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_7125627
_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         'C72 H60 Sn8, 2(C16 H32 Li O8)'
_chemical_formula_sum            'C112 H140 Li2 O18 Sn8'
_chemical_formula_weight         2737.63
_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   geom
_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                 90.276(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.253(2)
_cell_length_b                   14.3128(9)
_cell_length_c                   26.5807(17)
_cell_measurement_reflns_used    9386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.63
_cell_volume                     11129.0(13)
_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 0.996
_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  0.0723
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            96591
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.532
_exptl_absorpt_coefficient_mu    1.827
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker software'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       Block
_exptl_crystal_F_000             5448
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.152
_refine_diff_density_max         3.120
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         24221
_refine_ls_number_restraints     626
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+61.7884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15488
_reflns_number_total             24221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07976a2.cif
_cod_data_source_block           rf729
_cod_depositor_comments
'Adding full bibliography for 7125626--7125630.cif.'
_cod_original_cell_volume        11128.9(13)
_cod_database_code               7125627
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C80A-C79A \\sim C80-C79 \\sim C74-C73 \\sim C74A-C73A \\sim C76A-C75A \\sim
C76-C75 \\sim C78A-C77A 
 C78-C77
 with sigma of 0.005
 O1-C80A \\sim O1-C73A \\sim O2-C74A \\sim O2-C75A \\sim O3-C76A \\sim O3-C77A
\\sim O4-C78A \\sim O4-C79A
 \\sim O1-C80 \\sim O1-C73 \\sim O2-C74 \\sim O2-C75 \\sim O3-C76 \\sim O3-C77
\\sim O4-C78 \\sim O4-C79
 with sigma of 0.005
 O5-C81A \\sim O5-C81 \\sim O5-C88A \\sim O5-C88 \\sim O8-C87A \\sim O8-C87
\\sim O8-C86A \\sim O8-C86 
 O7-C84 \\sim O7-C84A \\sim O7-C85 \\sim O7-C85A \\sim O6-C82 \\sim O6-C82A
\\sim O6-C83 \\sim O6-C83A
 with sigma of 0.005
 C84A-C83A \\sim C84-C83 \\sim C86A-C85A \\sim C86-C85 \\sim C88A-C87A \\sim
C88-C87 \\sim C82A-C81A 
 C82-C81
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim
C76A \\sim C75A \\sim C78A \\sim C77A \\sim C73A \\sim C79A \\sim C74A \\sim
C80A \\sim C88A \\sim C87A \\sim C82A \\sim C81A \\sim C84A \\sim C83A \\sim
C86A \\sim C85A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01
Uanis(C82A) \\sim Ueq, Uanis(C82) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: C73(0.65) H73A(0.65) H73B(0.65) C74(0.65) H74A(0.65) H74B(0.65)
 C75(0.65) H75A(0.65) H75B(0.65) C76(0.65) H76A(0.65) H76B(0.65) C77(0.65)
 H77A(0.65) H77B(0.65) C78(0.65) H78A(0.65) H78B(0.65) C79(0.65) H79A(0.65)
 H79B(0.65) C80(0.65) H80A(0.65) H80B(0.65) C81(0.65) H81A(0.65) H81B(0.65)
 C82(0.65) H82A(0.65) H82B(0.65) C83(0.65) H83A(0.65) H83B(0.65) C84(0.65)
 H84A(0.65) H84B(0.65) C85(0.65) H85A(0.65) H85B(0.65) C86(0.65) H86A(0.65)
 H86B(0.65) C87(0.65) H87A(0.65) H87B(0.65) C88(0.65) H88A(0.65) H88B(0.65)
 C76A(0.35) H76C(0.35) H76D(0.35) C75A(0.35) H75C(0.35) H75D(0.35) C78A(0.35)
 H78C(0.35) H78D(0.35) C77A(0.35) H77C(0.35) H77D(0.35) C73A(0.35) H73C(0.35)
 H73D(0.35) C79A(0.35) H79C(0.35) H79D(0.35) C74A(0.35) H74C(0.35) H74D(0.35)
 C80A(0.35) H80C(0.35) H80D(0.35) C88A(0.35) H88C(0.35) H88D(0.35) C87A(0.35)
 H87C(0.35) H87D(0.35) C82A(0.35) H82C(0.35) H82D(0.35) C81A(0.35) H81C(0.35)
 H81D(0.35) C84A(0.35) H84C(0.35) H84D(0.35) C83A(0.35) H83C(0.35) H83D(0.35)
 C86A(0.35) H86C(0.35) H86D(0.35) C85A(0.35) H85C(0.35) H85D(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B),
  C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,
 H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J),
 C76A(H76C,H76D), C75A(H75C,H75D), C78A(H78C,H78D), C77A(H77C,H77D), C73A(H73C,
 H73D), C79A(H79C,H79D), C74A(H74C,H74D), C80A(H80C,H80D), C88A(H88C,H88D),
 C87A(H87C,H87D), C82A(H82C,H82D), C81A(H81C,H81D), C84A(H84C,H84D), C83A(H83C,
 H83D), C86A(H86C,H86D), C85A(H85C,H85D)
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), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_olex2_submission_special_instructions 'No special instructions were received'