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_4133404
_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      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.788(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3719(2)
_cell_length_b                   19.8321(4)
_cell_length_c                   12.1517(2)
_cell_measurement_reflns_used    17955
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.9800
_cell_measurement_theta_min      4.0720
_cell_volume                     2609.54(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43g (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      air
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -55.00  33.00   1.00    2.50    --  -36.45  38.00-120.00   88
  2  \w   -104.00 -10.00   1.00    2.50    --  -36.45 -77.00-180.00   94
  3  \w   -104.00 -20.00   1.00    2.50    --  -36.45 -57.00 -90.00   84
  4  \w   -104.00 -10.00   1.00    2.50    --  -36.45 -77.00-120.00   94
  5  \w    -63.00  31.00   1.00    2.50    --  -36.45  77.00 -60.00   94
  6  \w      8.00  46.00   1.00    2.50    --   36.45  80.00-149.86   38
  7  \w     10.00 104.00   1.00    2.50    --   36.45  77.00 -30.00   94
  8  \w     87.00 178.00   1.00   25.00    --  108.65  30.00  90.00   91
  9  \w     41.00 136.00   1.00   25.00    --  108.65 -79.00-159.97   95
 10  \w     41.00 137.00   1.00   25.00    --  108.65 -80.00 158.23   96
 11  \w     40.00 126.00   1.00   25.00    --  108.65 -45.00  30.00   86
 12  \w     41.00 137.00   1.00   25.00    --  108.65 -80.00-105.77   96
 13  \w     91.00 177.00   1.00   25.00    --  108.65  45.00 -30.00   86
 14  \w     40.00 126.00   1.00   25.00    --  108.65 -45.00 -60.00   86
 15  \w     41.00 137.00   1.00   25.00    --  108.65 -80.00  83.98   96
 16  \w     41.00 137.00   1.00   25.00    --  108.65 -80.00-132.39   96
 17  \w    -63.00  31.00   1.00    2.50    --  -36.45  77.00  90.00   94
 18  \w    -53.00  31.00   1.00    2.50    --  -36.45  57.00  30.00   84
 19  \w     20.00 104.00   1.00    2.50    --   36.45  57.00  90.00   84
 20  \w     91.00 116.00   1.00   25.00    --  108.03-111.00-180.00   25
 21  \w    124.00 150.00   1.00   25.00    --  108.03 178.00  30.00   26
 22  \w     60.00  96.00   1.00    2.50    --   36.70  57.00  60.00   36
 23  \w     59.00  89.00   1.00    2.50    --   36.70-131.00-151.00   30
 24  \w     75.00 101.00   1.00   25.00    --  108.03-111.00   0.00   26
 25  \w     66.00 117.00   1.00   25.00    --  108.03 -45.00-150.00   51
 26  \w     69.00  95.00   1.00   25.00    --  108.03 178.00-120.00   26
 27  \w     55.00 109.00   1.00   25.00    --  108.03 -94.00  30.00   54
 28  \w     41.00 113.00   1.00   25.00    --  108.03 -30.00 150.00   72
 29  \w     93.00 177.00   1.00   25.00    --  108.03  30.00 -90.00   84
;
_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      0.1064285000
_diffrn_orient_matrix_UB_12      -0.0346684000
_diffrn_orient_matrix_UB_13      -0.0318809000
_diffrn_orient_matrix_UB_21      -0.0507725000
_diffrn_orient_matrix_UB_22      -0.0695171000
_diffrn_orient_matrix_UB_23      0.0196393000
_diffrn_orient_matrix_UB_31      -0.0797541000
_diffrn_orient_matrix_UB_32      -0.0020806000
_diffrn_orient_matrix_UB_33      -0.1277844000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.832
_diffrn_reflns_theta_min         3.820
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.798
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43g (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    1.095
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 4407 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         11540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0659P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                11040
_reflns_number_total             11540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09862_si_004.cif
_cod_data_source_block           rk-1-02092017_4_comp_twin
_cod_database_code               4133404
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C36H84Si8Sn
_chemical_oxdiff_usercomment     Crop_1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.408(11) 0.098(7) 0.428(5) 0.066(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1), C10(H10), C19(H19), C28(H28)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C12(H12), C20(H20), C21(H21), C29(H29), C30(H30)
3.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), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              66214
_shelx_hkl_checksum              26434
_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 1.558
_oxdiff_exptl_absorpt_empirical_full_min 0.646
_oxdiff_twin_integration_method  simultaneous
_twin_special_details
;
Component 2 rotated by -179.9953\% 
 around [1.00 -0.00 -0.00] (reciprocal) or [0.96 -0.00 0.28] (direct)
;