#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:26 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179185 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/31/4313142.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_4313142
loop_
_publ_author_name
'Jeremiah S. Duncan'
'Tamim M. Nazif'
'Atul K. Verma'
'Sonny C. Lee'
_publ_section_title
;
 Iron-Arylimide Clusters [Fem(NAr)nCl4]2- (m,n= 2, 2; 3, 4; 4, 4) from a
 Ferric Amide Precursor: Synthesis, Characterization, and Comparison to
 Fe-S Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1211
_journal_page_last               1224
_journal_paper_doi               10.1021/ic025825j
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'Chemical synthesis, S.C. Lee lab'
_chemical_formula_moiety         '(Fe 3+) (Cl 1-) (C6H18NSi2 1-)2 (C4H8O)'
_chemical_formula_structural     Fe(N(SiC3H9)2)2Cl(C4H8O)
_chemical_formula_sum            'C16 H44 Cl Fe N2 O Si4'
_chemical_formula_weight         484.19
_chemical_name_common            FeCl[N(TMS)2]2(THF)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                105.188(2)
_cell_angle_beta                 92.640(2)
_cell_angle_gamma                109.323(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3297(4)
_cell_length_b                   11.4333(6)
_cell_length_c                   15.7784(8)
_cell_measurement_reflns_used    13271
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      1.35
_cell_volume                     1353.88(12)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'CIFTAB, Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      140(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13271
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.35
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       rods
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5535
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.147
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_obs          0.0384
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0456P)²+0.4259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0990
_refine_ls_wR_factor_obs         0.0901
_reflns_number_observed          4188
_reflns_number_total             5535
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic025825j-2_s1_1.cif
_cod_data_source_block           FeCl[N(TMS)2]2(THF)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.4259P] 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^)+(0.0456P)^2^+0.4259P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313142
#BEGIN Tags that were not found in dictionaries:
_expel_crystal_density_method    'not measured'
#END Tags that were not found in dictionaries
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe1 Fe 0.61059(4) 0.26766(3) 0.20769(2) 0.01661(11) Uani 1 d . .
Cl1 Cl 0.76642(9) 0.17850(7) 0.11666(5) 0.0287(2) Uani 1 d . .
Si1 Si 0.73540(9) 0.20231(7) 0.37030(5) 0.0202(2) Uani 1 d . .
Si2 Si 0.37296(9) 0.03952(7) 0.27674(5) 0.0223(2) Uani 1 d . .
Si3 Si 0.61299(8) 0.54016(7) 0.32691(5) 0.0177(2) Uani 1 d . .
Si4 Si 0.82601(8) 0.52760(7) 0.17398(5) 0.0199(2) Uani 1 d . .
O1 O 0.4019(2) 0.2218(2) 0.11559(11) 0.0226(4) Uani 1 d . .
N1 N 0.5603(2) 0.1743(2) 0.29263(13) 0.0173(4) Uani 1 d . .
N2 N 0.6845(2) 0.4526(2) 0.23842(13) 0.0159(4) Uani 1 d . .
C1 C 0.6999(4) 0.2706(3) 0.4863(2) 0.0319(7) Uani 1 d . .
H1A H 0.7908(15) 0.2715(17) 0.5285(2) 0.048 Uiso 1 calc R .
H1B H 0.5879(11) 0.2168(11) 0.4964(4) 0.048 Uiso 1 calc R .
H1C H 0.7025(24) 0.3593(7) 0.4949(4) 0.048 Uiso 1 calc R .
C2 C 0.7827(4) 0.0510(3) 0.3629(2) 0.0316(7) Uani 1 d . .
H2A H 0.8875(13) 0.0721(4) 0.4036(9) 0.047 Uiso 1 calc R .
H2B H 0.7992(23) 0.0135(10) 0.3021(3) 0.047 Uiso 1 calc R .
H2C H 0.6862(11) -0.0117(7) 0.3792(12) 0.047 Uiso 1 calc R .
C3 C 0.9349(3) 0.3221(3) 0.3509(2) 0.0276(6) Uani 1 d . .
H3A H 1.0296(6) 0.3405(14) 0.3973(7) 0.041 Uiso 1 calc R .
H3B H 0.9153(8) 0.4025(7) 0.3524(12) 0.041 Uiso 1 calc R .
H3C H 0.9643(13) 0.2862(8) 0.2928(6) 0.041 Uiso 1 calc R .
C4 C 0.3892(4) -0.1032(3) 0.1912(2) 0.0329(7) Uani 1 d . .
H4A H 0.2838(11) -0.1785(6) 0.1830(9) 0.049 Uiso 1 calc R .
