Highly Porous and Robust Scandium-based Metal-Organic Frameworks for Hydrogen Storage
Ilich A. Ibarra; Sihai Yang; Xiang Lin; Alexander J. Blake; Pierre J. Rizkallah; Harriott Nowell; David R. Allan; Neil R. Champness; Peter Hubberstey; Martin Schroder; Chem.Commun. 47 (2011) 8304–; doi:10.1039/c1cc11168j

data_7106668
_publ_section_title
;
 Highly Porous and Robust Scandium-based Metal-Organic Frameworks for
 Hydrogen Storage
;
_journal_name_full               Chem.Commun.
_journal_page_first              8304
_journal_paper_doi               10.1039/c1cc11168j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C6 H3 O5 Sc1, 2.6(H2 O)'
_chemical_formula_structural     '[Sc(C6H2O4S1)(OH)] (H2O)2.6'
_chemical_formula_sum            'C6 H8.2 O7.6 S Sc'
_chemical_formula_weight         278.95
_chemical_name_systematic
;
?
;
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_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            16
_cell_length_a                   22.605(4)
_cell_length_b                   22.605(4)
_cell_length_c                   12.474(2)
_cell_measurement_reflns_used    8272
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.79
_cell_measurement_theta_min      2.49
_cell_volume                     6374.0(19)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_publication_material
'enCIFer (Allen at el., 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 28.5714
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku Saturn 724+'
_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     0.6939
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24677
_diffrn_reflns_theta_full        30.97
_diffrn_reflns_theta_max         30.97
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998). Private communication'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       Block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Approximately 54% of the unit cell 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
for the solvent region and therefore produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total of 468 electrones per unit cell,
which are assigned to be 26 water molecules per unit cell. The final formula
was calculated considering elemental analysis results.
;
_refine_diff_density_max         1.36
_refine_diff_density_min         -0.57
_refine_diff_density_rms         0.10
_refine_ls_extinction_coef       0.0023(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.23
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         2747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.23
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.082P)^2^+13.01P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.177
_refine_ls_wR_factor_ref         0.182
_reflns_number_gt                2304
_reflns_number_total             2747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11168j.txt
_cod_data_source_block           2
_cod_original_cell_volume        6373.7(19)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_original_formula_sum        'C6 H8.2 O7.6 S1 Sc1'
_cod_database_code               7106668