#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000343.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_5000343 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C22 H18 Fe2 N8 O13' _chemical_formula_moiety 'C22 H18 Fe2 N8 O13' _chemical_formula_weight 714.125 _cell_length_a 8.759(2) _cell_length_b 18.811(6) _cell_length_c 16.618(5) _cell_angle_alpha 90 _cell_angle_beta 104.750(15) _cell_angle_gamma 90 _cell_volume 2647.7(22) _cell_formula_units_Z 4 _cell_measurement_reflns_used 60 _cell_measurement_theta_min 9.65 _cell_measurement_theta_max 15.15 _cell_measurement_temperature 107 _exptl_crystal_colour red _exptl_crystal_description prism _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.1808 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.945 _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 107 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5921 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 3.01745 _diffrn_reflns_theta_max 25.0521 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 4 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.6 _diffrn_standards_interval_count 300 _reflns_number_total 4689 _reflns_number_gt 3121 _reflns_threshold_expression F^2^>2.0\s(F^2^) _atom_sites_solution_primary direct _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 3121 _refine_ls_number_parameters 407 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.00000013(6) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0476 _refine_ls_goodness_of_fit_ref 0.9517 _refine_ls_shift/su_max 0.0036 _refine_diff_density_max 0.31 _refine_diff_density_min -0.39 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_disorder_group _atom_site_disorder_assembly Fe1 Fe 0.12186(10) 0.11859(4) 0.32507(5) 0.0127(3) Uani 1 0 . Fe2 Fe 0.36620(10) 0.10299(4) 0.19031(5) 0.0129(3) Uani 1 0 . O3 O 0.2168(4) 0.1000(2) 0.2446(2) 0.0158(14) Uani 1 0 . N4 N 0.0056(5) 0.1349(2) 0.4212(3) 0.0132(16) Uani 1 0 . C5 C 0.0249(7) 0.1934(3) 0.4691(4) 0.0176(19) Uani 1 0 . C6 C -0.0525(7) 0.2034(3) 0.5309(3) 0.0159(19) Uani 1 0 . C7 C -0.1572(7) 0.1517(3) 0.5421(3) 0.018(2) Uani 1 0 . C8 C -0.1785(6) 0.0910(3) 0.4933(3) 0.0143(18) Uani 1 0 . C9 C -0.0939(6) 0.0839(3) 0.4338(3) 0.0133(18) Uani 1 0 . C10 C -0.1040(7) 0.0195(3) 0.3808(3) 0.0145(19) Uani 1 0 . C11 C -0.2043(7) -0.0364(3) 0.3861(4) 0.018(2) Uani 1 0 . C12 C -0.2009(7) -0.0970(3) 0.3397(4) 0.0180(19) Uani 1 0 . C13 C -0.0993(7) -0.0997(3) 0.2878(3) 0.0150(18) Uani 1 0 . C14 C -0.0040(7) -0.0417(3) 0.2831(4) 0.0164(19) Uani 1 0 . N15 N -0.0057(5) 0.0174(2) 0.3287(3) 