#------------------------------------------------------------------------------ #$Date: 2012-02-28 12:14:52 +0000 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501630.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_1501630 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 (C26 O8 H10) (C2 H8 N), 2(C3 H7 N O), 2(H2 O)' _chemical_formula_sum 'C34 H36 In N3 O12' _chemical_formula_weight 793.48 _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 760 _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, 2003)' _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 0.977 _diffrn_measured_fraction_theta_max 0.977 _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 0.093 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 24009 _diffrn_reflns_theta_full 23.24 _diffrn_reflns_theta_max 23.24 _diffrn_reflns_theta_min 4.16 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_T_max 0.92 _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 0.993 _exptl_crystal_description Octahedron _exptl_crystal_F_000 812 _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 30 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 0.62 _refine_diff_density_min -0.26 _refine_diff_density_rms 0.05 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 1085 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.00 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0458 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.043P)^2^+2.000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.105 _reflns_number_gt 696 _reflns_number_total 1085 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c1fd00006c.txt _[local]_cod_data_source_block NOTT-213 _[local]_cod_cif_authors_sg_H-M 'P 42/mmc' _cod_original_cell_volume 2654.3(3) _cod_database_code 1501630 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 _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.5000 0.5000 0.2500 0.0562(3) Uani 1 8 d SU . . O1 O 0.2575(5) 0.5000 0.24041(15) 0.1041(18) Uani 1 2 d SU . . O2 O 0.5000 0.3581(4) 0.18774(17) 0.0848(14) Uani 1 2 d SU . . C1 C 0.5000 0.2525(7) 0.2136(3) 0.074(2) Uani 1 2 d SU . . C2 C 0.5000 0.1188(6) 0.1864(3) 0.0751(19) Uani 1 2 d SU . . C3 C 0.5000 0.0000 0.2131(3) 0.069(3) Uani 1 4 d SU . . H3A H 0.5000 0.0000 0.2478 0.083 Uiso 1 4 calc SR . . C4 C 0.5000 0.1202(7) 0.1350(2) 0.090(2) Uani 1 2 d SU . . H4A H 0.5000 0.2012 0.1177 0.108 Uiso 1 2 calc SR . . C5 C 0.5000 0.0000 0.1093(3) 0.103(4) Uani 1 4 d SU . . C6 C 0.5000 0.0000 0.0514(5) 0.109(4) Uiso 1 4 d SDU . . C7 C 0.3821(11) 0.0536(10) 0.02725(17) 0.118(4) Uiso 0.50 1 d PDU . . C8 C 0.2555(18) 0.094(2) 0.0501(10) 0.139(9) Uiso 0.25 1 d PDU . -1 H8A H 0.2485 0.0746 0.0852 0.167 Uiso 0.25 1 d PR . -1 C9 C 0.135(3) 0.148(2) 0.0272(2) 0.226(17) Uiso 0.25 1 d PD A -2 H9A H 0.0594 0.1830 0.0455 0.271 Uiso 0.25 1 d PR A -2 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 0.0666(4) 0.0666(4) 0.0355(4) 0.000 0.000 0.000 O1 0.081(3) 0.182(5) 0.049(3) 0.000 0.015(2) 0.000 O2 0.124(4) 0.050(3) 0.080(3) -0.008(3) 0.000 0.000 C1 0.084(5) 0.059(5) 0.079(5) -0.005(4) 0.000 0.000 C2 0.100(5) 0.049(4) 0.076(5) -0.006(4) 0.000 0.000 C3 0.101(8) 0.045(6) 0.062(6) 0.000 0.000 0.000 C4 0.166(8) 0.048(4) 0.056(4) -0.008(4) 0.000 0.000 C5 0.179(13) 0.076(8) 0.052(6) 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 125.53(16) . 11_566 O2 In1 O2 80.7(3) . 2_665 O2 In1 O1 136.39(16) . 11_566 O2 In1 O1 85.38(7) . . O2 In1 O1 55.73(16) 11_566 . O1 In1 O1 90.64(2) 11_566 . O1 In1 O1 167.88(19) 2_665 . C1 O1 In1 86.2(5) 11_566 . C1 O2 In1 96.9(4) . . O1 C1 O2 121.1(7) 12_656 . O1 C1 C2 120.9(7) 12_656 . O2 C1 C2 118.0(6) . . C4 C2 C3 121.6(7) . . C4 C2 C1 118.1(6) . . C3 C2 C1 120.3(6) . . C2 C3 C2 118.0(8) 2_655 . C2 C4 C5 119.3(7) . . C4 C5 C4 120.4(9) 2_655 . C4 C5 C6 119.8(4) 2_655 . C4 C5 C6 119.8(4) . . C8 C7 C7 120.0(10) . 6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 In1 O2 2.184(4) . In1 O1 2.430(5) . O1 C1 1.230(8) 11_566 O2 C1 1.259(7) . C1 C2 1.518(8) . C2 C4 1.377(9) . C2 C3 1.381(8) . C4 C5 1.380(7) . C5 C6 1.549(15) . C6 C7 1.443(8) . C7 C8 1.457(10) . C7 C7 1.458(9) 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 -0.019 0.436 -0.004 1529 30