# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H14 Br2 Fe K N6 O4'
_chemical_formula_weight         657.14

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.117(2)
_cell_length_b                   9.526(2)
_cell_length_c                   13.852(4)
_cell_angle_alpha                75.040(4)
_cell_angle_beta                 82.077(5)
_cell_angle_gamma                88.665(3)
_cell_volume                     1151.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1789
_cell_measurement_theta_min      2,345
_cell_measurement_theta_max      26.123

_exptl_crystal_description       block
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             646
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5252
_exptl_absorpt_correction_T_max  0.6234
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APEX II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5672
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3989
_reflns_number_gt                3129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0672P)²+2.3753P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3989
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Br1 Br 1.31694(7) 1.02521(8) 0.04651(5) 0.0467(2) Uani 1 1 d . . .
Br2 Br 1.07568(8) 1.29918(7) 0.04750(5) 0.0504(2) Uani 1 1 d . . .
Fe1 Fe 0.66027(9) 0.68107(9) 0.29058(6) 0.0297(2) Uani 1 1 d . . .
K1 K 1.43804(18) 1.33486(15) 0.11246(11) 0.0481(4) Uani 1 1 d . . .
O1 O 1.0656(5) 0.5329(5) 0.2215(4) 0.0529(12) Uani 1 1 d . . .
O2 O 0.5573(5) 1.1024(4) 0.2154(3) 0.0438(10) Uani 1 1 d . . .
O3 O 1.2615(6) 1.3166(6) 0.2918(3) 0.0578(13) Uani 1 1 d . . .
H1O3 H 1.2302 1.4013 0.2670 0.069 Uiso 1 1 d R . .
H2O3 H 1.2620 1.3068 0.3545 0.069 Uiso 1 1 d R . .
O4 O 1.7167(9) 1.3957(10) -0.0192(7) 0.136(3) Uani 1 1 d . . .
H1O4 H 1.8077 1.3864 -0.0115 0.164 Uiso 1 1 d R . .
H2O4 H 1.7117 1.4176 -0.0821 0.164 Uiso 1 1 d R . .
N1 N 0.7516(7) 0.7225(7) 0.4901(4) 0.0584(16) Uani 1 1 d . . .
N2 N 0.5434(8) 0.6166(7) 0.1055(5) 0.0638(18) Uani 1 1 d . . .
N3 N 0.8622(5) 0.6777(5) 0.2369(3) 0.0312(10) Uani 1 1 d . . .
N4 N 0.6806(5) 0.8844(5) 0.2347(3) 0.0317(11) Uani 1 1 d . . .
N5 N 0.6928(5) 0.4655(5) 0.3352(3) 0.0332(11) Uani 1 1 d . . .
N6 N 0.4506(5) 0.7344(5) 0.3312(3) 0.0338(11) Uani 1 1 d . . .
C1 C 0.7148(6) 0.7033(6) 0.4192(5) 0.0365(14) Uani 1 1 d . . .
C2 C 0.5868(7) 0.6423(6) 0.1724(5) 0.0384(14) Uani 1 1 d . . .
C3 C 0.9253(6) 0.8164(6) 0.1900(4) 0.0315(12) Uani 1 1 d . . .
C4 C 0.8234(6) 0.9297(6) 0.1890(4) 0.0296(12) Uani 1 1 d . . .
C5 C 0.8703(6) 1.0744(6) 0.1453(4) 0.0329(13) Uani 1 1 d . . .
H3 H 0.8040 1.1504 0.1438 0.040 Uiso 1 1 calc R . .
C6 C 1.0177(6) 1.1014(6) 0.1044(4) 0.0345(13) Uani 1 1 d . . .
C7 C 1.1161(6) 0.9898(6) 0.1042(4) 0.0329(13) Uani 1 1 d . . .
C8 C 1.0714(6) 0.8470(6) 0.1467(4) 0.0336(13) Uani 1 1 d . . .
H6 H 1.1386 0.7721 0.1463 0.040 Uiso 1 1 calc R . .
C9 C 0.4303(6) 0.8804(7) 0.3033(4) 0.0334(13) Uani 1 1 d . . .
C10 C 0.2952(7) 0.9444(8) 0.3232(5) 0.0435(15) Uani 1 1 d . . .
H8 H 0.2861 1.0450 0.3050 0.052 Uiso 1 1 calc R . .
C11 C 0.1741(7) 0.8558(8) 0.3706(5) 0.0466(16) Uani 1 1 d . . .
H9 H 0.0819 0.8960 0.3839 0.056 Uiso 1 1 calc R . .
C12 C 0.1920(7) 0.7076(8) 0.3978(5) 0.0478(17) Uani 1 1 d . . .
H10 H 0.1124 0.6460 0.4298 0.057 Uiso 1 1 calc R . .
C13 C 0.3310(7) 0.6522(7) 0.3765(4) 0.0424(15) Uani 1 1 d . . .
H11 H 0.3420 0.5519 0.3948 0.051 Uiso 1 1 calc R . .
C14 C 0.5633(6) 0.9707(6) 0.2462(4) 0.0321(13) Uani 1 1 d . . .
C15 C 0.9351(7) 0.5525(6) 0.2487(4) 0.0365(14) Uani 1 1 d . . .
C16 C 0.8308(7) 0.4277(6) 0.3050(4) 0.0358(13) Uani 1 1 d . . .
C17 C 0.8741(8) 0.2857(7) 0.3234(5) 0.0476(16) Uani 1 1 d . . .
H14 H 0.9709 0.2629 0.3022 0.057 Uiso 1 1 calc R . .
C18 C 0.7731(8) 0.1767(7) 0.3737(5) 0.0466(16) Uani 1 1 d . . .
H15 H 0.8003 0.0796 0.3860 0.056 Uiso 1 1 calc R . .
C19 C 0.6342(8) 0.2137(7) 0.4045(5) 0.0489(17) Uani 1 1 d . . .
H16 H 0.5646 0.1419 0.4387 0.059 Uiso 1 1 calc R . .
C20 C 0.5955(8) 0.3590(7) 0.3851(5) 0.0447(16) Uani 1 1 d . . .
H17 H 0.4997 0.3833 0.4072 0.054 Uiso 1 1 calc R . .


_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
Br1 C7 1.895(5) . ?
Br2 C6 1.901(6) . ?
Fe1 N3 1.891(5) . ?
Fe1 N4 1.894(5) . ?
Fe1 C2 1.972(7) . ?
Fe1 C1 1.978(7) . ?
Fe1 N6 2.008(5) . ?
Fe1 N5 2.013(5) . ?
K1 O2 2.608(4) 1_655 ?
K1 O3 2.735(5) . ?
K1 N2 2.845(7) 1_665 ?
K1 O4 2.892(9) . ?
K1 N2 2.916(6) 2_775 ?
K1 O4 2.979(9) 2_885 ?
K1 K1 3.875(3) 2_885 ?
K1 H1O3 2.8455 . ?
O1 C15 1.223(7) . ?
O2 C14 1.219(7) . ?
O2 K1 2.608(4) 1_455 ?
O3 H1O3 0.8500 . ?
O3 H2O3 0.8500 . ?
O4 K1 2.979(9) 2_885 ?
O4 H1O4 0.8500 . ?
O4 H2O4 0.8500 . ?
N1 C1 1.139(8) . ?
N2 C2 1.139(8) . ?
N2 K1 2.845(7) 1_445 ?
N2 K1 2.916(6) 2_775 ?
N3 C15 1.335(8) . ?
N3 C3 1.410(7) . ?
N4 C14 1.352(7) . ?
N4 C4 1.392(7) . ?
N5 C16 1.342(8) . ?
N5 C20 1.343(8) . ?
N6 C13 1.339(7) . ?
N6 C9 1.359(8) . ?
C3 C8 1.388(8) . ?
C3 C4 1.406(8) . ?
C4 C5 1.406(8) . ?
C5 C6 1.387(8) . ?
C5 H3 0.9300 . ?
C6 C7 1.375(9) . ?
C7 C8 1.381(8) . ?
C8 H6 0.9300 . ?
C9 C10 1.387(9) . ?
C9 C14 1.506(8) . ?
C10 C11 1.386(9) . ?
C10 H8 0.9300 . ?
C11 C12 1.376(10) . ?
C11 H9 0.9300 . ?
C12 C13 1.385(9) . ?
C12 H10 0.9300 . ?
C13 H11 0.9300 . ?
C15 C16 1.515(8) . ?
C16 C17 1.369(9) . ?
C17 C18 1.381(9) . ?
C17 H14 0.9300 . ?
C18 C19 1.348(10) . ?
C18 H15 0.9300 . ?
C19 C20 1.387(9) . ?
C19 H16 0.9300 . ?
C20 H17 0.9300 . ?

