Synthesis and Structure of Pentaorganostannate Having Five Carbon Substituents
Masaichi Saito; Sanae Imaizumi; Tomoyuki Tajima; Kazuya Ishimura; Shigeru Nagase; Journal of the American Chemical Society 129 (2007) 10974–10975; doi:10.1021/ja072478+

data_4111357
_publ_contact_author_address
;
Department of Chemistry, Saitama University,
Shimo-okubo, Sakura-ku, Saitama-city, Saitama, 338-8570 Japan
;
_publ_contact_author_email       masaichi@chem.saitama-u.ac.jp
_publ_contact_author_fax         +81-48-858-9029
_publ_contact_author_name        'Masaichi Saito'
_publ_contact_author_phone       +81-48-858-3700
_publ_section_title
;
 Synthesis and Structure of Pentaorganostannate Having Five Carbon
 Substituents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10974
_journal_page_last               10975
_journal_paper_doi               10.1021/ja072478+
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C12 H14 Li O6, C25 H19 Sn'
_chemical_formula_sum            'C37 H33 Li O6 Sn'
_chemical_formula_weight         699.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.415(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5850(10)
_cell_length_b                   20.8836(17)
_cell_length_c                   15.2368(12)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      26.88
_cell_measurement_theta_min      2.24
_cell_volume                     3600.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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     0.71069
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10560
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 1996
;
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.773
_refine_diff_density_min         -2.226
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+35.5358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                2760
_reflns_number_total             3208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072478rom20070409_095301.cif
_cod_data_source_block           pentamethylstannate
_cod_original_sg_symbol_Hall     -C2yc
_cod_database_code               4111357