Dynamic Behavior and Isomerization Equilibria of Distannenes Synthesized by Tin Hydride/Olefin Insertions: Characterization of the Elusive Monohydrido Bridged Isomer.
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 139 (2017) 6586–6595; doi:10.1021/jacs.7b02269

data_4131265
_publ_section_title
;
 Dynamic Behavior and Isomerization Equilibria of Distannenes Synthesized
 by Tin Hydride/Olefin Insertions: Characterization of the Elusive
 Monohydrido Bridged Isomer.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6586
_journal_page_last               6595
_journal_paper_doi               10.1021/jacs.7b02269
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C78 H111.77 O0.23 Sn2, 2(C7 H8)'
_chemical_formula_sum            'C92 H127.77 O0.23 Sn2'
_chemical_formula_weight         1474.66
_chemical_name_common
;[(Ar*)(3,3-dimethylbutyl)(H/OH)Sn-Sn(Ar*).2toluene
Ar* = C6H3-2,6(2,4,6-i-Pr3C6H3)2
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                84.9379(9)
_cell_angle_beta                 88.9163(9)
_cell_angle_gamma                88.8673(9)
_cell_formula_units_Z            2
_cell_length_a                   11.9437(7)
_cell_length_b                   16.5134(10)
_cell_length_c                   20.8121(13)
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.25
_cell_volume                     4087.4(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.511
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       needle
_exptl_crystal_F_000             1563
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.245
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         18744
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+3.3822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14005
_reflns_number_total             18744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02269_si_002.cif
_cod_data_source_block           vw114
_cod_database_code               4131265
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.856
_shelx_res_checksum              3230
_shelx_hkl_checksum              13973