# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_section_title ;Synthesis and Characterisation of Dewar Benzene-Ferrocene Conjugates ; _publ_contact_author_name 'Martin Kotora' _publ_contact_author_email KOTORA@NATUR.CUNI.CZ loop_ _publ_author_name M.Kotora I.Cisarova S.Jankova P.Stepnicka F.Uhlik data_js196 _database_code_depnum_ccdc_archive 'CCDC 718552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2-ethoxycarbonyl-3-ferrocenyl-1,4,5,6-tetramethylbicyclo[2.2.0]hexa-2,5-diene ; _chemical_name_common ;2-ethoxycarbonyl-3-ferrocenyl-1,4,5,6- tetramethylbicyclo(2.2.0)hexa-2,5-diene ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H26 Fe O2' _chemical_formula_sum 'C23 H26 Fe O2' _chemical_formula_weight 390.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3695(2) _cell_length_b 10.1814(5) _cell_length_c 13.4315(6) _cell_angle_alpha 89.394(2) _cell_angle_beta 86.159(3) _cell_angle_gamma 75.385(3) _cell_volume 972.97(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3964 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 14778 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.24 _reflns_number_total 4282 _reflns_number_gt 3653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0269P)^2^+0.6243P] 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 4282 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _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 0.51276(3) 0.53628(3) 0.718108(19) 0.02157(9) Uani 1 1 d . . . O1 O 0.57368(19) 0.14113(14) 0.58430(10) 0.0316(3) Uani 1 1 d . . . O2 O 0.81983(17) -0.03167(13) 0.61762(9) 0.0240(3) Uani 1 1 d . . . C1 C 0.4682(2) 0.36312(18) 0.78288(13) 0.0219(4) Uani 1 1 d . . . C2 C 0.4168(3) 0.4759(2) 0.85196(14) 0.0260(4) Uani 1 1 d . . . H2 H 0.4684 0.4801 0.9128 0.031 Uiso 1 1 calc R . . C3 C 0.2747(3) 0.5791(2) 0.81156(15) 0.0294(4) Uani 1 1 d . . . H3 H 0.2166 0.6625 0.8412 0.035 Uiso 1 1 calc R . . C4 C 0.2365(2) 0.5329(2) 0.71802(15) 0.0286(4) Uani 1 1 d . . . H4 H 0.1486 0.5810 0.6758 0.034 Uiso 1 1 calc R . . C5 C 0.3543(2) 0.40119(19) 0.69947(14) 0.0245(4) Uani 1 1 d . . . H5 H 0.3575 0.3484 0.6430 0.029 Uiso 1 1 calc R . . C6 C 0.7934(3) 0.5005(2) 0.67897(15) 0.0294(4) Uani 1 1 d . . . H6 H 0.8847 0.4221 0.6925 0.035 Uiso 1 1 calc R . . C7 C 0.7343(3) 0.6173(2) 0.74098(16) 0.0293(4) Uani 1 1 d . . . H7 H 0.7801 0.6291 0.8022 0.035 Uiso 1 1 calc R . . C8 C 0.5930(3) 0.7131(2) 0.69324(17) 0.0334(5) Uani 1 1 d . . . H8 H 0.5297 0.7986 0.7176 0.040 Uiso 1 1 calc R . . C9 C 0.5654(3) 0.6551(2) 0.60154(16) 0.0347(5) Uani 1 1 d . . . H9 H 0.4808 0.6961 0.5553 0.042 Uiso 1 1 calc R . . C10 C 0.6893(3) 0.5241(2) 0.59287(15) 0.0316(4) Uani 1 1 d . . . H10 H 0.7004 0.4639 0.5399 0.038 Uiso 1 1 calc R . . C11 C 0.6144(2) 0.23977(18) 0.79694(13) 0.0215(4) Uani 1 1 d . . . C12 C 0.7021(2) 0.12767(18) 0.74308(13) 0.0220(4) Uani 1 1 d . . . C13 C 0.8341(3) 0.06542(19) 0.82404(13) 0.0238(4) Uani 1 1 d . . . C14 C 1.0078(3) 0.1200(2) 0.82788(14) 0.0258(4) Uani 1 1 d . . . C15 C 0.9199(3) 0.2288(2) 0.88384(14) 0.0255(4) Uani 1 1 d . . . C16 C 0.7296(2) 0.19405(19) 0.88829(13) 0.0231(4) Uani 1 1 d . . . C17 C 0.6882(2) 0.08362(18) 0.64131(13) 0.0217(4) Uani 1 1 d . . . C18 C 0.8120(3) -0.0851(2) 0.51820(14) 0.0272(4) Uani 1 1 d . . . H18A H 0.8359 -0.0215 0.4678 0.033 Uiso 1 1 calc R . . H18B H 0.6887 -0.0998 0.5102 0.033 Uiso 1 1 calc R . . C19 C 0.9598(3) -0.2169(2) 0.50744(16) 0.0335(5) Uani 1 1 d . . . H19A H 1.0801 -0.2019 0.5191 0.050 Uiso 1 1 calc R . . H19B H 0.9632 -0.2524 0.4412 0.050 Uiso 1 1 calc R . . H19C H 0.9306 -0.2808 0.5551 0.050 Uiso 1 1 calc R . . C20 C 0.8425(3) -0.0783(2) 0.85941(15) 0.0320(4) Uani 1 1 d . . . H20A H 0.9149 -0.1421 0.8107 0.048 Uiso 1 1 calc R . . H20B H 0.7174 -0.0905 0.8679 0.048 Uiso 1 1 calc R . . H20C H 0.9004 -0.0930 0.9219 0.048 Uiso 1 1 calc R . . C21 C 1.1996(3) 0.0683(2) 0.77974(16) 0.0362(5) Uani 1 1 d . . . H21A H 1.1946 0.0751 0.7086 0.054 Uiso 1 1 calc R . . H21B H 1.2480 -0.0249 