Exceptional Adsorption and Binding of Sulfur Dioxide in a Robust Zirconium-Based Metal-Organic Framework.
Carter, Joseph H.; Han, Xue; Moreau, Florian Y.; da Silva, Ivan; Nevin, Adam; Godfrey, Harry G. W.; Tang, Chiu C.; Yang, Sihai; Schröder, Martin; Journal of the American Chemical Society 140 (2018) 15564–15567; doi:10.1021/jacs.8b08433

data_4133087
_publ_section_title
;
 Exceptional Adsorption and Binding of Sulfur Dioxide in a Robust
 Zirconium-Based Metal-Organic Framework.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15564
_journal_page_last               15567
_journal_paper_doi               10.1021/jacs.8b08433
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.08(C475.2 H248 N21.6 O139.2 Zr24)'
_chemical_formula_sum            'C38.13 H20 N1.73 O11.47 Zr2'
_chemical_formula_weight         868.33
_chemical_name_common            MFM-600
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            12
_cell_length_a                   20.5905(4)
_cell_length_b                   20.5905(4)
_cell_length_c                   66.874(2)
_cell_measurement_reflns_used    8186
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.7600
_cell_measurement_theta_min      2.2380
_cell_volume                     28352.5(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     88.99 245.99   1.00  180.00    --  112.00  73.87  -5.79  157
  2  \w    103.83 217.83   1.00  180.00    --  113.00  73.87-140.79  114
  3  \f    119.22 302.33   1.00  180.01 167.07  95.00  73.87    --   183
  4  \w    -24.56  66.44   1.00   60.00    --  -70.00  73.87 -25.79   91
  5  \f    219.72 330.86   1.00  180.01 165.15 105.00  73.87    --   111
  6  \f     47.04 128.09   1.00   30.00  64.27  40.00  73.87    --    81
  7  \w     58.79 131.79   1.00   30.00    --   15.50  73.87 116.71   73
  8  \w    149.47 228.47   1.00  180.00    --  110.00  73.87 109.21   79
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0694850000
_diffrn_orient_matrix_UB_12      -0.0221572000
_diffrn_orient_matrix_UB_13      -0.0051732000
_diffrn_orient_matrix_UB_21      0.0201109000
_diffrn_orient_matrix_UB_22      0.0090516000
_diffrn_orient_matrix_UB_23      0.0219786000
_diffrn_orient_matrix_UB_31      -0.0192054000
_diffrn_orient_matrix_UB_32      -0.0709088000
_diffrn_orient_matrix_UB_33      0.0044707000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            41406
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        58.934
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         2.25
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.610
_exptl_crystal_description       plate
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.000030(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5370
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1664P)^2^+87.6489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2340
_refine_ls_wR_factor_ref         0.2628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3833
_reflns_number_total             5370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08433_si_001.cif
_cod_data_source_block           xmsfm103j2_sq
_cod_original_cell_volume        28352(1)
_cod_original_sg_symbol_H-M      'I 41/a m d (Origin at -1)'
_cod_database_code               4133087
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zr6 C88 H48 N4 O32'
_cell_oxdiff_angle_alpha         89.881(3)
_cell_oxdiff_angle_beta          89.895(3)
_cell_oxdiff_angle_gamma         90.031(3)
_cell_oxdiff_length_a            20.5824(7)
_cell_oxdiff_length_b            20.5842(8)
_cell_oxdiff_length_c            66.9205(17)
_cell_oxdiff_measurement_reflns_used 8170
_cell_oxdiff_volume              28352(2)
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C19, C0AA, C1AA, C2AA, C3AA, C25, C17
 with sigma of 0.1
 C0AA, C19, O1, O0AA
 with sigma of 0.1
 C3AA, N4, C4AA, C5AA, C6AA, C15
 with sigma of 0.1
 C6AA_$1, C15_$1, C15_$2, C6AA_$2
 with sigma of 0.1
 C15_$3, C7AA_$3, C7AA_$4, C15_$2, C7AA_$2, C7AA_$1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
N1 \\sim C8 \\sim C10 \\sim C9 \\sim H9 \\sim C11 \\sim C12 \\sim H12 \\sim
C6AA \\sim C5AA \\sim H5AA \\sim C15 \\sim C7AA: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: C1AA(0.35) H1AA(0.35) C3AA(0.35) C2AA(0.35) H2AA(0.35) C0AA(0.35)
 C17(0.35) H17(0.35) C25(0.35) H25(0.35) O0AA(0.35) C19(0.35) N4(0.175)
 C6AA(0.175) C5AA(0.35) H5AA(0.35) C4AA(0.35) C15(0.175) C7AA(0.35)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6), C9(H9), C12(H12), C1AA(H1AA), C2AA(H2AA),
 C17(H17), C25(H25), C5AA(H5AA)
;
_shelx_res_checksum              68405
_shelx_hkl_checksum              46781
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.649
_oxdiff_exptl_absorpt_empirical_full_min 0.344