# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Elizabeth Hillard' _publ_contact_author_email ELIZABETHHILLARD@YAHOO.COM _publ_section_title ; Synthesis, oxidation chemistry and cytotoxicity studies on ferrocene derivatives of diethylstilbestrol ; loop_ _publ_author_name 'Elizabeth Hillard' 'Gerard Jaouen' 'Michael McGlinchey' 'Helge Muller-Bunz' 'Pascal Pigeon' ; M.-A.Plamont ; 'Yong Leng Kelvin Tan' 'Siden Top' 'Anne Vessieres' # Attachment 'B913570G.cif' data_mjm305(2a) _database_code_depnum_ccdc_archive 'CCDC 738753' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Fe' _chemical_formula_sum 'C26 H24 Fe' _chemical_formula_weight 392.30 _chemical_absolute_configuration ad 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.6189(6) _cell_length_b 15.2824(11) _cell_length_c 16.6026(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1933.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5656 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 31.72 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6015 _exptl_absorpt_correction_T_max 0.7981 _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) for selected reflections was 0.082 before and 0.028 after correction. The Ratio of minimum to maximum transmission is 0.753651. The \l/2 correction factor is 0.0015 ; _exptl_special_details ; All hydrogen atoms were located in the unit cell and allowed to refine freely. C-H bond distances vary from 0.90(2) \%A to 1.02(2) \%A. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23546 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 32.00 _reflns_number_total 6259 _reflns_number_gt 5952 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0514P)^2^+0.2126P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _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 -0.006(10) _refine_ls_number_reflns 6259 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Fe Fe 0.23776(2) 1.075102(12) 0.094576(11) 0.01370(5) Uani 1 1 d . . . C1 C 0.50289(19) 1.09275(10) 0.09231(10) 0.0220(3) Uani 1 1 d . . . H1 H 0.584(3) 1.0453(15) 0.0799(13) 0.032(6) Uiso 1 1 d . . . C2 C 0.4206(2) 1.14918(11) 0.03568(10) 0.0241(3) Uani 1 1 d . . . H2 H 0.445(3) 1.1475(12) -0.0199(13) 0.022(5) Uiso 1 1 d . . . C3 C 0.3007(2) 1.20427(10) 0.07799(10) 0.0241(3) Uani 1 1 d . . . H3 H 0.232(3) 1.2474(15) 0.0516(13) 0.031(5) Uiso 1 1 d . . . C4 C 0.3098(2) 1.18177(10) 0.16154(10) 0.0223(3) Uani 1 1 d . . . H4 H 0.242(3) 1.2056(13) 0.2025(12) 0.020(4) Uiso 1 1 d . . . C5 C 0.4350(2) 1.11288(10) 0.17040(9) 0.0204(3) Uani 1 1 d . . . H5 H 0.467(3) 1.0848(12) 0.2161(12) 0.021(5) Uiso 1 1 d . . . C6 C 0.19599(19) 0.94648(9) 0.06761(9) 0.0176(3) Uani 1 1 d . . . H6 H 0.288(3) 0.9071(13) 0.0546(11) 0.020(5) Uiso 1 1 d . . . C7 C 0.1127(2) 1.00131(10) 0.00966(8) 0.0188(3) Uani 1 1 d . . . H7 H 0.140(3) 1.0022(13) -0.0494(13) 0.030(5) Uiso 1 1 d . . . C8 C -0.00974(19) 1.05556(9) 0.05048(9) 0.0176(3) Uani 1 1 d . . . H8 H -0.081(3) 1.1010(13) 0.0280(13) 0.024(5) Uiso 1 1 d . . . C9 C -0.00337(19) 1.03434(9) 0.13390(9) 0.0171(2) Uani 1 1 d . . . H9 H -0.069(2) 1.0615(12) 0.1745(11) 0.015(4) Uiso 1 1 d . . . C10 C 0.12481(19) 0.96647(9) 0.14576(8) 0.0159(2) Uani 1 1 d . . . C11 C 0.16369(18) 0.93013(9) 0.22667(8) 0.0162(2) Uani 1 1 d . . . C12 C 0.05080(18) 0.96549(9) 0.29301(8) 0.0164(2) Uani 1 1 d . . . C13 C -0.10583(18) 0.92377(10) 0.31304(8) 0.0183(2) Uani 1 1 d . . . H13 H -0.142(3) 0.8712(14) 0.2843(13) 0.025(5) Uiso 1 1 d . . . C14 C -0.2143(2) 0.95778(10) 0.37301(9) 0.0224(3) Uani 1 1 d . . . H14 H -0.325(3) 0.9319(14) 0.3823(13) 0.025(5) Uiso 1 1 d . . . C15 C -0.1659(2) 1.03286(11) 0.41405(9) 0.0233(3) Uani 1 1 d . . . H15 H -0.232(3) 1.0534(13) 0.4570(12) 0.027(5) Uiso 1 1 d . . . C16 C -0.0111(2) 1.07516(10) 0.39417(9) 0.0218(3) Uani 1 1 d . . . H16 H 0.022(3) 1.1280(14) 0.4231(11) 0.019(5) Uiso 1 1 d . . . C17 C 0.0966(2) 1.04186(10) 0.33395(9) 0.0192(3) Uani 1 1 d . . . H17 H 0.210(3) 1.0751(13) 0.3217(13) 0.026(5) Uiso 1 1 d . . . C18 C 0.28423(18) 0.86869(9) 0.24379(8) 0.0171(3) Uani 1 1 d . . . C19 C 0.30666(19) 0.83211(9) 0.32774(8) 0.0178(2) Uani 1 1 d . . . H19A H 0.265(3) 0.8727(14) 0.3653(13) 0.030(5) Uiso 1 1 d . . . H19B H 0.427(3) 0.8187(14) 0.3382(13) 0.027(5) Uiso 1 1 d . . . C20 C 0.2024(2) 0.74794(10) 0.34035(10) 0.0243(3) Uani 1 1 d . . . H20A H 0.229(4) 0.7224(17) 0.3900(16) 0.047(7) Uiso 1 1 d . . . H20B H 0.226(3) 0.7037(14) 0.2999(12) 0.027(5) Uiso 1 1 d . . . H20C H 0.079(3) 0.7604(14) 0.3353(13) 0.027(5) Uiso 1 1 d . . . C21 C 0.40843(19) 0.83123(9) 0.18294(9) 0.0176(2) Uani 1 1 d . . . C22 C 0.5686(2) 0.87257(10) 0.16874(9) 0.0199(3) Uani 1 1 d . . . H22 H 0.593(3) 0.9258(14) 0.1960(12) 0.022(5) Uiso 1 1 d . . . C23 C 0.6905(2) 0.83745(11) 0.11521(9) 0.0226(3) Uani 1 1 d . . . H23 H 0.802(3) 0.8633(15) 0.1075(13) 0.029(5) Uiso 1 1 d . . . C24 C 0.6529(2) 0.75985(11) 0.07495(10) 0.0246(3) Uani 1 1 d . . . H24 H 0.729(3) 0.7389(14) 0.0378(13) 0.030(5) Uiso 1 1 d . . . C25 C 0.4944(2) 0.71784(10) 0.08896(10) 0.0242(3) Uani 1 1 d . . . H25 H 0.473(3) 0.6652(13) 0.0608(13) 0.025(5) Uiso 1 1 d . . . C26 C 0.3725(2) 0.75329(10) 0.14208(10) 0.0214(3) Uani 1 1 d . . . H26 H 0.266(3) 0.7248(15) 0.1518(14) 0.036(6) Uiso 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 Fe 0.01294(8) 0.01332(8) 0.01485(8) -0.00029(6) -0.00135(6) -0.00140(7) C1 0.0156(6) 0.0253(7) 0.0252(7) -0.0003(6) -0.0006(6) -0.0049(5) C2 0.0223(7) 0.0273(8) 0.0227(7) 0.0047(6) 0.0001(6) -0.0089(6) C3 0.0250(7) 0.0176(6) 0.0298(8) 0.0040(5) -0.0046(6) -0.0054(5) C4 0.0249(7) 0.0168(6) 0.0252(7) -0.0041(5) -0.0014(6) -0.0055(5) C5 0.0183(6) 0.0224(7) 0.0204(7) 0.0001(5) -0.0041(5) -0.0064(5) C6 0.0165(6) 0.0162(6) 0.0200(6) -0.0032(5) -0.0016(5) 0.0005(4) C7 0.0202(7) 0.0206(6) 0.0156(6) -0.0022(5) -0.0019(5) -0.0023(5) C8 0.0155(6) 0.0178(6) 0.0195(6) -0.0001(5) -0.0043(5) 0.0001(5) C9 0.0151(6) 0.0185(6) 0.0177(6) -0.0016(5) -0.0003(5) -0.0016(5) C10 0.0159(6) 0.0138(6) 0.0180(6) -0.0007(4) -0.0016(5) -0.0014(5) C11 0.0167(6) 0.0154(5) 0.0167(5) -0.0012(5) 0.0004(4) -0.0022(5) C12 0.0159(6) 0.0171(6) 0.0161(6) -0.0018(5) 0.0003(5) 0.0016(5) C13 0.0164(6) 0.0188(6) 0.0195(6) -0.0008(5) 0.0018(4) -0.0007(5) C14 0.0169(7) 0.0267(7) 0.0236(6) -0.0003(5) 0.0052(5) 0.0011(5) C15 0.0213(7) 0.0276(7) 0.0210(7) -0.0030(6) 0.0039(5) 0.0073(6) C16 0.0251(7) 0.0199(6) 0.0203(6) -0.0049(5) -0.0003(5) 0.0038(6) C17 0.0189(6) 0.0174(6) 0.0214(7) -0.0028(5) 0.0005(5) -0.0012(5) C18 0.0171(6) 0.0157(5) 0.0186(6) -0.0005(4) -0.0010(5) -0.0012(5) C19 0.0193(6) 0.0170(6) 0.0172(6) 0.0010(5) -0.0011(5) 0.0023(5) C20 0.0265(8) 0.0185(6) 0.0278(7) 0.0072(6) 0.0016(6) 0.0030(5) C21 0.0156(6) 0.0157(6) 0.0214(6) -0.0020(5) -0.0001(5) 0.0027(5) C22 0.0167(6) 0.0187(6) 0.0242(7) -0.0032(5) -0.0010(5) 0.0003(5) C23 0.0165(6) 0.0262(7) 0.0250(7) 0.0009(5) 0.0014(5) 0.0012(5) C24 0.0220(7) 0.0269(7) 0.0250(7) -0.0041(6) 0.0037(5) 0.0063(6) C25 0.0259(7) 0.0196(6) 0.0271(7) -0.0075(6) 0.0008(6) 0.0040(5) C26 0.0190(6) 0.0177(6) 0.0275(7) -0.0060(5) 0.0011(5) -0.0006(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 Fe C1 2.0383(14) . ? Fe C6 2.0410(14) . ? Fe C7 2.0414(14) . ? Fe C5 2.0436(15) . ? Fe C2 2.0438(15) . ? Fe C8 2.0447(14) . ? Fe C9 2.0468(15) . ? Fe C4 2.0482(15) . ? Fe C3 2.0500(15) . ? Fe C10 2.0540(14) . ? C1 C2 1.422(2) . ? C1 C5 1.429(2) . ? C1 H1 0.97(2) . ? C2 C3 1.427(2) . ? C2 H2 0.94(2) . ? C3 C4 1.431(2) . ? C3 H3 0.95(2) . ? C4 C5 1.428(2) . ? C4 H4 0.93(2) . ? C5 H5 0.90(2) . ? C6 C7 1.425(2) . ? C6 C10 1.439(2) . ? C6 H6 0.95(2) . ? C7 C8 1.420(2) . ? C7 H7 1.00(2) . ? C8 C9 1.4233(19) . ? C8 H8 0.96(2) . ? C9 C10 1.438(2) . ? C9 H9 0.936(19) . ? C10 C11 1.4835(19) . ? C11 C18 1.3438(19) . ? C11 C12 1.4983(19) . ? C12 C13 1.3933(19) . ? C12 C17 1.395(2) . ? C13 C14 1.394(2) . ? C13 H13 0.97(2) . ? C14 C15 1.384(2) . ? C14 H14 0.94(2) . ? C15 C16 1.385(2) . ? C15 H15 0.93(2) . ? C16 C17 1.390(2) . ? C16 H16 0.97(2) . ? C17 H17 1.02(2) . ? C18 C21 1.498(2) . ? C18 C19 1.5114(19) . ? C19 C20 1.526(2) . ? C19 H19A 0.93(2) . ? C19 H19B 0.95(2) . ? C20 H20A 0.93(3) . ? C20 H20B 0.97(2) . ? C20 H20C 0.96(2) . ? C21 C22 1.394(2) . ? C21 C26 1.398(2) . ? C22 C23 1.393(2) . ? C22 H22 0.95(2) . ? C23 C24 1.391(2) . ? C23 H23 0.95(2) . ? C24 C25 1.387(2) . ? C24 H24 0.91(2) . ? C25 C26 1.391(2) . ? C25 H25 0.94(2) . ? C26 H26 0.94(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 C1 Fe C6 106.14(6) . . ? C1 Fe C7 121.53(6) . . ? C6 Fe C7 40.86(6) . . ? C1 Fe C5 40.99(6) . . ? C6 Fe C5 121.46(6) . . ? C7 Fe C5 157.63(6) . . ? C1 Fe C2 40.76(6) . . ? C6 Fe C2 122.33(7) . . ? C7 Fe C2 107.08(6) . . ? C5 Fe C2 68.72(6) . . ? C1 Fe C8 157.92(6) . . ? C6 Fe C8 68.72(6) . . ? C7 Fe C8 40.68(6) . . ? C5 Fe C8 160.05(6) . . ? C2 Fe C8 122.55(6) . . ? C1 Fe C9 159.34(6) . . ? C6 Fe C9 68.71(6) . . ? C7 Fe C9 68.48(6) . . ? C5 Fe C9 123.34(6) . . ? C2 Fe C9 158.88(6) . . ? C8 Fe C9 40.71(6) . . ? C1 Fe C4 68.84(6) . . ? C6 Fe C4 158.04(6) . . ? C7 Fe C4 160.00(6) . . ? C5 Fe C4 40.86(6) . . ? C2 Fe C4 68.66(7) . . ? C8 Fe C4 123.91(6) . . ? C9 Fe C4 108.05(6) . . ? C1 Fe C3 68.80(7) . . ? C6 Fe C3 159.14(7) . . ? C7 Fe C3 123.25(6) . . ? C5 Fe C3 68.82(6) . . ? C2 Fe C3 40.81(7) . . ? C8 Fe C3 107.95(6) . . ? C9 Fe C3 123.08(6) . . ? C4 Fe C3 40.87(6) . . ? C1 Fe C10 121.99(6) . . ? C6 Fe C10 41.15(6) . . ? C7 Fe C10 69.12(6) . . ? C5 Fe C10 106.36(6) . . ? C2 Fe C10 158.61(7) . . ? C8 Fe C10 69.13(6) . . ? C9 Fe C10 41.06(6) . . ? C4 Fe C10 122.08(6) . . ? C3 Fe C10 158.73(6) . . ? C2 C1 C5 108.04(14) . . ? C2 C1 Fe 69.83(9) . . ? C5 C1 Fe 69.70(8) . . ? C2 C1 H1 126.3(13) . . ? C5 C1 H1 125.5(13) . . ? Fe C1 H1 122.2(14) . . ? C1 C2 C3 108.35(14) . . ? C1 C2 Fe 69.41(8) . . ? C3 C2 Fe 69.83(9) . . ? C1 C2 H2 123.1(13) . . ? C3 C2 H2 128.6(13) . . ? Fe C2 H2 125.9(12) . . ? C2 C3 C4 107.70(14) . . ? C2 C3 Fe 69.36(9) . . ? C4 C3 Fe 69.50(8) . . ? C2 C3 H3 122.4(14) . . ? C4 C3 H3 129.9(14) . . ? Fe C3 H3 127.1(14) . . ? C5 C4 C3 108.04(14) . . ? C5 C4 Fe 69.40(8) . . ? C3 C4 Fe 69.63(9) . . ? C5 C4 H4 125.9(12) . . ? C3 C4 H4 125.9(12) . . ? Fe C4 H4 123.9(13) . . ? C4 C5 C1 107.87(14) . . ? C4 C5 Fe 69.74(9) . . ? C1 C5 Fe 69.30(8) . . ? C4 C5 H5 127.9(13) . . ? C1 C5 H5 124.2(13) . . ? Fe C5 H5 125.4(12) . . ? C7 C6 C10 108.42(12) . . ? C7 C6 Fe 69.59(8) . . ? C10 C6 Fe 69.91(8) . . ? C7 C6 H6 123.2(12) . . ? C10 C6 H6 128.3(12) . . ? Fe C6 H6 123.1(12) . . ? C8 C7 C6 108.28(13) . . ? C8 C7 Fe 69.79(8) . . ? C6 C7 Fe 69.56(8) . . ? C8 C7 H7 126.4(13) . . ? C6 C7 H7 125.3(13) . . ? Fe C7 H7 125.0(12) . . ? C7 C8 C9 107.99(12) . . ? C7 C8 Fe 69.54(8) . . ? C9 C8 Fe 69.72(8) . . ? C7 C8 H8 127.7(13) . . ? C9 C8 H8 124.3(13) . . ? Fe C8 H8 123.9(13) . . ? C8 C9 C10 108.71(13) . . ? C8 C9 Fe 69.57(9) . . ? C10 C9 Fe 69.74(8) . . ? C8 C9 H9 125.6(11) . . ? C10 C9 H9 125.7(11) . . ? Fe