#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:33:33 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179251 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/71/4317177.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_4317177
loop_
_publ_author_name
'Christopher J. Whiteoak'
'Rafael Torres Martin de Rosales'
'Andrew J. P. White'
'George J. P. Britovsek'
_publ_section_title
;
 Iron(II) Complexes with Tetradentate Bis(aminophenolate) Ligands:
 Synthesis and Characterization, Solution Behavior, and Reactivity with O2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11106
_journal_page_last               11117
_journal_paper_doi               10.1021/ic1016998
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C46 H54 Fe2 N6 O5, 2(C5 H5 N)'
_chemical_formula_sum            'C56 H64 Fe2 N8 O5'
_chemical_formula_weight         1040.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6514(4)
_cell_length_b                   12.1264(3)
_cell_length_c                   23.1478(4)
_cell_measurement_reflns_used    6659
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.1294
_cell_measurement_theta_min      2.3670
_cell_volume                     5235.44(19)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13032
_diffrn_reflns_theta_full        71.00
_diffrn_reflns_theta_max         71.55
_diffrn_reflns_theta_min         3.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.888
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) 
(compiled Jan  8 2009,16:24:04) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Red/brown
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0324
_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)+(0.0623P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                3927
_reflns_number_total             4981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016998_si_001_6.cif
_cod_data_source_block           '[{Fe(SalanH)(Py)}2(mu-O)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317177
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-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_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
Fe Fe 0.593780(15) 0.20843(2) 0.264894(12) 0.02704(10) Uani 1 1 d . . .
O O 0.5000 0.20288(15) 0.2500 0.0336(4) Uani 1 2 d S . .
O1 O 0.58727(7) 0.09560(11) 0.32505(6) 0.0347(3) Uani 1 1 d . . .
C1 C 0.62905(10) 0.02868(16) 0.35563(8) 0.0323(4) Uani 1 1 d . . .
C2 C 0.60102(11) -0.07036(17) 0.37713(9) 0.0387(5) Uani 1 1 d . . .
H2A H 0.5532 -0.0906 0.3678 0.046 Uiso 1 1 calc R . .
C3 C 0.64164(12) -0.13897(18) 0.41160(9) 0.0433(5) Uani 1 1 d . . .
H3A H 0.6214 -0.2055 0.4258 0.052 Uiso 1 1 calc R . .
C4 C 0.71130(13) -0.11181(19) 0.42557(9) 0.0466(6) Uani 1 1 d . . .
H4A H 0.7386 -0.1576 0.4506 0.056 Uiso 1 1 calc R . .
C5 C 0.74100(11) -0.01660(19) 0.40251(9) 0.0421(5) Uani 1 1 d . . .
H5A H 0.7896 0.0007 0.4108 0.051 Uiso 1 1 calc R . .
C6 C 0.70132(11) 0.05431(16) 0.36753(8) 0.0349(4) Uani 1 1 d . . .
C7 C 0.73409(11) 0.15835(18) 0.34456(9) 0.0385(5) Uani 1 1 d . . .
H7A H 0.7161 0.2212 0.3677 0.046 Uiso 1 1 calc R . .
H7B H 0.7867 0.1545 0.3501 0.046 Uiso 1 1 calc R . .
N8 N 0.71926(9) 0.18100(13) 0.28235(7) 0.0334(4) Uani 1 1 d . . .
C9 C 0.74008(10) 0.08621(17) 0.24614(9) 0.0365(4) Uani 1 1 d . . .
H9A H 0.7271 0.0168 0.2661 0.044 Uiso 1 1 calc R . .
H9B H 0.7927 0.0867 0.2405 0.044 Uiso 1 1 calc R . .
C10 C 0.70307(10) 0.09029(17) 0.18771(8) 0.0365(4) Uani 1 1 d . . .
H10A H 0.7186 0.1571 0.1666 0.044 Uiso 1 1 calc R . .
H10B H 0.7171 0.0250 0.1647 0.044 Uiso 1 1 calc R . .
N11 N 0.62453(8) 0.09207(13) 0.19477(7) 0.0316(3) Uani 1 1 d . . .
C12 C 0.58912(10) 0.12868(17) 0.14038(8) 0.0347(4) Uani 1 1 d . . .
H12A H 0.5367 0.1314 0.1471 0.042 Uiso 1 1 calc R . .
H12B H 0.5981 0.0724 0.1103 0.042 Uiso 1 1 calc R . .
C13 C 0.61284(10) 0.23932(17) 0.11736(8) 0.0324(4) Uani 1 1 d . . .
C14 C 0.62083(11) 0.25195(18) 0.05793(9) 0.0369(4) Uani 1 1 d . . .
