# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2009

data_global

_journal_coden_Cambridge         440

loop_
_publ_author_name
'Lionel Salmon'
'Azzedine Bousseksou'
'Saioa Cobo'
'Phillippe Demont'
'Akira Eguchi'
'Michel Etienne'
'Tarik Mahfoud'
'Gabor Molnar'
'Pascal Oulie'
'Koichiro Tanaka'
'Hiroshi Watanabe'

_publ_contact_author_name        'Lionel Salmon'
_publ_contact_author_email       LIONEL.SALMON@LCC-TOULOUSE.FR

_publ_section_title              
;
Reinvestigation of the spin crossover phenomenon in
the ferrous complex [Fe(HB(pz)3)2]
;

# Submission details
_publ_requested_journal          'Acta Crystallographica Section C '

# Attachment 'Structure 180 K-3.cif'

data_sl3fin
_database_code_depnum_ccdc_archive 'CCDC 729351'
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C18 H20 B2 Fe1 N12'
_chemical_formula_sum            'C18 H20 B2 Fe N12'
_chemical_formula_weight         481.93
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.900(2)
_cell_length_b                   17.020(3)
_cell_length_c                   12.890(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.53(3)
_cell_angle_gamma                90
_cell_volume                     2157.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    6000
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_T_max  0.917

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180
_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 Kappa Apex II'
_diffrn_measurement_method       \w-\f
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_number            20045
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         24.58
_diffrn_reflns_theta_full        24.58
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_reflns_number_total             3575
_reflns_number_gt                3074
_reflns_threshold_expression     >2\s(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker Apex 2'
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_reduction        'Bruker Apex 2'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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.
;
_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^)+(0.0309P)^2^+1.0995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3575
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.071
_refine_ls_wR_factor_gt          0.0664
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.041

