#------------------------------------------------------------------------------ #$Date: 2012-02-28 12:14:52 +0000 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501628.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_1501628 loop_ _publ_author_name 'Yang, Sihai' 'Callear, Samantha K.' 'Ramirez-Cuesta, Anibal J.' 'David, William I. F.' 'Sun, Junliang' 'Blake, Alexander J.' 'Champness, Neil R.' 'Schr\"oder, Martin' _publ_section_title ; Pore with gate: modulating hydrogen storage in metal-organic framework materials via cation exchange ; _journal_name_full 'Faraday Discussions' _journal_page_first 19 _journal_volume 151 _journal_year 2011 _chemical_formula_moiety 'In (C24 O8 H12) (C2 H8 N), 2(C3 H7 N O), 2(H2 O)' _chemical_formula_sum 'C32 H38 In N3 O12' _chemical_formula_weight 771.47 _chemical_name_systematic ; ? ; _space_group_IT_number 131 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4c 2' _symmetry_space_group_name_H-M 'P 42/m m c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.9617(4) _cell_length_b 9.9617(4) _cell_length_c 26.747(2) _cell_measurement_reflns_used 790 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 33.22 _cell_measurement_theta_min 3.68 _cell_volume 2654.3(2) _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.5467 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device_type 'CrysAlis CCD area detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.130 _diffrn_reflns_av_sigmaI/netI 0.169 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 8753 _diffrn_reflns_theta_full 23.24 _diffrn_reflns_theta_max 23.24 _diffrn_reflns_theta_min 4.16 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 0.965 _exptl_crystal_description Octahedron _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _platon_squeeze_details ; Approximately 65% of the unit cell volume comprises a large region of disordered solvent and counter-cations which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent/cation region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 28 electrons per unit cell, which were assigned to be 2.0 DMF and 2.0 water molecules per indium. The final formula was calculated from the TGA combined with elemental analysis data. ; _refine_diff_density_max 1.12 _refine_diff_density_min -0.34 _refine_diff_density_rms 0.08 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 51 _refine_ls_number_reflns 1084 _refine_ls_number_restraints 21 _refine_ls_restrained_S_all 1.03 _refine_ls_R_factor_all 0.178 _refine_ls_R_factor_gt 0.0818 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.060P)^2^+6.000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.173 _refine_ls_wR_factor_ref 0.189 _reflns_number_gt 503 _reflns_number_total 1084 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c1fd00006c.txt _[local]_cod_data_source_block NOTT-211 _[local]_cod_cif_authors_sg_H-M 'P 42/mmc' _cod_original_cell_volume 2654.3(3) _cod_database_code 1501628 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, y, -z' 'x, -y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x, -y, z' '-x, y, z' '-y, -x, z-1/2' 'y, x, 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 In1 In 0.5000 0.5000 0.2500 0.0684(8) Uani 1 8 d SU O1 O 0.2608(11) 0.5000 0.2408(3) 0.121(4) Uani 1 2 d SU O2 O 0.5000 0.3562(9) 0.1878(3) 0.088(3) Uani 1 2 d SU C1 C 0.5000 0.2497(14) 0.2137(5) 0.083(4) Uani 1 2 d SU C2 C 0.5000 0.1196(13) 0.1871(5) 0.092(5) Uani 1 2 d SU C3 C 0.5000 0.0000 0.2122(7) 0.087(7) Uani 1 4 d SU H3A H 0.5000 0.0000 0.2470 0.105 Uiso 1 4 calc SR C4 C 0.5000 0.1194(13) 0.1337(5) 0.107(6) Uani 1 2 d SU H4A H 0.5000 0.2003 0.1163 0.128 Uiso 1 2 calc SR C5 C 0.5000 0.0000 0.1078(7) 0.126(10) Uani 1 4 d SDU C6 C 0.5000 0.0000 0.0512(7) 0.131(9) Uiso 1 4 d SDU C7 C 0.389(2) 0.058(2) 0.0298(6) 0.121(9) Uiso 0.50 1 d PDU C8 C 0.258(3) 0.117(5) 0.0477(17) 0.148(18) Uiso 0.25 1 d PDU H8A H 0.2083 0.1500 0.0196 0.177 Uiso 0.25 1 calc PR H8B H 0.2763 0.1896 0.0703 0.177 Uiso 0.25 1 calc PR H8C H 0.2073 0.0491 0.0645 0.177 Uiso 0.25 1 calc PR 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 In1 0.0824(11) 0.0824(11) 0.0404(9) 0.000 0.000 0.000 O1 0.127(8) 0.205(11) 0.031(6) 0.000 0.012(5) 0.000 O2 0.141(9) 0.044(6) 0.078(6) -0.007(5) 0.000 0.000 C1 0.139(13) 0.035(7) 0.075(9) 0.007(7) 0.000 0.000 C2 0.153(14) 0.024(7) 0.098(9) 0.005(7) 0.000 0.000 C3 0.15(2) 0.027(10) 0.086(12) 0.000 0.000 0.000 C4 0.219(18) 0.033(9) 0.069(8) -0.006(7) 0.000 0.000 C5 0.23(3) 0.092(17) 0.057(12) 0.000 0.000 0.000 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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' 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 O2 In1 O2 125.0(3) 11_566 . O2 In1 O2 81.5(5) 2_665 . O2 In1 O1 55.1(3) 11_566 . O2 In1 O1 85.53(14) . . O2 In1 O1 136.6(3) . 11_566 O1 In1 O1 90.61(4) . 11_566 O2 In1 O1 85.54(14) . 2_665 O1 In1 O1 168.2(4) . 2_665 C1 O1 In1 89.3(9) 11_566 . C1 O2 In1 97.7(8) . . O1 C1 O2 117.8(14) 12_656 . O1 C1 C2 124.0(14) 12_656 . O2 C1 C2 118.2(12) . . C3 C2 C4 119.3(14) . . C3 C2 C1 121.8(13) . . C4 C2 C1 118.9(12) . . C2 C3 C2 121.1(18) . 2_655 C5 C4 C2 120.3(13) . . C4 C5 C4 119.5(17) 2_655 . C4 C5 C6 120.2(9) 2_655 . C4 C5 C6 120.2(9) . . C7 C6 C5 114.6(11) 13 . C7 C6 C5 114.6(11) 14_655 . C7 C6 C5 114.6(11) 2_655 . C7 C6 C5 114.6(11) . . C8 C7 C7 119(2) . 6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 In1 O2 2.195(8) . In1 O1 2.395(11) . O1 C1 1.223(14) 11_566 O2 C1 1.266(13) . C1 C2 1.477(16) . C2 C3 1.368(15) . C2 C4 1.429(17) . C3 C2 1.368(15) 2_655 C4 C5 1.377(14) . C5 C4 1.376(14) 2_655 C5 C6 1.513(10) . C6 C7 1.38(2) . C7 C8 1.503(10) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.027 -0.017 -0.008 1660 28