# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound4a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H18 Fe P, I' _chemical_formula_sum 'C13 H18 Fe I P' _chemical_formula_weight 387.99 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_space_group_name_HALL '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' 'y, z, x' '-z+1/2, -x, y+1/2' '-y, z+1/2, -x+1/2' 'z+1/2, -x+1/2, -y' '-y+1/2, -z, x+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-z, -x, -y' '-y, -z, -x' 'z-1/2, x, -y-1/2' 'y, -z-1/2, x-1/2' '-z-1/2, x-1/2, y' 'y-1/2, z, -x-1/2' 'z, -x-1/2, y-1/2' '-y-1/2, z-1/2, x' _cell_length_a 20.3608(13) _cell_length_b 20.3608(13) _cell_length_c 20.3608(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8440.8(9) _cell_formula_units_Z 24 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2486 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.93 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 3.352 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 0.7442 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; A bad GooF-value (Goodness of Fit) has been found, which is attributable to the relatively weak dataset. ; _diffrn_ambient_temperature 100(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7968 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.1985 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.75 _reflns_number_total 2978 _reflns_number_gt 1217 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0000P)^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 2978 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0418 _refine_ls_wR_factor_gt 0.0320 _refine_ls_goodness_of_fit_ref 0.475 _refine_ls_restrained_S_all 0.475 _refine_ls_shift/su_max 0.023 _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 C1 C 0.5313(3) 0.9162(3) 0.7764(3) 0.0140(12) Uani 1 1 d . . . C5 C 0.5849(3) 0.9111(3) 0.8204(3) 0.0173(14) Uani 1 1 d . . . H5 H 0.6015 0.9456 0.8470 0.021 Uiso 1 1 calc R . . C4 C 0.6098(3) 0.8459(3) 0.8184(3) 0.0227(14) Uani 1 1 d . . . H4 H 0.6455 0.8291 0.8433 0.027 Uiso 1 1 calc R . . C3 C 0.5711(3) 0.8104(3) 0.7722(3) 0.0226(15) Uani 1 1 d . . . H3 H 0.5768 0.7655 0.7609 0.027 Uiso 1 1 calc R . . C2 C 0.5227(3) 0.8532(2) 0.7454(3) 0.0197(13) Uani 1 1 d . . . H2 H 0.4908 0.8423 0.7131 0.024 Uiso 1 1 calc R . . C11 C 0.4065(3) 0.9752(3) 0.8115(3) 0.0235(15) Uani 1 1 d . . . H11A H 0.3827 0.9364 0.7958 0.035 Uiso 1 1 calc R . . H11B H 0.3788 1.0143 0.8061 0.035 Uiso 1 1 calc R . . H11C H 0.4174 0.9696 0.8581 0.035 Uiso 1 1 calc R . . C13 C 0.5208(3) 1.0564(3) 0.7946(3) 0.0261(15) Uani 1 1 d . . . H13A H 0.5310 1.0512 0.8413 0.039 Uiso 1 1 calc R . . H13B H 0.4925 1.0948 0.7885 0.039 Uiso 1 1 calc R . . H13C H 0.5617 1.0625 0.7699 0.039 Uiso 1 1 calc R . . C12 C 0.4569(3) 0.9934(3) 0.6824(2) 0.0186(13) Uani 1 1 d . . . H12A H 0.4963 1.0004 0.6556 0.028 Uiso 1 1 calc R . . H12B H 0.4272 1.0310 0.6775 0.028 Uiso 1 1 calc R . . H12C H 0.4345 0.9533 0.6678 0.028 Uiso 1 1 calc R . . C6 C 0.6249(3) 0.9187(3) 0.6316(3) 0.0184(13) Uani 1 1 d . . . H6 H 0.5905 0.9291 0.6018 0.022 Uiso 1 1 calc R . . C7 C 0.6540(3) 0.8556(3) 0.6423(3) 0.0193(13) Uani 1 1 d . . . H7 H 0.6422 0.8163 0.6201 0.023 Uiso 1 1 calc R . . C8 C 0.7029(3) 0.8610(3) 0.6910(3) 0.0196(14) Uani 1 1 d . . . H8 H 0.7292 0.8262 0.7075 0.024 Uiso 1 1 calc R . . C9 C 0.7061(3) 0.9264(3) 0.7105(3) 0.0245(16) Uani 1 1 d . . . H9 H 0.7353 0.9440 0.7423 0.029 Uiso 1 1 calc R . . C10 C 0.6580(3) 0.9627(3) 0.6748(3) 0.0239(14) Uani 1 1 d . . . H10 H 0.6494 1.0084 0.6791 0.029 Uiso 1 1 calc R . . P1 P 0.47970(7) 0.98503(7) 0.76563(6) 0.0145(3) Uani 1 1 d . . . Fe1 Fe 0.61419(4) 0.88946(4) 0.72786(4) 0.01341(16) Uani 1 1 d . . . I1 I 0.5000 0.5000 1.0000 0.0131(2) Uani 1 6 d S . . I2 I 0.5000 1.0000 1.0000 0.0264(3) Uani 1 6 d S . . I3 I 0.65851(2) 0.65851(2) 0.65851(2) 0.01945(17) Uani 1 3 d S . . I4 I 0.83626(2) 0.83626(2) 0.83626(2) 0.02017(18) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.008(3) 0.020(3) 0.014(3) 0.006(2) 0.002(2) 0.003(2) C5 0.020(3) 0.019(3) 0.013(3) -0.001(2) 0.001(2) 0.007(2) C4 0.031(4) 0.030(4) 0.008(3) 0.006(3) -0.005(3) 0.001(3) C3 0.025(3) 0.017(3) 0.025(4) 0.014(3) 0.014(3) 0.007(3) C2 0.026(3) 0.016(3) 0.017(3) 0.002(3) 0.008(3) -0.001(2) C11 0.022(3) 0.021(3) 0.028(3) 0.010(3) 0.005(3) 0.008(3) C13 0.026(4) 0.027(4) 0.026(4) 0.000(3) -0.008(3) -0.003(3) C12 0.024(3) 0.012(3) 0.020(3) 0.001(3) -0.004(2) -0.005(3) C6 0.013(3) 0.028(4) 0.013(3) 0.006(3) 0.000(2) 0.002(3) C7 0.021(3) 0.018(3) 0.019(3) -0.002(2) 0.002(3) 0.007(3) C8 0.011(3) 0.028(4) 0.019(3) 0.002(3) 0.002(3) 0.005(2) C9 0.020(4) 0.042(4) 0.012(3) -0.010(3) -0.003(3) -0.014(3) C10 0.030(3) 0.020(3) 0.022(3) 