High Capacity Hydrogen Adsorption in Cu(II) Tetracarboxylate Framework Materials: The Role of Pore Size, Ligand Functionalization, and Exposed Metal Sites
Xiang Lin; Irvin Telepeni; Alexander J. Blake; Anne Dailly; Craig M. Brown; Jason M. Simmons; Marco Zoppi; Gavin S. Walker; K. Mark Thomas; Timothy J. Mays; Peter Hubberstey; Neil R. Champness; Martin Schröder; Journal of the American Chemical Society 131 (2009) 2159–2171; doi:10.1021/ja806624j

data_4103900
_publ_section_title
;
 High Capacity Hydrogen Adsorption in Cu(II) Tetracarboxylate Framework
 Materials: The Role of Pore Size, Ligand Functionalization, and Exposed
 Metal Sites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2159
_journal_page_last               2171
_journal_paper_doi               10.1021/ja806624j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_structural     '[Cu4 (C34 O8 H18)2 (H2 O)4] (C3H7NO) (H2O)3'
_chemical_formula_sum            'C74 H70 Cu4 N2 O28'
_chemical_formula_weight         1689.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   18.348(1)
_cell_length_b                   18.348(1)
_cell_length_c                   65.094(2)
_cell_measurement_reflns_used    2063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      2.34
_cell_volume                     18977.9(16)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.6907
_diffrn_reflns_av_R_equivalents  0.113
_diffrn_reflns_av_sigmaI/netI    0.076
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            47634
_diffrn_reflns_theta_full        20.21
_diffrn_reflns_theta_max         20.21
_diffrn_reflns_theta_min         1.29
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7812
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
Approximately 40.5% 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 157 electrons per formula.
The final formula was calculated from the SQUEEZE results combined with
elemental analysis and TGA data.
;
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.69
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.23
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2454
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.22
_refine_ls_R_factor_all          0.196
_refine_ls_R_factor_gt           0.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.372
_refine_ls_wR_factor_ref         0.402
_reflns_number_gt                1103
_reflns_number_total             2454
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja806624j_si_002_2.cif
_cod_data_source_block           NOTT104
_cod_original_cell_volume        18978(2)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4103900