A hydrothermally stable ytterbium metal‒organic framework as a bifunctional solid-acid catalyst for glucose conversion
Burnett, David L.; Oozeerally, Ryan; Pertiwi, Ralentri; Chamberlain, Thomas W.; Cherkasov, Nikolay; Clarkson, Guy J.; Krisnandi, Yuni K.; Degirmenci, Volkan; Walton, Richard I.; Chemical Communications  (2019) –; doi:10.1039/C9CC05364F

data_7124118
_publ_section_title
;
 A hydrothermally stable ytterbium metal--organic framework as a
 bifunctional solid-acid catalyst for glucose conversion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05364F
_journal_year                    2019
_chemical_formula_moiety         'C24 H12 O12 Yb2'
_chemical_formula_sum            'C24 H12 O12 Yb2'
_chemical_formula_weight         838.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2019-01-21 deposited with the CCDC.    2019-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.096(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5182(7)
_cell_length_b                   5.23670(10)
_cell_length_c                   22.1791(7)
_cell_measurement_reflns_used    22930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.7240
_cell_measurement_theta_min      2.8310
_cell_volume                     2263.31(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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    -13.00  86.00   1.00   42.50    --   11.26  38.00  60.00   99
  2  \w    -77.00  99.00   1.00   42.50    --   11.26   0.00   0.00  176
  3  \w    -37.00  62.00   1.00   42.50    --  -12.04  38.00 -90.00   99
  4  \w    -13.00  86.00   1.00   42.50    --   11.26  38.00-180.00   99
  5  \w    -99.00 -53.00   1.00   42.50    --  -12.04 178.00 -90.00   46
  6  \w    -25.00  29.00   1.00   42.50    --  -12.04 -99.00-120.00   54
  7  \w    -86.00 -37.00   1.00   42.50    --  -12.04 153.00  -3.00   49
  8  \w    -99.00 -53.00   1.00   42.50    --  -12.04 178.00-150.00   46
  9  \w    -99.00 -53.00   1.00   42.50    --  -12.04 178.00  60.00   46
 10  \w    -25.00 -19.00   1.00   42.50    --   11.26 -99.00-180.00    6
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0325733000
_diffrn_orient_matrix_UB_12      -0.0339922000
_diffrn_orient_matrix_UB_13      0.0251917000
_diffrn_orient_matrix_UB_21      -0.0153079000
_diffrn_orient_matrix_UB_22      -0.1016251000
_diffrn_orient_matrix_UB_23      0.0100357000
_diffrn_orient_matrix_UB_31      0.0054065000
_diffrn_orient_matrix_UB_32      -0.0829054000
_diffrn_orient_matrix_UB_33      -0.0226072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            18097
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.928
_diffrn_reflns_theta_min         2.766
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.628
_refine_diff_density_min         -1.992
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         18097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16023
_reflns_number_total             18097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05364f2.cif
_cod_data_source_block           db1_twin1_hklf5
_cod_original_cell_volume        2263.30(13)
_cod_database_code               7124118
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H20 N2 O2 Eu'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5321(9)
 0.4679(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C204(H204), C207(H207), C205(H205), C305(H305), C407(H407), C011(H011),
 C405(H405), C208(H208), C408(H408), C018(H018), C304(H304), C404(H404)
;
_shelx_res_checksum              6469
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.668
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 179.9976\% 
 around [0.67 0.00 0.74] (reciprocal) or [0.71 -0.00 0.71] (direct)
;