Mechanochemically Driven Transformations in Organotin Chemistry: Stereochemical Rearrangement, Redox Behavior, and Dispersion-Stabilized Complexes.
Koby, Ross F.; Hanusa, Timothy P.; Schley, Nathan D.; Journal of the American Chemical Society 140 (2018) 15934–15942; doi:10.1021/jacs.8b09862

data_4133403
_publ_section_title
;
 Mechanochemically Driven Transformations in Organotin Chemistry:
 Stereochemical Rearrangement, Redox Behavior, and Dispersion-Stabilized
 Complexes.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15934
_journal_page_last               15942
_journal_paper_doi               10.1021/jacs.8b09862
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C36 H84 Si8 Sn'
_chemical_formula_sum            'C36 H84 Si8 Sn'
_chemical_formula_weight         860.44
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                95.647(6)
_cell_angle_beta                 103.837(6)
_cell_angle_gamma                90.081(5)
_cell_formula_units_Z            2
_cell_length_a                   11.4372(6)
_cell_length_b                   11.5112(7)
_cell_length_c                   20.7806(17)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      69.1760
_cell_measurement_theta_min      3.8330
_cell_volume                     2642.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.311
_diffrn_measured_fraction_theta_max 0.291
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -104.00 -10.00   1.00   10.00    --  -36.45 -77.00 150.00   94
  2  \w    -63.00  31.00   1.00   10.00    --  -36.45  77.00-120.00   94
  3  \w   -106.00  33.00   1.00   10.00    --  -36.45   0.00-120.00  139
  4  \w     10.00 104.00   1.00   10.00    --   36.45  77.00 -60.00   94
  5  \w     10.00 104.00   1.00   10.00    --   36.45  77.00-180.00   94
  6  \w    -31.00  63.00   1.00   10.00    --   36.45 -77.00  60.00   94
  7  \w     10.00 104.00   1.00   10.00    --   36.45  77.00  60.00   94
  8  \w      9.00  49.00   1.00   10.00    --   36.45  78.00  -9.01   40
  9  \w     10.00 104.00   1.00   10.00    --   36.45  77.00 -30.00   94
 10  \w     41.00  60.00   1.00   40.00    --  108.65 -80.00-152.14   19
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1038073000
_diffrn_orient_matrix_UB_12      0.0759129000
_diffrn_orient_matrix_UB_13      0.0139751000
_diffrn_orient_matrix_UB_21      -0.0128574000
_diffrn_orient_matrix_UB_22      0.0510901000
_diffrn_orient_matrix_UB_23      -0.0670549000
_diffrn_orient_matrix_UB_31      -0.0914138000
_diffrn_orient_matrix_UB_32      -0.0986255000
_diffrn_orient_matrix_UB_33      -0.0346142000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.311
_diffrn_reflns_Laue_measured_fraction_max 0.291
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4288
_diffrn_reflns_point_group_measured_fraction_full 0.311
_diffrn_reflns_point_group_measured_fraction_max 0.291
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.642
_diffrn_reflns_theta_min         3.860
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.725
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     866
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0770P)^2^+12.5860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4023
_reflns_number_total             4288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09862_si_005.cif
_cod_data_source_block           rk-1-030_twin1_hklf4
_cod_database_code               4133403
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         SnC36Si8H78
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4572(19)
 0.5428(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Si3-C10 \\sim Si-C10
