data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Peter Tasker'
_publ_contact_author_email       P.A.TASKER@ED.AC.UK

_publ_section_title              
;
Surface binding vs. sequestration; the uptake of
benzohydroxamic acid at iron(III) oxide surfaces
;
loop_
_publ_author_name
'Peter Tasker'
'Euan K Brechin'
'Steven G Harris'
'Iria M Rio-Echevarria'
'Fraser White'

# Attachment 'PT0510 - [Fe2(mu2-bha)2(bha)2Br2].CIF'

data_pt0510
_database_code_depnum_ccdc_archive 'CCDC 689505'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_compound_source        'Iria Rio'
_exptl_crystal_recrystallization_method 'Evaporation of MeOH/MeCN solution'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H24 Br2 Fe2 N4 O8'
_chemical_formula_sum            'C28 H24 Br2 Fe2 N4 O8'
_chemical_formula_weight         816.03

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'
Br Br -0.2901 2.4595 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
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'

_cell_length_a                   14.5538(9)
_cell_length_b                   16.2543(10)
_cell_length_c                   12.9684(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.814(4)
_cell_angle_gamma                90.00
_cell_volume                     3066.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5257
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      28.5

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    3.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  0.6
_exptl_absorpt_process_details   'SADABS 2004/1'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43236
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         30.57
_reflns_number_total             4680
_reflns_number_gt                3511
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'Shelxs Sheldrick'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

>>> The Following ALERTS were generated <<<
#------------------------------------------
Format: alert-number_ALERT_alert-type_alert-level text

094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.19

There are heavy atoms, Br and Fe which have caused this.

220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.18 Ratio
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C14
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3'
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C16
301_ALERT_3_C Main Residue Disorder ......................... 19.00 Perc.
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 34.50 Deg.
C1' -C6 -C1 1.555 1.555 1.555
779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 33.10 Deg.
C5 -C6 -C5' 1.555 1.555 1.555

The benzene rings in the molecule have reasonably high thermal motion. In one
case disorder exists.

912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 33

The data collection strategy used was to collect fully complete data to
2TH= 53deg. Some higher angle data were collected in the process and these
have been included in the refinement. Please refer to the completeness
statistics below

INTENSITY STATISTICS FOR DATASET # 1 pt0510.hkl

Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma

Inf - 1.94 246 246 100.0 21.91 748.7 68.11 0.0267 0.0133
1.94 - 1.53 245 245 100.0 21.18 364.8 59.67 0.0325 0.0127
1.53 - 1.33 252 252 100.0 16.73 226.3 45.93 0.0390 0.0151
1.33 - 1.20 264 264 100.0 14.83 176.0 40.89 0.0470 0.0174
1.20 - 1.11 264 264 100.0 13.29 139.2 33.05 0.0529 0.0204
1.11 - 1.04 276 276 100.0 11.13 116.3 28.68 0.0589 0.0249
1.04 - 0.98 299 299 100.0 9.80 88.6 23.41 0.0729 0.0298
0.98 - 0.93 302 302 100.0 9.27 73.5 20.06 0.0782 0.0366
0.93 - 0.89 316 316 100.0 7.98 54.0 15.48 0.1027 0.0497
0.89 - 0.86 261 261 100.0 6.77 51.7 13.91 0.1057 0.0570
0.86 - 0.83 303 303 100.0 5.85 35.1 9.49 0.1396 0.0872
0.83 - 0.80 358 358 100.0 5.45 36.9 9.14 0.1331 0.0911
0.80 - 0.78 252 252 100.0 5.30 32.2 7.95 0.1462 0.1068
0.78 - 0.76 309 309 100.0 5.06 22.1 5.76 0.1964 0.1631
0.76 - 0.74 308 310 99.4 3.30 23.3 4.55 0.1900 0.2126
0.74 - 0.72 377 383 98.4 2.04 19.0 2.74 0.1938 0.3597
0.72 - 0.70 198 224 88.4 1.67 20.7 2.86 0.2106 0.3512
#-----------------------------------------------------------------------------
0.80 - 0.70 1576 1610 97.9 3.61 24.2 5.04 0.1716 0.2093
Inf - 0.70 4830 4864 99.3 9.07 120.6 21.72 0.0415 0.0338

