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_4115979
_publ_contact_author_address
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Department of Chemistry
University of Nebraska-Lincoln, Lincoln, NE 68588-0304
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_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
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 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_formula_moiety         'C27 H36 Br Fe P S3 Si3 . 1.71C6 H6'
_chemical_formula_sum            'C37.25 H46.25 Br Fe P S3 Si3'
_chemical_formula_weight         841.17
_chemical_melting_point          469(1)
_chemical_name_common
;
Bromo[tris(2-thio-3-trimethylsilylphenyl-kS)phosphine-kP]iron
;
_chemical_name_systematic
;
 Bromo[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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.623
_cell_length_b                   20.623
_cell_length_c                   20.623
_cell_measurement_temperature    293(2)
_cell_volume                     8771.130
_computing_cell_refinement       MARXDS
_computing_data_collection       MARDC
_computing_data_reduction        MARXDS
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'MARResearch Imaging Plate'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       3
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9482
_diffrn_reflns_theta_full        24.43
_diffrn_reflns_theta_max         24.43
_diffrn_reflns_theta_min         4.64
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       cube
_exptl_crystal_F_000             3486
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.29(7)
_refine_ls_extinction_coef       0.006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         701
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.620
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+13.6108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1624
_reflns_number_gt                647
_reflns_number_total             701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9939882B_2.cif
_cod_data_source_block           ni299,2-Br
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'cubic I' was replaced with
'cubic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        8771.1
_cod_database_code               4115979