#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/86/4318626.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4318626
loop_
_publ_author_name
'Takashi Komuro'
'Hiroyuki Kawaguchi'
'Kazuyuki Tatsumi'
_publ_contact_author_address
;
Research Center for Materials Science, and Department of Chemistry, 
Graduate School of Science, Nagoya University, Furo-cho, Chikusa-ku, 
Nagoya 464-8602, Japan,
;
_publ_contact_author_email       ' i45100a@nucc.cc.nagoya-u.ac.jp'
_publ_contact_author_fax         ' +81-52-789-2943'
_publ_contact_author_name        ' Kazuyuki Tatsumi'
_publ_section_title
;
 Synthesis and Reactions of Triphenylsilanethiolato Complexes of
 Manganese(II), Iron(II), Cobalt(II), and Nickel(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5083
_journal_page_last               5090
_journal_paper_doi               10.1021/ic025715c
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C52 H70 Cl4 Fe2 N2 S2 Si2 '
_chemical_formula_sum            'C52 H70 Cl4 Fe2 N2 S2 Si2'
_chemical_formula_weight         1096.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                94.42(4)
_cell_angle_beta                 102.93(2)
_cell_angle_gamma                108.65(2)
_cell_formula_units_Z            1
_cell_length_a                   10.855(2)
_cell_length_b                   13.914(5)
_cell_length_c                   9.983(3)
_cell_measurement_temperature    193.2
_cell_volume                     1374.2(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 2.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4188
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            coloreless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3128
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00016|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                3128
_reflns_number_total             0
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic025715c_s1_09.cif
_cod_data_source_block           (NEt4)2[Fe2Cl4(SSiPh3)2]
_cod_original_cell_volume        1374.4(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C52 H70 Cl4 Fe2 N2 S2 Si2 '
_cod_database_code               4318626
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.12425(7) 0.44838(6) 1.08200(9) 0.0230(2) Uani 1.00 d . . .
Cl1 Cl 1.1763(2) 0.4337(2) 1.3098(2) 0.0538(5) Uani 1.00 d . . .
Cl2 Cl 1.2419(2) 0.3917(1) 0.9544(2) 0.0464(5) Uani 1.00 d . . .
S1 S 0.8830(1) 0.3873(1) 0.9847(2) 0.0269(4) Uani 1.00 d . . .
Si1 Si 0.7960(1) 0.2391(1) 0.8630(2) 0.0203(4) Uani 1.00 d . . .
N1 N 0.5733(5) 0.3253(4) 1.2938(5) 0.027(1) Uani 1.00 d . . .
C1 C 0.8791(5) 0.2189(4) 0.7237(6) 0.022(1) Uani 1.00 d . . .
C2 C 0.9416(6) 0.2988(5) 0.6579(7) 0.030(2) Uani 1.00 d . . .
C3 C 0.9980(6) 0.2810(5) 0.5477(7) 0.041(2) Uani 1.00 d . . .
C4 C 0.9890(6) 0.1821(6) 0.5021(8) 0.047(2) Uani 1.00 d . . .
C5 C 0.9278(6) 0.1015(5) 0.5659(8) 0.040(2) Uani 1.00 d . . .
C6 C 0.8756(5) 0.1205(5) 0.6765(7) 0.031(2) Uani 1.00 d . . .
C7 C 0.8096(5) 0.1401(4) 0.9786(6) 0.025(2) Uani 1.00 d . . .
C8 C 0.9348(6) 0.1380(5) 1.0455(7) 0.034(2) Uani 1.00 d . . .
C9 C 0.9506(6) 0.0631(5) 1.1234(8) 0.041(2) Uani 1.00 d . . .
C10 C 0.8368(6) -0.0141(5) 1.1393(8) 0.039(2) Uani 1.00 d . . .
C11 C 0.7116(6) -0.0127(5) 1.0759(8) 0.038(2) Uani 1.00 d . . .
C12 C 0.6980(6) 0.0621(4) 0.9952(7) 0.033(2) Uani 1.00 d . . .
C13 C 0.6134(5) 0.2127(4) 0.7767(6) 0.021(1) Uani 1.00 d . . .
C14 C 0.5412(5) 0.2731(4) 0.8132(7) 0.029(2) Uani 1.00 d . . .
C15 C 0.4048(6) 0.2488(5) 0.7474(8) 0.040(2) Uani 1.00 d . . .