0.007(3) 0.015(3) -0.003(3) P1 0.0162(8) 0.0144(9) 0.0129(9) 0.0009(6) 0.0027(5) 0.0023(5) Fe1 0.0146(4) 0.0132(4) 0.0124(4) -0.0004(3) 0.0011(3) 0.0022(4) I1 0.0131(2) 0.0131(2) 0.0131(2) 0.0007(3) -0.0007(3) -0.0007(3) I2 0.0264(3) 0.0264(3) 0.0264(3) 0.0025(3) -0.0025(3) 0.0025(3) I3 0.01945(17) 0.01945(17) 0.01945(17) -0.0011(2) -0.0011(2) -0.0011(2) I4 0.02017(18) 0.02017(18) 0.02017(18) -0.0009(2) -0.0009(2) -0.0009(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.415(7) . ? C1 C2 1.441(7) . ? C1 P1 1.765(5) . ? C1 Fe1 2.030(5) . ? C5 C4 1.422(8) . ? C5 Fe1 2.025(5) . ? C5 H5 0.9500 . ? C4 C3 1.424(8) . ? C4 Fe1 2.049(5) . ? C4 H4 0.9500 . ? C3 C2 1.425(7) . ? C3 Fe1 2.043(6) . ? C3 H3 0.9500 . ? C2 Fe1 2.035(5) . ? C2 H2 0.9500 . ? C11 P1 1.771(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 P1 1.778(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 P1 1.766(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C6 C10 1.426(8) . ? C6 C7 1.432(7) . ? C6 Fe1 2.060(5) . ? C6 H6 0.9500 . ? C7 C8 1.410(7) . ? C7 Fe1 2.041(5) . ? C7 H7 0.9500 . ? C8 C9 1.391(8) . ? C8 Fe1 2.041(5) . ? C8 H8 0.9500 . ? C9 C10 1.426(8) . ? C9 Fe1 2.047(6) . ? C9 H9 0.9500 . ? C10 Fe1 2.045(5) . ? C10 H10 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 C5 C1 C2 107.8(5) . . ? C5 C1 P1 126.6(4) . . ? C2 C1 P1 125.4(4) . . ? C5 C1 Fe1 69.4(3) . . ? C2 C1 Fe1 69.4(3) . . ? P1 C1 Fe1 130.3(3) . . ? C1 C5 C4 109.0(5) . . ? C1 C5 Fe1 69.8(3) . . ? C4 C5 Fe1 70.5(3) . . ? C1 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Fe1 C5 H5 125.9 . . ? C5 C4 C3 107.2(5) . . ? C5 C4 Fe1 68.7(3) . . ? C3 C4 Fe1 69.4(3) . . ? C5 C4 H4 126.4 . . ? C3 C4 H4 126.4 . . ? Fe1 C4 H4 127.0 . . ? C4 C3 C2 109.0(5) . . ? C4 C3 Fe1 69.9(3) . . ? C2 C3 Fe1 69.3(3) . . ? C4 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? Fe1 C3 H3 127.0 . . ? C3 C2 C1 107.0(5) . . ? C3 C2 Fe1 69.8(3) . . ? C1 C2 Fe1 69.1(3) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? Fe1 C2 H2 126.2 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C6 C7 105.9(5) . . ? C10 C6 Fe1 69.1(3) . . ? C7 C6 Fe1 68.9(3) . . ? C10 C6 H6 127.0 . . ? C7 C6 H6 127.0 . . ? Fe1 C6 H6 126.5 . . ? C8 C7 C6 109.3(5) . . ? C8 C7 Fe1 69.8(3) . . ? C6 C7 Fe1 70.3(3) . . ? C8 C7 H7 125.4 . . ? C6 C7 H7 125.4 . . ? Fe1 C7 H7 126.2 . . ? C9 C8 C7 108.0(5) . . ? C9 C8 Fe1 70.3(3) . . ? C7 C8 Fe1 69.8(3) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe1 C8 H8 125.4 . . ? C8 C9 C10 108.6(5) . . ? C8 C9 Fe1 69.9(3) . . ? C10 C9 Fe1 69.6(3) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 126.5 . . ? C6 C10 C9 108.3(5) . . ? C6 C10 Fe1 70.2(3) . . ? C9 C10 Fe1 69.7(3) . . ? C6 C10 H10 125.9 . . ? C9 C10 H10 125.9 . . ? Fe1 C10 H10 125.8 . . ? C1 P1 C12 110.6(3) . . ? C1 P1 C11 110.3(3) . . ? C12 P1 C11 107.2(3) . . ? C1 P1 C13 109.1(3) . . ? C12 P1 C13 111.3(3) . . ? C11 P1 C13 108.3(3) . . ? C5 Fe1 C1 40.8(2) . . ? C5 Fe1 C2 69.3(2) . . ? C1 Fe1 C2 41.53(19) . . ? C5 Fe1 C8 131.7(2) . . ? C1 Fe1 C8 172.4(2) . . ? C2 Fe1 C8 140.5(2) . . ? C5 Fe1 C7 169.9(2) . . ? C1 Fe1 C7 146.8(2) . . ? C2 Fe1 C7 113.0(2) . . ? C8 Fe1 C7 40.4(2) . . ? C5 Fe1 C3 68.5(2) . . ? C1 Fe1 C3 68.9(2) . . ? C2 Fe1 C3 40.9(2) . . ? C8 Fe1 C3 108.6(2) . . ? C7 Fe1 C3 106.3(2) . . ? C5 Fe1 C10 117.5(2) . . ? C1 Fe1 C10 115.1(2) . . ? C2 Fe1 C10 139.1(2) . . ? C8 Fe1 C10 68.1(2) . . ? C7 Fe1 C10 67.8(2) . . ? C3 Fe1 C10 174.0(2) . . ? C5 Fe1 C9 110.5(2) . . ? C1 Fe1 C9 138.1(2) . . ? C2 Fe1 C9 179.7(3) . . ? C8 Fe1 C9 39.8(2) . . ? C7 Fe1 C9 67.3(2) . . ? C3 Fe1 C9 139.3(2) . . ? C10 Fe1 C9 40.8(2) . . ? C5 Fe1 C4 40.8(2) . . ? C1 Fe1 C4 69.0(2) . . ? C2 Fe1 C4 69.2(2) . . ? C8 Fe1 C4 104.3(3) . . ? C7 Fe1 C4 129.7(2) . . ? C3 Fe1 C4 40.7(2) . . ? C10 Fe1 C4 144.1(2) . . ? C9 Fe1 C4 110.8(3) . . ? C5 Fe1 C6 148.6(2) . . ? C1 Fe1 C6 118.3(2) . . ? C2 Fe1 C6 111.6(2) . . ? C8 Fe1 C6 68.8(2) . . ? C7 Fe1 C6 40.9(2) . . ? C3 Fe1 C6 133.9(2) . . ? C10 Fe1 C6 40.6(2) . . ? C9 Fe1 C6 68.5(2) . . ? C4 Fe1 C6 170.5(2) . . ? 