data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad # syn absolute configuration from synthetic procedure # ad absolute configuration from anomalous dispersion effects # rm absolute configuration from reference to a chiral # reference molecule of known abs. conf. # Hooft, R. W. W., Straver, L. H. and Spek, A. L. (2008). J. Appl. Cryst., # 41, 96-103. Determination of absolute structure using Bayesian # statistics on Bijvoet differences. _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 3 C14 H14 N2 O, Fe 2+, 2 C F3 S O3 1-, 1/2 C4 H8 O, 1/2 C2 H3 N ; _chemical_formula_sum 'C47 H50 F6 Fe N6.50 O9.50 S2' _chemical_formula_weight 1091.91 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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 30.495(2) _cell_length_b 12.5164(9) _cell_length_c 13.3325(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5088.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4781 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2262 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 1.12 _exptl_absorpt_process_details ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8743 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8743 _reflns_number_gt 5440 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Flack H D (1983), Acta Cryst. A39, 876-881. Hooft, R. W. W., Straver, L. H. and Spek, A. L. (2008). J. Appl. Cryst., 41, 96-103. Determination of absolute structure using Bayesian statistics on Bijvoet differences. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. The absolute configuration was determined by the method of Flack, (Flack, 1983) and corroborated by use of the Hooft y-parameter, (Hooft, Straver and Spek, 2008). The Hooft y-parameter refined to 0.01(1). The X-ray determination was consistent with the known configuration of the starting material. The triflate anions were all disordered. One anion was located on a general position. The other anion was located around two different two-fold rotation axes. In addition, one anion was disordered along with a molecule of acetonitrile. A molecule of diethyl ether was also disordered near a crystallographic two-fold rotation axes. The contribution to the scattering factors by the diethyl ether molecule was removed by use of the utility, SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). One triflate ion, composed of atoms with labels appended by C, was located near a crystallographic two-fold rotation axis at 1/2, 0, z. The atoms of this anion were assigned a site occupancy factor of 1/2. A second triflate ion, composed of atoms appended by A, was located near a crystallographic two-fold rotation axis at 1/2, 1/2, z. A molecule of acetontrile was located in the vicinity of this anion with the nitrogen atom, N3e, residing close to O1a of the triflate anion. The triflate anion found in a general position was also disordered. The disorder for this anion was modeled by assigning the variable x to the site occupancy factor of one component of the disorder and (1-x) to the site occupancy factor of the atoms of the other component. A common isotropic displacement parameter was refined for the oxygen and fluorine atoms of the two groups while refining