Exceeding flexpectations: a combined experimental and computational investigation of structural flexibility in 3-dimensional linker-based metal-organic frameworks.
Smoljan, Courtney S.; Formalik, Filip; Barsoum, Michael L.; Fahy, Kira M.; Gaidimas, Madeleine A.; Son, Florencia A.; Xie, Haomiao; Idrees, Karam B.; Farha, Omar K.; Snurr, Randall Q.; Chemical science 16 (2025) 4831–4841; doi:10.1039/d4sc06360k

data_1573870
_publ_section_title
;
 Exceeding flexpectations: a combined experimental and computational
 investigation of structural flexibility in 3-dimensional linker-based
 metal-organic frameworks.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              4831
_journal_page_last               4841
_journal_paper_doi               10.1039/d4sc06360k
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C7 O5 V'
_chemical_formula_sum            'C7 H2.4 O6.2 V'
_chemical_formula_weight         236.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.342(3)
_cell_length_b                   6.8717(8)
_cell_length_c                   10.284(3)
_cell_measurement_reflns_used    1411
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      69.8770
_cell_measurement_theta_min      5.0570
_cell_volume                     1154.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      111.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -71.00  11.00   0.50   10.00    --  -47.42  79.00  35.00  164
  2  \w    -21.00  54.00   0.50   10.00    --   47.42 -79.00 -89.00  150
  3  \w    -95.00 -69.00   0.50   20.00    -- -106.00  79.00  35.00   52
  4  \w   -174.00 -83.00   0.50   20.00    -- -106.00 -79.00 -89.00  182
  5  \w     72.00  98.00   0.50   20.00    --  113.25 -79.00 -89.00   52
  6  \w    140.00 166.00   0.50   20.00    --  113.25  79.00  35.00   52
  7  \w    -38.00  26.00   0.50   10.00    --  -47.42  37.00-180.00  128
  8  \w    -18.00  14.00   0.50   10.00    --  -47.42  19.00 -60.00   64
  9  \w   -108.00 -83.00   0.50   10.00    --  -47.42-125.00  60.00   50
 10  \w    -19.00  14.00   0.50   10.00    --  -47.42  19.00 -30.00   66
 11  \w   -117.00 -92.00   0.50   10.00    --  -47.42-125.00  30.00   50
 12  \w   -117.00 -85.00   0.50   10.00    --  -47.42   0.00-150.00   64
 13  \w     85.00 112.00   0.50   10.00    --   47.42 125.00-120.00   54
 14  \w    -23.00  36.00   0.50   10.00    --   47.42 -37.00 -30.00  118
 15  \w    -27.00  -2.00   0.50   10.00    --   47.42 -19.00  30.00   50
 16  \w    -64.00 -38.00   0.50   20.00    -- -106.00 125.00 150.00   52
 17  \w   -108.00 -70.00   0.50   20.00    -- -106.00 110.00 -15.66   76
 18  \w    -73.00 -47.00   0.50   20.00    -- -106.00  61.00-180.00   52
 19  \w   -177.00 -89.00   0.50   20.00    -- -106.00 -61.00 -30.00  176
 20  \w   -111.00 -80.00   0.50   20.00    -- -106.00 125.00 150.00   62
 21  \w    -68.00 -43.00   0.50   20.00    -- -106.00 107.00 -88.49   50
 22  \w    -73.00 -34.00   0.50   20.00    -- -106.00  61.00  30.00   78
 23  \w   -173.00 -98.00   0.50   20.00    -- -106.00 -61.00-120.00  150
 24  \w    -65.00 -38.00   0.50   20.00    -- -106.00  61.00-120.00   54
 25  \w   -106.00 -77.00   0.50   20.00    -- -106.00 107.00 -88.49   58
 26  \w   -176.00-107.00   0.50   20.00    -- -106.00 -61.00   0.00  138
 27  \w    -72.00 -43.00   0.50   20.00    -- -106.00  61.00-150.00   58
 28  \w    -66.00 -39.00   0.50   20.00    -- -106.00 110.00 -15.66   54
 29  \w    142.00 177.00   0.50   20.00    --  113.25  77.00 -60.00   70
 30  \w     95.00 130.00   0.50   20.00    --  113.25  77.00 -60.00   70
 31  \w     68.00 106.00   0.50   20.00    --  113.25 -94.00  90.00   76
 32  \w     44.00  71.00   0.50   20.00    --  113.25 -61.00  30.00   54
 33  \w     42.00  71.00   0.50   20.00    --  113.25 -61.00  60.00   58
 34  \w     43.00 106.00   0.50   20.00    --  113.25 -94.00-150.00  126
 35  \w     82.00 111.00   0.50   20.00    --  113.25-125.00  90.00   58
 36  \w     42.00  76.00   0.50   20.00    --  113.25-125.00  90.00   68
 37  \w     57.00  91.00   0.50   20.00    --  113.25 -94.00 -90.00   68
 38  \w     42.00  92.00   0.50   20.00    --  113.25 -94.00 120.00  100
 39  \w    123.00 177.00   0.50   20.00    --  113.25   0.00-180.00  108
 40  \w    102.00 178.00   0.50   20.00    --  113.25  77.00  60.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5436
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.441
_diffrn_reflns_theta_max         67.441
_diffrn_reflns_theta_min         5.081
_exptl_absorpt_coefficient_mu    7.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       needle
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.594
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         594
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.591
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1448
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3655
_refine_ls_wR_factor_ref         0.3719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                493
_reflns_number_total             594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06360k2.cif
_cod_data_source_block           nu-2003
_cod_depositor_comments          'Adding full bibliography for 1573870.cif.'
_cod_original_formula_sum        'C7 H2.40 O6.20 V'
_cod_database_code               1573870
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Restrained distances
 C3-C2 \\sim C3-C2_$3
 with sigma of 0.01
 C3-C2 \\sim C4_$1-C2
 with sigma of 0.01
 C4-C3 \\sim C4_$1-C3
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C4 \\sim C4 \\sim C3 \\sim C4 \\sim C3 \\sim C4: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: C4(0.5) C3(0.25)
;
_shelx_res_checksum              40829
_shelx_fab_checksum              44361
_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
;