Five-Coordinate Diamagnetic Iron(IV) Complexes With A Trigonal Planar Arrangement of Thiolate Ligand Atoms: Synthesis and Crystal Structure of [FeX(PS3)] (X = Cl, Br or I; PS3H3= [P(C'''6H3-3-Me3Si-2-SH)3])
Jodi D. Niemoth-Anderson; Kerry A. (Fusie) Clark; T. Adrian George; Charles R. Ross; Journal of the American Chemical Society 122 (2000) 3977–3978; doi:10.1021/ja993988+

data_4115978
_publ_contact_author_address
;
Department of Chemistry
University of Nebraska-Lincoln, Lincoln, NE 68588-0304
;
_publ_contact_author_email       tageorge@unlserve.unl.edu
_publ_contact_author_name        'George, T. Adrian'
_publ_contact_author_phone       1(402)4723513
_publ_section_title
;
 Five-Coordinate Diamagnetic Iron(IV) Complexes With A Trigonal Planar
 Arrangement of Thiolate Ligand Atoms: Synthesis and Crystal Structure of
 [FeX(PS3)] (X = Cl, Br or I; PS3H3= [P(C'''6H3-3-Me3Si-2-SH)3])
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3977
_journal_page_last               3978
_journal_paper_doi               10.1021/ja993988+
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'Fe2 P2 S6 Si6 C54 H72 '
_chemical_formula_structural     'Fe2 P2 S6 Si6 C54 H72'
_chemical_formula_sum            'C54 H72 Fe2 P2 S6 Si6'
_chemical_formula_weight         1259.74
_chemical_name_common
; 
Bis-(m-[tris(2-thio-3-trimethylsilylphenyl-1k2S;1:2k4S;2k2S)phosphine-1kP,2k
P]-diiron 
;
_chemical_name_systematic
; 
Bis-(m-[tris(2-thio-3-trimethylsilylphenyl-1k2S;1:2k4S;2k2S)phosphine-1kP,2k
P]-diiron 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8960(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.986(10)
_cell_length_b                   11.792(10)
_cell_length_c                   20.659(30)
_cell_measurement_reflns_used    24168
_cell_measurement_temperature    50(1)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      1.6
_cell_volume                     3106(6)
_computing_cell_refinement       'MARXDS 2.1 (MarResearch, 199?)'
_computing_data_collection       'XIPS (MarResearch, 199?)'
_computing_data_reduction        'MARXDS 2.1 (MarResearch, 199?)'
_computing_molecular_graphics    'Insight II (Biosym/MSI, 1995)'
_computing_publication_material  'SHELXTL4.2(Siemens, 1991)'
_computing_structure_refinement  'SHELXTL4.2(Siemens, 1991)'
_computing_structure_solution    'SHELXTL4.2(Siemens, 1991)'
_diffrn_ambient_temperature      50(1)
_diffrn_measurement_device       'MarResearch 18cm Image Plate'
_diffrn_measurement_method       phi
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3x3mm rotating anode'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.5608
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33876
_diffrn_reflns_theta_max         24.0
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      0.0
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.521
_refine_ls_hydrogen_treatment    'riding H'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         7916
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_obs          0.0583
_refine_ls_shift/esd_max         0.051
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(Fo)+0.0008Fo^2^]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0732
_refine_ls_wR_factor_obs         0.0660
_reflns_number_observed          7917
_reflns_number_total             9571
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            ja9939882B_1.cif
_cod_data_source_block           ni203,3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo)+0.0008Fo^2^]
' was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo)+0.0008Fo^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3106.(6)
_cod_original_formula_sum        'Fe2 P2 S6 Si6 C54 H72'
_cod_database_code               4115978