x. In addition, a second isotropic displacement parameter was refined for the carbon and sulfur atoms while refining x. The geometry of the two components was restrained to be equivalent throughout the refinement process. In this way, the site occupancy factor for the major component composed of atoms, S1b, C1b, F1b, F2b, F3b, O1b, O2b and O3b, refined to 64(2)%. Throughout the refinement procedure the geometry of the triflate anions was restrained to be equivalent. The anisotropic displacement parameters were restrained to be approximately isotropic. No hydrogen atoms were included for the acetonitrile molecule. ; _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^)+(0.0458P)^2^+4.4916P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 8743 _refine_ls_number_parameters 790 _refine_ls_number_restraints 1050 _refine_ls_R_factor_all 0.1689 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 1.373 _refine_ls_restrained_S_all 1.340 _refine_ls_shift/su_max 0.004 _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 0.31422(3) 0.16491(7) 0.74899(8) 0.0260(2) Uani 1 1 d U . . O1 O 0.16279(16) 0.1159(4) 0.9089(3) 0.0399(13) Uani 1 1 d U . . H1O H 0.1778 0.1455 0.9538 0.060 Uiso 1 1 calc R . . O2 O 0.32808(16) 0.1136(4) 0.3626(3) 0.0407(14) Uani 1 1 d U . . H2O H 0.3500 0.1333 0.3293 0.061 Uiso 1 1 calc R . . O3 O 0.45336(18) 0.1068(5) 0.9532(4) 0.0624(18) Uani 1 1 d U . . H3O H 0.4646 0.0813 1.0055 0.094 Uiso 1 1 calc R . . N1 N 0.25998(16) 0.0802(4) 0.7578(4) 0.0214(12) Uani 1 1 d U . . N2 N 0.28464(19) 0.2445(4) 0.8578(4) 0.0242(14) Uani 1 1 d U . . N3 N 0.28805(19) 0.2483(5) 0.6389(4) 0.0290(15) Uani 1 1 d U . . N4 N 0.33901(17) 0.0835(4) 0.6352(4) 0.0240(14) Uani 1 1 d U . . N5 N 0.34579(19) 0.0761(5) 0.8474(4) 0.0280(15) Uani 1 1 d U . . N6 N 0.36812(16) 0.2496(4) 0.7559(5) 0.0287(13) Uani 1 1 d U . . C1 C 0.2485(2) -0.0062(6) 0.7044(5) 0.0299(18) Uani 1 1 d U . . H1 H 0.2686 -0.0350 0.6571 0.036 Uiso 1 1 calc R . . C2 C 0.2077(2) -0.0547(6) 0.7168(5) 0.035(2) Uani 1 1 d U . . H2 H 0.2004 -0.1155 0.6776 0.042 Uiso 1 1 calc R . . C3 C 0.1783(2) -0.0161(6) 0.7839(5) 0.0331(19) Uani 1 1 d U . . H3 H 0.1505 -0.0492 0.7917 0.040 Uiso 1 1 calc R . . C4 C 0.1895(2) 0.0720(6) 0.8406(5) 0.0305(18) Uani 1 1 d U . . C5 C 0.2303(2) 0.1172(5) 0.8247(5) 0.0250(17) Uani 1 1 d U . . C6 C 0.2469(2) 0.2095(5) 0.8791(5) 0.0293(18) Uani 1 1 d U . . H6 H 0.2297 0.2428 0.9296 0.035 Uiso 1 1 calc R . . C7 C 0.3036(2) 0.3366(6) 0.9183(5) 0.0336(18) Uani 1 1 d U . . H7 H 0.3221 0.3813 0.8728 0.040 Uiso 1 1 calc R . . C8 C 0.3327(2) 0.2899(6) 0.9986(5) 0.0350(19) Uani 1 1 d U . . C9 C 0.3210(3) 0.2039(6) 1.0577(5) 0.042(2) Uani 1 1 d U . . H9 H 0.2934 0.1703 1.0474 0.051 Uiso 1 1 calc R . . C10 C 0.3484(3) 0.1663(7) 1.1309(6) 0.050(2) Uani 1 1 d U . . H10 H 0.3390 0.1077 1.1708 0.060 Uiso 1 1 calc R . . C11 C 0.3875(3) 0.2084(7) 1.1482(6) 0.050(2) Uani 1 1 d U . . H11 H 0.4061 0.1785 1.1980 0.059 Uiso 1 1 calc R . . C12 C 0.4007(3) 0.2943(8) 1.0945(7) 0.058(3) Uani 1 1 d U . . H12 H 0.4282 0.3269 1.1075 0.069 Uiso 1 1 calc R . . C13 C 0.3732(3) 0.3340(7) 1.0201(6) 0.047(2) Uani 1 1 d U . . H13 H 0.3827 0.3940 0.9824 0.056 Uiso 1 1 calc R . . C14 C 0.2686(2) 0.4086(6) 0.9660(5) 