860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2

Hydrogen atoms on the Two nitrogen atoms, N1 and N11 were found on a difference
map and their positions refined with a restraint of 0.88 ang placed on the N-H
distance.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.6372P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4680
_refine_ls_number_parameters     224
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 -0.10027(2) -0.013711(16) 0.55319(2) 0.02451(8) Uani 1 1 d . . .
Br1 Br -0.250463(14) -0.023187(13) 0.464098(15) 0.03276(8) Uani 1 1 d . . .
C1 C 0.11606(9) -0.26905(10) 0.6127(2) 0.0381(9) Uani 0.692(5) 1 d PG A 1
H1 H 0.1641 -0.2294 0.6122 0.046 Uiso 0.692(5) 1 calc PR A 1
C2 C 0.13707(10) -0.35245(11) 0.6161(3) 0.0507(11) Uani 0.692(5) 1 d PG A 1
H2 H 0.1994 -0.3698 0.6179 0.061 Uiso 0.692(5) 1 calc PR A 1
C3 C 0.06685(14) -0.41039(8) 0.6168(2) 0.052(2) Uani 0.692(5) 1 d PG A 1
H3 H 0.0812 -0.4674 0.6191 0.062 Uiso 0.692(5) 1 calc PR A 1
C4 C -0.02438(12) -0.38493(9) 0.6141(3) 0.0586(15) Uani 0.692(5) 1 d PG A 1
H4 H -0.0724 -0.4245 0.6146 0.070 Uiso 0.692(5) 1 calc PR A 1
C5 C -0.04538(8) -0.30153(10) 0.6107(3) 0.0402(9) Uani 0.692(5) 1 d PG A 1
H5 H -0.1077 -0.2841 0.6089 0.048 Uiso 0.692(5) 1 calc PR A 1
C6 C 0.02484(10) -0.24359(7) 0.60999(13) 0.0293(4) Uani 1 1 d G . .
C1' C 0.09607(16) -0.27148(10) 0.6706(2) 0.044(2) Uani 0.308(5) 1 d PG A 2
H1' H 0.1343 -0.2328 0.7062 0.053 Uiso 0.308(5) 1 calc PR A 2
C2' C 0.11465(18) -0.35492(12) 0.6820(2) 0.062(3) Uani 0.308(5) 1 d PG A 2
H2' H 0.1638 -0.3726 0.7266 0.074 Uiso 0.308(5) 1 calc PR A 2
C3' C 0.06129(15) -0.41252(8) 0.6282(2) 0.080(9) Uani 0.308(5) 1 d PG A 2
H3' H 0.0740 -0.4696 0.6360 0.096 Uiso 0.308(5) 1 calc PR A 2
C4' C -0.01064(16) -0.38668(9) 0.5630(3) 0.067(4) Uani 0.308(5) 1 d PG A 2
H4' H -0.0471 -0.4260 0.5262 0.080 Uiso 0.308(5) 1 calc PR A 2
C5' C -0.02921(15) -0.30325(11) 0.5515(2) 0.045(2) Uani 0.308(5) 1 d PG A 2
H5' H -0.0772 -0.2854 0.5055 0.054 Uiso 0.308(5) 1 calc PR A 2
C7 C 0.00133(13) -0.15715(12) 0.59370(13) 0.0255(4) Uani 1 1 d . A .
N1 N 0.06194(12) -0.09954(10) 0.61767(12) 0.0282(4) Uani 1 1 d D . .
H6 H 0.1146(12) -0.1037(14) 0.6515(16) 0.034 Uiso 1 1 d D . .
O1 O 0.04096(10) -0.02073(7) 0.58526(10) 0.0265(3) Uani 1 1 d . . .
O2 O -0.07530(9) -0.13564(8) 0.55234(10) 0.0281(3) Uani 1 1 d . . .
N11 N -0.14554(13) 0.05633(10) 0.73854(12) 0.0303(4) Uani 1 1 d D A .
H16 H -0.1585(15) 0.0540(14) 0.8026(13) 0.036 Uiso 1 1 d D . .
O11 O -0.13729(10) -0.02018(8) 0.69660(10) 0.0282(3) Uani 1 1 d . . .
O12 O -0.09843(10) 0.10658(8) 0.59131(10) 0.0328(3) Uani 1 1 d . . .
C11 C -0.1766(2) 0.22150(15) 0.8141(2) 0.0531(7) Uani 1 1 d . A .
H11 H -0.1929 0.1776 0.8583 0.064 Uiso 1 1 calc R . .
C12 C -0.1931(2) 0.30208(16) 0.8429(2) 0.0615(8) Uani 1 1 d . . .
H12 H -0.2217 0.3131 0.9063 0.074 Uiso 1 1 calc R . .
C13 C -0.16842(18) 0.36566(15) 0.7812(2) 0.0496(6) Uani 1 1 d . . .
H13 H -0.1804 0.4208 0.8010 0.060 Uiso 1 1 calc R . .
C14 C -0.1271(3) 0.35005(16) 0.6922(2) 0.0804(11) Uani 1 1 d . . .
H14 H -0.1097 0.3944 0.6493 0.097 Uiso 1 1 calc R . .
C15 C -0.1093(3) 0.26920(16) 0.6618(2) 0.0713(10) Uani 1 1 d . A .
H15 H -0.0781 0.2590 0.5998 0.086 Uiso 1 1 calc R . .
C16 C -0.13675(15) 0.20487(12) 0.72144(15) 0.0315(4) Uani 1 1 d . . .
C17 C -0.12488(14) 0.12042(12) 0.68234(14) 0.0283(4) Uani 1 1 d . A .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.03259(17) 0.02069(15) 0.02039(14) -0.00113(10) 0.00301(11) 0.00041(11)
Br1 0.02987(13) 0.04159(15) 0.02690(12) 0.00372(8) 0.00218(8) 0.00466(8)
C1 0.0318(18) 0.0325(18) 0.050(2) -0.0016(15) -0.0036(15) -0.0003(14)
C2 0.0316(19) 0.043(2) 0.077(3) -0.0047(19) -0.0109(18) 0.0121(16)
C3 0.046(5) 0.025(5) 0.085(5) 0.005(4) -0.007(4) 0.010(4)
C4 0.041(2) 0.032(2) 0.101(4) 0.005(2) -0.019(2) -0.0052(18)
C5 0.0314(18) 0.0266(17) 0.062(3) 0.0024(16) -0.0067(16) 0.0005(14)
C6 0.0288(11) 0.0287(10) 0.0304(10) 0.0025(8) 0.0008(8) -0.0002(8)
C1' 0.025(4) 0.036(4) 0.070(6) 0.017(4) -0.011(4) -0.003(3)
C2' 0.031(5) 0.041(5) 0.114(9) 0.025(5) -0.002(5) 0.013(4)
C3' 0.058(16) 0.033(14) 0.15(2) 0.011(12) -0.016(14) 0.004(11)
C4' 0.049(6) 0.023(5) 0.128(12) 0.000(5) 0.005(6) -0.003(4)
C5' 0.048(5) 0.032(4) 0.055(6) -0.005(4) 0.003(4) 0.001(4)
C7 0.0307(10) 0.0260(10) 0.0200(9) -0.0013(7) 0.0033(7) -0.0008(8)
N1 0.0330(9) 0.0263(9) 0.0249(8) 0.0030(6) -0.0045(7) -0.0024(7)
O1 0.0350(8) 0.0222(7) 0.0224(7) 0.0014(5) 0.0015(5) -0.0033(6)
O2 0.0278(7) 0.0238(7) 0.0324(7) -0.0035(5) -0.0030(6) 0.0022(6)
N11 0.0475(11) 0.0239(8) 0.0193(8) -0.0012(6) 0.0018(7) 0.0072(8)
O11 0.0424(9) 0.0207(7) 0.0217(7) -0.0012(5) 0.0030(6) 0.0029(6)
O12 0.0518(9) 0.0229(7) 0.0242(7) -0.0019(5) 0.0092(6) 0.0010(6)
C11 0.082(2) 0.0317(13) 0.0477(15) -0.0110(10) 0.0280(13) -0.0027(13)
C12 0.086(2) 0.0387(14) 0.0614(18) -0.0193(12) 0.0327(16) -0.0024(14)
C13 0.0617(17) 0.0287(12) 0.0581(16) -0.0143(11) -0.0037(12) 0.0078(12)
C14 0.165(4) 0.0249(13) 0.0532(18) 0.0038(11) 0.029(2) 0.0095(18)
C15 0.145(3) 0.0320(14) 0.0384(14) -0.0006(11) 0.0304(16) 0.0093(16)
C16 0.0412(12) 0.0257(10) 0.0274(10) -0.0034(8) -0.0027(8) 0.0050(9)
C17 0.0354(11) 0.0256(10) 0.0237(9) -0.0013(7) -0.0007(8) 0.0057(8)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O11 1.9554(13) . ?
Fe1 O2 2.0151(13) . ?
Fe1 O12 2.0167(14) . ?
Fe1 O1 2.0872(15) . ?
Fe1 O1 2.0930(13) 5_556 ?
Fe1 Br1 2.4448(4) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C1 H1 0.9500 . ?
C2 C3 1.3900 . ?
C2 H2 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 C1' 1.3586 . ?
C6 C5' 1.4478 . ?
C6 C7 1.460(2) . ?
C1' C2' 1.3901 . ?
C1' H1' 0.9500 . ?
C2' C3' 1.3901 . ?
C2' H2' 0.9500 . ?
C3' C4' 1.3899 . ?
C3' H3' 0.9500 . ?
C4' C5' 1.3899 . ?
C4' H4' 0.9500 . ?
C5' H5' 0.9500 . ?
C7 O2 1.271(2) . ?
C7 N1 1.317(2) . ?
N1 O1 1.379(2) . ?
N1 H6 0.874(15) . ?
O1 Fe1 2.0930(13) 5_556 ?
N11 C17 1.312(3) . ?
N11 O11 1.364(2) . ?
N11 H16 0.859(16) . ?
O12 C17 1.273(2) . ?
C11 C16 1.378(3) . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.362(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.343(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.398(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.368(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.475(3) . ?

