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_4326327
_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) 1.4Li 0.6(H3 O), 4(C3 H6 O), 11(H2 O)'
_chemical_formula_moiety
'C68 H36 In 2 O16 2-, 1.4Li 1.4+ 0.6(H3 O) 0.6+, 4(C3 H6 O), 11(H2 O)'
_chemical_formula_sum            'C80 H83.8 In2 Li1.4 O31.6'
_chemical_formula_weight         1790.23
_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                 102.053(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   45.20(2)
_cell_length_b                   9.738(5)
_cell_length_c                   9.944(3)
_cell_measurement_reflns_used    1609
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.14
_cell_measurement_theta_min      4.96
_cell_volume                     4280(3)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear (Rigaku, 2009)'
_computing_data_reduction        'Rigaku CrystalClear'
_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      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9656
_diffrn_reflns_theta_full        23.04
_diffrn_reflns_theta_max         23.04
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1838
_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 198 electrons per unit cell,
which were assigned to be 2.0 acetone and 5.5 water molecules per indium. 
The final formula was calculated from the TGA combined with elemental 
analysis data.
;
_refine_diff_density_max         1.03
_refine_diff_density_min         -1.08
_refine_diff_density_rms         0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3388
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0896
_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^)+(0.0200P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                2831
_reflns_number_total             3388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200967b_si_002_4.cif
_cod_data_source_block           NOTT-209
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C80 H83.80 In2 Li1.40 O31.60'
_cod_database_code               4326327