data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 Br Fe2 O6 P Se2' _chemical_formula_sum 'C22 H20 Br Fe2 O6 P Se2' _chemical_formula_weight 760.88 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' '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' 'Br' 'Br' -0.2901 2.4595 '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 10.383(5) _cell_length_b 11.346(5) _cell_length_c 11.524(5) _cell_angle_alpha 91.620(5) _cell_angle_beta 98.648(3) _cell_angle_gamma 106.563(7) _cell_volume 1282.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 3879 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 5.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4665 _exptl_absorpt_correction_T_max 0.5518 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9447 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0962 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6029 _reflns_number_gt 3904 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6029 _refine_ls_number_parameters 309 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.964 _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 Fe1 Fe 0.28945(6) 1.07823(6) 0.25690(6) 0.01419(16) Uani 1 1 d . . . Fe2 Fe 0.24428(6) 0.86306(6) 0.15503(6) 0.01363(16) Uani 1 1 d . . . P1 P 0.34367(11) 0.71919(10) 0.13669(11) 0.0132(3) Uani 1 1 d . . . Se1 Se 0.44484(4) 1.02607(4) 0.14697(4) 0.01497(12) Uani 1 1 d . . . Se2 Se 0.31329(4) 0.90703(4) 0.36243(4) 0.01549(12) Uani 1 1 d . . . Br1 Br 0.76050(5) 0.80588(5) 0.39025(5) 0.02407(14) Uani 1 1 d . . . O1 O 0.0308(3) 1.0685(3) 0.3344(3) 0.0231(8) Uani 1 1 d . . . O2 O 0.2071(4) 1.2009(3) 0.0498(3) 0.0293(9) Uani 1 1 d . . . O3 O 0.4810(3) 1.2836(3) 0.4124(3) 0.0247(8) Uani 1 1 d . . . O4 O 0.1385(4) 0.9014(3) -0.0850(3) 0.0301(9) Uani 1 1 d . . . O5 O -0.0227(3) 0.7038(3) 0.1820(4) 0.0324(10) Uani 1 1 d . . . O6 O 0.5035(3) 0.7531(3) 0.1963(3) 0.0152(7) Uani 1 1 d . . . C1 C 0.1330(4) 1.0707(4) 0.3048(4) 0.0161(10) Uani 1 1 d . . . C2 C 0.2403(5) 1.1540(4) 0.1305(5) 0.0199(11) Uani 1 1 d . . . C3 C 0.4059(5) 1.2040(5) 0.3545(5) 0.0205(11) Uani 1 1 d . . . C4 C 0.1817(5) 0.8862(4) 0.0095(5) 0.0198(11) Uani 1 1 d . . . C5 C 0.0822(5) 0.7682(4) 0.1723(5) 0.0217(11) Uani 1 1 d . . . C6 C 0.5950(4) 0.9791(4) 0.2430(4) 0.0170(10) Uani 1 1 d . . . H6A H 0.6811 1.0469 0.2504 0.020 Uiso 1 1 calc R . . H6B H 0.5740 0.9614 0.3228 0.020 Uiso 1 1 calc R . . C7 C 0.6087(4) 0.8622(4) 0.1788(5) 0.0176(10) Uani 1 1 d . . . H7 H 0.6030 0.8735 0.0926 0.021 Uiso 1 1 