#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2205071.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2205071 _space_group_IT_number 9 _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _[local]_cod_cif_authors_sg_H-M 'C c' loop_ _publ_author_name 'Chan, Wing Yan' 'Lough, Alan J.' 'Manners, Ian' _publ_section_title ; Methylchlorosila[1]ferrocenophane ; _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m375 _journal_page_last m376 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Fe (C11 H11 Cl Si)]' _chemical_formula_moiety 'C11 H11 Cl Fe Si' _chemical_formula_sum 'C11 H11 Cl Fe Si' _chemical_formula_weight 262.59 _chemical_name_systematic ; Methylchlorosila[1]ferrocenophane ; _symmetry_cell_setting Monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 95.295(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.4146(9) _cell_length_b 10.2135(8) _cell_length_c 7.8627(6) _cell_measurement_reflns_used 11776 _cell_measurement_temperature 150.0(10) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.6 _cell_volume 1072.67(14) _computing_cell_refinement 'DENZO--SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 2003)' _computing_data_reduction DENZO--SMN _computing_molecular_graphics 'SHELXTL and PLATON (Spek, 2004)' _computing_publication_material 'SHELXTL ' _computing_structure_refinement 'SHELXTL ' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _diffrn_ambient_temperature 150.0(10) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4024 _diffrn_reflns_theta_full 27.52 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_min 3.05 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.720 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing 1995)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.476 _refine_diff_density_min -0.502 _refine_ls_abs_structure_details 'Flack (1983), 845 Friedel pairs' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2078 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0389 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0418P)^2^+2.256P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.0976 _reflns_number_gt 1859 _reflns_number_total 2078 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hb6140.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Fe1 0.64830(4) 0.22608(6) 0.65546(5) 0.0285(2) Uani d . 1 Fe Cl1 0.92521(10) 0.06896(14) 0.59839(18) 0.0473(4) Uani d . 1 Cl Si1 0.82248(9) 0.21381(13) 0.52090(16) 0.0316(3) Uani d . 1 Si C1 0.6999(4) 0.1325(4) 0.4558(6) 0.0306(10) Uani d . 1 C C2 0.6605(3) 0.0403(5) 0.5714(6) 0.0335(10) Uani d . 1 C H2A 0.7002 -0.0305 0.6340 0.040 Uiso calc R 1 H C3 0.5571(4) 0.0668(5) 0.5864(6) 0.0347(11) Uani d . 