#------------------------------------------------------------------------------ #$Date: 2016-02-15 22:06:40 +0000 (Mon, 15 Feb 2016) $ #$Revision: 176451 $ #$URL: svn://www.crystallography.net/cod/cif/5/00/03/5000336.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_5000336 loop_ _publ_author_name 'Seddon, Elisa J.' 'Yoo, Jae' 'Folting, Kirsten' 'Huffman, John C.' 'Hendrickson, David N.' 'Christou, George' _publ_section_title ; Dinuclear and hexanuclear iron(III) carboxylate clusters with a bis(bipyridine) ligand: supramolecular aggregation of [Fe2O2] units to give a [Fe6O6] ladder structure † ; _journal_issue 20 _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _journal_page_first 3640 _journal_paper_doi 10.1039/b004925p _journal_year 2000 _chemical_formula_sum 'C22 H20 B2 F8 N4' _chemical_formula_weight 514.037 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _cell_angle_alpha 95.73(10) _cell_angle_beta 105.82(11) _cell_angle_gamma 90.06(5) _cell_formula_units_Z 1 _cell_length_a 9.341(7) _cell_length_b 11.460(14) _cell_length_c 5.383(6) _cell_measurement_reflns_used 10 _cell_measurement_temperature 173. _cell_measurement_theta_max 10.47 _cell_measurement_theta_min 9.73 _cell_volume 551.4(11) _computing_cell_refinement 'XTEL, local package' _computing_data_collection 'NPS, local program' _computing_data_reduction 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' _computing_structure_refinement 'XTEL, local package' _computing_structure_solution MULTAN78 _diffrn_ambient_temperature 173. _diffrn_measured_fraction_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 4434 _diffrn_reflns_theta_full 0 _diffrn_reflns_theta_max 24.9983 _diffrn_reflns_theta_min 3.57475 _diffrn_standards_decay_% 19.8 _diffrn_standards_interval_count 500 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 0.1394 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 262 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .25 _refine_diff_density_max 0.38 _refine_diff_density_min -0.47 _refine_ls_abs_structure_details none _refine_ls_extinction_coef -0.000011(3) _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_extinction_method Zachariasen _refine_ls_goodness_of_fit_ref 1.6417 _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 866 _refine_ls_R_factor_gt 0.0707 _refine_ls_shift/su_max 0.078 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0719 _reflns_number_gt 1016 _reflns_number_total 1943 _reflns_threshold_expression F^2^>2.33\s(F^2^) _cod_data_source_file b004925p.txt _cod_data_source_block MSC98127 _cod_database_code 5000336 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 B1 B 0.2303(7) 0.6797(7) 0.1845(13) 0.050(3) Uani 1 0 . F2 F 0.1107(3) 0.6051(3) 0.1450(6) 0.0603(15) Uani 1 0 . F3 F 0.3441(3) 0.6254(3) 0.1020(6) 0.0541(13) Uani 1 0 . F4 F 0.2841(4) 0.7220(4) 0.4443(6) 0.0663(15) Uani 1 0 . F5 F 0.1867(4) 0.7775(3) 0.0426(7) 0.0671(15) Uani 1 0 . C6 C 0.9465(7) 1.0295(5) 0.3974(12) 0.056(3) Uani 1 0 . C7 C 0.8115(6) 0.9527(5) 0.2605(11) 0.044(2) Uani 1 0 . C8 C 0.6765(7) 0.9644(6) 0.3216(12) 0.053(3) Uani 1 0 . C9 C 0.5574(7) 0.8922(6) 0.1860(12) 0.054(3) Uani 1 0 . C10 C 0.5740(6) 0.8094(5) -0.0104(11) 0.044(2) Uani 1 0 . C11 C 0.7120(6) 0.8031(5) -0.0552(10) 0.036(2) Uani 1 0 . N12 N 0.8285(5) 0.8716(4) 0.0756(9) 0.0393(17) Uani 