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
N3 Fe1 N4 84.3(2) . . ?
N3 Fe1 C2 94.3(2) . . ?
N4 Fe1 C2 94.9(2) . . ?
N3 Fe1 C1 91.0(2) . . ?
N4 Fe1 C1 90.2(2) . . ?
C2 Fe1 C1 173.0(2) . . ?
N3 Fe1 N6 166.6(2) . . ?
N4 Fe1 N6 82.34(19) . . ?
C2 Fe1 N6 85.8(2) . . ?
C1 Fe1 N6 90.1(2) . . ?
N3 Fe1 N5 81.3(2) . . ?
N4 Fe1 N5 165.5(2) . . ?
C2 Fe1 N5 86.2(2) . . ?
C1 Fe1 N5 90.1(2) . . ?
N6 Fe1 N5 112.14(19) . . ?
O2 K1 O3 83.35(14) 1_655 . ?
O2 K1 N2 120.80(18) 1_655 1_665 ?
O3 K1 N2 92.06(18) . 1_665 ?
O2 K1 O4 88.1(2) 1_655 . ?
O3 K1 O4 152.6(2) . . ?
N2 K1 O4 70.2(2) 1_665 . ?
O2 K1 N2 118.81(18) 1_655 2_775 ?
O3 K1 N2 147.31(19) . 2_775 ?
N2 K1 N2 95.47(18) 1_665 2_775 ?
O4 K1 N2 58.0(2) . 2_775 ?
O2 K1 O4 173.0(2) 1_655 2_885 ?
O3 K1 O4 89.8(2) . 2_885 ?
N2 K1 O4 57.8(2) 1_665 2_885 ?
O4 K1 O4 97.4(2) . 2_885 ?
N2 K1 O4 68.0(2) 2_775 2_885 ?
O2 K1 K1 137.61(12) 1_655 2_885 ?
O3 K1 K1 131.28(13) . 2_885 ?
N2 K1 K1 48.50(13) 1_665 2_885 ?
O4 K1 K1 49.66(17) . 2_885 ?
N2 K1 K1 46.97(13) 2_775 2_885 ?
O4 K1 K1 47.73(17) 2_885 2_885 ?
O2 K1 H1O3 100.4 1_655 . ?
O3 K1 H1O3 17.4 . . ?
N2 K1 H1O3 80.5 1_665 . ?
O4 K1 H1O3 149.5 . . ?
N2 K1 H1O3 135.4 2_775 . ?
O4 K1 H1O3 72.7 2_885 . ?
K1 K1 H1O3 114.5 2_885 . ?
C14 O2 K1 151.0(4) . 1_455 ?
K1 O3 H1O3 88.7 . . ?
K1 O3 H2O3 144.0 . . ?
H1O3 O3 H2O3 107.7 . . ?
K1 O4 K1 82.6(2) . 2_885 ?
K1 O4 H1O4 135.5 . . ?
K1 O4 H1O4 127.8 2_885 . ?
K1 O4 H2O4 116.2 . . ?
K1 O4 H2O4 60.4 2_885 . ?
H1O4 O4 H2O4 107.7 . . ?
C2 N2 K1 122.3(5) . 1_445 ?
C2 N2 K1 148.6(5) . 2_775 ?
K1 N2 K1 84.53(18) 1_445 2_775 ?
C15 N3 C3 125.3(5) . . ?
C15 N3 Fe1 120.7(4) . . ?
C3 N3 Fe1 114.0(4) . . ?
C14 N4 C4 126.5(5) . . ?
C14 N4 Fe1 119.5(4) . . ?
C4 N4 Fe1 114.0(4) . . ?
C16 N5 C20 117.9(5) . . ?
C16 N5 Fe1 112.8(4) . . ?
C20 N5 Fe1 129.2(4) . . ?
C13 N6 C9 116.7(5) . . ?
C13 N6 Fe1 131.4(4) . . ?
C9 N6 Fe1 111.9(4) . . ?
N1 C1 Fe1 176.0(5) . . ?
N2 C2 Fe1 178.4(6) . . ?
C8 C3 C4 120.2(5) . . ?
C8 C3 N3 126.5(5) . . ?
C4 C3 N3 113.3(5) . . ?
N4 C4 C3 114.4(5) . . ?
N4 C4 C5 125.7(5) . . ?
C3 C4 C5 119.8(5) . . ?
C6 C5 C4 118.5(5) . . ?
C6 C5 H3 120.7 . . ?
C4 C5 H3 120.7 . . ?
C7 C6 C5 121.3(5) . . ?
C7 C6 Br2 122.0(4) . . ?
C5 C6 Br2 116.8(4) . . ?
C6 C7 C8 120.8(5) . . ?
C6 C7 Br1 121.6(4) . . ?
C8 C7 Br1 117.6(4) . . ?
C7 C8 C3 119.4(6) . . ?
C7 C8 H6 120.3 . . ?
C3 C8 H6 120.3 . . ?
N6 C9 C10 122.9(5) . . ?
N6 C9 C14 116.1(5) . . ?
C10 C9 C14 121.0(6) . . ?
C11 C10 C9 118.8(6) . . ?
C11 C10 H8 120.6 . . ?
C9 C10 H8 120.6 . . ?
C12 C11 C10 119.1(6) . . ?
C12 C11 H9 120.4 . . ?
C10 C11 H9 120.4 . . ?
C11 C12 C13 118.6(6) . . ?
C11 C12 H10 120.7 . . ?
C13 C12 H10 120.7 . . ?
N6 C13 C12 123.9(6) . . ?
N6 C13 H11 118.0 . . ?
C12 C13 H11 118.0 . . ?
O2 C14 N4 127.9(5) . . ?
O2 C14 C9 121.9(5) . . ?
N4 C14 C9 110.2(5) . . ?
O1 C15 N3 128.4(6) . . ?
O1 C15 C16 121.8(5) . . ?
N3 C15 C16 109.7(5) . . ?
N5 C16 C17 122.2(6) . . ?
N5 C16 C15 115.5(5) . . ?
C17 C16 C15 122.3(6) . . ?
C16 C17 C18 119.6(6) . . ?
C16 C17 H14 120.2 . . ?
C18 C17 H14 120.2 . . ?
C19 C18 C17 118.7(6) . . ?
C19 C18 H15 120.7 . . ?
C17 C18 H15 120.7 . . ?
C18 C19 C20 119.8(6) . . ?
C18 C19 H16 120.1 . . ?
C20 C19 H16 120.1 . . ?
N5 C20 C19 121.8(6) . . ?
N5 C20 H17 119.1 . . ?
C19 C20 H17 119.1 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.117
_database_code_depnum_ccdc_archive 'CCDC 1000032'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H14 Br2 Fe N5 O3'
_chemical_formula_weight         588.03

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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.253(2)
_cell_length_b                   10.435(3)
_cell_length_c                   20.210(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2162.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1289
_cell_measurement_theta_min      2.490
_cell_measurement_theta_max      25.112

_exptl_crystal_description       block
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    4.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_T_max  0.5969
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APEX II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10469
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_sigmaI/netI    0.1010
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3805
_reflns_number_gt                2625
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0982P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_number_reflns         3805
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.1847
_refine_ls_wR_factor_gt          0.1620
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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 0.52070(11) 0.23962(11) 0.25309(7) 0.0320(3) Uani 1 1 d . . .
Br1 Br 1.13967(11) 0.49411(12) 0.29573(8) 0.0777(5) Uani 1 1 d . . .
Br2 Br 1.00983(13) 0.49455(15) 0.45023(8) 0.0882(5) Uani 1 1 d . . .
O1 O 0.8145(7) 0.3154(8) 0.1271(4) 0.060(2) Uani 1 1 d . . .
O2 O 0.5439(9) 0.3230(9) 0.4471(4) 0.076(3) Uani 1 1 d . . .
O3 O 0.759(3) 1.016(3) 0.4135(14) 0.266(12) Uani 1 1 d . . .
H3 H 0.6896 0.9806 0.4216 0.399 Uiso 1 1 calc R . .
N1 N 0.5474(9) -0.0658(10) 0.2630(4) 0.060(3) Uani 1 1 d . . .
N2 N 0.5934(7) 0.2848(7) 0.3365(4) 0.0316(18) Uani 1 1 d . . .
N3 N 0.6907(7) 0.2839(7) 0.2220(4) 0.0344(18) Uani 1 1 d . . .
N4 N 0.3613(7) 0.2092(7) 0.3107(4) 0.0325(18) Uani 1 1 d . . .
N5 N 0.4917(7) 0.2054(6) 0.1557(4) 0.0322(18) Uani 1 1 d . . .
C1 C 0.5490(9) 0.0387(9) 0.2599(5) 0.040(2) Uani 1 1 d . . .
C2 C 0.7227(9) 0.3351(8) 0.3336(5) 0.038(2) Uani 1 1 d . . .
C3 C 0.7733(8) 0.3324(8) 0.2711(5) 0.036(2) Uani 1 1 d . . .
C4 C 0.9031(8) 0.3769(8) 0.2617(5) 0.039(2) Uani 1 1 d . . .
H4 H 0.9417 0.3725 0.2201 0.047 Uiso 1 1 calc R . .
C5 C 0.9711(10) 0.4266(9) 0.3145(7) 0.061(3) Uani 1 1 d . . .
C6 C 0.9158(10) 0.4281(10) 0.3749(6) 0.048(3) Uani 1 1 d . . .
C7 C 0.7937(9) 0.3796(9) 0.3865(6) 0.049(3) Uani 1 1 d . . .
H7 H 0.7598 0.3768 0.4292 0.058 Uiso 1 1 calc R . .
C8 C 0.5164(10) 0.2857(10) 0.3901(5) 0.044(3) Uani 1 1 d . . .
C9 C 0.3800(9) 0.2366(9) 0.3758(5) 0.039(2) Uani 1 1 d . . .
C10 C 0.2904(12) 0.2257(11) 0.4225(6) 0.057(3) Uani 1 1 d . . .
H10 H 0.3073 0.2490 0.4661 0.069 Uiso 1 1 calc R . .
C11 C 0.1660(11) 0.1763(11) 0.4029(7) 0.061(3) Uani 1 1 d . . .
H11 H 0.1006 0.1636 0.4341 0.074 Uiso 1 1 calc R . .
C12 C 0.1450(11) 0.1483(9) 0.3390(6) 0.049(3) Uani 1 1 d . . .
H12 H 0.0644 0.1168 0.3255 0.059 Uiso 1 1 calc R . .
C13 C 0.2395(9) 0.1658(9) 0.2949(6) 0.043(2) Uani 1 1 d . . .
H13 H 0.2217 0.1474 0.2508 0.052 Uiso 1 1 calc R . .
C14 C 0.7140(10) 0.2813(9) 0.1562(5) 0.037(2) Uani 1 1 d . . .
C15 C 0.5983(9) 0.2314(9) 0.1205(5) 0.037(2) Uani 1 1 d . . .
C16 C 0.6014(12) 0.2110(11) 0.0530(6) 0.055(3) Uani 1 1 d . . .
H16 H 0.6779 0.2258 0.0294 0.066 Uiso 1 1 calc R . .
C17 C 0.4922(15) 0.1691(12) 0.0207(6) 0.073(4) Uani 1 1 d . . .
H17 H 0.4919 0.1604 -0.0251 0.087 Uiso 1 1 calc R . .
C18 C 0.3834(12) 0.1404(10) 0.0570(5) 0.054(3) Uani 1 1 d . . .
H18 H 0.3095 0.1077 0.0363 0.065 Uiso 1 1 calc R . .
C19 C 0.3838(10) 0.1604(10) 0.1252(6) 0.047(3) Uani 1 1 d . . .
H19 H 0.3094 0.1425 0.1498 0.056 Uiso 1 1 calc R . .
C20 C 0.842(2) 0.929(6) 0.3746(11) 0.39(4) Uani 1 1 d . . .
H20A H 0.8138 0.9302 0.3292 0.586 Uiso 1 1 calc R . .
H20B H 0.8338 0.8435 0.3917 0.586 Uiso 1 1 calc R . .
H20C H 0.9308 0.9563 0.3774 0.586 Uiso 1 1 calc R . .


