#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/83/2208337.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2208337
loop_
_publ_author_name
'Jäger, Ernst-Gottfried'
'Knaudt, Jutta'
'Imhof, Wolfgang'
_publ_section_title
;μ-Oxo-bis[(diethyl
 6,17-dimethyldibenzo[a,h]-5,9,14,18-tetraaza[14]annulene-7,16-dicarboxylato)iron(III)]
 sesquihydrate
;
_journal_coeditor_code           HG2003
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m492
_journal_page_last               m495
_journal_paper_doi               10.1107/S1600536806004636
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe2 (C26 H26 N4 O4) O], 1.5H2 O1'
_chemical_formula_moiety         'C52 H52 Fe2 N8 O9, 1.5H2 O1'
_chemical_formula_sum            'C52 H55 Fe2 N8 O10.5'
_chemical_formula_weight         1071.72
_chemical_name_systematic
;
μ-oxo-bis{[4,15-bis(ethoxycarbonyl)-5,14-dimethyl-2,7,13,17-
tetraazatricyclo[16.4.0.0^7,12^]docosa-3,5,7,9,11,13,15,18(1),19,21-decaene-
2,17-diido]iron(III)} sesquihydrate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.26(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.322(6)
_cell_length_b                   13.494(4)
_cell_length_c                   29.838(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      20.1
_cell_volume                     10252(4)
_computing_cell_refinement       'SET4 (Boer et al., 1984)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'MolEN (Nonius, 1990)'
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            9161
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        3.64
_diffrn_standards_interval_time  600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.8299
_exptl_absorpt_correction_T_min  0.7760
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0507P)²+35.0302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                6718
_reflns_number_total             8963
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg2003.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2208337
_cod_database_fobs_code          2208337
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.455878(18) 0.11981(4) 0.363464(18) 0.02613(14) Uani d . 1 . .
Fe Fe2 0.345151(18) 0.04404(4) 0.282503(17) 0.02348(13) Uani d . 1 . .
O O1 0.40880(9) 0.10002(18) 0.30446(8) 0.0287(5) Uani d . 1 . .
N N1 0.47942(11) -0.0180(2) 0.39148(10) 0.0299(7) Uani d . 1 . .
C C1 0.47211(14) -0.0668(3) 0.42675(12) 0.0320(8) Uani d . 1 . .
C C2 0.50456(16) -0.1576(3) 0.44782(15) 0.0418(10) Uani d . 1 . .
H H2A 0.4858 -0.2158 0.4323 0.050(5) Uiso calc R 1 . .
H H2B 0.5112 -0.1609 0.4817 0.050(5) Uiso calc R 1 . .
H H2C 0.5373 -0.1539 0.4429 0.050(5) Uiso calc R 1 . .
C C3 0.43734(14) -0.0282(3) 0.44852(12) 0.0317(8) Uani d . 1 . .
C C4 0.42105(16) -0.0860(3) 0.48288(14) 0.0393(9) Uani d . 1 . .
O O2 0.40931(14) -0.0512(2) 0.51489(11) 0.0558(8) Uani d . 1 . .
O O3 0.41855(12) -0.1836(2) 0.47378(10) 0.0491(8) Uani d . 1 B .
C C5 0.4070(2) -0.2457(4) 0.50843(19) 0.0659(15) Uani d . 1 . .
H H5A 0.3696 -0.2462 0.5021 0.15(2) Uiso calc R 1 A 1
H H5B 0.4253 -0.2217 0.5409 0.15(2) Uiso calc R 1 A 1
C C6 0.4269(8) -0.3538(9) 0.5018(5) 0.060(5) Uiso d P 0.46(3) B 1
H H6A 0.4205 -0.3985 0.5241 0.063(12) Uiso calc PR 0.46(3) B 1
H H6B 0.4639 -0.3517 0.5077 0.063(12) Uiso calc PR 0.46(3) B 1
H H6C 0.4083 -0.3763 0.4696 0.063(12) Uiso calc PR 0.46(3) B 1
C C6X 0.3989(8) -0.3424(8) 0.4914(4) 0.066(4) Uiso d P 0.54(3) B 2
H H6D 0.3681 -0.3450 0.4625 0.063(12) Uiso calc PR 0.54(3) B 2
H H6E 0.3941 -0.3848 0.5153 0.063(12) Uiso calc PR 0.54(3) B 2
H H6F 0.4288 -0.3643 0.4845 0.063(12) Uiso calc PR 0.54(3) B 2
C C7 0.41673(13) 0.0674(3) 0.44219(13) 0.0320(8) Uani d . 1 . .
H H7 0.3970 0.0845 0.4607 0.035(7) Uiso calc R 1 . .
N N2 0.42203(11) 0.1358(2) 0.41314(10) 0.0298(7) Uani d . 1 . .
C C8 0.40418(14) 0.2339(3) 0.41391(13) 0.0323(8) Uani d . 1 . .