0.7976 0.054 Uiso 1 1 calc R . . H21C H 1.2802 0.1213 0.8018 0.054 Uiso 1 1 calc R . . C22 C 0.9765(3) 0.3471(2) 0.92422(15) 0.0330(5) Uani 1 1 d . . . H22A H 1.1028 0.3444 0.8997 0.049 Uiso 1 1 calc R . . H22B H 0.9701 0.3435 0.9958 0.049 Uiso 1 1 calc R . . H22C H 0.8931 0.4297 0.9032 0.049 Uiso 1 1 calc R . . C23 C 0.6251(3) 0.1817(2) 0.98798(14) 0.0316(4) Uani 1 1 d . . . H23A H 0.7101 0.1267 1.0320 0.047 Uiso 1 1 calc R . . H23B H 0.5242 0.1402 0.9780 0.047 Uiso 1 1 calc R . . H23C H 0.5750 0.2703 1.0169 0.047 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 0.01675(13) 0.02312(15) 0.02473(15) -0.00050(10) -0.00069(9) -0.00498(10) O1 0.0336(7) 0.0317(8) 0.0271(7) -0.0019(6) -0.0125(6) -0.0008(6) O2 0.0250(6) 0.0248(7) 0.0211(6) -0.0035(5) -0.0041(5) -0.0036(5) C1 0.0189(8) 0.0232(10) 0.0245(9) 0.0009(7) 0.0000(7) -0.0073(7) C2 0.0234(9) 0.0300(11) 0.0231(9) -0.0015(8) 0.0029(7) -0.0051(8) C3 0.0213(9) 0.0279(11) 0.0351(11) -0.0009(8) 0.0082(8) -0.0018(8) C4 0.0151(8) 0.0334(11) 0.0373(11) 0.0074(9) -0.0025(7) -0.0060(8) C5 0.0189(9) 0.0281(10) 0.0289(10) 0.0021(8) -0.0044(7) -0.0093(7) C6 0.0167(9) 0.0303(11) 0.0411(12) -0.0013(9) 0.0020(8) -0.0068(8) C7 0.0241(9) 0.0314(11) 0.0365(11) -0.0001(9) -0.0034(8) -0.0139(8) C8 0.0280(10) 0.0227(10) 0.0503(13) 0.0024(9) 0.0015(9) -0.0090(8) C9 0.0301(11) 0.0419(13) 0.0350(11) 0.0149(10) -0.0045(8) -0.0145(9) C10 0.0287(10) 0.0384(12) 0.0293(11) -0.0031(9) 0.0075(8) -0.0135(9) C11 0.0195(8) 0.0238(9) 0.0221(9) 0.0022(7) -0.0029(7) -0.0071(7) C12 0.0209(9) 0.0240(10) 0.0218(9) 0.0014(7) -0.0047(7) -0.0061(7) C13 0.0255(9) 0.0245(10) 0.0209(9) -0.0001(7) -0.0050(7) -0.0046(7) C14 0.0253(9) 0.0301(10) 0.0228(9) 0.0052(8) -0.0061(7) -0.0073(8) C15 0.0267(9) 0.0301(11) 0.0218(9) 0.0041(8) -0.0062(7) -0.0099(8) C16 0.0239(9) 0.0236(10) 0.0217(9) -0.0009(7) -0.0036(7) -0.0051(7) C17 0.0221(9) 0.0212(9) 0.0226(9) -0.0001(7) -0.0023(7) -0.0066(7) C18 0.0339(10) 0.0280(10) 0.0205(9) -0.0040(8) -0.0034(7) -0.0088(8) C19 0.0354(11) 0.0306(11) 0.0331(11) -0.0063(9) 0.0028(8) -0.0070(9) C20 0.0369(11) 0.0262(11) 0.0327(11) 0.0013(8) -0.0079(8) -0.0062(8) C21 0.0301(11) 0.0437(13) 0.0339(11) 0.0032(10) -0.0023(8) -0.0074(9) C22 0.0391(11) 0.0354(12) 0.0287(11) 0.0002(9) -0.0049(8) -0.0164(9) C23 0.0372(11) 0.0323(11) 0.0267(10) 0.0027(8) -0.0042(8) -0.0109(9) _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 C2 2.0337(19) . ? Fe C6 2.0407(18) . ? Fe C10 2.0412(19) . ? Fe C3 2.0431(18) . ? Fe C5 2.0432(18) . ? Fe C9 2.045(2) . ? Fe C4 2.0450(18) . ? Fe C7 2.0474(18) . ? Fe C1 2.0481(18) . ? Fe C8 2.049(2) . ? O1 C17 1.212(2) . ? O2 C17 1.346(2) . ? O2 C18 1.457(2) . ? C1 C5 1.436(2) . ? C1 C2 1.442(3) . ? C1 C11 1.454(2) . ? C2 C3 1.416(3) . ? C2 H2 0.9300 . ? C3 C4 1.416(3) . ? C3 H3 0.9300 . ? C4 C5 1.416(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.416(3) . ? C6 C7 1.417(3) . ? C6 H6 0.9300 . ? C7 C8 1.417(3) . ? C7 H7 0.9300 . ? C8 C9 1.420(3) . ? C8 H8 0.9300 . ? C9 C10 1.414(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.352(3) . ? C11 C16 1.540(2) . ? C12 C17 1.461(2) . ? C12 C13 1.532(2) . ? C13 C20 1.521(3) . ? C13 C14 1.522(3) . ? C13 C16 1.575(2) . ? C14 C15 1.342(3) . ? C14 C21 1.484(3) . ? C15 C22 1.489(3) . ? C15 C16 1.528(3) . ? C16 C23 1.519(3) . ? C18 C19 1.501(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? 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 C2 Fe C6 121.51(8) . . ? C2 Fe C10 156.34(8) . . ? C6 Fe C10 40.58(8) . . ? C2 Fe C3 40.64(8) . . ? C6 Fe C3 156.72(8) . . ? C10 Fe C3 161.37(8) . . ? C2 Fe C5 68.92(8) . . ? C6 Fe C5 124.78(8) . . ? C10 Fe C5 106.83(8) . . ? C3 Fe C5 68.53(8) . . ? C2 Fe C9 162.02(8) . . ? C6 Fe C9 68.19(8) . . ? C10 Fe C9 40.49(9) . . ? C3 Fe C9 124.85(8) . . ? C5 Fe C9 119.87(8) . . ? C2 Fe C4 68.35(8) . . ? C6 Fe C4 161.46(8) . . ? C10 Fe C4 124.42(8) . . ? C3 Fe C4 40.53(8) . . ? C5 Fe C4 40.52(8) . . ? C9 Fe C4 107.27(8) . . ? C2 Fe C7 108.39(8) . . ? C6 Fe