_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 N2 1.902(8) . ?
Fe1 N3 1.910(7) . ?
Fe1 N5 2.022(8) . ?
Fe1 N4 2.032(7) . ?
Fe1 C1 2.121(10) . ?
Fe1 N1 2.171(11) 3_655 ?
Br1 C5 1.905(11) . ?
Br2 C6 1.931(11) . ?
O1 C14 1.237(11) . ?
O2 C8 1.249(12) . ?
O3 C20 1.47(5) . ?
O3 H3 0.8200 . ?
N1 C1 1.093(12) . ?
N1 Fe1 2.171(11) 3_645 ?
N2 C8 1.340(13) . ?
N2 C2 1.427(12) . ?
N3 C14 1.352(12) . ?
N3 C3 1.400(11) . ?
N4 C9 1.360(12) . ?
N4 C13 1.367(11) . ?
N5 C15 1.332(12) . ?
N5 C19 1.351(12) . ?
C2 C3 1.365(14) . ?
C2 C7 1.375(13) . ?
C3 C4 1.422(12) . ?
C4 C5 1.376(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.345(16) . ?
C6 C7 1.370(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.518(13) . ?
C9 C10 1.322(14) . ?
C10 C11 1.431(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.343(16) . ?
C11 H11 0.9300 . ?
C12 C13 1.328(14) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.483(14) . ?
C15 C16 1.382(14) . ?
C16 C17 1.367(16) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(16) . ?
C17 H17 0.9300 . ?
C18 C19 1.393(15) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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
N2 Fe1 N3 82.8(3) . . ?
N2 Fe1 N5 164.5(3) . . ?
N3 Fe1 N5 81.8(3) . . ?
N2 Fe1 N4 81.1(3) . . ?
N3 Fe1 N4 163.9(3) . . ?
N5 Fe1 N4 114.3(3) . . ?
N2 Fe1 C1 97.7(4) . . ?
N3 Fe1 C1 97.8(3) . . ?
N5 Fe1 C1 84.8(3) . . ?
N4 Fe1 C1 85.3(3) . . ?
N2 Fe1 N1 91.5(3) . 3_655 ?
N3 Fe1 N1 91.0(3) . 3_655 ?
N5 Fe1 N1 88.4(3) . 3_655 ?
N4 Fe1 N1 88.5(3) . 3_655 ?
C1 Fe1 N1 168.0(4) . 3_655 ?
C20 O3 H3 109.5 . . ?
C1 N1 Fe1 158.4(10) . 3_645 ?
C8 N2 C2 125.3(8) . . ?
C8 N2 Fe1 119.1(6) . . ?
C2 N2 Fe1 114.8(6) . . ?
C14 N3 C3 126.8(8) . . ?
C14 N3 Fe1 118.7(6) . . ?
C3 N3 Fe1 113.9(6) . . ?
C9 N4 C13 115.1(8) . . ?
C9 N4 Fe1 114.1(6) . . ?
C13 N4 Fe1 130.8(7) . . ?
C15 N5 C19 119.9(8) . . ?
C15 N5 Fe1 111.3(6) . . ?
C19 N5 Fe1 128.8(7) . . ?
N1 C1 Fe1 171.2(10) . . ?
C3 C2 C7 121.7(9) . . ?
C3 C2 N2 112.5(8) . . ?
C7 C2 N2 125.8(10) . . ?
C2 C3 N3 115.7(8) . . ?
C2 C3 C4 118.2(9) . . ?
N3 C3 C4 126.0(9) . . ?
C5 C4 C3 119.5(10) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 119.6(10) . . ?
C6 C5 Br1 123.9(9) . . ?
C4 C5 Br1 116.4(10) . . ?
C5 C6 C7 122.4(11) . . ?
C5 C6 Br2 120.6(8) . . ?
C7 C6 Br2 116.9(10) . . ?
C6 C7 C2 118.4(11) . . ?
C6 C7 H7 120.8 . . ?
C2 C7 H7 120.8 . . ?
O2 C8 N2 128.0(10) . . ?
O2 C8 C9 119.2(10) . . ?
N2 C8 C9 112.8(8) . . ?
C10 C9 N4 125.1(9) . . ?
C10 C9 C8 122.3(10) . . ?
N4 C9 C8 112.6(8) . . ?
C9 C10 C11 116.9(10) . . ?
C9 C10 H10 121.6 . . ?
C11 C10 H10 121.6 . . ?
C12 C11 C10 119.2(10) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C13 C12 C11 119.9(11) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 N4 123.8(10) . . ?
C12 C13 H13 118.1 . . ?
N4 C13 H13 118.1 . . ?
O1 C14 N3 127.5(10) . . ?
O1 C14 C15 122.4(9) . . ?
N3 C14 C15 110.1(8) . . ?
N5 C15 C16 121.0(9) . . ?
N5 C15 C14 118.0(8) . . ?
C16 C15 C14 121.1(9) . . ?
C17 C16 C15 120.1(11) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 118.8(10) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C17 C18 C19 119.6(10) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
N5 C19 C18 120.4(10) . . ?
N5 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.153
_database_code_depnum_ccdc_archive 'CCDC 1000033'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H27 Br4 Fe Mn N8 O6'
_chemical_formula_weight         1110.06

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.512(2)
_cell_length_b                   11.550(3)
_cell_length_c                   18.177(4)
_cell_angle_alpha                105.308(3)
_cell_angle_beta                 102.816(4)
_cell_angle_gamma                101.004(3)
_cell_volume                     2001.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1879
_cell_measurement_theta_min      2.590
_cell_measurement_theta_max      26.123

_exptl_crystal_description       block
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    4.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2414
_exptl_absorpt_correction_T_max  0.3845
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APEX II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10038
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.01
_reflns_number_total             7008
_reflns_number_gt                5451
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0702P)²+5.0453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7008
_refine_ls_number_parameters     525
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1383
_refine_ls_wR_factor_gt          0.1265
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT234_tnMn                
;
PROBLEM: Large Hirshfeld Difference C36    --  C37'    ..       0.28 Ang.  
RESPONSE: This may be caused by the disordered C37 and C37'.
;
_vrf_PLAT306_tnMn                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check 
RESPONSE: The electronic density around the O atoms of the solvent molecules 
is somewhat weak, making it 
impossible to accurately define the position of the 
hydrogen atoms bonded to the O atoms.
;
# end Validation Reply Form

