Pore with Gate: Enhancement of the Isosteric Heat of Adsorption of Dihydrogen via Postsynthetic Cation Exchange in Metal-Organic Frameworks
Sihai Yang; Gregory S. B. Martin; Jeremy J. Titman; Alexander J. Blake; David R. Allan; Neil R. Champness; Martin Schröder; Inorganic Chemistry 50 (2011) 9374–9384; doi:10.1021/ic200967b

data_4326326
_publ_section_title
;
 Pore with Gate: Enhancement of the Isosteric Heat of Adsorption of
 Dihydrogen via Postsynthetic Cation Exchange in Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9374
_journal_page_last               9384
_journal_paper_doi               10.1021/ic200967b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_iupac
'In (C34 O8 H18) (C2 H8 N), 2(C3 H7 N O), 2.5(H2 O)'
_chemical_formula_moiety
'C34 H18 In O8 -, C2 H8 N +, 2(C3 H7 N O), 2.5(H2 O)'
_chemical_formula_sum            'C42 H45 In N3 O12.5'
_chemical_formula_weight         906.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 102.486(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   45.040(5)
_cell_length_b                   9.7592(10)
_cell_length_c                   9.9522(10)
_cell_measurement_reflns_used    2897
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.86
_cell_measurement_theta_min      2.44
_cell_volume                     4271.1(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      120(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6941
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13352
_diffrn_reflns_theta_full        22.73
_diffrn_reflns_theta_max         22.73
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Approximately 40% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 127 electrons per unit cell,
which were assigned to be 2.0 DMF and 2.5 water molecules per indium. 
The final formula was calculated from the TGA combined with elemental 
analysis data.
;
_refine_diff_density_max         1.57
_refine_diff_density_min         -0.48
_refine_diff_density_rms         0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3257
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0800
_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^)+(0.142P)^2^+4.796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.213
_refine_ls_wR_factor_ref         0.226
_reflns_number_gt                2343
_reflns_number_total             3257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200967b_si_002_3.cif
_cod_data_source_block           NOTT-208
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C42 H45 In N3 O12.50'
_cod_database_code               4326326