# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 loop_ _publ_author_name O.Joseph 'Kim K. Baldridge' 'Kevin Bunker' 'Adam Closson' 'Bernadette T. Donovan-Merkert' ; M.Fouzi ; 'Daniel Frandrick' 'Peter Gantzel' 'Linda I. Lee' 'Tuan Tran' _publ_contact_author_name ; Prof Joseph O'Connor ; _publ_contact_author_address ; Chemistry and Biochemistry University of California, 9500 Gilman Drive La Jolla CA 92093-0358 UNITED STATES OF AMERICA ; _publ_contact_author_email JMOCONNO@UCSD.EDU _publ_section_title ; Ring-strain effects on the oxidation potential of enediynes and enediyne complexes ; data_h _database_code_CSD 170841 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H16 Fe' _chemical_formula_weight 288.16 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.295(3) _cell_length_b 18.220(8) _cell_length_c 20.779(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.67(3) _cell_angle_gamma 90.00 _cell_volume 2748.6(19) _cell_formula_units_Z 8 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method ? _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3915 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3593 _reflns_number_observed 2424 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+5.2012P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3593 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_obs 0.0544 _refine_ls_wR_factor_all 0.1308 _refine_ls_wR_factor_obs 0.1082 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max -0.015 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.14336(12) 0.78071(5) 0.35723(4) 0.0306(3) Uani 1 d . . C1 C 0.1518(8) 0.8551(3) 0.4306(3) 0.0302(15) Uani 1 d . . C2 C 0.2641(8) 0.7942(4) 0.4496(3) 0.037(2) Uani 1 d . . H2A H 0.2507(8) 0.7632(4) 0.4862(3) 0.044 Uiso 1 d R . C3 C 0.4000(9) 0.7882(4) 0.4061(3) 0.045(2) Uani 1 d . . H3A H 0.4950(9) 0.7516(4) 0.4078(3) 0.054 Uiso 1 d R . C4 C 0.3730(9) 0.8436(4) 0.3584(4) 0.049(2) Uani 1 d . . H4A H 0.4450(9) 0.8519(4) 0.3228(4) 0.059 Uiso 1 d R . C5 C 0.2180(8) 0.8864(3) 0.3731(3) 0.035(2) Uani 1 d . . C6 C 0.1275(9) 0.9490(4) 0.3432(3) 0.038(2) Uani 1 d . . C7 C 0.0247(10) 0.9993(4) 0.3318(3) 0.039(2) Uani 1 d . . C8 C -0.1066(10) 1.0605(4) 0.3260(3) 0.045(2) Uani 1 d . . H8A H -0.1998(10) 1.0517(4) 0.2888(3) 0.054 Uiso 1 calc R . H8B H -0.0408(10) 1.1065(4) 0.3178(3) 0.054 Uiso 1 calc R . C9 C -0.2035(9) 1.0687(3) 0.3881(3) 0.039(2) Uani 1 d . . H9A H -0.2666(9) 1.1168(3) 0.3870(3) 0.047 Uiso 1 calc R . H9B H -0.1087(9) 1.0689(3) 0.4256(3) 0.047 Uiso 1 calc R . C10 C -0.3454(9) 1.0082(4) 0.3985(3) 0.040(2) Uani 1 d . . H10A H -0.4693(9) 1.0308(4) 0.3963(3) 0.049 Uiso 1 calc R . H10B H -0.3461(9) 0.9724(4) 0.3626(3) 0.049 Uiso 1 calc R . C11 C -0.3094(9) 0.9671(4) 0.4627(3) 0.043(2) Uani 1 d . . H11A H -0.2925(9) 1.0027(4) 0.4988(3) 0.051 Uiso 1 calc R . H11B H -0.4166(9) 0.9357(4) 0.4695(3) 0.051 Uiso 1 calc R . C12 C -0.1406(9) 0.9206(3) 0.4621(3) 0.031(2) Uani 1 d . . C13 C -0.0113(9) 0.8848(3) 0.4542(3) 0.031(2) Uani 1 d . . C1A C 0.0800(11) 0.7442(5) 0.2654(3) 0.056(2) Uani 1 d . . H1 H 0.1466(11) 0.7552(5) 0.2289(3) 0.067 Uiso 1 d R . C2A C -0.0640(10) 0.7837(5) 0.2854(4) 0.058(2) Uani 1 d . . H2 H -0.1163(10) 0.8273(5) 0.2651(4) 0.069 Uiso 1 d R . C3A C -0.1223(11) 0.7500(6) 0.3393(5) 0.074(3) Uani 1 d . . H3 H -0.2212(11) 0.7659(6) 0.3632(5) 0.089 Uiso 1 d R . C4A C -0.0112(18) 0.6895(6) 0.3533(4) 0.087(3) Uani 1 d . . H4 H -0.0200(18) 0.6557(6) 0.3884(4) 0.104 Uiso 1 d R . C5A C 0.1139(13) 0.6852(5) 0.3078(4) 0.074(3) Uani 1 d . . H5 H 0.2073(13) 0.6485(5) 0.3056(4) 0.089 Uiso 1 d R . Fe2 Fe 0.38256(12) 0.96817(5) 0.13062(4) 0.0320(3) Uani 1 d . . C1B C 0.3745(9) 0.8946(4) 0.0563(3) 0.037(2) Uani 1 d . . C2B C 0.2659(9) 0.9573(4) 0.0372(3) 0.044(2) Uani 1 d . . H2B H 0.2821(9) 0.9890(4) 0.0013(3) 0.053 Uiso 1 d R . C3B C 0.1286(9) 0.9629(4) 0.0804(4) 0.055(2) Uani 1 d . . H3B H 0.0354(9) 1.0003(4) 0.0789(4) 0.065 Uiso 1 d R . C4B C 0.1523(9) 0.9061(4) 0.1271(4) 0.048(2) Uani 1 d . . H4B H 0.0784(9) 0.8976(4) 0.1621(4) 0.058 Uiso 1 d R . C5B C 0.3042(8) 0.8632(4) 0.1123(3) 0.039(2) Uani 1 d . . C6B C 0.3905(9) 0.7997(4) 0.1428(3) 0.040(2) Uani 1 d . . C7B C 0.4917(10) 0.7482(4) 0.1552(3) 0.040(2) Uani 1 d . . C8B C 0.6209(9) 0.6864(4) 0.1613(3) 0.040(2) Uani 1 d . . H8C H 0.5534(9) 0.6406(4) 0.1690(3) 0.048 Uiso 1 calc R . H8D H 0.7134(9) 0.6946(4) 0.1988(3) 0.048 Uiso 1 calc R . C9B C 0.7192(9) 0.6785(4) 0.0991(3) 0.040(2) Uani 1 d . . H9C H 0.7811(9) 0.6301(4) 0.0998(3) 0.048 Uiso 1 calc R . H9D H 0.6252(9) 0.6791(4) 0.0613(3) 0.048 Uiso 1 calc R . C10B C 0.8620(9) 0.7383(4) 0.0900(3) 0.044(2) Uani 1 d . . H10C H 0.9854(9) 0.7152(4) 0.0928(3) 0.052 Uiso 1 calc R . H10D H 0.8618(9) 0.7735(4) 0.1263(3) 0.052 Uiso 1 calc R . C11B C 0.8330(10) 0.7814(4) 0.0262(3) 0.043(2) Uani 1 d . . H11C H 0.9420(10) 0.8126(4) 0.0214(3) 0.051 Uiso 1 calc R . H11D H 0.8188(10) 0.7467(4) -0.0106(3) 0.051 Uiso 1 calc R . C12B C 0.6675(10) 0.8278(4) 0.0255(3) 0.038(2) Uani 1 d . . C13B C 0.5355(10) 0.8642(4) 0.0321(3) 0.037(2) Uani 1 d . . C1C C 0.4379(10) 1.0053(5) 0.2227(3) 0.055(2) Uani 1 d . . H1C H 0.3653(10) 0.9965(5) 0.2580(3) 0.066 Uiso 1 d R . C2C C 0.5820(10) 0.9649(4) 0.2052(4) 0.054(2) Uani 1 d . . H2C H 0.6270(10) 0.9210(4) 0.2269(4) 0.064 Uiso 1 d R . C3C C 0.6511(9) 0.9948(5) 0.1519(4) 0.056(2) Uani 1 d . . H3C H 0.7515(9) 0.9765(5) 0.1300(4) 0.067 Uiso 1 d R . C4C C 0.5508(13) 1.0566(4) 0.1349(4) 0.061(2) Uani 1 d . . H4C H 0.5679(13) 1.0892(4) 0.0996(4) 0.073 Uiso 1 d R . C5C C 0.4167(11) 1.0653(4) 0.1787(4) 0.067(3) Uani 1 d . . H5C H 0.3268(11) 1.1038(4) 0.1789(4) 0.080 Uiso 1 d R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0303(5) 0.0274(5) 0.0340(5) -0.0043(4) 0.0028(4) -0.0006(4) C1 0.030(4) 0.027(4) 0.032(4) -0.005(3) -0.002(3) 