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
O11 Fe1 O2 90.43(5) . . ?
O11 Fe1 O12 79.69(5) . . ?
O2 Fe1 O12 162.54(6) . . ?
O11 Fe1 O1 96.13(6) . . ?
O2 Fe1 O1 76.74(5) . . ?
O12 Fe1 O1 89.93(6) . . ?
O11 Fe1 O1 164.55(6) . 5_556 ?
O2 Fe1 O1 100.31(5) . 5_556 ?
O12 Fe1 O1 87.04(5) . 5_556 ?
O1 Fe1 O1 75.84(6) . 5_556 ?
O11 Fe1 Br1 100.19(5) . . ?
O2 Fe1 Br1 95.40(4) . . ?
O12 Fe1 Br1 100.46(4) . . ?
O1 Fe1 Br1 161.96(4) . . ?
O1 Fe1 Br1 89.90(4) 5_556 . ?
C2 C1 C6 120.0 . . ?
C2 C1 H1 120.0 . . ?
C6 C1 H1 120.0 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C1' C6 C5 108.5 . . ?
C1' C6 C1 34.5 . . ?
C5 C6 C1 120.0 . . ?
C1' C6 C5' 118.1 . . ?
C5 C6 C5' 33.1 . . ?
C1 C6 C5' 108.5 . . ?
C1' C6 C7 125.16(13) . . ?
C5 C6 C7 118.95(12) . . ?
C1 C6 C7 120.63(13) . . ?
C5' C6 C7 116.60(13) . . ?
C6 C1' C2' 122.0 . . ?
C6 C1' H1' 119.0 . . ?
C2' C1' H1' 119.0 . . ?
C1' C2' C3' 120.0 . . ?
C1' C2' H2' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C5' C4' C3' 120.0 . . ?
C5' C4' H4' 120.0 . . ?
C3' C4' H4' 120.0 . . ?
C4' C5' C6 119.8 . . ?
C4' C5' H5' 120.1 . . ?
C6 C5' H5' 120.1 . . ?
O2 C7 N1 118.44(17) . . ?
O2 C7 C6 121.62(16) . . ?
N1 C7 C6 119.87(17) . . ?
C7 N1 O1 116.63(16) . . ?
C7 N1 H6 129.3(16) . . ?
O1 N1 H6 114.1(16) . . ?
N1 O1 Fe1 108.58(11) . . ?
N1 O1 Fe1 114.61(11) . 5_556 ?
Fe1 O1 Fe1 104.16(6) . 5_556 ?
C7 O2 Fe1 115.10(12) . . ?
C17 N11 O11 118.55(16) . . ?
C17 N11 H16 129.3(16) . . ?
O11 N11 H16 111.8(16) . . ?
N11 O11 Fe1 111.13(10) . . ?
C17 O12 Fe1 113.36(12) . . ?
C16 C11 C12 120.1(2) . . ?
C16 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 119.7(2) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 120.8(3) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 120.0(2) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C11 118.8(2) . . ?
C15 C16 C17 118.52(19) . . ?
C11 C16 C17 122.6(2) . . ?
O12 C17 N11 117.14(17) . . ?
O12 C17 C16 121.68(18) . . ?
N11 C17 C16 121.10(17) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.089

# Attachment 'pt0512 - [Fe(bha)3]1.5MeOH.cif'

data_pt0512
_database_code_depnum_ccdc_archive 'CCDC 689506'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_compound_source        'Iria Rio'
_exptl_crystal_recrystallization_method 'Slow evaporation of Et2O/MeOH solution'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C21 H18 Fe N3 O6), 3(C H4 O)'
_chemical_formula_sum            'C45 H48 Fe2 N6 O15'
_chemical_formula_weight         1024.59

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 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.2477(8)
_cell_length_b                   11.3483(4)
_cell_length_c                   22.4035(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.874(2)
_cell_angle_gamma                90.00
_cell_volume                     4631.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5970
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.73

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2128
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7396
_exptl_absorpt_correction_T_max  0.9100
_exptl_absorpt_process_details   'SADABS 2004/1'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            62259
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.04
_reflns_number_total             10126
_reflns_number_gt                8129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART32'
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'Shelxs Sheldrick'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

>>> The Following ALERTS were generated <<<
#------------------------------------------
Format: alert-number_ALERT_alert-type_alert-level text

220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.62 Ratio

The shape and size of this ellipsoid is consistent with thermal motion in
the benzene rings.

910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1
911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 2
912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 32

One of the low angle relfections was affected by the beamstop and thus was
removed.

The data collection strategy used was to collect fully complete data to
2TH= 53deg. Some higher angle data were collected in the process and these
have been included in the refinement. Please refer to the completeness
statistics below

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 1.000 4851 4849 2
23.01 0.550 1.000 6461 6459 2
25.24 0.600 1.000 8396 8393 3
#----------------------------------------------------------- ACTA Min. Res. ---
27.04 0.640 0.997 10161 10126 35

794_ALERT_5_G Check Predicted Bond Valency for Fe1 (3) 3.00
794_ALERT_5_G Check Predicted Bond Valency for Fe2 (3) 3.03
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 9