0.038(2) Uani 1 1 d U . . H14A H 0.2469 0.4286 0.9152 0.056 Uiso 1 1 calc R . . H14B H 0.2825 0.4732 0.9927 0.056 Uiso 1 1 calc R . . H14C H 0.2541 0.3700 1.0206 0.056 Uiso 1 1 calc R . . C15 C 0.3681(2) 0.0037(6) 0.6360(6) 0.0338(18) Uani 1 1 d U . . H15 H 0.3776 -0.0241 0.6986 0.041 Uiso 1 1 calc R . . C16 C 0.3850(3) -0.0402(6) 0.5479(6) 0.040(2) Uani 1 1 d U . . H16 H 0.4061 -0.0959 0.5520 0.048 Uiso 1 1 calc R . . C17 C 0.3723(2) -0.0056(6) 0.4588(6) 0.0347(19) Uani 1 1 d U . . H17 H 0.3838 -0.0360 0.3990 0.042 Uiso 1 1 calc R . . C18 C 0.3416(2) 0.0763(6) 0.4549(5) 0.0316(18) Uani 1 1 d U . . C19 C 0.32637(19) 0.1215(5) 0.5437(5) 0.0227(16) Uani 1 1 d U . . C20 C 0.2972(2) 0.2120(6) 0.5517(6) 0.0340(19) Uani 1 1 d U . . H20 H 0.2851 0.2440 0.4933 0.041 Uiso 1 1 calc R . . C21 C 0.2573(2) 0.3382(6) 0.6469(5) 0.041(2) Uani 1 1 d U . . H21 H 0.2661 0.3808 0.7070 0.049 Uiso 1 1 calc R . . C22 C 0.2107(3) 0.3007(6) 0.6641(5) 0.040(2) Uani 1 1 d U . . C23 C 0.1923(3) 0.2242(6) 0.6036(6) 0.045(2) Uani 1 1 d U . . H23 H 0.2094 0.1918 0.5525 0.054 Uiso 1 1 calc R . . C24 C 0.1491(3) 0.1940(8) 0.6160(7) 0.061(3) Uani 1 1 d U . . H24 H 0.1373 0.1394 0.5747 0.073 Uiso 1 1 calc R . . C25 C 0.1226(3) 0.2422(7) 0.6882(7) 0.057(2) Uani 1 1 d U . . H25 H 0.0927 0.2226 0.6954 0.069 Uiso 1 1 calc R . . C26 C 0.1414(3) 0.3201(7) 0.7493(7) 0.061(2) Uani 1 1 d U . . H26 H 0.1241 0.3535 0.7997 0.074 Uiso 1 1 calc R . . C27 C 0.1857(3) 0.3502(6) 0.7377(6) 0.047(2) Uani 1 1 d U . . H27 H 0.1982 0.4036 0.7795 0.056 Uiso 1 1 calc R . . C28 C 0.2587(3) 0.4128(6) 0.5572(5) 0.047(2) Uani 1 1 d U . . H28A H 0.2893 0.4290 0.5405 0.070 Uiso 1 1 calc R . . H28B H 0.2432 0.4792 0.5735 0.070 Uiso 1 1 calc R . . H28C H 0.2445 0.3784 0.4997 0.070 Uiso 1 1 calc R . . C29 C 0.3333(3) -0.0150(6) 0.8893(5) 0.037(2) Uani 1 1 d U . . H29 H 0.3049 -0.0419 0.8747 0.044 Uiso 1 1 calc R . . C30 C 0.3607(3) -0.0735(7) 0.9551(6) 0.053(2) Uani 1 1 d U . . H30 H 0.3512 -0.1400 0.9819 0.063 Uiso 1 1 calc R . . C31 C 0.4007(3) -0.0332(8) 0.9793(6) 0.054(3) Uani 1 1 d U . . H31 H 0.4190 -0.0701 1.0252 0.065 Uiso 1 1 calc R . . C32 C 0.4144(3) 0.0610(7) 0.9371(6) 0.041(2) Uani 1 1 d U . . C33 C 0.3866(2) 0.1146(6) 0.8688(5) 0.0320(18) Uani 1 1 d U . . C34 C 0.3967(2) 0.2117(6) 0.8179(6) 0.038(2) Uani 1 1 d U . . H34 H 0.4237 0.2476 0.8293 0.045 Uiso 1 1 calc R . . C35 C 0.3775(3) 0.3483(6) 0.6971(5) 0.040(2) Uani 1 1 d U . . H35 H 0.3495 0.3886 0.6876 0.048 Uiso 1 1 calc R . . C36 C 0.3957(2) 0.3198(6) 0.5955(6) 0.039(2) Uani 1 1 d U . . C37 C 0.4253(2) 0.2375(6) 0.5791(6) 0.044(2) Uani 1 1 d U . . H37 H 0.4340 0.1937 0.6338 0.053 Uiso 1 1 calc R . . C38 C 0.4427(3) 0.2177(7) 0.4835(7) 0.057(3) Uani 1 1 d U . . H38 H 0.4625 0.1602 0.4734 0.068 Uiso 1 1 calc R . . C39 C 0.4310(3) 0.2808(9) 0.4059(7) 0.068(3) Uani 1 1 d U . . H39 H 0.4429 0.2679 0.3411 0.081 Uiso 1 1 calc R . . C40 C 0.4017(3) 0.3650(8) 0.4201(7) 0.063(3) Uani 1 1 d U . . H40 H 0.3938 0.4093 0.3652 0.075 Uiso 1 1 calc R . . C41 C 0.3840(3) 0.3843(7) 0.5147(6) 0.047(2) Uani 1 1 d U . . H41 H 0.3639 0.4414 0.5240 0.057 Uiso 1 1 calc R . . C42 C 0.4112(3) 0.4226(6) 0.7513(7) 0.066(3) Uani 1 1 d U . . H42A H 0.4019 0.4339 0.8208 0.098 Uiso 1 