C C9 0.36520(15) 0.2631(3) 0.43082(14) 0.0413(10) Uani d . 1 . .
H H9 0.3481 0.2163 0.4428 0.044(4) Uiso calc R 1 . .
C C10 0.35202(17) 0.3624(3) 0.42971(16) 0.0495(11) Uani d . 1 . .
H H10 0.3269 0.3828 0.4420 0.044(4) Uiso calc R 1 . .
C C11 0.37628(17) 0.4312(3) 0.41032(17) 0.0515(12) Uani d . 1 . .
H H11 0.3669 0.4976 0.4093 0.044(4) Uiso calc R 1 . .
C C12 0.41401(16) 0.4029(3) 0.39252(16) 0.0450(10) Uani d . 1 . .
H H12 0.4296 0.4498 0.3791 0.044(4) Uiso calc R 1 . .
C C13 0.42877(14) 0.3046(3) 0.39460(14) 0.0344(8) Uani d . 1 . .
N N3 0.46826(11) 0.2654(2) 0.37936(11) 0.0310(7) Uani d . 1 . .
C C14 0.50674(14) 0.3208(3) 0.37633(13) 0.0339(8) Uani d . 1 . .
H H14 0.5040 0.3887 0.3802 0.035(7) Uiso calc R 1 . .
C C15 0.55094(14) 0.2887(3) 0.36793(13) 0.0337(8) Uani d . 1 . .
C C16 0.58724(18) 0.3652(3) 0.36345(18) 0.0528(12) Uani d . 1 C .
O O4 0.57978(16) 0.4520(3) 0.38086(18) 0.0863(13) Uani d . 1 . .
O O5 0.62041(15) 0.3554(3) 0.34659(17) 0.0843(13) Uani d . 1 . .
C C17 0.6168(7) 0.5338(13) 0.3897(7) 0.064(4) Uiso d P 0.33 C 3
H H17A 0.6519 0.5063 0.3989 0.055(13) Uiso calc PR 0.33 C 3
H H17B 0.6096 0.5693 0.3598 0.055(13) Uiso calc PR 0.33 C 3
C C18 0.6166(18) 0.600(3) 0.4239(14) 0.20(2) Uiso d P 0.33 C 3
H H18A 0.5818 0.6259 0.4162 0.15(3) Uiso calc PR 0.33 C 3
H H18B 0.6403 0.6535 0.4249 0.15(3) Uiso calc PR 0.33 C 3
H H18C 0.6277 0.5679 0.4547 0.15(3) Uiso calc PR 0.33 C 3
C C17X 0.6038(4) 0.5365(7) 0.3616(4) 0.085(3) Uiso d P 0.67 C 4
H H17C 0.6405 0.5235 0.3672 0.055(13) Uiso calc PR 0.67 C 4
H H17D 0.5850 0.5460 0.3274 0.055(13) Uiso calc PR 0.67 C 4
C C18X 0.5987(7) 0.6169(12) 0.3870(6) 0.142(5) Uiso d P 0.67 C 4
H H18D 0.5621 0.6320 0.3786 0.15(3) Uiso calc PR 0.67 C 4
H H18E 0.6162 0.6726 0.3795 0.15(3) Uiso calc PR 0.67 C 4
H H18F 0.6141 0.6029 0.4208 0.15(3) Uiso calc PR 0.67 C 4
C C19 0.56351(14) 0.1871(3) 0.36384(13) 0.0325(8) Uani d . 1 . .
C C20 0.61972(15) 0.1584(3) 0.37214(16) 0.0475(11) Uani d . 1 . .
H H20A 0.6432 0.2019 0.3956 0.050(5) Uiso calc R 1 . .
H H20B 0.6258 0.1637 0.3425 0.050(5) Uiso calc R 1 . .
H H20C 0.6258 0.0913 0.3836 0.050(5) Uiso calc R 1 . .
N N4 0.52804(11) 0.1178(2) 0.35791(10) 0.0294(7) Uani d . 1 . .
C C21 0.53450(13) 0.0183(3) 0.34651(13) 0.0328(8) Uani d . 1 . .
C C22 0.55615(15) -0.0084(3) 0.31257(15) 0.0418(10) Uani d . 1 . .
H H22 0.5725 0.0393 0.3003 0.044(4) Uiso calc R 1 . .
C C23 0.55339(16) -0.1051(3) 0.29719(17) 0.0512(12) Uani d . 1 . .
H H23 0.5682 -0.1228 0.2748 0.044(4) Uiso calc R 1 . .
C C24 0.52890(16) -0.1755(3) 0.31477(17) 0.0497(11) Uani d . 1 . .
H H24 0.5277 -0.2408 0.3045 0.044(4) Uiso calc R 1 . .
C C25 0.50607(15) -0.1505(3) 0.34748(15) 0.0399(9) Uani d . 1 . .
H H25 0.4887 -0.1985 0.3585 0.044(4) Uiso calc R 1 . .
