#------------------------------------------------------------------------------
#$Date: 2015-07-09 00:46:09 +0300 (Thu, 09 Jul 2015) $
#$Revision: 141379 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/59/4085925.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_4085925
loop_
_publ_author_name
'Lichtenberg, Crispin'
'Adelhardt, Mario'
'Wörle, Michael'
'Büttner, Torsten'
'Meyer, Karsten'
'Grützmacher, Hansjörg'
_publ_section_title
;
 Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by
 an Amidinato-diolefin Ligand: Characterization and Catalytic Application
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3079
_journal_paper_doi               10.1021/acs.organomet.5b00395
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C37 H27 Br3 Fe2 N2'
_chemical_formula_sum            'C37 H27 Br3 Fe2 N2'
_chemical_formula_weight         851.04
_chemical_name_systematic
; 
 ? 
;
_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                 113.228(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8426(8)
_cell_length_b                   17.7906(7)
_cell_length_c                   13.3967(6)
_cell_measurement_reflns_used    4567
_cell_measurement_temperature    105.4(2)
_cell_measurement_theta_max      30.0800
_cell_measurement_theta_min      3.2450
_cell_volume                     3250.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      105.4(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω and π 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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11621
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         30.71
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    4.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.2300
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.0700
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0179P)²+6.7078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                3725
_reflns_number_total             4432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00395_si_003.cif
_cod_data_source_block           Compound_9
_cod_depositor_comments
'Adding full bibliography for 4085916--4085926.cif.'
_cod_database_code               4085925
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C8 C 0.68454(16) 0.30700(15) 0.14974(18) 0.0288(5) Uani 1 1 d .
H8 H 0.6744 0.2571 0.1221 0.035 Uiso 1 1 calc R
C1 C 0.84978(15) 0.26633(12) 0.28504(17) 0.0182(4) Uani 1 1 d .
H1 H 0.8310 0.2210 0.2370 0.022 Uiso 1 1 calc R
C7 C 0.76976(15) 0.32437(13) 0.23902(16) 0.0193(4) Uani 1 1 d .
C6 C 0.78196(16) 0.39713(12) 0.28221(17) 0.0214(4) Uani 1 1 d .
C9 C 0.61446(18) 0.36135(19) 0.10073(19) 0.0386(7) Uani 1 1 d .
H9 H 0.5556 0.3484 0.0412 0.046 Uiso 1 1 calc R
C11 C 0.71257(19) 0.45202(15) 0.2278(2) 0.0334(6) Uani 1 1 d .
H11 H 0.7227 0.5024 0.2532 0.040 Uiso 1 1 calc R
C10 C 0.62977(19) 0.43405(18) 0.1379(2) 0.0405(7) Uani 1 1 d .
H10 H 0.5833 0.4719 0.1016 0.049 Uiso 1 1 calc R
C2 C 0.86179(15) 0.24282(13) 0.39776(18) 0.0221(4) Uani 1 1 d .
C3 C 0.89503(16) 0.29393(14) 0.48413(17) 0.0254(5) Uani 1 1 d .
C5 C 0.86147(16) 0.41889(13) 0.38469(19) 0.0253(5) Uani 1 1 d .
H5 H 0.8807 0.4702 0.3915 0.030 Uiso 1 1 calc R
C4 C 0.91103(17) 0.37372(14) 0.47145(18) 0.0263(5) Uani 1 1 d .
H4 H 0.9621 0.3970 0.5307 0.032 Uiso 1 1 calc R
C15 C 0.83810(18) 0.16997(14) 0.4158(2) 0.0337(6) Uani 1 1 d .
H15 H 0.8147 0.1354 0.3571 0.040 Uiso 1 1 calc R
C12 C 0.90823(18) 0.26821(18) 0.5880(2) 0.0385(7) Uani 1 1 d .