 with sigma of 0.02
 Si3-C15 \\sim Si-C13B
 with sigma of 0.02
 Si3-C13 \\sim Si-C14A
 with sigma of 0.02
 Si3-C14 \\sim Si-C13A
 with sigma of 0.02
 C10-C15 \\sim C10-C13B
 with sigma of 0.04
 C10-C13 \\sim C10-C14A
 with sigma of 0.04
 C10-C14 \\sim C10-C13A
 with sigma of 0.04
 C15-C13 \\sim C13B-C14A
 with sigma of 0.04
 C15-C14 \\sim C13B-C13A
 with sigma of 0.04
 C13-C14 \\sim C14A-C13A
 with sigma of 0.04
 Si1A-C1 \\sim Si1-C1
 with sigma of 0.02
 Si1A-C6A \\sim Si1-C6
 with sigma of 0.02
 Si1A-C4A \\sim Si1-C4
 with sigma of 0.02
 Si1A-C4B \\sim Si1-C1
 with sigma of 0.02
 C1-C6A \\sim C1-C6
 with sigma of 0.04
 C1-C4A \\sim C1-C4
 with sigma of 0.04
 C1-C4B \\sim C1-C1
 with sigma of 0.04
 C6A-C4A \\sim C6-C4
 with sigma of 0.04
 C6A-C4B \\sim C6-C1
 with sigma of 0.04
 C4A-C4B \\sim C4-C1
 with sigma of 0.04
 Si7A-C28 \\sim Si7-C28
 with sigma of 0.02
 Si7A-C31 \\sim Si7-C33
 with sigma of 0.02
 Si7A-C32A \\sim Si7-C2
 with sigma of 0.02
 Si7A-C32B \\sim Si7-C31A
 with sigma of 0.02
 C28-C31 \\sim C28-C33
 with sigma of 0.04
 C28-C32A \\sim C28-C2
 with sigma of 0.04
 C28-C32B \\sim C28-C31A
 with sigma of 0.04
 C31-C32A \\sim C33-C2
 with sigma of 0.04
 C31-C32B \\sim C33-C31A
 with sigma of 0.04
 C32A-C32B \\sim C2-C31A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Si3A)=Sof(C14A)=Sof(H14A1)=Sof(H14A2)=Sof(H14A3)=Sof(C13B)=Sof(H13B1)=Sof(H13B2)=
 Sof(H13B3)=Sof(H10A)=Sof(C13A)=Sof(H13A1)=Sof(H13A2)=Sof(H13A3)=1-FVAR(1)
 Sof(Si3)=Sof(H10)=Sof(C15)=Sof(H15C)=Sof(H15A)=Sof(H15B)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C13)=Sof(H13C)=Sof(H13A)=Sof(H13B)=FVAR(1)
 Sof(Si1)=Sof(H1)=Sof(C1)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(H6C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=1-FVAR(2)
 Sof(Si1A)=Sof(H5A)=Sof(C6A)=Sof(H6A1)=Sof(H6A2)=Sof(H6A3)=Sof(C4A)=
 Sof(H4A3)=Sof(H4A1)=Sof(H4A2)=Sof(C4B)=Sof(H4B3)=Sof(H4B1)=Sof(H4B2)=FVAR(2)
 Sof(Si7)=Sof(H28)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H00Q)=Sof(C2)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C31A)=Sof(H31A1)=Sof(H31A2)=Sof(H31A3)=1-FVAR(3)
 Sof(Si7A)=Sof(H28A)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32B)=
 Sof(H32B1)=Sof(H32B2)=Sof(H32B3)=Sof(C32A)=Sof(H32A1)=Sof(H32A2)=Sof(H32A3)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C19(H19), C10(H10), C10(H10A), C28(H28A), C28(H28), C1(H5A), C1(H1)
7.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C11(H11), C29(H29), C3(H3), C21(H21),
 C12(H12), C30(H30)
7.c Idealised Me refined as rotating group:
 C14A(H14A1,H14A2,H14A3), C13B(H13B1,H13B2,H13B3), C22(H22A,H22B,H22C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C6A(H6A1,H6A2,H6A3), C27(H27A,H27B,H27C),
 C18(H18C,H18A,H18B), C17(H17C,H17A,H17B), C25(H25C,H25A,H25B), C7(H7C,H7A,H7B),
 C15(H15C,H15A,H15B), C4A(H4A3,H4A1,H4A2), C16(H16C,H16A,H16B), C8(H8C,H8A,H8B),
 C1(H5A,H5B,H5C), C6(H6A,H6B,H6C), C23(H23A,H23B,H23C), C32B(H32B1,H32B2,H32B3),
 C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C14(H14A,H14B,H14C), C13A(H13A1,
 H13A2,H13A3), C2(H32A,H32B,H32C), C4(H4A,H4B,H4C), C31A(H31A1,H31A2,H31A3),
 C24(H24A,H24B,H24C), C32A(H32A1,H32A2,H32A3), C9(H9C,H9A,H9B), C34(H34C,H34A,H34B),
  C4B(H4B3,H4B1,H4B2), C35(H35C,H35B,H35A), C13(H13C,H13A,H13B)
;
_shelx_res_checksum              34231
_shelx_hkl_checksum              63512
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.541
_oxdiff_exptl_absorpt_empirical_full_min 0.701
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 179.9851\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.39 0.16 0.90] (direct)
;