calc R . . C8 C 0.7419(4) 0.8351(4) 0.2244(4) 0.0182(10) Uani 1 1 d . . . H8A H 0.8190 0.9056 0.2118 0.022 Uiso 1 1 calc R . . H8B H 0.7465 0.7616 0.1788 0.022 Uiso 1 1 calc R . . C9 C 0.1574(5) 0.8485(5) 0.4488(5) 0.0262(12) Uani 1 1 d . . . H9A H 0.1654 0.9100 0.5142 0.031 Uiso 1 1 calc R . . H9B H 0.0711 0.8402 0.3949 0.031 Uiso 1 1 calc R . . C10 C 0.1544(7) 0.7264(6) 0.4972(7) 0.053(2) Uani 1 1 d U . . H10A H 0.1370 0.6635 0.4321 0.079 Uiso 1 1 calc R . . H10B H 0.0819 0.7031 0.5451 0.079 Uiso 1 1 calc R . . H10C H 0.2423 0.7330 0.5461 0.079 Uiso 1 1 calc R . . C11 C 0.3410(4) 0.6551(4) -0.0096(4) 0.0145(9) Uani 1 1 d . . . C12 C 0.2215(5) 0.6267(4) -0.0947(5) 0.0215(11) Uani 1 1 d . . . H12 H 0.1427 0.6444 -0.0756 0.026 Uiso 1 1 calc R . . C13 C 0.2168(5) 0.5742(5) -0.2038(5) 0.0270(12) Uani 1 1 d . . . H13 H 0.1350 0.5552 -0.2594 0.032 Uiso 1 1 calc R . . C14 C 0.3314(5) 0.5484(4) -0.2341(5) 0.0258(12) Uani 1 1 d . . . H14 H 0.3278 0.5113 -0.3099 0.031 Uiso 1 1 calc R . . C15 C 0.4513(6) 0.5776(5) -0.1522(6) 0.0304(13) Uani 1 1 d . . . H15 H 0.5306 0.5624 -0.1731 0.036 Uiso 1 1 calc R . . C16 C 0.4554(5) 0.6284(4) -0.0409(5) 0.0214(11) Uani 1 1 d . . . H16 H 0.5368 0.6453 0.0151 0.026 Uiso 1 1 calc R . . C17 C 0.2865(4) 0.5843(4) 0.2186(4) 0.0145(10) Uani 1 1 d . . . C18 C 0.1726(4) 0.4871(4) 0.1730(5) 0.0188(10) Uani 1 1 d . . . H18 H 0.1270 0.4874 0.0952 0.023 Uiso 1 1 calc R . . C19 C 0.1249(5) 0.3893(4) 0.2407(5) 0.0241(12) Uani 1 1 d . . . H19 H 0.0472 0.3230 0.2086 0.029 Uiso 1 1 calc R . . C20 C 0.1888(5) 0.3879(4) 0.3526(5) 0.0192(10) Uani 1 1 d . . . H20 H 0.1550 0.3215 0.3988 0.023 Uiso 1 1 calc R . . C21 C 0.3044(5) 0.4846(4) 0.3994(5) 0.0216(11) Uani 1 1 d . . . H21 H 0.3501 0.4835 0.4771 0.026 Uiso 1 1 calc R . . C22 C 0.3519(5) 0.5819(4) 0.3322(5) 0.0194(10) Uani 1 1 d . . . H22 H 0.4302 0.6477 0.3643 0.023 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 Fe1 0.0132(3) 0.0112(3) 0.0173(4) -0.0015(3) 0.0005(3) 0.0035(3) Fe2 0.0110(3) 0.0101(3) 0.0186(4) -0.0006(3) -0.0001(3) 0.0026(2) P1 0.0106(5) 0.0106(6) 0.0169(7) -0.0002(5) -0.0001(5) 0.0019(4) Se1 0.0136(2) 0.0111(2) 0.0195(3) 0.00020(19) 0.00275(19) 0.00252(17) Se2 0.0138(2) 0.0152(3) 0.0178(3) 0.0016(2) 0.00205(19) 0.00490(18) Br1 0.0188(2) 0.0305(3) 0.0210(3) 0.0040(2) -0.0022(2) 0.0068(2) O1 0.0155(16) 0.0252(19) 0.030(2) 0.0025(16) 0.0051(15) 0.0072(14) O2 0.035(2) 0.034(2) 0.025(2) 0.0070(19) 0.0058(18) 0.0189(18) O3 0.0243(18) 0.0192(19) 0.025(2) -0.0059(17) 0.0008(16) 