#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/69/2206951.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_2206951
loop_
_publ_author_name
'Mata, Ignasi'
'Rodríguez, E.'
'Molins, Elies'
_publ_section_title
;Dodeca-μ₂-hydroxo-di-μ₃-oxo-hexakis(1,4,7-triazacyclononane-κ³N,N',N'')octairon(III)
 octabromide octahydrate
;
_journal_coeditor_code           HB6243
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1988
_journal_page_last               m1990
_journal_paper_doi               10.1107/S1600536805028436
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe8 O2 (O H)12 (C6 H12 N3)6] Br8, 8H2 O'
_chemical_formula_moiety         'C36 H118 Br8 Fe8 N18 O22'
_chemical_formula_sum            'C36 H118 Br8 Fe8 N18 O22'
_chemical_formula_weight         2241.56
_chemical_name_systematic
;
dodeca-μ₂-hydroxo-di-μ₃-oxo-hexakis(1,4,7-triazacyclononane-
κ³N,N',N'')octairon(III) octabromide octahydrate
;
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.150(10)
_cell_angle_beta                 113.340(10)
_cell_angle_gamma                101.430(10)
_cell_formula_units_Z            1
_cell_length_a                   13.257(2)
_cell_length_b                   13.5640(10)
_cell_length_c                   14.831(4)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      10.8
_cell_volume                     2163.0(8)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled ω/2θ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13602
_diffrn_reflns_theta_full        30.41
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 90
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.061
_exptl_absorpt_correction_T_max  0.241
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.528
_refine_diff_density_min         -1.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         13085
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.116P)²+2.3967P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.2094
_reflns_number_gt                8217
_reflns_number_total             13085
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6243.cif
_cod_data_source_block           I
_cod_database_code               2206951
_cod_database_fobs_code          2206951
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
Fe1 0.38470(5) 0.41654(5) 0.45841(4) 0.02143(14) Uani d . 1 . . Fe
Fe3 0.17949(5) 0.37903(5) 0.24373(5) 0.02466(14) Uani d . 1 . . Fe
Fe4 0.46203(5) 0.42176(5) 0.26224(5) 0.02378(14) Uani d . 1 . . Fe
