# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1853 data_1 #======================================================== # SUBMISSION DETAILS _publ_contact_author ; Dr. Mike Ward School of Chemistry Cantock's Close BRISTOL BS8 1TS ; _publ_contact_author_fax '0117 9287655' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'Reversible switching of the first hyperpolarisability of an NLO-active donor/acceptor molecule based on redox interconversion of the octamethylferrocene donor unit' by M. Malaun, et al, submitted to Chem. Commun. for publication. ; #======================================================== data_mdw _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H29 Fe N O2 S' _chemical_formula_weight 451.39 _chemical_melting_point ? _chemical_compound_source ? 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' '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 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 14.960(2) _cell_length_b 9.443(2) _cell_length_c 15.639(4) _cell_angle_alpha 90.000(13) _cell_angle_beta 102.200(14) _cell_angle_gamma 90.00(2) _cell_volume 2159.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method ? _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13766 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4931 _reflns_number_observed 3407 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+2.7000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4930 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_obs 0.0393 _refine_ls_wR_factor_all 0.1155 _refine_ls_wR_factor_obs 0.0934 _refine_ls_goodness_of_fit_all 0.794 _refine_ls_goodness_of_fit_obs 0.781 _refine_ls_restrained_S_all 0.794 _refine_ls_restrained_S_obs 0.781 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.75496(3) 0.18856(4) 0.08019(2) 0.01962(11) Uani 1 d . . S1 S 1.15024(5) 0.34281(8) 0.10972(5) 0.0345(2) Uani 1 d . . O2 O 1.3939(2) 0.4650(3) 0.2133(2) 0.0579(7) Uani 1 d . . O1 O 1.3415(2) 0.2815(3) 0.1335(2) 0.0605(8) Uani 1 d . . N1 N 1.3310(2) 0.3942(4) 0.1711(2) 0.0438(7) Uani 1 d . . C22 C 0.6536(2) -0.1118(3) 0.0647(2) 0.0385(7) Uani 1 d . . H22A H 0.6436(13) -0.1916(11) 0.1017(3) 0.058 Uiso 1 calc R . H22B H 0.6874(7) -0.1443(17) 0.0212(10) 0.058 Uiso 1 calc R . H22C H 0.5944(7) -0.0730(7) 0.0349(12) 0.058 Uiso 1 calc R . C23 C 0.8723(2) -0.0977(3) 0.1246(2) 0.0385(7) Uani 1 d . . H23A H 0.8486(8) -0.1361(18) 0.0660(6) 0.058 Uiso 1 calc R . H23B H 0.8806(12) -0.1749(13) 0.1675(9) 0.058 Uiso 1 calc R . H23C H 0.9312(5) -0.0513(7) 0.1261(15) 0.058 Uiso 1 calc R . C24 C 0.9225(2) 0.1752(3) 0.2470(2) 0.0348(7) Uani 1 d . . H24A H 0.9667(3) 0.1487(21) 0.2116(7) 0.052 Uiso 1 calc R . H24B H 0.9389(6) 0.1286(18) 0.3042(6) 0.052 Uiso 1 calc R . H24C H 0.9234(4) 0.2781(4) 0.2551(13) 0.052 Uiso 1 calc R . C21 C 0.5714(2) 0.1484(4) 0.1550(2) 0.0378(7) Uani 1 d . . H21A H 0.5638(3) 0.2486(7) 0.1683(15) 0.057 Uiso 1 calc R . H21B H 0.5492(4) 0.0895(18) 0.1977(10) 0.057 Uiso 1 calc R . H21C H 0.5363(3) 0.1272(23) 0.0961(5) 0.057 Uiso 1 calc R . C18 C 0.7077(2) 0.0011(3) 0.1206(2) 0.0279(6) Uani 1 d . . C19 C 0.8056(2) 0.0083(3) 0.1466(2) 0.0256(6) Uani 1 d . . C20 C 0.8285(2) 0.1292(3) 0.2013(2) 0.0259(6) Uani 1 d . . C16 C 