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_7250138
_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
'C24 H4 Cl8 La2 O18, C14 H12 N2, 4(C2 H3 N), 11(H2 O)'
_chemical_formula_sum            'C46 H50 Cl8 La2 N6 O29'
_chemical_formula_weight         1712.34
_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             2025-02-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-17 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                92.5410(10)
_cell_angle_beta                 90.2890(10)
_cell_angle_gamma                101.0080(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0706(2)
_cell_length_b                   13.8311(2)
_cell_length_c                   18.0949(2)
_cell_measurement_reflns_used    35256
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      79.3900
_cell_measurement_theta_min      2.4570
_cell_volume                     3207.56(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.111a 64-bit (release 27-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_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 0.975
_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    -82.00  -2.00   0.50    1.00    --  -48.11 111.00 -61.00  160
  2  \w     24.00  84.00   0.50    1.00    --   48.11-111.00-155.00  120
  3  \w   -158.00 -81.00   0.50    2.50    --  -90.00-111.00-155.00  154
  4  \w    -63.00 -37.00   0.50    2.50    --  -90.00 111.00 -61.00   52
  5  \w     51.00  76.00   0.50    2.50    --  111.50-111.00-155.00   50
  6  \w    129.00 155.00   0.50    2.50    --  111.50 111.00 -61.00   52
  7  \w    -29.00  24.00   0.50    1.00    --  -48.11  19.00 120.00  106
  8  \w    -39.00 -14.00   0.50    1.00    --  -48.11 125.00 150.00   50
  9  \w    -83.00 -49.00   0.50    1.00    --  -48.11 125.00  30.00   68
 10  \w    -29.00  20.00   0.50    1.00    --  -48.11  19.00   0.00   98
 11  \w   -115.00 -89.00   0.50    1.00    --  -48.11 -38.00 -90.00   52
 12  \w   -118.00 -26.00   0.50    1.00    --  -48.11 -77.00-120.00  184
 13  \w    -30.00  25.00   0.50    1.00    --  -48.11  19.00-150.00  110
 14  \w    -84.00 -46.00   0.50    1.00    --  -48.11 125.00 150.00   76
 15  \w      4.00  79.00   0.50    1.00    --   48.11 -99.00   0.00  150
 16  \w    -25.00   0.00   0.50    1.00    --   48.11 -19.00 120.00   50
 17  \w    -50.00 -25.00   0.50    2.50    --  -90.00  45.00  60.00   50
 18  \w   -160.00 -84.00   0.50    2.50    --  -90.00 -58.00 -78.74  152
 19  \w     40.00  66.00   0.50    2.50    --  111.50 -61.00-120.00   52
 20  \w     41.00 103.00   0.50    2.50    --  111.50 -94.00 -30.00  124
 21  \w     79.00 105.00   0.50    2.50    --  111.50 -94.00-120.00   52
 22  \w    106.00 166.00   0.50    2.50    --  111.50  30.00   0.00  120
 23  \w     79.00 105.00   0.50    2.50    --  111.50 -94.00  90.00   52
 24  \w    120.00 173.00   0.50    2.50    --  111.50  15.00 120.00  106
 25  \w     43.00  71.00   0.50    2.50    --  111.50 -61.00   0.00   56
 26  \w    153.00 178.00   0.50    2.50    --  111.50  15.00  30.00   50
 27  \w    101.00 154.00   0.50    2.50    --  111.50  30.00-180.00  106
 28  \w    106.00 147.00   0.50    2.50    --  111.50  15.00 -30.00   82
 29  \w     45.00 109.00   0.50    2.50    --  111.50-125.00 120.00  128
 30  \w     43.00 104.00   0.50    2.50    --  111.50 -94.00 -90.00  122
 31  \w     51.00 107.00   0.50    2.50    --  111.50-103.00-175.00  112
 32  \w     47.00  72.00   0.50    2.50    --  111.50 -94.00   0.00   50
 33  \w     74.00 104.00   0.50    2.50    --  111.50 -94.00   0.00   60
 34  \w     90.00 176.00   0.50    2.50    --  111.50  77.00 -90.00  172
 35  \w     47.00  72.00   0.50    2.50    --  111.50 -94.00 120.00   50
 36  \w     74.00 104.00   0.50    2.50    --  111.50 -94.00 120.00   60
 37  \w     40.00 101.00   0.50    2.50    --  111.50 -94.00-150.00  122
 38  \w     55.00 104.00   0.50    2.50    --  111.50 -94.00 -60.00   98
 39  \w     48.00 110.00   0.50    2.50    --  111.50-125.00  90.00  124
 40  \w    151.00 176.00   0.50    2.50    --  111.50  45.00 -30.00   50
 41  \w     45.00  78.00   0.50    2.50    --  111.50 -77.00   0.00   66
