Bismuth(III) Complex of the [S<sub>4</sub>]<sup>•-</sup> Radical Anion: Dimer Formation via Pancake Bonds.
Schwamm, Ryan J.; Lein, Matthias; Coles, Martyn P.; Fitchett, Christopher M.; Journal of the American Chemical Society 139 (2017) 16490–16493; doi:10.1021/jacs.7b10454

data_4131769
_publ_section_title
;
 Bismuth(III) Complex of the [S<sub>4</sub>]<sup>&#x2022;-</sup> Radical
 Anion: Dimer Formation via Pancake Bonds.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16490
_journal_page_last               16493
_journal_paper_doi               10.1021/jacs.7b10454
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C76 H80 N2 O Si2, 2(C4 H8 O)'
_chemical_formula_sum            'C84 H96 N2 O3 Si2'
_chemical_formula_weight         1237.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.2141(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7886(3)
_cell_length_b                   12.3313(2)
_cell_length_c                   18.8823(3)
_cell_measurement_reflns_used    10135
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.4780
_cell_measurement_theta_min      3.5670
_cell_volume                     3530.05(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -39.00    3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000 -150.0000 42

  2 omega  -49.00   28.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  -30.0000 77

  3 omega   46.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255  -99.0000  -60.0000 30

  4 omega   67.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255 -125.0000  120.0000 26

  5 omega   18.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255   57.0000   90.0000 70

  6 omega   52.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 57

  7 omega   58.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 26

  8 omega   38.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 34

  9 omega   59.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 31

 10 omega  104.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -30.0000 71

 11 omega   42.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 49

 12 omega   87.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 25

 13 omega  125.00  167.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 42

 14 omega   61.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 26

 15 omega   41.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 44

 16 omega   39.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 46

 17 omega   68.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 50

 18 omega   78.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -115.0000 -173.0000 26

 19 omega   42.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   60.0000 49

 20 omega   46.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 59

 21 omega  106.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  120.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0776450000
_diffrn_orient_matrix_UB_12      -0.0761107000
_diffrn_orient_matrix_UB_13      0.0009167000
_diffrn_orient_matrix_UB_21      -0.0527162000
_diffrn_orient_matrix_UB_22      -0.0969228000
_diffrn_orient_matrix_UB_23      0.0170605000
_diffrn_orient_matrix_UB_31      -0.0388549000
_diffrn_orient_matrix_UB_32      -0.0207150000
_diffrn_orient_matrix_UB_33      -0.0832316000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.665
_diffrn_reflns_theta_min         3.236
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0477P)^2^+2.1883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6599
_reflns_number_total             7360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10454_si_002.cif
_cod_data_source_block           Compound-5
_cod_original_cell_volume        3530.05(10)
_cod_database_code               4131769
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C60h20n2o2si2
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed U12: O(0)
 Fixed U23: O(0)
 Fixed Uiso: H3(0.024) H5(0.024) H7(0.023) H9(0.031) H10(0.037) H11(0.041)
 H12(0.048) H13(0.038) H15(0.031) H16(0.041) H17(0.043) H18(0.036) H19(0.029)
 H21A(0.042) H21B(0.042) H21C(0.042) H22A(0.043) H22B(0.043) H22C(0.043)
 H23A(0.04) H23B(0.04) H23C(0.04) H24(0.025) H26(0.033) H27(0.039) H28(0.04)
 H29(0.044) H30(0.036) H32(0.033) H33(0.041) H34(0.046) H35(0.044) H36(0.034)
 H37A(0.042) H37B(0.042) H37C(0.042) H38A(0.047) H38B(0.047) H38C(0.047)
 H39A(0.073) H39B(0.073) H40A(0.1) H40B(0.1) H41A(0.087) H41B(0.087)
 H42A(0.079) H42B(0.079)
 Fixed X: O(0.75) H3(0.3375) H5(0.4331) H7(0.5096) H9(0.4984) H10(0.4224)
 H11(0.2727) H12(0.2019) H13(0.278) H15(0.3558) H16(0.3438) H17(0.4024)
 H18(0.4709) H19(0.4867) H21A(0.22) H21B(0.1687) H21C(0.1993) H22A(0.2744)
 H22B(0.2467) H22C(0.3463) H23A(0.3792) H23B(0.2782) H23C(0.3277) H24(0.616)
 H26(0.3947) H27(0.3432) H28(0.4408) H29(0.5911) H30(0.6431) H32(0.4985)
 H33(0.5438) H34(0.6639) H35(0.7372) H36(0.6899) H37A(0.7231) H37B(0.6265)
 H37C(0.6436) H38A(0.6967) H38B(0.6804) H38C(0.773) H39A(0.4195) H39B(0.4027)
 H40A(0.3575) H40B(0.3774) H41A(0.4854) H41B(0.4859) H42A(0.6087) H42B(0.5741)
 Fixed Y: H3(0.1311) H5(0.0135) H7(0.3177) H9(0.5017) H10(0.6597) H11(0.6528)
 H12(0.4868) H13(0.329) H15(0.3761) H16(0.3159) H17(0.1504) H18(0.043)
 H19(0.1046) H21A(0.0498) H21B(-0.0337) H21C(0.0772) H22A(-0.0216) H22B(-
 0.1336) H22C(-0.1092) H23A(-0.1581) H23B(-0.1803) H23C(-0.1007) H24(0.189)
 H26(0.2083) H27(0.3091) H28(0.3922) H29(0.3726) H30(0.2721) H32(0.0352) H33(-
 0.1295) H34(-0.2184) H35(-0.1438) H36(0.019) H37A(0.1704) H37B(0.2089)
 H37C(0.1155) H38A(0.4734) H38B(0.434) H38C(0.4176) H39A(0.4266) H39B(0.4888)
 H40A(0.6296) H40B(0.5687) H41A(0.7157) H41B(0.6873) H42A(0.6163) H42B(0.544)
 Fixed Z: O(0.25) H3(0.0503) H5(0.2545) H7(0.0622) H9(0.0694) H10(0.076)
 H11(0.0666) H12(0.0538) H13(0.0474) H15(-0.0815) H16(-0.1999) H17(-0.219) H18(-
 0.1186) H19(-0.0005) H21A(0.1811) H21B(0.122) H21C(0.0969) H22A(0.0177)
 H22B(0.0437) H22C(0.0513) H23A(0.1848) H23B(0.1717) H23C(0.2343) H24(0.3084)
 H26(0.3121) H27(0.3948) H28(0.4941) H29(0.5115) H30(0.4293) H32(0.4081)
 H33(0.4647) H34(0.4444) H35(0.3661) H36(0.3067) H37A(0.0971) H37B(0.059)
 H37C(0.1177) H38A(0.1835) H38B(0.1018) H38C(0.1587) H39A(0.2785) H39B(0.203)
 H40A(0.2523) H40B(0.3287) H41A(0.284) H41B(0.3657) H42A(0.3161) H42B(0.371)
;