C7 40.56(8) . . ? C10 Fe C7 68.21(8) . . ? C3 Fe C7 121.59(8) . . ? C5 Fe C7 162.30(8) . . ? C9 Fe C7 68.17(8) . . ? C4 Fe C7 156.26(8) . . ? C2 Fe C1 41.36(7) . . ? C6 Fe C1 107.36(8) . . ? C10 Fe C1 120.11(8) . . ? C3 Fe C1 69.06(8) . . ? C5 Fe C1 41.09(7) . . ? C9 Fe C1 155.08(8) . . ? C4 Fe C1 68.74(7) . . ? C7 Fe C1 125.38(8) . . ? C2 Fe C8 125.41(8) . . ? C6 Fe C8 68.20(8) . . ? C10 Fe C8 68.21(9) . . ? C3 Fe C8 107.99(8) . . ? C5 Fe C8 155.24(8) . . ? C9 Fe C8 40.59(9) . . ? C4 Fe C8 120.87(8) . . ? C7 Fe C8 40.49(8) . . ? C1 Fe C8 162.65(8) . . ? C17 O2 C18 114.84(14) . . ? C5 C1 C2 106.59(16) . . ? C5 C1 C11 128.76(16) . . ? C2 C1 C11 124.59(16) . . ? C5 C1 Fe 69.27(10) . . ? C2 C1 Fe 68.79(10) . . ? C11 C1 Fe 124.65(12) . . ? C3 C2 C1 108.49(17) . . ? C3 C2 Fe 70.03(11) . . ? C1 C2 Fe 69.85(10) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe C2 H2 125.9 . . ? C2 C3 C4 108.00(17) . . ? C2 C3 Fe 69.33(10) . . ? C4 C3 Fe 69.81(10) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Fe C3 H3 126.4 . . ? C5 C4 C3 108.68(17) . . ? C5 C4 Fe 69.67(10) . . ? C3 C4 Fe 69.66(10) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe C4 H4 126.6 . . ? C4 C5 C1 108.25(17) . . ? C4 C5 Fe 69.81(10) . . ? C1 C5 Fe 69.64(10) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 126.3 . . ? C10 C6 C7 108.06(18) . . ? C10 C6 Fe 69.73(11) . . ? C7 C6 Fe 69.98(11) . . ? C10 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Fe C6 H6 125.9 . . ? C6 C7 C8 107.99(18) . . ? C6 C7 Fe 69.47(10) . . ? C8 C7 Fe 69.82(11) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? Fe C7 H7 126.3 . . ? C7 C8 C9 107.84(18) . . ? C7 C8 Fe 69.69(11) . . ? C9 C8 Fe 69.53(11) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? Fe C8 H8 126.3 . . ? C10 C9 C8 108.05(18) . . ? C10 C9 Fe 69.63(11) . . ? C8 C9 Fe 69.88(12) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe C9 H9 126.1 . . ? C9 C10 C6 108.06(18) . . ? C9 C10 Fe 69.88(11) . . ? C6 C10 Fe 69.69(11) . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Fe C10 H10 126.0 . . ? C12 C11 C1 137.21(17) . . ? C12 C11 C16 93.49(14) . . ? C1 C11 C16 129.30(16) . . ? C11 C12 C17 133.38(17) . . ? C11 C12 C13 94.82(14) . . ? C17 C12 C13 131.67(16) . . ? C20 C13 C14 119.20(16) . . ? C20 C13 C12 119.58(15) . . ? C14 C13 C12 114.95(15) . . ? C20 C13 C16 122.21(16) . . ? C14 C13 C16 85.74(13) . . ? C12 C13 C16 85.56(13) . . ? C15 C14 C21 135.28(19) . . ? C15 C14 C13 94.47(15) . . ? C21 C14 C13 130.17(18) . . ? C14 C15 C22 134.69(18) . . ? C14 C15 C16 94.25(15) . . ? C22 C15 C16 130.99(17) . . ? C23 C16 C15 120.66(15) . . ? C23 C16 C11 118.48(15) . . ? C15 C16 C11 114.64(15) . . ? C23 C16 C13 121.71(16) . . ? C15 C16 C13 85.52(13) . . ? C11 C16 C13 86.10(13) . . ? O1 C17 O2 123.19(16) . . ? O1 C17 C12 125.51(17) . . ? O2 C17 C12 111.30(15) . . ? O2 C18 C19 107.36(15) . . ? O2 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O2 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C20 H20A 109.5 . . ? C13 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C13 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 H23A 109.5 . . ? C16 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C16 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.24 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.470 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.054 #===END# data_js214twin _database_code_depnum_ccdc_archive 'CCDC 718553' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2-ethoxycarbonyl-3,4,5,6-tetramethylphenyl)ferrocene ; _chemical_formula_moiety 'C23 H26 Fe O2' _chemical_formula_sum 'C23 H26 Fe O2' _chemical_formula_weight 390.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.9261(5) _cell_length_b 7.3837(2) _cell_length_c 18.0000(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.6586(14) _cell_angle_gamma 90.00 _cell_volume 1890.30(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3967 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type none _exptl_special_details ; Twinning resulting into the formation of orthorhombic C centered superlattice was detected.The contribution of second part was included in the refinement by applying the matrix [1 0 0.5; 0 -1 0; 0 0 -1] on (hkl). The ratio was 0.525:0.475. