#------------------------------------------------------------------------------ #$Date: 2016-03-25 13:41:51 +0200 (Fri, 25 Mar 2016) $ #$Revision: 179858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/54/7015454.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_7015454 loop_ _publ_author_name 'Child, Chloe R.' 'Kealey, Steven' 'Jones, Harriet' 'Miller, Philip W.' 'White, Andrew J. P.' 'Gee, Anthony D.' 'Long, Nicholas J.' _publ_section_title ; Binding and photodissociation of CO in iron(ii) complexes for application in positron emission tomography (PET) radiolabelling. ; _journal_issue 23 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 6210 _journal_page_last 6215 _journal_paper_doi 10.1039/c0dt01614d _journal_volume 40 _journal_year 2011 _chemical_formula_moiety 'C14 H24 Fe I2 N2' _chemical_formula_sum 'C14 H24 Fe I2 N2' _chemical_formula_weight 530.00 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 98.020(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.0697(4) _cell_length_b 7.0217(2) _cell_length_c 20.4319(8) _cell_measurement_reflns_used 2880 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 71.2134 _cell_measurement_theta_min 3.7895 _cell_volume 1856.73(11) _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 8.2556 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 4163 _diffrn_reflns_theta_full 71.31 _diffrn_reflns_theta_max 71.31 _diffrn_reflns_theta_min 4.37 _exptl_absorpt_coefficient_mu 32.535 _exptl_absorpt_correction_T_max 0.115 _exptl_absorpt_correction_T_min 0.017 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blocks _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.932 _refine_diff_density_min -2.293 _refine_diff_density_rms 0.293 _refine_ls_extinction_coef 0.00063(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 88 _refine_ls_number_reflns 1789 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0623 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+2.5751P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1536 _refine_ls_wR_factor_ref 0.1584 _reflns_number_gt 1604 _reflns_number_total 1789 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c0dt01614d.txt _cod_data_source_block (c-C6H11-DAB)FeI2 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_original_sg_symbol_H-M I2/a _cod_database_code 7015454 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 0.7500 0.69732(17) 0.5000 0.0271(4) Uani 1 2 d S . . I I 0.60815(3) 0.88815(6) 0.42903(2) 0.0420(3) Uani 1 1 d . . . N1 N 0.6978(4) 0.4661(7) 0.5517(2) 0.0260(9) Uani 1 1 d . . . C1 C 0.7206(6) 0.3077(9) 0.5282(3) 0.0377(15) Uani 1 1 d . . . H1A H 0.7004 0.1915 0.5466 0.045 Uiso 1 1 calc R . . C2 C 0.6411(4) 0.4663(9) 0.6097(3) 0.0269(11) Uani 1 1 d . . . H2A H 0.6068 0.3398 0.6124 0.032 Uiso 1 1 calc R . . C3 C 0.7173(5) 0.4963(11) 0.6720(3) 0.0358(14) Uani 1 1 d . . . H3A H 0.7548 0.6177 0.6687 0.043 Uiso 1 1 calc R . . H3B H 0.7685 0.3917 0.6768 0.043 Uiso 1 1 calc R . . C4 C 0.6597(5) 0.5015(13) 0.7331(3) 0.0446(18) Uani 1 1 d . . . H4A H 0.6274 0.3760 0.7386 0.053 Uiso 1 1 calc R . . H4B H 0.7096 0.5272 0.7732 0.053 Uiso 1 1 calc R . . C5 C 0.5763(6) 0.6561(13) 0.7254(3) 0.0456(16) Uani 1 1 d . . . H5A H 0.5377 0.6525 0.7638 0.055 Uiso 1 1 calc R . . H5B H 0.6091 0.7828 0.7243 0.055 Uiso 1 1 calc R . . C6 C 0.5024(5) 0.6264(10) 0.6627(4) 0.0385(15) Uani 1 1 d . . . H6A H 0.4512 0.7311 0.6575 0.046 Uiso 1 1 calc R . . H6B H 0.4646 0.5053 0.6658 0.046 Uiso 1 1 calc R . . C7 C 0.5590(5) 0.6203(9) 0.6021(3) 0.0327(14) Uani 1 1 d . . . H7A H 0.5088 0.5949 0.5621 0.039 Uiso 1 1 calc R . . H7B H 0.5917 0.7454 0.5964 0.039 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 0.0284(7) 0.0284(7) 0.0251(6) 0.000 0.0063(5) 0.000 I 0.0399(4) 0.0496(4) 0.0348(4) 0.00342(15) -0.0009(2) 0.00843(15) N1 0.021(2) 0.036(2) 0.021(2) -0.0019(18) 0.0010(17) -0.0001(18) C1 0.054(4) 0.027(3) 0.036(3) 0.004(2) 0.019(3) -0.003(3) C2 0.022(2) 0.036(3) 0.024(3) 0.004(2) 0.008(2) -0.002(2) C3 0.028(3) 0.058(4) 0.021(3) 0.007(2) 0.004(2) 0.001(3) C4 0.037(3) 0.079(5) 0.020(3) 0.009(3) 0.010(3) 0.001(3) C5 0.046(4) 0.064(4) 0.030(3) 0.000(3) 0.014(3) 0.001(3) C6 0.028(3) 0.052(4) 0.037(4) 0.001(3) 0.011(3) 0.007(3) C7 0.026(3) 0.049(4) 0.024(3) 0.004(2) 0.004(2) 0.008(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 Fe N1 78.9(3) . 2_656 ? N1 Fe I 112.28(13) . 2_656 ? N1 Fe I 115.31(13) 2_656 2_656 ? N1 Fe I 115.31(13) . . ? N1 Fe I 112.28(13) 2_656 . ? I Fe I 117.05(5) 2_656 . ? C1 N1 C2 118.4(5) . . ? C1 N1 Fe 112.3(4) . . ? C2 N1 Fe 129.4(4) . . ? N1 C1 C1 118.3(4) . 2_656 ? N1 C2 C7 110.1(5) . . ? N1 C2 C3 109.2(4) . . ? C7 C2 C3 111.0(5) . . ? C2 C3 C4 110.2(5) . . ? C5 C4 C3 110.7(6) . . ? C6 C5 C4 110.6(6) . . ? C5 C6 C7 111.6(6) . . ? C2 C7 C6 110.6(5) . . ? 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 N1 2.102(5) . ? Fe N1 2.102(5) 2_656 ? Fe I 2.5662(7) 2_656 ? Fe I 2.5662(7) . ? N1 C1 1.263(9) . ? N1 C2 1.481(7) . ? C1 C1 1.473(12) 2_656 ? C2 C7 1.516(8) . ? C2 C3 1.517(8) . ? C3 C4 1.546(8) . ? C4 C5 1.531(11) . ? C5 C6 1.507(10) . ? C6 C7 1.529(8) . ?