# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Guillem Aromi'
_publ_contact_author_email       GUILLEM.AROMI@QI.UB.ES

_publ_section_title              
;
Synthesis of a novel hepta-coordinated Fe(III) dinuclear complex:
Experimental and theoretical study of the magnetic properties
;
loop_
_publ_author_name
'Guillem Aromi'
'Leoni A Barrios'
'Jose Sanchez Costa'
'Gavin A. Craig'
'Olivier Roubeau'
'Eliseo Ruiz'
;
S.J.Teat
;
'Lynne H. Thomas'
'Chick C. Wilson'

data_lms13b
_database_code_depnum_ccdc_archive 'CCDC 756458'
#TrackingRef 'web_deposit_cif_file_0_OlivierRoubeau_1259610432.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H17 N5 O2'
_chemical_formula_sum            'C23 H17 N5 O2'
_chemical_formula_weight         395.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   13.173(2)
_cell_length_b                   13.384(2)
_cell_length_c                   11.211(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.931(2)
_cell_angle_gamma                90.00
_cell_volume                     1846.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5686
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      34.49

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI US'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            18451
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         32.55
_reflns_number_total             5151
_reflns_number_gt                4037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.36a'
_computing_data_reduction        'Bruker SAINT v7.36a'
_computing_structure_solution    'SIR97 (Altomare 1999)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_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. All non hydrogens were
refined anisotropically. ll hydrogens were found in difference Fourier
maps. Those on the pyrazole and phenol N2, N4, O1 and O2 atoms were
refined freely with their thermal parameter 1.5 times that of their
carrier atom. The rest of the hydrogens were placed geometrically
on their carrier atom and refined with a riding model.
;

_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^)+(0.0835P)^2^+0.1516P] 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         5151
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1498
_refine_ls_wR_factor_gt          0.1390
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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
O1 O -0.13214(8) 0.57288(8) -0.15377(9) 0.0278(2) Uani 1 1 d . . .
H1B H -0.0820(17) 0.5664(16) -0.0692(19) 0.042 Uiso 1 1 d . . .
O2 O 0.62034(8) 0.40216(8) 0.64550(9) 0.0252(2) Uani 1 1 d . . .
H2B H 0.5531(16) 0.4320(15) 0.6057(18) 0.038 Uiso 1 1 d . . .
N1 N 0.12296(9) 0.58299(8) 0.47923(10) 0.0192(2) Uani 1 1 d . . .
N2 N 0.01646(9) 0.58347(9) 0.22076(10) 0.0221(2) Uani 1 1 d . . .
H2 H 0.0812(16) 0.5499(14) 0.2457(17) 0.033 Uiso 1 1 d . . .
N3 N -0.04879(9) 0.58448(9) 0.09677(10) 0.0224(2) Uani 1 1 d . . .
N4 N 0.33297(9) 0.52145(9) 0.55959(11) 0.0226(2) Uani 1 1 d . . .
H4 H 0.3112(15) 0.5494(15) 0.4753(18) 0.034 Uiso 1 1 d . . .
N5 N 0.43216(9) 0.48031(9) 0.60993(10) 0.0230(2) Uani 1 1 d . . .
C1 C -0.22295(11) 0.61616(10) -0.14477(12) 0.0214(3) Uani 1 1 d . . .
C2 C -0.30989(12) 0.63227(10) -0.25892(13) 0.0245(3) Uani 1 1 d . . .
H2A H -0.3038 0.6131 -0.3377 0.029 Uiso 1 1 calc R . .
C3 C -0.40482(12) 0.67599(10) -0.25807(13) 0.0252(3) Uani 1 1 d . . .
H3A H -0.4638 0.6865 -0.3361 0.030 Uiso 1 1 calc R . .
C4 C -0.41390(11) 0.70454(11) -0.14295(13) 0.0255(3) Uani 1 1 d . . .
H4A H -0.4791 0.7344 -0.1420 0.031 Uiso 1 1 calc R . .
C5 C -0.32736(11) 0.68923(10) -0.02963(12) 0.0233(3) Uani 1 1 d . . .
H5A H -0.3340 0.7093 0.0485 0.028 Uiso 1 1 calc R . .
C6 C -0.23047(11) 0.64503(9) -0.02731(12) 0.0193(2) Uani 1 1 d . . .
C7 C -0.14034(10) 0.62991(10) 0.09427(12) 0.0194(3) Uani 1 1 d . . .
C8 C -0.13300(10) 0.65699(10) 0.21915(12) 0.0191(2) Uani 1 1 d . . .
H8A H -0.1863 0.6901 0.2436 0.023 Uiso 1 1 calc R . .
C9 C -0.03125(11) 0.62469(10) 0.29783(12) 0.0202(3) Uani 1 1 d . . .
C10 C 0.02256(10) 0.62185(9) 0.43689(12) 0.0193(3) Uani 1 1 d . . .