0.7456(2) 0.1971(3) 0.2084(2) 0.0262(6) Uani 1 d . . H16A H 0.7405(2) 0.2854(3) 0.2423(2) 0.031 Uiso 1 calc R . C17 C 0.6706(2) 0.1178(3) 0.1595(2) 0.0262(6) Uani 1 d . . C14 C 0.6396(2) 0.1186(3) -0.1155(2) 0.0340(7) Uani 1 d . . H14A H 0.6653(7) 0.0232(7) -0.1157(11) 0.051 Uiso 1 calc R . H14B H 0.6301(11) 0.1589(13) -0.1745(3) 0.051 Uiso 1 calc R . H14C H 0.5810(5) 0.1137(18) -0.0971(8) 0.051 Uiso 1 calc R . C15 C 0.8566(2) 0.0915(3) -0.0711(2) 0.0326(7) Uani 1 d . . H15A H 0.9123(7) 0.0683(17) -0.0279(5) 0.049 Uiso 1 calc R . H15B H 0.8732(12) 0.1306(9) -0.1237(8) 0.049 Uiso 1 calc R . H15C H 0.8201(6) 0.0055(9) -0.0865(13) 0.049 Uiso 1 calc R . C12 C 0.7631(2) 0.5221(3) 0.0989(2) 0.0353(7) Uani 1 d . . H12A H 0.7766(15) 0.6065(4) 0.0673(5) 0.053 Uiso 1 calc R . H12B H 0.8106(10) 0.5101(10) 0.1521(7) 0.053 Uiso 1 calc R . H12C H 0.7035(5) 0.5333(13) 0.1146(12) 0.053 Uiso 1 calc R . C13 C 0.5843(2) 0.3832(3) -0.0123(2) 0.0357(7) Uani 1 d . . H13A H 0.5700(6) 0.4561(17) -0.0578(10) 0.054 Uiso 1 calc R . H13B H 0.5794(4) 0.4239(21) 0.0441(5) 0.054 Uiso 1 calc R . H13C H 0.5410(2) 0.3045(6) -0.0268(14) 0.054 Uiso 1 calc R . C10 C 0.7046(2) 0.2104(3) -0.0531(2) 0.0237(6) Uani 1 d . . C11 C 0.8018(2) 0.1988(3) -0.0331(2) 0.0231(5) Uani 1 d . . C7 C 0.8376(2) 0.3151(3) 0.0240(2) 0.0230(5) Uani 1 d . . C8 C 0.7612(2) 0.3940(3) 0.0414(2) 0.0245(6) Uani 1 d . . C9 C 0.6798(2) 0.3300(3) -0.0070(2) 0.0246(6) Uani 1 d . . C6 C 0.9343(2) 0.3382(3) 0.0579(2) 0.0269(6) Uani 1 d . . H6A H 0.9738(2) 0.2644(3) 0.0473(2) 0.032 Uiso 1 calc R . C5 C 0.9755(2) 0.4508(3) 0.1025(2) 0.0292(6) Uani 1 d . . H5A H 0.9375(2) 0.5256(3) 0.1146(2) 0.035 Uiso 1 calc R . C4 C 1.0729(2) 0.4665(3) 0.1333(2) 0.0281(6) Uani 1 d . . C1 C 1.2399(2) 0.4427(3) 0.1655(2) 0.0334(7) Uani 1 d . . C2 C 1.2132(2) 0.5626(4) 0.2005(2) 0.0370(7) Uani 1 d . . H2A H 1.2541(2) 0.6291(4) 0.2335(2) 0.044 Uiso 1 calc R . C3 C 1.1175(2) 0.5766(3) 0.1823(2) 0.0348(7) Uani 1 d . . H3A H 1.0867(2) 0.6542(3) 0.2018(2) 0.042 Uiso 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 0.0199(2) 0.0208(2) 0.0180(2) 0.0003(2) 0.00357(13) 0.0002(2) S1 0.0284(4) 0.0366(4) 0.0360(4) -0.0011(3) 0.0013(3) -0.0054(3) O2 0.0333(13) 0.093(2) 0.0441(15) 0.0000(14) 0.0006(11) -0.0201(14) O1 0.0384(15) 0.071(2) 0.071(2) -0.006(2) 0.0088(13) 0.0069(13) N1 0.0280(14) 0.068(2) 0.033(2) 0.0104(14) 0.0016(12) -0.0083(14) C22 0.043(2) 0.030(2) 0.040(2) 0.0058(14) 0.0028(14) -0.0107(14) C23 0.044(2) 0.031(2) 0.042(2) 0.0086(14) 0.0114(15) 0.0090(14) C24 0.0258(15) 0.047(2) 0.028(2) 0.0050(14) -0.0016(12) -0.0023(14) C21 0.024(2) 0.054(2) 0.037(2) 0.0056(15) 0.0101(13) -0.0008(14) C18 0.030(2) 0.0296(14) 0.0238(14) 0.0051(11) 0.0045(12) -0.0052(12) C19 0.0279(15) 0.0232(14) 0.0264(14) 0.0081(11) 0.0074(11) 0.0032(11) C20 0.0238(14) 0.0320(15) 0.0209(14) 0.0069(11) 0.0028(11) 0.0006(11) C16 0.0275(14) 0.0320(14) 0.0194(13) 0.0015(11) 0.0060(10) -0.0001(12) C17 0.0242(14) 0.0335(15) 0.0215(14) 0.0051(11) 0.0059(11) -0.0022(12) C14 0.032(2) 0.038(2) 0.028(2) -0.0023(13) -0.0021(12) -0.0056(13) C15 0.037(2) 0.032(2) 0.031(2) -0.0035(13) 0.0131(13) 0.0035(13) C12 0.038(2) 0.026(2) 0.044(2) -0.0069(13) 0.0142(15) 0.0013(13) C13 