Fe2 0.37002(6) 0.28676(5) 0.59163(5) 0.02721(15) Uani d . 1 . . Fe
Br1 0.14652(10) 0.03211(6) 0.18139(7) 0.0703(3) Uani d P 0.818(2) A 1 Br
Br2 0.28821(7) 0.55595(10) 0.05697(9) 0.0798(4) Uani d P 0.842(2) . . Br
Br3 0.95535(13) 0.59745(13) 0.48690(12) 0.0614(3) Uani d P 0.5 B 2 Br
Br4 0.14384(18) 0.80749(17) 0.5326(2) 0.0904(6) Uani d P 0.5 C 3 Br
Br5 0.6200(2) 0.1003(2) 0.0123(3) 0.1045(14) Uani d P 0.355(3) . . Br
Br6 0.6718(8) 0.2531(8) 0.5427(5) 0.078(2) Uani d P 0.193(4) D 4 Br
Br7 0.7576(2) 0.2517(2) 0.7566(2) 0.0673(9) Uani d P 0.304(3) E 5 Br
Br8 0.6862(4) 0.2526(4) 0.5888(7) 0.118(3) Uani d P 0.307(4) F 6 Br
Br9 0.3279(8) 0.9238(13) 0.2042(11) 0.203(6) Uani d P 0.182(2) G 7 Br
N21 0.2714(4) 0.2378(4) 0.6676(4) 0.0389(9) Uani d . 1 . . N
H21 0.2522 0.296 0.6967 0.047 Uiso calc R 1 . . H
C22 0.3545(7) 0.2210(7) 0.7575(5) 0.0654(19) Uani d U 1 . . C
H22A 0.3122 0.1877 0.7877 0.078 Uiso calc R 1 . . H
H22B 0.4142 0.2926 0.8148 0.078 Uiso calc R 1 . . H
C23 0.4116(7) 0.1483(8) 0.7194(8) 0.081(2) Uani d U 1 . . C
H23A 0.357 0.0713 0.6812 0.097 Uiso calc R 1 . . H
H23B 0.4801 0.1549 0.7819 0.097 Uiso calc R 1 . . H
N24 0.4497(5) 0.1767(4) 0.6448(5) 0.0574(14) Uani d U 1 . . N
H24 0.5298 0.2108 0.6808 0.069 Uiso calc R 1 . . H
C25 0.4121(9) 0.0782(6) 0.5427(9) 0.091(3) Uani d U 1 . . C
H25A 0.4528 0.0991 0.5058 0.109 Uiso calc R 1 . . H
H25B 0.4349 0.0202 0.5606 0.109 Uiso calc R 1 . . H
C26 0.2833(10) 0.0337(5) 0.4686(8) 0.088(3) Uani d U 1 . . C
H26A 0.2654 -0.0148 0.396 0.105 Uiso calc R 1 . . H
H26B 0.2436 -0.0106 0.4935 0.105 Uiso calc R 1 . . H
N27 0.2383(5) 0.1243(4) 0.4638(4) 0.0518(13) Uani d . 1 . . N
H27 0.222 0.1254 0.3986 0.062 Uiso calc R 1 . . H
C28 0.1306(6) 0.1135(6) 0.4728(5) 0.0641(19) Uani d . 1 . . C
H28A 0.0728 0.0383 0.4244 0.077 Uiso calc R 1 . . H
H28B 0.0967 0.165 0.4513 0.077 Uiso calc R 1 . . H
C29 0.1604(6) 0.1388(5) 0.5898(5) 0.0542(15) Uani d . 1 . . C
H29A 0.0962 0.1527 0.6007 0.065 Uiso calc R 1 . . H
H29B 0.1695 0.0748 0.6034 0.065 Uiso calc R 1 . . H
N31 0.0464(4) 0.2338(3) 0.0927(3) 0.0362(9) Uani d . 1 . . N
H31 0.0786 0.1809 0.0811 0.043 Uiso calc R 1 . . H
C32 -0.0611(5) 0.1845(5) 0.0954(5) 0.0537(15) Uani d . 1 . . C
H32A -0.0851 0.1039 0.0645 0.064 Uiso calc R 1 . . H
H32B -0.1248 0.2027 0.0517 0.064 Uiso calc R 1 . . H
C33 -0.0388(6) 0.2283(6) 0.2101(5) 0.0610(17) Uani d . 1 . . C
H33A 0.0072 0.1926 0.2483 0.073 Uiso calc R 1 . . H
H33B -0.1133 0.2113 0.2102 0.073 Uiso calc R 1 . . H
N34 0.0268(4) 0.3516(4) 0.2666(4) 0.0454(11) Uani d . 1 . . N
