 C32 -63.4(13) . . . . ? Re1 P1 C31 C32 171.7(10) . . . . ? Re2 P1 C31 C32 60.6(12) . . . . ? C41 P1 C31 C36 64.1(13) . . . . ? Re1 P1 C31 C36 -60.7(12) . . . . ? Re2 P1 C31 C36 -171.9(10) . . . . ? C36 C31 C32 C33 57.9(16) . . . . ? P1 C31 C32 C33 -170.3(11) . . . . ? C31 C32 C33 C34 -55.8(19) . . . . ? C32 C33 C34 C35 52(2) . . . . ? C33 C34 C35 C36 -53(2) . . . . ? C34 C35 C36 C31 57.8(19) . . . . ? C32 C31 C36 C35 -58.3(17) . . . . ? P1 C31 C36 C35 169.8(12) . . . . ? C31 P1 C41 C46 132(2) . . . . ? Re1 P1 C41 C46 -107(2) . . . . ? Re2 P1 C41 C46 13(2) . . . . ? C31 P1 C41 C42 -93.0(18) . . . . ? Re1 P1 C41 C42 27(2) . . . . ? Re2 P1 C41 C42 147.6(16) . . . . ? C46 C41 C42 C43 -49(3) . . . . ? P1 C41 C42 C43 171.6(17) . . . . ? C41 C42 C43 C44 58(3) . . . . ? C42 C43 C44 C45 -64(3) . . . . ? C43 C44 C45 C46 64(3) . . . . ? C42 C41 C46 C45 49(3) . . . . ? P1 C41 C46 C45 -174.7(17) . . . . ? C44 C45 C46 C41 -61(4) . . . . ? C61 P2 C51 C56 -53.0(12) . . . . ? Re4 P2 C51 C56 68.8(11) . . . . ? Re3 P2 C51 C56 179.2(9) . . . . ? C61 P2 C51 C52 72.3(12) . . . . ? Re4 P2 C51 C52 -165.9(9) . . . . ? Re3 P2 C51 C52 -55.5(11) . . . . ? C56 C51 C52 C53 -65.5(15) . . . . ? P2 C51 C52 C53 165.8(10) . . . . ? C51 C52 C53 C54 64.3(16) . . . . ? C52 C53 C54 C55 -59.5(18) . . . . ? C53 C54 C55 C56 55.4(18) . . . . ? C54 C55 C56 C51 -56.6(17) . . . . ? C52 C51 C56 C55 61.0(16) . . . . ? P2 C51 C56 C55 -168.9(10) . . . . ? C51 P2 C61 C66 158.3(12) . . . . ? Re4 P2 C61 C66 40.4(14) . . . . ? Re3 P2 C61 C66 -79.3(13) . . . . ? C51 P2 C61 C62 -72.0(12) . . . . ? Re4 P2 C61 C62 170.1(10) . . . . ? Re3 P2 C61 C62 50.4(12) . . . . ? C66 C61 C62 C63 -58.5(19) . . . . ? P2 C61 C62 C63 168.9(12) . . . . ? C61 C62 C63 C64 56(2) . . . . ? C62 C63 C64 C65 -52(2) . . . . ? C63 C64 C65 C66 53(2) . . . . ? C62 C61 C66 C65 57.1(19) . . . . ? P2 C61 C66 C65 -170.5(12) . . . . ? C64 C65 C66 C61 -56(2) . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.830 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.280 #===END data_4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Fe4 O28 P2 Re4 Se4' _chemical_formula_sum 'C52 H44 Fe4 O28 P2 Re4 Se4' _chemical_formula_weight 2462.85 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' 'Se' 'Se' -0.0929 2.2259 '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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3334(7) _cell_length_b 11.9734(9) _cell_length_c 17.0212(13) _cell_angle_alpha 69.958(2) _cell_angle_beta 79.061(1) _cell_angle_gamma 77.534(1) _cell_volume 1730.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 3138 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.18 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.30 _exptl_crystal_density_meas not_measured _exptl_crystal_density_method 'none' _exptl_crystal_density_diffrn 2.363 _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 10.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.470 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 1420 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 11004 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7669 _reflns_number_gt 5656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0054P)^2^] 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 7669 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 0.778 _refine_ls_restrained_S_all 0.778 _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 Re1 Re 0.39749(3) 0.85946(2) 0.163472(15) 0.02144(7) Uani 1 1 d . . . Re2 Re 0.03993(3) 0.72823(2) 0.309146(16) 0.02108(7) Uani 1 1 d . . . Fe1 Fe 0.09707(10) 1.08279(8) 0.31515(5) 0.0223(2) Uani 1 1 d . . . Fe2 Fe 0.28651(9) 0.92362(8) 0.40647(5) 0.0220(2) Uani 1 1 d . . . Se1 Se 0.20269(7) 0.89378(6) 0.29116(4) 0.01874(14) Uani 1 1 d . . . Se2 Se 0.02932(7) 0.94600(6) 0.44839(4) 0.02246(15) Uani 1 1 d . . . P1 P 0.26113(17) 0.68193(15) 0.20595(10) 0.0195(4) Uani 1 1 d . . . O1 O 0.5623(5) 1.0769(4) 0.1141(3) 0.0409(13) Uani 1 1 d . . . C1 C 0.4964(7) 0.9987(6) 0.1354(4) 0.0304(17) Uani 1 1 d . . . O2 O 0.6115(5) 0.7166(4) 0.2986(3) 0.0394(13) Uani 1 1 d . . . C2 C 0.5325(7) 0.7690(6) 0.2487(4) 0.0269(16) Uani 1 1 d . . . O3 O 0.1676(6) 1.0121(5) 0.0383(3) 0.0521(15) Uani 1 1 d . . . C3 C 0.2498(8) 0.9548(6) 0.0830(4) 0.0291(17) Uani 1 1 d . . . O4 O 0.6300(5) 0.7819(5) 0.0302(3) 0.0453(14) Uani 1 1 d . . . C4 C 0.5389(8) 0.8107(6) 0.0786(4) 0.0288(16) Uani 1 1 d . . . O5 O -0.1307(6) 0.9176(5) 0.1658(3) 0.0548(16) Uani 1 1 d . . . C5 C -0.0655(8) 0.8494(7) 0.2162(4) 0.0346(18) Uani 1 1 d . . . O6 O -0.1073(5) 0.5300(5) 0.2974(3) 0.0552(16) Uani 1 1 d . . . C6 C -0.0527(7) 0.6043(6) 0.3029(4) 0.0297(16) Uani 1 1 d . . . O7 O 0.1789(6) 0.5428(5) 0.4670(3) 0.0527(15) Uani 1 1 d . . . C7 C 0.1334(7) 0.6125(7) 0.4076(4) 0.0333(18) Uani 1 1 d . . . O8 O -0.2340(5) 0.7696(5) 0.4371(3) 0.0445(14) Uani 1 1 d . . . C8 C -0.1284(8) 0.7612(6) 0.3903(4) 0.0278(16) Uani 1 1 d . . . O9 O 0.2781(6) 1.2221(5) 0.1696(3) 0.0567(16) Uani 1 1 d . . . C9 C 0.2108(8) 1.1640(6) 0.2272(4) 0.0337(17) Uani 1 1 d . . . O10 O 0.0258(6) 1.2828(4) 0.3840(3) 0.0507(15) Uani 1 1 d . . . C10 C 0.0561(7) 1.2048(6) 0.3569(4) 0.0306(17) Uani 1 1 d . . . O11 O -0.1751(6) 1.1264(5) 0.2382(3) 0.0554(16) Uani 1 1 d . . . C11 C -0.0715(8) 1.1114(6) 0.2674(4) 0.0312(17) Uani 1 1 d . . . O12 O 0.3429(5) 1.0090(5) 