Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'J. Woollins' 'Petr Kilian' 'Sahrah Parveen' 'A. Slawin' _publ_contact_author_name 'J Woollins' _publ_contact_author_address ; Department of Chemistry University of St Andrews St Andrews FIFE SCOTLAND KY16 9ST UNITED KINGDOM ; _publ_contact_author_email JDW3@ST-ANDREWS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Characterisation of P-Se Heterocycles ; # Attachment '5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 291575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Fe2 P2 Se4' _chemical_formula_sum 'C20 H18 Fe2 P2 Se4' _chemical_formula_weight 747.82 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.623(2) _cell_length_b 12.720(4) _cell_length_c 13.847(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.470(12) _cell_angle_gamma 90.00 _cell_volume 1162.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3381 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.63 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 7.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7626 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6129 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1952 _reflns_number_gt 1376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.1752P] 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 1952 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Se1 Se 0.87850(9) 0.10255(5) 0.39171(5) 0.0374(2) Uani 1 1 d . . . Se2 Se 0.35856(9) 0.10333(5) 0.46469(5) 0.0303(2) Uani 1 1 d . . . Fe1 Fe 0.73297(15) 0.29084(7) 0.63437(7) 0.0379(3) Uani 1 1 d . . . P1 P 0.6903(2) 0.07092(12) 0.50306(12) 0.0242(4) Uani 1 1 d . . . C1 C 0.7558(9) 0.1339(4) 0.6138(4) 0.0267(15) Uani 1 1 d . . . C2 C 0.6202(10) 0.1564(5) 0.6885(5) 0.0375(17) Uani 1 1 d . . . H2A H 0.4811 0.1378 0.6871 0.045 Uiso 1 1 calc R . . C3 C 0.7312(12) 0.2107(5) 0.7630(5) 0.0432(18) Uani 1 1 d . . . H3A H 0.6794 0.2347 0.8212 0.052 Uiso 1 1 calc R . . C4 C 0.9321(12) 0.2241(5) 0.7380(5) 0.049(2) Uani 1 1 d . . . H4A H 1.0377 0.2586 0.7761 0.059 Uiso 1 1 calc R . . C5 C 0.9488(10) 0.1782(5) 0.6481(5) 0.0403(18) Uani 1 1 d . . . H5A H 1.0684 0.1763 0.6144 0.048 Uiso 1 1 calc R . . C6 C 0.8107(19) 0.3962(7) 0.5335(8) 0.086(3) Uani 1 1 d . . . H6A H 0.9188 0.3875 0.4930 0.103 Uiso 1 1 calc R . . C7 C 0.618(2) 0.3636(7) 0.5121(8) 0.088(4) Uani 1 1 d . . . H7A H 0.5678 0.3286 0.4546 0.105 Uiso 1 1 calc R . . C8 C 0.5053(15) 0.3916(7) 0.5919(11) 0.092(4) Uani 1 1 d . . . H8A H 0.3655 0.3792 0.5982 0.110 Uiso 1 1 calc R . . C9 C 0.6445(19) 0.4417(7) 0.6595(7) 0.075(3) Uani 1 1 d . . . H9A H 0.6151 0.4693 0.7206 0.090 Uiso 1 1 calc R . . C10 C 0.8265(17) 0.4433(7) 0.6220(8) 0.083(3) Uani 1 1 d . . . H10A H 0.9468 0.4727 0.6526 0.099 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 Se1 0.0297(4) 0.0457(5) 0.0376(4) 0.0075(4) 0.0088(3) -0.0002(3) Se2 0.0247(4) 0.0229(4) 0.0428(4) 0.0052(3) -0.0009(3) 0.0001(3) Fe1 0.0543(7) 0.0211(5) 0.0381(6) -0.0036(5) 0.0022(5) -0.0016(5) P1 0.0228(9) 0.0204(8) 0.0291(10) -0.0010(7) 0.0006(7) -0.0023(7) C1 0.035(4) 0.017(3) 0.027(4) 0.000(3) -0.005(3) 0.000(3) C2 0.043(5) 0.023(4) 0.046(5) 0.003(3) 0.004(3) 0.006(3) C3 0.067(6) 0.031(4) 0.032(4) 0.001(4) 0.005(4) 0.005(4) C4 0.056(5) 0.053(5) 0.035(5) -0.018(4) -0.012(4) -0.005(4) C5 0.030(4) 0.035(4) 0.054(5) -0.009(4) -0.010(3) 0.004(3) C6 0.154(11) 0.040(5) 0.070(7) 0.020(5) 0.051(7) -0.011(6) C7 0.164(12) 0.025(5) 0.068(8) 0.023(5) -0.032(8) -0.003(6) C8 0.062(7) 0.040(6) 0.172(13) 0.058(8) 0.008(8) 0.022(5) C9 0.128(10) 0.033(5) 0.067(7) -0.006(5) 0.024(7) 0.007(6) C10 0.116(9) 0.034(5) 0.100(9) -0.004(5) 0.021(7) -0.032(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 Se1 P1 2.0957(18) . ? Se2 P1 2.2577(18) . ? Se2 P1 2.2889(18) 3_656 ? Fe1 C5 2.022(6) . ? Fe1 C1 2.023(6) . ? Fe1 C7 2.025(9) . ? Fe1 C6 2.030(8) . ? Fe1 C8 2.031(8) . ? Fe1 C2 2.032(7) . ? Fe1 C9 2.044(8) . ? Fe1 C10 2.046(8) . ? Fe1 C3 2.053(7) . ? Fe1 C4 2.055(7) . ? P1 C1 1.754(6) . ? P1 Se2 2.2889(18) 3_656 ? C1 C5 1.443(8) . ? C1 C2 1.450(9) . ? C2 C3 1.402(9) . ? C2 H2A 0.9500 . ? C3 C4 1.411(10) . ? C3 H3A 0.9500 . ? C4 C5 1.387(9) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.350(14) . ? C6 C10 1.361(13) . ? C6 H6A 0.9500 . ? C7 C8 1.428(13) . ? C7 H7A 0.9500 . ? C8 C9 1.413(13) . ? C8 H8A 0.9500 . ? C9 C10 1.349(13) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? 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 P1 Se2 P1 85.82(6) . 3_656 ? C5 Fe1 C1 41.8(2) . . ? C5 Fe1 C7 128.2(4) . . ? C1 Fe1 C7 111.1(3) . . ? C5 Fe1 C6 108.5(4) . . ? C1 Fe1 C6 121.9(3) . . ? C7 Fe1 C6 38.9(4) . . ? C5 Fe1 C8 167.9(5) . . ? C1 Fe1 C8 130.1(4) . . ? C7 Fe1 C8 41.2(4) . . ? C6 Fe1 C8 66.8(4) . . ? C5 Fe1 C2 69.3(3) . . ? C1 Fe1 C2 41.9(2) . . ? C7 Fe1 C2 124.6(4) . . ? C6 Fe1 C2 158.3(4) . . ? C8 Fe1 C2 110.6(3) . . ? C5 Fe1 C9 149.2(4) . . ? C1 Fe1 C9 167.3(4) . . ? C7 Fe1 C9 67.6(4) . . ? C6 Fe1 C9 65.7(4) . . ? C8 Fe1 C9 40.6(4) . . ? C2 Fe1 C9 127.5(4) . . ? C5 Fe1 C10 117.6(4) . . ? C1 Fe1 C10 153.7(4) . . ? C7 Fe1 C10 66.0(4) . . ? C6 Fe1 C10 39.0(4) . . ? C8 Fe1 C10 66.5(4) . . ? C2 Fe1 C10 161.8(4) . . ? C9 Fe1 C10 38.5(4) . . ? C5 Fe1 C3 67.6(3) . . ? C1 Fe1 C3 68.8(3) . . ? C7 Fe1 C3 157.7(5) . . ? C6 Fe1 C3 160.6(4) . . ? C8 Fe1 C3 120.7(4) . . ? C2 Fe1 C3 40.1(3) . . ? C9 Fe1 C3 107.3(3) . . ? C10 Fe1 C3 124.4(4) . . ? C5 Fe1 C4 39.8(3) . . ? C1 Fe1 C4 68.9(3) . . ? C7 Fe1 C4 162.0(5) . . ? C6 Fe1 C4 124.7(4) . . ? C8 Fe1 C4 152.2(5) . . ? C2 Fe1 C4 68.2(3) . . ? C9 Fe1 C4 116.5(4) . . ? C10 Fe1 C4 105.5(4) . . ? C3 Fe1 C4 40.2(3) . . ? C1 P1 Se1 115.8(2) . . ? C1 P1 Se2 107.0(2) . . ? Se1 P1 Se2 114.55(8) . . ? C1 P1 Se2 107.5(2) . 3_656 ? Se1 P1 Se2 115.51(7) . 3_656 ? Se2 P1 Se2 94.18(6) . 3_656 ? C5 C1 C2 105.7(5) . . ? C5 C1 P1 128.2(5) . . ? C2 C1 P1 126.1(5) . . ? C5 C1 Fe1 69.1(3) . . ? C2 C1 Fe1 69.4(3) . . ? P1 C1 Fe1 123.9(3) . . ? C3 C2 C1 107.7(6) . . ? C3 C2 Fe1 70.7(4) . . ? C1 C2 Fe1 68.7(3) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? Fe1 C2 H2A 125.9 . . ? C2 C3 C4 109.2(6) . . ? C2 C3 Fe1 69.1(4) . . ? C4 C3 Fe1 70.0(4) . . ? C2 C3 H3A 125.4 . . ? C4 C3 H3A 125.4 . . ? Fe1 C3 H3A 127.1 . . ? C5 C4 C3 108.2(6) . . ? C5 C4 Fe1 68.9(4) . . ? C3 C4 Fe1 69.8(4) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Fe1 C4 H4A 127.0 . . ? C4 C5 C1 109.2(6) . . ? C4 C5 Fe1 71.4(4) . . ? C1 C5 Fe1 69.1(3) . . ? C4 C5 H5A 125.4 . . ? C1 C5 H5A 125.4 . . ? Fe1 C5 H5A 125.6 . . ? C7 C6 C10 109.8(10) . . ? C7 C6 Fe1 70.3(5) . . ? C10 C6 Fe1 71.2(5) . . ? C7 C6 H6A 125.1 . . ? C10 C6 H6A 125.1 . . ? Fe1 C6 H6A 125.0 . . ? C6 C7 C8 107.2(10) . . ? C6 C7 Fe1 70.8(6) . . ? C8 C7 Fe1 69.6(5) . . ? C6 C7 H7A 126.4 . . ? C8 C7 H7A 126.4 . . ? Fe1 C7 H7A 124.8 . . ? C9 C8 C7 105.7(9) . . ? C9 C8 Fe1 70.2(5) . . ? C7 C8 Fe1 69.2(5) . . ? C9 C8 H8A 127.2 . . ? C7 C8 H8A 127.2 . . ? Fe1 C8 H8A 125.1 . . ? C10 C9 C8 107.9(9) . . ? C10 C9 Fe1 70.9(5) . . ? C8 C9 Fe1 69.2(5) . . ? C10 C9 H9A 126.0 . . ? C8 C9 H9A 126.0 . . ? Fe1 C9 H9A 125.5 . . ? C9 C10 C6 109.4(10) . . ? C9 C10 Fe1 70.6(5) . . ? C6 C10 Fe1 69.9(5) . . ? C9 C10 H10A 125.3 . . ? C6 C10 H10A 125.3 . . ? Fe1 C10 H10A 125.8 . . ? 