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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'
N N 0.0061 0.0033 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C11 C 0.5175(2) 0.38308(12) 0.82853(18) 0.0442(5) Uani 1 1 d . . .
H11 H 0.5204 0.4337 0.8599 0.053 Uiso 1 1 calc R . .
C12 C 0.4350(2) 0.36151(13) 0.74117(19) 0.0508(6) Uani 1 1 d . . .
H12 H 0.3701 0.3931 0.7002 0.061 Uiso 1 1 calc R . .
C13 C 0.4666(2) 0.28369(13) 0.72528(17) 0.0431(5) Uani 1 1 d . . .
H13 H 0.4257 0.2522 0.6694 0.052 Uiso 1 1 calc R . .
C21 C 0.6010(2) 0.24436(12) 1.12438(15) 0.0391(5) Uani 1 1 d . . .
H21 H 0.6133 0.287 1.172 0.047 Uiso 1 1 calc R . .
C22 C 0.5496(2) 0.17261(13) 1.14496(17) 0.0455(5) Uani 1 1 d . . .
H22 H 0.5192 0.1553 1.2084 0.055 Uiso 1 1 calc R . .
C23 C 0.5513(2) 0.13028(12) 1.05366(16) 0.0407(5) Uani 1 1 d . . .
H23 H 0.5212 0.0775 1.0441 0.049 Uiso 1 1 calc R . .
C31 C 0.9557(2) 0.29727(12) 0.95092(16) 0.0407(5) Uani 1 1 d . . .
H31 H 0.9868 0.3426 0.9895 0.049 Uiso 1 1 calc R . .
C32 C 1.0359(2) 0.24404(13) 0.90790(18) 0.0468(5) Uani 1 1 d . . .
H32 H 1.1321 0.2448 0.9097 0.056 Uiso 1 1 calc R . .
C33 C 0.9467(2) 0.18869(13) 0.86116(16) 0.0416(5) Uani 1 1 d . . .
H33 H 0.973 0.1438 0.8245 0.05 Uiso 1 1 calc R . .
C41 C 0.3396(2) 0.11460(13) 0.81662(18) 0.0471(5) Uani 1 1 d . . .
H41 H 0.3116 0.1575 0.8562 0.056 Uiso 1 1 calc R . .
C42 C 0.2533(2) 0.05704(14) 0.7710(2) 0.0542(6) Uani 1 1 d . . .
H42 H 0.1579 0.0528 0.7727 0.065 Uiso 1 1 calc R . .
C43 C 0.3354(2) 0.00794(13) 0.72329(18) 0.0456(5) Uani 1 1 d . . .
H43 H 0.3068 -0.038 0.685 0.055 Uiso 1 1 calc R . .
C51 C 0.7606(2) 0.17601(13) 0.62956(16) 0.0415(5) Uani 1 1 d . . .
H51 H 0.7914 0.2285 0.641 0.05 Uiso 1 1 calc R . .
C52 C 0.7834(2) 0.13051(14) 0.54420(18) 0.0513(6) Uani 1 1 d . . .
H52 H 0.8318 0.1449 0.4876 0.062 Uiso 1 1 calc R . .
C53 C 0.7214(2) 0.06078(13) 0.55887(16) 0.0464(5) Uani 1 1 d . . .
H53 H 0.7187 0.0167 0.5134 0.056 Uiso 1 1 calc R . .
C61 C 0.8053(2) 0.02421(13) 0.95538(17) 0.0458(5) Uani 1 1 d . . .
H61 H 0.8421 0.0551 1.0132 0.055 Uiso 1 1 calc R . .
C62 C 0.8325(2) -0.05428(14) 0.9423(2) 0.0548(6) Uani 1 1 d . . .
H62 H 0.8897 -0.0871 0.9878 0.066 Uiso 1 1 calc R . .
C63 C 0.7601(2) -0.07473(12) 0.85019(19) 0.0466(6) Uani 1 1 d . . .
H63 H 0.7583 -0.1253 0.819 0.056 Uiso 1 1 calc R . .
N11 N 0.59370(17) 0.32132(9) 0.86300(13) 0.0363(4) Uani 1 1 d . . .
N12 N 0.56165(16) 0.25895(9) 0.79869(12) 0.0356(4) Uani 1 1 d . . .
N21 N 0.63099(16) 0.24476(9) 1.02613(12) 0.0348(4) Uani 1 1 d . . .
N22 N 0.60071(16) 0.17369(9) 0.98131(12) 0.0346(4) Uani 1 1 d . . .
N31 N 0.82552(16) 0.27487(9) 0.92971(12) 0.0346(4) Uani 1 1 d . . .
N32 N 0.81956(16) 0.20676(9) 0.87436(12) 0.0344(4) Uani 1 1 d . . .
N41 N 0.46620(16) 0.10157(9) 0.79756(13) 0.0366(4) Uani 1 1 d . . .
N42 N 0.46320(16) 0.03497(9) 0.73917(13) 0.0367(4) Uani 1 1 d . . .
N51 N 0.69003(16) 0.13606(9) 0.69291(12) 0.0348(4) Uani 1 1 d . . .
N52 N 0.66482(17) 0.06464(9) 0.64810(12) 0.0370(4) Uani 1 1 d . . .
N61 N 0.72029(16) 0.05065(9) 0.87599(12) 0.0359(4) Uani 1 1 d . . .
N62 N 0.69182(17) -0.01146(9) 0.81084(13) 0.0359(4) Uani 1 1 d . . .
Fe1 Fe 0.64214(3) 0.154886(14) 0.83641(2) 0.02939(10) Uani 1 1 d . . .
B1 B 0.6931(2) 0.30829(13) 0.96177(18) 0.0369(5) Uani 1 1 d . . .
H1 H 0.7095 0.358 1.0025 0.044 Uiso 1 1 calc R . .
B2 B 0.5978(2) 0.00178(13) 0.71005(19) 0.0393(5) Uani 1 1 d . . .
H2 H 0.5831 -0.048 0.6691 0.047 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
C11 0.0517(13) 0.0317(11) 0.0523(14) 0.0071(10) 0.0187(11) 0.0105(10)
C12 0.0478(13) 0.0527(13) 0.0525(14) 0.0146(11) 0.0080(11) 0.0161(11)
C13 0.0398(12) 0.0513(13) 0.0376(12) 0.0028(10) 0.0022(10) 0.0055(10)
C21 0.0444(12) 0.0430(11) 0.0311(11) -0.0075(9) 0.0094(9) 0.0014(9)
C22 0.0527(13) 0.0493(13) 0.0368(12) 0.0024(10) 0.0159(10) -0.0020(10)
C23 0.0467(12) 0.0358(11) 0.0416(12) 0.0014(9) 0.0136(10) -0.0038(9)
C31 0.0402(12) 0.0410(11) 0.0395(12) 0.0060(9) -0.0017(9) -0.0105(9)
C32 0.0318(11) 0.0563(13) 0.0515(14) 0.0069(11) 0.0019(10) -0.0010(10)
C33 0.0389(12) 0.0464(12) 0.0400(12) 0.0028(10) 0.0060(10) 0.0066(9)
C41 0.0395(12) 0.0465(12) 0.0570(14) -0.0013(11) 0.0135(11) 0.0048(10)
C42 0.0352(12) 0.0559(14) 0.0715(17) 0.0036(12) 0.0062(12) -0.0033(10)
C43 0.0460(13) 0.0427(12) 0.0462(13) 0.0017(10) -0.0030(10) -0.0099(10)
C51 0.0404(12) 0.0446(12) 0.0405(12) 0.0070(10) 0.0084(10) 0.0004(9)
C52 0.0550(14) 0.0625(15) 0.0395(13) 0.0087(11) 0.0191(11) 0.0091(11)
C53 0.0553(14) 0.0528(13) 0.0326(11) -0.0052(10) 0.0112(10) 0.0117(11)
C61 0.0460(13) 0.0529(13) 0.0374(12) 0.0066(10) 0.0003(10) 0.0067(10)
C62 0.0523(14) 0.0541(14) 0.0581(16) 0.0191(12) 0.0067(12) 0.0156(11)
C63 0.0475(13) 0.0333(11) 0.0623(15) 0.0063(10) 0.0199(12) 0.0081(9)
N11 0.0410(10) 0.0288(8) 0.0401(10) -0.0011(7) 0.0095(8) 0.0026(7)
N12 0.0382(9) 0.0354(9) 0.0333(9) -0.0020(7) 0.0049(8) 0.0022(7)
N21 0.0409(9) 0.0315(8) 0.0327(9) -0.0057(7) 0.0076(7) -0.0009(7)
N22 0.0404(9) 0.0300(8) 0.0342(9) -0.0042(7) 0.0083(7) -0.0020(7)
N31 0.0387(9) 0.0306(8) 0.0345(9) -0.0010(7) 0.0041(7) -0.0042(7)
N32 0.0349(9) 0.0347(9) 0.0336(9) -0.0017(7) 0.0041(7) 0.0011(7)
N41 0.0389(10) 0.0328(9) 0.0389(9) -0.0043(7) 0.0075(8) 0.0010(7)
N42 0.0403(10) 0.0336(9) 0.0361(9) -0.0046(7) 0.0034(8) -0.0037(7)
N51 0.0380(9) 0.0339(9) 0.0328(9) -0.0013(7) 0.0052(7) 0.0015(7)
N52 0.0457(10) 0.0350(9) 0.0311(9) -0.0053(7) 0.0070(8) 0.0040(7)
N61 0.0399(9) 0.0349(9) 0.0331(9) -0.0017(7) 0.0051(8) 0.0032(7)
N62 0.0422(9) 0.0282(8) 0.0388(9) -0.0012(7) 0.0106(8) 0.0036(7)
Fe1 0.03232(16) 0.02761(15) 0.02863(16) -0.00309(11) 0.00518(11) 0.00103(11)
B1 0.0450(13) 0.0284(11) 0.0380(13) -0.0047(10) 0.0074(11) -0.0038(10)
B2 0.0488(14) 0.0314(12) 0.0386(13) -0.0095(10) 0.0087(11) -0.0010(10)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
C11 N11 1.340(3) . ?
C11 C12 1.364(3) . ?
C11 H11 0.95 . ?
C12 C13 1.381(3) . ?
C12 H12 0.95 . ?
C13 N12 1.325(3) . ?
C13 H13 0.95 . ?
C21 N21 1.333(3) . ?
C21 C22 1.360(3) . ?
C21 H21 0.95 . ?
C22 C23 1.382(3) . ?
C22 H22 0.95 . ?
C23 N22 1.326(3) . ?
C23 H23 0.95 . ?
C31 N31 1.342(3) . ?
C31 C32 1.363(3) . ?
C31 H31 0.95 . ?
C32 C33 1.382(3) . ?
C32 H32 0.95 . ?
C33 N32 1.326(3) . ?
C33 H33 0.95 . ?
C41 N41 1.323(3) . ?
C41 C42 1.386(3) . ?
C41 H41 0.95 . ?
C42 C43 1.360(3) . ?
C42 H42 0.95 . ?
C43 N42 1.340(3) . ?
C43 H43 0.95 . ?
C51 N51 1.322(3) . ?
C51 C52 1.385(3) . ?
C51 H51 0.95 . ?
C52 C53 1.359(3) . ?
C52 H52 0.95 . ?
C53 N52 1.337(3) . ?
C53 H53 0.95 . ?
C61 N61 1.327(3) . ?
C61 C62 1.377(3) . ?
C61 H61 0.95 . ?
C62 C63 1.360(3) . ?
C62 H62 0.95 . ?
C63 N62 1.340(3) . ?
C63 H63 0.95 . ?
N11 N12 1.362(2) . ?
N11 B1 1.534(3) . ?
N12 Fe1 1.9800(16) . ?
N21 N22 1.359(2) . ?
N21 B1 1.533(3) . ?
N22 Fe1 1.9833(16) . ?
N31 N32 1.359(2) . ?
N31 B1 1.529(3) . ?
N32 Fe1 1.9770(16) . ?
N41 N42 1.359(2) . ?
N41 Fe1 1.9774(17) . ?
N42 B2 1.533(3) . ?
N51 N52 1.357(2) . ?
N51 Fe1 1.9871(17) . ?
N52 B2 1.530(3) . ?
N61 N62 1.360(2) . ?
N61 Fe1 1.9790(16) . ?
N62 B2 1.526(3) . ?
B1 H1 1 . ?
B2 H2 1 . ?

