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_4131773
_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 Bi N2 O Si2, 2(C4 H10 O)'
_chemical_formula_sum            'C84 H98 Bi N2 O3 Si2'
_chemical_formula_weight         1448.8
_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             2017-07-08T11:13:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.143(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7552(5)
_cell_length_b                   24.9034(7)
_cell_length_c                   24.5987(7)
_cell_measurement_reflns_used    13089
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      74.577
_cell_measurement_theta_min      4.004
_cell_measurement_wavelength     1.54184
_cell_volume                     7609.0(4)
_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 0.9958
_diffrn_measured_fraction_theta_max 0.9887
_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      -0.0714254
_diffrn_orient_matrix_UB_12      -0.050552
_diffrn_orient_matrix_UB_13      -0.0089633
_diffrn_orient_matrix_UB_21      -0.0941712
_diffrn_orient_matrix_UB_22      0.0334649
_diffrn_orient_matrix_UB_23      -0.0338341
_diffrn_orient_matrix_UB_31      0.0374393
_diffrn_orient_matrix_UB_32      -0.0125675
_diffrn_orient_matrix_UB_33      -0.0539083
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        74.3338
_diffrn_reflns_theta_max         75.174
_diffrn_reflns_theta_min         3.5496
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.2
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.29
_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            red
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3004
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.181
_refine_diff_density_max         5.872
_refine_diff_density_min         -3.712
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     749
_refine_ls_number_reflns         15518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.07
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+60.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                13695
_reflns_number_total             15518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10454_si_002.cif
_cod_data_source_block           Compound-7-{P21/n}
_cod_original_cell_volume        7609.1(4)
_cod_database_code               4131773