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 C2 C1 C5 C4 -0.7(6) . . . . ? P1 C1 C5 C4 174.7(4) . . . . ? Fe1 C1 C5 C4 -59.7(4) . . . . ? C2 C1 C5 Fe1 59.0(4) . . . . ? P1 C1 C5 Fe1 -125.6(4) . . . . ? C1 C5 C4 C3 0.3(6) . . . . ? Fe1 C5 C4 C3 -59.0(4) . . . . ? C1 C5 C4 Fe1 59.3(4) . . . . ? C5 C4 C3 C2 0.2(6) . . . . ? Fe1 C4 C3 C2 -58.3(4) . . . . ? C5 C4 C3 Fe1 58.5(4) . . . . ? C4 C3 C2 C1 -0.6(6) . . . . ? Fe1 C3 C2 C1 -59.3(3) . . . . ? C4 C3 C2 Fe1 58.7(4) . . . . ? C5 C1 C2 C3 0.8(6) . . . . ? P1 C1 C2 C3 -174.7(4) . . . . ? Fe1 C1 C2 C3 59.8(3) . . . . ? C5 C1 C2 Fe1 -59.0(4) . . . . ? P1 C1 C2 Fe1 125.5(4) . . . . ? C10 C6 C7 C8 0.5(6) . . . . ? Fe1 C6 C7 C8 -59.0(4) . . . . ? C10 C6 C7 Fe1 59.5(4) . . . . ? C6 C7 C8 C9 -0.9(6) . . . . ? Fe1 C7 C8 C9 -60.3(4) . . . . ? C6 C7 C8 Fe1 59.3(4) . . . . ? C7 C8 C9 C10 1.0(6) . . . . ? Fe1 C8 C9 C10 -58.9(4) . . . . ? C7 C8 C9 Fe1 59.9(4) . . . . ? C7 C6 C10 C9 0.1(6) . . . . ? Fe1 C6 C10 C9 59.5(4) . . . . ? C7 C6 C10 Fe1 -59.3(4) . . . . ? C8 C9 C10 C6 -0.7(6) . . . . ? Fe1 C9 C10 C6 -59.8(4) . . . . ? C8 C9 C10 Fe1 59.1(4) . . . . ? C5 C1 P1 C12 143.9(5) . . . . ? C2 C1 P1 C12 -41.4(5) . . . . ? Fe1 C1 P1 C12 50.7(5) . . . . ? C5 C1 P1 C11 -97.6(5) . . . . ? C2 C1 P1 C11 77.0(5) . . . . ? Fe1 C1 P1 C11 169.2(4) . . . . ? C5 C1 P1 C13 21.2(6) . . . . ? C2 C1 P1 C13 -164.2(5) . . . . ? Fe1 C1 P1 C13 -72.1(4) . . . . ? C4 C5 Fe1 C1 120.0(5) . . . . ? C1 C5 Fe1 C2 -38.2(3) . . . . ? C4 C5 Fe1 C2 81.8(4) . . . . ? C1 C5 Fe1 C8 -178.4(3) . . . . ? C4 C5 Fe1 C8 -58.4(5) . . . . ? C1 C5 Fe1 C7 -143.0(13) . . . . ? C4 C5 Fe1 C7 -23.0(15) . . . . ? C1 C5 Fe1 C3 -82.2(4) . . . . ? C4 C5 Fe1 C3 37.8(3) . . . . ? C1 C5 Fe1 C10 97.4(4) . . . . ? C4 C5 Fe1 C10 -142.6(4) . . . . ? C1 C5 Fe1 C9 141.6(3) . . . . ? C4 C5 Fe1 C9 -98.4(4) . . . . ? C1 C5 Fe1 C4 -120.0(5) . . . . ? C1 C5 Fe1 C6 59.6(6) . . . . ? C4 C5 Fe1 C6 179.6(4) . . . . ? C2 C1 Fe1 C5 -119.3(5) . . . . ? P1 C1 Fe1 C5 121.1(5) . . . . ? C5 C1 Fe1 C2 119.3(5) . . . . ? P1 C1 Fe1 C2 -119.5(5) . . . . ? C5 C1 Fe1 C7 168.9(4) . . . . ? C2 C1 Fe1 C7 49.6(5) . . . . ? P1 C1 Fe1 C7 -70.0(6) . . . . ? C5 C1 Fe1 C3 81.2(4) . . . . ? C2 C1 Fe1 C3 -38.2(3) . . . . ? P1 C1 Fe1 C3 -157.7(5) . . . . ? C5 C1 Fe1 C10 -103.8(4) . . . . ? C2 C1 Fe1 C10 136.9(3) . . . . ? P1 C1 Fe1 C10 17.4(5) . . . . ? C5 C1 Fe1 C9 -60.7(5) . . . . ? C2 C1 Fe1 C9 180.0(4) . . . . ? P1 C1 Fe1 C9 60.4(6) . . . . ? C5 C1 Fe1 C4 37.4(3) . . . . ? C2 C1 Fe1 C4 -82.0(3) . . . . ? P1 C1 Fe1 C4 158.5(5) . . . . ? C5 C1 Fe1 C6 -149.4(3) . . . . ? C2 C1 Fe1 C6 91.3(3) . . . . ? P1 C1 Fe1 C6 -28.2(5) . . . . ? C3 C2 Fe1 C5 -80.7(4) . . . . ? C1 C2 Fe1 C5 37.6(3) . . . . ? C3 C2 Fe1 C1 -118.3(5) . . . . ? C3 C2 Fe1 C8 50.5(5) . . . . ? C1 C2 Fe1 C8 168.8(4) . . . . ? C3 C2 Fe1 C7 88.6(4) . . . . ? C1 C2 Fe1 C7 -153.1(3) . . . . ? C1 C2 Fe1 C3 118.3(5) . . . . ? C3 C2 Fe1 C10 170.8(4) . . . . ? C1 C2 Fe1 C10 -70.9(4) . . . . ? C3 C2 Fe1 C4 -36.9(3) . . . . ? C1 C2 Fe1 C4 81.4(3) . . . . ? C3 C2 Fe1 C6 132.9(4) . . . . ? C1 C2 Fe1 C6 -108.8(3) . . . . ? C9 C8 Fe1 C5 -70.3(4) . . . . ? C7 C8 Fe1 C5 171.0(3) . . . . ? C9 C8 Fe1 C2 -179.9(4) . . . . ? C7 C8 Fe1 C2 61.4(5) . . . . ? C9 C8 Fe1 C7 118.7(5) . . . . ? C9 C8 Fe1 C3 -147.7(4) . . . . ? C7 C8 Fe1 C3 93.6(4) . . . . ? C9 C8 Fe1 C10 37.6(3) . . . . ? C7 C8 Fe1 C10 -81.1(4) . . . . ? C7 C8 Fe1 C9 -118.7(5) . . . . ? C9 C8 Fe1 C4 -105.4(4) . . . . ? C7 C8 Fe1 C4 135.9(3) . . . . ? C9 C8 Fe1 C6 81.4(4) . . . . ? C7 C8 Fe1 C6 -37.3(3) . . . . ? C8 C7 Fe1 C5 -41.9(15) . . . . ? C6 C7 Fe1 C5 -162.2(13) . . . . ? C8 C7 Fe1 C1 -175.9(4) . . . . ? C6 C7 Fe1 C1 63.7(5) . . . . ? C8 C7 Fe1 C2 -142.7(3) . . . . ? C6 C7 Fe1 C2 96.9(4) . . . . ? C6 C7 Fe1 C8 -120.4(5) . . . . ? C8 C7 Fe1 C3 -99.7(4) . . . . ? C6 C7 Fe1 C3 139.9(3) . . . . ? C8 C7 Fe1 C10 81.8(4) . . . . ? C6 C7 Fe1 C10 -38.6(3) . . . . ? C8 C7 Fe1 C9 37.5(3) . . . . ? C6 C7 Fe1 C9 -82.9(4) . . . . ? C8 C7 Fe1 C4 -61.3(4) . . . . ? C6 C7 Fe1 C4 178.4(3) . . . . ? C8 C7 Fe1 C6 120.4(5) . . . . ? C4 C3 Fe1 C5 -37.9(3) . . . . ? C2 C3 Fe1 C5 82.7(4) . . . . ? C4 C3 Fe1 C1 -81.9(4) . . . . ? C2 C3 Fe1 C1 38.7(3) . . . . ? C4 C3 Fe1 C2 -120.6(5) . . . . ? C4 C3 Fe1 C8 90.5(4) . . . . ? C2 C3 Fe1 C8 -148.9(3) . . . . ? C4 C3 Fe1 C7 132.9(3) . . . . ? C2 C3 Fe1 C7 -106.5(4) . . . . ? C4 C3 Fe1 C9 58.9(5) . . . . ? C2 C3 Fe1 C9 179.6(4) . . . . ? C2 C3 Fe1 C4 120.6(5) . . . . ? C4 C3 Fe1 C6 168.6(4) . . . . ? C2 C3 Fe1 C6 -70.7(4) . . . . ? C6 C10 Fe1 C5 -150.7(3) . . . . ? C9 C10 Fe1 C5 90.1(4) . . . . ? C6 C10 Fe1 C1 -105.0(3) . . . . ? C9 C10 Fe1 C1 135.8(3) . . . . ? C6 C10 Fe1 C2 -61.2(4) . . . . ? C9 C10 Fe1 C2 179.5(4) . . . . ? C6 C10 Fe1 C8 82.5(4) . . . . ? C9 C10 Fe1 C8 -36.7(3) . . . . ? C6 C10 Fe1 C7 38.8(3) . . . . ? C9 C10 Fe1 C7 -80.5(3) . . . . ? C6 C10 Fe1 C9 119.3(5) . . . . ? C6 C10 Fe1 C4 166.7(4) . . . . ? C9 C10 Fe1 C4 47.5(5) . . . . ? C9 C10 Fe1 C6 -119.3(5) . . . . ? C8 C9 Fe1 C5 131.4(3) . . . . ? C10 C9 Fe1 C5 -108.7(3) . . . . ? C8 C9 Fe1 C1 168.8(3) . . . . ? C10 C9 Fe1 C1 -71.2(4) . . . . ? C10 C9 Fe1 C8 119.9(5) . . . . ? C8 C9 Fe1 C7 -38.0(3) . . . . ? C10 C9 Fe1 C7 81.9(3) . . . . ? C8 C9 Fe1 C3 50.9(5) . . . . ? C10 C9 Fe1 C3 170.8(4) . . . . ? C8 C9 Fe1 C10 -119.9(5) . . . . ? C8 C9 Fe1 C4 87.6(4) . . . . ? C10 C9 Fe1 C4 -152.5(3) . . . . ? C8 C9 Fe1 C6 -82.3(4) . . . . ? C10 C9 Fe1 C6 