0.000(3) C2 0.032(4) 0.034(4) 0.042(4) 0.000(3) -0.007(3) 0.008(3) C3 0.031(4) 0.037(4) 0.065(5) -0.008(4) -0.007(4) 0.008(3) C4 0.038(4) 0.042(5) 0.070(5) -0.006(4) 0.019(4) -0.008(4) C5 0.035(4) 0.023(4) 0.046(4) -0.004(3) 0.003(3) -0.007(3) C6 0.041(4) 0.031(4) 0.044(4) -0.001(3) 0.015(3) -0.009(4) C7 0.054(5) 0.032(4) 0.030(4) 0.005(3) 0.005(3) -0.007(4) C8 0.057(5) 0.035(4) 0.041(4) 0.016(3) -0.011(4) -0.011(4) C9 0.037(4) 0.024(4) 0.053(4) -0.003(3) -0.012(3) 0.004(3) C10 0.032(4) 0.034(4) 0.055(4) 0.004(3) -0.002(3) -0.001(3) C11 0.039(4) 0.046(5) 0.041(4) -0.002(4) -0.001(3) 0.006(4) C12 0.048(4) 0.023(4) 0.023(3) -0.001(3) 0.003(3) -0.004(3) C13 0.044(4) 0.027(4) 0.021(3) -0.005(3) 0.002(3) -0.002(3) C1A 0.058(5) 0.081(6) 0.031(4) -0.010(4) 0.009(4) -0.001(5) C2A 0.054(5) 0.057(5) 0.056(5) -0.017(4) -0.027(4) 0.014(4) C3A 0.041(5) 0.116(9) 0.069(6) -0.042(6) 0.020(5) -0.036(5) C4A 0.146(10) 0.060(7) 0.050(6) 0.001(5) -0.019(7) -0.062(7) C5A 0.093(7) 0.055(6) 0.065(6) -0.036(5) -0.038(5) 0.032(5) Fe2 0.0290(5) 0.0291(5) 0.0374(5) -0.0014(4) 0.0004(4) 0.0025(4) C1B 0.037(4) 0.038(4) 0.034(4) -0.008(3) -0.005(3) -0.004(3) C2B 0.043(4) 0.040(5) 0.046(4) -0.007(4) -0.009(4) 0.007(4) C3B 0.032(4) 0.045(5) 0.081(6) 0.000(4) -0.017(4) 0.006(4) C4B 0.023(4) 0.049(5) 0.074(5) 0.001(4) 0.008(4) -0.002(3) C5B 0.029(4) 0.032(4) 0.057(5) 0.000(3) 0.002(3) -0.007(3) C6B 0.037(4) 0.037(5) 0.049(4) 0.001(4) 0.013(4) -0.011(4) C7B 0.045(4) 0.032(4) 0.045(4) -0.003(3) 0.013(4) -0.012(4) C8B 0.041(4) 0.032(4) 0.046(4) -0.003(3) -0.006(3) -0.008(3) C9B 0.037(4) 0.033(4) 0.046(4) -0.006(3) -0.010(3) 0.003(3) C10B 0.042(4) 0.044(5) 0.044(4) 0.003(3) -0.002(3) -0.001(4) C11B 0.060(5) 0.034(4) 0.035(4) -0.007(3) 0.004(3) 0.006(4) C12B 0.057(5) 0.030(4) 0.024(4) -0.003(3) -0.006(3) -0.002(4) C13B 0.058(5) 0.025(4) 0.025(4) -0.004(3) -0.005(3) 0.003(4) C1C 0.052(5) 0.085(6) 0.030(4) -0.003(4) 0.011(4) -0.007(5) C2C 0.060(5) 0.039(5) 0.058(5) 0.005(4) -0.017(4) 0.003(4) C3C 0.022(4) 0.084(7) 0.062(5) -0.025(5) 0.004(4) -0.014(4) C4C 0.091(7) 0.047(5) 0.041(5) 0.008(4) -0.015(5) -0.028(5) C5C 0.066(6) 0.043(5) 0.083(6) -0.035(5) -0.029(5) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C4A 2.006(8) . ? Fe1 C3A 2.016(8) . ? Fe1 C2A 2.018(7) . ? Fe1 C5 2.020(6) . ? Fe1 C5A 2.021(7) . ? Fe1 C4 2.028(7) . ? Fe1 C1A 2.031(7) . ? Fe1 C1 2.037(6) . ? Fe1 C3 2.045(7) . ? Fe1 C2 2.046(6) . ? C1 C2 1.412(8) . ? C1 C13 1.436(9) . ? C1 C5 1.451(8) . ? C2 C3 1.411(9) . ? C3 C4 1.414(9) . ? C4 C5 1.431(9) . ? C5 C6 1.427(9) . ? C6 C7 1.194(9) . ? C7 C8 1.467(10) . ? C8 C9 1.538(9) . ? C9 C10 1.541(8) . ? C10 C11 1.531(9) . ? C11 C12 1.497(9) . ? C12 C13 1.171(8) . ? C1A C2A 1.371(10) . ? C1A C5A 1.396(11) . ? C2A C3A 1.381(11) . ? C3A C4A 1.382(12) . ? C4A C5A 1.380(13) . ? Fe2 C2C 2.018(7) . ? Fe2 C4B 2.020(7) . ? Fe2 C5B 2.022(7) . ? Fe2 C4C 2.023(7) . ? Fe2 C3C 2.025(7) . ? Fe2 C1C 2.032(7) . ? Fe2 C5C 2.036(7) . ? Fe2 C3B 2.037(7) . ? Fe2 C1B 2.041(6) . ? Fe2 C2B 2.050(7) . ? C1B C2B 1.425(9) . ? C1B C13B 1.435(9) . ? C1B C5B 1.436(9) . ? C2B C3B 1.412(9) . ? C3B C4B 1.418(10) . ? C4B C5B 1.415(9) . ? C5B C6B 1.434(10) . ? C6B C7B 1.206(9) . ? C7B C8B 1.465(9) . ? C8B C9B 1.546(8) . ? C9B C10B 1.533(9) . ? C10B C11B 1.537(9) . ? C11B C12B 1.473(9) . ? C12B C13B 1.188(9) . ? C1C C2C 1.362(10) . ? C1C C5C 1.424(11) . ? C2C C3C 1.373(10) . ? C3C C4C 1.371(10) . ? C4C C5C 1.411(11) . ? 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 C4A Fe1 C3A 40.2(4) . . ? C4A Fe1 C2A 67.4(4) . . ? C3A Fe1 C2A 40.0(3) . . ? C4A Fe1 C5 159.8(5) . . ? C3A Fe1 C5 122.2(4) . . ? C2A Fe1 C5 105.4(3) . . ? C4A Fe1 C5A 40.1(4) . . ? C3A Fe1 C5A 67.4(4) . . ? C2A Fe1 C5A 67.2(3) . . ? C5 Fe1 C5A 156.5(4) . . ? C4A Fe1 C4 158.3(5) . . ? C3A Fe1 C4 159.5(4) . . ? C2A Fe1 C4 123.5(3) . . ? C5 Fe1 C4 41.4(3) . . ? C5A Fe1 C4 122.6(4) . . ? C4A Fe1 C1A 67.4(3) . . ? C3A Fe1 C1A 67.1(3) . . ? C2A Fe1 C1A 39.6(3) . . ? C5 Fe1 C1A 119.9(3) . . ? C5A Fe1 C1A 40.3(3) . . ? C4 Fe1 C1A 107.9(3) . . ? C4A Fe1 C1 123.8(4) . . ? C3A Fe1 C1 106.3(3) . . ? C2A Fe1 C1 120.0(3) . . ? C5 Fe1 C1 41.9(2) . . ? C5A Fe1 C1 161.3(4) . . ? C4 Fe1 C1 69.6(3) . . ? C1A Fe1 C1 155.4(3) . . ? C4A Fe1 C3 124.0(4) . . ? C3A Fe1 C3 157.9(4) . . ? C2A Fe1 C3 161.5(3) . . ? C5 Fe1 C3 68.7(3) . . ? C5A Fe1 C3 110.9(3) . . ? C4 Fe1 C3 40.6(3) . . ? C1A Fe1 C3 126.9(3) . . ? C1 Fe1 C3 68.0(3) . . ? C4A Fe1 C2 109.0(3) . . ? C3A Fe1 C2 121.5(3) . . ? C2A Fe1 C2 155.8(3) . . ? C5 Fe1 C2 69.4(3) . . ? C5A Fe1 C2 126.5(3) . . ? C4 Fe1 C2 69.1(3) . . ? C1A Fe1 C2 163.3(3) . . ? C1 Fe1 C2 40.5(2) . . ? C3 Fe1 C2 40.4(2) . . ? C2 C1 C13 132.7(6) . . ? C2 C1 C5 108.0(5) . . ? C13 C1 C5 119.1(6) . . ? C2 C1 Fe1 70.1(4) . . ? C13 C1 Fe1 122.8(4) . . ? C5 C1 Fe1 68.4(3) . . ? C3 C2 C1 107.9(6) . . ? C3 C2 Fe1 69.8(4) . . ? C1 C2 Fe1 69.4(3) . . ? C2 C3 C4 109.6(6) . . ? C2 C3 Fe1 69.9(4) . . ? C4 C3 Fe1 69.0(4) . . ? C3 C4 C5 107.3(6) . . ? C3 C4 Fe1 70.3(4) . . ? C5 C4 Fe1 69.0(4) . . ? C6 C5 C4 133.1(6) . . ? C6 C5 C1 119.7(6) . . ? C4 C5 C1 107.2(6) . . ? C6 C5 Fe1 125.8(5) . . ? C4 C5 Fe1 69.6(4) . . ? C1 C5 Fe1 69.7(3) . . ? C7 C6 C5 162.6(7) . . ? C6 C7 C8 172.9(7) . . ? C7 C8 C9 110.8(5) . . ? C8 C9 C10 114.7(5) . . ? C11 C10 C9 114.3(6) . . ? C12 C11 C10 109.9(5) . . ? C13 C12 C11 172.5(6) . . ? C12 C13 C1 164.4(7) . . ? C2A C1A C5A 107.8(7) . . ? C2A C1A Fe1 69.7(4) . . ? C5A C1A Fe1 69.5(4) . . ? C1A C2A C3A 108.6(8) . . ? C1A C2A Fe1 70.7(4) . . ? C3A C2A Fe1 69.9(5) . . ? C4A C3A C2A 107.7(8) . . ? C4A C3A Fe1 69.5(5) . . ? C2A C3A Fe1 70.0(4) . . ? C5A C4A C3A 108.3(8) . . ? C5A C4A Fe1 70.6(5) . . ? C3A C4A Fe1 70.3(5) . . ? C4A C5A C1A 107.5(8) . . ? C4A C5A Fe1 69.4(4) . . ? C1A C5A Fe1 70.2(4) . . ? C2C