Expanding the Series of Alkali Metal Plumbolyl Complexes to Na and K
Diaz-Rodriguez, Roberto; Kitos, Alexandros; Murugesu, Muralee; Dalton Transactions  (2022) –; doi:10.1039/D2DT02615E

data_7711282
_publ_section_title
;
 Expanding the Series of Alkali Metal Plumbolyl Complexes to Na and K
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02615E
_journal_year                    2022
_chemical_formula_moiety         'C36 H56 K2 O2 Pb Si2'
_chemical_formula_sum            'C36 H56 K2 O2 Pb Si2'
_chemical_formula_weight         862.37
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9365(3)
_cell_length_b                   19.0723(3)
_cell_length_c                   15.3540(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.65
_cell_volume                     4081.11(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50293
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.973
_exptl_absorpt_coefficient_mu    4.424
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       rod
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Alkanes/tetrahydrofuran'
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.190(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8719
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+2.8987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0434
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                6535
_reflns_number_total             8719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02615e2.cif
_cod_data_source_block           1
_cod_database_code               7711282
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.393
_shelx_estimated_absorpt_t_max   0.619
_shelx_res_checksum              45113
_shelx_hkl_checksum              41414