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_7235797
_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         'C15 H12 N O4 Zn'
_chemical_formula_sum            'C15 H12 N O4 Zn'
_chemical_formula_weight         335.65
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.052(5)
_cell_length_b                   21.172(5)
_cell_length_c                   9.625(5)
_cell_measurement_reflns_used    5646
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     3271(2)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_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.
  PLATON for Windows -- 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      153(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12121
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
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    0.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1650
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0720
_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^)+(0.1181P)^2^+16.8721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2116
_refine_ls_wR_factor_ref         0.2145
_reflns_number_gt                1332
_reflns_number_total             1650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ta04393f2.cif
_cod_data_source_block           MOF649_ccdc922544
_cod_database_code               7235797