H14A H 0.6153 0.1892 0.0338 0.044 Uiso 1 1 calc R . .
C15 C 0.63648(11) 0.35212(19) 0.03284(9) 0.0412(5) Uani 1 1 d . . .
H15A H 0.6410 0.3586 -0.0079 0.049 Uiso 1 1 calc R . .
C16 C 0.64552(11) 0.44361(18) 0.06840(9) 0.0404(5) Uani 1 1 d . . .
H16A H 0.6556 0.5136 0.0519 0.048 Uiso 1 1 calc R . .
C17 C 0.63991(10) 0.43297(16) 0.12767(8) 0.0343(4) Uani 1 1 d . . .
H17A H 0.6469 0.4960 0.1513 0.041 Uiso 1 1 calc R . .
C18 C 0.62409(10) 0.33116(16) 0.15384(8) 0.0305(4) Uani 1 1 d . . .
O18 O 0.62213(8) 0.32524(11) 0.21072(6) 0.0346(3) Uani 1 1 d . . .
C19 C 0.76162(13) 0.27952(18) 0.26650(11) 0.0482(6) Uani 1 1 d . . .
H19A H 0.8125 0.2655 0.2740 0.072 Uiso 1 1 calc R . .
H19B H 0.7456 0.3427 0.2896 0.072 Uiso 1 1 calc R . .
H19C H 0.7548 0.2957 0.2254 0.072 Uiso 1 1 calc R . .
C20 C 0.59646(12) -0.01947(16) 0.20796(10) 0.0416(5) Uani 1 1 d . . .
H20A H 0.6102 -0.0705 0.1770 0.062 Uiso 1 1 calc R . .
H20B H 0.5441 -0.0165 0.2109 0.062 Uiso 1 1 calc R . .
H20C H 0.6166 -0.0451 0.2447 0.062 Uiso 1 1 calc R . .
N21 N 0.58491(8) 0.34212(14) 0.33037(7) 0.0337(4) Uani 1 1 d . . .
C22 C 0.57409(11) 0.44658(17) 0.31321(9) 0.0403(5) Uani 1 1 d . . .
H22A H 0.5810 0.4640 0.2736 0.048 Uiso 1 1 calc R . .
C23 C 0.55348(12) 0.52965(19) 0.35016(10) 0.0490(6) Uani 1 1 d . . .
H23A H 0.5464 0.6025 0.3361 0.059 Uiso 1 1 calc R . .
C24 C 0.54327(11) 0.5057(2) 0.40789(10) 0.0488(6) Uani 1 1 d . . .
H24A H 0.5288 0.5614 0.4342 0.059 Uiso 1 1 calc R . .
C25 C 0.55450(12) 0.3996(2) 0.42638(9) 0.0469(5) Uani 1 1 d . . .
H25A H 0.5484 0.3808 0.4659 0.056 Uiso 1 1 calc R . .
C26 C 0.57493(11) 0.32010(19) 0.38657(9) 0.0405(5) Uani 1 1 d . . .
H26A H 0.5822 0.2467 0.3997 0.049 Uiso 1 1 calc R . .
N31 N 0.45168(14) 0.7643(2) 0.42671(12) 0.0729(7) Uani 1 1 d . . .
C32 C 0.3854(2) 0.7415(2) 0.40669(13) 0.0714(9) Uani 1 1 d . . .
H32A H 0.3807 0.6884 0.3767 0.086 Uiso 1 1 calc R . .
C33 C 0.32506(16) 0.7908(3) 0.42732(13) 0.0712(8) Uani 1 1 d . . .
H33A H 0.2793 0.7720 0.4122 0.085 Uiso 1 1 calc R . .
C34 C 0.33139(14) 0.8669(2) 0.46959(12) 0.0662(7) Uani 1 1 d . . .
H34A H 0.2899 0.9023 0.4846 0.079 Uiso 1 1 calc R . .
C35 C 0.39637(13) 0.8922(2) 0.49024(10) 0.0550(6) Uani 1 1 d . . .
H35A H 0.4016 0.9457 0.5199 0.066 Uiso 1 1 calc R . .
C36 C 0.45456(14) 0.8405(2) 0.46820(12) 0.0619(7) Uani 1 1 d . . .
H36A H 0.5003 0.8597 0.4832 0.074 Uiso 1 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
O Fe O1 92.89(6) . . ?
O Fe O18 99.66(6) . . ?
O1 Fe O18 167.32(6) . . ?
O Fe N21 94.94(6) . . ?
O1 Fe N21 91.15(6) . . ?
O18 Fe N21 85.95(6) . . ?
O Fe N11 95.04(6) . . ?
O1 Fe N11 95.26(6) . . ?
O18 Fe N11 85.54(6) . . ?