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+1.4434P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10126
_refine_ls_number_parameters     643
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.521946(15) 0.67732(2) 0.662166(13) 0.01884(8) Uani 1 1 d . . .
Fe2 Fe 0.128316(14) 0.19414(2) 0.113601(13) 0.01890(8) Uani 1 1 d . . .
C1A C 0.29426(11) 0.74048(18) 0.55212(11) 0.0301(5) Uani 1 1 d . . .
C2A C 0.24371(12) 0.7744(2) 0.57605(13) 0.0397(6) Uani 1 1 d . . .
H2A H 0.2602 0.8055 0.6196 0.048 Uiso 1 1 calc R . .
C3A C 0.16925(14) 0.7620(2) 0.53537(16) 0.0514(7) Uani 1 1 d . . .
H3A H 0.1346 0.7851 0.5512 0.062 Uiso 1 1 calc R . .
C4A C 0.14493(14) 0.7164(2) 0.47222(15) 0.0522(8) Uani 1 1 d . . .
H4A H 0.0938 0.7082 0.4449 0.063 Uiso 1 1 calc R . .
C5A C 0.19478(14) 0.6828(2) 0.44866(14) 0.0475(7) Uani 1 1 d . . .
H5A H 0.1778 0.6519 0.4050 0.057 Uiso 1 1 calc R . .
C6A C 0.26942(13) 0.69396(19) 0.48848(12) 0.0367(6) Uani 1 1 d . . .
H6A H 0.3036 0.6699 0.4724 0.044 Uiso 1 1 calc R . .
C10A C 0.37450(11) 0.74518(17) 0.59516(10) 0.0249(4) Uani 1 1 d . . .
O12A O 0.41898(8) 0.67826(12) 0.58484(7) 0.0266(3) Uani 1 1 d . . .
N11A N 0.40053(9) 0.81622(14) 0.64633(9) 0.0248(4) Uani 1 1 d D . .
H11A H 0.3766(12) 0.8747(18) 0.6527(12) 0.037 Uiso 1 1 d D . .
O11A O 0.47470(7) 0.81057(11) 0.68723(7) 0.0228(3) Uani 1 1 d . . .
C1B C 0.68109(11) 0.87747(17) 0.63368(10) 0.0225(4) Uani 1 1 d . . .
C2B C 0.75024(12) 0.92201(18) 0.67498(11) 0.0298(5) Uani 1 1 d . . .
H2B H 0.7710 0.9076 0.7214 0.036 Uiso 1 1 calc R . .
C3B C 0.78845(13) 0.9872(2) 0.64830(12) 0.0352(5) Uani 1 1 d . . .
H3B H 0.8358 1.0168 0.6764 0.042 Uiso 1 1 calc R . .
C4B C 0.75809(13) 1.0097(2) 0.58063(13) 0.0370(5) Uani 1 1 d . . .
H4B H 0.7843 1.0557 0.5627 0.044 Uiso 1 1 calc R . .
C5B C 0.68983(13) 0.9653(2) 0.53946(12) 0.0349(5) Uani 1 1 d . . .
H5B H 0.6690 0.9809 0.4932 0.042 Uiso 1 1 calc R . .
C6B C 0.65178(12) 0.89807(19) 0.56564(10) 0.0279(5) Uani 1 1 d . . .
H6B H 0.6054 0.8657 0.5370 0.033 Uiso 1 1 calc R . .
C10B C 0.63657(11) 0.80632(16) 0.65800(10) 0.0208(4) Uani 1 1 d . . .
O12B O 0.57463(7) 0.76489(12) 0.61767(6) 0.0224(3) Uani 1 1 d . . .
N11B N 0.66042(9) 0.78270(15) 0.72124(8) 0.0236(4) Uani 1 1 d D . .
H11B H 0.6998(10) 0.8093(19) 0.7517(10) 0.028 Uiso 1 1 d D . .
O11B O 0.61665(7) 0.71304(12) 0.73933(7) 0.0244(3) Uani 1 1 d . . .
C1C C 0.52176(10) 0.30762(16) 0.62989(10) 0.0211(4) Uani 1 1 d . . .
C2C C 0.49427(11) 0.21406(18) 0.65261(10) 0.0262(4) Uani 1 1 d . . .
H2C H 0.4753 0.2276 0.6840 0.031 Uiso 1 1 calc R . .
C3C C 0.49482(12) 0.10097(18) 0.62912(10) 0.0292(5) Uani 1 1 d . . .
H3C H 0.4766 0.0370 0.6449 0.035 Uiso 1 1 calc R . .
C4C C 0.52180(12) 0.08102(18) 0.58293(11) 0.0295(5) Uani 1 1 d . . .
H4C H 0.5228 0.0033 0.5676 0.035 Uiso 1 1 calc R . .
C5C C 0.54729(12) 0.17454(18) 0.55910(11) 0.0294(5) Uani 1 1 d . . .
H5C H 0.5650 0.1610 0.5268 0.035 Uiso 1 1 calc R . .
C6C C 0.54714(11) 0.28776(18) 0.58224(10) 0.0247(4) Uani 1 1 d . . .
H6C H 0.5644 0.3517 0.5655 0.030 Uiso 1 1 calc R . .
C10C C 0.52269(10) 0.42984(17) 0.65394(9) 0.0200(4) Uani 1 1 d . . .
O12C O 0.53594(7) 0.51777(11) 0.62545(7) 0.0221(3) Uani 1 1 d . . .
N11C N 0.50755(9) 0.44869(13) 0.70455(8) 0.0201(3) Uani 1 1 d D . .
H11C H 0.5052(11) 0.3963(17) 0.7325(9) 0.024 Uiso 1 1 d D . .
O11C O 0.50487(7) 0.56412(11) 0.72251(7) 0.0227(3) Uani 1 1 d . . .
C1D C 0.26508(10) 0.12477(16) 0.01991(10) 0.0210(4) Uani 1 1 d . . .
C2D C 0.33705(11) 0.08656(18) 0.04224(10) 0.0266(4) Uani 1 1 d . . .
H2D H 0.3661 0.0721 0.0881 0.032 Uiso 1 1 calc R . .
C3D C 0.36646(11) 0.06958(18) -0.00235(11) 0.0274(5) Uani 1 1 d . . .
H3D H 0.4159 0.0439 0.0131 0.033 Uiso 1 1 calc R . .
C4D C 0.32465(12) 0.08966(18) -0.06928(11) 0.0274(5) Uani 1 1 d . . .