C C26 0.50887(13) -0.0540(3) 0.36408(13) 0.0317(8) Uani d . 1 . .
N N5 0.29887(11) 0.1301(2) 0.30736(10) 0.0280(6) Uani d . 1 . .
C C27 0.27784(13) 0.1125(3) 0.34000(12) 0.0292(8) Uani d . 1 . .
C C28 0.23440(15) 0.1776(3) 0.34246(15) 0.0418(10) Uani d . 1 . .
H H28A 0.2484 0.2248 0.3680 0.051(5) Uiso calc R 1 . .
H H28B 0.2084 0.1376 0.3485 0.051(5) Uiso calc R 1 . .
H H28C 0.2186 0.2120 0.3125 0.051(5) Uiso calc R 1 . .
C C29 0.29145(13) 0.0259(3) 0.36951(12) 0.0277(8) Uani d . 1 . .
C C30 0.27606(14) 0.0208(3) 0.41182(13) 0.0345(9) Uani d . 1 . .
O O6 0.26572(13) 0.0907(2) 0.43203(10) 0.0530(8) Uani d . 1 . .
O O7 0.27648(13) -0.0720(2) 0.42814(10) 0.0481(7) Uani d . 1 E .
C C31 0.2684(2) -0.0826(4) 0.47340(16) 0.0542(12) Uani d . 1 . .
H H31A 0.2829 -0.0254 0.4935 0.080(9) Uiso calc R 1 D 5
H H31B 0.2870 -0.1410 0.4901 0.080(9) Uiso calc R 1 D 5
C C32 0.2125(4) -0.0918(9) 0.4660(4) 0.071(4) Uiso d P 0.539(14) E 5
H H32A 0.1976 -0.1459 0.4445 0.092(14) Uiso calc PR 0.539(14) E 5
H H32B 0.1947 -0.0315 0.4524 0.092(14) Uiso calc PR 0.539(14) E 5
H H32C 0.2088 -0.1040 0.4963 0.092(14) Uiso calc PR 0.539(14) E 5
C C32X 0.2382(6) -0.1653(12) 0.4724(5) 0.087(5) Uiso d P 0.461(14) E 6
H H32D 0.2354 -0.1742 0.5033 0.092(14) Uiso calc PR 0.461(14) E 6
H H32E 0.2543 -0.2227 0.4647 0.092(14) Uiso calc PR 0.461(14) E 6
H H32F 0.2037 -0.1565 0.4485 0.092(14) Uiso calc PR 0.461(14) E 6
C C33 0.31809(13) -0.0560(3) 0.36091(12) 0.0286(8) Uani d . 1 . .
H H33 0.3215 -0.1108 0.3807 0.029(7) Uiso calc R 1 . .
N N6 0.33886(10) -0.0633(2) 0.32762(9) 0.0245(6) Uani d . 1 . .
C C34 0.35855(13) -0.1543(3) 0.31836(12) 0.0259(7) Uani d . 1 . .
C C35 0.37697(14) -0.2313(3) 0.35113(13) 0.0315(8) Uani d . 1 . .
H H35 0.3775 -0.2248 0.3823 0.038(4) Uiso calc R 1 . .
C C36 0.39440(15) -0.3174(3) 0.33706(14) 0.0360(9) Uani d . 1 . .
H H36 0.4061 -0.3693 0.3588 0.038(4) Uiso calc R 1 . .
C C37 0.39470(15) -0.3277(3) 0.29101(14) 0.0367(9) Uani d . 1 . .
H H37 0.4062 -0.3864 0.2819 0.038(4) Uiso calc R 1 . .
C C38 0.37778(14) -0.2504(3) 0.25874(13) 0.0310(8) Uani d . 1 . .
H H38 0.3787 -0.2567 0.2280 0.038(4) Uiso calc R 1 . .
C C39 0.35946(13) -0.1634(3) 0.27180(12) 0.0261(7) Uani d . 1 . .
N N7 0.34043(10) -0.0792(2) 0.24262(10) 0.0249(6) Uani d . 1 . .
C C40 0.32261(13) -0.0847(3) 0.19529(12) 0.0262(7) Uani d . 1 . .
H H40 0.3279 -0.1447 0.1823 0.029(7) Uiso calc R 1 . .
C C41 0.29677(13) -0.0110(3) 0.16235(12) 0.0265(7) Uani d . 1 . .
C C42 0.28416(14) -0.0345(3) 0.11098(12) 0.0311(8) Uani d . 1 . .
O O8 0.26757(12) 0.0217(2) 0.07774(9) 0.0477(7) Uani d . 1 . .
O O9 0.29414(12) -0.1307(2) 0.10434(9) 0.0422(7) Uani d . 1 . .
C C43 0.29166(18) -0.1593(3) 0.05698(14) 0.0466(11) Uani d . 1 . .
H H43A 0.2644 -0.1216 0.0329 0.080(9) Uiso calc R 1 . .