C11 C -0.03062(11) 0.65272(10) 0.51858(13) 0.0226(3) Uani 1 1 d . . .
H11A H -0.1012 0.6814 0.4854 0.027 Uiso 1 1 calc R . .
C12 C 0.02198(11) 0.64054(10) 0.64893(13) 0.0233(3) Uani 1 1 d . . .
H12A H -0.0121 0.6608 0.7067 0.028 Uiso 1 1 calc R . .
C13 C 0.12529(11) 0.59829(10) 0.69427(12) 0.0216(3) Uani 1 1 d . . .
H13A H 0.1625 0.5880 0.7831 0.026 Uiso 1 1 calc R . .
C14 C 0.17303(10) 0.57134(10) 0.60590(12) 0.0189(3) Uani 1 1 d . . .
C15 C 0.28205(10) 0.52749(10) 0.64507(12) 0.0195(3) Uani 1 1 d . . .
C16 C 0.35199(10) 0.48647(10) 0.75763(12) 0.0196(2) Uani 1 1 d . . .
H16A H 0.3400 0.4792 0.8359 0.023 Uiso 1 1 calc R . .
C17 C 0.44497(10) 0.45773(10) 0.73139(11) 0.0192(2) Uani 1 1 d . . .
C18 C 0.54548(10) 0.40947(9) 0.81400(12) 0.0191(3) Uani 1 1 d . . .
C19 C 0.55982(11) 0.38436(10) 0.94044(12) 0.0213(3) Uani 1 1 d . . .
H19A H 0.5050 0.4017 0.9734 0.026 Uiso 1 1 calc R . .
C20 C 0.65208(12) 0.33486(11) 1.01842(13) 0.0252(3) Uani 1 1 d . . .
H20A H 0.6599 0.3179 1.1035 0.030 Uiso 1 1 calc R . .
C21 C 0.73325(12) 0.31013(11) 0.97111(13) 0.0274(3) Uani 1 1 d . . .
H21A H 0.7967 0.2762 1.0242 0.033 Uiso 1 1 calc R . .
C22 C 0.72184(11) 0.33478(11) 0.84697(13) 0.0253(3) Uani 1 1 d . . .
H22A H 0.7778 0.3185 0.8155 0.030 Uiso 1 1 calc R . .
C23 C 0.62843(11) 0.38344(10) 0.76822(12) 0.0208(3) Uani 1 1 d . . .

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
O1 0.0246(5) 0.0396(6) 0.0188(5) 0.0004(4) 0.0071(4) 0.0101(4)
O2 0.0224(5) 0.0353(6) 0.0199(5) 0.0040(4) 0.0100(4) 0.0064(4)
N1 0.0165(5) 0.0227(5) 0.0170(5) 0.0007(4) 0.0044(4) -0.0002(4)
N2 0.0163(5) 0.0309(6) 0.0177(5) 0.0006(4) 0.0045(4) 0.0037(4)
N3 0.0184(5) 0.0304(6) 0.0168(5) 0.0006(4) 0.0043(4) 0.0034(4)
N4 0.0172(5) 0.0334(6) 0.0171(5) 0.0034(4) 0.0061(4) 0.0042(4)
N5 0.0170(5) 0.0326(6) 0.0182(5) 0.0030(4) 0.0051(4) 0.0036(4)
C1 0.0200(6) 0.0227(6) 0.0203(6) 0.0021(5) 0.0058(5) 0.0021(5)
C2 0.0257(7) 0.0263(6) 0.0182(6) 0.0013(5) 0.0037(5) -0.0001(5)
C3 0.0232(7) 0.0260(7) 0.0215(6) 0.0053(5) 0.0022(5) 0.0004(5)
C4 0.0191(6) 0.0287(7) 0.0265(7) 0.0055(5) 0.0053(5) 0.0043(5)
C5 0.0211(6) 0.0276(6) 0.0208(6) 0.0027(5) 0.0068(5) 0.0030(5)
C6 0.0175(6) 0.0211(6) 0.0177(6) 0.0014(5) 0.0044(4) 0.0002(5)
C7 0.0167(6) 0.0224(6) 0.0182(6) 0.0009(5) 0.0051(5) -0.0001(5)
C8 0.0171(6) 0.0216(6) 0.0178(6) 0.0007(4) 0.0054(4) 0.0010(5)
C9 0.0179(6) 0.0224(6) 0.0201(6) 0.0014(5) 0.0065(5) 0.0002(5)
C10 0.0168(6) 0.0209(6) 0.0196(6) 0.0003(5) 0.0058(5) -0.0001(5)
C11 0.0192(6) 0.0255(6) 0.0224(6) -0.0011(5) 0.0063(5) 0.0032(5)
C12 0.0234(6) 0.0261(6) 0.0213(6) -0.0034(5) 0.0091(5) 0.0014(5)
C13 0.0214(6) 0.0255(6) 0.0172(6) -0.0019(5) 0.0059(5) -0.0004(5)
C14 0.0164(6) 0.0216(6) 0.0173(6) -0.0012(4) 0.0044(4) -0.0013(5)
C15 0.0174(6) 0.0238(6) 0.0175(6) -0.0008(5) 0.0065(5) -0.0013(5)
C16 0.0176(6) 0.0241(6) 0.0160(5) -0.0003(5) 0.0048(4) 0.0005(5)
C17 0.0176(6) 0.0226(6) 0.0163(5) -0.0010(5) 0.0048(4) -0.0011(5)
C18 0.0173(6) 0.0215(6) 0.0174(6) -0.0012(4) 0.0047(4) -0.0008(5)
C19 0.0206(6) 0.0243(6) 0.0178(6) -0.0011(5) 0.0055(5) 0.0003(5)
C20 0.0263(7) 0.0274(6) 0.0176(6) 0.0010(5) 0.0027(5) 0.0014(5)
C21 0.0242(7) 0.0282(7) 0.0244(7) -0.0001(5) 0.0020(5) 0.0063(5)
C22 0.0208(6) 0.0289(7) 0.0248(7) -0.0009(5) 0.0064(5) 0.0064(5)
C23 0.0213(6) 0.0215(6) 0.0190(6) -0.0007(5) 0.0065(5) 0.0006(5)

_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
O1 C1 1.3649(16) . ?
