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_1516261
_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_sum            'C36 H56 Li2 O2 Si2 Sn'
_chemical_formula_weight         709.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.022(2)
_cell_angle_beta                 67.3540(10)
_cell_angle_gamma                75.564(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3909(9)
_cell_length_b                   12.4427(9)
_cell_length_c                   13.7240(10)
_cell_measurement_reflns_used    5048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.30
_cell_volume                     1890.4(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13397
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                7308
_reflns_number_total             8611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5003717_si_002.cif
_cod_data_source_block           mm755
_cod_depositor_comments
'Adding full bibliography for 1516259--1516261.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1516261