#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/02/2200268.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_2200268 loop_ _publ_author_name 'Damgaard Poulsen, Rasmus' 'Hazell, Alan' _publ_section_title ; Bis(2,2'-bipyridine-N,N')dicyanoiron(III) nitrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m186 _journal_page_last m187 _journal_paper_doi 10.1107/S1600536801005918 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Fe (C10 H8 N2)2 (C N)2] (N O3)' _chemical_formula_moiety 'C22 H16 Fe1 N6 1+, N1 O3 1-' _chemical_formula_sum 'C22 H16 Fe N7 O3' _chemical_formula_weight 482.28 _chemical_name_systematic ; bis(2,2'-bipyridine-N,N')-dicyano-iron(III) nitrate ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 4 _cell_length_a 10.7902(6) _cell_length_b 11.7031(6) _cell_length_c 16.1857(9) _cell_measurement_reflns_used 8263 _cell_measurement_temperature 120 _cell_measurement_theta_max 29.8 _cell_measurement_theta_min 2.1 _cell_volume 2043.91(19) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL' _computing_publication_material KRYSTAL _computing_structure_refinement 'modified ORFLS (Busing et al., 1962) and KRYSTAL' _computing_structure_solution 'SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995)' _diffrn_ambient_temperature 120 _diffrn_measured_fraction_theta_full .98 _diffrn_measured_fraction_theta_max .98 _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .058 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 19837 _diffrn_reflns_reduction_process 19837 _diffrn_reflns_theta_full 29.8 _diffrn_reflns_theta_max 29.8 _diffrn_reflns_theta_min 2.1 _exptl_absorpt_coefficient_mu .780 _exptl_absorpt_correction_T_max .836 _exptl_absorpt_correction_T_min .718 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(XPREP; Siemens, 1995)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 988.0 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .34 _refine_diff_density_max .80(8) _refine_diff_density_min -.64(8) _refine_ls_abs_structure_details '1815 Friedel pairs (84%)' _refine_ls_abs_structure_Rogers 1.02(3) _refine_ls_extinction_coef 24(8) _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 300 _refine_ls_number_reflns 4302 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt .031 _refine_ls_shift/su_max .0011 _refine_ls_shift/su_mean .00015 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .038 _reflns_number_gt 4302 _reflns_number_total 5807 _reflns_threshold_expression I>3\s(I) _[local]_cod_data_source_file bt6032.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'C22 H16 Fe1 N7 O3' _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 33 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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 2043.90(10) _cod_database_code 2200268 _cod_database_fobs_code 2200268 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z 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 Fe .01870(10) .01710(10) .01480(10) .0010(2) .0002(2) .00000(10) O1 .0510(10) .0480(10) .0340(10) -.0190(10) .0000(10) .0000(10) O2 .090(2) .0220(10) .0310(10) -.0030(10) -.010(2) -.0010(10) O3 .0650(10) .0380(10) .0280(10) .0250(10) -.0050(10) -.0030(10) N1 .0250(10) .0180(10) .0170(10) -.0010(10) -.0010(10) -.0020(10) N2 .0210(10) .0180(10) .0170(10) .0000(10) -.0010(10) .0020(10) N3 .0190(10) .0170(10) .0180(10) .0020(10) -.0020(10) .0020(10) N4 .0180(10) .0170(10) .0180(10) .0030(10) -.0020(10) .0010(10) N5 .0260(10) .0270(10) .0200(10) .0030(10) -.0010(10) -.0030(10) N6 .0320(10) .0290(10) .0210(10) -.0050(10) .0020(10) -.0040(10) N7 .0350(10) .0260(10) .0220(10) .0010(10) .0120(10) .0000(10) C1 .0310(10) .0260(10) .0230(10) .0060(10) .0030(10) -.0010(10) C2 .0400(10) .0260(10) .0200(10) .0040(10) .0070(10) -.0030(10) C3 .0400(10) .0260(10) .0160(10) -.0050(10) .0020(10) -.0010(10) C4 .0280(10) .0190(10) .0210(10) -.0020(10) -.0010(10) .0010(10) C5 .0230(10) .0150(10) .0210(10) -.0040(10) .0000(10) .0010(10) C6 .0200(10) .0160(10) .0190(10) -.0050(10) .0000(10) .0000(10) C7 .0230(10) .0220(10) .0230(10) -.0030(10) -.0030(10) .0030(10) C8 .0190(10) .0220(10) .0320(10) .0030(10) .0000(10) .0040(10) C9 .0250(10) .0250(10) .0250(10) .0030(10) .0030(10) -.0020(10) C10 .0260(10) .0250(10) .0210(10) .0000(10) .0010(10) .0010(10) C11 .0230(10) .0240(10) .0220(10) .0030(10) -.0010(10) .0030(10) C12 .0270(10) .0210(10) .028(2) -.0020(10) .0020(10) .0050(10) C13 .0240(10) .0200(10) .0290(10) -.0040(10) -.0050(10) .0010(10) C14 .0240(10) .0210(10) .0210(10) .0020(10) -.0040(10) -.0010(10) C15 .0180(10) .0190(10) .0210(10) .0040(10) -.0010(10) .0010(10) C16 .0170(10) .0170(10) .0190(10) .0020(10) -.0020(10) -.0010(10) C17 .0260(10) .0200(10) .0190(10) .0010(10) -.0020(10) -.0020(10) C18 .0270(10) .0270(10) .0160(10) .0030(10) .0040(10) -.0010(10) C19 .0220(10) .0240(10) .0210(10) .0020(10) .0030(10) .0060(10) C20 .0210(10) .0190(10) .0220(10) .0000(10) .0000(10) .0000(10) C21 .0240(10) .0180(10) .0130(10) -.0040(10) .0010(10) -.0030(10) C22 .0200(10) .0230(10) .0170(10) .0040(10) -.0010(10) -.0010(10) 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 Fe .49538(3) .22630(3) .62687(2) .01680(10) Uani O1 .5776(2) -.1398(2) .42010(10) .0440(10) Uani O2 .4937(2) -.29400(10) .37580(10) .0480(10) Uani O3 .4399(2) -.1339(2) .32240(10) .0440(10) Uani N1 .4888(2) .2189(2) .74790(10) .0200(10) Uani N2 .6404(2) .1270(2) .64540(10) .0190(10) Uani N3 .3930(2) .0895(2) .60650(10) .0180(10) Uani N4 .5049(2) .2250(2) .50620(10) .0180(10) Uani N5 .2773(2) .3905(2) .60180(10) .0240(10) Uani N6 .6502(2) .4433(2) .65090(10) .0270(10) Uani N7 .5029(2) -.1892(2) .37230(10) .0280(10) Uani C1 .4020(2) .2661(2) .7959(2) .0270(10) Uani C2 .4070(3) .2606(2) .8808(2) .0290(10) Uani C3 .5053(3) .2051(2) .91790(10) .0270(10) Uani C4 .5949(2) .1555(2) .8687(2) .0230(10) Uani C5 .5848(2) .1635(2) .7837(2) .0200(10) Uani C6 .6728(2) .1131(2) .72540(10) .0180(10) Uani C7 .7779(2) .0543(2) .7481(2) .0230(10) Uani C8 .8487(2) .0046(2) .6867(2) .0240(10) Uani C9 .8142(2) .0150(2) .6060(2) .0250(10) Uani C10 .7092(2) .0782(2) .5865(2) .0240(10) Uani C11 .3366(2) .0256(2) .6645(2) .0230(10) Uani C12 .2670(2) -.0687(2) .6441(2) .0250(10) Uani C13 .2556(2) -.0994(2) .5621(2) .0240(10) Uani C14 .3151(2) -.0353(2) .5021(2) .0220(10) Uani C15 .3824(2) .0594(2) .52580(10) .0200(10) Uani C16 .4445(2) .1375(2) .46870(10) .0180(10) Uani C17 .4414(2) .1270(2) .3837(2) .0210(10) Uani C18 .4979(3) .2090(2) .33600(10) .0230(10) Uani C19 .5576(2) .2980(2) .3745(2) .0220(10) Uani C20 .5602(2) .3038(2) .4587(2) .0210(10) Uani C21 .3578(2) .3289(2) .61290(10) .0190(10) Uani C22 .5937(2) .3617(2) .64170(10) .0200(10) Uani H1 .3345 .3047 .7706 .032 Uiso H2 .3437 .2946 .9134 .034 Uiso H3 .5112 .2012 .9764 .033 Uiso H4 .6628 .1163 .8929 .027 Uiso H7 .8011 .0480 .8045 .027 Uiso H8 .9216 -.0368 .7007 .029 Uiso H9 .8614 -.0206 .5636 .030 Uiso H10 .6859 .0869 .5303 .028 Uiso H11 .3451 .0461 .7210 .028 Uiso H12 .2271 -.1122 .6860 .030 Uiso H13 .2074 -.1641 .5470 .029 Uiso H14 .3096 -.0563 .4455 .026 Uiso H17 .4007 .0640 .3585 .026 Uiso H18 .4957 .2042 .2774 .028 Uiso H19 .5971 .3555 .3425 .027 Uiso H20 .6025 .3655 .4844 .025 Uiso 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 C21 Fe C22 85.80(10) yes N4 Fe C22 95.89(9) yes N1 Fe C22 86.07(9) yes N2 Fe C22 91.66(9) yes N3 Fe C22 177.47(9) yes N4 Fe C21 85.86(9) yes N1 Fe C21 96.74(9) yes N2 Fe C21 176.95(9) yes N3 Fe C21 93.15(9) yes N1 Fe N4 176.87(8) yes N2 Fe N4 96.05(8) yes N3 Fe N4 81.74(8) yes N1 Fe N2 81.43(8) yes N1 Fe N3 96.34(8) yes N2 Fe N3 89.49(8) yes Fe N1 C1 126.0(2) no Fe N1 C5 114.9(2) no Fe N2 C10 125.8(2) no Fe N2 C6 114.9(2) no Fe N3 C11 126.0(2) no Fe N3 C15 114.7(2) no Fe N4 C20 126.2(2) no Fe N4 C16 115.4(2) no Fe C21 N5 177.6(2) no Fe C22 N6 178.7(2) no C1 N1 C5 119.1(2) no C6 N2 C10 119.2(2) no C11 N3 C15 119.2(2) no C16 N4 C20 118.3(2) no O2 N7 O3 120.4(3) no O1 N7 O2 118.7(2) no O1 N7 O3 120.8(2) no N1 C1 C2 122.3(2) no C1 C2 C3 119.1(2) no C2 C3 C4 118.9(2) no C3 C4 C5 119.4(2) no N1 C5 C4 121.3(2) no N1 C5 C6 114.5(2) no C4 C5 C6 124.3(2) no N2 C6 C7 121.9(2) no N2 C6 C5 113.7(2) no C5 C6 C7 124.4(2) no C6 C7 C8 118.4(2) no C7 C8 C9 120.0(2) no C8 C9 C10 119.2(2) no N2 C10 C9 121.3(2) no N3 C11 C12 121.7(2) no C11 C12 C13 119.3(2) no C12 C13 C14 119.4(2) no C13 C14 C15 119.0(2) no N3 C15 C14 121.3(2) no N3 C15 C16 114.0(2) no C14 C15 C16 124.6(2) no N4 C16 C17 121.6(2) no N4 C16 C15 114.1(2) no C15 C16 C17 124.3(2) no C16 C17 C18 119.1(2) no C17 C18 C19 118.9(2) no C18 C19 C20 120.0(2) no N4 C20 C19 122.0(2) no N1 C1 H1 118.9 no C2 C1 H1 118.9 no C1 C2 H2 120.4 no C3 C2 H2 120.4 no C4 C3 H3 120.6 no C2 C3 H3 120.5 no C3 C4 H4 120.3 no C5 C4 H4 120.3 no C6 C7 H7 120.8 no C8 C7 H7 120.8 no C9 C8 H8 120.0 no C7 C8 H8 120.0 no C8 C9 H9 120.4 no C10 C9 H9 120.4 no N2 C10 H10 119.3 no C9 C10 H10 119.4 no N3 C11 H11 119.2 no C12 C11 H11 119.1 no C11 C12 H12 120.4 no C13 C12 H12 120.3 no C12 C13 H13 120.3 no C14 C13 H13 120.3 no C15 C14 H14 120.5 no C13 C14 H14 120.5 no C18 C17 H17 120.4 no C16 C17 H17 120.5 no C19 C18 H18 120.6 no C17 C18 H18 120.5 no C20 C19 H19 120.0 no C18 C19 H19 120.0 no N4 C20 H20 119.0 no C19 C20 H20 119.0 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe C21 1.923(2) yes Fe C22 1.922(3) yes Fe N1 1.962(2) yes Fe N2 1.972(2) yes Fe N3 1.973(2) yes Fe N4 1.955(2) yes O1 N7 1.258(3) no O2 N7 1.232(3) no O3 N7 1.238(3) no N1 C1 1.337(3) no N1 C5 1.352(3) no N2 C10 1.336(3) no N2 C6 1.352(3) no N3 C11 1.345(3) no N3 C15 1.359(3) no N4 C20 1.342(3) no N4 C16 1.358(3) no N5 C21 1.143(3) no N6 C22 1.143(3) no C1 C2 1.375(4) no C2 C3 1.382(4) no C3 C4 1.381(4) no C4 C5 1.383(3) no C5 C6 1.463(3) no C6 C7 1.376(3) no C7 C8 1.382(4) no C8 C9 1.364(4) no C9 C10 1.389(4) no C11 C12 1.375(3) no C12 C13 1.380(4) no C13 C14 1.385(4) no C14 C15 1.379(3) no C15 C16 1.462(3) no C16 C17 1.382(3) no C17 C18 1.374(3) no C18 C19 1.374(3) no C19 C20 1.365(4) no C1 H1 .95 no C2 H2 .95 no C3 H3 .95 no C4 H4 .95 no C7 H7 .95 no C8 H8 .95 no C9 H9 .95 no C10 H10 .95 no C11 H11 .95 no C12 H12 .95 no C13 H13 .95 no C14 H14 .95 no C17 H17 .95 no C18 H18 .95 no C19 H19 .95 no C20 H20 .95 no 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 _geom_torsion_publ_flag N1 C5 C6 N2 -2.4(3) no N3 C15 C16 N4 1.6(3) no