#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:23:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179375 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/72/4327203.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_4327203
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
'(Fe 3+)2 (NC6H5 2-)2 (Cl -)2 (NH2C4H9)2 (C4H8O)2'
_chemical_formula_structural     'Fe2(NC6H5)2Cl2(NC4H9)2(C4H8O)2 '
_chemical_formula_sum            'C28 H48 Cl2 Fe2 N4 O2'
_chemical_formula_weight         655.3
_chemical_name_common            Fe2(mu-NPh)2Cl2(NH2tBu)2.2THF
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.784(2)
_cell_length_b                   8.840(2)
_cell_length_c                   17.492(4)
_cell_measurement_reflns_used    8067
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.16
_cell_volume                     1664.2(6)
_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  0.056
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8067
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.306
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         0.001
_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         0.1319
_refine_ls_wR_factor_obs         0.1163
_reflns_number_observed          2302
_reflns_number_total             3280
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic0611332Bsi20060622_121538_01.cif
_cod_data_source_block           Fe2(mu-NPh)2Cl2(NH2tBu)2.2THF
_cod_original_cell_volume        1664.3(6)
_cod_database_code               4327203
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Fe1 Fe 0.01067(4) 1.14209(5) -0.00678(3) 0.0319(2) Uani 1 d .
Cl1 Cl -0.07286(9) 1.32535(10) -0.08389(6) 0.0518(3) Uani 1 d .
N1 N 0.0893(2) 0.9787(3) -0.05243(15) 0.0316(6) Uani 1 d .
N2 N 0.1411(3) 1.2744(3) 0.0581(2) 0.0337(6) Uani 1 d .
H1 H 0.2018(30) 1.2858(38) 0.0307(19) 0.040 Uiso 1 d .
H2 H 0.0996(32) 1.3594(39) 0.0615(20) 0.040 Uiso 1 d .
O1S O 0.6342(2) 0.6930(3) 0.0253(2) 0.0592(8) Uani 1 d .
C1 C 0.1792(3) 0.9585(3) -0.1049(2) 0.0297(7) Uani 1 d .
C2 C 0.2606(3) 0.8363(4) -0.0986(2) 0.0362(8) Uani 1 d .
H2B H 0.2540(3) 0.7652(4) -0.0583(2) 0.043 Uiso 1 calc R
C3 C 0.3513(3) 0.8173(4) -0.1506(2) 0.0413(8) Uani 1 d .
H3A H 0.4067(3) 0.7339(4) -0.1451(2) 0.050 Uiso 1 calc R
C4 C 0.3622(3) 0.9177(4) -0.2102(2) 0.0402(8) Uani 1 d .
H4A H 0.4245(3) 0.9040(4) -0.2456(2) 0.048 Uiso 1 calc R
C5 C 0.2813(3) 1.0382(4) -0.2175(2) 0.0410(8) Uani 1 d .
H5A H 0.2872(3) 1.1071(4) -0.2589(2) 0.049 Uiso 1 calc R
C6 C 0.1914(3) 1.0602(4) -0.1653(2) 0.0358(8) Uani 1 d .
H6A H 0.1376(3) 1.1452(4) -0.1705(2) 0.043 Uiso 1 calc R
C7 C 0.1948(3) 1.2368(4) 0.1368(2) 0.0412(8) Uani 1 d .
C8 C 0.0908(4) 1.2416(6) 0.1915(2) 0.0702(14) Uani 1 d .
H8A H 0.0452(19) 1.3371(17) 0.1848(13) 0.105 Uiso 1 calc R
H8B H 0.1262(4) 1.2342(36) 0.2444(2) 0.105 Uiso 1 calc R
H8C H 0.0340(17) 1.1567(22) 0.1806(12) 0.105 Uiso 1 calc R
C9 C 0.2518(4) 1.0786(5) 0.1337(2) 0.0615(11) Uani 1 d .
H9A H 0.1860(5) 1.0042(6) 0.1219(16) 0.092 Uiso 1 calc R
H9B H 0.2943(23) 1.0545(14) 0.1835(6) 0.092 Uiso 1 calc R
H9C H 0.3117(20) 1.0757(10) 0.0939(11) 0.092 Uiso 1 calc R
C10 C 0.2936(3) 1.3516(4) 0.1616(2) 0.0469(9) Uani 1 d .
H10A H 0.2559(5) 1.4523(6) 0.1635(13) 0.070 Uiso 1 calc R
H10B H 0.3585(12) 1.3521(20) 0.1249(8) 0.070 Uiso 1 calc R
H10C H 0.3302(16) 1.3247(15) 0.2125(6) 0.070 Uiso 1 calc R
C3S C 0.4643(3) 0.7291(5) 0.0995(2) 0.0546(10) Uani 1 d .
H3SA H 0.3945(3) 0.6718(5) 0.0739(2) 0.066 Uiso 1 calc R
H3SB H 0.4307(3) 0.8052(5) 0.1342(2) 0.066 Uiso 1 calc R
C2S C 0.5549(3) 0.6245(4) 0.1425(2) 0.0467(9) Uani 1 d .