1 calc R . . H42B H 0.4126 0.4915 0.7165 0.098 Uiso 1 1 calc R . . H42C H 0.4402 0.3890 0.7505 0.098 Uiso 1 1 calc R . . S1B S 0.27306(9) 0.6800(2) 0.7553(3) 0.0396(7) Uani 0.64 1 d PDU A 1 F1B F 0.3343(3) 0.6017(8) 0.6424(7) 0.060(4) Uani 0.64 1 d PDU A 1 F2B F 0.3560(3) 0.6484(10) 0.7890(7) 0.087(5) Uani 0.64 1 d PDU A 1 F3B F 0.3428(3) 0.7671(6) 0.6774(7) 0.080(3) Uani 0.64 1 d PDU A 1 O1B O 0.2497(4) 0.7074(11) 0.6645(8) 0.045(5) Uani 0.64 1 d PDU A 1 O2B O 0.2738(3) 0.7638(9) 0.8291(8) 0.041(4) Uani 0.64 1 d PDU A 1 O3B O 0.2645(4) 0.5749(6) 0.7934(9) 0.055(4) Uani 0.64 1 d PDU A 1 C1B C 0.3285(3) 0.6732(7) 0.7144(7) 0.068(4) Uani 0.64 1 d PDU A 1 S1BA S 0.2879(2) 0.6299(5) 0.6915(5) 0.0445(16) Uani 0.36 1 d PDU B 2 F1BA F 0.3333(5) 0.8012(12) 0.7330(13) 0.068(5) Uani 0.36 1 d PDU B 2 F2BA F 0.3469(6) 0.6673(17) 0.8303(13) 0.063(6) Uani 0.36 1 d PDU B 2 F3BA F 0.2882(6) 0.7541(18) 0.8511(14) 0.050(6) Uani 0.36 1 d PDU B 2 O1BA O 0.2709(8) 0.5515(12) 0.7601(14) 0.044(6) Uani 0.36 1 d PDU B 2 O2BA O 0.3201(6) 0.5911(17) 0.6221(14) 0.059(8) Uani 0.36 1 d PDU B 2 O3BA O 0.2556(7) 0.700(2) 0.6485(16) 0.044(9) Uani 0.36 1 d PDU B 2 C1BA C 0.3145(5) 0.7160(11) 0.7791(10) 0.058(6) Uani 0.36 1 d PDU B 2 S1A S 0.45209(12) 0.6549(3) 1.0892(3) 0.0432(10) Uani 0.50 1 d PDU C -1 F1A F 0.4458(3) 0.6091(8) 0.8999(5) 0.088(3) Uani 0.50 1 d PDU C -1 F2A F 0.5071(3) 0.6762(8) 0.9409(6) 0.086(3) Uani 0.50 1 d PDU C -1 F3A F 0.4925(4) 0.5143(8) 0.9807(6) 0.104(4) Uani 0.50 1 d PDU C -1 O1A O 0.4192(4) 0.5741(10) 1.1083(10) 0.050(6) Uani 0.50 1 d PDU C -1 O2A O 0.4883(3) 0.6536(7) 1.1576(6) 0.053(3) Uani 0.50 1 d PDU C -1 O3A O 0.4346(3) 0.7585(6) 1.0669(7) 0.061(3) Uani 0.50 1 d PDU C -1 C1A C 0.4753(3) 0.6127(8) 0.9738(7) 0.083(5) Uani 0.50 1 d PDU C -1 S1C S 0.51298(12) 0.0641(3) 1.1949(3) 0.0395(10) Uani 0.50 1 d PDU . . F1C F 0.4861(2) -0.0069(8) 1.3680(4) 0.057(3) Uani 0.50 1 d PDU . . F2C F 0.4891(3) -0.1257(5) 1.2535(7) 0.070(3) Uani 0.50 1 d PDU . . F3C F 0.4377(2) -0.0094(8) 1.2522(8) 0.069(3) Uani 0.50 1 d PDU . . O1C O 0.4958(3) 0.1676(5) 1.2228(7) 0.057(3) Uani 0.50 1 d PDU . . O2C O 0.5570(2) 0.0440(9) 1.2255(8) 0.050(3) Uani 0.50 1 d PDU . . O3C O 0.5026(4) 0.0318(6) 1.0940(4) 0.039(3) Uani 0.50 1 d PDU . . C1C C 0.4807(3) -0.0238(7) 1.2695(6) 0.061(3) Uani 0.50 1 d PDU . . N1E N 0.4240(7) 0.5677(16) 1.1419(19) 0.047(6) Uani 0.50 1 d PU D 2 C2E C 0.4538(7) 0.5666(15) 1.1891(15) 0.057(5) Uani 0.50 1 d PU D 2 C3E C 0.4897(5) 0.5725(13) 1.2516(15) 0.057(4) Uani 0.50 1 d PU . 2 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 0.0329(5) 0.0244(5) 0.0208(5) -0.0001(6) 0.0009(6) 0.0023(4) O1 0.050(3) 0.044(3) 0.026(3) -0.006(3) 0.007(3) 0.002(3) O2 0.051(3) 0.050(3) 0.021(3) 0.001(3) 0.007(3) -0.003(3) O3 0.041(4) 0.098(5) 0.048(4) -0.016(3) -0.018(3) 0.004(3) N1 0.033(3) 0.016(3) 0.015(3) 0.001(3) 0.001(3) 0.004(2) N2 0.028(3) 0.025(3) 0.020(3) -0.005(3) 0.005(3) 0.004(3) N3 0.041(4) 0.032(4) 0.014(3) -0.004(3) 0.011(3) 0.006(3) N4 0.024(3) 0.026(4) 0.022(3) 0.005(3) 0.003(3) 0.004(3) N5 0.038(4) 0.028(4) 0.018(3) -0.002(3) 0.008(3) -0.006(3) N6 0.028(3) 0.024(3) 0.033(3) -0.001(3) 0.000(3) 0.000(2) C1 0.037(4) 0.025(4) 0.028(4) 0.011(3) 0.004(3) 0.009(3) C2 