C9 H9 125.0(11) . . ? C9 C10 C6 106.59(12) . . ? C9 C10 C11 121.98(12) . . ? C6 C10 C11 131.43(13) . . ? C9 C10 Fe 69.20(8) . . ? C6 C10 Fe 68.94(8) . . ? C11 C10 Fe 126.41(10) . . ? C18 C11 C10 126.13(13) . . ? C18 C11 C12 119.26(12) . . ? C10 C11 C12 114.58(12) . . ? C13 C12 C17 118.74(13) . . ? C13 C12 C11 120.14(12) . . ? C17 C12 C11 121.09(13) . . ? C12 C13 C14 120.50(14) . . ? C12 C13 H13 120.1(13) . . ? C14 C13 H13 119.4(13) . . ? C15 C14 C13 120.16(14) . . ? C15 C14 H14 120.3(13) . . ? C13 C14 H14 119.3(13) . . ? C14 C15 C16 119.76(14) . . ? C14 C15 H15 120.8(13) . . ? C16 C15 H15 119.3(13) . . ? C15 C16 C17 120.21(14) . . ? C15 C16 H16 119.5(12) . . ? C17 C16 H16 120.3(12) . . ? C16 C17 C12 120.62(14) . . ? C16 C17 H17 117.4(12) . . ? C12 C17 H17 122.0(12) . . ? C11 C18 C21 123.79(13) . . ? C11 C18 C19 122.06(13) . . ? C21 C18 C19 114.15(12) . . ? C18 C19 C20 112.30(12) . . ? C18 C19 H19A 109.4(13) . . ? C20 C19 H19A 107.0(14) . . ? C18 C19 H19B 110.9(13) . . ? C20 C19 H19B 107.0(13) . . ? H19A C19 H19B 110.1(19) . . ? C19 C20 H20A 111.2(16) . . ? C19 C20 H20B 113.2(13) . . ? H20A C20 H20B 106(2) . . ? C19 C20 H20C 109.2(13) . . ? H20A C20 H20C 112(2) . . ? H20B C20 H20C 105.1(18) . . ? C22 C21 C26 118.40(13) . . ? C22 C21 C18 119.59(13) . . ? C26 C21 C18 121.94(13) . . ? C23 C22 C21 121.13(14) . . ? C23 C22 H22 120.4(12) . . ? C21 C22 H22 118.5(12) . . ? C24 C23 C22 119.83(15) . . ? C24 C23 H23 118.4(13) . . ? C22 C23 H23 121.6(13) . . ? C25 C24 C23 119.57(14) . . ? C25 C24 H24 120.7(14) . . ? C23 C24 H24 119.6(14) . . ? C24 C25 C26 120.50(14) . . ? C24 C25 H25 117.7(13) . . ? C26 C25 H25 121.8(14) . . ? C25 C26 C21 120.57(14) . . ? C25 C26 H26 120.5(14) . . ? C21 C26 H26 118.9(14) . . ? 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 C6 Fe C1 C2 121.13(10) . . . . ? C7 Fe C1 C2 79.39(11) . . . . ? C5 Fe C1 C2 -119.18(14) . . . . ? C8 Fe C1 C2 48.11(19) . . . . ? C9 Fe C1 C2 -166.57(15) . . . . ? C4 Fe C1 C2 -81.46(10) . . . . ? C3 Fe C1 C2 -37.48(10) . . . . ? C10 Fe C1 C2 163.09(9) . . . . ? C6 Fe C1 C5 -119.69(9) . . . . ? C7 Fe C1 C5 -161.42(9) . . . . ? C2 Fe C1 C5 119.18(14) . . . . ? C8 Fe C1 C5 167.29(14) . . . . ? C9 Fe C1 C5 -47.4(2) . . . . ? C4 Fe C1 C5 37.72(9) . . . . ? C3 Fe C1 C5 81.70(10) . . . . ? C10 Fe C1 C5 -77.72(10) . . . . ? C5 C1 C2 C3 -0.29(17) . . . . ? Fe C1 C2 C3 59.16(11) . . . . ? C5 C1 C2 Fe -59.45(10) . . . . ? C6 Fe C2 C1 -76.68(11) . . . . ? C7 Fe C2 C1 -118.78(10) . . . . ? C5 Fe C2 C1 37.92(9) . . . . ? C8 Fe C2 C1 -160.61(9) . . . . ? C9 Fe C2 C1 166.86(15) . . . . ? C4 Fe C2 C1 81.93(10) . . . . ? C3 Fe C2 C1 119.75(14) . . . . ? C10 Fe C2 C1 -42.5(2) . . . . ? C1 Fe C2 C3 -119.75(14) . . . . ? C6 Fe C2 C3 163.57(9) . . . . ? C7 Fe C2 C3 121.46(10) . . . . ? C5 Fe C2 C3 -81.83(10) . . . . ? C8 Fe C2 C3 79.63(11) . . . . ? C9 Fe C2 C3 47.1(2) . . . . ? C4 Fe C2 C3 -37.83(9) . . . . ? C10 Fe C2 C3 -162.30(15) . . . . ? C1 C2 C3 C4 0.23(18) . . . . ? Fe C2 C3 C4 59.13(11) . . . . ? C1 C2 C3 Fe -58.90(11) . . . . ? C1 Fe C3 C2 37.44(10) . . . . ? C6 Fe C3 C2 -42.2(2) . . . . ? C7 Fe C3 C2 -77.17(11) . . . . ? C5 Fe C3 C2 81.56(10) . . . . ? C8 Fe C3 C2 -119.36(10) . . . . ? C9 Fe C3 C2 -161.64(9) . . . . ? C4 Fe C3 C2 119.19(14) . . . . ? C10 Fe C3 C2 162.20(15) . . . . ? C1 Fe C3 C4 -81.75(10) . . . . ? C6 Fe C3 C4 -161.34(15) . . . . ? C7 Fe C3 C4 163.64(9) . . . . ? C5 Fe C3 C4 -37.63(10) . . . . ? C2 Fe C3 C4 -119.19(14) . . . . ? C8 Fe C3 C4 121.45(10) . . . . ? C9 Fe C3 C4 79.18(11) . . . . ? C10 Fe C3 C4 43.0(2) . . . . ? C2 C3 C4 C5 -0.09(17) . . . . ? Fe C3 C4 C5 58.96(10) . . . . ? C2 C3 C4 Fe -59.05(11) . . . . ? C1 Fe C4 C5 -37.85(9) . . . . ? C6 Fe C4 C5 42.8(2) . . . . ? C7 Fe C4 C5 -163.01(16) . . . . ? C2 Fe C4 C5 -81.73(10) . . . . ? C8 Fe C4 C5 162.59(9) . . . . ? C9 Fe C4 C5 120.45(9) . . . . ? C3 Fe C4 C5 -119.50(14) . . . . ? C10 Fe C4 C5 77.49(11) . . . . ? C1 Fe C4 C3 81.65(10) . . . . ? C6 Fe C4 C3 162.26(15) . . . . ? C7 Fe C4 C3 -43.5(2) . . . . ? C5 Fe C4 C3 119.50(14) . . . . ? C2 Fe C4 C3 37.77(10) . . . . ? C8 Fe C4 C3 -77.91(11) . . . . ? C9 Fe C4 C3 -120.05(10) . . . . ? C10 Fe C4 C3 -163.02(9) . . . . ? C3 C4 C5 C1 -0.09(17) . . . . ? Fe C4 C5 C1 59.02(10) . . . . ? C3 C4 C5 Fe -59.11(10) . . . . ? C2 C1 C5 C4 0.24(17) . . . . ? Fe C1 C5 C4 -59.29(10) . . . . ? C2 C1 C5 Fe 59.53(10) . . . . ? C1 Fe C5 C4 119.28(13) . . . . ? C6 Fe C5 C4 -162.68(9) . . . . ? C7 Fe C5 C4 164.78(14) . . . . ? C2 Fe C5 C4 81.57(10) . . . . ? C8 Fe C5 C4 -46.7(2) . . . . ? C9 Fe C5 C4 -78.83(10) . . . . ? C3 Fe C5 C4 37.64(9) . . . . ? C10 Fe C5 C4 -120.45(9) . . . . ? C6 Fe C5 C1 78.04(10) . . . . ? C7 Fe C5 C1 45.50(19) . . . . ? C2 Fe C5 C1 -37.71(9) . . . . ? C8 Fe C5 C1 -165.98(15) . . . . ? C9 Fe C5 C1 161.89(9) . . . . ? C4 Fe C5 C1 -119.28(13) . . . . ? C3 Fe C5 C1 -81.64(10) . . . . ? C10 Fe C5 C1 120.27(9) . . . . ? C1 Fe C6 C7 -119.85(9) . . . . ? C5 Fe C6 C7 -161.76(9) . . . . ? C2 Fe C6 C7 -78.44(10) . . . . ? C8 Fe C6 C7 37.46(9) . . . . ? C9 Fe C6 C7 81.30(9) . . . . ? C4 Fe C6 C7 166.86(15) . . . . ? C3 Fe C6 C7 -47.2(2) . . . . ? C10 Fe C6 C7 119.68(12) . . . . ? C1 Fe C6 C10 120.47(9) . . . . ? C7 Fe C6 C10 -119.68(12) . . . . ? C5 Fe C6 C10 78.56(10) . . . . ? C2 Fe C6 C10 161.88(9) . . . . ? C8 Fe C6 C10 -82.22(9) . . . . ? C9 Fe C6 C10 -38.38(8) . . . . ? C4 Fe C6 C10 47.18(19) . . . . ? C3 Fe C6 C10 -166.85(16) . . . . ? C10 C6 C7 C8 0.08(16) . . . . ? Fe C6 C7 C8 -59.24(10) . . . . ? C10 C6 C7 Fe 59.32(10) . . . . ? C1 Fe C7 C8 -162.57(8) . . . . ? C6 Fe C7 C8 119.60(12) . . . . ? C5 Fe C7 C8 164.13(14) . . . . ? C2 Fe C7 C8 -120.40(9) . . . . ? C9 Fe C7 C8 37.69(8) . . . . ? C4 Fe C7 C8 -46.0(2) . . . . ? C3 Fe C7 C8 -78.60(10) . . . . ? C10 Fe C7 C8 81.88(9) . . . . ? C1 Fe C7 C6 77.83(10) . . . . ? C5 Fe C7 C6 44.53(19) . . . . ? C2 Fe C7 C6 120.00(9) . . . . ? C8 Fe C7 C6 -119.60(12) . . . . ? C9 Fe C7 C6 -81.91(9) . . . . ? C4 Fe C7 C6 -165.60(16) . . . . ? C3 Fe C7 C6 161.80(9) . . . . ? C10 Fe C7 C6 -37.72(8) . . . . ? C6 C7 C8 C9 -0.23(16) . . . . ? Fe C7 C8 C9 -59.33(10) . . . . ? C6 C7 C8 Fe 59.09(10) . . . . ? C1 Fe C8 C7 42.77(18) . . . . ? C6 Fe C8 C7 -37.62(9) . . . . ? C5 Fe C8 C7 -162.24(16) . . . . ? C2 Fe C8 C7 77.98(11) . . . . ? C9 Fe C8 C7 -119.30(12) . . . . ? C4 Fe C8 C7 162.76(9) . . . . ? C3 Fe C8 C7 120.49(9) . . . . ? C10 Fe C8 C7 -81.87(9) . . . . ? C1 Fe C8 C9 162.07(14) . . . . ? C6 Fe C8 C9 81.68(9) . . . . ? C7 Fe C8 C9 119.30(12) . . . . ? C5 Fe C8 C9 -42.9(2) . . . . ? C2 Fe C8 C9 -162.72(9) . . . . ? C4 Fe C8 C9 -77.94(10) . . . . ? C3 Fe C8 C9 -120.21(9) . . . . ? C10 Fe C8 C9 37.43(8) . . . . ? C7 C8 C9 C10 0.30(16) . . . . ? Fe C8 C9 C10 -58.91(10) . . . . ? C7 C8 C9 Fe 59.21(10) . . . . ? C1 Fe C9 C8 -160.86(15) . . . . ? C6 Fe C9 C8 -81.70(9) . . . . ? C7 Fe C9 C8 -37.66(8) . . . . ? C5 Fe C9 C8 163.84(8) . . . . ? C2 Fe C9 C8 44.0(2) . . . . ? C4 Fe C9 C8 121.39(9) . . . . ? C3 Fe C9 C8 78.87(10) . . . . ? C10 Fe C9 C8 -120.16(12) . . . . ? C1 Fe C9 C10 -40.7(2) . . . . ? C6 Fe C9 C10 38.46(8) . . . . ? C7 Fe C9 C10 82.50(9) . . . . ? C5 Fe C9 C10 -76.00(10) . . . . ? C2 Fe C9 C10 164.18(16) . . . . ? C8 Fe C9 C10 120.16(12) . . . . ? C4 Fe C9 C10 -118.45(9) . . . . ? C3 Fe C9 C10 -160.98(8) . . . . ? C8 C9 C10 C6 -0.24(16) . . . . ? Fe C9 C10 C6 -59.05(9) . . . . ? C8 C9 C10 C11 179.56(13) . . . . ? Fe C9 C10 C11 120.75(13) . . . . ? C8 C9 C10 Fe 58.81(10) . . . . ? C7 C6 C10 C9 0.10(16) . . . . ? Fe C6 C10 C9 59.22(10) . . . . ? C7 C6 C10 C11 -179.68(14) . . . . ? Fe C6 C10 C11 -120.56(16) . . . . ? C7 C6 C10 Fe -59.12(10) . . . . ? C1 Fe C10 C9 164.26(8) . . . . ? C6 Fe C10 C9 -118.27(11) . . . . ? C7 Fe C10 C9 -80.80(9) . . . . ? C5 Fe C10 C9 122.34(9) . . . . ? C2 Fe C10 C9 -164.38(15) . . . . ? C8 Fe C10 C9 -37.13(8) . . . . ? C4 Fe C10 C9 80.62(10) . . . . ? C3 Fe C10 C9 48.8(2) . . . . ? C1 Fe C10 C6 -77.47(10) . . . . ? C7 Fe C10 C6 37.47(8) . . . . ? C5 Fe C10 C6 -119.39(9) . . . . ? C2 Fe C10 C6 -46.1(2) . . . . ? C8 Fe C10 C6 81.14(9) . . . . ? C9 Fe C10 C6 118.27(11) . . . . ? C4 Fe C10 C6 -161.11(8) . . . . ? C3 Fe C10 C6 167.10(15) . . . . ? C1 Fe C10 C11 49.19(14) . . . . ? C6 Fe C10 C11 126.66(16) . . . . ? C7 Fe C10 C11 164.13(14) . . . . ? C5 Fe C10 C11 7.27(14) . . . . ? C2 Fe C10 C11 80.6(2) . . . . ? C8 Fe C10 C11 -152.20(14) . . . . ? C9 Fe C10 C11 -115.07(15) . . . . ? C4 Fe C10 C11 -34.45(15) . . . . ? C3 Fe C10 C11 -66.2(2) . . . . ? C9 C10 C11 C18 -177.98(14) . . . . ? C6 C10 C11 C18 1.8(2) . . . . ? Fe C10 C11 C18 -91.41(16) . . . . ? C9 C10 C11 C12 3.91(19) . . . . ? C6 C10 C11 C12 -176.34(14) . . . . ? Fe C10 C11 C12 90.49(14) . . . . ? C18 C11 C12 C13 -87.70(17) . . . . ? C10 C11 C12 C13 90.55(16) . . . . ? C18 C11 C12 C17 94.47(17) . . . . ? C10 C11 C12 C17 -87.28(16) . . . . ? C17 C12 C13 C14 -0.1(2) . . . . ? C11 C12 C13 C14 -178.00(14) . . . . ? C12 C13 C14 C15 -0.9(2) . . . . ? C13 C14 C15 C16 1.4(2) . . . . ? C14 C15 C16 C17 -0.8(2) . . . . ? C15 C16 C17 C12 -0.2(2) . . . . ? C13 C12 C17 C16 0.7(2) . . . . ? C11 C12 C17 C16 178.55(14) . . . . ? C10 C11 C18 C21 4.3(2) . . . . ? C12 C11 C18 C21 -177.63(13) . . . . ? C10 C11 C18 C19 -176.36(13) . . . . ? C12 C11 C18 C19 1.7(2) . . . . ? C11 C18 C19 C20 94.44(16) . . . . ? C21 C18 C19 C20 -86.20(15) . . . . ? C11 C18 C21 C22 87.72(18) . . . . ? C19 C18 C21 C22 -91.62(16) . . . . ? C11 C18 C21 C26 -95.25(18) . . . . ? C19 C18 C21 C26 85.41(17) . . . . ? C26 C21 C22 C23 0.0(2) . . . . ? C18 C21 C22 C23 177.14(14) . . . . ? C21 C22 C23 C24 0.0(2) . . . . ? C22 C23 C24 C25 -0.4(2) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C24 C25 C26 C21 -0.8(3) . . . . ? C22 C21 C26 C25 0.4(2) . . . . ? C18 C21 C26 C25 -176.69(15) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.839 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.068 #===END data_2g _database_code_depnum_ccdc_archive 'CCDC 738754' _audit_creation_date 06-12-01 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '10271549 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.0998(8) _cell_length_b 10.4180(11) _cell_length_c 12.3362(12) _cell_angle_alpha 97.949(7) _cell_angle_beta 96.147(7) _cell_angle_gamma 96.436(6) _cell_volume 1142.0(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C28 H28 Fe1 O2 # Dc = 1.32 Fooo = 476.00 Mu = 6.82 M = 452.38 # Found Formula = C28 H28 Fe1 O2 # Dc = 1.32 FOOO = 476.00 Mu = 6.82 M = 452.38 _chemical_formula_sum 'C28 H28 Fe1 O2' _chemical_formula_moiety 'C28 H28 Fe1 O2' _chemical_compound_source ? _chemical_formula_weight 452.38 _cell_measurement_reflns_used 135 _cell_measurement_theta_min 4 _cell_measurement_theta_max 23 _cell_measurement_temperature 250 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.682 # Sheldrick geometric approximatio 0.93 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.0 