H34 0.0525 0.3746 0.3391 0.054 Uiso calc R 1 . . H
C35 -0.0454(5) 0.4157(6) 0.2277(5) 0.0624(19) Uani d . 1 . . C
H35A -0.0682 0.4499 0.2806 0.075 Uiso calc R 1 . . H
H35B -0.1168 0.3652 0.1595 0.075 Uiso calc R 1 . . H
C36 0.0222(6) 0.5046(5) 0.2110(6) 0.0568(16) Uani d . 1 . . C
H36A -0.0318 0.5317 0.1681 0.068 Uiso calc R 1 . . H
H36B 0.0792 0.5668 0.281 0.068 Uiso calc R 1 . . H
N37 0.0846(4) 0.4594(3) 0.1540(3) 0.0381(9) Uani d . 1 . . N
H37 0.1377 0.5173 0.1585 0.046 Uiso calc R 1 . . H
C38 0.0040(5) 0.3795(5) 0.0365(4) 0.0487(13) Uani d . 1 . . C
H38A 0.015 0.4146 -0.0084 0.058 Uiso calc R 1 . . H
H38B -0.0773 0.3629 0.0211 0.058 Uiso calc R 1 . . H
C39 0.0254(5) 0.2721(5) 0.0063(4) 0.0446(12) Uani d . 1 . . C
H39A -0.0426 0.2154 -0.0615 0.054 Uiso calc R 1 . . H
H39B 0.0934 0.2832 -0.0047 0.054 Uiso calc R 1 . . H
N41 0.6287(4) 0.4085(4) 0.2840(4) 0.0400(10) Uani d . 1 . . N
H41 0.6864 0.474 0.3396 0.048 Uiso calc R 1 . . H
C42 0.6394(6) 0.3212(6) 0.3224(6) 0.0622(18) Uani d U 1 . . C
H42A 0.6533 0.349 0.3966 0.075 Uiso calc R 1 . . H
H42B 0.7064 0.3029 0.3222 0.075 Uiso calc R 1 . . H
C43 0.5302(7) 0.2193(6) 0.2515(7) 0.0684(19) Uani d U 1 . . C
H43A 0.5271 0.1746 0.2908 0.082 Uiso calc R 1 . . H
H43B 0.5335 0.1754 0.1878 0.082 Uiso calc R 1 . . H
N44 0.4207(4) 0.2446(3) 0.2154(3) 0.0380(9) Uani d U 1 . . N
H44 0.3816 0.2238 0.2489 0.046 Uiso calc R 1 . . H
C45 0.3415(6) 0.1840(5) 0.0975(5) 0.0558(16) Uani d . 1 . . C
H45A 0.2634 0.1854 0.0808 0.067 Uiso calc R 1 . . H
H45B 0.3349 0.1067 0.0739 0.067 Uiso calc R 1 . . H
C46 0.3842(6) 0.2330(5) 0.0368(5) 0.0618(18) Uani d . 1 . . C
H46A 0.3188 0.2094 -0.0354 0.074 Uiso calc R 1 . . H
H46B 0.4434 0.205 0.0283 0.074 Uiso calc R 1 . . H
N47 0.4359(4) 0.3564(4) 0.0928(3) 0.0413(10) Uani d . 1 . . N
H47 0.3849 0.3827 0.0541 0.05 Uiso calc R 1 . . H
C48 0.6458(6) 0.3927(7) 0.1890(6) 0.0625(18) Uani d . 1 . . C
H48A 0.6495 0.3195 0.1606 0.075 Uiso calc R 1 . . H
H48B 0.7207 0.4479 0.212 0.075 Uiso calc R 1 . . H
C49 0.5495(6) 0.4026(7) 0.1005(6) 0.0657(19) Uani d . 1 . . C
H49A 0.5667 0.4806 0.1149 0.079 Uiso calc R 1 . . H
H49B 0.5457 0.3632 0.0316 0.079 Uiso calc R 1 . . H
O1 0.4947(2) 0.4541(2) 0.4054(2) 0.0224(5) Uani d . 1 . . O
O2 0.4408(3) 0.3007(2) 0.5006(3) 0.0293(6) Uani d . 1 . . O
H2 0.4871 0.2644 0.4819 0.035 Uiso calc R 1 . . H
O3 0.2873(3) 0.3726(3) 0.5304(3) 0.0294(6) Uani d . 1 . . O
H3 0.2233 0.3892 0.5325 0.035 Uiso calc R 1 . . H
