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_4114037
_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         'C34 H76 N2 O2 Si4 Sn '
_chemical_formula_sum            'C34 H76 N2 O2 Si4 Sn'
_chemical_formula_weight         776.02
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 114.6052(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.219(1)
_cell_length_b                   10.9777(5)
_cell_length_c                   20.4742(5)
_cell_measurement_reflns_used    8639
_cell_measurement_temperature    173.2
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.0
_cell_volume                     4131.8(3)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21066
_diffrn_reflns_theta_max         30.50
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.30
_refine_diff_density_min         -0.58
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     195
_refine_ls_number_reflns         5189
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                5189
_reflns_number_total             5871
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja0356784si20030417_094501.cif
_cod_data_source_block           hm2_stannylene-TEMPO_adduct
_cod_original_cell_volume        4131.7(3)
_cod_original_formula_sum        'C34 H76 N2 O2 Si4 Sn '
_cod_database_code               4114037