C16 C 0.3385(5) 0.1642(5) 0.6449(7) 0.031(2) Uani 1.00 d . . .
C17 C 0.4079(5) 0.1024(4) 0.6060(7) 0.028(2) Uani 1.00 d . . .
C18 C 0.5425(5) 0.1267(4) 0.6716(7) 0.028(2) Uani 1.00 d . . .
C19 C 0.8225(7) 0.4340(6) 1.3449(9) 0.055(2) Uani 1.00 d . . .
C20 C 0.6257(8) 0.1594(6) 1.321(1) 0.062(3) Uani 1.00 d . . .
C21 C 0.3217(7) 0.2145(7) 1.237(1) 0.074(3) Uani 1.00 d . . .
C22 C 0.5303(8) 0.4949(6) 1.272(1) 0.098(3) Uani 1.00 d . . .
C23 C 0.701(1) 0.382(1) 1.410(1) 0.039(4) Uani 0.50 d P . .
C24 C 0.684(1) 0.3714(9) 1.226(1) 0.029(3) Uani 0.50 d P . .
C25 C 0.603(1) 0.2584(9) 1.397(1) 0.032(3) Uani 0.50 d P . .
C26 C 0.597(1) 0.231(1) 1.216(2) 0.044(4) Uani 0.50 d P . .
C27 C 0.460(1) 0.291(1) 1.360(2) 0.044(4) Uani 0.50 d P . .
C28 C 0.445(1) 0.2670(9) 1.171(1) 0.028(3) Uani 0.50 d P . .
C29 C 0.542(1) 0.4111(9) 1.378(1) 0.033(3) Uani 0.50 d P . .
C30 C 0.553(1) 0.3910(10) 1.181(2) 0.047(4) Uani 0.50 d P . .
H1 H 0.9454(6) 0.3678(5) 0.6884(7) 0.036(2) Uiso 1.00 calc . . .
H2 H 1.0422(6) 0.3376(5) 0.5044(7) 0.048(2) Uiso 1.00 calc . . .
H3 H 1.0267(6) 0.1686(6) 0.4264(8) 0.051(2) Uiso 1.00 calc . . .
H4 H 0.9212(6) 0.0321(5) 0.5331(8) 0.047(2) Uiso 1.00 calc . . .
H5 H 0.8353(5) 0.0639(5) 0.7218(7) 0.036(2) Uiso 1.00 calc . . .
H6 H 1.0150(6) 0.1919(5) 1.0389(7) 0.041(2) Uiso 1.00 calc . . .
H7 H 1.0400(6) 0.0627(5) 1.1656(8) 0.049(2) Uiso 1.00 calc . . .
H8 H 0.8461(6) -0.0663(5) 1.1959(8) 0.047(2) Uiso 1.00 calc . . .
H9 H 0.6318(6) -0.0657(5) 1.0853(8) 0.045(2) Uiso 1.00 calc . . .
H10 H 0.6082(6) 0.0605(4) 0.9500(7) 0.039(2) Uiso 1.00 calc . . .
H11 H 0.5868(5) 0.3329(4) 0.8854(7) 0.034(2) Uiso 1.00 calc . . .
H12 H 0.3570(6) 0.2922(5) 0.7735(8) 0.047(2) Uiso 1.00 calc . . .
H13 H 0.2435(5) 0.1472(5) 0.6000(7) 0.037(2) Uiso 1.00 calc . . .
H14 H 0.3620(5) 0.0423(4) 0.5344(7) 0.034(2) Uiso 1.00 calc . . .