0.0004(15) O4 0.037(2) 0.022(2) 0.023(2) 0.0040(17) -0.0078(17) -0.0002(16) O5 0.0149(17) 0.026(2) 0.053(3) 0.0032(19) 0.0036(17) 0.0016(16) O6 0.0101(14) 0.0123(16) 0.021(2) 0.0007(14) 0.0003(13) 0.0007(12) C1 0.020(2) 0.005(2) 0.017(3) -0.0020(19) -0.005(2) 0.0000(18) C2 0.019(2) 0.021(3) 0.021(3) -0.003(2) 0.001(2) 0.009(2) C3 0.016(2) 0.020(3) 0.027(3) 0.005(2) 0.007(2) 0.005(2) C4 0.019(2) 0.010(2) 0.025(3) 0.001(2) -0.002(2) 0.0001(19) C5 0.020(2) 0.017(3) 0.030(3) -0.001(2) 0.002(2) 0.009(2) C6 0.010(2) 0.018(2) 0.021(3) -0.005(2) -0.0010(19) 0.0030(18) C7 0.012(2) 0.018(3) 0.021(3) 0.001(2) 0.0016(19) 0.0026(19) C8 0.014(2) 0.021(3) 0.019(3) 0.001(2) -0.0009(19) 0.0059(19) C9 0.026(3) 0.031(3) 0.032(3) 0.011(3) 0.017(2) 0.016(2) C10 0.047(3) 0.059(4) 0.071(5) 0.045(4) 0.039(3) 0.028(3) C11 0.020(2) 0.007(2) 0.015(3) -0.0024(19) 0.0018(19) 0.0010(18) C12 0.019(2) 0.021(3) 0.024(3) 0.001(2) 0.004(2) 0.005(2) C13 0.031(3) 0.021(3) 0.023(3) -0.001(2) 0.001(2) 0.000(2) C14 0.042(3) 0.017(3) 0.013(3) -0.008(2) 0.003(2) 0.002(2) C15 0.033(3) 0.020(3) 0.045(4) 0.005(3) 0.016(3) 0.013(2) C16 0.026(2) 0.014(2) 0.028(3) 0.005(2) 0.008(2) 0.009(2) C17 0.015(2) 0.012(2) 0.019(3) 0.000(2) 0.0033(19) 0.0076(18) C18 0.016(2) 0.016(2) 0.021(3) 0.002(2) -0.004(2) 0.0028(19) C19 0.015(2) 0.013(3) 0.041(4) 0.001(2) 0.001(2) -0.0002(19) C20 0.023(2) 0.013(2) 0.022(3) 0.002(2) 0.006(2) 0.006(2) C21 0.028(3) 0.020(3) 0.015(3) 0.002(2) 0.001(2) 0.006(2) C22 0.021(2) 0.014(2) 0.020(3) -0.003(2) -0.001(2) 0.0023(19) _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 Fe1 C1 1.773(5) . ? Fe1 C2 1.794(5) . ? Fe1 C3 1.811(6) . ? Fe1 Se2 2.3729(11) . ? Fe1 Se1 2.3822(10) . ? Fe1 Fe2 2.5647(14) . ? Fe2 C4 1.760(5) . ? Fe2 C5 1.763(5) . ? Fe2 P1 2.1865(14) . ? Fe2 Se1 2.3744(11) . ? Fe2 Se2 2.3851(13) . ? P1 O6 1.628(3) . ? P1 C11 1.810(5) . ? P1 C17 1.821(5) . ? Se1 C6 1.982(4) . ? Se2 C9 1.990(4) . ? Br1 C8 1.939(5) . ? O1 C1 1.156(5) . ? O2 C2 1.142(6) . ? O3 C3 1.130(6) . ? O4 C4 1.151(6) . ? O5 C5 1.149(5) . ? O6 C7 1.441(5) . ? C6 C7 1.552(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.522(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.501(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.401(6) . ? C11 C12 1.413(7) . ? C12 C13 1.364(7) . ? C12 H12 0.9500 . ? C13 C14 1.393(7) . ? C13 H13 0.9500 . ? C14 C15 1.395(8) . ? C14 H14 0.9500 . ? C15 C16 1.381(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.386(7) . ? C17 C18 1.389(6) . ? C18 C19 