# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2013 ####################################################################### # # 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_vollhardt10 _database_code_depnum_ccdc_archive 'CCDC 924375' #TrackingRef 'Compound3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; vollhardt10 ; _chemical_name_common FvFe _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H8 Fe2 O4' _chemical_formula_weight 351.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 12.6185(16) _cell_length_b 6.6178(8) _cell_length_c 15.4350(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.150(7) _cell_angle_gamma 90.00 _cell_volume 1202.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.35 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7599 _exptl_absorpt_correction_T_max 0.9094 _exptl_absorpt_process_details SADABS _diffrn_refln_scan_width 1.0 _diffrn_refln_scan_rate 10 _space_group.centring_type primitive _space_group.IT_number 14 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 17939 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.04 _reflns_number_total 2306 _reflns_number_gt 1506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0186P)^2^+1.6575P] 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 2306 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.2424(4) 0.4159(7) 0.0096(3) 0.0180(11) Uani 1 1 d . . . C2 C 0.1564(4) 0.3915(6) 0.0492(3) 0.0201(11) Uani 1 1 d . . . H2 H 0.0771 0.3781 0.0155 0.024 Uiso 1 1 calc R . . C3 C 0.2098(4) 0.3907(7) 0.1470(3) 0.0228(11) Uani 1 1 d . . . H3 H 0.1726 0.3788 0.1904 0.027 Uiso 1 1 calc R . . C4 C 0.3284(4) 0.4107(7) 0.1689(3) 0.0216(11) Uani 1 1 d . . . H4 H 0.3846 0.4152 0.2296 0.026 Uiso 1 1 calc R . . C5 C 0.3487(4) 0.4231(7) 0.0840(3) 0.0219(11) Uani 1 1 d . . . H5 H 0.4209 0.4342 0.0783 0.026 Uiso 1 1 calc R . . C6 C 0.2281(4) 0.3630(7) -0.0864(3) 0.0174(10) Uani 1 1 d . . . C7 C 0.3169(4) 0.3027(6) -0.1166(3) 0.0172(10) Uani 1 1 d . . . H7 H 0.3957 0.3271 -0.0849 0.021 Uiso 1 1 calc R . . C8 C 0.2674(4) 0.1993(6) -0.2028(3) 0.0207(11) Uani 1 1 d . . . H8 H 0.3075 0.1429 -0.2386 0.025 Uiso 1 1 calc R . . C9 C 0.1482(4) 0.1950(6) -0.2259(3) 0.0195(11) Uani 1 1 d . . . H9 H 0.0944 0.1349 -0.2797 0.023 Uiso 1 1 calc R . . C10 C 0.1228(4) 0.2967(6) -0.1541(3) 0.0187(11) Uani 1 1 d . . . H10 H 0.0494 0.3166 -0.1517 0.022 Uiso 1 1 calc R . . C11 C 0.3850(4) -0.0141(7) 0.1310(3) 0.0201(11) Uani 1 1 d . . . C12 C 0.1690(4) -0.0372(7) 0.0915(2) 