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_7124119
_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         'C28 H20 O18 Yb3, H2 O'
_chemical_formula_sum            'C28 H22 O19 Yb3'
_chemical_formula_weight         1181.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                86.7541(12)
_cell_angle_beta                 67.0669(13)
_cell_angle_gamma                72.1561(13)
_cell_formula_units_Z            2
_cell_length_a                   11.34947(16)
_cell_length_b                   11.97590(19)
_cell_length_c                   12.97316(18)
_cell_measurement_reflns_used    29780
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3660
_cell_measurement_theta_min      3.0650
_cell_volume                     1541.85(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.920
_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 -20.00 28.00 1.00 28.00 -- -13.15 -99.00 -60.00 48 2 \w 35.00 103.00 1.00 28.00 -- 14.24 178.00 90.00 68 3 \w -14.00 87.00 1.00 28.00 -- 14.24 57.00-150.00 101 4 \w -60.00 39.00 1.00 28.00 -- 14.24 -37.00-150.00 99 5 \w -62.00 47.00 1.00 28.00 -- 14.24 -77.00 -60.00 109 6 \w -20.00 55.00 1.00 28.00 -- 14.24 -99.00 90.00 75 7 \w -88.00 11.00 1.00 28.00 -- -13.15 -37.00 -90.00 99 8 \w -102.00 -57.00 1.00 28.00 -- -13.15-178.00 30.00 45 9 \w -20.00 28.00 1.00 28.00 -- -13.15 -99.00 30.00 48 10 \w -58.00 42.00 1.00 28.00 -- 14.24 -57.00-180.00 100 11 \w -10.00 89.00 1.00 28.00 -- 14.24 37.00 -60.00 99 12 \w -20.00 55.00 1.00 28.00 -- 14.24 -99.00 150.00 75 13 \w -20.00 55.00 1.00 28.00 -- 14.24 -99.00 0.00 75 14 \w -20.00 5.00 1.00 28.00 -- 14.24 -99.00 -90.00 25 15 \w -10.00 89.00 1.00 28.00 -- 14.24 37.00 120.00 99'
_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      -0.0017796000
_diffrn_orient_matrix_UB_12      -0.0587243000
_diffrn_orient_matrix_UB_13      0.0068260000
_diffrn_orient_matrix_UB_21      -0.0612934000
_diffrn_orient_matrix_UB_22      0.0195891000
_diffrn_orient_matrix_UB_23      0.0477279000
_diffrn_orient_matrix_UB_31      -0.0364958000
_diffrn_orient_matrix_UB_32      0.0076850000
_diffrn_orient_matrix_UB_33      -0.0349003000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51354
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.640
_diffrn_reflns_theta_min         2.563
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43f (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    2.545
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8766
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      28.053
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+1.3052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8167
_reflns_number_total             8766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05364f2.cif
_cod_data_source_block           ymt2
_cod_database_code               7124119
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H20 N2 O2 S Yb'
_chemical_oxdiff_usercomment     yst028
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
There is water (O1) of crystallization and four oxygens bound to Yb ions (O2, O3, O4 and O5). 
Two hydrogen atoms were located on the free water and bound water O3 and O5. Only one hydrogen 
was located on O2 and O4 which are triply bound to Yb ions.
Several DFIX restraints were used in the refinement of the hydrogens on these oxygens and these 
hydrogens were given thermal parameters Uiso 1.5 times the Uequiv of the parent oxygen.
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B = O2-H2 = O4-H4
 0.85 with sigma of 0.0006
 H3B-H3A
 1.4 with sigma of 0.0001
3.a Free rotating group:
 O1(H1A,H1B)
3.b Rotating group:
 O5(H5A,H5B), O3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C4C(H4C), C4D(H4D), C4E(H4E), C5A(H5AA), C5B(H5BA),
 C5C(H5C), C5D(H5D), C5E(H5E), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B)
;
_shelx_res_checksum              15774
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.479