A mesoporous metal-organic framework constructed from a nanosized C3‒symmetric linker and [Cu24(isophthalate)24] cuboctahedra
Yan Yong; Sihai Yang; Alexander Blake; William Lewis; Eric Poirier; Sarah Barnett; Neil Champness; Martin Schroder; Chem.Commun. 47 (2011) 9995–; doi:10.1039/c1cc13170b

data_7106813
_publ_section_title
;
 A mesoporous metal-organic framework constructed from a nanosized
 C3--symmetric linker and [Cu24(isophthalate)24] cuboctahedra
;
_journal_name_full               Chem.Commun.
_journal_page_first              9995
_journal_paper_doi               10.1039/c1cc13170b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_iupac          '(Cu3 C66 H42 O15) (C3 H7 N O)35 (H2 O)35'
_chemical_formula_moiety         'Cu3 C66 H42 O15, 35(C3 H7 N O), 35(H2 O)'
_chemical_formula_sum            'C171 H357 Cu3 N35 O85'
_chemical_formula_weight         4454.54
_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                   56.296(7)
_cell_length_b                   56.296(7)
_cell_length_c                   56.296(7)
_cell_measurement_reflns_used    2623
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.02
_cell_measurement_theta_min      2.3
_cell_volume                     178416(4)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_molecular_graphics    'Bruker SHELXTL'
_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_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.141
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            45135
_diffrn_reflns_theta_full        15.99
_diffrn_reflns_theta_max         15.99
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             76640
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Approximately 80% 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 35541 electrons
per unit cell, and thereby produced a set of solvent-free diffraction
intensities. The final formula was calculated from the TGA combined with
elemental analysis data.
;
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.42
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.53
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2377
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.55
_refine_ls_R_factor_all          0.150
_refine_ls_R_factor_gt           0.131
_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^)+(0.200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.371
_refine_ls_wR_factor_ref         0.391
_reflns_number_gt                2010
_reflns_number_total             2377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13170b.txt
_cod_data_source_block           cuyylf
_cod_original_cell_volume        178416(36)
_cod_database_code               7106813