Fe2 C4B 123.0(3) . . ? C2C Fe2 C5B 106.6(3) . . ? C4B Fe2 C5B 41.0(3) . . ? C2C Fe2 C4C 66.5(3) . . ? C4B Fe2 C4C 161.2(3) . . ? C5B Fe2 C4C 157.1(3) . . ? C2C Fe2 C3C 39.7(3) . . ? C4B Fe2 C3C 157.7(3) . . ? C5B Fe2 C3C 121.2(3) . . ? C4C Fe2 C3C 39.6(3) . . ? C2C Fe2 C1C 39.3(3) . . ? C4B Fe2 C1C 107.9(3) . . ? C5B Fe2 C1C 121.2(3) . . ? C4C Fe2 C1C 68.3(3) . . ? C3C Fe2 C1C 67.4(3) . . ? C2C Fe2 C5C 66.7(3) . . ? C4B Fe2 C5C 124.4(3) . . ? C5B Fe2 C5C 159.0(3) . . ? C4C Fe2 C5C 40.7(3) . . ? C3C Fe2 C5C 67.4(3) . . ? C1C Fe2 C5C 41.0(3) . . ? C2C Fe2 C3B 160.4(3) . . ? C4B Fe2 C3B 40.9(3) . . ? C5B Fe2 C3B 68.5(3) . . ? C4C Fe2 C3B 125.2(3) . . ? C3C Fe2 C3B 159.2(3) . . ? C1C Fe2 C3B 125.8(3) . . ? C5C Fe2 C3B 110.7(3) . . ? C2C Fe2 C1B 121.7(3) . . ? C4B Fe2 C1B 69.1(3) . . ? C5B Fe2 C1B 41.4(3) . . ? C4C Fe2 C1B 121.9(3) . . ? C3C Fe2 C1B 106.1(3) . . ? C1C Fe2 C1B 156.8(3) . . ? C5C Fe2 C1B 159.3(3) . . ? C3B Fe2 C1B 68.0(3) . . ? C2C Fe2 C2B 157.5(3) . . ? C4B Fe2 C2B 69.3(3) . . ? C5B Fe2 C2B 69.4(3) . . ? C4C Fe2 C2B 108.1(3) . . ? C3C Fe2 C2B 122.2(3) . . ? C1C Fe2 C2B 161.6(3) . . ? C5C Fe2 C2B 124.6(3) . . ? C3B Fe2 C2B 40.4(3) . . ? C1B Fe2 C2B 40.8(2) . . ? C2B C1B C13B 131.7(6) . . ? C2B C1B C5B 108.2(6) . . ? C13B C1B C5B 120.0(6) . . ? C2B C1B Fe2 70.0(4) . . ? C13B C1B Fe2 123.8(4) . . ? C5B C1B Fe2 68.6(4) . . ? C3B C2B C1B 106.9(6) . . ? C3B C2B Fe2 69.3(4) . . ? C1B C2B Fe2 69.3(4) . . ? C2B C3B C4B 109.6(6) . . ? C2B C3B Fe2 70.3(4) . . ? C4B C3B Fe2 68.9(4) . . ? C5B C4B C3B 107.4(6) . . ? C5B C4B Fe2 69.6(4) . . ? C3B C4B Fe2 70.2(4) . . ? C4B C5B C6B 132.0(6) . . ? C4B C5B C1B 107.8(6) . . ? C6B C5B C1B 120.2(6) . . ? C4B C5B Fe2 69.4(4) . . ? C6B C5B Fe2 125.2(5) . . ? C1B C5B Fe2 70.0(4) . . ? C7B C6B C5B 162.6(7) . . ? C6B C7B C8B 172.4(7) . . ? C7B C8B C9B 110.3(5) . . ? C10B C9B C8B 114.4(5) . . ? C9B C10B C11B 115.6(6) . . ? C12B C11B C10B 110.2(5) . . ? C13B C12B C11B 172.9(7) . . ? C12B C13B C1B 163.1(7) . . ? C2C C1C C5C 106.3(7) . . ? C2C C1C Fe2 69.8(4) . . ? C5C C1C Fe2 69.7(4) . . ? C1C C2C C3C 110.8(7) . . ? C1C C2C Fe2 70.9(4) . . ? C3C C2C Fe2 70.4(4) . . ? C4C C3C C2C 107.8(7) . . ? C4C C3C Fe2 70.1(4) . . ? C2C C3C Fe2 69.9(4) . . ? C3C C4C C5C 108.1(7) . . ? C3C C4C Fe2 70.3(4) . . ? C5C C4C Fe2 70.2(4) . . ? C4C C5C C1C 106.9(7) . . ? C4C C5C Fe2 69.1(4) . . ? C1C C5C Fe2 69.4(4) . . ? _refine_diff_density_max 0.332 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.078 data_bi _database_code_CSD 170842 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H16 Fe' _chemical_formula_weight 288.16 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.316(5) _cell_length_b 11.656(8) _cell_length_c 17.244(17) _cell_angle_alpha 75.28(7) _cell_angle_beta 80.66(7) _cell_angle_gamma 76.67(5) _cell_volume 1375.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method ? _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3740 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.51 _reflns_number_total 3558 _reflns_number_observed 2760 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+0.9114P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3557 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_obs 0.0611 _refine_ls_wR_factor_all 0.1733 _refine_ls_wR_factor_obs 0.1522 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.069 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.069 _refine_ls_shift/esd_max 0.024 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.23882(12) 0.73093(7) 0.03385(5) 0.0336(3) Uani 1 d . . C1 C 0.3140(9) 0.6949(5) -0.0777(3) 0.0365(14) Uani 1 d . . C2 C 0.2264(10) 0.6016(6) -0.0249(4) 0.049(2) Uani 1 d . . H2A H 0.2815(10) 0.5170(6) -0.0113(4) 0.059 Uiso 1 d R . C3 C 0.0413(10) 0.6587(7) 0.0026(4) 0.057(2) Uani 1 d . . H3A H -0.0500(10) 0.6179(7) 0.0387(4) 0.069 Uiso 1 d R . C4 C 0.0146(10) 0.7841(7) -0.0315(4) 0.059(2) Uani 1 d . . H4A H -0.0971(10) 0.8436(7) -0.0228(4) 0.070 Uiso 1 d R . C5 C 0.1839(8) 0.8083(6) -0.0814(3) 0.042(2) Uani 1 d . . C6 C 0.2369(9) 0.9183(6) -0.1283(4) 0.045(2) Uani 1 d . . C7 C 0.3215(9) 0.9908(6) -0.1720(4) 0.045(2) Uani 1 d . . C8 C 0.4454(10) 1.0636(5) -0.2307(4) 0.046(2) Uani 1 d . . H8A H 0.4967(10) 1.1119(5) -0.2029(4) 0.056 Uiso 1 calc R . H8B H 0.3710(10) 1.1203(5) -0.2729(4) 0.056 Uiso 1 calc R . C9 C 0.6086(10) 0.9807(6) -0.2698(4) 0.047(2) Uani 1 d . . H9A H 0.5562(10) 0.9228(6) -0.2886(4) 0.057 Uiso 1 calc R . H9B H 0.6701(10) 1.0306(6) -0.3178(4) 0.057 Uiso 1 calc R . C10 C 0.7584(10) 0.9097(6) -0.2140(4) 0.047(2) Uani 1 d . . H10A H 0.7170(10) 0.9270(6) -0.1599(4) 0.057 Uiso 1 calc R . H10B H 0.8775(10) 0.9393(6) -0.2345(4) 0.057 Uiso 1 calc R . C11 C 0.7994(9) 0.7726(6) -0.2052(4) 0.046(2) Uani 1 d . . H11A H 0.8252(9) 0.7542(6) -0.2594(4) 0.056 Uiso 1 calc R . H11B H 0.9134(9) 0.7357(6) -0.1769(4) 0.056 Uiso 1 calc R . C12 C 0.6397(10) 0.7202(5) -0.1601(4) 0.0408(15) Uani 1 d . . C13 C 0.5004(10) 0.6919(5) -0.1202(3) 0.0381(14) Uani 1 d . . C1A C 0.1932(11) 0.8237(14) 0.1251(9) 0.050(3) Uani 0.64(4) d PG 1 H1E H 0.0803(17) 0.8796(24) 0.1379(16) 0.060 Uiso 0.64(4) d PG 1 C2A C 0.3514(22) 0.8533(7) 0.0702(7) 0.049(4) Uani 0.64(4) d PG 1 H2E H 0.3642(41) 0.9327(12) 0.0394(11) 0.058 Uiso 0.64(4) d PG 1 C3A C 0.4873(10) 0.7447(17) 0.0688(7) 0.047(3) Uani 0.64(4) d PG 1 H3E H 0.6081(13) 0.7379(30) 0.0370(12) 0.056 Uiso 0.64(4) d PG 1 C4A C 0.4131(29) 0.6481(6) 0.1230(9) 0.047(4) Uani 0.64(4) d PG 1 H4E H 0.4750(45) 0.5645(8) 0.1341(15) 0.056 Uiso 0.64(4) d PG 1 C5A C 0.2313(28) 0.6969(16) 0.1577(4) 0.043(4) Uani 0.64(4) d PG 1 H5E H 0.1488(43) 0.6521(27) 0.1964(6) 0.051 Uiso 0.64(4) d PG 1 C1C C 0.3346(47) 0.6501(12) 0.1400(13) 0.040 Uiso 0.36(4) d PG 2 H1C H 0.3514(75) 0.5653(14) 0.1650(21) 0.040 Uiso 0.36(4) d PG 2 C2C