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
N11 C11 C12 108.92(19) . . ?
N11 C11 H11 125.5 . . ?
C12 C11 H11 125.5 . . ?
C11 C12 C13 104.85(19) . . ?
C11 C12 H12 127.6 . . ?
C13 C12 H12 127.6 . . ?
N12 C13 C12 110.7(2) . . ?
N12 C13 H13 124.7 . . ?
C12 C13 H13 124.7 . . ?
N21 C21 C22 108.57(18) . . ?
N21 C21 H21 125.7 . . ?
C22 C21 H21 125.7 . . ?
C21 C22 C23 105.14(19) . . ?
C21 C22 H22 127.4 . . ?
C23 C22 H22 127.4 . . ?
N22 C23 C22 110.46(18) . . ?
N22 C23 H23 124.8 . . ?
C22 C23 H23 124.8 . . ?
N31 C31 C32 108.58(19) . . ?
N31 C31 H31 125.7 . . ?
C32 C31 H31 125.7 . . ?
C31 C32 C33 104.93(19) . . ?
C31 C32 H32 127.5 . . ?
C33 C32 H32 127.5 . . ?
N32 C33 C32 110.78(19) . . ?
N32 C33 H33 124.6 . . ?
C32 C33 H33 124.6 . . ?
N41 C41 C42 110.7(2) . . ?
N41 C41 H41 124.6 . . ?
C42 C41 H41 124.6 . . ?
C43 C42 C41 104.8(2) . . ?
C43 C42 H42 127.6 . . ?
C41 C42 H42 127.6 . . ?
N42 C43 C42 108.79(19) . . ?
N42 C43 H43 125.6 . . ?
C42 C43 H43 125.6 . . ?
N51 C51 C52 110.4(2) . . ?
N51 C51 H51 124.8 . . ?
C52 C51 H51 124.8 . . ?
C53 C52 C51 105.1(2) . . ?
C53 C52 H52 127.4 . . ?
C51 C52 H52 127.4 . . ?
N52 C53 C52 108.46(19) . . ?
N52 C53 H53 125.8 . . ?
C52 C53 H53 125.8 . . ?
N61 C61 C62 110.5(2) . . ?
N61 C61 H61 124.7 . . ?
C62 C61 H61 124.7 . . ?
C63 C62 C61 105.3(2) . . ?
C63 C62 H62 127.3 . . ?
C61 C62 H62 127.3 . . ?
N62 C63 C62 108.5(2) . . ?
N62 C63 H63 125.7 . . ?
C62 C63 H63 125.7 . . ?
C11 N11 N12 109.04(17) . . ?
C11 N11 B1 132.26(18) . . ?
N12 N11 B1 118.40(15) . . ?
C13 N12 N11 106.52(16) . . ?
C13 N12 Fe1 133.86(14) . . ?
N11 N12 Fe1 119.23(12) . . ?
C21 N21 N22 109.69(16) . . ?
C21 N21 B1 131.60(17) . . ?
N22 N21 B1 118.70(15) . . ?
C23 N22 N21 106.15(16) . . ?
C23 N22 Fe1 134.81(14) . . ?
N21 N22 Fe1 118.98(12) . . ?
C31 N31 N32 109.43(16) . . ?
C31 N31 B1 132.27(17) . . ?
N32 N31 B1 118.16(15) . . ?
C33 N32 N31 106.27(16) . . ?
C33 N32 Fe1 134.00(14) . . ?
N31 N32 Fe1 119.68(12) . . ?
C41 N41 N42 106.33(17) . . ?
C41 N41 Fe1 134.57(15) . . ?
N42 N41 Fe1 119.09(12) . . ?
C43 N42 N41 109.38(17) . . ?
C43 N42 B2 131.93(18) . . ?
N41 N42 B2 118.56(16) . . ?
C51 N51 N52 106.41(16) . . ?
C51 N51 Fe1 133.70(14) . . ?
N52 N51 Fe1 119.28(12) . . ?
C53 N52 N51 109.61(17) . . ?
C53 N52 B2 131.55(17) . . ?
N51 N52 B2 118.28(15) . . ?
C61 N61 N62 106.33(16) . . ?
C61 N61 Fe1 134.24(15) . . ?
N62 N61 Fe1 119.36(12) . . ?
C63 N62 N61 109.31(17) . . ?
C63 N62 B2 132.33(18) . . ?
N61 N62 B2 118.32(15) . . ?
N32 Fe1 N41 179.09(7) . . ?
N32 Fe1 N61 91.51(7) . . ?
N41 Fe1 N61 87.77(7) . . ?
N32 Fe1 N12 89.01(7) . . ?
N41 Fe1 N12 91.72(7) . . ?
N61 Fe1 N12 178.98(7) . . ?
N32 Fe1 N22 88.16(7) . . ?
N41 Fe1 N22 92.41(7) . . ?
N61 Fe1 N22 91.06(7) . . ?
N12 Fe1 N22 88.07(7) . . ?
N32 Fe1 N51 90.18(7) . . ?
N41 Fe1 N51 89.24(7) . . ?
N61 Fe1 N51 88.15(7) . . ?
N12 Fe1 N51 92.73(7) . . ?
N22 Fe1 N51 178.15(7) . . ?
N31 B1 N21 107.02(16) . . ?
N31 B1 N11 108.56(17) . . ?
N21 B1 N11 107.00(16) . . ?
N31 B1 H1 111.3 . . ?
N21 B1 H1 111.3 . . ?
N11 B1 H1 111.3 . . ?
N62 B2 N52 106.81(17) . . ?
N62 B2 N42 107.99(17) . . ?
N52 B2 N42 108.09(17) . . ?
N62 B2 H2 111.3 . . ?
N52 B2 H2 111.3 . . ?
N42 B2 H2 111.3 . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF

# Attachment 'Structure_298K.cif'

data_structure298k
_database_code_depnum_ccdc_archive 'CCDC 729352'

_chemical_compound_source        'Local laboratory'
_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Violet
_cell_measurement_temperature    298
_refine_ls_hydrogen_treatment    constr
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_F_000             992
_diffrn_measurement_device       KappaCCD
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

loop_
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_wavelength_id  all

_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
?
;
_chemical_formula_weight         481.91
_diffrn_radiation_type           ' MoK\a'

loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z
'-X+ 1/2,+Y+ 1/2,-Z+ 1/2'
'+X+ 1/2,-Y+ 1/2,+Z+ 1/2'

_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_cell_setting           Monoclinic
_chemical_formula_moiety         'C18 H20 B2 Fe N12 '
_chemical_formula_sum            'C18 H20 B2 Fe N12 '
_chemical_name_systematic        
;
?
;
_cell_length_a                   9.9386(7)
_cell_length_b                   17.072(2)
_cell_length_c                   12.9414(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.658(7)
_cell_angle_gamma                90.00
_cell_volume                     2181.0(3)
_diffrn_reflns_number            12676
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.13
_diffrn_reflns_theta_full        26.00
_cell_measurement_reflns_used    12676
_cell_measurement_theta_min      4.13
_cell_measurement_theta_max      26.00
_diffrn_measurement_method       CCD
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_diffrn_reflns_av_R_equivalents  0.031
_computing_structure_solution    'DIRDIF (Buerskens et al., 1992)'
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
# Absorption correction

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

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'
B B 0.0013 0.0007 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_exptl_absorpt_coefficient_mu    0.726
_reflns_number_total             3218
_reflns_number_gt                2152
_reflns_threshold_expression     >2sigma(I)

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.
;

