Optimised synthesis and further structural diversity of ytterbium benzene-1,4-dicarboxylate MOFs
Chamberlain, Thomas W.; Yasmine,; Coulthard, Claire T.; Clarkson, Guy J.; Degirmenci, Volkan; Krisnandi, Yuni K.; Walton, Richard I.; CrystEngComm 25 (2023) 5629–5640; doi:10.1039/D3CE00865G

data_7247398
_publ_section_title
;
 Optimised synthesis and further structural diversity of ytterbium
 benzene-1,4-dicarboxylate MOFs
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              5629
_journal_page_last               5640
_journal_paper_doi               10.1039/D3CE00865G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C24 H12 O21 Yb5'
_chemical_formula_sum            'C24 H12 O21 Yb5'
_chemical_formula_weight         1501.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-03
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-04-17 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.6081(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.82977(6)
_cell_length_b                   22.43648(14)
_cell_length_c                   13.79565(9)
_cell_measurement_reflns_used    54553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.8480
_cell_measurement_theta_min      3.7440
_cell_volume                     2883.51(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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   -121.00 -68.00   0.50    1.00    --  -48.05-134.00  89.00  106
  2  \w    -93.00 -24.00   0.50    1.00    --  -48.05 135.00 -23.00  138
  3  \w   -121.00 -76.00   0.50    1.00    --  -48.05-135.00 -89.00   90
  4  \w    -93.00 -18.00   0.50    1.00    --  -48.05 134.00 156.00  150
  5  \w     39.00 101.00   0.50    1.00    --   48.05-134.00  89.00  124
  6  \w     40.00 101.00   0.50    1.00    --   48.05-135.00 -89.00  122
  7  \w   -160.00 -94.00   0.50    4.00    --  -91.75-135.00 -89.00  132
  8  \w   -161.00 -68.00   0.50    4.00    --  -91.75-134.00  89.00  186
  9  \w    -93.00 -36.00   0.50    4.00    --  -91.75 135.00 -23.00  114
 10  \w     42.00 118.00   0.50    4.00    --  113.25-134.00  89.00  152
 11  \w     89.00 178.00   0.50    4.00    --  113.25 134.00 156.00  178
 12  \w     89.00 178.00   0.50    4.00    --  113.25 135.00 -23.00  178
 13  \w     54.00 119.00   0.50    4.00    --  113.25-135.00 -89.00  130
 14  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00-180.00  100
 15  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00   0.00  100
 16  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00 -30.00  100
 17  \w   -121.00 -73.00   0.50    1.00    --  -48.05-125.00-180.00   96
 18  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00  90.00  100
 19  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00 -90.00  100
 20  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00 150.00  100
 21  \w    -23.00  27.00   0.50    1.00    --  -48.05  19.00-120.00  100
 22  \w    -50.00 -20.00   0.50    4.00    --  -91.75  45.00-180.00   60
 23  \w    101.00 178.00   0.50    4.00    --  113.25  45.00 -60.00  154
 24  \w     42.00  72.00   0.50    4.00    --  113.25 -61.00  30.00   60
 25  \w    100.00 178.00   0.50    4.00    --  113.25  15.00 150.00  156
 26  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00-150.00  128
 27  \w     42.00 108.00   0.50    4.00    --  113.25-111.00 -87.33  132
 28  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00 -60.00  128
 29  \w     95.00 178.00   0.50    4.00    --  113.25 125.00-150.00  166
 30  \w     42.00  72.00   0.50    4.00    --  113.25 -61.00 -30.00   60
 31  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00 -30.00  128
 32  \w     42.00 111.00   0.50    4.00    --  113.25-125.00 150.00  138
 33  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00 120.00  128
 34  \w    101.00 178.00   0.50    4.00    --  113.25  45.00  60.00  154
 35  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00 150.00  128
 36  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00  30.00  128
 37  \w    101.00 178.00   0.50    4.00    --  113.25  45.00-180.00  154
 38  \w     42.00  72.00   0.50    4.00    --  113.25 -61.00 -60.00   60
 39  \w     42.00 111.00   0.50    4.00    --  113.25-125.00 120.00  138
 40  \w    100.00 178.00   0.50    4.00    --  113.25  15.00 -90.00  156
 41  \w     95.50 178.00   0.50    4.00    --  113.25  77.00 -30.00  165
 42  \w     42.00 111.00   0.50    4.00    --  113.25-125.00 -30.00  138
 43  \w    101.00 178.00   0.50    4.00    --  113.25  45.00  90.00  154
 44  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00-180.00  128
 45  \w     42.00 111.00   0.50    4.00    --  113.25-125.00  90.00  138
 46  \w     42.00  72.00   0.50    4.00    --  113.25 -61.00 120.00   60
 47  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00-120.00  128
 48  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00   0.00  128
 49  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00 -90.00  128
 50  \w     42.00 106.00   0.50    4.00    --  113.25 -94.00  90.00  128
 51  \w     42.00 106.00   0.50    4.00    --  113.25 -98.00 -77.70  128
 52  \w     42.00  72.00   0.50    4.00    --  113.25 -61.00 -90.00   60
 53  \w   -121.00 -25.00   0.50    1.00    --  -48.05 -77.00  30.00  192
 54  \w    -64.50 -25.00   0.50    1.00    --  -48.05 -77.00 -60.00   79
 55  \w   -121.00 -25.00   0.50    1.00    --  -48.05 -77.00 120.00  192
 56  \w   -121.00 -84.00   0.50    1.00    --  -48.05 -77.00-120.00   74
 57  \w   -121.00 -46.00   0.50    1.00    --  -48.05 -77.00   0.00  150
 58  \w    -65.00 -25.00   0.50    1.00    --  -48.05 -77.00-150.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0806476000
_diffrn_orient_matrix_UB_12      0.0369662000
_diffrn_orient_matrix_UB_13      0.0584426000
_diffrn_orient_matrix_UB_21      -0.0504458000
_diffrn_orient_matrix_UB_22      -0.0578737000
_diffrn_orient_matrix_UB_23      0.0380303000
_diffrn_orient_matrix_UB_31      0.1352850000
_diffrn_orient_matrix_UB_32      0.0004754000
_diffrn_orient_matrix_UB_33      0.0949406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            66412
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.186
_diffrn_reflns_theta_min         3.913
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    29.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.306
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    3.459
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.016
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.803
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.000035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0483P)^2^+16.1276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6167
_reflns_number_total             6230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00865g2.cif
_cod_data_source_block           twc3
_cod_depositor_comments
'Adding full bibliography for 7247398--7247400.cif.'
_cod_database_code               7247398
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Yb5'
_chemical_oxdiff_usercomment
'C20 H20 N2 O2 Yb  colourless plate 1783  0.0005 0.08 0.08n Walton'
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.120
_olex2_refinement_description
;
No hydrogens were located on any of the bridging oxides or the carboxylate ligands.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C105(H105), C104(H104), C204(H204), C107(H107), C108(H108), C307(H307),
 C304(H304), C207(H207), C305(H305), C308(H308), C208(H208), C205(H205)
;
_shelx_res_checksum              42641
_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 4.775
_oxdiff_exptl_absorpt_empirical_full_min 0.621