Reductive dehydrocoupling of diphenyltin dihydride with LiAlH<sub>4</sub>: selective synthesis and structures of the first bicyclo[2.2.1]heptastannane-1,4-diide and bicyclo[2.2.2]octastannane-1,4-diide.
Steller, Beate G.; Fischer, Roland C.; Flock, Michaela; Hill, Michael S.; Liptrot, David J.; McMullin, Claire L.; Rajabi, Nasir A.; Tiefling, Kathrin; Wilson, Andrew S. S.; Chemical communications (Cambridge, England) 56 (2020) 336–339; doi:10.1039/c9cc07976a

data_7125630
_publ_section_title
;
 Reductive dehydrocoupling of diphenyltin dihydride with
 LiAlH<sub>4</sub>: selective synthesis and structures of the first
 bicyclo[2.2.1]heptastannane-1,4-diide and
 bicyclo[2.2.2]octastannane-1,4-diide.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              336
_journal_page_last               339
_journal_paper_doi               10.1039/c9cc07976a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C94 H90 Li O8 Sn8'
_chemical_formula_weight         2304.11
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-07-11 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                70.797(2)
_cell_angle_beta                 67.696(2)
_cell_angle_gamma                60.735(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2707(6)
_cell_length_b                   14.2569(6)
_cell_length_c                   31.4766(13)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.67
_cell_volume                     5086.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_l_max       40
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_diffrn_reflns_number            23104
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.421
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             2242
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.011
_platon_squeeze_details
;
;
_refine_diff_density_max         8.437
_refine_diff_density_min         -4.225
_refine_diff_density_rms         0.486
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         23104
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.1291
_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^)+(0.1425P)^2^+208.9215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3265
_refine_ls_wR_factor_ref         0.3742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15660
_reflns_number_total             23104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07976a2.cif
_cod_data_source_block           rf732_sq
_cod_depositor_comments
'Adding full bibliography for 7125626--7125630.cif.'
_cod_database_code               7125630
_shelxl_version_number           2014-3
_shelx_res_checksum              7955
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              35899