1 C H3A 0.5128 0.0194 0.6614 0.042 Uiso calc R 1 H C4 0.5298(4) 0.1738(6) 0.4797(6) 0.0415(13) Uani d . 1 C H4A 0.4625 0.2166 0.4677 0.050 Uiso calc R 1 H C5 0.6152(4) 0.2168(5) 0.3998(6) 0.0364(12) Uani d . 1 C H5A 0.6168 0.2920 0.3186 0.044 Uiso calc R 1 H C6 0.7848(4) 0.3022(5) 0.7134(6) 0.0337(10) Uani d . 1 C C7 0.7549(4) 0.2259(5) 0.8556(6) 0.0298(11) Uani d . 1 C H7A 0.7904 0.1467 0.9053 0.036 Uiso calc R 1 H C8 0.6650(4) 0.2804(5) 0.9105(6) 0.0332(11) Uani d . 1 C H8A 0.6262 0.2445 1.0026 0.040 Uiso calc R 1 H C9 0.6379(4) 0.3911(5) 0.8065(6) 0.0373(11) Uani d . 1 C H9A 0.5770 0.4467 0.8129 0.045 Uiso calc R 1 H C10 0.7112(4) 0.4050(5) 0.6856(6) 0.0370(11) Uani d . 1 C H10A 0.7107 0.4741 0.5953 0.044 Uiso calc R 1 H C11 0.8705(4) 0.3170(6) 0.3533(7) 0.0459(13) Uani d . 1 C H11A 0.9377 0.2875 0.3318 0.069 Uiso calc R 1 H H11B 0.8735 0.4084 0.3913 0.069 Uiso calc R 1 H H11C 0.8257 0.3099 0.2480 0.069 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0272(3) 0.0308(3) 0.0267(3) 0.0016(3) -0.0015(2) -0.0030(3) Cl1 0.0372(7) 0.0523(8) 0.0515(8) 0.0108(6) 0.0004(6) 0.0069(7) Si1 0.0268(6) 0.0379(7) 0.0303(7) -0.0003(6) 0.0033(5) 0.0035(5) C1 0.035(2) 0.029(2) 0.027(2) 0.000(2) 0.0022(18) -0.0052(19) C2 0.035(2) 0.037(3) 0.029(2) 0.000(2) 0.0016(19) -0.008(2) C3 0.029(2) 0.043(3) 0.032(3) -0.007(2) 0.004(2) -0.009(2) C4 0.029(2) 0.061(4) 0.034(3) 0.004(3) -0.004(2) -0.016(3) C5 0.034(3) 0.044(3) 0.029(2) 0.001(2) -0.007(2) -0.002(2) C6 0.034(2) 0.038(3) 0.028(2) -0.006(2) -0.0053(19) 0.0031(19) C7 0.033(3) 0.031(3) 0.024(2) -0.001(2) -0.0037(18) -0.0005(18) C8 0.034(3) 0.038(3) 0.028(2) 0.001(2) 0.002(2) -0.006(2) C9 0.039(3) 0.037(3) 0.033(3) 0.008(2) -0.007(2) -0.009(2) C10 0.045(3) 0.028(2) 0.035(2) -0.005(2) -0.007(2) -0.0009(19) C11 0.044(3) 0.053(3) 0.042(3) -0.003(3) 0.010(2) 0.009(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe1 C6 2.002(5) ? Fe1 C1 2.014(4) ? Fe1 C10 2.018(5) ? Fe1 C5 2.021(5) ? Fe1 C2 2.021(5) ? Fe1 C7 2.026(5) ? Fe1 C8 2.072(5) ? Fe1 C9 2.073(5) ? Fe1 C4 2.078(5) ? Fe1 C3 2.078(5) ? Fe1 Si1 2.6554(13) ? Cl1 Si1 2.0746(18) y Si1 C11 1.849(5) y Si1 C1 1.871(5) y Si1 C6 1.872(5) y C1 C2 1.442(7) ? C1 C5 1.461(7) ? C2 C3 1.429(7) ? C2 H2A 1.0000 ? C3 C4 1.406(8) ? C3 H3A 1.0000 ? C4 C5 1.426(8) ? C4 H4A 1.0000 ? C5 H5A 1.0000 ? C6 C10 1.444(7) ? C6 C7 1.450(7) ? C7 C8 1.430(7) ? C7 H7A 1.0000 ? C8 C9 1.422(7) ? C8 H8A 1.0000 ? C9 C10 1.436(7) ? C9 H9A 1.0000 ? C10 H10A 1.0000 ? C11 H11A 0.9800 ? C11 H11B 0.9800 ? C11 H11C 0.9800 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C6 Fe1 C1 89.36(19) ? C6 Fe1 C10 42.1(2) ? C1 Fe1 C10 110.6(2) ? C6 Fe1 C5 110.9(2) ? C1 Fe1 C5 42.5(2) ? C10 Fe1 C5 102.1(2) ? C6 Fe1 C2 109.8(2) ? C1 