#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318283.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_4318283
loop_
_publ_author_name
'Arunashree Panda'
'Matthias Stender'
'Robert J. Wright'
'Marilyn M. Olmstead'
'Peter Klavins'
'Philip P. Power'
_publ_section_title
;
 Synthesis and Characterization of Three-Coordinate and Related
 β-Diketiminate Derivatives of Manganese, Iron, and Cobalt
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3909
_journal_page_last               3916
_journal_paper_doi               10.1021/ic025552s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C34 H14 F20 Fe N4'
_chemical_formula_weight         914.34
_chemical_name_common            '[(F10)NacNac]2Fe'
_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-97
_cell_angle_alpha                100.0590(10)
_cell_angle_beta                 95.2390(10)
_cell_angle_gamma                110.0380(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1625(4)
_cell_length_b                   11.3316(4)
_cell_length_c                   15.9244(6)
_cell_measurement_reflns_used    8034
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.37
_cell_measurement_theta_min      2.33
_cell_volume                     1673.52(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22450
_diffrn_reflns_theta_full        31.46
_diffrn_reflns_theta_max         31.46
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.8885
_exptl_absorpt_correction_T_min  0.8828
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick
using the method described by Blessing, R. H.; Acta Cryst.
A51, 1995, 33.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         10055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0413P)²+0.4302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                8004
_reflns_number_total             10055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025552s_s1_8.cif
_cod_data_source_block           mas73
_cod_database_code               4318283
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.74894(2) 0.84812(2) -0.262897(13) 0.01553(5) Uani 1 1 d . . .
N1 N 0.91019(12) 0.78794(12) -0.23027(8) 0.0167(2) Uani 1 1 d . . .
N2 N 0.77245(13) 0.93861(11) -0.13878(8) 0.0165(2) Uani 1 1 d . . .
C1 C 0.92301(15) 0.75201(13) -0.15526(9) 0.0168(3) Uani 1 1 d . . .
C2 C 0.85545(15) 0.78531(14) -0.08670(9) 0.0177(3) Uani 1 1 d . . .
H2A H 0.8446 0.7348 -0.0443 0.021 Uiso 1 1 calc R . .
C3 C 0.80206(14) 0.88531(13) -0.07402(9) 0.0165(3) Uani 1 1 d . . .
C4 C 1.01788(17) 0.67799(15) -0.13974(10) 0.0214(3) Uani 1 1 d . . .
H4A H 1.1161 0.7382 -0.1204 0.032 Uiso 1 1 calc R . .
H4B H 1.0123 0.6180 -0.1935 0.032 Uiso 1 1 calc R . .
H4C H 0.9869 0.6297 -0.0952 0.032 Uiso 1 1 calc R . .
C5 C 0.78870(16) 0.93812(15) 0.01696(9) 0.0199(3) Uani 1 1 d . . .
H5A H 0.6985 0.9517 0.0169 0.030 Uiso 1 1 calc R . .
H5B H 0.8675 1.0203 0.0404 0.030 Uiso 1 1 calc R . .
H5C H 0.7914 0.8768 0.0529 0.030 Uiso 1 1 calc R . .
C6 C 1.00088(15) 0.77368(14) -0.29038(9) 0.0167(3) Uani 1 1 d . . .
F7 F 1.20860(10) 0.92637(9) -0.20005(6) 0.0256(2) Uani 1 1 d . . .
C7 C 1.14666(15) 0.84521(14) -0.27665(9) 0.0190(3) Uani 1 1 d . . .
F8 F 1.36823(9) 0.91108(10) -0.32473(6) 0.0273(2) Uani 1 1 d . . .
C8 C 1.22975(15) 0.83848(15) -0.33999(10) 0.0207(3) Uani 1 1 d . . .
F9 F 1.24575(10) 0.75158(9) -0.48376(6) 0.02415(19) Uani 1 1 d . . .
C9 C 1.16821(16) 0.75847(15) -0.42052(10) 0.0192(3) Uani 1 1 d . . .
F10 F 0.96424(10) 0.60870(9) -0.51456(6) 0.0256(2) Uani 1 1 d . . .
C10 C 1.02464(16) 0.68626(14) -0.43655(9) 0.0193(3) Uani 1 1 d . . .
C11 C 0.94335(15) 0.69449(14) -0.37242(10) 0.0190(3) Uani 1 1 d . . .
F11 F 0.80421(9) 0.62537(10) -0.39044(6) 0.0276(2) Uani 1 1 d . . .