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 250 _diffrn_reflns_number 36861 _reflns_number_total 13211 _diffrn_reflns_av_R_equivalents 0.030 # Number of reflections with Friedels Law is 13211 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14150 _diffrn_reflns_theta_min 1.680 _diffrn_reflns_theta_max 39.995 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 30.396 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min -18 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.57 _refine_diff_density_max 0.48 _refine_ls_number_reflns 7611 _refine_ls_number_restraints 0 _refine_ls_number_parameters 281 #_refine_ls_R_factor_ref 0.0347 _refine_ls_wR_factor_ref 0.0401 _refine_ls_goodness_of_fit_ref 1.1069 #_reflns_number_all 13208 _refine_ls_R_factor_all 0.0798 _refine_ls_wR_factor_all 0.0812 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 7611 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_gt 0.0401 _refine_ls_shift/su_max 0.000402 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refu # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.994 0.135 0.633 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.240891(18) 0.169605(16) 0.245588(13) 0.0219 1.0000 Uani . . . . . . C1 C 0.51909(11) 0.27096(10) 0.43141(8) 0.0210 1.0000 Uani . . . . . . C2 C 0.66282(12) 0.26839(10) 0.40951(8) 0.0231 1.0000 Uani . . . . . . C3 C 0.78265(13) 0.22341(12) 0.48667(10) 0.0280 1.0000 Uani . . . . . . C4 C 0.90362(15) 0.33285(16) 0.54496(13) 0.0408 1.0000 Uani . . . . . . C5 C 0.71438(12) 0.30741(11) 0.30565(9) 0.0236 1.0000 Uani . . . . . . C6 C 0.75013(13) 0.44000(11) 0.29571(9) 0.0264 1.0000 Uani . . . . . . C7 C 0.79349(14) 0.47737(11) 0.19803(10) 0.0291 1.0000 Uani . . . . . . C8 C 0.80272(14) 0.38193(12) 0.10737(10) 0.0280 1.0000 Uani . . . . . . C9 C 0.77141(14) 0.24897(12) 0.11637(10) 0.0288 1.0000 Uani . . . . . . C10 C 0.72802(14) 0.21336(11) 0.21526(10) 0.0273 1.0000 Uani . . . . . . C11 C 0.47728(12) 0.24590(10) 0.54237(8) 0.0223 1.0000 Uani . . . . . . C12 C 0.53507(13) 0.33470(11) 0.63721(9) 0.0261 1.0000 Uani . . . . . . C13 C 0.49371(14) 0.31882(12) 0.74153(9) 0.0290 1.0000 Uani . . . . . . C14 C 0.39068(14) 0.21260(13) 0.75121(9) 0.0293 1.0000 Uani . . . . . . C15 C 0.33063(17) 0.12302(14) 0.65736(10) 0.0354 1.0000 Uani . . . . . . C16 C 0.37456(16) 0.13891(12) 0.55467(9) 0.0317 1.0000 Uani . . . . . . C17 C 0.39451(11) 0.30269(10) 0.35454(8) 0.0213 1.0000 Uani . . . . . . C18 C 0.24473(13) 0.30897(12) 0.38305(9) 0.0262 1.0000 Uani . . . . . . C19 C 0.15239(13) 0.34056(12) 0.29147(10) 0.0297 1.0000 Uani . . . . . . C20 C 0.24271(14) 0.35520(12) 0.20517(9) 0.0285 1.0000 Uani . . . . . . C21 C 0.39069(12) 0.33101(11) 0.24234(9) 0.0248 1.0000 Uani . . . . . . C22 C 0.29830(17) -0.01525(13) 0.25616(12) 0.0379 1.0000 Uani . . . . . . C23 C 0.14760(18) -0.01025(14) 0.27744(13) 0.0389 1.0000 Uani . . . . . . C24 C 0.06610(16) 0.02490(14) 0.18220(14) 0.0400 1.0000 Uani . . . . . . C25 C 0.16634(18) 0.04220(14) 0.10242(11) 0.0400 1.0000 Uani . . . . . . C26 C 0.31030(17) 0.01677(14) 0.14832(13) 0.0395 1.0000 Uani . . . . . . C27 C 0.8752(2) 0.33599(17) -0.07432(13) 0.0462 1.0000 Uani . . . . . . C28 C 0.4061(2) 0.2697(2) 0.94713(12) 0.0554 1.0000 Uani . . . . . . O1 O 0.84014(15) 0.42831(11) 0.01356(9) 0.0436 1.0000 Uani . . . . . . O2 O 0.33960(15) 0.18728(14) 0.84852(8) 0.0491 1.0000 Uani . . . . . . H31 H 0.7330 0.1827 0.5443 0.0550(12) 1.0000 Uiso . . . . . . H32 H 0.8318 0.1567 0.4424 0.0550(12) 1.0000 Uiso . . . . . . H41 H 0.9773 0.2954 0.5936 0.0550(12) 1.0000 Uiso . . . . . . H42 H 0.8568 0.4002 0.5906 0.0550(12) 1.0000 Uiso . . . . . . H43 H 0.9556 0.3741 0.4886 0.0550(12) 1.0000 Uiso . . . . . . H61 H 0.7444 0.5088 0.3596 0.0550(12) 1.0000 Uiso . . . . . . H71 H 0.8181 0.5720 0.1927 0.0550(12) 1.0000 Uiso . . . . . . H91 H 0.7799 0.1802 0.0530 0.0550(12) 1.0000 Uiso . . . . . . H101 H 0.7063 0.1186 0.2213 0.0550(12) 1.0000 Uiso . . . . . . H121 H 0.6077 0.4117 0.6304 0.0550(12) 1.0000 Uiso . . . . . . H131 H 0.5378 0.3829 0.8081 0.0550(12) 1.0000 Uiso . . . . . . H151 H 0.2546 0.0541 0.6625 0.0550(12) 1.0000 Uiso . . . . . . H161 H 0.3682 0.1088 0.4736 0.0550(12) 1.0000 Uiso . . . . . . H181 H 0.2121 0.2950 0.4543 0.0550(12) 1.0000 Uiso . . . . . . H191 H 0.0442 0.3506 0.2886 0.0550(12) 1.0000 Uiso . . . . . . H201 H 0.2086 0.3783 0.1315 0.0550(12) 1.0000 Uiso . . . . . . H211 H 0.4725 0.3325 0.1990 0.0550(12) 1.0000 Uiso . . . . . . H221 H 0.3808 -0.0373 0.3079 0.0550(12) 1.0000 Uiso . . . . . . H231 H 0.1063 -0.0282 0.3464 0.0550(12) 1.0000 Uiso . . . . . . H241 H -0.0422 0.0355 0.1735 0.0550(12) 1.0000 Uiso . . . . . . H251 H 0.1410 0.0674 0.0280 0.0550(12) 1.0000 Uiso . . . . . . H261 H 0.4028 0.0209 0.1112 0.0550(12) 1.0000 Uiso . . . . . . H271 H 0.8999 0.3828 -0.1371 0.0550(12) 1.0000 Uiso . . . . . . H272 H 0.9624 0.2939 -0.0476 0.0550(12) 1.0000 Uiso . . . . . . H273 H 0.7872 0.2681 -0.0999 0.0550(12) 1.0000 Uiso . . . . . . H281 H 0.3595 0.2416 1.0112 0.0550(12) 1.0000 Uiso . . . . . . H282 H 0.5152 0.2643 0.9578 0.0550(12) 1.0000 Uiso . . . . . . H283 H 0.3891 0.3622 0.9414 0.0550(12) 1.0000 Uiso . . . . . . 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 0.02094(6) 0.02238(6) 0.02055(6) -0.00058(4) -0.00184(4) 0.00384(4) C1 0.0221(4) 0.0222(4) 0.0173(3) 0.0013(3) 0.0006(3) 0.0013(3) C2 0.0229(4) 0.0238(4) 0.0219(4) 0.0027(3) 0.0012(3) 0.0022(3) C3 0.0245(4) 0.0300(5) 0.0285(5) 0.0046(4) -0.0021(4) 0.0051(4) C4 0.0280(5) 0.0459(7) 0.0424(7) -0.0021(6) -0.0068(5) -0.0001(5) C5 0.0206(4) 0.0262(4) 0.0239(4) 0.0027(3) 0.0043(3) 0.0034(3) C6 0.0261(4) 0.0245(4) 0.0279(5) -0.0003(4) 0.0071(4) 0.0020(3) C7 0.0312(5) 0.0247(4) 0.0315(5) 0.0029(4) 0.0090(4) 0.0005(4) C8 0.0291(5) 0.0296(5) 0.0263(5) 0.0041(4) 0.0081(4) 0.0029(4) C9 0.0340(5) 0.0272(5) 0.0255(4) 0.0005(4) 0.0080(4) 0.0056(4) C10 0.0328(5) 0.0225(4) 0.0270(5) 0.0024(3) 0.0061(4) 0.0047(4) C11 0.0254(4) 0.0229(4) 0.0174(3) 0.0016(3) 0.0012(3) 0.0017(3) C12 0.0311(5) 0.0248(4) 0.0203(4) -0.0006(3) 0.0040(3) -0.0006(4) C13 0.0355(5) 0.0315(5) 0.0184(4) -0.0012(3) 0.0039(4) 0.0027(4) C14 0.0337(5) 0.0364(6) 0.0191(4) 0.0067(4) 0.0051(4) 0.0049(4) C15 0.0433(7) 0.0347(6) 0.0258(5) 0.0082(4) 0.0035(4) -0.0092(5) C16 0.0411(6) 0.0296(5) 0.0205(4) 0.0019(4) 0.0009(4) -0.0079(4) C17 0.0222(4) 0.0218(4) 0.0185(4) -0.0003(3) 0.0004(3) 0.0028(3) C18 0.0258(4) 0.0308(5) 0.0219(4) -0.0004(3) 0.0037(3) 0.0078(4) C19 0.0264(5) 0.0311(5) 0.0313(5) -0.0005(4) 0.0001(4) 0.0117(4) C20 0.0322(5) 0.0275(5) 0.0250(4) 0.0046(4) -0.0043(4) 0.0070(4) C21 0.0265(4) 0.0269(4) 0.0201(4) 0.0033(3) 0.0012(3) 0.0018(3) C22 0.0423(7) 0.0261(5) 0.0417(7) -0.0020(5) -0.0088(5) 0.0106(5) C23 0.0431(7) 0.0287(6) 0.0421(7) 0.0058(5) -0.0003(5) -0.0025(5) C24 0.0301(6) 0.0345(6) 0.0490(8) 0.0004(5) -0.0092(5) -0.0028(5) C25 0.0487(8) 0.0336(6) 0.0298(6) -0.0062(5) -0.0119(5) 0.0009(5) C26 0.0415(7) 0.0329(6) 0.0392(6) -0.0115(5) 0.0033(5) 0.0070(5) C27 0.0589(9) 0.0474(8) 0.0323(6) 0.0012(6) 0.0209(6) -0.0015(7) C28 0.0669(11) 0.0793(13) 0.0197(5) 0.0082(6) 0.0090(6) 0.0043(9) O1 0.0640(7) 0.0364(5) 0.0329(5) 0.0066(4) 0.0217(5) 0.0010(5) O2 0.0592(7) 0.0644(8) 0.0234(4) 0.0107(4) 0.0127(4) -0.0062(6) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C17 . 2.0810(10) yes Fe1 . C18 . 2.0688(11) yes Fe1 . C19 . 2.0692(11) yes Fe1 . C20 . 2.0612(12) yes Fe1 . C21 . 2.0503(11) yes Fe1 . C22 . 2.0686(13) yes Fe1 . C23 . 2.0747(14) yes Fe1 . C24 . 2.0698(13) yes Fe1 . C25 . 2.0578(12) yes Fe1 . C26 . 2.0575(13) yes C1 . C2 . 1.3660(15) yes C1 . C11 . 1.5082(14) yes C1 . C17 . 1.4947(14) yes C2 . C3 . 1.5266(15) yes C2 . C5 . 1.5023(15) yes C3 . C4 . 1.5333(18) yes C3 . H31 . 1.000 no C3 . H32 . 0.999 no C4 . H41 . 1.000 no C4 . H42 . 0.999 no C4 . H43 . 1.000 no C5 . C6 . 1.4084(16) yes C5 . C10 . 1.4049(15) yes C6 . C7 . 1.3987(17) yes C6 . H61 . 1.000 no C7 . C8 . 1.4063(17) yes C7 . H71 . 0.999 no C8 . C9 . 1.4047(17) yes C8 . O1 . 1.3751(15) yes C9 . C10 . 1.4061(17) yes C9 . H91 . 1.000 no C10 . H101 . 0.999 no C11 . C12 . 1.4004(14) yes C11 . C16 . 1.4081(16) yes C12 . C13 . 1.4050(16) yes C12 . H121 . 1.000 no C13 . C14 . 1.3948(18) yes C13 . H131 . 1.000 no C14 . C15 . 1.4005(18) yes C14 . O2 . 1.3807(15) yes C15 . C16 . 1.3941(17) yes C15 . H151 . 0.953 no C16 . H161 . 1.000 no C17 . C18 . 1.4498(15) yes C17 . C21 . 1.4523(14) yes C18 . C19 . 1.4326(16) yes C18 . H181 . 0.981 no C19 . C20 . 1.4271(18) yes C19 . H191 . 0.999 no C20 . C21 . 1.4362(16) yes C20 . H201 . 0.999 no C21 . H211 . 0.962 no C22 . C23 . 1.429(2) yes C22 . C26 . 1.428(2) yes C22 . H221 . 1.000 no C23 . C24 . 1.434(2) yes C23 . H231 . 0.999 no C24 . C25 . 1.427(2) yes C24 . H241 . 1.000 no C25 . C26 . 1.438(2) yes C25 . H251 . 0.999 no C26 . H261 . 1.000 no C27 . O1 . 1.4341(19) yes C27 . H271 . 1.002 no C27 . H272 . 0.997 no C27 . H273 . 0.999 no C28 . O2 . 1.422(2) yes C28 . H281 . 1.000 no C28 . H282 . 0.997 no C28 . H283 . 1.003 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C17 . Fe1 . C18 . 40.90(4) yes C17 . Fe1 . C19 . 69.02(4) yes C18 . Fe1 . C19 . 40.51(5) yes C17 . Fe1 . C20 . 69.01(4) yes C18 . Fe1 . C20 . 68.00(5) yes C19 . Fe1 . C20 . 40.42(5) yes C17 . Fe1 . C21 . 41.15(4) yes C18 . Fe1 . C21 . 68.44(5) yes C19 . Fe1 . C21 . 68.62(5) yes C20 . Fe1 . C21 . 40.89(5) yes C17 . Fe1 . C22 . 107.66(5) yes C18 . Fe1 . C22 . 122.58(5) yes C19 . Fe1 . C22 . 157.58(6) yes C20 . Fe1 . C22 . 160.92(6) yes C21 . Fe1 . C22 . 124.36(5) yes C17 . Fe1 . C23 . 125.29(5) yes C18 . Fe1 . C23 . 109.39(6) yes C19 . Fe1 . C23 . 122.33(6) yes C20 . Fe1 . C23 . 156.63(6) yes C21 . Fe1 . C23 . 161.76(5) yes C17 . Fe1 . C24 . 162.37(6) yes C18 . Fe1 . C24 . 125.78(6) yes C19 . Fe1 . C24 . 108.03(6) yes C20 . Fe1 . C24 . 120.76(5) yes C21 . Fe1 . C24 . 155.47(6) yes C17 . Fe1 . C25 . 155.66(6) yes C18 . Fe1 . C25 . 161.39(6) yes C19 . Fe1 . C25 . 123.89(6) yes C20 . Fe1 . C25 . 106.43(5) yes C21 . Fe1 . C25 . 119.80(6) yes C17 . Fe1 . C26 . 120.47(5) yes C18 . Fe1 . C26 . 156.96(6) yes C19 . Fe1 . C26 . 160.58(6) yes C20 . Fe1 . C26 . 123.76(6) yes C21 . Fe1 . C26 . 106.47(6) yes C22 . Fe1 . C23 . 40.35(6) yes C22 . Fe1 . C24 . 68.05(6) yes C23 . Fe1 . C24 . 40.50(6) yes C22 . Fe1 . C25 . 68.43(6) yes C23 . Fe1 . C25 . 68.24(6) yes C24 . Fe1 . C25 . 40.46(7) yes C22 . Fe1 . C26 . 40.49(6) yes C23 . Fe1 . C26 . 68.03(7) yes C24 . Fe1 . C26 . 68.18(6) yes C25 . Fe1 . C26 . 40.90(6) yes C2 . C1 . C11 . 120.02(9) yes C2 . C1 . C17 . 125.25(9) yes C11 . C1 . C17 . 114.68(9) yes C1 . C2 . C3 . 123.07(10) yes C1 . C2 . C5 . 122.23(9) yes C3 . C2 . C5 . 114.69(9) yes C2 . C3 . C4 . 114.47(11) yes C2 . C3 . H31 . 108.2 no C4 . C3 . H31 . 108.2 no C2 . C3 . H32 . 108.2 no C4 . C3 . H32 . 108.2 no H31 . C3 . H32 . 109.5 no C3 . C4 . H41 . 109.4 no C3 . C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no C3 . C4 . H43 . 