#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100891.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_1100891 _publ_section_title ; Synthesis and structure of ethenyl and ethynyl ferrocene polyaromatic dyads. ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M P21/c loop_ _publ_author_name 'Hudson R.D.A' 'Gallagher, J.' 'Jennings, S.' 'McAdam C. John' 'Manning Anthony R.' 'Robinson, Brian H.' 'Simpson, Jim' _chemical_name_systematic ; (E)-1-ferrocenyl-2-(1-pyrenyl) ethene ; _chemical_formula_moiety 'C28 H20 Fe' _chemical_formula_sum 'C28 H20 Fe' _chemical_formula_weight 412.29 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' _symmetry_cell_setting monoclinic 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 19.12(3) _cell_length_b 7.379(9) _cell_length_c 14.89(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.62(3) _cell_angle_gamma 90.00 _cell_volume 1966(5) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 3254 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.65 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845189 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS Bruker 1997' _diffrn_ambient_temperature 168(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 23370 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 26.47 _reflns_number_total 4001 _reflns_number_gt 2081 _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^)+(0.0270P)^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 4001 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.829 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean '< 0.001' 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 0.47603(17) 0.8951(4) 0.7826(2) 0.0460(8) Uani 1 1 d . . . H1 H 0.5126 0.8191 0.7722 0.055 Uiso 1 1 calc R . . C2 C 0.48342(17) 0.9905(4) 0.8678(2) 0.0482(8) Uani 1 1 d . . . H2 H 0.5264 0.9914 0.9247 0.058 Uiso 1 1 calc R . . C3 C 0.41642(19) 1.0836(4) 0.8538(2) 0.0538(9) Uani 1 1 d . . . H3 H 0.4060 1.1573 0.8998 0.065 Uiso 1 1 calc R . . C4 C 0.36763(18) 1.0493(4) 0.7603(2) 0.0548(9) Uani 1 1 d . . . H4 H 0.3184 1.0958 0.7319 0.066 Uiso 1 1 calc R . . C5 C 0.40428(19) 0.9337(4) 0.7156(2) 0.0514(9) Uani 1 1 d . . . H5 H 0.3842 0.8895 0.6517 0.062 Uiso 1 1 calc R . . Fe1 Fe 0.39580(2) 0.81332(5) 0.83414(3) 0.03032(12) Uani 1 1 d . . . C6 C 0.41067(14) 0.5420(3) 0.85998(19) 0.0345(7) Uani 1 1 d . . . H6 H 0.4493 0.4697 0.8524 0.041 Uiso 1 1 calc R . . C7 C 0.41370(14) 0.6338(3) 0.94409(19) 0.0334(7) Uani 1 1 d . . . H7 H 0.4549 0.6340 1.0030 0.040 Uiso 1 1 calc R . . C8 C 0.34496(14) 0.7260(3) 0.92630(19) 0.0354(7) Uani 1 1 d . . . H8 H 0.3321 0.7981 0.9710 0.043 Uiso 1 1 calc R . . C9 C 0.29906(13) 0.6917(3) 0.83035(19) 0.0342(6) Uani 1 1 d . . . H9 H 0.2499 0.7373 0.7994 0.041 Uiso 1 1 calc R . . C10 C 0.33874(13) 0.5770(3) 0.78740(19) 0.0288(6) Uani 1 1 d . . . C11 C 0.31499(14) 0.5140(3) 0.68919(19) 0.0310(7) Uani 1 1 d . . . H11 H 0.3498 0.4434 0.6718 0.037 Uiso 1 1 calc R . . C12 C 0.24877(14) 0.5454(3) 0.62043(19) 0.0335(7) Uani 1 1 d . . . H12 H 0.2135 0.6132 0.6383 0.040 Uiso 1 1 calc R . . C13 C 0.22527(14) 0.4855(3) 0.52025(19) 0.0317(7) Uani 1 1 d . . . C14 C 0.24930(14) 0.3173(4) 0.4973(2) 0.0396(7) Uani 1 1 d . . . H14 H 0.2797 0.2416 0.5476 0.047 Uiso 1 1 calc R . . C15 C 0.22978(15) 0.2597(4) 0.4036(2) 