C 0.4716(24) 0.7090(24) 0.0868(16) 0.040 Uiso 0.36(4) d PG 2 H2C H 0.5973(29) 0.6710(41) 0.0695(26) 0.040 Uiso 0.36(4) d PG 2 C3C C 0.3899(38) 0.8339(20) 0.0637(12) 0.040 Uiso 0.36(4) d PG 2 H3C H 0.4507(63) 0.8952(33) 0.0281(19) 0.040 Uiso 0.36(4) d PG 2 C4C C 0.2025(31) 0.8522(17) 0.1027(16) 0.040 Uiso 0.36(4) d PG 2 H4C H 0.1143(50) 0.9280(25) 0.0980(27) 0.040 Uiso 0.36(4) d PG 2 C5C C 0.1683(31) 0.7386(28) 0.1499(12) 0.040 Uiso 0.36(4) d PG 2 H5C H 0.0530(44) 0.7242(46) 0.1827(20) 0.040 Uiso 0.36(4) d PG 2 Fe2 Fe 0.27651(11) 0.57425(7) 0.65355(5) 0.0329(3) Uani 1 d . . C1B C 0.2171(8) 0.7569(5) 0.6100(3) 0.0344(13) Uani 1 d . . C2B C 0.3116(9) 0.7294(5) 0.6803(4) 0.0429(15) Uani 1 d . . H2B H 0.2669(9) 0.7614(5) 0.7276(4) 0.051 Uiso 1 d R . C3B C 0.4893(9) 0.6524(6) 0.6660(4) 0.050(2) Uani 1 d . . H3B H 0.5817(9) 0.6199(6) 0.7036(4) 0.060 Uiso 1 d R . C4B C 0.5082(9) 0.6317(6) 0.5872(4) 0.050(2) Uani 1 d . . H4B H 0.6142(9) 0.5833(6) 0.5621(4) 0.060 Uiso 1 d R . C5B C 0.3417(8) 0.6962(5) 0.5510(3) 0.0373(14) Uani 1 d . . C6B C 0.2807(9) 0.7094(6) 0.4738(4) 0.0426(15) Uani 1 d . . C7B C 0.1916(9) 0.7415(5) 0.4172(4) 0.0401(14) Uani 1 d . . C8B C 0.0698(9) 0.7938(6) 0.3513(3) 0.045(2) Uani 1 d . . H8C H 0.0133(9) 0.7302(6) 0.3414(3) 0.054 Uiso 1 calc R . H8D H 0.1466(9) 0.8261(6) 0.3011(3) 0.054 Uiso 1 calc R . C9B C -0.0878(9) 0.8961(6) 0.3740(4) 0.044(2) Uani 1 d . . H9C H -0.1491(9) 0.9418(6) 0.3252(4) 0.053 Uiso 1 calc R . H9D H -0.0297(9) 0.9524(6) 0.3919(4) 0.053 Uiso 1 calc R . C10B C -0.2412(9) 0.8540(6) 0.4409(3) 0.0433(15) Uani 1 d . . H10C H -0.2071(9) 0.7650(6) 0.4599(3) 0.052 Uiso 1 calc R . H10D H -0.3626(9) 0.8729(6) 0.4175(3) 0.052 Uiso 1 calc R . C11B C -0.2696(9) 0.9127(5) 0.5145(3) 0.0397(14) Uani 1 d . . H11C H -0.2882(9) 1.0018(5) 0.4956(3) 0.048 Uiso 1 calc R . H11D H -0.3841(9) 0.8932(5) 0.5500(3) 0.048 Uiso 1 calc R . C12B C -0.1058(8) 0.8683(5) 0.5597(3) 0.0326(13) Uani 1 d . . C13B C 0.0329(9) 0.8236(5) 0.5919(3) 0.0327(13) Uani 1 d . . C1D C 0.3010(10) 0.3941(8) 0.6515(7) 0.042(3) Uani 0.66(3) d PG 1 H1D H 0.4055(16) 0.3450(13) 0.6261(13) 0.050 Uiso 0.66(3) d PG 1 C2D C 0.1386(17) 0.4655(9) 0.6152(5) 0.039(3) Uani 0.66(3) d PG 1 H2D H 0.1141(33) 0.4732(16) 0.5608(6) 0.047 Uiso 0.66(3) d PG 1 C3D C 0.0188(8) 0.5237(6) 0.6732(11) 0.046(4) Uani 0.66(3) d PG 1 H3D H -0.1008(10) 0.5775(10) 0.6651(18) 0.055 Uiso 0.66(3) d PG 1 C4D C 0.1071(25) 0.4881(9) 0.7455(6) 0.048(4) Uani 0.66(3) d PG 1 H4D H 0.0577(40) 0.5137(16) 0.7948(9) 0.057 Uiso 0.66(3) d PG 1 C5D C 0.2815(22) 0.4081(8) 0.7320(6) 0.047(3) Uani 0.66(3) d PG 1 H5D H 0.3706(34) 0.3701(12) 0.7706(11) 0.056 Uiso 0.66(3) d PG 1 C1E C 0.0422(24) 0.5180(15) 0.7102(16) 0.040 Uiso 0.34(3) d PG 2 H1E' H -0.0737(33) 0.5673(24) 0.7278(27) 0.040 Uiso 0.34(3) d PG 2 C2E C 0.1947(38) 0.4599(21) 0.7569(8) 0.040 Uiso 0.34(3) d PG 2 H2E' H 0.2000(63) 0.4630(35) 0.8115(9) 0.040 Uiso 0.34(3) d PG 2 C3E C 0.3381(22) 0.3964(18) 0.7085(15) 0.040 Uiso 0.34(3) d PG 2 H3E' H 0.4573(29) 0.3490(28) 0.7247(25) 0.040 Uiso 0.34(3) d PG 2 C4E C 0.2741(35) 0.4152(21) 0.6319(11) 0.040 Uiso 0.34(3) d PG 2 H4E' H 0.3425(56) 0.3827(33) 0.5872(17) 0.040 Uiso 0.34(3) d PG 2 C5E C 0.0914(33) 0.4903(21) 0.6329(12) 0.040 Uiso 0.34(3) d PG 2 H5E' H 0.0145(52) 0.5176(33) 0.5892(18) 0.040 Uiso 0.34(3) d PG 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0388(5) 0.0367(5) 0.0264(5) -0.0036(4) -0.0045(4) -0.0131(4) C1 0.049(4) 0.036(3) 0.030(3) -0.006(2) -0.013(3) -0.014(3) C2 0.074(5) 0.051(4) 0.035(3) -0.009(3) -0.014(3) -0.032(4) C3 0.053(4) 0.076(5) 0.050(4) 0.002(4) -0.017(3) -0.037(4) C4 0.044(4) 0.075(5) 0.055(4) -0.001(4) -0.019(3) -0.015(4) C5 0.035(3) 0.061(4) 0.030(3) 0.001(3) -0.012(3) -0.012(3) C6 0.044(4) 0.048(4) 0.037(3) -0.001(3) -0.013(3) -0.002(3) C7 0.054(4) 0.039(3) 0.035(3) 0.007(3) -0.020(3) 0.001(3) C8 0.068(4) 0.038(3) 0.035(3) 0.007(3) -0.021(3) -0.019(3) C9 0.063(4) 0.056(4) 0.030(3) -0.005(3) -0.009(3) -0.029(3) C10 0.057(4) 0.055(4) 0.035(3) -0.011(3) -0.001(3) -0.023(3) C11 0.053(4) 0.048(4) 0.035(3) -0.011(3) 0.005(3) -0.012(3) C12 0.059(4) 0.030(3) 0.032(3) -0.008(3) -0.006(3) -0.004(3) C13 0.064(4) 0.031(3) 0.024(3) -0.007(2) -0.010(3) -0.014(3) C1A 0.086(9) 0.037(7) 0.026(7) -0.011(5) 0.003(6) -0.014(6) C2A 0.062(11) 0.046(7) 0.049(6) -0.018(6) -0.005(6) -0.024(6) C3A 0.051(7) 0.064(9) 0.033(6) 0.005(6) -0.019(5) -0.037(7) C4A 0.038(9) 0.068(8) 0.038(7) -0.019(6) -0.010(6) -0.005(6) C5A 0.052(9) 0.051(8) 0.025(5) -0.002(5) -0.006(5) -0.016(8) Fe2 0.0335(5) 0.0299(5) 0.0327(5) 0.0012(4) -0.0073(4) -0.0079(4) C1B 0.044(4) 0.026(3) 0.034(3) 0.000(2) -0.008(3) -0.015(3) C2B 0.056(4) 0.037(3) 0.043(4) -0.007(3) -0.016(3) -0.019(3) C3B 0.045(4) 0.057(4) 0.048(4) 0.007(3) -0.019(3) -0.024(3) C4B 0.031(3) 0.051(4) 0.057(4) 0.007(3) -0.003(3) -0.008(3) C5B 0.037(3) 0.040(3) 0.032(3) 0.001(3) 0.002(3) -0.015(3) C6B 0.043(4) 0.041(3) 0.040(4) -0.007(3) 0.007(3) -0.010(3) C7B 0.046(4) 0.041(3) 0.032(3) -0.011(3) 0.005(3) -0.008(3) C8B 0.067(4) 0.053(4) 0.022(3) -0.009(3) -0.005(3) -0.027(3) C9B 0.063(4) 0.045(4) 0.032(3) 0.002(3) -0.018(3) -0.029(3) C10B 0.049(4) 0.051(4) 0.036(3) -0.010(3) -0.009(3) -0.019(3) C11B 0.043(4) 0.039(3) 0.035(3) -0.004(3) -0.010(3) -0.005(3) C12B 0.039(3) 0.030(3) 0.026(3) -0.005(2) 0.000(3) -0.007(3) C13B 0.048(4) 0.029(3) 0.024(3) -0.008(2) -0.005(3) -0.010(3) C1D 0.050(6) 0.018(5) 0.060(8) -0.008(5) -0.020(6) -0.003(4) C2D 0.038(7) 0.031(6) 0.055(6) -0.013(5) -0.017(5) -0.007(5) C3D 0.038(6) 0.039(5) 0.063(10) -0.004(5) -0.005(6) -0.017(5) C4D 0.054(10) 0.040(6) 0.042(6) 0.002(5) 0.010(6) -0.020(6) C5D 0.077(8) 0.021(5) 0.034(6) 0.009(5) -0.008(6) -0.011(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 Fe1 C1C 1.99(2) . ? Fe1 C2C 2.00(2) . ? Fe1 