H4D H 0.3452 0.0778 -0.0997 0.033 Uiso 1 1 calc R . .
C5D C 0.25241(12) 0.1273(2) -0.09186(11) 0.0315(5) Uani 1 1 d . . .
H5D H 0.2232 0.1403 -0.1379 0.038 Uiso 1 1 calc R . .
C6D C 0.22326(12) 0.14563(19) -0.04740(10) 0.0284(5) Uani 1 1 d . . .
H6D H 0.1742 0.1728 -0.0629 0.034 Uiso 1 1 calc R . .
C10D C 0.23010(10) 0.14282(17) 0.06487(10) 0.0210(4) Uani 1 1 d . . .
O12D O 0.17250(7) 0.20726(12) 0.04843(7) 0.0221(3) Uani 1 1 d . . .
N11D N 0.25753(9) 0.09240(15) 0.12303(8) 0.0226(4) Uani 1 1 d D . .
H11D H 0.2929(11) 0.0398(18) 0.1385(11) 0.034 Uiso 1 1 d D . .
O11D O 0.22327(7) 0.11125(12) 0.16327(7) 0.0233(3) Uani 1 1 d . . .
C1E C 0.00672(10) -0.04841(17) 0.16955(10) 0.0227(4) Uani 1 1 d . . .
C2E C -0.02528(12) -0.15610(18) 0.14316(10) 0.0278(5) Uani 1 1 d . . .
H2E H -0.0271 -0.1823 0.1022 0.033 Uiso 1 1 calc R . .
C3E C -0.05456(12) -0.2253(2) 0.17671(11) 0.0333(5) Uani 1 1 d . . .
H3E H -0.0770 -0.2984 0.1582 0.040 Uiso 1 1 calc R . .
C4E C -0.05153(14) -0.1890(2) 0.23663(12) 0.0369(5) Uani 1 1 d . . .
H4E H -0.0720 -0.2365 0.2593 0.044 Uiso 1 1 calc R . .
C5E C -0.01861(15) -0.0835(2) 0.26310(13) 0.0455(6) Uani 1 1 d . . .
H5E H -0.0157 -0.0587 0.3047 0.055 Uiso 1 1 calc R . .
C6E C 0.01035(13) -0.0131(2) 0.23009(12) 0.0363(5) Uani 1 1 d . . .
H6E H 0.0328 0.0598 0.2490 0.044 Uiso 1 1 calc R . .
C10E C 0.04030(10) 0.02811(17) 0.13721(10) 0.0221(4) Uani 1 1 d . . .
O12E O 0.08679(7) 0.10758(12) 0.16944(6) 0.0239(3) Uani 1 1 d . . .
N11E N 0.02335(10) 0.01466(16) 0.07431(8) 0.0252(4) Uani 1 1 d D . .
H11E H -0.0069(11) -0.0336(18) 0.0473(10) 0.030 Uiso 1 1 d D . .
O11E O 0.05874(8) 0.08367(13) 0.04716(7) 0.0271(3) Uani 1 1 d . . .
C1F C 0.17131(11) 0.52796(17) 0.20887(10) 0.0239(4) Uani 1 1 d . . .
C2F C 0.13080(13) 0.6310(2) 0.20090(12) 0.0393(6) Uani 1 1 d . . .
H2F H 0.0825 0.6367 0.1661 0.047 Uiso 1 1 calc R . .
C3F C 0.16101(14) 0.7250(2) 0.24367(13) 0.0439(6) Uani 1 1 d . . .
H3F H 0.1330 0.7946 0.2387 0.053 Uiso 1 1 calc R . .
C4F C 0.23139(13) 0.7181(2) 0.29335(11) 0.0344(5) Uani 1 1 d . . .
H4F H 0.2520 0.7829 0.3224 0.041 Uiso 1 1 calc R . .
C5F C 0.27193(12) 0.61670(19) 0.30086(11) 0.0323(5) Uani 1 1 d . . .
H5F H 0.3207 0.6121 0.3350 0.039 Uiso 1 1 calc R . .
C6F C 0.24199(11) 0.52190(18) 0.25901(10) 0.0269(4) Uani 1 1 d . . .
H6F H 0.2701 0.4522 0.2647 0.032 Uiso 1 1 calc R . .
C10F C 0.14139(11) 0.42306(17) 0.16648(10) 0.0222(4) Uani 1 1 d . . .
O12F O 0.17282(7) 0.32282(11) 0.18374(7) 0.0231(3) Uani 1 1 d . . .
N11F N 0.08273(9) 0.43036(15) 0.10985(8) 0.0247(4) Uani 1 1 d D . .
H11F H 0.0566(11) 0.4936(17) 0.0911(11) 0.030 Uiso 1 1 d D . .
O11F O 0.05785(7) 0.32720(12) 0.07428(7) 0.0247(3) Uani 1 1 d . . .
O2S O 0.34060(9) 1.01569(13) 0.67073(8) 0.0358(4) Uani 1 1 d D . .
H2S H 0.3623(14) 1.062(2) 0.7011(11) 0.054 Uiso 1 1 d D . .
C2S C 0.29125(13) 1.0868(2) 0.61864(12) 0.0382(6) Uani 1 1 d . . .
H21 H 0.2644 1.1382 0.6355 0.057 Uiso 1 1 calc R . .
H22 H 0.2565 1.0364 0.5834 0.057 Uiso 1 1 calc R . .
H23 H 0.3187 1.1350 0.6008 0.057 Uiso 1 1 calc R . .
O3S O 0.35994(8) 0.56574(15) 0.69593(8) 0.0367(4) Uani 1 1 d D . .
H3S H 0.4054(10) 0.570(3) 0.7112(13) 0.055 Uiso 1 1 d D . .
C3S C 0.33069(13) 0.6280(2) 0.73397(12) 0.0365(5) Uani 1 1 d . . .
H31 H 0.3516 0.5963 0.7792 0.055 Uiso 1 1 calc R . .
H32 H 0.2772 0.6188 0.7136 0.055 Uiso 1 1 calc R . .
H33 H 0.3431 0.7117 0.7354 0.055 Uiso 1 1 calc R . .
O1S O -0.02051(8) 0.60432(14) 0.05122(7) 0.0321(4) Uani 1 1 d D . .
H1S H -0.0263(15) 0.634(2) 0.0158(10) 0.048 Uiso 1 1 d D . .
C1S C -0.08791(14) 0.5539(2) 0.04437(13) 0.0418(6) Uani 1 1 d . . .
H11 H -0.1046 0.4954 0.0086 0.063 Uiso 1 1 calc R . .
H12 H -0.1250 0.6160 0.0337 0.063 Uiso 1 1 calc R . .
H13 H -0.0805 0.5156 0.0861 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.02124(15) 0.01497(14) 0.02062(15) -0.00031(10) 0.00942(12) -0.00063(10)