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 P1 Se2 P1 C1 -109.7(2) 3_656 . . . ? P1 Se2 P1 Se1 120.54(9) 3_656 . . . ? P1 Se2 P1 Se2 0.0 3_656 . . 3_656 ? Se1 P1 C1 C5 -20.3(6) . . . . ? Se2 P1 C1 C5 -149.3(5) . . . . ? Se2 P1 C1 C5 110.5(5) 3_656 . . . ? Se1 P1 C1 C2 156.5(4) . . . . ? Se2 P1 C1 C2 27.5(5) . . . . ? Se2 P1 C1 C2 -72.6(5) 3_656 . . . ? Se1 P1 C1 Fe1 68.6(4) . . . . ? Se2 P1 C1 Fe1 -60.4(4) . . . . ? Se2 P1 C1 Fe1 -160.6(3) 3_656 . . . ? C7 Fe1 C1 C5 124.2(6) . . . . ? C6 Fe1 C1 C5 82.2(6) . . . . ? C8 Fe1 C1 C5 167.5(6) . . . . ? C2 Fe1 C1 C5 -117.0(5) . . . . ? C9 Fe1 C1 C5 -153.8(15) . . . . ? C10 Fe1 C1 C5 45.9(9) . . . . ? C3 Fe1 C1 C5 -79.7(4) . . . . ? C4 Fe1 C1 C5 -36.4(4) . . . . ? C5 Fe1 C1 C2 117.0(5) . . . . ? C7 Fe1 C1 C2 -118.8(6) . . . . ? C6 Fe1 C1 C2 -160.9(6) . . . . ? C8 Fe1 C1 C2 -75.6(7) . . . . ? C9 Fe1 C1 C2 -36.9(16) . . . . ? C10 Fe1 C1 C2 162.9(8) . . . . ? C3 Fe1 C1 C2 37.3(4) . . . . ? C4 Fe1 C1 C2 80.5(4) . . . . ? C5 Fe1 C1 P1 -122.7(6) . . . . ? C7 Fe1 C1 P1 1.5(7) . . . . ? C6 Fe1 C1 P1 -40.5(7) . . . . ? C8 Fe1 C1 P1 44.7(7) . . . . ? C2 Fe1 C1 P1 120.3(6) . . . . ? C9 Fe1 C1 P1 83.5(16) . . . . ? C10 Fe1 C1 P1 -76.8(9) . . . . ? C3 Fe1 C1 P1 157.6(5) . . . . ? C4 Fe1 C1 P1 -159.1(5) . . . . ? C5 C1 C2 C3 -0.4(7) . . . . ? P1 C1 C2 C3 -177.9(4) . . . . ? Fe1 C1 C2 C3 -60.3(4) . . . . ? C5 C1 C2 Fe1 59.8(4) . . . . ? P1 C1 C2 Fe1 -117.6(5) . . . . ? C5 Fe1 C2 C3 79.4(4) . . . . ? C1 Fe1 C2 C3 118.8(6) . . . . ? C7 Fe1 C2 C3 -157.8(6) . . . . ? C6 Fe1 C2 C3 167.5(10) . . . . ? C8 Fe1 C2 C3 -113.6(6) . . . . ? C9 Fe1 C2 C3 -70.8(6) . . . . ? C10 Fe1 C2 C3 -36.5(13) . . . . ? C4 Fe1 C2 C3 36.6(4) . . . . ? C5 Fe1 C2 C1 -39.4(4) . . . . ? C7 Fe1 C2 C1 83.5(6) . . . . ? C6 Fe1 C2 C1 48.7(11) . . . . ? C8 Fe1 C2 C1 127.6(6) . . . . ? C9 Fe1 C2 C1 170.4(5) . . . . ? C10 Fe1 C2 C1 -155.3(11) . . . . ? C3 Fe1 C2 C1 -118.8(6) . . . . ? C4 Fe1 C2 C1 -82.2(4) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? Fe1 C2 C3 C4 -58.6(5) . . . . ? C1 C2 C3 Fe1 59.0(4) . . . . ? C5 Fe1 C3 C2 -84.1(4) . . . . ? C1 Fe1 C3 C2 -38.9(4) . . . . ? C7 Fe1 C3 C2 55.3(10) . . . . ? C6 Fe1 C3 C2 -166.0(10) . . . . ? C8 Fe1 C3 C2 86.0(6) . . . . ? C9 Fe1 C3 C2 128.3(5) . . . . ? C10 Fe1 C3 C2 167.0(5) . . . . ? C4 Fe1 C3 C2 -120.9(6) . . . . ? C5 Fe1 C3 C4 36.8(4) . . . . ? C1 Fe1 C3 C4 82.0(4) . . . . ? C7 Fe1 C3 C4 176.2(8) . . . . ? C6 Fe1 C3 C4 -45.1(12) . . . . ? C8 Fe1 C3 C4 -153.1(6) . . . . ? C2 Fe1 C3 C4 120.9(6) . . . . ? C9 Fe1 C3 C4 -110.8(5) . . . . ? C10 Fe1 C3 C4 -72.1(6) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? Fe1 C3 C4 C5 -58.3(5) . . . . ? C2 C3 C4 Fe1 58.1(5) . . . . ? C1 Fe1 C4 C5 38.2(4) . . . . ? C7 Fe1 C4 C5 -55.4(12) . . . . ? C6 Fe1 C4 C5 -76.7(6) . . . . ? C8 Fe1 C4 C5 176.6(7) . . . . ? C2 Fe1 C4 C5 83.4(5) . . . . ? C9 Fe1 C4 C5 -154.4(5) . . . . ? C10 Fe1 C4 C5 -114.6(5) . . . . ? C3 Fe1 C4 C5 120.0(6) . . . . ? C5 Fe1 C4 C3 -120.0(6) . . . . ? C1 Fe1 C4 C3 -81.7(4) . . . . ? C7 Fe1 C4 C3 -175.3(10) . . . . ? C6 Fe1 C4 C3 163.4(5) . . . . ? C8 Fe1 C4 C3 56.6(9) . . . . ? C2 Fe1 C4 C3 -36.5(4) . . . . ? C9 Fe1 C4 C3 85.7(5) . . . . ? C10 Fe1 C4 C3 125.4(5) . . . . ? C3 C4 C5 C1 -0.1(8) . . . . ? Fe1 C4 C5 C1 -59.0(4) . . . . ? C3 C4 C5 Fe1 58.9(5) . . . . ? C2 C1 C5 C4 0.3(7) . . . . ? P1 C1 C5 C4 177.7(5) . . . . ? Fe1 C1 C5 C4 60.4(5) . . . . ? C2 C1 C5 Fe1 -60.0(4) . . . . ? P1 C1 C5 Fe1 117.3(5) . . . . ? C1 Fe1 C5 C4 -120.0(6) . . . . ? C7 Fe1 C5 C4 161.1(6) . . . . ? C6 Fe1 C5 C4 122.5(6) . . . . ? C8 Fe1 C5 C4 -172.4(15) . . . . ? C2 Fe1 C5 C4 -80.5(5) . . . . ? C9 Fe1 C5 C4 49.1(8) . . . . ? C10 Fe1 C5 C4 81.1(6) . . . . ? C3 Fe1 C5 C4 -37.2(4) . . . . ? C7 Fe1 C5 C1 -78.9(6) . . . . ? C6 Fe1 C5 C1 -117.5(5) . . . . ? C8 Fe1 C5 C1 -52.4(17) . . . . ? C2 Fe1 C5 C1 39.5(4) . . . . ? C9 Fe1 C5 C1 169.1(6) . . . . ? C10 Fe1 C5 C1 -158.9(5) . . . . ? C3 Fe1 C5 C1 82.8(4) . . . . ? C4 Fe1 C5 C1 120.0(6) . . . . ? C5 Fe1 C6 C7 128.7(7) . . . . ? C1 Fe1 C6 C7 84.5(7) . . . . ? C8 Fe1 C6 C7 -39.4(6) . . . . ? C2 Fe1 C6 C7 48.3(13) . . . . ? C9 Fe1 C6 C7 -83.9(7) . . . . ? C10 Fe1 C6 C7 -120.1(10) . . . . ? C3 Fe1 C6 C7 -156.5(10) . . . . ? C4 Fe1 C6 C7 169.7(6) . . . . ? C5 Fe1 C6 C10 -111.3(7) . . . . ? C1 Fe1 C6 C10 -155.4(6) . . . . ? C7 Fe1 C6 C10 120.1(10) . . . . ? C8 Fe1 C6 C10 80.7(7) . . . . ? C2 Fe1 C6 C10 168.4(8) . . . . ? C9 Fe1 C6 C10 36.2(7) . . . . ? C3 Fe1 C6 C10 -36.5(14) . . . . ? C4 Fe1 C6 C10 -70.3(8) . . . . ? C10 C6 C7 C8 -0.1(11) . . . . ? Fe1 C6 C7 C8 60.4(6) . . . . ? C10 C6 C7 Fe1 -60.5(7) . . . . ? C5 Fe1 C7 C6 -70.5(7) . . . . ? C1 Fe1 C7 C6 -115.0(6) . . . . ? C8 Fe1 C7 C6 117.7(9) . . . . ? C2 Fe1 C7 C6 -160.4(6) . . . . ? C9 Fe1 C7 C6 78.6(6) . . . . ? C10 Fe1 C7 C6 36.6(6) . . . . ? C3 Fe1 C7 C6 159.5(8) . . . . ? C4 Fe1 C7 C6 -28.4(15) . . . . ? C5 Fe1 C7 C8 171.8(6) . . . . ? C1 Fe1 C7 C8 127.3(6) . . . . ? C6 Fe1 C7 C8 -117.7(9) . . . . ? C2 Fe1 C7 C8 82.0(7) . . . . ? C9 Fe1 C7 C8 -39.1(6) . . . . ? C10 Fe1 C7 C8 -81.1(7) . . . . ? C3 Fe1 C7 C8 41.9(12) . . . . ? C4 Fe1 C7 C8 -146.1(11) . . . . ? C6 C7 C8 C9 0.0(10) . . . . ? Fe1 C7 C8 C9 61.1(6) . . . . ? C6 C7 C8 Fe1 -61.1(6) . . . . ? C5 Fe1 C8 C9 -148.6(15) . . . . ? C1 Fe1 C8 C9 167.8(5) . . . . ? C7 Fe1 C8 C9 -116.4(8) . . . . ? C6 Fe1 C8 C9 -79.2(6) . . . . ? C2 Fe1 C8 C9 124.1(6) . . . . ? C10 Fe1 C8 C9 -36.6(6) . . . . ? C3 Fe1 C8 C9 80.7(7) . . . . ? C4 Fe1 C8 C9 41.9(11) . . . . ? C5 Fe1 C8 C7 -32.1(19) . . . . ? C1 Fe1 C8 C7 -75.8(7) . . . . ? C6 Fe1 C8 C7 37.2(6) . . . . ? C2 Fe1 C8 C7 -119.5(6) . . . . ? C9 Fe1 C8 C7 116.4(8) . . . . ? C10 Fe1 C8 C7 79.8(7) . . . . ? C3 Fe1 C8 C7 -162.9(6) . . . . ? C4 Fe1 C8 C7 158.3(7) . . . . ? C7 C8 C9 C10 0.2(10) . . . . ? Fe1 C8 C9 C10 60.6(7) . . . . ? C7 C8 C9 Fe1 -60.4(5) . . . . ? C5 Fe1 C9 C10 49.0(10) . . . . ? C1 Fe1 C9 C10 -166.1(12) . . . . ? C7 Fe1 C9 C10 -79.1(7) . . . . ? C6 Fe1 C9 C10 -36.6(7) . . . . ? C8 Fe1 C9 C10 -118.7(9) . . . . ? C2 Fe1 C9 C10 163.6(6) . . . . ? C3 Fe1 C9 C10 124.0(7) . . . . ? C4 Fe1 C9 C10 81.6(7) . . . . ? C5 Fe1 C9 C8 167.7(7) . . . . ? C1 Fe1 C9 C8 -47.3(17) . . . . ? C7 Fe1 C9 C8 39.7(6) . . . . ? C6 Fe1 C9 C8 82.1(7) . . . . ? C2 Fe1 C9 C8 -77.7(7) . . . . ? C10 Fe1 C9 C8 118.7(9) . . . . ? C3 Fe1 C9 C8 -117.3(7) . . . . ? C4 Fe1 C9 C8 -159.6(6) . . . . ? C8 C9 C10 C6 -0.2(11) . . . . ? Fe1 C9 C10 C6 59.3(7) . . . . ? C8 C9 C10 Fe1 -59.5(6) . . . . ? C7 C6 C10 C9 0.2(11) . . . . ? Fe1 C6 C10 C9 -59.8(7) . . . . ? C7 C6 C10 Fe1 60.0(7) . . . . ? C5 Fe1 C10 C9 -154.2(6) . . . . ? C1 Fe1 C10 C9 173.1(6) . . . . ? C7 Fe1 C10 C9 83.7(7) . . . . ? C6 Fe1 C10 C9 120.2(10) . . . . ? C8 Fe1 C10 C9 38.5(7) . . . . ? C2 Fe1 C10 C9 -45.9(15) . . . . ? C3 Fe1 C10 C9 -73.6(8) . . . . ? C4 Fe1 C10 C9 -113.2(7) . . . . ? C5 Fe1 C10 C6 85.6(8) . . . . ? C1 Fe1 C10 C6 52.9(11) . . . . ? C7 Fe1 C10 C6 -36.5(7) . . . . ? C8 Fe1 C10 C6 -81.7(8) . . . . ? C2 Fe1 C10 C6 -166.2(10) . . . . ? C9 Fe1 C10 C6 -120.2(10) . . . . ? C3 Fe1 C10 C6 166.2(6) . . . . ? C4 Fe1 C10 C6 126.