H H43B 0.2828 -0.2291 0.0518 0.080(9) Uiso calc R 1 . .
C C44 0.3433(2) -0.1409(4) 0.05182(18) 0.0657(14) Uani d . 1 . .
H H44A 0.3503 -0.0710 0.0536 0.109(13) Uiso calc R 1 . .
H H44B 0.3422 -0.1657 0.0213 0.109(13) Uiso calc R 1 . .
H H44C 0.3706 -0.1742 0.0772 0.109(13) Uiso calc R 1 . .
C C45 0.28257(13) 0.0840(3) 0.17507(12) 0.0282(8) Uani d . 1 . .
C C46 0.24108(15) 0.1450(3) 0.13775(13) 0.0384(9) Uani d . 1 . .
H H46A 0.2144 0.1019 0.1172 0.051(5) Uiso calc R 1 . .
H H46B 0.2569 0.1813 0.1189 0.051(5) Uiso calc R 1 . .
H H46C 0.2256 0.1905 0.1535 0.051(5) Uiso calc R 1 . .
N N8 0.30255(11) 0.1152(2) 0.22006(10) 0.0263(6) Uani d . 1 . .
C C47 0.29520(13) 0.2122(3) 0.23481(13) 0.0299(8) Uani d . 1 . .
C C48 0.29926(14) 0.2980(3) 0.21042(14) 0.0346(8) Uani d . 1 . .
H H48 0.3020 0.2935 0.1803 0.038(4) Uiso calc R 1 . .
C C49 0.29919(15) 0.3895(3) 0.23075(15) 0.0403(9) Uani d . 1 . .
H H49 0.3013 0.4465 0.2140 0.038(4) Uiso calc R 1 . .
C C50 0.29606(16) 0.3974(3) 0.27569(16) 0.0435(10) Uani d . 1 . .
H H50 0.2953 0.4596 0.2889 0.038(4) Uiso calc R 1 . .
C C51 0.29405(15) 0.3134(3) 0.30102(14) 0.0370(9) Uani d . 1 . .
H H51 0.2933 0.3193 0.3318 0.038(4) Uiso calc R 1 . .
C C52 0.29306(13) 0.2198(3) 0.28127(12) 0.0284(8) Uani d . 1 . .
O O10 0.44529(18) 0.2355(4) 0.24846(15) 0.1080(17) Uani d . 1 . .
O O11 0.4385(7) -0.5757(12) 0.2695(6) 0.096(5) Uiso d P 0.30 . .
O O11X 0.4666(8) -0.5359(16) 0.2685(7) 0.078(5) Uiso d P 0.20 . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3010 0.8450 '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_publ_flag
O1 Fe1 N3 112.13(12) y
O1 Fe1 N2 112.42(11) y
N3 Fe1 N2 78.82(12) y
O1 Fe1 N4 106.88(11) y
N3 Fe1 N4 87.00(12) y
N2 Fe1 N4 140.70(12) y
O1 Fe1 N1 105.93(12) y
N3 Fe1 N1 141.93(12) y
N2 Fe1 N1 87.56(12) y
N4 Fe1 N1 81.42(12) y
O1 Fe1 C21 94.35(11) ?
N3 Fe1 C21 116.94(12) ?
N2 Fe1 C21 141.67(12) ?
N4 Fe1 C21 29.94(11) ?
N1 Fe1 C21 58.00(12) ?
O1 Fe1 C26 93.92(11) ?
N3 Fe1 C26 141.62(11) ?
N2 Fe1 C26 117.73(12) ?
N4 Fe1 C26 57.79(11) ?
N1 Fe1 C26 30.19(11) ?
C21 Fe1 C26 29.66(11) ?
O1 Fe1 C13 105.84(11) ?
N3 Fe1 C13 27.66(11) ?
N2 Fe1 C13 54.97(12) ?
N4 Fe1 C13 114.31(11) ?
N1 Fe1 C13 137.96(12) ?
C21 Fe1 C13 144.07(11) ?
C26 Fe1 C13 160.24(11) ?
O1 Fe1 C8 106.45(10) ?
N3 Fe1 C8 54.93(11) ?
N2 Fe1 C8 27.41(11) ?
N4 Fe1 C8 136.68(11) ?
N1 Fe1 C8 114.63(11) ?
C21 Fe1 C8 159.20(10) ?
C26 Fe1 C8 144.52(11) ?
C13 Fe1 C8 28.49(11) ?
O1 Fe1 Fe2 23.52(7) ?
N3 Fe1 Fe2 120.52(9) ?
N2 Fe1 Fe2 91.63(9) ?
N4 Fe1 Fe2 126.71(8) ?
N1 Fe1 Fe2 94.99(8) ?
C21 Fe1 Fe2 106.46(8) ?
C26 Fe1 Fe2 94.70(8) ?
C13 Fe1 Fe2 103.51(8) ?
C8 Fe1 Fe2 93.20(7) ?