N21 Fe N11 167.84(6) . . ?
O Fe N8 169.77(7) . . ?
O1 Fe N8 81.00(5) . . ?
O18 Fe N8 86.84(6) . . ?
N21 Fe N8 93.37(6) . . ?
N11 Fe N8 77.49(6) . . ?
Fe O Fe 175.68(12) . 3_655 ?
C1 O1 Fe 140.34(12) . . ?
O1 C1 C2 119.58(18) . . ?
O1 C1 C6 121.99(17) . . ?
C2 C1 C6 118.43(18) . . ?
C3 C2 C1 121.2(2) . . ?
C4 C3 C2 120.6(2) . . ?
C3 C4 C5 119.0(2) . . ?
C4 C5 C6 121.7(2) . . ?
C5 C6 C1 119.01(19) . . ?
C5 C6 C7 120.58(19) . . ?
C1 C6 C7 120.38(17) . . ?
N8 C7 C6 114.93(16) . . ?
C9 N8 C19 110.37(17) . . ?
C9 N8 C7 110.87(16) . . ?
C19 N8 C7 106.80(16) . . ?
C9 N8 Fe 105.63(11) . . ?
C19 N8 Fe 111.56(13) . . ?
C7 N8 Fe 111.67(12) . . ?
N8 C9 C10 111.16(16) . . ?
N11 C10 C9 110.69(15) . . ?
C10 N11 C20 111.13(16) . . ?
C10 N11 C12 110.57(14) . . ?
C20 N11 C12 106.82(15) . . ?
C10 N11 Fe 110.26(11) . . ?
C20 N11 Fe 109.71(11) . . ?
C12 N11 Fe 108.25(11) . . ?
N11 C12 C13 115.67(15) . . ?
C14 C13 C18 119.20(19) . . ?
C14 C13 C12 118.55(18) . . ?
C18 C13 C12 122.19(17) . . ?
C15 C14 C13 122.4(2) . . ?
C14 C15 C16 118.63(19) . . ?
C17 C16 C15 120.24(19) . . ?
C16 C17 C18 121.70(19) . . ?
O18 C18 C17 118.91(17) . . ?
O18 C18 C13 123.33(18) . . ?
C17 C18 C13 117.74(17) . . ?
C18 O18 Fe 133.14(12) . . ?
C26 N21 C22 117.00(18) . . ?
C26 N21 Fe 121.73(14) . . ?
C22 N21 Fe 119.80(14) . . ?
N21 C22 C23 123.3(2) . . ?
C22 C23 C24 119.1(2) . . ?
C25 C24 C23 118.6(2) . . ?
C24 C25 C26 119.1(2) . . ?
N21 C26 C25 123.0(2) . . ?
C36 N31 C32 115.3(2) . . ?
N31 C32 C33 123.2(3) . . ?
C34 C33 C32 118.8(3) . . ?
C35 C34 C33 119.7(3) . . ?
C34 C35 C36 119.0(3) . . ?
N31 C36 C35 124.1(3) . . ?
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
Fe O 1.7840(3) . ?
Fe O1 1.9560(13) . ?
Fe O18 1.9643(13) . ?
Fe N21 2.2255(16) . ?
Fe N11 2.2259(15) . ?
Fe N8 2.3981(16) . ?
O Fe 1.7840(3) 3_655 ?
O1 C1 1.329(2) . ?
C1 C2 1.401(3) . ?
C1 C6 1.410(3) . ?
C2 C3 1.379(3) . ?
C3 C4 1.379(3) . ?
C4 C5 1.387(3) . ?
C5 C6 1.394(3) . ?
C6 C7 1.499(3) . ?
C7 N8 1.492(2) . ?
N8 C9 1.475(3) . ?
N8 C19 1.479(3) . ?
C9 C10 1.519(3) . ?
C10 N11 1.474(2) . ?
N11 C20 1.482(2) . ?
N11 C12 1.489(2) . ?
C12 C13 1.510(3) . ?
C13 C14 1.392(3) . ?
C13 C18 1.413(3) . ?
C14 C15 1.378(3) . ?
C15 C16 1.392(3) . ?
C16 C17 1.382(3) . ?
C17 C18 1.407(3) . ?
C18 O18 1.319(2) . ?
N21 C26 1.341(3) . ?
N21 C22 1.343(3) . ?
C22 C23 1.376(3) . ?
C23 C24 1.381(3) . ?
C24 C25 1.372(3) . ?
C25 C26 1.387(3) . ?
N31 C36 1.334(4) . ?
N31 C32 1.348(4) . ?
C32 C33 1.362(4) . ?
C33 C34 1.350(4) . ?
C34 C35 1.338(3) . ?
C35 C36 1.353(4) . ?
