Disproportionation of Sn(II){CH(SiMe<sub>3</sub>)<sub>2</sub>}<sub>2</sub> to ˙Sn(III){CH(SiMe<sub>3</sub>)<sub>2</sub>}<sub>3</sub> and ˙Sn(I){CH(SiMe<sub>3</sub>)<sub>2</sub>}: characterization of the Sn(I) product.
Mears, Kristian L.; Ruiz, Bronson; Nguyen, Gia-Ann; Zou, Wenxing; Fettinger, James C.; Power, Philip P.; Chemical communications (Cambridge, England) 59 (2023) 6399–6402; doi:10.1039/d3cc01542d

data_7131604
_publ_section_title
;
 Disproportionation of
 Sn(II){CH(SiMe<sub>3</sub>)<sub>2</sub>}<sub>2</sub> to
 &#x2d9;Sn(III){CH(SiMe<sub>3</sub>)<sub>2</sub>}<sub>3</sub> and
 &#x2d9;Sn(I){CH(SiMe<sub>3</sub>)<sub>2</sub>}: characterization of the
 Sn(I) product.
;
_journal_issue                   42
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6399
_journal_page_last               6402
_journal_paper_doi               10.1039/d3cc01542d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C42 H114 Si12 Sn6'
_chemical_formula_sum            'C42 H114 Si12 Sn6'
_chemical_formula_weight         1668.55
_chemical_name_systematic        Hexa-((bis-trimethylsilyl)methyl)-hexa-stannane
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_date             2023-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2023-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                86.4949(14)
_cell_angle_beta                 76.8746(14)
_cell_angle_gamma                72.0005(13)
_cell_formula_units_Z            2
_cell_length_a                   13.2745(4)
_cell_length_b                   13.7262(3)
_cell_length_c                   22.6390(6)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.39
_cell_volume                     3820.46(18)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30190
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         1.653
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            'clear pinkish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_preparation
'A mixture of stannylene Sn(CH(SiMe3)2)2 and MgBDI(Dip) in toluene'
_exptl_crystal_recrystallization_method
'Grown from a saturated toluene solution at minus 30 degC overnight'
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         17603
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+5.4771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14741
_reflns_number_total             17603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01542d2.cif
_cod_data_source_block           KLM88FMI
_cod_depositor_comments          'Adding full bibliography for 7131604.cif.'
_cod_database_code               7131604
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.468
_olex2_refinement_description
;
1. Restrained distances
 Sn2-C8 = Sn2-C8B
 2.205 with sigma of 0.01
 Si3-C8 = Si3B-C8B = Si4-C8 = Si4B-C8B
 1.87 with sigma of 0.005
 C9-C10 = C10-C11 = C11-C9 = C9B-C10B = C10B-C11B = C11B-C9B
 3.05 with sigma of 0.01
 Si3-Si4 = Si3B-Si4B
 3.2 with sigma of 0.01
 C12-C13 = C13-C14 = C14-C12 = C12B-C13B = C13B-C14B = C14B-C12B
 3.05 with sigma of 0.01
 Si4-C12 = Si4-C13 = Si4-C14 = Si4B-C12B = Si4B-C13B = Si4B-C14B
 1.87 with sigma of 0.01
 Si1-C2 \\sim Si1B-C2B \\sim Si1-C3 \\sim Si1B-C3B \\sim Si1-C4 \\sim Si1B-C4B
 with sigma of 0.01
 C1-Si1 \\sim C1B-Si1B
 with sigma of 0.01
 Sn1-C1 \\sim Sn1-C1B
 with sigma of 0.01
 C8-Si3 \\sim C8-Si4 \\sim C8B-Si3B \\sim C8B-Si4B
 with sigma of 0.01
 Si3-C9 \\sim Si3-C10 \\sim Si3-C11 \\sim Si3B-C9B \\sim Si3B-C10B \\sim
Si3B-C11B
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C1 \\sim C1B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C2 \\sim C2B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C3 \\sim C3B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C4 \\sim C4B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C8 \\sim C8B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C9 \\sim C9B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
Si3 \\sim Si3B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C10 \\sim C10B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
C11 \\sim C11B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006 within 2A
Uanis(C12) = Uanis(C12B)
Uanis(C13) = Uanis(C13B)
Uanis(C14) = Uanis(C14B)
Uanis(Si4) = Uanis(Si4B)
3. Others
 Fixed Sof: Si1(0.64) Si1B(0.36) Si3(0.71) Si4(0.71) Si3B(0.29) Si4B(0.29)
 C1(0.64) H1(0.64) C2(0.64) H2A(0.64) H2B(0.64) H2C(0.64) C3(0.64) H3A(0.64)
 H3B(0.64) H3C(0.64) C4(0.64) H4A(0.64) H4B(0.64) H4C(0.64) C1B(0.36) H1B(0.36)
 C2B(0.36) H2B1(0.36) H2B2(0.36) H2B3(0.36) C3B(0.36) H3B1(0.36) H3B2(0.36)
 H3B3(0.36) C4B(0.36) H4B1(0.36) H4B2(0.36) H4B3(0.36) C8(0.71) H8(0.71)
 C9(0.71) H9A(0.71) H9B(0.71) H9C(0.71) C10(0.71) H10A(0.71) H10B(0.71)
 H10C(0.71) C11(0.71) H11A(0.71) H11B(0.71) H11C(0.71) C12(0.71) H12A(0.71)
 H12B(0.71) H12C(0.71) C13(0.71) H13A(0.71) H13B(0.71) H13C(0.71) C14(0.71)
 H14A(0.71) H14B(0.71) H14C(0.71) C8B(0.29) H8B(0.29) C9B(0.29) H9B1(0.29)
 H9B2(0.29) H9B3(0.29) C10B(0.29) H10D(0.29) H10E(0.29) H10F(0.29) C11B(0.29)
 H11D(0.29) H11E(0.29) H11F(0.29) C12B(0.29) H12D(0.29) H12E(0.29) H12F(0.29)
 C13B(0.29) H13D(0.29) H13E(0.29) H13F(0.29) C14B(0.29) H14D(0.29) H14E(0.29)
 H14F(0.29)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C1B(H1B), C8(H8), C8B(H8B), C15(H15), C22(H22), C29(H29), C36(H36)
4.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C2B(H2B1,H2B2,H2B3), C4B(H4B1,H4B2,H4B3),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
  C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C9B(H9B1,H9B2,H9B3), C10B(H10D,H10E,
 H10F), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F),
 C14B(H14D,H14E,H14F)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3B(H3B1,H3B2,H3B3), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
  C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              76998
_shelx_hkl_checksum              7597
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop '
_olex2_submission_original_sample_id KLM88
_olex2_submission_special_instructions 'No special instructions were received'