O1 Fe2 N7 114.15(11) y
O1 Fe2 N6 111.34(11) y
N7 Fe2 N6 78.50(11) y
O1 Fe2 N8 107.00(11) y
N7 Fe2 N8 87.49(11) y
N6 Fe2 N8 141.63(11) y
O1 Fe2 N5 105.92(11) y
N7 Fe2 N5 139.93(11) y
N6 Fe2 N5 87.27(11) y
N8 Fe2 N5 80.85(11) y
O1 Fe2 C52 94.03(11) ?
N7 Fe2 C52 140.96(11) ?
N6 Fe2 C52 117.09(11) ?
N8 Fe2 C52 57.54(11) ?
N5 Fe2 C52 29.82(11) ?
O1 Fe2 C47 94.29(11) ?
N7 Fe2 C47 117.29(11) ?
N6 Fe2 C47 141.65(11) ?
N8 Fe2 C47 29.83(11) ?
N5 Fe2 C47 57.65(11) ?
C52 Fe2 C47 29.63(10) ?
O1 Fe2 C34 106.45(10) ?
N7 Fe2 C34 54.67(10) ?
N6 Fe2 C34 27.36(10) ?
N8 Fe2 C34 137.32(11) ?
N5 Fe2 C34 114.13(11) ?
C52 Fe2 C34 143.69(10) ?
C47 Fe2 C34 159.25(10) ?
O1 Fe2 C39 107.47(10) ?
N7 Fe2 C39 27.30(10) ?
N6 Fe2 C39 54.75(10) ?
N8 Fe2 C39 114.45(11) ?
N5 Fe2 C39 136.41(11) ?
C52 Fe2 C39 158.50(10) ?
C47 Fe2 C39 143.96(10) ?
C34 Fe2 C39 28.43(9) ?
O1 Fe2 Fe1 23.46(7) ?
N7 Fe2 Fe1 122.38(8) ?
N6 Fe2 Fe1 90.65(8) ?
N8 Fe2 Fe1 126.44(8) ?
N5 Fe2 Fe1 94.73(8) ?
C52 Fe2 Fe1 94.33(8) ?
C47 Fe2 Fe1 105.97(8) ?
C34 Fe2 Fe1 93.31(7) ?
C39 Fe2 Fe1 105.11(7) ?
Fe1 O1 Fe2 133.01(14) y
C1 N1 C26 124.7(3) ?
C1 N1 Fe1 131.7(3) ?
C26 N1 Fe1 103.6(2) ?
N1 C1 C3 119.9(3) ?
N1 C1 C2 120.2(3) ?
C3 C1 C2 119.6(3) ?
C1 C2 H2A 109.5 ?
C1 C2 H2B 109.5 ?
H2A C2 H2B 109.5 ?
C1 C2 H2C 109.5 ?
H2A C2 H2C 109.5 ?
H2B C2 H2C 109.5 ?
C7 C3 C1 125.4(3) ?
C7 C3 C4 112.0(3) ?
C1 C3 C4 122.6(3) ?
O2 C4 O3 122.2(4) ?
O2 C4 C3 125.2(4) ?
O3 C4 C3 112.6(3) ?
C4 O3 C5 115.5(3) ?
C6X C5 O3 109.1(6) ?
C6X C5 C6 27.3(6) ?
O3 C5 C6 105.5(6) ?
C6X C5 H5A 84.6 ?
O3 C5 H5A 110.6 ?
C6 C5 H5A 110.6 ?
C6X C5 H5B 129.4 ?
O3 C5 H5B 110.6 ?
C6 C5 H5B 110.6 ?
H5A C5 H5B 108.8 ?
C5 C6 H6A 109.5 ?
C5 C6 H6B 109.5 ?
C5 C6 H6C 109.5 ?
C5 C6X H6D 109.5 ?
C5 C6X H6E 109.5 ?
H6D C6X H6E 109.5 ?
C5 C6X H6F 109.5 ?
H6D C6X H6F 109.5 ?
H6E C6X H6F 109.5 ?
N2 C7 C3 127.3(3) ?
N2 C7 H7 116.3 ?
C3 C7 H7 116.3 ?
C7 N2 C8 121.8(3) ?
C7 N2 Fe1 126.8(2) ?
C8 N2 Fe1 111.4(2) ?
C9 C8 C13 119.9(4) ?
C9 C8 N2 125.9(4) ?
C13 C8 N2 114.2(3) ?
C9 C8 Fe1 159.0(3) ?
C13 C8 Fe1 75.4(2) ?
N2 C8 Fe1 41.23(16) ?
C10 C9 C8 119.5(4) ?
C10 C9 H9 120.2 ?
C8 C9 H9 120.2 ?
C11 C10 C9 120.0(4) ?
C11 C10 H10 120.0 ?
C9 C10 H10 120.0 ?
C12 C11 C10 121.0(4) ?
C12 C11 H11 119.5 ?
C10 C11 H11 119.5 ?