1 0 . C13 C 0.7435(5) 0.7176(4) -0.2598(9) 0.0332(19) Uani 1 0 . C14 C 0.6417(6) 0.6471(5) -0.4439(11) 0.043(2) Uani 1 0 . C15 C 0.6856(6) 0.5764(5) -0.6356(10) 0.045(2) Uani 1 0 . C16 C 0.8325(6) 0.5814(5) -0.6404(11) 0.041(2) Uani 1 0 . C17 C 0.9328(6) 0.6513(5) -0.4529(11) 0.042(2) Uani 1 0 . N18 N 0.8868(4) 0.7172(4) -0.2690(8) 0.0359(17) Uani 1 0 . H1 H 0.9818 1.0488 0.2561 0.0783 Uiso 1 0 . H2 H 0.9028 1.0955 0.468 0.0502 Uiso 1 0 . H3 H 0.667 1.0205 0.4576 0.0788 Uiso 1 0 . H4 H 0.4642 0.8996 0.2245 0.0802 Uiso 1 0 . H5 H 0.4959 0.7563 -0.1071 0.0682 Uiso 1 0 . H6 H 0.5408 0.6475 -0.4397 0.0669 Uiso 1 0 . H7 H 0.6181 0.5225 -0.7568 0.0702 Uiso 1 0 . H8 H 0.8599 0.5377 -0.779 0.0692 Uiso 1 0 . H9 H 1.035 0.6522 -0.4489 0.0653 Uiso 1 0 . H10 H 0.9579 0.7662 -0.1415 0.0626 Uiso 1 0 . 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 B1 0.031(6) 0.08(3) 0.042(5) 0.021(4) 0.021(3) 0.023(4) F2 0.041(7) 0.08(3) 0.062(5) 0.0080(19) 0.0213(16) 0.016(2) F3 0.037(6) 0.07(2) 0.057(4) 0.0191(17) 0.0188(15) -0.0045(19) F4 0.049(8) 0.11(4) 0.040(3) 0.024(2) 0.0046(16) -0.009(2) F5 0.057(9) 0.07(2) 0.072(5) 0.020(2) 0.0100(17) 0.025(2) C6 0.060(10) 0.050(17) 0.054(5) 0.021(4) 0.007(3) 0.005(4) C7 0.043(8) 0.037(13) 0.047(5) 0.011(3) 0.004(3) 0.010(3) C8 0.058(10) 0.056(19) 0.051(5) 0.017(4) 0.022(3) 0.002(4) C9 0.047(8) 0.07(2) 0.055(5) 0.012(4) 0.026(3) 0.003(4) C10 0.040(7) 0.046(15) 0.048(5) -0.001(3) 0.017(3) 0.006(3) C11 0.033(6) 0.039(13) 0.034(4) 0.011(3) 0.004(3) 0.013(3) N12 0.034(6) 0.036(12) 0.046(4) 0.014(2) 0.007(2) 0.004(3) C13 0.030(5) 0.036(12) 0.030(4) 0.013(3) 0.001(2) 0.005(3) C14 0.037(7) 0.050(17) 0.043(5) 0.019(3) 0.008(3) 0.005(3) C15 0.048(8) 0.040(14) 0.041(4) 0.010(3) 0.002(3) -0.001(3) C16 0.041(7) 0.043(15) 0.041(4) 0.018(3) 0.011(3) 0.009(3) C17 0.041(7) 0.043(14) 0.044(5) 0.019(3) 0.012(3) 0.011(3) N18 0.034(6) 0.034(12) 0.038(4) 0.013(2) 0.007(2) 0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F F 0.014 0.01 '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' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 N12 C11 118.5(5) . . . no C13 N18 C17 122.9(5) . . . no C6 C6 C7 111.7(7) 2_776 . . no N12 C7 C6 116.1(5) . . . no N12 C7 C8 121.2(6) . . . no C6 C7 C8 122.7(5) . . . no C7 C8 C9 119.7(6) . . . no C8 C9 C10 119.2(5) . . . no C9 C10 C11 117.2(6) . . . no N12 C11 C10 124.1(5) . . . no N12 C11 C13 113.7(4) . . . no C10 C11 C13 122.2(5) . . . no N18 C13 C11 115.1(5) . . . no N18 C13 C14 118.3(5) . . . no C11 C13 C14 126.5(5) . . . no C13 C14 C15 120.4(5) . . . no C14 C15 C16 119.2(6) . . . no C15 C16 C17 119.5(5) . . . no N18 C17 C16 119.8(5) . . . no F2 B1 F3 111.2(6) . . . no F2 B1 F4 111.3(5) . . . no F2 B1 F5 109.2(5) . . . no F3 B1 F4 109.1(5) . . . no F3 B1 F5 108.4(5) . . . no F4 B1 F5 107.5(6) . . . no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag F2 B1 1.366(9) . . no F3 B1 1.384(6) . . no F4 B1 1.387(8) . . no F5 B1 1.417(7) . . no N12 C7 1.337(7) . . no N12 C11 1.331(7) . . no N18 C13 1.351(6) . . no N18 C17 1.349(6) . . no C6 C6 1.497(10) . 2_776 no C6 C7 1.509(9) . . no C7 C8 1.388(8) . . no C8 C9 1.372(9) . . no C9 C10 1.393(8) . . no C10 C11 1.374(7) . . no C11 C13 1.492(7) . . no C13 C14 1.366(8) . . no C14 C15 1.396(8) . . no C15 C16 1.380(8) . . no C16 C17 1.362(8) . . no