0.5372(3) 0.0423(13) Uani 1 1 d . . . C12 C 0.3192(7) 0.9782(6) 0.4841(4) 0.0277(16) Uani 1 1 d . . . O13 O 0.5557(5) 1.0043(5) 0.3015(3) 0.0444(14) Uani 1 1 d . . . C13 C 0.4478(8) 0.9743(6) 0.3411(4) 0.0302(17) Uani 1 1 d . . . O14 O 0.4083(6) 0.6704(5) 0.4882(3) 0.0560(16) Uani 1 1 d . . . C14 C 0.3601(8) 0.7677(7) 0.4580(4) 0.0323(17) Uani 1 1 d . . . C21 C 0.3799(6) 0.5405(5) 0.2625(4) 0.0224(14) Uani 1 1 d . . . H21A H 0.3997 0.5552 0.3136 0.027 Uiso 1 1 calc R . . C22 C 0.3057(7) 0.4281(6) 0.2966(4) 0.0314(17) Uani 1 1 d . . . H22A H 0.2080 0.4469 0.3283 0.038 Uiso 1 1 calc R . . H22B H 0.2892 0.4053 0.2488 0.038 Uiso 1 1 calc R . . C23 C 0.3968(7) 0.3240(6) 0.3532(4) 0.0379(19) Uani 1 1 d . . . H23A H 0.3463 0.2529 0.3720 0.046 Uiso 1 1 calc R . . H23B H 0.4052 0.3439 0.4039 0.046 Uiso 1 1 calc R . . C24 C 0.5499(7) 0.2931(6) 0.3099(4) 0.0388(18) Uani 1 1 d . . . H24A H 0.5427 0.2638 0.2632 0.047 Uiso 1 1 calc R . . H24B H 0.6088 0.2279 0.3505 0.047 Uiso 1 1 calc R . . C25 C 0.6278(7) 0.4046(6) 0.2748(4) 0.0383(18) Uani 1 1 d . . . H25A H 0.6434 0.4296 0.3219 0.046 Uiso 1 1 calc R . . H25B H 0.7258 0.3844 0.2439 0.046 Uiso 1 1 calc R . . C26 C 0.5349(7) 0.5066(6) 0.2163(4) 0.0299(16) Uani 1 1 d . . . H26A H 0.5235 0.4826 0.1680 0.036 Uiso 1 1 calc R . . H26B H 0.5858 0.5778 0.1941 0.036 Uiso 1 1 calc R . . C31 C 0.2110(8) 0.6457(7) 0.1170(4) 0.040(2) Uani 1 1 d . . . H31A H 0.2105 0.5570 0.1411 0.048 Uiso 1 1 calc R . . C32 C 0.0659(9) 0.6911(10) 0.0916(5) 0.090(4) Uani 1 1 d . . . H32A H 0.0532 0.7802 0.0706 0.108 Uiso 1 1 calc R . . H32B H -0.0077 0.6684 0.1421 0.108 Uiso 1 1 calc R . . C33 C 0.0307(9) 0.6481(9) 0.0244(5) 0.065(3) Uani 1 1 d . . . H33A H 0.0151 0.5632 0.0500 0.078 Uiso 1 1 calc R . . H33B H -0.0627 0.6968 0.0038 0.078 Uiso 1 1 calc R . . C34 C 0.1473(11) 0.6564(11) -0.0476(5) 0.089(4) Uani 1 1 d . . . H34A H 0.1290 0.6092 -0.0813 0.107 Uiso 1 1 calc R . . H34B H 0.1405 0.7416 -0.0838 0.107 Uiso 1 1 calc R . . C35 C 0.2935(11) 0.6145(11) -0.0255(6) 0.099(4) Uani 1 1 d . . . H35A H 0.3638 0.6414 -0.0769 0.119 Uiso 1 1 calc R . . H35B H 0.3104 0.5253 -0.0066 0.119 Uiso 1 1 calc R . . C36 C 0.3299(8) 0.6545(8) 0.0417(4) 0.051(2) Uani 1 1 d . . . H36A H 0.3467 0.7391 0.0168 0.061 Uiso 1 1 calc R . . H36B H 0.4234 0.6047 0.0616 0.061 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 Re1 0.01948(14) 0.02076(15) 0.02145(14) -0.00591(12) 0.00134(11) -0.00245(12) Re2 0.01713(14) 0.02174(16) 0.02527(15) -0.00935(12) -0.00051(11) -0.00372(12) Fe1 0.0219(5) 0.0190(5) 0.0250(5) -0.0078(4) -0.0011(4) -0.0015(4) Fe2 0.0192(5) 0.0239(5) 0.0245(5) -0.0099(4) -0.0036(4) -0.0021(4) Se1 0.0170(3) 0.0195(4) 0.0201(3) -0.0076(3) -0.0011(3) -0.0027(3) Se2 0.0213(3) 0.0248(4) 0.0232(3) -0.0109(3) 0.0011(3) -0.0055(3) P1 0.0180(9) 0.0205(10) 0.0203(9) -0.0081(8) -0.0011(7) -0.0021(7) O1 0.040(3) 0.035(3) 0.045(3) -0.008(3) 0.000(2) -0.014(3) C1 0.024(4) 0.033(4) 0.027(4) -0.007(3) -0.004(3) 0.008(3) O2 0.036(3) 0.038(3) 0.049(3) -0.017(3) -0.021(3) 0.003(3) C2 0.018(4) 0.033(4) 0.031(4) -0.011(3) 0.005(3) -0.014(3) O3 0.049(4) 0.049(4) 0.049(4) 0.002(3) -0.024(3) -0.001(3) C3 0.033(4) 0.034(5) 0.021(4) -0.009(3) 0.004(3) -0.013(4) O4 0.042(3) 0.052(4) 0.036(3) -0.018(3) 0.016(2) -0.007(3) C4 0.036(4) 0.025(4) 0.023(4) -0.001(3) -0.006(3) -0.007(3) O5 0.045(4) 0.065(4) 0.049(4) -0.013(3) -0.024(3) 0.008(3) C5 0.032(4) 0.038(5) 0.038(5) -0.015(4) 0.000(3) -0.015(4) O6 0.035(3) 0.035(3) 0.104(5) -0.028(3) -0.017(3) -0.005(3) C6 0.016(4) 0.021(4) 0.049(5) -0.011(4) -0.008(3) 0.006(3) O7 0.064(4) 0.048(4) 0.039(3) -0.002(3) -0.015(3) -0.008(3) C7 0.026(4) 0.034(5) 0.039(5) -0.012(4) 0.004(3) -0.010(4) O8 0.031(3) 0.046(4) 0.060(4) -0.030(3) 0.019(3) -0.014(3) C8 0.038(4) 0.021(4) 0.026(4) -0.007(3) -0.010(3) -0.006(3) O9 0.070(4) 0.031(3) 0.052(4) -0.004(3) 0.022(3) -0.012(3) C9 0.038(4) 0.019(4) 0.043(5) -0.015(4) -0.002(4) 0.002(3) O10 0.069(4) 0.027(3) 0.054(3) -0.019(3) 0.013(3) -0.011(3) C10 0.027(4) 0.029(4) 0.032(4) -0.008(3) 0.002(3) -0.007(3) O11 0.037(3) 0.062(4) 0.069(4) -0.020(3) -0.023(3) 0.002(3) C11 0.034(4) 0.023(4) 0.034(4) -0.011(3) -0.002(3) 0.004(3) O12 0.030(3) 0.057(4) 0.055(3) -0.038(3) -0.015(2) 0.004(3) C12 0.018(4) 0.035(4) 0.032(4) -0.013(3) -0.004(3) -0.001(3) O13 0.035(3) 0.069(4) 0.040(3) -0.023(3) 0.001(2) -0.025(3) C13 0.037(4) 0.033(4) 0.031(4) -0.020(3) -0.012(3) -0.004(4) O14 0.066(4) 0.033(3) 0.068(4) -0.005(3) -0.031(3) -0.003(3) C14 0.034(4) 0.033(5) 0.032(4) -0.006(4) -0.011(3) -0.011(4) C21 0.023(4) 0.017(4) 0.022(3) -0.004(3) 0.001(3) 0.001(3) C22 0.028(4) 0.022(4) 0.047(5) -0.013(4) -0.003(3) -0.006(3) C23 0.030(4) 0.026(4) 0.053(5) 0.001(4) -0.011(4) -0.011(4) C24 0.037(5) 0.019(4) 0.055(5) -0.004(4) -0.017(4) 0.003(3) C25 0.026(4) 0.030(4) 0.051(5) -0.010(4) -0.001(3) 0.006(3) C26 0.029(4) 0.028(4) 0.030(4) -0.012(3) 0.000(3) 0.003(3) C31 0.043(5) 0.055(6) 0.028(4) -0.023(4) 0.001(3) -0.007(4) C32 0.049(6) 0.179(12) 0.069(7) -0.071(8) -0.016(5) -0.013(7) C33 0.060(6) 0.093(8) 0.064(6) -0.047(6) -0.032(5) 0.002(6) C34 0.088(8) 0.163(12) 0.036(5) -0.048(7) -0.018(5) -0.027(8) C35 0.080(8) 0.186(13) 0.067(7) -0.093(8) -0.003(6) -0.013(8) C36 0.053(5) 0.068(7) 0.035(5) -0.024(4) 0.005(4) -0.014(5) _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 Re1 C4 1.921(7) . ? Re1 