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.523 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.129 # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 291576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Fe2 P2 Se6.C7 H8' _chemical_formula_sum 'C27 H26 Fe2 P2 Se6' _chemical_formula_weight 997.88 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3608(9) _cell_length_b 11.4041(10) _cell_length_c 14.3898(13) _cell_angle_alpha 98.515(4) _cell_angle_beta 90.548(5) _cell_angle_gamma 94.704(4) _cell_volume 1513.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 6242 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 28.10 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 8.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4820 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11027 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4898 _reflns_number_gt 4507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+5.9892P] 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 4898 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Se1 Se 0.18466(6) 0.71640(5) 0.17789(4) 0.02919(14) Uani 1 1 d . . . P1 P 0.00501(14) 0.80809(10) 0.21827(8) 0.0176(3) Uani 1 1 d . . . Se2 Se 0.05007(5) 0.88842(4) 0.36948(3) 0.01831(12) Uani 1 1 d . . . Se3 Se -0.14468(5) 1.00419(4) 0.38983(3) 0.01974(12) Uani 1 1 d . . . C1 C -0.1610(6) 0.7194(4) 0.2094(3) 0.0219(11) Uani 1 1 d . . . C2 C -0.1766(6) 0.5901(4) 0.1954(3) 0.0236(11) Uani 1 1 d . . . H2A H -0.1008 0.5391 0.1914 0.028 Uiso 1 1 calc R . . C3 C -0.3254(6) 0.5538(5) 0.1888(3) 0.0282(12) Uani 1 1 d . . . H3A H -0.3666 0.4739 0.1793 0.034 Uiso 1 1 calc R . . C4 C -0.4026(6) 0.6572(5) 0.1987(3) 0.0312(13) Uani 1 1 d . . . H4A H -0.5041 0.6575 0.1976 0.037 Uiso 1 1 calc R . . C5 C -0.3039(6) 0.7597(5) 0.2107(3) 0.0248(11) Uani 1 1 d . . . H5A H -0.3272 0.8400 0.2182 0.030 Uiso 1 1 calc R . . Fe1 Fe -0.26640(8) 0.65611(6) 0.08561(5) 0.01997(16) Uani 1 1 d . . . C6 C -0.2734(7) 0.7584(5) -0.0216(3) 0.0296(12) Uani 1 1 d . . . H6A H -0.2830 0.8415 -0.0145 0.036 Uiso 1 1 calc R . . C7 C -0.1418(6) 0.7028(5) -0.0236(3) 0.0281(12) Uani 1 1 d . . . H7A H -0.0481 0.7425 -0.0176 0.034 Uiso 1 1 calc R . . C8 C -0.1760(6) 0.5777(5) -0.0361(3) 0.0290(12) Uani 1 1 d . . . H8A H -0.1090 0.5190 -0.0401 0.035 Uiso 1 1 calc R . . C9 C -0.3287(6) 0.5551(5) -0.0418(3) 0.0275(12) Uani 1 1 d . . . H9A H -0.3807 0.4790 -0.0505 0.033 Uiso 1 1 calc R . . C10 C -0.3883(7) 0.6660(5) -0.0323(4) 0.0298(12) Uani 1 1 d . . . H10A H -0.4876 0.6775 -0.0328 0.036 Uiso 1 1 calc R . . Se11 Se -0.21235(7) 1.27407(5) 0.30748(5) 0.03943(16) Uani 1 1 d . . . P11 P -0.04582(15) 1.17234(11) 0.33902(9) 0.0204(3) Uani 1 1 d . . . Se12 Se 0.10478(6) 1.11107(4) 0.22115(3) 0.02423(13) Uani 1 1 d . . . Se13 Se -0.05164(6) 0.96083(4) 0.14065(3) 0.02348(13) Uani 1 1 d . . . C11 C 0.0769(6) 1.2461(4) 0.4283(3) 0.0200(10) Uani 1 1 d . . . C12 C 0.2133(6) 1.2090(4) 0.4542(3) 0.0202(10) Uani 1 1 d . . . H12A H 0.2569 1.1408 0.4256 0.024 Uiso 1 1 calc R . . C13 C 0.2703(6) 1.2942(4) 0.5308(3) 0.0222(10) Uani 1 1 d . . . H13A H 0.3595 1.2923 0.5625 0.027 Uiso 1 1 calc R . . C14 C 0.1713(6) 1.3830(4) 0.5524(3) 0.0226(11) Uani 1 1 d . . . H14A H 0.1830 1.4498 0.6007 0.027 Uiso 1 1 calc R . . C15 C 0.0524(6) 1.3536(4) 0.4888(3) 0.0224(11) Uani 1 1 d . . . H15A H -0.0291 1.3977 0.4868 0.027 Uiso 1 1 calc R . . Fe11 Fe 0.23457(8) 1.37490(6) 0.41364(5) 0.02057(17) Uani 1 1 d . . . C16 C 0.3658(7) 1.3733(5) 0.2991(4) 0.0337(13) Uani 1 1 d . . . H16A H 0.4065 1.3058 0.2665 0.040 Uiso 1 1 calc R . . C17 C 0.4287(7) 1.4514(6) 0.3776(4) 0.0382(15) Uani 1 1 d . . . H17A H 0.5188 1.4455 0.4068 0.046 Uiso 1 1 calc R . . C18 C 0.3329(7) 1.5400(5) 0.4047(4) 0.0356(14) Uani 1 1 d . . . H18A H 0.3481 1.6039 0.4551 0.043 Uiso 1 1 calc R . . C19 C 0.2098(7) 1.5168(5) 0.3434(4) 0.0338(14) Uani 1 1 d . . . H19A H 0.1285 1.5618 0.3459 0.041 Uiso 1 1 calc R . . C20 C 0.2312(7) 1.4138(5) 0.2778(4) 0.0318(13) Uani 1 1 d . . . H20A H 0.1667 1.3783 0.2283 0.038 Uiso 1 1 calc R . . C21 C -0.4281(8) 1.0426(6) -0.0746(5) 0.0452(16) Uani 1 1 d . . . C22 C -0.5456(8) 0.9583(6) -0.0930(5) 0.0449(16) Uani 1 1 d . . . C23 C -0.6176(7) 0.9157(5) -0.0187(5) 0.0431(16) Uani 1 1 d . . . C24 C -0.7326(12) 0.8248(10) -0.0416(7) 0.030(2) Uani 0.50 1 d P . . C31 C 0.4862(13) 1.0005(14) 0.4412(12) 0.051(4) Uani 0.50 1 d P . . C32 C 0.5472(8) 1.1001(8) 0.4968(8) 0.061(2) Uani 1 1 d . . . C33 C 0.5732(13) 1.1241(13) 0.5874(10) 0.044(3) Uani 0.50 1 d P . . C34 C 0.5414(10) 1.0264(12) 0.6503(9) 0.092(4) Uani 1 1 d . . . C35 C 0.478(2) 0.922(3) 0.592(3) 0.112(13) Uani 0.50 1 d P . . 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 Se1 0.0246(3) 0.0264(3) 0.0365(3) 0.0010(2) 0.0041(2) 0.0075(2) P1 0.0191(7) 0.0169(6) 0.0164(6) 0.0013(4) -0.0026(5) 0.0013(5) Se2 0.0208(3) 0.0171(2) 0.0165(2) 0.00099(17) -0.00391(19) 0.00167(19) Se3 0.0192(3) 0.0171(2) 0.0214(2) -0.00132(17) -0.0008(2) 0.00008(18) C1 0.025(3) 0.024(2) 0.016(2) 0.0035(19) -0.001(2) 0.001(2) C2 0.032(3) 0.021(2) 0.017(2) 0.0031(19) -0.003(2) -0.001(2) C3 0.029(3) 0.032(3) 0.020(2) 0.004(2) -0.003(2) -0.016(2) C4 0.019(3) 0.054(4) 0.017(2) -0.003(2) 0.000(2) -0.002(3) C5 0.025(3) 0.028(3) 0.018(2) -0.007(2) 0.001(2) 0.000(2) Fe1 0.0226(4) 0.0215(3) 0.0144(3) -0.0003(3) -0.0040(3) -0.0007(3) C6 0.044(4) 0.027(3) 0.017(2) 0.003(2) -0.008(2) 0.000(2) C7 0.035(3) 0.039(3) 0.008(2) 0.003(2) -0.004(2) -0.009(2) C8 0.036(3) 0.035(3) 0.015(2) -0.003(2) 0.000(2) 0.005(2) C9 0.034(3) 0.031(3) 0.014(2) -0.002(2) -0.008(2) -0.005(2) C10 0.036(4) 0.033(3) 0.020(2) 0.004(2) -0.011(2) 0.005(2) Se11 0.0364(4) 0.0248(3) 0.0572(4) 0.0037(3) -0.0198(3) 0.0096(2) P11 0.0226(7) 0.0159(6) 0.0222(6) 0.0012(5) -0.0051(5) 0.0017(5) Se12 0.0336(3) 0.0200(2) 0.0179(2) 0.00241(18) 0.0004(2) -0.0042(2) Se13 0.0348(3) 0.0182(2) 0.0169(2) 0.00184(18) -0.0077(2) 0.0017(2) C11 0.025(3) 0.018(2) 0.018(2) 0.0055(18) 0.000(2) 0.000(2) C12 0.028(3) 0.013(2) 0.020(2) 0.0043(18) 0.002(2) -0.0010(19) C13 0.020(3) 0.025(2) 0.022(2) 