_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^)+(0.0321P)^2^+1.6854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3218
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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 0.64204(6) 0.15495(3) 0.83638(3) 0.0296(2) Uani 1 1 d . . .
N11 N 0.5933(3) 0.32125(15) 0.8632(2) 0.0337(8) Uani 1 1 d . . .
N12 N 0.5617(3) 0.25865(15) 0.7986(2) 0.0326(8) Uani 1 1 d . . .
N21 N 0.6312(3) 0.24494(14) 1.02602(19) 0.0325(8) Uani 1 1 d . . .
N22 N 0.6009(3) 0.17328(14) 0.9811(2) 0.0329(8) Uani 1 1 d . . .
N31 N 0.8258(4) 0.27506(15) 0.9297(2) 0.0321(9) Uani 1 1 d . . .
N32 N 0.8192(4) 0.20671(15) 0.8741(2) 0.0333(9) Uani 1 1 d . . .
N41 N 0.4669(4) 0.10190(15) 0.7978(2) 0.0348(9) Uani 1 1 d . . .
N42 N 0.4637(4) 0.03505(15) 0.7391(2) 0.0343(9) Uani 1 1 d . . .
N51 N 0.6901(3) 0.13628(15) 0.6932(2) 0.0323(8) Uani 1 1 d . . .
N52 N 0.6644(3) 0.06462(15) 0.64809(19) 0.0359(8) Uani 1 1 d . . .
N61 N 0.7198(3) 0.05114(15) 0.8757(2) 0.0336(8) Uani 1 1 d . . .
N62 N 0.6920(3) -0.01154(15) 0.8110(2) 0.0331(8) Uani 1 1 d . . .
C11 C 0.5169(4) 0.3832(2) 0.8283(3) 0.0433(11) Uani 1 1 d . . .
C12 C 0.4350(5) 0.3615(2) 0.7411(3) 0.0496(12) Uani 1 1 d . . .
C13 C 0.4660(4) 0.2839(2) 0.7253(3) 0.0400(11) Uani 1 1 d . . .
C21 C 0.6005(4) 0.2446(2) 1.1246(3) 0.0374(10) Uani 1 1 d . . .
C22 C 0.5495(4) 0.1721(2) 1.1452(3) 0.0443(11) Uani 1 1 d . . .
C23 C 0.5514(4) 0.13025(19) 1.0541(3) 0.0380(10) Uani 1 1 d . . .
C31 C 0.9557(5) 0.2972(2) 0.9508(3) 0.0370(11) Uani 1 1 d . . .
C32 C 1.0357(4) 0.2438(2) 0.9073(3) 0.0432(11) Uani 1 1 d . . .
C33 C 0.9467(5) 0.1888(2) 0.8609(3) 0.0372(11) Uani 1 1 d . . .
C41 C 0.3400(5) 0.1145(2) 0.8168(3) 0.0446(12) Uani 1 1 d . . .
C42 C 0.2528(5) 0.0570(2) 0.7711(3) 0.0514(12) Uani 1 1 d . . .
C43 C 0.3355(5) 0.0084(2) 0.7237(3) 0.0432(12) Uani 1 1 d . . .
C51 C 0.7607(4) 0.1760(2) 0.6294(3) 0.0405(11) Uani 1 1 d . . .
C52 C 0.7830(4) 0.1306(2) 0.5441(3) 0.0479(12) Uani 1 1 d . . .
C53 C 0.7222(4) 0.0610(2) 0.5587(3) 0.0448(11) Uani 1 1 d . . .
C61 C 0.8047(4) 0.0246(2) 0.9552(3) 0.0425(10) Uani 1 1 d . . .
C62 C 0.8328(4) -0.0542(2) 0.9421(3) 0.0519(12) Uani 1 1 d . . .
C63 C 0.7603(4) -0.0748(2) 0.8505(3) 0.0447(11) Uani 1 1 d . . .
B1 B 0.6937(5) 0.3080(2) 0.9615(3) 0.0363(12) Uani 1 1 d . . .
B2 B 0.5974(5) 0.0020(2) 0.7101(3) 0.0367(12) Uani 1 1 d . . .
H11 H 0.5275 0.4322 0.8648 0.052 Uiso 1 1 d R . .
H12 H 0.3733 0.3989 0.7062 0.060 Uiso 1 1 d R . .
H13 H 0.4292 0.2484 0.6718 0.048 Uiso 1 1 d R . .
H21 H 0.6161 0.2910 1.1662 0.045 Uiso 1 1 d R . .
H22 H 0.5213 0.1613 1.2123 0.053 Uiso 1 1 d R . .
H23 H 0.5248 0.0771 1.0388 0.046 Uiso 1 1 d R . .
H31 H 0.9771 0.3440 0.9904 0.044 Uiso 1 1 d R . .
H32 H 1.1320 0.2517 0.9152 0.052 Uiso 1 1 d R . .
H33 H 0.9650 0.1425 0.8229 0.045 Uiso 1 1 d R . .
H41 H 0.3198 0.1591 0.8576 0.054 Uiso 1 1 d R . .
H42 H 0.1580 0.0601 0.7788 0.062 Uiso 1 1 d R . .
H43 H 0.3166 -0.0388 0.6842 0.052 Uiso 1 1 d R . .
H51 H 0.7872 0.2289 0.6467 0.049 Uiso 1 1 d R . .
H52 H 0.8331 0.1515 0.4913 0.058 Uiso 1 1 d R . .
H53 H 0.7146 0.0135 0.5187 0.054 Uiso 1 1 d R . .
H61 H 0.8361 0.0597 1.0108 0.051 Uiso 1 1 d R . .
H62 H 0.8931 -0.0813 0.9934 0.062 Uiso 1 1 d R . .
H63 H 0.7512 -0.1234 0.8130 0.054 Uiso 1 1 d R . .
H1 H 0.7089 0.3546 1.0027 0.044 Uiso 1 1 d R . .
H2 H 0.5840 -0.0447 0.6688 0.044 Uiso 1 1 d 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 0.0347(5) 0.0262(3) 0.0280(3) -0.0029(2) 0.0039(3) 0.0012(2)
N11 0.036(3) 0.0270(15) 0.0379(17) -0.0020(12) 0.0051(17) 0.0030(15)
N12 0.033(3) 0.0346(16) 0.0304(16) -0.0045(13) 0.0024(16) 0.0019(15)
N21 0.038(2) 0.0300(15) 0.0299(15) -0.0039(12) 0.0064(15) -0.0010(14)
N22 0.036(2) 0.0273(15) 0.0355(16) -0.0036(12) 0.0060(16) -0.0019(14)
N31 0.031(3) 0.0300(16) 0.0342(17) -0.0020(12) -0.0008(18) -0.0021(16)
N32 0.034(3) 0.0329(16) 0.0320(16) -0.0036(12) 0.0011(17) -0.0013(15)
N41 0.037(3) 0.0312(16) 0.0363(17) -0.0052(12) 0.0061(18) -0.0030(15)
N42 0.036(3) 0.0306(16) 0.0357(16) -0.0054(12) -0.0002(18) -0.0026(16)
N51 0.034(2) 0.0321(16) 0.0307(15) -0.0014(12) 0.0026(15) 0.0007(14)
N52 0.045(3) 0.0346(16) 0.0286(15) -0.0061(12) 0.0063(16) 0.0044(15)
N61 0.038(3) 0.0337(16) 0.0282(15) -0.0005(13) -0.0001(16) 0.0036(15)
N62 0.039(3) 0.0248(15) 0.0359(16) -0.0016(12) 0.0050(16) 0.0035(14)
C11 0.050(4) 0.033(2) 0.049(2) 0.0065(17) 0.017(2) 0.010(2)
C12 0.051(4) 0.047(2) 0.051(3) 0.0145(19) 0.009(2) 0.019(2)
C13 0.035(4) 0.049(2) 0.035(2) 0.0037(17) -0.004(2) 0.006(2)
C21 0.040(3) 0.039(2) 0.034(2) -0.0067(16) 0.007(2) 0.0037(19)
C22 0.052(4) 0.050(2) 0.033(2) 0.0005(16) 0.015(2) 0.001(2)
C23 0.040(3) 0.0331(19) 0.043(2) 0.0016(16) 0.011(2) -0.0019(18)
C31 0.030(4) 0.041(2) 0.037(2) 0.0030(16) -0.007(2) -0.005(2)
C32 0.021(3) 0.053(2) 0.054(2) 0.0050(19) -0.002(2) -0.005(2)
C33 0.028(4) 0.042(2) 0.041(2) 0.0008(17) 0.002(2) 0.003(2)
C41 0.035(4) 0.045(2) 0.055(3) -0.0019(18) 0.011(3) 0.000(2)
C42 0.027(4) 0.056(3) 0.071(3) 0.004(2) 0.005(3) 0.003(2)
C43 0.043(4) 0.039(2) 0.046(2) 0.0032(17) -0.003(2) -0.009(2)
C51 0.041(3) 0.045(2) 0.036(2) 0.0061(16) 0.008(2) -0.0008(19)
C52 0.051(4) 0.060(3) 0.036(2) 0.0119(18) 0.014(2) 0.007(2)
C53 0.053(3) 0.048(2) 0.034(2) -0.0042(17) 0.008(2) 0.014(2)
C61 0.043(3) 0.046(2) 0.038(2) 0.0039(18) 0.003(2) 0.007(2)
C62 0.046(4) 0.055(3) 0.053(3) 0.022(2) 0.000(2) 0.015(2)
C63 0.045(4) 0.034(2) 0.058(3) 0.0081(18) 0.016(2) 0.008(2)
B1 0.047(4) 0.027(2) 0.035(2) -0.0079(17) 0.005(2) -0.005(2)
B2 0.042(4) 0.029(2) 0.040(2) -0.0103(18) 0.008(3) -0.002(2)