O4 0.2782(3) 0.4932(2) 0.3937(2) 0.0270(6) Uani d . 1 . . O
H4 0.2768 0.5632 0.4265 0.032 Uiso calc R 1 . . H
O5 0.2535(3) 0.2935(2) 0.3108(3) 0.0319(7) Uani d . 1 . . O
H5 0.2345 0.2167 0.2834 0.038 Uiso calc R 1 . . H
O6 0.2930(3) 0.4050(3) 0.1919(3) 0.0300(6) Uani d . 1 . . O
H6 0.2641 0.4101 0.1259 0.036 Uiso calc R 1 . . H
O7 0.5151(3) 0.5772(3) 0.2746(3) 0.0318(7) Uani d . 1 . . O
H7 0.4819 0.5857 0.2106 0.038 Uiso calc R 1 . . H
O1W 0.9176(6) 0.9244(5) 0.1886(5) 0.099(2) Uani d . 1 . . O
O2W 0.2056(6) 0.3635(6) 0.8483(10) 0.164(5) Uani d . 1 . . O
O3W 0.7496(10) 0.0277(6) 0.2135(9) 0.167(5) Uani d . 1 . . O
O4W 0.0220(10) 0.7811(8) 0.2762(9) 0.160(4) Uani d . 1 . . O
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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-8 3 2
-2 2 -7
2 7 -4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Fe1 O1 2_666 . 83.91(12)
O1 Fe1 O2 2_666 . 95.91(13)
O1 Fe1 O2 . . 96.38(12)
O1 Fe1 O4 2_666 . 98.71(12)
O1 Fe1 O4 . . 95.91(12)
O2 Fe1 O4 . . 161.78(13)
O1 Fe1 O5 2_666 . 173.99(13)
O1 Fe1 O5 . . 94.96(13)
O2 Fe1 O5 . . 90.08(13)
O4 Fe1 O5 . . 75.50(12)
O1 Fe1 O3 2_666 . 92.34(12)
O1 Fe1 O3 . . 171.78(12)
O2 Fe1 O3 . . 76.68(12)
O4 Fe1 O3 . . 91.88(12)
O5 Fe1 O3 . . 89.51(13)
O1 Fe1 Fe1 2_666 2_666 42.06(8)
O1 Fe1 Fe1 . 2_666 41.85(8)
O2 Fe1 Fe1 . 2_666 98.28(9)
O4 Fe1 Fe1 . 2_666 99.85(9)
O5 Fe1 Fe1 . 2_666 136.52(10)
O3 Fe1 Fe1 . 2_666 133.97(9)
O5 Fe3 O4 . . 80.12(13)
O5 Fe3 O6 . . 91.56(14)
O4 Fe3 O6 . . 98.27(13)
O5 Fe3 N37 . . 174.22(14)
O4 Fe3 N37 . . 105.55(14)
O6 Fe3 N37 . . 88.72(16)
O5 Fe3 N34 . . 99.76(18)
O4 Fe3 N34 . . 90.68(15)
O6 Fe3 N34 . . 166.65(16)
N37 Fe3 N34 . . 79.30(18)
O5 Fe3 N31 . . 94.51(14)
O4 Fe3 N31 . . 166.15(15)
O6 Fe3 N31 . . 94.61(15)
N37 Fe3 N31 . . 79.71(16)
N34 Fe3 N31 . . 77.58(17)
O1 Fe4 O6 . . 101.07(13)
O1 Fe4 O7 . . 100.17(13)
O6 Fe4 O7 . . 91.81(13)
O1 Fe4 N41 . . 96.46(15)
O6 Fe4 N41 . . 161.28(15)
O7 Fe4 N41 . . 91.53(16)
O1 Fe4 N44 . . 93.52(15)
O6 Fe4 N44 . . 93.53(16)
O7 Fe4 N44 . . 164.07(15)
N41 Fe4 N44 . . 78.78(17)
O1 Fe4 N47 . . 168.91(16)
O6 Fe4 N47 . . 85.47(15)
O7 Fe4 N47 . . 88.46(15)
N41 Fe4 N47 . . 76.20(17)
N44 Fe4 N47 . . 77.03(17)
O3 Fe2 O2 . . 81.87(13)
O3 Fe2 O7 . 2_666 90.92(14)
O2 Fe2 O7 . 2_666 98.43(14)
O3 Fe2 N24 . . 174.30(19)
O2 Fe2 N24 . . 97.05(17)
O7 Fe2 N24 2_666 . 94.8(2)
O3 Fe2 N21 . . 100.72(16)
O2 Fe2 N21 . . 168.66(15)
O7 Fe2 N21 2_666 . 92.59(15)
N24 Fe2 N21 . . 79.26(19)
O3 Fe2 N27 . . 95.36(18)
O2 Fe2 N27 . . 90.87(16)
O7 Fe2 N27 2_666 . 169.44(16)
