#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:23:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179375 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/72/4327205.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_4327205
loop_
_publ_author_name
'Jeremiah S. Duncan'
'Michael J. Zdilla'
'Sonny C. Lee'
_publ_contact_author_address
;                                                                               
 Department of Chemistry
 University of Waterloo
 200 University Avenue West
 Waterloo, Ontario  N2L 3G1
 CANADA  
;
_publ_contact_author_email       sclee@uwaterloo.ca
_publ_contact_author_fax         519-746-0435
_publ_contact_author_name        'Sonny C. Lee'
_publ_contact_author_phone       '519-885-1211 x7501'
_publ_section_title
;
 Synthesis and Elaboration of the Dinuclear Iron-Imide Cluster Core
 [Fe2(μ-NR)2]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1071
_journal_page_last               1080
_journal_paper_doi               10.1021/ic061133+
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'Chemical synthesis, S.C. Lee lab'
_chemical_formula_moiety         '(C8H20N +)2 (Fe 3+)2 (C6H5N 2-)2 (Cl-1)4'
_chemical_formula_structural     (C8H20N)2(Fe2(NC6H5)2Cl4)
_chemical_formula_sum            'C28 H50 Cl4 Fe2 N4'
_chemical_formula_weight         696.22
_chemical_name_common            (NEt4)2[Fe2(mu-NPh)2Cl4]
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 107.954(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2101(10)
_cell_length_b                   13.4726(11)
_cell_length_c                   9.2165(5)
_cell_measurement_reflns_used    4533
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.13
_cell_volume                     1678.5(2)
_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      200(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  0.040
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4533
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple-black
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       needles
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_obs          0.0377
_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)+(0.0454P)²+1.3777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0983
_refine_ls_wR_factor_obs         0.0889
_reflns_number_observed          1367
_reflns_number_total             1736
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic0611332Bsi20060622_121538_03.cif
_cod_data_source_block           (NEt4)2[Fe2(mu-NPh)2Cl4]
_cod_database_code               4327205
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Fe' Fe -0.5000 -0.2873(31) -0.5000 0.028 Uiso 0.0130(9) d SP 2
Cl' Cl -0.4575(29) 0.0000 -0.2931(44) 0.045 Uiso 0.026(2) d SP 2
Fe1 Fe -0.5000 -0.09522(4) -0.5000 0.0278(2) Uani 0.9870(9) d SP .
Cl1 Cl -0.46075(5) -0.19728(6) -0.29376(8) 0.0444(2) Uani 0.9870(9) d P .
N1 N -0.4016(2) 0.0000 -0.4914(3) 0.0305(7) Uani 1 d S .
C1 C -0.3013(2) 0.0000 -0.4688(4) 0.0313(9) Uani 1 d S .
C2 C -0.2480(2) -0.0879(3) -0.4549(4) 0.0532(9) Uani 1 d . .
H2 H -0.2817(2) -0.1496(3) -0.4643(4) 0.064 Uiso 1 calc R .
C3 C -0.1464(3) -0.0869(4) -0.4275(4) 0.0757(13) Uani 1 d . .
H3 H -0.1115(3) -0.1478(4) -0.4196(4) 0.091 Uiso 1 calc R .
C4 C -0.0963(3) 0.0000 -0.4119(5) 0.077(2) Uani 1 d S .
H4 H -0.0264(3) 0.0000 -0.3901(5) 0.093 Uiso 1 calc SR .
