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_7247400
_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         'C48 H36 O30 Yb4'
_chemical_formula_sum            'C48 H36 O30 Yb4'
_chemical_formula_weight         1784.93
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-10 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.59605(10)
_cell_length_b                   26.1011(3)
_cell_length_c                   37.7873(4)
_cell_measurement_reflns_used    46236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.7850
_cell_measurement_theta_min      4.6680
_cell_volume                     9464.49(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_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 0.989
_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 -24.00 67.00 0.50 4.00 -- 48.05 -67.00 -28.00 182 2 \w -81.00 -19.00 0.50 16.00 -- -91.75 104.00-168.00 124 3 \w -67.00 -19.00 0.50 16.00 -- -91.75 58.00 -41.00 96 4 \w 42.00 82.00 0.50 16.00 -- 113.25 -67.00 -28.00 80 5 \w 98.00 178.00 0.50 16.00 -- 113.25 58.00 -41.00 160 6 \w 42.00 107.00 0.50 16.00 -- 113.25-104.00 91.00 130 7 \w -23.00 27.00 0.50 4.00 -- -48.05 19.00 90.00 100 8 \w -121.00 -73.00 0.50 4.00 -- -48.05-125.00-120.00 96 9 \w -23.00 27.00 0.50 4.00 -- -48.05 19.00-150.00 100 10 \w -121.00 -73.00 0.50 4.00 -- -48.05-125.00 120.00 96 11 \w -121.00 -73.00 0.50 4.00 -- -48.05-125.00 -60.00 96 12 \w 42.00 106.00 0.50 16.00 -- 113.25 -94.00 120.00 128 13 \w 101.00 178.00 0.50 16.00 -- 113.25 30.00 -90.00 154 14 \w 42.00 72.00 0.50 16.00 -- 113.25 -61.00 90.00 60 15 \w 100.00 178.00 0.50 16.00 -- 113.25 15.00-180.00 156 16 \w 42.00 111.00 0.50 16.00 -- 113.25-125.00 60.00 138 17 \w 91.00 178.00 0.50 16.00 -- 113.25 77.00 30.00 174 18 \w 42.00 111.00 0.50 16.00 -- 113.25-125.00 -30.00 138 19 \w 42.00 72.00 0.50 16.00 -- 113.25 -61.00-120.00 60 20 \w 42.00 106.00 0.50 16.00 -- 113.25 -94.00 0.00 128 21 \w 42.00 72.00 0.50 16.00 -- 113.25 -61.00 -60.00 60 22 \w 42.00 72.00 0.50 16.00 -- 113.25 -61.00-180.00 60 23 \w 101.00 178.00 0.50 16.00 -- 113.25 30.00-120.00 154 24 \w 42.00 72.00 0.50 16.00 -- 113.25 -61.00 120.00 60 25 \w -121.00 -66.00 0.50 4.00 -- -48.05 -67.00 -28.00 110 26 \w 29.00 121.00 0.50 4.00 -- 48.05 67.00 105.00 184'
_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      -0.0964459000
_diffrn_orient_matrix_UB_12      -0.0157213000
_diffrn_orient_matrix_UB_13      0.0306828000
_diffrn_orient_matrix_UB_21      -0.0752934000
_diffrn_orient_matrix_UB_22      -0.0381532000
_diffrn_orient_matrix_UB_23      -0.0245784000
_diffrn_orient_matrix_UB_31      0.1038729000
_diffrn_orient_matrix_UB_32      -0.0421764000
_diffrn_orient_matrix_UB_33      0.0105552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            91168
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.858
_diffrn_reflns_theta_min         3.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.41.120a (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    2.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             6752
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         10210
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+38.8240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9349
_reflns_number_total             10210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00865g2.cif
_cod_data_source_block           twc2
_cod_depositor_comments
'Adding full bibliography for 7247398--7247400.cif.'
_cod_original_cell_volume        9464.49(17)
_cod_database_code               7247400
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 O4 Yb'
_chemical_oxdiff_usercomment
'C20 H20 O4 Yb   colourless block   0.002 0.01 0.06     Walton'
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.466
_diffrn_oxdiff_digest_frames
;
01600548f3deb2807a3a90a189243eab020002657d5
;
_diffrn_oxdiff_digest_hkl
;
01daf59caa97d626bb9b7bb83678ba8084eb83
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.08
_olex2_refinement_description
;
The hydrogens were located on the coordinated 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,H,H,H,H,H,H,H,H,H,H) groups
2. Restrained distances
 O10-H10A = O10-H10B = O30-H30A = O30-H30B = O40-H40A = O40-H40B = O41-H41A =
 O41-H41B
 0.85 with sigma of 0.015
 O20-H20A = O20-H20B
 0.85 with sigma of 0.01
 O402_$1-H20A
 2.2 with sigma of 0.02
 O20-H20A = O20-H20B = O31-H31A = O31-H31B
 0.85 with sigma of 0.004
 H20B-O302_$5
 2.4 with sigma of 0.01
 H20A-H20B = H31A-H31B
 1.38 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C107(H107), C108(H108), C204(H204), C205(H205),
 C207(H207), C208(H208), C304(H304), C305(H305), C307(H307), C308(H308),
 C404(H404), C405(H405), C407(H407), C408(H408), C504(H504), C505(H505),
 C507(H507), C508(H508), C604(H604), C605(H605), C607(H607), C608(H608)
;
_shelx_res_checksum              27230
_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 3.023
_oxdiff_exptl_absorpt_empirical_full_min 0.489