#------------------------------------------------------------------------------ #$Date: 2016-02-13 19:28:24 +0000 (Sat, 13 Feb 2016) $ #$Revision: 176429 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/66/2006635.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_2006635 loop_ _publ_author_name 'Powell, Madison' 'Bailey, Rosa D.' 'Eagle, Cassandra T.' 'Schimek, George L.' 'Hanks, T. W.' 'Pennington, William T.' _publ_contact_author ; William T. Pennington Department of Chemistry Clemson University Clemson, SC 29634-1905 U.S.A. ; _publ_section_title ; Dicarbonyl(\h^5^-cyclopentadienyl)(pyrrolyl-N)iron(II) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1611 _journal_page_last 1613 _journal_paper_doi 10.1107/S0108270197008718 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[Fe (C5 H5) (C4 H4 N) (C O)2]' _chemical_formula_sum 'C11 H9 Fe N O2' _chemical_formula_weight 243.04 _chemical_name_systematic Dicarbonyl(\h^5^-cyclopentadienyl)(\h^1^-pyrrolyl)iron(II) _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source 'Cromer & Waber (1974)' _audit_creation_method 'manual editing of form.cif' _cell_angle_alpha 90 _cell_angle_beta 95.5(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.309(5) _cell_length_b 11.420(4) _cell_length_c 10.766(4) _cell_measurement_reflns_used 24 _cell_measurement_temperature 148 _cell_measurement_theta_max 8.58 _cell_measurement_theta_min 4.68 _cell_volume 1016.9(11) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1991)' _computing_molecular_graphics SHELXTL-Plus _computing_structure_refinement SHELXTL-Plus _computing_structure_solution SHELXTL-Plus _diffrn_ambient_temperature 148 _diffrn_measurement_device 'Rigaku AFC-7 diffractometer' _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source '18 kW rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2025 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.75 _diffrn_standards_decay_% -3.2 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.46 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_type 'empirical via \y scans (Sheldrick, 1991)' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.51 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.12 _refine_ls_hydrogen_treatment 'H-atom positional parameters and U's refined' _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 172 _refine_ls_number_reflns 1300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_obs .032 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)+0.0005F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0418 _refine_ls_wR_factor_obs .0383 _reflns_number_observed 1300 _reflns_number_total 1786 _reflns_observed_criterion F>4\s(F) _cod_data_source_file bk1322.cif _cod_data_source_block BD0628 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.0005F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F)+0.0005F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1017.0(7) _cod_original_sg_symbol_H-M 'P 21/n' _cod_original_formula_sum 'C11 H9 Fe1 N1 O2' _cod_database_code 2006635 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x+0.5, +y+0.5, -z+0.5' ' -x, -y, -z' ' +x+0.5, -y+0.5, z+0.5' 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 _atom_site_aniso_type_symbol Fe(1) .0210(10) .0250(10) .0190(10) .0030(10) -.0020(10) .0010(10) Fe O(1) .047(2) .034(2) .046(2) .0150(10) -.0050(10) -.0040(10) O O(2) .062(2) .057(2) .029(2) .000(2) .0140(10) .0100(10) O N(1) .024(2) .029(2) .0220(10) .0020(10) -.0030(10) .0020(10) N C(1) .025(2) .031(2) .027(2) -.001(2) -.0030(10) .003(2) C C(2) .033(2) .031(2) .032(2) .003(2) -.003(2) .003(2) C C(3) .034(2) .037(2) .018(2) -.005(2) .004(2) -.001(2) C C(4) .030(2) .045(2) .029(2) -.013(2) .003(2) .002(2) C C(5) .046(2) .032(2) .027(2) -.006(2) -.005(2) .000(2) C C(6) .034(2) .033(2) .030(2) .006(2) -.005(2) -.006(2) C C(7) .036(2) .047(2) .019(2) .010(2) -.003(2) .005(2) C C(8) .038(2) .027(2) .029(2) .001(2) -.007(2) .008(2) C C(9) .033(2) .033(2) .030(2) .016(2) -.008(2) -.003(2) C C(10) .023(2) .043(2) .031(2) .009(2) -.005(2) -.001(2) C C(11) .035(2) .036(2) .024(2) .005(2) -.012(2) -.007(2) C loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags Fe(1) .21160(10) .68950(10) .35330(10) .0220(10) Uani d . O(1) .0589(3) .9130(2) .3986(3) .0430(10) Uani d . O(2) .3160(4) .7494(3) .1104(3) .0490(10) Uani d . N(1) .0149(3) .6160(2) .2732(2) .0250(10) Uani d . C(1) .1146(4) .8249(3) .3790(3) .0280(10) Uani d . C(2) .2736(4) .7271(3) .2052(3) .0320(10) Uani d . C(3) -.1417(5) .6424(3) .2907(3) .0300(10) Uani d . C(4) -.2450(5) .5716(4) .2170(3) .0350(10) Uani d . C(5) -.1490(5) .4973(4) .1521(3) .0350(10) Uani d . C(6) .0092(5) .5266(3) .1894(3) .0330(10) Uani d . C(7) .2391(5) .6391(4) .5430(3) .0340(10) Uani d . C(8) .2458(5) .5396(3) .4682(3) .0320(10) Uani d . C(9) .3747(5) .5522(3) .3929(3) .0330(10) Uani d . C(10) .4498(5) .6606(3) .4246(3) .0330(10) Uani d . C(11) .3669(5) .7155(3) .5157(3) .0320(10) Uani d . H(1) -.167(4) .703(3) .343(3) .022(9) Uiso d . H(2) -.357(5) .572(3) .209(4) .043(12) Uiso d . H(3) -.175(5) .441(4) .093(4) .047(12) Uiso d . H(4) .110(5) .496(3) .162(3) .032(10) Uiso d . H(5) .164(5) .652(4) .601(4) .055(13) Uiso d . H(6) .181(5) .479(4) .465(4) .040(12) Uiso d . H(7) .403(4) .502(3) .333(3) .037(11) Uiso d . H(8) .529(5) .693(3) .391(3) .032(11) Uiso d . H(9) .389(4) .784(3) .553(3) .015(8) Uiso d . loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 2 -1 -2 2 0 -2 2 -2 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 N(1) Fe(1) C(1) 94.00(10) yes N(1) Fe(1) C(2) 90.50(10) yes C(1) Fe(1) C(2) 96.0(2) yes N(1) Fe(1) C(7) 108.50(10) no C(1) Fe(1) C(7) 95.5(2) no C(2) Fe(1) C(7) 157.0(2) no N(1) Fe(1) C(8) 88.30(10) no C(1) Fe(1) C(8) 130.6(2) no C(2) Fe(1) C(8) 133.4(2) no C(7) Fe(1) C(8) 38.6(2) no N(1) Fe(1) C(9) 105.40(10) no C(1) Fe(1) C(9) 156.30(10) no C(2) Fe(1) C(9) 97.3(2) no C(7) Fe(1) C(9) 65.8(2) no C(8) Fe(1) C(9) 39.2(2) no N(1) Fe(1) C(10) 144.80(10) no C(1) Fe(1) C(10) 120.7(2) no C(2) Fe(1) C(10) 91.3(2) no C(7) Fe(1) C(10) 65.7(2) no C(8) Fe(1) C(10) 65.5(2) no C(9) Fe(1) C(10) 39.60(10) no N(1) Fe(1) C(11) 148.10(10) no C(1) Fe(1) C(11) 90.0(2) no C(2) Fe(1) C(11) 120.5(2) no C(7) Fe(1) C(11) 39.6(2) no C(8) Fe(1) C(11) 65.70(10) no C(9) Fe(1) C(11) 66.40(10) no C(10) Fe(1) C(11) 39.2(2) no Fe(1) N(1) C(3) 127.5(2) yes Fe(1) N(1) C(6) 126.0(2) yes C(3) N(1) C(6) 106.5(3) yes Fe(1) C(1) O(1) 176.9(3) yes Fe(1) C(2) O(2) 178.5(3) yes N(1) C(3) C(4) 109.9(3) yes N(1) C(3) H(1) 122(2) no C(4) C(3) H(1) 128(2) no C(3) C(4) C(5) 106.9(4) yes C(3) C(4) H(2) 128(2) no C(5) C(4) H(2) 125(2) no C(4) C(5) C(6) 106.4(3) yes C(4) C(5) H(3) 131(3) no C(6) C(5) H(3) 122(3) no N(1) C(6) C(5) 110.3(3) yes N(1) C(6) H(4) 120(2) no C(5) C(6) H(4) 130(2) no Fe(1) C(7) C(8) 70.8(2) no Fe(1) C(7) C(11) 69.4(2) no C(8) C(7) C(11) 107.9(3) yes Fe(1) C(7) H(5) 126(3) no C(8) C(7) H(5) 125(3) no C(11) C(7) H(5) 127(3) no Fe(1) C(8) C(7) 70.6(2) no Fe(1) C(8) C(9) 69.4(2) no C(7) C(8) C(9) 108.8(3) yes Fe(1) C(8) H(6) 125(2) no C(7) C(8) H(6) 127(3) no C(9) C(8) H(6) 124(3) no Fe(1) C(9) C(8) 71.4(2) no Fe(1) C(9) C(10) 69.8(2) no C(8) C(9) C(10) 107.0(3) yes Fe(1) C(9) H(7) 123(2) no C(8) C(9) H(7) 127(2) no C(10) C(9) H(7) 126(2) no Fe(1) C(10) C(9) 70.6(2) no Fe(1) C(10) C(11) 70.9(2) no C(9) C(10) C(11) 109.0(4) yes Fe(1) C(10) H(8) 121(2) no C(9) C(10) H(8) 128(2) no C(11) C(10) H(8) 123(2) no Fe(1) C(11) C(7) 70.9(2) no Fe(1) C(11) C(10) 69.9(2) no C(7) C(11) C(10) 107.2(3) yes Fe(1) C(11) H(9) 126(2) no C(7) C(11) H(9) 125(2) no C(10) C(11) H(9) 128(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe(1) N(1) 1.962(3) yes Fe(1) C(1) 1.777(4) yes Fe(1) C(2) 1.774(4) yes Fe(1) C(7) 2.113(4) yes Fe(1) C(8) 2.116(4) yes Fe(1) C(9) 2.090(4) yes Fe(1) C(10) 2.079(4) yes Fe(1) C(11) 2.093(3) yes O(1) C(1) 1.136(4) yes O(2) C(2) 1.141(5) yes N(1) C(3) 1.367(5) yes N(1) C(6) 1.361(5) yes C(3) C(4) 1.375(5) yes C(3) H(1) .92(3) no C(4) C(5) 1.396(6) yes C(4) H(2) .92(4) no C(5) C(6) 1.379(6) yes C(5) H(3) .92(4) no C(6) H(4) .98(4) no C(7) C(8) 1.398(5) yes C(7) C(11) 1.426(6) yes C(7) H(5) .94(5) no C(8) C(9) 1.410(6) yes C(8) H(6) .87(4) no C(9) C(10) 1.413(5) yes C(9) H(7) .91(4) no C(10) C(11) 1.400(6) yes C(10) H(8) .87(4) no C(11) H(9) .89(3) no