O1 H1B 0.95(2) . ?
O2 C23 1.3647(15) . ?
O2 H2B 0.93(2) . ?
N1 C10 1.3403(16) . ?
N1 C14 1.3441(16) . ?
N2 N3 1.3482(15) . ?
N2 C9 1.3542(16) . ?
N2 H2 0.91(2) . ?
N3 C7 1.3419(17) . ?
N4 N5 1.3423(16) . ?
N4 C15 1.3543(15) . ?
N4 H4 0.960(19) . ?
N5 C17 1.3453(16) . ?
C1 C2 1.3960(18) . ?
C1 C6 1.4093(18) . ?
C2 C3 1.384(2) . ?
C2 H2A 0.9500 . ?
C3 C4 1.392(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3860(18) . ?
C4 H4A 0.9500 . ?
C5 C6 1.3985(18) . ?
C5 H5A 0.9500 . ?
C6 C7 1.4671(17) . ?
C7 C8 1.4157(17) . ?
C8 C9 1.3845(18) . ?
C8 H8A 0.9500 . ?
C9 C10 1.4646(18) . ?
C10 C11 1.3995(17) . ?
C11 C12 1.3852(18) . ?
C11 H11A 0.9500 . ?
C12 C13 1.3914(19) . ?
C12 H12A 0.9500 . ?
C13 C14 1.3973(17) . ?
C13 H13A 0.9500 . ?
C14 C15 1.4660(18) . ?
C15 C16 1.3827(18) . ?
C16 C17 1.4114(17) . ?
C16 H16A 0.9500 . ?
C17 C18 1.4670(18) . ?
C18 C19 1.4024(17) . ?
C18 C23 1.4070(17) . ?
C19 C20 1.3861(19) . ?
C19 H19A 0.9500 . ?
C20 C21 1.393(2) . ?
C20 H20A 0.9500 . ?
C21 C22 1.385(2) . ?
C21 H21A 0.9500 . ?
C22 C23 1.3935(19) . ?
C22 H22A 0.9500 . ?

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
C1 O1 H1B 106.3(12) . . ?
C23 O2 H2B 106.3(12) . . ?
C10 N1 C14 117.96(11) . . ?
N3 N2 C9 112.55(11) . . ?
N3 N2 H2 120.1(11) . . ?
C9 N2 H2 126.8(11) . . ?
C7 N3 N2 105.26(11) . . ?
N5 N4 C15 112.38(11) . . ?
N5 N4 H4 118.5(11) . . ?
C15 N4 H4 128.6(11) . . ?
N4 N5 C17 105.60(10) . . ?
O1 C1 C2 116.83(12) . . ?
O1 C1 C6 122.78(12) . . ?
C2 C1 C6 120.38(12) . . ?
C3 C2 C1 120.43(13) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 119.99(13) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C5 C4 C3 119.63(13) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 121.73(12) . . ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 . . ?
C5 C6 C1 117.84(12) . . ?
C5 C6 C7 120.39(11) . . ?
C1 C6 C7 121.77(12) . . ?
N3 C7 C8 110.61(11) . . ?
N3 C7 C6 120.33(11) . . ?
C8 C7 C6 129.06(12) . . ?
C9 C8 C7 104.99(11) . . ?
C9 C8 H8A 127.5 . . ?
C7 C8 H8A 127.5 . . ?
N2 C9 C8 106.56(11) . . ?
N2 C9 C10 120.67(12) . . ?