C5C 2.00(2) . ? Fe1 C3C 2.01(2) . ? Fe1 C4C 2.01(2) . ? Fe1 C5 2.026(6) . ? Fe1 C4 2.030(7) . ? Fe1 C3 2.033(7) . ? Fe1 C1 2.034(6) . ? Fe1 C2 2.044(6) . ? Fe1 C4A 2.058(8) . ? Fe1 C3A 2.058(9) . ? C1 C2 1.432(8) . ? C1 C5 1.433(9) . ? C1 C13 1.437(9) . ? C2 C3 1.427(10) . ? C3 C4 1.411(10) . ? C4 C5 1.430(9) . ? C5 C6 1.432(9) . ? C6 C7 1.197(9) . ? C7 C8 1.478(9) . ? C8 C9 1.534(9) . ? C9 C10 1.527(9) . ? C10 C11 1.529(9) . ? C11 C12 1.461(9) . ? C12 C13 1.197(9) . ? C1A C5A 1.42 . ? C1A C2A 1.42 . ? C2A C3A 1.42 . ? C3A C4A 1.42 . ? C4A C5A 1.42 . ? C1C C5C 1.42 . ? C1C C2C 1.42 . ? C2C C3C 1.42 . ? C3C C4C 1.42 . ? C4C C5C 1.42 . ? Fe2 C5E 1.97(2) . ? Fe2 C4E 1.99(2) . ? Fe2 C1E 1.99(2) . ? Fe2 C3E 2.03(2) . ? Fe2 C2E 2.03(2) . ? Fe2 C4B 2.033(6) . ? Fe2 C5B 2.033(6) . ? Fe2 C1B 2.038(6) . ? Fe2 C3B 2.040(6) . ? Fe2 C4D 2.045(7) . ? Fe2 C3D 2.054(8) . ? Fe2 C2B 2.056(6) . ? C1B C2B 1.422(8) . ? C1B C13B 1.431(8) . ? C1B C5B 1.461(8) . ? C2B C3B 1.424(9) . ? C3B C4B 1.418(10) . ? C4B C5B 1.422(9) . ? C5B C6B 1.433(9) . ? C6B C7B 1.195(9) . ? C7B C8B 1.477(9) . ? C8B C9B 1.536(9) . ? C9B C10B 1.541(8) . ? C10B C11B 1.553(8) . ? C11B C12B 1.457(8) . ? C12B C13B 1.184(8) . ? C1D C5D 1.42 . ? C1D C2D 1.42 . ? C2D C3D 1.42 . ? C3D C4D 1.42 . ? C4D C5D 1.42 . ? C1E C5E 1.42 . ? C1E C2E 1.42 . ? C2E C3E 1.42 . ? C3E C4E 1.42 . ? C4E C5E 1.42 . ? 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 C1C Fe1 C2C 41.7(4) . . ? C1C Fe1 C5C 41.6(3) . . ? C2C Fe1 C5C 70.1(4) . . ? C1C Fe1 C3C 70.1(5) . . ? C2C Fe1 C3C 41.5(4) . . ? C5C Fe1 C3C 69.9(5) . . ? C1C Fe1 C4C 70.0(4) . . ? C2C Fe1 C4C 69.9(5) . . ? C5C Fe1 C4C 41.4(3) . . ? C3C Fe1 C4C 41.3(4) . . ? C1C Fe1 C5 171.1(10) . . ? C2C Fe1 C5 130.4(8) . . ? C5C Fe1 C5 145.8(10) . . ? C3C Fe1 C5 106.4(5) . . ? C4C Fe1 C5 113.1(7) . . ? C1C Fe1 C4 147.2(10) . . ? C2C Fe1 C4 169.0(9) . . ? C5C Fe1 C4 113.3(8) . . ? C3C Fe1 C4 128.6(8) . . ? C4C Fe1 C4 105.4(6) . . ? C5 Fe1 C4 41.3(3) . . ? C1C Fe1 C3 116.1(7) . . ? C2C Fe1 C3 149.8(8) . . ? C5C Fe1 C3 107.2(5) . . ? C3C Fe1 C3 167.8(9) . . ? C4C Fe1 C3 128.9(7) . . ? C5 Fe1 C3 69.0(3) . . ? C4 Fe1 C3 40.6(3) . . ? C1C Fe1 C1 132.1(8) . . ? C2C Fe1 C1 109.1(6) . . ? C5C Fe1 C1 171.1(9) . . ? C3C Fe1 C1 115.8(6) . . ? C4C Fe1 C1 147.3(8) . . ? C5 Fe1 C1 41.3(3) . . ? C4 Fe1 C1 69.1(3) . . ? C3 Fe1 C1 68.7(3) . . ? C1C Fe1 C2 109.0(5) . . ? C2C Fe1 C2 117.1(6) . . ? C5C Fe1 C2 130.7(7) . . ? C3C Fe1 C2 149.5(8) . . ? C4C Fe1 C2 168.9(8) . . ? C5 Fe1 C2 69.7(3) . . ? C4 Fe1 C2 69.2(3) . . ? C3 Fe1 C2 41.0(3) . . ? C1 Fe1 C2 41.1(2) . . ? C5 Fe1 C4A 154.2(7) . . ? C4 Fe1 C4A 163.2(6) . . ? C3 Fe1 C4A 125.9(5) . . ? C1 Fe1 C4A 119.3(5) . . ? C2 Fe1 C4A 106.8(3) . . ? C5 Fe1 C3A 118.5(5) . . ? C4 Fe1 C3A 155.7(6) . . ? C3 Fe1 C3A 160.6(5) . . ? C1 Fe1 C3A 104.4(3) . . ? C2 Fe1 C3A 122.1(4) . . ? C4A Fe1 C3A 40.4(2) . . ? C2 C1 C5 108.5(6) . . ? C2 C1 C13 131.7(6) . . ? C5 C1 C13 119.7(5) . . ? C2 C1 Fe1 69.8(3) . . ? C5 C1 Fe1 69.0(3) . . ? C13 C1 Fe1 124.2(4) . . ? C3 C2 C1 106.8(6) . . ? C3 C2 Fe1 69.1(4) . . ? C1 C2 Fe1 69.1(3) . . ? C4 C3 C2 109.3(6) . . ? C4 C3 Fe1 69.6(4) . . ? C2 C3 Fe1 69.9(4) . . ? C3 C4 C5 108.1(7) . . ? C3 C4 Fe1 69.8(4) . . ? C5 C4 Fe1 69.2(3) . . ? C4 C5 C6 132.1(6) . . ? C4 C5 C1 107.3(6) . . ? C6 C5 C1 120.5(6) . . ? C4 C5 Fe1 69.5(4) . . ? C6 C5 Fe1 125.0(4) . . ? C1 C5 Fe1 69.6(3) . . ? C7 C6 C5 163.7(7) . . ? C6 C7 C8 170.8(7) . . ? C7 C8 C9 110.2(5) . . ? C10 C9 C8 114.2(5) . . ? C9 C10 C11 115.0(5) . . ? C12 C11 C10 111.0(5) . . ? C13 C12 C11 171.1(6) . . ? C12 C13 C1 163.5(6) . . ? C5A C1A C2A 108.0 . . ? C5A C1A Fe1 69.7(3) . . ? C2A C1A Fe1 69.8(3) . . ? C3A C2A C1A 108.0 . . ? C3A C2A Fe1 69.6(3) . . ? C1A C2A Fe1 70.1(3) . . ? C2A C3A C4A 108.0 . . ? C2A C3A Fe1 70.2(3) . . ? C4A C3A Fe1 69.8(3) . . ? C5A C4A C3A 108.0 . . ? C5A C4A Fe1 70.1(3) . . ? C3A C4A Fe1 69.8(4) . . ? C4A C5A C1A 108.0 . . ? C4A C5A Fe1 69.6(3) . . ? C1A C5A Fe1 70.1(4) . . ? C5C C1C C2C 108.0 . . ? C5C C1C Fe1 69.6(7) . . ? C2C C1C Fe1 69.3(8) . . ? C1C C2C C3C 108.0 . . ? C1C C2C Fe1 69.0(8) . . ? C3C C2C Fe1 69.8(8) . . ? C4C C3C C2C 108.0 . . ? C4C C3C Fe1 69.5(7) . . ? C2C C3C Fe1 68.7(7) . . ? C3C C4C C5C 108.0 . . ? C3C C4C Fe1 69.2(8) . . ? C5C C4C Fe1 68.9(8) . . ? C1C C5C C4C 108.0 . . ? C1C C5C Fe1 68.8(7) . . ? C4C C5C Fe1 69.7(8) . . ? C5E Fe2 C4E 42.1(4) . . ? C5E Fe2 C1E 42.0(4) . . ? C4E Fe2 C1E 70.5(5) . . ? C5E Fe2 C3E 70.3(5) . . ? C4E Fe2 C3E 41.4(4) . . ? C1E Fe2 C3E 69.7(4) . . ? C5E Fe2 C2E 70.2(4) . . ? C4E Fe2 C2E 69.8(4) . . ? C1E Fe2 C2E 41.3(3) . . ? C3E Fe2 C2E 41.0(3) . . ? C5E Fe2 C4B 133.7(8) . . ? C4E Fe2 C4B 107.2(6) . . ? C1E Fe2 C4B 175.4(9) . . ? C3E Fe2 C4B 111.5(6) . . ? C2E Fe2 C4B 142.3(8) . . ? C5E Fe2 C5B 108.8(5) . . ? C4E Fe2 C5B 112.1(6) . . ? C1E Fe2 C5B 135.6(8) . . ? C3E Fe2 C5B 142.5(7) . . ? C2E Fe2 C5B 176.2(8) . . ? C4B Fe2 C5B 40.9(2) . . ? C5E Fe2 C1B 113.7(6) . . ? C4E Fe2 C1B 144.7(7) . . ? C1E Fe2 C1B 109.7(5) . . ? C3E Fe2 C1B 173.8(8) . . ? C2E Fe2 C1B 134.7(7) . . ? C4B Fe2 C1B 69.6(3) . . ? C5B Fe2 C1B 42.1(2) . . ? C5E Fe2 C3B 173.7(8) . . ? C4E Fe2 C3B 132.7(8) . . ? C1E Fe2 C3B 143.7(8) . . ? C3E Fe2 C3B 107.9(6) . . ? C2E Fe2 C3B 112.7(6) . . ? C4B Fe2 C3B 40.7(3) . . ? C5B Fe2 C3B 68.7(3) . . ? C1B Fe2 C3B 68.7(3) . . ? C4B Fe2 C4D 161.4(6) . . ? C5B Fe2 C4D 157.2(6) . . ? C1B Fe2 C4D 122.0(4) . . ? C3B Fe2 C4D 126.0(5) . . ? C4B Fe2 C3D 156.4(6) . . ? C5B Fe2 C3D 119.6(5) . . ? C1B Fe2 C3D 104.6(3) . . ? C3B Fe2 C3D 160.1(5) . . ? C4D Fe2 C3D 40.53(14) . . ? C5E Fe2 C2B 144.7(8) . . ? C4E Fe2 C2B 172.9(8) . . ? C1E Fe2 C2B 113.7(6) . . ? C3E Fe2 C2B 133.5(7) . . ? C2E Fe2 C2B 109.3(5) . . ? C4B Fe2 C2B 69.0(3) . . ? C5B Fe2 C2B 69.3(3) . . ? C1B Fe2 C2B 40.7(2) . . ? C3B