Synthesis and hydrogen adsorption properties of internally polarized 2,6-azulenedicarboxylate based metal‒organic frameworks
Barman, Samir; Khutia, Anupam; Koitz, Ralph; Blacque, Olivier; Furukawa, Hiroyasu; Iannuzzi, Marcella; Yaghi, Omar M.; Janiak, Christoph; Hutter, Jürg; Berke, Heinz; J. Mater. Chem. A 2 (2014) 18823–; doi:10.1039/C4TA04393F

data_7235796
_publ_section_title
;
 Synthesis and hydrogen adsorption properties of internally polarized
 2,6-azulenedicarboxylate based metal--organic frameworks
;
_journal_issue                   44
_journal_name_full               'J. Mater. Chem. A'
_journal_page_first              18823
_journal_paper_doi               10.1039/C4TA04393F
_journal_volume                  2
_journal_year                    2014
_chemical_formula_moiety
' 4(C36 H18 O13 Zn4), 4(C3 H7 N O), 4(C5 H9 N O), 13(H2 O)'
_chemical_formula_sum            'C320 H234 N8 O125 Zn32'
_chemical_formula_weight         8282.98
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_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-2013
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   30.5557(17)
_cell_length_b                   30.5557(17)
_cell_length_c                   30.5557(17)
_cell_measurement_reflns_used    709
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.7
_cell_volume                     28528(3)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_molecular_graphics
; ORTEP-3 for Windows.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX -- Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97 -- Sheldrick, G. M (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
  SQUEEZE/PLATON -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1979
_diffrn_reflns_av_sigmaI/netI    0.1335
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13859
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.35.11 (Oxford Diffraction, 2010)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    0.482
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4170
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The unit cell contains 4 DMF, 4 NMP and 13 water solvent molecules (3920
 electrons) which have been treated as a diffuse contribution to the overall
 scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         1353
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.2245
_refine_ls_R_factor_gt           0.1443
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3390
_refine_ls_wR_factor_ref         0.3752
_reflns_number_gt                744
_reflns_number_total             1353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ta04393f2.cif
_cod_data_source_block           MOF650_ccdc922543
_cod_database_code               7235796