Large shortening of the lead-lead bond in a diplumbyne upon its one-electron reduction
Queen, Joshua D.; Power, Philip P.; Chemical Communications  (2026) –; doi:10.1039/D6CC00657D

data_7135631
_publ_section_title
;
 Large shortening of the lead-lead bond in a diplumbyne upon its
 one-electron reduction.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7404
_journal_page_last               7407
_journal_paper_doi               10.1039/d6cc00657d
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C72 H98 Pb2 1-, C12 H24 O6 K 1+, 1.25(C4H10O)'
_chemical_formula_sum            'C89 H134.5 K O7.25 Pb2'
_chemical_formula_weight         1773.94
_chemical_properties_physical    Air-sensitive,Heat-sensitive,Light-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2026-03-12 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                75.3410(10)
_cell_angle_beta                 70.5950(10)
_cell_angle_gamma                65.8440(10)
_cell_formula_units_Z            2
_cell_length_a                   15.9819(4)
_cell_length_b                   16.1583(3)
_cell_length_c                   22.8325(5)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      3.03
_cell_volume                     5027.2(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26313
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.334
_diffrn_reflns_theta_min         3.025
_exptl_absorpt_coefficient_mu    7.133
_exptl_absorpt_correction_T_max  0.297
_exptl_absorpt_correction_T_min  0.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1819
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.096
_refine_diff_density_max         2.730
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         17458
_refine_ls_number_restraints     518
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1439P)^2^+8.7516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15033
_reflns_number_total             17458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00657d2.cif
_cod_data_source_block           jq112_sq
_cod_depositor_comments          'Adding full bibliography for 7135631.cif.'
_cod_original_formula_sum        'C89 H134.50 K O7.25 Pb2'
_cod_database_code               7135631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.263
_shelx_estimated_absorpt_t_max   0.548
_exptl_absorpt_special_details
;
Reflections not merged
65515 Corrected reflections written to file cu_JQ112_0m.hkl
Estimated minimum and maximum transmission:  0.1611  0.2973
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r =  1.0900
Lambda/2 correction factor = 0.00150
;
_shelx_res_checksum              82284
_shelx_hkl_checksum              58344
_shelx_fab_checksum              30890