N2 N -0.2345(3) -0.0118(24) 0.0548(4) 0.024(4) Uani 0.50 d P -1
C5 C -0.3419(3) 0.0238(4) -0.0135(5) 0.033(2) Uani 0.50 d P -1
H5A H -0.3451(3) 0.0694(4) -0.0990(5) 0.040 Uiso 0.50 calc PR -1
H5B H -0.3839(3) -0.0344(4) -0.0564(5) 0.040 Uiso 0.50 calc PR -1
C6 C -0.3857(4) 0.0763(5) 0.0965(7) 0.0472(15) Uani 0.50 d P -1
H6A H -0.4518(13) 0.1010(26) 0.0409(10) 0.071 Uiso 0.50 calc PR -1
H6B H -0.3431(16) 0.1321(18) 0.1441(35) 0.071 Uiso 0.50 calc PR -1
H6C H -0.3903(27) 0.0296(9) 0.1756(26) 0.071 Uiso 0.50 calc PR -1
C7 C -0.2207(4) -0.0738(4) 0.1964(5) 0.0346(13) Uani 0.50 d P -1
H7A H -0.1515(4) -0.0978(4) 0.2325(5) 0.042 Uiso 0.50 calc PR -1
H7B H -0.2315(4) -0.0313(4) 0.2774(5) 0.042 Uiso 0.50 calc PR -1
C8 C -0.2891(4) -0.1614(4) 0.1722(6) 0.0416(14) Uani 0.50 d P -1
H8A H -0.2695(18) -0.2040(16) 0.2628(19) 0.062 Uiso 0.50 calc PR -1
H8B H -0.2853(22) -0.1993(17) 0.0834(27) 0.062 Uiso 0.50 calc PR -1
H8C H -0.3570(6) -0.1382(5) 0.1548(45) 0.062 Uiso 0.50 calc PR -1
C9 C -0.2095(4) -0.0670(4) -0.0708(6) 0.0323(12) Uani 0.50 d P -1
H9A H -0.2182(4) -0.0214(4) -0.1582(6) 0.039 Uiso 0.50 calc PR -1
H9B H -0.2571(4) -0.1222(4) -0.1056(6) 0.039 Uiso 0.50 calc PR -1
C10 C -0.1049(5) -0.1093(5) -0.0261(7) 0.044(2) Uani 0.50 d P -1
H10A H -0.0922(11) -0.1374(27) -0.1164(11) 0.066 Uiso 0.50 calc PR -1
H10B H -0.0982(10) -0.1615(21) 0.0506(34) 0.066 Uiso 0.50 calc PR -1
H10C H -0.0571(5) -0.0563(8) 0.0163(42) 0.066 Uiso 0.50 calc PR -1
C11 C -0.1669(4) 0.0801(4) 0.1031(6) 0.0351(13) Uani 0.50 d P -1
H11A H -0.1894(4) 0.1188(4) 0.1775(6) 0.042 Uiso 0.50 calc PR -1
H11B H -0.0988(4) 0.0570(4) 0.1560(6) 0.042 Uiso 0.50 calc PR -1
C12 C -0.1635(5) 0.1482(5) -0.0245(6) 0.0436(15) Uani 0.50 d P -1
H12A H -0.1231(26) 0.2065(16) 0.0178(7) 0.065 Uiso 0.50 calc PR -1
H12B H -0.2308(6) 0.1694(25) -0.0812(30) 0.065 Uiso 0.50 calc PR -1
H12C H -0.1343(28) 0.1130(11) -0.0934(26) 0.065 Uiso 0.50 calc PR -1
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'
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
Cl1 Fe' Cl1 112.3(18) 2_454 .
Cl1 Fe' Fe1 56.2(9) 2_454 .
Cl1 Fe' Fe1 56.2(9) . .
Fe1 Cl' Fe1 70.5(11) . 5_454
N1 Fe1 N1 94.02(12) . 5_454
N1 Fe1 Cl' 69.2(9) . 5_454
N1 Fe1 Cl' 64.4(9) 5_454 5_454
N1 Fe1 Cl' 64.4(9) . .
N1 Fe1 Cl' 69.2(9) 5_454 .
Cl' Fe1 Cl' 109.5(12) 5_454 .
N1 Fe1 Cl1 115.83(8) . 2_454
N1 Fe1 Cl1 112.94(8) 5_454 2_454
Cl' Fe1 Cl1 72.5(6) 5_454 2_454
Cl' Fe1 Cl1 177.7(7) . 2_454
N1 Fe1 Cl1 112.94(8) . .
