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_7134791
_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         'C4 H2 Li O2'
_chemical_formula_sum            'C4 H2 Li O2'
_chemical_formula_weight         89.00
_chemical_name_systematic        Li2BDC
_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   geom
_atom_sites_solution_primary     iterative
_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                 93.1870(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.35839(16)
_cell_length_b                   5.13401(12)
_cell_length_c                   8.47960(16)
_cell_measurement_reflns_used    4401
_cell_measurement_temperature    290.8(4)
_cell_measurement_theta_max      75.7460
_cell_measurement_theta_min      5.2110
_cell_volume                     363.314(13)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.8(4)
_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 0.999
_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  36.00   1.00    1.00    --  -39.87  57.00 -60.00  107
  2  \w    -71.00  36.00   1.00    1.00    --  -39.87  57.00-180.00  107
  3  \w     27.00  96.00   1.00    1.00    --   39.87-125.00-180.00   69
  4  \w     28.00 106.00   1.00    1.00    --  113.00 -94.00   0.00   78
  5  \w     31.00 148.00   1.00    1.00    --  113.00 -77.00  90.00  117
  6  \w     79.00 178.00   1.00    1.00    --  113.00  30.00 -30.00   99
  7  \w    103.00 178.00   1.00    1.00    --  113.00  77.00-180.00   75
  8  \w     61.00 146.00   1.00    1.00    --  113.00 178.00 150.00   85
  9  \w     33.00 147.00   1.00    1.00    --  113.00 -30.00-180.00  114
 10  \w    103.00 178.00   1.00    1.00    --  113.00  77.00 -90.00   75
 11  \w    103.00 178.00   1.00    1.00    --  113.00  77.00 150.00   75
 12  \w   -116.00  -9.00   1.00    1.00    --  -39.87 -57.00  30.00  107
 13  \w    -87.00  -6.00   1.00    1.00    --  -39.87 125.00   0.00   81
 14  \w   -116.00  -9.00   1.00    1.00    --  -39.87 -57.00-180.00  107
 15  \w   -116.00  -9.00   1.00    1.00    --  -39.87 -57.00 -90.00  107
 16  \w     81.00 178.00   1.00    1.00    --  113.00  61.00 -90.00   97
 17  \w     36.00 109.00   1.00    1.00    --  113.00-111.00 -60.00   73
 18  \w     81.00 178.00   1.00    1.00    --  113.00  61.00-120.00   97
 19  \w     81.00 178.00   1.00    1.00    --  113.00  61.00 120.00   97
 20  \w     36.00 178.00   1.00    1.00    --  113.00  15.00 120.00  142
 21  \w     81.00 178.00   1.00    1.00    --  113.00  61.00 -30.00   97
 22  \w     79.00 178.00   1.00    1.00    --  113.00  30.00-180.00   99
 23  \w     81.00 178.00   1.00    1.00    --  113.00  61.00   0.00   97
 24  \w   -118.00 -11.00   1.00    1.00    --  -39.87 -37.00  60.00  107
 25  \w   -116.00  -9.00   1.00    1.00    --  -39.87 -57.00 -60.00  107
 26  \w   -116.00  -9.00   1.00    1.00    --  -39.87 -57.00 120.00  107
 27  \w      6.00  82.00   1.00    1.00    --   39.87 -99.00 -31.00   76
 28  \w     81.00 178.00   1.00    1.00    --  113.00  61.00  90.00   97
 29  \w     81.00 178.00   1.00    1.00    --  113.00  61.00-180.00   97
 30  \w     81.00 178.00   1.00    1.00    --  113.00  61.00-150.00   97
 31  \w     28.00 106.00   1.00    1.00    --  113.00 -94.00-180.00   78
 32  \w     81.00 107.00   1.00    1.00    --  113.00  61.00  30.00   26
;
_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      -0.0761872000
_diffrn_orient_matrix_UB_12      -0.0807268000
_diffrn_orient_matrix_UB_13      -0.1622625000
_diffrn_orient_matrix_UB_21      0.1681421000
_diffrn_orient_matrix_UB_22      -0.0354578000
_diffrn_orient_matrix_UB_23      -0.0626293000
_diffrn_orient_matrix_UB_31      0.0006716000
_diffrn_orient_matrix_UB_32      -0.2868227000
_diffrn_orient_matrix_UB_33      0.0534609000
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.881
_diffrn_reflns_theta_min         5.300
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71160
_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            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             180
_exptl_crystal_preparation       oil
_exptl_crystal_recrystallization_method 'H2O / acetone vapour diffusion'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0445P)^2^+0.1026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                738
_reflns_number_total             761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03043a2.cif
_cod_data_source_block           jg200_auto
_cod_depositor_comments
'Adding full bibliography for 7134789--7134792.cif.'
_cod_original_cell_volume        363.315(13)
_cod_database_code               7134791
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Li'
_chemical_oxdiff_usercomment     LiBDC
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              96293
_shelx_hkl_checksum              66227
_olex2_exptl_crystal_mounting_method 'Mitegen loop'
_olex2_submission_original_sample_id JG200_auto
_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 2.076
_oxdiff_exptl_absorpt_empirical_full_min 0.602