H15 H 0.5904(5) 0.0839(4) 0.6435(7) 0.033(2) Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Si Si 0.082 0.070
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Fe Fe 0.346 0.844
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL1 FE1 CL2 115.06(8) . . . yes
CL1 FE1 S1 110.86(7) . . . yes
CL1 FE1 S1 119.57(7) . . 2_767 yes
CL2 FE1 S1 115.68(6) . . . yes
CL2 FE1 S1 107.43(7) . . 2_767 yes
S1 FE1 S1 84.92(5) . . 2_767 yes
FE1 S1 FE1 95.08(5) . . 2_767 yes
FE1 S1 SI1 116.35(8) . . . yes
FE1 S1 SI1 128.80(9) 2_767 . . yes
S1 SI1 C1 114.4(2) . . . yes
S1 SI1 C7 109.3(2) . . . yes
S1 SI1 C13 110.1(2) . . . yes
C1 SI1 C7 106.2(3) . . . yes
C1 SI1 C13 107.5(3) . . . yes
C7 SI1 C13 109.1(2) . . . yes
C23 N1 C24 73.0(7) . . . yes
C23 N1 C25 67.6(7) . . . yes
C23 N1 C26 107.4(8) . . . yes
C23 N1 C27 107.1(8) . . . yes
C23 N1 C28 178.3(9) . . . yes
C23 N1 C29 73.6(8) . . . yes
C23 N1 C30 111.5(8) . . . yes
C24 N1 C25 114.9(8) . . . yes
C24 N1 C26 74.1(8) . . . yes
C24 N1 C27 173.2(9) . . . yes
C24 N1 C28 105.5(7) . . . yes
C24 N1 C29 111.2(7) . . . yes
C24 N1 C30 59.5(8) . . . yes
C25 N1 C26 71.1(8) . . . yes
C25 N1 C27 70.9(8) . . . yes
C25 N1 C28 112.7(7) . . . yes
C25 N1 C29 104.7(8) . . . yes
C25 N1 C30 173.8(10) . . . yes
C26 N1 C27 112.0(8) . . . yes
C26 N1 C28 71.3(7) . . . yes
C26 N1 C29 174.5(8) . . . yes
C26 N1 C30 103.8(9) . . . yes
C27 N1 C28 74.5(7) . . . yes
C27 N1 C29 62.8(7) . . . yes
C27 N1 C30 114.9(9) . . . yes
C28 N1 C29 107.8(7) . . . yes
C28 N1 C30 68.1(7) . . . yes
C29 N1 C30 80.6(8) . . . yes
SI1 C1 C2 122.4(5) . . . yes
SI1 C1 C6 120.4(5) . . . yes
C2 C1 C6 117.1(6) . . . yes
C1 C2 C3 121.6(6) . . . yes
C2 C3 C4 119.3(6) . . . yes
C3 C4 C5 120.2(7) . . . yes
C4 C5 C6 119.9(7) . . . yes
C1 C6 C5 121.9(6) . . . yes
SI1 C7 C8 120.2(4) . . . yes
SI1 C7 C12 123.4(4) . . . yes
C8 C7 C12 116.3(6) . . . yes
C7 C8 C9 122.7(5) . . . yes
C8 C9 C10 119.9(6) . . . yes
C9 C10 C11 118.5(7) . . . yes
C10 C11 C12 120.6(6) . . . yes
C7 C12 C11 121.9(6) . . . yes
SI1 C13 C14 123.4(4) . . . yes
SI1 C13 C18 119.4(5) . . . yes
C14 C13 C18 117.1(5) . . . yes
C13 C14 C15 121.0(5) . . . yes
C14 C15 C16 120.4(6) . . . yes
C15 C16 C17 119.9(5) . . . yes
C16 C17 C18 119.4(5) . . . yes
C13 C18 C17 122.1(6) . . . yes
C23 C19 C24 67.9(7) . . . yes
C25 C20 C26 68.5(9) . . . yes
C27 C21 C28 68.0(7) . . . yes
C29 C22 C30 71.8(8) . . . yes
N1 C23 C19 109.6(9) . . . yes
N1 C23 C24 52.8(6) . . . yes
N1 C23 C25 55.2(6) . . . yes
C19 C23 C24 56.8(6) . . . yes
C19 C23 C25 131(1) . . . yes
C24 C23 C25 92.7(8) . . . yes
N1 C24 C19 109.5(9) . . . yes
N1 C24 C23 54.2(6) . . . yes
N1 C24 C30 61.2(8) . . . yes
C19 C24 C23 55.3(6) . . . yes
C19 C24 C30 132(1) . . . yes
C23 C24 C30 99(1) . . . yes
N1 C25 C20 110.6(10) . . . yes
