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_4115980
_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])
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_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 Fe I P S3 Si3 . 3 C6 H4 Cl2'
_chemical_formula_sum            'C90 H96 Cl12 Fe2 I2 P2 S6 Si6'
_chemical_formula_weight         2391.41
_chemical_melting_point          469(1)
_chemical_name_common
;
Iodo[tris(2-thio-3-trimethylsilylphenyl-kS)phosphine-kP]iron
;
_chemical_name_systematic
;
  Iodo[tris(2-thio-3-trimethylsilylphenyl-kS)phosphine-kP]iron
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 112.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.317(6)
_cell_length_b                   16.919(3)
_cell_length_c                   21.301(4)
_cell_measurement_temperature    293(2)
_cell_volume                     10449(4)
_computing_cell_refinement       MARXDS
_computing_data_collection       MARDC
_computing_data_reduction        MARXDS
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31134
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       chunk
_exptl_crystal_F_000             4832
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .2
_refine_diff_density_max         2.189
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00041(18)
_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   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7085
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1493P)^2^+16.8947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.2083
_reflns_number_gt                5531
_reflns_number_total             7085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9939882B_3.cif
_cod_data_source_block           ni298c,2-I
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'monoclinic C' was replaced with
'monoclinic' 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_database_code               4115980