Fe2 0.01871(15) 0.01967(15) 0.01757(15) -0.00219(10) 0.00721(11) -0.00143(10)
C1A 0.0252(11) 0.0192(10) 0.0387(13) 0.0017(9) 0.0071(9) 0.0014(8)
C2A 0.0294(12) 0.0334(13) 0.0496(15) 0.0019(11) 0.0110(11) -0.0004(10)
C3A 0.0278(13) 0.0435(15) 0.078(2) 0.0063(14) 0.0182(14) 0.0010(11)
C4A 0.0260(13) 0.0386(14) 0.070(2) 0.0027(14) 0.0002(13) -0.0055(11)
C5A 0.0376(14) 0.0314(13) 0.0481(16) -0.0011(11) -0.0048(12) -0.0018(10)
C6A 0.0347(13) 0.0238(11) 0.0401(14) 0.0010(10) 0.0056(11) 0.0027(9)
C10A 0.0261(10) 0.0174(9) 0.0293(11) 0.0031(8) 0.0103(9) 0.0001(8)
O12A 0.0244(8) 0.0244(7) 0.0266(8) -0.0042(6) 0.0072(6) 0.0019(6)
N11A 0.0221(9) 0.0178(8) 0.0324(10) -0.0007(7) 0.0100(8) 0.0021(6)
O11A 0.0216(7) 0.0184(7) 0.0263(7) -0.0028(5) 0.0085(6) 0.0012(5)
C1B 0.0261(10) 0.0179(9) 0.0256(10) -0.0003(8) 0.0134(9) 0.0020(8)
C2B 0.0328(12) 0.0286(11) 0.0299(11) -0.0052(9) 0.0153(10) -0.0073(9)
C3B 0.0328(12) 0.0315(12) 0.0470(14) -0.0079(10) 0.0229(11) -0.0095(9)
C4B 0.0454(14) 0.0270(11) 0.0538(15) 0.0055(11) 0.0359(12) -0.0012(10)
C5B 0.0432(14) 0.0324(12) 0.0369(12) 0.0108(10) 0.0248(11) 0.0048(10)
C6B 0.0282(11) 0.0297(11) 0.0269(11) 0.0032(9) 0.0131(9) 0.0012(9)
C10B 0.0230(10) 0.0172(9) 0.0229(10) -0.0007(8) 0.0107(8) 0.0013(7)
O12B 0.0224(7) 0.0237(7) 0.0198(7) -0.0002(6) 0.0079(6) -0.0031(5)
N11B 0.0222(9) 0.0253(9) 0.0216(9) 0.0015(7) 0.0080(7) -0.0062(7)
O11B 0.0260(7) 0.0253(7) 0.0216(7) 0.0041(6) 0.0101(6) -0.0048(6)
C1C 0.0192(10) 0.0204(10) 0.0202(10) -0.0004(8) 0.0054(8) 0.0005(7)
C2C 0.0317(11) 0.0217(10) 0.0248(11) -0.0014(8) 0.0120(9) -0.0012(8)
C3C 0.0350(12) 0.0185(10) 0.0278(11) 0.0007(8) 0.0080(9) -0.0026(8)
C4C 0.0325(12) 0.0201(10) 0.0281(11) -0.0067(8) 0.0059(9) 0.0025(8)
C5C 0.0304(12) 0.0293(11) 0.0278(11) -0.0077(9) 0.0121(9) 0.0024(9)
C6C 0.0230(10) 0.0237(10) 0.0257(11) -0.0018(8) 0.0090(9) -0.0010(8)
C10C 0.0166(9) 0.0199(9) 0.0216(10) 0.0013(8) 0.0065(8) 0.0000(7)
O12C 0.0277(7) 0.0175(7) 0.0242(7) -0.0004(5) 0.0144(6) -0.0009(5)
N11C 0.0261(9) 0.0125(7) 0.0234(8) -0.0005(6) 0.0121(7) -0.0013(6)
O11C 0.0322(8) 0.0128(6) 0.0280(7) -0.0033(5) 0.0178(6) -0.0019(5)
C1D 0.0242(10) 0.0178(9) 0.0224(10) -0.0013(8) 0.0115(8) -0.0016(7)
C2D 0.0251(11) 0.0294(11) 0.0223(10) -0.0001(8) 0.0077(9) 0.0001(8)
C3D 0.0239(11) 0.0272(11) 0.0318(11) -0.0036(9) 0.0126(9) 0.0000(8)
C4D 0.0347(12) 0.0252(10) 0.0295(11) -0.0028(9) 0.0208(10) -0.0040(9)
C5D 0.0347(12) 0.0389(13) 0.0218(11) 0.0059(9) 0.0131(9) 0.0025(10)
C6D 0.0263(11) 0.0324(11) 0.0269(11) 0.0040(9) 0.0118(9) 0.0036(9)
C10D 0.0219(10) 0.0173(9) 0.0225(10) -0.0028(8) 0.0084(8) -0.0031(8)
O12D 0.0214(7) 0.0235(7) 0.0214(7) 0.0017(6) 0.0095(6) 0.0025(5)
N11D 0.0237(9) 0.0225(8) 0.0235(9) 0.0018(7) 0.0121(7) 0.0051(7)
O11D 0.0239(7) 0.0276(7) 0.0206(7) 0.0030(6) 0.0118(6) 0.0046(6)
C1E 0.0213(10) 0.0240(10) 0.0239(10) -0.0005(8) 0.0109(8) -0.0002(8)
C2E 0.0320(12) 0.0265(11) 0.0208(10) 0.0010(8) 0.0076(9) -0.0007(9)
C3E 0.0360(12) 0.0269(11) 0.0315(12) 0.0049(9) 0.0096(10) -0.0052(9)
C4E 0.0435(14) 0.0356(13) 0.0405(14) 0.0072(10) 0.0266(12) -0.0040(10)
C5E 0.0643(17) 0.0486(15) 0.0404(14) -0.0095(12) 0.0387(14) -0.0137(13)
C6E 0.0485(14) 0.0337(12) 0.0375(13) -0.0119(10) 0.0289(11) -0.0146(10)
C10E 0.0211(10) 0.0234(10) 0.0223(10) -0.0019(8) 0.0100(8) 0.0004(8)
O12E 0.0261(7) 0.0268(7) 0.0200(7) -0.0062(6) 0.0111(6) -0.0076(6)
N11E 0.0294(9) 0.0270(9) 0.0191(8) -0.0037(7) 0.0103(7) -0.0114(7)
O11E 0.0312(8) 0.0312(8) 0.0200(7) -0.0046(6) 0.0123(6) -0.0125(6)
C1F 0.0253(10) 0.0228(10) 0.0237(10) -0.0033(8) 0.0109(8) -0.0020(8)
C2F 0.0328(13) 0.0311(12) 0.0378(13) -0.0107(10) 0.0004(10) 0.0066(10)
C3F 0.0427(14) 0.0267(12) 0.0488(15) -0.0111(11) 0.0073(12) 0.0087(10)