N24 Fe2 N27 . . 79.0(2)
N21 Fe2 N27 . . 77.93(18)
C22 N21 C29 . . 113.4(5)
C22 N21 Fe2 . . 105.5(4)
C29 N21 Fe2 . . 113.1(3)
C22 N21 H21 . . 108.2
C29 N21 H21 . . 108.2
Fe2 N21 H21 . . 108.2
N21 C22 C23 . . 110.9(6)
N21 C22 H22A . . 109.5
C23 C22 H22A . . 109.5
N21 C22 H22B . . 109.5
C23 C22 H22B . . 109.5
H22A C22 H22B . . 108.1
C22 C23 N24 . . 112.4(5)
C22 C23 H23A . . 109.1
N24 C23 H23A . . 109.1
C22 C23 H23B . . 109.1
N24 C23 H23B . . 109.1
H23A C23 H23B . . 107.8
C25 N24 C23 . . 113.4(6)
C25 N24 Fe2 . . 104.8(5)
C23 N24 Fe2 . . 110.7(4)
C25 N24 H24 . . 109.3
C23 N24 H24 . . 109.3
Fe2 N24 H24 . . 109.3
C26 C25 N24 . . 112.2(6)
C26 C25 H25A . . 109.2
N24 C25 H25A . . 109.2
C26 C25 H25B . . 109.2
N24 C25 H25B . . 109.2
H25A C25 H25B . . 107.9
N27 C26 C25 . . 111.5(6)
N27 C26 H26A . . 109.3
C25 C26 H26A . . 109.3
N27 C26 H26B . . 109.3
C25 C26 H26B . . 109.3
H26A C26 H26B . . 108
C28 N27 C26 . . 115.4(5)
C28 N27 Fe2 . . 106.6(4)
C26 N27 Fe2 . . 111.7(5)
C28 N27 H27 . . 107.6
C26 N27 H27 . . 107.6
Fe2 N27 H27 . . 107.6
N27 C28 C29 . . 109.6(5)
N27 C28 H28A . . 109.8
C29 C28 H28A . . 109.8
N27 C28 H28B . . 109.8
C29 C28 H28B . . 109.8
H28A C28 H28B . . 108.2
N21 C29 C28 . . 110.7(5)
N21 C29 H29A . . 109.5
C28 C29 H29A . . 109.5
N21 C29 H29B . . 109.5
C28 C29 H29B . . 109.5
H29A C29 H29B . . 108.1
C32 N31 C39 . . 114.0(4)
C32 N31 Fe3 . . 113.4(3)
C39 N31 Fe3 . . 105.2(3)
C32 N31 H31 . . 108
C39 N31 H31 . . 108
Fe3 N31 H31 . . 108
N31 C32 C33 . . 110.2(4)
N31 C32 H32A . . 109.6
C33 C32 H32A . . 109.6
N31 C32 H32B . . 109.6
C33 C32 H32B . . 109.6
H32A C32 H32B . . 108.1
C32 C33 N34 . . 109.6(5)
C32 C33 H33A . . 109.7
N34 C33 H33A . . 109.7
C32 C33 H33B . . 109.7
N34 C33 H33B . . 109.7
H33A C33 H33B . . 108.2
C35 N34 C33 . . 113.8(5)
C35 N34 Fe3 . . 112.0(4)
C33 N34 Fe3 . . 106.0(4)
C35 N34 H34 . . 108.3
C33 N34 H34 . . 108.3
Fe3 N34 H34 . . 108.3
N34 C35 C36 . . 111.1(5)
N34 C35 H35A . . 109.4
C36 C35 H35A . . 109.4
N34 C35 H35B . . 109.4
C36 C35 H35B . . 109.4
H35A C35 H35B . . 108
N37 C36 C35 . . 110.3(5)
N37 C36 H36A . . 109.6
C35 C36 H36A . . 109.6
N37 C36 H36B . . 109.6
C35 C36 H36B . . 109.6
H36A C36 H36B . . 108.1
C36 N37 C38 . . 113.8(4)
C36 N37 Fe3 . . 105.7(4)
C38 N37 Fe3 . . 110.9(3)
C36 N37 H37 . . 108.8
C38 N37 H37 . . 108.8
Fe3 N37 H37 . . 108.8
N37 C38 C39 . . 112.8(4)
N37 C38 H38A . . 109
C39 C38 H38A . . 109
N37 C38 H38B . . 109
C39 C38 H38B . . 109
H38A C38 H38B . . 107.8
N31 C39 C38 . . 110.8(5)
N31 C39 H39A . . 109.5