109.4 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no C2 . C5 . C6 . 120.89(9) yes C2 . C5 . C10 . 121.31(10) yes C6 . C5 . C10 . 117.80(10) yes C5 . C6 . C7 . 121.27(10) yes C5 . C6 . H61 . 119.4 no C7 . C6 . H61 . 119.3 no C6 . C7 . C8 . 120.10(11) yes C6 . C7 . H71 . 120.0 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 119.62(11) yes C7 . C8 . O1 . 115.83(11) yes C9 . C8 . O1 . 124.53(11) yes C8 . C9 . C10 . 119.41(10) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 120.3 no C9 . C10 . C5 . 121.75(10) yes C9 . C10 . H101 . 119.1 no C5 . C10 . H101 . 119.2 no C1 . C11 . C12 . 119.89(9) yes C1 . C11 . C16 . 122.44(9) yes C12 . C11 . C16 . 117.58(10) yes C11 . C12 . C13 . 121.92(10) yes C11 . C12 . H121 . 119.0 no C13 . C12 . H121 . 119.1 no C12 . C13 . C14 . 119.31(10) yes C12 . C13 . H131 . 120.3 no C14 . C13 . H131 . 120.3 no C13 . C14 . C15 . 119.77(10) yes C13 . C14 . O2 . 124.84(11) yes C15 . C14 . O2 . 115.39(12) yes C14 . C15 . C16 . 120.27(11) yes C14 . C15 . H151 . 120.1 no C16 . C15 . H151 . 119.5 no C11 . C16 . C15 . 121.14(10) yes C11 . C16 . H161 . 88.6 no C15 . C16 . H161 . 150.3 no C1 . C17 . Fe1 . 126.52(7) yes C1 . C17 . C18 . 123.27(9) yes Fe1 . C17 . C18 . 69.10(6) yes C1 . C17 . C21 . 130.81(9) yes Fe1 . C17 . C21 . 68.29(6) yes C18 . C17 . C21 . 105.91(9) yes C17 . C18 . Fe1 . 70.00(6) yes C17 . C18 . C19 . 109.31(10) yes Fe1 . C18 . C19 . 69.76(6) yes C17 . C18 . H181 . 125.3 no Fe1 . C18 . H181 . 127.1 no C19 . C18 . H181 . 125.4 no C18 . C19 . Fe1 . 69.73(6) yes C18 . C19 . C20 . 107.72(10) yes Fe1 . C19 . C20 . 69.49(7) yes C18 . C19 . H191 . 126.1 no Fe1 . C19 . H191 . 126.3 no C20 . C19 . H191 . 126.1 no C19 . C20 . Fe1 . 70.09(7) yes C19 . C20 . C21 . 108.39(9) yes Fe1 . C20 . C21 . 69.15(6) yes C19 . C20 . H201 . 125.7 no Fe1 . C20 . H201 . 126.5 no C21 . C20 . H201 . 125.9 no C17 . C21 . C20 . 108.65(10) yes C17 . C21 . Fe1 . 70.56(6) yes C20 . C21 . Fe1 . 69.96(7) yes C17 . C21 . H211 . 126.3 no C20 . C21 . H211 . 125.0 no Fe1 . C21 . H211 . 124.8 no Fe1 . C22 . C23 . 70.06(8) yes Fe1 . C22 . C26 . 69.34(8) yes C23 . C22 . C26 . 108.05(12) yes Fe1 . C22 . H221 . 126.2 no C23 . C22 . H221 . 125.9 no C26 . C22 . H221 . 126.1 no C22 . C23 . Fe1 . 69.60(8) yes C22 . C23 . C24 . 107.95(14) yes Fe1 . C23 . C24 . 69.57(8) yes C22 . C23 . H231 . 126.0 no Fe1 . C23 . H231 . 126.5 no C24 . C23 . H231 . 126.0 no C23 . C24 . Fe1 . 69.93(8) yes C23 . C24 . C25 . 108.19(13) yes Fe1 . C24 . C25 . 69.31(7) yes C23 . C24 . H241 . 125.7 no Fe1 . C24 . H241 . 126.4 no C25 . C24 . H241 . 126.1 no C24 . C25 . Fe1 . 70.22(8) yes C24 . C25 . C26 . 107.68(13) yes Fe1 . C25 . C26 . 69.54(7) yes C24 . C25 . H251 . 126.2 no Fe1 . C25 . H251 . 125.7 no C26 . C25 . H251 . 126.1 no C25 . C26 . C22 . 108.14(14) yes C25 . C26 . Fe1 . 69.56(8) yes C22 . C26 . Fe1 . 70.17(7) yes C25 . C26 . H261 . 125.9 no C22 . C26 . H261 . 125.9 no Fe1 . C26 . H261 . 125.9 no O1 . C27 . H271 . 109.1 no O1 . C27 . H272 . 109.5 no H271 . C27 . H272 . 109.6 no O1 . C27 . H273 . 109.4 no H271 . C27 . H273 . 109.4 no H272 . C27 . H273 . 109.8 no O2 . C28 . H281 . 109.4 no O2 . C28 . H282 . 109.7 no H281 . C28 . H282 . 109.8 no O2 . C28 . H283 . 109.2 no H281 . C28 . H283 . 109.3 no H282 . C28 . H283 . 109.5 no C27 . O1 . C8 . 117.66(12) yes C28 . O2 . C14 . 117.28(13) yes #===END data_2h _database_code_depnum_ccdc_archive 'CCDC 738755' _audit_creation_date 06-12-01 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '10271549 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.0998(8) _cell_length_b 10.4180(11) _cell_length_c 12.3362(12) _cell_angle_alpha 97.949(7) _cell_angle_beta 96.147(7) _cell_angle_gamma 96.436(6) _cell_volume 1142.0(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C28 H28 Fe1 O2 # Dc = 1.32 Fooo = 476.00 Mu = 6.82 M = 452.38 # Found Formula = C28 H28 Fe1 O2 # Dc = 1.32 FOOO = 476.00 Mu = 6.82 M = 452.38 _chemical_formula_sum 'C28 H28 Fe1 O2' _chemical_formula_moiety 'C28 H28 Fe1 O2' _chemical_compound_source ? _chemical_formula_weight 452.38 _cell_measurement_reflns_used 135 _cell_measurement_theta_min 4 _cell_measurement_theta_max 23 _cell_measurement_temperature 250 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.682 # Sheldrick geometric approximatio 0.93 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.0 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 250 _diffrn_reflns_number 36861 _reflns_number_total 13211 _diffrn_reflns_av_R_equivalents 0.030 # Number of reflections with Friedels Law is 13211 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14150 _diffrn_reflns_theta_min 1.680 _diffrn_reflns_theta_max 39.995 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 30.396 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min -18 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.57 _refine_diff_density_max 0.48 _refine_ls_number_reflns 7611 _refine_ls_number_restraints 0 _refine_ls_number_parameters 281 #_refine_ls_R_factor_ref 0.0347 _refine_ls_wR_factor_ref 0.0401 _refine_ls_goodness_of_fit_ref 1.1069 #_reflns_number_all 13208 _refine_ls_R_factor_all 0.0798 _refine_ls_wR_factor_all 0.0812 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 7611 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_gt 0.0401 _refine_ls_shift/su_max 0.000402 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refu # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.994 0.135 0.633 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.240891(18) 0.169605(16) 0.245588(13) 0.0219 1.0000 Uani . . . . . . C1 C 0.51909(11) 0.27096(10) 0.43141(8) 0.0210 1.0000 Uani . . . . . . C2 C 0.66282(12) 0.26839(10) 0.40951(8) 0.0231 1.0000 Uani . . . . . . C3 C 0.78265(13) 0.22341(12) 0.48667(10) 0.0280 1.0000 Uani . . . . . . C4 C 0.90362(15) 0.33285(16) 0.54496(13) 0.0408 1.0000 Uani . . . . . . C5 C 0.71438(12) 0.30741(11) 0.30565(9) 0.0236 1.0000 Uani . . . . . . C6 C 0.75013(13) 0.44000(11) 0.29571(9) 0.0264 1.0000 Uani . . . . . . C7 C 0.79349(14) 0.47737(11) 0.19803(10) 0.0291 1.0000 Uani . . . . . . C8 C 0.80272(14) 0.38193(12) 0.10737(10) 0.0280 1.0000 Uani . . . . . . C9 C 0.77141(14) 0.24897(12) 0.11637(10) 0.0288 1.0000 Uani . . . . . . C10 C 0.72802(14) 0.21336(11) 0.21526(10) 0.0273 1.0000 Uani . . . . . . C11 C 0.47728(12) 0.24590(10) 0.54237(8) 0.0223 1.0000 Uani . . . . . . C12 C 0.53507(13) 0.33470(11) 0.63721(9) 0.0261 1.0000 Uani . . . . . . C13 C 0.49371(14) 0.31882(12) 0.74153(9) 0.0290 1.0000 Uani . . . . . . C14 C 0.39068(14) 0.21260(13) 0.75121(9) 0.0293 1.0000 Uani . . . . . . C15 C 0.33063(17) 0.12302(14) 0.65736(10) 0.0354 1.0000 Uani . . . . . . C16 C 0.37456(16) 0.13891(12) 0.55467(9) 0.0317 1.0000 Uani . . . . . . C17 C 0.39451(11) 0.30269(10) 0.35454(8) 0.0213 1.0000 Uani . . . . . . C18 C 0.24473(13) 0.30897(12) 0.38305(9) 0.0262 1.0000 Uani . . . . . . C19 C 0.15239(13) 0.34056(12) 0.29147(10) 0.0297 1.0000 Uani . . . . . . C20 C 0.24271(14) 0.35520(12) 0.20517(9) 0.0285 1.0000 Uani . . . . . . C21 C 0.39069(12) 0.33101(11) 0.24234(9) 0.0248 1.0000 Uani . . . . . . C22 C 0.29830(17) -0.01525(13) 0.25616(12) 0.0379 1.0000 Uani . . . . . . C23 C 0.14760(18) -0.01025(14) 0.27744(13) 0.0389 1.0000 Uani . . . . . . C24 C 0.06610(16) 0.02490(14) 0.18220(14) 0.0400 1.0000 Uani . . . . . . C25 C 0.16634(18) 0.04220(14) 0.10242(11) 0.0400 1.0000 Uani . . . . . . C26 C 0.31030(17) 0.01677(14) 0.14832(13) 0.0395 1.0000 Uani . . . . . . C27 C 0.8752(2) 0.33599(17) -0.07432(13) 0.0462 1.0000 Uani . . . . . . C28 C 0.4061(2) 0.2697(2) 0.94713(12) 0.0554 1.0000 Uani . . . . . . O1 O 0.84014(15) 0.42831(11) 0.01356(9) 0.0436 1.0000 Uani . . . . . . O2 O 0.33960(15) 0.18728(14) 0.84852(8) 0.0491 1.0000 Uani . . . . . . H31 H 0.7330 0.1827 0.5443 0.0550(12) 1.0000 Uiso . . . . . . H32 H 0.8318 0.1567 0.4424 0.0550(12) 1.0000 Uiso . . . . . . H41 H 0.9773 0.2954 0.5936 0.0550(12) 1.0000 Uiso . . . . . . H42 H 0.8568 0.4002 0.5906 0.0550(12) 1.0000 Uiso . . . . . . H43 H 0.9556 0.3741 0.4886 0.0550(12) 1.0000 Uiso . . . . . . H61 H 0.7444 0.5088 0.3596 0.0550(12) 1.0000 Uiso . . . . . . H71 H 0.8181 0.5720 0.1927 0.0550(12) 1.0000 Uiso . . . . . . H91 H 0.7799 0.1802 0.0530 0.0550(12) 1.0000 Uiso . . . . . . H101 H 0.7063 0.1186 0.2213 0.0550(12) 1.0000 Uiso . . . . . . H121 H 0.6077 0.4117 0.6304 0.0550(12) 1.0000 Uiso . . . . . . H131 H 0.5378 0.3829 0.8081 0.0550(12) 1.0000 Uiso . . . . . . H151 H 0.2546 0.0541 0.6625 0.0550(12) 1.0000 Uiso . . . . . . H161 H 0.3682 0.1088 0.4736 0.0550(12) 1.0000 Uiso . . . . . . H181 H 0.2121 0.2950 0.4543 0.0550(12) 1.0000 Uiso . . . . . . H191 H 0.0442 0.3506 0.2886 0.0550(12) 1.0000 Uiso . . . . . . H201 H 0.2086 0.3783 0.1315 0.0550(12) 1.0000 Uiso . . . . . . H211 H 0.4725 0.3325 0.1990 0.0550(12) 1.0000 Uiso . . . . . . H221 H 0.3808 -0.0373 0.3079 0.0550(12) 1.0000 Uiso . . . . . . H231 H 0.1063 -0.0282 0.3464 0.0550(12) 1.0000 Uiso . . . . . . H241 H -0.0422 0.0355 0.1735 0.0550(12) 1.0000 Uiso . . . . . . H251 H 0.1410 0.0674 0.0280 0.0550(12) 1.0000 Uiso . . . . . . H261 H 0.4028 0.0209 0.1112 0.0550(12) 1.0000 Uiso . . . . . . H271 H 0.8999 0.3828 -0.1371 0.0550(12) 1.0000 Uiso . . . . . . H272 H 0.9624 0.2939 -0.0476 0.0550(12) 1.0000 Uiso . . . . . . H273 H 0.7872 0.2681 -0.0999 0.0550(12) 1.0000 Uiso . . . . . . H281 H 0.3595 0.2416 1.0112 0.0550(12) 1.0000 Uiso . . . . . . H282 H 0.5152 0.2643 0.9578 0.0550(12) 1.0000 Uiso . . . . . . H283 H 0.3891 0.3622 0.9414 0.0550(12) 1.0000 Uiso . . . . . . 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 0.02094(6) 0.02238(6) 0.02055(6) -0.00058(4) -0.00184(4) 0.00384(4) C1 0.0221(4) 0.0222(4) 0.0173(3) 0.0013(3) 0.0006(3) 0.0013(3) C2 0.0229(4) 0.0238(4) 0.0219(4) 0.0027(3) 0.0012(3) 0.0022(3) C3 0.0245(4) 0.0300(5) 0.0285(5) 0.0046(4) -0.0021(4) 0.0051(4) C4 0.0280(5) 0.0459(7) 0.0424(7) -0.0021(6) -0.0068(5) -0.0001(5) C5 0.0206(4) 0.0262(4) 0.0239(4) 0.0027(3) 0.0043(3) 0.0034(3) C6 0.0261(4) 0.0245(4) 0.0279(5) -0.0003(4) 0.0071(4) 0.0020(3) C7 0.0312(5) 0.0247(4) 0.0315(5) 0.0029(4) 0.0090(4) 0.0005(4) C8 0.0291(5) 0.0296(5) 0.0263(5) 0.0041(4) 0.0081(4) 0.0029(4) C9 0.0340(5) 0.0272(5) 0.0255(4) 0.0005(4) 0.0080(4) 0.0056(4) C10 0.0328(5) 0.0225(4) 0.0270(5) 0.0024(3) 0.0061(4) 0.0047(4) C11 0.0254(4) 0.0229(4) 0.0174(3) 0.0016(3) 0.0012(3) 0.0017(3) C12 0.0311(5) 0.0248(4) 0.0203(4) -0.0006(3) 0.0040(3) -0.0006(4) C13 0.0355(5) 0.0315(5) 0.0184(4) -0.0012(3) 0.0039(4) 0.0027(4) C14 0.0337(5) 0.0364(6) 0.0191(4) 0.0067(4) 0.0051(4) 0.0049(4) C15 0.0433(7) 0.0347(6) 0.0258(5) 0.0082(4) 0.0035(4) -0.0092(5) C16 0.0411(6) 0.0296(5) 0.0205(4) 0.0019(4) 0.0009(4) -0.0079(4) C17 0.0222(4) 0.0218(4) 0.0185(4) -0.0003(3) 0.0004(3) 0.0028(3) C18 0.0258(4) 0.0308(5) 0.0219(4) -0.0004(3) 0.0037(3) 0.0078(4) C19 0.0264(5) 0.0311(5) 0.0313(5) -0.0005(4) 0.0001(4) 0.0117(4) C20 0.0322(5) 0.0275(5) 0.0250(4) 0.0046(4) -0.0043(4) 0.0070(4) C21 0.0265(4) 0.0269(4) 0.0201(4) 0.0033(3) 0.0012(3) 0.0018(3) C22 0.0423(7) 0.0261(5) 0.0417(7) -0.0020(5) -0.0088(5) 0.0106(5) C23 0.0431(7) 0.0287(6) 0.0421(7) 0.0058(5) -0.0003(5) -0.0025(5) C24 0.0301(6) 0.0345(6) 0.0490(8) 0.0004(5) -0.0092(5) -0.0028(5) C25 0.0487(8) 0.0336(6) 0.0298(6) -0.0062(5) -0.0119(5) 0.0009(5) C26 0.0415(7) 0.0329(6) 0.0392(6) -0.0115(5) 0.0033(5) 0.0070(5) C27 0.0589(9) 0.0474(8) 0.0323(6) 0.0012(6) 0.0209(6) -0.0015(7) C28 0.0669(11) 0.0793(13) 0.0197(5) 0.0082(6) 0.0090(6) 0.0043(9) O1 0.0640(7) 0.0364(5) 0.0329(5) 0.0066(4) 0.0217(5) 0.0010(5) O2 0.0592(7) 0.0644(8) 0.0234(4) 0.0107(4) 0.0127(4) -0.0062(6) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C17 . 