C1 1.952(7) . ? Re1 C2 1.973(7) . ? Re1 C3 2.011(7) . ? Re1 P1 2.5350(16) . ? Re1 Se1 2.6435(6) . ? Re2 C6 1.912(7) . ? Re2 C8 1.954(7) . ? Re2 C7 1.983(8) . ? Re2 C5 1.994(8) . ? Re2 P1 2.5401(16) . ? Re2 Se1 2.6529(6) . ? Fe1 C10 1.776(7) . ? Fe1 C9 1.777(7) . ? Fe1 C11 1.820(7) . ? Fe1 Se2 2.3627(11) . ? Fe1 Se1 2.4036(11) . ? Fe1 Fe2 2.5947(13) . ? Fe2 C12 1.760(6) . ? Fe2 C13 1.780(7) . ? Fe2 C14 1.810(8) . ? Fe2 Se2 2.3550(11) . ? Fe2 Se1 2.4034(10) . ? Se2 Se2 2.4383(12) 2_576 ? P1 C21 1.871(6) . ? P1 C31 1.873(6) . ? O1 C1 1.148(7) . ? O2 C2 1.154(7) . ? O3 C3 1.129(8) . ? O4 C4 1.150(7) . ? O5 C5 1.131(8) . ? O6 C6 1.154(7) . ? O7 C7 1.153(8) . ? O8 C8 1.153(7) . ? O9 C9 1.152(7) . ? O10 C10 1.138(7) . ? O11 C11 1.124(7) . ? O12 C12 1.158(6) . ? O13 C13 1.153(7) . ? O14 C14 1.130(8) . ? C21 C22 1.531(8) . ? C21 C26 1.553(8) . ? C22 C23 1.495(9) . ? C23 C24 1.510(9) . ? C24 C25 1.541(8) . ? C25 C26 1.507(9) . ? C31 C32 1.435(10) . ? C31 C36 1.518(8) . ? C32 C33 1.516(9) . ? C33 C34 1.467(10) . ? C34 C35 1.423(12) . ? C35 C36 1.499(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 C4 Re1 C1 87.1(3) . . ? C4 Re1 C2 90.1(3) . . ? C1 Re1 C2 89.3(3) . . ? C4 Re1 C3 93.9(3) . . ? C1 Re1 C3 91.0(3) . . ? C2 Re1 C3 176.0(3) . . ? C4 Re1 P1 95.76(19) . . ? C1 Re1 P1 177.13(18) . . ? C2 Re1 P1 90.40(18) . . ? C3 Re1 P1 89.11(18) . . ? C4 Re1 Se1 171.90(19) . . ? C1 Re1 Se1 99.87(18) . . ? C2 Re1 Se1 85.92(18) . . ? C3 Re1 Se1 90.10(18) . . ? P1 Re1 Se1 77.26(4) . . ? C6 Re2 C8 87.8(3) . . ? C6 Re2 C7 89.9(3) . . ? C8 Re2 C7 86.4(3) . . ? C6 Re2 C5 90.9(3) . . ? C8 Re2 C5 89.3(3) . . ? C7 Re2 C5 175.7(3) . . ? C6 Re2 P1 92.04(19) . . ? C8 Re2 P1 178.9(2) . . ? C7 Re2 P1 92.45(19) . . ? C5 Re2 P1 91.8(2) . . ? C6 Re2 Se1 168.71(19) . . ? C8 Re2 Se1 103.20(18) . . ? C7 Re2 Se1 93.25(19) . . ? C5 Re2 Se1 86.82(19) . . ? P1 Re2 Se1 77.00(4) . . ? C10 Fe1 C9 91.0(3) . . ? C10 Fe1 C11 98.5(3) . . ? C9 Fe1 C11 99.5(3) . . ? C10 Fe1 Se2 91.6(2) . . ? C9 Fe1 Se2 159.5(2) . . ? C11 Fe1 Se2 100.1(2) . . ? C10 Fe1 Se1 162.4(2) . . ? C9 Fe1 Se1 92.6(2) . . ? C11 Fe1 Se1 97.9(2) . . ? Se2 Fe1 Se1 79.23(3) . . ? C10 Fe1 Fe2 105.1(2) . . ? C9 Fe1 Fe2 103.3(2) . . ? C11 Fe1 Fe2 146.6(2) . . ? Se2 Fe1 Fe2 56.49(3) . . ? Se1 Fe1 Fe2 57.33(3) . . ? C12 Fe2 C13 90.4(3) . . ? C12 Fe2 C14 95.5(3) . . ? C13 Fe2 C14 100.6(3) . . ? C12 Fe2 Se2 93.0(2) . . ? C13 Fe2 Se2 152.4(2) . . ? C14 Fe2 Se2 106.3(2) . . ? C12 Fe2 Se1 166.4(2) . . ? C13 Fe2 Se1 91.29(19) . . ? C14 Fe2 Se1 97.5(2) . . ? Se2 Fe2 Se1 79.39(3) . . ? C12 Fe2 Fe1 109.1(2) . . ? C13 Fe2 Fe1 96.3(2) . . ? C14 Fe2 Fe1 150.0(2) . . ? Se2 Fe2 Fe1 56.78(3) . . ? Se1 Fe2 Fe1 57.34(3) . . ? Fe2 Se1 Fe1 65.34(3) . . ? Fe2 Se1 Re1 119.28(3) . . ? Fe1 Se1 Re1 127.07(3) . . ? Fe2 Se1 Re2 123.98(3) . . ? Fe1 Se1 Re2 122.21(3) . . ? Re1 Se1 Re2 98.95(2) . . ? Fe2 Se2 Fe1 66.73(3) . . ? Fe2 Se2 Se2 108.43(4) . 2_576 ? Fe1 Se2 Se2 108.23(4) . 2_576 ? C21 P1 C31 103.9(3) . . ? C21 P1 Re1 110.22(19) . . ? C31 P1 Re1 115.6(2) . . ? C21 P1 Re2 108.31(18) . . ? C31 P1 Re2 113.6(2) . . ? Re1 P1 Re2 104.98(6) . . ? O1 C1 Re1 174.4(6) . . ? O2 C2 Re1 179.6(6) . . ? O3 C3 Re1 177.5(6) . . ? O4 C4 Re1 175.9(6) . . ? O5 C5 Re2 177.1(6) . . ? O6 C6 Re2 178.6(6) . . ? O7 C7 Re2 175.5(6) . . ? O8 C8 Re2 171.9(5) . . ? O9 C9 Fe1 176.1(6) . . ? O10 C10 Fe1 178.1(6) . . ? O11 C11 Fe1 178.5(6) . . ? O12 C12 Fe2 177.0(7) . . ? O13 C13 Fe2 177.1(6) . . ? O14 C14 Fe2 178.2(7) . . ? C22 C21 C26 107.8(5) . . ? C22 C21 P1 115.1(4) . . ? C26 C21 P1 117.3(4) . . ? C23 C22 C21 112.1(5) . . ? C22 C23 C24 112.1(6) . . ? C23 C24 C25 110.5(6) . . ? C26 C25 C24 109.9(6) . . ? C25 C26 C21 111.2(5) . . ? C32 C31 C36 111.8(6) . . ? C32 C31 P1 119.8(6) . . ? C36 C31 P1 114.8(5) . . ? C31 C32 C33 116.0(8) . . ? C34 C33 C32 113.4(7) . . ? C35 C34 C33 114.6(8) . . ? C34 C35 C36 116.2(8) . . ? C35 C36 C31 114.0(6) . . ? 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 C10 Fe1 Fe2 C12 0.9(3) . . . . ? C9 Fe1 Fe2 C12 95.7(3) . . . . ? C11 Fe1 Fe2 C12 -132.4(4) . . . . ? Se2 Fe1 Fe2 C12 -80.8(2) . . . . ? Se1 Fe1 Fe2 C12 -179.9(2) . . . . ? C10 Fe1 Fe2 C13 -91.7(3) . . . . ? C9 Fe1 Fe2 C13 3.0(3) . . . . ? C11 Fe1 Fe2 C13 135.0(4) . . . . ? Se2 Fe1 Fe2 C13 -173.4(2) . . . . ? Se1 Fe1 Fe2 C13 87.48(19) . . . . ? C10 Fe1 Fe2 C14 144.1(5) . . . . ? C9 Fe1 Fe2 C14 -121.1(5) . . . . ? C11 Fe1 Fe2 C14 10.8(6) . . . . ? Se2 Fe1 Fe2 C14 62.4(5) . . . . ? Se1 Fe1 Fe2 C14 -36.7(5) . . . . ? C10 Fe1 Fe2 Se2 81.7(2) . . . . ? C9 Fe1 Fe2 Se2 176.4(2) . . . . ? C11 Fe1 Fe2 Se2 -51.6(4) . . . . ? Se1 Fe1 Fe2 Se2 -99.12(4) . . . . ? C10 Fe1 Fe2 Se1 -179.2(2) . . . . ? C9 Fe1 Fe2 Se1 -84.4(2) . . . . ? C11 Fe1 Fe2 Se1 47.5(4) . . . . ? Se2 Fe1 Fe2 Se1 99.12(4) . . . . ? C12 Fe2 Se1 Fe1 0.5(8) . . . . ? C13 Fe2 Se1 Fe1 -96.7(2) . . . . ? C14 Fe2 Se1 Fe1 162.5(2) . . . . ? Se2 Fe2 Se1 Fe1 57.18(3) . . . . ? C12 Fe2 Se1 Re1 120.7(8) . . . . ? C13 Fe2 Se1 Re1 23.5(2) . . . . ? C14 Fe2 Se1 Re1 -77.3(2) . . . . ? Se2 Fe2 Se1 Re1 177.37(3) . . . . ? Fe1 Fe2 Se1 Re1 120.19(4) . . . . ? C12 Fe2 Se1 Re2 -113.0(8) . . . . ? C13 Fe2 Se1 Re2 149.9(2) . . . . ? C14 Fe2 Se1 Re2 49.0(2) . . . . ? Se2 Fe2 Se1 Re2 -56.26(4) . . . . ? Fe1 Fe2 Se1 Re2 -113.44(4) . . . . ? C10 Fe1 Se1 Fe2 2.6(7) . . . . ? C9 Fe1 Se1 Fe2 104.2(2) . . . . ? C11 Fe1 Se1 Fe2 -155.8(2) . . . . ? Se2 Fe1 Se1 Fe2 -56.93(3) . . . . ? C10 Fe1 Se1 Re1 -106.5(7) . . . . ? C9 Fe1 Se1 Re1 -4.9(2) . . . . ? C11 Fe1 Se1 Re1 95.1(2) . . . . ? Se2 Fe1 Se1 Re1 -166.06(3) . . . . ? Fe2 Fe1 Se1 Re1 -109.13(4) . . . . ? C10 Fe1 Se1 Re2 118.5(7) . . . . ? C9 Fe1 Se1 Re2 -139.9(2) . . . . ? C11 Fe1 Se1 Re2 -39.9(2) . . . . ? Se2 Fe1 Se1 Re2 59.02(4) . . . . ? Fe2 Fe1 Se1 Re2 115.95(4) . . . . ? C4 Re1 Se1 Fe2 96.6(13) . . . . ? C1 Re1 Se1 Fe2 -52.37(19) . . . . ? C2 Re1 Se1 Fe2 36.20(18) . . . . ? C3 Re1 Se1 Fe2 -143.39(18) . . . . ? P1 Re1 Se1 Fe2 127.54(5) . . . . ? C4 Re1 Se1 Fe1 176.5(13) . . . . ? C1 Re1 Se1 Fe1 27.5(2) . . . . ? C2 Re1 Se1 Fe1 116.06(18) . . . . ? C3 Re1 Se1 Fe1 -63.53(19) . . . . ? P1 Re1 Se1 Fe1 -152.60(6) . . . . ? C4 Re1 Se1 Re2 -40.9(13) . . . . ? C1 Re1 Se1 Re2 170.15(19) . . . . ? C2 Re1 Se1 Re2 -101.27(18) . . . . ? C3 Re1 Se1 Re2 79.13(18) . . . . ? P1 Re1 Se1 Re2 -9.94(4) . . . . ? C6 Re2 Se1 Fe2 -138.9(10) . . . . ? C8 Re2 Se1 Fe2 54.1(2) . . . . ? C7 Re2 Se1 Fe2 -33.0(2) . . . . ? C5 Re2 Se1 Fe2 142.7(2) . . . . ? P1 Re2 Se1 Fe2 -124.76(6) . . . . ? C6 Re2 Se1 Fe1 140.9(10) . . . . ? C8 Re2 Se1 Fe1 -26.1(2) . . . . ? C7 Re2 Se1 Fe1 -113.2(2) . . . . ? C5 Re2 Se1 Fe1 62.5(2) . . . . ? P1 Re2 Se1 Fe1 155.04(5) . . . . ? C6 Re2 Se1 Re1 -4.3(10) . . . . ? C8 Re2 Se1 Re1 -171.22(19) . . . . ? C7 Re2 Se1 Re1 101.69(19) . . . . ? C5 Re2 Se1 Re1 -82.6(2) . . . . ? P1 Re2 Se1 Re1 9.93(4) . . . . ? C12 Fe2 Se2 Fe1 110.9(2) . . . . ? C13 Fe2 Se2 Fe1 14.3(4) . . . . ? C14 Fe2 Se2 Fe1 -152.5(2) . . . . ? Se1 Fe2 Se2 Fe1 -57.74(3) . . . . ? C12 Fe2 Se2 Se2 8.4(2) . . . 2_576 ? C13 Fe2 Se2 Se2 -88.2(4) . . . 2_576 ? C14 Fe2 Se2 Se2 105.0(2) . . . 2_576 ? Se1 Fe2 Se2 Se2 -160.20(4) . . . 2_576 ? Fe1 Fe2 Se2 Se2 -102.46(5) . . . 2_576 ? C10 Fe1 Se2 Fe2 -107.1(2) . . . . ? C9 Fe1 Se2 Fe2 -9.9(6) . . . . ? C11 Fe1 Se2 Fe2 154.0(2) . . . . ? Se1 Fe1 Se2 Fe2 57.78(3) . . . . ? C10 Fe1 Se2 Se2 -4.4(2) . . . 2_576 ? C9 Fe1 Se2 Se2 92.8(6) . . . 2_576 ? C11 Fe1 Se2 Se2 -103.3(2) . . . 2_576 ? Se1 Fe1 Se2 Se2 160.53(4) . . . 2_576 ? Fe2 Fe1 Se2 Se2 102.75(5) . . . 2_576 ? C4 Re1 P1 C21 70.0(3) . . . . ? C1 Re1 P1 C21 -104(4) . . . . ? C2 Re1 P1 C21 -20.1(3) . . . . ? C3 Re1 P1 C21 163.9(3) . . . . ? Se1 Re1 P1 C21 -105.8(2) . . . . ? C4 Re1 P1 C31 -47.5(3) . . . . ? C1 Re1 P1 C31 138(4) . . . . ? C2 Re1 P1 C31 -137.6(3) . . . . ? C3 Re1 P1 C31 46.4(3) . . . . ? Se1 Re1 P1 C31 136.7(3) . . . . ? C4 Re1 P1 Re2 -173.6(2) . . . . ? C1 Re1 P1 Re2 12(4) . . . . ? C2 Re1 P1 Re2 96.34(19) . . . . ? C3 Re1 P1 Re2 -79.68(19) . . . . ? Se1 Re1 P1 Re2 10.62(4) . . . . ? C6 Re2 P1 C21 -75.6(3) . . . . ? C8 Re2 P1 C21 7(9) . . . . ? C7 Re2 P1 C21 14.4(3) . . . . ? C5 Re2 P1 C21 -166.5(3) . . . . ? Se1 Re2 P1 C21 107.1(2) . . . . ? C6 Re2 P1 C31 39.4(3) . . . . ? C8 Re2 P1 C31 122(9) . . . . ? C7 Re2 P1 C31 129.3(3) . . . . ? C5 Re2 P1 C31 -51.6(3) . . . . ? Se1 Re2 P1 C31 -137.9(3) . . . . ? C6 Re2 P1 Re1 166.7(2) . . . . ? C8 Re2 P1 Re1 -111(9) . . . . ? C7 Re2 P1 Re1 -103.4(2) . . . . ? C5 Re2 P1 Re1 75.73(19) . . . . ? Se1 Re2 P1 Re1 -10.59(4) . . . . ? C4 Re1 C1 O1 0(6) . . . . ? C2 Re1 C1 O1 90(6) . . . . ? C3 Re1 C1 O1 -94(6) . . . . ? P1 Re1 C1 O1 174(3) . . . . ? Se1 Re1 C1 O1 176(6) . . . . ? C4 Re1 C2 O2 115(100) . . . . ? C1 Re1 C2 O2 28(100) . . . . ? C3 Re1 C2 O2 -66(100) . . . . ? P1 Re1 C2 O2 -149(100) . . . . ? Se1 Re1 C2 O2 -72(100) . . . . ? C4 Re1 C3 O3 -114(14) . . . . ? C1 Re1 C3 O3 -27(14) . . . . ? C2 Re1 C3 O3 67(15) . . . . ? P1 Re1 C3 O3 150(14) . . . . ? Se1 Re1 C3 O3 73(14) . . . . ? C1 Re1 C4 O4 54(9) . . . . ? C2 Re1 C4 O4 -35(9) . . . . ? C3 Re1 C4 O4 145(9) . . . . ? P1 Re1 C4 O4 -125(9) . . . . ? Se1 Re1 C4 O4 -95(9) . . . . ? C6 Re2 C5 O5 68(13) . . . . ? C8 Re2 C5 O5 -20(13) . . . . ? C7 Re2 C5 O5 -32(15) . . . . ? P1 Re2 C5 O5 160(13) . . . . ? Se1 Re2 C5 O5 -123(13) . . . . ? C8 Re2 C6 O6 149(24) . . . . ? C7 Re2 C6 O6 -125(24) . . . . ? C5 Re2 C6 O6 59(24) . . . . ? P1 Re2 C6 O6 -33(24) . . . . ? Se1 Re2 C6 O6 -19(25) . . . . ? C6 Re2 C7 O7 -46(8) . . . . ? C8 Re2 C7 O7 42(8) . . . . ? C5 Re2 C7 O7 54(10) . . . . ? P1 Re2 C7 O7 -138(8) . . . . ? Se1 Re2 C7 O7 145(8) . . . . ? C6 Re2 C8 O8 1(4) . . . . ? C7 Re2 C8 O8 -89(4) . . . . ? C5 Re2 C8 O8 92(4) . . . . ? P1 Re2 C8 O8 -81(11) . . . . ? Se1 Re2 C8 O8 179(100) . . . . ? C10 Fe1 C9 O9 -49(9) . . . . ? C11 Fe1 C9 O9 50(9) . . . . ? Se2 Fe1 C9 O9 -146(9) . . . . ? Se1 Fe1 C9 O9 148(9) . . . . ? Fe2 Fe1 C9 O9 -155(9) . . . . ? C9 Fe1 C10 O10 131(19) . . . . ? C11 Fe1 C10 O10 31(19) . . . . ? Se2 Fe1 C10 O10 -70(19) . . . . ? Se1 Fe1 C10 O10 -128(19) . . . . ? Fe2 Fe1 C10 O10 -125(19) . . . . ? C10 Fe1 C11 O11 -153(25) . . . . ? C9 Fe1 C11 O11 114(25) . . . . ? Se2 Fe1 C11 O11 -60(25) . . . . ? Se1 Fe1 C11 O11 20(25) . . . . ? Fe2 Fe1 C11 O11 -19(26) . . . . ? C13 Fe2 C12 O12 -105(11) . . . . ? C14 Fe2 C12 O12 -4(11) . . . . ? Se2 Fe2 C12 O12 103(11) . . . . ? Se1 Fe2 C12 O12 158(10) . . . . ? Fe1 Fe2 C12 O12 159(10) . . . . ? C12 Fe2 C13 O13 56(12) . . . . ? C14 Fe2 C13 O13 -39(12) . . . . ? Se2 Fe2 C13 O13 154(11) . . . . ? Se1 Fe2 C13 O13 -137(12) . . . . ? Fe1 Fe2 C13 O13 166(12) . . . . ? C12 Fe2 C14 O14 -130(21) . . . . ? C13 Fe2 C14 O14 -38(21) . . . . ? Se2 Fe2 C14 O14 136(21) . . . . ? Se1 Fe2 C14 O14 55(21) . . . . ? Fe1 