#------------------------------------------------------------------------------ #$Date: 2008-02-24 20:27:26 +0000 (Sun, 24 Feb 2008) $ #$Revision: 175 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100888.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100888 _publ_section_title ; Synthesis and structure of ethenyl and ethynyl ferrocene polyaromatic dyads. ; loop_ _publ_author_name 'Hudson R.D.A' 'Gallagher, J.' 'Jennings, S.' 'McAdam C. John' 'Manning Anthony R.' 'Robinson, Brian H.' 'Simpson, Jim' _chemical_formula_moiety 'C28 H18 Fe' _chemical_formula_sum 'C28 H18 Fe' _chemical_formula_weight 410.27 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 7.810(5) _cell_length_b 9.956(6) _cell_length_c 13.205(8) _cell_angle_alpha 107.540(6) _cell_angle_beta 101.733(7) _cell_angle_gamma 100.521(6) _cell_volume 925.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 4181 _cell_measurement_theta_min 2.759 _cell_measurement_theta_max 26.128 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747516 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS Bruker 1999' _diffrn_ambient_temperature 163(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 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11682 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3719 _reflns_number_gt 2932 _reflns_threshold_expression I>2\s(I) ##; ##SHELXS-97 (Sheldrick, 1997) & TITAN2000 (Hunter & Simpson 1999) ##; ##; ##SHELXL-97 (Sheldrick, 1997) & TITAN2000 (Hunter & Simpson 1999) ##; _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^)+(0.0542P)^2^+0.0000P] 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 3719 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 C1 C 0.1980(3) 0.0861(3) 0.3521(2) 0.0340(6) Uani 1 1 d . . . H1 H 0.1635 0.0377 0.3997 0.041 Uiso 1 1 calc R . . C2 C 0.1999(3) 0.2331(3) 0.3627(2) 0.0328(6) Uani 1 1 d . . . H2 H 0.1670 0.3003 0.4187 0.039 Uiso 1 1 calc R . . C3 C 0.2595(3) 0.2613(3) 0.2749(2) 0.0298(6) Uani 1 1 d . . . H3 H 0.2736 0.3510 0.2620 0.036 Uiso 1 1 calc R . . C4 C 0.2943(3) 0.1333(3) 0.2099(2) 0.0275(6) Uani 1 1 d . . . H4 H 0.3355 0.1220 0.1456 0.033 Uiso 1 1 calc R . . C5 C 0.2571(3) 0.0247(3) 0.2575(2) 0.0282(6) Uani 1 1 d . . . H5 H 0.2694 -0.0719 0.2308 0.034 Uiso 1 1 calc R . . Fe1 Fe 0.45496(4) 0.20244(3) 0.36941(3) 0.02010(12) Uani 1 1 d . . . C6 C 0.6214(3) 0.1998(3) 0.51043(19) 0.0234(5) Uani 1 1 d . . . H6 H 0.5857 0.1541 0.5592 0.028 Uiso 1 1 calc R . . C7 C 0.6244(3) 0.3460(3) 0.5174(2) 0.0267(6) Uani 1 1 d . . . H7 H 0.5901 0.4146 0.5717 0.032 Uiso 1 1 calc R . . C8 C 0.6871(3) 0.3719(3) 0.4296(2) 0.0285(6) Uani 1 1 d . . . H8 H 0.7032 0.4610 0.4158 0.034 Uiso 1 1 calc R . . C9 C 0.7216(3) 0.2420(2) 0.3660(2) 0.0248(5) Uani 1 1 d . . . H9 H 0.7632 0.2286 0.3018 0.030 Uiso 1 1 calc R . . C10 C 0.6823(3) 0.1340(2) 0.41594(18) 0.0205(5) Uani 1 1 d . . . C11 C 0.6986(3) -0.0135(3) 0.37773(18) 0.0214(5) Uani 1 1 d . . . C12 C 0.7138(3) -0.1352(3) 0.34459(19) 0.0228(5) Uani 1 1 d . . . C13 C 0.7384(3) -0.2790(2) 0.29776(19) 0.0222(5) Uani 1 1 d . . . C14 C 0.9100(3) -0.3035(3) 0.3270(2) 0.0262(5) Uani 1 1 d . . . H14 H 1.0042 -0.2291 0.3847 0.031 Uiso 1 1 calc R . . C15 C 0.9443(3) -0.4337(3) 0.2736(2) 0.0255(5) Uani 1 1 d . . . H15 H 1.0612 -0.4480 0.2957 0.031 Uiso 1 1 calc