0.0448(8) Uani 1 1 d . . . H15 H 0.2482 0.1468 0.3907 0.054 Uiso 1 1 calc R . . C16 C 0.18381(14) 0.3629(4) 0.3275(2) 0.0370(7) Uani 1 1 d . . . C17 C 0.16191(15) 0.3073(4) 0.2295(2) 0.0482(8) Uani 1 1 d . . . H17 H 0.1791 0.1938 0.2153 0.058 Uiso 1 1 calc R . . C18 C 0.11794(16) 0.4093(5) 0.1566(2) 0.0528(9) Uani 1 1 d . . . H18 H 0.1045 0.3663 0.0926 0.063 Uiso 1 1 calc R . . C19 C 0.09101(14) 0.5832(4) 0.1745(2) 0.0421(8) Uani 1 1 d . . . C20 C 0.04480(15) 0.6926(5) 0.1008(2) 0.0534(9) Uani 1 1 d . . . H20 H 0.0299 0.6521 0.0362 0.064 Uiso 1 1 calc R . . C21 C 0.02045(16) 0.8602(5) 0.1209(2) 0.0572(10) Uani 1 1 d . . . H21 H -0.0116 0.9320 0.0701 0.069 Uiso 1 1 calc R . . C22 C 0.04236(15) 0.9227(4) 0.2137(2) 0.0506(8) Uani 1 1 d . . . H22 H 0.0263 1.0389 0.2261 0.061 Uiso 1 1 calc R . . C23 C 0.08794(13) 0.8178(4) 0.29012(19) 0.0365(7) Uani 1 1 d . . . C24 C 0.11216(14) 0.8773(4) 0.3870(2) 0.0413(8) Uani 1 1 d . . . H24 H 0.0975 0.9941 0.4006 0.050 Uiso 1 1 calc R . . C25 C 0.15535(14) 0.7735(4) 0.4606(2) 0.0373(7) Uani 1 1 d . . . H25 H 0.1704 0.8195 0.5242 0.045 Uiso 1 1 calc R . . C26 C 0.17904(13) 0.5946(4) 0.44466(19) 0.0292(6) Uani 1 1 d . . . C27 C 0.15775(13) 0.5336(4) 0.34842(19) 0.0313(7) Uani 1 1 d . . . C28 C 0.11207(13) 0.6432(3) 0.2708(2) 0.0332(7) 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 0.050(2) 0.0432(19) 0.055(2) 0.0017(17) 0.0305(19) -0.0091(16) C2 0.053(2) 0.045(2) 0.046(2) 0.0003(16) 0.0162(18) -0.0220(17) C3 0.089(3) 0.0251(18) 0.055(3) -0.0032(16) 0.035(2) -0.0116(18) C4 0.058(2) 0.038(2) 0.066(3) 0.0237(18) 0.020(2) 0.0053(17) C5 0.072(2) 0.050(2) 0.034(2) 0.0032(17) 0.020(2) -0.0208(19) Fe1 0.0332(2) 0.0253(2) 0.0340(2) 0.0028(2) 0.01381(18) 0.0005(2) C6 0.0370(19) 0.0274(16) 0.043(2) 0.0037(14) 0.0193(16) 0.0030(13) C7 0.0320(16) 0.0318(17) 0.0341(18) 0.0085(13) 0.0090(14) 0.0041(12) C8 0.0390(17) 0.0371(18) 0.0354(18) 0.0001(14) 0.0195(15) 0.0012(14) C9 0.0266(14) 0.0347(15) 0.0450(18) 0.0057(16) 0.0172(14) 0.0060(14) C10 0.0249(16) 0.0276(16) 0.0332(17) 0.0040(13) 0.0092(14) -0.0002(12) C11 0.0330(17) 0.0223(15) 0.0407(19) 0.0019(13) 0.0170(15) -0.0008(12) C12 0.0338(17) 0.0302(16) 0.0393(19) 0.0030(14) 0.0165(15) 0.0022(13) C13 0.0283(16) 0.0312(17) 0.0359(18) -0.0009(14) 0.0119(14) -0.0033(13) C14 0.0400(17) 0.0311(16) 0.0440(19) 0.0003(16) 0.0102(14) 0.0001(15) C15 0.0457(19) 0.0321(18) 0.059(2) -0.0073(16) 0.0222(18) 0.0014(14) C16 0.0317(17) 0.0383(18) 0.041(2) -0.0071(15) 0.0135(15) -0.0064(13) C17 0.0435(18) 0.0472(19) 0.057(2) -0.014(2) 0.0220(17) -0.0067(17) C18 0.042(2) 0.073(2) 0.043(2) -0.0140(19) 0.0141(17) -0.0129(18) C19 0.0250(17) 0.065(2) 0.038(2) 0.0013(18) 0.0130(15) -0.0064(16) C20 0.0287(17) 0.099(3) 0.0331(19) 0.001(2) 0.0112(15) -0.009(2) C21 0.0328(19) 0.094(3) 0.046(2) 0.025(2) 0.0155(17) 0.0081(18) C22 0.0330(18) 0.068(2) 0.056(2) 0.021(2) 0.0221(17) 0.0140(16) C23 0.0228(15) 0.0519(18) 0.0385(18) 0.0077(18) 0.0153(14) 0.0025(15) C24 0.0345(18) 0.0397(18) 0.054(2) 0.0021(16) 0.0211(16) 0.0105(14) C25 0.0325(16) 0.0419(18) 0.0398(19) -0.0016(15) 0.0154(15) 0.0034(14) C26 0.0217(15) 0.0338(16) 0.0319(18) 0.0008(14) 0.0093(13) -0.0012(13) C27 0.0230(16) 0.0353(17) 0.0389(19) -0.0024(14) 0.0151(14) -0.0062(13) C28 0.0219(15) 0.0423(19) 0.0384(19) -0.0002(14) 0.0144(14) -0.0046(13)