Fe2 C14 O14 85(21) . . . . ? C31 P1 C21 C22 -59.4(5) . . . . ? Re1 P1 C21 C22 176.1(4) . . . . ? Re2 P1 C21 C22 61.8(5) . . . . ? C31 P1 C21 C26 69.0(5) . . . . ? Re1 P1 C21 C26 -55.5(5) . . . . ? Re2 P1 C21 C26 -169.8(4) . . . . ? C26 C21 C22 C23 56.7(7) . . . . ? P1 C21 C22 C23 -170.3(5) . . . . ? C21 C22 C23 C24 -56.8(8) . . . . ? C22 C23 C24 C25 55.2(8) . . . . ? C23 C24 C25 C26 -56.3(8) . . . . ? C24 C25 C26 C21 59.1(7) . . . . ? C22 C21 C26 C25 -58.5(7) . . . . ? P1 C21 C26 C25 169.6(5) . . . . ? C21 P1 C31 C32 142.7(7) . . . . ? Re1 P1 C31 C32 -96.3(7) . . . . ? Re2 P1 C31 C32 25.2(8) . . . . ? C21 P1 C31 C36 -79.9(6) . . . . ? Re1 P1 C31 C36 41.0(7) . . . . ? Re2 P1 C31 C36 162.5(5) . . . . ? C36 C31 C32 C33 46.8(11) . . . . ? P1 C31 C32 C33 -174.7(6) . . . . ? C31 C32 C33 C34 -47.4(13) . . . . ? C32 C33 C34 C35 44.6(14) . . . . ? C33 C34 C35 C36 -44.7(15) . . . . ? C34 C35 C36 C31 44.5(14) . . . . ? C32 C31 C36 C35 -44.5(11) . . . . ? P1 C31 C36 C35 174.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.543 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.174 #===END data_4c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Fe4 O28 P2 Re4 Te4' _chemical_formula_sum 'C52 H44 Fe4 O28 P2 Re4 Te4' _chemical_formula_weight 2657.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.351(2) _cell_length_b 12.026(3) _cell_length_c 17.270(4) _cell_angle_alpha 108.910(4) _cell_angle_beta 90.285(4) _cell_angle_gamma 102.955(4) _cell_volume 1784.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2079 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.40 _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1222 _exptl_absorpt_coefficient_mu 9.269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1190 _exptl_absorpt_correction_T_max 0.7081 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 1170 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 11021 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.1428 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7833 _reflns_number_gt 4712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0416P)^2^] 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 7833 _refine_ls_number_parameters 424 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.880 _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 Te1 Te 0.28356(9) 0.67137(7) 0.28236(5) 0.0253(2) Uani 1 1 d . . . Te2 Te 0.46818(10) 0.88120(8) 0.44430(6) 0.0337(2) Uani 1 1 d . . . Re1 Re 0.08689(6) 0.50707(5) 0.15566(3) 0.03135(16) Uani 1 1 d . . . Re2 Re 0.45011(6) 0.51351(5) 0.29587(4) 0.03162(16) Uani 1 1 d . . . Fe1 Fe 0.3958(2) 0.89366(16) 0.30646(12) 0.0322(5) Uani 1 1 d . . . Fe2 Fe 0.1962(2) 0.82388(16) 0.40077(12) 0.0306(4) Uani 1 1 d . . . P1 P 0.2263(4) 0.3744(3) 0.1983(2) 0.0306(8) Uani 1 1 d . . . O1 O -0.0667(12) 0.6842(10) 0.1123(7) 0.057(3) Uani 1 1 d . . . C1 C -0.0081(15) 0.6223(12) 0.1301(8) 0.035(3) Uani 1 1 d . . . O2 O -0.1369(13) 0.2986(10) 0.0300(7) 0.069(4) Uani 1 1 d . . . C2 C -0.053(2) 0.3741(13) 0.0735(9) 0.052(4) Uani 1 1 d . . . O3 O 0.3218(13) 0.5435(11) 0.0315(7) 0.068(4) Uani 1 1 d . . . C3 C 0.2349(19) 0.5286(13) 0.0758(9) 0.047(4) Uani 1 1 d . . . O4 O -0.1205(12) 0.5014(9) 0.2944(7) 0.056(3) Uani 1 1 d . . . C4 C -0.0438(18) 0.5004(12) 0.2431(9) 0.042(4) Uani 1 1 d . . . O5 O 0.5928(12) 0.2991(10) 0.2752(10) 0.092(5) Uani 1 1 d . . . C5 C 0.5403(15) 0.3780(14) 0.2853(10) 0.050(4) Uani 1 1 d . . . O6 O 0.6207(14) 0.5738(11) 0.1538(8) 0.074(4) Uani 1 1 d . . . C6 C 0.5516(18) 0.5462(13) 0.2018(9) 0.046(4) Uani 1 1 d . . . O7 O 0.7178(11) 0.6809(10) 0.4175(7) 0.054(3) Uani 1 1 d . . . C7 C 0.6178(18) 0.6256(12) 0.3736(9) 0.044(4) Uani 1 1 d . . . O8 O 0.3027(15) 0.4885(12) 0.4519(8) 0.081(4) Uani 1 1 d . . . C8 C 0.3533(18) 0.4988(13) 0.3932(9) 0.044(4) Uani 1 1 d . . . O9 O 0.4601(13) 1.1586(10) 0.3754(7) 0.065(3) Uani 1 1 d . . . C9 C 0.4337(16) 1.0535(14) 0.3489(10) 0.047(4) Uani 1 1 d . . . O10 O 0.6644(14) 0.8596(11) 0.2288(8) 0.074(4) Uani 1 1 d . . . C10 C 0.5627(16) 0.8763(13) 0.2594(10) 0.047(4) Uani 1 1 d . . . O11 O 0.2101(15) 0.8898(10) 0.1684(8) 0.073(4) Uani 1 1 d . . . C11 C 0.2852(18) 0.8898(12) 0.2236(10) 0.048(4) Uani 1 1 d . . . O12 O 0.0761(13) 0.6626(10) 0.4928(7) 0.069(4) Uani 1 1 d . . . C12 C 0.1239(17) 0.7255(16) 0.4576(9) 0.050(4) Uani 1 1 d . . . O13 O 0.1565(11) 1.0515(9) 0.5173(7) 0.060(3) Uani 1 1 d . . . C13 C 0.1724(15) 0.9611(14) 0.4701(9) 0.040(4) Uani 1 1 d . . . O14 O -0.0717(11) 0.7929(9) 0.2985(7) 0.052(3) Uani 1 1 d . . . C14 C 0.0363(17) 0.8064(12) 0.3387(8) 0.038(3) Uani 1 1 d . . . C21 C 0.2808(18) 0.2515(13) 0.1118(10) 0.058(4) Uani 1 1 d U . . H21A H 0.2899 0.1899 0.1378 0.070 Uiso 1 1 calc R . . C22 C 0.420(2) 0.276(2) 0.0799(14) 0.123(8) Uani 1 1 d U . . H22A H 0.4972 0.3072 0.1260 0.148 Uiso 1 1 calc R . . H22B H 0.4223 0.3420 0.0566 0.148 Uiso 1 1 calc R . . C23 C 0.456(2) 0.1714(17) 0.0151(13) 0.095(7) Uani 1 1 d U . . H23A H 0.5412 0.2029 -0.0122 0.114 Uiso 1 1 calc R . . H23B H 0.4881 0.1191 0.0424 0.114 Uiso 1 1 calc R . . C24 C 0.339(2) 0.097(2) -0.0473(13) 0.113(8) Uani 1 1 d U . . H24A H 0.3393 0.1352 -0.0904 0.135 Uiso 1 1 calc R . . H24B H 0.3609 0.0173 -0.0730 0.135 Uiso 1 1 calc R . . C25 C 0.201(2) 0.080(2) -0.0212(14) 0.140(10) Uani 1 1 d U . . H25A H 0.1862 0.0105 -0.0010 0.169 Uiso 1 1 calc