#------------------------------------------------------------------------------ #$Date: 2014-10-04 09:13:39 +0300 (Sat, 04 Oct 2014) $ #$Revision: 124550 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/20/4512067.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_4512067 loop_ _publ_author_name 'Wu, Xue-Ru' 'Yang, X\"u' 'Wei, Rong-Jia' 'Li, Jia' 'Zheng, Lan-Sun' 'Tao, Jun' _publ_section_title ; Solvent-Mediated Isomerization of FeIIComplexes from a 3D 65·8 Framework to a 2D 44Rhombus-Grid Network ; _journal_issue 10 _journal_name_full 'Crystal Growth & Design' _journal_page_first 4891 _journal_paper_doi 10.1021/cg5011506 _journal_volume 14 _journal_year 2014 _chemical_formula_sum 'C34 H29 Fe N6 O2.5 S2' _chemical_formula_weight 681.60 _chemical_name_systematic ; ? ; _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/c 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 99.639(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.4071(7) _cell_length_b 15.8882(12) _cell_length_c 13.1892(7) _cell_measurement_reflns_used 2904 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.0178 _cell_measurement_theta_min 3.3398 _cell_volume 2356.6(3) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _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 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10154 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.35 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_correction_T_min 0.9784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 0.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 706 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _platon_squeeze_details ; ; _refine_diff_density_max 0.999 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 194 _refine_ls_number_reflns 4632 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0683 _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^)+(0.1392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2051 _refine_ls_wR_factor_ref 0.2247 _reflns_number_gt 3271 _reflns_number_total 4632 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cg5011506_si_002.cif _[local]_cod_data_source_block complex_2 _[local]_cod_cif_authors_sg_H-M P2/c _[local]_cod_chemical_formula_sum_orig 'C34 H29 Fe N6 O2.50 S2' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/COD-crude-data--automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius ; _cod_database_code 4512067 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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 Fe1 Fe 0.5000 0.60767(3) 0.7500 0.0329(2) Uani 