Biporous Metal-Organic Framework with Tunable CO<sub>2</sub>/CH<sub>4</sub> Separation Performance Facilitated by Intrinsic Flexibility.
Gładysiak, Andrzej; Deeg, Kathryn S.; Dovgaliuk, Iurii; Chidambaram, Arunraj; Ordiz, Kaili; Boyd, Peter G.; Moosavi, Seyed Mohamad; Ongari, Daniele; Navarro, Jorge A. R.; Smit, Berend; Stylianou, Kyriakos C.; ACS applied materials & interfaces 10 (2018) 36144–36156; doi:10.1021/acsami.8b13362

data_4515325
_publ_section_title
;
 Biporous Metal-Organic Framework with Tunable
 CO<sub>2</sub>/CH<sub>4</sub> Separation Performance Facilitated by
 Intrinsic Flexibility.
;
_journal_issue                   42
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              36144
_journal_page_last               36156
_journal_paper_doi               10.1021/acsami.8b13362
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.25(C88 H44 Ca4 O20)'
_chemical_formula_sum            'C25 H20 Ca N O6'
_chemical_formula_weight         470.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.88590(11)
_cell_length_b                   20.0624(4)
_cell_length_c                   16.6453(4)
_cell_measurement_reflns_used    6691
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.4030
_cell_measurement_theta_min      2.0480
_cell_volume                     2299.51(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -95.00  140.00   1.0000    1.9977
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000    0.0000 235

  2 omega  -15.00  130.00   1.0000    1.9977
omega____ theta____ kappa____ phi______ frames
    -        0.0000   40.0000    0.0000 145

  3 omega  -80.00   60.00   1.0000    1.9977
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -40.0000    0.0000 140

  4 omega  -90.00   65.00   1.0000    1.9977
omega____ theta____ kappa____ phi______ frames
    -        0.0000   65.0000    0.0000 155
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0434413000
_diffrn_orient_matrix_UB_12      -0.0307612000
_diffrn_orient_matrix_UB_13      0.0120672000
_diffrn_orient_matrix_UB_21      -0.0476447000
_diffrn_orient_matrix_UB_22      -0.0166477000
_diffrn_orient_matrix_UB_23      -0.0324861000
_diffrn_orient_matrix_UB_31      0.0815207000
_diffrn_orient_matrix_UB_32      0.0066858000
_diffrn_orient_matrix_UB_33      -0.0254591000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7153
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14679
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.405
_diffrn_reflns_theta_max         25.405
_diffrn_reflns_theta_min         2.043
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.234
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2064
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.915
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.1024
_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          0.3739
_refine_ls_wR_factor_ref         0.3805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1911
_reflns_number_total             2064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b13362_si_002.cif
_cod_data_source_block           SION-8
_cod_database_code               4515325
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ca C22 H13 O4'
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.962
_reflns_odcompleteness_completeness 95.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.41
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C2, C7, C3A, C4A, C5A, C6A
 with sigma of 0.05
 C2, C7, C3B, C4B, C5B, C6B
 with sigma of 0.1
3. Rigid bond restraints
 C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3A \\sim C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C3B \\sim C4B \\sim C5B \\sim C6B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C3B) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C4B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=1-
 FVAR(1)
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A)
;
_olex2_submission_special_instructions 'No special instructions were received'