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
N2 N -0.0182(5) 0.6934(4) 0.2958(3) 0.0350(11) Uani 1 1 d . . .
Fe1 Fe 0.26847(7) 0.74946(7) 0.27075(4) 0.02356(18) Uani 1 1 d . . .
Mn1 Mn 0.78570(8) 0.76049(7) 0.30050(4) 0.02429(19) Uani 1 1 d . . .
Br1 Br 0.08777(8) 0.58862(7) -0.14061(4) 0.0534(2) Uani 1 1 d . . .
Br2 Br 0.03694(11) 0.87191(8) -0.08206(4) 0.0754(3) Uani 1 1 d . . .
Br3 Br 0.58095(7) 0.12410(6) 0.32248(5) 0.0565(2) Uani 1 1 d . . .
Br4 Br 1.01106(6) 1.43588(5) 0.36659(4) 0.04168(18) Uani 1 1 d . . .
O1 O 0.8803(4) 0.9118(3) 0.3812(2) 0.0296(8) Uani 1 1 d . . .
O2 O 0.7481(4) 0.6741(3) 0.3713(2) 0.0321(9) Uani 1 1 d . . .
O3 O 0.1774(5) 1.0521(4) 0.2262(2) 0.0501(12) Uani 1 1 d . . .
O4 O 0.2358(6) 0.4373(4) 0.0974(3) 0.0617(14) Uani 1 1 d . . .
O5 O 0.376(2) 0.235(2) 0.0645(9) 0.344(13) Uani 1 1 d . . .
O6 O 0.504(3) 0.958(3) 0.0948(15) 0.400(14) Uani 1 1 d . . .
N1 N 0.5798(5) 0.8174(5) 0.2902(3) 0.0364(11) Uani 1 1 d . . .
N3 N 0.2308(4) 0.6356(4) 0.1672(3) 0.0273(10) Uani 1 1 d . . .
N4 N 0.2171(4) 0.8575(4) 0.2138(2) 0.0268(10) Uani 1 1 d . . .
N5 N 0.3088(4) 0.6019(4) 0.3022(3) 0.0291(10) Uani 1 1 d . . .
N6 N 0.2930(4) 0.8997(4) 0.3644(2) 0.0266(10) Uani 1 1 d . . .
N7 N 0.6837(5) 0.6114(4) 0.2062(3) 0.0309(10) Uani 1 1 d . . .
N8 N 0.8161(5) 0.8337(4) 0.2159(3) 0.0321(10) Uani 1 1 d . . .
C1 C 0.4653(6) 0.7995(5) 0.2829(3) 0.0272(11) Uani 1 1 d . . .
C2 C 0.0862(6) 0.7041(5) 0.2848(3) 0.0287(12) Uani 1 1 d . . .
C3 C 0.1903(5) 0.6812(5) 0.1045(3) 0.0283(11) Uani 1 1 d . . .
C4 C 0.1802(6) 0.8046(5) 0.1305(3) 0.0316(12) Uani 1 1 d . . .
C5 C 0.1363(7) 0.8618(6) 0.0737(3) 0.0395(14) Uani 1 1 d . . .
H5 H 0.1278 0.9427 0.0898 0.047 Uiso 1 1 calc R . .
C6 C 0.1056(7) 0.7955(6) -0.0069(4) 0.0445(16) Uani 1 1 d . . .
C7 C 0.1207(6) 0.6754(6) -0.0315(3) 0.0371(14) Uani 1 1 d . . .
C8 C 0.1609(6) 0.6181(6) 0.0237(3) 0.0380(14) Uani 1 1 d . . .
H8 H 0.1685 0.5370 0.0069 0.046 Uiso 1 1 calc R . .
C9 C 0.2120(6) 0.9726(5) 0.2539(3) 0.0304(12) Uani 1 1 d . . .
C10 C 0.2539(5) 0.9930(5) 0.3416(3) 0.0291(12) Uani 1 1 d . . .
C11 C 0.2473(6) 1.0998(6) 0.3959(3) 0.0368(13) Uani 1 1 d . . .
H11 H 0.2181 1.1615 0.3783 0.044 Uiso 1 1 calc R . .
C12 C 0.2845(6) 1.1143(6) 0.4765(3) 0.0410(15) Uani 1 1 d . . .
H12 H 0.2809 1.1854 0.5138 0.049 Uiso 1 1 calc R . .
C13 C 0.3271(6) 1.0202(6) 0.4998(3) 0.0408(14) Uani 1 1 d . . .
H13 H 0.3549 1.0279 0.5536 0.049 Uiso 1 1 calc R . .
C14 C 0.3281(6) 0.9143(6) 0.4428(3) 0.0370(13) Uani 1 1 d . . .
H14 H 0.3541 0.8505 0.4592 0.044 Uiso 1 1 calc R . .
C15 C 0.2474(6) 0.5194(5) 0.1589(3) 0.0366(13) Uani 1 1 d . . .
C16 C 0.2856(6) 0.5005(5) 0.2385(3) 0.0327(12) Uani 1 1 d . . .
C17 C 0.2960(7) 0.3863(6) 0.2449(4) 0.0456(16) Uani 1 1 d . . .
H17 H 0.2742 0.3176 0.1995 0.055 Uiso 1 1 calc R . .
C18 C 0.3393(6) 0.3750(6) 0.3199(4) 0.0476(17) Uani 1 1 d . . .
H18 H 0.3470 0.2990 0.3261 0.057 Uiso 1 1 calc R . .
C19 C 0.3708(7) 0.4810(6) 0.3857(4) 0.0454(16) Uani 1 1 d . . .
H19 H 0.4029 0.4775 0.4368 0.054 Uiso 1 1 calc R . .
C20 C 0.3544(6) 0.5899(6) 0.3746(4) 0.0394(14) Uani 1 1 d . . .
H20 H 0.3757 0.6597 0.4193 0.047 Uiso 1 1 calc R . .
C21 C 0.6611(5) 0.4645(5) 0.2802(3) 0.0301(12) Uani 1 1 d . . .
C22 C 0.7103(5) 0.5534(5) 0.3575(3) 0.0285(12) Uani 1 1 d . . .
C23 C 0.7189(6) 0.5086(6) 0.4227(4) 0.0362(13) Uani 1 1 d . . .
H23 H 0.7500 0.5648 0.4741 0.043 Uiso 1 1 calc R . .
C24 C 0.6820(6) 0.3820(6) 0.4116(4) 0.0416(15) Uani 1 1 d . . .
H24 H 0.6898 0.3540 0.4555 0.050 Uiso 1 1 calc R . .
C25 C 0.6336(6) 0.2973(5) 0.3356(4) 0.0377(14) Uani 1 1 d . . .
C26 C 0.6226(6) 0.3365(5) 0.2703(4) 0.0370(13) Uani 1 1 d . . .
H26 H 0.5897 0.2786 0.2194 0.044 Uiso 1 1 calc R . .
C27 C 0.6454(6) 0.5005(5) 0.2082(3) 0.0337(13) Uani 1 1 d . . .
H27 H 0.6042 0.4375 0.1597 0.040 Uiso 1 1 calc R . .
C28 C 0.8979(5) 1.0482(5) 0.3018(3) 0.0303(12) Uani 1 1 d . . .
C29 C 0.9060(5) 1.0247(5) 0.3755(3) 0.0277(11) Uani 1 1 d . . .
C30 C 0.9462(6) 1.1277(5) 0.4452(3) 0.0322(12) Uani 1 1 d . . .
H30 H 0.9525 1.1142 0.4939 0.039 Uiso 1 1 calc R . .
C31 C 0.9765(5) 1.2475(5) 0.4432(3) 0.0326(12) Uani 1 1 d . . .
H31 H 1.0016 1.3142 0.4900 0.039 Uiso 1 1 calc R . .
C32 C 0.9695(6) 1.2689(5) 0.3699(4) 0.0329(13) Uani 1 1 d . . .
C33 C 0.9323(6) 1.1724(5) 0.3009(4) 0.0348(13) Uani 1 1 d . . .
H33 H 0.9295 1.1879 0.2530 0.042 Uiso 1 1 calc R . .
C34 C 0.8602(6) 0.9503(5) 0.2268(3) 0.0339(13) Uani 1 1 d . . .
H34 H 0.8685 0.9734 0.1825 0.041 Uiso 1 1 calc R . .
C35 C 0.6612(8) 0.6378(6) 0.1296(4) 0.056(2) Uani 1 1 d . . .
H35 H 0.6645 0.5620 0.0910 0.067 Uiso 1 1 calc R . .
C36 C 0.7868(8) 0.7364(6) 0.1366(4) 0.0499(17) Uani 1 1 d . . .
H36 H 0.8616 0.6969 0.1403 0.060 Uiso 1 1 calc R . .
C37' C 0.777(2) 0.775(2) 0.0706(12) 0.104(7) Uani 0.50 1 d P . .
H37A H 0.7186 0.8295 0.0706 0.156 Uiso 0.50 1 calc PR . .
H37B H 0.7413 0.7042 0.0233 0.156 Uiso 0.50 1 calc PR . .
H37C H 0.8656 0.8192 0.0720 0.156 Uiso 0.50 1 calc PR . .
C37 C 0.545(2) 0.655(2) 0.1003(12) 0.095(6) Uani 0.50 1 d P . .
H37D H 0.4913 0.5833 0.0563 0.142 Uiso 0.50 1 calc PR . .
H37E H 0.5585 0.7267 0.0823 0.142 Uiso 0.50 1 calc PR . .
H37F H 0.4989 0.6695 0.1406 0.142 Uiso 0.50 1 calc PR . .