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 26499 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.05 _reflns_number_total 3694 _reflns_number_gt 3349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0189P)^2^+1.3520P] 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 3694 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _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 0.10840(3) 0.30542(4) 0.66743(2) 0.02459(10) Uani 1 1 d . . . O1 O 0.34780(14) 0.2210(3) 0.51733(11) 0.0425(5) Uani 1 1 d . . . O2 O 0.30086(12) -0.0497(2) 0.54868(9) 0.0305(4) Uani 1 1 d . . . C1 C 0.21875(16) 0.1452(3) 0.65756(13) 0.0239(5) Uani 1 1 d . . . C2 C 0.17547(17) 0.2457(3) 0.58773(14) 0.0270(5) Uani 1 1 d . . . H2 H 0.2056 0.3294 0.5649 0.032 Uiso 1 1 calc R . . C3 C 0.07910(18) 0.1968(3) 0.55908(15) 0.0330(6) Uani 1 1 d . . . H3 H 0.0356 0.2418 0.5142 0.040 Uiso 1 1 calc R . . C4 C 0.06069(18) 0.0675(3) 0.61070(16) 0.0331(6) Uani 1 1 d . . . H4 H 0.0031 0.0124 0.6057 0.040 Uiso 1 1 calc R . . C5 C 0.14567(17) 0.0371(3) 0.67133(15) 0.0287(5) Uani 1 1 d . . . H5 H 0.1528 -0.0407 0.7134 0.034 Uiso 1 1 calc R . . C6 C 0.15818(19) 0.5000(3) 0.75070(16) 0.0358(6) Uani 1 1 d . . . H6 H 0.2205 0.5187 0.7800 0.043 Uiso 1 1 calc R . . C7 C 0.1116(2) 0.5796(3) 0.67723(17) 0.0400(6) Uani 1 1 d . . . H7 H 0.1382 0.6585 0.6496 0.048 Uiso 1 1 calc R . . C8 C 0.0166(2) 0.5168(4) 0.65333(17) 0.0409(7) Uani 1 1 d . . . H8 H -0.0298 0.5485 0.6077 0.049 Uiso 1 1 calc R . . C9 C 0.00575(19) 0.3971(4) 0.71192(16) 0.0360(6) Uani 1 1 d . . . H9 H -0.0490 0.3360 0.7111 0.043 Uiso 1 1 calc R . . C10 C 0.09252(18) 0.3870(3) 0.77150(15) 0.0332(6) Uani 1 1 d . . . H10 H 0.1047 0.3180 0.8167 0.040 Uiso 1 1 calc R . . C11 C 0.32209(16) 0.1385(3) 0.69908(14) 0.0247(5) Uani 1 1 d . . . C12 C 0.38288(17) 0.1336(3) 0.65240(14) 0.0253(5) Uani 1 1 d . . . C13 C 0.48058(17) 0.1335(3) 0.68516(15) 0.0268(5) Uani 1 1 d . . . C14 C 0.51917(17) 0.1353(3) 0.76673(15) 0.0279(5) Uani 1 1 d . . . C15 C 0.46030(18) 0.1317(3) 0.81392(14) 0.0276(5) Uani 1 1 d . . . C16 C 0.36172(17) 0.1337(3) 0.78071(14) 0.0256(5) Uani 1 1 d . . . C17 C 0.34227(17) 0.1129(3) 0.56620(15) 0.0293(5) Uani 1 1 d . . . C18 C 0.2535(2) -0.0854(4) 0.46678(15) 0.0415(7) Uani 1 1 d . . . H18A H 0.2984 -0.0855 0.4375 0.050 Uiso 1 1 calc R . . H18B H 0.2064 0.0066 0.4452 0.050 Uiso 1 1 calc R . . C19 C 0.2082(3) -0.2683(5) 0.4628(2) 0.0623(10) Uani 1 1 d . . . H19A H 0.2553 -0.3572 0.4860 0.093 Uiso 1 1 calc R . . H19B H 0.1777 -0.2996 0.4093 0.093 Uiso 1 1 calc R . . H19C H 0.1625 -0.2651 0.4906 0.093 Uiso 1 1 calc R . . C20 C 0.54466(18) 0.1250(4) 0.63455(16) 0.0342(6) Uani 1 1 d . . . H20A H 0.5075 0.1194 0.5807 0.051 Uiso 1 1 calc R . . H20B H 0.5836 0.0191 0.6476 0.051 Uiso 1 1 calc R . . H20C H 0.5836 0.2311 0.6431 0.051 Uiso 1 1 calc R . . C21 C 0.62518(18) 0.1349(4) 0.80208(17) 0.0366(6) Uani 1 1 d . . . H21A H 0.6412 0.1612 0.8568 0.055 Uiso 1 1 calc R . . H21B H 0.6521 0.2252 0.7769 0.055 Uiso 1 1 calc R . . H21C H 0.6494 0.0179 0.7949 0.055 Uiso 1 1 calc R . . C22 C 0.50355(19) 0.1233(4) 0.90161(15) 0.0369(6) Uani 1 1 d . . . H22A H 0.4546 0.1122 0.9258 0.055 Uiso 1 1 calc R . . H22B H 0.5388 0.2319 0.9196 0.055 Uiso 1 1 calc R . . H22C H 0.5446 0.0204 0.9151 0.055 Uiso 1 1 calc R . . C23 C 0.30052(19) 0.1286(4) 0.83388(15) 0.0345(6) Uani 1 1 d . . . H23A H 0.3042 0.0107 0.8572 0.052 Uiso 1 1 calc R . . H23B H 0.2366 0.1536 0.8042 0.052 Uiso 1 1 calc R . . H23C H 0.3219 0.2181 0.8741 0.052 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 0.02905(16) 0.02005(16) 0.02761(18) -0.00454(13) 0.01300(16) -0.00295(14) O1 0.0518(12) 0.0510(12) 0.0290(10) 0.0100(9) 0.0189(9) -0.0029(10) O2 