0.007(2) -0.006(2) -0.004(2) C14 0.035(3) 0.016(2) 0.016(2) 0.0020(18) 0.000(2) -0.003(2) C15 0.031(3) 0.015(2) 0.022(2) 0.0040(18) 0.003(2) 0.003(2) Fe11 0.0265(4) 0.0186(3) 0.0159(3) 0.0039(3) -0.0027(3) -0.0040(3) C16 0.039(4) 0.035(3) 0.030(3) 0.013(2) 0.012(3) -0.003(3) C17 0.033(4) 0.052(4) 0.030(3) 0.017(3) -0.002(3) -0.018(3) C18 0.054(4) 0.021(3) 0.028(3) 0.003(2) -0.003(3) -0.020(3) C19 0.056(4) 0.021(3) 0.026(3) 0.012(2) 0.001(3) -0.003(2) C20 0.050(4) 0.028(3) 0.017(2) 0.006(2) -0.001(2) -0.010(3) C21 0.043(4) 0.039(3) 0.056(4) 0.015(3) -0.006(3) 0.003(3) C22 0.046(4) 0.036(3) 0.055(4) 0.016(3) -0.013(3) 0.003(3) C23 0.041(4) 0.027(3) 0.061(4) 0.013(3) -0.017(3) -0.003(3) C24 0.022(6) 0.043(6) 0.027(5) 0.006(5) -0.009(5) 0.007(5) C31 0.003(6) 0.056(9) 0.083(11) -0.024(9) -0.001(7) 0.009(5) C32 0.021(4) 0.056(5) 0.102(7) -0.009(5) 0.010(5) 0.011(3) C33 0.024(7) 0.064(9) 0.051(8) 0.018(7) 0.013(6) 0.031(6) C34 0.031(5) 0.119(9) 0.114(9) -0.028(7) 0.003(5) 0.023(5) C35 0.037(11) 0.116(19) 0.22(3) 0.12(3) 0.057(18) 0.044(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Se1 P1 2.0943(13) . ? P1 C1 1.776(5) . ? P1 Se2 2.2540(13) . ? P1 Se13 2.2977(13) . ? Se2 Se3 2.3329(7) . ? Se3 P11 2.2815(13) . ? C1 C5 1.449(7) . ? C1 C2 1.454(7) . ? C1 Fe1 2.033(5) . ? C2 C3 1.418(8) . ? C2 Fe1 2.049(5) . ? C2 H2A 0.9500 . ? C3 C4 1.423(8) . ? C3 Fe1 2.072(5) . ? C3 H3A 0.9500 . ? C4 C5 1.417(8) . ? C4 Fe1 2.077(5) . ? C4 H4A 0.9500 . ? C5 Fe1 2.051(5) . ? C5 H5A 0.9500 . ? Fe1 C10 2.057(5) . ? Fe1 C8 2.067(5) . ? Fe1 C9 2.067(5) . ? Fe1 C6 2.070(5) . ? Fe1 C7 2.072(5) . ? C6 C7 1.430(8) . ? C6 C10 1.432(8) . ? C6 H6A 0.9500 . ? C7 C8 1.421(8) . ? C7 H7A 0.9500 . ? C8 C9 1.430(8) . ? C8 H8A 0.9500 . ? C9 C10 1.413(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? Se11 P11 2.1027(14) . ? P11 C11 1.781(5) . ? P11 Se12 2.2823(14) . ? Se12 Se13 2.3216(7) . ? C11 C15 1.431(7) . ? C11 C12 1.440(7) . ? C11 Fe11 2.031(5) . ? C12 C13 1.425(7) . ? C12 Fe11 2.056(4) . ? C12 H12A 0.9500 . ? C13 C14 1.432(7) . ? C13 Fe11 2.075(5) . ? C13 H13A 0.9500 . ? C14 C15 1.420(8) . ? C14 Fe11 2.079(5) . ? C14 H14A 0.9500 . ? C15 Fe11 2.045(5) . ? C15 H15A 0.9500 . ? Fe11 C18 2.049(5) . ? Fe11 C17 2.056(6) . ? Fe11 C19 2.058(5) . ? Fe11 C16 2.064(5) . ? Fe11 C20 2.068(5) . ? C16 C17 1.421(9) . ? C16 C20 1.423(9) . ? C16 H16A 0.9500 . ? C17 C18 1.420(9) . ? C17 H17A 0.9500 . ? C18 C19 1.427(9) . ? C18 H18A 0.9500 . ? C19 C20 1.422(8) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.396(10) . ? C21 C23 1.407(10) 2_475 ? C22 C23 1.395(10) . ? C23 C21 1.407(10) 2_475 ? C23 C24 1.432(13) . ? C31 C35 1.09(2) 2_676 ? C31 C34 1.32(2) 2_676 ? C31 C32 1.369(17) . ? C31 C33 1.48(2) 2_676 ? C31 C32 1.57(2) 2_676 ? C31 C31 1.71(4) 2_676 ? C32 C35 1.28(4) 2_676 ? C32 C33 1.308(17) . ? C32 C31 1.57(2) 2_676 ? C33 C31 1.48(2) 2_676 ? C33 C34 1.548(19) . ? C34 C31 1.32(2) 2_676 ? C34 C35 1.43(4) . ? C35 C31 1.09(2) 2_676 ? C35 C32 1.28(4) 2_676 ? 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 P1 Se1 115.28(17) . . ? C1 P1 Se2 109.44(16) . . ? Se1 P1 Se2 104.98(6) . . ? C1 P1 Se13 100.85(17) . . ? Se1 P1 Se13 119.34(6) . . ? Se2 P1 Se13 106.52(5) . . ? P1 Se2 Se3 98.10(4) . . ? P11 Se3 Se2 99.32(4) . . ? C5 C1 C2 107.3(4) . . ? C5 C1 P1 127.6(4) . . ? C2 C1 P1 125.0(4) . . ? C5 C1 Fe1 69.9(3) . . ? C2 C1 Fe1 69.7(3) . . ? P1 C1 Fe1 123.8(3) . . ? C3 C2 C1 107.6(5) . . ? C3 C2 Fe1 70.7(3) . . ? C1 C2 Fe1 68.6(3) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? Fe1 C2 H2A 126.1 . . ? C2 C3 C4 108.6(5) . . ? C2 C3 Fe1 69.0(3) . . ? C4 C3 Fe1 70.1(3) . . ? C2 C3 H3A 125.7 . . ? C4 C3 H3A 125.7 . . ? Fe1 C3 H3A 126.7 . . ? C5 C4 C3 109.1(5) . . ? C5 C4 Fe1 69.0(3) . . ? C3 C4 Fe1 69.8(3) . . ? C5 C4 H4A 125.5 . . ? C3 C4 H4A 125.5 . . ? Fe1 C4 H4A 127.4 . . ? C4 C5 C1 107.5(5) . . ? C4 C5 Fe1 70.9(3) . . ? C1 C5 Fe1 68.6(3) . . ? C4 C5 H5A 126.3 . . ? C1 C5 H5A 126.3 . . ? Fe1 C5 H5A 125.8 . . ? C1 Fe1 C2 41.71(19) . . ? C1 Fe1 C5 41.5(2) . . ? C2 Fe1 C5 69.5(2) . . ? C1 Fe1 C10 155.9(2) . . ? C2 Fe1 C10 161.0(2) . . ? C5 Fe1 C10 120.2(2) . . ? C1 Fe1 C8 126.2(2) . . ? C2 Fe1 C8 107.2(2) . . ? C5 Fe1 C8 164.7(2) . . ? C10 Fe1 C8 67.7(2) . . ? C1 Fe1 C9 162.9(2) . . ? C2 Fe1 C9 124.3(2) . . ? C5 Fe1 C9 153.7(2) . . ? C10 Fe1 C9 40.1(2) . . ? C8 Fe1 C9 40.5(2) . . ? C1 Fe1 C6 121.3(2) . . ? C2 Fe1 C6 156.3(2) . . ? C5 Fe1 C6 109.0(2) . . ? C10 Fe1 C6 40.6(2) . . ? C8 Fe1 C6 67.7(2) . . ? C9 Fe1 C6 67.8(2) . . ? C1 Fe1 C3 68.7(2) . . ? C2 Fe1 C3 40.3(2) . . ? C5 Fe1 C3 68.3(2) . . ? C10 Fe1 C3 124.8(2) . . ? C8 Fe1 C3 119.5(2) . . ? C9 Fe1 C3 106.7(2) . . ? C6 Fe1 C3 162.8(2) . . ? C1 Fe1 C7 108.7(2) . . ? C2 Fe1 C7 120.7(2) . . ? C5 Fe1 C7 127.7(2) . . ? C10 Fe1 C7 68.0(2) . . ? C8 Fe1 C7 40.2(2) . . ? C9 Fe1 C7 67.9(2) . . ? C6 Fe1 C7 40.4(2) . . ? C3 Fe1 C7 154.5(2) . . ? C1 Fe1 C4 68.4(2) . . ? C2 Fe1 C4 68.0(2) . . ? C5 Fe1 C4 40.2(2) . . ? C10 Fe1 C4 108.0(2) . . ? C8 Fe1 C4 153.8(2) . . ? C9 Fe1 C4 119.4(2) . . ? C6 Fe1 C4 127.0(2) . . ? C3 Fe1 C4 40.1(2) . . ? C7 Fe1 C4 164.5(2) . . ? C7 C6 C10 107.6(5) . . ? C7 C6 Fe1 69.9(3) . . ? C10 C6 Fe1 69.2(3) . . ? C7 C6 H6A 126.2 . . ? C10 C6 H6A 126.2 . . ? Fe1 C6 H6A 126.3 . . ? C8 C7 C6 107.8(5) . . ? C8 C7 Fe1 69.7(3) . . ? C6 C7 Fe1 69.7(3) . . ? C8 C7 H7A 126.1 . . ? C6 C7 H7A 126.1 . . ? Fe1 C7 H7A 126.0 . . ? C7 C8 C9 108.4(5) . . ? C7 C8 Fe1 70.1(3) . . ? C9 C8 Fe1 69.8(3) . . ? C7 C8 H8A 125.8 . . ? C9 C8 H8A 125.8 . . ? Fe1 C8 H8A 125.9 . . ? C10 C9 C8 107.8(5) . . ? C10 C9 Fe1 69.6(3) . . ? C8 C9 Fe1 69.7(3) . . ? C10 C9 H9A 126.1 . . ? C8 C9 H9A 126.1 . . ? Fe1 C9 H9A 126.2 . . ? C9 C10 C6 108.4(5) . . ? C9 C10 Fe1 70.4(3) . . ? C6 C10 Fe1 70.2(3) . . ? C9 C10 H10A 125.8 . . ? C6 C10 H10A 125.8 . . ? Fe1 C10 H10A 125.3 . . ? C11 P11 Se11 114.27(17) . . ? C11 P11 Se3 107.40(15) . . ? Se11 P11 Se3 108.46(6) . . ? C11 P11 Se12 101.85(17) . . ? Se11 P11 Se12 117.78(6) . . ? Se3 P11 Se12 106.36(5) . . ? P11 Se12 Se13 97.09(4) . . ? P1 Se13 Se12 98.47(4) . . ? C15 C11 C12 108.3(4) . . ? C15 C11 P11 124.4(4) . . ? C12 C11 P11 127.3(4) . . ? C15 C11 Fe11 70.0(3) . . ? C12 C11 Fe11 70.3(3) . . ? P11 C11 Fe11 126.5(2) . . ? C13 C12 C11 107.0(4) . . ? C13 C12 Fe11 70.5(3) . . ? C11 C12 Fe11 68.4(3) . . ? C13 C12 H12A 126.5 . . ? C11 C12 H12A 126.5 . . ? Fe11 C12 H12A 126.1 . . ? C12 C13 C14 108.8(5) . . ? C12 C13 Fe11 69.1(3) . . ? C14 C13 Fe11 70.0(3) . . ? C12 C13 H13A 125.6 . . ? C14 C13 H13A 125.6 . . ? Fe11 C13 H13A 126.9 . . ? C15 C14 C13 107.8(4) . . ? C15 C14 Fe11 68.6(3) . . ? C13 C14 Fe11 69.7(3) . . ? C15 C14 H14A 126.1 . . ? C13 C14 H14A 126.1 . . ? Fe11 C14 H14A 127.3 . . ? C14 C15 C11 108.1(5) . . ? C14 C15 Fe11 71.2(3) . . ? C11 C15 Fe11 68.9(3) . . ? C14 C15 H15A 126.0 . . ? C11 C15 H15A 126.0 . . ? Fe11 