H4B H 0.4880(15) -0.1228(12) 0.2111(6) 0.049 Uiso 1 calc R .
H4C H 0.4044(25) -0.0829(7) 0.1348(4) 0.049 Uiso 1 calc R .
C5 C 0.3277(4) -0.0057(3) 0.3813(2) 0.0379(8) Uani 1 d . .
H5A H 0.2244(15) -0.0839(11) 0.3684(3) 0.057 Uiso 1 calc R .
H5B H 0.3093(25) 0.0656(8) 0.4249(5) 0.057 Uiso 1 calc R .
H5C H 0.4257(12) -0.0225(19) 0.4054(7) 0.057 Uiso 1 calc R .
C6 C 0.1770(3) 0.0678(3) 0.2393(2) 0.0294(7) Uani 1 d . .
H6A H 0.0745(3) -0.0067(8) 0.2376(11) 0.044 Uiso 1 calc R .
H6B H 0.1828(11) 0.0789(17) 0.1798(5) 0.044 Uiso 1 calc R .
H6C H 0.1707(12) 0.1462(10) 0.2807(7) 0.044 Uiso 1 calc R .
C7 C 0.5190(3) 0.6534(3) 0.2949(2) 0.0260(6) Uani 1 d . .
H7A H 0.6114(4) 0.7355(7) 0.2992(11) 0.039 Uiso 1 calc R .
H7B H 0.4374(17) 0.6699(13) 0.3350(7) 0.039 Uiso 1 calc R .
H7C H 0.4592(19) 0.6141(8) 0.2338(4) 0.039 Uiso 1 calc R .
C8 C 0.7920(3) 0.6392(3) 0.4211(2) 0.0286(6) Uani 1 d . .
H8A H 0.7501(7) 0.6920(14) 0.4678(6) 0.043 Uiso 1 calc R .
H8B H 0.8869(10) 0.6960(13) 0.3997(3) 0.043 Uiso 1 calc R .
H8C H 0.8326(16) 0.5814(3) 0.4450(8) 0.043 Uiso 1 calc R .
C9 C 0.4374(3) 0.4300(3) 0.3690(2) 0.0234(6) Uani 1 d . .
H9A H 0.4085(15) 0.4805(4) 0.4226(7) 0.035 Uiso 1 calc R .
H9B H 0.4757(8) 0.3641(10) 0.3831(11) 0.035 Uiso 1 calc R .
H9C H 0.3357(8) 0.3876(13) 0.3234(5) 0.035 Uiso 1 calc R .
C10 C 1.0425(3) 0.5175(3) 0.1942(2) 0.0347(7) Uani 1 d . .
H10A H 1.1174(8) 0.5584(17) 0.1560(10) 0.052 Uiso 1 calc R .
H10B H 1.0317(5) 0.4263(3) 0.1806(13) 0.052 Uiso 1 calc R .
H10C H 1.0922(11) 0.5625(16) 0.2565(4) 0.052 Uiso 1 calc R .
C11 C 0.7394(4) 0.4535(3) 0.0532(2) 0.0340(7) Uani 1 d . .
H11A H 0.8252(11) 0.4916(14) 0.0182(2) 0.051 Uiso 1 calc R .
H11B H 0.6341(14) 0.4704(16) 0.0409(3) 0.051 Uiso 1 calc R .
H11C H 0.7135(23) 0.3597(4) 0.0372(3) 0.051 Uiso 1 calc R .
C12 C 0.8658(4) 0.7054(3) 0.1980(2) 0.0277(6) Uani 1 d . .
H12A H 0.9539(17) 0.7430(4) 0.1640(9) 0.042 Uiso 1 calc R .
H12B H 0.9052(21) 0.7486(4) 0.2615(3) 0.042 Uiso 1 calc R .
H12C H 0.7589(7) 0.7173(3) 0.1809(11) 0.042 Uiso 1 calc R .
C13 C 0.3494(4) 0.1143(3) 0.0325(2) 0.0303(7) Uani 1 d D .