0.028(2) 0.043(2) 0.036(2) 0.0067(14) 0.0055(13) 0.0101(13) C10 0.0243(14) 0.0271(14) 0.0187(13) -0.0003(10) 0.0026(10) -0.0007(11) C11 0.0257(13) 0.0242(13) 0.0196(13) 0.0007(11) 0.0055(10) 0.0016(11) C7 0.0260(14) 0.0223(13) 0.0210(13) 0.0003(11) 0.0058(10) -0.0016(11) C8 0.031(2) 0.0196(13) 0.0231(13) 0.0024(11) 0.0058(11) -0.0014(11) C9 0.0228(14) 0.0262(14) 0.0244(14) 0.0034(11) 0.0041(11) 0.0034(11) C6 0.0264(14) 0.0294(15) 0.0252(14) 0.0027(11) 0.0063(11) -0.0023(11) C5 0.028(2) 0.031(2) 0.029(2) 0.0046(12) 0.0050(12) -0.0034(12) C4 0.032(2) 0.031(2) 0.0214(14) 0.0040(11) 0.0060(11) -0.0070(12) C1 0.027(2) 0.044(2) 0.027(2) 0.0071(13) 0.0020(12) -0.0109(13) C2 0.037(2) 0.041(2) 0.031(2) 0.0032(14) 0.0018(13) -0.0178(14) C3 0.039(2) 0.034(2) 0.031(2) -0.0005(13) 0.0047(13) -0.0081(14) _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 C11 2.040(3) . ? Fe1 C16 2.041(3) . ? Fe1 C8 2.041(3) . ? Fe1 C7 2.046(3) . ? Fe1 C19 2.054(3) . ? Fe1 C18 2.055(3) . ? Fe1 C17 2.060(3) . ? Fe1 C20 2.057(3) . ? Fe1 C9 2.064(3) . ? Fe1 C10 2.071(3) . ? S1 C1 1.719(3) . ? S1 C4 1.738(3) . ? O2 N1 1.228(4) . ? O1 N1 1.242(4) . ? N1 C1 1.423(4) . ? C22 C18 1.502(4) . ? C23 C19 1.504(4) . ? C24 C20 1.501(4) . ? C21 C17 1.498(4) . ? C18 C17 1.427(4) . ? C18 C19 1.437(4) . ? C19 C20 1.425(4) . ? C20 C16 1.422(4) . ? C16 C17 1.428(4) . ? C14 C10 1.499(4) . ? C15 C11 1.504(4) . ? C12 C8 1.504(4) . ? C13 C9 1.501(4) . ? C10 C9 1.430(4) . ? C10 C11 1.426(4) . ? C11 C7 1.444(4) . ? C7 C8 1.437(4) . ? C7 C6 1.449(4) . ? C8 C9 1.426(4) . ? C6 C5 1.348(4) . ? C5 C4 1.442(4) . ? C4 C3 1.377(4) . ? C1 C2 1.354(5) . ? C2 C3 1.405(4) . ? 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 C11 Fe1 C16 163.46(11) . . ? C11 Fe1 C8 69.57(11) . . ? C16 Fe1 C8 105.76(11) . . ? C11 Fe1 C7 41.40(10) . . ? C16 Fe1 C7 124.90(11) . . ? C8 Fe1 C7 41.18(11) . . ? C11 Fe1 C19 108.70(11) . . ? C16 Fe1 C19 68.33(11) . . ? C8 Fe1 C19 154.57(12) . . ? C7 Fe1 C19 120.62(11) . . ? C11 Fe1 C18 120.78(11) . . ? C16 Fe1 C18 68.41(11) . . ? C8 Fe1 C18 161.96(12) . . ? C7 Fe1 C18 156.01(11) . . ? C19 Fe1 C18 40.94(11) . . ? C11 Fe1 C17 154.85(11) . . ? C16 Fe1 C17 40.77(11) . . ? C8 Fe1 C17 124.05(11) . . ? C7 Fe1 C17 161.98(11) . . ? C19 Fe1 C17 68.55(11) . . ? C18 Fe1 C17 40.58(11) . . ? C11 Fe1 C20 126.69(11) . . ? C16 Fe1 C20 40.59(11) . . ? C8 Fe1 C20 118.91(11) . . ? C7 Fe1 C20 107.49(11) . . ? C19 Fe1 C20 40.57(11) . . ? C18 Fe1 C20 68.52(11) . . ? C17 Fe1 C20 68.50(11) . . ? C11 Fe1 C9 68.56(11) . . ? C16 Fe1 C9 118.87(11) . . ? C8 Fe1 C9 40.64(11) . . ? C7 Fe1 C9 68.43(11) . . ? C19 Fe1 C9 164.09(11) . . ? C18 Fe1 C9 125.87(11) . . ? C17 Fe1 C9 106.89(11) . . ? C20 Fe1 C9 153.56(11) . . ? C11 Fe1 C10 40.57(10) . . ? C16 Fe1 C10 153.97(11) . . ? C8 Fe1 C10 68.66(11) . . ? C7 Fe1 C10 68.54(11) . . ? C19 Fe1 C10 127.44(11) . . ? C18 Fe1 C10 108.64(11) . . ? C17 Fe1 C10 119.96(11) . . ? C20 Fe1 C10 164.52(11) . . ? C9 Fe1 C10 40.45(10) . . ? C1 S1 C4 90.4(2) . . ? O2 N1 O1 124.2(3) . . ? O2 N1 C1 118.2(3) . . ? O1 N1 C1 117.5(3) . . ? C17 C18 C19 108.0(2) . . ? C17 C18 C22 125.9(3) . . ? C19 C18 C22 126.1(3) . . ? C17 C18 Fe1 69.9(2) . . ? C19 C18 Fe1 69.5(2) . . ? C22 C18 Fe1 127.6(2) . . ? C20 