2.0810(10) yes Fe1 . C18 . 2.0688(11) yes Fe1 . C19 . 2.0692(11) yes Fe1 . C20 . 2.0612(12) yes Fe1 . C21 . 2.0503(11) yes Fe1 . C22 . 2.0686(13) yes Fe1 . C23 . 2.0747(14) yes Fe1 . C24 . 2.0698(13) yes Fe1 . C25 . 2.0578(12) yes Fe1 . C26 . 2.0575(13) yes C1 . C2 . 1.3660(15) yes C1 . C11 . 1.5082(14) yes C1 . C17 . 1.4947(14) yes C2 . C3 . 1.5266(15) yes C2 . C5 . 1.5023(15) yes C3 . C4 . 1.5333(18) yes C3 . H31 . 1.000 no C3 . H32 . 0.999 no C4 . H41 . 1.000 no C4 . H42 . 0.999 no C4 . H43 . 1.000 no C5 . C6 . 1.4084(16) yes C5 . C10 . 1.4049(15) yes C6 . C7 . 1.3987(17) yes C6 . H61 . 1.000 no C7 . C8 . 1.4063(17) yes C7 . H71 . 0.999 no C8 . C9 . 1.4047(17) yes C8 . O1 . 1.3751(15) yes C9 . C10 . 1.4061(17) yes C9 . H91 . 1.000 no C10 . H101 . 0.999 no C11 . C12 . 1.4004(14) yes C11 . C16 . 1.4081(16) yes C12 . C13 . 1.4050(16) yes C12 . H121 . 1.000 no C13 . C14 . 1.3948(18) yes C13 . H131 . 1.000 no C14 . C15 . 1.4005(18) yes C14 . O2 . 1.3807(15) yes C15 . C16 . 1.3941(17) yes C15 . H151 . 0.953 no C16 . H161 . 1.000 no C17 . C18 . 1.4498(15) yes C17 . C21 . 1.4523(14) yes C18 . C19 . 1.4326(16) yes C18 . H181 . 0.981 no C19 . C20 . 1.4271(18) yes C19 . H191 . 0.999 no C20 . C21 . 1.4362(16) yes C20 . H201 . 0.999 no C21 . H211 . 0.962 no C22 . C23 . 1.429(2) yes C22 . C26 . 1.428(2) yes C22 . H221 . 1.000 no C23 . C24 . 1.434(2) yes C23 . H231 . 0.999 no C24 . C25 . 1.427(2) yes C24 . H241 . 1.000 no C25 . C26 . 1.438(2) yes C25 . H251 . 0.999 no C26 . H261 . 1.000 no C27 . O1 . 1.4341(19) yes C27 . H271 . 1.002 no C27 . H272 . 0.997 no C27 . H273 . 0.999 no C28 . O2 . 1.422(2) yes C28 . H281 . 1.000 no C28 . H282 . 0.997 no C28 . H283 . 1.003 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C17 . Fe1 . C18 . 40.90(4) yes C17 . Fe1 . C19 . 69.02(4) yes C18 . Fe1 . C19 . 40.51(5) yes C17 . Fe1 . C20 . 69.01(4) yes C18 . Fe1 . C20 . 68.00(5) yes C19 . Fe1 . C20 . 40.42(5) yes C17 . Fe1 . C21 . 41.15(4) yes C18 . Fe1 . C21 . 68.44(5) yes C19 . Fe1 . C21 . 68.62(5) yes C20 . Fe1 . C21 . 40.89(5) yes C17 . Fe1 . C22 . 107.66(5) yes C18 . Fe1 . C22 . 122.58(5) yes C19 . Fe1 . C22 . 157.58(6) yes C20 . Fe1 . C22 . 160.92(6) yes C21 . Fe1 . C22 . 124.36(5) yes C17 . Fe1 . C23 . 125.29(5) yes C18 . Fe1 . C23 . 109.39(6) yes C19 . Fe1 . C23 . 122.33(6) yes C20 . Fe1 . C23 . 156.63(6) yes C21 . Fe1 . C23 . 161.76(5) yes C17 . Fe1 . C24 . 162.37(6) yes C18 . Fe1 . C24 . 125.78(6) yes C19 . Fe1 . C24 . 108.03(6) yes C20 . Fe1 . C24 . 120.76(5) yes C21 . Fe1 . C24 . 155.47(6) yes C17 . Fe1 . C25 . 155.66(6) yes C18 . Fe1 . C25 . 161.39(6) yes C19 . Fe1 . C25 . 123.89(6) yes C20 . Fe1 . C25 . 106.43(5) yes C21 . Fe1 . C25 . 119.80(6) yes C17 . Fe1 . C26 . 120.47(5) yes C18 . Fe1 . C26 . 156.96(6) yes C19 . Fe1 . C26 . 160.58(6) yes C20 . Fe1 . C26 . 123.76(6) yes C21 . Fe1 . C26 . 106.47(6) yes C22 . Fe1 . C23 . 40.35(6) yes C22 . Fe1 . C24 . 68.05(6) yes C23 . Fe1 . C24 . 40.50(6) yes C22 . Fe1 . C25 . 68.43(6) yes C23 . Fe1 . C25 . 68.24(6) yes C24 . Fe1 . C25 . 40.46(7) yes C22 . Fe1 . C26 . 40.49(6) yes C23 . Fe1 . C26 . 68.03(7) yes C24 . Fe1 . C26 . 68.18(6) yes C25 . Fe1 . C26 . 40.90(6) yes C2 . C1 . C11 . 120.02(9) yes C2 . C1 . C17 . 125.25(9) yes C11 . C1 . C17 . 114.68(9) yes C1 . C2 . C3 . 123.07(10) yes C1 . C2 . C5 . 122.23(9) yes C3 . C2 . C5 . 114.69(9) yes C2 . C3 . C4 . 114.47(11) yes C2 . C3 . H31 . 108.2 no C4 . C3 . H31 . 108.2 no C2 . C3 . H32 . 108.2 no C4 . C3 . H32 . 108.2 no H31 . C3 . H32 . 109.5 no C3 . C4 . H41 . 109.4 no C3 . C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no C3 . C4 . H43 . 109.4 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no C2 . C5 . C6 . 120.89(9) yes C2 . C5 . C10 . 121.31(10) yes C6 . C5 . C10 . 117.80(10) yes C5 . C6 . C7 . 121.27(10) yes C5 . C6 . H61 . 119.4 no C7 . C6 . H61 . 119.3 no C6 . C7 . C8 . 120.10(11) yes C6 . C7 . H71 . 120.0 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 119.62(11) yes C7 . C8 . O1 . 115.83(11) yes C9 . C8 . O1 . 124.53(11) yes C8 . C9 . C10 . 119.41(10) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 120.3 no C9 . C10 . C5 . 121.75(10) yes C9 . C10 . H101 . 119.1 no C5 . C10 . H101 . 119.2 no C1 . C11 . C12 . 119.89(9) yes C1 . C11 . C16 . 122.44(9) yes C12 . C11 . C16 . 117.58(10) yes C11 . C12 . C13 . 121.92(10) yes C11 . C12 . H121 . 119.0 no C13 . C12 . H121 . 119.1 no C12 . C13 . C14 . 119.31(10) yes C12 . C13 . H131 . 120.3 no C14 . C13 . H131 . 120.3 no C13 . C14 . C15 . 119.77(10) yes C13 . C14 . O2 . 124.84(11) yes C15 . C14 . O2 . 115.39(12) yes C14 . C15 . C16 . 120.27(11) yes C14 . C15 . H151 . 120.1 no C16 . C15 . H151 . 119.5 no C11 . C16 . C15 . 121.14(10) yes C11 . C16 . H161 . 88.6 no C15 . C16 . H161 . 150.3 no C1 . C17 . Fe1 . 126.52(7) yes C1 . C17 . C18 . 123.27(9) yes Fe1 . C17 . C18 . 69.10(6) yes C1 . C17 . C21 . 130.81(9) yes Fe1 . C17 . C21 . 68.29(6) yes C18 . C17 . C21 . 105.91(9) yes C17 . C18 . Fe1 . 70.00(6) yes C17 . C18 . C19 . 109.31(10) yes Fe1 . C18 . C19 . 69.76(6) yes C17 . C18 . H181 . 125.3 no Fe1 . C18 . H181 . 127.1 no C19 . C18 . H181 . 125.4 no C18 . C19 . Fe1 . 69.73(6) yes C18 . C19 . C20 . 107.72(10) yes Fe1 . C19 . C20 . 69.49(7) yes C18 . C19 . H191 . 126.1 no Fe1 . C19 . H191 . 126.3 no C20 . C19 . H191 . 126.1 no C19 . C20 . Fe1 . 70.09(7) yes C19 . C20 . C21 . 108.39(9) yes Fe1 . C20 . C21 . 69.15(6) yes C19 . C20 . H201 . 125.7 no Fe1 . C20 . H201 . 126.5 no C21 . C20 . H201 . 125.9 no C17 . C21 . C20 . 108.65(10) yes C17 . C21 . Fe1 . 70.56(6) yes C20 . C21 . Fe1 . 69.96(7) yes C17 . C21 . H211 . 126.3 no C20 . C21 . H211 . 125.0 no Fe1 . C21 . H211 . 124.8 no Fe1 . C22 . C23 . 70.06(8) yes Fe1 . C22 . C26 . 69.34(8) yes C23 . C22 . C26 . 108.05(12) yes Fe1 . C22 . H221 . 126.2 no C23 . C22 . H221 . 125.9 no C26 . C22 . H221 . 126.1 no C22 . C23 . Fe1 . 69.60(8) yes C22 . C23 . C24 . 107.95(14) yes Fe1 . C23 . C24 . 69.57(8) yes C22 . C23 . H231 . 126.0 no Fe1 . C23 . H231 . 126.5 no C24 . C23 . H231 . 126.0 no C23 . C24 . Fe1 . 69.93(8) yes C23 . C24 . C25 . 108.19(13) yes Fe1 . C24 . C25 . 69.31(7) yes C23 . C24 . H241 . 125.7 no Fe1 . C24 . H241 . 126.4 no C25 . C24 . H241 . 126.1 no C24 . C25 . Fe1 . 70.22(8) yes C24 . C25 . C26 . 107.68(13) yes Fe1 . C25 . C26 . 69.54(7) yes C24 . C25 . H251 . 126.2 no Fe1 . C25 . H251 . 125.7 no C26 . C25 . H251 . 126.1 no C25 . C26 . C22 . 108.14(14) yes C25 . C26 . Fe1 . 69.56(8) yes C22 . C26 . Fe1 . 70.17(7) yes C25 . C26 . H261 . 125.9 no C22 . C26 . H261 . 125.9 no Fe1 . C26 . H261 . 125.9 no O1 . C27 . H271 . 109.1 no O1 . C27 . H272 . 109.5 no H271 . C27 . H272 . 109.6 no O1 . C27 . H273 . 109.4 no H271 . C27 . H273 . 109.4 no H272 . C27 . H273 . 109.8 no O2 . C28 . H281 . 109.4 no O2 . C28 . H282 . 109.7 no H281 . C28 . H282 . 109.8 no O2 . C28 . H283 . 109.2 no H281 . C28 . H283 . 109.3 no H282 . C28 . H283 . 109.5 no C27 . O1 . C8 . 117.66(12) yes C28 . O2 . C14 . 117.28(13) yes #===END data_2i _database_code_depnum_ccdc_archive 'CCDC 738756' _audit_creation_date 09-06-17 _audit_creation_method CRYSTALS_ver_12.87 _oxford_structure_analysis_title '6171430 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 5.9954(4) _cell_length_b 24.330(2) _cell_length_c 14.9313(16) _cell_angle_alpha 90 _cell_angle_beta 95.613(6) _cell_angle_gamma 90 _cell_volume 2167.6(3) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C27 H26 Fe1 O2 # Dc = 1.34 Fooo = 920.00 Mu = 7.16 M = 438.35 # Found Formula = C27 H26 Fe1 O2 # Dc = 1.34 FOOO = 920.00 Mu = 7.16 M = 438.35 _chemical_formula_sum 'C27 H26 Fe1 O2' _chemical_formula_moiety 'C27 H26 Fe1 O2' _chemical_compound_source ? _chemical_formula_weight 438.35 _cell_measurement_reflns_used 100 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _cell_measurement_temperature 200 _exptl_crystal_description stick _exptl_crystal_colour orange _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.716 # Sheldrick geometric approximatio 0.90 0.94 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.94 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 6246 _reflns_number_total 6246 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections with Friedels Law is 6246 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6331 _diffrn_reflns_theta_min 2.164 _diffrn_reflns_theta_max 30.014 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.613 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 34 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 1.83 _oxford_diffrn_Wilson_scale 3.15 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.81 _refine_diff_density_max 1.01 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 6242 _refine_ls_number_restraints 0 _refine_ls_number_parameters 273 _oxford_refine_ls_R_factor_ref 0.0870 _refine_ls_wR_factor_ref 0.1133 _refine_ls_goodness_of_fit_ref 0.9573 _refine_ls_shift/su_max 0.0013809 _refine_ls_shift/su_mean 0.3091143 # The values computed from all data _oxford_reflns_number_all 6242 _refine_ls_R_factor_all 0.0870 _refine_ls_wR_factor_all 0.1133 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4164 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_gt 0.0974 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 1.01P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.39065(5) 0.616622(12) 0.519641(19) 0.0227 1.0000 Uani . . . . . . . O2 O 0.2900(3) 0.88861(6) 0.42348(11) 0.0357 1.0000 Uani . . . . . . . O3 O 0.6438(3) 0.43225(6) 0.12711(11) 0.0360 1.0000 Uani . . . . . . . C4 C 0.6098(3) 0.59458(8) 0.22196(13) 0.0214 1.0000 Uani . . . . . . . C5 C 0.4452(3) 0.72768(8) 0.34666(13) 0.0219 1.0000 Uani . . . . . . . C6 C 0.5953(3) 0.65327(8) 0.25373(13) 0.0217 1.0000 Uani . . . . . . . C7 C 0.3690(3) 0.62754(8) 0.37959(13) 0.0207 1.0000 Uani . . . . . . . C8 C 0.4267(3) 0.51530(9) 0.14607(15) 0.0303 1.0000 Uani . . . . . . . C9 C 0.1567(3) 0.63629(9) 0.41508(14) 0.0258 1.0000 Uani . . . . . . . C10 C 0.5989(3) 0.75726(8) 0.40435(15) 0.0274 1.0000 Uani . . . . . . . C11 C 0.4824(3) 0.66801(8) 0.32407(13) 0.0206 1.0000 Uani . . . . . . . C12 C 