C8 C9 C10 132.58(12) . . ?
N1 C10 C11 122.96(12) . . ?
N1 C10 C9 115.36(11) . . ?
C11 C10 C9 121.59(12) . . ?
C12 C11 C10 118.49(12) . . ?
C12 C11 H11A 120.8 . . ?
C10 C11 H11A 120.8 . . ?
C11 C12 C13 119.25(12) . . ?
C11 C12 H12A 120.4 . . ?
C13 C12 H12A 120.4 . . ?
C12 C13 C14 118.36(12) . . ?
C12 C13 H13A 120.8 . . ?
C14 C13 H13A 120.8 . . ?
N1 C14 C13 122.95(12) . . ?
N1 C14 C15 114.92(11) . . ?
C13 C14 C15 122.13(11) . . ?
N4 C15 C16 106.57(11) . . ?
N4 C15 C14 119.46(11) . . ?
C16 C15 C14 133.98(11) . . ?
C15 C16 C17 105.24(11) . . ?
C15 C16 H16A 127.4 . . ?
C17 C16 H16A 127.4 . . ?
N5 C17 C16 110.20(11) . . ?
N5 C17 C18 119.77(11) . . ?
C16 C17 C18 130.02(11) . . ?
C19 C18 C23 117.88(12) . . ?
C19 C18 C17 120.60(11) . . ?
C23 C18 C17 121.47(11) . . ?
C20 C19 C18 121.55(12) . . ?
C20 C19 H19A 119.2 . . ?
C18 C19 H19A 119.2 . . ?
C19 C20 C21 119.53(12) . . ?
C19 C20 H20A 120.2 . . ?
C21 C20 H20A 120.2 . . ?
C22 C21 C20 120.24(13) . . ?
C22 C21 H21A 119.9 . . ?
C20 C21 H21A 119.9 . . ?
C21 C22 C23 120.14(13) . . ?
C21 C22 H22A 119.9 . . ?
C23 C22 H22A 119.9 . . ?
O2 C23 C22 117.25(12) . . ?
O2 C23 C18 122.09(12) . . ?
C22 C23 C18 120.65(12) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        32.55
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.061

data_cut
_database_code_depnum_ccdc_archive 'CCDC 756459'
#TrackingRef '19_web_deposit_cif_file_1_OlivierRoubeau_1259610432.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H34 Fe2 N14 O8 S4, C H4 O'
_chemical_formula_sum            'C53 H38 Fe2 N14 O9 S4'
_chemical_formula_weight         1254.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0018
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0038
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0069
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
S S 0.1150 0.1392
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2117 0.9395
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   11.493(3)
_cell_length_b                   23.530(5)
_cell_length_c                   10.094(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.62(3)
_cell_angle_gamma                90.00
_cell_volume                     2571.2(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3610
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      23.3

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.75140
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ESRF BM16'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'phi rotation at various kappa'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            2970
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         23.30
_reflns_number_total             2970
_reflns_number_gt                2316
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       MxCube
_computing_cell_refinement       'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. All non-hydrogens were
refined anisotropically. The methanol molecule is sitting close to an
inversion center and is thus disordered over two positions by symmetry.
Hydrogens were found in difference Fourier maps, except those on the
methanol molecule. All hydrogens were fixed at geometrically
calculated position and refined with a riding model. Data were cut
at 0.95 angstrom as then I/sigma(I)<2. This poor diffraction at
high angles is probably resulting from sensitivity to crystalization
solvent loss upon mounting and is at the origin of the poor
completeness and data/parameters ratio. In addition, geometrical
limitations of the single-axis goniometer on BM16 may also participate to
this problem.
;
_vrf_THETM01_cut                 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystallization solvent loss upon mounting is likely
at the origin of the reproducibly observed poor diffraction, with
virtually no diffraction below 0.95 angstroms. In addition geometrical
limitations of the single-axis goniometer set-up on BM16 result in a best
resolution of 0.79 angstroms and important blind area. In the present
case two full-sphere datasets were collected for two kappa positions of
the crystal.
;
_vrf_PLAT023_cut                 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.30 Deg.
RESPONSE: Crystallization solvent loss upon mounting is likely
at the origin of the reproducibly observed poor diffraction, with
virtually no diffraction below 0.95 angstroms. In addition geometrical
limitations of the single-axis goniometer set-up on BM16 result in a best
resolution of 0.79 angstroms and important blind area. In the present
case two full-sphere datasets were collected for two kappa positions of
the crystal.
;

_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^)+(0.1390P)^2^+0.8603P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2970
_refine_ls_number_parameters     384
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1874
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_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 0.56093(7) 0.11717(3) 0.55319(8) 0.0791(4) Uani 1 1 d . . .
S1 S 0.92977(13) 0.09955(7) 0.45148(16) 0.0923(6) Uani 1 1 d . . .
