#------------------------------------------------------------------------------ #$Date: 2012-10-08 19:35:59 +0300 (Mon, 08 Oct 2012) $ #$Revision: 67906 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/45/4114576.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_4114576 loop_ _publ_author_name 'Mohamed Eddaoudi' 'Jaheon Kim' 'Michael O'Keeffe' 'Omar M. Yaghi' _publ_contact_author ; Omar M. Yaghi Department of Chemistry University of Michigan 930 N. University Ave. Ann Arbor, MI 48109-1055, USA ; _publ_contact_author_email oyaghi@umich.edu _publ_section_title ; Cu2[o-Br-C6H3(CO2)2]2(H2O)2.(DMF)8(H2O)2: A Framework Deliberately Designed To Have the NbO Structure Type ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 376 _journal_page_last 377 _journal_volume 124 _journal_year 2002 _chemical_formula_sum 'C40 H70 Br2 Cu2 N8 O20' _chemical_formula_weight 1269.94 _chemical_name_systematic ; ? ; _space_group_IT_number 229 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-I 4 2 3' _symmetry_space_group_name_H-M 'I m -3 m' _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 90.00 _cell_formula_units_Z 6 _cell_length_a 21.607(3) _cell_length_b 21.607(3) _cell_length_c 21.607(3) _cell_measurement_reflns_used 1244 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 15.25 _cell_measurement_theta_min 2.31 _cell_volume 10087(2) _computing_cell_refinement SAINT _computing_data_collection SMART _computing_data_reduction SAINT _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method 'omega & phi scan' _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 0.3281 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 33854 _diffrn_reflns_theta_full 23.29 _diffrn_reflns_theta_max 23.29 _diffrn_reflns_theta_min 1.33 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 1.884 _exptl_absorpt_correction_T_max 0.9423 _exptl_absorpt_correction_T_min 0.7140 _exptl_absorpt_correction_type SADABS _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.254 _exptl_crystal_description block _exptl_crystal_F_000 3924 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.327 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.081 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 752 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 0.961 _refine_ls_R_factor_all 0.1693 _refine_ls_R_factor_gt 0.0788 _refine_ls_shift/su_max 1.349 _refine_ls_shift/su_mean 0.115 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2215 _refine_ls_wR_factor_ref 0.2840 _reflns_number_gt 321 _reflns_number_total 752 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ja017154e_s2.cif _[local]_cod_data_source_block MOF-101 _[local]_cod_chemical_formula_sum_orig 'C40 H70 N8 O20 Cu2 Br2' _cod_original_cell_volume 10088(2) _cod_database_code 4114576 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, -x+1/2' 'z+1/2, y+1/2, x+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 Cu Cu 0.0000 0.0000 0.43841(14) 0.0756(14) Uani 1 8 d S O1 O 0.0899(4) 0.0000 0.4480(4) 0.091(3) Uani 1 2 d S O2 O 0.0000 