37.6(3) . . . . ? C3 C4 Fe1 C5 119.0(5) . . . . ? C5 C4 Fe1 C1 -37.3(3) . . . . ? C3 C4 Fe1 C1 81.7(4) . . . . ? C5 C4 Fe1 C2 -81.9(3) . . . . ? C3 C4 Fe1 C2 37.1(3) . . . . ? C5 C4 Fe1 C8 139.0(3) . . . . ? C3 C4 Fe1 C8 -102.0(4) . . . . ? C5 C4 Fe1 C7 174.9(3) . . . . ? C3 C4 Fe1 C7 -66.1(4) . . . . ? C5 C4 Fe1 C3 -119.0(5) . . . . ? C5 C4 Fe1 C10 66.7(5) . . . . ? C3 C4 Fe1 C10 -174.3(4) . . . . ? C5 C4 Fe1 C9 97.7(4) . . . . ? C3 C4 Fe1 C9 -143.3(3) . . . . ? C10 C6 Fe1 C5 56.6(6) . . . . ? C7 C6 Fe1 C5 174.1(4) . . . . ? C10 C6 Fe1 C1 96.4(4) . . . . ? C7 C6 Fe1 C1 -146.1(3) . . . . ? C10 C6 Fe1 C2 141.9(3) . . . . ? C7 C6 Fe1 C2 -100.6(4) . . . . ? C10 C6 Fe1 C8 -80.6(4) . . . . ? C7 C6 Fe1 C8 36.9(3) . . . . ? C10 C6 Fe1 C7 -117.5(5) . . . . ? C10 C6 Fe1 C3 -176.5(3) . . . . ? C7 C6 Fe1 C3 -59.0(5) . . . . ? C7 C6 Fe1 C10 117.5(5) . . . . ? C10 C6 Fe1 C9 -37.8(3) . . . . ? C7 C6 Fe1 C9 79.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.553 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 974963' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound5f _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H36 Fe P, C2 F6 N O4 S2' _chemical_formula_sum 'C24 H36 F6 Fe N O4 P S2' _chemical_formula_weight 667.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_HALL '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6934(3) _cell_length_b 14.4249(6) _cell_length_c 20.1051(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.508(3) _cell_angle_gamma 90.00 _cell_volume 3074.65(19) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 16155 _cell_measurement_theta_min 3.48 _cell_measurement_theta_max 54.08 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7568 _exptl_absorpt_correction_T_max 1.1785 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23096 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.79 _reflns_number_total 6538 _reflns_number_gt 4300 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0796P)^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 6538 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.840 _refine_ls_restrained_S_all 0.840 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7993(3) 1.0084(2) 0.78094(14) 0.0303(7) Uani 1 1 d . . . C2 C 0.6783(3) 1.0515(2) 0.77391(15) 0.0343(7) Uani 1 1 d . . . H2 H 0.6017 1.0222 0.7767 0.041 Uiso 1 1 calc R . . C3 C 0.6957(3) 1.1466(2) 0.76201(15) 0.0361(7) Uani 1 1 d . . . H3 H 0.6320 1.1908 0.7556 0.043 Uiso 1 1 calc R . . C4 C 0.8254(4) 1.1636(2) 0.76134(15) 0.0379(8) Uani 1 1 d . . . H4 H 0.8616 1.2209 0.7546 0.045 Uiso 1 1 calc R . . C5 C 0.8915(3) 1.0785(2) 0.77270(15) 0.0336(7) Uani 1 1 d . . . H5 H 0.9781 1.0699 0.7745 0.040 Uiso 1 1 calc R . . C6 C 0.7117(4) 1.1011(3) 0.93684(15) 0.0413(8) Uani 1 1 d . . . H6 H 0.6355 1.0722 0.9412 0.050 Uiso 1 1 calc R . . C7 C 0.7275(4) 1.1947(3) 0.91846(17) 0.0425(8) Uani 1 1 d . . . H7 H 0.6636 1.2383 0.9086 0.051 Uiso 1 1 calc R . . C8 C 0.8570(4) 1.2099(3) 0.91773(16) 0.0454(9) Uani 1 1 d . . . H8 H 0.8935 1.2656 0.9070 0.054 Uiso 1 1 calc R . . C9 C 0.9220(3) 1.1276(3) 0.93571(16) 0.0445(9) Uani 1 1 d . . . H9 H 1.0088 1.1192 0.9393 0.053 Uiso 1 1 calc R . . C10 C 0.8320(4) 1.0595(3) 0.94740(15) 0.0427(9) Uani 1 1 d . . . H10 H 0.8491 0.9982 0.9598 0.051 Uiso 1 1 calc R . . C11 C 0.6920(3) 0.8248(2) 0.80233(15) 0.0340(7) Uani 1 1 d . . . H11A H 0.6238 0.8397 0.7672 0.041 Uiso 1 1 calc R . . H11B H 0.7095 0.7591 0.7988 0.041 Uiso 1 1 calc R . . C12 C 0.6451(3) 0.8420(2) 0.87055(15) 0.0337(7) Uani 1 1 d . . . H12A H 0.7150 0.8356 0.9062 0.040 Uiso 1 1 calc R . . H12B H 0.6128 0.9047 0.8719 0.040 Uiso 1 1 calc R . . C13 C 0.5420(3) 0.7735(2) 0.88152(16) 0.0365(7) Uani 1 1 d . . . H13A H 0.4757 0.7769 0.8438 0.044 Uiso 1 1 calc R . . H13B H 0.5766 0.7113 0.8828 0.044 Uiso 1 1 calc R . . C14 C 0.4855(4) 0.7907(3) 0.94540(18) 0.0439(8) Uani 1 1 d . . . H14A H 0.5512 0.7912 0.9828 0.066 Uiso 1 1 calc R . . H14B H 0.4263 0.7423 0.9515 0.066 Uiso 1 1 calc R . . H14C H 0.4429 0.8494 0.9425 0.066 Uiso 1 1 calc R . . C15 C 0.9619(3) 0.8616(2) 0.84806(15) 0.0330(7) Uani 1 1 d . . . H15A H 1.0379 0.8851 0.8324 0.040 Uiso 1 1 calc R . . H15B H 0.9514 0.8942 0.8891 0.040 Uiso 1 1 calc R . . C16 C 0.9801(3) 0.7583(2) 0.86404(15) 0.0362(7) Uani 1 1 d . . . H16A H 0.9156 0.7379 0.8905 0.043 Uiso 1 1 calc R . . H16B H 0.9703 0.7232 0.8225 0.043 Uiso 1 1 calc R . . C17 C 1.1090(3) 0.7389(3) 0.90236(16) 0.0429(8) Uani 1 1 d . . . H17A H 1.1220 0.7788 0.9415 0.052 Uiso 1 1 calc R . . H17B H 1.1732 0.7537 0.8741 0.052 Uiso 1 1 calc R . . C18 C 1.1240(5) 0.6385(3) 0.9247(2) 0.0609(12) Uani 1 1 d . . . H18A H 1.0591 0.6229 0.9515 0.091 Uiso 1 1 calc R . . H18B H 1.2052 0.6302 0.9506 0.091 Uiso 