#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100722.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_1100722 loop_ _publ_author_name 'Andrea C. Sudik' 'Adrien P. C\^ot\'e' 'Omar M. Yaghi' _publ_contact_author_address ; department of chemistry university of michigan 930 n. university ave. ann arbor, mi 48109-1055 united states of america ; _publ_contact_author_email oyaghi@umich.edu _publ_contact_author_name 'professor omar m. yaghi' _publ_section_title ; Metal-Organic Frameworks Based on Trigonal Prismatic Building Blocks and the New "acs" Topology ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2998 _journal_page_last 3000 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '(C33 H15 Fe3 N3 O16), (Cl4 Fe), O' _chemical_formula_sum 'C33 H15 Cl4 Fe4 N3 O17' _chemical_formula_weight 1090.61 _chemical_name_systematic ; ? ; _space_group_IT_number 190 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P -6c -2c' _symmetry_space_group_name_H-M 'P -6 2 c' _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 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 12.531(3) _cell_length_b 12.531(3) _cell_length_c 18.476(11) _cell_measurement_reflns_used 715 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 25.14 _cell_measurement_theta_min 1.88 _cell_volume 2512.5(17) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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 153(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.1441 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 11323 _diffrn_reflns_theta_full 25.15 _diffrn_reflns_theta_max 25.15 _diffrn_reflns_theta_min 1.88 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_correction_T_min 0.9433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_description octahedral _exptl_crystal_F_000 1084 _exptl_crystal_size_max 0.042 _exptl_crystal_size_mid 0.041 _exptl_crystal_size_min 0.037 _refine_diff_density_max 0.718 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.159 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(10) _refine_ls_extinction_coef 0.015(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 116 _refine_ls_number_reflns 1543 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.260 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.1044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+5.2365P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2454 _refine_ls_wR_factor_ref 0.2550 _reflns_number_gt 1292 _reflns_number_total 1543 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic050064gsi20050115_040515_2.cif _[local]_cod_data_source_block MOF-235 _[local]_cod_cif_authors_sg_Hall P-6c-2c _cod_original_cell_volume 2512.6(17) _cod_database_code 1100722 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z+1/2' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -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 _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.7270(2) 1.2195(2) 0.7500 0.0233(6) Uani 1 2 d S . . O1 O 0.6667 1.3333 0.7500 0.018(4) Uani 1 6 d S . . O2 O 0.8499(8) 1.3019(7) 0.6692(4) 0.034(2) Uani 1 1 d . . . O3 O 0.7800(11) 1.0882(12) 0.7500 0.047(3) Uani 1 2 d S . . O4 O 0.6106(8) 1.1159(8) 0.6719(5) 0.042(2) Uani 1 1 d . . . C1 C 0.716(3) 0.982(3) 0.7500 0.21(3) Uani 1 2 d S . . H1 H 0.6321 0.9569 0.7500 0.255 Uiso 1 2 calc SR . . N1 N 0.738(2) 0.893(2) 0.7500 0.119(10) Uani 1 2 d SD . . C3 C 0.5160(11) 1.1110(13) 0.6423(8) 0.046(3) Uani 1 1 d . . . C4 C 0.5680(13) 1.0240(18) 0.5353(7) 0.064(5) Uani 1 1 d . . . H4 H 0.6384 1.0371 0.5598 0.03(3) Uiso 1 1 calc R . . C5 C 0.4835(12) 1.0521(13) 0.5685(7) 0.047(4) Uani 1 1 d . . . C6 C 0.3754(11) 1.0259(11) 0.5325(6) 0.041(3) Uani 1 1 d . . . H6 H 0.3204 1.0452 0.5545 0.050 Uiso 1 1 calc R . . C7 C 0.805(6) 0.896(5) 0.692(3) 0.16(3) Uani 0.50 1 d P . . C8 C 0.643(5) 0.767(3) 0.7500 0.30(4) Uani 1 2 d SD . . O1W O 0.3333 0.6667 0.594(6) 0.22(4) Uani 0.50 3 d SP . . Fe2 Fe 0.0000 1.0000 0.5000 0.099(3) Uani 1 6 d S . . Cl1 Cl -0.1618(12) 1.0000 0.5000 0.051(4) Uani 0.333 2 d SP . . Cl2 Cl -0.1453(17) 0.9805(19) 0.574(2) 0.31(2) Uani 0.50 1 d P . . 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 0.0169(11) 0.0207(12) 0.0349(10) 0.000 0.000 0.0114(10) O1 0.001(5) 0.001(5) 0.053(11) 0.000 0.000 0.000(2) O2 0.040(5) 0.030(5) 0.041(5) 0.012(4) 0.018(4) 0.024(4) O3 0.041(8) 0.033(8) 0.069(9) 0.000 0.000 0.019(6) O4 0.041(6) 0.037(5) 0.054(5) -0.017(4) -0.010(4) 0.024(4) C1 0.042(16) 0.032(17) 0.56(10) 0.000 0.000 0.018(14) N1 0.11(2) 0.053(14) 0.23(3) 0.000 0.000 0.069(15) C3 0.037(8) 0.032(8) 0.072(9) -0.017(7) -0.018(6) 0.018(7) C4 0.051(9) 0.116(14) 0.038(7) -0.038(9) -0.021(7) 0.052(10) C5 0.037(9) 0.042(8) 0.052(7) -0.011(6) 0.000(6) 0.014(7) C6 0.022(6) 0.054(8) 0.047(6) 0.000(6) -0.003(6) 0.019(6) C7 0.31(8) 0.17(5) 0.15(4) 0.06(4) 0.13(5) 0.21(7) C8 0.21(6) 0.06(3) 0.63(14) 0.000 0.000 0.07(4) O1W 0.13(4) 0.13(4) 0.39(12) 0.000 0.000 0.065(18) Fe2 0.097(4) 0.097(4) 0.105(5) 0.000 0.000 0.0483(19) Cl1 0.020(5) 0.050(9) 0.095(12) -0.004(9) -0.002(5) 0.025(4) Cl2 0.105(12) 0.118(16) 0.65(5) -0.14(3) 0.12(2) 0.004(11) 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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 _geom_angle_publ_flag O1 Fe1 O4 93.0(2) . 4_556 ? O1 Fe1 O4 93.0(2) . . ? O4 Fe1 O4 92.3(6) 4_556 . ? O1 Fe1 O2 95.9(2) . 4_556 ? O4 Fe1 O2 85.5(4) 4_556 4_556 ? O4 Fe1 O2 170.9(3) . 4_556 ? O1 Fe1 O2 95.9(2) . . ? O4 Fe1 O2 170.9(3) 4_556 . ? O4 Fe1 O2 85.4(4) . . ? O2 Fe1 O2 95.4(5) 4_556 . ? O1 Fe1 O3 176.3(4) . . ? O4 Fe1 O3 84.5(3) 4_556 . ? O4 Fe1 O3 84.5(3) . . ? O2 Fe1 O3 86.6(3) 4_556 . ? O2 Fe1 O3 86.6(3) . . ? Fe1 O1 Fe1 120.000(2) 3_575 . ? Fe1 O1 Fe1 120.0 3_575 2_775 ? Fe1 O1 Fe1 120.001(1) . 