R . . H25B H 0.1297 0.0568 -0.0694 0.169 Uiso 1 1 calc R . . C26 C 0.163(2) 0.1852(17) 0.0457(11) 0.087(6) Uani 1 1 d U . . H26A H 0.1390 0.2425 0.0202 0.104 Uiso 1 1 calc R . . H26B H 0.0735 0.1537 0.0699 0.104 Uiso 1 1 calc R . . C31 C 0.1038(13) 0.2883(12) 0.2583(9) 0.036(3) Uani 1 1 d U . . H31A H 0.0872 0.3508 0.3098 0.043 Uiso 1 1 calc R . . C32 C 0.1826(17) 0.2084(13) 0.2851(10) 0.051(4) Uani 1 1 d U . . H32A H 0.2832 0.2545 0.3095 0.062 Uiso 1 1 calc R . . H32B H 0.1909 0.1383 0.2372 0.062 Uiso 1 1 calc R . . C33 C 0.0939(17) 0.1640(16) 0.3494(11) 0.064(4) Uani 1 1 d U . . H33A H 0.1440 0.1113 0.3677 0.076 Uiso 1 1 calc R . . H33B H 0.0885 0.2342 0.3980 0.076 Uiso 1 1 calc R . . C34 C -0.0631(17) 0.0927(16) 0.3111(12) 0.069(5) Uani 1 1 d U . . H34A H -0.0580 0.0181 0.2660 0.083 Uiso 1 1 calc R . . H34B H -0.1218 0.0688 0.3532 0.083 Uiso 1 1 calc R . . C35 C -0.1366(15) 0.1703(14) 0.2780(10) 0.052(4) Uani 1 1 d U . . H35A H -0.2344 0.1220 0.2502 0.062 Uiso 1 1 calc R . . H35B H -0.1520 0.2398 0.3243 0.062 Uiso 1 1 calc R . . C36 C -0.0458(15) 0.2160(11) 0.2188(9) 0.041(3) Uani 1 1 d U . . H36A H -0.0961 0.2672 0.1991 0.049 Uiso 1 1 calc R . . H36B H -0.0357 0.1467 0.1708 0.049 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 Te1 0.0206(4) 0.0245(4) 0.0283(5) 0.0060(4) 0.0032(4) 0.0044(3) Te2 0.0271(5) 0.0320(5) 0.0357(6) 0.0015(4) -0.0031(4) 0.0092(4) Re1 0.0257(3) 0.0315(3) 0.0338(3) 0.0120(2) -0.0016(2) -0.0006(2) Re2 0.0209(3) 0.0307(3) 0.0426(4) 0.0111(3) 0.0027(2) 0.0064(2) Fe1 0.0254(10) 0.0288(10) 0.0411(13) 0.0114(9) 0.0061(9) 0.0043(8) Fe2 0.0227(10) 0.0317(10) 0.0351(12) 0.0068(9) 0.0086(9) 0.0080(8) P1 0.0246(19) 0.0271(18) 0.037(2) 0.0074(16) 0.0054(16) 0.0046(15) O1 0.053(7) 0.070(8) 0.061(8) 0.041(7) -0.001(6) 0.012(6) C1 0.029(8) 0.042(8) 0.027(8) 0.009(7) -0.013(6) -0.001(6) O2 0.066(8) 0.067(8) 0.055(8) 0.015(7) -0.016(6) -0.018(7) C2 0.082(13) 0.038(9) 0.025(9) 0.005(7) -0.006(8) 0.002(9) O3 0.062(8) 0.095(10) 0.055(8) 0.038(7) 0.027(7) 0.018(7) C3 0.064(11) 0.040(9) 0.037(10) 0.015(7) -0.002(8) 0.012(8) O4 0.045(7) 0.044(6) 0.076(9) 0.016(6) 0.017(6) 0.008(5) C4 0.062(11) 0.019(7) 0.044(10) 0.005(7) -0.014(8) 0.019(7) O5 0.039(7) 0.045(7) 0.203(16) 0.044(9) 0.013(9) 0.028(6) C5 0.020(8) 0.056(10) 0.075(12) 0.026(9) 0.001(8) 0.007(7) O6 0.073(9) 0.075(9) 0.067(9) 0.021(7) 0.031(7) 0.007(7) C6 0.056(11) 0.036(8) 0.042(10) -0.006(7) 0.006(8) 0.030(8) O7 0.032(6) 0.062(7) 0.059(8) 0.011(6) -0.009(6) 0.009(5) C7 0.061(11) 0.024(7) 0.039(10) -0.004(7) -0.007(8) 0.016(7) O8 0.094(11) 0.110(11) 0.056(9) 0.045(8) 0.007(8) 0.031(9) C8 0.066(11) 0.042(9) 0.033(9) 0.006(7) -0.004(8) 0.038(8) O9 0.077(9) 0.042(7) 0.062(8) 0.007(6) -0.026(6) 0.004(6) C9 0.042(9) 0.039(9) 0.056(11) 0.008(8) -0.020(8) 0.010(7) O10 0.060(8) 0.072(8) 0.085(10) 0.024(7) 0.031(7) 0.012(7) C10 0.030(8) 0.044(9) 0.063(12) 0.017(8) 0.015(8) 0.003(7) O11 0.100(10) 0.052(7) 0.068(9) 0.031(7) -0.020(8) 0.000(7) C11 0.057(11) 0.027(8) 0.059(12) 0.023(8) 0.000(9) -0.003(7) O12 0.077(9) 0.069(8) 0.080(10) 0.051(7) 0.035(7) 0.015(7) C12 0.037(9) 0.082(13) 0.041(10) 0.025(9) 0.001(8) 0.027(9) O13 0.045(7) 0.043(6) 0.079(9) -0.002(6) 0.027(6) 0.013(5) C13 0.025(8) 0.054(9) 0.039(9) 0.016(8) -0.012(6) 0.002(7) O14 0.037(6) 0.054(7) 0.072(8) 0.024(6) 0.012(6) 0.019(5) C14 0.045(9) 0.038(8) 0.029(9) 0.003(7) 0.001(7) 0.018(7) C21 0.053(9) 0.038(8) 0.058(10) -0.013(7) 0.014(7) 0.006(7) C22 0.073(10) 0.107(14) 0.123(16) -0.044(11) 0.050(10) 0.012(11) C23 0.071(10) 0.073(12) 0.101(15) -0.026(10) 0.031(9) 0.018(10) C24 0.093(13) 0.122(16) 0.078(14) -0.022(10) 0.024(10) 0.020(12) C25 0.085(11) 0.134(16) 0.099(15) -0.082(11) 0.021(11) 0.000(12) C26 0.078(10) 0.076(12) 0.067(12) -0.023(9) 0.012(8) 0.008(10) C31 0.016(6) 0.039(7) 0.065(10) 0.031(7) 0.025(6) 0.008(5) C32 0.047(8) 0.039(8) 0.091(11) 0.043(8) 0.033(7) 0.023(6) C33 0.041(7) 0.085(11) 0.098(13) 0.067(10) 0.031(8) 0.026(8) C34 0.043(8) 0.089(12) 0.106(13) 0.071(10) 0.028(9) 0.018(7) C35 0.026(7) 0.060(9) 0.082(11) 0.041(8) 0.023(7) 0.010(6) C36 0.042(7) 0.023(7) 0.057(9) 0.017(6) 0.015(6) 0.002(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 Te1 Fe1 2.537(2) . ? Te1 Fe2 2.5438(19) . ? Te1 Re1 2.7572(11) . ? Te1 Re2 2.7736(10) . ? Te2 Fe2 2.523(2) . ? Te2 Fe1 2.531(2) . ? Te2 Te2 2.8075(18) 2_676 ? Re1 C4 1.958(17) . ? Re1 C1 1.962(14) . ? Re1 C2 1.963(16) . ? Re1 C3 1.993(17) . ? Re1 P1 2.543(4) . ? Re2 C8 1.952(16) . ? Re2 C5 1.956(15) . ? Re2 C7 1.984(16) . ? Re2 C6 1.989(17) . ? Re2 P1 2.566(4) . ? Fe1 C11 1.744(17) . ? Fe1 C9 1.771(15) . ? Fe1 C10 1.785(15) . ? Fe1 Fe2 2.656(3) . ? Fe2 C13 1.759(16) . ? Fe2 C14 1.768(15) . ? Fe2 C12 1.795(17) . ? P1 C21 1.895(14) . ? P1 C31 1.906(12) . ? O1 C1 1.131(15) . ? O2 C2 1.113(17) . ? O3 C3 1.143(16) . ? O4 C4 1.142(16) . ? O5 C5 1.129(16) . ? O6 C6 1.141(17) . ? O7 C7 1.131(17) . ? O8 C8 1.152(17) . ? O9 C9 1.163(16) . ? O10 C10 1.116(16) . ? O11 C11 1.181(17) . ? O12 C12 1.136(16) . ? O13 C13 1.170(16) . ? O14 C14 1.172(16) . ? C21 C22 1.42(2) . ? C21 C26 1.47(2) . ? C22 C23 1.50(2) . ? C23 C24 1.44(3) . ? C24 C25 1.36(2) . ? C25 C26 1.52(2) . ? C31 C36 1.496(18) . ? C31 C32 1.512(17) . ? C32 C33 1.550(18) . ? C33 C34 1.54(2) . ? C34 C35 1.516(19) . ? C35 C36 1.495(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 Fe1 Te1 Fe2 63.04(6) . . ? Fe1 Te1 Re1 128.75(6) . . ? Fe2 Te1 Re1 120.71(6) . . ? Fe1 Te1 Re2 122.49(5) . . ? Fe2 Te1 Re2 126.14(6) . . ? Re1 Te1 Re2 96.72(3) . . ? Fe2 Te2 Fe1 63.40(6) . . ? Fe2 Te2 Te2 106.87(6) . 