C15 H15A 125.5 . . ? C11 Fe11 C15 41.11(19) . . ? C11 Fe11 C18 159.7(2) . . ? C15 Fe11 C18 121.7(2) . . ? C11 Fe11 C12 41.3(2) . . ? C15 Fe11 C12 69.14(19) . . ? C18 Fe11 C12 156.1(2) . . ? C11 Fe11 C17 159.2(2) . . ? C15 Fe11 C17 158.0(2) . . ? C18 Fe11 C17 40.5(3) . . ? C12 Fe11 C17 122.2(2) . . ? C11 Fe11 C19 124.4(2) . . ? C15 Fe11 C19 106.3(2) . . ? C18 Fe11 C19 40.7(2) . . ? C12 Fe11 C19 162.6(2) . . ? C17 Fe11 C19 68.3(3) . . ? C11 Fe11 C16 124.5(2) . . ? C15 Fe11 C16 159.3(2) . . ? C18 Fe11 C16 67.8(2) . . ? C12 Fe11 C16 110.0(2) . . ? C17 Fe11 C16 40.4(2) . . ? C19 Fe11 C16 68.0(2) . . ? C11 Fe11 C20 110.0(2) . . ? C15 Fe11 C20 122.6(2) . . ? C18 Fe11 C20 67.8(2) . . ? C12 Fe11 C20 127.1(2) . . ? C17 Fe11 C20 67.9(2) . . ? C19 Fe11 C20 40.3(2) . . ? C16 Fe11 C20 40.3(2) . . ? C11 Fe11 C13 68.2(2) . . ? C15 Fe11 C13 68.0(2) . . ? C18 Fe11 C13 120.0(2) . . ? C12 Fe11 C13 40.36(19) . . ? C17 Fe11 C13 107.4(2) . . ? C19 Fe11 C13 155.0(2) . . ? C16 Fe11 C13 125.6(2) . . ? C20 Fe11 C13 162.9(2) . . ? C11 Fe11 C14 68.31(19) . . ? C15 Fe11 C14 40.3(2) . . ? C18 Fe11 C14 105.2(2) . . ? C12 Fe11 C14 68.36(18) . . ? C17 Fe11 C14 122.4(2) . . ? C19 Fe11 C14 119.6(2) . . ? C16 Fe11 C14 160.1(2) . . ? C20 Fe11 C14 156.3(2) . . ? C13 Fe11 C14 40.3(2) . . ? C17 C16 C20 108.1(5) . . ? C17 C16 Fe11 69.5(3) . . ? C20 C16 Fe11 70.0(3) . . ? C17 C16 H16A 125.9 . . ? C20 C16 H16A 125.9 . . ? Fe11 C16 H16A 126.1 . . ? C18 C17 C16 107.8(6) . . ? C18 C17 Fe11 69.5(3) . . ? C16 C17 Fe11 70.1(3) . . ? C18 C17 H17A 126.1 . . ? C16 C17 H17A 126.1 . . ? Fe11 C17 H17A 125.8 . . ? C17 C18 C19 108.5(5) . . ? C17 C18 Fe11 70.0(3) . . ? C19 C18 Fe11 70.0(3) . . ? C17 C18 H18A 125.8 . . ? C19 C18 H18A 125.8 . . ? Fe11 C18 H18A 125.8 . . ? C20 C19 C18 107.4(6) . . ? C20 C19 Fe11 70.2(3) . . ? C18 C19 Fe11 69.3(3) . . ? C20 C19 H19A 126.3 . . ? C18 C19 H19A 126.3 . . ? Fe11 C19 H19A 125.7 . . ? C19 C20 C16 108.2(5) . . ? C19 C20 Fe11 69.5(3) . . ? C16 C20 Fe11 69.7(3) . . ? C19 C20 H20A 125.9 . . ? C16 C20 H20A 125.9 . . ? Fe11 C20 H20A 126.6 . . ? C22 C21 C23 120.0(6) . 2_475 ? C23 C22 C21 119.9(6) . . ? C22 C23 C21 120.1(6) . 2_475 ? C22 C23 C24 117.6(7) . . ? C21 C23 C24 122.2(7) 2_475 . ? C35 C31 C34 72(3) 2_676 2_676 ? C35 C31 C32 62(2) 2_676 . ? C34 C31 C32 133.4(18) 2_676 . ? C35 C31 C33 138(3) 2_676 2_676 ? C34 C31 C33 66.8(10) 2_676 2_676 ? C32 C31 C33 159.6(18) . 2_676 ? C35 C31 C32 170(3) 2_676 2_676 ? C34 C31 C32 117.5(13) 2_676 2_676 ? C32 C31 C32 109.1(13) . 2_676 ? C33 C31 C32 50.7(8) 2_676 2_676 ? C35 C31 C31 121(3) 2_676 2_676 ? C34 C31 C31 166(2) 2_676 2_676 ? C32 C31 C31 60.0(10) . 2_676 ? C33 C31 C31 99.8(16) 2_676 2_676 ? C32 C31 C31 49.1(10) 2_676 2_676 ? C35 C32 C33 179.5(18) 2_676 . ? C35 C32 C31 48.6(13) 2_676 . ? C33 C32 C31 132.0(15) . . ? C35 C32 C31 119.4(15) 2_676 2_676 ? C33 C32 C31 61.1(10) . 2_676 ? C31 C32 C31 70.9(13) . 2_676 ? C32 C33 C31 68.1(11) . 2_676 ? C32 C33 C34 120.0(13) . . ? C31 C33 C34 51.8(9) 2_676 . ? C31 C34 C35 46.6(12) 2_676 . ? C31 C34 C33 61.4(12) 2_676 . ? C35 C34 C33 107.9(15) . . ? C31 C35 C32 69.8(19) 2_676 2_676 ? C31 C35 C34 62(2) 2_676 . ? C32 C35 C34 131.5(18) 2_676 . ? 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 P1 Se2 Se3 -63.23(18) . . . . ? Se1 P1 Se2 Se3 172.49(4) . . . . ? Se13 P1 Se2 Se3 45.01(5) . . . . ? P1 Se2 Se3 P11 -87.36(5) . . . . ? Se1 P1 C1 C5 -164.3(4) . . . . ? Se2 P1 C1 C5 77.6(4) . . . . ? Se13 P1 C1 C5 -34.4(4) . . . . ? Se1 P1 C1 C2 13.0(5) . . . . ? Se2 P1 C1 C2 -105.0(4) . . . . ? Se13 P1 C1 C2 142.9(4) . . . . ? Se1 P1 C1 Fe1 -74.7(3) . . . . ? Se2 P1 C1 Fe1 167.2(2) . . . . ? Se13 P1 C1 Fe1 55.2(3) . . . . ? C5 C1 C2 C3 -0.2(5) . . . . ? P1 C1 C2 C3 -178.0(4) . . . . ? Fe1 C1 C2 C3 -60.2(3) . . . . ? C5 C1 C2 Fe1 60.1(3) . . . . ? P1 C1 C2 Fe1 -117.7(4) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? Fe1 C2 C3 C4 -59.1(3) . . . . ? C1 C2 C3 Fe1 58.9(3) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? Fe1 C3 C4 C5 -57.8(4) . . . . ? C2 C3 C4 Fe1 58.5(3) . . . . ? C3 C4 C5 C1 -0.7(6) . . . . ? Fe1 C4 C5 C1 -59.0(3) . . . . ? C3 C4 C5 Fe1 58.3(4) . . . . ? C2 C1 C5 C4 0.6(5) . . . . ? P1 C1 C5 C4 178.3(4) . . . . ? Fe1 C1 C5 C4 60.5(3) . . . . ? C2 C1 C5 Fe1 -60.0(3) . . . . ? P1 C1 C5 Fe1 117.8(4) . . . . ? C5 C1 Fe1 C2 -118.3(4) . . . . ? P1 C1 Fe1 C2 119.3(5) . . . . ? C2 C1 Fe1 C5 118.3(4) . . . . ? P1 C1 Fe1 C5 -122.5(5) . . . . ? C5 C1 Fe1 C10 48.3(6) . . . . ? C2 C1 Fe1 C10 166.6(5) . . . . ? P1 C1 Fe1 C10 -74.1(7) . . . . ? C5 C1 Fe1 C8 167.5(3) . . . . ? C2 C1 Fe1 C8 -74.3(4) . . . . ? P1 C1 Fe1 C8 45.0(4) . . . . ? C5 C1 Fe1 C9 -158.2(6) . . . . ? C2 C1 Fe1 C9 -39.9(8) . . . . ? P1 C1 Fe1 C9 79.4(8) . . . . ? C5 C1 Fe1 C6 83.5(4) . . . . ? C2 C1 Fe1 C6 -158.2(3) . . . . ? P1 C1 Fe1 C6 -38.9(4) . . . . ? C5 C1 Fe1 C3 -80.8(3) . . . . ? C2 C1 Fe1 C3 37.5(3) . . . . ? P1 C1 Fe1 C3 156.7(4) . . . . ? C5 C1 Fe1 C7 126.2(3) . . . . ? C2 C1 Fe1 C7 -115.5(3) . . . . ? P1 C1 Fe1 C7 3.8(4) . . . . ? C5 C1 Fe1 C4 -37.6(3) . . . . ? C2 C1 Fe1 C4 80.7(3) . . . . ? P1 C1 Fe1 C4 -160.0(4) . . . . ? C3 C2 Fe1 C1 118.7(4) . . . . ? C3 C2 Fe1 C5 80.2(3) . . . . ? C1 C2 Fe1 C5 -38.6(3) . . . . ? C3 C2 Fe1 C10 -44.3(8) . . . . ? C1 C2 Fe1 C10 -163.1(6) . . . . ? C3 C2 Fe1 C8 -115.6(3) . . . . ? C1 C2 Fe1 C8 125.6(3) . . . . ? C3 C2 Fe1 C9 -74.5(4) . . . . ? C1 C2 Fe1 C9 166.8(3) . . . . ? C3 C2 Fe1 C6 170.9(5) . . . . ? C1 C2 Fe1 C6 52.2(6) . . . . ? C1 C2 Fe1 C3 -118.7(4) . . . . ? C3 C2 Fe1 C7 -157.3(3) . . . . ? C1 C2 Fe1 C7 83.9(3) . . . . ? C3 C2 Fe1 C4 37.0(3) . . . . ? C1 C2 Fe1 C4 -81.8(3) . . . . ? C4 C5 Fe1 C1 -118.5(5) . . . . ? C4 C5 Fe1 C2 -79.8(4) . . . . ? C1 C5 Fe1 C2 38.7(3) . . . . ? C4 C5 Fe1 C10 82.2(4) . . . . ? C1 C5 Fe1 C10 -159.3(3) . . . . ? C4 C5 Fe1 C8 -160.1(8) . . . . ? C1 C5 Fe1 C8 -41.6(10) . . . . ? C4 C5 Fe1 C9 47.2(6) . . . . ? C1 C5 Fe1 C9 165.7(4) . . . . ? C4 C5 Fe1 C6 125.4(4) . . . . ? C1 C5 Fe1 C6 -116.1(3) . . . . ? C4 C5 Fe1 C3 -36.5(3) . . . . ? C1 C5 Fe1 C3 82.0(3) . . . . ? C4 C5 Fe1 C7 166.6(3) . . . . ? C1 C5 Fe1 C7 -74.9(4) . . . . ? C1 C5 Fe1 C4 118.5(5) . . . . ? C2 C3 Fe1 C1 -38.8(3) . . . . ? C4 C3 Fe1 C1 81.3(3) . . . . ? C4 C3 Fe1 C2 120.1(4) . . . . ? C2 C3 Fe1 C5 -83.6(3) . . . . ? C4 C3 Fe1 C5 36.5(3) . . . . ? C2 C3 Fe1 C10 163.9(3) . . . . ? C4 C3 Fe1 C10 -76.0(4) . . . . ? C2 C3 Fe1 C8 81.8(3) . . . . ? C4 C3 Fe1 C8 -158.1(3) . . . . ? C2 C3 Fe1 C9 123.8(3) . . . . ? C4 C3 Fe1 C9 -116.1(3) . . . . ? C2 C3 Fe1 C6 -167.6(6) . . . . ? C4 C3 Fe1 C6 -47.5(8) . . . . ? C2 C3 Fe1 C7 50.3(6) . . . . ? C4 C3 Fe1 C7 170.4(4) . . . . ? C2 C3 Fe1 C4 -120.1(4) . . . . ? C5 C4 Fe1 C1 38.8(3) . . . . ? C3 C4 Fe1 C1 -82.2(3) . . . . ? C5 C4 Fe1 C2 83.9(3) . . . . ? C3 C4 Fe1 C2 -37.1(3) . . . . ? C3 C4 Fe1 C5 -121.0(5) . . . . ? C5 C4 Fe1 C10 -115.9(3) . . . . ? C3 C4 Fe1 C10 123.1(3) . . . . ? C5 C4 Fe1 C8 168.2(5) . . . . ? C3 C4 Fe1 C8 47.2(6) . . . . ? C5 C4 Fe1 C9 -158.1(3) . . . . ? C3 C4 Fe1 C9 80.9(4) . . . . ? C5 C4 Fe1 C6 -74.9(4) . . . . ? C3 C4 Fe1 C6 164.1(3) . . . . ? C5 C4 Fe1 C3 121.0(5) . . . . ? C5 C4 Fe1 C7 -43.4(9) . . . . ? C3 C4 Fe1 C7 -164.4(7) . . . . ? C1 Fe1 C6 C7 82.2(4) . . . . ? C2 Fe1 C6 C7 44.3(6) . . . . ? C5 Fe1 C6 C7 126.4(3) . . . . ? C10 Fe1 C6 C7 -119.0(5) . . . . ? C8 Fe1 C6 C7 -37.6(3) . . . . ? C9 Fe1 C6 C7 -81.5(3) . . . . ? C3 Fe1 C6 C7 -155.9(6) . . . . ? C4 Fe1 C6 C7 167.6(3) . . . . ? C1 Fe1 C6 C10 -158.8(3) . . . . ? C2 Fe1 C6 C10 163.2(5) . . . . ? C5 Fe1 C6 C10 -114.6(3) . . . . ? C8 Fe1 C6 C10 81.4(4) . . . . ? C9 Fe1 C6 C10 37.4(3) . . . . ? C3 Fe1 C6 C10 -36.9(8) . . . . ? C7 Fe1 C6 C10 119.0(5) . . . . ? C4 Fe1 C6 C10 -73.5(4) . . . . ? C10 C6 C7 C8 0.5(5) . . . . ? Fe1 C6 C7 C8 59.6(3) . . . . ? C10 C6 C7 Fe1 -59.1(3) . . . . ? C1 Fe1 C7 C8 124.5(3) . . . . ? C2 Fe1 C7 C8 80.1(4) . . . . ? C5 Fe1 C7 C8 167.0(3) . . . . ? C10 Fe1 C7 C8 -81.0(4) . . . . ? C9 Fe1 C7 C8 -37.6(3) . . . . ? C6 Fe1 C7 C8 -118.9(5) . . . . ? C3 Fe1 C7 C8 44.8(6) . . . . ? C4 Fe1 C7 C8 -159.0(7) . . . . ? C1 Fe1 C7 C6 -116.7(3) . . . . ? C2 Fe1 C7 C6 -161.0(3) . . . . ? C5 Fe1 C7 C6 -74.1(4) . . . . ? C10 Fe1 C7 C6 37.9(3) . . . . ? C8 Fe1 C7 C6 118.9(5) . . . . ? C9 Fe1 C7 C6 81.3(3) . . . . ? C3 Fe1 C7 C6 163.7(4) . . . . ? C4 Fe1 C7 C6 -40.1(9) . . . . ? C6 C7 C8 C9 -0.1(5) . . . . ? Fe1 C7 C8 C9 59.5(3) . . . . ? C6 C7 C8 Fe1 -59.6(3) . . . . ? C1 Fe1 C8 C7 -75.5(4) . . . . ? C2 Fe1 C8 C7 -117.6(3) . . . . ? C5 Fe1 C8 C7 -42.4(10) . . . . ? C10 Fe1 C8 C7 81.9(4) . . . . ? C9 Fe1 C8 C7 119.4(5) . . . . ? C6 Fe1 C8 C7 37.8(3) . . . . ? C3 Fe1 C8 C7 -159.6(3) . . . . ? C4 Fe1 C8 C7 167.5(5) . . . . ? C1 Fe1 C8 C9 165.2(3) . . . . ? C2 Fe1 C8 C9 123.1(3) . . . . ? C5 Fe1 C8 C9 -161.8(8) . . . . ? C10 Fe1 C8 C9 -37.5(3) . . . . ? C6 Fe1 C8 C9 -81.5(3) . . . . ? C3 Fe1 C8 C9 81.0(4) . . . . ? C7 Fe1 C8 C9 -119.4(5) . . . . ? C4 Fe1 C8 C9 48.1(6) . . . . ? C7 C8 C9 C10 -0.3(5) . . . . ? Fe1 C8 C9 C10 59.4(3) . . . . ? C7 C8 C9 Fe1 -59.7(3) . . . . ? C1 Fe1 C9 C10 -163.6(6) . . . . ? C2 Fe1 C9 C10 165.3(3) . . . . ? C5 Fe1 C9 C10 50.2(6) . . . . ? C8 Fe1 C9 C10 -119.0(5) . . . . ? C6 Fe1 C9 C10 -37.9(3) . . . . ? C3 Fe1 C9 C10 124.8(4) . . . . ? C7 Fe1 C9 C10 -81.7(4) . . . . ? C4 Fe1 C9 C10 83.1(4) . . . . ? C1 Fe1 C9 C8 -44.6(8) . . . . ? C2 Fe1 C9 C8 -75.7(4) . . . . ? C5 Fe1 C9 C8 169.2(4) . . . . ? C10 Fe1 C9 C8 119.0(5) . . . . ? C6 Fe1 C9 C8 81.1(3) . . . . ? C3 Fe1 C9 C8 -116.2(3) . . . . ? C7 Fe1 C9 C8 37.3(3) . . . . ? C4 Fe1 C9 C8 -157.8(3) . . . . ? C8 C9 C10 C6 0.6(6) . . . . ? Fe1 C9 C10 C6 60.1(3) . . . . ? C8 C9 C10 Fe1 -59.5(3) . . . . ? C7 C6 C10 C9 -0.7(5) . . . . ? Fe1 C6 C10 C9 -60.2(3) . . . . ? C7 C6 C10 Fe1 59.5(3) . . . . ? C1 Fe1 C10 C9 168.2(5) . . . . ? C2 Fe1 C10 C9 -40.1(8) . . . . ? C5 Fe1 C10 C9 -156.8(3) . . . . ? C8 Fe1 C10 C9 37.8(3) . . . . ? C6 Fe1 C10 C9 119.0(5) . . . . ? C3 Fe1 C10 C9 -73.5(4) . . . . ? C7 Fe1 C10 C9 81.4(4) . . . . ? C4 Fe1 C10 C9 -114.6(4) . . . . ? C1 Fe1 C10 C6 49.2(7) . . . . ? C2 Fe1 C10 C6 -159.1(6) . . . . ? C5 Fe1 C10 C6 84.2(4) . . . . ? C8 Fe1 C10 C6 -81.2(4) . . . . ? C9 Fe1 C10 C6 -119.0(5) . . . . ? C3 Fe1 C10 C6 167.5(3) . . . . ? C7 Fe1 C10 C6 -37.7(3) . . . . ? C4 Fe1 C10 C6 126.4(3) . . . . ? Se2 Se3 P11 C11 -74.06(18) . . . . ? Se2 Se3 P11 Se11 161.98(5) . . . . ? Se2 Se3 P11 Se12 34.38(5) . . . . ? C11 P11 Se12 Se13 158.80(15) . . . . ? Se11 P11 Se12 Se13 -75.38(6) . . . . ? Se3 P11 Se12 Se13 46.46(5) . . . . ? C1 P1 Se13 Se12 150.25(16) . . . . ? Se1 P1 Se13 Se12 -82.40(6) . . . . ? Se2 P1 Se13 Se12 36.02(5) . . . . ? P11 Se12 Se13 P1 -88.64(5) . . . . ? Se11 P11 C11 C15 12.9(4) . . . . ? Se3 P11 C11 C15 -107.4(4) . . . . ? Se12 P11 C11 C15 141.0(4) . . . . ? Se11 P11 C11 C12 -168.7(4) . . . . ? Se3 P11 C11 C12 71.0(4) . . . . ? Se12 P11 C11 C12 -40.6(4) . . . . ? Se11 P11 C11 Fe11 -76.6(3) . . . . ? Se3 P11 C11 Fe11 163.1(2) . . . . ? Se12 P11 C11 Fe11 51.5(3) . . . . ? C15 C11 C12 C13 0.4(5) . . . . ? P11 C11 C12 C13 -178.3(3) . . . . ? Fe11 C11 C12 C13 60.3(3) . . . . ? C15 C11 C12 Fe11 -59.9(3) . . . . ? P11 C11 C12 Fe11 121.4(4) . . . . ? C11 C12 C13 C14 -0.1(5) . . . . ? Fe11 C12 C13 C14 58.9(3) . . . . ? C11 C12 C13 Fe11 -59.0(3) . . . . ? C12 C13 C14 C15 -0.3(5) . . . . ? Fe11 C13 C14 C15 58.1(3) . . . . ? C12 C13 C14 Fe11 -58.3(3) . . . . ? C13 C14 C15 C11 0.5(5) . . . . ? Fe11 C14 C15 C11 59.2(3) . . . . ? C13 C14 C15 Fe11 -58.8(3) . . . . ? C12 C11 C15 C14 -0.5(5) . . . . ? P11 C11 C15 C14 178.2(3) . . . . ? Fe11 C11 C15 C14 -60.7(3) . . . . ? C12 C11 C15 Fe11 60.1(3) . . . . ? P11 C11 C15 Fe11 -121.2(4) . . . . ? C12 C11 Fe11 C15 -119.0(4) . . . . ? P11 C11 Fe11 C15 118.6(5) . . . . ? C15 C11 Fe11 C18 -37.2(7) . . . . ? C12 C11 Fe11 C18 -156.2(6) . . . . ? P11 C11 Fe11 C18 81.4(7) . . . . ? C15 C11 Fe11 C12 119.0(4) . . . . ? P11 C11 Fe11 C12 -122.4(4) . . . . ? C15 C11 Fe11 C17 162.7(6) . . . . ? C12 C11 Fe11 C17 43.7(7) . . . . ? P11 C11 Fe11 C17 -78.7(7) . . . . ? C15 C11 Fe11 C19 -74.3(4) . . . . ? C12 C11 Fe11 C19 166.7(3) . . . . ? P11 C11 Fe11 C19 44.2(4) . . . . ? C15 C11 Fe11 C16 -159.8(3) . . . . ? C12 C11 Fe11 C16 81.2(3) . . . . ? P11 C11 Fe11 C16 -41.2(4) . . . . ? C15 C11 Fe11 C20 -117.1(3) . . . . ? C12 C11 Fe11 C20 123.9(3) . . . . ? P11 C11 Fe11 C20 1.5(4) . . . . ? C15 C11 Fe11 C13 81.1(3) . . . . ? C12 C11 Fe11 C13 -37.9(3) . . . . ? P11 C11 Fe11 C13 -160.3(4) . . . . ? C15 C11 Fe11 C14 37.5(3) . . . . ? C12 C11 Fe11 C14 -81.5(3) . . . . ? P11 C11 Fe11 C14 156.1(4) . . . . ? C14 C15 Fe11 C11 118.9(4) . . . . ? C14 C15 Fe11 C18 -75.4(3) . . . . ? C11 C15 Fe11 C18 165.7(3) . . . . ? C14 C15 Fe11 C12 80.8(3) . . . . ? C11 C15 Fe11 C12 -38.1(3) . . . . ? C14 C15 Fe11 C17 -44.7(7) . . . . ? C11 C15 Fe11 C17 -163.6(6) . . . . ? C14 C15 Fe11 C19 -116.9(3) . . . . ? C11 C15 Fe11 C19 124.2(3) . . . . ? C14 C15 Fe11 C16 172.4(5) . . . . ? C11 C15 Fe11 C16 53.5(7) . . . . ? C14 C15 Fe11 C20 -157.8(3) . . . . ? C11 C15 Fe11 C20 83.3(3) . . . . ? C14 C15 Fe11 C13 37.3(3) . . . . ? C11 C15 Fe11 C13 -81.6(3) . . . . ? C11 C15 Fe11 C14 -118.9(4) . . . . ? C13 C12 Fe11 C11 -118.2(4) . . . . ? C13 C12 Fe11 C15 -80.2(3) . . . . ? C11 C12 Fe11 C15 38.0(3) . . . . ? C13 C12 Fe11 C18 41.6(6) . . . . ? C11 C12 Fe11 C18 159.8(5) . . . . ? C13 C12 Fe11 C17 78.7(4) . . . . ? C11 C12 Fe11 C17 -163.1(3) . . . . ? C13 C12 Fe11 C19 -157.8(7) . . . . ? C11 C12 Fe11 C19 -39.6(8) . . . . ? C13 C12 Fe11 C16 121.9(3) . . . . ? C11 C12 Fe11 C16 -119.9(3) . . . . ? C13 C12 Fe11 C20 164.0(3) . . . . ? C11 C12 Fe11 C20 -77.8(4) . . . . ? C11 C12 Fe11 