C4F 0.0397(13) 0.0259(11) 0.0319(12) -0.0076(9) 0.0104(10) -0.0058(9)
C5F 0.0286(12) 0.0290(12) 0.0308(12) -0.0024(9) 0.0052(10) -0.0045(9)
C6F 0.0274(11) 0.0218(10) 0.0290(11) 0.0008(8) 0.0100(9) 0.0013(8)
C10F 0.0222(10) 0.0234(10) 0.0228(10) -0.0016(8) 0.0114(8) 0.0010(8)
O12F 0.0223(7) 0.0204(7) 0.0219(7) -0.0028(5) 0.0053(6) 0.0015(5)
N11F 0.0264(9) 0.0210(9) 0.0223(9) -0.0027(7) 0.0067(7) 0.0037(7)
O11F 0.0228(7) 0.0240(7) 0.0225(7) -0.0063(6) 0.0054(6) 0.0010(5)
O2S 0.0351(9) 0.0246(8) 0.0339(9) -0.0056(7) 0.0023(7) 0.0082(7)
C2S 0.0385(13) 0.0374(13) 0.0343(13) 0.0042(10) 0.0118(11) 0.0088(10)
O3S 0.0268(8) 0.0401(9) 0.0463(10) -0.0190(8) 0.0187(8) -0.0098(7)
C3S 0.0322(12) 0.0400(13) 0.0384(13) -0.0117(11) 0.0163(10) -0.0037(10)
O1S 0.0339(9) 0.0325(9) 0.0218(8) 0.0002(6) 0.0045(7) 0.0078(7)
C1S 0.0426(14) 0.0404(14) 0.0372(13) 0.0055(11) 0.0128(11) 0.0034(11)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O11B 1.9841(14) . ?
Fe1 O11A 1.9965(13) . ?
Fe1 O11C 2.0014(13) . ?
Fe1 O12B 2.0117(14) . ?
Fe1 O12A 2.0483(14) . ?
Fe1 O12C 2.0588(13) . ?
Fe2 O11E 1.9853(13) . ?
Fe2 O11D 1.9880(13) . ?
Fe2 O11F 1.9988(14) . ?
Fe2 O12D 2.0235(14) . ?
Fe2 O12E 2.0382(14) . ?
Fe2 O12F 2.0440(13) . ?
C1A C6A 1.392(3) . ?
C1A C2A 1.401(3) . ?
C1A C10A 1.485(3) . ?
C2A C3A 1.387(3) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.379(4) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.381(4) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.385(3) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C10A O12A 1.274(2) . ?
C10A N11A 1.309(3) . ?
N11A O11A 1.378(2) . ?
N11A H11A 0.869(16) . ?
C1B C6B 1.393(3) . ?
C1B C2B 1.393(3) . ?
C1B C10B 1.480(3) . ?
C2B C3B 1.381(3) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.388(3) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.379(3) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.384(3) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C10B O12B 1.273(2) . ?
C10B N11B 1.310(3) . ?
N11B O11B 1.374(2) . ?
N11B H11B 0.847(16) . ?
C1C C6C 1.391(3) . ?
C1C C2C 1.394(3) . ?
C1C C10C 1.485(3) . ?
C2C C3C 1.389(3) . ?
C2C H2C 0.9500 . ?
C3C C4C 1.383(3) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.385(3) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.386(3) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
C10C O12C 1.275(2) . ?
C10C N11C 1.315(2) . ?
N11C O11C 1.3783(19) . ?
N11C H11C 0.879(15) . ?
C1D C2D 1.388(3) . ?
C1D C6D 1.390(3) . ?
C1D C10D 1.477(3) . ?
C2D C3D 1.382(3) . ?
C2D H2D 0.9500 . ?
C3D C4D 1.382(3) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.390(3) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.377(3) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
C10D O12D 1.287(2) . ?
C10D N11D 1.305(3) . ?
N11D O11D 1.373(2) . ?
N11D H11D 0.879(16) . ?
C1E C6E 1.385(3) . ?
C1E C2E 1.389(3) . ?
C1E C10E 1.474(3) . ?
C2E C3E 1.386(3) . ?
C2E H2E 0.9500 . ?
C3E C4E 1.380(3) . ?
C3E H3E 0.9500 . ?
C4E C5E 1.372(3) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.382(3) . ?
C5E H5E 0.9500 . ?
C6E H6E 0.9500 . ?
C10E O12E 1.276(2) . ?
C10E N11E 1.306(3) . ?
N11E O11E 1.370(2) . ?
N11E H11E 0.847(16) . ?
C1F C6F 1.383(3) . ?
C1F C2F 1.394(3) . ?
C1F C10F 1.478(3) . ?
C2F C3F 1.385(3) . ?
C2F H2F 0.9500 . ?
C3F C4F 1.375(3) . ?
C3F H3F 0.9500 . ?
C4F C5F 1.380(3) . ?
C4F H4F 0.9500 . ?
C5F C6F 1.381(3) . ?
C5F H5F 0.9500 . ?
C6F H6F 0.9500 . ?
C10F O12F 1.278(2) . ?
C10F N11F 1.309(3) . ?
N11F O11F 1.382(2) . ?
N11F H11F 0.882(16) . ?
O2S C2S 1.412(3) . ?
O2S H2S 0.818(17) . ?
C2S H21 0.9800 . ?
C2S H22 0.9800 . ?
C2S H23 0.9800 . ?
O3S C3S 1.420(3) . ?
O3S H3S 0.831(17) . ?
C3S H31 0.9800 . ?
C3S H32 0.9800 . ?
C3S H33 0.9800 . ?
O1S C1S 1.425(3) . ?
O1S H1S 0.819(17) . ?
C1S H11 0.9800 . ?
C1S H12 0.9800 . ?
C1S H13 0.9800 . ?