_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
N2 C2 1.149(7) . ?
N2 Mn1 2.347(5) 1_455 ?
Fe1 N3 1.895(4) . ?
Fe1 N4 1.902(4) . ?
Fe1 C2 1.979(6) . ?
Fe1 C1 1.984(6) . ?
Fe1 N6 2.013(4) . ?
Fe1 N5 2.023(4) . ?
Mn1 O1 1.879(4) . ?
Mn1 O2 1.886(4) . ?
Mn1 N7 1.993(5) . ?
Mn1 N8 1.995(4) . ?
Mn1 N2 2.347(5) 1_655 ?
Mn1 N1 2.362(5) . ?
Br1 C7 1.889(6) . ?
Br2 C6 1.900(6) . ?
Br3 C25 1.905(6) . ?
Br4 C32 1.914(5) . ?
O1 C29 1.318(6) . ?
O2 C22 1.313(6) . ?
O3 C9 1.232(6) . ?
O4 C15 1.224(7) . ?
N1 C1 1.153(7) . ?
N3 C15 1.360(7) . ?
N3 C3 1.394(7) . ?
N4 C9 1.354(7) . ?
N4 C4 1.406(7) . ?
N5 C20 1.350(7) . ?
N5 C16 1.351(7) . ?
N6 C14 1.345(7) . ?
N6 C10 1.353(7) . ?
N7 C27 1.281(7) . ?
N7 C35 1.481(8) . ?
N8 C34 1.283(7) . ?
N8 C36 1.500(7) . ?
C3 C8 1.391(8) . ?
C3 C4 1.410(8) . ?
C4 C5 1.407(8) . ?
C5 C6 1.394(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.392(9) . ?
C7 C8 1.376(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.497(8) . ?
C10 C11 1.386(8) . ?
C11 C12 1.385(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.381(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.498(8) . ?
C16 C17 1.377(8) . ?
C17 C18 1.388(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.390(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.362(9) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C26 1.408(8) . ?
C21 C22 1.417(8) . ?
C21 C27 1.458(8) . ?
C22 C23 1.405(8) . ?
C23 C24 1.386(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.382(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.368(9) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C33 1.417(8) . ?
C28 C29 1.422(7) . ?
C28 C34 1.438(8) . ?
C29 C30 1.404(8) . ?
C30 C31 1.372(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.406(8) . ?
C31 H31 0.9300 . ?
C32 C33 1.359(8) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C37 1.30(2) . ?
C35 C36 1.527(10) . ?
C35 H35 0.9800 . ?
C36 C37' 1.38(2) . ?
C36 H36 0.9800 . ?
C37' H37A 0.9600 . ?
C37' H37B 0.9600 . ?
C37' H37C 0.9600 . ?
C37 H37D 0.9600 . ?
C37 H37E 0.9600 . ?
C37 H37F 0.9600 . ?

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
C2 N2 Mn1 151.6(4) . 1_455 ?
N3 Fe1 N4 83.24(18) . . ?
N3 Fe1 C2 97.7(2) . . ?
N4 Fe1 C2 91.8(2) . . ?
N3 Fe1 C1 92.9(2) . . ?
N4 Fe1 C1 97.2(2) . . ?
C2 Fe1 C1 166.9(2) . . ?
N3 Fe1 N6 164.85(18) . . ?
N4 Fe1 N6 81.62(18) . . ?
C2 Fe1 N6 82.5(2) . . ?
C1 Fe1 N6 89.37(19) . . ?
N3 Fe1 N5 81.70(18) . . ?
N4 Fe1 N5 164.90(18) . . ?
C2 Fe1 N5 89.2(2) . . ?
C1 Fe1 N5 84.64(19) . . ?
N6 Fe1 N5 113.43(18) . . ?
O1 Mn1 O2 94.69(16) . . ?
O1 Mn1 N7 173.38(17) . . ?
O2 Mn1 N7 91.63(17) . . ?
O1 Mn1 N8 91.70(17) . . ?
O2 Mn1 N8 173.59(18) . . ?
N7 Mn1 N8 82.01(18) . . ?
O1 Mn1 N2 93.68(17) . 1_655 ?
O2 Mn1 N2 92.21(17) . 1_655 ?
N7 Mn1 N2 88.02(18) . 1_655 ?
N8 Mn1 N2 86.79(18) . 1_655 ?
O1 Mn1 N1 91.33(17) . . ?
O2 Mn1 N1 90.97(17) . . ?
N7 Mn1 N1 86.60(18) . . ?
N8 Mn1 N1 89.46(18) . . ?
N2 Mn1 N1 173.82(17) 1_655 . ?
C29 O1 Mn1 128.3(3) . . ?
C22 O2 Mn1 128.6(3) . . ?
C1 N1 Mn1 154.6(4) . . ?
C15 N3 C3 125.0(5) . . ?
C15 N3 Fe1 119.4(4) . . ?
C3 N3 Fe1 115.6(3) . . ?
C9 N4 C4 125.7(4) . . ?
C9 N4 Fe1 119.8(3) . . ?
C4 N4 Fe1 114.4(3) . . ?
C20 N5 C16 116.7(5) . . ?
C20 N5 Fe1 130.9(4) . . ?
C16 N5 Fe1 112.4(3) . . ?
C14 N6 C10 117.7(5) . . ?
C14 N6 Fe1 129.8(4) . . ?
C10 N6 Fe1 112.1(3) . . ?
C27 N7 C35 121.0(5) . . ?
C27 N7 Mn1 125.3(4) . . ?
C35 N7 Mn1 113.6(4) . . ?
C34 N8 C36 122.3(5) . . ?
C34 N8 Mn1 125.1(4) . . ?
C36 N8 Mn1 112.6(4) . . ?
N1 C1 Fe1 173.5(5) . . ?
N2 C2 Fe1 171.5(5) . . ?
C8 C3 N3 126.8(5) . . ?
C8 C3 C4 120.3(5) . . ?
N3 C3 C4 112.9(5) . . ?
N4 C4 C5 126.8(5) . . ?
N4 C4 C3 113.8(5) . . ?
C5 C4 C3 119.4(5) . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C7 C6 C5 121.0(5) . . ?
C7 C6 Br2 121.1(4) . . ?
C5 C6 Br2 117.9(5) . . ?
C8 C7 C6 120.2(5) . . ?
C8 C7 Br1 118.8(4) . . ?
C6 C7 Br1 120.9(4) . . ?
C7 C8 C3 120.1(5) . . ?
C7 C8 H8 119.9 . . ?
C3 C8 H8 119.9 . . ?
O3 C9 N4 128.0(5) . . ?
O3 C9 C10 122.3(5) . . ?
N4 C9 C10 109.8(4) . . ?
N6 C10 C11 122.1(5) . . ?
N6 C10 C9 116.5(5) . . ?
C11 C10 C9 121.4(5) . . ?
C12 C11 C10 119.7(6) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 118.1(5) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C12 C13 C14 119.6(5) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
N6 C14 C13 122.8(6) . . ?
N6 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
O4 C15 N3 128.1(5) . . ?
O4 C15 C16 121.4(5) . . ?
N3 C15 C16 110.5(5) . . ?
N5 C16 C17 123.0(5) . . ?
N5 C16 C15 115.7(5) . . ?
C17 C16 C15 121.3(5) . . ?
C16 C17 C18 119.2(6) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 117.9(6) . . ?
C17 C18 H18 121.1 . . ?
C19 C18 H18 121.1 . . ?
C20 C19 C18 119.5(6) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
N5 C20 C19 123.5(6) . . ?
N5 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
C26 C21 C22 120.4(5) . . ?
C26 C21 C27 117.3(5) . . ?
C22 C21 C27 122.3(5) . . ?
O2 C22 C23 118.7(5) . . ?
O2 C22 C21 123.8(5) . . ?
C23 C22 C21 117.5(5) . . ?
C24 C23 C22 121.1(6) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C25 C24 C23 120.2(6) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 120.8(5) . . ?
C26 C25 Br3 120.0(5) . . ?
C24 C25 Br3 119.1(5) . . ?
C25 C26 C21 119.9(6) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
N7 C27 C21 125.5(5) . . ?
N7 C27 H27 117.3 . . ?
C21 C27 H27 117.3 . . ?
C33 C28 C29 119.7(5) . . ?
C33 C28 C34 117.4(5) . . ?
C29 C28 C34 122.8(5) . . ?
O1 C29 C30 118.9(5) . . ?
O1 C29 C28 123.1(5) . . ?
C30 C29 C28 117.9(5) . . ?
C31 C30 C29 121.7(5) . . ?
C31 C30 H30 119.1 . . ?
C29 C30 H30 119.1 . . ?
C30 C31 C32 119.6(5) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C33 C32 C31 120.9(5) . . ?
C33 C32 Br4 119.2(4) . . ?
C31 C32 Br4 119.9(4) . . ?
C32 C33 C28 120.2(5) . . ?
C32 C33 H33 119.9 . . ?
C28 C33 H33 119.9 . . ?
N8 C34 C28 125.6(5) . . ?
N8 C34 H34 117.2 . . ?
C28 C34 H34 117.2 . . ?
C37 C35 N7 117.5(11) . . ?
C37 C35 C36 116.7(11) . . ?
N7 C35 C36 106.9(5) . . ?
C37 C35 H35 104.8 . . ?
N7 C35 H35 104.8 . . ?
C36 C35 H35 104.8 . . ?
C37' C36 N8 117.8(10) . . ?
C37' C36 C35 113.4(10) . . ?
N8 C36 C35 105.6(5) . . ?
C37' C36 H36 106.4 . . ?
N8 C36 H36 106.4 . . ?
C35 C36 H36 106.4 . . ?
C36 C37' H37A 109.5 . . ?
C36 C37' H37B 109.5 . . ?
H37A C37' H37B 109.5 . . ?
C36 C37' H37C 109.5 . . ?
H37A C37' H37C 109.5 . . ?
H37B C37' H37C 109.5 . . ?
C35 C37 H37D 109.5 . . ?
C35 C37 H37E 109.5 . . ?
H37D C37 H37E 109.5 . . ?
C35 C37 H37F 109.5 . . ?
H37D C37 H37F 109.5 . . ?
H37E C37 H37F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.223
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.115
_database_code_depnum_ccdc_archive 'CCDC 1000034'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H27 Br2 Cl2 Fe Mn N9 O4'
_chemical_formula_weight         1027.21

