Some aspects of MOF-74 (Zn2DOBDC) metal–organic framework formation using THF as the solvent
Starodubtseva, Alena A.; Dubrovskiy, Vladislav A.; Malik, Seiilbek D.; Lyssenko, Konstantin A.; Sembayeva, Aliya M.; Morontsev, Aleksandr A.; Galeyeva, Alina K.; Trussov, Ivan A.; CrystEngComm 26 (2024) 6161–6171; doi:10.1039/D4CE00905C

data_7249499
_publ_section_title
;
 Some aspects of MOF-74 (Zn2DOBDC) metal--organic framework formation
 using THF as the solvent
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6161
_journal_page_last               6171
_journal_paper_doi               10.1039/D4CE00905C
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C8 H2 O6 Zn2, 1.5[H2O]'
_chemical_formula_sum            'C8 H5 O7.5 Zn2'
_chemical_formula_weight         351.86
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-08 deposited with the CCDC.	2024-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   22.9353(4)
_cell_length_b                   22.9353(4)
_cell_length_c                   15.9392(3)
_cell_measurement_reflns_used    19917
_cell_measurement_temperature    295.00(10)
_cell_measurement_theta_max      27.9030
_cell_measurement_theta_min      1.7640
_cell_volume                     7261.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.99a 64-bit (release 05-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  20.00   0.50   15.00    --    0.00 -24.00-140.53  142
  2  \w    -51.00  20.00   0.50   15.00    --    0.00 -24.00-140.53  142
  3  \w    -47.00  22.00   0.50   15.00    --    4.00 -25.00 -75.88  138
  4  \w    -47.00  22.00   0.50   15.00    --    4.00 -25.00 179.76  138
  5  \w    -47.00  22.00   0.50   15.00    --    4.00 -25.00-121.51  138
  6  \w    -46.00  19.00   0.50   15.00    --    5.35 -26.00 109.19  130
  7  \w    -46.00  28.00   0.50   15.00    --    5.35 -23.00 143.06  148
  8  \w    -46.00  31.00   0.50   15.00    --    5.35 -22.00-169.10  154
  9  \w    -46.00  28.00   0.50   15.00    --    5.35 -23.00 143.06  148
 10  \w    -46.00  23.00   0.50   15.00    --    5.35 -25.00-168.51  138
 11  \w    -46.00  28.00   0.50   15.00    --    5.35 -23.00  11.45  148
 12  \w    -46.00  23.00   0.50   15.00    --    5.35 -25.00  -4.10  138
 13  \w    -46.00  19.00   0.50   15.00    --    5.35 -26.00 109.19  130
 14  \w    -40.00  28.00   0.50   15.00    --    5.35 -23.00 -51.47  136
 15  \w    -45.00  23.00   0.50   15.00    --    5.35 -25.00 -12.52  136
 16  \w     11.00  52.00   0.50   15.00    --    5.35  58.00  53.99   82
 17  \w    -15.00  31.00   0.50   15.00    --    5.35 -22.00  33.61   92
 18  \w     -5.00  28.00   0.50   15.00    --    5.35 -23.00 -42.07   66
 19  \w    -46.00 -17.00   0.50   15.00    --    5.35 -24.00  78.13   58
 20  \w     -7.00  25.00   0.50   15.00    --    5.35 -24.00  78.13   64
 21  \w    -41.00  -3.00   0.50   15.00    --    5.35 -23.00  11.45   76
 22  \w      3.00  28.00   0.50   15.00    --    5.35 -23.00 122.14   50
 23  \w    -45.00 -13.00   0.50   15.00    --    5.35 -24.00 -97.52   64
 24  \w     -7.00  25.00   0.50   15.00    --    5.35 -24.00 -97.52   64
 25  \w    -44.00  24.00   0.50   15.00    --    5.35 -24.00 119.77  136
 26  \w      8.00  43.00   0.50   15.00    --    5.35  71.00 167.86   70
 27  \w      3.00  42.00   0.50   15.00    --    5.35  83.00   7.91   78
 28  \w     10.00  48.00   0.50   15.00    --    5.35  69.00  70.09   76
 29  \w      7.00  45.00   0.50   15.00    --    5.35  74.00-112.84   76
 30  \w     10.00  47.00   0.50   15.00    --    5.35  67.00 -43.28   74
 31  \w    -34.00   0.00   0.50   15.00    --    5.35 -23.00 122.14   68
