The effect of viologen counterions on the topologies of La(iii)–tetraoxolene metal–organic frameworks
Feng, Yuying; Hua, Carol; van Koeverden, Martin P.; CrystEngComm 27 (2025) 2559–2569; doi:10.1039/D5CE00026B

data_7250132
_publ_section_title
;
 The effect of viologen counterions on the topologies of
 La(iii)--tetraoxolene metal--organic frameworks
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2559
_journal_page_last               2569
_journal_paper_doi               10.1039/D5CE00026B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C9 H6 F3 La O9, 9(H2 O)'
_chemical_formula_sum            'C9 H24 F3 La O18'
_chemical_formula_weight         616.19
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.5860(3)
_cell_length_b                   14.5860(3)
_cell_length_c                   17.4069(3)
_cell_measurement_reflns_used    2592
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.8660
_cell_measurement_theta_min      3.5670
_cell_volume                     3207.19(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.949
_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     33.00  80.00   0.50    0.40    --  105.30 -73.00 -46.00   94
  2  \w     38.00  65.00   0.50    0.40    --  105.30 -61.00   0.00   54
  3  \w     33.00  61.00   0.50    0.40    --  105.30 -61.00  30.00   56
  4  \w     40.00  66.00   0.50    0.40    --  105.30 -61.00 120.00   52
  5  \w    147.00 173.00   0.50    0.40    --  105.30  30.00  90.00   52
  6  \w     94.00 120.00   0.50    0.40    --  105.30  30.00  90.00   52
  7  \w    -17.00  30.00   0.50    0.20    --   47.26 -19.00 -30.00   94
  8  \w     36.00 107.00   0.50    0.40    --  105.30-103.00 -74.00  142
  9  \w   -107.00 -37.00   0.50    0.20    --  -47.26 -51.00 152.00  140
 10  \w   -154.00 -92.00   0.50    0.40    --  -91.75 -94.00  30.00  124
 11  \w    -49.00 -23.00   0.50    0.40    --  -91.75  45.00   0.00   52
 12  \w    -49.00 -28.00   0.50    0.40    --  -91.75  45.00 120.00   42
;
_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      -0.1073514000
_diffrn_orient_matrix_UB_12      -0.0714561000
_diffrn_orient_matrix_UB_13      0.0392989000
_diffrn_orient_matrix_UB_21      0.0460983000
_diffrn_orient_matrix_UB_22      -0.0629714000
_diffrn_orient_matrix_UB_23      0.0389094000
_diffrn_orient_matrix_UB_31      0.0349414000
_diffrn_orient_matrix_UB_32      0.0759915000
_diffrn_orient_matrix_UB_33      0.0691880000
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3641
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.404
_diffrn_reflns_theta_min         4.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.480
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1419
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+21.4064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1378
_reflns_number_total             1419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           mf-1-32b_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_original_cell_volume        3207.19(14)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7250132
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C9 H24 F3 La O18'
_chemical_oxdiff_usercomment     'solvent:acetone and water'
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.342
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6A = O6-H6B
 0.84 with sigma of 0.02
 H6A-H6B
 1.34 with sigma of 0.04
 O7-H7A = O7-H7B
 0.84 with sigma of 0.02
 H7A-H7B
 1.34 with sigma of 0.04
 O8-H8A = O8-H8B
 0.84 with sigma of 0.02
 H8A-H8B
 1.34 with sigma of 0.04
 O9-H9A = O9-H9B
 0.84 with sigma of 0.02
 H9A-H9B
 1.34 with sigma of 0.04
;
_shelx_res_checksum              45320
_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 1.334
_oxdiff_exptl_absorpt_empirical_full_min 0.821