0.035(4) 0.037(4) 0.034(5) -0.008(3) -0.004(4) -0.006(4) C3 0.034(4) 0.038(4) 0.028(4) 0.004(3) -0.005(3) -0.009(3) C4 0.031(4) 0.042(4) 0.018(4) 0.005(3) 0.005(3) -0.002(4) C5 0.024(4) 0.031(4) 0.020(4) 0.003(3) 0.002(3) 0.006(3) C6 0.033(4) 0.031(4) 0.024(4) 0.002(3) 0.006(3) 0.005(3) C7 0.042(4) 0.030(4) 0.029(4) -0.004(4) -0.001(3) -0.003(4) C8 0.034(4) 0.047(5) 0.024(4) -0.013(4) 0.008(3) 0.001(4) C9 0.056(5) 0.050(5) 0.022(4) -0.004(4) 0.004(4) -0.001(4) C10 0.056(5) 0.064(5) 0.031(4) -0.005(4) -0.004(4) 0.010(5) C11 0.051(5) 0.068(6) 0.030(4) -0.013(4) -0.013(4) 0.010(4) C12 0.051(5) 0.072(6) 0.050(5) -0.026(5) -0.015(5) 0.003(5) C13 0.041(4) 0.056(5) 0.044(5) -0.022(4) 0.005(4) 0.007(4) C14 0.054(5) 0.029(5) 0.030(4) -0.023(4) 0.006(4) 0.005(4) C15 0.037(4) 0.036(4) 0.028(4) -0.002(4) -0.003(4) 0.000(4) C16 0.043(5) 0.033(5) 0.044(5) -0.013(4) 0.009(4) 0.009(4) C17 0.040(4) 0.040(4) 0.024(4) -0.005(4) 0.000(4) 0.006(4) C18 0.038(4) 0.035(4) 0.022(4) 0.004(4) -0.002(4) -0.007(4) C19 0.016(4) 0.027(4) 0.025(4) -0.002(3) 0.004(3) -0.002(3) C20 0.038(4) 0.037(4) 0.027(4) 0.006(4) 0.001(3) 0.001(4) C21 0.052(5) 0.035(4) 0.035(4) 0.011(4) 0.004(4) 0.015(4) C22 0.057(5) 0.043(5) 0.019(4) 0.010(4) 0.007(4) 0.019(4) C23 0.045(5) 0.050(5) 0.041(5) 0.009(4) 0.008(4) 0.018(4) C24 0.060(5) 0.066(6) 0.058(5) 0.013(5) -0.002(5) 0.008(5) C25 0.051(5) 0.074(6) 0.048(5) 0.027(5) 0.004(4) 0.014(5) C26 0.065(5) 0.079(5) 0.039(4) 0.009(5) 0.014(5) 0.034(4) C27 0.053(4) 0.056(5) 0.032(4) 0.010(4) -0.002(4) 0.023(4) C28 0.075(6) 0.032(5) 0.034(5) 0.011(4) 0.018(4) 0.020(4) C29 0.047(4) 0.038(5) 0.026(4) 0.004(4) -0.001(4) 0.006(4) C30 0.078(6) 0.046(5) 0.035(5) 0.012(4) 0.004(5) 0.010(5) C31 0.044(5) 0.069(6) 0.049(5) 0.002(5) -0.005(4) 0.025(5) C32 0.039(5) 0.056(5) 0.027(4) -0.014(4) -0.006(4) 0.017(4) C33 0.035(4) 0.039(4) 0.022(4) -0.004(4) 0.000(3) 0.000(4) C34 0.029(4) 0.043(5) 0.040(4) -0.020(4) 0.001(4) 0.005(4) C35 0.053(5) 0.025(4) 0.042(4) -0.005(4) 0.018(4) -0.008(4) C36 0.044(4) 0.030(4) 0.044(5) -0.011(4) 0.008(4) -0.021(4) C37 0.050(5) 0.034(5) 0.049(5) 0.003(4) 0.023(4) -0.008(4) C38 0.056(5) 0.056(5) 0.058(5) -0.010(5) 0.020(5) -0.010(4) C39 0.067(6) 0.085(6) 0.051(5) -0.032(5) 0.004(5) -0.014(5) C40 0.045(5) 0.086(6) 0.056(6) 0.006(5) -0.011(4) -0.014(5) C41 0.045(5) 0.055(5) 0.042(5) -0.003(4) 0.009(4) -0.001(4) C42 0.093(6) 0.050(5) 0.054(5) -0.010(6) 0.018(6) -0.041(5) S1B 0.0415(18) 0.0383(19) 0.0390(19) 0.005(2) -0.0017(19) -0.0067(14) F1B 0.066(6) 0.057(6) 0.057(6) -0.042(5) 0.013(6) -0.003(5) F2B 0.073(7) 0.110(9) 0.078(9) -0.026(7) -0.014(6) 0.029(6) F3B 0.093(7) 0.057(6) 0.091(8) -0.006(6) 0.030(6) -0.033(5) O1B 0.051(8) 0.042(8) 0.043(8) 0.006(6) -0.012(7) -0.011(6) O2B 0.049(8) 0.039(6) 0.035(7) -0.017(5) -0.008(6) 0.006(6) O3B 0.079(8) 0.041(7) 0.045(8) 0.009(6) 0.011(6) -0.017(6) C1B 0.073(8) 0.064(7) 0.067(8) -0.015(7) -0.001(7) -0.004(7) S1BA 0.051(4) 0.042(4) 0.040(3) -0.006(3) 0.003(3) 0.007(3) F1BA 0.076(9) 0.059(9) 0.070(10) 0.007(9) -0.006(9) -0.027(7) F2BA 0.054(9) 0.080(11) 0.055(10) -0.027(9) -0.032(8) 0.020(8) F3BA 0.048(10) 0.057(10) 0.045(10) -0.021(8) -0.015(9) 0.007(8) O1BA 0.069(11) 0.029(9) 0.033(11) -0.006(9) 0.003(10) -0.011(8) O2BA 