N1 Fe1 Cl1 115.83(8) 5_454 .
Cl' Fe1 Cl1 177.7(7) 5_454 .
Cl' Fe1 Cl1 72.5(6) . .
Cl1 Fe1 Cl1 105.50(4) 2_454 .
N1 Fe1 Fe1 47.01(6) . 5_454
N1 Fe1 Fe1 47.01(6) 5_454 5_454
Cl' Fe1 Fe1 54.7(6) 5_454 5_454
Cl' Fe1 Fe1 54.7(6) . 5_454
Cl1 Fe1 Fe1 127.25(2) 2_454 5_454
Cl1 Fe1 Fe1 127.25(2) . 5_454
N1 Fe1 Fe' 132.99(6) . .
N1 Fe1 Fe' 132.99(6) 5_454 .
Cl' Fe1 Fe' 125.3(6) 5_454 .
Cl' Fe1 Fe' 125.3(6) . .
Cl1 Fe1 Fe' 52.75(2) 2_454 .
Cl1 Fe1 Fe' 52.75(2) . .
Fe1 Fe1 Fe' 180.000(3) 5_454 .
Fe' Cl1 Fe1 71.1(9) . .
C1 N1 Fe1 136.77(6) . .
C1 N1 Fe1 136.77(6) . 5_454
Fe1 N1 Fe1 85.98(12) . 5_454
N1 C1 C2 121.6(2) . 6
N1 C1 C2 121.6(2) . .
C2 C1 C2 116.8(4) 6 .
C3 C2 C1 121.1(4) . .
C4 C3 C2 120.7(4) . .
C3 C4 C3 119.6(5) . 6
C9 N2 C7 113.1(20) . .
C9 N2 C5 106.2(5) . .
C7 N2 C5 112.0(6) . .
C9 N2 C11 110.0(7) . .
C7 N2 C11 106.9(6) . .
C5 N2 C11 108.6(19) . .
C6 C5 N2 115.5(6) . .
C8 C7 N2 113.7(9) . .
N2 C9 C10 114.7(5) . .
C12 C11 N2 115.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe' Cl1 2.18(2) 2_454
Fe' Cl1 2.18(2) .
Fe' Fe1 2.59(4) .
Cl' Fe1 2.22(3) .
Cl' Fe1 2.22(3) 5_454
Fe1 N1 1.881(2) .
Fe1 N1 1.881(2) 5_454
Fe1 Cl' 2.22(3) 5_454
Fe1 Cl1 2.2719(8) 2_454
Fe1 Cl1 2.2719(8) .
Fe1 Fe1 2.5656(11) 5_454
N1 C1 1.375(4) .
N1 Fe1 1.881(2) 5_454
C1 C2 1.390(4) 6
C1 C2 1.390(4) .
C2 C3 1.387(4) .
C3 C4 1.355(5) .
C4 C3 1.355(5) 6
N2 C9 1.51(2) .
N2 C7 1.51(2) .
N2 C5 1.538(11) .
N2 C11 1.55(3) .
C5 C6 1.518(7) .
C7 C8 1.501(8) .
C9 C10 1.525(7) .
C11 C12 1.504(8) .
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_4
Fe1 Cl' Fe1 N1 54.0(5) 5_454 .
Fe1 Cl' Fe1 N1 -51.3(5) 5_454 5_454
Fe1 Cl' Fe1 Cl' 0.001(3) 5_454 5_454
Fe1 Cl' Fe1 Cl1 150.5(216) 5_454 2_454
Fe1 Cl' Fe1 Cl1 -178.8(10) 5_454 .
Fe1 Cl' Fe1 Fe1 0.000(1) 5_454 5_454
Fe1 Cl' Fe1 Fe' 180.000(4) 5_454 .
