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_4131770
_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         'C40 H43 Li0.5 N O Si, C8 H16 Li0.5 O2'
_chemical_formula_sum            'C48 H59 Li N O3 Si'
_chemical_formula_weight         732.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4128(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.9315(5)
_cell_length_b                   19.5340(4)
_cell_length_c                   18.5814(3)
_cell_measurement_reflns_used    7353
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.1050
_cell_measurement_theta_min      2.9140
_cell_volume                     8671.0(3)
_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      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -61.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000   30.0000 91

  2 omega   52.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7505 -125.0000 -180.0000 30

  3 omega   72.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360 -125.0000 -180.0000 40

  4 omega   47.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  -30.0000  -60.0000 43

  5 omega   69.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  -45.0000  -30.0000 26

  6 omega   42.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  -45.0000   60.0000 53

  7 omega   37.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  -45.0000  120.0000 55

  8 omega   28.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  -94.0000    0.0000 79

  9 omega   51.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  -30.0000 -150.0000 35

 10 omega   86.00  161.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360   45.0000  -30.0000 75

 11 omega  152.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  125.0000  -30.0000 25

 12 omega   96.00  127.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9360  125.0000  -30.0000 31

 13 omega -107.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -120.0000 94
;
_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      -0.0389564000
_diffrn_orient_matrix_UB_12      0.0367652000
_diffrn_orient_matrix_UB_13      0.0507446000
_diffrn_orient_matrix_UB_21      -0.0108601000
_diffrn_orient_matrix_UB_22      -0.0684022000
_diffrn_orient_matrix_UB_23      0.0380546000
_diffrn_orient_matrix_UB_31      0.0501629000
_diffrn_orient_matrix_UB_32      0.0137662000
_diffrn_orient_matrix_UB_33      0.0537047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17355
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.046
_diffrn_reflns_theta_min         2.922
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78842
_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    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8574
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0989P)^2^+9.4936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7283
_reflns_number_total             8574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10454_si_002.cif
_cod_data_source_block           Li-salt
_cod_database_code               4131770
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 97.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.88
_olex2_refinement_description
;
1. Others
 Fixed U12: O1(0) O2(0) Li1(0) Li2(0)
 Fixed U23: O1(0) O2(0) Li1(0) Li2(0)
 Fixed Uiso: H3(0.045) H5(0.043) H7(0.045) H9(0.059) H10(0.074) H11(0.081)
 H12(0.077) H13(0.062) H15(0.076) H16(0.087) H17(0.078) H18(0.077) H19(0.063)
 H21A(0.106) H21B(0.106) H21C(0.106) H22A(0.105) H22B(0.105) H22C(0.105)
 H23A(0.118) H23B(0.118) H23C(0.118) H24(0.044) H26(0.079) H27(0.102)
 H28(0.084) H29(0.07) H30(0.058) H32(0.067) H33(0.091) H34(0.097) H35(0.105)
 H36(0.079) H37A(0.072) H37B(0.072) H37C(0.072) H38A(0.078) H38B(0.078)
 H38C(0.078) H39A(0.078) H39B(0.078) H40A(0.169) H40B(0.169) H41A(0.189)
 H41B(0.189) H42A(0.15) H42B(0.15) H43A(0.123) H43B(0.123) H44A(0.164)
 H44B(0.164) H45A(0.098) H45B(0.098) H46A(0.144) H46B(0.144) H47A(0.179)
 H47B(0.179) H48A(0.12) H48B(0.12)
 Fixed X: O1(0.5) O2(0.5) H3(0.3073) H5(0.3083) H7(0.4181) H9(0.47)
 H10(0.4885) H11(0.4212) H12(0.3365) H13(0.318) H15(0.3985) H16(0.3446)
 H17(0.2569) H18(0.2226) H19(0.2762) H21A(0.3006) H21B(0.2599) H21C(0.3167)
 H22A(0.1912) H22B(0.1827) H22C(0.2237) H23A(0.2643) H23B(0.209) H23C(0.2141)
 H24(0.4241) H26(0.4566) H27(0.4566) H28(0.3842) H29(0.3128) H30(0.313)
 H32(0.2971) H33(0.2559) H34(0.2863) H35(0.3602) H36(0.4034) H37A(0.3812)
 H37B(0.3559) H37C(0.3997) H38A(0.4888) H38B(0.4371) H38C(0.494) H39A(0.5798)
 H39B(0.547) H40A(0.5335) H40B(0.5521) Li1(0.5) H41A(0.477) H41B(0.4307)
 H42A(0.4511) H42B(0.4692) H43A(0.5376) H43B(0.5586) H44A(0.5861) H44B(0.5456)
 H45A(0.448) H45B(0.465) H46A(0.3824) H46B(0.3663) H47A(0.3139) H47B(0.3369)
 H48A(0.3762) H48B(0.3677) Li2(0.5)
 Fixed Y: H3(0.3243) H5(0.3838) H7(0.2058) H9(0.2931) H10(0.3491) H11(0.3525)
 H12(0.2989) H13(0.2415) H15(0.1093) H16(0.0129) H17(0.0057) H18(0.0963)
 H19(0.1932) H21A(0.4951) H21B(0.5268) H21C(0.4941) H22A(0.3738) H22B(0.4531)
 H22C(0.4235) H23A(0.4201) H23B(0.4554) H23C(0.3754) H24(0.2874) H26(0.4042)
 H27(0.5084) H28(0.5378) H29(0.4608) H30(0.356) H32(0.2193) H33(0.1307)
 H34(0.1023) H35(0.1617) H36(0.2495) H37A(0.0766) H37B(0.0967) H37C(0.0372)
 H38A(0.0893) H38B(0.1323) H38C(0.1689) H39A(0.4075) H39B(0.4135) H40A(0.52)
 H40B(0.5079) H41A(0.0487) H41B(0.0985) H42A(0.0773) H42B(0.0068) H43A(0.0739)
 H43B(0.0319) H44A(0.1321) H44B(0.1723) H45A(0.3019) H45B(0.3526) H46A(0.395)
 H46B(0.3467) H47A(0.2955) H47B(0.3367) H48A(0.241) H48B(0.2079)
 Fixed Z: O1(0.25) O2(0.25) H3(0.1191) H5(0.3245) H7(0.1441) H9(0.0859) H10(-
 0.019) H11(-0.114) H12(-0.1033) H13(0.0012) H15(0.0569) H16(0.0356)
 H17(0.0798) H18(0.1428) H19(0.164) H21A(0.259) H21B(0.1987) H21C(0.1784)
 H22A(0.2444) H22B(0.237) H22C(0.2983) H23A(0.0895) H23B(0.1115) H23C(0.1132)
 H24(0.3856) H26(0.3921) H27(0.4498) H28(0.5212) H29(0.5349) H30(0.4779)
 H32(0.3466) H33(0.406) H34(0.5213) H35(0.577) H36(0.5175) H37A(0.2247)
 H37B(0.2977) H37C(0.2957) H38A(0.3981) H38B(0.4199) H38C(0.4072) H39A(0.2633)
 H39B(0.3342) H40A(0.3053) H40B(0.2265) Li1(0.25) H41A(0.7002) H41B(0.6665)
 H42A(0.5591) H42B(0.5945) H43A(0.527) H43B(0.596) H44A(0.6391) H44B(0.5841)
 H45A(0.6305) H45B(0.694) H46A(0.688) H46B(0.6223) H47A(0.6872) H47B(0.7554)
 H48A(0.7916) H48B(0.7143) Li2(0.75)
;