EPR spectroscopic characterization of persistent germyl-substituted Pb(III)- and Sn(III)-radicals.
Kurzbach, Dennis; Yao, Shenglai; Hinderberger, Dariush; Klinkhammer, Karl W.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 6449–6459; doi:10.1039/c001144d

data_7025480
_publ_section_title
;
 EPR spectroscopic characterization of persistent germyl-substituted
 Pb(III)- and Sn(III)-radicals.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6449
_journal_page_last               6459
_journal_paper_doi               10.1039/c001144d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C51 H129 Ge3 K O6 Pb Si9'
_chemical_formula_weight         1555.41
_chemical_name_common
potassium-tris(tris(trimethylsilyl)germyl)plumbanide
_chemical_name_systematic
;
potassium-tris[tris(trimethylsilyl)germyl]plumbanide
;
_space_group_IT_number           161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.0699(7)
_cell_length_b                   19.0699(7)
_cell_length_c                   38.370(3)
_cell_measurement_temperature    173(2)
_cell_volume                     12084.2(11)
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'Bruker APEX-2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            92116
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    3.413
_exptl_absorpt_correction_T_max  0.3422
_exptl_absorpt_correction_T_min  0.2339
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4836
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.078(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6394
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+29.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                5692
_reflns_number_total             6394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001144d.txt
_cod_data_source_block           kpbge3
_cod_original_cell_volume        12084.4(11)
_cod_database_code               7025480