H13A H 0.2640(4) 0.0356(3) 0.0410(2) 0.036 Uiso 0.519(8) calc PR 1
H13B H 0.4499(4) 0.0935(3) 0.0119(2) 0.036 Uiso 0.519(8) calc PR 1
H13C H 0.3370(4) 0.0308(3) 0.0439(2) 0.036 Uiso 0.481(8) d PR 2
H13D H 0.4331(4) 0.1303(3) -0.0094(2) 0.036 Uiso 0.481(8) d PR 2
C14 C 0.2708(7) 0.1626(5) -0.0338(3) 0.023(2) Uani 0.519(8) d PD 1
H14A H 0.1841(7) 0.0900(5) -0.0800(3) 0.027 Uiso 0.519(8) calc PR 1
H14B H 0.3599(7) 0.2138(5) -0.0625(3) 0.027 Uiso 0.519(8) calc PR 1
C14' C 0.1719(7) 0.1113(5) -0.0046(4) 0.032(2) Uani 0.481(8) d PD 2
H14C H 0.1510(7) 0.0789(5) -0.0703(4) 0.038 Uiso 0.481(8) calc PR 2
H14D H 0.0777(7) 0.0560(5) 0.0192(4) 0.038 Uiso 0.481(8) calc PR 2
C15 C 0.1867(3) 0.2484(3) 0.0267(2) 0.0344(7) Uani 1 d D .
H15A H 0.1817(3) 0.3187(3) 0.0021(2) 0.041 Uiso 0.519(8) calc PR 1
H15B H 0.0684(3) 0.1960(3) 0.0319(2) 0.041 Uiso 0.519(8) calc PR 1
H15C H 0.0721(3) 0.2554(3) 0.0323(2) 0.041 Uiso 0.481(8) d PR 2
H15D H 0.2399(3) 0.2952(3) -0.0154(2) 0.041 Uiso 0.481(8) d PR 2
C16 C 0.2996(3) 0.3046(3) 0.1166(2) 0.0269(6) Uani 1 d D .
H16A H 0.3751(3) 0.3955(3) 0.1249(2) 0.032 Uiso 1 calc R .
H16B H 0.2284(3) 0.3024(3) 0.1651(2) 0.032 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
_geom_angle_publ_flag
N1 Fe1 N2 123.16(9) . . ?
N1 Fe1 O1 112.54(8) . . ?
N2 Fe1 O1 98.96(8) . . ?
N1 Fe1 Cl1 106.49(7) . . ?
N2 Fe1 Cl1 114.96(6) . . ?
O1 Fe1 Cl1 97.61(5) . . ?
N1 Si1 C3 110.86(11) . . ?
N1 Si1 C1 111.66(11) . . ?
C3 Si1 C1 106.89(13) . . ?
N1 Si1 C2 111.93(12) . . ?
C3 Si1 C2 106.41(13) . . ?
C1 Si1 C2 108.83(14) . . ?
N1 Si2 C6 112.64(12) . . ?
N1 Si2 C5 112.66(12) . . ?
C6 Si2 C5 104.45(14) . . ?
N1 Si2 C4 110.05(11) . . ?
C6 Si2 C4 108.05(13) . . ?
C5 Si2 C4 108.72(15) . . ?
N2 Si3 C9 111.14(11) . . ?
N2 Si3 C8 111.35(11) . . ?
C9 Si3 C8 108.41(12) . . ?
N2 Si3 C7 112.75(11) . . ?
C9 Si3 C7 105.29(12) . . ?
C8 Si3 C7 107.61(13) . . ?
N2 Si4 C10 111.65(12) . . ?
N2 Si4 C11 110.95(12) . . ?
C10 Si4 C11 109.29(15) . . ?
N2 Si4 C12 113.57(11) . . ?
C10 Si4 C12 105.12(13) . . ?
C11 Si4 C12 105.93(13) . . ?
C16 O1 C13 110.1(2) . . ?
C16 O1 Fe1 123.75(13) . . ?
C13 O1 Fe1 125.45(15) . . ?
Si2 N1 Si1 120.50(12) . . ?
Si2 N1 Fe1 122.05(11) . . ?
Si1 N1 Fe1 115.17(10) . . ?
Si3 N2 Si4 122.43(12) . . ?
Si3 N2 Fe1 120.87(11) . . ?
Si4 N2 Fe1 116.69(11) . . ?
O1 C13 C14 105.1(2) . . ?
O1 C13 C14' 103.9(3) . . ?
C13 C14 C15 101.5(3) . . ?
C15 C14' C13 103.3(3) . . ?
C14' C15 C16 105.9(3) . . ?
C16 C15 C14 106.0(2) . . ?
O1 C16 C15 105.2(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.902(2) . ?
Fe1 N2 1.913(2) . ?
Fe1 O1 2.043(2) . ?
Fe1 Cl1 2.2510(7) . ?
Si1 N1 1.747(2) . ?
Si1 C3 1.868(3) . ?
Si1 C1 1.872(3) . ?
Si1 C2 1.874(3) . ?
Si2 N1 1.744(2) . ?
Si2 C6 1.865(3) . ?
Si2 C5 1.873(3) . ?
Si2 C4 1.874(3) . ?
Si3 N2 1.745(2) . ?