0.0368(10) 0.0339(10) 0.0205(9) -0.0039(7) 0.0080(8) 0.0028(8) C1 0.0318(12) 0.0209(11) 0.0210(12) -0.0039(9) 0.0112(10) -0.0004(9) C2 0.0318(12) 0.0281(12) 0.0239(12) -0.0006(10) 0.0127(10) 0.0009(10) C3 0.0349(14) 0.0355(14) 0.0269(13) -0.0086(11) 0.0069(11) 0.0017(11) C4 0.0342(13) 0.0277(12) 0.0378(16) -0.0116(11) 0.0117(12) -0.0086(10) C5 0.0446(13) 0.0167(11) 0.0290(13) -0.0034(9) 0.0176(12) -0.0054(10) C6 0.0385(15) 0.0303(13) 0.0429(16) -0.0178(12) 0.0188(13) -0.0083(11) C7 0.0601(17) 0.0178(11) 0.0501(18) -0.0054(11) 0.0287(16) -0.0024(12) C8 0.0478(16) 0.0332(14) 0.0432(17) -0.0039(12) 0.0162(14) 0.0137(12) C9 0.0315(13) 0.0389(15) 0.0423(16) -0.0104(12) 0.0181(12) 0.0010(11) C10 0.0397(15) 0.0320(13) 0.0328(14) -0.0109(11) 0.0185(12) -0.0013(11) C11 0.0320(12) 0.0181(10) 0.0268(12) -0.0003(9) 0.0129(10) -0.0005(9) C12 0.0347(13) 0.0182(11) 0.0249(12) -0.0001(9) 0.0119(10) -0.0008(10) C13 0.0311(13) 0.0186(11) 0.0337(14) -0.0006(10) 0.0145(11) 0.0004(10) C14 0.0336(13) 0.0190(11) 0.0313(14) -0.0022(10) 0.0100(11) 0.0015(9) C15 0.0379(14) 0.0218(12) 0.0223(13) -0.0002(9) 0.0079(11) 0.0026(10) C16 0.0340(13) 0.0201(11) 0.0253(13) -0.0010(9) 0.0129(11) 0.0006(10) C17 0.0320(13) 0.0324(13) 0.0285(13) 0.0013(11) 0.0166(11) 0.0040(10) C18 0.0426(16) 0.0575(18) 0.0211(14) -0.0080(12) 0.0046(12) 0.0039(13) C19 0.059(2) 0.074(2) 0.0443(19) -0.0194(17) 0.0012(15) -0.0171(18) C20 0.0355(14) 0.0356(14) 0.0360(15) 0.0006(11) 0.0176(12) 0.0008(11) C21 0.0347(14) 0.0338(14) 0.0400(16) -0.0066(12) 0.0094(13) 0.0037(11) C22 0.0389(15) 0.0408(15) 0.0274(14) -0.0003(12) 0.0049(12) 0.0024(12) C23 0.0440(15) 0.0376(15) 0.0249(13) 0.0010(11) 0.0150(12) 0.0023(12) _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 C3 2.030(3) . ? Fe C2 2.031(2) . ? Fe C7 2.031(2) . ? Fe C8 2.041(3) . ? Fe C6 2.047(3) . ? Fe C9 2.047(2) . ? Fe C4 2.048(2) . ? Fe C10 2.049(2) . ? Fe C5 2.054(2) . ? Fe C1 2.079(2) . ? O1 C17 1.209(3) . ? O2 C17 1.343(3) . ? O2 C18 1.452(3) . ? C1 C5 1.433(3) . ? C1 C2 1.434(3) . ? C1 C11 1.497(3) . ? C2 C3 1.420(4) . ? C2 H2 0.9300 . ? C3 C4 1.416(4) . ? C3 H3 0.9300 . ? C4 C5 1.418(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.421(4) . ? C6 C10 1.421(4) . ? C6 H6 0.9300 . ? C7 C8 1.428(4) . ? C7 H7 0.9300 . ? C8 C9 1.423(4) . ? C8 H8 0.9300 . ? C9 C10 1.411(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.408(3) . ? C11 C12 1.412(3) . ? C12 C13 1.397(3) . ? C12 C17 1.493(4) . ? C13 C14 1.405(4) . ? C13 C20 1.509(3) . ? C14 C15 1.395(3) . ? C14 C21 1.516(3) . ? C15 C16 1.410(3) . ? C15 C22 1.515(3) . ? C16 C23 1.511(3) . ? C18 C19 1.503(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? 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 C3 Fe C2 40.92(10) . . ? C3 Fe C7 118.02(11) . . ? C2 Fe C7 105.91(11) . . ? C3 Fe C8 103.99(11) . . ? C2 Fe C8 122.28(11) . . ? C7 Fe C8 41.05(12) . . ? C3 Fe C6 154.91(11) . . ? C2 Fe C6 121.49(10) . . ? C7 Fe C6 40.79(12) . . ? C8 Fe C6 68.59(12) . . ? C3 Fe C9 122.53(11) . . ? C2 Fe C9 159.34(11) . . ? C7 Fe C9 68.73(11) . . ? C8 Fe C9 40.73(11) . . ? C6 Fe C9 68.28(11) . . ? C3 Fe C4 40.64(11) . . ? C2 Fe C4 68.47(10) . . ? C7 Fe C4 153.32(12) . . ? C8 Fe C4 118.37(11) . . ? C6 Fe C4 164.06(11) . . ? C9 Fe C4 106.87(11) . . ? C3 Fe C10 160.68(10) . . ? C2 Fe C10 158.13(10) . . ? C7 Fe C10 68.52(11) . . ? C8 Fe C10 68.25(11) . . ? C6 Fe C10 40.62(10) . . ? C9 Fe C10 40.30(10) . . ? C4 Fe C10 126.07(11) . . ? C3 Fe C5 68.22(10) . . ? C2 Fe C5 68.18(10) . . ? C7 Fe C5 163.67(12) . . ? C8 Fe C5 155.06(11) . . ? C6 Fe C5 128.17(11) . . ? C9 Fe C5 122.19(11) . . ? C4 Fe C5 40.45(10) . . ? C10 Fe C5 110.95(10) . . ? C3 Fe C1 68.81(10) . . ? C2 Fe C1 40.82(9) . . ? C7 Fe C1 125.20(11) . . ? C8 Fe C1 160.71(11) . . ? C6 Fe C1 109.95(10) . . ? C9 Fe C1 158.11(10) . . ? C4 Fe C1 68.52(10) . . ? C10 Fe C1 124.04(10) . . ? C5 Fe C1 40.56(9) . . ? C17 O2 C18 116.6(2) . . ? C5 C1 C2 106.0(2) . . ? C5 C1 C11 128.2(2) . . ? C2 C1 C11 