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3171(7)
_cell_length_b                   11.5913(7)
_cell_length_c                   17.7730(16)
_cell_angle_alpha                102.5200(10)
_cell_angle_beta                 102.0700(10)
_cell_angle_gamma                104.9780(10)
_cell_volume                     1923.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1793
_cell_measurement_theta_min      2.832
_cell_measurement_theta_max      26.712

_exptl_crystal_description       block
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1022
_exptl_absorpt_coefficient_mu    2.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4492
_exptl_absorpt_correction_T_max  0.5351
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APEX II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9625
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.01
_reflns_number_total             6712
_reflns_number_gt                5398
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0506P)²+0.8598P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6712
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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 -0.00367(4) 0.47850(4) 0.22989(3) 0.02370(12) Uani 1 1 d . . .
Mn1 Mn 0.48752(4) 0.45909(4) 0.20928(3) 0.02330(12) Uani 1 1 d . . .
Br1 Br 0.25133(4) 0.75628(5) 0.63924(2) 0.05668(14) Uani 1 1 d . . .
Br2 Br 0.16158(6) 0.97773(5) 0.56585(3) 0.07860(18) Uani 1 1 d . . .
Cl1 Cl 0.26635(11) -0.19657(9) 0.17367(8) 0.0601(3) Uani 1 1 d . . .
Cl2 Cl 0.63403(11) 1.05229(9) 0.12703(8) 0.0588(3) Uani 1 1 d . . .
O1 O 0.1287(3) 0.3523(2) 0.41489(15) 0.0534(7) Uani 1 1 d . . .
O2 O -0.0338(3) 0.8227(2) 0.25913(15) 0.0476(7) Uani 1 1 d . . .
O3 O 0.3669(2) 0.30607(19) 0.13598(12) 0.0296(5) Uani 1 1 d . . .
O4 O 0.5117(2) 0.52800(19) 0.12462(12) 0.0288(5) Uani 1 1 d . . .
N1 N 0.3009(3) 0.5368(3) 0.21566(17) 0.0330(6) Uani 1 1 d . . .
N2 N -0.3239(3) 0.3876(3) 0.21101(17) 0.0343(6) Uani 1 1 d . . .
N3 N 0.4494(3) 0.3930(2) 0.30133(15) 0.0293(6) Uani 1 1 d . . .
N4 N 0.6252(3) 0.6163(2) 0.29028(15) 0.0289(6) Uani 1 1 d . . .
N5 N 0.0601(3) 0.4741(2) 0.33657(15) 0.0284(6) Uani 1 1 d . . .
N6 N 0.0075(3) 0.6437(2) 0.28051(15) 0.0271(6) Uani 1 1 d . . .
N7 N 0.0028(3) 0.3030(2) 0.20550(16) 0.0300(6) Uani 1 1 d . . .
N8 N -0.0731(3) 0.5273(2) 0.13068(15) 0.0279(6) Uani 1 1 d . . .
N9 N 0.5417(8) 0.8464(7) 0.5341(5) 0.138(2) Uani 1 1 d . . .
C1 C 0.1887(3) 0.5225(3) 0.21882(18) 0.0265(7) Uani 1 1 d . . .
C2 C -0.2061(3) 0.4125(3) 0.21902(18) 0.0268(7) Uani 1 1 d . . .
C3 C 0.4098(3) 0.2765(3) 0.2961(2) 0.0337(8) Uani 1 1 d . . .
H3 H 0.4047 0.2551 0.3432 0.040 Uiso 1 1 calc R . .
C4 C 0.3725(3) 0.1758(3) 0.2237(2) 0.0314(7) Uani 1 1 d . . .
C5 C 0.3462(3) 0.1951(3) 0.14728(19) 0.0278(7) Uani 1 1 d . . .
C6 C 0.2910(3) 0.0899(3) 0.0802(2) 0.0361(8) Uani 1 1 d . . .
H6 H 0.2698 0.1002 0.0291 0.043 Uiso 1 1 calc R . .
C7 C 0.2675(4) -0.0285(3) 0.0885(2) 0.0436(9) Uani 1 1 d . . .
H7 H 0.2322 -0.0971 0.0431 0.052 Uiso 1 1 calc R . .
C8 C 0.2962(4) -0.0462(3) 0.1641(2) 0.0406(9) Uani 1 1 d . . .
C9 C 0.3456(4) 0.0534(3) 0.2309(2) 0.0399(8) Uani 1 1 d . . .
H9 H 0.3617 0.0409 0.2816 0.048 Uiso 1 1 calc R . .
C10 C 0.6582(3) 0.7206(3) 0.2742(2) 0.0342(8) Uani 1 1 d . . .
H10 H 0.7212 0.7884 0.3155 0.041 Uiso 1 1 calc R . .
C11 C 0.6085(3) 0.7444(3) 0.1992(2) 0.0311(7) Uani 1 1 d . . .
C12 C 0.5400(3) 0.6470(3) 0.12695(19) 0.0290(7) Uani 1 1 d . . .
C13 C 0.5060(3) 0.6793(3) 0.0554(2) 0.0350(8) Uani 1 1 d . . .
H13 H 0.4643 0.6166 0.0070 0.042 Uiso 1 1 calc R . .
C14 C 0.5332(3) 0.8016(3) 0.0553(2) 0.0401(9) Uani 1 1 d . . .
H14 H 0.5071 0.8210 0.0075 0.048 Uiso 1 1 calc R . .
C15 C 0.5997(4) 0.8966(3) 0.1269(2) 0.0413(9) Uani 1 1 d . . .
C16 C 0.6398(4) 0.8700(3) 0.1974(2) 0.0405(8) Uani 1 1 d . . .
H16 H 0.6879 0.9343 0.2444 0.049 Uiso 1 1 calc R . .
C17 C 0.4624(4) 0.4839(4) 0.3763(2) 0.0467(9) Uani 1 1 d . . .
H17A H 0.4275 0.4393 0.4120 0.056 Uiso 1 1 calc R . .
H17B H 0.4036 0.5345 0.3645 0.056 Uiso 1 1 calc R . .
C18 C 0.6074(4) 0.5676(4) 0.4188(2) 0.0576(11) Uani 1 1 d . . .
H18A H 0.6523 0.5263 0.4532 0.069 Uiso 1 1 calc R . .
H18B H 0.6018 0.6423 0.4535 0.069 Uiso 1 1 calc R . .
C19 C 0.7000(4) 0.6069(4) 0.3683(2) 0.0435(9) Uani 1 1 d . . .
H19A H 0.7687 0.6873 0.3983 0.052 Uiso 1 1 calc R . .
H19B H 0.7500 0.5475 0.3583 0.052 Uiso 1 1 calc R . .
C20 C 0.0890(3) 0.5861(3) 0.39563(19) 0.0290(7) Uani 1 1 d . . .
C21 C 0.1439(4) 0.6101(4) 0.4780(2) 0.0385(8) Uani 1 1 d . . .
H21 H 0.1640 0.5478 0.4990 0.046 Uiso 1 1 calc R . .
C22 C 0.1683(4) 0.7268(4) 0.52823(19) 0.0391(8) Uani 1 1 d . . .
C23 C 0.1359(4) 0.8188(3) 0.4975(2) 0.0396(8) Uani 1 1 d . . .
C24 C 0.0809(3) 0.7980(3) 0.4164(2) 0.0365(8) Uani 1 1 d . . .
H24 H 0.0587 0.8607 0.3968 0.044 Uiso 1 1 calc R . .
C25 C 0.0589(3) 0.6816(3) 0.36415(19) 0.0292(7) Uani 1 1 d . . .
C26 C 0.0812(3) 0.3688(3) 0.3504(2) 0.0336(8) Uani 1 1 d . . .
C27 C 0.0406(3) 0.2688(3) 0.2732(2) 0.0322(7) Uani 1 1 d . . .
C28 C 0.0452(4) 0.1504(3) 0.2703(3) 0.0441(9) Uani 1 1 d . . .
H28 H 0.0685 0.1286 0.3175 0.053 Uiso 1 1 calc R . .
C29 C 0.0151(4) 0.0647(3) 0.1974(3) 0.0481(10) Uani 1 1 d . . .
H29 H 0.0168 -0.0160 0.1944 0.058 Uiso 1 1 calc R . .
C30 C -0.0175(4) 0.1001(3) 0.1286(2) 0.0465(9) Uani 1 1 d . . .
H30 H -0.0355 0.0443 0.0785 0.056 Uiso 1 1 calc R . .
C31 C -0.0230(4) 0.2185(3) 0.1347(2) 0.0393(8) Uani 1 1 d . . .
H31 H -0.0457 0.2414 0.0878 0.047 Uiso 1 1 calc R . .
C32 C -0.0323(3) 0.7149(3) 0.23560(19) 0.0297(7) Uani 1 1 d . . .
C33 C -0.0818(3) 0.6446(3) 0.14876(19) 0.0293(7) Uani 1 1 d . . .
C34 C -0.1380(4) 0.6931(3) 0.0904(2) 0.0387(8) Uani 1 1 d . . .
H34 H -0.1431 0.7736 0.1046 0.046 Uiso 1 1 calc R . .
C35 C -0.1864(4) 0.6233(4) 0.0114(2) 0.0421(9) Uani 1 1 d . . .
H35 H -0.2239 0.6554 -0.0284 0.051 Uiso 1 1 calc R . .
C36 C -0.1781(4) 0.5050(4) -0.0072(2) 0.0418(9) Uani 1 1 d . . .
H36 H -0.2106 0.4552 -0.0602 0.050 Uiso 1 1 calc R . .
C37 C -0.1210(4) 0.4604(3) 0.05324(19) 0.0361(8) Uani 1 1 d . . .
H37 H -0.1156 0.3800 0.0396 0.043 Uiso 1 1 calc R . .
C38 C 0.4295(7) 0.8455(6) 0.3890(4) 0.104(2) Uani 1 1 d . . .
H38A H 0.5034 0.8841 0.3686 0.156 Uiso 1 1 calc R . .
H38B H 0.3660 0.8931 0.3904 0.156 Uiso 1 1 calc R . .
H38C H 0.3803 0.7623 0.3548 0.156 Uiso 1 1 calc R . .
C39 C 0.4870(8) 0.8412(7) 0.4677(6) 0.109(2) Uani 1 1 d . . .