H12 H 0.9345 0.3013 0.6483 0.046 Uiso 1 1 calc R
C13 C 0.8838(2) 0.1960(2) 0.6041(2) 0.0492(9) Uani 1 1 d .
H13 H 0.8917 0.1801 0.6747 0.059 Uiso 1 1 calc R
C14 C 0.8482(2) 0.14714(18) 0.5188(3) 0.0468(8) Uani 1 1 d .
H14 H 0.8304 0.0975 0.5299 0.056 Uiso 1 1 calc R
N1 N 0.94030(12) 0.29824(9) 0.28117(13) 0.0160(3) Uani 1 1 d .
C16 C 1.0000 0.25815(15) 0.2500 0.0123(5) Uani 1 2 d S
Fe1 Fe 1.00601(2) 0.387971(17) 0.36836(2) 0.01915(7) Uani 1 1 d .
C17 C 1.0000 0.17439(16) 0.2500 0.0154(5) Uani 1 2 d S
C18 C 1.06997(15) 0.13567(12) 0.33533(17) 0.0201(4) Uani 1 1 d .
H18 H 1.1176 0.1623 0.3938 0.024 Uiso 1 1 calc R
C19 C 1.06989(18) 0.05788(13) 0.3347(2) 0.0291(5) Uani 1 1 d .
H19 H 1.1180 0.0310 0.3925 0.035 Uiso 1 1 calc R
C20 C 1.0000 0.01926(19) 0.2500 0.0325(8) Uani 1 2 d S
H20 H 1.0000 -0.0341 0.2500 0.039 Uiso 1 2 calc SR
Br1 Br 1.162408(17) 0.387651(14) 0.513445(19) 0.02954(7) Uani 1 1 d .
Br2 Br 1.0000 0.499010(18) 0.2500 0.02899(8) Uani 1 2 d S
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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
C9 C8 C7 120.8(2) . .
C9 C8 H8 119.6 . .
C7 C8 H8 119.6 . .
N1 C1 C2 113.04(17) . .
N1 C1 C7 107.61(17) . .
C2 C1 C7 111.21(16) . .
N1 C1 H1 108.3 . .
C2 C1 H1 108.3 . .
C7 C1 H1 108.3 . .
C8 C7 C6 119.1(2) . .
C8 C7 C1 120.1(2) . .
C6 C7 C1 120.72(18) . .
C11 C6 C7 118.8(2) . .
C11 C6 C5 117.4(2) . .
C7 C6 C5 123.8(2) . .
C10 C9 C8 120.1(2) . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
C10 C11 C6 120.9(3) . .
C10 C11 H11 119.5 . .
C6 C11 H11 119.5 . .
C9 C10 C11 120.0(2) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C15 C2 C3 119.5(2) . .
C15 C2 C1 119.7(2) . .
C3 C2 C1 120.77(19) . .
C2 C3 C12 118.3(2) . .
C2 C3 C4 123.8(2) . .
C12 C3 C4 117.8(2) . .
C4 C5 C6 127.3(2) . .
C4 C5 Fe1 74.42(13) . .
C6 C5 Fe1 106.47(14) . .
C4 C5 H5 116.3 . .
C6 C5 H5 116.3 . .
Fe1 C5 H5 89.0 . .
C5 C4 C3 127.8(2) . .
C5 C4 Fe1 71.46(13) . .
C3 C4 Fe1 109.69(14) . .
C5 C4 H4 116.1 . .
C3 C4 H4 116.1 . .
Fe1 C4 H4 88.8 . .
C14 C15 C2 120.7(3) . .
C14 C15 H15 119.6 . .
C2 C15 H15 119.6 . .
C13 C12 C3 121.2(3) . .
C13 C12 H12 119.4 . .
C3 C12 H12 119.4 . .
C14 C13 C12 120.2(2) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C13 C14 C15 120.0(3) . .
C13 C14 H14 120.0 . .
C15 C14 H14 120.0 . .
C16 N1 C1 122.26(17) . .