0.076(14) 0.047(12) 0.054(12) -0.017(9) -0.014(11) 0.010(10) O3BA 0.047(13) 0.051(15) 0.035(12) 0.003(10) -0.004(10) 0.017(11) C1BA 0.053(9) 0.058(9) 0.063(10) 0.004(8) -0.003(8) -0.005(8) S1A 0.042(2) 0.043(3) 0.044(2) 0.006(2) 0.008(2) -0.001(2) F1A 0.081(7) 0.130(8) 0.052(6) -0.029(6) -0.017(6) 0.004(6) F2A 0.084(7) 0.095(7) 0.080(7) -0.013(6) 0.038(6) -0.027(6) F3A 0.114(10) 0.105(8) 0.093(6) -0.022(9) 0.039(8) 0.025(7) O1A 0.045(9) 0.055(9) 0.050(10) 0.005(7) 0.000(7) 0.001(7) O2A 0.042(6) 0.058(7) 0.058(7) 0.002(6) -0.014(5) -0.014(6) O3A 0.060(7) 0.041(7) 0.084(8) 0.021(6) 0.004(6) 0.015(6) C1A 0.084(8) 0.090(8) 0.075(8) -0.011(7) 0.013(7) 0.000(7) S1C 0.035(2) 0.048(3) 0.036(2) -0.010(2) 0.002(2) 0.000(2) F1C 0.066(7) 0.064(5) 0.040(4) -0.005(5) 0.016(4) 0.005(6) F2C 0.085(6) 0.060(5) 0.064(5) -0.007(5) 0.018(5) 0.003(5) F3C 0.067(5) 0.065(6) 0.074(6) -0.001(6) 0.007(5) -0.010(5) O1C 0.059(6) 0.055(6) 0.056(6) -0.015(5) 0.001(5) 0.004(5) O2C 0.038(5) 0.064(6) 0.049(6) 0.005(5) -0.003(5) -0.002(5) O3C 0.040(5) 0.048(7) 0.030(4) 0.001(4) -0.004(5) 0.007(6) C1C 0.066(6) 0.057(5) 0.058(5) -0.007(5) 0.006(5) 0.000(5) N1E 0.044(11) 0.040(10) 0.057(12) -0.013(8) 0.007(9) 0.001(9) C2E 0.056(8) 0.055(8) 0.059(9) -0.003(7) -0.005(8) 0.001(7) C3E 0.052(7) 0.066(8) 0.054(8) -0.006(8) -0.002(8) 0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.958(5) . ? Fe1 N1 1.968(5) . ? Fe1 N3 1.970(6) . ? Fe1 N5 1.971(6) . ? Fe1 N2 1.978(5) . ? Fe1 N4 1.978(6) . ? O1 C4 1.339(8) . ? O1 H1O 0.8400 . ? O2 C18 1.380(8) . ? O2 H2O 0.8400 . ? O3 C32 1.336(9) . ? O3 H3O 0.8400 . ? N1 C1 1.341(8) . ? N1 C5 1.352(8) . ? N2 C6 1.264(8) . ? N2 C7 1.522(9) . ? N3 C20 1.279(8) . ? N3 C21 1.469(9) . ? N4 C15 1.336(8) . ? N4 C19 1.365(8) . ? N5 C29 1.326(9) . ? N5 C33 1.365(9) . ? N6 C34 1.292(9) . ? N6 C35 1.490(9) . ? C1 C2 1.394(9) . ? C1 H1 0.9500 . ? C2 C3 1.355(9) . ? C2 H2 0.9500 . ? C3 C4 1.380(9) . ? C3 H3 0.9500 . ? C4 C5 1.385(9) . ? C5 C6 1.455(9) . ? C6 H6 0.9500 . ? C7 C8 1.509(10) . ? C7 C14 1.534(9) . ? C7 H7 1.0000 . ? C8 C13 1.382(10) . ? C8 C9 1.381(10) . ? C9 C10 1.369(10) . ? C9 H9 0.9500 . ? C10 C11 1.322(10) . ? C10 H10 0.9500 . ? C11 C12 1.353(11) . ? C11 H11 0.9500 . ? C12 C13 1.391(11) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.395(10) . ? C15 H15 0.9500 . ? C16 C17 1.323(9) . ? C16 H16 0.9500 . ? C17 C18 1.388(10) . ? C17 H17 0.9500 . ? C18 C19 1.392(9) . ? C19 C20 1.443(9) . ? C20 H20 0.9500 . ? C21 C28 1.517(9) . ? C21 C22 1.515(10) . ? C21 H21 1.0000 . ? C22 C23 1.372(10) . ? C22 C27 1.388(10) . ? C23 C24 1.379(11) . ? C23 H23 0.9500 . ? C24 C25 1.394(11) . ? C24 H24 0.9500 . ? C25 C26 1.394(12) . ? C25 H25 0.9500 . ? C26 C27 1.413(11) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.416(10) . ? C29 H29 0.9500 . ? C30 C31 1.359(11) . ? C30 H30 0.9500 . ? C31 C32 1.372(12) . ? C31 H31 0.9500 . ? C32 C33 1.415(10) . ? C33 C34 1.426(10) . ? C34 H34 0.9500 . ? C35 C36 1.507(10) . ? C35 C42 1.562(10) . ? C35 H35 1.0000 . ? C36 C37 1.387(10) . ? C36 C41 1.394(11) . ? C37 C38 1.402(10) . ? C37 H37 0.9500 . ? C38 C39 1.350(12) . ? C38 H38 0.9500 . ? C39 C40 1.394(12) . ? C39 H39 0.9500 . ? C40 C41 1.393(11) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? S1B