S2 S 0.24979(17) 0.04423(8) 0.6690(2) 0.1138(7) Uani 1 1 d . . .
O1 O 0.5966(3) 0.03235(16) 0.6494(4) 0.0819(10) Uani 1 1 d . . .
O2 O 0.4550(3) 0.05927(16) 0.3931(4) 0.0806(10) Uani 1 1 d . . .
O3 O 0.8148(4) -0.00325(18) 1.0179(5) 0.1032(13) Uani 1 1 d . . .
H3 H 0.7592 0.0000 1.0542 0.155 Uiso 1 1 calc R . .
O4 O 0.2727(4) 0.11165(16) -0.0123(5) 0.1011(13) Uani 1 1 d . . .
H4 H 0.2526 0.0871 -0.0765 0.152 Uiso 1 1 calc R . .
N1 N 0.6942(4) 0.12749(19) 0.7637(5) 0.0813(12) Uani 1 1 d . . .
N2 N 0.7601(4) 0.0888(2) 0.8579(5) 0.0833(12) Uani 1 1 d . . .
H2A H 0.7442 0.0521 0.8514 0.100 Uiso 1 1 calc R . .
N3 N 0.6058(4) 0.21050(19) 0.6025(5) 0.0795(12) Uani 1 1 d . . .
N4 N 0.3752(4) 0.1586(2) 0.2462(5) 0.0842(12) Uani 1 1 d . . .
H4B H 0.3548 0.1239 0.2144 0.101 Uiso 1 1 calc R . .
N5 N 0.4568(4) 0.1702(2) 0.3746(5) 0.0839(12) Uani 1 1 d . . .
N6 N 0.7011(5) 0.10877(19) 0.4868(5) 0.0817(12) Uani 1 1 d . . .
N7 N 0.4175(5) 0.1195(2) 0.6279(5) 0.0866(13) Uani 1 1 d . . .
C1 C 0.5402(5) -0.0082(3) 0.5728(6) 0.0785(14) Uani 1 1 d . . .
C2 C 0.9202(5) 0.0230(3) 1.1020(6) 0.0863(16) Uani 1 1 d . . .
C3 C 1.0048(5) -0.0064(3) 1.2085(6) 0.0851(15) Uani 1 1 d . . .
H3A H 0.9900 -0.0452 1.2238 0.102 Uiso 1 1 calc R . .
C4 C 1.1111(5) 0.0196(3) 1.2938(6) 0.0868(16) Uani 1 1 d . . .
H4A H 1.1691 -0.0011 1.3677 0.104 Uiso 1 1 calc R . .
C5 C 1.1326(5) 0.0758(3) 1.2709(6) 0.0886(16) Uani 1 1 d . . .
H5A H 1.2051 0.0942 1.3298 0.106 Uiso 1 1 calc R . .
C6 C 1.0486(5) 0.1051(2) 1.1624(6) 0.0820(15) Uani 1 1 d . . .
H6A H 1.0655 0.1435 1.1459 0.098 Uiso 1 1 calc R . .
C7 C 0.9401(5) 0.0801(2) 1.0765(5) 0.0801(14) Uani 1 1 d . . .
C8 C 0.8539(5) 0.1126(2) 0.9640(6) 0.0811(15) Uani 1 1 d . . .
C9 C 0.8460(5) 0.1707(2) 0.9350(6) 0.0833(15) Uani 1 1 d . . .
H9A H 0.8985 0.1996 0.9890 0.100 Uiso 1 1 calc R . .
C10 C 0.7471(5) 0.1779(2) 0.8127(6) 0.0812(15) Uani 1 1 d . . .
C11 C 0.6913(5) 0.2258(2) 0.7235(6) 0.0830(15) Uani 1 1 d . . .
C12 C 0.7218(5) 0.2822(3) 0.7562(6) 0.0900(16) Uani 1 1 d . . .
H12A H 0.7837 0.2925 0.8421 0.108 Uiso 1 1 calc R . .
C13 C 0.6592(5) 0.3236(3) 0.6597(6) 0.0899(16) Uani 1 1 d . . .
H13A H 0.6775 0.3627 0.6800 0.108 Uiso 1 1 calc R . .
C14 C 0.5714(5) 0.3080(3) 0.5360(6) 0.0874(16) Uani 1 1 d . . .
H14A H 0.5278 0.3359 0.4698 0.105 Uiso 1 1 calc R . .
C15 C 0.5470(5) 0.2500(2) 0.5087(6) 0.0819(15) Uani 1 1 d . . .
C16 C 0.4606(5) 0.2274(3) 0.3826(6) 0.0826(15) Uani 1 1 d . . .
C17 C 0.3824(5) 0.2510(2) 0.2583(6) 0.0825(15) Uani 1 1 d . . .
H17A H 0.3690 0.2903 0.2371 0.099 Uiso 1 1 calc R . .
C18 C 0.3279(5) 0.2061(2) 0.1715(6) 0.0802(15) Uani 1 1 d . . .