C12 C 0.76256(15) 1.06204(14) -0.11783(9) 0.0169(3) Uani 1 1 d . . .
F13 F 0.99884(9) 1.15640(9) -0.14160(6) 0.02272(19) Uani 1 1 d . . .
C13 C 0.87859(15) 1.17031(14) -0.12136(9) 0.0176(3) Uani 1 1 d . . .
F14 F 0.98974(10) 1.39397(9) -0.11001(7) 0.0260(2) Uani 1 1 d . . .
C14 C 0.87477(16) 1.29287(14) -0.10582(10) 0.0201(3) Uani 1 1 d . . .
F15 F 0.74637(11) 1.42882(9) -0.07477(7) 0.0282(2) Uani 1 1 d . . .
C15 C 0.75213(17) 1.31095(14) -0.08718(10) 0.0214(3) Uani 1 1 d . . .
F16 F 0.51763(10) 1.22287(10) -0.06107(7) 0.0291(2) Uani 1 1 d . . .
C16 C 0.63535(16) 1.20585(15) -0.08181(10) 0.0211(3) Uani 1 1 d . . .
F17 F 0.52540(9) 0.98434(9) -0.09229(6) 0.02429(19) Uani 1 1 d . . .
C17 C 0.64093(15) 1.08349(14) -0.09750(10) 0.0191(3) Uani 1 1 d . . .
N3 N 0.56629(12) 0.69914(11) -0.31499(8) 0.0163(2) Uani 1 1 d . . .
N4 N 0.74450(13) 0.92914(12) -0.36449(8) 0.0173(2) Uani 1 1 d . . .
C18 C 0.50453(14) 0.66967(14) -0.39734(9) 0.0167(3) Uani 1 1 d . . .
C19 C 0.55220(15) 0.74886(14) -0.45580(9) 0.0180(3) Uani 1 1 d . . .
H19A H 0.5063 0.7135 -0.5141 0.022 Uiso 1 1 calc R . .
C20 C 0.65678(15) 0.87149(14) -0.44072(9) 0.0170(3) Uani 1 1 d . . .
C21 C 0.37554(16) 0.54895(14) -0.43120(10) 0.0215(3) Uani 1 1 d . . .
H21A H 0.3036 0.5469 -0.3939 0.032 Uiso 1 1 calc R . .
H21B H 0.4021 0.4735 -0.4316 0.032 Uiso 1 1 calc R . .
H21C H 0.3369 0.5478 -0.4902 0.032 Uiso 1 1 calc R . .
C22 C 0.66871(16) 0.94197(15) -0.51310(10) 0.0214(3) Uani 1 1 d . . .
H22A H 0.7678 0.9746 -0.5220 0.032 Uiso 1 1 calc R . .
H22B H 0.6367 1.0142 -0.4982 0.032 Uiso 1 1 calc R . .
H22C H 0.6093 0.8830 -0.5663 0.032 Uiso 1 1 calc R . .
C23 C 0.50574(14) 0.61322(14) -0.26166(9) 0.0169(3) Uani 1 1 d . . .
F24 F 0.39090(10) 0.74778(9) -0.19941(6) 0.02478(19) Uani 1 1 d . . .
C24 C 0.42271(15) 0.64177(14) -0.20239(9) 0.0183(3) Uani 1 1 d . . .
F25 F 0.28144(11) 0.59032(10) -0.09490(7) 0.0304(2) Uani 1 1 d . . .
C25 C 0.36489(16) 0.56068(16) -0.14872(10) 0.0218(3) Uani 1 1 d . . .
F26 F 0.33063(12) 0.36734(11) -0.10232(7) 0.0368(3) Uani 1 1 d . . .
C26 C 0.38868(17) 0.44718(16) -0.15289(11) 0.0253(3) Uani 1 1 d . . .
F27 F 0.49001(12) 0.30331(10) -0.21931(8) 0.0352(2) Uani 1 1 d . . .
C27 C 0.46979(17) 0.41545(15) -0.21155(11) 0.0243(3) Uani 1 1 d . . .
F28 F 0.60191(11) 0.46141(10) -0.32243(7) 0.0284(2) Uani 1 1 d . . .
C28 C 0.52757(16) 0.49763(15) -0.26463(10) 0.0206(3) Uani 1 1 d . . .
C29 C 0.83447(15) 1.05974(14) -0.35302(9) 0.0174(3) Uani 1 1 d . . .
F30 F 0.65095(10) 1.13257(9) -0.31752(7) 0.0290(2) Uani 1 1 d . . .