0.8092(3) 0.56443(8) 0.23181(13) 0.0243 1.0000 Uani . . . . . . . C13 C 0.3535(4) 0.83627(8) 0.39814(14) 0.0263 1.0000 Uani . . . . . . . C14 C 0.8180(3) 0.51014(9) 0.20045(14) 0.0274 1.0000 Uani . . . . . . . C15 C 0.2677(4) 0.54746(8) 0.45185(15) 0.0304 1.0000 Uani . . . . . . . C16 C 0.6270(3) 0.48570(8) 0.15732(14) 0.0251 1.0000 Uani . . . . . . . C17 C 0.5550(4) 0.81149(8) 0.43009(15) 0.0302 1.0000 Uani . . . . . . . C18 C 0.0939(3) 0.58668(10) 0.45778(15) 0.0308 1.0000 Uani . . . . . . . C19 C 0.4375(3) 0.57236(8) 0.40439(13) 0.0244 1.0000 Uani . . . . . . . C20 C 0.6950(3) 0.69530(9) 0.19269(14) 0.0273 1.0000 Uani . . . . . . . C21 C 0.5459(4) 0.70258(10) 0.10312(16) 0.0375 1.0000 Uani . . . . . . . C22 C 0.6696(4) 0.65430(10) 0.58557(16) 0.0338 1.0000 Uani . . . . . . . C23 C 0.2486(4) 0.75483(9) 0.31255(15) 0.0324 1.0000 Uani . . . . . . . C24 C 0.4169(4) 0.91308(9) 0.50004(15) 0.0362 1.0000 Uani . . . . . . . C25 C 0.2020(4) 0.80845(9) 0.33796(16) 0.0352 1.0000 Uani . . . . . . . C26 C 0.4197(3) 0.56906(9) 0.17841(15) 0.0283 1.0000 Uani . . . . . . . C27 C 0.3259(4) 0.65203(12) 0.63984(16) 0.0438 1.0000 Uani . . . . . . . C28 C 0.6441(5) 0.60147(11) 0.62118(17) 0.0435 1.0000 Uani . . . . . . . C29 C 0.4756(4) 0.68534(9) 0.59689(16) 0.0346 1.0000 Uani . . . . . . . C30 C 0.4297(6) 0.59924(12) 0.65481(16) 0.0549 1.0000 Uani . . . . . . . H11 H 0.5145 0.4211 0.1203 0.0436(14) 1.0000 Uiso . . . . . . . H81 H 0.2927 0.4993 0.1150 0.0436(14) 1.0000 Uiso . . . . . . . H91 H 0.0698 0.6692 0.4098 0.0436(14) 1.0000 Uiso . . . . . . . H101 H 0.7369 0.7397 0.4287 0.0436(14) 1.0000 Uiso . . . . . . . H121 H 0.9419 0.5812 0.2593 0.0436(14) 1.0000 Uiso . . . . . . . H141 H 0.9579 0.4897 0.2092 0.0436(14) 1.0000 Uiso . . . . . . . H151 H 0.2689 0.5106 0.4745 0.0436(14) 1.0000 Uiso . . . . . . . H171 H 0.6634 0.8314 0.4690 0.0436(14) 1.0000 Uiso . . . . . . . H181 H -0.0415 0.5805 0.4856 0.0436(14) 1.0000 Uiso . . . . . . . H191 H 0.5741 0.5554 0.3916 0.0436(14) 1.0000 Uiso . . . . . . . H201 H 0.7057 0.7306 0.2221 0.0436(14) 1.0000 Uiso . . . . . . . H202 H 0.8399 0.6844 0.1798 0.0436(14) 1.0000 Uiso . . . . . . . H211 H 0.6148 0.7293 0.0677 0.0436(14) 1.0000 Uiso . . . . . . . H212 H 0.4043 0.7147 0.1155 0.0436(14) 1.0000 Uiso . . . . . . . H213 H 0.5385 0.6686 0.0732 0.0436(14) 1.0000 Uiso . . . . . . . H221 H 0.7960 0.6664 0.5584 0.0436(14) 1.0000 Uiso . . . . . . . H231 H 0.1422 0.7358 0.2703 0.0436(14) 1.0000 Uiso . . . . . . . H241 H 0.3586 0.9481 0.5114 0.0436(14) 1.0000 Uiso . . . . . . . H242 H 0.5695 0.9157 0.4895 0.0436(14) 1.0000 Uiso . . . . . . . H243 H 0.4043 0.8899 0.5514 0.0436(14) 1.0000 Uiso . . . . . . . H251 H 0.0665 0.8266 0.3124 0.0436(14) 1.0000 Uiso . . . . . . . H261 H 0.2841 0.5897 0.1705 0.0436(14) 1.0000 Uiso . . . . . . . H271 H 0.1789 0.6621 0.6564 0.0436(14) 1.0000 Uiso . . . . . . . H281 H 0.7499 0.5723 0.6227 0.0436(14) 1.0000 Uiso . . . . . . . H291 H 0.4522 0.7232 0.5782 0.0436(14) 1.0000 Uiso . . . . . . . H301 H 0.3692 0.5673 0.6836 0.0436(14) 1.0000 Uiso . . . . . . . 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 0.02783(17) 0.02225(15) 0.01832(15) -0.00264(12) 0.00306(11) -0.00123(12) O2 0.0500(10) 0.0210(8) 0.0339(9) -0.0075(6) -0.0070(7) 0.0117(7) O3 0.0421(9) 0.0219(8) 0.0456(10) -0.0080(7) 0.0128(7) -0.0022(6) C4 0.0261(10) 0.0215(9) 0.0174(10) -0.0022(7) 0.0062(8) -0.0029(8) C5 0.0281(10) 0.0175(9) 0.0196(10) 0.0001(7) 0.0002(8) 0.0015(8) C6 0.0218(9) 0.0209(9) 0.0214(10) -0.0022(8) -0.0026(8) -0.0031(8) C7 0.0249(10) 0.0201(10) 0.0165(9) -0.0034(7) -0.0011(7) 0.0002(7) C8 0.0276(11) 0.0285(11) 0.0348(12) -0.0085(9) 0.0028(9) -0.0074(9) C9 0.0235(10) 0.0283(10) 0.0250(11) -0.0043(8) 0.0002(8) 0.0020(8) C10 0.0255(10) 0.0211(10) 0.0339(12) -0.0029(8) -0.0052(9) 0.0028(8) C11 0.0217(9) 0.0184(9) 0.0205(10) -0.0019(7) -0.0037(7) -0.0004(7) C12 0.0255(10) 0.0270(10) 0.0204(10) -0.0013(8) 0.0031(8) -0.0047(8) C13 0.0377(12) 0.0174(9) 0.0228(11) -0.0009(8) -0.0016(9) 0.0056(8) C14 0.0273(11) 0.0292(11) 0.0264(11) 0.0021(9) 0.0070(8) 0.0035(8) C15 0.0444(13) 0.0215(10) 0.0258(11) -0.0036(8) 0.0060(9) -0.0081(9) C16 0.0340(11) 0.0198(10) 0.0233(10) -0.0012(8) 0.0121(8) -0.0022(8) C17 0.0328(11) 0.0222(10) 0.0333(12) -0.0041(9) -0.0082(9) -0.0014(8) C18 0.0272(11) 0.0367(12) 0.0293(12) -0.0068(9) 0.0064(9) -0.0102(9) C19 0.0326(11) 0.0196(10) 0.0213(10) -0.0017(8) 0.0030(8) 0.0015(8) C20 0.0305(11) 0.0250(10) 0.0262(11) -0.0007(8) 0.0020(9) -0.0078(8) C21 0.0441(14) 0.0372(13) 0.0305(13) 0.0048(10) 0.0008(10) -0.0079(10) C22 0.0301(11) 0.0382(13) 0.0319(12) -0.0104(10) -0.0024(9) -0.0018(10) C23 0.0352(12) 0.0267(11) 0.0317(12) -0.0060(9) -0.0146(9) 0.0058(9) C24 0.0551(15) 0.0252(11) 0.0283(12) -0.0071(9) 0.0037(10) 0.0019(10) C25 0.0386(13) 0.0288(11) 0.0350(13) -0.0031(9) -0.0127(10) 0.0120(9) C26 0.0245(10) 0.0277(11) 0.0321(12) -0.0067(9) 0.0007(9) 0.0009(8) C27 0.0376(13) 0.0669(18) 0.0278(13) -0.0194(12) 0.0077(10) -0.0044(12) C28 0.0554(16) 0.0412(14) 0.0303(13) -0.0044(10) -0.0138(11) 0.0125(12) C29 0.0399(13) 0.0312(12) 0.0316(12) -0.0138(9) -0.0027(10) 0.0026(10) C30 0.093(2) 0.0546(17) 0.0162(12) 0.0043(11) -0.0017(13) -0.0313(16) _refine_ls_extinction_coef 160(20) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.5656(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C7 . 2.0994(19) yes Fe1 . C9 . 2.051(2) yes Fe1 . C15 . 2.063(2) yes Fe1 . C18 . 2.056(2) yes Fe1 . C19 . 2.072(2) yes Fe1 . C22 . 2.070(2) yes Fe1 . C27 . 2.062(2) yes Fe1 . C28 . 2.072(2) yes Fe1 . C29 . 2.066(2) yes Fe1 . C30 . 2.053(2) yes O2 . C13 . 1.392(2) yes O2 . C24 . 1.439(3) yes O3 . C16 . 1.383(2) yes O3 . H11 . 0.818 no C4 . C6 . 1.510(3) yes C4 . C12 . 1.398(3) yes C4 . C26 . 1.401(3) yes C5 . C10 . 1.398(3) yes C5 . C11 . 1.512(3) yes C5 . C23 . 1.403(3) yes C6 . C11 . 1.352(3) yes C6 . C20 . 1.530(3) yes C7 . C9 . 1.442(3) yes C7 . C11 . 1.493(3) yes C7 . C19 . 1.442(3) yes C8 . C16 . 1.396(3) yes C8 . C26 . 1.396(3) yes C8 . H81 . 0.969 no C9 . C18 . 1.432(3) yes C9 . H91 . 0.954 no C10 . C17 . 1.406(3) yes C10 . H101 . 0.971 no C12 . C14 . 1.404(3) yes C12 . H121 . 0.950 no C13 . C17 . 1.392(3) yes C13 . C25 . 1.390(3) yes C14 . C16 . 1.392(3) yes C14 . H141 . 0.973 no C15 . C18 . 1.422(3) yes C15 . C19 . 1.431(3) yes C15 . H151 . 0.958 no C17 . H171 . 0.960 no C18 . H181 . 0.960 no C19 . H191 . 0.953 no C20 . C21 . 1.544(3) yes C20 . H201 . 0.964 no C20 . H202 . 0.945 no C21 . H211 . 0.957 no C21 . H212 . 0.934 no C21 . H213 . 0.940 no C22 . C28 . 1.405(4) yes C22 . C29 . 1.411(3) yes C22 . H221 . 0.941 no C23 . C25 . 1.395(3) yes C23 . H231 . 0.970 no C24 . H241 . 0.943 no C24 . H242 . 0.946 no C24 . H243 . 0.960 no C25 . H251 . 0.970 no C26 . H261 . 0.953 no C27 . C29 . 1.409(4) yes C27 . C30 . 1.435(4) yes C27 . H271 . 0.970 no C28 . C30 . 1.426(4) yes C28 . H281 . 0.951 no C29 . H291 . 0.968 no C30 . H301 . 0.975 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 . Fe1 . C9 . 40.64(8) yes C7 . Fe1 . C15 . 68.29(8) yes C9 . Fe1 . C15 . 68.39(9) yes C7 . Fe1 . C18 . 68.34(8) yes C9 . Fe1 . C18 . 40.83(9) yes C15 . Fe1 . C18 . 40.39(9) yes C7 . Fe1 . C19 . 40.43(7) yes C9 . Fe1 . C19 . 68.12(8) yes C15 . Fe1 . C19 . 40.49(8) yes C18 . Fe1 . C19 . 67.95(8) yes C7 . Fe1 . C22 . 112.71(9) yes C9 . Fe1 . C22 . 136.01(9) yes C15 . Fe1 . C22 . 145.91(9) yes C18 . Fe1 . C22 . 173.69(9) yes C19 . Fe1 . C22 . 117.14(9) yes C7 . Fe1 . C27 . 144.66(10) yes C9 . Fe1 . C27 . 113.09(10) yes C15 . Fe1 . C27 . 132.81(10) yes C18 . Fe1 . C27 . 108.12(9) yes C19 . Fe1 . C27 . 172.95(10) yes C7 . Fe1 . C28 . 136.12(10) yes C9 . Fe1 . C28 . 175.32(10) yes C15 . Fe1 . C28 . 114.54(10) yes C18 . Fe1 . C28 . 143.72(11) yes C19 . Fe1 . C28 . 111.46(9) yes C7 . Fe1 . C29 . 116.19(9) yes C9 . Fe1 . C29 . 110.42(9) yes C15 . Fe1 . C29 . 172.22(9) yes C18 . Fe1 . C29 . 133.84(9) yes C19 . Fe1 . C29 . 146.92(9) yes C7 . Fe1 . C30 . 174.46(11) yes C9 . Fe1 . C30 . 143.14(11) yes C15 . Fe1 . C30 . 108.38(10) yes C18 . Fe1 . C30 . 112.27(10) yes C19 . Fe1 . C30 . 134.24(11) yes C22 . Fe1 . C27 . 67.23(9) yes C22 . Fe1 . C28 . 39.66(10) yes C27 . Fe1 . C28 . 67.93(10) yes C22 . Fe1 . C29 . 39.89(9) yes C27 . Fe1 . C29 . 39.92(10) yes C28 . Fe1 . C29 . 67.20(9) yes C22 . Fe1 . C30 . 67.33(10) yes C27 . Fe1 . C30 . 40.82(12) yes C28 . Fe1 . C30 . 40.46(12) yes C29 . Fe1 . C30 . 67.65(10) yes C13 . O2 . C24 . 117.21(16) yes C16 . O3 . H11 . 104.7 no C6 . C4 . C12 . 122.57(17) yes C6 . C4 . C26 . 119.71(17) yes C12 . C4 . C26 . 117.70(18) yes C10 . C5 . C11 . 121.97(17) yes C10 . C5 . C23 . 117.45(18) yes C11 . C5 . C23 . 120.53(17) yes C4 . C6 . C11 . 122.92(17) yes C4 . C6 . C20 . 114.01(16) yes C11 . C6 . C20 . 122.68(18) yes Fe1 . C7 . C9 . 67.87(11) yes Fe1 . C7 . C11 . 130.50(13) yes C9 . C7 . C11 . 124.96(17) yes Fe1 . C7 . C19 . 68.78(11) yes C9 . C7 . C19 . 106.42(17) yes C11 . C7 . C19 . 128.54(17) yes C16 . C8 . C26 . 119.74(18) yes C16 . C8 . H81 . 120.9 no C26 . C8 . H81 . 119.4 no C7 . C9 . Fe1 . 71.49(11) yes C7 . C9 . C18 . 108.59(18) yes Fe1 . C9 . C18 . 69.78(12) yes C7 . C9 . H91 . 126.0 no Fe1 . C9 . H91 . 125.9 no C18 . C9 . H91 . 125.4 no C5 . C10 . C17 . 121.48(18) yes C5 . C10 . H101 . 119.4 no C17 . C10 . H101 . 119.1 no C5 . C11 . C7 . 115.12(16) yes C5 . C11 . C6 . 121.58(18) yes C7 . C11 . C6 . 123.09(17) yes C4 . C12 . C14 . 121.21(18) yes C4 . C12 . H121 . 119.4 no C14 . C12 . H121 . 119.3 no O2 . C13 . C17 . 123.66(18) yes O2 . C13 . C25 . 116.28(18) yes C17 . C13 . C25 . 120.06(18) yes C12 . C14 . C16 . 120.03(18) yes C12 . C14 . H141 . 119.8 no C16 . C14 . H141 . 120.2 no Fe1 . C15 . C18 . 69.56(12) yes Fe1 . C15 . C19 . 70.12(11) yes C18 . C15 . C19 . 107.94(18) yes Fe1 . C15 . H151 . 126.9 no C18 . C15 . H151 . 125.9 no C19 . C15 . H151 . 126.1 no C8 . C16 . C14 . 119.64(18) yes C8 . C16 . O3 . 122.34(18) yes C14 . C16 . O3 . 118.02(18) yes C10 . C17 . C13 . 119.46(18) yes C10 . C17 . H171 . 120.4 no C13 . C17 . H171 . 120.1 no C9 . C18 . C15 . 108.18(18) yes C9 . C18 . Fe1 . 69.40(11) yes C15 . C18 . Fe1 . 70.05(12) yes C9 . C18 . H181 . 126.5 no C15 . C18 . H181 . 125.3 no Fe1 . C18 . H181 . 126.3 no C7 . C19 . C15 . 108.83(17) yes C7 . C19 . Fe1 . 70.79(11) yes C15 . C19 . Fe1 . 69.38(12) yes C7 . C19 . H191 . 125.5 no C15 . C19 . H191 . 125.6 no Fe1 . C19 . H191 . 125.5 no C6 . C20 . C21 . 111.45(16) yes C6 . C20 . H201 . 109.6 no C21 . C20 . H201 . 107.5 no C6 . C20 . H202 . 110.8 no C21 . C20 . H202 . 108.8 no H201 . C20 . H202 . 108.7 no C20 . C21 . H211 . 108.2 no C20 . C21 . H212 . 109.0 no H211 . C21 . H212 . 110.2 no C20 . C21 . H213 . 107.9 no H211 . C21 . H213 . 109.7 no H212 . C21 . H213 . 111.8 no Fe1 . C22 . C28 . 70.25(13) yes Fe1 . C22 . C29 . 69.92(12) yes C28 . C22 . C29 . 108.8(2) yes Fe1 . C22 . H221 . 125.5 no C28 . C22 . H221 . 124.8 no C29 . C22 . H221 . 