C19 C 0.2350(5) 0.2071(2) 0.0337(6) 0.0812(15) Uani 1 1 d . . .
C20 C 0.1672(5) 0.2572(2) -0.0134(6) 0.0863(16) Uani 1 1 d . . .
H20A H 0.1839 0.2896 0.0463 0.104 Uiso 1 1 calc R . .
C21 C 0.0771(5) 0.2605(2) -0.1442(6) 0.0883(16) Uani 1 1 d . . .
H21A H 0.0313 0.2946 -0.1731 0.106 Uiso 1 1 calc R . .
C22 C 0.0538(5) 0.2142(3) -0.2326(7) 0.0934(17) Uani 1 1 d . . .
H22A H -0.0078 0.2164 -0.3230 0.112 Uiso 1 1 calc R . .
C23 C 0.1198(5) 0.1647(3) -0.1901(7) 0.0909(16) Uani 1 1 d . . .
H23A H 0.1045 0.1330 -0.2519 0.109 Uiso 1 1 calc R . .
C24 C 0.2070(5) 0.1611(2) -0.0598(7) 0.0862(16) Uani 1 1 d . . .
C25 C 0.7981(6) 0.1051(2) 0.4727(6) 0.0813(15) Uani 1 1 d . . .
C26 C 0.3475(5) 0.0881(3) 0.6473(6) 0.0827(15) Uani 1 1 d . . .
O1S O 0.3814(9) -0.0367(4) 0.8909(12) 0.123(3) Uani 0.50 1 d PDU . .
H1S H 0.3472 -0.0236 0.8096 0.184 Uiso 0.50 1 calc PR . .
C1S C 0.491(4) -0.003(2) 0.963(3) 0.162(13) Uani 0.50 1 d PDU . .
H1S1 H 0.4697 0.0370 0.9526 0.244 Uiso 0.50 1 calc PR . .
H1S2 H 0.5548 -0.0114 0.9214 0.244 Uiso 0.50 1 calc PR . .
H1S3 H 0.5209 -0.0136 1.0627 0.244 Uiso 0.50 1 calc PR . .

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 0.0848(6) 0.0636(7) 0.0878(7) 0.0039(4) 0.0278(4) 0.0024(3)
S1 0.0880(10) 0.0896(12) 0.1011(12) 0.0017(8) 0.0341(8) 0.0038(7)
S2 0.1060(12) 0.0903(13) 0.1558(17) -0.0212(10) 0.0582(12) -0.0177(9)
O1 0.087(2) 0.068(3) 0.089(3) 0.0041(19) 0.0260(19) 0.0021(18)
O2 0.087(2) 0.063(3) 0.087(2) 0.0076(18) 0.0226(18) 0.0044(17)
O3 0.104(3) 0.070(3) 0.114(3) 0.001(2) 0.008(3) -0.001(2)
O4 0.101(3) 0.063(3) 0.136(4) -0.004(2) 0.035(3) 0.002(2)
N1 0.095(3) 0.061(3) 0.089(3) 0.004(2) 0.032(2) 0.007(2)
N2 0.098(3) 0.067(3) 0.083(3) 0.003(2) 0.028(3) 0.002(2)
N3 0.086(3) 0.065(3) 0.090(3) 0.002(2) 0.033(3) 0.005(2)
N4 0.089(3) 0.065(3) 0.097(3) 0.004(2) 0.029(3) 0.001(2)
N5 0.085(3) 0.071(4) 0.095(3) 0.006(2) 0.029(3) 0.000(2)
N6 0.091(3) 0.064(3) 0.086(3) 0.003(2) 0.025(3) 0.002(2)
N7 0.098(3) 0.069(3) 0.093(3) 0.003(2) 0.033(3) 0.007(2)
C1 0.081(3) 0.068(4) 0.088(4) -0.001(3) 0.030(3) 0.003(3)
C2 0.093(4) 0.074(4) 0.086(4) -0.002(3) 0.022(3) -0.004(3)
C3 0.094(4) 0.072(4) 0.089(4) 0.006(3) 0.030(3) -0.001(3)
C4 0.088(4) 0.077(4) 0.095(4) 0.007(3) 0.030(3) 0.008(3)
C5 0.081(3) 0.086(5) 0.098(4) -0.002(3) 0.028(3) 0.002(3)
C6 0.092(4) 0.070(4) 0.090(4) -0.002(3) 0.038(3) -0.004(3)
C7 0.093(4) 0.067(4) 0.080(3) -0.003(3) 0.028(3) 0.002(3)
C8 0.089(4) 0.074(5) 0.081(4) -0.006(3) 0.028(3) -0.003(3)
C9 0.103(4) 0.060(4) 0.091(4) -0.006(3) 0.037(3) -0.004(3)
C10 0.094(4) 0.062(4) 0.089(4) -0.004(3) 0.033(3) -0.002(3)
C11 0.096(4) 0.063(4) 0.096(4) -0.004(3) 0.041(3) 0.000(3)
C12 0.094(4) 0.080(5) 0.098(4) -0.003(3) 0.035(3) -0.001(3)
C13 0.107(4) 0.066(4) 0.100(4) 0.001(3) 0.040(4) 0.004(3)
