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_7125629
_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_moiety         'C6 H8 Al, C16 H32 Li O8'
_chemical_formula_sum            'C22 H40 Al Li O8'
_chemical_formula_weight         466.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-11 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.856(11)
_cell_length_b                   14.196(10)
_cell_length_c                   23.825(16)
_cell_measurement_reflns_used    8987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.006
_cell_measurement_theta_min      1.709
_cell_volume                     5025(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            149530
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         28.006
_diffrn_reflns_theta_min         1.709
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       Block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.159
_refine_diff_density_max         1.462
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0576P)^2^+15.2709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4602
_reflns_number_total             6067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07976a2.cif
_cod_data_source_block           rf258_fin
_cod_depositor_comments
'Adding full bibliography for 7125626--7125630.cif.'
_cod_original_cell_volume        5024(6)
_cod_database_code               7125629
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'