#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012407.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_2012407 loop_ _publ_author_name 'McMullen, Sarah E.' 'Hagen, Karl S.' _publ_section_title ; trans-Bis(benzoato-O)tetrakis(methanol-O)iron(II): ligand bulk is not structure-determining ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m48 _journal_page_last m49 _journal_paper_doi 10.1107/S010827010101873X _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Fe (C7 H5 O2)2 (C H4 O)4]' _chemical_formula_moiety 'C18 H26 Fe O8' _chemical_formula_sum 'C18 H26 Fe O8' _chemical_formula_weight 426.24 _chemical_name_systematic ; trans-Bis(benzoato-O)tetrakis(methanol-O)iron(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 101.450(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.8630(10) _cell_length_b 12.065(2) _cell_length_c 8.6050(10) _cell_measurement_reflns_used 9801 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.9 _cell_measurement_theta_min 2.7 _cell_volume 1003.6(2) _computing_cell_refinement 'SMART and SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker SMART-APEX CCD on D8 diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .022 _diffrn_reflns_av_sigmaI/netI .015 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11390 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.11 _diffrn_standards_decay_% <2 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .792 _exptl_absorpt_correction_T_max .89 _exptl_absorpt_correction_T_min .79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Blessing, 1995; Sheldrick, 2001)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 448 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .15 _refine_diff_density_max .58 _refine_diff_density_min -.21 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 2922 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all .029 _refine_ls_R_factor_gt .027 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.2157P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .077 _refine_ls_wR_factor_ref .078 _reflns_number_gt 2731 _reflns_number_total 2922 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bk1620.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _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 1527 2010-12-29 10:47:43Z saulius 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_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 1003.5(3) _cod_database_code 2012407 _cod_database_fobs_code 2012407 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' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Fe1 .5000 .0000 .5000 .01320(7) Uani d S 1 . . Fe O1 .67049(7) .04085(6) .40014(9) .01874(15) Uani d . 1 . . O O2 .60217(8) .19438(6) .26267(9) .02054(15) Uani d . 1 . . O O3 .39268(8) .14316(6) .39495(9) .01811(15) Uani d . 1 . . O H1 .4489(18) .1732(14) .349(2) .034(4) Uiso d . 1 . . H O4 .59133(8) .09086(6) .70638(8) .02078(16) Uani d . 1 . . O H2 .5979(17) .1587(15) .7091(19) .031(4) Uiso d . 1 . . H C1 .68961(10) .11862(8) .30922(11) .01524(17) Uani d . 1 . . C C2 .82386(10) .11968(8) .25182(11) .01584(17) Uani d . 1 . . C C3 .92079(11) .03605(10) .29936(13) .0228(2) Uani d . 1 . . C H3 .9015(19) -.0227(14) .366(2) .030(4) Uiso d . 1 . . H C4 1.04542(12) .03587(12) .24770(16) .0305(3) Uani d . 1 . . C H4 1.113(2) -.0209(16) .279(2) .041(5) Uiso d . 1 . . H C5 1.07343(12) .11922(11) .14676(15) .0296(2) Uani d . 1 . . C H5 1.1585(18) .1194(15) .111(2) .038(4) Uiso d . 1 . . H C6 .97772(11) .20244(10) .09859(13) .0254(2) Uani d . 1 . . C H6 .9944(16) .2597(17) .032(2) .037(5) Uiso d . 1 . . H C7 .85335(10) .20335(9) .15155(12) .02016(19) Uani d . 1 . . C H7 .7864(16) .2600(14) .1187(18) .029(4) Uiso d . 1 . . H C8 .31935(11) .22182(9) .47091(14) .0230(2) Uani d . 1 . . C H8B .3826(18) .2680(14) .5435(19) .033(4) Uiso d . 1 . . H H8A .2596(17) .2673(15) .3905(19) .034(4) Uiso d . 1 . . H H8C .2617(18) .1824(15) .533(2) .039(4) Uiso d . 1 . . H C9 .59115(19) .05311(10) .86254(14) .0345(3) Uani d . 