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_7250139
_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
'C12 H2 Cl4 La O9, 0.5(C14 H12 N2), 2(C3 H6 O), H2 O'
_chemical_formula_sum            'C25 H22 Cl4 La N O12'
_chemical_formula_weight         809.168
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                103.513(3)
_cell_angle_beta                 94.393(3)
_cell_angle_gamma                106.749(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7781(4)
_cell_length_b                   11.4423(4)
_cell_length_c                   12.9249(4)
_cell_measurement_reflns_used    11172
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9550
_cell_measurement_theta_min      4.3370
_cell_volume                     1466.26(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.80a 64-bit (release 13-01-2023))'
_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  'olex2.refine 1.5 (Bourhis et al., 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 0.9962
_diffrn_measured_fraction_theta_max 0.9248
_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    -24.00   6.00   0.50    0.20    --   47.26 -60.00 -53.00   60
  2  \w    -22.00   5.00   0.50    0.20    --   47.26 -19.00 -60.00   54
  3  \w     35.00  62.00   0.50    0.20    --   47.26 -60.00 -53.00   54
  4  \w     57.00 106.00   0.50    0.40    --  105.30-125.00  30.00   98
  5  \w     84.00 110.00   0.50    0.40    --  105.30-125.00   0.00   52
  6  \w     40.00 110.00   0.50    0.40    --  105.30-125.00 -30.00  140
  7  \w     39.00 108.00   0.50    0.40    --  105.30-106.00-131.44  138
  8  \w     34.00  79.00   0.50    0.40    --  105.30 -94.00-180.00   90
  9  \w     36.00  67.00   0.50    0.40    --  105.30-125.00-180.00   62
 10  \w     34.00  81.00   0.50    0.20    --   47.26-125.00 -60.00   94
 11  \w     83.00 109.00   0.50    0.40    --  105.30-125.00-180.00   52
 12  \w     59.00 106.00   0.50    0.40    --  105.30-105.00 171.31   94
 13  \w     54.00 101.00   0.50    0.40    --  105.30 -94.00  60.00   94
 14  \w     74.00 105.00   0.50    0.40    --  105.30 -94.00   0.00   62
 15  \w     33.00  70.00   0.50    0.40    --  105.30 -61.00 -60.00   74
 16  \w     36.00  68.00   0.50    0.40    --  105.30 -60.00 -53.00   64
 17  \w    107.00 134.00   0.50    0.40    --  105.30  30.00-120.00   54
 18  \w    137.00 165.00   0.50    0.40    --  105.30  30.00-120.00   56
 19  \w     40.00  70.00   0.50    0.40    --  105.30 -61.00  90.00   60
 20  \w    101.00 174.00   0.50    0.40    --  105.30  60.00  85.00  146
 21  \w     32.00 117.00   0.50    0.20    --   47.26  60.00  85.00  170
 22  \w    -32.00  -7.00   0.50    0.20    --  -47.26  60.00  85.00   50
 23  \w    -62.00 -37.00   0.50    0.20    --  -47.26  60.00  85.00   50
 24  \w    -64.00 -21.00   0.50    0.40    --  -91.75  61.00 150.00   86
 25  \w    -29.00  27.00   0.50    0.20    --  -47.26  19.00-120.00  112
 26  \w    -66.00 -41.00   0.50    0.40    --  -91.75  61.00 -90.00   50
 27  \w    -48.00 -23.00   0.50    0.40    --  -91.75  45.00 -60.00   50
 28  \w    -69.00 -20.00   0.50    0.40    --  -91.75  60.00  85.00   98
 29  \w    -50.00 -21.00   0.50    0.40    --  -91.75  45.00  90.00   58
 30  \w   -120.00 -35.00   0.50    0.20    --  -47.26 -38.00  90.00  170
 31  \w    -62.00 -27.00   0.50    0.40    --  -91.75 125.00 -90.00   70
 32  \w    -83.00 -23.00   0.50    0.40    --  -91.75 125.00-150.00  120
 33  \w   -119.00 -38.00   0.50    0.20    --  -47.26 -60.00 -53.00  162
 34  \w   -162.00-109.00   0.50    0.40    --  -91.75 -60.00 -53.00  106
 35  \w   -159.00-126.00   0.50    0.40    --  -91.75 -45.00-150.00   66
 36  \w   -121.00 -88.00   0.50    0.40    --  -91.75 -45.00-150.00   66
 37  \w   -111.00 -83.00   0.50    0.40    --  -91.75 -15.00-180.00   56
 38  \w   -166.00-140.00   0.50    0.40    --  -91.75 -15.00-180.00   52
 39  \w   -163.00 -80.00   0.50    0.40    --  -91.75 -45.00   0.00  166
 40  \w   -154.00 -90.00   0.50    0.40    --  -91.75 -94.00  60.00  128
;
_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      -0.1157123000
_diffrn_orient_matrix_UB_12      -0.0939891000
_diffrn_orient_matrix_UB_13      -0.0844560000
_diffrn_orient_matrix_UB_21      0.0792772000
_diffrn_orient_matrix_UB_22      -0.0930550000
_diffrn_orient_matrix_UB_23      -0.0247818000
_diffrn_orient_matrix_UB_31      -0.0561431000
_diffrn_orient_matrix_UB_32      -0.0616759000
_diffrn_orient_matrix_UB_33      0.0874557000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.9962
_diffrn_reflns_Laue_measured_fraction_max 0.9248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17670
_diffrn_reflns_point_group_measured_fraction_full 0.9962
_diffrn_reflns_point_group_measured_fraction_max 0.9248
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.92
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.186
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.362
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       prism
_exptl_crystal_F_000             800.000
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.7369
_refine_diff_density_min         -1.7232
_refine_diff_density_rms         0.1388
_refine_ls_d_res_high            0.7915
_refine_ls_d_res_low             12.4160
_refine_ls_goodness_of_fit_ref   1.0331
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5739
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.0206
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.2416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5383
_reflns_number_total             5739
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           MF-1-33B_1-mask_avg_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250139
_chemical_oxdiff_formula         'C25 H22 Cl4 La N O12'
_chemical_oxdiff_usercomment     'solvent:acetone and water'
_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
 C35-C36
 1.35 with sigma of 0.02
 C28-C35 = C36-C37
 1.43 with sigma of 0.02
 C32-C33
 1.51 with sigma of 0.02
 N30-C32 = N34-C33
 1.48 with sigma of 0.02
 O25-H25a = O25-H25b
 0.84 with sigma of 0.02
 H25a-H25b
 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
 C27-H27 = C31-H31
 0.95 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C29 \\sim C31 \\sim C28 \\sim C33 \\sim N34 \\sim N30 \\sim
C37 \\sim C32 \\sim C36 \\sim C35: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C28) = Uanis(N34)
Uanis(C33) = Uanis(C35)
Uanis(N30) = Uanis(C37)
Uanis(C32) = Uanis(C36)
4. Rigid body (RIGU) restrains
 C39, C40, O38, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C29, C31, C28, C33, N34, N30, C37, C32, C36, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C28(0.5) C33(0.5) H33a(0.5) H33b(0.5) N34(0.5) N30(0.5) C37(0.5)
 C32(0.5) H32a(0.5) H32b(0.5) C36(0.5) H36(0.5) C35(0.5) H35(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C33(H33a,H33b), C32(H32a,H32b)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C36(H36), C35(H35)
6.c Idealised Me refined as rotating group:
 C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C45(H45a,H45b,
 H45c)
;
_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 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.728