High capacity gas storage by a 4,8-connected metal - organic polyhedral framework
Chenrong Tan; Sihai Yang; Neil R. Champness; Xiang Lin; Alexander Blake; William Lewis; Martin Schroder; Chem.Commun. 47 (2011) 4487–; doi:10.1039/c1cc10378d

data_7106230
_publ_section_title
;
 High capacity gas storage by a 4,8-connected metal - organic polyhedral
 framework
;
_journal_name_full               Chem.Commun.
_journal_page_first              4487
_journal_paper_doi               10.1039/c1cc10378d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'(C57 H36 Cu4 O20), 10(C3 H7 N O), (C4 H8 O2), 8(H2 O)'
_chemical_formula_sum            'C91 H130 Cu4 N10 O40'
_chemical_formula_weight         2258.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :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            4
_cell_length_a                   18.900(3)
_cell_length_b                   18.900(3)
_cell_length_c                   33.561(7)
_cell_measurement_reflns_used    752
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.43
_cell_measurement_theta_min      2.35
_cell_volume                     11988(4)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_publication_material
'enCIFer (Allen et al., 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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.194
_diffrn_reflns_av_sigmaI/netI    0.093
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51240
_diffrn_reflns_theta_full        21.26
_diffrn_reflns_theta_max         21.26
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998). Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       plate
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.002
_platon_squeeze_details
;
Approximately 71% 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 3175 electrons per unit cell,
which were assigned to be 40 DMF, 4 dioxane and 32 water molecules per unit
cell.
The final formula was calculated from TGA combined with elemental analysis data.
;
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.00
_refine_ls_R_factor_all          0.113
_refine_ls_R_factor_gt           0.0463
_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^)+(0.012P)^2^+1.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                2142
_reflns_number_total             3660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10378d.txt
_cod_data_source_block           CUTPDM
_cod_original_cell_volume        11988(3)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               7106230