1 1 calc R . . H18C H 1.1172 0.5989 0.8860 0.091 Uiso 1 1 calc R . . C19 C 0.8710(3) 0.8531(2) 0.70574(15) 0.0349(7) Uani 1 1 d . . . H19A H 0.9513 0.8811 0.6999 0.042 Uiso 1 1 calc R . . H19B H 0.8821 0.7864 0.7058 0.042 Uiso 1 1 calc R . . C20 C 0.7750(4) 0.8795(2) 0.64612(16) 0.0406(8) Uani 1 1 d . . . H20A H 0.7549 0.9448 0.6487 0.049 Uiso 1 1 calc R . . H20B H 0.6979 0.8445 0.6478 0.049 Uiso 1 1 calc R . . C21 C 0.8252(5) 0.8600(3) 0.57983(17) 0.0535(10) Uani 1 1 d . . . H21A H 0.9034 0.8937 0.5788 0.064 Uiso 1 1 calc R . . H21B H 0.8435 0.7943 0.5769 0.064 Uiso 1 1 calc R . . C22 C 0.7324(6) 0.8878(3) 0.52005(19) 0.0740(15) Uani 1 1 d . . . H22A H 0.6523 0.8592 0.5232 0.111 Uiso 1 1 calc R . . H22B H 0.7630 0.8679 0.4796 0.111 Uiso 1 1 calc R . . H22C H 0.7228 0.9540 0.5194 0.111 Uiso 1 1 calc R . . C23 C 0.2914(4) 0.9963(3) 0.65381(17) 0.0437(8) Uani 1 1 d . . . C24 C 0.2969(3) 1.0542(2) 0.90207(16) 0.0386(8) Uani 1 1 d . . . N1 N 0.3761(3) 1.0170(2) 0.78450(13) 0.0352(6) Uani 1 1 d . . . O1 O 0.1701(2) 0.93051(18) 0.74637(12) 0.0454(6) Uani 1 1 d . . . O2 O 0.3776(3) 0.86487(17) 0.73279(13) 0.0484(6) Uani 1 1 d . . . O3 O 0.1936(2) 1.12885(17) 0.79154(12) 0.0427(6) Uani 1 1 d . . . O4 O 0.4114(2) 1.17093(16) 0.83442(12) 0.0415(6) Uani 1 1 d . . . F1 F 0.2305(2) 1.07630(16) 0.65066(10) 0.0570(6) Uani 1 1 d . . . F2 F 0.2322(3) 0.93960(16) 0.60829(10) 0.0614(6) Uani 1 1 d . . . F3 F 0.4059(2) 1.01220(18) 0.63782(11) 0.0617(6) Uani 1 1 d . . . F4 F 0.2176(2) 0.98250(15) 0.89649(10) 0.0503(6) Uani 1 1 d . . . F5 F 0.2493(2) 1.11936(16) 0.93858(10) 0.0504(5) Uani 1 1 d . . . F6 F 0.4055(2) 1.02662(15) 0.93540(10) 0.0463(5) Uani 1 1 d . . . P1 P 0.82936(8) 0.88775(6) 0.78602(4) 0.03015(19) Uani 1 1 d . . . S1 S 0.29940(8) 0.94389(6) 0.73719(4) 0.0358(2) Uani 1 1 d . . . S2 S 0.31745(8) 1.10136(6) 0.81962(4) 0.03418(19) Uani 1 1 d . . . Fe1 Fe 0.79611(4) 1.10865(3) 0.85147(2) 0.03029(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0317(17) 0.0356(16) 0.0240(14) 0.0004(12) 0.0050(12) -0.0004(14) C2 0.0304(17) 0.0459(19) 0.0257(14) 0.0007(13) 0.0003(13) 0.0011(14) C3 0.0405(19) 0.0404(17) 0.0271(14) 0.0037(13) 0.0034(13) 0.0046(15) C4 0.049(2) 0.0365(17) 0.0293(15) 0.0045(13) 0.0090(14) -0.0035(15) C5 0.0327(17) 0.0425(18) 0.0273(14) -0.0024(13) 0.0104(13) -0.0018(14) C6 0.0416(19) 0.057(2) 0.0281(15) -0.0012(15) 0.0166(14) -0.0053(17) C7 0.046(2) 0.049(2) 0.0339(16) -0.0059(15) 0.0124(15) 0.0108(17) C8 0.063(3) 0.0435(19) 0.0306(16) -0.0070(15) 0.0080(16) -0.0102(19) C9 0.0355(19) 0.070(3) 0.0278(15) -0.0106(16) 0.0018(14) -0.0004(18) C10 0.059(2) 0.047(2) 0.0228(14) 0.0020(14) 0.0096(15) 0.0075(18) C11 0.0357(18) 0.0361(16) 0.0308(15) 0.0011(13) 0.0072(13) -0.0042(14) C12 0.0366(18) 0.0371(17) 0.0288(15) -0.0023(13) 0.0094(13) -0.0001(14) C13 0.0371(18) 0.0413(18) 0.0322(15) -0.0012(14) 0.0085(13) -0.0044(15) C14 0.049(2) 0.043(2) 0.0436(18) 0.0007(16) 0.0219(16) 0.0015(17) C15 0.0329(17) 0.0389(17) 0.0278(14) 0.0004(13) 0.0055(13) 0.0009(14) C16 0.0421(19) 0.0368(17) 0.0308(15) 0.0008(13) 0.0087(14) 0.0030(15) C17 0.047(2) 0.050(2) 0.0305(15) -0.0022(15) 0.0013(15) 0.0105(17) C18 0.077(3) 0.051(2) 0.053(2) 0.0045(19) -0.002(2) 0.020(2) C19 0.0390(19) 0.0390(17) 0.0279(15) -0.0021(13) 0.0094(13) -0.0016(15) C20 0.050(2) 0.0411(18) 0.0304(16) 0.0009(14) 0.0050(15) -0.0092(16) C21 0.081(3) 0.050(2) 0.0310(17) -0.0024(16) 0.0128(18) -0.008(2) C22 0.115(4) 0.076(3) 0.0283(18) -0.0008(19) -0.002(2) -0.023(3) C23 0.053(2) 0.0421(19) 0.0374(18) 0.0014(15) 0.0125(16) -0.0012(17) C24 0.0363(19) 0.0450(19) 0.0342(16) -0.0013(15) 0.0036(14) -0.0060(16) N1 0.0310(15) 0.0418(15) 0.0336(14) 0.0009(12) 0.0070(11) 0.0006(12) O1 0.0362(13) 0.0577(15) 0.0437(13) -0.0025(12) 0.0104(11) -0.0137(12) O2 0.0576(17) 0.0381(13) 0.0488(14) 0.0014(11) 0.0043(12) 0.0067(12) O3 0.0389(14) 0.0464(14) 0.0418(13) 0.0007(11) 0.0022(11) 0.0050(11) O4 0.0390(14) 0.0399(13) 0.0456(13) 0.0014(11) 0.0054(11) -0.0064(11) F1 0.0827(17) 0.0479(12) 0.0405(11) 0.0092(9) 0.0089(11) 0.0126(12) F2 0.0856(18) 0.0598(14) 0.0374(11) -0.0039(10) 0.0023(11) -0.0131(13) F3 0.0678(16) 0.0722(16) 0.0514(13) 0.0062(11) 0.0312(12) -0.0081(13) F4 0.0536(13) 0.0617(13) 0.0363(10) 0.0005(9) 0.0087(9) -0.0249(11) F5 0.0478(12) 0.0629(14) 0.0424(11) -0.0082(10) 0.0128(9) 0.0005(11) F6 0.0459(12) 0.0525(12) 0.0390(10) 0.0057(9) -0.0001(9) 0.0005(10) P1 0.0317(4) 0.0345(4) 0.0246(3) -0.0011(3) 0.0049(3) -0.0016(4) S1 0.0375(5) 0.0365(4) 0.0337(4) 0.0044(3) 0.0061(3) -0.0025(4) S2 0.0314(4) 0.0366(4) 0.0347(4) 0.0035(3) 0.0047(3) -0.0007(3) Fe1 0.0314(3) 0.0352(2) 0.0252(2) 0.00017(18) 0.00733(17) -0.0001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.426(5) . ? C1 