125.2(2) . . ? C5 C1 Fe 68.77(13) . . ? C2 C1 Fe 67.80(13) . . ? C11 C1 Fe 134.37(16) . . ? C3 C2 C1 108.9(2) . . ? C3 C2 Fe 69.49(14) . . ? C1 C2 Fe 71.38(13) . . ? C3 C2 H2 125.5 . . ? C1 C2 H2 125.5 . . ? Fe C2 H2 125.2 . . ? C4 C3 C2 108.1(2) . . ? C4 C3 Fe 70.38(14) . . ? C2 C3 Fe 69.59(14) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe C3 H3 125.6 . . ? C3 C4 C5 107.8(2) . . ? C3 C4 Fe 68.99(14) . . ? C5 C4 Fe 69.98(13) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Fe C4 H4 126.5 . . ? C4 C5 C1 109.2(2) . . ? C4 C5 Fe 69.57(14) . . ? C1 C5 Fe 70.67(13) . . ? C4 C5 H5 125.4 . . ? C1 C5 H5 125.4 . . ? Fe C5 H5 125.9 . . ? C7 C6 C10 107.8(2) . . ? C7 C6 Fe 69.03(14) . . ? C10 C6 Fe 69.78(14) . . ? C7 C6 H6 126.1 . . ? C10 C6 H6 126.1 . . ? Fe C6 H6 126.7 . . ? C6 C7 C8 107.9(2) . . ? C6 C7 Fe 70.18(14) . . ? C8 C7 Fe 69.85(14) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? Fe C7 H7 125.5 . . ? C9 C8 C7 107.7(3) . . ? C9 C8 Fe 69.87(15) . . ? C7 C8 Fe 69.11(14) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? Fe C8 H8 126.5 . . ? C10 C9 C8 108.1(2) . . ? C10 C9 Fe 69.91(14) . . ? C8 C9 Fe 69.40(15) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Fe C9 H9 126.3 . . ? C9 C10 C6 108.4(2) . . ? C9 C10 Fe 69.79(14) . . ? C6 C10 Fe 69.61(14) . . ? C9 C10 H10 125.8 . . ? C6 C10 H10 125.8 . . ? Fe C10 H10 126.4 . . ? C16 C11 C12 118.6(2) . . ? C16 C11 C1 124.4(2) . . ? C12 C11 C1 117.0(2) . . ? C13 C12 C11 121.7(2) . . ? C13 C12 C17 118.8(2) . . ? C11 C12 C17 119.3(2) . . ? C12 C13 C14 119.0(2) . . ? C12 C13 C20 121.1(2) . . ? C14 C13 C20 119.8(2) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 C21 120.9(2) . . ? C13 C14 C21 118.9(2) . . ? C14 C15 C16 120.7(2) . . ? C14 C15 C22 119.2(2) . . ? C16 C15 C22 120.1(2) . . ? C11 C16 C15 119.8(2) . . ? C11 C16 C23 121.2(2) . . ? C15 C16 C23 119.0(2) . . ? O1 C17 O2 123.2(2) . . ? O1 C17 C12 126.4(2) . . ? O2 C17 C12 110.4(2) . . ? O2 C18 C19 106.5(2) . . ? O2 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? O2 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C20 H20A 109.5 . . ? C13 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C13 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 H23A 109.5 . . ? C16 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C16 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.370 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.057 _chemical_name_common (2-ethoxycarbonyl-3,4,5,6-tetramethylphenyl)ferrocene #===END# data_js228p _database_code_depnum_ccdc_archive 'CCDC 718554' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-ferrocenyl-2,3,4,5,6-pentamethylbenzene ; _chemical_formula_moiety 'C21 H24 Fe' _chemical_formula_sum 'C21 H24 Fe' _chemical_formula_weight 332.25 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 P21/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 20.1331(2) _cell_length_b 9.1392(2) _cell_length_c 8.9108(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.700(1) _cell_angle_gamma 90.00 _cell_volume 1599.48(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3825 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour block _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 22400 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3665 _reflns_number_gt 3133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' _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^)+(0.0390P)^2^+0.8081P] 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 3665 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.121929(11) 0.51858(2) 0.37193(2) 0.02090(9) Uani 1 1 d . . . C1 C 0.20360(8) 0.39162(17) 0.48535(18) 0.0224(3) Uani 1 1 d . . . C2 C 0.17979(9) 0.48602(17) 0.59031(18) 0.0231(3) Uani 1 1 d . . . H2 H 0.2059 0.5559 0.6528 0.028 Uiso 1 1 calc R . . C3 C 0.10974(9) 0.45600(19) 0.58396(19) 0.0262(3) Uani 1 1 d . . . H3 H 0.0825 0.5022 0.6413 0.031 Uiso 1 1 calc R . . C4 C 0.08904(9) 0.34282(18) 0.47427(19) 0.0269(4) Uani 1 1 