Cl1 Fe' Fe1 N1 -92.26(12) 2_454 .
Cl1 Fe' Fe1 N1 87.74(12) . .
Cl1 Fe' Fe1 N1 87.74(12) 2_454 5_454
Cl1 Fe' Fe1 N1 -92.26(12) . 5_454
Cl1 Fe' Fe1 Cl' 1.4(12) 2_454 5_454
Cl1 Fe' Fe1 Cl' -178.6(12) . 5_454
Cl1 Fe' Fe1 Cl' -178.6(12) 2_454 .
Cl1 Fe' Fe1 Cl' 1.4(12) . .
Cl1 Fe' Fe1 Cl1 0.000(4) 2_454 2_454
Cl1 Fe' Fe1 Cl1 180.002(2) . 2_454
Cl1 Fe' Fe1 Cl1 179.998(4) 2_454 .
Cl1 Fe' Fe1 Cl1 0.000(2) . .
Cl1 Fe' Fe1 Fe1 -89.1(274) 2_454 5_454
Cl1 Fe' Fe1 Fe1 90.9(310) . 5_454
Cl1 Fe' Cl1 Fe1 -0.002(3) 2_454 .
Fe1 Fe' Cl1 Fe1 0.000(2) . .
N1 Fe1 Cl1 Fe' -127.47(7) . .
N1 Fe1 Cl1 Fe' 125.70(7) 5_454 .
Cl' Fe1 Cl1 Fe' 30.3(231) 5_454 .
Cl' Fe1 Cl1 Fe' -178.8(10) . .
Cl1 Fe1 Cl1 Fe' 0.001(3) 2_454 .
Fe1 Fe1 Cl1 Fe' 180.000(3) 5_454 .
Fe' Fe1 Cl1 Fe' 0.000(3) . .
N1 Fe1 N1 C1 172.5(4) 5_454 .
Cl' Fe1 N1 C1 -126.8(9) 5_454 .
Cl' Fe1 N1 C1 107.9(9) . .
Cl1 Fe1 N1 C1 -69.6(3) 2_454 .
Cl1 Fe1 N1 C1 52.3(3) . .
Fe1 Fe1 N1 C1 172.5(4) 5_454 .
Fe' Fe1 N1 C1 -7.5(4) . .
N1 Fe1 N1 Fe1 0.0 5_454 5_454
Cl' Fe1 N1 Fe1 60.7(8) 5_454 5_454
Cl' Fe1 N1 Fe1 -64.6(8) . 5_454
Cl1 Fe1 N1 Fe1 117.91(7) 2_454 5_454
Cl1 Fe1 N1 Fe1 -120.27(7) . 5_454
Fe1 Fe1 N1 Fe1 0.0 5_454 5_454
Fe' Fe1 N1 Fe1 180.0 . 5_454
Fe1 N1 C1 C2 -173.7(3) . 6
Fe1 N1 C1 C2 -4.6(5) 5_454 6
Fe1 N1 C1 C2 4.6(5) . .
Fe1 N1 C1 C2 173.7(3) 5_454 .
N1 C1 C2 C3 -178.0(3) . .
C2 C1 C2 C3 0.4(6) 6 .
C1 C2 C3 C4 0.7(6) . .
C2 C3 C4 C3 -1.9(7) . 6
C9 N2 C5 C6 176.3(10) . .
C7 N2 C5 C6 52.4(21) . .
C11 N2 C5 C6 -65.4(8) . .
C9 N2 C7 C8 -64.4(6) . .
C5 N2 C7 C8 55.5(19) . .
C11 N2 C7 C8 174.3(7) . .
C7 N2 C9 C10 -56.6(12) . .
C5 N2 C9 C10 -179.8(10) . .
C11 N2 C9 C10 62.9(15) . .
C9 N2 C11 C12 52.2(14) . .
C7 N2 C11 C12 175.4(7) . .
C5 N2 C11 C12 -63.6(6) . .