_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 N5 1.889(3) . ?
Fe1 N6 1.893(3) . ?
Fe1 C1 1.980(3) . ?
Fe1 C2 1.982(3) . ?
Fe1 N7 2.008(3) . ?
Fe1 N8 2.014(3) . ?
Mn1 O4 1.881(2) . ?
Mn1 O3 1.890(2) . ?
Mn1 N3 2.019(3) . ?
Mn1 N4 2.020(3) . ?
Mn1 N2 2.301(3) 1_655 ?
Mn1 N1 2.340(3) . ?
Br1 C22 1.896(3) . ?
Br2 C23 1.893(3) . ?
Cl1 C8 1.741(3) . ?
Cl2 C15 1.746(3) . ?
O1 C26 1.225(4) . ?
O2 C32 1.234(4) . ?
O3 C5 1.315(4) . ?
O4 C12 1.324(4) . ?
N1 C1 1.142(4) . ?
N2 C2 1.144(4) . ?
N2 Mn1 2.301(3) 1_455 ?
N3 C3 1.282(4) . ?
N3 C17 1.466(4) . ?
N4 C10 1.280(4) . ?
N4 C19 1.481(4) . ?
N5 C26 1.356(4) . ?
N5 C20 1.399(4) . ?
N6 C32 1.346(4) . ?
N6 C25 1.397(4) . ?
N7 C31 1.343(4) . ?
N7 C27 1.360(4) . ?
N8 C37 1.340(4) . ?
N8 C33 1.359(4) . ?
N9 C39 1.178(9) . ?
C3 C4 1.441(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.406(4) . ?
C4 C9 1.413(5) . ?
C5 C6 1.399(5) . ?
C6 C7 1.377(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.386(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.361(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.434(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.415(4) . ?
C11 C16 1.417(5) . ?
C12 C13 1.403(5) . ?
C13 C14 1.372(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.362(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.486(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.495(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.392(5) . ?
C20 C25 1.417(4) . ?
C21 C22 1.377(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(5) . ?
C23 C24 1.376(5) . ?
C24 C25 1.395(5) . ?
C24 H24 0.9300 . ?
C26 C27 1.490(5) . ?
C27 C28 1.375(5) . ?
C28 C29 1.370(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.376(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.370(5) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C33 1.489(5) . ?
C33 C34 1.378(4) . ?
C34 C35 1.370(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.368(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.379(5) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.418(10) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

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
N5 Fe1 N6 83.37(11) . . ?
N5 Fe1 C1 91.93(12) . . ?
N6 Fe1 C1 95.42(12) . . ?
N5 Fe1 C2 96.63(11) . . ?
N6 Fe1 C2 92.99(12) . . ?
C1 Fe1 C2 168.63(13) . . ?
N5 Fe1 N7 81.84(11) . . ?
N6 Fe1 N7 165.21(11) . . ?
C1 Fe1 N7 84.83(11) . . ?
C2 Fe1 N7 88.99(11) . . ?
N5 Fe1 N8 165.01(11) . . ?
N6 Fe1 N8 81.70(11) . . ?
C1 Fe1 N8 90.86(11) . . ?
C2 Fe1 N8 82.79(11) . . ?
N7 Fe1 N8 113.09(11) . . ?
O4 Mn1 O3 91.16(9) . . ?
O4 Mn1 N3 175.02(10) . . ?
O3 Mn1 N3 89.68(10) . . ?
O4 Mn1 N4 90.75(10) . . ?
O3 Mn1 N4 176.09(10) . . ?
N3 Mn1 N4 88.72(11) . . ?
O4 Mn1 N2 93.14(10) . 1_655 ?
O3 Mn1 N2 90.64(10) . 1_655 ?
N3 Mn1 N2 91.76(10) . 1_655 ?
N4 Mn1 N2 85.85(10) . 1_655 ?
O4 Mn1 N1 89.07(9) . . ?
O3 Mn1 N1 91.82(10) . . ?
N3 Mn1 N1 85.99(10) . . ?
N4 Mn1 N1 91.62(10) . . ?
N2 Mn1 N1 176.65(10) 1_655 . ?
C5 O3 Mn1 126.63(19) . . ?
C12 O4 Mn1 126.92(19) . . ?
C1 N1 Mn1 150.1(3) . . ?
C2 N2 Mn1 146.8(3) . 1_455 ?
C3 N3 C17 119.2(3) . . ?
C3 N3 Mn1 123.3(2) . . ?
C17 N3 Mn1 117.5(2) . . ?
C10 N4 C19 119.1(3) . . ?
C10 N4 Mn1 122.5(2) . . ?
C19 N4 Mn1 118.2(2) . . ?
C26 N5 C20 125.3(3) . . ?
C26 N5 Fe1 119.6(2) . . ?
C20 N5 Fe1 115.0(2) . . ?
C32 N6 C25 125.1(3) . . ?
C32 N6 Fe1 119.6(2) . . ?
C25 N6 Fe1 115.2(2) . . ?
C31 N7 C27 117.5(3) . . ?
C31 N7 Fe1 130.2(2) . . ?
C27 N7 Fe1 112.3(2) . . ?
C37 N8 C33 117.1(3) . . ?
C37 N8 Fe1 130.6(2) . . ?
C33 N8 Fe1 112.1(2) . . ?
N1 C1 Fe1 172.3(3) . . ?
N2 C2 Fe1 171.8(3) . . ?
N3 C3 C4 125.7(3) . . ?
N3 C3 H3 117.2 . . ?
C4 C3 H3 117.2 . . ?
C5 C4 C9 120.1(3) . . ?
C5 C4 C3 121.8(3) . . ?
C9 C4 C3 117.6(3) . . ?
O3 C5 C6 118.8(3) . . ?
O3 C5 C4 123.4(3) . . ?
C6 C5 C4 117.8(3) . . ?
C7 C6 C5 121.2(3) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 Cl1 119.9(3) . . ?
C7 C8 Cl1 119.9(3) . . ?
C8 C9 C4 120.3(3) . . ?
C8 C9 H9 119.9 . . ?
C4 C9 H9 119.9 . . ?
N4 C10 C11 127.0(3) . . ?
N4 C10 H10 116.5 . . ?
C11 C10 H10 116.5 . . ?
C12 C11 C16 119.5(3) . . ?
C12 C11 C10 122.2(3) . . ?
C16 C11 C10 118.1(3) . . ?
O4 C12 C13 119.5(3) . . ?
O4 C12 C11 122.3(3) . . ?
C13 C12 C11 118.2(3) . . ?
C14 C13 C12 121.3(3) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 Cl2 119.1(3) . . ?
C14 C15 Cl2 120.1(3) . . ?
C15 C16 C11 120.1(3) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
N3 C17 C18 114.4(3) . . ?
N3 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N3 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 C19 117.4(3) . . ?
C17 C18 H18A 108.0 . . ?
C19 C18 H18A 108.0 . . ?
C17 C18 H18B 108.0 . . ?
C19 C18 H18B 108.0 . . ?
H18A C18 H18B 107.2 . . ?
N4 C19 C18 114.3(3) . . ?
N4 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
N4 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C21 C20 N5 126.7(3) . . ?
C21 C20 C25 119.9(3) . . ?
N5 C20 C25 113.3(3) . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 120.5(3) . . ?
C21 C22 Br1 117.6(3) . . ?
C23 C22 Br1 122.0(3) . . ?
C24 C23 C22 121.5(3) . . ?
C24 C23 Br2 117.3(3) . . ?
C22 C23 Br2 121.1(3) . . ?
C23 C24 C25 119.1(3) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C24 C25 N6 127.6(3) . . ?
C24 C25 C20 119.5(3) . . ?
N6 C25 C20 112.9(3) . . ?
O1 C26 N5 128.0(3) . . ?
O1 C26 C27 121.6(3) . . ?
N5 C26 C27 110.4(3) . . ?
N7 C27 C28 121.9(3) . . ?
N7 C27 C26 115.7(3) . . ?
C28 C27 C26 122.4(3) . . ?
C29 C28 C27 119.6(4) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 118.8(3) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C31 C30 C29 119.3(4) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
N7 C31 C30 122.8(4) . . ?
N7 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
O2 C32 N6 127.7(3) . . ?
O2 C32 C33 121.6(3) . . ?
N6 C32 C33 110.7(3) . . ?
N8 C33 C34 121.8(3) . . ?
N8 C33 C32 115.8(3) . . ?
C34 C33 C32 122.4(3) . . ?
C35 C34 C33 120.2(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C34 118.3(3) . . ?
C36 C35 H35 120.8 . . ?
C34 C35 H35 120.8 . . ?
C35 C36 C37 119.4(3) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
N8 C37 C36 123.1(3) . . ?
N8 C37 H37 118.4 . . ?
C36 C37 H37 118.4 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N9 C39 C38 174.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 1000035'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 Br2 Cl Cu Fe N10 O7'
_chemical_formula_weight         977.37

