A unique magnesium-based 3D MOF with nanoscale cages and temperature dependent selective gas sorption properties.
Huang, Yong-Liang; Gong, Yun-Nan; Jiang, Long; Lu, Tong-Bu; Chemical communications (Cambridge, England) 49 (2013) 1753–1755; doi:10.1039/c3cc38730e

data_7112461
_publ_section_title
;
 A unique magnesium-based 3D MOF with nanoscale cages and temperature
 dependent selective gas sorption properties.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1753
_journal_page_last               1755
_journal_paper_doi               10.1039/c3cc38730e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
;
Mg16(C20H6O8)8(H2O)8(H2O)16(C4H8O2)8 (H2O)13 (C3H7NO)26
;
_chemical_formula_sum            'C270 H368 Mg16 N26 O143'
_chemical_formula_weight         6654.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I 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            6
_cell_length_a                   35.19380(10)
_cell_length_b                   35.19380(10)
_cell_length_c                   35.19380(10)
_cell_measurement_reflns_used    36463
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.1188
_cell_measurement_theta_min      3.0732
_cell_volume                     43591.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5058
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.1188
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            85861
_diffrn_reflns_theta_full        65.22
_diffrn_reflns_theta_max         65.22
_diffrn_reflns_theta_min         7.34
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.7200
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             21036
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
Approximately 40.2% 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 5742 electrons per asymmetric unit,
which were assigned to be 13 water and 26 DMF molecules per unit cell.
The final formula was calculated from the TGA combined
with elemental analysis data.
;
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.000110(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3203
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1712
_refine_ls_R_factor_gt           0.1487
_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^)+(0.0001P)^2^+459.4681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2497
_refine_ls_wR_factor_ref         0.2602
_reflns_number_gt                2348
_reflns_number_total             3203
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7108876
_cod_data_source_file            c3cc38730e.txt
_cod_data_source_block           1
_cod_database_code               7112461