0.0173(11) Uani 1 1 d . . . C13 C 0.3407(4) -0.1244(7) -0.0631(3) 0.0176(10) Uani 1 1 d . . . C14 C 0.1230(4) -0.1290(7) -0.1046(3) 0.0210(11) Uani 1 1 d . . . O1 O 0.4629(3) -0.1169(5) 0.16432(19) 0.0277(8) Uani 1 1 d . . . O2 O 0.1041(3) -0.1531(5) 0.09785(19) 0.0269(8) Uani 1 1 d . . . O3 O 0.4152(3) -0.2386(5) -0.04532(18) 0.0239(8) Uani 1 1 d . . . O4 O 0.0504(3) -0.2442(5) -0.11568(19) 0.0257(8) Uani 1 1 d . . . Fe1 Fe 0.26668(5) 0.14848(10) 0.08545(4) 0.01767(18) Uani 1 1 d . . . Fe2 Fe 0.22896(5) 0.05122(9) -0.09602(4) 0.01708(18) 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 0.019(3) 0.019(3) 0.019(2) 0.0018(18) 0.010(2) 0.004(2) C2 0.022(3) 0.019(3) 0.023(2) -0.0020(19) 0.013(2) 0.001(2) C3 0.030(3) 0.021(3) 0.023(2) -0.001(2) 0.015(2) -0.002(2) C4 0.028(3) 0.021(3) 0.018(2) -0.0043(19) 0.010(2) 0.001(2) C5 0.025(3) 0.020(3) 0.022(2) -0.003(2) 0.010(2) -0.008(2) C6 0.020(2) 0.019(3) 0.016(2) 0.0055(19) 0.0098(19) 0.000(2) C7 0.017(3) 0.016(3) 0.018(2) 0.0073(18) 0.0062(19) 0.002(2) C8 0.029(3) 0.021(3) 0.015(2) 0.0045(19) 0.011(2) 0.002(2) C9 0.022(3) 0.022(3) 0.013(2) -0.0002(18) 0.0044(19) 0.000(2) C10 0.019(3) 0.022(3) 0.017(2) 0.0088(19) 0.008(2) 0.003(2) C11 0.022(3) 0.027(3) 0.017(2) -0.002(2) 0.014(2) -0.009(2) C12 0.018(3) 0.024(3) 0.012(2) -0.0013(19) 0.0073(19) 0.009(2) C13 0.029(3) 0.015(3) 0.013(2) -0.0015(19) 0.012(2) -0.010(2) C14 0.027(3) 0.022(3) 0.014(2) 0.001(2) 0.007(2) 0.007(2) O1 0.024(2) 0.033(2) 0.0255(17) 0.0027(15) 0.0074(15) 0.0055(17) O2 0.032(2) 0.027(2) 0.0286(17) -0.0016(15) 0.0193(16) -0.0022(17) O3 0.024(2) 0.025(2) 0.0238(16) 0.0011(14) 0.0095(15) 0.0038(17) O4 0.026(2) 0.023(2) 0.0305(17) -0.0030(15) 0.0141(15) -0.0038(17) Fe1 0.0209(4) 0.0194(4) 0.0157(3) 0.0003(3) 0.0102(3) 0.0011(3) Fe2 0.0196(4) 0.0181(4) 0.0162(3) 0.0010(3) 0.0098(3) 0.0005(3) _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 C1 C5 1.416(6) . ? C1 C2 1.435(5) . ? C1 C6 1.469(5) . ? C1 Fe1 2.083(4) . ? C2 C3 1.413(5) . ? C2 Fe1 2.067(4) . ? C2 H2 0.9500 . ? C3 C4 1.416(6) . ? C3 Fe1 2.116(4) . ? C3 H3 0.9500 . ? C4 C5 1.426(5) . ? C4 Fe1 2.134(4) . ? C4 H4 0.9500 . ? C5 Fe1 2.095(4) . ? C5 H5 0.9500 . ? C6 C7 1.418(5) . ? C6 C10 1.431(6) . ? C6 Fe2 2.069(4) . ? C7 C8 1.424(5) . ? C7 Fe2 2.088(4) . ? C7 H7 0.9500 . ? C8 C9 1.415(6) . ? C8 Fe2 2.118(4) . ? C8 H8 0.9500 . ? C9 C10 1.428(5) . ? C9 Fe2 2.118(4) . ? C9 H9 0.9500 . ? C10 Fe2 2.090(4) . ? C10 H10 0.9500 . ? C11 O1 1.153(5) . ? C11 Fe1 1.767(5) . ? C12 O2 1.152(5) . ? C12 Fe1 1.766(5) . ? C13 O3 1.160(5) . ? C13 Fe2 1.755(5) . ? C14 O4 1.156(5) . ? C14 Fe2 1.761(5) . ? Fe1 Fe2 2.7431(8) . ? 