2_775 ? C3 O2 Fe1 129.4(8) 2_775 . ? C1 O3 Fe1 126.8(17) . . ? C3 O4 Fe1 134.2(8) . . ? O3 C1 N1 132(3) . . ? O3 C1 H1 114.0 . . ? N1 C1 H1 114.0 . . ? C1 N1 C7 113(2) . . ? C1 N1 C7 113(2) . 4_556 ? C7 N1 C7 105(6) . 4_556 ? C1 N1 C8 123(3) . . ? C7 N1 C8 101(3) . . ? C7 N1 C8 101(3) 4_556 . ? O2 C3 O4 125.4(12) 3_575 . ? O2 C3 C5 119.3(12) 3_575 . ? O4 C3 C5 115.3(12) . . ? C4 C4 C5 118.9(8) 8_676 . ? C4 C4 H4 120.6 8_676 . ? C5 C4 H4 120.6 . . ? C6 C5 C4 119.8(12) . . ? C6 C5 C3 122.7(12) . . ? C4 C5 C3 117.5(12) . . ? C6 C6 C5 121.2(8) 8_676 . ? C6 C6 H6 119.4 8_676 . ? C5 C6 H6 119.4 . . ? Cl1 Fe2 Cl1 119.998(1) 3_575 1_455 ? Cl1 Fe2 Cl1 120.001(6) 3_575 2_665 ? Cl1 Fe2 Cl1 120.001(10) 1_455 2_665 ? Cl2 Cl1 Cl2 153(2) 8_676 . ? Cl2 Cl1 Fe2 76.6(11) 8_676 1_655 ? Cl2 Cl1 Fe2 76.6(11) . 1_655 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.920(2) . ? Fe1 O4 2.001(9) 4_556 ? Fe1 O4 2.001(9) . ? Fe1 O2 2.019(8) 4_556 ? Fe1 O2 2.019(8) . ? Fe1 O3 2.059(13) . ? O1 Fe1 1.920(2) 3_575 ? O1 Fe1 1.920(2) 2_775 ? O2 C3 1.235(16) 2_775 ? O3 C1 1.16(3) . ? O4 C3 1.278(15) . ? C1 N1 1.27(3) . ? C1 H1 0.9300 . ? N1 C7 1.36(4) . ? N1 C7 1.36(4) 4_556 ? N1 C8 1.43(2) . ? C3 O2 1.235(16) 3_575 ? C3 C5 1.507(18) . ? C4 C4 1.41(3) 8_676 ? C4 C5 1.412(19) . ? C4 H4 0.9300 . ? C5 C6 1.393(17) . ? C6 C6 1.33(2) 8_676 ? C6 H6 0.9300 . ? Fe2 Cl1 2.028(16) . ? Fe2 Cl1 2.028(16) . ? Fe2 Cl1 2.028(16) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Cl1 Fe2 2.028(16) . ? Cl2 Fe2 2.19(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Fe1 O1 Fe1 -46.3(3) 4_556 . . 3_575 ? O4 Fe1 O1 Fe1 46.3(3) . . . 3_575 ? O2 Fe1 O1 Fe1 -132.0(3) 4_556 . . 3_575 ? O2 Fe1 O1 Fe1 132.0(3) . . . 3_575 ? O4 Fe1 O1 Fe1 133.7(3) 4_556 . . 2_775 ? O4 Fe1 O1 Fe1 -133.7(3) . . . 2_775 ? O2 Fe1 O1 Fe1 48.0(3) 4_556 . . 2_775 ? O2 Fe1 O1 Fe1 -48.0(3) . . . 2_775 ? O1 Fe1 O2 C3 13.9(12) . . . 2_775 ? O4 Fe1 O2 C3 106.4(12) . . . 2_775 ? O2 Fe1 O2 C3 -82.7(12) 4_556 . . 2_775 ? O3 Fe1 O2 C3 -168.9(12) . . . 2_775 ? O4 Fe1 O3 C1 46.5(3) 4_556 . . . ? O4 Fe1 O3 C1 -46.5(3) . . . . ? O2 Fe1 O3 C1 132.2(3) 4_556 . . . ? O2 Fe1 O3 C1 -132.2(3) . . . . ? O1 Fe1 O4 C3 -11.8(13) . . . . ? O4 Fe1 O4 C3 81.2(13) 4_556 . . . ? O2 Fe1 O4 C3 -107.5(13) . . . . ? O3 Fe1 O4 C3 165.5(13) . . . . ? Fe1 O3 C1 N1 180.0 . . . . ? O3 C1 N1 C7 -59(4) . . . . ? O3 C1 N1 C7 59(4) . . . 4_556 ? O3 C1 N1 C8 180.0 . . . . ? Fe1 O4 C3 O2 -21(2) . . . 3_575 ? Fe1 O4 C3 C5 158.7(9) . . . . ? C4 C4 C5 C6 3(3) 8_676 . . . ? C4 C4 C5 C3 -176(2) 8_676 . . . ? O2 C3 C5 C6 -8(2) 3_575 . . . ? O4 C3 C5 C6 172.1(13) . . . . ? O2 C3 C5 C4 171.5(15) 3_575 . . . ? O4 C3 C5 C4 -8(2) . . . . ? C4 C5 C6 C6 0(3) . . . 8_676 ? C3 C5 C6 C6 179.9(15) . . . 8_676 ? Cl2 Cl1 Cl2 Fe2 0.00(2) 8_676 . . 1_655 ?