A novel hexairon cluster with one disulfide and two Ph~2~PCS^3{-^} ligands
Shi, Yao-Cheng; Cheng, Huan-Ren; Cheng, Da-Cong; Acta Crystallographica Section C 69 (2013) 581–583; doi:10.1107/S0108270113009049

data_2019009
_publ_section_title
;
 A novel hexairon cluster with one disulfide and two Ph~2~PCS^3{-^}
 ligands
;
_journal_coeditor_code           WQ3029
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              581
_journal_page_last               583
_journal_paper_doi               10.1107/S0108270113009049
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe6 (C13 H10 P S)2 (S2) (C O)16]'
_chemical_formula_moiety         'C42 H20 Fe6 O16 P2 S4'
_chemical_formula_sum            'C42 H20 Fe6 O16 P2 S4'
_chemical_formula_weight         1305.90
_chemical_name_systematic
'Hexadecacarbonylbis{\m~3~-[(diphenylphosphanyl)methanediidyl]sulfanido}-\m~4~-disulfido(2-)-hexairon(4 <i>Fe</i>---<i>Fe</i>)'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                83.6258(14)
_cell_angle_beta                 87.7599(11)
_cell_angle_gamma                60.5657(14)
_cell_formula_units_Z            1
_cell_length_a                   10.5129(13)
_cell_length_b                   10.5849(13)
_cell_length_c                   12.7572(16)
_cell_measurement_reflns_used    4455
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.61
_cell_volume                     1228.5(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and WinGX (Farrugia, 2012)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10572
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange--red
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.4153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                4453
_reflns_number_total             5486
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3029.cif
_cod_data_source_block           I
_cod_database_code               2019009
_cod_database_fobs_code          2019009