Addition of Stable Nitroxide Radical to Stable Divalent Compounds of Heavier Group 14 Elements
Takeaki Iwamoto; Hidenori Masuda; Shintaro Ishida; Chizuko Kabuto; Mitsuo Kira; Journal of the American Chemical Society 125 (2003) 9300–9301; doi:10.1021/ja0356784

data_4114036
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science,
Tohoku University, Aoba-ku, Sendai 980-8578, Japan
;
_publ_contact_author_email       mkira@si.chem.tohoku.ac.jp
_publ_contact_author_fax         +81-22-217-6589
_publ_contact_author_name        ' MITSUO KIRA'
_publ_contact_author_phone       +81-22-217-6585
_publ_section_title
;
 Addition of Stable Nitroxide Radical to Stable Divalent Compounds of
 Heavier Group 14 Elements
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9300
_journal_page_last               9301
_journal_paper_doi               10.1021/ja0356784
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C40 H82 Ge N2 O2 Si4 '
_chemical_formula_sum            'C40 H82 Ge N2 O2 Si4'
_chemical_formula_weight         808.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.798(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4137(5)
_cell_length_b                   18.2468(11)
_cell_length_c                   22.1105(8)
_cell_measurement_reflns_used    21579
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      0.9
_cell_volume                     4572.4(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36422
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         9197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                5878
_reflns_number_total             9197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0356784si20030417_094421.cif
_cod_data_source_block           GermyleneTEMPOadduct
_cod_original_formula_sum        'C40 H82 Ge N2 O2 Si4 '
_cod_database_code               4114036