2_676 ? Fe1 Te2 Te2 106.48(6) . 2_676 ? C4 Re1 C1 90.2(5) . . ? C4 Re1 C2 92.0(6) . . ? C1 Re1 C2 89.1(6) . . ? C4 Re1 C3 173.8(6) . . ? C1 Re1 C3 89.8(6) . . ? C2 Re1 C3 94.2(6) . . ? C4 Re1 P1 89.7(4) . . ? C1 Re1 P1 174.7(4) . . ? C2 Re1 P1 96.2(5) . . ? C3 Re1 P1 89.7(4) . . ? C4 Re1 Te1 84.0(4) . . ? C1 Re1 Te1 97.7(4) . . ? C2 Re1 Te1 172.1(4) . . ? C3 Re1 Te1 89.8(5) . . ? P1 Re1 Te1 77.02(8) . . ? C8 Re2 C5 93.1(6) . . ? C8 Re2 C7 86.0(7) . . ? C5 Re2 C7 90.2(6) . . ? C8 Re2 C6 174.3(6) . . ? C5 Re2 C6 91.5(6) . . ? C7 Re2 C6 90.6(7) . . ? C8 Re2 P1 92.7(5) . . ? C5 Re2 P1 91.9(5) . . ? C7 Re2 P1 177.6(4) . . ? C6 Re2 P1 90.5(5) . . ? C8 Re2 Te1 90.3(4) . . ? C5 Re2 Te1 167.9(5) . . ? C7 Re2 Te1 101.6(4) . . ? C6 Re2 Te1 85.9(4) . . ? P1 Re2 Te1 76.35(8) . . ? C11 Fe1 C9 92.7(6) . . ? C11 Fe1 C10 100.6(7) . . ? C9 Fe1 C10 100.0(7) . . ? C11 Fe1 Te2 159.8(5) . . ? C9 Fe1 Te2 90.5(5) . . ? C10 Fe1 Te2 98.4(5) . . ? C11 Fe1 Te1 91.0(4) . . ? C9 Fe1 Te1 161.1(5) . . ? C10 Fe1 Te1 97.5(5) . . ? Te2 Fe1 Te1 79.91(6) . . ? C11 Fe1 Fe2 101.8(5) . . ? C9 Fe1 Fe2 102.5(5) . . ? C10 Fe1 Fe2 147.2(5) . . ? Te2 Fe1 Fe2 58.15(6) . . ? Te1 Fe1 Fe2 58.60(6) . . ? C13 Fe2 C14 91.7(6) . . ? C13 Fe2 C12 99.0(7) . . ? C14 Fe2 C12 100.2(7) . . ? C13 Fe2 Te2 91.5(4) . . ? C14 Fe2 Te2 156.5(5) . . ? C12 Fe2 Te2 102.2(5) . . ? C13 Fe2 Te1 161.9(5) . . ? C14 Fe2 Te1 90.1(4) . . ? C12 Fe2 Te1 98.3(5) . . ? Te2 Fe2 Te1 79.93(6) . . ? C13 Fe2 Fe1 103.6(5) . . ? C14 Fe2 Fe1 98.3(5) . . ? C12 Fe2 Fe1 150.2(5) . . ? Te2 Fe2 Fe1 58.44(6) . . ? Te1 Fe2 Fe1 58.36(6) . . ? C21 P1 C31 104.0(7) . . ? C21 P1 Re1 116.2(6) . . ? C31 P1 Re1 109.2(4) . . ? C21 P1 Re2 111.6(5) . . ? C31 P1 Re2 107.4(5) . . ? Re1 P1 Re2 107.98(12) . . ? O1 C1 Re1 176.7(12) . . ? O2 C2 Re1 176.4(16) . . ? O3 C3 Re1 178.3(15) . . ? O4 C4 Re1 177.0(12) . . ? O5 C5 Re2 176.6(16) . . ? O6 C6 Re2 172.9(15) . . ? O7 C7 Re2 174.0(12) . . ? O8 C8 Re2 176.3(13) . . ? O9 C9 Fe1 178.6(16) . . ? O10 C10 Fe1 176.6(14) . . ? O11 C11 Fe1 178.5(14) . . ? O12 C12 Fe2 178.9(15) . . ? O13 C13 Fe2 178.9(13) . . ? O14 C14 Fe2 178.3(13) . . ? C22 C21 C26 111.4(16) . . ? C22 C21 P1 119.6(12) . . ? C26 C21 P1 113.4(12) . . ? C21 C22 C23 115.6(17) . . ? C24 C23 C22 115.8(19) . . ? C25 C24 C23 115.8(19) . . ? C24 C25 C26 117.9(19) . . ? C21 C26 C25 114.0(17) . . ? C36 C31 C32 109.2(11) . . ? C36 C31 P1 117.5(10) . . ? C32 C31 P1 111.0(8) . . ? C31 C32 C33 108.7(11) . . ? C34 C33 C32 109.6(14) . . ? C35 C34 C33 109.9(13) . . ? C36 C35 C34 111.5(12) . . ? C35 C36 C31 111.0(12) . . ? 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 Fe1 Te1 Re1 C4 -116.9(4) . . . . ? Fe2 Te1 Re1 C4 -38.4(4) . . . . ? Re2 Te1 Re1 C4 101.1(4) . . . . ? Fe1 Te1 Re1 C1 -27.5(4) . . . . ? Fe2 Te1 Re1 C1 51.0(4) . . . . ? Re2 Te1 Re1 C1 -169.5(4) . . . . ? Fe1 Te1 Re1 C2 -177(4) . . . . ? Fe2 Te1 Re1 C2 -98(4) . . . . ? Re2 Te1 Re1 C2 41(4) . . . . ? Fe1 Te1 Re1 C3 62.3(4) . . . . ? Fe2 Te1 Re1 C3 140.8(4) . . . . ? Re2 Te1 Re1 C3 -79.7(4) . . . . ? Fe1 Te1 Re1 P1 152.03(10) . . . . ? Fe2 Te1 Re1 P1 -129.47(10) . . . . ? Re2 Te1 Re1 P1 10.04(8) . . . . ? Fe1 Te1 Re2 C8 112.0(5) . . . . ? Fe2 Te1 Re2 C8 33.6(5) . . . . ? Re1 Te1 Re2 C8 -102.7(5) . . . . ? Fe1 Te1 Re2 C5 -141(2) . . . . ? Fe2 Te1 Re2 C5 140(2) . . . . ? Re1 Te1 Re2 C5 4(2) . . . . ? Fe1 Te1 Re2 C7 26.0(5) . . . . ? Fe2 Te1 Re2 C7 -52.4(5) . . . . ? Re1 Te1 Re2 C7 171.3(5) . . . . ? Fe1 Te1 Re2 C6 -63.8(5) . . . . ? Fe2 Te1 Re2 C6 -142.2(5) . . . . ? Re1 Te1 Re2 C6 81.5(5) . . . . ? Fe1 Te1 Re2 P1 -155.27(10) . . . . ? Fe2 Te1 Re2 P1 126.30(10) . . . . ? Re1 Te1 Re2 P1 -9.98(8) . . . . ? Fe2 Te2 Fe1 C11 5.2(14) . . . . ? Te2 Te2 Fe1 C11 -95.7(14) 2_676 . . . ? Fe2 Te2 Fe1 C9 104.5(5) . . . . ? Te2 Te2 Fe1 C9 3.5(5) 2_676 . . . ? Fe2 Te2 Fe1 C10 -155.4(5) . . . . ? Te2 Te2 Fe1 C10 103.7(5) 2_676 . . . ? Fe2 Te2 Fe1 Te1 -59.18(6) . . . . ? Te2 Te2 Fe1 Te1 -160.14(6) 2_676 . . . ? Te2 Te2 Fe1 Fe2 -100.97(7) 2_676 . . . ? Fe2 Te1 Fe1 C11 -103.2(5) . . . . ? Re1 Te1 Fe1 C11 5.9(5) . . . . ? Re2 Te1 Fe1 C11 139.4(5) . . . . ? Fe2 Te1 Fe1 C9 -1.6(15) . . . . ? Re1 Te1 Fe1 C9 107.4(15) . . . . ? Re2 Te1 Fe1 C9 -119.0(15) . . . . ? Fe2 Te1 Fe1 C10 156.0(5) . . . . ? Re1 Te1 Fe1 C10 -95.0(5) . . . . ? Re2 Te1 Fe1 C10 38.5(5) . . . . ? Fe2 Te1 Fe1 Te2 58.72(6) . . . . ? Re1 Te1 Fe1 Te2 167.77(5) . . . . ? Re2 Te1 Fe1 Te2 -58.70(7) . . . . ? Re1 Te1 Fe1 Fe2 109.05(8) . . . . ? Re2 Te1 Fe1 Fe2 -117.42(7) . . . . ? Fe1 Te2 Fe2 C13 -105.1(5) . . . . ? Te2 Te2 Fe2 C13 -4.7(5) 2_676 . . . ? Fe1 Te2 Fe2 C14 -7.2(11) . . . . ? Te2 Te2 Fe2 C14 93.2(11) 2_676 . . . ? Fe1 Te2 Fe2 C12 155.4(5) . . . . ? Te2 Te2 Fe2 C12 -104.3(5) 2_676 . . . ? Fe1 Te2 Fe2 Te1 58.92(6) . . . . ? Te2 Te2 Fe2 Te1 159.28(6) 2_676 . . . ? Te2 Te2 Fe2 Fe1 100.36(7) 2_676 . . . ? Fe1 Te1 Fe2 C13 3.8(14) . . . . ? Re1 Te1 Fe2 C13 -117.1(14) . . . . ? Re2 Te1 Fe2 C13 115.8(14) . . . . ? Fe1 Te1 Fe2 C14 99.7(5) . . . . ? Re1 Te1 Fe2 C14 -21.3(5) . . . . ? Re2 Te1 Fe2 C14 -148.3(5) . . . . ? Fe1 Te1 Fe2 C12 -160.0(5) . . . . ? Re1 Te1 Fe2 C12 79.0(5) . . . . ? Re2 Te1 Fe2 C12 -48.0(5) . . . . ? Fe1 