1 2 d S S1 S 0.81429(11) 0.62546(11) 0.54553(11) 0.1011(6) Uani 1 1 d . N1 N 0.6461(2) 0.61203(15) 0.88960(19) 0.0373(6) Uani 1 1 d . N2 N 0.5000 1.4650(2) 0.7500 0.0391(8) Uani 1 2 d S N3 N 0.5000 0.7485(3) 0.7500 0.0516(10) Uani 1 2 d S N4 N 0.6300(2) 0.60505(16) 0.6557(2) 0.0435(7) Uani 1 1 d . C1 C 0.7604(3) 0.6151(2) 0.8857(3) 0.0597(11) Uani 1 1 d . H1A H 0.7825 0.6169 0.8210 0.072 Uiso 1 1 calc R C2 C 0.8499(3) 0.6158(3) 0.9694(3) 0.0663(13) Uani 1 1 d . H2B H 0.9289 0.6179 0.9602 0.080 Uiso 1 1 calc R C3 C 0.8225(3) 0.6133(2) 1.0673(3) 0.0457(8) Uani 1 1 d . C4 C 0.7018(3) 0.6110(2) 1.0722(3) 0.0567(10) Uani 1 1 d . H4A H 0.6770 0.6098 1.1358 0.068 Uiso 1 1 calc R C5 C 0.6190(3) 0.6103(2) 0.9839(3) 0.0534(10) Uani 1 1 d . H5A H 0.5390 0.6085 0.9902 0.064 Uiso 1 1 calc R C6 C 0.9129(3) 0.6129(2) 1.1609(3) 0.0567(8) Uani 1 1 d . C7 C 1.0211(6) 0.6540(6) 1.1627(5) 0.0567(8) Uani 0.50 1 d P H7A H 1.0373 0.6806 1.1012 0.068 Uiso 0.50 1 d PR C7' C 1.0208(6) 0.5724(6) 1.1635(5) 0.060(2) Uani 0.50 1 d P H7'A H 1.0327 0.5401 1.1046 0.072 Uiso 0.50 1 d PR C8 C 0.8940(6) 0.6544(5) 1.2493(5) 0.0567(8) Uani 0.50 1 d P H8A H 0.8207 0.6844 1.2477 0.068 Uiso 0.50 1 d PR C8' C 0.8948(6) 0.5721(6) 1.2494(5) 0.060(2) Uani 0.50 1 d P H8'A H 0.8213 0.5423 1.2475 0.072 Uiso 0.50 1 d PR C9 C 0.4275(3) 1.4207(2) 0.6801(2) 0.0485(8) Uani 1 1 d . H9A H 0.3757 1.4499 0.6304 0.058 Uiso 1 1 calc R C10 C 0.4250(3) 1.3341(2) 0.6772(3) 0.0522(9) Uani 1 1 d . H10A H 0.3727 1.3067 0.6261 0.063 Uiso 1 1 calc R C11 C 0.5000 1.2874(3) 0.7500 0.0528(12) Uani 1 2 d S C12 C 0.5000 1.1949(3) 0.7500 0.0616(14) Uani 1 2 d S C13 C 0.4772(6) 1.1502(3) 0.6608(4) 0.1153(15) Uani 1 1 d . H13A H 0.4592 1.1789 0.5987 0.138 Uiso 1 1 calc R C14 C 0.4801(6) 1.0630(3) 0.6601(4) 0.1153(15) Uani 1 1 d . H14A H 0.4684 1.0343 0.5977 0.138 Uiso 1 1 calc R C15 C 0.5000 1.0189(4) 0.7500 0.1153(15) Uani 1 2 d S C16 C 0.5000 0.9267(4) 0.7500 0.0696(15) Uani 1 2 d S C17 C 0.5569(8) 0.8800(3) 0.6871(6) 0.137(3) Uani 1 1 d . H17A H 0.5976 0.9069 0.6409 0.164 Uiso 1 1 calc R C18 C 0.5555(6) 0.7935(3) 0.6908(5) 0.125(2) Uani 1 1 d . H18A H 0.5978 0.7648 0.6472 0.150 Uiso 1 1 calc R C19 C 0.7066(3) 0.6134(2) 0.6107(3) 0.0469(8) 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 Fe1 0.0322(4) 0.0348(4) 0.0290(4) 0.000 -0.0032(2) 0.000 S1 0.0561(7) 0.1656(16) 0.0877(10) 0.0155(8) 0.0301(7) -0.0060(7) N1 0.0345(13) 0.0445(16) 0.0297(13) 0.0012(10) -0.0041(10) -0.0010(10) N2 0.0391(19) 0.037(2) 0.0408(19) 0.000 0.0043(15) 0.000 N3 0.056(2) 0.042(2) 0.053(2) 0.000 -0.0021(19) 0.000 N4 0.0355(14) 