126.3 no C5 . C23 . C25 . 121.71(19) yes C5 . C23 . H231 . 119.1 no C25 . C23 . H231 . 119.1 no O2 . C24 . H241 . 109.9 no O2 . C24 . H242 . 109.9 no H241 . C24 . H242 . 110.5 no O2 . C24 . H243 . 108.3 no H241 . C24 . H243 . 109.2 no H242 . C24 . H243 . 109.0 no C23 . C25 . C13 . 119.72(19) yes C23 . C25 . H251 . 120.1 no C13 . C25 . H251 . 120.1 no C4 . C26 . C8 . 121.68(19) yes C4 . C26 . H261 . 118.0 no C8 . C26 . H261 . 120.3 no Fe1 . C27 . C29 . 70.23(13) yes Fe1 . C27 . C30 . 69.27(14) yes C29 . C27 . C30 . 107.5(2) yes Fe1 . C27 . H271 . 125.5 no C29 . C27 . H271 . 127.3 no C30 . C27 . H271 . 125.3 no Fe1 . C28 . C22 . 70.09(13) yes Fe1 . C28 . C30 . 69.06(14) yes C22 . C28 . C30 . 107.7(2) yes Fe1 . C28 . H281 . 126.1 no C22 . C28 . H281 . 126.5 no C30 . C28 . H281 . 125.8 no C22 . C29 . C27 . 108.4(2) yes C22 . C29 . Fe1 . 70.19(12) yes C27 . C29 . Fe1 . 69.86(13) yes C22 . C29 . H291 . 124.9 no C27 . C29 . H291 . 126.7 no Fe1 . C29 . H291 . 126.0 no C27 . C30 . C28 . 107.6(2) yes C27 . C30 . Fe1 . 69.91(14) yes C28 . C30 . Fe1 . 70.49(14) yes C27 . C30 . H301 . 127.5 no C28 . C30 . H301 . 124.9 no Fe1 . C30 . H301 . 125.8 no #===END data_mjm302(3) _database_code_depnum_ccdc_archive 'CCDC 738757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 O3 Fe' _chemical_formula_sum 'C26 H24 O3 Fe' _chemical_formula_weight 440.30 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 'P 21/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 9.1008(4) _cell_length_b 10.2954(4) _cell_length_c 21.5897(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.042(1) _cell_angle_gamma 90.00 _cell_volume 1985.43(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9193 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 31.40 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6206 _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) for selected reflections was 0.030 before and 0.020 after correction. The Ratio of minimum to maximum transmission is 0.834279. The \l/2 correction factor is 0.0015 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22874 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0227 _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 -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 31.60 _reflns_number_total 6227 _reflns_number_gt 5408 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0762P)^2^+0.8026P] 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 6227 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.003 _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 Fe Fe -0.25978(2) 0.79214(2) 0.858314(9) 0.01694(8) Uani 1 1 d . . . C1 C -0.27590(18) 0.84254(16) 0.76520(7) 0.0223(3) Uani 1 1 d . . . H1 H -0.2139 0.9020 0.7485 0.027 Uiso 1 1 calc R . . C2 C -0.40926(19) 0.87392(17) 0.78615(8) 0.0262(3) Uani 1 1 d . . . H2 H -0.4514 0.9583 0.7864 0.031 Uiso 1 1 calc R . . C3 C -0.46977(18) 0.75821(19) 0.80681(8) 0.0257(3) Uani 1 1 d . . . H3 H -0.5597 0.7512 0.8228 0.031 Uiso 1 1 calc R . . C4 C -0.37070(18) 0.65406(16) 0.79916(8) 0.0246(3) Uani 1 1 d . . . H4 H -0.3830 0.5655 0.8094 0.030 Uiso 1 1 calc R . . C5 C -0.25006(18) 0.70648(15) 0.77340(7) 0.0213(3) Uani 1 1 d . . . H5 H -0.1678 0.6594 0.7635 0.026 Uiso 1 1 calc R . . C6 C -0.11087(18) 0.91245(17) 0.91425(8) 0.0238(3) Uani 1 1 d . . . H6 H -0.0601 0.9849 0.9010 0.029 Uiso 1 1 calc R . . C7 C -0.2529(2) 0.9162(2) 0.93245(8) 0.0311(4) Uani 1 1 d . . . H7 H -0.3138 0.9911 0.9328 0.037 Uiso 1 1 calc R . . C8 C -0.2877(2) 0.7898(2) 0.94990(8) 0.0319(4) Uani 1 1 d . . . H8 H -0.3757 0.7648 0.9645 0.038 Uiso 1 1 calc R . . C9 C -0.16810(19) 0.70541(18) 0.94189(7) 0.0261(3) Uani 1 1 d . . . H9 H -0.1629 0.6147 0.9502 0.031 Uiso 1 1 calc R . . C10 C -0.05698(17) 0.78127(15) 0.91918(7) 0.0186(3) Uani 1 1 d . . . C11 C 0.10201(15) 0.74352(14) 0.91282(6) 0.0150(2) Uani 1 1 d . . . C12 C 0.17144(15) 0.85530(13) 0.88144(6) 0.0145(2) Uani 1 1 d . . . C13 C 0.27841(18) 0.93836(15) 0.91554(6) 0.0200(3) Uani 1 1 d . . . H13 H 0.3126 0.9234 0.9594 0.024 Uiso 1 1 calc R . . C14 C 0.33623(19) 1.04265(16) 0.88683(7) 0.0233(3) Uani 1 1 d . . . H14 H 0.4079 1.0989 0.9110 0.028 Uiso 1 1 calc R . . C15 C 0.28838(17) 1.06377(14) 0.82274(7) 0.0194(3) Uani 1 1 d . . . O1 O 0.35018(17) 1.16552(12) 0.79550(5) 0.0310(3) Uani 1 1 d . . . H1O1 H 0.3299 1.1578 0.7560 0.047 Uiso 1 1 calc R . . C16 C 0.18038(16) 0.98391(14) 0.78762(6) 0.0164(2) Uani 1 1 d . . . H16 H 0.1471 0.9989 0.7438 0.020 Uiso 1 1 calc R . . C17 C 0.12172(15) 0.88215(14) 0.81728(6) 0.0147(2) Uani 1 1 d . . . H17 H 0.0458 0.8293 0.7934 0.018 Uiso 1 1 calc R . . C18 C 0.19723(16) 0.71466(14) 0.97835(6) 0.0172(3) Uani 1 1 d . . . C19 C 0.1554(2) 0.75412(19) 1.03384(7) 0.0269(3) Uani 1 1 d . . . H19 H 0.0624 0.7974 1.0321 0.032 Uiso 1 1 calc R . . C20 C 0.2480(2) 0.73118(19) 1.09237(8) 0.0325(4) Uani 1 1 d . . . H20 H 0.2179 0.7592 1.1300 0.039 Uiso 1 1 calc R . . C21 C 0.3824(2) 0.66818(17) 1.09567(7) 0.0272(4) Uani 1 1 d . . . O2 O 0.47175(18) 0.63855(14) 1.15302(6) 0.0412(4) Uani 1 1 d . . . H2O2 H 0.5192 0.7051 1.1678 0.062 Uiso 1 1 calc R . . C22 C 0.4258(2) 0.6284(2) 1.04077(9) 0.0362(4) Uani 1 1 d . . . H22 H 0.5184 0.5844 1.0427 0.043 Uiso 1 1 calc R . . C23 C 0.33378(19) 0.6528(2) 0.98247(8) 0.0306(4) Uani 1 1 d . . . H23 H 0.3653 0.6264 0.9449 0.037 Uiso 1 1 calc R . . C24 C 0.10626(17) 0.61656(14) 0.87438(7) 0.0189(3) Uani 1 1 d . . . O3 O 0.16807(16) 0.61324(12) 0.82924(6) 0.0289(3) Uani 1 1 d . . . C25 C 0.04065(19) 0.49271(15) 0.89500(7) 0.0232(3) Uani 1 1 d . . . H25A H -0.0668 0.4882 0.8753 0.028 Uiso 1 1 calc R . . H25B H 0.0482 0.4946 0.9413 0.028 Uiso 1 1 calc R . . C26 C 0.1193(2) 0.37170(16) 0.87713(9) 0.0299(3) Uani 1 1 d . . . H26A H 0.1125 0.3695 0.8313 0.045 Uiso 1 1 calc R . . H26B H 0.0711 0.2942 0.8905 0.045 Uiso 1 1 calc R . . H26C H 0.2247 0.3735 0.8981 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.01468(12) 0.02235(13) 0.01413(12) -0.00125(7) 0.00362(8) -0.00145(7) C1 0.0249(7) 0.0267(7) 0.0150(6) 0.0033(5) 0.0033(5) -0.0010(6) C2 0.0224(7) 0.0304(8) 0.0242(7) 0.0038(6) 0.0004(6) 0.0043(6) C3 0.0153(6) 0.0374(9) 0.0234(7) 0.0001(6) 0.0013(5) -0.0035(6) C4 0.0239(7) 0.0254(7) 0.0230(7) -0.0027(6) 0.0007(6) -0.0058(6) C5 0.0217(7) 0.0257(7) 0.0153(6) -0.0030(5) 0.0007(5) 0.0003(5) C6 0.0203(7) 0.0292(8) 0.0225(7) -0.0124(6) 0.0058(6) -0.0025(6) C7 0.0238(8) 0.0448(10) 0.0266(8) -0.0157(7) 0.0098(6) 0.0012(7) C8 0.0216(8) 0.0584(12) 0.0182(7) -0.0025(7) 0.0099(6) -0.0030(7) C9 0.0202(7) 0.0428(10) 0.0157(7) 0.0059(6) 0.0050(5) -0.0046(6) C10 0.0156(6) 0.0298(7) 0.0104(6) -0.0005(5) 0.0028(5) -0.0030(5) C11 0.0144(6) 0.0213(6) 0.0090(5) 0.0003(5) 0.0015(4) -0.0032(5) C12 0.0144(6) 0.0196(6) 0.0096(5) 0.0000(4) 0.0024(4) -0.0009(5) C13 0.0255(7) 0.0241(7) 0.0091(5) 0.0007(5) -0.0001(5) -0.0058(6) C14 0.0316(8) 0.0242(7) 0.0118(6) 0.0000(5) -0.0012(5) -0.0104(6) C15 0.0264(7) 0.0190(6) 0.0121(6) 0.0012(5) 0.0024(5) -0.0047(5) O1 0.0510(8) 0.0271(6) 0.0124(5) 0.0033(4) -0.0004(5) -0.0196(6) C16 0.0188(6) 0.0199(6) 0.0096(5) 0.0008(4) 0.0008(4) 0.0001(5) C17 0.0132(5) 0.0207(6) 0.0097(5) -0.0005(4) 0.0007(4) -0.0008(5) C18 0.0168(6) 0.0226(7) 0.0109(6) 0.0028(4) -0.0008(5) -0.0060(5) C19 0.0318(8) 0.0355(8) 0.0118(6) -0.0010(6) 0.0001(6) 0.0032(7) C20 0.0466(11) 0.0359(9) 0.0115(6) -0.0012(6) -0.0032(7) -0.0008(8) C21 0.0306(8) 0.0273(7) 0.0179(7) 0.0100(6) -0.0099(6) -0.0159(6) O2 0.0483(8) 0.0386(7) 0.0251(6) 0.0166(5) -0.0221(6) -0.0227(6) C22 0.0238(8) 0.0557(12) 0.0263(8) 0.0170(8) -0.0021(6) 0.0034(8) C23 0.0225(7) 0.0504(11) 0.0182(7) 0.0107(7) 0.0024(6) 0.0065(7) C24 0.0220(7) 0.0210(6) 0.0129(6) 0.0008(5) 0.0011(5) -0.0019(5) O3 0.0476(7) 0.0240(5) 0.0187(5) 0.0011(4) 0.0156(5) 0.0026(5) C25 0.0286(7) 0.0217(7) 0.0184(7) 0.0022(5) 0.0021(6) -0.0053(6) C26 0.0362(9) 0.0218(7) 0.0298(8) 0.0014(6) 0.0013(7) -0.0018(6) _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 Fe C7 2.0396(17) . ? Fe C8 2.0416(17) . ? Fe C9 2.0427(16) . ? Fe C2 2.0432(16) . ? Fe C4 2.0438(16) . ? Fe C3 2.0486(16) . ? Fe C6 2.0499(16) . ? Fe C5 2.0514(15) . ? Fe C10 2.0535(15) . ? Fe C1 2.0540(15) . ? C1 C2 1.411(2) . ? C1 C5 1.426(2) . ? C1 H1 0.9500 . ? C2 C3 1.420(2) . ? C2 H2 0.9500 . ? C3 C4 1.431(2) . ? C3 H3 0.9500 . ? C4 C5 1.428(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.422(2) . ? C6 C10 1.434(2) . ? C6 H6 0.9500 . ? C7 C8 1.408(3) . ? C7 H7 0.9500 . ? C8 C9 1.429(3) . ? C8 H8 0.9500 . ? C9 C10 1.436(2) . ? C9 H9 0.9500 . ? C10 C11 1.530(2) . ? C11 C12 1.5318(19) . ? C11 C18 1.5399(18) . ? C11 C24 1.553(2) . ? C12 C13 1.3952(19) . ? C12 C17 1.4000(17) . ? C13 C14 1.393(2) . ? C13 H13 0.9500 . ? C14 C15 1.3857(19) . ? C14 H14 0.9500 . ? C15 O1 1.3735(18) . ? C15 C16 1.390(2) . ? O1 H1O1 0.8400 . ? C16 C17 1.3869(19) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.384(2) . ? C18 C19 1.386(2) . ? C19 C20 1.398(2) . ? C19 H19 0.9500 . ? C20 C21 1.374(3) . ? C20 H20 0.9500 . ? C21 O2 1.3791(18) . ? C21 C22 1.382(3) . ? O2 H2O2 0.8400 . ? C22 C23 1.395(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O3 1.2155(18) . ? C24 C25 1.511(2) . ? C25 C26 1.523(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 C7 Fe C8 40.37(8) . . ? C7 Fe C9 68.57(8) . . ? C8 Fe C9 40.96(7) . . ? C7 Fe C2 104.84(8) . . ? C8 Fe C2 123.72(7) . . ? C9 Fe C2 162.42(7) . . ? C7 Fe C4 149.68(7) . . ? C8 Fe C4 117.29(7) . . ? C9 Fe C4 108.50(7) . . ? C2 Fe C4 68.48(7) . . ? C7 Fe C3 114.69(7) . . ? C8 Fe C3 104.31(7) . . ? C9 Fe C3 125.85(7) . . ? C2 Fe C3 40.60(7) . . ? C4 Fe C3 40.93(7) . . ? C7 Fe C6 40.70(6) . . ? C8 Fe C6 68.14(7) . . ? C9 Fe C6 68.39(7) . . ? C2 Fe C6 117.95(7) . . ? C4 Fe C6 168.54(7) . . ? C3 Fe C6 149.94(7) . . ? C7 Fe C5 166.06(8) . . ? C8 Fe C5 153.52(7) . . ? C9 Fe C5 121.42(7) . . ? C2 Fe C5 68.41(7) . . ? C4 Fe C5 40.82(6) . . ? C3 Fe C5 68.72(7) . . ? C6 Fe C5 130.50(6) . . ? C7 Fe C10 69.10(7) . . ? C8 Fe C10 69.09(7) . . ? C9 Fe C10 41.05(6) . . ? C2 Fe C10 153.63(7) . . ? C4 Fe C10 129.63(7) . . ? C3 Fe C10 165.64(7) . . ? C6 Fe C10 40.90(6) . . ? C5 Fe C10 111.17(6) . . ? C7 Fe C1 126.55(8) . . ? C8 Fe C1 162.20(7) . . ? C9 Fe C1 156.28(7) . . ? C2 Fe C1 40.30(7) . . ? C4 Fe C1 68.29(7) . . ? C3 Fe C1 68.13(7) . . ? C6 Fe C1 109.82(7) . . ? C5 Fe C1 40.64(6) . . ? C10 Fe C1 121.81(6) . . ? C2 C1 C5 108.45(14) . . ? C2 C1 Fe 69.44(9) . . ? C5 C1 Fe 69.58(8) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe C1 H1 126.8 . . ? C1 C2 C3 108.53(15) . . ? C1 C2 Fe 70.26(9) . . ? C3 C2 Fe 69.90(9) . . ? C1 C2 H2 125.7 . . ? C3 C2 H2 125.7 . . ? Fe C2 H2 125.7 . . ? C2 C3 C4 107.55(14) . . ? C2 C3 Fe 69.50(9) . . ? C4 C3 Fe 69.36(9) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Fe C3 H3 126.5 . . ? C5 C4 C3 108.07(15) . . ? C5 C4 Fe 69.88(9) . . ? C3 C4 Fe 69.72(9) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Fe C4 H4 126.0 . . ? C1 C5 