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_4131775
_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, C6 H12'
_chemical_formula_sum            'C82 H90 N2 O Pb Si2'
_chemical_formula_weight         1382.92
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2017-03-31T11:29:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.9327(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.51169(15)
_cell_length_b                   31.3488(5)
_cell_length_c                   20.9410(3)
_cell_measurement_reflns_used    14320
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.266
_cell_measurement_theta_min      3.741
_cell_measurement_wavelength     0.71073
_cell_volume                     6899.75(18)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
;
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1712
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.8461
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0674123
_diffrn_orient_matrix_UB_12      0.0011271
_diffrn_orient_matrix_UB_13      -0.0000353
_diffrn_orient_matrix_UB_21      -0.0026609
_diffrn_orient_matrix_UB_22      -0.0121316
_diffrn_orient_matrix_UB_23      -0.0285712
_diffrn_orient_matrix_UB_31      -0.0022692
_diffrn_orient_matrix_UB_32      -0.0190754
_diffrn_orient_matrix_UB_33      0.0181612
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39124
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         29.4356
_diffrn_reflns_theta_min         3.3499
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
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    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.1857
_exptl_crystal_size_mid          0.1459
_exptl_crystal_size_min          0.0958
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     803
_refine_ls_number_reflns         16170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+9.2712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                13259
_reflns_number_total             16170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10454_si_002.cif
_cod_data_source_block           Pb-{P21/n}
_cod_original_cell_volume        6899.77(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4131775