0.0533(17) 0.0391(14) 0.0010(12) -0.0012(11) 0.0004(11) C1 0.0407(19) 0.105(3) 0.0314(16) 0.0042(17) 0.0009(14) -0.0105(17) C2 0.0328(17) 0.129(4) 0.0341(17) 0.0024(19) -0.0047(13) -0.0132(18) C3 0.0377(17) 0.059(2) 0.0360(16) 0.0005(14) -0.0060(13) -0.0005(13) C4 0.0384(18) 0.098(3) 0.0315(16) -0.0039(16) -0.0026(13) 0.0007(16) C5 0.0313(16) 0.090(3) 0.0359(17) -0.0032(16) -0.0045(13) -0.0001(15) C6 0.0393(15) 0.091(3) 0.0357(14) 0.0012(14) -0.0057(11) 0.0018(14) C7 0.0393(15) 0.091(3) 0.0357(14) 0.0012(14) -0.0057(11) 0.0018(14) C7' 0.041(4) 0.103(6) 0.033(3) -0.012(4) -0.005(3) 0.017(4) C8 0.0393(15) 0.091(3) 0.0357(14) 0.0012(14) -0.0057(11) 0.0018(14) C8' 0.036(4) 0.099(6) 0.040(4) 0.016(4) -0.011(3) -0.016(4) C9 0.052(2) 0.0408(18) 0.050(2) 0.0005(16) 0.0003(15) 0.0000(15) C10 0.056(2) 0.0428(19) 0.054(2) -0.0051(16) -0.0027(16) -0.0032(15) C11 0.057(3) 0.039(3) 0.064(3) 0.000 0.011(2) 0.000 C12 0.080(4) 0.038(3) 0.066(3) 0.000 0.012(3) 0.000 C13 0.209(5) 0.0493(18) 0.079(2) -0.0061(17) -0.003(3) -0.004(2) C14 0.209(5) 0.0493(18) 0.079(2) -0.0061(17) -0.003(3) -0.004(2) C15 0.209(5) 0.0493(18) 0.079(2) -0.0061(17) -0.003(3) -0.004(2) C16 0.085(4) 0.041(3) 0.079(4) 0.000 0.003(3) 0.000 C17 0.222(9) 0.050(3) 0.166(7) 0.006(3) 0.114(7) -0.012(3) C18 0.185(6) 0.043(3) 0.175(6) -0.001(3) 0.114(5) 0.006(3) C19 0.0387(18) 0.061(2) 0.0365(17) 0.0036(14) -0.0067(14) 0.0028(14) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 '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 N4 Fe1 N4 177.72(14) . 2_656 N4 Fe1 N3 91.14(7) . . N4 Fe1 N3 91.14(7) 2_656 . N4 Fe1 N2 88.86(7) . 1_545 N4 Fe1 N2 88.86(7) 2_656 1_545 N3 Fe1 N2 180.000(1) . 1_545 N4 Fe1 N1 89.18(10) . . N4 Fe1 N1 90.89(9) 2_656 . N3 Fe1 N1 88.25(6) . . N2 Fe1 N1 91.75(6) 1_545 . N4 Fe1 N1 90.89(9) . 2_656 N4 Fe1 N1 89.18(10) 2_656 2_656 N3 Fe1 N1 88.25(6) . 2_656 N2 Fe1 N1 91.75(6) 1_545 2_656 N1 Fe1 N1 176.50(12) . 2_656 C1 N1 C5 115.1(3) . . C1 N1 Fe1 124.6(2) . . C5 N1 Fe1 120.2(2) . . C9 N2 C9 116.2(4) . 2_656 C9 N2 Fe1 121.9(2) . 1_565 C9 N2 Fe1 121.9(2) 2_656 1_565 C18 N3 C18 113.2(5) . 2_656 C18 N3 Fe1 123.4(3) . . C18 N3 Fe1 123.4(3) 2_656 . C19 N4 Fe1 170.8(2) . . N1 C1 C2 125.3(3) . . C1 C2 C3 119.9(3) . . C2 C3 C4 115.2(3) . . C2 C3 C6 123.3(3) . . C4 C3 C6 121.5(3) . . C5 C4 C3 120.5(3) . . N1 C5 C4 123.9(3) . . C8' C6 C7' 91.1(5) . . C8' C6 C8 56.4(5) . . C7' C6 C8 117.5(5) . . C8' C6 C7 117.6(5) . . C7' C6 C7 55.7(5) . . C8 C6 C7 91.4(5) . . C8' C6 C3 121.9(4) . . C7' C6 C3 121.3(4) . . C8 C6 C3 121.2(4) . . C7 C6 C3 120.5(4) . . C7' C7 C8 90.0(6) . 