Unexpected formation of stannolanes and trigonal bipyramidal tin complexes by radical cyclization reaction
Akio Kamimura; Shingo Ishikawa; Fumiaki Noguchi; Takaaki Moriyama; Masahiro So; Toshihiro Murafuji; Hidemitsu Uno; Chem.Commun. 48 (2012) 6592–; doi:10.1039/c2cc31753b

data_7107937
_publ_section_title
;
 Unexpected formation of stannolanes and trigonal bipyramidal tin
 complexes by radical cyclization reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              6592
_journal_paper_doi               10.1039/c2cc31753b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C30 H41 N O4 S Sn'
_chemical_formula_sum            'C30 H41 N O4 S Sn'
_chemical_formula_weight         630.41
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                82.273(4)
_cell_angle_beta                 80.021(3)
_cell_angle_gamma                89.854(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6061(8)
_cell_length_b                   9.5866(11)
_cell_length_c                   19.364(2)
_cell_measurement_reflns_used    12658
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.19
_cell_volume                     1558.8(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15205
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.950
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 4483 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.023(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     678
_refine_ls_number_reflns         11512
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0711P)^2^+1.6641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                9234
_reflns_number_total             11512
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc31753b.txt
_cod_data_source_block           FN03034O
_cod_database_code               7107937