Fe2 C2B 40.7(3) . . ? C4D Fe2 C2B 109.4(3) . . ? C3D Fe2 C2B 122.3(4) . . ? C2B C1B C13B 132.3(6) . . ? C2B C1B C5B 107.5(5) . . ? C13B C1B C5B 120.1(5) . . ? C2B C1B Fe2 70.4(3) . . ? C13B C1B Fe2 123.4(4) . . ? C5B C1B Fe2 68.8(3) . . ? C1B C2B C3B 107.8(6) . . ? C1B C2B Fe2 69.0(3) . . ? C3B C2B Fe2 69.1(4) . . ? C4B C3B C2B 109.2(6) . . ? C4B C3B Fe2 69.4(4) . . ? C2B C3B Fe2 70.3(3) . . ? C3B C4B C5B 108.0(6) . . ? C3B C4B Fe2 69.9(4) . . ? C5B C4B Fe2 69.5(3) . . ? C4B C5B C6B 133.4(6) . . ? C4B C5B C1B 107.5(5) . . ? C6B C5B C1B 119.1(5) . . ? C4B C5B Fe2 69.5(3) . . ? C6B C5B Fe2 125.9(4) . . ? C1B C5B Fe2 69.1(3) . . ? C7B C6B C5B 162.7(7) . . ? C6B C7B C8B 173.0(6) . . ? C7B C8B C9B 110.0(5) . . ? C8B C9B C10B 114.9(5) . . ? C9B C10B C11B 114.1(5) . . ? C12B C11B C10B 110.4(5) . . ? C13B C12B C11B 173.4(6) . . ? C12B C13B C1B 163.4(6) . . ? C5D C1D C2D 108.0 . . ? C5D C1D Fe2 69.3(3) . . ? C2D C1D Fe2 69.9(3) . . ? C3D C2D C1D 108.0 . . ? C3D C2D Fe2 69.2(3) . . ? C1D C2D Fe2 70.0(3) . . ? C4D C3D C2D 108.0 . . ? C4D C3D Fe2 69.4(3) . . ? C2D C3D Fe2 70.6(3) . . ? C5D C4D C3D 108.0 . . ? C5D C4D Fe2 70.2(3) . . ? C3D C4D Fe2 70.1(3) . . ? C1D C5D C4D 108.0 . . ? C1D C5D Fe2 70.5(3) . . ? C4D C5D Fe2 69.3(3) . . ? C5E C1E C2E 108.0 . . ? C5E C1E Fe2 67.9(8) . . ? C2E C1E Fe2 70.8(7) . . ? C3E C2E C1E 108.0 . . ? C3E C2E Fe2 69.4(8) . . ? C1E C2E Fe2 67.9(7) . . ? C2E C3E C4E 108.0 . . ? C2E C3E Fe2 69.7(7) . . ? C4E C3E Fe2 67.8(8) . . ? C5E C4E C3E 108.0 . . ? C5E C4E Fe2 68.1(7) . . ? C3E C4E Fe2 70.8(7) . . ? C4E C5E C1E 108.0 . . ? C4E C5E Fe2 69.8(8) . . ? C1E C5E Fe2 70.0(7) . . ? _refine_diff_density_max 1.103 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.093 data_d _database_code_CSD 170843 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Fe' _chemical_formula_weight 302.18 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.055(7) _cell_length_b 11.047(6) _cell_length_c 14.409(8) _cell_angle_alpha 107.38(4) _cell_angle_beta 91.75(5) _cell_angle_gamma 103.08(5) _cell_volume 1479.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5395 _exptl_absorpt_correction_T_max 0.8846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5076 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4904 _reflns_number_gt 3751 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+1.8366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4904 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.77062(7) 0.17456(6) 0.64964(5) 0.0305(2) Uani 1 1 d . . . Fe2 Fe 0.35694(6) 0.54322(6) 0.66813(4) 0.0272(2) Uani 1 1 d . . . C1A C 0.6475(6) 0.2103(5) 0.5518(4) 0.0504(14) Uani 1 1 d . . . H1A H 0.6139 0.1537 0.4867 0.060 Uiso 1 1 d R . . C2A C 0.7694(7) 0.3098(6) 0.5799(5) 0.0584(17) Uani 1 1 d . . . H2A H 0.8342 0.3327 0.5366 0.070 Uiso 1 1 d R . . C3A C 0.7809(6) 0.3690(5) 0.6811(5) 0.0512(15) Uani 1 1 d . . . H3A H 0.8546 0.4398 0.7195 0.061 Uiso 1 1 d R . . C4A C 0.6649(5) 0.3078(4) 0.7187(3) 0.0349(11) Uani 1 1 d . . . C5A C 0.5793(5) 0.2066(4) 0.6370(3) 0.0343(10) Uani 1 1 d . . . C1B C 0.7492(5) -0.0120(5) 0.6524(5) 0.0493(14) Uani 1 1 d . . . H1B H 0.6640 -0.0772 0.6416 0.059 Uiso 1 1 d R . . C2B C 0.8330(6) 0.0104(5) 0.5792(4) 0.0467(13) Uani 1 1 d . . . H2B H 0.8155 -0.0366 0.5105 0.056 Uiso 1 1 d R . . C3B C 0.9490(5) 0.1151(5) 0.6264(4) 0.0476(13) Uani 1 1 d . . . H3B H 1.0233 0.1512 0.5946 0.057 Uiso 1 1 d R . . C4B C 0.9344(6) 0.1555(6) 0.7267(4) 0.0507(14) Uani 1 1 d . . . H4B H 0.9979 0.2248 0.7758 0.061 Uiso 1 1 d R . . C5B C 0.8119(6) 0.0785(6) 0.7428(4) 0.0508(14) Uani 1 1 d . . . H5B H 0.7768 0.0853 0.8049 0.061 Uiso 1 1 d R . . C1C C 0.1960(5) 0.4360(5) 0.5651(4) 0.0402(12) Uani 1 1 d . . . H1A' H 0.1830 0.4406 0.5001 0.048 Uiso 1 1 d R . . C2C C 0.2641(5) 0.3524(4) 0.5942(4) 0.0438(13) Uani 1 1 d . . . H2A' H 0.3058 0.2898 0.5517 0.053 Uiso 1 1 d R . . C3C C 0.2617(5) 0.3752(4) 0.6958(4) 0.0403(12) Uani 1 1 d . . . H3A' H 0.3004 0.3319 0.7345 0.048 Uiso 1 1 d R . . C4C C 0.1898(5) 0.4758(4) 0.7319(3) 0.0377(11) Uani 1 1 d . . . C5C C 0.1484(5) 0.5144(4) 0.6500(3) 0.0344(11) Uani 1 1 d . . . C1D C 0.4428(5) 0.7337(4) 0.6789(3) 0.0365(11) Uani 1 1 d . . . H1B' H 0.3949 0.7956 0.6693 0.044 Uiso 1 1 d R . . C2D C 0.5007(5) 0.6489(4) 0.6062(3) 0.0357(11) Uani 1 1 d . . . H2B' H 0.4990 0.6439 0.5385 0.043 Uiso 1 1 d R . . C3D C 0.5628(5) 0.5740(5) 0.6513(4) 0.0372(11) Uani 1 1 d . . . H3B' H 0.6097 0.5089 0.6191 0.045 Uiso 1 1 d R . . C4D C 0.5415(5) 0.6108(5) 0.7509(4) 0.0406(12) Uani 1 1 d . . . H4B' H 0.5721 0.5757 0.7987 0.049 Uiso 1 1 d R . . C5D C 0.4682(5) 0.7098(5) 0.7683(3) 0.0403(12) Uani 1 1 d . . . H5B' H 0.4402 0.7531 0.8300 0.048 Uiso 1 1 d R . . C1 C 0.4551(5) 0.1247(5) 0.6489(4) 0.0471(13) Uani 1 1 d . . . C2 C 0.3543(5) 0.0694(5) 0.6734(5) 0.0551(16) Uani 1 1 d . . . C3 C 0.2381(7) 0.0171(6) 0.7192(6) 0.072(2) Uani 1 1 d . . . H3A'' H 0.1525 0.0288 0.6913 0.087 Uiso 1 1 calc R . . H3B'' H 0.2284 -0.0776 0.7077 0.087 Uiso 1 1 calc R . . C4 C 0.2625(7) 0.0863(8) 0.8218(6) 0.080(2) Uani 1 1 d . . . H4A H 0.1796 0.0583 0.8529 0.097 Uiso 1 1 calc R . . H4B'' H 0.2760 0.1810 0.8312 0.097 Uiso 1 1 calc R . . C5 C 0.3857(9) 0.0664(8) 0.8742(5) 0.094(3) Uani 1 1 d . . . H5A H 0.3575 -0.0181 0.8875 0.113 Uiso 1 1 calc R . . H5B'' H 0.4578 0.0589 0.8290 0.113 Uiso 1 1 calc R . . C6 C 0.4473(9) 0.1685(10) 0.9669(6) 0.105(3) Uani 1 1 d . . . H6A H 0.5289 0.1448 0.9894 0.126 Uiso 1 1 calc R . . H6B H 0.3805 0.1624 1.0154 0.126 Uiso 1 1 calc R . . C7 C 0.4933(11) 0.3162(9) 0.9728(5) 0.112(4) Uani 1 1 d . . . H7A H 0.4112 0.3512 0.9709 0.134 Uiso 1 1 calc R . . H7B H 0.5503 0.3669 1.0355 0.134 Uiso 1 1 calc R . . C8 C 0.5747(7) 0.3329(7) 0.8887(4) 0.0657(17) Uani 1 1 d . . . C9 C 0.6272(6) 0.3314(5) 0.8157(4) 