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_4131776
_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 H78 N2 O Pb Si2, 2(C4 H10 O)'
_chemical_formula_sum            'C84 H98 N2 O3 Pb Si2'
_chemical_formula_weight         1447.01
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-09-21T14:17:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.0090(19)
_cell_angle_beta                 97.9369(18)
_cell_angle_gamma                99.1671(19)
_cell_formula_units_Z            2
_cell_length_a                   9.9952(2)
_cell_length_b                   18.9141(4)
_cell_length_c                   20.7293(4)
_cell_measurement_reflns_used    18613
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.125
_cell_measurement_theta_min      3.785
_cell_measurement_wavelength     0.71073
_cell_volume                     3707.38(14)
_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    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_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      0.0429145
_diffrn_orient_matrix_UB_12      0.0273513
_diffrn_orient_matrix_UB_13      0.0273483
_diffrn_orient_matrix_UB_21      0.0072013
_diffrn_orient_matrix_UB_22      -0.0272817
_diffrn_orient_matrix_UB_23      0.0180673
_diffrn_orient_matrix_UB_31      0.0587215
_diffrn_orient_matrix_UB_32      -0.0070018
_diffrn_orient_matrix_UB_33      -0.0141653
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35896
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         26.3725
_diffrn_reflns_theta_min         3.2775
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.646
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1500.0
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.725
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     835
_refine_ls_number_reflns         15137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+2.0922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                13865
_reflns_number_total             15137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10454_si_002.cif
_cod_data_source_block           Pb-P-bar-1
_cod_database_code               4131776