C19 C18 108.0(2) . . ? C20 C19 C23 125.7(3) . . ? C18 C19 C23 126.2(3) . . ? C20 C19 Fe1 69.9(2) . . ? C18 C19 Fe1 69.6(2) . . ? C23 C19 Fe1 128.9(2) . . ? C16 C20 C19 107.8(2) . . ? C16 C20 C24 125.3(3) . . ? C19 C20 C24 126.9(3) . . ? C16 C20 Fe1 69.1(2) . . ? C19 C20 Fe1 69.6(2) . . ? C24 C20 Fe1 128.7(2) . . ? C20 C16 C17 108.8(3) . . ? C20 C16 Fe1 70.3(2) . . ? C17 C16 Fe1 70.3(2) . . ? C18 C17 C16 107.5(2) . . ? C18 C17 C21 126.8(3) . . ? C16 C17 C21 125.6(3) . . ? C18 C17 Fe1 69.5(2) . . ? C16 C17 Fe1 68.9(2) . . ? C21 C17 Fe1 129.5(2) . . ? C9 C10 C11 108.1(2) . . ? C9 C10 C14 125.7(2) . . ? C11 C10 C14 126.1(2) . . ? C9 C10 Fe1 69.50(15) . . ? C11 C10 Fe1 68.54(14) . . ? C14 C10 Fe1 130.2(2) . . ? C10 C11 C7 107.8(2) . . ? C10 C11 C15 125.6(2) . . ? C7 C11 C15 126.5(2) . . ? C10 C11 Fe1 70.89(14) . . ? C7 C11 Fe1 69.51(14) . . ? C15 C11 Fe1 128.9(2) . . ? C11 C7 C8 107.8(2) . . ? C11 C7 C6 123.5(2) . . ? C8 C7 C6 128.7(2) . . ? C11 C7 Fe1 69.09(15) . . ? C8 C7 Fe1 69.21(15) . . ? C6 C7 Fe1 125.3(2) . . ? C9 C8 C7 107.7(2) . . ? C9 C8 C12 124.4(3) . . ? C7 C8 C12 127.9(3) . . ? C9 C8 Fe1 70.57(15) . . ? C7 C8 Fe1 69.61(15) . . ? C12 C8 Fe1 125.7(2) . . ? C10 C9 C8 108.6(2) . . ? C10 C9 C13 125.6(3) . . ? C8 C9 C13 125.7(3) . . ? C10 C9 Fe1 70.05(15) . . ? C8 C9 Fe1 68.79(15) . . ? C13 C9 Fe1 129.2(2) . . ? C5 C6 C7 128.3(3) . . ? C6 C5 C4 125.0(3) . . ? C3 C4 C5 126.9(3) . . ? C3 C4 S1 111.1(2) . . ? C5 C4 S1 122.1(2) . . ? C2 C1 N1 127.2(3) . . ? C2 C1 S1 113.5(2) . . ? N1 C1 S1 119.3(3) . . ? C1 C2 C3 111.8(3) . . ? C4 C3 C2 113.3(3) . . ? _refine_diff_density_max 0.335 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.062 #=END data_goerm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H31 Cl2 F6 Fe N O2 P S' _chemical_formula_weight 681.29 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' 'Cl' 'Cl' 0.1484 0.1585 '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 10.2058(9) _cell_length_b 12.1655(11) _cell_length_c 13.0266(11) _cell_angle_alpha 73.439(2) _cell_angle_beta 68.807(2) _cell_angle_gamma 77.176(2) _cell_volume 1432.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15090 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6498 _reflns_number_gt 4586 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0532P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6498 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.17927(3) 0.25807(3) 0.27506(3) 0.01886(10) Uani 1 1 d . . . S1 S 0.34218(6) -0.17448(5) 0.61128(5) 0.02528(14) Uani 1 1 d . . . N1 N 0.3192(2) -0.36027(19) 0.7874(2) 0.0337(5) Uani 1 1 d . . . O1 O 0.3592(2) -0.41563(16) 0.71321(17) 0.0451(5) Uani 1 1 d . . . O2 O 0.2916(2) -0.40501(17) 0.88935(16) 0.0450(5) Uani 1 1 d . . . C1 C 0.3036(3) -0.2370(2) 0.7530(2) 0.0268(5) Uani 1 1 d . . . C2 C 0.2583(3) -0.1605(2) 0.8208(2) 0.0292(6) Uani 1 1 d . . . H2A H 0.2341 -0.1813 0.9008 0.035 Uiso 1 1 calc R . . C3 C 0.2519(3) -0.0466(2) 0.7565(2) 0.0293(6) Uani 1 1 d . . . H3A H 0.2220 0.0191 0.7890 0.035 Uiso 1 1 calc R . . C4 C 0.2930(2) -0.0389(2) 0.6418(2) 0.0254(5) Uani 1 1 d . . . C5 C 0.2963(3) 0.0656(2) 0.5538(2) 0.0269(5) Uani 1 1 d . . . H5A H 0.2774 0.1375 0.5749 0.032 Uiso 1 1 calc R . . C6 C 0.3240(2) 0.0677(2) 0.44491(19) 0.0236(5) Uani 1 1 d . . . H6A H 0.3364 -0.0055 0.4275 0.028 Uiso 1 1 calc R . . C7 C 0.3380(2) 0.16717(19) 0.34895(19) 0.0213(5) Uani 1 1 d . . . C8 C 0.3790(2) 0.1559(2) 0.2338(2) 0.0239(5) Uani 1 1 d . . . C9 C 0.3863(2) 0.2693(2) 0.1622(2) 0.0253(5) Uani 1 1 d . . . C10 C 0.3483(2) 0.3508(2) 0.2320(2) 0.0244(5) Uani 1 1 d . . . C11 C 0.3165(2) 0.28869(19) 0.3479(2) 0.0230(5) Uani 1 1 d . . . C12 C 0.4121(3) 0.0452(2) 0.1951(2) 0.0328(6) Uani 1 1 d . . . H12A H 0.3942 0.0601 0.1229 0.049 Uiso 1 1 calc R . . H12B H 0.3518 -0.0109 0.2517 0.049 Uiso 1 1 calc R . . H12C H 0.5119 0.0140 0.1852 0.049 Uiso 1 1 calc R . . C13 C 0.4342(3) 0.2978(2) 0.0353(2) 0.0369(7) Uani 1 1 d . . . H13A H 0.5359 0.3037 0.0061 0.055 Uiso 1 1 calc R . . H13B H 0.3819 0.3716 0.0081 0.055 Uiso 1 1 calc R . . H13C H 0.4159 0.2365 0.0090 0.055 Uiso 1 1 calc R . . C14 C 0.3448(3) 0.4796(2) 0.1900(2) 0.0351(6) Uani 1 1 d . . . H14A H 0.4370 0.5010 0.1785 0.053 Uiso 1 1 calc R . . H14B H 0.2709 0.5182 0.2459 0.053 Uiso 1 1 calc R . . H14C H 0.3243 0.5036 0.1183 0.053 Uiso 1 1 calc R . . C15 C 0.2763(3) 0.3430(2) 0.4463(2) 0.0320(6) Uani 1 1 d . . . H15A H 0.3540 0.3233 0.4784 0.048 Uiso 1 1 calc R . . H15B H 0.1908 0.3141 0.5039 0.048 Uiso 1 1 calc R . . H15C H 0.2577 0.4272 0.4212 0.048 Uiso 1 1 calc R . . C16 C 0.0201(2) 0.1686(2) 0.2907(2) 0.0244(5) Uani 1 1 d . . . H16A H 0.0302 0.0836 0.2964 0.029 Uiso 1 1 calc R . . C17 C 0.0429(2) 0.2552(2) 0.1887(2) 0.0248(5) Uani 1 1 d . . . C18 C 0.0145(2) 0.3650(2) 0.2182(2) 0.0257(5) Uani 1 1 d . . . C19 C -0.0271(2) 0.3444(2) 0.3385(2) 0.0236(5) Uani 1 1 d . . . C20 C -0.0242(2) 0.2224(2) 0.38347(19) 0.0236(5) Uani 1 1 d . . . C21 C 0.0849(3) 0.2359(3) 0.0710(2) 0.0403(7) Uani 1 1 d . . . H21A H 0.1184 0.1537 0.0723 0.061 Uiso 1 1 calc R . . H21B H 0.1610 0.2817 0.0204 0.061 Uiso 1 1 calc R . . H21C H 0.0028 0.2597 0.0439 0.061 Uiso 1 1 calc R . . C22 C 0.0197(3) 0.4816(2) 0.1390(2) 0.0381(7) Uani 1 1 d . . . H22A H -0.0720 0.5092 0.1259 0.057 Uiso 1 1 calc R . . H22B H 0.0942 0.4760 0.0670 0.057 Uiso 1 1 calc R . . H22C H 0.0404 0.5361 0.1721 0.057 Uiso 1 1 calc R . . C23 C -0.0728(3) 0.4362(2) 0.4051(2) 0.0365(6) Uani 1 1 d . . . H23A H -0.0157 0.4997 0.3644 0.055 Uiso 1 1 calc R . . H23B H -0.0596 0.4032 0.4792 0.055 Uiso 1 1 calc R . . H23C H -0.1732 0.4657 0.4153 0.055 Uiso 1 1 calc R . . C24 C -0.0619(3) 0.1641(2) 0.5068(2) 0.0339(6) Uani 1 1 d . . . H24A H -0.1653 0.1725 0.5411 0.051 Uiso 1 1 calc R . . H24B H -0.0209 0.2001 0.5445 0.051 Uiso 1 1 calc R . . H24C H -0.0242 0.0818 0.5152 0.051 Uiso 1 1 calc R . . P P 0.12838(8) 0.81947(6) 0.17073(6) 0.03103(17) Uani 1 1 d . . . F1 F 0.0870(3) 0.91628(16) 0.23961(16) 0.0861(8) Uani 1 1 d . . . F2 F 0.2774(7) 0.8583(7) 0.0922(7) 0.098(3) Uani 0.50 1 d P . . F3 F 0.2541(8) 0.7840(8) 0.2149(7) 0.102(3) Uani 0.50 1 d P . . F4 F 0.1741(2) 0.72247(15) 0.10000(15) 0.0650(6) Uani 1 1 d . . . F5 F 0.0450(9) 0.7258(5) 0.2730(5) 0.087(3) Uani 0.50 1 d P . . F6 F 0.0589(9) 0.9061(6) 0.0893(6) 0.081(2) Uani 0.50 1 d P . . F2A F 0.2091(11) 0.9080(6) 0.0662(5) 0.094(3) Uani 0.50 1 d P . . F3A F 0.2054(9) 0.7339(6) 0.2563(6) 0.080(3) Uani 0.50 1 d P . . F5A F -0.0131(7) 0.7830(6) 0.2543(6) 0.085(2) Uani 0.50 1 d P . . F6A F -0.0031(7) 0.8533(7) 0.1230(7) 0.097(3) Uani 0.50 1 d P . . C100 C 0.4671(3) 0.3088(3) 0.7368(2) 0.0439(7) Uani 1 1 d . . . H10A H 0.4476 0.3740 0.7739 0.053 Uiso 1 1 calc R . . H10B H 0.5303 0.2462 0.7700 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.30701(10) 0.25822(9) 0.76343(8) 0.0673(3) Uani 1 1 d . . . Cl2 Cl 0.55337(10) 0.35516(10) 0.59172(7) 0.0703(3) 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 Fe1 0.01714(18) 0.01999(17) 0.01958(17) -0.00230(13) -0.00716(13) -0.00331(12) S1 0.0225(3) 0.0261(3) 0.0254(3) -0.0015(2) -0.0090(3) -0.0030(2) N1 0.0270(12) 0.0303(12) 0.0397(13) 0.0056(11) -0.0145(10) -0.0069(9) O1 0.0543(14) 0.0298(10) 0.0499(13) -0.0062(10) -0.0191(11) -0.0022(9) O2 0.0449(12) 0.0388(11) 0.0381(11) 0.0131(9) -0.0120(9) -0.0101(9) C1 0.0225(13) 0.0288(13) 0.0257(13) 0.0044(10) -0.0102(10) -0.0065(10) C2 0.0233(13) 0.0374(15) 0.0251(13) 0.0012(11) -0.0106(11) -0.0067(11) C3 0.0275(14) 0.0335(14) 0.0280(13) -0.0066(11) -0.0111(11) -0.0031(11) C4 0.0220(13) 0.0266(12) 0.0292(13) -0.0039(10) -0.0119(10) -0.0032(10) C5 0.0269(13) 0.0252(13) 0.0294(13) -0.0020(10) -0.0128(11) -0.0038(10) C6 0.0218(13) 0.0216(12) 0.0298(13) -0.0032(10) -0.0133(10) -0.0022(9) C7 0.0169(12) 0.0226(12) 0.0259(12) -0.0035(10) -0.0099(10) -0.0027(9) C8 0.0175(12) 0.0249(12) 0.0292(13) -0.0047(10) -0.0081(10) -0.0031(9) C9 0.0163(12) 0.0311(13) 0.0245(12) 0.0004(10) -0.0064(10) -0.0038(10) C10 0.0182(12) 0.0232(12) 0.0306(13) 0.0004(10) -0.0096(10) -0.0057(9) C11 0.0192(12) 0.0227(12) 0.0300(13) -0.0041(10) -0.0131(10) -0.0022(9) C12 0.0352(15) 0.0289(14) 0.0343(14) -0.0103(12) -0.0117(12) 0.0010(11) C13 0.0279(15) 0.0432(16) 0.0267(14) 0.0017(12) -0.0012(11) -0.0048(12) C14 0.0335(15) 0.0220(13) 0.0487(17) 0.0041(12) -0.0181(13) -0.0087(11) C15 0.0362(15) 0.0281(13) 0.0382(15) -0.0100(12) -0.0197(12) -0.0003(11) C16 0.0193(12) 0.0256(12) 0.0305(13) -0.0064(10) -0.0076(10) -0.0075(10) C17 0.0196(12) 0.0347(14) 0.0249(12) -0.0086(11) -0.0104(10) -0.0049(10) C18 0.0203(13) 0.0304(13) 0.0264(12) -0.0006(10) -0.0117(10) -0.0037(10) C19 0.0182(12) 0.0269(12) 0.0275(13) -0.0086(10) -0.0086(10) -0.0009(9) C20 0.0174(12) 0.0298(13) 0.0234(12) -0.0015(10) -0.0073(10) -0.0069(10) C21 0.0379(17) 0.0614(19) 0.0279(14) -0.0149(14) -0.0112(12) -0.0111(14) C22 0.0365(16) 0.0353(15) 0.0408(16) 0.0072(13) -0.0218(13) -0.0060(12) C23 0.0306(15) 0.0377(15) 0.0443(16) -0.0195(13) -0.0123(13) 0.0033(12) C24 0.0290(14) 0.0421(16) 0.0237(13) 0.0019(12) -0.0061(11) -0.0074(12) P 0.0346(4) 0.0279(4) 0.0318(4) -0.0087(3) -0.0133(3) 0.0009(3) F1 0.160(2) 0.0439(11) 0.0525(12) -0.0280(10) -0.0324(14) 0.0090(13) F2 0.058(4) 0.111(7) 0.108(7) -0.052(5) 0.033(4) -0.043(4) F3 0.058(4) 0.148(8) 0.126(8) -0.039(6) -0.071(5) 0.014(4) F4 0.1101(17) 0.0391(10) 0.0513(11) -0.0172(9) -0.0335(11) 0.0020(10) F5 0.147(8) 0.062(4) 0.036(3) -0.010(3) 0.012(4) -0.057(4) F6 0.116(7) 0.065(4) 0.062(3) -0.008(3) -0.057(5) 0.032(4) F2A 0.179(10) 0.052(4) 0.040(3) 0.003(3) -0.007(5) -0.060(5) F3A 0.124(8) 0.068(4) 0.072(4) -0.044(3) -0.075(5) 0.055(4) F5A 0.052(3) 0.101(5) 0.087(4) 0.002(4) -0.003(3) -0.045(3) F6A 