Fe1 C2 41.89(18) ? C10 Fe1 C2 147.5(2) ? C5 Fe1 C2 69.4(2) ? C6 Fe1 C7 42.18(19) ? C1 Fe1 C7 109.7(2) ? C10 Fe1 C7 69.6(2) ? C5 Fe1 C7 147.9(2) ? C2 Fe1 C7 100.41(19) ? C6 Fe1 C8 70.19(19) ? C1 Fe1 C8 150.1(2) ? C10 Fe1 C8 68.7(2) ? C5 Fe1 C8 165.8(2) ? C2 Fe1 C8 124.3(2) ? C7 Fe1 C8 40.8(2) ? C6 Fe1 C9 70.3(2) ? C1 Fe1 C9 151.39(19) ? C10 Fe1 C9 41.1(2) ? C5 Fe1 C9 126.0(2) ? C2 Fe1 C9 164.18(19) ? C7 Fe1 C9 68.64(19) ? C8 Fe1 C9 40.1(2) ? C6 Fe1 C4 151.4(2) ? C1 Fe1 C4 69.9(2) ? C10 Fe1 C4 126.6(2) ? C5 Fe1 C4 40.7(2) ? C2 Fe1 C4 67.7(2) ? C7 Fe1 C4 163.4(2) ? C8 Fe1 C4 136.07(19) ? C9 Fe1 C4 120.1(2) ? C6 Fe1 C3 150.2(2) ? C1 Fe1 C3 70.19(19) ? C10 Fe1 C3 165.9(2) ? C5 Fe1 C3 68.5(2) ? C2 Fe1 C3 40.77(19) ? C7 Fe1 C3 124.0(2) ? C8 Fe1 C3 118.1(2) ? C9 Fe1 C3 135.8(2) ? C4 Fe1 C3 39.6(2) ? C6 Fe1 Si1 44.71(14) ? C1 Fe1 Si1 44.67(14) ? C10 Fe1 Si1 73.49(15) ? C5 Fe1 Si1 73.86(15) ? C2 Fe1 Si1 74.01(13) ? C7 Fe1 Si1 74.07(14) ? C8 Fe1 Si1 112.18(14) ? C9 Fe1 Si1 111.99(15) ? C4 Fe1 Si1 111.73(14) ? C3 Fe1 Si1 112.18(13) ? C11 Si1 C1 114.4(2) y C11 Si1 C6 116.0(3) y C1 Si1 C6 98.0(2) y C11 Si1 Cl1 110.5(2) y C1 Si1 Cl1 107.90(16) y C6 Si1 Cl1 109.18(16) y C11 Si1 Fe1 129.3(2) ? C1 Si1 Fe1 49.17(13) ? C6 Si1 Fe1 48.82(15) ? Cl1 Si1 Fe1 120.11(7) ? C2 C1 C5 104.8(4) ? C2 C1 Si1 118.8(3) ? C5 C1 Si1 117.4(4) ? C2 C1 Fe1 69.3(2) ? C5 C1 Fe1 69.0(3) ? Si1 C1 Fe1 86.16(18) ? C3 C2 C1 110.1(4) ? C3 C2 Fe1 71.7(3) ? C1 C2 Fe1 68.8(3) ? C3 C2 H2A 125.0 ? C1 C2 H2A 125.0 ? Fe1 C2 H2A 125.0 ? C4 C3 C2 107.4(4) ? C4 C3 Fe1 70.2(3) ? C2 C3 Fe1 67.5(3) ? C4 C3 H3A 126.3 ? C2 C3 H3A 126.3 ? Fe1 C3 H3A 126.3 ? C3 C4 C5 109.1(4) ? C3 C4 Fe1 70.2(3) ? C5 C4 Fe1 67.5(3) ? C3 C4 H4A 125.4 ? C5 C4 H4A 125.4 ? Fe1 C4 H4A 125.4 ? C4 C5 C1 108.6(5) ? C4 C5 Fe1 71.8(3) ? C1 C5 Fe1 68.5(3) ? C4 C5 H5A 125.7 ? C1 C5 H5A 125.7 ? Fe1 C5 H5A 125.7 ? C10 C6 C7 105.9(4) ? C10 C6 Si1 117.4(3) ? C7 C6 Si1 118.6(4) ? C10 C6 Fe1 69.5(3) ? C7 C6 Fe1 69.8(3) ? Si1 C6 Fe1 86.5(2) ? C8 C7 C6 108.9(4) ? C8 C7 Fe1 71.3(3) ? C6 C7 Fe1 68.0(3) ? C8 C7 H7A 125.5 ? C6 C7 H7A 125.5 ? Fe1 C7 H7A 125.5 ? C9 C8 C7 108.3(4) ? C9 C8 Fe1 70.0(3) ? C7 C8 Fe1 67.8(3) ? C9 C8 H8A 125.8 ? C7 C8 H8A 125.8 ? Fe1 C8 H8A 125.8 ? C8 C9 C10 107.8(4) ? C8 C9 Fe1 69.9(3) ? C10 C9 Fe1 67.4(3) ? C8 C9 H9A 126.1 ? C10 C9 H9A 126.1 ? Fe1 C9 H9A 126.1 ? C9 C10 C6 109.1(4) ? C9 C10 Fe1 71.5(3) ? C6 C10 Fe1 68.4(3) ? C9 C10 H10A 125.4 ? C6 C10 H10A 125.4 ? Fe1 C10 H10A 125.4 ? Si1 C11 H11A 109.5 ? Si1 C11 H11B 109.5 ? H11A C11 H11B 109.5 ? Si1 C11 H11C 109.5 ? H11A C11 H11C 109.5 ? H11B C11 H11C 109.5 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C9 H9A Cl1 3_455 1.00 2.81 3.641(5) 141 _cod_database_code 2205071