2_757 C7' C7 C6 61.8(5) . . C8 C7 C6 120.7(6) 2_757 . C7' C7 C8' 46.3(4) . 2_757 C8 C7 C8' 43.7(4) 2_757 2_757 C6 C7 C8' 92.5(5) . 2_757 C7' C7 C8 89.7(5) . . C8 C7 C8 89.6(5) 2_757 . C6 C7 C8 44.2(3) . . C8' C7 C8 89.6(4) 2_757 . C7 C7' C8' 90.5(6) . 2_757 C7 C7' C6 62.5(5) . . C8' C7' C6 121.3(6) 2_757 . C7 C7' C8 46.8(4) . 2_757 C8' C7' C8 43.7(5) 2_757 2_757 C6 C7' C8 93.4(5) . 2_757 C7 C7' C8' 90.6(5) . . C8' C7' C8' 89.8(5) 2_757 . C6 C7' C8' 44.4(3) . . C8 C7' C8' 90.1(4) 2_757 . C8' C8 C7 89.5(6) . 2_757 C8' C8 C6 61.5(5) . . C7 C8 C6 121.2(6) 2_757 . C8' C8 C7' 46.3(4) . 2_757 C7 C8 C7' 43.2(5) 2_757 2_757 C6 C8 C7' 92.7(5) . 2_757 C8' C8 C7 89.5(5) . . C7 C8 C7 90.4(5) 2_757 . C6 C8 C7 44.4(3) . . C7' C8 C7 89.9(4) 2_757 . C8 C8' C7' 90.0(6) . 2_757 C8 C8' C6 62.1(5) . . C7' C8' C6 121.6(6) 2_757 . C8 C8' C7 46.8(4) . 2_757 C7' C8' C7 43.2(5) 2_757 2_757 C6 C8' C7 93.6(5) . 2_757 C8 C8' C7' 90.2(5) . . C7' C8' C7' 90.2(5) 2_757 . C6 C8' C7' 44.5(3) . . C7 C8' C7' 90.4(4) 2_757 . N2 C9 C10 123.7(3) . . C9 C10 C11 120.5(3) . . C10 C11 C10 115.4(4) 2_656 . C10 C11 C12 122.3(2) 2_656 . C10 C11 C12 122.3(2) . . C13 C12 C13 117.0(6) 2_656 . C13 C12 C11 121.5(3) 2_656 . C13 C12 C11 121.5(3) . . C12 C13 C14 121.8(5) . . C15 C14 C13 120.5(5) . . C14 C15 C14 118.2(7) 2_656 . C14 C15 C16 120.9(3) 2_656 . C14 C15 C16 120.9(3) . . C17 C16 C17 113.7(6) 2_656 . C17 C16 C15 123.1(3) 2_656 . C17 C16 C15 123.1(3) . . C16 C17 C18 121.0(5) . . N3 C18 C17 125.5(5) . . N4 C19 S1 179.3(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 N4 2.089(3) . Fe1 N4 2.089(3) 2_656 Fe1 N3 2.237(4) . Fe1 N2 2.266(4) 1_545 Fe1 N1 2.268(2) . Fe1 N1 2.268(2) 2_656 S1 C19 1.624(4) . N1 C1 1.315(4) . N1 C5 1.331(4) . N2 C9 1.332(4) . N2 C9 1.332(4) 2_656 N2 Fe1 2.266(4) 1_565 N3 C18 1.298(5) . N3 C18 1.298(5) 2_656 N4 C19 1.144(4) . C1 C2 1.373(5) . C2 C3 1.379(5) . C3 C4 1.389(5) . C3 C6 1.470(5) . C4 C5 1.372(5) . C6 C8' 1.380(8) . C6 C7' 1.384(7) . C6 C8 1.388(8) . C6 C7 1.393(8) . C7 C7' 1.297(12) . C7 C8 1.381(9) 2_757 C7 C8' 1.895(11) 2_757 C7 C8 1.990(9) . C7' C8' 1.370(9) 2_757 C7' C8 1.895(11) 2_757 C7' C8' 1.973(9) . C8 C8' 1.309(12) . C8 C7 1.381(9) 2_757 C8 C7' 1.895(11) 2_757 C8' C7' 1.370(9) 2_757 C8' C7 1.895(11) 2_757 C9 C10 1.376(5) . C10 C11 1.389(4) . C11 C10 1.389(4) 2_656 C11 C12 1.469(7) . C12 C13 1.362(6) 2_656 C12 C13 1.362(6) . C13 C14 1.385(7) . C14 C15 1.363(6) . C15 C14 1.363(6) 2_656 C15 C16 1.466(9) . C16 C17 1.356(6) 2_656 C16 C17 1.356(6) . C17 C18 1.376(7) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.005 979.4 15.8