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_7250140
_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         'Br5 C15 La O10, C12 H12 N2, 3(H2 O)'
_chemical_formula_sum            'C27 H18 Br5 La N2 O13'
_chemical_formula_weight         1116.873
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-24
_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                90
_cell_angle_beta                 108.823(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1099(1)
_cell_length_b                   26.3460(2)
_cell_length_c                   10.5165(1)
_cell_measurement_reflns_used    33130
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.4930
_cell_measurement_theta_min      3.3590
_cell_volume                     3175.82(5)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9673
_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     71.00  96.00   0.50    0.14    --   48.11 161.00 -87.00   50
  2  \w     90.00 115.00   0.50    0.43    --  105.08 161.00 -87.00   50
  3  \w    -26.00  26.00   0.50    0.14    --  -48.11  19.00 -30.00  104
  4  \w    -26.00  21.00   0.50    0.14    --  -48.11  19.00  60.00   94
  5  \w    -27.00  23.00   0.50    0.14    --  -48.11  19.00 150.00  100
  6  \w    112.00 137.00   0.50    0.43    --  105.08 117.00 121.00   50
  7  \w    102.00 160.00   0.50    0.43    --  105.08 125.00 -30.00  116
  8  \w     73.00 103.00   0.50    0.14    --   48.11  38.00  90.00   60
  9  \w     41.00  67.00   0.50    0.43    --  105.08 -77.00  60.00   52
 10  \w     75.00 101.00   0.50    0.43    --  105.08 -77.00  60.00   52
 11  \w     44.00  71.00   0.50    0.43    --  105.08 -61.00  60.00   54
 12  \w     95.00 174.00   0.50    0.43    --  105.08  15.00 -60.00  158
 13  \w    122.00 178.00   0.50    0.43    --  105.08  30.00-150.00  112
 14  \w     65.00  91.00   0.50    0.43    --  105.08 -77.00-180.00   52
 15  \w     37.00 101.00   0.50    0.43    --  105.08 -77.00-150.00  128
 16  \w     38.00  68.00   0.50    0.43    --  105.08 -61.00 -90.00   60
 17  \w     34.00  70.00   0.50    0.43    --  105.08 -61.00 -60.00   72
 18  \w     34.00  59.00   0.50    0.43    --  105.08 -61.00   0.00   50
 19  \w     42.00  71.00   0.50    0.43    --  105.08 -61.00  90.00   58
 20  \w    -11.00  14.00   0.50    0.14    --   48.11 -19.00 120.00   50
 21  \w     36.00  62.00   0.50    0.43    --  105.08 -94.00 -60.00   52
 22  \w     81.00 108.00   0.50    0.14    --   48.11-161.00-117.00   54
 23  \w     65.00 135.00   0.50    0.43    --  105.08-161.00-117.00  140
 24  \w     81.00 112.00   0.50    0.43    --  105.08-125.00 -30.00   62
 25  \w     38.00  64.00   0.50    0.43    --  105.08-125.00 -30.00   52
 26  \w     34.00  59.00   0.50    0.14    --   48.11-117.00  34.00   50
 27  \w     84.00 109.00   0.50    0.43    --  105.08-125.00  90.00   50
 28  \w     85.00 112.00   0.50    0.43    --  105.08-125.00 120.00   54
 29  \w     36.00  62.00   0.50    0.43    --  105.08-125.00 120.00   52
 30  \w     39.00  72.00   0.50    0.43    --  105.08-125.00  90.00   66
 31  \w     65.00  94.00   0.50    0.43    --  105.08-117.00  34.00   58
 32  \w     81.00 106.00   0.50    0.43    --  105.08 -94.00 -60.00   50
 33  \w     81.00 106.00   0.50    0.43    --  105.08 -94.00-150.00   50
 34  \w    -82.00 -12.00   0.50    0.14    --  -48.11 117.00 121.00  140
 35  \w    -79.00 -22.00   0.50    0.43    --  -90.00 117.00 121.00  114
 36  \w    -84.00 -52.00   0.50    0.43    --  -90.00 125.00   0.00   64
 37  \w    -92.00 -66.00   0.50    0.14    --  -48.11 161.00 -87.00   52
 38  \w    -95.00 -70.00   0.50    0.43    --  -90.00 161.00 -87.00   50
 39  \w    -71.00 -18.00   0.50    0.43    --  -90.00  61.00 -30.00  106
 40  \w    -50.00 -19.00   0.50    0.43    --  -90.00  45.00 -90.00   62
 41  \w    -50.00 -18.00   0.50    0.43    --  -90.00  45.00-120.00   64
 42  \w    -45.00 -20.00   0.50    0.43    --  -90.00  45.00 -60.00   50
 43  \w    -50.00 -22.00   0.50    0.43    --  -90.00  45.00 120.00   56
 44  \w    -51.00 -26.00   0.50    0.43    --  -90.00  45.00 150.00   50
 45  \w   -163.00-125.00   0.50    0.43    --  -90.00 -15.00  90.00   76
 46  \w   -105.00 -80.00   0.50    0.43    --  -90.00 -15.00  90.00   50
 47  \w   -116.00 -28.00   0.50    0.14    --  -48.11 -77.00   0.00  176
 48  \w   -129.00-103.00   0.50    0.43    --  -90.00 -45.00 -60.00   52
 49  \w   -161.00-135.00   0.50    0.43    --  -90.00 -45.00 -60.00   52
 50  \w   -161.00 -72.00   0.50    0.43    --  -90.00 -77.00   0.00  178
 51  \w   -112.00 -78.00   0.50    0.43    --  -90.00-117.00  34.00   68
 52  \w   -119.00 -94.00   0.50    0.43    --  -90.00-161.00-117.00   50
 53  \w    -97.00 -49.00   0.50    0.14    --  -48.11-161.00-117.00   96
;
_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      0.0615885000
_diffrn_orient_matrix_UB_12      -0.0123968000
_diffrn_orient_matrix_UB_13      0.1493283000
_diffrn_orient_matrix_UB_21      0.0044237000
_diffrn_orient_matrix_UB_22      -0.0565182000
_diffrn_orient_matrix_UB_23      -0.0356149000
_diffrn_orient_matrix_UB_31      0.1193779000
_diffrn_orient_matrix_UB_32      0.0084835000
_diffrn_orient_matrix_UB_33      -0.0195089000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9673
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            44705
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9673
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.72
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.392
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.153
_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    2.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             2110.207
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.7433
_refine_diff_density_min         -1.7805
_refine_diff_density_rms         0.1426
_refine_ls_d_res_high            0.7921
_refine_ls_d_res_low             13.1730
_refine_ls_goodness_of_fit_ref   1.0592
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    22
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0592
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+10.6129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                6399
_reflns_number_total             6481
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           MF-1-16B_1-mask_smrt_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250140
_chemical_oxdiff_formula         'C27 H18 Br5 La1 N2 O13'
_chemical_oxdiff_usercomment     'Solvent:actone and water'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C43(H43a,H43b), C44(H44a,H44b)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41)
;
_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 1.327
_oxdiff_exptl_absorpt_empirical_full_min 0.773