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_7250136
_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         'C15 Cl5 La O10, C12 H12 N2, 3(H2 O)'
_chemical_formula_sum            'C27 H18 Cl5 La N2 O13'
_chemical_formula_weight         894.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-04-17
_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                 108.089(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7957(3)
_cell_length_b                   26.3110(5)
_cell_length_c                   10.5813(3)
_cell_measurement_reflns_used    12510
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.1670
_cell_measurement_theta_min      3.3460
_cell_volume                     3121.67(14)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.987
_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     47.00  81.00   0.50    0.20    --  111.50-125.00  30.00   68
  2  \w     86.00 111.00   0.50    0.20    --  111.50-125.00  30.00   50
  3  \w     34.00  93.00   0.50    0.10    --   48.11-125.00 -30.00  118
  4  \w     41.00  85.00   0.50    0.10    --   48.11-125.00 -90.00   88
  5  \w     43.00 110.00   0.50    0.20    --  111.50-125.00-180.00  134
  6  \w     76.00 106.00   0.50    0.20    --  111.50-102.00 -55.35   60
  7  \w     58.00 107.00   0.50    0.20    --  111.50-125.00   0.00   98
  8  \w     82.00 107.00   0.50    0.20    --  111.50-102.00  30.22   50
  9  \w     46.00  72.00   0.50    0.20    --  111.50-102.00 -55.35   52
 10  \w     43.00  78.00   0.50    0.20    --  111.50-102.00  30.22   70
 11  \w     45.00 100.00   0.50    0.20    --  111.50 -94.00  30.00  110
 12  \w     77.00 106.00   0.50    0.20    --  111.50-103.00  84.75   58
 13  \w     48.00  73.00   0.50    0.20    --  111.50-103.00  84.75   50
 14  \w     58.00 107.00   0.50    0.20    --  111.50-112.00 177.42   98
 15  \w     77.00 102.00   0.50    0.20    --  111.50 -94.00 -30.00   50
 16  \w     42.00  70.00   0.50    0.20    --  111.50 -94.00 -30.00   56
 17  \w     53.00  95.00   0.50    0.20    --  111.50 -94.00 -90.00   84
 18  \w     41.00  67.00   0.50    0.20    --  111.50 -94.00-120.00   52
 19  \w     51.00 105.00   0.50    0.20    --  111.50 -94.00-150.00  108
 20  \w     79.00 105.00   0.50    0.20    --  111.50 -94.00-180.00   52
 21  \w     42.00  73.00   0.50    0.20    --  111.50 -94.00-180.00   62
 22  \w     76.00 102.00   0.50    0.20    --  111.50 -94.00-120.00   52
 23  \w     81.00 106.00   0.50    0.20    --  111.50 -93.00  71.15   50
 24  \w     79.00 104.00   0.50    0.20    --  111.50 -94.00 150.00   50
 25  \w     40.00  66.00   0.50    0.20    --  111.50 -93.00  71.15   52
 26  \w     -1.00  27.00   0.50    0.10    --   48.11 -19.00 -90.00   56
 27  \w     53.00  86.00   0.50    0.20    --  111.50 -77.00  60.00   66
 28  \w     41.00  69.00   0.50    0.20    --  111.50 -77.00  90.00   56
 29  \w     40.00  65.00   0.50    0.20    --  111.50 -61.00  90.00   50
 30  \w     40.00  65.00   0.50    0.20    --  111.50 -61.00  60.00   50
 31  \w     40.00  68.00   0.50    0.20    --  111.50 -61.00-120.00   56
 32  \w     40.00  69.00   0.50    0.20    --  111.50 -77.00-180.00   58
 33  \w     45.00  71.00   0.50    0.20    --  111.50 -61.00-150.00   52
 34  \w     41.00  67.00   0.50    0.20    --  111.50 -61.00 -90.00   52
 35  \w     43.00  71.00   0.50    0.20    --  111.50 -61.00 -60.00   56
 36  \w    102.00 153.00   0.50    0.20    --  111.50  15.00  30.00  102
 37  \w     99.00 146.00   0.50    0.20    --  111.50  61.00  90.00   94
 38  \w    102.00 140.00   0.50    0.20    --  111.50  45.00-120.00   76
 39  \w    101.00 151.00   0.50    0.20    --  111.50  30.00-180.00  100
 40  \w    118.00 144.00   0.50    0.20    --  111.50  61.00-180.00   52
 41  \w    149.00 178.00   0.50    0.20    --  111.50  61.00-180.00   58
 42  \w    149.00 176.00   0.50    0.20    --  111.50  45.00-120.00   54
 43  \w    104.00 177.00   0.50    0.20    --  111.50  30.00-120.00  146
 44  \w    115.00 178.00   0.50    0.20    --  111.50  15.00 -60.00  126
 45  \w    103.00 162.00   0.50    0.20    --  111.50  15.00 -30.00  118
 46  \w    102.00 164.00   0.50    0.20    --  111.50  30.00  60.00  124
 47  \w    109.00 167.00   0.50    0.20    --  111.50  30.00 150.00  116
 48  \w    -68.00  22.00   0.50    0.10    --  -48.11  77.00  90.00  180
 49  \w    -44.00  24.00   0.50    0.10    --  -48.11  38.00  60.00  136
 50  \w    -28.00  23.00   0.50    0.10    --  -48.11  19.00 150.00  102
 51  \w    -51.00 -26.00   0.50    0.20    --  -90.00  45.00 -60.00   50
 52  \w    -41.00  24.00   0.50    0.10    --  -48.11  38.00-180.00  130
 53  \w   -155.00 -86.00   0.50    0.20    --  -90.00 -30.00-150.00  138
 54  \w    -53.00 -13.00   0.50    0.10    --  -48.11 125.00-120.00   80
;
_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      -0.0778618000
_diffrn_orient_matrix_UB_12      0.0279002000
_diffrn_orient_matrix_UB_13      -0.1248101000
_diffrn_orient_matrix_UB_21      0.0862003000
_diffrn_orient_matrix_UB_22      0.0455481000
_diffrn_orient_matrix_UB_23      0.0331674000
_diffrn_orient_matrix_UB_31      0.0734325000
_diffrn_orient_matrix_UB_32      -0.0239763000
_diffrn_orient_matrix_UB_33      -0.0823017000
_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  0.1074
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            45204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.871
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.151
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.325
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.116
_refine_diff_density_min         -2.502
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0656P)^2^+8.2914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5754
_reflns_number_total             6725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           mf-1-15b_2_1-mask_smrt_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250136
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H18 N2 O13 Cl5 La '
_chemical_oxdiff_usercomment     'Purple plate in oil'
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.255
_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 O(H,H) groups
2. Restrained distances
 O45-H45A = O45-H45B
 0.84 with sigma of 0.02
 H45A-H45B
 1.34 with sigma of 0.04
 O46-H46A = O46-H46B
 0.84 with sigma of 0.02
 H46A-H46B
 1.34 with sigma of 0.04
 O47-H47A = O47-H47B
 0.84 with sigma of 0.02
 H47A-H47B
 1.34 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              41576
_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 1.580
_oxdiff_exptl_absorpt_empirical_full_min 0.683