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 107.4(3) . . ? C5 C1 C6 124.2(4) . . ? C2 C1 C6 124.5(4) . . ? C5 C1 Fe1 70.7(2) . . ? C2 C1 Fe1 69.2(2) . . ? C6 C1 Fe1 107.7(3) . . ? C3 C2 C1 108.2(4) . . ? C3 C2 Fe1 72.1(2) . . ? C1 C2 Fe1 70.3(2) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe1 C2 H2 123.3 . . ? C2 C3 C4 108.1(3) . . ? C2 C3 Fe1 68.4(2) . . ? C4 C3 Fe1 71.2(3) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Fe1 C3 H3 126.0 . . ? C3 C4 C5 108.1(4) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 Fe1 68.8(2) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 126.9 . . ? C1 C5 C4 108.2(4) . . ? C1 C5 Fe1 69.7(3) . . ? C4 C5 Fe1 71.8(2) . . ? C1 C5 H5 125.9 . . ? C4 C5 H5 125.9 . . ? Fe1 C5 H5 124.2 . . ? C7 C6 C10 108.0(4) . . ? C7 C6 C1 125.1(4) . . ? C10 C6 C1 123.7(4) . . ? C7 C6 Fe2 70.8(2) . . ? C10 C6 Fe2 70.7(2) . . ? C1 C6 Fe2 108.0(3) . . ? C6 C7 C8 108.1(4) . . ? C6 C7 Fe2 69.4(2) . . ? C8 C7 Fe2 71.4(2) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? Fe2 C7 H7 124.9 . . ? C9 C8 C7 108.2(4) . . ? C9 C8 Fe2 70.5(2) . . ? C7 C8 Fe2 69.0(2) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Fe2 C8 H8 126.2 . . ? C8 C9 C10 108.1(4) . . ? C8 C9 Fe2 70.5(2) . . ? C10 C9 Fe2 69.1(2) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe2 C9 H9 126.0 . . ? C9 C10 C6 107.6(4) . . ? C9 C10 Fe2 71.2(2) . . ? C6 C10 Fe2 69.1(2) . . ? C9 C10 H10 126.2 . . ? C6 C10 H10 126.2 . . ? Fe2 C10 H10 125.1 . . ? O1 C11 Fe1 177.2(4) . . ? O2 C12 Fe1 177.1(4) . . ? O3 C13 Fe2 176.7(3) . . ? O4 C14 Fe2 176.0(4) . . ? C12 Fe1 C11 93.5(2) . . ? C12 Fe1 C2 98.09(18) . . ? C11 Fe1 C2 166.11(19) . . ? C12 Fe1 C1 131.07(18) . . ? C11 Fe1 C1 132.27(18) . . ? C2 Fe1 C1 40.46(15) . . ? C12 Fe1 C5 163.84(18) . . ? C11 Fe1 C5 100.53(19) . . ? C2 Fe1 C5 67.01(18) . . ? C1 Fe1 C5 39.63(16) . . ? C12 Fe1 C3 98.46(18) . . ? C11 Fe1 C3 131.08(17) . . ? C2 Fe1 C3 39.46(15) . . ? C1 Fe1 C3 66.65(15) . . ? C5 Fe1 C3 66.21(16) . . ? C12 Fe1 C4 130.04(16) . . ? C11 Fe1 C4 100.54(19) . . ? C2 Fe1 C4 66.05(17) . . ? C1 Fe1 C4 66.16(16) . . ? C5 Fe1 C4 39.40(14) . . ? C3 Fe1 C4 38.92(16) . . ? C12 Fe1 Fe2 91.33(12) . . ? C11 Fe1 Fe2 94.25(12) . . ? C2 Fe1 Fe2 93.12(11) . . ? C1 Fe1 Fe2 71.90(11) . . ? C5 Fe1 Fe2 95.56(10) . . ? C3 Fe1 Fe2 132.37(12) . . ? C4 Fe1 Fe2 134.30(11) . . ? C13 Fe2 C14 94.7(2) . . ? C13 Fe2 C6 