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_7134790
_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         'C6 H3 Li2 O2'
_chemical_formula_sum            'C6 H3 Li2 O2'
_chemical_formula_weight         120.96
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   difmap
_audit_creation_date             2025-05-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, 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                 105.758(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7425(5)
_cell_length_b                   5.9515(3)
_cell_length_c                   8.3569(6)
_cell_measurement_reflns_used    3220
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      74.1130
_cell_measurement_theta_min      4.6970
_cell_volume                     466.34(5)
_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 (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_temperature      102.15
_diffrn_detector_area_resol_mean 5.2282
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_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   -120.00   1.00   1.00    5.00    --  -39.93 -19.00-120.00  121
  2  \w      6.00  80.00   1.00    5.00    --   39.93 -99.00 120.00   74
  3  \w    -21.00  73.00   1.00    5.00    --   39.93 -77.00 -90.00   94
  4  \w    104.00 178.00   1.00   20.00    --  107.34 111.00   0.00   74
  5  \w    104.00 178.00   1.00   20.00    --  107.34 111.00-180.00   74
  6  \w     79.00 178.00   1.00   20.00    --  107.34  30.00  30.00   99
  7  \w     25.00 106.00   1.00   20.00    --  107.34 -94.00-150.00   81
  8  \w     35.00 136.00   1.00   20.00    --  107.34 -61.00  30.00  101
  9  \w     34.00 109.00   1.00   20.00    --  107.34-111.00   0.00   75
 10  \w    104.00 178.00   1.00   20.00    --  107.34 111.00 -60.00   74
 11  \w     81.00 178.00   1.00   20.00    --  107.34  45.00-180.00   97
 12  \w   -114.00 -58.00   1.00    5.00    --  -39.93-153.00-136.00   56
 13  \w   -112.00 -12.00   1.00    5.00    --  -39.93 -57.00 150.00  100
 14  \w   -112.00 -12.00   1.00    5.00    --  -39.93 -57.00  30.00  100
 15  \w     78.00 178.00   1.00   20.00    --  107.34  61.00 120.00  100
 16  \w     79.00 178.00   1.00   20.00    --  107.34  30.00 -90.00   99
 17  \w     81.00 178.00   1.00   20.00    --  107.34  45.00 -30.00   97
 18  \w     78.00 178.00   1.00   20.00    --  107.34  61.00-150.00  100
 19  \w    104.00 178.00   1.00   20.00    --  107.34 111.00  30.00   74
 20  \w     81.00 178.00   1.00   20.00    --  107.34  45.00  90.00   97
 21  \w   -112.00 -12.00   1.00    5.00    --  -39.93 -57.00-120.00  100
 22  \w   -112.00 -12.00   1.00    5.00    --  -39.93 -57.00  90.00  100
 23  \w     12.00 112.00   1.00    5.00    --   39.93  57.00  30.00  100
 24  \w     78.00 178.00   1.00   20.00    --  107.34  61.00  30.00  100
 25  \w     25.00 106.00   1.00   20.00    --  107.34 -94.00  30.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5116
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.597
_diffrn_reflns_theta_min         4.716
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69107
_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    1.723
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0996P)^2^+0.2325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                809
_reflns_number_total             931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03043a2.cif
_cod_data_source_block           jg208_auto
_cod_depositor_comments
'Adding full bibliography for 7134789--7134792.cif.'
_cod_database_code               7134790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
;
_shelx_res_checksum              26532
_shelx_hkl_checksum              89578
_olex2_exptl_crystal_mounting_method 'mounted on a Mitegen loop'
_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
;