C11 C12 C13 119.8(4) ?
C11 C12 H12 120.1 ?
C13 C12 H12 120.1 ?
C12 C13 C8 119.7(4) ?
C12 C13 N3 126.0(4) ?
C8 C13 N3 114.3(3) ?
C12 C13 Fe1 158.7(3) ?
C8 C13 Fe1 76.1(2) ?
N3 C13 Fe1 41.47(16) ?
C14 N3 C13 121.9(3) ?
C14 N3 Fe1 127.2(3) ?
C13 N3 Fe1 110.9(2) ?
N3 C14 C15 127.1(4) ?
N3 C14 H14 116.5 ?
C15 C14 H14 116.5 ?
C14 C15 C19 124.4(3) ?
C14 C15 C16 117.2(4) ?
C19 C15 C16 118.3(3) ?
O5 C16 O4 120.7(4) ?
O5 C16 C15 127.0(4) ?
O4 C16 C15 112.3(4) ?
C16 O4 C17 123.1(8) ?
C16 O4 C17X 111.3(5) ?
C17 O4 C17X 30.4(7) ?
C18 C17 O4 116(2) ?
C18 C17 H17A 108.2 ?
O4 C17 H17A 108.2 ?
C18 C17 H17B 108.2 ?
O4 C17 H17B 108.2 ?
H17A C17 H17B 107.3 ?
C18X C17X O4 103.8(10) ?
C18X C17X H17C 111.0 ?
O4 C17X H17C 111.0 ?
C18X C17X H17D 111.0 ?
O4 C17X H17D 111.0 ?
H17C C17X H17D 109.0 ?
N4 C19 C15 120.5(3) ?
N4 C19 C20 119.7(3) ?
C15 C19 C20 119.4(3) ?
C19 C20 H20A 109.5 ?
C19 C20 H20B 109.5 ?
H20A C20 H20B 109.5 ?
C19 C20 H20C 109.5 ?
H20A C20 H20C 109.5 ?
H20B C20 H20C 109.5 ?
C19 N4 C21 124.0(3) ?
C19 N4 Fe1 132.0(3) ?
C21 N4 Fe1 104.0(2) ?
C22 C21 C26 119.5(4) ?
C22 C21 N4 122.9(4) ?
C26 C21 N4 116.5(3) ?
C22 C21 Fe1 146.1(3) ?
C26 C21 Fe1 75.5(2) ?
N4 C21 Fe1 46.08(15) ?
C23 C22 C21 120.0(4) ?
C23 C22 H22 120.0 ?
C21 C22 H22 120.0 ?
C24 C23 C22 120.3(4) ?
C24 C23 H23 119.8 ?
C22 C23 H23 119.8 ?
C23 C24 C25 120.7(4) ?
C23 C24 H24 119.7 ?
C25 C24 H24 119.7 ?
C24 C25 C26 120.2(4) ?
C24 C25 H25 119.9 ?
C26 C25 H25 119.9 ?
C25 C26 C21 119.2(3) ?
C25 C26 N1 123.8(3) ?
C21 C26 N1 116.0(3) ?
C25 C26 Fe1 146.9(3) ?
C21 C26 Fe1 74.9(2) ?
N1 C26 Fe1 46.24(16) ?
C27 N5 C52 124.6(3) ?
C27 N5 Fe2 131.1(3) ?
C52 N5 Fe2 104.3(2) ?
N5 C27 C29 121.1(3) ?
N5 C27 C28 119.7(3) ?
C29 C27 C28 118.9(3) ?
C27 C28 H28A 109.5 ?
C27 C28 H28B 109.5 ?
H28A C28 H28B 109.5 ?
C27 C28 H28C 109.5 ?
H28A C28 H28C 109.5 ?
H28B C28 H28C 109.5 ?
C33 C29 C27 124.8(3) ?
C33 C29 C30 116.8(3) ?
C27 C29 C30 118.4(3) ?
O6 C30 O7 121.4(3) ?
O6 C30 C29 125.7(4) ?
O7 C30 C29 112.8(3) ?
C30 O7 C31 116.5(3) ?
C32X C31 O7 110.5(7) ?
C32X C31 C32 49.2(7) ?
O7 C31 C32 111.7(5) ?
C32X C31 H31A 139.8 ?
O7 C31 H31A 109.3 ?
C32 C31 H31A 109.3 ?
C32X C31 H31B 63.5 ?
O7 C31 H31B 109.3 ?
C32 C31 H31B 109.3 ?
H31A C31 H31B 107.9 ?
C31 C32 H32A 109.5 ?
C31 C32 H32B 109.5 ?
C31 C32 H32C 109.5 ?
C31 C32X H32D 109.5 ?
C31 C32X H32E 109.5 ?
C31 C32X H32F 109.5 ?
N6 C33 C29 126.5(3) ?
N6 C33 H33 116.8 ?
C29 C33 H33 116.8 ?
C33 N6 C34 120.9(3) ?
