Metal-Organic Polyhedral Frameworks: High H2 Adsorption Capacities and Neutron Powder Diffraction Studies
Yong Yan; Irvin Telepeni; Sihai Yang; Xiang Lin; Winfried Kockelmann; Anne Dailly; Alexander J. Blake; William Lewis; Gavin S. Walker; David R. Allan; Sarah A. Barnett; Neil R. Champness; Martin Schröder; Journal of the American Chemical Society 132 (2010) 4092–4094; doi:10.1021/ja1001407

data_4102152
_publ_section_title
;
 Metal-Organic Polyhedral Frameworks: High H2 Adsorption Capacities and
 Neutron Powder Diffraction Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4092
_journal_page_last               4094
_journal_paper_doi               10.1021/ja1001407
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'Cu3 (C54 O12 H24) 3(H2 O), 16(C3 H7 N O), 26(H2 O)'
_chemical_formula_sum            'C102 H194 Cu3 N16 O57'
_chemical_formula_weight         2747.26
_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           '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            32
_cell_length_a                   51.670(6)
_cell_length_b                   51.670(6)
_cell_length_c                   51.670(6)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      37.0120
_cell_measurement_theta_min      2.1610
_cell_volume                     137948(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      120(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.163
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            35350
_diffrn_reflns_theta_full        15.99
_diffrn_reflns_theta_max         15.99
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             46749
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Approximately 81% 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 37961 electrons per unit cell,
which were assigned to be 5 DMF and 5 water molecules per copper. 
The final formula was calculated from TGA combined with elemental 
analysis data.
;
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.03
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.18
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.18
_refine_ls_R_factor_all          0.115
_refine_ls_R_factor_gt           0.104
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.156P)^2^+412.2P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.297
_refine_ls_wR_factor_ref         0.308
_reflns_number_gt                1701
_reflns_number_total             1864
_reflns_threshold_expression     >2I\s(I)
_cod_data_source_file            ja1001407_si_002.cif
_cod_data_source_block           NOTT-116
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        137948(28)
_cod_database_code               4102152