0.0135(16) Uani 1 0 . C16 C 0.1069(7) -0.0466(3) 0.2263(4) 0.019(2) Uani 1 0 . C17 C 0.2804(7) -0.0539(3) 0.2761(4) 0.017(2) Uani 1 0 . N18 N 0.4463(6) -0.0071(2) 0.1879(3) 0.0140(16) Uani 1 0 . C19 C 0.3912(7) -0.0646(3) 0.2212(4) 0.0162(19) Uani 1 0 . C20 C 0.4370(7) -0.1330(3) 0.2068(4) 0.0176(19) Uani 1 0 . C21 C 0.5433(7) -0.1441(3) 0.1589(4) 0.020(2) Uani 1 0 . C22 C 0.6031(7) -0.0851(3) 0.1268(4) 0.019(2) Uani 1 0 . C23 C 0.5520(7) -0.0173(3) 0.1418(3) 0.0152(19) Uani 1 0 . C24 C 0.6063(6) 0.0466(3) 0.1060(3) 0.0132(18) Uani 1 0 . C25 C 0.7223(7) 0.0457(3) 0.0624(4) 0.022(2) Uani 1 0 . C26 C 0.7556(7) 0.1069(3) 0.0239(4) 0.025(2) Uani 1 0 . C27 C 0.6754(7) 0.1682(3) 0.0313(4) 0.022(2) Uani 1 0 . C28 C 0.5662(7) 0.1675(3) 0.0786(4) 0.020(2) Uani 1 0 . N29 N 0.5320(6) 0.1078(2) 0.1153(3) 0.0162(16) Uani 1 0 . O30 O 0.3180(5) 0.1773(2) 0.4045(3) 0.0193(14) Uani 1 0 . N31 N 0.3694(6) 0.1249(3) 0.4524(3) 0.0188(18) Uani 1 0 . O32 O 0.2996(5) 0.0660(2) 0.4289(2) 0.0188(14) Uani 1 0 . O33 O 0.4742(5) 0.1308(2) 0.5165(3) 0.0274(16) Uani 1 0 . O34 O 0.0624(5) 0.2285(2) 0.2923(2) 0.0193(14) Uani 1 0 . N35 N -0.0754(6) 0.2138(3) 0.2468(3) 0.0189(18) Uani 1 0 . O36 O -0.1102(5) 0.1478(2) 0.2408(2) 0.0196(14) Uani 1 0 . O37 O -0.1681(5) 0.2598(2) 0.2111(3) 0.0240(15) Uani 1 0 . O38 O 0.5628(5) 0.1057(2) 0.3014(2) 0.0175(13) Uani 1 0 . N39 N 0.5677(6) 0.1736(3) 0.3006(3) 0.0151(16) Uani 1 0 . O40 O 0.4665(5) 0.20299(19) 0.2400(2) 0.0160(14) Uani 1 0 . O41 O 0.6610(5) 0.2084(2) 0.3528(2) 0.0200(14) Uani 1 0 . O42 O 0.2068(5) 0.0631(2) 0.0729(2) 0.0179(14) Uani 1 0 . N43 N 0.1738(6) 0.1255(3) 0.0441(3) 0.0171(17) Uani 1 0 . O44 O 0.2322(5) 0.1759(2) 0.0936(2) 0.0184(14) Uani 1 0 . O45 O 0.0966(5) 0.1361(2) -0.0274(3) 0.0234(15) Uani 1 0 . H1 H 0.095 0.2294 0.4601 0.0305 Uiso 1 0 . H2 H -0.0342 0.2448 0.565 0.0285 Uiso 1 0 . H3 H -0.2149 0.1578 0.583 0.0307 Uiso 1 0 . H4 H -0.2505 0.0552 0.5003 0.027 Uiso 1 0 . H5 H -0.2743 -0.0331 0.4213 0.0304 Uiso 1 0 . H6 H -0.2674 -0.1361 0.343 0.0309 Uiso 1 0 . H7 H -0.0949 -0.1412 0.2558 0.0276 Uiso 1 0 . H8 H 0.0788 -0.0867 0.1911 0.0315 Uiso 1 0 . H9 H 0.0962 -0.0046 0.1933 0.0315 Uiso 1 0 . H10 H 0.3106 -0.012 0.308 0.03 Uiso 1 0 . H11 H 0.2891 -0.0936 0.3123 0.03 Uiso 1 0 . H12 H 0.3954 -0.1725 0.2299 0.0306 Uiso 1 0 . H13 H 0.5747 -0.1908 0.1482 0.0324 Uiso 1 0 . H14 H 0.6783 -0.0908 0.0949 0.0318 Uiso 1 0 . H15 H 0.7785 0.0031 0.0589 0.0351 Uiso 1 0 . H16 H 0.8327 0.1064 -0.0072 0.0378 Uiso 1 0 . H17 H 0.6951 0.2107 0.0046 0.0345 Uiso 1 0 . H18 H 0.5131 0.2104 0.0852 0.0322 Uiso 1 0 .