 42  \w    101.00 147.00   0.50    2.50    --  111.50  45.00 -30.00   92
 43  \w     43.00  85.00   0.50    2.50    --  111.50-125.00-180.00   84
 44  \w     41.00  66.00   0.50    2.50    --  111.50 -61.00-150.00   50
 45  \w     42.00  71.00   0.50    2.50    --  111.50 -94.00-180.00   58
 46  \w     77.00 105.00   0.50    2.50    --  111.50 -94.00-180.00   56
 47  \w     97.00 157.00   0.50    2.50    --  111.50 125.00 -30.00  120
 48  \w    116.00 157.00   0.50    2.50    --  111.50  15.00 -90.00   82
 49  \w    105.00 163.00   0.50    2.50    --  111.50  61.00  60.00  116
 50  \w    102.00 175.00   0.50    2.50    --  111.50  45.00-150.00  146
 51  \w     50.00 101.00   0.50    2.50    --  111.50 -77.00-150.00  102
 52  \w     48.00  73.00   0.50    2.50    --  111.50 -77.00  90.00   50
 53  \w     71.00 101.00   0.50    2.50    --  111.50 -94.00  30.00   60
 54  \w    109.00 135.00   0.50    2.50    --  111.50  45.00 120.00   52
 55  \w     41.00  69.00   0.50    2.50    --  111.50 -61.00 -30.00   56
 56  \w     40.00  65.00   0.50    2.50    --  111.50 -61.00  60.00   50
;
_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      0.0995473000
_diffrn_orient_matrix_UB_12      0.0720714000
_diffrn_orient_matrix_UB_13      0.0265484000
_diffrn_orient_matrix_UB_21      -0.0424949000
_diffrn_orient_matrix_UB_22      -0.0000553000
_diffrn_orient_matrix_UB_23      0.0792583000
_diffrn_orient_matrix_UB_31      0.0520101000
_diffrn_orient_matrix_UB_32      -0.0878008000
_diffrn_orient_matrix_UB_33      0.0166547000
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53712
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.765
_diffrn_reflns_theta_min         2.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.001
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (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            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.056
_refine_diff_density_max         2.181
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         13646
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+3.0536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12904
_reflns_number_total             13646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           mpvk-mpf-2-044b_2_1-mask_smrt_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250138
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H50 Cl8 La2 N6 O29'
_chemical_oxdiff_usercomment     'Thin maroon plate'
_shelx_estimated_absorpt_t_max   0.508
_shelx_estimated_absorpt_t_min   0.112
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O19-H19A = O19-H19B
 0.84 with sigma of 0.02
 H19A-H19B
 1.34 with sigma of 0.04
 O50-H50A = O50-H50B
 0.84 with sigma of 0.02
 H50A-H50B
 1.34 with sigma of 0.04
 O79-H79A = O79-H79B
 0.84 with sigma of 0.02
 H79A-H79B
 1.34 with sigma of 0.04
 O80-H80A = O80-H80B
 0.84 with sigma of 0.02
 H80A-H80B
 1.34 with sigma of 0.04
 O81-H81A = O81-H81B
 0.84 with sigma of 0.02
 H81A-H81B
 1.34 with sigma of 0.04
 O82-H82A = O82-H82B
 0.84 with sigma of 0.02
 H82A-H82B
 1.34 with sigma of 0.04
 O83-H83A = O83-H83B
 0.84 with sigma of 0.02
 H83A-H83B
 1.34 with sigma of 0.04
 O84-H84A = O84-H84B
 0.84 with sigma of 0.02
 H84A-H84B
 1.34 with sigma of 0.04
 O85-H85A = O85-H85B
 0.84 with sigma of 0.02
 H85A-H85B
 1.34 with sigma of 0.04
 O86-H86A = O86-H86B
 0.84 with sigma of 0.02
 H86A-H86B
 1.34 with sigma of 0.04
 O87-H87A = O87-H87B
 0.84 with sigma of 0.02
 H87A-H87B
 1.34 with sigma of 0.04
 O88-H88A = O88-H88B
 0.84 with sigma of 0.02
 H88A-H88B
 1.34 with sigma of 0.04
 O89-H89A = O89-H89B
 0.84 with sigma of 0.02
 H89A-H89B
 1.34 with sigma of 0.04
 H79B-O80_$2
 1.92 with sigma of 0.04
 H83B-O38_$1
 2.02 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, N64, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C66(H66A,H66B)
4.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C53(H53), C54(H54), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63)
4.c Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C78(H78A,H78B,
 H78C)
;
_shelx_res_checksum              54493
_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 2.277
_oxdiff_exptl_absorpt_empirical_full_min 0.448