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
O11B Fe1 O11A 89.98(6) . . ?
O11B Fe1 O11C 85.92(6) . . ?
O11A Fe1 O11C 92.92(6) . . ?
O11B Fe1 O12B 79.10(5) . . ?
O11A Fe1 O12B 100.83(6) . . ?
O11C Fe1 O12B 159.56(6) . . ?
O11B Fe1 O12A 167.38(6) . . ?
O11A Fe1 O12A 78.36(5) . . ?
O11C Fe1 O12A 99.35(6) . . ?
O12B Fe1 O12A 98.19(6) . . ?
O11B Fe1 O12C 106.18(6) . . ?
O11A Fe1 O12C 160.89(5) . . ?
O11C Fe1 O12C 78.46(5) . . ?
O12B Fe1 O12C 92.36(5) . . ?
O12A Fe1 O12C 86.18(5) . . ?
O11E Fe2 O11D 108.51(6) . . ?
O11E Fe2 O11F 90.58(6) . . ?
O11D Fe2 O11F 159.09(6) . . ?
O11E Fe2 O12D 84.14(6) . . ?
O11D Fe2 O12D 79.32(5) . . ?
O11F Fe2 O12D 94.69(6) . . ?
O11E Fe2 O12E 78.94(5) . . ?
O11D Fe2 O12E 89.17(6) . . ?
O11F Fe2 O12E 103.19(6) . . ?
O12D Fe2 O12E 155.37(6) . . ?
O11E Fe2 O12F 163.34(6) . . ?
O11D Fe2 O12F 85.04(5) . . ?
O11F Fe2 O12F 77.85(5) . . ?
O12D Fe2 O12F 108.47(6) . . ?
O12E Fe2 O12F 91.95(5) . . ?
C6A C1A C2A 119.9(2) . . ?
C6A C1A C10A 118.9(2) . . ?
C2A C1A C10A 121.1(2) . . ?
C3A C2A C1A 119.1(3) . . ?
C3A C2A H2A 120.4 . . ?
C1A C2A H2A 120.4 . . ?
C4A C3A C2A 120.7(3) . . ?
C4A C3A H3A 119.6 . . ?
C2A C3A H3A 119.6 . . ?
C3A C4A C5A 120.1(2) . . ?
C3A C4A H4A 119.9 . . ?
C5A C4A H4A 119.9 . . ?
C4A C5A C6A 120.2(3) . . ?
C4A C5A H5A 119.9 . . ?
C6A C5A H5A 119.9 . . ?
C5A C6A C1A 120.0(3) . . ?
C5A C6A H6A 120.0 . . ?
C1A C6A H6A 120.0 . . ?
O12A C10A N11A 118.66(18) . . ?
O12A C10A C1A 121.37(18) . . ?
N11A C10A C1A 119.93(19) . . ?
C10A O12A Fe1 112.89(13) . . ?
C10A N11A O11A 117.33(16) . . ?
C10A N11A H11A 125.0(16) . . ?
O11A N11A H11A 116.8(16) . . ?
N11A O11A Fe1 111.42(10) . . ?
C6B C1B C2B 119.39(19) . . ?
C6B C1B C10B 117.21(18) . . ?
C2B C1B C10B 123.39(18) . . ?
C3B C2B C1B 119.8(2) . . ?
C3B C2B H2B 120.1 . . ?
C1B C2B H2B 120.1 . . ?
C2B C3B C4B 120.4(2) . . ?
C2B C3B H3B 119.8 . . ?
C4B C3B H3B 119.8 . . ?
C5B C4B C3B 120.0(2) . . ?
C5B C4B H4B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C4B C5B C6B 119.9(2) . . ?
C4B C5B H5B 120.0 . . ?
C6B C5B H5B 120.0 . . ?
C5B C6B C1B 120.4(2) . . ?
C5B C6B H6B 119.8 . . ?
C1B C6B H6B 119.8 . . ?
O12B C10B N11B 118.41(18) . . ?
O12B C10B C1B 120.66(17) . . ?
N11B C10B C1B 120.92(18) . . ?
C10B O12B Fe1 113.70(12) . . ?
C10B N11B O11B 117.14(16) . . ?
C10B N11B H11B 124.9(16) . . ?
O11B N11B H11B 117.9(16) . . ?
N11B O11B Fe1 111.29(11) . . ?
C6C C1C C2C 119.81(18) . . ?
C6C C1C C10C 118.65(18) . . ?
C2C C1C C10C 121.52(18) . . ?
C3C C2C C1C 119.7(2) . . ?
C3C C2C H2C 120.2 . . ?
C1C C2C H2C 120.2 . . ?
C4C C3C C2C 120.4(2) . . ?
C4C C3C H3C 119.8 . . ?
C2C C3C H3C 119.8 . . ?
C3C C4C C5C 119.88(19) . . ?
C3C C4C H4C 120.1 . . ?
C5C C4C H4C 120.1 . . ?
C4C C5C C6C 120.3(2) . . ?
C4C C5C H5C 119.9 . . ?
C6C C5C H5C 119.9 . . ?
C5C C6C C1C 119.9(2) . . ?
C5C C6C H6C 120.0 . . ?
C1C C6C H6C 120.0 . . ?
O12C C10C N11C 118.93(17) . . ?
O12C C10C C1C 121.44(17) . . ?
N11C C10C C1C 119.60(17) . . ?
C10C O12C Fe1 113.12(12) . . ?
C10C N11C O11C 117.39(15) . . ?
C10C N11C H11C 127.5(15) . . ?
O11C N11C H11C 114.4(15) . . ?
N11C O11C Fe1 111.86(11) . . ?
C2D C1D C6D 119.41(19) . . ?
C2D C1D C10D 122.56(18) . . ?
C6D C1D C10D 118.03(18) . . ?
C3D C2D C1D 119.93(19) . . ?
C3D C2D H2D 120.0 . . ?
C1D C2D H2D 120.0 . . ?
C2D C3D C4D 120.6(2) . . ?
C2D C3D H3D 119.7 . . ?
C4D C3D H3D 119.7 . . ?
C3D C4D C5D 119.6(2) . . ?
C3D C4D H4D 120.2 . . ?
C5D C4D H4D 120.2 . . ?
C6D C5D C4D 119.9(2) . . ?
C6D C5D H5D 120.1 . . ?
C4D C5D H5D 120.1 . . ?
C5D C6D C1D 120.6(2) . . ?
C5D C6D H6D 119.7 . . ?
C1D C6D H6D 119.7 . . ?
O12D C10D N11D 118.21(18) . . ?
O12D C10D C1D 121.88(17) . . ?
N11D C10D C1D 119.91(17) . . ?
C10D O12D Fe2 112.49(12) . . ?
C10D N11D O11D 118.08(16) . . ?
C10D N11D H11D 127.6(16) . . ?
O11D N11D H11D 113.9(16) . . ?
N11D O11D Fe2 110.39(10) . . ?
C6E C1E C2E 119.16(19) . . ?
C6E C1E C10E 118.17(18) . . ?
C2E C1E C10E 122.61(18) . . ?
C3E C2E C1E 119.9(2) . . ?
C3E C2E H2E 120.1 . . ?
C1E C2E H2E 120.1 . . ?
C4E C3E C2E 120.7(2) . . ?
C4E C3E H3E 119.6 . . ?
C2E C3E H3E 119.6 . . ?
C5E C4E C3E 119.2(2) . . ?
C5E C4E H4E 120.4 . . ?
C3E C4E H4E 120.4 . . ?
C4E C5E C6E 120.9(2) . . ?
C4E C5E H5E 119.6 . . ?
C6E C5E H5E 119.6 . . ?
C5E C6E C1E 120.2(2) . . ?
C5E C6E H6E 119.9 . . ?
C1E C6E H6E 119.9 . . ?
O12E C10E N11E 118.36(18) . . ?
O12E C10E C1E 121.55(17) . . ?
N11E C10E C1E 120.09(18) . . ?
C10E O12E Fe2 113.17(12) . . ?
C10E N11E O11E 118.05(16) . . ?
C10E N11E H11E 127.8(16) . . ?
O11E N11E H11E 114.1(16) . . ?
N11E O11E Fe2 111.44(11) . . ?
C6F C1F C2F 119.22(19) . . ?
C6F C1F C10F 118.08(18) . . ?
C2F C1F C10F 122.69(19) . . ?
C3F C2F C1F 120.0(2) . . ?
C3F C2F H2F 120.0 . . ?
C1F C2F H2F 120.0 . . ?
C4F C3F C2F 120.3(2) . . ?
C4F C3F H3F 119.8 . . ?
C2F C3F H3F 119.8 . . ?
C3F C4F C5F 119.8(2) . . ?
C3F C4F H4F 120.1 . . ?
C5F C4F H4F 120.1 . . ?
C4F C5F C6F 120.3(2) . . ?
C4F C5F H5F 119.8 . . ?
C6F C5F H5F 119.8 . . ?
C5F C6F C1F 120.32(19) . . ?
C5F C6F H6F 119.8 . . ?
C1F C6F H6F 119.8 . . ?
O12F C10F N11F 118.10(18) . . ?
O12F C10F C1F 120.81(17) . . ?
N11F C10F C1F 121.08(18) . . ?
C10F O12F Fe2 114.14(12) . . ?
C10F N11F O11F 116.99(16) . . ?
C10F N11F H11F 127.9(15) . . ?
O11F N11F H11F 115.1(15) . . ?
N11F O11F Fe2 112.05(11) . . ?
C2S O2S H2S 105(2) . . ?
O2S C2S H21 109.5 . . ?
O2S C2S H22 109.5 . . ?
H21 C2S H22 109.5 . . ?
O2S C2S H23 109.5 . . ?
H21 C2S H23 109.5 . . ?
H22 C2S H23 109.5 . . ?
C3S O3S H3S 114(2) . . ?
O3S C3S H31 109.5 . . ?
O3S C3S H32 109.5 . . ?
H31 C3S H32 109.5 . . ?
O3S C3S H33 109.5 . . ?
H31 C3S H33 109.5 . . ?
H32 C3S H33 109.5 . . ?
C1S O1S H1S 109(2) . . ?
O1S C1S H11 109.5 . . ?
O1S C1S H12 109.5 . . ?
H11 C1S H12 109.5 . . ?
O1S C1S H13 109.5 . . ?
H11 C1S H13 109.5 . . ?
H12 C1S H13 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.065