A highly porous metal organic framework, constructed from a cuboctahedral super-molecular building block, with exceptionally high methane uptake
Ulrich Stoeck; Simon Krause; Volodymyr Bon; Irena Senkovska; Stefan Kaskel; Chem.Commun. 48 (2012) 10841–; doi:10.1039/c2cc34840c

data_7108519
_publ_section_title
;
 A highly porous metal organic framework, constructed from a cuboctahedral
 super-molecular building block, with exceptionally high methane uptake
;
_journal_name_full               Chem.Commun.
_journal_page_first              10841
_journal_paper_doi               10.1039/c2cc34840c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C40 H20 N2 O10 Zn2'
_chemical_formula_weight         819.32
_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            24
_cell_length_a                   46.806(5)
_cell_length_b                   46.806(5)
_cell_length_c                   46.806(5)
_cell_measurement_reflns_used    735
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.65
_cell_volume                     102543(19)
_computing_cell_refinement       Mosflm
_computing_data_collection       'marCCD 1994-2002'
_computing_data_reduction        Scala
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       '\D\f scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       2
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9434
_diffrn_reflns_theta_full        34.12
_diffrn_reflns_theta_max         34.12
_diffrn_reflns_theta_min         3.21
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.9843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Scala
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The SQUEEZE procedure (PLATON) was used to correct intensities
corresponding to disordered solvent molecules, located in pores.
The resulted hkl file was used at the final refinement stage.
Crystal data from original dataset:
Overall formula: C40H20N2O10Zn2x5.3C5H9NO(NMP)
Formula weight: 1344.72
Calculated density: 0.523
F(OOO): 16805
_exptl_absorpt_coefficient_mu 0.553
_refine_ls_R_factor_all 0.1454
_refine_ls_R_factor_gt 0.1047
_refine_ls_wR_factor_ref 0.3419
_refine_ls_wR_factor_gt 0.3231
_refine_ls_goodness_of_fit_ref 2.005
_refine_ls_restrained_S_all 2.005
_refine_diff_density_max 0.561
_refine_diff_density_min -0.299
_refine_diff_density_rms 0.083
;
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         5206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0548
_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^)+(0.1343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                2841
_reflns_number_total             5206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34840c.txt
_cod_data_source_block           DUT-49(Zn)
_cod_original_cell_volume        102541(20)
_cod_original_sg_symbol_H-M      Fm-3m
_cod_database_code               7108519