d . . . H4 H 0.0459 0.3012 0.4477 0.032 Uiso 1 1 calc R . . C5 C 0.14603(9) 0.30459(17) 0.41245(19) 0.0247(3) Uani 1 1 d . . . H5 H 0.1461 0.2344 0.3369 0.030 Uiso 1 1 calc R . . C6 C 0.15024(9) 0.63793(18) 0.20184(18) 0.0276(4) Uani 1 1 d . . . H6 H 0.1932 0.6399 0.1794 0.033 Uiso 1 1 calc R . . C7 C 0.12681(10) 0.73181(18) 0.3063(2) 0.0289(4) Uani 1 1 d . . . H7 H 0.1518 0.8061 0.3641 0.035 Uiso 1 1 calc R . . C8 C 0.05862(9) 0.69264(19) 0.3073(2) 0.0314(4) Uani 1 1 d . . . H8 H 0.0311 0.7363 0.3659 0.038 Uiso 1 1 calc R . . C9 C 0.04000(9) 0.5747(2) 0.2027(2) 0.0324(4) Uani 1 1 d . . . H9 H -0.0020 0.5279 0.1806 0.039 Uiso 1 1 calc R . . C10 C 0.09645(10) 0.54049(19) 0.13773(19) 0.0293(4) Uani 1 1 d . . . H10 H 0.0980 0.4673 0.0660 0.035 Uiso 1 1 calc R . . C11 C 0.27316(8) 0.37137(18) 0.45578(18) 0.0240(3) Uani 1 1 d . . . C12 C 0.29625(9) 0.22597(19) 0.44738(18) 0.0263(4) Uani 1 1 d . . . C13 C 0.35457(9) 0.1988(2) 0.3907(2) 0.0322(4) Uani 1 1 d . . . C14 C 0.39343(9) 0.3154(2) 0.3544(2) 0.0348(4) Uani 1 1 d . . . C15 C 0.37548(9) 0.4593(2) 0.3817(2) 0.0318(4) Uani 1 1 d . . . C16 C 0.31521(9) 0.48819(19) 0.43130(19) 0.0266(4) Uani 1 1 d . . . C17 C 0.26108(10) 0.09954(19) 0.5085(2) 0.0324(4) Uani 1 1 d . . . H17A H 0.2317 0.0501 0.4243 0.049 Uiso 1 1 calc R . . H17B H 0.2346 0.1362 0.5778 0.049 Uiso 1 1 calc R . . H17C H 0.2947 0.0323 0.5622 0.049 Uiso 1 1 calc R . . C18 C 0.37595(12) 0.0421(2) 0.3674(3) 0.0465(5) Uani 1 1 d . . . H18A H 0.4115 0.0133 0.4530 0.070 Uiso 1 1 calc R . . H18B H 0.3923 0.0361 0.2743 0.070 Uiso 1 1 calc R . . H18C H 0.3375 -0.0218 0.3604 0.070 Uiso 1 1 calc R . . C19 C 0.45444(11) 0.2821(3) 0.2864(3) 0.0509(6) Uani 1 1 d . . . H19A H 0.4863 0.2232 0.3572 0.076 Uiso 1 1 calc R . . H19B H 0.4759 0.3720 0.2676 0.076 Uiso 1 1 calc R . . H19C H 0.4398 0.2300 0.1913 0.076 Uiso 1 1 calc R . . C20 C 0.41946(10) 0.5860(3) 0.3518(3) 0.0475(5) Uani 1 1 d . . . H20A H 0.4664 0.5568 0.3755 0.071 Uiso 1 1 calc R . . H20B H 0.4134 0.6675 0.4154 0.071 Uiso 1 1 calc R . . H20C H 0.4065 0.6140 0.2455 0.071 Uiso 1 1 calc R . . C21 C 0.29753(9) 0.6455(2) 0.4590(2) 0.0332(4) Uani 1 1 d . . . H21A H 0.2521 0.6502 0.4756 0.050 Uiso 1 1 calc R . . H21B H 0.3004 0.7036 0.3709 0.050 Uiso 1 1 calc R . . H21C H 0.3289 0.6825 0.5480 0.050 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 0.02615(14) 0.01617(12) 0.02023(13) 0.00117(9) 0.00479(9) -0.00011(9) C1 0.0281(8) 0.0162(7) 0.0217(7) 0.0020(6) 0.0030(6) 0.0008(6) C2 0.0301(9) 0.0202(8) 0.0183(7) 0.0010(6) 0.0039(6) -0.0019(6) C3 0.0325(9) 0.0241(8) 0.0235(8) 0.0041(7) 0.0095(7) 0.0006(7) C4 0.0295(9) 0.0202(8) 0.0307(9) 0.0062(7) 0.0060(7) -0.0036(7) C5 0.0329(9) 0.0144(7) 0.0251(8) 0.0010(6) 0.0025(7) -0.0013(6) C6 0.0371(9) 0.0242(8) 0.0230(8) 0.0049(7) 0.0095(7) -0.0001(7) C7 0.0443(10) 0.0156(8) 0.0267(8) 0.0046(7) 0.0076(7) -0.0001(7) C8 0.0386(10) 0.0240(9) 0.0330(9) 0.0073(7) 0.0109(8) 0.0109(8) C9 0.0315(9) 0.0301(9) 0.0321(9) 0.0070(8) -0.0006(7) 0.0026(7) C10 0.0418(10) 0.0245(8) 0.0193(8) 0.0018(7) 0.0018(7) 0.0029(7) C11 0.0283(8) 0.0229(8) 0.0191(7) -0.0010(6) 0.0018(6) 0.0000(7) C12 0.0294(9) 0.0252(8) 0.0218(8) -0.0008(7) 0.0003(6) 0.0023(7) C13 0.0336(9) 0.0337(10) 0.0264(9) -0.0034(7) -0.0001(7) 0.0087(8) C14 0.0283(9) 0.0504(12) 0.0240(8) -0.0001(8) 0.0025(7) 0.0092(8) C15 0.0257(9) 0.0420(11) 0.0263(9) 0.0044(8) 0.0023(7) -0.0016(8) C16 0.0275(8) 0.0278(9) 0.0226(8) 0.0021(7) 0.0014(6) -0.0013(7) C17 0.0405(10) 0.0201(8) 0.0330(9) 0.0016(7) 0.0001(8) 0.0040(7) C18 0.0486(12) 0.0429(12) 0.0455(12) -0.0091(10) 0.0048(10) 0.0176(10) C19 0.0397(11) 0.0732(16) 0.0418(12) -0.0017(11) 0.0130(9) 0.0131(11) C20 0.0331(11) 0.0570(14) 0.0532(13) 0.0136(11) 0.0109(9) -0.0067(10) C21 0.0319(9) 0.0255(9) 0.0406(10) 0.0010(8) 0.0042(8) -0.0076(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C5 2.0282(16) . ? Fe C4 2.0288(16) . ? Fe C3 2.0399(16) . ? Fe C9 2.0405(17) . ? Fe C8 2.0406(17) . ? Fe C7 2.0430(16) . ? Fe