C5 1.438(5) . ? C1 P1 1.770(3) . ? C1 Fe1 2.029(3) . ? C2 C3 1.408(5) . ? C2 Fe1 2.045(3) . ? C2 H2 0.9300 . ? C3 C4 1.411(5) . ? C3 Fe1 2.045(3) . ? C3 H3 0.9300 . ? C4 C5 1.420(5) . ? C4 Fe1 2.039(3) . ? C4 H4 0.9300 . ? C5 Fe1 2.040(3) . ? C5 H5 0.9300 . ? C6 C10 1.410(5) . ? C6 C7 1.416(5) . ? C6 Fe1 2.044(3) . ? C6 H6 0.9300 . ? C7 C8 1.404(6) . ? C7 Fe1 2.038(3) . ? C7 H7 0.9300 . ? C8 C9 1.399(5) . ? C8 Fe1 2.027(3) . ? C8 H8 0.9300 . ? C9 C10 1.417(5) . ? C9 Fe1 2.040(3) . ? C9 H9 0.9300 . ? C10 Fe1 2.044(3) . ? C10 H10 0.9300 . ? C11 C12 1.541(4) . ? C11 P1 1.794(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.518(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.510(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.531(4) . ? C15 P1 1.802(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.514(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.518(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.521(4) . ? C19 P1 1.800(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.527(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.510(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 F1 1.322(4) . ? C23 F3 1.325(5) . ? C23 F2 1.326(4) . ? C23 S1 1.831(4) . ? C24 F6 1.323(4) . ? C24 F4 1.333(4) . ? C24 F5 1.334(4) . ? C24 S2 1.832(4) . ? N1 S2 1.577(3) . ? N1 S1 1.577(3) . ? O1 S1 1.432(3) . ? O2 S1 1.423(3) . ? O3 S2 1.427(2) . ? O4 S2 1.424(2) . ? 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 C1 C5 108.0(3) . . ? C2 C1 P1 126.2(2) . . ? C5 C1 P1 125.2(3) . . ? C2 C1 Fe1 70.13(18) . . ? C5 C1 Fe1 69.70(17) . . ? P1 C1 Fe1 132.84(16) . . ? C3 C2 C1 107.7(3) . . ? C3 C2 Fe1 69.86(18) . . ? C1 C2 Fe1 68.89(17) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? Fe1 C2 H2 126.7 . . ? C4 C3 C2 108.8(3) . . ? C4 C3 Fe1 69.57(18) . . ? C2 C3 Fe1 69.88(17) . . ? C4 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? Fe1 C3 H3 126.6 . . ? C3 C4 C5 108.5(3) . . ? C3 C4 Fe1 70.01(19) . . ? C5 C4 Fe1 69.64(18) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe1 C4 H4 126.2 . . ? C4 C5 C1 107.0(3) . . ? C4 C5 Fe1 69.63(19) . . ? C1 C5 Fe1 68.91(18) . . ? C4 C5 H5 126.5 . . ? C1 C5 H5 126.5 . . ? Fe1 C5 H5 126.5 . . ? C10 C6 C7 108.0(3) . . ? C10 C6 Fe1 69.83(19) . . ? C7 C6 Fe1 69.47(19) . . ? C10 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Fe1 C6 H6 126.2 . . ? C8 C7 C6 107.7(3) . . ? C8 C7 Fe1 69.4(2) . . ? C6 C7 Fe1 69.92(19) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Fe1 C7 H7 126.1 . . ? C9 C8 C7 108.8(3) . . ? C9 C8 Fe1 70.4(2) . . ? C7 C8 Fe1 70.2(2) . . ? C9 C8 H8 125.6 . . ? C7 C8 H8 125.6 . . ? Fe1 C8 H8 125.4 . . ? C8 C9 C10 107.8(3) . . ? C8 C9 Fe1 69.37(19) . . ? C10 C9 Fe1 69.85(18) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 126.3 . . ? C6 C10 C9 107.8(3) . . ? C6 C10 Fe1 69.82(18) . . ? C9 C10 Fe1 69.54(19) . . ? C6 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.1 . . ? C12 C11 P1 116.8(2) . . ? C12 C11 H11A 108.1 . . ? P1 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? P1 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C13 C12 C11 110.6(3) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 113.3(3) . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P1 114.6(2) . . ? C16 C15 H15A 108.6 . . ? P1 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? P1 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 111.7(3) . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 112.4(3) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 P1 114.6(2) . . ? C20 C19 H19A 108.6 . . ? P1 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? P1 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C19 C20 C21 111.3(3) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 112.1(4) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? F1 C23 F3 107.6(3) . . ? F1 C23 F2 108.5(3) . . ? F3 C23 F2 108.2(3) . . ? F1 C23 S1 111.6(3) . . ? F3 C23 S1 111.1(3) . . ? F2 C23 S1 109.7(2) . . ? F6 C24 F4 108.4(3) . . ? F6 C24 F5 107.8(3) . . ? F4 C24 F5 108.0(3) . . ? F6 C24 S2 111.7(2) . . ? F4 C24 S2 111.2(2) . . ? F5 C24 S2 109.6(2) . . ? S2 N1 S1 125.49(18) . . ? C1 P1 C11 111.19(16) . . ? C1 P1 C19 106.57(15) . . ? C11 P1 C19 109.13(16) . . ? C1 P1 C15 111.51(15) . . ? C11 P1 C15 110.89(15) . . ? C19 P1 C15 107.35(16) . . ? O2 S1 O1 119.03(17) . . ? O2 S1 N1 108.06(16) . . ? O1 S1 N1 116.56(16) . . ? O2 S1 C23 103.39(17) . . ? O1 S1 C23 104.09(17) . . ? N1 S1 C23 103.54(16) . . ? O4 S2 O3 118.69(15) . . ? O4 S2 N1 109.06(15) . . ? O3 S2 N1 116.11(14) . . ? O4 S2 C24 103.73(15) . . ? O3 S2 C24 104.27(16) . . ? N1 S2 C24 102.73(16) . . ? C8 Fe1 C1 160.08(15) . . ? C8 Fe1 C4 103.31(15) . . ? C1 Fe1 C4 68.76(13) . . ? C8 Fe1 C7 