1.392(7) . ? C18 H18 0.9500 . ? C19 C20 1.361(7) . ? C19 H19 0.9500 . ? C20 C21 1.399(7) . ? C20 H20 0.9500 . ? C21 C22 1.384(6) . ? C21 H21 0.9500 . ? C22 H22 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 C1 Fe1 C2 89.9(2) . . ? C1 Fe1 C3 101.1(2) . . ? C2 Fe1 C3 103.1(2) . . ? C1 Fe1 Se2 92.02(14) . . ? C2 Fe1 Se2 155.47(17) . . ? C3 Fe1 Se2 100.53(16) . . ? C1 Fe1 Se1 158.93(16) . . ? C2 Fe1 Se1 86.05(15) . . ? C3 Fe1 Se1 99.93(14) . . ? Se2 Fe1 Se1 83.43(3) . . ? C1 Fe1 Fe2 103.11(15) . . ? C2 Fe1 Fe2 98.18(17) . . ? C3 Fe1 Fe2 147.59(14) . . ? Se2 Fe1 Fe2 57.61(4) . . ? Se1 Fe1 Fe2 57.22(3) . . ? C4 Fe2 C5 91.0(2) . . ? C4 Fe2 P1 104.46(16) . . ? C5 Fe2 P1 98.51(15) . . ? C4 Fe2 Se1 88.92(15) . . ? C5 Fe2 Se1 167.38(15) . . ? P1 Fe2 Se1 93.73(5) . . ? C4 Fe2 Se2 157.69(16) . . ? C5 Fe2 Se2 92.10(18) . . ? P1 Fe2 Se2 96.92(4) . . ? Se1 Fe2 Se2 83.34(3) . . ? C4 Fe2 Fe1 101.18(16) . . ? C5 Fe2 Fe1 110.21(16) . . ? P1 Fe2 Fe1 140.83(5) . . ? Se1 Fe2 Fe1 57.52(3) . . ? Se2 Fe2 Fe1 57.15(3) . . ? O6 P1 C11 103.33(19) . . ? O6 P1 C17 95.62(19) . . ? C11 P1 C17 104.0(2) . . ? O6 P1 Fe2 116.33(13) . . ? C11 P1 Fe2 118.59(15) . . ? C17 P1 Fe2 115.73(14) . . ? C6 Se1 Fe2 105.64(14) . . ? C6 Se1 Fe1 114.61(14) . . ? Fe2 Se1 Fe1 65.26(4) . . ? C9 Se2 Fe1 109.66(14) . . ? C9 Se2 Fe2 111.77(18) . . ? Fe1 Se2 Fe2 65.24(3) . . ? C7 O6 P1 125.5(3) . . ? O1 C1 Fe1 178.2(4) . . ? O2 C2 Fe1 178.9(5) . . ? O3 C3 Fe1 177.6(4) . . ? O4 C4 Fe2 178.7(4) . . ? O5 C5 Fe2 178.1(5) . . ? C7 C6 Se1 107.0(3) . . ? C7 C6 H6A 110.3 . . ? Se1 C6 H6A 110.3 . . ? C7 C6 H6B 110.3 . . ? Se1 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? O6 C7 C8 105.0(3) . . ? O6 C7 C6 111.8(3) . . ? C8 C7 C6 112.6(4) . . ? O6 C7 H7 109.1 . . ? C8 C7 H7 109.1 . . ? C6 C7 H7 109.1 . . ? C7 C8 Br1 112.5(3) . . ? C7 C8 H8A 109.1 . . ? Br1 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? Br1 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C10 C9 Se2 111.0(3) . . ? C10 C9 H9A 109.4 . . ? Se2 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? Se2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 117.9(5) . . ? C16 C11 P1 121.3(4) . . ? C12 C11 P1 120.8(3) . . ? C13 C12 C11 121.3(4) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 120.3(5) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 120.7(5) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C22 C17 C18 118.9(4) . . ? C22 C17 P1 119.5(4) . . ? C18 C17 P1 121.4(4) . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.8(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C17 120.7(5) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? 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 Fe1 Fe2 C4 90.2(2) . . . . ? C2 Fe1 Fe2 C4 -1.5(2) . . . . ? C3 Fe1 Fe2 C4 -132.3(3) . . . . ? Se2 Fe1 Fe2 C4 174.23(15) . . . . ? Se1 Fe1 Fe2 C4 -81.46(15) . . . . ? C1 Fe1 Fe2 C5 -5.0(2) . . . . ? C2 Fe1 Fe2 C5 -96.8(2) . . . . ? C3 Fe1 Fe2 C5 132.4(3) . . . . ? Se2 Fe1 Fe2 C5 78.98(18) . . . . ? Se1 Fe1 Fe2 C5 -176.70(18) . . . . ? C1 Fe1 Fe2 P1 -139.55(17) . . . . ? C2 Fe1 Fe2 P1 128.66(16) . . . . ? C3 Fe1 Fe2 P1 -2.1(3) . . . . ? Se2 Fe1 Fe2 P1 -55.56(7) . . . . ? Se1 Fe1 Fe2 P1 48.75(7) . . . . ? C1 Fe1 Fe2 Se1 171.70(16) . . . . ? C2 Fe1 Fe2 Se1 79.91(15) . . . . ? C3 Fe1 Fe2 Se1 -50.9(3) . . . . ? Se2 Fe1 Fe2 Se1 -104.32(3) . . . . ? C1 Fe1 Fe2 Se2 -83.98(16) . . . . ? C2 Fe1 Fe2 Se2 -175.77(15) . . . . ? C3 Fe1 Fe2 Se2 53.5(3) . . . . ? Se1 Fe1 Fe2 Se2 104.32(3) . . . . ? C4 Fe2 P1 O6 123.3(2) . . . . ? C5 Fe2 P1 O6 -143.5(2) . . . . ? Se1 Fe2 P1 O6 33.46(14) . . . . ? Se2 Fe2 P1 O6 -50.27(14) . . . . ? Fe1 Fe2 P1 O6 -6.00(17) . . . . ? C4 Fe2 P1 C11 -0.9(2) . . . . ? C5 Fe2 P1 C11 92.3(2) . . . . ? Se1 Fe2 P1 C11 -90.78(17) . . . . ? Se2 Fe2 P1 C11 -174.51(16) . . . . ? Fe1 Fe2 P1 C11 -130.25(17) . . . . ? C4 Fe2 P1 C17 -125.6(2) . . . . ? C5 Fe2 P1 C17 -32.4(3) . . . . ? Se1 Fe2 P1 C17 144.55(18) . . . . ? Se2 Fe2 P1 C17 60.82(19) . . . . ? Fe1 Fe2 P1 C17 105.09(19) . . . . ? C4 Fe2 Se1 C6 -145.7(2) . . . . ? C5 Fe2 Se1 C6 124.6(8) . . . . ? P1 Fe2 Se1 C6 -41.27(15) . . . . ? Se2 Fe2 Se1 C6 55.27(15) . . . . ? Fe1 Fe2 Se1 C6 110.31(15) . . . . ? C4 Fe2 Se1 Fe1 104.00(16) . . . . ? C5 Fe2 Se1 Fe1 14.3(8) . . . . ? P1 Fe2 Se1 Fe1 -151.58(5) . . . . ? Se2 Fe2 Se1 Fe1 -55.04(3) . . . . ? C1 Fe1 Se1 C6 -119.6(4) . . . . ? C2 Fe1 Se1 C6 161.0(2) . . . . ? C3 Fe1 Se1 C6 58.4(2) . . . . ? Se2 Fe1 Se1 C6 -41.18(15) . . . . ? Fe2 Fe1 Se1 C6 -96.62(15) . . . . ? C1 Fe1 Se1 Fe2 -23.0(4) . . . . ? C2 Fe1 Se1 Fe2 -102.36(16) . . . . ? C3 Fe1 Se1 Fe2 155.03(16) . . . . ? Se2 Fe1 Se1 Fe2 55.45(3) . . . . ? C1 Fe1 Se2 C9 -1.3(2) . . . . ? C2 Fe1 Se2 C9 -95.5(4) . . . . ? C3 Fe1 Se2 C9 100.4(2) . . . . ? Se1 Fe1 Se2 C9 -160.69(19) . . . . ? Fe2 Fe1 Se2 C9 -105.6(2) . . . . ? C1 Fe1 Se2 Fe2 104.27(16) . . . . ? C2 Fe1 Se2 Fe2 10.1(3) . . . . ? C3 Fe1 Se2 Fe2 -154.02(14) . . . . ? Se1 Fe1 Se2 Fe2 -55.09(3) . . . . ? C4 Fe2 Se2 C9 87.3(4) . . . . ? C5 Fe2 Se2 C9 -10.4(2) . . . . ? P1 Fe2 Se2 C9 -109.25(15) . . . . ? Se1 Fe2 Se2 C9 157.78(15) . . . . ? Fe1 Fe2 Se2 C9 102.40(15) . . . . ? C4 Fe2 Se2 Fe1 -15.1(4) . . . . ? C5 Fe2 Se2 Fe1 -112.81(15) . . . . ? P1 Fe2 Se2 Fe1 148.35(4) . . . . ? Se1 Fe2 Se2 Fe1 55.38(3) . . . . ? C11 P1 O6 C7 81.0(4) . . . . ? C17 P1 O6 C7 -173.2(4) . . . . ? Fe2 P1 O6 C7 -50.8(4) . . . . ? C2 Fe1 C1 O1 -25(15) . . . . ? C3 Fe1 C1 O1 78(15) . . . . ? Se2 Fe1 C1 O1 179(100) . . . . ? Se1 Fe1 C1 O1 -104(15) . . . . ? Fe2 Fe1 C1 O1 -124(15) . . . . ? C1 Fe1 C2 O2 -44(25) . . . . ? C3 Fe1 C2 O2 -146(25) . . . . ? Se2 Fe1 C2 O2 50(25) . . . . ? Se1 Fe1 C2 O2 115(25) . . . . ? Fe2 Fe1 C2 O2 59(25) . . . . ? C1 Fe1 C3 O3 -146(10) . . . . ? C2 Fe1 C3 O3 -53(10) . . . . ? Se2 Fe1 C3 O3 120(10) . . . . ? Se1 Fe1 C3 O3 35(10) . . . . ? Fe2 Fe1 C3 O3 77(10) . . . . ? C5 Fe2 C4 O4 39(20) . . . . ? P1 Fe2 C4 O4 138(20) . . . . ? Se1 Fe2 C4 O4 -129(20) . . . . ? Se2 Fe2 C4 O4 -59(20) . . . . ? Fe1 Fe2 C4 O4 -72(20) . . . . ? C4 Fe2 C5 O5 81(15) . . . . ? P1 Fe2 C5 O5 -24(15) . . . . ? Se1 Fe2 C5 O5 171(15) . . . . ? Se2 Fe2 C5 O5 -121(15) . . . . ? Fe1 Fe2 C5 O5 -177(100) . . . . ? Fe2 Se1 C6 C7 65.7(3) . . . . ? Fe1 Se1 C6 C7 135.2(3) . . . . ? P1 O6 C7 C8 -165.3(3) . . . . ? P1 O6 C7 C6 72.4(5) . . . . ? Se1 C6 C7 O6 -77.0(4) . . . . ? Se1 C6 C7 C8 165.1(3) . . . . ? O6 C7 C8 Br1 -61.2(4) . . . . ? C6 C7 C8 Br1 60.7(4) . . . . ? Fe1 Se2 C9 C10 169.0(4) . . . . ? Fe2 Se2 C9 C10 98.7(5) . . . . ? O6 P1 C11 C16 9.4(4) . . . . ? C17 P1 C11 C16 -90.0(4) . . . . ? Fe2 P1 C11 C16 139.8(3) . . . . ? O6 P1 C11 C12 -172.8(4) . . . . ? C17 P1 C11 C12 87.8(4) . . . . ? Fe2 P1 C11 C12 -42.4(4) . . . . ? C16 C11 C12 C13 0.3(7) . . . . ? P1 C11 C12 C13 -177.6(4) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C12 C13 C14 C15 -0.5(7) . . . . ? C13 C14 C15 C16 1.8(7) . . . . ? C14 C15 C16 C11 -2.1(7) . . . . ? C12 C11 C16 C15 1.0(7) . . . . ? P1 C11 C16 C15 178.9(4) . . . . ? O6 P1 C17 C22 32.3(4) . . . . ? C11 P1 C17 C22 137.6(4) . . . . ? Fe2 P1 C17 C22 -90.6(4) . . . . ? O6 P1 C17 C18 -152.3(4) . . . . ? C11 P1 C17 C18 -47.0(4) . . . . ? Fe2 P1 C17 C18 84.9(4) . . . . ? C22 C17 C18 C19 0.2(7) . . . . ? P1 C17 C18 C19 -175.2(3) . . . . ? C17 C18 C19 C20 0.3(7) . . . . ? C18 C19 C20 C21 -0.9(7) . . . . ? C19 C20 C21 C22 0.9(7) . . . . ? C20 C21 C22 C17 -0.3(7) . . . . ? C18 C17 C22 C21 -0.3(7) . . . . ? P1 C17 C22 C21 175.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.207 _refine_diff_density_min -1.617 _refine_diff_density_rms 0.189