C14 0.093(4) 0.072(5) 0.103(5) 0.004(3) 0.040(4) 0.007(3)
C15 0.089(4) 0.063(4) 0.099(4) 0.004(3) 0.037(3) 0.005(3)
C16 0.086(4) 0.064(4) 0.101(4) 0.006(3) 0.036(3) 0.006(3)
C17 0.094(4) 0.065(4) 0.094(4) 0.009(3) 0.039(3) 0.005(3)
C18 0.090(4) 0.064(4) 0.089(4) 0.012(3) 0.035(3) 0.007(3)
C19 0.096(4) 0.060(4) 0.094(4) 0.010(3) 0.041(3) 0.002(3)
C20 0.101(4) 0.071(4) 0.087(4) 0.005(3) 0.031(3) 0.004(3)
C21 0.111(4) 0.065(4) 0.094(4) 0.005(3) 0.041(4) 0.005(3)
C22 0.099(4) 0.082(5) 0.098(4) 0.005(3) 0.031(3) -0.008(3)
C23 0.095(4) 0.074(4) 0.107(5) -0.004(3) 0.039(4) -0.004(3)
C24 0.088(4) 0.069(4) 0.109(5) 0.005(3) 0.042(3) -0.002(3)
C25 0.100(4) 0.060(4) 0.080(4) 0.004(2) 0.025(3) 0.002(3)
C26 0.083(4) 0.077(4) 0.088(4) -0.003(3) 0.029(3) -0.003(3)
O1S 0.121(7) 0.085(7) 0.160(9) 0.009(6) 0.044(7) 0.001(5)
C1S 0.092(13) 0.20(2) 0.15(3) 0.05(3) -0.02(2) 0.012(10)

_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 N6 1.952(5) . ?
Fe1 N7 2.030(5) . ?
Fe1 O2 2.151(4) . ?
Fe1 N1 2.176(5) . ?
Fe1 N5 2.189(5) . ?
Fe1 O1 2.197(4) . ?
Fe1 N3 2.273(5) . ?
S1 C25 1.603(7) . ?
S2 C26 1.593(7) . ?
O1 C1 1.261(7) . ?
O2 C1 1.247(7) 3_656 ?
O3 C2 1.371(7) . ?
O3 H3 0.8400 . ?
O4 C24 1.382(7) . ?
O4 H4 0.8400 . ?
N1 C10 1.349(7) . ?
N1 N2 1.351(6) . ?
N2 C8 1.359(7) . ?
N2 H2A 0.8800 . ?
N3 C11 1.334(7) . ?
N3 C15 1.338(7) . ?
N4 N5 1.348(6) . ?
N4 C18 1.356(7) . ?
N4 H4B 0.8800 . ?
N5 C16 1.347(7) . ?
N6 C25 1.173(7) . ?
N7 C26 1.158(7) . ?
C1 O2 1.247(7) 3_656 ?
C1 C1 1.501(11) 3_656 ?
C2 C3 1.370(8) . ?
C2 C7 1.402(8) . ?
C3 C4 1.379(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.380(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.377(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.389(7) . ?
C6 H6A 0.9500 . ?
C7 C8 1.450(8) . ?
C8 C9 1.394(8) . ?
C9 C10 1.380(7) . ?
C9 H9A 0.9500 . ?
C10 C11 1.450(8) . ?
C11 C12 1.385(8) . ?
C12 C13 1.394(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.366(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.400(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.429(8) . ?
C16 C17 1.391(7) . ?
C17 C18 1.382(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.441(8) . ?
C19 C24 1.402(8) . ?
C19 C20 1.405(7) . ?
C20 C21 1.380(7) . ?
C20 H20A 0.9500 . ?
C21 C22 1.376(8) . ?
C21 H21A 0.9500 . ?
C22 C23 1.378(8) . ?
C22 H22A 0.9500 . ?
C23 C24 1.363(8) . ?
C23 H23A 0.9500 . ?
O1S C1S 1.45(2) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 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
N6 Fe1 N7 175.50(18) . . ?
N6 Fe1 O2 90.13(16) . . ?
N7 Fe1 O2 88.36(17) . . ?
N6 Fe1 N1 87.40(18) . . ?
N7 Fe1 N1 91.56(19) . . ?
O2 Fe1 N1 147.08(16) . . ?
N6 Fe1 N5 93.52(18) . . ?
N7 Fe1 N5 90.14(18) . . ?
O2 Fe1 N5 74.20(17) . . ?
N1 Fe1 N5 138.71(17) . . ?