0.0469(13) Uani 1 1 d . . . C11 C 0.0701(5) 0.6104(5) 0.6606(4) 0.0379(11) Uani 1 1 d . A . C12 C 0.0016(5) 0.6883(5) 0.6878(4) 0.0417(12) Uani 1 1 d . . . C13A C -0.074(3) 0.789(3) 0.7518(14) 0.034(5) Uani 0.50 1 d P A 1 H13A H -0.0485 0.8712 0.7354 0.041 Uiso 0.50 1 calc PR A 1 H13B H -0.1746 0.7530 0.7344 0.041 Uiso 0.50 1 calc PR A 1 C14A C -0.043(2) 0.8187(19) 0.8586(17) 0.076(7) Uani 0.50 1 d P A 1 H14A H 0.0573 0.8428 0.8758 0.091 Uiso 0.50 1 calc PR A 1 H14B H -0.0797 0.8939 0.8940 0.091 Uiso 0.50 1 calc PR A 1 C15A C -0.1070(14) 0.7022(13) 0.8889(10) 0.070(4) Uani 0.50 1 d P A 1 H15A H -0.0976 0.6221 0.8383 0.084 Uiso 0.50 1 calc PR A 1 H15B H -0.2063 0.6968 0.8924 0.084 Uiso 0.50 1 calc PR A 1 C16A C -0.0444(15) 0.7060(18) 0.9853(9) 0.067(4) Uani 0.50 1 d P A 1 H16A H -0.1024 0.6339 1.0043 0.080 Uiso 0.50 1 calc PR A 1 H16B H -0.0505 0.7889 1.0341 0.080 Uiso 0.50 1 calc PR A 1 C17A C 0.101(2) 0.696(2) 0.9946(13) 0.073(5) Uani 0.50 1 d P A 1 H17A H 0.1198 0.6717 1.0536 0.087 Uiso 0.50 1 calc PR A 1 H17B H 0.1650 0.7806 0.9998 0.087 Uiso 0.50 1 calc PR A 1 C13B C -0.087(4) 0.771(4) 0.7177(17) 0.040(5) Uani 0.50 1 d P A 2 H13C H -0.1766 0.7346 0.6772 0.048 Uiso 0.50 1 calc PR A 2 H13D H -0.0463 0.8593 0.7139 0.048 Uiso 0.50 1 calc PR A 2 C14B C -0.1030(17) 0.7738(15) 0.8315(13) 0.051(4) Uani 0.50 1 d P A 2 H14C H -0.1635 0.8318 0.8593 0.061 Uiso 0.50 1 calc PR A 2 H14D H -0.1488 0.6846 0.8317 0.061 Uiso 0.50 1 calc PR A 2 C15B C 0.0365(16) 0.8222(14) 0.8997(11) 0.061(4) Uani 0.50 1 d P A 2 H15C H 0.1074 0.7914 0.8592 0.074 Uiso 0.50 1 calc PR A 2 H15D H 0.0621 0.9190 0.9194 0.074 Uiso 0.50 1 calc PR A 2 C16B C 0.046(2) 0.7853(15) 0.9885(11) 0.080(5) Uani 0.50 1 d P A 2 H16C H -0.0245 0.8156 1.0293 0.096 Uiso 0.50 1 calc PR A 2 H16D H 0.1368 0.8345 1.0254 0.096 Uiso 0.50 1 calc PR A 2 C17B C 0.030(3) 0.6387(18) 0.9777(15) 0.082(7) Uani 0.50 1 d P A 2 H17C H 0.0603 0.6287 1.0405 0.099 Uiso 0.50 1 calc PR A 2 H17D H -0.0670 0.5897 0.9581 0.099 Uiso 0.50 1 calc PR A 2 C18 C 0.1174(8) 0.5887(7) 0.9013(5) 0.079(2) Uani 1 1 d . . . C19 C 0.1554(6) 0.5332(5) 0.8285(4) 0.0486(13) Uani 1 1 d . A . 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 0.0304(4) 0.0259(4) 0.0373(4) 0.0117(3) 0.0091(3) 0.0076(3) Fe2 0.0284(4) 0.0251(3) 0.0278(3) 0.0086(3) 0.0071(3) 0.0053(3) C1A 0.081(4) 0.052(3) 0.032(3) 0.017(2) 0.008(3) 0.038(3) C2A 0.075(4) 0.051(3) 0.076(4) 0.042(3) 0.048(3) 0.034(3) C3A 0.047(3) 0.027(3) 0.085(4) 0.021(3) 0.026(3) 0.011(2) C4A 0.040(3) 0.023(2) 0.043(3) 0.0096(19) 0.012(2) 0.0105(19) C5A 0.032(3) 0.034(2) 0.041(3) 0.015(2) 0.003(2) 0.013(2) C1B 0.031(3) 0.035(3) 0.089(4) 0.029(3) 0.006(3) 0.008(2) C2B 0.050(3) 0.038(3) 0.050(3) 0.003(2) -0.001(3) 0.022(2) C3B 0.028(3) 0.053(3) 0.065(4) 0.020(3) 0.014(2) 0.013(2) C4B 0.040(3) 0.053(3) 0.056(3) 0.010(3) -0.005(3) 0.015(3) C5B 0.058(4) 0.060(4) 0.051(3) 0.027(3) 0.013(3) 0.034(3) C1C 0.036(3) 0.036(3) 0.039(3) 0.006(2) 0.008(2) -0.004(2) C2C 0.041(3) 0.026(2) 0.054(3) 0.001(2) 0.020(2) 0.000(2) C3C 0.042(3) 0.031(2) 0.056(3) 0.022(2) 0.022(2) 0.011(2) C4C 0.039(3) 0.034(2) 0.044(3) 0.017(2) 0.019(2) 0.008(2) C5C 0.027(3) 0.032(2) 0.046(3) 0.017(2) 0.008(2) 0.0021(19) C1D 0.038(3) 0.028(2) 0.043(3) 0.012(2) 0.007(2) 0.005(2) C2D 0.032(3) 0.038(3) 0.035(2) 0.014(2) 0.010(2) 0.000(2) C3D 0.026(3) 0.034(3) 0.046(3) 0.006(2) 0.008(2) 0.006(2) C4D 0.036(3) 0.043(3) 0.041(3) 0.015(2) -0.002(2) 0.006(2) C5D 0.042(3) 0.040(3) 0.032(2) 0.004(2) 0.005(2) 0.007(2) C1 0.033(3) 0.035(3) 0.070(4) 0.009(3) -0.004(3) 0.012(2) C2 0.019(3) 0.039(3) 0.105(5) 0.019(3) 0.003(3) 0.008(2) C3 0.049(4) 0.048(4) 0.123(6) 0.024(4) 0.022(4) 0.019(3) C4 0.065(5) 0.085(5) 0.106(6) 0.055(5) 0.036(4) 0.012(4) C5 0.152(8) 0.112(6) 0.065(5) 0.049(5) 0.045(5) 0.093(6) C6 0.092(6) 0.151(9) 0.092(6) 0.074(6) 0.027(5) 0.019(6) C7 0.210(10) 0.135(7) 0.034(3) 0.029(4) 0.056(5) 0.120(8) C8 0.081(5) 0.078(4) 0.044(3) 0.012(3) 0.011(3) 0.042(4) C9 0.052(3) 0.052(3) 0.038(3) 0.007(2) 0.007(2) 0.026(3) C11 0.029(3) 0.042(3) 0.045(3) 0.023(2) 0.005(2) 0.001(2) C12 0.025(3) 0.037(3) 0.065(3) 0.024(2) 0.000(2) 0.000(2) C13A 0.030(9) 0.029(9) 0.046(16) 0.009(12) 0.001(11) 0.014(7) C14A 0.063(16) 0.037(10) 0.102(18) -0.009(10) 0.022(12) 0.001(9) C15A 0.058(8) 0.070(9) 0.077(9) 0.005(7) 0.016(7) 0.028(7) C16A 0.061(10) 0.081(11) 0.052(8) 0.000(7) 0.013(7) 0.035(9) C17A 0.086(15) 0.081(15) 0.055(9) 0.019(10) 0.034(10) 0.028(10) C13B 0.039(9) 0.037(12) 0.044(15) 0.013(12) -0.004(10) 0.010(8) C14B 0.054(11) 0.033(9) 0.071(11) 0.018(8) 0.034(9) 0.015(7) C15B 0.065(11) 0.043(7) 0.061(9) -0.005(6) 0.005(7) 0.014(7) C16B 0.092(13) 0.067(10) 0.067(9) 0.005(8) 0.038(9) 0.010(10) C17B 0.13(2) 0.062(12) 0.073(12) 0.033(10) 0.074(14) 0.027(12) C18 0.120(6) 0.099(5) 0.056(4) 0.044(4) 0.048(4) 0.070(5) C19 0.058(4) 0.056(3) 0.048(3) 0.029(3) 0.025(3) 0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C5B 2.029(5) . ? Fe1 C1A 2.030(5) . ? Fe1 C3A 2.035(5) . ? Fe1 C1B 2.036(5) . ? Fe1 C2A 2.036(5) . ? Fe1 C2B 2.041(5) . ? Fe1 C4B 2.043(5) . ? Fe1 C5A 2.046(5) . ? Fe1 C4A 2.045(5) . ? Fe1 C3B 2.049(5) . ? Fe2 C5D 2.026(5) . ? Fe2 C4D 2.031(5) . ? Fe2 C1C 2.039(5) . ? Fe2 C2C 2.039(5) . ? Fe2 C4C 2.040(5) . ? Fe2 C1D 2.043(5) . ? Fe2 C5C 2.044(5) . ? Fe2 C3C 2.045(5) . ? Fe2 C2D 2.046(4) . ? Fe2 C3D 2.055(5) . ? C1A C2A 1.402(8) . ? C1A C5A 1.431(7) . ? C2A C3A 1.398(8) . ? C3A C4A 1.418(7) . ? C4A C9 1.423(7) . ? C4A C5A 1.447(7) . ? C5A C1 1.415(7) . ? C1B C5B 1.407(8) . ? C1B C2B 1.414(8) . ? C2B C3B 1.425(7) . ? C3B C4B 1.403(8) . ? C4B C5B 1.398(8) . ? C1C C2C 1.414(7) . ? C1C C5C 1.437(7) . ? C2C C3C 1.410(7) . ? C3C C4C 1.439(6) . ? C4C C19 1.434(7) . ? C4C C5C 1.449(7) . ? C5C C11 1.434(7) . ? C1D C5D 1.416(7) . ? C1D C2D 1.418(6) . ? C2D C3D 1.424(7) . ? C3D C4D 1.407(7) . ? C4D C5D 1.419(7) . ? C1 C2 1.181(7) . ? C2 C3 1.450(8) . ? C3 C4 1.431(10) . ? C4 C5 1.523(10) . ? C5 C6 1.474(12) . ? C6 C7 1.567(12) . ? C7 C8 1.516(9) . ? C8 C9 1.189(8) . ? C11 C12 1.205(7) . ? C12 C13B 1.40(4) . ? C12 C13A 1.57(3) . ? C13A C14A 1.48(3) . ? C14A C15A 1.50(2) . ? C15A C16A 1.493(19) . ? C16A C17A 1.49(3) . ? C17A C18 1.55(2) . ? C13B C14B 1.64(3) . ? C14B C15B 1.57(2) . ? C15B C16B 1.46(2) . ? C16B C17B 1.55(2) . ? C17B C18 1.483(19) . ? C18 C19 1.170(7) . ? 