Tin(II) Hydrides as Intermediates in Rearrangements of Tin(II) Alkyl Derivatives.
Wang, Shuai; McCrea-Hendrick, Madison L; Weinstein, Cory M.; Caputo, Christine A.; Hoppe, Elke; Fettinger, James C.; Olmstead, Marilyn M.; Power, Philip P.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b02271

data_4126016
_publ_section_title
;
 Tin(II) Hydrides as Intermediates in Rearrangements of Tin(II) Alkyl
 Derivatives.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b02271
_journal_year                    2017
_chemical_formula_moiety         'C43 H60 Sn'
_chemical_formula_sum            'C43 H60 Sn'
_chemical_formula_weight         695.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 110.392(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.486(2)
_cell_length_b                   9.6854(8)
_cell_length_c                   24.5785(16)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      72.4
_cell_measurement_theta_min      3.9
_cell_volume                     7471.9(9)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'Apex2 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker D8 DUO'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38598
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.728
_diffrn_reflns_theta_min         2.816
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.595
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6589
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+47.5977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6017
_reflns_number_total             6589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02271_si_002.cif
_cod_data_source_block           mmh88
_cod_database_code               4126016
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.457
_shelx_estimated_absorpt_t_max   0.577
_shelx_res_checksum              24407
_shelx_hkl_checksum              21186