C16 N1 Fe1 112.46(13) . .
C1 N1 Fe1 121.94(12) . .
N1 C16 N1 115.0(2) . 2_755
N1 C16 C17 122.52(12) . .
N1 C16 C17 122.51(12) 2_755 .
N1 Fe1 C5 89.32(7) . .
N1 Fe1 C4 89.40(7) . .
C5 Fe1 C4 34.12(8) . .
N1 Fe1 Br1 125.05(5) . .
C5 Fe1 Br1 124.74(6) . .
C4 Fe1 Br1 97.98(6) . .
N1 Fe1 Br2 111.89(5) . .
C5 Fe1 Br2 93.99(6) . .
C4 Fe1 Br2 125.24(6) . .
Br1 Fe1 Br2 107.410(13) . .
C18 C17 C18 120.4(3) 2_755 .
C18 C17 C16 119.78(14) 2_755 .
C18 C17 C16 119.78(14) . .
C19 C18 C17 119.5(2) . .
C19 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
C20 C19 C18 120.1(2) . .
C20 C19 H19 120.0 . .
C18 C19 H19 120.0 . .
C19 C20 C19 120.3(3) . 2_755
C19 C20 H20 119.8 . .
C19 C20 H20 119.8 2_755 .
Fe1 Br2 Fe1 76.329(16) 2_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C8 C9 1.382(4) .
C8 C7 1.390(3) .
C8 H8 0.9500 .
C1 N1 1.478(3) .
C1 C2 1.508(3) .
C1 C7 1.510(3) .
C1 H1 1.0000 .
C7 C6 1.400(3) .
C6 C11 1.398(3) .
C6 C5 1.466(3) .
C9 C10 1.372(4) .
C9 H9 0.9500 .
C11 C10 1.377(4) .
C11 H11 0.9500 .
C10 H10 0.9500 .
C2 C15 1.389(3) .
C2 C3 1.399(3) .
C3 C12 1.404(3) .
C3 C4 1.460(3) .
C5 C4 1.365(3) .
C5 Fe1 2.307(2) .
C5 H5 0.9500 .
C4 Fe1 2.344(2) .
C4 H4 0.9500 .
C15 C14 1.388(4) .
C15 H15 0.9500 .
C12 C13 1.374(4) .
C12 H12 0.9500 .
C13 C14 1.366(5) .
C13 H13 0.9500 .
C14 H14 0.9500 .
N1 C16 1.327(2) .
N1 Fe1 1.9914(16) .
C16 N1 1.327(2) 2_755
C16 C17 1.490(4) .
Fe1 Br1 2.3681(4) .
Fe1 Br2 2.5125(4) .
C17 C18 1.387(2) 2_755
C17 C18 1.387(2) .
C18 C19 1.384(3) .
C18 H18 0.9500 .
C19 C20 1.381(3) .
C19 H19 0.9500 .
C20 C19 1.381(3) 2_755
C20 H20 0.9500 .
Br2 Fe1 2.5125(4) 2_755
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
C9 C8 C7 C6 2.9(3) . .
C9 C8 C7 C1 -174.2(2) . .
N1 C1 C7 C8 121.8(2) . .
C2 C1 C7 C8 -113.9(2) . .
N1 C1 C7 C6 -55.3(2) . .
C2 C1 C7 C6 69.0(2) . .
C8 C7 C6 C11 -6.2(3) . .
C1 C7 C6 C11 170.94(19) . .
C8 C7 C6 C5 170.9(2) . .
C1 C7 C6 C5 -11.9(3) . .
C7 C8 C9 C10 2.0(3) . .
C7 C6 C11 C10 4.8(3) . .
C5 C6 C11 C10 -172.5(2) . .
C8 C9 C10 C11 -3.5(4) . .
C6 C11 C10 C9 0.1(4) . .
N1 C1 C2 C15 -125.7(2) . .
C7 C1 C2 C15 113.1(2) . .
