Chemical lithiation reveals the structures of conjugated tetralithium dicarboxylates.
Griffiths, Kieran; Cook, Chris; Seymour, Valerie R.; Bragg, Ryan J.; Halcovitch, Nathan R.; Griffin, John M.; Chemical communications (Cambridge, England) 61 (2025) 11991–11994; doi:10.1039/d5cc03043a

data_7134789
_publ_section_title
;
 Chemical lithiation reveals the structures of conjugated tetralithium
 dicarboxylates.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11991
_journal_page_last               11994
_journal_paper_doi               10.1039/d5cc03043a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C8 H4 Li4 O4'
_chemical_formula_sum            'C8 H4 Li4 O4'
_chemical_formula_weight         191.87
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-03
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.445(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4602(5)
_cell_length_b                   5.1400(2)
_cell_length_c                   16.5862(9)
_cell_measurement_reflns_used    2365
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.9670
_cell_measurement_theta_min      5.3910
_cell_volume                     711.48(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2282
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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   -115.00 -16.00   1.00    1.00    --  -40.68 -37.00-120.00   99
  2  \w   -113.00 -13.00   1.00    1.00    --  -40.68 -57.00 150.00  100
  3  \w    -87.00  -6.00   1.00    1.00    --  -40.68 125.00-120.00   81
  4  \w     27.00  95.00   1.00    1.00    --   40.68-125.00-180.00   68
  5  \w     39.00 138.00   1.00    1.00    --  112.00 -45.00-180.00   99
  6  \w     39.00 109.00   1.00    1.00    --  112.00-111.00 120.00   70
  7  \w    104.00 178.00   1.00    1.00    --  112.00 111.00 -90.00   74
  8  \w    103.00 178.00   1.00    1.00    --  112.00  77.00-180.00   75
  9  \w     30.00 165.00   1.00    1.00    --  112.00 -15.00 120.00  135
 10  \w    104.00 178.00   1.00    1.00    --  112.00 111.00-120.00   74
 11  \w    104.00 178.00   1.00    1.00    --  112.00 111.00 150.00   74
 12  \w    103.00 178.00   1.00    1.00    --  112.00  77.00 -60.00   75
 13  \w     39.00 138.00   1.00    1.00    --  112.00 -45.00 -30.00   99
 14  \w     61.00 146.00   1.00    1.00    --  112.00 178.00-180.00   85
 15  \w    103.00 178.00   1.00    1.00    --  112.00  77.00-150.00   75
 16  \w   -113.00 -13.00   1.00    1.00    --  -40.68 -57.00  60.00  100
 17  \w    -69.00  32.00   1.00    1.00    --  -40.68  57.00-150.00  101
 18  \w   -113.00 -13.00   1.00    1.00    --  -40.68 -57.00   0.00  100
 19  \w    -65.00  34.00   1.00    1.00    --  -40.68  37.00  30.00   99
 20  \w   -114.00 -60.00   1.00    1.00    --  -40.68-151.00 -60.00   54
 21  \w     39.00 109.00   1.00    1.00    --  112.00-111.00   0.00   70
 22  \w     84.00 178.00   1.00    1.00    --  112.00  30.00 150.00   94
 23  \w     84.00 178.00   1.00    1.00    --  112.00  30.00  30.00   94
 24  \w     39.00 109.00   1.00    1.00    --  112.00-111.00-120.00   70
 25  \w     83.00 178.00   1.00    1.00    --  112.00  61.00  60.00   95
 26  \w     84.00 178.00   1.00    1.00    --  112.00  30.00 -60.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1311124000
_diffrn_orient_matrix_UB_12      0.0611896000
_diffrn_orient_matrix_UB_13      0.0735144000
_diffrn_orient_matrix_UB_21      0.1043655000
_diffrn_orient_matrix_UB_22      0.1208913000
_diffrn_orient_matrix_UB_23      -0.0581383000
_diffrn_orient_matrix_UB_31      -0.0772235000
_diffrn_orient_matrix_UB_32      0.2673299000
_diffrn_orient_matrix_UB_33      0.0094217000
_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  0.0949
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8592
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.561
_diffrn_reflns_theta_min         5.407
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.4238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1135
_reflns_number_total             1491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03043a2.cif
_cod_data_source_block           jg_209_auto
_cod_depositor_comments
'Adding full bibliography for 7134789--7134792.cif.'
_cod_database_code               7134789
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Li H C O'
_chemical_oxdiff_usercomment     'Li Li2BDC'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
;
_shelx_res_checksum              61959
_shelx_hkl_checksum              19366
_olex2_exptl_crystal_mounting_method
'mounted on a Mitegen loop using Paratone-N oil'
_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 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.596