_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 N41 1.975(3) . ?
Fe1 N61 1.976(3) . ?
Fe1 N32 1.980(3) . ?
Fe1 N12 1.980(3) . ?
Fe1 N22 1.988(3) . ?
Fe1 N51 1.992(3) . ?
N11 C11 1.349(4) . ?
N11 N12 1.371(3) . ?
N11 B1 1.540(5) . ?
N12 C13 1.335(4) . ?
N21 C21 1.346(4) . ?
N21 N22 1.373(3) . ?
N21 B1 1.536(4) . ?
N22 C23 1.335(4) . ?
N31 C31 1.342(4) . ?
N31 N32 1.369(3) . ?
N31 B1 1.528(5) . ?
N32 C33 1.334(4) . ?
N41 C41 1.331(4) . ?
N41 N42 1.369(3) . ?
N42 C43 1.346(4) . ?
N42 B2 1.530(5) . ?
N51 C51 1.330(4) . ?
N51 N52 1.367(3) . ?
N52 C53 1.351(4) . ?
N52 B2 1.535(4) . ?
N61 C61 1.333(4) . ?
N61 N62 1.367(3) . ?
N62 C63 1.345(4) . ?
N62 B2 1.535(5) . ?
C11 C12 1.364(5) . ?
C12 C13 1.381(5) . ?
C21 C22 1.376(4) . ?
C22 C23 1.380(4) . ?
C31 C32 1.373(5) . ?
C32 C33 1.379(5) . ?
C41 C42 1.395(5) . ?
C42 C43 1.363(5) . ?
C51 C52 1.387(5) . ?
C52 C53 1.357(5) . ?
C61 C62 1.388(5) . ?
C62 C63 1.360(5) . ?
C11 H11 0.9601 . ?
C12 H12 0.9601 . ?
C13 H13 0.9600 . ?
C21 H21 0.9602 . ?
C22 H22 0.9601 . ?
C23 H23 0.9599 . ?
C31 H31 0.9601 . ?
C32 H32 0.9600 . ?
C33 H33 0.9600 . ?
C41 H41 0.9600 . ?
C42 H42 0.9600 . ?
C43 H43 0.9599 . ?
C51 H51 0.9599 . ?
C52 H52 0.9600 . ?
C53 H53 0.9600 . ?
C61 H61 0.9600 . ?
C62 H62 0.9600 . ?
C63 H63 0.9600 . ?
B1 H1 0.9599 . ?
B2 H2 0.9599 . ?

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
N41 Fe1 N61 87.75(12) . . ?
N41 Fe1 N32 179.08(13) . . ?
N61 Fe1 N32 91.54(12) . . ?
N41 Fe1 N12 91.68(12) . . ?
N61 Fe1 N12 179.02(12) . . ?
N32 Fe1 N12 89.04(12) . . ?
N41 Fe1 N22 92.24(12) . . ?
N61 Fe1 N22 90.90(11) . . ?
N32 Fe1 N22 88.35(11) . . ?
N12 Fe1 N22 88.32(10) . . ?
N41 Fe1 N51 89.47(11) . . ?
N61 Fe1 N51 88.11(11) . . ?
N32 Fe1 N51 89.93(12) . . ?
N12 Fe1 N51 92.68(11) . . ?
N22 Fe1 N51 177.99(13) . . ?
C11 N11 N12 109.1(3) . . ?
C11 N11 B1 132.7(3) . . ?
N12 N11 B1 118.0(3) . . ?
C13 N12 N11 106.0(3) . . ?
C13 N12 Fe1 134.3(2) . . ?
N11 N12 Fe1 119.3(2) . . ?
C21 N21 N22 109.6(3) . . ?
C21 N21 B1 131.9(3) . . ?
N22 N21 B1 118.5(2) . . ?
C23 N22 N21 105.8(3) . . ?
C23 N22 Fe1 135.5(2) . . ?
N21 N22 Fe1 118.70(19) . . ?
C31 N31 N32 109.5(3) . . ?
C31 N31 B1 132.7(3) . . ?
N32 N31 B1 117.7(3) . . ?
C33 N32 N31 105.9(3) . . ?
C33 N32 Fe1 134.2(2) . . ?
N31 N32 Fe1 119.8(3) . . ?
C41 N41 N42 106.0(3) . . ?
C41 N41 Fe1 134.9(3) . . ?
N42 N41 Fe1 119.1(3) . . ?
C43 N42 N41 109.0(3) . . ?
C43 N42 B2 132.3(3) . . ?
N41 N42 B2 118.6(3) . . ?
C51 N51 N52 106.1(3) . . ?
C51 N51 Fe1 134.2(2) . . ?
N52 N51 Fe1 119.17(19) . . ?
C53 N52 N51 109.3(3) . . ?
C53 N52 B2 132.0(3) . . ?
N51 N52 B2 118.1(2) . . ?
C61 N61 N62 105.8(3) . . ?
C61 N61 Fe1 134.2(2) . . ?
N62 N61 Fe1 119.9(2) . . ?
C63 N62 N61 109.7(3) . . ?
C63 N62 B2 132.6(3) . . ?
N61 N62 B2 117.6(3) . . ?
N11 C11 C12 108.9(3) . . ?
C11 C12 C13 105.1(4) . . ?
N12 C13 C12 111.0(3) . . ?
N21 C21 C22 108.5(3) . . ?
C21 C22 C23 105.0(3) . . ?
N22 C23 C22 111.3(3) . . ?
N31 C31 C32 108.6(4) . . ?
C31 C32 C33 105.0(4) . . ?
N32 C33 C32 111.0(4) . . ?
N41 C41 C42 111.3(4) . . ?
C43 C42 C41 104.0(4) . . ?
N42 C43 C42 109.7(4) . . ?
N51 C51 C52 110.7(3) . . ?
C53 C52 C51 105.3(3) . . ?
N52 C53 C52 108.7(3) . . ?
N61 C61 C62 110.7(3) . . ?
C63 C62 C61 105.3(3) . . ?
N62 C63 C62 108.5(3) . . ?
N31 B1 N21 107.6(3) . . ?
N31 B1 N11 109.1(3) . . ?
N21 B1 N11 106.7(3) . . ?
N42 B2 N52 108.2(3) . . ?
N42 B2 N62 108.1(3) . . ?
N52 B2 N62 106.8(3) . . ?
N11 C11 H11 119.5 . . ?
C12 C11 H11 131.6 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 135.2 . . ?
N12 C13 H13 119.2 . . ?
C12 C13 H13 129.8 . . ?
N21 C21 H21 119.2 . . ?
C22 C21 H21 132.4 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 135.0 . . ?
N22 C23 H23 119.3 . . ?
C22 C23 H23 129.4 . . ?
N31 C31 H31 119.4 . . ?
C32 C31 H31 132.0 . . ?
C31 C32 H32 118.8 . . ?
C33 C32 H32 136.3 . . ?
N32 C33 H33 119.6 . . ?
C32 C33 H33 129.4 . . ?
N41 C41 H41 119.5 . . ?
C42 C41 H41 129.2 . . ?
C43 C42 H42 136.9 . . ?
C41 C42 H42 119.1 . . ?
N42 C43 H43 119.1 . . ?
C42 C43 H43 131.2 . . ?
N51 C51 H51 119.0 . . ?
C52 C51 H51 130.3 . . ?
C53 C52 H52 134.6 . . ?
C51 C52 H52 120.1 . . ?
N52 C53 H53 119.1 . . ?
C52 C53 H53 132.2 . . ?
N61 C61 H61 119.3 . . ?
C62 C61 H61 130.0 . . ?
C63 C62 H62 134.7 . . ?
C61 C62 H62 120.0 . . ?
N62 C63 H63 119.2 . . ?
C62 C63 H63 132.4 . . ?
N31 B1 H1 111.7 . . ?
N21 B1 H1 109.0 . . ?
N11 B1 H1 112.5 . . ?
N42 B2 H2 112.0 . . ?
N52 B2 H2 109.2 . . ?
N62 B2 H2 112.3 . . ?