0.057(4) 0.151(7) 0.132(7) -0.099(6) -0.068(4) 0.045(4) C100 0.0494(19) 0.0482(18) 0.0401(17) -0.0131(14) -0.0194(15) -0.0054(14) Cl1 0.0677(6) 0.0732(6) 0.0650(6) -0.0214(5) -0.0078(5) -0.0325(5) Cl2 0.0511(5) 0.1205(9) 0.0445(5) -0.0286(5) -0.0068(4) -0.0231(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 Fe1 C16 2.070(2) . ? Fe1 C10 2.090(2) . ? Fe1 C17 2.092(2) . ? Fe1 C11 2.096(2) . ? Fe1 C9 2.101(2) . ? Fe1 C20 2.104(2) . ? Fe1 C18 2.109(2) . ? Fe1 C8 2.110(2) . ? Fe1 C19 2.115(2) . ? Fe1 C7 2.121(2) . ? S1 C1 1.718(2) . ? S1 C4 1.731(2) . ? N1 O1 1.232(3) . ? N1 O2 1.235(3) . ? N1 C1 1.428(3) . ? C1 C2 1.356(4) . ? C2 C3 1.401(3) . ? C3 C4 1.379(3) . ? C4 C5 1.446(3) . ? C5 C6 1.336(3) . ? C6 C7 1.461(3) . ? C7 C11 1.442(3) . ? C7 C8 1.443(3) . ? C8 C9 1.429(3) . ? C8 C12 1.498(3) . ? C9 C10 1.431(3) . ? C9 C13 1.502(3) . ? C10 C11 1.435(3) . ? C10 C14 1.501(3) . ? C11 C15 1.493(3) . ? C16 C17 1.420(3) . ? C16 C20 1.421(3) . ? C17 C18 1.433(3) . ? C17 C21 1.508(3) . ? C18 C19 1.429(3) . ? C18 C22 1.497(3) . ? C19 C20 1.429(3) . ? C19 C23 1.499(3) . ? C20 C24 1.502(3) . ? P F3 1.520(7) . ? P F6 1.521(5) . ? P F5A 1.529(6) . ? P F2A 1.562(6) . ? P F1 1.5742(19) . ? P F2 1.582(6) . ? P F4 1.5886(19) . ? P F5 1.595(6) . ? P F3A 1.598(7) . ? P F6A 1.604(6) . ? F2 F2A 0.913(9) . ? F2 F3 1.558(11) . ? F3 F3A 0.813(10) . ? F5 F5A 0.849(8) . ? F5 F3A 1.594(11) . ? F6 F6A 0.909(8) . ? F6 F2A 1.456(10) . ? F5A F6A 1.658(10) . ? C100 Cl2 1.753(3) . ? C100 Cl1 1.756(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Fe1 C10 170.98(9) . . ? C16 Fe1 C17 39.90(9) . . ? C10 Fe1 C17 132.33(9) . . ? C16 Fe1 C11 148.18(9) . . ? C10 Fe1 C11 40.12(9) . . ? C17 Fe1 C11 170.85(9) . . ? C16 Fe1 C9 132.87(10) . . ? C10 Fe1 C9 39.93(10) . . ? C17 Fe1 C9 109.93(9) . . ? C11 Fe1 C9 67.37(9) . . ? C16 Fe1 C20 39.78(9) . . ? C10 Fe1 C20 147.93(10) . . ? C17 Fe1 C20 66.93(9) . . ? C11 Fe1 C20 116.99(9) . . ? C9 Fe1 C20 171.54(10) . . ? C16 Fe1 C18 66.81(9) . . ? C10 Fe1 C18 110.00(9) . . ? C17 Fe1 C18 39.88(9) . . ? C11 Fe1 C18 132.50(9) . . ? C9 Fe1 C18 116.44(9) . . ? C20 Fe1 C18 66.67(9) . . ? C16 Fe1 C8 110.81(9) . . ? C10 Fe1 C8 66.95(9) . . ? C17 Fe1 C8 116.57(10) . . ? C11 Fe1 C8 67.43(9) . . ? C9 Fe1 C8 39.68(9) . . ? C20 Fe1 C8 133.68(9) . . ? C18 Fe1 C8 147.40(10) . . ? C16 Fe1 C19 66.57(9) . . ? C10 Fe1 C19 116.85(9) . . ? C17 Fe1 C19 66.68(9) . . ? C11 Fe1 C19 110.51(9) . . ? C9 Fe1 C19 147.54(9) . . ? C20 Fe1 C19 39.61(9) . . ? C18 Fe1 C19 39.54(9) . . ? C8 Fe1 C19 172.08(9) . . ? C16 Fe1 C7 117.58(9) . . ? C10 Fe1 C7 66.80(9) . . ? C17 Fe1 C7 148.09(10) . . ? C11 Fe1 C7 40.00(8) . . ? C9 Fe1 C7 66.71(9) . . ? C20 Fe1 C7 111.44(9) . . ? C18 Fe1 C7 171.42(10) . . ? C8 Fe1 C7 39.88(9) . . ? C19 Fe1 C7 133.77(9) . . ? C1 S1 C4 89.81(12) . . ? O1 N1 O2 124.0(2) . . ? O1 N1 C1 117.8(2) . . ? O2 N1 C1 118.2(2) . . ? C2 C1 N1 127.2(2) . . ? C2 C1 S1 114.48(18) . . ? N1 C1 S1 118.3(2) . . ? C1 C2 C3 110.7(2) . . ? C4 C3 C2 113.7(2) . . ? C3 C4 C5 127.1(2) . . ? C3 C4 S1 111.31(18) . . ? C5 C4 S1 121.61(19) . . ? C6 C5 C4 124.4(2) . . ? C5 C6 C7 128.8(2) . . ? C11 C7 C8 108.04(19) . . ? C11 C7 C6 129.2(2) . . ? C8 C7 C6 122.8(2) . . ? C11 C7 Fe1 69.07(12) . . ? C8 