Supercritical Processing as a Route to High Internal Surface Areas and Permanent Microporosity in Metal-Organic Framework Materials
Andrew P. Nelson; Omar K. Farha; Karen L. Mulfort; Joseph T. Hupp; Journal of the American Chemical Society 131 (2009) 458–460; doi:10.1021/ja808853q

data_4103786
_publ_contact_author             'Joseph T. Hupp'
_publ_contact_author_email       j-hupp@northwestern.edu
_publ_section_title
;
 Supercritical Processing as a Route to High Internal Surface Areas and
 Permanent Microporosity in Metal-Organic Framework Materials
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              458
_journal_page_last               460
_journal_paper_doi               10.1021/ja808853q
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C106 H83 N8 O29 Zn4'
_chemical_formula_weight         2194.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 117.409(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.275(4)
_cell_length_b                   25.486(4)
_cell_length_c                   49.521(7)
_cell_measurement_reflns_used    7182
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.29
_cell_volume                     26078(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1842
_diffrn_reflns_av_sigmaI/netI    0.4321
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            241409
_diffrn_reflns_theta_full        28.91
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.9135
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            light
_exptl_crystal_density_diffrn    0.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             4508
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.074
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.563
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         63399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.563
_refine_ls_R_factor_all          0.2194
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                12538
_reflns_number_total             63399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808853q_si_002.cif
_cod_data_source_block           INSERTSTRUCTURENAMEHERE
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4103786