C4 107.39(14) . . ? C1 C5 Fe 69.77(9) . . ? C4 C5 Fe 69.30(9) . . ? C1 C5 H5 126.3 . . ? C4 C5 H5 126.3 . . ? Fe C5 H5 126.2 . . ? C7 C6 C10 108.75(16) . . ? C7 C6 Fe 69.26(9) . . ? C10 C6 Fe 69.68(9) . . ? C7 C6 H6 125.6 . . ? C10 C6 H6 125.6 . . ? Fe C6 H6 127.0 . . ? C8 C7 C6 108.15(16) . . ? C8 C7 Fe 69.89(10) . . ? C6 C7 Fe 70.04(9) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 125.7 . . ? C7 C8 C9 108.30(15) . . ? C7 C8 Fe 69.74(10) . . ? C9 C8 Fe 69.56(9) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe C8 H8 126.4 . . ? C8 C9 C10 108.27(16) . . ? C8 C9 Fe 69.48(10) . . ? C10 C9 Fe 69.88(9) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 126.4 . . ? C6 C10 C9 106.52(14) . . ? C6 C10 C11 123.28(13) . . ? C9 C10 C11 129.23(14) . . ? C6 C10 Fe 69.41(9) . . ? C9 C10 Fe 69.07(9) . . ? C11 C10 Fe 134.91(10) . . ? C10 C11 C12 109.04(12) . . ? C10 C11 C18 110.00(11) . . ? C12 C11 C18 110.13(11) . . ? C10 C11 C24 112.50(12) . . ? C12 C11 C24 109.97(11) . . ? C18 C11 C24 105.15(11) . . ? C13 C12 C17 117.50(13) . . ? C13 C12 C11 122.16(12) . . ? C17 C12 C11 120.23(12) . . ? C14 C13 C12 121.51(13) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 119.49(14) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? O1 C15 C14 118.11(13) . . ? O1 C15 C16 121.49(13) . . ? C14 C15 C16 120.41(13) . . ? C15 O1 H1O1 109.5 . . ? C17 C16 C15 119.30(12) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C12 121.74(12) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? C23 C18 C19 118.14(14) . . ? C23 C18 C11 119.22(13) . . ? C19 C18 C11 122.56(14) . . ? C18 C19 C20 120.91(17) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 120.22(17) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 O2 121.14(18) . . ? C20 C21 C22 119.59(15) . . ? O2 C21 C22 119.21(18) . . ? C21 O2 H2O2 109.5 . . ? C21 C22 C23 119.97(18) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 121.17(17) . . ? C18 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? O3 C24 C25 118.83(14) . . ? O3 C24 C11 120.99(13) . . ? C25 C24 C11 120.09(12) . . ? C24 C25 C26 112.61(14) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 C7 Fe C1 C2 -67.58(13) . . . . ? C8 Fe C1 C2 -30.1(3) . . . . ? C9 Fe C1 C2 168.60(16) . . . . ? C4 Fe C1 C2 81.90(11) . . . . ? C3 Fe C1 C2 37.66(11) . . . . ? C6 Fe C1 C2 -110.19(11) . . . . ? C5 Fe C1 C2 120.02(14) . . . . ? C10 Fe C1 C2 -153.99(10) . . . . ? C7 Fe C1 C5 172.40(10) . . . . ? C8 Fe C1 C5 -150.1(2) . . . . ? C9 Fe C1 C5 48.6(2) . . . . ? C2 Fe C1 C5 -120.02(14) . . . . ? C4 Fe C1 C5 -38.13(10) . . . . ? C3 Fe C1 C5 -82.36(11) . . . . ? C6 Fe C1 C5 129.78(10) . . . . ? C10 Fe C1 C5 85.99(11) . . . . ? C5 C1 C2 C3 -0.84(18) . . . . ? Fe C1 C2 C3 -59.65(11) . . . . ? C5 C1 C2 Fe 58.80(11) . . . . ? C7 Fe C2 C1 129.81(11) . . . . ? C8 Fe C2 C1 169.39(10) . . . . ? C9 Fe C2 C1 -164.7(2) . . . . ? C4 Fe C2 C1 -81.38(11) . . . . ? C3 Fe C2 C1 -119.40(15) . . . . ? C6 Fe C2 C1 88.16(11) . . . . ? C5 Fe C2 C1 -37.34(10) . . . . ? C10 Fe C2 C1 57.05(19) . . . . ? C7 Fe C2 C3 -110.80(11) . . . . ? C8 Fe C2 C3 -71.22(13) . . . . ? C9 Fe C2 C3 -45.3(3) . . . . ? C4 Fe C2 C3 38.01(10) . . . . ? C6 Fe C2 C3 -152.44(10) . . . . ? C5 Fe C2 C3 82.06(11) . . . . ? C10 Fe C2 C3 176.44(13) . . . . ? C1 Fe C2 C3 119.40(15) . . . . ? C1 C2 C3 C4 0.74(18) . . . . ? Fe C2 C3 C4 -59.13(11) . . . . ? C1 C2 C3 Fe 59.87(11) . . . . ? C7 Fe C3 C2 84.06(12) . . . . ? C8 Fe C3 C2 125.64(11) . . . . ? C9 Fe C3 C2 164.63(10) . . . . ? C4 Fe C3 C2 -119.01(14) . . . . ? C6 Fe C3 C2 54.68(17) . . . . ? C5 Fe C3 C2 -81.24(10) . . . . ? C10 Fe C3 C2 -173.6(2) . . . . ? C1 Fe C3 C2 -37.39(10) . . . . ? C7 Fe C3 C4 -156.93(10) . . . . ? C8 Fe C3 C4 -115.35(11) . . . . ? C9 Fe C3 C4 -76.36(12) . . . . ? C2 Fe C3 C4 119.01(14) . . . . ? C6 Fe C3 C4 173.69(13) . . . . ? C5 Fe C3 C4 37.77(9) . . . . ? C10 Fe C3 C4 -54.6(3) . . . . ? C1 Fe C3 C4 81.62(10) . . . . ? C2 C3 C4 C5 -0.36(18) . . . . ? Fe C3 C4 C5 -59.57(11) . . . . ? C2 C3 C4 Fe 59.22(11) . . . . ? C7 Fe C4 C5 164.04(14) . . . . ? C8 Fe C4 C5 -160.63(10) . . . . ? C9 Fe C4 C5 -116.98(10) . . . . ? C2 Fe C4 C5 81.47(10) . . . . ? C3 Fe C4 C5 119.19(14) . . . . ? C6 Fe C4 C5 -44.7(4) . . . . ? C10 Fe C4 C5 -76.04(11) . . . . ? C1 Fe C4 C5 37.97(9) . . . . ? C7 Fe C4 C3 44.86(19) . . . . ? C8 Fe C4 C3 80.18(12) . . . . ? C9 Fe C4 C3 123.84(10) . . . . ? C2 Fe C4 C3 -37.72(10) . . . . ? C6 Fe C4 C3 -163.9(3) . . . . ? C5 Fe C4 C3 -119.19(14) . . . . ? C10 Fe C4 C3 164.78(9) . . . . ? C1 Fe C4 C3 -81.22(10) . . . . ? C2 C1 C5 C4 0.61(17) . . . . ? Fe C1 C5 C4 59.33(11) . . . . ? C2 C1 C5 Fe -58.72(11) . . . . ? C3 C4 C5 C1 -0.16(17) . . . . ? Fe C4 C5 C1 -59.63(10) . . . . ? C3 C4 C5 Fe 59.48(11) . . . . ? C7 Fe C5 C1 -26.2(3) . . . . ? C8 Fe C5 C1 160.03(14) . . . . ? C9 Fe C5 C1 -159.30(9) . . . . ? C2 Fe C5 C1 37.03(10) . . . . ? C4 Fe C5 C1 118.66(14) . . . . ? C3 Fe C5 C1 80.80(10) . . . . ? C6 Fe C5 C1 -71.93(12) . . . . ? C10 Fe C5 C1 -114.62(10) . . . . ? C7 Fe C5 C4 -144.8(3) . . . . ? C8 Fe C5 C4 41.37(19) . . . . ? C9 Fe C5 C4 82.04(11) . . . . ? C2 Fe C5 C4 -81.63(10) . . . . ? C3 Fe C5 C4 -37.86(10) . . . . ? C6 Fe C5 C4 169.41(10) . . . . ? C10 Fe C5 C4 126.72(10) . . . . ? C1 Fe C5 C4 -118.66(14) . . . . ? C8 Fe C6 C7 -37.59(12) . . . . ? C9 Fe C6 C7 -81.84(12) . . . . ? C2 Fe C6 C7 80.08(13) . . . . ? C4 Fe C6 C7 -158.1(3) . . . . ? C3 Fe C6 C7 43.12(19) . . . . ? C5 Fe C6 C7 164.65(11) . . . . ? C10 Fe C6 C7 -120.44(15) . . . . ? C1 Fe C6 C7 123.48(12) . . . . ? C7 Fe C6 C10 120.44(15) . . . . ? C8 Fe C6 C10 82.86(10) . . . . ? C9 Fe C6 C10 38.61(9) . . . . ? C2 Fe C6 C10 -159.48(9) . . . . ? C4 Fe C6 C10 -37.7(4) . . . . ? C3 Fe C6 C10 163.57(12) . . . . ? C5 Fe C6 C10 -74.91(12) . . . . ? C1 Fe C6 C10 -116.07(9) . . . . ? C10 C6 C7 C8 1.10(19) . . . . ? Fe C6 C7 C8 59.73(12) . . . . ? C10 C6 C7 Fe -58.63(11) . . . . ? C9 Fe C7 C8 -37.73(11) . . . . ? C2 Fe C7 C8 125.10(11) . . . . ? C4 Fe C7 C8 52.5(2) . . . . ? C3 Fe C7 C8 83.06(12) . . . . ? C6 Fe C7 C8 -119.08(16) . . . . ? C5 Fe C7 C8 -175.7(3) . . . . ? C10 Fe C7 C8 -81.90(11) . . . . ? C1 Fe C7 C8 163.31(10) . . . . ? C8 Fe C7 C6 119.08(16) . . . . ? C9 Fe C7 C6 81.34(12) . . . . ? C2 Fe C7 C6 -115.82(11) . . . . ? C4 Fe C7 C6 171.57(13) . . . . ? C3 Fe C7 C6 -157.86(11) . . . . ? C5 Fe C7 C6 -56.7(3) . . . . ? C10 Fe C7 C6 37.17(10) . . . . ? C1 Fe C7 C6 -77.62(13) . . . . ? C6 C7 C8 C9 -0.8(2) . . . . ? Fe C7 C8 C9 59.07(12) . . . . ? C6 C7 C8 Fe -59.82(12) . . . . ? C9 Fe C8 C7 119.65(15) . . . . ? C2 Fe C8 C7 -71.96(13) . . . . ? C4 Fe C8 C7 -153.22(11) . . . . ? C3 Fe C8 C7 -111.44(11) . . . . ? C6 Fe C8 C7 37.89(11) . . . . ? C5 Fe C8 C7 177.70(14) . . . . ? C10 Fe C8 C7 81.95(11) . . . . ? C1 Fe C8 C7 -49.0(3) . . . . ? C7 Fe C8 C9 -119.65(15) . . . . ? C2 Fe C8 C9 168.40(10) . . . . ? C4 Fe C8 C9 87.14(12) . . . . ? C3 Fe C8 C9 128.91(11) . . . . ? C6 Fe C8 C9 -81.76(11) . . . . ? C5 Fe C8 C9 58.05(19) . . . . ? C10 Fe C8 C9 -37.69(10) . . . . ? C1 Fe C8 C9 -168.7(2) . . . . ? C7 C8 C9 C10 0.13(19) . . . . ? Fe C8 C9 C10 59.31(11) . . . . ? C7 C8 C9 Fe -59.18(12) . . . . ? C7 Fe C9 C8 37.21(11) . . . . ? C2 Fe C9 C8 -33.6(3) . . . . ? C4 Fe C9 C8 -110.63(11) . . . . ? C3 Fe C9 C8 -68.46(13) . . . . ? C6 Fe C9 C8 81.12(11) . . . . ? C5 Fe C9 C8 -153.68(11) . . . . ? C10 Fe C9 C8 119.58(15) . . . . ? C1 Fe C9 C8 171.41(16) . . . . ? C7 Fe C9 C10 -82.37(10) . . . . ? C8 Fe C9 C10 -119.58(15) . . . . ? C2 Fe C9 C10 -153.2(2) . . . . ? C4 Fe C9 C10 129.79(10) . . . . ? C3 Fe C9 C10 171.96(9) . . . . ? C6 Fe C9 C10 -38.47(9) . . . . ? C5 Fe C9 C10 86.74(11) . . . . ? C1 Fe C9 C10 51.8(2) . . . . ? C7 C6 C10 C9 -1.00(18) . . . . ? Fe C6 C10 C9 -59.37(10) . . . . ? C7 C6 C10 C11 -170.66(13) . . . . ? Fe C6 C10 C11 130.97(13) . . . . ? C7 C6 C10 Fe 58.37(11) . . . . ? C8 C9 C10 C6 0.54(18) . . . . ? Fe C9 C10 C6 59.60(10) . . . . ? C8 C9 C10 C11 169.36(14) . . . . ? Fe C9 C10 C11 -131.58(15) . . . . ? C8 C9 C10 Fe -59.06(12) . . . . ? C7 Fe C10 C6 -37.00(10) . . . . ? C8 Fe C10 C6 -80.35(11) . . . . ? C9 Fe C10 C6 -117.96(13) . . . . ? C2 Fe C10 C6 44.20(18) . . . . ? C4 Fe C10 C6 170.93(10) . . . . ? C3 Fe C10 C6 -145.2(2) . . . . ? C5 Fe C10 C6 128.06(9) . . . . ? C1 Fe C10 C6 83.89(11) . . . . ? C7 Fe C10 C9 80.96(11) . . . . ? C8 Fe C10 C9 37.61(11) . . . . ? C2 Fe C10 C9 162.16(14) . . . . ? C4 Fe C10 C9 -71.11(12) . . . . ? C3 Fe C10 C9 -27.2(3) . . . . ? C6 Fe C10 C9 117.96(13) . . . . ? C5 Fe C10 C9 -113.98(10) . . . . ? C1 Fe C10 C9 -158.15(10) . . . . ? C7 Fe C10 C11 -153.94(17) . . . . ? C8 Fe C10 C11 162.70(17) . . . . ? C9 Fe C10 C11 125.09(19) . . . . ? C2 Fe C10 C11 -72.7(2) . . . . ? C4 Fe C10 C11 53.98(17) . . . . ? C3 Fe C10 C11 97.9(3) . . . . ? C6 Fe C10 C11 -116.95(18) . . . . ? C5 Fe C10 C11 11.11(17) . . . . ? C1 Fe C10 C11 -33.06(18) . . . . ? C6 C10 C11 C12 -17.12(18) . . . . ? C9 C10 C11 C12 175.72(14) . . . . ? Fe C10 C11 C12 76.35(17) . . . . ? C6 C10 C11 C18 103.75(16) . . . . ? C9 C10 C11 C18 -63.41(19) . . . . ? Fe C10 C11 C18 -162.79(12) . . . . ? C6 C10 C11 C24 -139.39(14) . . . . ? C9 C10 C11 C24 53.44(19) . . . . ? Fe C10 C11 C24 -45.93(19) . . . . ? C10 C11 C12 C13 104.44(15) . . . . ? C18 C11 C12 C13 -16.34(19) . . . . ? C24 C11 C12 C13 -131.76(14) . . . . ? C10 C11 C12 C17 -71.62(16) . . . . ? C18 C11 C12 C17 167.59(13) . . . . ? C24 C11 C12 C17 52.17(17) . . . . ? C17 C12 C13 C14 -1.3(2) . . . . ? C11 C12 C13 C14 -177.45(14) . . . . ? C12 C13 C14 C15 -0.9(3) . . . . ? C13 C14 C15 O1 -178.43(15) . . . . ? C13 C14 C15 C16 1.8(2) . . . . ? O1 C15 C16 C17 179.80(14) . . . . ? C14 C15 C16 C17 -0.5(2) . . . . ? C15 C16 C17 C12 -1.8(2) . . . . ? C13 C12 C17 C16 2.7(2) . . . . ? C11 C12 C17 C16 178.92(13) . . . . ? C10 C11 C18 C23 166.45(15) . . . . ? C12 C11 C18 C23 -73.34(18) . . . . ? C24 C11 C18 C23 45.09(18) . . . . ? C10 C11 C18 C19 -16.9(2) . . . . ? C12 C11 C18 C19 103.29(16) . . . . ? C24 C11 C18 C19 -138.29(15) . . . . ? C23 C18 C19 C20 -0.5(3) . . . . ? C11 C18 C19 C20 -177.12(16) . . . . ? C18 C19 C20 C21 -0.3(3) . . . . ? C19 C20 C21 O2 -176.57(17) . . . . ? C19 C20 C21 C22 0.4(3) . . . . ? C20 C21 C22 C23 0.3(3) . . . . ? O2 C21 C22 C23 177.33(17) . . . . ? C19 C18 C23 C22 1.2(3) . . . . ? C11 C18 C23 C22 177.95(17) . . . . ? C21 C22 C23 C18 -1.1(3) . . . . ? C10 C11 C24 O3 126.68(15) . . . . ? C12 C11 C24 O3 4.93(19) . . . . ? C18 C11 C24 O3 -113.60(16) . . . . ? C10 C11 C24 C25 -56.78(17) . . . . ? C12 C11 C24 C25 -178.53(12) . . . . ? C18 C11 C24 C25 62.94(16) . . . . ? O3 C24 C25 C26 26.5(2) . . . . ? C11 C24 C25 C26 -150.10(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O1 O3 0.84 1.90 2.7199(16) 164.6 2_556 O2 H2O2 O1 0.84 1.86 2.6908(17) 170.8 3_677 _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.865 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.103