C30 C 0.78719(15) 1.16012(15) -0.32696(10) 0.0197(3) Uani 1 1 d . . .
F31 F 0.82747(11) 1.38163(9) -0.28493(7) 0.0310(2) Uani 1 1 d . . .
C31 C 0.87631(16) 1.28799(15) -0.30987(10) 0.0208(3) Uani 1 1 d . . .
F32 F 1.10464(10) 1.44302(9) -0.30114(6) 0.0276(2) Uani 1 1 d . . .
C32 C 1.01756(16) 1.31907(14) -0.31821(10) 0.0211(3) Uani 1 1 d . . .
F33 F 1.20444(10) 1.25242(10) -0.35542(8) 0.0361(3) Uani 1 1 d . . .
C33 C 1.06791(16) 1.22237(15) -0.34526(11) 0.0228(3) Uani 1 1 d . . .
F34 F 1.02810(10) 1.00262(9) -0.38946(7) 0.0309(2) Uani 1 1 d . . .
C34 C 0.97742(16) 1.09520(14) -0.36219(10) 0.0204(3) Uani 1 1 d . . .
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N4 Fe1 N2 125.03(5) . . ?
N4 Fe1 N3 92.67(5) . . ?
N2 Fe1 N3 118.54(5) . . ?
N4 Fe1 N1 121.00(5) . . ?
N2 Fe1 N1 89.52(5) . . ?
N3 Fe1 N1 112.02(5) . . ?
C1 N1 C6 119.98(12) . . ?
C1 N1 Fe1 120.06(9) . . ?
C6 N1 Fe1 119.72(9) . . ?
C3 N2 C12 118.57(12) . . ?
C3 N2 Fe1 120.73(10) . . ?
C12 N2 Fe1 120.68(9) . . ?
N1 C1 C2 122.48(13) . . ?
N1 C1 C4 120.33(13) . . ?
C2 C1 C4 117.13(13) . . ?
C1 C2 C3 127.14(13) . . ?
N2 C3 C2 122.15(13) . . ?
N2 C3 C5 120.31(13) . . ?
C2 C3 C5 117.40(13) . . ?
C11 C6 C7 115.95(13) . . ?
C11 C6 N1 119.77(12) . . ?
C7 C6 N1 123.92(13) . . ?
F7 C7 C8 118.21(13) . . ?
F7 C7 C6 119.27(13) . . ?
C8 C7 C6 122.49(14) . . ?
F8 C8 C7 120.49(14) . . ?
F8 C8 C9 119.87(13) . . ?
C7 C8 C9 119.61(13) . . ?
F9 C9 C10 119.43(13) . . ?
F9 C9 C8 120.95(13) . . ?
C10 C9 C8 119.61(13) . . ?
F10 C10 C9 119.92(13) . . ?
F10 C10 C11 120.18(13) . . ?
C9 C10 C11 119.90(14) . . ?
F11 C11 C10 118.50(13) . . ?
F11 C11 C6 119.06(13) . . ?
C10 C11 C6 122.43(13) . . ?
C17 C12 C13 116.41(13) . . ?
C17 C12 N2 124.46(13) . . ?
C13 C12 N2 119.06(12) . . ?
F13 C13 C14 118.03(13) . . ?
F13 C13 C12 119.54(12) . . ?
C14 C13 C12 122.42(13) . . ?
F14 C14 C15 120.11(13) . . ?
F14 C14 C13 120.00(13) . . ?
C15 C14 C13 119.89(14) . . ?
F15 C15 C14 120.16(14) . . ?
F15 C15 C16 120.54(13) . . ?
C14 C15 C16 119.30(13) . . ?
F16 C16 C15 119.78(13) . . ?
F16 C16 C17 120.14(14) . . ?
C15 C16 C17 120.08(13) . . ?
F17 C17 C16 118.22(13) . . ?
F17 C17 C12 119.91(13) . . ?
C16 C17 C12 121.87(13) . . ?
C18 N3 C23 117.67(12) . . ?
C18 N3 Fe1 124.84(10) . . ?
C23 N3 Fe1 117.26(9) . . ?
C20 N4 C29 117.95(12) . . ?
C20 N4 Fe1 125.02(10) . . ?
C29 N4 Fe1 116.91(9) . . ?
N3 C18 C19 122.95(13) . . ?
N3 C18 C21 120.21(13) . . ?
C19 C18 C21 116.81(13) . . ?
C20 C19 C18 129.51(14) . . ?
N4 C20 C19 123.02(13) . . ?
N4 C20 C22 119.45(13) . . ?