C33 N6 Fe2 127.8(2) ?
C34 N6 Fe2 111.3(2) ?
C35 C34 C39 120.0(3) ?
C35 C34 N6 125.5(3) ?
C39 C34 N6 114.5(3) ?
C35 C34 Fe2 158.2(3) ?
C39 C34 Fe2 75.9(2) ?
N6 C34 Fe2 41.38(15) ?
C36 C35 C34 119.5(3) ?
C36 C35 H35 120.2 ?
C34 C35 H35 120.2 ?
C35 C36 C37 121.0(3) ?
C35 C36 H36 119.5 ?
C37 C36 H36 119.5 ?
C38 C37 C36 119.7(4) ?
C38 C37 H37 120.2 ?
C36 C37 H37 120.2 ?
C37 C38 C39 120.5(3) ?
C37 C38 H38 119.8 ?
C39 C38 H38 119.8 ?
C38 C39 C34 119.3(3) ?
C38 C39 N7 126.7(3) ?
C34 C39 N7 114.0(3) ?
C38 C39 Fe2 159.7(2) ?
C34 C39 Fe2 75.7(2) ?
N7 C39 Fe2 41.09(15) ?
C40 N7 C39 121.7(3) ?
C40 N7 Fe2 126.6(2) ?
C39 N7 Fe2 111.6(2) ?
N7 C40 C41 127.6(3) ?
N7 C40 H40 116.2 ?
C41 C40 H40 116.2 ?
C40 C41 C45 124.6(3) ?
C40 C41 C42 116.4(3) ?
C45 C41 C42 118.9(3) ?
O8 C42 O9 121.3(3) ?
O8 C42 C41 126.8(4) ?
O9 C42 C41 111.9(3) ?
C42 O9 C43 117.3(3) ?
O9 C43 C44 110.2(4) ?
O9 C43 H43A 109.6 ?
C44 C43 H43A 109.6 ?
O9 C43 H43B 109.6 ?
C44 C43 H43B 109.6 ?
H43A C43 H43B 108.1 ?
C43 C44 H44A 109.5 ?
C43 C44 H44B 109.5 ?
H44A C44 H44B 109.5 ?
C43 C44 H44C 109.5 ?
H44A C44 H44C 109.5 ?
H44B C44 H44C 109.5 ?
N8 C45 C41 120.3(3) ?
N8 C45 C46 119.8(3) ?
C41 C45 C46 119.7(3) ?
C45 C46 H46A 109.5 ?
C45 C46 H46B 109.5 ?
H46A C46 H46B 109.5 ?
C45 C46 H46C 109.5 ?
H46A C46 H46C 109.5 ?
H46B C46 H46C 109.5 ?
C45 N8 C47 123.8(3) ?
C45 N8 Fe2 131.7(2) ?
C47 N8 Fe2 104.4(2) ?
C48 C47 C52 119.5(3) ?
C48 C47 N8 123.9(3) ?
C52 C47 N8 115.6(3) ?
C48 C47 Fe2 146.5(2) ?
C52 C47 Fe2 75.0(2) ?
N8 C47 Fe2 45.76(15) ?
C49 C48 C47 120.1(4) ?
C49 C48 H48 119.9 ?
C47 C48 H48 119.9 ?
C48 C49 C50 120.6(4) ?
C48 C49 H49 119.7 ?
C50 C49 H49 119.7 ?
C51 C50 C49 120.0(4) ?
C51 C50 H50 120.0 ?
C49 C50 H50 120.0 ?
C50 C51 C52 121.0(4) ?
C50 C51 H51 119.5 ?
C52 C51 H51 119.5 ?
C51 C52 C47 118.7(3) ?
C51 C52 N5 124.2(3) ?
C47 C52 N5 116.2(3) y
C51 C52 Fe2 147.7(3) ?
C47 C52 Fe2 75.3(2) ?
N5 C52 Fe2 45.89(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O1 1.784(2) y
Fe1 N3 2.020(3) y
Fe1 N2 2.023(3) y
Fe1 N4 2.038(3) y
Fe1 N1 2.045(3) y
Fe1 C21 2.745(3) ?
Fe1 C26 2.753(4) ?
Fe1 C13 2.851(4) ?
Fe1 C8 2.859(4) ?
Fe1 Fe2 3.2762(11) ?
Fe2 O1 1.788(2) y
Fe2 N7 2.022(3) y
Fe2 N6 2.026(3) y
Fe2 N8 2.043(3) y
Fe2 N5 2.044(3) y
Fe2 C52 2.759(4) ?
Fe2 C47 2.762(4) ?
Fe2 C34 2.857(4) ?
Fe2 C39 2.860(4) ?
N1 C1 1.317(5) ?
N1 C26 1.424(4) ?
C1 C3 1.429(5) ?
C1 C2 1.509(5) ?
C2 H2A 0.9600 ?
C2 H2B 0.9600 ?