O3B 1.434(6) . ? S1B O2B 1.438(6) . ? S1B O1B 1.446(6) . ? S1B C1B 1.778(9) . ? F1B C1B 1.325(8) . ? F2B C1B 1.338(8) . ? F3B C1B 1.347(8) . ? S1BA O2BA 1.433(7) . ? S1BA O1BA 1.439(7) . ? S1BA O3BA 1.441(7) . ? S1BA C1BA 1.783(10) . ? F1BA C1BA 1.358(9) . ? F2BA C1BA 1.347(10) . ? F3BA C1BA 1.338(10) . ? S1A O2A 1.432(6) . ? S1A O3A 1.434(6) . ? S1A O1A 1.447(7) . ? S1A C1A 1.775(9) . ? F1A C1A 1.335(8) . ? F2A C1A 1.328(8) . ? F3A C1A 1.343(8) . ? S1C O2C 1.424(6) . ? S1C O3C 1.440(6) . ? S1C O1C 1.446(6) . ? S1C C1C 1.779(9) . ? F1C C1C 1.340(8) . ? F2C C1C 1.318(8) . ? F3C C1C 1.344(8) . ? N1E C2E 1.11(3) . ? C2E C3E 1.38(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 N6 Fe1 N1 173.9(3) . . ? N6 Fe1 N3 95.1(2) . . ? N1 Fe1 N3 89.4(2) . . ? N6 Fe1 N5 82.2(2) . . ? N1 Fe1 N5 93.8(2) . . ? N3 Fe1 N5 173.1(2) . . ? N6 Fe1 N2 94.4(2) . . ? N1 Fe1 N2 81.0(2) . . ? N3 Fe1 N2 95.5(2) . . ? N5 Fe1 N2 91.1(2) . . ? N6 Fe1 N4 89.6(2) . . ? N1 Fe1 N4 95.1(2) . . ? N3 Fe1 N4 81.7(2) . . ? N5 Fe1 N4 91.9(2) . . ? N2 Fe1 N4 175.3(2) . . ? C4 O1 H1O 109.5 . . ? C18 O2 H2O 109.5 . . ? C32 O3 H3O 109.5 . . ? C1 N1 C5 116.9(6) . . ? C1 N1 Fe1 128.5(5) . . ? C5 N1 Fe1 114.6(4) . . ? C6 N2 C7 119.3(6) . . ? C6 N2 Fe1 114.0(5) . . ? C7 N2 Fe1 126.7(4) . . ? C20 N3 C21 118.5(6) . . ? C20 N3 Fe1 113.6(5) . . ? C21 N3 Fe1 127.6(4) . . ? C15 N4 C19 117.1(6) . . ? C15 N4 Fe1 129.3(5) . . ? C19 N4 Fe1 113.5(4) . . ? C29 N5 C33 118.6(6) . . ? C29 N5 Fe1 128.7(5) . . ? C33 N5 Fe1 112.7(5) . . ? C34 N6 C35 120.7(6) . . ? C34 N6 Fe1 113.4(5) . . ? C35 N6 Fe1 125.9(5) . . ? N1 C1 C2 121.4(6) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 120.9(7) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 118.9(7) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? O1 C4 C3 123.4(6) . . ? O1 C4 C5 118.9(6) . . ? C3 C4 C5 117.6(6) . . ? N1 C5 C4 124.3(6) . . ? N1 C5 C6 111.7(6) . . ? C4 C5 C6 124.0(6) . . ? N2 C6 C5 118.6(6) . . ? N2 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 N2 107.8(6) . . ? C8 C7 C14 110.0(6) . . ? N2 C7 C14 113.6(5) . . ? C8 C7 H7 108.4 . . ? N2 C7 H7 108.4 . . ? C14 C7 H7 108.4 . . ? C13 C8 C9 115.1(8) . . ? C13 C8 C7 121.2(7) . . ? C9 C8 C7 123.7(7) . . ? C10 C9 C8 121.1(8) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 122.6(9) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 C11 C12 119.5(8) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 118.8(8) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C8 C13 C12 123.0(9) . . ? C8 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 C16 122.3(7) . . ? N4 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C17 C16 C15 121.2(7) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 118.3(7) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? O2 C18 C17 119.0(6) . . ? O2 C18 C19 121.4(6) . . ? C17 C18 C19 119.6(6) . . ? N4 C19 C18 121.6(6) . . ? N4 C19 C20 112.4(6) . . ? C18 C19 C20 126.0(6) . . ? N3 C20 C19 118.7(7) . . ? N3 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N3 C21 C28 113.4(6) . . ? N3 C21 C22 111.9(6) . . ? C28 C21 C22 109.7(6) . . ? N3 C21 H21 107.2 . . ? C28 C21 H21 107.2 . . ? C22 C21 H21 107.2 . . ? C23 C22 C27 120.2(8) . . ? C23 