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_7250134
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-08
_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                 107.882(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8532(2)
_cell_length_b                   26.2857(4)
_cell_length_c                   10.5597(2)
_cell_measurement_reflns_used    11246
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.7160
_cell_measurement_theta_min      3.3660
_cell_volume                     3131.14(10)
_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  (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 0.997
_diffrn_measured_fraction_theta_max 0.969
_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    -85.00 -13.00   0.50    0.20    --  -54.99 125.00  60.00  144
  2  \w    -77.00 -39.00   0.50    0.20    -- -106.00 111.00 -30.00   76
  3  \w    -81.00 -22.00   0.50    0.20    -- -106.00 111.00-180.00  118
  4  \w    -65.00 -38.00   0.50    0.20    -- -106.00  63.00  30.00   54
  5  \w    -55.00 -29.00   0.50    0.20    -- -106.00  63.00 -60.00   52
  6  \w    -48.00 -23.00   0.50    0.20    -- -106.00  50.00 -90.00   50
  7  \w    -56.00 -26.00   0.50    0.20    -- -106.00  50.00-150.00   60
  8  \w    -50.00 -24.00   0.50    0.20    -- -106.00  50.00-180.00   52
  9  \w    -52.00 -26.00   0.50    0.20    -- -106.00  50.00-120.00   52
 10  \w    -52.00 -26.00   0.50    0.20    -- -106.00  50.00 150.00   52
 11  \w    -19.00  18.00   0.50    0.20    --  -54.99  34.00  59.00   74
 12  \w     49.00  97.00   0.50    0.20    --  109.99-111.00 150.00   96
 13  \w      0.00  32.00   0.50    0.10    --    0.00 -99.00-180.00   64
 14  \w   -109.00   4.00   0.50    0.20    --  -54.99 -34.00 -98.00  226
 15  \w   -111.00 -74.00   0.50    0.20    --  -54.99-125.00  60.00   74
 16  \w   -136.00 -74.00   0.50    0.20    --  -54.99-125.00  30.00  124
 17  \w   -176.00 -47.00   0.50    0.20    -- -106.00 -34.00 -98.00  258
 18  \w   -143.00-112.00   0.50    0.20    --  -54.99 -34.00 -98.00   62
 19  \w   -142.00 -86.00   0.50    0.20    --  -54.99 -99.00 -30.00  112
 20  \w    -83.00 -32.00   0.50    0.10    --    0.00 -34.00 -98.00  102
 21  \w     36.00  62.00   0.50    0.20    --  109.99 -77.00  90.00   52
 22  \w     67.00  93.00   0.50    0.20    --  109.99 -77.00  90.00   52
 23  \w     33.00  71.00   0.50    0.20    --  109.99 -63.00  30.00   76
 24  \w     32.00  61.00   0.50    0.20    --  109.99 -63.00 -30.00   58
 25  \w     32.00  57.00   0.50    0.20    --  109.99 -63.00 -90.00   50
 26  \w     34.00  69.00   0.50    0.20    --  109.99 -63.00-120.00   70
 27  \w     28.00  53.00   0.50    0.20    --  109.99 -50.00-120.00   50
 28  \w     28.00  96.00   0.50    0.20    --  109.99 -77.00 -30.00  136
 29  \w     28.00  53.00   0.50    0.20    --  109.99 -50.00-150.00   50
 30  \w     29.00  56.00   0.50    0.20    --  109.99 -50.00   0.00   54
 31  \w     31.00  57.00   0.50    0.20    --  109.99 -50.00  90.00   52
 32  \w     30.00  56.00   0.50    0.20    --  109.99 -50.00 150.00   52
 33  \w     45.00  70.00   0.50    0.20    --   54.99  35.00  58.00   50
 34  \w     44.00  69.00   0.50    0.20    --   54.99  34.00  59.00   50
 35  \w      5.00  50.00   0.50    0.10    --    0.00  34.00  59.00   90
 36  \w    -37.00  -4.00   0.50    0.10    --    0.00  34.00  59.00   66
 37  \w     65.00 102.00   0.50    0.20    --  109.99  34.00  59.00   74
 38  \w    145.00 173.00   0.50    0.20    --  109.99 111.00 -60.00   56
 39  \w    103.00 161.00   0.50    0.20    --  109.99 111.00 -90.00  116
 40  \w    114.00 140.00   0.50    0.20    --  109.99 111.00 -60.00   52
;
_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      0.0939777000
_diffrn_orient_matrix_UB_12      -0.0239051000
_diffrn_orient_matrix_UB_13      0.1198805000
_diffrn_orient_matrix_UB_21      0.0955217000
_diffrn_orient_matrix_UB_22      0.0088224000
_diffrn_orient_matrix_UB_23      -0.0690687000
_diffrn_orient_matrix_UB_31      0.0265945000
_diffrn_orient_matrix_UB_32      0.0527759000
_diffrn_orient_matrix_UB_33      0.0658631000
_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  0.0457
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19634
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.800
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.105
_exptl_absorpt_correction_T_max  0.548
_exptl_absorpt_correction_T_min  0.214
_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    1.898
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.078
_refine_diff_density_min         -1.790
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+11.3662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5627
_reflns_number_total             5950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           mf-1-15a_1_twin_auto_abs_a_sq
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250134
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H18 Cl5 La N2 O13'
_chemical_oxdiff_usercomment     'Solvent:actone and water'
_shelx_estimated_absorpt_t_max   0.357
_shelx_estimated_absorpt_t_min   0.210
_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
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              58399
_shelx_fab_checksum              26178
_platon_squeeze_void_probe_radius 1.20
_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 1.637
_oxdiff_exptl_absorpt_empirical_full_min 0.651