Post-synthetic Structural Processing in a Metal-Organic Framework Material as a Mechanism for Exceptional CO2/N2 Selectivity
Witold M. Bloch; Ravichandar Babarao; Matthew R. Hill; Christian J. Doonan; Christopher J. Sumby; Journal of the American Chemical Society 135 (2013) 10441–10448; doi:10.1021/ja4032049

data_4120102
_publ_contact_author_address
;School of Chemistry & Physics
The University of Adelaide
Adelaide
SA 5005
Australia
;
_publ_contact_author_email       christopher.sumby@adelaide.edu.au
_publ_contact_author_fax         '+61 8 83134358'
_publ_contact_author_name        'Christopher Sumby'
_publ_contact_author_phone       '+61 8 83137406'
_publ_section_title
;
 Post-synthetic Structural Processing in a Metal-Organic Framework
 Material as a Mechanism for Exceptional CO2/N2 Selectivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10441
_journal_page_last               10448
_journal_paper_doi               10.1021/ja4032049
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C21 H16 Cu N4 O5'
_chemical_formula_weight         467.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   8.800(3)
_cell_length_b                   20.734(2)
_cell_length_c                   13.110(5)
_cell_measurement_reflns_used    1244
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3613
_cell_measurement_theta_min      2.7821
_cell_volume                     2392.0(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'X-Seed (Barbour, 2003)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -21.00   14.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9401  -99.0000  120.0000 35

  2 omega  -89.00    5.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9401  -37.0000  -30.0000 94

  3 omega  -36.00   -6.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9401  -19.0000 -180.0000 30

  4 omega  -98.00  -34.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9401 -179.0000    0.0000 64

  5 omega  -91.00  -66.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9401  -77.0000 -120.0000 25

  6 omega  -52.00   51.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9401   77.0000  -60.0000 103

;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11882
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            teal
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         2.383
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.548
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2159
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.562
_refine_ls_R_factor_all          0.2551
_refine_ls_R_factor_gt           0.1937
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4670
_refine_ls_wR_factor_ref         0.4948
_reflns_number_gt                1133
_reflns_number_total             2159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4032049_si_002_3.cif
_cod_data_source_block           '[Cu(bcppm)H2O]-heated'
_cod_database_code               4120102