R . . C16 C 0.8086(3) -0.5458(2) 0.18692(19) 0.0212(5) Uani 1 1 d . . . C17 C 0.8432(3) -0.6796(2) 0.1249(2) 0.0243(5) Uani 1 1 d . . . H17 H 0.9607 -0.6942 0.1432 0.029 Uiso 1 1 calc R . . C18 C 0.7113(3) -0.7840(2) 0.04151(19) 0.0246(5) Uani 1 1 d . . . H18 H 0.7394 -0.8695 0.0008 0.029 Uiso 1 1 calc R . . C19 C 0.5286(3) -0.7703(2) 0.01194(19) 0.0210(5) Uani 1 1 d . . . C20 C 0.3895(3) -0.8791(3) -0.0730(2) 0.0261(5) Uani 1 1 d . . . H20 H 0.4150 -0.9654 -0.1147 0.031 Uiso 1 1 calc R . . C21 C 0.2134(3) -0.8627(3) -0.0976(2) 0.0287(6) Uani 1 1 d . . . H21 H 0.1199 -0.9393 -0.1541 0.034 Uiso 1 1 calc R . . C22 C 0.1739(3) -0.7369(3) -0.0410(2) 0.0262(5) Uani 1 1 d . . . H22 H 0.0538 -0.7270 -0.0591 0.031 Uiso 1 1 calc R . . C23 C 0.3108(3) -0.6221(2) 0.04419(18) 0.0212(5) Uani 1 1 d . . . C24 C 0.2769(3) -0.4877(3) 0.10440(19) 0.0235(5) Uani 1 1 d . . . H24 H 0.1581 -0.4750 0.0876 0.028 Uiso 1 1 calc R . . C25 C 0.4114(3) -0.3786(3) 0.18487(19) 0.0227(5) Uani 1 1 d . . . H25 H 0.3847 -0.2905 0.2221 0.027 Uiso 1 1 calc R . . C26 C 0.5935(3) -0.3928(2) 0.21538(18) 0.0193(5) Uani 1 1 d . . . C27 C 0.6308(3) -0.5261(2) 0.15896(18) 0.0191(5) Uani 1 1 d . . . C28 C 0.4892(3) -0.6400(2) 0.07191(18) 0.0198(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0192(13) 0.0449(16) 0.0314(14) 0.0163(13) -0.0005(11) -0.0038(11) C2 0.0224(13) 0.0393(16) 0.0285(14) 0.0015(12) 0.0030(11) 0.0108(11) C3 0.0275(14) 0.0275(13) 0.0313(14) 0.0098(11) -0.0017(11) 0.0118(11) C4 0.0285(14) 0.0285(13) 0.0198(12) 0.0044(10) 0.0020(10) 0.0060(11) C5 0.0215(13) 0.0232(13) 0.0307(14) 0.0053(11) -0.0035(11) 0.0029(10) Fe1 0.01817(19) 0.01909(19) 0.02013(18) 0.00495(13) 0.00273(13) 0.00404(13) C6 0.0175(12) 0.0282(13) 0.0208(12) 0.0069(10) 0.0011(9) 0.0044(10) C7 0.0218(13) 0.0232(13) 0.0252(12) -0.0038(10) 0.0037(10) 0.0061(10) C8 0.0234(13) 0.0183(12) 0.0374(15) 0.0073(11) 0.0022(11) 0.0010(10) C9 0.0193(12) 0.0241(13) 0.0297(13) 0.0097(11) 0.0070(10) 0.0017(10) C10 0.0165(11) 0.0205(12) 0.0194(11) 0.0035(9) 0.0012(9) 0.0028(9) C11 0.0180(12) 0.0262(13) 0.0183(11) 0.0083(10) 0.0023(9) 0.0037(10) C12 0.0214(12) 0.0241(13) 0.0220(12) 0.0093(10) 0.0049(10) 0.0027(10) C13 0.0261(13) 0.0202(12) 0.0210(12) 0.0078(10) 0.0074(10) 0.0060(10) C14 0.0227(13) 0.0252(13) 0.0255(12) 0.0076(10) 0.0009(10) 0.0026(10) C15 0.0183(12) 0.0279(13) 0.0297(13) 0.0106(11) 0.0037(10) 0.0073(10) C16 0.0206(12) 0.0225(12) 0.0240(12) 0.0122(10) 0.0066(10) 0.0064(10) C17 0.0230(13) 0.0278(13) 0.0309(13) 0.0152(11) 0.0122(11) 0.0137(10) C18 0.0316(14) 0.0197(12) 0.0283(13) 0.0101(10) 0.0146(11) 0.0108(10) C19 0.0226(12) 0.0216(12) 0.0215(12) 0.0104(10) 0.0086(10) 0.0047(10) C20 0.0331(14) 0.0205(12) 0.0245(12) 0.0076(10) 0.0109(11) 0.0038(10) C21 0.0292(14) 0.0263(13) 0.0227(12) 0.0069(10) 0.0024(11) -0.0032(11) C22 0.0183(12) 0.0329(14) 0.0278(13) 0.0154(11) 0.0039(10) 0.0023(10) C23 0.0215(12) 0.0257(12) 0.0201(11) 0.0130(10) 0.0079(10) 0.0043(10) C24 0.0190(12) 0.0285(13) 0.0286(13) 0.0154(11) 0.0075(10) 0.0094(10) C25 0.0246(13) 0.0238(12) 0.0251(12) 0.0118(10) 0.0102(10) 0.0102(10) C26 0.0193(12) 0.0221(12) 0.0204(11) 0.0114(10) 0.0072(9) 0.0062(9) C27 0.0197(12) 0.0209(12) 0.0198(11) 0.0105(9) 0.0067(9) 0.0053(9) C28 0.0186(12) 0.0229(12) 0.0202(11) 0.0119(10) 0.0057(9) 0.0032(9)