131.63(19) . . ? C14 Fe2 C6 131.09(19) . . ? C13 Fe2 C7 99.02(18) . . ? C14 Fe2 C7 163.66(18) . . ? C6 Fe2 C7 39.89(15) . . ? C13 Fe2 C10 164.24(17) . . ? C14 Fe2 C10 98.18(19) . . ? C6 Fe2 C10 40.24(16) . . ? C7 Fe2 C10 66.96(16) . . ? C13 Fe2 C9 129.32(16) . . ? C14 Fe2 C9 98.03(18) . . ? C6 Fe2 C9 66.85(16) . . ? C7 Fe2 C9 66.33(16) . . ? C10 Fe2 C9 39.65(15) . . ? C13 Fe2 C8 98.42(17) . . ? C14 Fe2 C8 129.44(17) . . ? C6 Fe2 C8 66.63(15) . . ? C7 Fe2 C8 39.58(15) . . ? C10 Fe2 C8 66.30(16) . . ? C9 Fe2 C8 39.03(15) . . ? C13 Fe2 Fe1 91.96(12) . . ? C14 Fe2 Fe1 94.78(12) . . ? C6 Fe2 Fe1 72.30(10) . . ? C7 Fe2 Fe1 93.58(11) . . ? C10 Fe2 Fe1 95.96(10) . . ? C9 Fe2 Fe1 135.05(12) . . ? C8 Fe2 Fe1 132.98(12) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.489 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.116 _iucr_refine_instructions_details ; TITL vollhardt10_0m in P2(1)/n CELL 0.71073 12.6185 6.6178 15.4350 90.000 111.150 90.000 ZERR 4.00 0.0016 0.0008 0.0019 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O FE UNIT 56 32 16 8 MERG 2 FMAP 2 PLAN 25 SIZE 0.04 0.12 0.06 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.018600 1.657500 FVAR 0.12198 C1 1 0.242446 0.415942 0.009615 11.00000 0.01891 0.01852 = 0.01934 0.00180 0.01023 0.00397 C2 1 0.156355 0.391456 0.049224 11.00000 0.02160 0.01921 = 0.02340 -0.00204 0.01287 0.00125 AFIX 43 H2 2 0.077128 0.378067 0.015547 11.00000 -1.20000 AFIX 0 C3 1 0.209779 0.390702 0.146963 11.00000 0.02998 0.02080 = 0.02263 -0.00139 0.01549 -0.00235 AFIX 43 H3 2 0.172607 0.378818 0.190395 11.00000 -1.20000 AFIX 0 C4 1 0.328366 0.410739 0.168933 11.00000 0.02753 0.02080 = 0.01769 -0.00429 0.00971 0.00149 AFIX 43 H4 2 0.384572 0.415177 0.229649 11.00000 -1.20000 AFIX 0 C5 1 0.348665 0.423090 0.083989 11.00000 0.02480 0.02032 = 0.02153 -0.00309 0.00964 -0.00778 AFIX 43 H5 2 0.420920 0.434190 0.078275 11.00000 -1.20000 AFIX 0 C6 1 0.228077 0.363026 -0.086388 11.00000 0.01988 0.01876 = 0.01636 0.00548 0.00981 -0.00022 C7 1 0.316904 0.302744 -0.116621 11.00000 0.01665 0.01635 = 0.01848 0.00725 0.00623 0.00151 AFIX 43 H7 2 0.395681 0.327113 -0.084937 11.00000 -1.20000 AFIX 0 C8 1 0.267377 0.199275 -0.202790 11.00000 0.02854 0.02090 = 0.01507 0.00449 0.01064 0.00230 AFIX 43 H8 2 0.307450 0.142851 -0.238608 11.00000 -1.20000 AFIX 0 C9 1 0.148203 0.194985 -0.225868 11.00000 0.02206 0.02237 = 0.01260 -0.00025 0.00443 0.00032 AFIX 43 H9 2 0.094447 0.134907 -0.279736 11.00000 -1.20000 AFIX 0 C10 1 0.122819 0.296661 -0.154107 11.00000 0.01859 0.02188 = 0.01696 0.00884 0.00817 0.00332 AFIX 43 H10 2 0.049358 0.316640 -0.151741 11.00000 -1.20000 AFIX 0 C11 1 0.385007 -0.014054 0.131034 11.00000 0.02169 0.02670 = 0.01746 -0.00203 0.01373 -0.00860 C12 1 0.169020 -0.037160 0.091471 11.00000 0.01822 0.02369 = 0.01151 -0.00133 0.00733 0.00860 C13 1 0.340682 -0.124445 -0.063072 11.00000 0.02858 0.01522 = 0.01299 -0.00152 0.01249 -0.00994 C14 1 0.122989 -0.128972 -0.104645 11.00000 0.02682 0.02169 = 0.01442 0.00051 0.00721 0.00744 O1 3 0.462934 -0.116907 0.164319 11.00000 0.02382 0.03266 = 0.02554 0.00266 0.00743 0.00550 O2 3 0.104081 -0.153050 0.097850 11.00000 0.03198 0.02702 = 0.02856 -0.00161 0.01930 -0.00220 O3 3 0.415233 -0.238601 -0.045321 11.00000 0.02387 0.02476 = 0.02378 0.00113 0.00953 0.00384 O4 3 0.050414 -0.244239 -0.115680 11.00000 0.02648 0.02336 = 0.03049 -0.00298 0.01413 -0.00375 FE1 4 0.266682 0.148485 0.085451 11.00000 0.02088 0.01941 = 0.01574 0.00033 0.01024 0.00111 FE2 4 0.228959 0.051222 -0.096025 11.00000 0.01965 0.01814 = 0.01622 0.00097 0.00981 0.00047 HKLF 4 REM vollhardt10_0m in P2(1)/n REM R1 = 0.0405 for 1506 Fo > 4sig(Fo) and 0.0875 for all 2306 data REM 181 parameters refined using 0 restraints END WGHT 0.0183 1.6696 REM Highest difference peak 0.489, deepest hole -0.468, 1-sigma level 0.116 Q1 1 0.2374 0.6385 -0.0887 11.00000 0.05 0.49 Q2 1 0.2644 -0.0440 0.0911 11.00000 0.05 0.47 Q3 1 0.4202 0.5251 -0.0395 11.00000 0.05 0.46 Q4 1 0.3048 0.4030 -0.2445 11.00000 0.05 0.45 Q5 1 0.2763 0.2187 -0.2933 11.00000 0.05 0.43 Q6 1 0.4425 0.0021 0.1784 11.00000 0.05 0.43 Q7 1 0.2189 0.2385 -0.0981 11.00000 0.05 0.41 Q8 1 0.1264 -0.3589 0.0956 11.00000 0.05 0.40 Q9 1 0.1800 0.3572 -0.1410 11.00000 0.05 0.40 Q10 1 0.3165 0.3061 0.1004 11.00000 0.05 0.39 Q11 1 0.3421 0.1495 -0.3185 11.00000 0.05 0.39 Q12 1 0.2227 0.3610 -0.2778 11.00000 0.05 0.38 Q13 1 0.0537 -0.0043 -0.1791 11.00000 0.05 0.38 Q14 1 0.1659 0.3714 0.1008 11.00000 0.05 0.38 Q15 1 -0.0407 -0.0689 -0.1508 11.00000 0.05 0.37 Q16 1 0.4420 0.4543 0.2964 11.00000 0.05 0.37 Q17 1 0.4211 -0.2007 0.1951 11.00000 0.05 0.37 Q18 1 0.3391 -0.1252 0.1770 11.00000 0.05 0.37 Q19 1 0.2733 -0.2505 0.1002 11.00000 0.05 0.36 Q20 1 0.2017 0.0932 -0.0238 11.00000 0.05 0.36 Q21 1 0.2357 0.3018 0.0239 11.00000 0.05 0.35 Q22 1 0.4812 -0.3541 0.2186 11.00000 0.05 0.35 Q23 1 -0.0611 -0.2573 -0.1759 11.00000 0.05 0.34 Q24 1 0.0823 -0.4134 -0.0862 11.00000 0.05 0.34 Q25 1 0.1454 0.1871 0.1594 11.00000 0.05 0.34 ;