_diffrn_measured_fraction_theta_max 0.752
_diffrn_measured_fraction_theta_full 0.752
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.055

_publ_section_references         
;
Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K.
(1999). maXus Computer Program for the Solution and Refinement of
Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan
& The University of Glasgow.

Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot
Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.

Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276,
edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326,
New York:Academic Press.

Beurskens, P.T., Beurskens, G., Bosman, W.P., de Gelder, R.
S. Garc\'ia-Granda, S., Gould, R.O. & Smits, J.M.M. (1996).
The DIRDIF96 program system, Technical Report of the Crystallography
Laboratory, University of Nijmegen, The Netherlands.

Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal
Structures. University of G\"ottingen, Germany.

;

# Attachment 'Structure_420K.cif'

data_structure420k
_database_code_depnum_ccdc_archive 'CCDC 729353'

_chemical_compound_source        'Local laboratory'
_exptl_crystal_description       prismatic
_exptl_crystal_colour            'Violet '
_cell_measurement_temperature    420
_refine_ls_hydrogen_treatment    constr
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_F_000             992
_diffrn_measurement_device       KappaCCD
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16

loop_
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_wavelength_id  all

_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
?
;
_chemical_formula_weight         481.911
_diffrn_radiation_type           ' MoK\a'

loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z
'-X+ 1/2,+Y+ 1/2,-Z+ 1/2'
'+X+ 1/2,-Y+ 1/2,+Z+ 1/2'

_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_cell_setting           Monoclinic
_chemical_formula_moiety         'C18 H20 B2 Fe N12 '
_chemical_formula_sum            'C18 H20 B2 Fe N12 '
_chemical_name_systematic        
;
?
;
_cell_length_a                   9.8404(6)
_cell_length_b                   17.621(2)
_cell_length_c                   13.3148(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.068(7)
_cell_angle_gamma                90.00
_cell_volume                     2291.2(4)
_diffrn_reflns_number            13117
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.05
_diffrn_reflns_theta_full        26.00
_cell_measurement_reflns_used    13117
_cell_measurement_theta_min      4.05
_cell_measurement_theta_max      26.00
_diffrn_measurement_method       CCD
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_diffrn_reflns_av_R_equivalents  0.034
_computing_structure_solution    'DIRDIF (Buerskens et al., 1992)'
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
# Absorption correction

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

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'
B B 0.0013 0.0007 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_exptl_absorpt_coefficient_mu    0.691
_reflns_number_total             3411
_reflns_number_gt                1535
_reflns_threshold_expression     >2sigma(I)

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.
;