C38 C39 H39A . . 109.5
N31 C39 H39B . . 109.5
C38 C39 H39B . . 109.5
H39A C39 H39B . . 108.1
C48 N41 C42 . . 114.8(5)
C48 N41 Fe4 . . 114.9(4)
C42 N41 Fe4 . . 105.8(4)
C48 N41 H41 . . 106.9
C42 N41 H41 . . 106.9
Fe4 N41 H41 . . 106.9
N41 C42 C43 . . 110.7(5)
N41 C42 H42A . . 109.5
C43 C42 H42A . . 109.5
N41 C42 H42B . . 109.5
C43 C42 H42B . . 109.5
H42A C42 H42B . . 108.1
C42 C43 N44 . . 112.9(5)
C42 C43 H43A . . 109
N44 C43 H43A . . 109
C42 C43 H43B . . 109
N44 C43 H43B . . 109
H43A C43 H43B . . 107.8
C45 N44 C43 . . 112.6(5)
C45 N44 Fe4 . . 108.8(4)
C43 N44 Fe4 . . 111.0(4)
C45 N44 H44 . . 108.1
C43 N44 H44 . . 108.1
Fe4 N44 H44 . . 108.1
N44 C45 C46 . . 112.0(5)
N44 C45 H45A . . 109.2
C46 C45 H45A . . 109.2
N44 C45 H45B . . 109.2
C46 C45 H45B . . 109.2
H45A C45 H45B . . 107.9
C45 C46 N47 . . 112.2(5)
C45 C46 H46A . . 109.2
N47 C46 H46A . . 109.2
C45 C46 H46B . . 109.2
N47 C46 H46B . . 109.2
H46A C46 H46B . . 107.9
C49 N47 C46 . . 113.0(5)
C49 N47 Fe4 . . 107.5(4)
C46 N47 Fe4 . . 111.9(4)
C49 N47 H47 . . 108.1
C46 N47 H47 . . 108.1
Fe4 N47 H47 . . 108.1
N41 C48 C49 . . 112.7(5)
N41 C48 H48A . . 109
C49 C48 H48A . . 109
N41 C48 H48B . . 109
C49 C48 H48B . . 109
H48A C48 H48B . . 107.8
N47 C49 C48 . . 111.0(6)
N47 C49 H49A . . 109.4
C48 C49 H49A . . 109.4
N47 C49 H49B . . 109.4
C48 C49 H49B . . 109.4
H49A C49 H49B . . 108
Fe4 O1 Fe1 . 2_666 129.53(15)
Fe4 O1 Fe1 . . 128.80(15)
Fe1 O1 Fe1 2_666 . 96.09(12)
Fe2 O2 Fe1 . . 100.32(13)
Fe2 O2 H2 . . 129.8
Fe1 O2 H2 . . 129.8
Fe2 O3 Fe1 . . 99.07(14)
Fe2 O3 H3 . . 130.5
Fe1 O3 H3 . . 130.5
Fe3 O4 Fe1 . . 100.53(13)
Fe3 O4 H4 . . 129.7
Fe1 O4 H4 . . 129.7
Fe3 O5 Fe1 . . 101.18(14)
Fe3 O5 H5 . . 129.4
Fe1 O5 H5 . . 129.4
Fe3 O6 Fe4 . . 128.36(16)
Fe3 O6 H6 . . 115.8
Fe4 O6 H6 . . 115.8
Fe2 O7 Fe4 2_666 . 126.63(17)
Fe2 O7 H7 2_666 . 116.7
Fe4 O7 H7 . . 116.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O1 2_666 1.959(3) y
Fe1 O1 . 1.967(3) y
Fe1 O2 . 2.030(3) y
Fe1 O4 . 2.031(3) y
Fe1 O5 . 2.040(3) y
Fe1 O3 . 2.084(3) y
Fe1 Fe1 2_666 2.9193(12) ?
Fe3 O5 . 1.922(3) y
Fe3 O4 . 1.950(3) y
Fe3 O6 . 1.964(3) y
Fe3 N37 . 2.159(4) y
Fe3 N34 . 2.161(4) y
Fe3 N31 . 2.181(4) y
Fe4 O1 . 1.872(3) y
Fe4 O6 . 1.989(3) y
Fe4 O7 . 2.011(3) y
Fe4 N41 . 2.156(4) y
Fe4 N44 . 2.167(4) y
Fe4 N47 . 2.241(4) y
Fe2 O3 . 1.939(3) y
Fe2 O2 . 1.957(3) y
Fe2 O7 2_666 1.967(3) ?
Fe2 N24 . 2.160(5) y
Fe2 N21 . 2.170(4) y
Fe2 N27 . 2.179(5) y
N21 C22 . 1.473(8) ?
N21 C29 . 1.485(7) ?
N21 H21 . 0.91 ?
C22 C23 . 1.468(12) ?