N1 C1 C2 C3 55.3(3) . .
C7 C1 C2 C3 -65.8(2) . .
C15 C2 C3 C12 3.4(3) . .
C1 C2 C3 C12 -177.7(2) . .
C15 C2 C3 C4 -172.7(2) . .
C1 C2 C3 C4 6.3(3) . .
C11 C6 C5 C4 150.6(2) . .
C7 C6 C5 C4 -26.5(3) . .
C11 C6 C5 Fe1 -126.64(18) . .
C7 C6 C5 Fe1 56.2(2) . .
C6 C5 C4 C3 -1.9(4) . .
Fe1 C5 C4 C3 -100.9(2) . .
C6 C5 C4 Fe1 99.1(2) . .
C2 C3 C4 C5 31.7(4) . .
C12 C3 C4 C5 -144.4(2) . .
C2 C3 C4 Fe1 -49.7(3) . .
C12 C3 C4 Fe1 134.26(18) . .
C3 C2 C15 C14 -0.8(3) . .
C1 C2 C15 C14 -179.8(2) . .
C2 C3 C12 C13 -3.8(3) . .
C4 C3 C12 C13 172.5(2) . .
C3 C12 C13 C14 1.6(4) . .
C12 C13 C14 C15 1.0(4) . .
C2 C15 C14 C13 -1.4(4) . .
C2 C1 N1 C16 99.4(2) . .
C7 C1 N1 C16 -137.39(16) . .
C2 C1 N1 Fe1 -58.4(2) . .
C7 C1 N1 Fe1 64.80(19) . .
C1 N1 C16 N1 160.21(19) . 2_755
Fe1 N1 C16 N1 -40.08(6) . 2_755
C1 N1 C16 C17 -19.78(19) . .
Fe1 N1 C16 C17 139.92(6) . .
C16 N1 Fe1 C5 -179.76(13) . .
C1 N1 Fe1 C5 -19.98(15) . .
C16 N1 Fe1 C4 -145.64(13) . .
C1 N1 Fe1 C4 14.14(15) . .
C16 N1 Fe1 Br1 -46.30(14) . .
C1 N1 Fe1 Br1 113.48(14) . .
C16 N1 Fe1 Br2 86.22(12) . .
C1 N1 Fe1 Br2 -114.00(14) . .
C4 C5 Fe1 N1 89.95(14) . .
C6 C5 Fe1 N1 -35.09(15) . .
C6 C5 Fe1 C4 -125.0(2) . .
C4 C5 Fe1 Br1 -43.74(16) . .
C6 C5 Fe1 Br1 -168.77(12) . .
C4 C5 Fe1 Br2 -158.15(13) . .
C6 C5 Fe1 Br2 76.81(15) . .
C5 C4 Fe1 N1 -89.66(14) . .
C3 C4 Fe1 N1 34.90(15) . .
C3 C4 Fe1 C5 124.6(2) . .
C5 C4 Fe1 Br1 144.99(13) . .
C3 C4 Fe1 Br1 -90.44(15) . .
C5 C4 Fe1 Br2 27.03(16) . .
C3 C4 Fe1 Br2 151.60(13) . .
N1 C16 C17 C18 80.84(13) . 2_755
N1 C16 C17 C18 -99.16(13) 2_755 2_755
N1 C16 C17 C18 -99.16(13) . .
N1 C16 C17 C18 80.84(13) 2_755 .
C18 C17 C18 C19 0.29(15) 2_755 .
C16 C17 C18 C19 -179.71(15) . .
C17 C18 C19 C20 -0.6(3) . .
C18 C19 C20 C19 0.30(15) . 2_755
N1 Fe1 Br2 Fe1 -27.52(5) . 2_755
C5 Fe1 Br2 Fe1 -118.38(6) . 2_755
C4 Fe1 Br2 Fe1 -133.19(7) . 2_755
Br1 Fe1 Br2 Fe1 113.260(17) . 2_755
