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_7125628
_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         'C12 H26 Li O6, C18 H16 Al'
_chemical_formula_sum            'C30 H42 Al Li O6'
_chemical_formula_weight         532.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 106.3590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8667(4)
_cell_length_b                   20.5281(8)
_cell_length_c                   12.5639(5)
_cell_measurement_reflns_used    5511
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.61
_cell_volume                     2936.67(19)
_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      100.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14532
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       Block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0713P)^2^+1.5137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4290
_reflns_number_total             5737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07976a2.cif
_cod_data_source_block           rf224_0m
_cod_depositor_comments
'Adding full bibliography for 7125626--7125630.cif.'
_cod_database_code               7125628
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C25 \\sim O4A-C25 \\sim O3-C23A \\sim O3-C23
 with sigma of 0.005
 C24-C23 \\sim C24A-C23A
 with sigma of 0.005
 O6-C30 \\sim O6A-C30A \\sim O5A-C27A \\sim O5-C27
 with sigma of 0.005
 O5A-C28A \\sim O5-C28 \\sim O6A-C29A \\sim O6-C29
 with sigma of 0.005
 C29-C28 \\sim C29A-C28A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24)
Uanis(O4A) = Uanis(O4)
Uanis(C23A) = Uanis(C23)
Uanis(O6A) = Uanis(O6)
Uanis(C30) = Uanis(C30A)
Uanis(C29A) = Uanis(C29)
Uanis(C28) = Uanis(C28A)
Uanis(C27A) = Uanis(C27)
Uanis(O5A) = Uanis(O5)
4. Others
 Fixed Sof: O4(0.8) O5(0.8) O6(0.8) O4A(0.2) O5A(0.2) O6A(0.2) H25A(0.8)
 H25B(0.8) H25C(0.2) H25D(0.2) C23(0.8) H23A(0.8) H23B(0.8) C24(0.8) H24A(0.8)
 H24B(0.8) C27(0.8) H27A(0.8) H27B(0.8) H27C(0.8) C28(0.8) H28A(0.8) H28B(0.8)
 C29(0.8) H29A(0.8) H29B(0.8) C30(0.8) H30A(0.8) H30B(0.8) H30C(0.8) C23A(0.2)
 H23C(0.2) H23D(0.2) C24A(0.2) H24C(0.2) H24D(0.2) C27A(0.2) H27D(0.2)
 H27E(0.2) H27F(0.2) C28A(0.2) H28C(0.2) H28D(0.2) C29A(0.2) H29C(0.2)
 H29D(0.2) C30A(0.2) H30D(0.2) H30E(0.2) H30F(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C25(H25A,
 H25B), C25(H25C,H25D), C26(H26A,H26B), C23(H23A,H23B), C24(H24A,H24B),
 C28(H28A,H28B), C29(H29A,H29B), C23A(H23C,H23D), C24A(H24C,H24D), C28A(H28C,
 H28D), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C27A(H27D,H27E,H27F), C30A(H30D,
 H30E,H30F)
;
_olex2_submission_special_instructions 'No special instructions were received'