N6 Fe1 O1 90.39(16) . . ?
N7 Fe1 O1 85.12(16) . . ?
O2 Fe1 O1 74.41(14) . . ?
N1 Fe1 O1 72.79(16) . . ?
N5 Fe1 O1 148.36(17) . . ?
N6 Fe1 N3 91.15(17) . . ?
N7 Fe1 N3 92.57(17) . . ?
O2 Fe1 N3 143.72(16) . . ?
N1 Fe1 N3 69.18(17) . . ?
N5 Fe1 N3 69.53(18) . . ?
O1 Fe1 N3 141.82(17) . . ?
C1 O1 Fe1 115.8(4) . . ?
C1 O2 Fe1 116.2(3) 3_656 . ?
C2 O3 H3 109.5 . . ?
C24 O4 H4 109.5 . . ?
C10 N1 N2 105.0(4) . . ?
C10 N1 Fe1 122.6(4) . . ?
N2 N1 Fe1 131.0(4) . . ?
N1 N2 C8 112.6(5) . . ?
N1 N2 H2A 123.7 . . ?
C8 N2 H2A 123.7 . . ?
C11 N3 C15 120.2(5) . . ?
C11 N3 Fe1 120.3(4) . . ?
C15 N3 Fe1 119.6(4) . . ?
N5 N4 C18 112.7(4) . . ?
N5 N4 H4B 123.6 . . ?
C18 N4 H4B 123.6 . . ?
C16 N5 N4 105.0(4) . . ?
C16 N5 Fe1 121.5(4) . . ?
N4 N5 Fe1 133.4(4) . . ?
C25 N6 Fe1 167.6(5) . . ?
C26 N7 Fe1 138.0(5) . . ?
O2 C1 O1 126.5(5) 3_656 . ?
O2 C1 C1 118.2(7) 3_656 3_656 ?
O1 C1 C1 115.3(7) . 3_656 ?
C3 C2 O3 120.4(6) . . ?
C3 C2 C7 120.8(5) . . ?
O3 C2 C7 118.8(5) . . ?
C2 C3 C4 120.8(6) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 C5 119.5(5) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C6 C5 C4 119.8(6) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C7 121.8(6) . . ?
C5 C6 H6A 119.1 . . ?
C7 C6 H6A 119.1 . . ?
C6 C7 C2 117.3(5) . . ?
C6 C7 C8 120.0(6) . . ?
C2 C7 C8 122.6(5) . . ?
N2 C8 C9 105.2(5) . . ?
N2 C8 C7 123.5(5) . . ?
C9 C8 C7 131.4(5) . . ?
C10 C9 C8 106.5(5) . . ?
C10 C9 H9A 126.7 . . ?
C8 C9 H9A 126.7 . . ?
N1 C10 C9 110.7(5) . . ?
N1 C10 C11 113.9(5) . . ?
C9 C10 C11 135.3(5) . . ?
N3 C11 C12 121.7(5) . . ?
N3 C11 C10 113.3(5) . . ?
C12 C11 C10 125.0(6) . . ?
C11 C12 C13 118.3(6) . . ?
C11 C12 H12A 120.9 . . ?
C13 C12 H12A 120.9 . . ?
C14 C13 C12 120.0(6) . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C13 C14 C15 118.7(6) . . ?
C13 C14 H14A 120.7 . . ?
C15 C14 H14A 120.7 . . ?
N3 C15 C14 121.2(6) . . ?
N3 C15 C16 114.0(5) . . ?
C14 C15 C16 124.9(6) . . ?
N5 C16 C17 110.3(5) . . ?
N5 C16 C15 115.1(5) . . ?
C17 C16 C15 134.5(6) . . ?
C18 C17 C16 106.5(5) . . ?
C18 C17 H17A 126.7 . . ?
C16 C17 H17A 126.7 . . ?
N4 C18 C17 105.5(5) . . ?
N4 C18 C19 125.4(5) . . ?
C17 C18 C19 129.0(5) . . ?
C24 C19 C20 116.4(5) . . ?
C24 C19 C18 124.4(5) . . ?
C20 C19 C18 119.2(5) . . ?
C21 C20 C19 121.6(5) . . ?
C21 C20 H20A 119.2 . . ?
C19 C20 H20A 119.2 . . ?
C22 C21 C20 119.8(6) . . ?
C22 C21 H21A 120.1 . . ?
C20 C21 H21A 120.1 . . ?
C21 C22 C23 120.0(6) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C24 C23 C22 120.2(6) . . ?
C24 C23 H23A 119.9 . . ?
C22 C23 H23A 119.9 . . ?
C23 C24 O4 121.8(5) . . ?
C23 C24 C19 122.0(5) . . ?
O4 C24 C19 116.2(5) . . ?
N6 C25 S1 179.2(6) . . ?
N7 C26 S2 178.2(5) . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        23.30
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.069