40.40(16) . . ? C1 Fe1 C7 159.51(15) . . ? C4 Fe1 C7 117.44(15) . . ? C8 Fe1 C5 120.90(15) . . ? C1 Fe1 C5 41.40(13) . . ? C4 Fe1 C5 40.73(14) . . ? C7 Fe1 C5 154.52(15) . . ? C8 Fe1 C9 40.26(15) . . ? C1 Fe1 C9 127.34(14) . . ? C4 Fe1 C9 121.61(16) . . ? C7 Fe1 C9 67.96(15) . . ? C5 Fe1 C9 109.30(14) . . ? C8 Fe1 C6 68.00(15) . . ? C1 Fe1 C6 126.77(14) . . ? C4 Fe1 C6 154.55(15) . . ? C7 Fe1 C6 40.60(15) . . ? C5 Fe1 C6 164.02(15) . . ? C9 Fe1 C6 68.01(15) . . ? C8 Fe1 C10 68.00(15) . . ? C1 Fe1 C10 113.19(14) . . ? C4 Fe1 C10 160.35(15) . . ? C7 Fe1 C10 68.10(14) . . ? C5 Fe1 C10 127.42(14) . . ? C9 Fe1 C10 40.61(15) . . ? C6 Fe1 C10 40.35(15) . . ? C8 Fe1 C2 154.75(15) . . ? C1 Fe1 C2 40.98(13) . . ? C4 Fe1 C2 68.30(14) . . ? C7 Fe1 C2 120.68(14) . . ? C5 Fe1 C2 69.09(13) . . ? C9 Fe1 C2 163.96(15) . . ? C6 Fe1 C2 108.86(14) . . ? C10 Fe1 C2 126.91(15) . . ? C8 Fe1 C3 118.16(14) . . ? C1 Fe1 C3 68.34(13) . . ? C4 Fe1 C3 40.42(14) . . ? C7 Fe1 C3 103.02(14) . . ? C5 Fe1 C3 68.45(14) . . ? C9 Fe1 C3 155.25(15) . . ? C6 Fe1 C3 120.94(15) . . ? C10 Fe1 C3 159.22(16) . . ? C2 Fe1 C3 40.26(13) . . ? 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 C5 C1 C2 C3 -0.4(3) . . . . ? P1 C1 C2 C3 -171.5(2) . . . . ? Fe1 C1 C2 C3 59.3(2) . . . . ? C5 C1 C2 Fe1 -59.7(2) . . . . ? P1 C1 C2 Fe1 129.2(2) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? Fe1 C2 C3 C4 58.8(2) . . . . ? C1 C2 C3 Fe1 -58.7(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? Fe1 C3 C4 C5 59.2(2) . . . . ? C2 C3 C4 Fe1 -59.0(2) . . . . ? C3 C4 C5 C1 -0.4(3) . . . . ? Fe1 C4 C5 C1 59.0(2) . . . . ? C3 C4 C5 Fe1 -59.4(2) . . . . ? C2 C1 C5 C4 0.5(3) . . . . ? P1 C1 C5 C4 171.8(2) . . . . ? Fe1 C1 C5 C4 -59.5(2) . . . . ? C2 C1 C5 Fe1 59.9(2) . . . . ? P1 C1 C5 Fe1 -128.8(2) . . . . ? C10 C6 C7 C8 0.1(4) . . . . ? Fe1 C6 C7 C8 -59.3(2) . . . . ? C10 C6 C7 Fe1 59.4(2) . . . . ? C6 C7 C8 C9 -0.4(4) . . . . ? Fe1 C7 C8 C9 -60.0(2) . . . . ? C6 C7 C8 Fe1 59.7(2) . . . . ? C7 C8 C9 C10 0.5(4) . . . . ? Fe1 C8 C9 C10 -59.5(2) . . . . ? C7 C8 C9 Fe1 60.0(2) . . . . ? C7 C6 C10 C9 0.2(4) . . . . ? Fe1 C6 C10 C9 59.4(2) . . . . ? C7 C6 C10 Fe1 -59.2(2) . . . . ? C8 C9 C10 C6 -0.4(4) . . . . ? Fe1 C9 C10 C6 -59.6(2) . . . . ? C8 C9 C10 Fe1 59.2(2) . . . . ? P1 C11 C12 C13 -171.1(2) . . . . ? C11 C12 C13 C14 -176.0(3) . . . . ? P1 C15 C16 C17 165.7(2) . . . . ? C15 C16 C17 C18 174.3(3) . . . . ? P1 C19 C20 C21 172.1(3) . . . . ? C19 C20 C21 C22 -178.6(3) . . . . ? C2 C1 P1 C11 -14.5(3) . . . . ? C5 C1 P1 C11 175.8(2) . . . . ? Fe1 C1 P1 C11 81.5(3) . . . . ? C2 C1 P1 C19 104.3(3) . . . . ? C5 C1 P1 C19 -65.4(3) . . . . ? Fe1 C1 P1 C19 -159.7(2) . . . . ? C2 C1 P1 C15 -138.8(3) . . . . ? C5 C1 P1 C15 51.5(3) . . . . ? Fe1 C1 P1 C15 -42.8(3) . . . . ? C12 C11 P1 C1 -65.3(3) . . . . ? C12 C11 P1 C19 177.4(2) . . . . ? C12 C11 P1 C15 59.4(3) . . . . ? C20 C19 P1 C1 -54.3(3) . . . . ? C20 C19 P1 C11 65.9(3) . . . . ? C20 C19 P1 C15 -173.9(2) . . . . ? C16 C15 P1 C1 170.0(2) . . . . ? C16 C15 P1 C11 45.5(3) . . . . ? C16 C15 P1 C19 -73.6(3) . . . . ? S2 N1 S1 O2 -162.1(2) . . . . ? S2 N1 S1 O1 -24.9(3) . . . . ? S2 N1 S1 C23 88.7(2) . . . . ? F1 C23 S1 O2 -174.5(3) . . . . ? F3 C23 S1 O2 -54.4(3) . . . . ? F2 C23 S1 O2 65.2(3) . . . . ? F1 C23 S1 O1 60.5(3) . . . . ? F3 C23 S1 O1 -179.4(3) . . . . ? F2 C23 S1 O1 -59.8(3) . . . . ? F1 C23 S1 N1 -61.8(3) . . . . ? F3 C23 S1 N1 58.3(3) . . . . ? F2 C23 S1 N1 177.9(3) . . . . ? S1 N1 S2 O4 -156.4(2) . . . . ? S1 N1 S2 O3 -19.1(3) . . . . ? S1 N1 S2 C24 94.0(2) . . . . ? F6 C24 S2 O4 -54.1(3) . . . . ? F4 C24 S2 O4 -175.3(2) . . . . ? F5 C24 S2 O4 65.3(3) . . . . ? F6 C24 S2 O3 -179.0(2) . . . . ? F4 C24 S2 O3 59.8(3) . . . . ? F5 C24 S2 O3 -59.6(3) . . . . ? F6 C24 S2 N1 59.5(3) . . . . ? F4 C24 S2 N1 -61.8(3) . . . . ? F5 C24 S2 N1 178.9(2) . . . . ? C9 C8 Fe1 C1 -59.7(5) . . . . ? C7 C8 Fe1 C1 -179.2(3) . . . . ? C9 C8 Fe1 C4 -123.7(2) . . . . ? C7 C8 Fe1 C4 116.9(2) . . . . ? C9 C8 Fe1 C7 119.4(3) . . . . ? C9 C8 Fe1 C5 -83.6(3) . . . . ? C7 C8 Fe1 C5 156.9(2) . . . . ? C7 C8 Fe1 C9 -119.4(3) . . . . ? C9 C8 Fe1 C6 81.5(2) . . . . ? C7 C8 Fe1 C6 -37.9(2) . . . . ? C9 C8 Fe1 C10 37.8(2) . . . . ? C7 C8 Fe1 C10 -81.6(2) . . . . ? C9 C8 Fe1 C2 169.3(3) . . . . ? C7 C8 Fe1 C2 49.8(4) . . . . ? C9 C8 Fe1 C3 -164.1(2) . . . . ? C7 C8 Fe1 C3 76.4(2) . . . . ? C2 C1 Fe1 C8 -150.6(4) . . . . ? C5 C1 Fe1 C8 -31.7(5) . . . . ? P1 C1 Fe1 C8 88.0(5) . . . . ? C2 C1 Fe1 C4 -80.9(2) . . . . ? C5 C1 Fe1 C4 37.95(19) . . . . ? P1 C1 Fe1 C4 157.6(3) . . . . ? C2 C1 Fe1 C7 30.9(5) . . . . ? C5 C1 Fe1 C7 149.8(4) . . . . ? P1 C1 Fe1 C7 -90.5(4) . . . . ? C2 C1 Fe1 C5 -118.9(3) . . . . ? P1 C1 Fe1 C5 119.7(3) . . . . ? C2 C1 Fe1 