Si3 C9 1.864(3) . ?
Si3 C8 1.874(3) . ?
Si3 C7 1.877(3) . ?
Si4 N2 1.748(2) . ?
Si4 C10 1.863(3) . ?
Si4 C11 1.869(3) . ?
Si4 C12 1.877(3) . ?
O1 C16 1.467(3) . ?
O1 C13 1.472(3) . ?
C13 C14 1.519(4) . ?
C13 C14' 1.552(4) . ?
C14 C15 1.545(4) . ?
C14' C15 1.476(4) . ?
C15 C16 1.520(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Fe1 O1 C16 103.0(2) . . . . ?
N2 Fe1 O1 C16 -28.7(2) . . . . ?
Cl1 Fe1 O1 C16 -145.5(2) . . . . ?
N1 Fe1 O1 C13 -87.2(2) . . . . ?
N2 Fe1 O1 C13 141.1(2) . . . . ?
Cl1 Fe1 O1 C13 24.2(2) . . . . ?
C6 Si2 N1 Si1 151.18(14) . . . . ?
C5 Si2 N1 Si1 33.3(2) . . . . ?
C4 Si2 N1 Si1 -88.2(2) . . . . ?
C6 Si2 N1 Fe1 -46.8(2) . . . . ?
C5 Si2 N1 Fe1 -164.66(14) . . . . ?
C4 Si2 N1 Fe1 73.8(2) . . . . ?
C3 Si1 N1 Si2 163.78(14) . . . . ?
C1 Si1 N1 Si2 -77.2(2) . . . . ?
C2 Si1 N1 Si2 45.1(2) . . . . ?
C3 Si1 N1 Fe1 0.6(2) . . . . ?
C1 Si1 N1 Fe1 119.65(14) . . . . ?
C2 Si1 N1 Fe1 -118.05(14) . . . . ?
N2 Fe1 N1 Si2 132.18(12) . . . . ?
O1 Fe1 N1 Si2 14.0(2) . . . . ?
Cl1 Fe1 N1 Si2 -91.84(12) . . . . ?
N2 Fe1 N1 Si1 -64.91(14) . . . . ?
O1 Fe1 N1 Si1 176.88(10) . . . . ?
Cl1 Fe1 N1 Si1 71.07(12) . . . . ?
C9 Si3 N2 Si4 170.66(13) . . . . ?
C8 Si3 N2 Si4 -68.4(2) . . . . ?
C7 Si3 N2 Si4 52.7(2) . . . . ?
C9 Si3 N2 Fe1 -9.6(2) . . . . ?
C8 Si3 N2 Fe1 111.42(14) . . . . ?
C7 Si3 N2 Fe1 -127.52(13) . . . . ?
C10 Si4 N2 Si3 110.0(2) . . . . ?
C11 Si4 N2 Si3 -127.9(2) . . . . ?
C12 Si4 N2 Si3 -8.7(2) . . . . ?
C10 Si4 N2 Fe1 -69.8(2) . . . . ?
C11 Si4 N2 Fe1 52.3(2) . . . . ?
C12 Si4 N2 Fe1 171.53(12) . . . . ?
N1 Fe1 N2 Si3 -32.3(2) . . . . ?
O1 Fe1 N2 Si3 92.21(12) . . . . ?
Cl1 Fe1 N2 Si3 -165.00(9) . . . . ?
N1 Fe1 N2 Si4 147.49(11) . . . . ?
O1 Fe1 N2 Si4 -88.00(12) . . . . ?
Cl1 Fe1 N2 Si4 14.79(13) . . . . ?
C16 O1 C13 C14 24.2(3) . . . . ?
Fe1 O1 C13 C14 -146.8(3) . . . . ?
C16 O1 C13 C14' -16.9(4) . . . . ?
Fe1 O1 C13 C14' 172.1(3) . . . . ?
O1 C13 C14 C15 -33.7(4) . . . . ?
C14' C13 C14 C15 60.0(3) . . . . ?
O1 C13 C14' C15 31.1(5) . . . . ?
C14 C13 C14' C15 -65.9(4) . . . . ?
C13 C14' C15 C16 -33.8(5) . . . . ?
C13 C14' C15 C14 62.4(3) . . . . ?
C13 C14 C15 C14' -64.0(4) . . . . ?
C13 C14 C15 C16 31.9(4) . . . . ?
C13 O1 C16 C15 -3.6(3) . . . . ?
Fe1 O1 C16 C15 167.6(2) . . . . ?
C14' C15 C16 O1 23.9(4) . . . . ?
C14 C15 C16 O1 -18.1(4) . . . . ?
