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_4133405
_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         'C27 H63 K Si6 Sn'
_chemical_formula_sum            'C27 H63 K Si6 Sn'
_chemical_formula_weight         714.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.864(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5863(3)
_cell_length_b                   16.2257(4)
_cell_length_c                   20.9657(6)
_cell_measurement_reflns_used    14718
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.9200
_cell_measurement_theta_min      3.3770
_cell_volume                     4204.91(19)
_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      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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    -54.00  30.00   1.00    1.00    --  -37.19  57.00-180.00   84
  2  \w    -56.00  32.00   1.00    1.00    --  -37.19  38.00 -90.00   88
  3  \w    -67.00  34.00   1.00    1.00    --  -37.19  19.00  90.00  101
  4  \w    -56.00  32.00   1.00    1.00    --  -37.19  38.00-180.00   88
  5  \w   -109.00  -8.00   1.00    1.00    --  -37.19 -19.00  30.00  101
  6  \w   -104.00 -20.00   1.00    1.00    --  -37.19 -57.00  30.00   84
  7  \w     20.00 104.00   1.00    1.00    --   37.19  57.00 -90.00   84
  8  \w      8.00 109.00   1.00    1.00    --   37.19  19.00 -90.00  101
  9  \w    -30.00  54.00   1.00    1.00    --   37.19 -57.00 120.00   84
 10  \w     94.00 178.00   1.00    5.00    --  111.00  45.00 120.00   84
 11  \w     43.00 128.00   1.00    5.00    --  111.00 -45.00 -60.00   85
 12  \w     43.00 128.00   1.00    5.00    --  111.00 -45.00 120.00   85
 13  \w     90.00 178.00   1.00    5.00    --  111.00  30.00-180.00   88
 14  \w     93.00 178.00   1.00    5.00    --  111.00  61.00-150.00   85
 15  \w     94.00 178.00   1.00    5.00    --  111.00  45.00 -90.00   84
 16  \w     84.00 178.00   1.00    5.00    --  111.00  77.00-180.00   94
 17  \w     44.00 129.00   1.00    5.00    --  111.00 -61.00  30.00   85
 18  \w     94.00 178.00   1.00    5.00    --  111.00  45.00  60.00   84
 19  \w   -105.00 -10.00   1.00    1.00    --  -37.19 -77.00 150.00   95
 20  \w   -105.00 -10.00   1.00    1.00    --  -37.19 -77.00 -30.00   95
 21  \w    -64.00  30.00   1.00    1.00    --  -37.19  77.00  60.00   94
 22  \w   -105.00 -10.00   1.00    1.00    --  -37.19 -77.00-120.00   95
 23  \w    -64.00  30.00   1.00    1.00    --  -37.19  77.00-120.00   94
 24  \w   -105.00 -10.00   1.00    1.00    --  -37.19 -77.00  60.00   95
 25  \w    -64.00  30.00   1.00    1.00    --  -37.19  77.00 150.00   94
 26  \w    -64.00  30.00   1.00    1.00    --  -37.19  77.00 -30.00   94
;
_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      -0.0307622000
_diffrn_orient_matrix_UB_12      0.0331050000
_diffrn_orient_matrix_UB_13      0.0629585000
_diffrn_orient_matrix_UB_21      -0.0807200000
_diffrn_orient_matrix_UB_22      0.0603031000
_diffrn_orient_matrix_UB_23      -0.0401157000
_diffrn_orient_matrix_UB_31      -0.0898723000
_diffrn_orient_matrix_UB_32      -0.0654227000
_diffrn_orient_matrix_UB_33      -0.0052058000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.530
_diffrn_reflns_theta_min         3.468
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.447
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.328
_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    1.128
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.878
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8332
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+15.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7110
_reflns_number_total             8332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09862_si_002.cif
_cod_data_source_block           rk-1-130
_cod_original_cell_volume        4204.92(19)
_cod_database_code               4133405
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C27H63KSi6Sn
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.258
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si6-C26A \\sim Si6-C26 \\sim Si6-C25A \\sim Si6-C25 \\sim Si6-C27A \\sim
Si6-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C27 \\sim C27A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C25 \\sim C25A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C26 \\sim C26A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C10(H10), C19(H19)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C12(H12), C20(H20), C21(H21)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C25A(H25D,H25E,H25F), C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F),
 C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F)
;
_shelx_res_checksum              76166
_shelx_hkl_checksum              59442
_olex2_date_sample_data_collection 2017-08-31
_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 1.412
_oxdiff_exptl_absorpt_empirical_full_min 0.590