C22 H22A . 0.97 ?
C22 H22B . 0.97 ?
C23 N24 . 1.503(9) ?
C23 H23A . 0.97 ?
C23 H23B . 0.97 ?
N24 C25 . 1.485(11) ?
N24 H24 . 0.91 ?
C25 C26 . 1.477(14) ?
C25 H25A . 0.97 ?
C25 H25B . 0.97 ?
C26 N27 . 1.477(10) ?
C26 H26A . 0.97 ?
C26 H26B . 0.97 ?
N27 C28 . 1.469(9) ?
N27 H27 . 0.91 ?
C28 C29 . 1.522(9) ?
C28 H28A . 0.97 ?
C28 H28B . 0.97 ?
C29 H29A . 0.97 ?
C29 H29B . 0.97 ?
N31 C32 . 1.471(7) ?
N31 C39 . 1.475(7) ?
N31 H31 . 0.91 ?
C32 C33 . 1.496(9) ?
C32 H32A . 0.97 ?
C32 H32B . 0.97 ?
C33 N34 . 1.493(8) ?
C33 H33A . 0.97 ?
C33 H33B . 0.97 ?
N34 C35 . 1.487(9) ?
N34 H34 . 0.91 ?
C35 C36 . 1.500(11) ?
C35 H35A . 0.97 ?
C35 H35B . 0.97 ?
C36 N37 . 1.485(8) ?
C36 H36A . 0.97 ?
C36 H36B . 0.97 ?
N37 C38 . 1.498(7) ?
N37 H37 . 0.91 ?
C38 C39 . 1.503(8) ?
C38 H38A . 0.97 ?
C38 H38B . 0.97 ?
C39 H39A . 0.97 ?
C39 H39B . 0.97 ?
N41 C48 . 1.471(8) ?
N41 C42 . 1.473(8) ?
N41 H41 . 0.91 ?
C42 C43 . 1.486(10) ?
C42 H42A . 0.97 ?
C42 H42B . 0.97 ?
C43 N44 . 1.486(8) ?
C43 H43A . 0.97 ?
C43 H43B . 0.97 ?
N44 C45 . 1.463(7) ?
N44 H44 . 0.91 ?
C45 C46 . 1.484(9) ?
C45 H45A . 0.97 ?
C45 H45B . 0.97 ?
C46 N47 . 1.480(8) ?
C46 H46A . 0.97 ?
C46 H46B . 0.97 ?
N47 C49 . 1.455(7) ?
N47 H47 . 0.91 ?
C48 C49 . 1.490(10) ?
C48 H48A . 0.97 ?
C48 H48B . 0.97 ?
C49 H49A . 0.97 ?
C49 H49B . 0.97 ?
O1 Fe1 2_666 1.959(3) ?
O2 H2 . 0.93 ?
O3 H3 . 0.93 ?
O4 H4 . 0.93 ?
O5 H5 . 0.93 ?
O6 H6 . 0.93 ?
O7 Fe2 2_666 1.967(3) ?
O7 H7 . 0.93 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O5 H5 Br1 . 0.93 2.24 3.142(3) 165
O6 H6 Br2 . 0.93 2.52 3.271(3) 139
O7 H7 Br2 . 0.93 2.52 3.306(3) 143
O3 H3 Br3 2_666 0.93 2.32 3.242(3) 171
O2 H2 Br6 . 0.93 2.31 3.116(10) 145
O4 H4 Br6 2_666 0.93 2.29 3.123(10) 149
O2 H2 Br8 . 0.93 2.55 3.274(5) 135
O4 H4 Br8 2_666 0.93 2.55 3.298(5) 138
N24 H24 Br7 . 0.91 2.64 3.519(6) 164
N24 H24 Br8 . 0.91 2.96 3.591(8) 128
N27 H27 Br1 . 0.91 2.72 3.562(5) 155
N31 H31 Br1 . 0.91 2.94 3.643(4) 136
N34 H34 Br3 2_666 0.91 2.54 3.403(5) 159
N37 H37 Br7 2_666 0.91 2.79 3.578(5) 146
N37 H37 Br2 . 0.91 3.00 3.731(5) 139
N41 H41 Br3 . 0.91 3.08 3.853(5) 144
N47 H47 Br2 . 0.91 2.89 3.689(5) 148