 32  \w     11.00  43.00   0.50   15.00    --    5.35  62.00 -73.04   64
 33  \w     13.00  53.00   0.50   15.00    --    5.35  51.00-132.78   80
 34  \w    -45.00 -12.00   0.50   15.00    --    5.35 -23.00 -51.47   66
 35  \w     15.00  55.00   0.50   15.00    --    5.35  42.00   6.21   80
 36  \w      9.00  48.00   0.50   15.00    --    5.35  68.00 112.87   78
 37  \w    -44.00 -18.00   0.50   15.00    --    5.35 -23.00 -42.07   52
 38  \w      4.00  30.00   0.50   15.00    --    5.35 -22.00 150.90   52
 39  \w     12.00  56.00   0.50   15.00    --    5.35  37.00 -62.93   88
 40  \w    -44.00 -18.00   0.50   15.00    --    5.35 -22.00 -66.83   52
 41  \w     -2.00  31.00   0.50   15.00    --    5.35 -22.00 -66.83   66
 42  \w    -16.00  23.00   0.50   15.00    --    5.35 -25.00  71.33   78
 43  \w      7.00  45.00   0.50   15.00    --    5.35  75.00 142.84   76
 44  \w      7.00  44.00   0.50   15.00    --    5.35  73.00-157.85   74
 45  \w    -16.00  19.00   0.50   15.00    --    5.35 -26.00  35.23   70
 46  \w    -45.00 -13.00   0.50   15.00    --    5.35 -22.00 150.90   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0184634000
_diffrn_orient_matrix_UB_12      -0.0356909000
_diffrn_orient_matrix_UB_13      -0.0009979000
_diffrn_orient_matrix_UB_21      -0.0258852000
_diffrn_orient_matrix_UB_22      0.0010193000
_diffrn_orient_matrix_UB_23      -0.0231409000
_diffrn_orient_matrix_UB_31      0.0162603000
_diffrn_orient_matrix_UB_32      0.0003161000
_diffrn_orient_matrix_UB_33      -0.0380048000
_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  0.1554
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            169979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.358
_diffrn_reflns_theta_min         1.776
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (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            'yellowish white'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       plate
_exptl_crystal_F_000             3114
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.757
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         3296
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0724
_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^)+(0.1513P)^2^+17.3124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1974
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3064
_reflns_number_total             3296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00905c2.cif
_cod_data_source_block           s2_18h_exp15_res0p6_scanw0p5_red6
_cod_depositor_comments
'Adding full bibliography for 7249498--7249499.cif.'
_cod_original_cell_volume        7261.2(3)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_original_formula_sum        'C8 H5 O7.50 Zn2'
_cod_database_code               7249499
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Zn2 C8 H2 O6 H2 O'
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(4)
 0.50(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 Zn2B-O2 \\sim Zn2A-O2
 with sigma of 0.02
 Zn2B-O3 \\sim Zn2A-O3
 with sigma of 0.02
4. Restrained planarity
 C5, C6, C1, C2, C3, C4, C7, C8
 with sigma of 0.0001
5. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C8)
Uanis(O2) = Uanis(O1)
Uanis(O5) = Uanis(O3)
Uanis(C4) = Uanis(C1)
Uanis(C3) = Uanis(C6)
Uanis(Zn2A) = Uanis(Zn2B)
Uanis(O4) = Uanis(O6)
Uanis(C2) = Uanis(C5)
6. Others
 Sof(Zn2A)=1-FVAR(1)
 Sof(Zn2B)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              717
_shelx_hkl_checksum              11896
_shelx_fab_checksum              4457
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.872