Preparation and structural characterization of trimethyltin(IV) tropolonate. Investigation of a rare methyl-migrational dismutation in the solution, solid and liquid states.
Deák, Andrea; Király, Péter; Tárkányi, Gábor; Dalton transactions (Cambridge, England : 2003)  (2007) 234–239; doi:10.1039/b613692c

data_7004927
_publ_section_title
;
 Preparation and structural characterization of trimethyltin(IV)
 tropolonate. Investigation of a rare methyl-migrational dismutation in
 the solution, solid and liquid states.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              234
_journal_page_last               239
_journal_paper_doi               10.1039/b613692c
_journal_year                    2007
_chemical_compound_source
'obtained from the melt, from Me3Sn(trop) dismutation'
_chemical_formula_moiety         'C16 H16 O4 Sn'
_chemical_formula_sum            'C16 H16 O4 Sn'
_chemical_formula_weight         390.98
_chemical_name_common            dimethyltin(IV)-bis(tropolonate)
_chemical_name_systematic
;
dimethyltin(IV)-bis(tropolonate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.24(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.732(4)
_cell_length_b                   14.192(6)
_cell_length_c                   10.561(4)
_cell_measurement_reflns_used    11252
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      3.14
_cell_volume                     1591.9(11)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'R Axis Rapid'
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10055
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  0.6933
_exptl_absorpt_correction_T_min  0.5459
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            chunk
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellowish
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0616P)^2^+1.0454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                2242
_reflns_number_total             2750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613692c.txt
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7004927