_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^)+(0.0229P)^2^+0.5126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3411
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.0866
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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 0.64455(6) 0.15082(3) 0.83722(4) 0.0533(3) Uani 1 1 d . . .
N11 N 0.5950(4) 0.3170(2) 0.8632(3) 0.0570(10) Uani 1 1 d . . .
N12 N 0.5612(4) 0.25791(19) 0.7991(3) 0.0619(10) Uani 1 1 d . . .
N21 N 0.6339(3) 0.24412(19) 1.0250(3) 0.0575(10) Uani 1 1 d . . .
N22 N 0.6033(3) 0.17372(19) 0.9850(2) 0.0621(10) Uani 1 1 d . . .
N31 N 0.8312(5) 0.2734(2) 0.9310(2) 0.0549(11) Uani 1 1 d . . .
N32 N 0.8307(5) 0.2076(2) 0.8774(2) 0.0567(11) Uani 1 1 d . . .
N41 N 0.4594(5) 0.0956(2) 0.7908(3) 0.0657(12) Uani 1 1 d . . .
N42 N 0.4606(6) 0.0305(2) 0.7359(3) 0.0579(11) Uani 1 1 d . . .
N51 N 0.6967(3) 0.1279(2) 0.6910(2) 0.0598(10) Uani 1 1 d . . .
N52 N 0.6687(3) 0.0577(2) 0.6511(3) 0.0598(10) Uani 1 1 d . . .
N61 N 0.7213(4) 0.0427(2) 0.8773(3) 0.0676(11) Uani 1 1 d . . .
N62 N 0.6909(4) -0.0158(2) 0.8110(3) 0.0607(10) Uani 1 1 d . . .
C11 C 0.5221(6) 0.3784(3) 0.8305(4) 0.0715(15) Uani 1 1 d . . .
C12 C 0.4385(5) 0.3599(3) 0.7444(5) 0.0902(17) Uani 1 1 d . . .
C13 C 0.4668(5) 0.2853(3) 0.7277(4) 0.0750(15) Uani 1 1 d . . .
C21 C 0.6044(4) 0.2466(3) 1.1203(3) 0.0645(13) Uani 1 1 d . . .
C22 C 0.5537(4) 0.1779(3) 1.1442(3) 0.0762(15) Uani 1 1 d . . .
C23 C 0.5551(4) 0.1343(2) 1.0592(4) 0.0708(13) Uani 1 1 d . . .
C31 C 0.9606(7) 0.2983(3) 0.9529(3) 0.0649(15) Uani 1 1 d . . .
C32 C 1.0457(6) 0.2485(4) 0.9126(4) 0.0792(16) Uani 1 1 d . . .
C33 C 0.9614(7) 0.1939(3) 0.8668(3) 0.0651(15) Uani 1 1 d . . .
C41 C 0.3295(8) 0.1074(3) 0.8039(4) 0.0853(18) Uani 1 1 d . . .
C42 C 0.2451(6) 0.0508(4) 0.7575(4) 0.0949(19) Uani 1 1 d . . .
C43 C 0.3316(8) 0.0042(3) 0.7167(3) 0.0714(16) Uani 1 1 d . . .
C51 C 0.7697(4) 0.1631(3) 0.6265(4) 0.0723(14) Uani 1 1 d . . .
C52 C 0.7878(5) 0.1164(4) 0.5461(4) 0.0895(17) Uani 1 1 d . . .
C53 C 0.7238(5) 0.0506(3) 0.5640(3) 0.0785(15) Uani 1 1 d . . .
C61 C 0.8051(5) 0.0132(4) 0.9536(4) 0.0862(16) Uani 1 1 d . . .
C62 C 0.8293(6) -0.0632(4) 0.9377(5) 0.102(2) Uani 1 1 d . . .
C63 C 0.7571(6) -0.0782(3) 0.8479(5) 0.0768(16) Uani 1 1 d . . .
B1 B 0.6942(7) 0.3041(3) 0.9598(4) 0.0587(16) Uani 1 1 d . . .
B2 B 0.5978(7) -0.0010(3) 0.7123(4) 0.0621(16) Uani 1 1 d . . .
H11 H 0.5326 0.4274 0.8670 0.086 Uiso 1 1 d R . .
H12 H 0.3768 0.3972 0.7096 0.108 Uiso 1 1 d R . .
H13 H 0.4301 0.2498 0.6742 0.090 Uiso 1 1 d R . .
H21 H 0.6200 0.2930 1.1619 0.077 Uiso 1 1 d R . .
H22 H 0.5255 0.1671 1.2113 0.091 Uiso 1 1 d R . .
H23 H 0.5285 0.0811 1.0438 0.085 Uiso 1 1 d R . .
H31 H 0.9821 0.3451 0.9925 0.078 Uiso 1 1 d R . .
H32 H 1.1420 0.2564 0.9204 0.095 Uiso 1 1 d R . .
H33 H 0.9796 0.1476 0.8288 0.078 Uiso 1 1 d R . .
H41 H 0.3094 0.1519 0.8447 0.102 Uiso 1 1 d R . .
H42 H 0.1504 0.0539 0.7651 0.114 Uiso 1 1 d R . .
H43 H 0.3127 -0.0429 0.6773 0.086 Uiso 1 1 d R . .
H51 H 0.7962 0.2160 0.6439 0.087 Uiso 1 1 d R . .
H52 H 0.8380 0.1373 0.4933 0.107 Uiso 1 1 d R . .
H53 H 0.7162 0.0031 0.5239 0.094 Uiso 1 1 d R . .
H61 H 0.8366 0.0483 1.0091 0.103 Uiso 1 1 d R . .
H62 H 0.8895 -0.0903 0.9890 0.123 Uiso 1 1 d R . .
H63 H 0.7480 -0.1268 0.8103 0.092 Uiso 1 1 d R . .
H1 H 0.7094 0.3507 1.0010 0.070 Uiso 1 1 d R . .
H2 H 0.5845 -0.0477 0.6710 0.074 Uiso 1 1 d 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 0.0596(6) 0.0491(4) 0.0512(4) -0.0069(3) 0.0063(3) -0.0003(4)
N11 0.061(3) 0.047(3) 0.064(3) 0.000(2) 0.009(2) 0.004(2)
N12 0.064(3) 0.062(3) 0.057(3) -0.012(2) -0.005(2) 0.004(2)
N21 0.068(3) 0.051(2) 0.056(3) -0.007(2) 0.017(2) -0.005(2)
N22 0.075(3) 0.049(2) 0.065(3) -0.004(2) 0.018(2) -0.008(2)
N31 0.058(4) 0.051(3) 0.055(2) -0.002(2) 0.003(3) -0.009(3)
N32 0.045(4) 0.061(3) 0.062(3) -0.008(2) 0.001(2) 0.003(2)
N41 0.064(4) 0.062(3) 0.075(3) -0.012(2) 0.020(3) 0.000(3)
N42 0.055(4) 0.054(3) 0.065(3) -0.010(2) 0.007(3) 0.000(3)
N51 0.062(3) 0.054(3) 0.063(3) 0.000(2) 0.009(2) -0.009(2)
N52 0.076(3) 0.058(3) 0.047(2) -0.001(2) 0.014(2) -0.001(2)
N61 0.072(3) 0.073(3) 0.055(3) -0.005(2) -0.003(2) 0.011(2)
N62 0.065(3) 0.055(3) 0.064(3) 0.006(2) 0.014(2) 0.012(2)
C11 0.071(5) 0.056(3) 0.091(4) 0.007(3) 0.023(3) 0.010(4)
C12 0.069(5) 0.087(5) 0.113(5) 0.031(4) 0.007(4) 0.029(4)
C13 0.063(5) 0.091(4) 0.066(4) 0.007(3) -0.012(3) 0.010(3)
C21 0.069(4) 0.070(4) 0.055(3) -0.013(3) 0.010(3) 0.003(3)
C22 0.088(4) 0.088(4) 0.057(3) -0.002(3) 0.026(3) -0.002(3)
C23 0.082(4) 0.061(3) 0.072(3) 0.001(3) 0.020(3) -0.008(3)
C31 0.057(5) 0.060(4) 0.072(4) 0.004(3) -0.010(4) -0.017(4)
C32 0.056(5) 0.089(4) 0.090(4) 0.008(3) -0.002(4) -0.011(4)
C33 0.057(5) 0.072(4) 0.066(3) -0.001(3) 0.005(3) 0.008(4)
C41 0.087(6) 0.068(4) 0.104(4) -0.008(3) 0.025(4) -0.006(4)
C42 0.060(6) 0.093(5) 0.136(5) 0.013(4) 0.028(4) 0.018(4)
C43 0.052(6) 0.073(4) 0.087(4) 0.000(3) -0.002(4) -0.019(4)
C51 0.060(4) 0.081(4) 0.076(4) 0.012(3) 0.008(3) -0.006(3)
C52 0.096(5) 0.104(5) 0.075(4) 0.023(4) 0.035(3) 0.012(4)
C53 0.105(5) 0.079(4) 0.053(3) 0.001(3) 0.019(3) 0.023(3)
C61 0.080(5) 0.110(5) 0.067(4) 0.010(4) 0.001(3) 0.012(4)
C62 0.096(6) 0.114(5) 0.095(5) 0.046(4) 0.002(4) 0.032(4)
C63 0.076(5) 0.059(4) 0.100(4) 0.025(3) 0.028(4) 0.022(3)
B1 0.075(6) 0.047(3) 0.054(4) -0.009(3) 0.009(4) -0.006(3)
B2 0.079(6) 0.044(3) 0.064(4) -0.011(3) 0.011(4) 0.001(4)

