Bis(tetra-<i>n</i>-butylammonium) Hexa-μ~3~-sulfido-hexakis(nitrosoiron)
Geiser, Urs; Williams, Jack M.; Acta Crystallographica Section C 54 (1998) 292–293; doi:10.1107/S0108270197013802

data_2007056
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium)
 Hexa-\m~3~-sulfido-hexakis(nitrosoiron)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              292
_journal_page_last               293
_journal_paper_doi               10.1107/S0108270197013802
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[N (C4 H9)4]2 [Fe6 S6 (N1 O1)6]'
_chemical_formula_moiety         '(N (C4 H9)4)2 (Fe6 S6 (NO)6)'
_chemical_formula_sum            'C32 H72 Fe6 N8 O6 S6'
_chemical_formula_weight         1192.43
_chemical_name_systematic
;
 Bis(tetra-n-butylammonium) hexakis((\m~3~-sulfido)-nitroso-iron)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'manual editing of SHELXTL cif file'
_cell_angle_alpha                90
_cell_angle_beta                 99.4440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6451(6)
_cell_length_b                   11.5793(6)
_cell_length_c                   17.7855(9)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2568.9(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'XPREP SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       'area detector \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16370
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.94
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'slanted block'
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.3
_refine_diff_density_min         -0.6
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_all   1.019
_refine_ls_goodness_of_fit_obs   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.017
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_obs          .041
_refine_ls_shift/esd_max         -0.029
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.051P)^2^+4.29P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.114
_refine_ls_wR_factor_obs         .104
_reflns_number_observed          4912
_reflns_number_total             5937
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            bk1352.cif
_cod_data_source_block           tbafe6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2007056