Enhancement of Stannylene Character in Stannole Dianion Equivalents Evidenced by NMR and Mössbauer Spectroscopy and Theoretical Studies of Newly Synthesized Silyl-Substituted Dilithiostannoles
Kuwabara, Takuya; Guo, Jing-Dong; Nagase, Shigeru; Minoura, Mao; Herber, Rolfe H.; Saito, Masaichi; Organometallics 33 (2014) 2910–; doi:10.1021/om5003717

data_1516260
_publ_section_title
;
 Enhancement of Stannylene Character in Stannole Dianion Equivalents
 Evidenced by NMR and M\"ossbauer Spectroscopy and Theoretical Studies of
 Newly Synthesized Silyl-Substituted Dilithiostannoles
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2910
_journal_paper_doi               10.1021/om5003717
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C30 H44 Li2 O2 Si2 Sn, C7 H8'
_chemical_formula_sum            'C37 H52 Li2 O2 Si2 Sn'
_chemical_formula_weight         717.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4097(16)
_cell_length_b                   13.856(2)
_cell_length_c                   32.621(6)
_cell_measurement_reflns_used    2318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.26
_cell_measurement_theta_min      2.50
_cell_volume                     3801.2(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_sigmaI/netI    0.1126
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            27616
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                7447
_reflns_number_total             9134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5003717_si_002.cif
_cod_data_source_block           masa564
_cod_depositor_comments
'Adding full bibliography for 1516259--1516261.cif.'
_cod_original_cell_volume        3801.2(12)
_cod_original_formula_sum        'C37 H52 Li2 O2 Si2 Sn '
_cod_database_code               1516260