_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 N41 2.091(4) . ?
Fe1 N61 2.094(4) . ?
Fe1 N22 2.097(3) . ?
Fe1 N12 2.095(4) . ?
Fe1 N32 2.099(4) . ?
Fe1 N51 2.113(3) . ?
N11 C11 1.341(4) . ?
N11 N12 1.362(4) . ?
N11 B1 1.532(6) . ?
N12 C13 1.335(5) . ?
N21 C21 1.337(4) . ?
N21 N22 1.369(4) . ?
N21 B1 1.533(5) . ?
N22 C23 1.341(4) . ?
N31 C31 1.344(5) . ?
N31 N32 1.361(4) . ?
N31 B1 1.544(6) . ?
N32 C33 1.332(5) . ?
N41 C41 1.327(5) . ?
N41 N42 1.362(4) . ?
N42 C43 1.346(4) . ?
N42 B2 1.528(6) . ?
N51 C51 1.338(4) . ?
N51 N52 1.360(4) . ?
N52 C53 1.345(4) . ?
N52 B2 1.536(5) . ?
N61 C61 1.332(5) . ?
N61 N62 1.367(4) . ?
N62 C63 1.341(5) . ?
N62 B2 1.529(6) . ?
C11 C12 1.366(5) . ?
C12 C13 1.367(5) . ?
C21 C22 1.361(5) . ?
C22 C23 1.370(5) . ?
C31 C32 1.367(5) . ?
C32 C33 1.364(5) . ?
C41 C42 1.393(6) . ?
C42 C43 1.343(5) . ?
C51 C52 1.380(5) . ?
C52 C53 1.354(5) . ?
C61 C62 1.389(6) . ?
C62 C63 1.340(5) . ?
C11 H11 0.9896 . ?
C12 H12 0.9734 . ?
C13 H13 0.9829 . ?
C21 H21 0.9889 . ?
C22 H22 0.9854 . ?
C23 H23 0.9876 . ?
C31 H31 0.9879 . ?
C32 H32 0.9505 . ?
C33 H33 0.9887 . ?
C41 H41 0.9884 . ?
C42 H42 0.9521 . ?
C43 H43 0.9881 . ?
C51 H51 0.9875 . ?
C52 H52 0.9792 . ?
C53 H53 0.9898 . ?
C61 H61 0.9845 . ?
C62 H62 0.9731 . ?
C63 H63 0.9896 . ?
B1 H1 0.9887 . ?
B2 H2 0.9890 . ?

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
N41 Fe1 N61 85.76(16) . . ?
N41 Fe1 N22 95.98(15) . . ?
N61 Fe1 N22 92.36(14) . . ?
N41 Fe1 N12 92.64(16) . . ?
N61 Fe1 N12 177.94(14) . . ?
N22 Fe1 N12 86.50(13) . . ?
N41 Fe1 N32 177.59(13) . . ?
N61 Fe1 N32 95.32(16) . . ?
N22 Fe1 N32 86.14(14) . . ?
N12 Fe1 N32 86.32(16) . . ?
N41 Fe1 N51 86.59(15) . . ?
N61 Fe1 N51 86.57(14) . . ?
N22 Fe1 N51 177.14(13) . . ?
N12 Fe1 N51 94.64(13) . . ?
N32 Fe1 N51 91.32(15) . . ?
C11 N11 N12 109.5(4) . . ?
C11 N11 B1 130.7(5) . . ?
N12 N11 B1 119.6(4) . . ?
C13 N12 N11 105.4(4) . . ?
C13 N12 Fe1 135.7(4) . . ?
N11 N12 Fe1 118.6(3) . . ?
C21 N21 N22 109.6(3) . . ?
C21 N21 B1 131.3(4) . . ?
N22 N21 B1 119.1(4) . . ?
C23 N22 N21 105.3(3) . . ?
C23 N22 Fe1 135.9(3) . . ?
N21 N22 Fe1 118.7(3) . . ?
C31 N31 N32 109.5(4) . . ?
C31 N31 B1 131.7(5) . . ?
N32 N31 B1 118.8(5) . . ?
C33 N32 N31 105.6(4) . . ?
C33 N32 Fe1 135.2(4) . . ?
N31 N32 Fe1 119.1(4) . . ?
C41 N41 N42 105.9(4) . . ?
C41 N41 Fe1 135.0(4) . . ?
N42 N41 Fe1 119.1(4) . . ?
C43 N42 N41 108.8(4) . . ?
C43 N42 B2 132.3(5) . . ?
N41 N42 B2 118.8(5) . . ?
C51 N51 N52 105.7(4) . . ?
C51 N51 Fe1 135.5(4) . . ?
N52 N51 Fe1 118.2(3) . . ?
C53 N52 N51 109.7(4) . . ?
C53 N52 B2 130.7(4) . . ?
N51 N52 B2 119.2(4) . . ?
C61 N61 N62 105.3(4) . . ?
C61 N61 Fe1 136.0(4) . . ?
N62 N61 Fe1 118.6(3) . . ?
C63 N62 N61 108.9(4) . . ?
C63 N62 B2 131.9(5) . . ?
N61 N62 B2 119.2(4) . . ?
N11 C11 C12 108.8(5) . . ?
C11 C12 C13 104.7(5) . . ?
N12 C13 C12 111.7(5) . . ?
N21 C21 C22 108.7(4) . . ?
C21 C22 C23 105.3(4) . . ?
N22 C23 C22 111.0(4) . . ?
N31 C31 C32 108.4(5) . . ?
C33 C32 C31 105.0(6) . . ?
N32 C33 C32 111.5(5) . . ?
N41 C41 C42 111.2(5) . . ?
C43 C42 C41 104.1(6) . . ?
C42 C43 N42 110.0(5) . . ?
N51 C51 C52 110.6(4) . . ?
C53 C52 C51 105.5(4) . . ?
N52 C53 C52 108.5(4) . . ?
N61 C61 C62 111.4(5) . . ?
C63 C62 C61 104.2(5) . . ?
C62 C63 N62 110.2(5) . . ?
N21 B1 N11 109.1(4) . . ?
N21 B1 N31 108.1(4) . . ?
N11 B1 N31 109.2(4) . . ?
N42 B2 N62 109.6(4) . . ?
N42 B2 N52 109.6(4) . . ?
N62 B2 N52 107.9(4) . . ?
N11 C11 H11 121.6 . . ?
C12 C11 H11 129.6 . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 134.4 . . ?
N12 C13 H13 116.5 . . ?
C12 C13 H13 131.8 . . ?
N21 C21 H21 121.4 . . ?
C22 C21 H21 129.8 . . ?
C21 C22 H22 122.4 . . ?
C23 C22 H22 132.3 . . ?
N22 C23 H23 116.6 . . ?
C22 C23 H23 132.3 . . ?
N31 C31 H31 121.5 . . ?
C32 C31 H31 130.1 . . ?
C33 C32 H32 134.1 . . ?
C31 C32 H32 120.9 . . ?
N32 C33 H33 116.3 . . ?
C32 C33 H33 132.2 . . ?
N41 C41 H41 117.2 . . ?
C42 C41 H41 131.6 . . ?
C43 C42 H42 139.1 . . ?
C41 C42 H42 116.7 . . ?
C42 C43 H43 129.9 . . ?
N42 C43 H43 120.1 . . ?
N51 C51 H51 115.8 . . ?
C52 C51 H51 133.6 . . ?
C53 C52 H52 137.3 . . ?
C51 C52 H52 117.2 . . ?
N52 C53 H53 122.1 . . ?
C52 C53 H53 129.4 . . ?
N61 C61 H61 115.8 . . ?
C62 C61 H61 132.8 . . ?
C63 C62 H62 137.8 . . ?
C61 C62 H62 118.0 . . ?
C62 C63 H63 128.8 . . ?
N62 C63 H63 121.0 . . ?
N21 B1 H1 107.5 . . ?
N11 B1 H1 112.3 . . ?
N31 B1 H1 110.6 . . ?
N42 B2 H2 110.8 . . ?
N62 B2 H2 111.1 . . ?
N52 B2 H2 107.6 . . ?

_diffrn_measured_fraction_theta_max 0.757
_diffrn_measured_fraction_theta_full 0.757
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.048

_publ_section_references         
;
Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K.
(1999). maXus Computer Program for the Solution and Refinement of
Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan
& The University of Glasgow.

Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot
Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.

Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276,
edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326,
New York:Academic Press.

Beurskens, P.T., Beurskens, G., Bosman, W.P., de Gelder, R.
S. Garc\'ia-Granda, S., Gould, R.O. & Smits, J.M.M. (1996).
The DIRDIF96 program system, Technical Report of the Crystallography
Laboratory, University of Nijmegen, The Netherlands.

Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal
Structures. University of G\"ottingen, Germany.

;