N1 C25 C23 57.2(6) . . . yes
N1 C25 C26 57.0(7) . . . yes
N1 C25 C27 54.4(7) . . . yes
C20 C25 C23 125(1) . . . yes
C20 C25 C26 53.7(8) . . . yes
C20 C25 C27 127.1(8) . . . yes
C23 C25 C26 92.6(9) . . . yes
C23 C25 C27 90.7(9) . . . yes
C26 C25 C27 92.8(10) . . . yes
N1 C26 C20 109(1) . . . yes
N1 C26 C25 51.9(7) . . . yes
N1 C26 C28 53.8(6) . . . yes
C20 C26 C25 57.9(8) . . . yes
C20 C26 C28 127(1) . . . yes
C25 C26 C28 88.9(10) . . . yes
N1 C27 C21 108(1) . . . yes
N1 C27 C25 54.7(7) . . . yes
N1 C27 C28 54.8(7) . . . yes
N1 C27 C29 61.4(8) . . . yes
C21 C27 C25 120(1) . . . yes
C21 C27 C28 54.1(7) . . . yes
C21 C27 C29 130(1) . . . yes
C25 C27 C28 90(1) . . . yes
C25 C27 C29 93.9(9) . . . yes
C28 C27 C29 94.7(10) . . . yes
N1 C28 C21 108.3(9) . . . yes
N1 C28 C26 54.9(6) . . . yes
N1 C28 C27 50.8(6) . . . yes
N1 C28 C30 54.9(6) . . . yes
C21 C28 C26 118.9(10) . . . yes
C21 C28 C27 57.9(7) . . . yes
C21 C28 C30 135(1) . . . yes
C26 C28 C27 87.4(9) . . . yes
C26 C28 C30 86.7(8) . . . yes
C27 C28 C30 90.4(8) . . . yes
N1 C29 C22 105.2(9) . . . yes
N1 C29 C27 55.8(8) . . . yes
C22 C29 C27 130.4(9) . . . yes
N1 C30 C22 102.1(10) . . . yes
N1 C30 C24 59.3(8) . . . yes
N1 C30 C28 57.0(6) . . . yes
C22 C30 C24 119.6(9) . . . yes
C22 C30 C28 119(1) . . . yes
C24 C30 C28 97(1) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE1 CL1 2.259(2) . . yes
FE1 CL2 2.257(2) . . yes
FE1 S1 2.416(2) . . yes
FE1 S1 2.450(2) . 2_767 yes
S1 SI1 2.116(2) . . yes
SI1 C1 1.868(7) . . yes
SI1 C7 1.883(6) . . yes
SI1 C13 1.878(5) . . yes
N1 C23 1.53(1) . . yes
N1 C24 1.50(1) . . yes
N1 C25 1.49(1) . . yes
N1 C26 1.59(2) . . yes
N1 C27 1.48(2) . . yes
N1 C28 1.57(1) . . yes
N1 C29 1.58(2) . . yes
N1 C30 1.53(2) . . yes
C1 C2 1.399(9) . . yes
C1 C6 1.398(9) . . yes
C2 C3 1.41(1) . . yes
C3 C4 1.38(1) . . yes
C4 C5 1.39(1) . . yes
C5 C6 1.39(1) . . yes
C7 C8 1.385(8) . . yes
C7 C12 1.397(8) . . yes
C8 C9 1.38(1) . . yes
C9 C10 1.404(9) . . yes
C10 C11 1.372(9) . . yes
C11 C12 1.39(1) . . yes
C13 C14 1.399(9) . . yes
C13 C18 1.407(7) . . yes
C14 C15 1.396(8) . . yes
C15 C16 1.376(8) . . yes
C16 C17 1.40(1) . . yes
C17 C18 1.378(8) . . yes
C19 C23 1.60(2) . . yes
C19 C24 1.62(1) . . yes
C20 C25 1.63(2) . . yes
C20 C26 1.55(2) . . yes
C21 C27 1.69(1) . . yes
C21 C28 1.61(2) . . yes
C22 C29 1.65(2) . . yes
C22 C30 1.76(2) . . yes
C23 C24 1.80(2) . . yes
C23 C25 1.68(2) . . yes
C24 C30 1.50(2) . . yes
C25 C26 1.79(2) . . yes
C25 C27 1.72(2) . . yes
C26 C28 1.84(2) . . yes
C27 C28 1.85(2) . . yes
C27 C29 1.60(2) . . yes
C28 C30 1.73(2) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
CL1 C23 3.35(1) . 2_768 ?
C9 C9 3.47(2) . 2_757 ?
C10 C16 3.550(10) . 2_657 ?
C15 C22 3.44(1) . 2_667 ?
C18 C25 3.48(2) . 1_554 ?