C13 118.2(4) . . . . ? C13 C12 Fe11 C14 -36.9(3) . . . . ? C11 C12 Fe11 C14 81.3(3) . . . . ? C12 C13 Fe11 C11 38.7(3) . . . . ? C14 C13 Fe11 C11 -81.7(3) . . . . ? C12 C13 Fe11 C15 83.2(3) . . . . ? C14 C13 Fe11 C15 -37.2(3) . . . . ? C12 C13 Fe11 C18 -161.9(3) . . . . ? C14 C13 Fe11 C18 77.7(4) . . . . ? C14 C13 Fe11 C12 -120.4(4) . . . . ? C12 C13 Fe11 C17 -119.6(3) . . . . ? C14 C13 Fe11 C17 120.0(3) . . . . ? C12 C13 Fe11 C19 164.5(5) . . . . ? C14 C13 Fe11 C19 44.1(7) . . . . ? C12 C13 Fe11 C16 -78.9(4) . . . . ? C14 C13 Fe11 C16 160.7(3) . . . . ? C12 C13 Fe11 C20 -48.6(9) . . . . ? C14 C13 Fe11 C20 -169.0(7) . . . . ? C12 C13 Fe11 C14 120.4(4) . . . . ? C15 C14 Fe11 C11 -38.3(3) . . . . ? C13 C14 Fe11 C11 81.5(3) . . . . ? C13 C14 Fe11 C15 119.8(4) . . . . ? C15 C14 Fe11 C18 121.4(3) . . . . ? C13 C14 Fe11 C18 -118.8(3) . . . . ? C15 C14 Fe11 C12 -82.9(3) . . . . ? C13 C14 Fe11 C12 36.9(3) . . . . ? C15 C14 Fe11 C17 161.9(3) . . . . ? C13 C14 Fe11 C17 -78.4(4) . . . . ? C15 C14 Fe11 C19 80.0(3) . . . . ? C13 C14 Fe11 C19 -160.2(3) . . . . ? C15 C14 Fe11 C16 -172.1(6) . . . . ? C13 C14 Fe11 C16 -52.3(7) . . . . ? C15 C14 Fe11 C20 52.2(6) . . . . ? C13 C14 Fe11 C20 172.0(5) . . . . ? C15 C14 Fe11 C13 -119.8(4) . . . . ? C11 Fe11 C16 C17 -160.5(4) . . . . ? C15 Fe11 C16 C17 159.7(5) . . . . ? C18 Fe11 C16 C17 37.9(4) . . . . ? C12 Fe11 C16 C17 -116.5(4) . . . . ? C19 Fe11 C16 C17 81.9(4) . . . . ? C20 Fe11 C16 C17 119.3(5) . . . . ? C13 Fe11 C16 C17 -74.0(4) . . . . ? C14 Fe11 C16 C17 -35.0(8) . . . . ? C11 Fe11 C16 C20 80.3(4) . . . . ? C15 Fe11 C16 C20 40.4(7) . . . . ? C18 Fe11 C16 C20 -81.4(4) . . . . ? C12 Fe11 C16 C20 124.2(3) . . . . ? C17 Fe11 C16 C20 -119.3(5) . . . . ? C19 Fe11 C16 C20 -37.3(3) . . . . ? C13 Fe11 C16 C20 166.8(3) . . . . ? C14 Fe11 C16 C20 -154.2(5) . . . . ? C20 C16 C17 C18 0.0(6) . . . . ? Fe11 C16 C17 C18 -59.6(4) . . . . ? C20 C16 C17 Fe11 59.6(4) . . . . ? C11 Fe11 C17 C18 169.5(5) . . . . ? C15 Fe11 C17 C18 -42.0(8) . . . . ? C12 Fe11 C17 C18 -157.9(3) . . . . ? C19 Fe11 C17 C18 37.6(3) . . . . ? C16 Fe11 C17 C18 118.8(5) . . . . ? C20 Fe11 C17 C18 81.3(4) . . . . ? C13 Fe11 C17 C18 -116.2(3) . . . . ? C14 Fe11 C17 C18 -74.6(4) . . . . ? C11 Fe11 C17 C16 50.8(8) . . . . ? C15 Fe11 C17 C16 -160.8(5) . . . . ? C18 Fe11 C17 C16 -118.8(5) . . . . ? C12 Fe11 C17 C16 83.3(4) . . . . ? C19 Fe11 C17 C16 -81.1(4) . . . . ? C20 Fe11 C17 C16 -37.5(4) . . . . ? C13 Fe11 C17 C16 125.0(4) . . . . ? C14 Fe11 C17 C16 166.7(3) . . . . ? C16 C17 C18 C19 0.3(6) . . . . ? Fe11 C17 C18 C19 -59.6(4) . . . . ? C16 C17 C18 Fe11 59.9(4) . . . . ? C11 Fe11 C18 C17 -169.2(5) . . . . ? C15 Fe11 C18 C17 162.9(3) . . . . ? C12 Fe11 C18 C17 51.8(7) . . . . ? C19 Fe11 C18 C17 -119.4(5) . . . . ? C16 Fe11 C18 C17 -37.8(3) . . . . ? C20 Fe11 C18 C17 -81.5(4) . . . . ? C13 Fe11 C18 C17 81.6(4) . . . . ? C14 Fe11 C18 C17 122.5(3) . . . . ? C11 Fe11 C18 C19 -49.8(7) . . . . ? C15 Fe11 C18 C19 -77.7(4) . . . . ? C12 Fe11 C18 C19 171.2(5) . . . . ? C17 Fe11 C18 C19 119.4(5) . . . . ? C16 Fe11 C18 C19 81.6(4) . . . . ? C20 Fe11 C18 C19 37.9(4) . . . . ? C13 Fe11 C18 C19 -159.0(3) . . . . ? C14 Fe11 C18 C19 -118.1(4) . . . . ? C17 C18 C19 C20 -0.5(6) . . . . ? Fe11 C18 C19 C20 -60.2(4) . . . . ? C17 C18 C19 Fe11 59.7(4) . . . . ? C11 Fe11 C19 C20 -80.3(4) . . . . ? C15 Fe11 C19 C20 -121.6(4) . . . . ? C18 Fe11 C19 C20 118.4(5) . . . . ? C12 Fe11 C19 C20 -49.7(9) . . . . ? C17 Fe11 C19 C20 80.9(4) . . . . ? C16 Fe11 C19 C20 37.3(4) . . . . ? C13 Fe11 C19 C20 165.6(5) . . . . ? C14 Fe11 C19 C20 -163.1(3) . . . . ? C11 Fe11 C19 C18 161.3(3) . . . . ? C15 Fe11 C19 C18 120.0(4) . . . . ? C12 Fe11 C19 C18 -168.1(7) . . . . ? C17 Fe11 C19 C18 -37.5(4) . . . . ? C16 Fe11 C19 C18 -81.1(4) . . . . ? C20 Fe11 C19 C18 -118.4(5) . . . . ? C13 Fe11 C19 C18 47.3(7) . . . . ? C14 Fe11 C19 C18 78.5(4) . . . . ? C18 C19 C20 C16 0.5(6) . . . . ? Fe11 C19 C20 C16 -59.1(4) . . . . ? C18 C19 C20 Fe11 59.6(3) . . . . ? C17 C16 C20 C19 -0.4(6) . . . . ? Fe11 C16 C20 C19 58.9(4) . . . . ? C17 C16 C20 Fe11 -59.3(4) . . . . ? C11 Fe11 C20 C19 120.1(4) . . . . ? C15 Fe11 C20 C19 76.1(4) . . . . ? C18 Fe11 C20 C19 -38.3(4) . . . . ? C12 Fe11 C20 C19 163.4(4) . . . . ? C17 Fe11 C20 C19 -82.1(4) . . . . ? C16 Fe11 C20 C19 -119.7(5) . . . . ? C13 Fe11 C20 C19 -159.1(7) . . . . ? C14 Fe11 C20 C19 38.8(7) . . . . ? C11 Fe11 C20 C16 -120.2(3) . . . . ? C15 Fe11 C20 C16 -164.2(3) . . . . ? C18 Fe11 C20 C16 81.4(4) . . . . ? C12 Fe11 C20 C16 -76.9(4) . . . . ? C17 Fe11 C20 C16 37.6(4) . . . . ? C19 Fe11 C20 C16 119.7(5) . . . . ? C13 Fe11 C20 C16 -39.4(9) . . . . ? C14 Fe11 C20 C16 158.5(5) . . . . ? C23 C21 C22 C23 0.1(11) 2_475 . . . ? C21 C22 C23 C21 -0.1(11) . . . 2_475 ? C21 C22 C23 C24 -176.8(7) . . . . ? C34 C31 C32 C35 -0.1(15) 2_676 . . 2_676 ? C33 C31 C32 C35 169(3) 2_676 . . 2_676 ? C32 C31 C32 C35 176.3(15) 2_676 . . 2_676 ? C31 C31 C32 C35 176.3(15) 2_676 . . 2_676 ? C35 C31 C32 C33 -180.0(16) 2_676 . . . ? C34 C31 C32 C33 180.0(12) 2_676 . . . ? C33 C31 C32 C33 -11(4) 2_676 . . . ? C32 C31 C32 C33 -3.7(13) 2_676 . . . ? C31 C31 C32 C33 -3.7(13) 2_676 . . . ? C35 C31 C32 C31 -176.3(15) 2_676 . . 2_676 ? C34 C31 C32 C31 -176.4(18) 2_676 . . 2_676 ? C33 C31 C32 C31 -7(3) 2_676 . . 2_676 ? C32 C31 C32 C31 0.000(1) 2_676 . . 2_676 ? C35 C32 C33 C31 -173(100) 2_676 . . 2_676 ? C31 C32 C33 C31 4.0(14) . . . 2_676 ? C35 C32 C33 C34 -173(100) 2_676 . . . ? C31 C32 C33 C34 4.1(17) . . . . ? C31 C32 C33 C34 0.1(9) 2_676 . . . ? C32 C33 C34 C31 -0.1(10) . . . 2_676 ? C32 C33 C34 C35 -3.2(14) . . . . ? C31 C33 C34 C35 -3.1(10) 2_676 . . . ? C33 C34 C35 C31 3.7(12) . . . 2_676 ? C31 C34 C35 C32 0.1(14) 2_676 . . 2_676 ? C33 C34 C35 C32 4(2) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 1.247 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.124 # Attachment '8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 291577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 P2 Se6' _chemical_formula_sum 'C12 H10 P2 Se6' _chemical_formula_weight 689.90 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.6219(10) _cell_length_b 9.9779(15) _cell_length_c 28.146(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1859.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 121 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max .18 _exptl_crystal_size_mid .03 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 11.