H2SA H 0.6007(3) 0.6778(4) 0.1853(2) 0.056 Uiso 1 calc R
H2SB H 0.5119(3) 0.5357(4) 0.1629(2) 0.056 Uiso 1 calc R
C4S C 0.5423(3) 0.8023(4) 0.0421(2) 0.0433(9) Uani 1 d .
H4SA H 0.4909(3) 0.8292(4) -0.0048(2) 0.052 Uiso 1 calc R
H4SB H 0.5819(3) 0.8953(4) 0.0636(2) 0.052 Uiso 1 calc R
C1S C 0.6396(4) 0.5789(5) 0.0829(2) 0.0626(12) Uani 1 d .
H1SA H 0.7256(4) 0.5687(5) 0.1057(2) 0.075 Uiso 1 calc R
H1SB H 0.6134(4) 0.4803(5) 0.0604(2) 0.075 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'
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'
O O 0.0106 0.0060 '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
N1 Fe1 N1 95.01(10) 3_575 .
N1 Fe1 N2 113.97(11) 3_575 .
N1 Fe1 N2 110.64(11) . .
N1 Fe1 Cl1 121.13(9) 3_575 .
N1 Fe1 Cl1 118.12(9) . .
N2 Fe1 Cl1 98.69(9) . .
N1 Fe1 Fe1 47.55(7) 3_575 3_575
N1 Fe1 Fe1 47.46(7) . 3_575
N2 Fe1 Fe1 124.16(8) . 3_575
Cl1 Fe1 Fe1 137.01(4) . 3_575
C1 N1 Fe1 137.9(2) . 3_575
C1 N1 Fe1 137.1(2) . .
Fe1 N1 Fe1 84.98(10) 3_575 .
C7 N2 Fe1 125.4(2) . .
C1S O1S C4S 109.3(3) . .
N1 C1 C2 120.7(3) . .
N1 C1 C6 121.3(3) . .
C2 C1 C6 118.0(3) . .
C3 C2 C1 120.6(3) . .
C4 C3 C2 121.0(3) . .
C5 C4 C3 119.0(3) . .
C4 C5 C6 120.8(3) . .
C5 C6 C1 120.7(3) . .
N2 C7 C10 109.8(3) . .
N2 C7 C8 108.3(3) . .
C10 C7 C8 109.5(3) . .
N2 C7 C9 107.7(3) . .
C10 C7 C9 110.2(3) . .
C8 C7 C9 111.2(3) . .
C4S C3S C2S 103.0(3) . .
C1S C2S C3S 102.9(3) . .
O1S C4S C3S 105.8(3) . .
O1S C1S C2S 107.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.875(2) 3_575
Fe1 N1 1.878(2) .
Fe1 N2 2.106(3) .
Fe1 Cl1 2.2586(11) .
Fe1 Fe1 2.5354(10) 3_575
N1 C1 1.389(4) .
N1 Fe1 1.875(2) 3_575
N2 C7 1.496(4) .
O1S C1S 1.425(5) .
O1S C4S 1.428(4) .
C1 C2 1.392(4) .
C1 C6 1.400(5) .
C2 C3 1.387(4) .
C3 C4 1.380(5) .
C4 C5 1.377(5) .
C5 C6 1.388(4) .
C7 C10 1.515(5) .
C7 C8 1.520(4) .
C7 C9 1.530(5) .
C3S C4S 1.497(5) .
C3S C2S 1.511(5) .
C2S C1S 1.485(5) .
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
N1 Fe1 N1 C1 -179.7(4) 3_575 .
N2 Fe1 N1 C1 -61.8(3) . .
Cl1 Fe1 N1 C1 50.8(3) . .
Fe1 Fe1 N1 C1 -179.7(4) 3_575 .
N1 Fe1 N1 Fe1 0.0 3_575 3_575
N2 Fe1 N1 Fe1 117.96(11) . 3_575
Cl1 Fe1 N1 Fe1 -129.44(7) . 3_575
Fe1 Fe1 N1 Fe1 0.0 3_575 3_575
N1 Fe1 N2 C7 26.4(3) 3_575 .
N1 Fe1 N2 C7 -79.2(3) . .
Cl1 Fe1 N2 C7 156.2(2) . .
Fe1 Fe1 N2 C7 -27.3(3) 3_575 .
Fe1 N1 C1 C2 -33.0(5) 3_575 .
Fe1 N1 C1 C2 146.6(3) . .
Fe1 N1 C1 C6 147.3(3) 3_575 .
Fe1 N1 C1 C6 -33.1(5) . .
N1 C1 C2 C3 -179.3(3) . .
C6 C1 C2 C3 0.4(5) . .
C1 C2 C3 C4 -0.7(5) . .
C2 C3 C4 C5 0.0(5) . .
C3 C4 C5 C6 1.1(5) . .
C4 C5 C6 C1 -1.4(5) . .
N1 C1 C6 C5 -179.7(3) . .
C2 C1 C6 C5 0.7(5) . .
Fe1 N2 C7 C10 175.0(2) . .
Fe1 N2 C7 C8 -65.5(4) . .
Fe1 N2 C7 C9 54.9(4) . .
C4S C3S C2S C1S -32.5(4) . .
C1S O1S C4S C3S -16.3(4) . .
C2S C3S C4S O1S 30.4(4) . .
C4S O1S C1S C2S -4.9(5) . .
C3S C2S C1S O1S 23.7(4) . .