C19 C20 C22 117.53(13) . . ?
C24 C23 C28 116.42(13) . . ?
C24 C23 N3 121.18(13) . . ?
C28 C23 N3 122.40(13) . . ?
F24 C24 C25 118.20(13) . . ?
F24 C24 C23 119.56(13) . . ?
C25 C24 C23 122.15(14) . . ?
F25 C25 C26 119.97(14) . . ?
F25 C25 C24 119.83(14) . . ?
C26 C25 C24 120.15(14) . . ?
F26 C26 C25 120.30(14) . . ?
F26 C26 C27 120.51(14) . . ?
C25 C26 C27 119.16(14) . . ?
F27 C27 C26 120.38(14) . . ?
F27 C27 C28 119.44(14) . . ?
C26 C27 C28 120.15(14) . . ?
F28 C28 C27 118.24(13) . . ?
F28 C28 C23 119.74(13) . . ?
C27 C28 C23 121.97(14) . . ?
C30 C29 C34 116.31(13) . . ?
C30 C29 N4 121.68(13) . . ?
C34 C29 N4 121.91(13) . . ?
F30 C30 C31 118.45(13) . . ?
F30 C30 C29 119.25(13) . . ?
C31 C30 C29 122.31(13) . . ?
F31 C31 C32 119.65(14) . . ?
F31 C31 C30 120.70(14) . . ?
C32 C31 C30 119.65(14) . . ?
F32 C32 C31 119.84(14) . . ?
F32 C32 C33 120.39(13) . . ?
C31 C32 C33 119.76(14) . . ?
F33 C33 C34 120.27(14) . . ?
F33 C33 C32 119.89(14) . . ?
C34 C33 C32 119.83(13) . . ?
F34 C34 C33 118.89(13) . . ?
F34 C34 C29 118.97(13) . . ?
C33 C34 C29 122.13(14) . . ?
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 N4 1.9991(12) . ?
Fe1 N2 2.0131(12) . ?
Fe1 N3 2.0164(12) . ?
Fe1 N1 2.0382(12) . ?
N1 C1 1.3369(18) . ?
N1 C6 1.4146(18) . ?
N2 C3 1.3432(18) . ?
N2 C12 1.4203(18) . ?
C1 C2 1.406(2) . ?
C1 C4 1.509(2) . ?
C2 C3 1.407(2) . ?
C3 C5 1.505(2) . ?
C6 C11 1.395(2) . ?
C6 C7 1.398(2) . ?
F7 C7 1.3420(17) . ?
C7 C8 1.382(2) . ?
F8 C8 1.3382(17) . ?
C8 C9 1.384(2) . ?
F9 C9 1.3419(16) . ?
C9 C10 1.380(2) . ?
F10 C10 1.3424(17) . ?
C10 C11 1.381(2) . ?
C11 F11 1.3356(17) . ?
C12 C17 1.394(2) . ?
C12 C13 1.394(2) . ?
F13 C13 1.3447(16) . ?
C13 C14 1.382(2) . ?
F14 C14 1.3437(17) . ?
C14 C15 1.380(2) . ?
F15 C15 1.3379(17) . ?
C15 C16 1.386(2) . ?
F16 C16 1.3362(17) . ?
C16 C17 1.387(2) . ?
F17 C17 1.3394(16) . ?
N3 C18 1.3335(19) . ?
N3 C23 1.4218(18) . ?
N4 C20 1.3496(19) . ?
N4 C29 1.4168(18) . ?
C18 C19 1.408(2) . ?
C18 C21 1.505(2) . ?
C19 C20 1.394(2) . ?
C20 C22 1.504(2) . ?
C23 C24 1.390(2) . ?
C23 C28 1.395(2) . ?
F24 C24 1.3411(17) . ?
C24 C25 1.384(2) . ?
F25 C25 1.3393(17) . ?
C25 C26 1.380(2) . ?
F26 C26 1.3380(17) . ?
C26 C27 1.381(2) . ?
F27 C27 1.3420(18) . ?
C27 C28 1.385(2) . ?
F28 C28 1.3394(17) . ?
C29 C30 1.394(2) . ?
C29 C34 1.397(2) . ?
F30 C30 1.3398(16) . ?
C30 C31 1.383(2) . ?
F31 C31 1.3341(17) . ?
C31 C32 1.381(2) . ?
F32 C32 1.3419(17) . ?
C32 C33 1.381(2) . ?
F33 C33 1.3431(17) . ?
C33 C34 1.380(2) . ?
F34 C34 1.3440(17) . ?