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.242662 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7962 _diffrn_reflns_av_R_equivalents 0.1927 _diffrn_reflns_av_sigmaI/netI 0.1381 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2641 _reflns_number_gt 1798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 2641 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Se1 Se 0.5637(2) 0.79513(15) 0.04347(5) 0.0489(4) Uani 1 1 d . . . P1 P 0.4028(6) 0.6183(4) 0.05765(11) 0.0371(9) Uani 1 1 d . . . Se2 Se 0.5878(2) 0.51450(16) 0.11389(4) 0.0461(4) Uani 1 1 d . . . Se3 Se 0.3633(2) 0.34738(16) 0.13550(5) 0.0499(4) Uani 1 1 d . . . P11 P 0.1687(6) 0.4519(4) 0.18928(12) 0.0465(11) Uani 1 1 d . . . Se11 Se -0.0919(2) 0.3330(2) 0.19429(5) 0.0645(5) Uani 1 1 d . . . Se12 Se 0.1470(3) 0.66941(17) 0.16465(5) 0.0563(5) Uani 1 1 d . . . Se13 Se 0.0768(2) 0.64216(18) 0.08442(5) 0.0507(4) Uani 1 1 d . . . C1 C 0.3824(19) 0.5040(13) 0.0089(4) 0.034(3) Uani 1 1 d . . . C2 C 0.227(2) 0.4064(14) 0.0071(5) 0.046(4) Uani 1 1 d . . . H2A H 0.1326 0.4008 0.0314 0.055 Uiso 1 1 calc R . . C3 C 0.218(3) 0.3191(18) -0.0313(5) 0.070(5) Uani 1 1 d . . . H3A H 0.1158 0.2557 -0.0330 0.084 Uiso 1 1 calc R . . C4 C 0.361(3) 0.3260(19) -0.0668(5) 0.069(5) Uani 1 1 d . . . H4A H 0.3540 0.2658 -0.0919 0.083 Uiso 1 1 calc R . . C5 C 0.512(3) 0.4198(19) -0.0659(5) 0.068(5) Uani 1 1 d . . . H5A H 0.6067 0.4239 -0.0902 0.082 Uiso 1 1 calc R . . C6 C 0.520(2) 0.5079(16) -0.0281(5) 0.052(4) Uani 1 1 d . . . H6A H 0.6221 0.5721 -0.0275 0.062 Uiso 1 1 calc R . . C7 C 0.308(2) 0.4721(15) 0.2446(5) 0.052(4) Uani 1 1 d . . . C8 C 0.231(3) 0.4135(17) 0.2849(5) 0.079(6) Uani 1 1 d . . . H8A H 0.1113 0.3651 0.2838 0.095 Uiso 1 1 calc R . . C9 C 0.336(4) 0.428(2) 0.3273(6) 0.097(7) Uani 1 1 d . . . H9A H 0.2818 0.3938 0.3553 0.116 Uiso 1 1 calc R . . C10 C 0.520(4) 0.494(2) 0.3282(8) 0.098(7) Uani 1 1 d . . . H10A H 0.5940 0.4994 0.3561 0.117 Uiso 1 1 calc R . . C11 C 0.586(3) 0.547(2) 0.2891(7) 0.100(7) Uani 1 1 d . . . H11A H 0.7099 0.5910 0.2900 0.120 Uiso 1 1 calc R . . C12 C 0.482(3) 0.5433(18) 0.2451(5) 0.070(6) Uani 1 1 d . . . H12A H 0.5300 0.5870 0.2182 0.084 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 Se1 0.0516(10) 0.0454(10) 0.0498(8) -0.0025(8) 0.0003(8) -0.0125(8) P1 0.036(2) 0.040(2) 0.0356(17) 0.0003(17) 0.0049(18) 0.0000(19) Se2 0.0382(9) 0.0565(11) 0.0436(8) 0.0050(7) -0.0002(7) -0.0004(8) Se3 0.0586(11) 0.0449(10) 0.0462(8) 0.0008(8) 0.0079(8) -0.0023(9) P11 0.044(2) 0.055(3) 0.041(2) 0.005(2) 0.007(2) 0.003(2) Se11 0.0489(10) 0.0826(14) 0.0618(9) 0.0135(10) 0.0010(9) -0.0128(11) Se12 0.0715(11) 0.0477(11) 0.0498(8) -0.0006(8) 0.0135(8) 0.0085(10) Se13 0.0370(8) 0.0614(11) 0.0538(8) 0.0070(8) 0.0072(7) 0.0051(9) C1 0.038(8) 0.024(8) 0.039(7) 0.017(6) -0.011(7) 0.008(7) C2 0.050(10) 0.030(9) 0.057(9) 0.004(8) -0.001(8) -0.006(8) C3 0.081(13) 0.066(14) 0.065(10) -0.013(11) -0.011(10) -0.026(11) C4 0.108(15) 0.059(13) 0.041(9) -0.023(9) -0.003(10) 0.002(13) C5 0.097(15) 0.053(13) 0.054(10) -0.004(9) 0.021(9) -0.007(11) C6 0.059(10) 0.048(11) 0.048(8) 0.000(8) 0.017(8) -0.019(9) C7 0.051(10) 0.040(11) 0.066(10) -0.005(9) -0.004(9) -0.001(8) C8 0.122(16) 0.074(14) 0.042(9) 0.039(9) -0.027(10) -0.048(12) C9 0.14(2) 0.093(18) 0.061(12) 0.040(11) -0.014(14) -0.007(16) C10 0.111(19) 0.098(19) 0.084(14) 0.002(14) -0.044(14) -0.013(15) C11 0.098(17) 0.102(19) 0.101(15) -0.035(14) 0.002(16) -0.006(15) C12 0.068(11) 0.113(17) 0.029(8) -0.015(9) 0.010(8) -0.019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 P1 2.100(4) . ? P1 C1 1.790(13) . ? P1 Se2 2.253(4) . ? P1 Se13 2.299(4) . ? Se2 Se3 2.315(2) . ? Se3 P11 2.245(4) . ? P11 C7 1.821(15) . ? P11 Se11 2.099(4) . ? P11 Se12 2.283(5) . ? Se12 Se13 2.322(2) . ? C1 C6 1.385(17) . ? C1 C2 1.416(18) . ? C2 C3 1.389(19) . ? C2 H2A 0.9300 . ? C3 C4 1.37(2) . ? C3 H3A 0.9300 . ? C4 C5 1.37(2) . ? C4 H4A 0.9300 . ? C5 C6 1.38(2) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.35(2) . ? C7 C8 1.374(19) . ? C8 C9 1.39(2) . ? C8 H8A 0.9300 . ? C9 C10 1.38(3) . ? C9 H9A 0.9300 . ? C10 C11 1.30(3) . ? C10 H10A 0.9300 . ? C11 C12 1.42(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? 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 P1 Se1 115.3(4) . . ? C1 P1 Se2 106.7(4) . . ? Se1 P1 Se2 104.11(16) . . ? C1 P1 Se13 104.3(5) . . ? Se1 P1 Se13 116.85(18) . . ? Se2 P1 Se13 109.15(14) . . ? P1 Se2 Se3 99.58(11) . . ? P11 Se3 Se2 102.19(13) . . ? C7 P11 Se11 115.0(6) . . ? C7 P11 Se3 109.7(5) . . ? Se11 P11 Se3 104.76(18) . . ? C7 P11 Se12 100.7(5) . . ? Se11 P11 Se12 120.40(19) . . ? Se3 P11 Se12 105.84(16) . . ? P11 Se12 Se13 101.34(12) . . ? P1 Se13 Se12 98.22(11) . . ? C6 C1 C2 118.1(13) . . ? C6 C1 P1 120.6(11) . . ? C2 C1 P1 121.3(10) . . ? C3 C2 C1 119.3(14) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C4 C3 C2 120.3(17) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 121.4(16) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 118.6(16) . . ? C4 C5 H5A 120.7 . . ? C6 C5 H5A 120.7 . . ? C5 C6 C1 122.3(15) . . ? C5 C6 H6A 118.9 . . ? C1 C6 H6A 118.9 . . ? C12 C7 C8 122.1(15) . . ? C12 C7 P11 119.9(13) . . ? C8 C7 P11 118.0(12) . . ? C7 C8 C9 118.7(17) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C10 C9 C8 120.3(19) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 119(2) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C10 C11 C12 124(2) . . ? C10 C11 H11A 117.9 . . ? C12 C11 H11A 117.9 . . ? C7 C12 C11 115.9(17) . . ? C7 C12 H12A 122.0 . . ? C11 C12 H12A 122.0 . . ? 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 P1 Se2 Se3 -68.0(5) . . . . ? Se1 P1 Se2 Se3 169.57(12) . . . . ? Se13 P1 Se2 Se3 44.10(16) . . . . ? P1 Se2 Se3 P11 -84.81(15) . . . . ? Se2 Se3 P11 C7 -74.1(6) . . . . ? Se2 Se3 P11 Se11 161.98(13) . . . . ? Se2 Se3 P11 Se12 33.76(17) . . . . ? C7 P11 Se12 Se13 160.7(5) . . . . ? Se11 P11 Se12 Se13 -71.74(19) . . . . ? Se3 P11 Se12 Se13 46.52(17) . . . . ? C1 P1 Se13 Se12 146.6(4) . . . . ? Se1 P1 Se13 Se12 -84.82(16) . . . . ? Se2 P1 Se13 Se12 32.89(16) . . . . ? P11 Se12 Se13 P1 -84.90(16) . . . . ? Se1 P1 C1 C6 22.5(12) . . . . ? Se2 P1 C1 C6 -92.5(11) . . . . ? Se13 P1 C1 C6 152.0(10) . . . . ? Se1 P1 C1 C2 -158.2(9) . . . . ? Se2 P1 C1 C2 86.7(11) . . . . ? Se13 P1 C1 C2 -28.7(11) . . . . ? C6 C1 C2 C3 0(2) . . . . ? P1 C1 C2 C3 -179.5(11) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C2 C3 C4 C5 -1(3) . . . . ? C3 C4 C5 C6 0(3) . . . . ? C4 C5 C6 C1 0(3) . . . . ? C2 C1 C6 C5 -1(2) . . . . ? P1 C1 C6 C5 178.7(13) . . . . ? Se11 P11 C7 C12 178.0(12) . . . . ? Se3 P11 C7 C12 60.3(15) . . . . ? Se12 P11 C7 C12 -51.0(14) . . . . ? Se11 P11 C7 C8 -2.2(15) . . . . ? Se3 P11 C7 C8 -119.9(12) . . . . ? Se12 P11 C7 C8 128.8(13) . . . . ? C12 C7 C8 C9 0(3) . . . . ? P11 C7 C8 C9 -179.9(16) . . . . ? C7 C8 C9 C10 -4(3) . . . . ? C8 C9 C10 C11 4(4) . . . . ? C9 C10 C11 C12 0(4) . . . . ? C8 C7 C12 C11 4(3) . . . . ? P11 C7 C12 C11 -176.5(13) . . . . ? C10 C11 C12 C7 -4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.928 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.179