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_7124120
_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         'C14 H17 N2 O9 S Yb'
_chemical_formula_sum            'C14 H17 N2 O9 S Yb'
_chemical_formula_weight         562.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2019-01-21 deposited with the CCDC.    2019-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.35690(19)
_cell_length_b                   14.18712(18)
_cell_length_c                   16.9515(2)
_cell_measurement_reflns_used    19226
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3310
_cell_measurement_theta_min      3.7220
_cell_volume                     3693.23(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.944
_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    -51.00  58.00   1.00   60.00    --  -18.31  77.00 120.00  109
  2  \w   -107.00 -57.00   1.00   60.00    --  -18.31-178.00 150.00   50
  3  \w    -20.00  60.00   1.00   60.00    --   19.24 -99.00  30.00   80
  4  \w    -61.00  60.00   1.00   60.00    --   19.24 -19.00-180.00  121
  5  \w     -9.00  33.00   1.00   60.00    --   19.24  57.00 -30.00   42
  6  \w    -13.00  95.00   1.00   60.00    --   19.24  77.00-180.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388573000
_diffrn_orient_matrix_UB_12      -0.0191559000
_diffrn_orient_matrix_UB_13      0.0159618000
_diffrn_orient_matrix_UB_21      -0.0240501000
_diffrn_orient_matrix_UB_22      0.0381741000
_diffrn_orient_matrix_UB_23      -0.0159801000
_diffrn_orient_matrix_UB_31      -0.0066893000
_diffrn_orient_matrix_UB_32      -0.0259938000
_diffrn_orient_matrix_UB_33      -0.0352236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54685
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.775
_diffrn_reflns_theta_min         3.098
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.228
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    2.023
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6447
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+7.8062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5316
_reflns_number_total             6447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05364f2.cif
_cod_data_source_block           ymt1
_cod_original_cell_volume        3693.22(8)
_cod_database_code               7124120
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C14 H17 N2 O9 S Yb'
_chemical_oxdiff_usercomment     ymt27
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
The methyl groups of one of the DMF molecules (C1B-C5B) is undergoing large thermal motion and 
had large thermal parameters so this DMF was refined with a SIMU restraint.
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1B \\sim C2B \\sim N3B \\sim C3B \\sim C4B: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C4(H4), C5(H5), C7(H7)
3.b Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC), C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,
 H4BC)
;
_shelx_res_checksum              40610
_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 1.551
_oxdiff_exptl_absorpt_empirical_full_min 0.709