1 . . C H9B .525(3) .083(3) .898(4) .102(10) Uiso d . 1 . . H H9A .656(3) .081(2) .933(3) .074(7) Uiso d . 1 . . H H9C .586(2) -.0266(18) .864(2) .040(5) Uiso d . 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 .01604(11) .00979(11) .01447(11) .00015(6) .00472(7) .00021(5) O1 .0199(3) .0169(3) .0207(3) .0017(3) .0073(3) .0052(3) O2 .0214(3) .0155(3) .0263(4) .0029(3) .0086(3) .0057(3) O3 .0208(3) .0136(3) .0215(3) .0028(2) .0080(3) .0016(2) O4 .0326(4) .0135(3) .0164(3) -.0041(3) .0054(3) -.0015(2) C1 .0175(4) .0134(4) .0149(4) -.0016(3) .0036(3) -.0009(3) C2 .0159(4) .0166(4) .0149(4) -.0020(3) .0029(3) .0002(3) C3 .0206(5) .0231(5) .0259(5) .0024(4) .0072(4) .0082(4) C4 .0208(5) .0343(6) .0385(6) .0078(5) .0108(4) .0142(5) C5 .0190(5) .0377(6) .0342(6) .0007(4) .0101(4) .0104(5) C6 .0212(5) .0298(6) .0260(5) -.0035(4) .0072(4) .0097(4) C7 .0185(4) .0201(5) .0219(4) -.0013(3) .0038(3) .0050(3) C8 .0240(5) .0178(5) .0284(5) .0051(4) .0082(4) -.0021(4) C9 .0677(9) .0194(5) .0161(5) -.0048(5) .0077(5) -.0009(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe .3463 .8444 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 Fe1 O1 . 3_656 180.00(2) O1 Fe1 O4 . . 88.84(3) O1 Fe1 O4 3_656 . 91.16(3) O1 Fe1 O4 . 3_656 91.16(3) O1 Fe1 O4 3_656 3_656 88.84(3) O4 Fe1 O4 . 3_656 180.0 O1 Fe1 O3 . 3_656 89.61(3) O1 Fe1 O3 3_656 3_656 90.39(3) O4 Fe1 O3 . 3_656 88.35(3) O4 Fe1 O3 3_656 3_656 91.65(3) O1 Fe1 O3 . . 90.39(3) O1 Fe1 O3 3_656 . 89.61(3) O4 Fe1 O3 . . 91.65(3) O4 Fe1 O3 3_656 . 88.35(3) O3 Fe1 O3 3_656 . 180.0 C1 O1 Fe1 . . 131.44(6) C8 O3 Fe1 . . 126.78(6) C8 O3 H1 . . 112.0(10) Fe1 O3 H1 . . 104.0(10) C9 O4 Fe1 . . 123.01(7) C9 O4 H2 . . 108.0(10) Fe1 O4 H2 . . 124.0(10) O1 C1 O2 . . 123.91(9) O1 C1 C2 . . 117.44(8) O2 C1 C2 . . 118.65(8) C3 C2 C7 . . 119.34(9) C3 C2 C1 . . 119.68(9) C7 C2 C1 . . 120.99(9) C4 C3 C2 . . 120.40(10) C4 C3 H3 . . 119.0(10) C2 C3 H3 . . 121.0(10) C3 C4 C5 . . 119.80(10) C3 C4 H4 . . 121.0(10) C5 C4 H4 . . 119.0(10) C6 C5 C4 . . 120.20(10) C6 C5 H5 . . 120.0(10) C4 C5 H5 . . 120.0(10) C5 C6 C7 . . 120.10(10) C5 C6 H6 . . 122.0(10) C7 C6 H6 . . 118.0(10) C6 C7 C2 . . 120.20(10) C6 C7 H7 . . 120.8(9) C2 C7 H7 . . 119.0(9) O3 C8 H8B . . 111.0(10) O3 C8 H8A . . 110.0(10) H8B C8 H8A . . 111.0(10) O3 C8 H8C . . 109.0(10) H8B C8 H8C . . 107.0(10) H8A C8 H8C . . 109.0(10) O4 C9 H9B . . 110(2) O4 C9 H9A . . 114(2) H9B C9 H9A . . 96(2) O4 C9 H9C . . 110.0(10) H9B C9 H9C . . 112(2) H9A C9 H9C . . 115(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 O1 . 2.0933(7) ? Fe1 O1 3_656 2.0933(7) ? Fe1 O4 . 2.1288(8) ? Fe1 O4 3_656 2.1288(8) ? Fe1 O3 3_656 2.1310(7) ? Fe1 O3 . 2.1310(7) ? O1 C1 . 1.2600(10) ? O2 C1 . 1.2660(10) ? O3 C8 . 1.4280(10) ? O3 H1 . .82(2) ? O4 C9 . 1.4190(10) ? O4 H2 . .82(2) ? C1 C2 . 1.5020(10) ? C2 C3 . 1.3940(10) ? C2 C7 . 1.3960(10) ? C3 C4 . 1.388(2) ? C3 H3 . .95(2) ? C4 C5 . 1.392(2) ? C4 H4 . .95(2) ? C5 C6 . 1.384(2) ? C5 H5 . .95(2) ? C6 C7 . 1.391(2) ? C6 H6 . .93(2) ? C7 H7 . .95(2) ? C8 H8B . .97(2) ? C8 H8A . .98(2) ? C8 H8C . .98(2) ? C9 H9B . .86(3) ? C9 H9A . .86(3) ? C9 H9C . .96(2) ? 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 O3 H1 O2 . .82(2) 1.83(2) 2.6230(10) 161(2) O4 H2 O2 4_566 .82(2) 1.83(2) 2.6340(10) 166(2) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion O4 Fe1 O1 C1 . -94.37(9) O4 Fe1 O1 C1 3_656 85.63(9) O3 Fe1 O1 C1 3_656 177.27(9) O3 Fe1 O1 C1 . -2.73(9) O1 Fe1 O3 C8 . -133.21(8) O1 Fe1 O3 C8 3_656 46.79(8) O4 Fe1 O3 C8 . -44.36(8) O4 Fe1 O3 C8 3_656 135.64(8) O1 Fe1 O4 C9 . -138.40(10) O1 Fe1 O4 C9 3_656 41.60(10) O3 Fe1 O4 C9 3_656 -48.80(10) O3 Fe1 O4 C9 . 131.20(10) Fe1 O1 C1 O2 . 2.6(2) Fe1 O1 C1 C2 . -176.55(6) O1 C1 C2 C3 . .30(10) O2 C1 C2 C3 . -178.92(9) O1 C1 C2 C7 . -179.62(9) O2 C1 C2 C7 . 1.20(10) C7 C2 C3 C4 . .0(2) C1 C2 C3 C4 . -179.90(10) C2 C3 C4 C5 . -.5(2) C3 C4 C5 C6 . .3(2) C4 C5 C6 C7 . .3(2) C5 C6 C7 C2 . -.8(2) C3 C2 C7 C6 . .6(2) C1 C2 C7 C6 . -179.47(9)