C2 H2C 0.9600 ?
C3 C7 1.392(5) ?
C3 C4 1.480(5) ?
C4 O2 1.207(5) ?
C4 O3 1.342(5) ?
O3 C5 1.452(5) ?
C5 C6X 1.390(11) ?
C5 C6 1.595(15) ?
C5 H5A 0.9700 ?
C5 H5B 0.9700 ?
C6 H6A 0.9600 ?
C6 H6B 0.9600 ?
C6 H6C 0.9600 ?
C6X H6D 0.9600 ?
C6X H6E 0.9600 ?
C6X H6F 0.9600 ?
C7 N2 1.311(5) ?
C7 H7 0.9300 ?
N2 C8 1.413(5) ?
C8 C9 1.391(5) ?
C8 C13 1.405(5) ?
C9 C10 1.385(6) ?
C9 H9 0.9300 ?
C10 C11 1.384(6) ?
C10 H10 0.9300 ?
C11 C12 1.374(6) ?
C11 H11 0.9300 ?
C12 C13 1.381(5) ?
C12 H12 0.9300 ?
C13 N3 1.416(5) ?
N3 C14 1.320(5) ?
C14 C15 1.388(5) ?
C14 H14 0.9300 ?
C15 C19 1.430(5) ?
C15 C16 1.470(6) ?
C16 O5 1.192(5) ?
C16 O4 1.327(6) ?
O4 C17 1.455(17) ?
O4 C17X 1.530(11) ?
C17 C18 1.36(4) ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C18 H18A 0.9600 ?
C18 H18B 0.9600 ?
C18 H18C 0.9600 ?
C17X C18X 1.360(17) ?
C17X H17C 0.9700 ?
C17X H17D 0.9700 ?
C18X H18D 0.9600 ?
C18X H18E 0.9600 ?
C18X H18F 0.9600 ?
C19 N4 1.311(5) ?
C19 C20 1.515(5) ?
C20 H20A 0.9600 ?
C20 H20B 0.9600 ?
C20 H20C 0.9600 ?
N4 C21 1.412(5) ?
C21 C22 1.393(5) ?
C21 C26 1.407(5) ?
C22 C23 1.377(6) ?
C22 H22 0.9300 ?
C23 C24 1.371(6) ?
C23 H23 0.9300 ?
C24 C25 1.377(6) ?
C24 H24 0.9300 ?
C25 C26 1.385(5) ?
C25 H25 0.9300 ?
N5 C27 1.320(4) ?
N5 C52 1.416(4) ?
C27 C29 1.429(5) ?
C27 C28 1.499(5) ?
C28 H28A 0.9600 ?
C28 H28B 0.9600 ?
C28 H28C 0.9600 ?
C29 C33 1.397(5) ?
C29 C30 1.470(5) ?
C30 O6 1.207(5) ?
C30 O7 1.342(5) ?
O7 C31 1.452(5) ?
C31 C32X 1.382(14) ?
C31 C32 1.466(11) ?
C31 H31A 0.9700 ?
C31 H31B 0.9700 ?
C32 H32A 0.9600 ?
C32 H32B 0.9600 ?
C32 H32C 0.9600 ?
C32X H32D 0.9600 ?
C32X H32E 0.9600 ?
C32X H32F 0.9600 ?
C33 N6 1.314(4) ?
C33 H33 0.9300 ?
N6 C34 1.409(4) ?
C34 C35 1.390(5) ?
C34 C39 1.404(5) ?
C35 C36 1.377(5) ?
C35 H35 0.9300 ?
C36 C37 1.384(5) ?
C36 H36 0.9300 ?
C37 C38 1.381(5) ?
C37 H37 0.9300 ?
C38 C39 1.386(5) ?
C38 H38 0.9300 ?
C39 N7 1.411(4) ?
N7 C40 1.318(4) ?
C40 C41 1.397(5) ?
C40 H40 0.9300 ?
C41 C45 1.429(5) ?
C41 C42 1.478(5) ?
C42 O8 1.199(4) ?
C42 O9 1.356(5) ?
O9 C43 1.443(4) ?
C43 C44 1.495(6) ?
C43 H43A 0.9700 ?
C43 H43B 0.9700 ?
C44 H44A 0.9600 ?
C44 H44B 0.9600 ?
C44 H44C 0.9600 ?
C45 N8 1.322(4) ?
C45 C46 1.512(5) ?
C46 H46A 0.9600 ?
C46 H46B 0.9600 ?
C46 H46C 0.9600 ?
N8 C47 1.419(5) ?
C47 C48 1.393(5) ?
C47 C52 1.412(5) ?
C48 C49 1.375(5) ?
C48 H48 0.9300 ?
C49 C50 1.378(6) ?
C49 H49 0.9300 ?
C50 C51 1.374(6) ?
C50 H50 0.9300 ?
C51 C52 1.391(5) ?
C51 H51 0.9300 ?
O11 O11X 0.95(2) ?
