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_7247399
_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         'C12 H12 O9 Yb'
_chemical_formula_sum            'C12 H12 O9 Yb'
_chemical_formula_weight         473.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-05
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-07-10 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                68.823(4)
_cell_angle_beta                 70.748(3)
_cell_angle_gamma                74.995(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7973(3)
_cell_length_b                   9.4775(4)
_cell_length_c                   10.6851(4)
_cell_measurement_reflns_used    21841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0850
_cell_measurement_theta_min      2.8060
_cell_volume                     686.30(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (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 0.999
_diffrn_measured_fraction_theta_max 0.893
_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    -23.00   2.35   0.65    1.81    --    9.17 -99.00-150.00   39
  2  \w     31.00  76.50   0.65    1.81    --    9.17-161.00-162.00   70
  3  \w      2.00  81.30   0.65    1.81    --    9.17  37.00-150.00  122
  4  \w     11.00  52.60   0.65    1.81    --    9.17-122.00  21.65   64
  5  \w    -63.00  29.30   0.65    1.81    --    9.17 -77.00  90.00  142
  6  \w      2.00  81.30   0.65    1.81    --    9.17  37.00  90.00  122
  7  \w    -31.00  21.00   0.65    1.81    --   -8.70  80.00 -68.60   80
  8  \w    -16.00  64.60   0.65    1.81    --   -8.70  19.00-180.00  124
  9  \w    -21.00  61.55   0.65    1.81    --   -8.70  57.00 -90.00  127
 10  \w    -29.00  62.00   0.65    1.81    --   -8.70  77.00  60.00  140
 11  \w    -41.00  -4.60   0.65    1.81    --   -8.70 101.00 115.00   56
 12  \w    -42.00 -14.70   0.65    1.81    --   -8.70 103.00 163.99   42
 13  \w    -42.00 -14.70   0.65    1.81    --   -8.70 103.00  77.57   42
 14  \w    -41.00  -4.60   0.65    1.81    --   -8.70 101.00   7.11   56
 15  \w    -42.00 -14.70   0.65    1.81    --   -8.70 103.00 -33.13   42
 16  \w    -42.00 -14.70   0.65    1.81    --   -8.70 103.00-123.85   42
 17  \w    -42.00  -7.55   0.65    1.81    --   -8.70 102.00-146.05   53
 18  \w    -80.00  11.00   0.65    1.81    --   -8.70 -77.00 150.00  140
 19  \w    -23.00  22.50   0.65    1.81    --   -8.70 -99.00  30.00   70
 20  \w    -23.00  22.50   0.65    1.81    --   -8.70 -99.00 -30.00   70
 21  \w    -23.00  22.50   0.65    1.81    --   -8.70 -99.00 -90.00   70
 22  \w    -23.00  22.50   0.65    1.81    --   -8.70 -99.00-120.00   70
;
_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      -0.0301435000
_diffrn_orient_matrix_UB_12      0.0339135000
_diffrn_orient_matrix_UB_13      -0.0616962000
_diffrn_orient_matrix_UB_21      0.0879050000
_diffrn_orient_matrix_UB_22      -0.0261377000
_diffrn_orient_matrix_UB_23      -0.0389959000
_diffrn_orient_matrix_UB_31      -0.0298110000
_diffrn_orient_matrix_UB_32      -0.0691023000
_diffrn_orient_matrix_UB_33      0.0107262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30267
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.980
_diffrn_reflns_theta_min         2.334
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
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    2.290
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0261P)^2^+0.0769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4352
_reflns_number_total             4604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00865g2.cif
_cod_data_source_block           rw37
_cod_depositor_comments
'Adding full bibliography for 7247398--7247400.cif.'
_cod_database_code               7247399
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Yb'
_chemical_oxdiff_usercomment
'C20 H20 N2 O2 Yb  colourless bl;ock 0.04 0.1 0.14    Walton'
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.447
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_refinement_description
;
The phenylene ring of terephthalic acid O1 to O15 was modelled as disordered by a small rotation
around its long axis. The occupancy of the two components was linked to a free variable which 
refined to 50:50.  The hydrogens were located in a difference map on the bound waters and refined 
with restraints. 

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C8A)=Sof(H8A)=Sof(C7A)=Sof(H7A)=1-
 FVAR(1)
 Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C8)=Sof(H8)=Sof(C7)=Sof(H7)=FVAR(1)
3.a Free rotating group:
 O16(H16A,H16B)
3.b Rotating group:
 O17(H17A,H17B), O18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C8(H8), C7(H7), C5A(H5A), C4A(H4A), C8A(H8A), C7A(H7A),
 C15(H15), C14(H14)
;
_shelx_res_checksum              37951
_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 1.528
_oxdiff_exptl_absorpt_empirical_full_min 0.808