C9 164.8(2) . . . . ? C5 C1 Fe1 C9 -76.3(2) . . . . ? P1 C1 Fe1 C9 43.4(3) . . . . ? C2 C1 Fe1 C6 75.8(2) . . . . ? C5 C1 Fe1 C6 -165.3(2) . . . . ? P1 C1 Fe1 C6 -45.6(3) . . . . ? C2 C1 Fe1 C10 120.2(2) . . . . ? C5 C1 Fe1 C10 -120.9(2) . . . . ? P1 C1 Fe1 C10 -1.2(3) . . . . ? C5 C1 Fe1 C2 118.9(3) . . . . ? P1 C1 Fe1 C2 -121.4(3) . . . . ? C2 C1 Fe1 C3 -37.36(19) . . . . ? C5 C1 Fe1 C3 81.5(2) . . . . ? P1 C1 Fe1 C3 -158.8(3) . . . . ? C3 C4 Fe1 C8 -118.0(2) . . . . ? C5 C4 Fe1 C8 122.3(2) . . . . ? C3 C4 Fe1 C1 81.1(2) . . . . ? C5 C4 Fe1 C1 -38.55(19) . . . . ? C3 C4 Fe1 C7 -77.4(2) . . . . ? C5 C4 Fe1 C7 162.9(2) . . . . ? C3 C4 Fe1 C5 119.7(3) . . . . ? C3 C4 Fe1 C9 -157.2(2) . . . . ? C5 C4 Fe1 C9 83.1(2) . . . . ? C3 C4 Fe1 C6 -51.5(4) . . . . ? C5 C4 Fe1 C6 -171.2(3) . . . . ? C3 C4 Fe1 C10 -179.2(4) . . . . ? C5 C4 Fe1 C10 61.1(5) . . . . ? C3 C4 Fe1 C2 36.9(2) . . . . ? C5 C4 Fe1 C2 -82.7(2) . . . . ? C5 C4 Fe1 C3 -119.7(3) . . . . ? C6 C7 Fe1 C8 -118.9(3) . . . . ? C8 C7 Fe1 C1 179.2(3) . . . . ? C6 C7 Fe1 C1 60.4(4) . . . . ? C8 C7 Fe1 C4 -77.9(2) . . . . ? C6 C7 Fe1 C4 163.3(2) . . . . ? C8 C7 Fe1 C5 -51.4(4) . . . . ? C6 C7 Fe1 C5 -170.3(3) . . . . ? C8 C7 Fe1 C9 37.4(2) . . . . ? C6 C7 Fe1 C9 -81.5(2) . . . . ? C8 C7 Fe1 C6 118.9(3) . . . . ? C8 C7 Fe1 C10 81.3(2) . . . . ? C6 C7 Fe1 C10 -37.5(2) . . . . ? C8 C7 Fe1 C2 -157.7(2) . . . . ? C6 C7 Fe1 C2 83.4(2) . . . . ? C8 C7 Fe1 C3 -118.4(2) . . . . ? C6 C7 Fe1 C3 122.7(2) . . . . ? C4 C5 Fe1 C8 -73.5(2) . . . . ? C1 C5 Fe1 C8 167.96(19) . . . . ? C4 C5 Fe1 C1 118.5(3) . . . . ? C1 C5 Fe1 C4 -118.5(3) . . . . ? C4 C5 Fe1 C7 -37.3(4) . . . . ? C1 C5 Fe1 C7 -155.8(3) . . . . ? C4 C5 Fe1 C9 -116.4(2) . . . . ? C1 C5 Fe1 C9 125.1(2) . . . . ? C4 C5 Fe1 C6 166.2(5) . . . . ? C1 C5 Fe1 C6 47.7(6) . . . . ? C4 C5 Fe1 C10 -158.2(2) . . . . ? C1 C5 Fe1 C10 83.2(2) . . . . ? C4 C5 Fe1 C2 80.6(2) . . . . ? C1 C5 Fe1 C2 -37.92(18) . . . . ? C4 C5 Fe1 C3 37.3(2) . . . . ? C1 C5 Fe1 C3 -81.26(19) . . . . ? C10 C9 Fe1 C8 119.1(3) . . . . ? C8 C9 Fe1 C1 158.3(2) . . . . ? C10 C9 Fe1 C1 -82.6(3) . . . . ? C8 C9 Fe1 C4 72.0(3) . . . . ? C10 C9 Fe1 C4 -168.8(2) . . . . ? C8 C9 Fe1 C7 -37.5(2) . . . . ? C10 C9 Fe1 C7 81.6(2) . . . . ? C8 C9 Fe1 C5 115.4(2) . . . . ? C10 C9 Fe1 C5 -125.5(2) . . . . ? C8 C9 Fe1 C6 -81.5(3) . . . . ? C10 C9 Fe1 C6 37.7(2) . . . . ? C8 C9 Fe1 C10 -119.1(3) . . . . ? C8 C9 Fe1 C2 -163.3(5) . . . . ? C10 C9 Fe1 C2 -44.1(6) . . . . ? C8 C9 Fe1 C3 35.2(5) . . . . ? C10 C9 Fe1 C3 154.3(3) . . . . ? C10 C6 Fe1 C8 -81.5(2) . . . . ? C7 C6 Fe1 C8 37.8(2) . . . . ? C10 C6 Fe1 C1 83.1(2) . . . . ? C7 C6 Fe1 C1 -157.7(2) . . . . ? C10 C6 Fe1 C4 -155.7(3) . . . . ? C7 C6 Fe1 C4 -36.5(4) . . . . ? C10 C6 Fe1 C7 -119.2(3) . . . . ? C10 C6 Fe1 C5 45.5(6) . . . . ? C7 C6 Fe1 C5 164.7(4) . . . . ? C10 C6 Fe1 C9 -37.9(2) . . . . ? C7 C6 Fe1 C9 81.3(2) . . . . ? C7 C6 Fe1 C10 119.2(3) . . . . ? C10 C6 Fe1 C2 125.3(2) . . . . ? C7 C6 Fe1 C2 -115.5(2) . . . . ? C10 C6 Fe1 C3 168.0(2) . . . . ? C7 C6 Fe1 C3 -72.8(2) . . . . ? C6 C10 Fe1 C8 81.5(2) . . . . ? C9 C10 Fe1 C8 -37.5(2) . . . . ? C6 C10 Fe1 C1 -120.1(2) . . . . ? C9 C10 Fe1 C1 120.9(2) . . . . ? C6 C10 Fe1 C4 148.3(4) . . . . ? C9 C10 Fe1 C4 29.3(5) . . . . ? C6 C10 Fe1 C7 37.7(2) . . . . ? C9 C10 Fe1 C7 -81.2(2) . . . . ? C6 C10 Fe1 C5 -165.7(2) . . . . ? C9 C10 Fe1 C5 75.3(3) . . . . ? C6 C10 Fe1 C9 119.0(3) . . . . ? C9 C10 Fe1 C6 -119.0(3) . . . . ? C6 C10 Fe1 C2 -75.0(3) . . . . ? C9 C10 Fe1 C2 166.1(2) . . . . ? C6 C10 Fe1 C3 -30.2(5) . . . . ? C9 C10 Fe1 C3 -149.2(4) . . . . ? C3 C2 Fe1 C8 37.7(4) . . . . ? C1 C2 Fe1 C8 156.9(3) . . . . ? C3 C2 Fe1 C1 -119.2(3) . . . . ? C3 C2 Fe1 C4 -37.1(2) . . . . ? C1 C2 Fe1 C4 82.2(2) . . . . ? C3 C2 Fe1 C7 72.8(2) . . . . ? C1 C2 Fe1 C7 -167.93(19) . . . . ? C3 C2 Fe1 C5 -80.9(2) . . . . ? C1 C2 Fe1 C5 38.30(19) . . . . ? C3 C2 Fe1 C9 -168.2(5) . . . . ? C1 C2 Fe1 C9 -48.9(6) . . . . ? C3 C2 Fe1 C6 115.9(2) . . . . ? C1 C2 Fe1 C6 -124.8(2) . . . . ? C3 C2 Fe1 C10 157.3(2) . . . . ? C1 C2 Fe1 C10 -83.5(2) . . . . ? C1 C2 Fe1 C3 119.2(3) . . . . ? C4 C3 Fe1 C8 77.0(2) . . . . ? C2 C3 Fe1 C8 -162.8(2) . . . . ? C4 C3 Fe1 C1 -82.2(2) . . . . ? C2 C3 Fe1 C1 38.0(2) . . . . ? C2 C3 Fe1 C4 120.2(3) . . . . ? C4 C3 Fe1 C7 117.2(2) . . . . ? C2 C3 Fe1 C7 -122.5(2) . . . . ? C4 C3 Fe1 C5 -37.6(2) . . . . ? C2 C3 Fe1 C5 82.7(2) . . . . ? C4 C3 Fe1 C9 52.0(4) . . . . ? C2 C3 Fe1 C9 172.2(3) . . . . ? C4 C3 Fe1 C6 156.9(2) . . . . ? C2 C3 Fe1 C6 -82.9(2) . . . . ? C4 C3 Fe1 C10 179.3(4) . . . . ? C2 C3 Fe1 C10 -60.5(5) . . . . ? C4 C3 Fe1 C2 -120.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.878 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 974964'