C7 Fe1 69.67(13) . . ? C6 C7 Fe1 127.08(16) . . ? C9 C8 C7 107.8(2) . . ? C9 C8 C12 125.7(2) . . ? C7 C8 C12 126.4(2) . . ? C9 C8 Fe1 69.80(13) . . ? C7 C8 Fe1 70.45(13) . . ? C12 C8 Fe1 126.47(17) . . ? C8 C9 C10 108.2(2) . . ? C8 C9 C13 125.9(2) . . ? C10 C9 C13 125.8(2) . . ? C8 C9 Fe1 70.53(13) . . ? C10 C9 Fe1 69.62(13) . . ? C13 C9 Fe1 128.29(17) . . ? C9 C10 C11 108.6(2) . . ? C9 C10 C14 125.4(2) . . ? C11 C10 C14 126.0(2) . . ? C9 C10 Fe1 70.45(13) . . ? C11 C10 Fe1 70.17(13) . . ? C14 C10 Fe1 126.01(17) . . ? C10 C11 C7 107.3(2) . . ? C10 C11 C15 124.8(2) . . ? C7 C11 C15 127.8(2) . . ? C10 C11 Fe1 69.71(13) . . ? C7 C11 Fe1 70.93(13) . . ? C15 C11 Fe1 126.97(17) . . ? C17 C16 C20 109.1(2) . . ? C17 C16 Fe1 70.88(13) . . ? C20 C16 Fe1 71.38(13) . . ? C16 C17 C18 107.5(2) . . ? C16 C17 C21 126.4(2) . . ? C18 C17 C21 126.1(2) . . ? C16 C17 Fe1 69.21(13) . . ? C18 C17 Fe1 70.71(13) . . ? C21 C17 Fe1 126.86(18) . . ? C19 C18 C17 107.8(2) . . ? C19 C18 C22 125.3(2) . . ? C17 C18 C22 126.8(2) . . ? C19 C18 Fe1 70.45(13) . . ? C17 C18 Fe1 69.41(13) . . ? C22 C18 Fe1 127.83(17) . . ? C18 C19 C20 108.2(2) . . ? C18 C19 C23 125.3(2) . . ? C20 C19 C23 126.4(2) . . ? C18 C19 Fe1 70.02(13) . . ? C20 C19 Fe1 69.77(13) . . ? C23 C19 Fe1 128.31(17) . . ? C16 C20 C19 107.4(2) . . ? C16 C20 C24 127.2(2) . . ? C19 C20 C24 125.3(2) . . ? C16 C20 Fe1 68.83(13) . . ? C19 C20 Fe1 70.63(13) . . ? C24 C20 Fe1 125.90(17) . . ? F3 P F6 147.2(4) . . ? F3 P F5A 116.1(4) . . ? F6 P F5A 93.2(4) . . ? F3 P F2A 91.9(5) . . ? F6 P F2A 56.3(4) . . ? F5A P F2A 148.4(4) . . ? F3 P F1 83.9(4) . . ? F6 P F1 86.4(3) . . ? F5A P F1 81.7(3) . . ? F2A P F1 87.5(3) . . ? F3 P F2 60.3(4) . . ? F6 P F2 89.6(4) . . ? F5A P F2 175.6(4) . . ? F2A P F2 33.7(3) . . ? F1 P F2 95.2(3) . . ? F3 P F4 95.0(4) . . ? F6 P F4 93.9(3) . . ? F5A P F4 99.6(3) . . ? F2A P F4 91.5(3) . . ? F1 P F4 178.57(14) . . ? F2 P F4 83.4(3) . . ? F3 P F5 89.6(4) . . ? F6 P F5 122.5(4) . . ? F5A P F5 31.4(3) . . ? F2A P F5 177.0(4) . . ? F1 P F5 95.2(2) . . ? F2 P F5 146.8(4) . . ? F4 P F5 85.8(2) . . ? F3 P F3A 30.1(4) . . ? F6 P F3A 176.9(4) . . ? F5A P F3A 88.6(4) . . ? F2A P F3A 121.4(5) . . ? F1 P F3A 91.4(2) . . ? F2 P F3A 88.4(4) . . ? F4 P F3A 88.2(2) . . ? F5 P F3A 59.9(4) . . ? F3 P F6A 178.3(4) . . ? F6 P F6A 33.7(3) . . ? F5A P F6A 63.8(4) . . ? F2A P F6A 88.6(4) . . ? F1 P F6A 97.8(3) . . ? F2 P F6A 119.8(4) . . ? F4 P F6A 83.3(3) . . ? F5 P F6A 89.8(4) . . ? F3A P F6A 149.1(4) . . ? F2A F2 F3 125.4(9) . . ? F2A F2 P 71.9(7) . . ? F3 F2 P 57.9(4) . . ? F3A F3 P 80.3(9) . . ? F3A F3 F2 136.1(12) . . ? P F3 F2 61.8(4) . . ? F5A F5 F3A 124.0(9) . . ? F5A F5 P 70.0(6) . . ? F3A F5 P 60.2(3) . . ? F6A F6 F2A 137.1(9) . . ? F6A F6 P 78.1(7) . . ? F2A F6 P 63.2(3) . . ? F2 F2A F6 133.7(9) . . ? F2 F2A P 74.3(6) . . ? F6 F2A P 60.4(3) . . ? F3 F3A F5 128.7(11) . . ? F3 F3A P 69.6(9) . . ? F5 F3A P 60.0(3) . . ? F5 F5A P 78.5(7) . . ? F5 F5A F6A 125.4(10) . . ? P F5A F6A 60.3(3) . . ? F6 F6A P 68.2(6) . . ? F6 F6A F5A 116.4(8) . . ? P F6A F5A 55.9(3) . . ? Cl2 C100 Cl1 111.98(16) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.136 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.064 #=END