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 C5B Fe1 C1A 153.8(3) . . ? C5B Fe1 C3A 127.8(2) . . ? C1A Fe1 C3A 68.0(2) . . ? C5B Fe1 C1B 40.5(2) . . ? C1A Fe1 C1B 119.6(2) . . ? C3A Fe1 C1B 166.0(2) . . ? C5B Fe1 C2A 164.8(3) . . ? C1A Fe1 C2A 40.3(2) . . ? C3A Fe1 C2A 40.1(2) . . ? C1B Fe1 C2A 153.0(3) . . ? C5B Fe1 C2B 68.2(2) . . ? C1A Fe1 C2B 108.0(2) . . ? C3A Fe1 C2B 151.8(2) . . ? C1B Fe1 C2B 40.6(2) . . ? C2A Fe1 C2B 118.6(2) . . ? C5B Fe1 C4B 40.2(2) . . ? C1A Fe1 C4B 164.6(2) . . ? C3A Fe1 C4B 108.0(2) . . ? C1B Fe1 C4B 67.8(2) . . ? C2A Fe1 C4B 127.2(3) . . ? C2B Fe1 C4B 68.0(2) . . ? C5B Fe1 C5A 119.3(2) . . ? C1A Fe1 C5A 41.1(2) . . ? C3A Fe1 C5A 68.9(2) . . ? C1B Fe1 C5A 108.4(2) . . ? C2A Fe1 C5A 68.7(2) . . ? C2B Fe1 C5A 127.7(2) . . ? C4B Fe1 C5A 153.0(2) . . ? C5B Fe1 C4A 108.3(2) . . ? C1A Fe1 C4A 68.9(2) . . ? C3A Fe1 C4A 40.66(19) . . ? C1B Fe1 C4A 128.4(2) . . ? C2A Fe1 C4A 68.3(2) . . ? C2B Fe1 C4A 166.4(2) . . ? C4B Fe1 C4A 118.5(2) . . ? C5A Fe1 C4A 41.43(19) . . ? C5B Fe1 C3B 67.8(2) . . ? C1A Fe1 C3B 127.3(2) . . ? C3A Fe1 C3B 117.9(2) . . ? C1B Fe1 C3B 68.1(2) . . ? C2A Fe1 C3B 107.7(2) . . ? C2B Fe1 C3B 40.8(2) . . ? C4B Fe1 C3B 40.1(2) . . ? C5A Fe1 C3B 165.7(2) . . ? C4A Fe1 C3B 151.5(2) . . ? C5D Fe2 C4D 40.9(2) . . ? C5D Fe2 C1C 153.9(2) . . ? C4D Fe2 C1C 164.3(2) . . ? C5D Fe2 C2C 163.8(2) . . ? C4D Fe2 C2C 126.3(2) . . ? C1C Fe2 C2C 40.6(2) . . ? C5D Fe2 C4C 106.5(2) . . ? C4D Fe2 C4C 117.5(2) . . ? C1C Fe2 C4C 69.2(2) . . ? C2C Fe2 C4C 68.7(2) . . ? C5D Fe2 C1D 40.74(19) . . ? C4D Fe2 C1D 68.7(2) . . ? C1C Fe2 C1D 120.0(2) . . ? C2C Fe2 C1D 154.3(2) . . ? C4C Fe2 C1D 126.68(19) . . ? C5D Fe2 C5C 118.4(2) . . ? C4D Fe2 C5C 152.6(2) . . ? C1C Fe2 C5C 41.21(19) . . ? C2C Fe2 C5C 69.0(2) . . ? C4C Fe2 C5C 41.57(19) . . ? C1D Fe2 C5C 107.63(19) . . ? C5D Fe2 C3C 126.0(2) . . ? C4D Fe2 C3C 106.2(2) . . ? C1C Fe2 C3C 68.7(2) . . ? C2C Fe2 C3C 40.4(2) . . ? C4C Fe2 C3C 41.26(18) . . ? C1D Fe2 C3C 164.38(19) . . ? C5C Fe2 C3C 69.6(2) . . ? C5D Fe2 C2D 68.3(2) . . ? C4D Fe2 C2D 68.3(2) . . ? C1C Fe2 C2D 109.0(2) . . ? C2C Fe2 C2D 120.1(2) . . ? C4C Fe2 C2D 165.29(19) . . ? C1D Fe2 C2D 40.60(18) . . ? C5C Fe2 C2D 127.55(19) . . ? C3C Fe2 C2D 152.88(19) . . ? C5D Fe2 C3D 68.2(2) . . ? C4D Fe2 C3D 40.29(19) . . ? C1C Fe2 C3D 127.75(19) . . ? C2C Fe2 C3D 108.3(2) . . ? C4C Fe2 C3D 151.8(2) . . ? C1D Fe2 C3D 68.4(2) . . ? C5C Fe2 C3D 165.67(19) . . ? C3C Fe2 C3D 118.0(2) . . ? C2D Fe2 C3D 40.64(19) . . ? C2A C1A C5A 108.7(5) . . ? C2A C1A Fe1 70.1(3) . . ? C5A C1A Fe1 70.0(3) . . ? C3A C2A C1A 108.6(5) . . ? C3A C2A Fe1 69.9(3) . . ? C1A C2A Fe1 69.6(3) . . ? C2A C3A C4A 108.9(5) . . ? C2A C3A Fe1 70.0(3) . . ? C4A C3A Fe1 70.0(3) . . ? C3A C4A C9 131.3(5) . . ? C3A C4A C5A 107.3(4) . . ? C9 C4A C5A 121.4(4) . . ? C3A C4A Fe1 69.3(3) . . ? C9 C4A Fe1 126.5(4) . . ? C5A C4A Fe1 69.3(3) . . ? C1 C5A C1A 131.3(5) . . ? C1 C5A C4A 122.2(4) . . ? C1A C5A C4A 106.4(4) . . ? C1 C5A Fe1 125.8(3) . . ? C1A C5A Fe1 68.9(3) . . ? C4A C5A Fe1 69.3(3) . . ? C5B C1B C2B 108.0(5) . . ? C5B C1B Fe1 69.5(3) . . ? C2B C1B Fe1 69.9(3) . . ? C1B C2B C3B 107.4(5) . . ? C1B C2B Fe1 69.5(3) . . ? C3B C2B Fe1 69.9(3) . . ? C4B C3B C2B 107.7(5) . . ? C4B C3B Fe1 69.7(3) . . ? C2B C3B Fe1 69.3(3) . . ? C5B C4B C3B 108.5(5) . . ? C5B C4B Fe1 69.4(3) . . ? C3B C4B Fe1 70.2(3) . . ? C4B C5B C1B 108.4(5) . . ? C4B C5B Fe1 70.5(3) . . ? C1B C5B Fe1 70.0(3) . . ? C2C C1C C5C 108.4(4) . . ? C2C C1C Fe2 69.7(3) . . ? C5C C1C Fe2 69.6(3) . . ? C3C C2C C1C 109.4(4) . . ? C3C C2C Fe2 70.0(3) . . ? C1C C2C Fe2 69.7(3) . . ? C2C C3C C4C 107.6(4) . . ? C2C C3C Fe2 69.6(3) . . ? C4C C3C Fe2 69.2(3) . . ? C19 C4C C3C 130.7(5) . . ? C19 C4C C5C 121.4(4) . . ? C3C C4C C5C 107.9(4) . . ? C19 C4C Fe2 127.7(4) . . ? C3C C4C Fe2 69.6(3) . . ? C5C C4C Fe2 69.4(3) . . ? C11 C5C C1C 131.2(4) . . ? C11 C5C C4C 122.0(4) . . ? C1C C5C C4C 106.7(4) . . ? C11 C5C Fe2 128.4(3) . . ? C1C C5C Fe2 69.2(3) . . ? C4C C5C Fe2 69.0(3) . . ? C5D C1D C2D 107.4(4) . . ? C5D C1D Fe2 69.0(3) . . ? C2D C1D Fe2 69.8(3) . . ? C1D C2D C3D 108.2(4) . . ? C1D C2D Fe2 69.6(3) . . ? C3D C2D Fe2 70.0(3) . . ? C4D C3D C2D 107.9(4) . . ? C4D C3D Fe2 69.0(3) . . ? C2D C3D Fe2 69.3(3) . . ? C3D C4D C5D 108.1(4) . . ? C3D C4D Fe2 70.7(3) . . ? C5D C4D Fe2 69.3(3) . . ? C1D C5D C4D 108.4(4) . . ? C1D C5D Fe2 70.3(3) . . ? C4D C5D Fe2 69.7(3) . . ? C2 C1 C5A 169.7(6) . . ? C1 C2 C3 170.6(7) . . ? C4 C3 C2 107.8(6) . . ? C3 C4 C5 114.7(6) . . ? C6 C5 C4 116.7(7) . . ? C5 C6 C7 121.1(7) . . ? C8 C7 C6 111.1(6) . . ? C9 C8 C7 171.6(8) . . ? C8 C9 C4A 167.8(7) . . ? C12 C11 C5C 166.9(5) . . ? C11 C12 C13B 175.6(16) . . ? C11 C12 C13A 164.1(10) . . ? C13B C12 C13A 17.0(15) . . ? C14A C13A C12 114(2) . . ? C15A C14A C13A 110.0(19) . . ? C14A C15A C16A 113.4(15) . . ? C15A C16A C17A 119.0(13) . . ? C16A C17A C18 106.5(14) . . ? C12 C13B C14B 103(2) . . ? C15B C14B C13B 114.5(16) . . ? C16B C15B C14B 120.1(15) . . ? C15B C16B C17B 118.2(13) . . ? C18 C17B C16B 106.9(12) . . ? C19 C18 C17B 163.5(14) . . ? C19 C18 C17A 163.0(11) . . ? C17B C18 C17A 30.9(8) . . ? C18 C19 C4C 170.8(6) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.628 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.096