Exceptionally high H2 storage by a metal-organic polyhedral framework.
Yan, Yong; Lin, Xiang; Yang, Sihai; Blake, Alexander J; Dailly, Anne; Champness, Neil R; Hubberstey, Peter; Schröder, Martin; Chemical communications (Cambridge, England) 34 (2009) 1025–1027; doi:10.1039/b900013e

data_7104225
_publ_section_title
;
 Exceptionally high H2 storage by a metal-organic polyhedral framework.
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1025
_journal_page_last               1027
_journal_paper_doi               10.1039/b900013e
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety
'(Cu3 C48 H30 O15) (C2 H6 S O)8 (C3 H7 N O)15 (H2 O)3'
_chemical_formula_sum            'C109 H189 Cu3 N15 O41 S8'
_chemical_formula_weight         2812.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   47.005(3)
_cell_length_b                   47.005(3)
_cell_length_c                   47.005(3)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      43.95
_cell_measurement_theta_min      5.00
_cell_volume                     103856(11)
_computing_cell_refinement       'Bruker SAINT version 7.12A (Bruker, 2004)'
_computing_data_collection       'Bruker APEX2 Version 1.0-27 (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ' ? '
_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      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SMART APEXII CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6939
_diffrn_reflns_av_R_equivalents  0.126
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            159321
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             47712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Approximately 75% 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. SQUEEZE estimated a total count of 11071 electrons
per unit cell, and thereby produced a set of solvent-free diffraction
intensities. The final formula was calculated from the TGA results combined
with elemental analysis data.
;
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         5075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1857P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.243
_refine_ls_wR_factor_ref         0.253
_reflns_number_gt                3877
_reflns_number_total             5086
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b900013e.txt
_cod_data_source_block           cupyda1
_cod_original_sg_symbol_H-M      Fm-3m
_cod_database_code               7104225