C10 2.0464(17) . ? Fe C6 2.0474(16) . ? Fe C2 2.0581(16) . ? Fe C1 2.0835(16) . ? C1 C2 1.430(2) . ? C1 C5 1.438(2) . ? C1 C11 1.492(2) . ? C2 C3 1.426(2) . ? C2 H2 0.9300 . ? C3 C4 1.421(2) . ? C3 H3 0.9300 . ? C4 C5 1.421(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.421(2) . ? C6 C10 1.421(2) . ? C6 H6 0.9300 . ? C7 C8 1.421(3) . ? C7 H7 0.9300 . ? C8 C9 1.420(3) . ? C8 H8 0.9300 . ? C9 C10 1.419(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.409(2) . ? C11 C12 1.415(2) . ? C12 C13 1.399(2) . ? C12 C17 1.517(2) . ? C13 C14 1.401(3) . ? C13 C18 1.522(3) . ? C14 C15 1.399(3) . ? C14 C19 1.515(3) . ? C15 C16 1.405(3) . ? C15 C20 1.517(3) . ? C16 C21 1.514(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe C4 41.02(7) . . ? C5 Fe C3 68.75(7) . . ? C4 Fe C3 40.89(7) . . ? C5 Fe C9 119.80(7) . . ? C4 Fe C9 103.92(7) . . ? C3 Fe C9 120.83(7) . . ? C5 Fe C8 155.79(7) . . ? C4 Fe C8 119.91(7) . . ? C3 Fe C8 106.56(7) . . ? C9 Fe C8 40.73(7) . . ? C5 Fe C7 161.09(7) . . ? C4 Fe C7 157.63(7) . . ? C3 Fe C7 123.75(7) . . ? C9 Fe C7 68.33(7) . . ? C8 Fe C7 40.72(7) . . ? C5 Fe C10 105.81(7) . . ? C4 Fe C10 120.16(7) . . ? C3 Fe C10 156.60(7) . . ? C9 Fe C10 40.64(7) . . ? C8 Fe C10 68.59(7) . . ? C7 Fe C10 68.41(7) . . ? C5 Fe C6 123.43(7) . . ? C4 Fe C6 157.84(7) . . ? C3 Fe C6 160.88(7) . . ? C9 Fe C6 68.31(7) . . ? C8 Fe C6 68.54(7) . . ? C7 Fe C6 40.65(7) . . ? C10 Fe C6 40.64(7) . . ? C5 Fe C2 68.20(6) . . ? C4 Fe C2 68.49(7) . . ? C3 Fe C2 40.72(7) . . ? C9 Fe C2 158.84(7) . . ? C8 Fe C2 124.62(7) . . ? C7 Fe C2 110.83(7) . . ? C10 Fe C2 160.27(7) . . ? C6 Fe C2 125.81(7) . . ? C5 Fe C1 40.91(6) . . ? C4 Fe C1 69.01(7) . . ? C3 Fe C1 68.74(7) . . ? C9 Fe C1 157.23(7) . . ? C8 Fe C1 161.52(7) . . ? C7 Fe C1 125.98(7) . . ? C10 Fe C1 122.91(7) . . ? C6 Fe C1 109.71(7) . . ? C2 Fe C1 40.40(6) . . ? C2 C1 C5 106.04(14) . . ? C2 C1 C11 130.74(14) . . ? C5 C1 C11 123.11(14) . . ? C2 C1 Fe 68.84(9) . . ? C5 C1 Fe 67.48(9) . . ? C11 C1 Fe 130.89(11) . . ? C3 C2 C1 109.20(14) . . ? C3 C2 Fe 68.96(9) . . ? C1 C2 Fe 70.75(9) . . ? C3 C2 H2 125.4 . . ? C1 C2 H2 125.4 . . ? Fe C2 H2 126.5 . . ? C4 C3 C2 107.78(15) . . ? C4 C3 Fe 69.14(9) . . ? C2 C3 Fe 70.33(9) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Fe C3 H3 126.0 . . ? C3 C4 C5 107.81(15) . . ? C3 C4 Fe 69.97(9) . . ? C5 C4 Fe 69.47(9) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Fe C4 H4 126.0 . . ? C4 C5 C1 109.16(14) . . ? C4 C5 Fe 69.51(9) . . ? C1 C5 Fe 71.61(9) . . ? C4 C5 H5 125.4 . . ? C1 C5 H5 125.4 . . ? Fe C5 H5 125.0 . . ? C7 C6 C10 107.95(16) . . ? C7 C6 Fe 69.51(9) . . ? C10 C6 Fe 69.64(9) . . ? C7 C6 H6 126.0 . . ? C10 C6 H6 126.0 . . ? Fe C6 H6 126.4 . . ? C8 C7 C6 108.21(16) . . ? C8 C7 Fe 69.55(9) . . ? C6 C7 Fe 69.84(9) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.3 . . ? C9 C8 C7 107.65(16) . . ? C9 C8 Fe 69.63(10) . . ? C7 C8 Fe 69.73(10) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? Fe C8 H8 126.0 . . ? C10 C9 C8 108.40(16) . . ? C10 C9 Fe 69.90(10) . . ? C8 C9 Fe 69.64(10) . . ? C10 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? Fe C9 H9 126.2 . . ? C9 C10 C6 107.80(16) . . ? C9 C10 Fe 69.46(10) . . ? C6 C10 Fe 69.72(9) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 126.3 . . ? C16 C11 C12 119.20(15) . . ? C16 C11 C1 123.53(15) . . ? C12 C11 C1 117.24(14) . . ? C13 C12 C11 119.82(16) . . ? C13 C12 C17 119.30(16) . . ? C11 C12 C17 120.76(15) . . ? C12 C13 C14 120.27(17) . . ? C12 C13 C18 120.07(18) . . ? C14 C13 C18 119.66(18) . . ? C15 C14 C13 119.74(17) . . ? C15 C14 C19 121.42(19) . . ? C13 C14 C19 118.84(19) . . ? C14 C15 C16 120.35(17) . . ? C14 C15 C20 120.29(18) . . ? C16 C15 C20 119.32(18) . . ? C15 C16 C11 119.75(16) . . ? C15 C16 C21 118.68(16) . . ? C11 C16 C21 121.56(16) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.330 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.051 #===END# _chemical_name_common 1-ferrocenyl-2,3,4,5,6-pentamethylbenzene