C22 C21 120.8(7) . . ? C27 C22 C21 118.9(8) . . ? C22 C23 C24 120.7(8) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 121.2(9) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C26 117.9(9) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? C25 C26 C27 121.0(8) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.0(8) . . ? C22 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C21 C28 H28A 109.5 . . ? C21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 C30 122.4(7) . . ? N5 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C31 C30 C29 119.0(8) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 119.8(8) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? O3 C32 C31 125.1(8) . . ? O3 C32 C33 115.7(8) . . ? C31 C32 C33 119.2(8) . . ? N5 C33 C32 121.0(7) . . ? N5 C33 C34 113.5(7) . . ? C32 C33 C34 125.5(7) . . ? N6 C34 C33 118.2(7) . . ? N6 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? N6 C35 C36 110.3(6) . . ? N6 C35 C42 112.2(6) . . ? C36 C35 C42 108.3(6) . . ? N6 C35 H35 108.7 . . ? C36 C35 H35 108.7 . . ? C42 C35 H35 108.7 . . ? C37 C36 C41 118.4(7) . . ? C37 C36 C35 123.9(7) . . ? C41 C36 C35 117.6(7) . . ? C36 C37 C38 121.4(8) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C39 C38 C37 119.6(9) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 120.4(9) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 120.3(9) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C36 120.0(8) . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? C35 C42 H42A 109.5 . . ? C35 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C35 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3B S1B O2B 115.5(5) . . ? O3B S1B O1B 115.1(5) . . ? O2B S1B O1B 114.0(5) . . ? O3B S1B C1B 103.8(5) . . ? O2B S1B C1B 103.2(4) . . ? O1B S1B C1B 102.9(5) . . ? F1B C1B F2B 107.3(7) . . ? F1B C1B F3B 106.3(7) . . ? F2B C1B F3B 105.8(7) . . ? F1B C1B S1B 112.5(6) . . ? F2B C1B S1B 112.3(6) . . ? F3B C1B S1B 112.2(6) . . ? O2BA S1BA O1BA 115.2(7) . . ? O2BA S1BA O3BA 114.7(7) . . ? O1BA S1BA O3BA 115.0(7) . . ? O2BA S1BA C1BA 108.5(12) . . ? O1BA S1BA C1BA 99.2(10) . . ? O3BA S1BA C1BA 101.7(13) . . ? F3BA C1BA F2BA 103.7(15) . . ? F3BA C1BA F1BA 107.4(17) . . ? F2BA C1BA F1BA 106.0(16) . . ? F3BA C1BA S1BA 114.4(12) . . ? F2BA C1BA S1BA 113.0(11) . . ? F1BA C1BA S1BA 111.7(11) . . ? O2A S1A O3A 115.5(5) . . ? O2A S1A O1A 114.5(5) . . ? O3A S1A O1A 114.2(5) . . ? O2A S1A C1A 104.0(4) . . ? O3A S1A C1A 103.7(4) . . ? O1A S1A C1A 102.8(5) . . ? F2A C1A F1A 105.7(7) . . ? F2A C1A F3A 106.7(7) . . ? F1A C1A F3A 106.5(7) . . ? F2A C1A S1A 113.6(6) . . ? F1A C1A S1A 112.3(6) . . ? F3A C1A S1A 111.7(6) . . ? O2C S1C O3C 115.1(5) . . ? O2C S1C O1C 115.3(5) . . ? O3C S1C O1C 114.3(5) . . ? O2C S1C C1C 104.5(4) . . ? O3C S1C C1C 103.1(4) . . ? O1C S1C C1C 102.1(4) . . ? F2C C1C F1C 106.7(7) . . ? F2C C1C F3C 106.9(7) . . ? F1C C1C F3C 105.5(7) . . ? F2C C1C S1C 113.6(6) . . ? F1C C1C S1C 112.5(6) . . ? F3C C1C S1C 111.1(6) . . ? N1E C2E C3E 175(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.703 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.091 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.013 0.361 302 60 ' ' 2 0.500 -0.028 0.639 302 60 ' '