0.0000 0.3396(8) 0.137(7) Uani 1 8 d S C1 C 0.1147(8) 0.0000 0.5000 0.084(6) Uani 1 4 d S C2 C 0.1844(8) 0.0000 0.5000 0.092(5) Uani 1 4 d S C3 C 0.2145(14) 0.0000 0.4466(14) 0.127(13) Uani 0.50 2 d SP C4 C 0.2162(14) 0.0511(14) 0.5000 0.150(18) Uani 0.50 2 d SP Br Br 0.1770(4) 0.1309(4) 0.5000 0.387(12) Uani 0.25 2 d SP O3 O 0.0000 0.188(5) 0.274(5) 0.48(6) Uiso 0.25 2 d SP O4 O 0.051(3) 0.051(3) 0.051(3) 0.28(7) Uiso 0.25 6 d SP O1S O 0.0331(18) 0.0331(18) 0.235(4) 0.37(3) Uiso 0.25 2 d SPD N1S N 0.111(4) 0.111(4) 0.292(5) 0.37(3) Uiso 0.25 2 d SPD C1S C 0.073(2) 0.073(2) 0.248(6) 0.37(3) Uiso 0.25 2 d SPD C2S C 0.105(3) 0.170(3) 0.326(5) 0.37(3) Uiso 0.25 1 d PD 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 Cu 0.0601(15) 0.0601(15) 0.106(3) 0.000 0.000 0.000 O1 0.063(6) 0.098(6) 0.113(8) 0.000 0.003(5) 0.000 O2 0.152(11) 0.152(11) 0.107(15) 0.000 0.000 0.000 C1 0.053(14) 0.061(11) 0.14(2) 0.000 0.000 0.000 C2 0.066(14) 0.089(17) 0.12(2) 0.000 0.000 0.000 C3 0.07(2) 0.22(5) 0.10(3) 0.000 0.012(18) 0.000 C4 0.07(2) 0.09(3) 0.30(7) 0.000 0.000 0.005(19) Br 0.079(5) 0.101(6) 0.98(4) 0.000 0.000 0.000(4) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 O1 Cu O1 167.9(5) 62 61 O1 Cu O1 89.36(5) 62 2 O1 Cu O1 89.36(6) 61 2 O1 Cu O1 89.36(6) 62 . O1 Cu O1 89.36(5) 61 . O1 Cu O1 167.9(5) 2 . O1 Cu O2 96.1(3) 62 . O1 Cu O2 96.1(3) 61 . O1 Cu O2 96.1(3) 2 . O1 Cu O2 96.1(3) . . O1 Cu Cu 83.9(3) 62 49_556 O1 Cu Cu 83.9(3) 61 49_556 O1 Cu Cu 83.9(3) 2 49_556 O1 Cu Cu 83.9(3) . 49_556 O2 Cu Cu 180.000(1) . 49_556 C1 O1 Cu 121.6(10) . . O1 C1 O1 129.0(18) . 50_556 O1 C1 C2 115.5(9) . . O1 C1 C2 115.5(9) 50_556 . C4 C2 C4 116(3) 51 . C4 C2 C3 75.0(10) 51 50_556 C4 C2 C3 75.0(10) . 50_556 C4 C2 C3 75.0(10) 51 . C4 C2 C3 75.0(10) . . C3 C2 C3 121(3) 50_556 . C4 C2 C1 121.9(15) 51 . C4 C2 C1 121.9(15) . . C3 C2 C1 119.4(15) 50_556 . C3 C2 C1 119.4(15) . . C2 C3 C4 118(3) . 43 C2 C3 C4 51.8(17) . 51 C4 C3 C4 87(2) 43 51 C2 C3 C4 51.8(17) . . C4 C3 C4 87(2) 43 . C4 C3 C4 87(3) 51 . C2 C4 C3 124(3) . 89 C2 C4 C3 53.2(16) . 50_556 C3 C4 C3 93(2) 89 50_556 C2 C4 C3 53.2(16) . . C3 C4 C3 93(2) 89 . C3 C4 C3 92(3) 50_556 . C2 C4 Br 122(2) . . C3 C4 Br 114(3) 89 . C3 C4 Br 127.6(15) 50_556 . C3 C4 Br 127.6(15) . . Br Br C4 161.2(10) 13_556 . C1S O1S O1S 133.5(19) . 52 C1S O1S O1S 133.6(19) . 51 O1S O1S O1S 89.997(3) 52 51 C1S N1S C2S 137.8(18) . . C1S N1S C2S 136.7(17) . 62 C2S N1S C2S 85(3) . 62 O1S C1S N1S 154(10) . . N1S C2S C2S 47.7(17) . 62 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu O1 1.954(8) 62 Cu O1 1.954(8) 61 Cu O1 1.954(8) 2 Cu O1 1.954(8) . Cu O2 2.135(18) . Cu Cu 2.662(6) 49_556 O1 C1 1.245(9) . C1 O1 1.245(9) 50_556 C1 C2 1.51(2) . C2 C4 1.30(3) 51 C2 C4 1.30(3) . C2 C3 1.32(3) 50_556 C2 C3 1.32(3) . C3 C4 1.50(3) 43 C3 C4 1.60(2) 51 C3 C4 1.60(2) . C4 C3 1.50(3) 89 C4 C3 1.60(2) 50_556 C4 Br 1.92(3) . Br Br 1.410(17) 13_556 O1S C1S 1.262(11) . O1S O1S 1.43(8) 52 O1S O1S 1.45(8) 51 N1S C1S 1.486(11) . N1S C2S 1.466(11) . N1S C2S 1.483(11) 62 C2S C2S 2.00(7) 62