Te1 Fe2 Te2 -59.01(6) . . . . ? Re1 Te1 Fe2 Te2 -179.98(4) . . . . ? Re2 Te1 Fe2 Te2 53.00(7) . . . . ? Re1 Te1 Fe2 Fe1 -120.97(7) . . . . ? Re2 Te1 Fe2 Fe1 112.01(7) . . . . ? C11 Fe1 Fe2 C13 -94.8(7) . . . . ? C9 Fe1 Fe2 C13 0.7(7) . . . . ? C10 Fe1 Fe2 C13 133.0(11) . . . . ? Te2 Fe1 Fe2 C13 83.3(5) . . . . ? Te1 Fe1 Fe2 C13 -178.8(5) . . . . ? C11 Fe1 Fe2 C14 -1.0(7) . . . . ? C9 Fe1 Fe2 C14 94.5(7) . . . . ? C10 Fe1 Fe2 C14 -133.2(10) . . . . ? Te2 Fe1 Fe2 C14 177.1(4) . . . . ? Te1 Fe1 Fe2 C14 -85.0(4) . . . . ? C11 Fe1 Fe2 C12 126.8(12) . . . . ? C9 Fe1 Fe2 C12 -137.7(12) . . . . ? C10 Fe1 Fe2 C12 -5.4(15) . . . . ? Te2 Fe1 Fe2 C12 -55.1(11) . . . . ? Te1 Fe1 Fe2 C12 42.8(11) . . . . ? C11 Fe1 Fe2 Te2 -178.2(5) . . . . ? C9 Fe1 Fe2 Te2 -82.6(5) . . . . ? C10 Fe1 Fe2 Te2 49.6(10) . . . . ? Te1 Fe1 Fe2 Te2 97.90(6) . . . . ? C11 Fe1 Fe2 Te1 83.9(5) . . . . ? C9 Fe1 Fe2 Te1 179.5(5) . . . . ? C10 Fe1 Fe2 Te1 -48.3(10) . . . . ? Te2 Fe1 Fe2 Te1 -97.90(6) . . . . ? C4 Re1 P1 C21 138.5(7) . . . . ? C1 Re1 P1 C21 -133(4) . . . . ? C2 Re1 P1 C21 46.6(7) . . . . ? C3 Re1 P1 C21 -47.7(7) . . . . ? Te1 Re1 P1 C21 -137.6(6) . . . . ? C4 Re1 P1 C31 21.2(6) . . . . ? C1 Re1 P1 C31 110(4) . . . . ? C2 Re1 P1 C31 -70.7(7) . . . . ? C3 Re1 P1 C31 -164.9(7) . . . . ? Te1 Re1 P1 C31 105.2(5) . . . . ? C4 Re1 P1 Re2 -95.3(4) . . . . ? C1 Re1 P1 Re2 -7(4) . . . . ? C2 Re1 P1 Re2 172.8(5) . . . . ? C3 Re1 P1 Re2 78.5(5) . . . . ? Te1 Re1 P1 Re2 -11.35(9) . . . . ? C8 Re2 P1 C21 -130.1(7) . . . . ? C5 Re2 P1 C21 -36.9(8) . . . . ? C7 Re2 P1 C21 171(11) . . . . ? C6 Re2 P1 C21 54.6(7) . . . . ? Te1 Re2 P1 C21 140.2(6) . . . . ? C8 Re2 P1 C31 -16.7(5) . . . . ? C5 Re2 P1 C31 76.5(6) . . . . ? C7 Re2 P1 C31 -76(11) . . . . ? C6 Re2 P1 C31 168.0(6) . . . . ? Te1 Re2 P1 C31 -106.4(4) . . . . ? C8 Re2 P1 Re1 101.0(4) . . . . ? C5 Re2 P1 Re1 -165.8(5) . . . . ? C7 Re2 P1 Re1 42(11) . . . . ? C6 Re2 P1 Re1 -74.3(4) . . . . ? Te1 Re2 P1 Re1 11.31(9) . . . . ? C4 Re1 C1 O1 -100(22) . . . . ? C2 Re1 C1 O1 -8(22) . . . . ? C3 Re1 C1 O1 86(22) . . . . ? P1 Re1 C1 O1 171(18) . . . . ? Te1 Re1 C1 O1 176(100) . . . . ? C4 Re1 C2 O2 1(25) . . . . ? C1 Re1 C2 O2 -89(25) . . . . ? C3 Re1 C2 O2 -179(100) . . . . ? P1 Re1 C2 O2 91(25) . . . . ? Te1 Re1 C2 O2 60(27) . . . . ? C4 Re1 C3 O3 -8(49) . . . . ? C1 Re1 C3 O3 83(46) . . . . ? C2 Re1 C3 O3 172(46) . . . . ? P1 Re1 C3 O3 -92(46) . . . . ? Te1 Re1 C3 O3 -15(46) . . . . ? C1 Re1 C4 O4 -27(27) . . . . ? C2 Re1 C4 O4 -116(27) . . . . ? C3 Re1 C4 O4 63(29) . . . . ? P1 Re1 C4 O4 147(27) . . . . ? Te1 Re1 C4 O4 70(27) . . . . ? C8 Re2 C5 O5 156(22) . . . . ? C7 Re2 C5 O5 -118(22) . . . . ? C6 Re2 C5 O5 -27(22) . . . . ? P1 Re2 C5 O5 63(22) . . . . ? Te1 Re2 C5 O5 50(23) . . . . ? C8 Re2 C6 O6 48(14) . . . . ? C5 Re2 C6 O6 -96(10) . . . . ? C7 Re2 C6 O6 -6(10) . . . . ? P1 Re2 C6 O6 172(10) . . . . ? Te1 Re2 C6 O6 96(10) . . . . ? C8 Re2 C7 O7 88(14) . . . . ? C5 Re2 C7 O7 -5(14) . . . . ? C6 Re2 C7 O7 -97(14) . . . . ? P1 Re2 C7 O7 147(9) . . . . ? Te1 Re2 C7 O7 177(100) . . . . ? C5 Re2 C8 O8 36(24) . . . . ? C7 Re2 C8 O8 -54(24) . . . . ? C6 Re2 C8 O8 -107(23) . . . . ? P1 Re2 C8 O8 128(24) . . . . ? Te1 Re2 C8 O8 -155(24) . . . . ? C11 Fe1 C9 O9 -65(58) . . . . ? C10 Fe1 C9 O9 36(58) . . . . ? Te2 Fe1 C9 O9 135(58) . . . . ? Te1 Fe1 C9 O9 -167(57) . . . . ? Fe2 Fe1 C9 O9 -168(58) . . . . ? C11 Fe1 C10 O10 -87(27) . . . . ? C9 Fe1 C10 O10 178(100) . . . . ? Te2 Fe1 C10 O10 86(27) . . . . ? Te1 Fe1 C10 O10 5(27) . . . . ? Fe2 Fe1 C10 O10 45(28) . . . . ? C9 Fe1 C11 O11 -15(55) . . . . ? C10 Fe1 C11 O11 -116(55) . . . . ? Te2 Fe1 C11 O11 84(55) . . . . ? Te1 Fe1 C11 O11 147(55) . . . . ? Fe2 Fe1 C11 O11 88(55) . . . . ? C13 Fe2 C12 O12 99(81) . . . . ? C14 Fe2 C12 O12 6(81) . . . . ? Te2 Fe2 C12 O12 -167(81) . . . . ? Te1 Fe2 C12 O12 -86(81) . . . . ? Fe1 Fe2 C12 O12 -121(81) . . . . ? C14 Fe2 C13 O13 123(63) . . . . ? C12 Fe2 C13 O13 22(63) . . . . ? Te2 Fe2 C13 O13 -81(63) . . . . ? Te1 Fe2 C13 O13 -142(62) . . . . ? Fe1 Fe2 C13 O13 -139(63) . . . . ? C13 Fe2 C14 O14 -96(47) . . . . ? C12 Fe2 C14 O14 3(47) . . . . ? Te2 Fe2 C14 O14 166(46) . . . . ? Te1 Fe2 C14 O14 102(47) . . . . ? Fe1 Fe2 C14 O14 160(47) . . . . ? C31 P1 C21 C22 -149.2(18) . . . . ? Re1 P1 C21 C22 90.7(19) . . . . ? Re2 P1 C21 C22 -34(2) . . . . ? C31 P1 C21 C26 76.1(15) . . . . ? Re1 P1 C21 C26 -43.9(15) . . . . ? Re2 P1 C21 C26 -168.3(12) . . . . ? C26 C21 C22 C23 -48(3) . . . . ? P1 C21 C22 C23 176.6(17) . . . . ? C21 C22 C23 C24 44(3) . . . . ? C22 C23 C24 C25 -37(4) . . . . ? C23 C24 C25 C26 37(4) . . . . ? C22 C21 C26 C25 46(3) . . . . ? P1 C21 C26 C25 -175.8(16) . . . . ? C24 C25 C26 C21 -42(4) . . . . ? C21 P1 C31 C36 -71.2(12) . . . . ? Re1 P1 C31 C36 53.5(11) . . . . ? Re2 P1 C31 C36 170.4(9) . . . . ? C21 P1 C31 C32 55.5(13) . . . . ? Re1 P1 C31 C32 -179.8(10) . . . . ? Re2 P1 C31 C32 -62.9(11) . . . . ? C36 C31 C32 C33 -61.7(16) . . . . ? P1 C31 C32 C33 167.2(11) . . . . ? C31 C32 C33 C34 59.3(17) . . . . ? C32 C33 C34 C35 -55.7(18) . . . . ? C33 C34 C35 C36 55.1(19) . . . . ? C34 C35 C36 C31 -58.3(17) . . . . ? C32 C31 C36 C35 61.5(15) . . . . ? P1 C31 C36 C35 -171.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max '1.381 near Re position' _refine_diff_density_min -0.872 _refine_diff_density_rms 0.278 #===END