Octakis(μ~3~-<i>tert</i>-butylthiolato)bis(<i>tert</i>-butylthiolato)hexakis(1-methylpyrrolidin-2-one)-μ~6~-sulfido-hexabarium(II)
Butcher, Ray J.; Purdy, Andrew P.; Acta Crystallographica Section E 62 (2006) m342–m344; doi:10.1107/S1600536805042017

data_2207950
_publ_section_title
Octakis(\m~3~-<i>tert</i>-butylthiolato)bis(<i>tert</i>-butylthiolato)hexakis(1-methylpyrrolidin-2-one)-\m~6~-sulfido-hexabarium(II)
_journal_coeditor_code           AC6221
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m342
_journal_page_last               m344
_journal_paper_doi               10.1107/S1600536805042017
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ba6 (C4 H9 S)10 S (C5 H9 N O)6]'
_chemical_formula_moiety         'C70 H144 Ba6 N6 O6 S11'
_chemical_formula_sum            'C70 H144 Ba6 N6 O6 S11'
_chemical_formula_weight         2340.60
_chemical_name_systematic
;
Octakis(\m~3~-tert-butylthiolato)bis(tert-butylthiolato)hexakis(1-
methylpyrrolidin-2-one)-\m~6~-sulfido-hexabarium(II)
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.3910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.0316(11)
_cell_length_b                   21.7686(11)
_cell_length_c                   15.2669(8)
_cell_measurement_reflns_used    7746
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.227
_cell_measurement_theta_min      2.582
_cell_volume                     5243.7(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21162
_diffrn_reflns_theta_full        29.33
_diffrn_reflns_theta_max         29.33
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.630
_refine_ls_abs_structure_details 'Flack (1983), 4126 Friedel pairs?'
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         11503
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.029P)^2^+14.7453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                9871
_reflns_number_total             11503
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac6221.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2207950
_cod_database_fobs_code          2207950