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_4115981
_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         'Fe P S3 Si3 Cl C27 H36 '
_chemical_formula_structural     'Fe P S3 Si3 Cl C27 H36 . C6 H6'
_chemical_formula_sum            'C27 H36 Cl Fe P S3 Si3'
_chemical_formula_weight         663.28
_chemical_melting_point          476(2)
_chemical_name_common
; 
Chloro[tris(2-thio-3-trimethylsilylphenyl-kS)phosphine-kP]iron
;
_chemical_name_systematic
; 
   Chloro[tris(2-thio-3-trimethylsilylphenyl-kS)phosphine-kP]iron
;
_space_group_IT_number           217
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4710(10)
_cell_length_b                   20.4710(10)
_cell_length_c                   20.4710(10)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.0
_cell_measurement_theta_min      9.9
_cell_volume                     8578.6(7)
_computing_cell_refinement       'XSCANS 2.0 (Siemens, 1991)'
_computing_data_collection       'XSCANS 2.0 (Siemens, 1991)'
_computing_data_reduction        'XSCANS 2.0 (Siemens, 1991)'
_computing_molecular_graphics    'Insight II (Biosym/MSI, 1995)'
_computing_publication_material  'SHELXTL5.03 (Siemens, 1994)'
_computing_structure_refinement  'SHELXTL5.03 (Siemens, 1994)'
_computing_structure_solution    'SHELXTL5.03 (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4904
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep reddish-purple'
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_meas      0.0
_exptl_crystal_density_method    none
_exptl_crystal_description       'truncated cube'
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.113
_refine_ls_hydrogen_treatment    'riding H'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         888
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_obs          0.0336
_refine_ls_shift/esd_max         -0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+1.6033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0924
_refine_ls_wR_factor_obs         0.0900
_reflns_number_observed          811
_reflns_number_total             888
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9939882B_4.cif
_cod_data_source_block           n185,2-Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+1.6033P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0612P)^2^+1.6033P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'Fe P S3 Si3 Cl C27 H36 '
_cod_database_code               4115981