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8178(14)
_cell_length_b                   13.1598(17)
_cell_length_c                   14.3844(18)
_cell_angle_alpha                78.246(2)
_cell_angle_beta                 71.433(2)
_cell_angle_gamma                86.186(2)
_cell_volume                     1900.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1243
_cell_measurement_theta_min      2.591
_cell_measurement_theta_max      25.901

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_T_max  0.7020
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APEX II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9540
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         25.01
_reflns_number_total             6623
_reflns_number_gt                5095
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0642P)²+0.7492P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6623
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 0.24425(5) 0.30358(4) 0.19455(4) 0.02415(14) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.0000 0.0000 0.03718(19) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.5000 0.5000 0.03771(19) Uani 1 2 d S . .
Br1 Br 0.63535(5) 0.12333(5) 0.49063(4) 0.06464(18) Uani 1 1 d . . .
Br2 Br 0.78277(4) 0.34407(4) 0.33923(4) 0.05045(15) Uani 1 1 d . . .
Cl1 Cl 0.00099(14) 0.75225(10) 0.13741(9) 0.0592(3) Uani 1 1 d . . .
O1 O 0.1933(3) 0.0727(2) 0.4330(2) 0.0531(8) Uani 1 1 d . . .
O2 O 0.4791(3) 0.5426(2) 0.1508(2) 0.0512(8) Uani 1 1 d . . .
O3 O -0.0331(8) 0.6530(5) 0.1881(5) 0.163(3) Uani 1 1 d . . .
O4 O -0.0099(8) 0.7670(6) 0.0472(4) 0.177(3) Uani 1 1 d . . .
O5 O 0.1339(6) 0.7585(5) 0.1301(6) 0.156(3) Uani 1 1 d . . .
O6 O -0.0700(5) 0.8241(4) 0.1945(4) 0.1168(18) Uani 1 1 d . . .
O7 O 0.5405(6) 0.7200(3) 0.1984(4) 0.115(2) Uani 1 1 d . . .
H7 H 0.5588 0.6956 0.1476 0.173 Uiso 1 1 calc R . .
N1 N 0.4375(4) 0.1805(3) 0.0447(3) 0.0457(9) Uani 1 1 d . . .
N2 N 0.0466(3) 0.4237(3) 0.3449(3) 0.0407(8) Uani 1 1 d . . .
N3 N 0.2772(3) 0.2110(2) 0.3035(2) 0.0257(7) Uani 1 1 d . . .
N4 N 0.3823(3) 0.3800(2) 0.1998(2) 0.0279(7) Uani 1 1 d . . .
N5 N 0.2428(3) 0.4233(2) 0.0833(2) 0.0297(7) Uani 1 1 d . . .
N6 N 0.1009(3) 0.2018(2) 0.2225(2) 0.0289(7) Uani 1 1 d . . .
N7 N 0.3121(3) -0.0462(3) 0.0556(3) 0.0409(8) Uani 1 1 d . . .
H7A H 0.3118 -0.1148 0.0534 0.049 Uiso 1 1 calc R . .
N8 N 0.5404(4) -0.0539(3) 0.1288(2) 0.0412(8) Uani 1 1 d . . .
H8 H 0.5542 -0.1233 0.1318 0.049 Uiso 1 1 calc R . .
N9 N 0.0423(3) 0.3654(3) 0.5811(2) 0.0380(8) Uani 1 1 d . . .
H9 H 0.0358 0.3789 0.6421 0.046 Uiso 1 1 calc R . .
N10 N 0.1804(3) 0.5579(3) 0.4601(2) 0.0381(8) Uani 1 1 d . . .
H10 H 0.1836 0.5838 0.5133 0.046 Uiso 1 1 calc R . .
C1 C 0.3642(4) 0.2267(3) 0.0964(3) 0.0294(8) Uani 1 1 d . . .
C2 C 0.1150(3) 0.3817(3) 0.2860(3) 0.0273(8) Uani 1 1 d . . .
C3 C 0.3887(3) 0.2351(3) 0.3244(3) 0.0282(8) Uani 1 1 d . . .
C4 C 0.4473(3) 0.3298(3) 0.2661(3) 0.0282(8) Uani 1 1 d . . .
C5 C 0.5602(4) 0.3628(3) 0.2762(3) 0.0329(9) Uani 1 1 d . . .
H5 H 0.5968 0.4264 0.2399 0.039 Uiso 1 1 calc R . .
C6 C 0.6182(4) 0.3014(3) 0.3401(3) 0.0359(9) Uani 1 1 d . . .
C7 C 0.5589(4) 0.2084(3) 0.4000(3) 0.0378(10) Uani 1 1 d . . .
C8 C 0.4450(4) 0.1758(3) 0.3922(3) 0.0337(9) Uani 1 1 d . . .
H8A H 0.4057 0.1144 0.4321 0.040 Uiso 1 1 calc R . .
C9 C 0.4025(4) 0.4790(3) 0.1473(3) 0.0342(9) Uani 1 1 d . . .
C10 C 0.3203(4) 0.5020(3) 0.0802(3) 0.0327(9) Uani 1 1 d . . .
C11 C 0.3233(4) 0.5968(3) 0.0176(3) 0.0427(10) Uani 1 1 d . . .
H11 H 0.3752 0.6501 0.0182 0.051 Uiso 1 1 calc R . .
C12 C 0.2485(5) 0.6122(4) -0.0462(3) 0.0506(12) Uani 1 1 d . . .
H12 H 0.2471 0.6763 -0.0875 0.061 Uiso 1 1 calc R . .
C13 C 0.1768(5) 0.5311(4) -0.0471(3) 0.0548(13) Uani 1 1 d . . .
H13 H 0.1289 0.5385 -0.0916 0.066 Uiso 1 1 calc R . .
C14 C 0.1753(4) 0.4369(4) 0.0187(3) 0.0431(10) Uani 1 1 d . . .
H14 H 0.1259 0.3823 0.0175 0.052 Uiso 1 1 calc R . .
C15 C 0.1912(4) 0.1346(3) 0.3571(3) 0.0319(9) Uani 1 1 d . . .
C16 C 0.0883(4) 0.1309(3) 0.3078(3) 0.0309(9) Uani 1 1 d . . .
C17 C -0.0077(4) 0.0559(3) 0.3451(3) 0.0414(10) Uani 1 1 d . . .
H17 H -0.0154 0.0100 0.4050 0.050 Uiso 1 1 calc R . .
C18 C -0.0923(4) 0.0503(4) 0.2918(4) 0.0512(12) Uani 1 1 d . . .
H18 H -0.1583 0.0008 0.3152 0.061 Uiso 1 1 calc R . .
C19 C -0.0766(5) 0.1194(4) 0.2032(4) 0.0538(12) Uani 1 1 d . . .
H19 H -0.1303 0.1155 0.1647 0.065 Uiso 1 1 calc R . .
C20 C 0.0189(4) 0.1947(3) 0.1713(3) 0.0408(10) Uani 1 1 d . . .
H20 H 0.0264 0.2422 0.1122 0.049 Uiso 1 1 calc R . .
C21 C 0.6653(5) -0.0100(4) 0.1198(4) 0.0557(13) Uani 1 1 d . . .
H21A H 0.7030 -0.0518 0.1679 0.067 Uiso 1 1 calc R . .
H21B H 0.6528 0.0600 0.1329 0.067 Uiso 1 1 calc R . .
C22 C 0.4372(5) -0.0431(4) 0.2235(3) 0.0539(13) Uani 1 1 d . . .
H22A H 0.4230 0.0299 0.2262 0.065 Uiso 1 1 calc R . .
H22B H 0.4664 -0.0760 0.2797 0.065 Uiso 1 1 calc R . .
C23 C 0.3106(5) -0.0917(4) 0.2323(3) 0.0593(14) Uani 1 1 d . . .
H23A H 0.2522 -0.0943 0.2998 0.071 Uiso 1 1 calc R . .
H23B H 0.3279 -0.1626 0.2223 0.071 Uiso 1 1 calc R . .
C24 C 0.2421(5) -0.0363(4) 0.1599(3) 0.0531(13) Uani 1 1 d . . .
H24A H 0.1550 -0.0646 0.1792 0.064 Uiso 1 1 calc R . .
H24B H 0.2336 0.0366 0.1639 0.064 Uiso 1 1 calc R . .
C25 C 0.2452(4) 0.0090(4) -0.0152(4) 0.0550(12) Uani 1 1 d . . .
H25A H 0.2246 0.0794 -0.0047 0.066 Uiso 1 1 calc R . .
H25B H 0.1644 -0.0261 -0.0048 0.066 Uiso 1 1 calc R . .
C26 C -0.0637(5) 0.2920(3) 0.5978(4) 0.0505(12) Uani 1 1 d . . .
H26A H -0.0644 0.2354 0.6529 0.061 Uiso 1 1 calc R . .
H26B H -0.0508 0.2632 0.5384 0.061 Uiso 1 1 calc R . .
C27 C 0.1729(4) 0.3196(4) 0.5439(3) 0.0496(12) Uani 1 1 d . . .
H27A H 0.1809 0.2972 0.4820 0.060 Uiso 1 1 calc R . .
H27B H 0.1825 0.2590 0.5923 0.060 Uiso 1 1 calc R . .
C28 C 0.2812(5) 0.3966(4) 0.5255(4) 0.0551(13) Uani 1 1 d . . .
H28A H 0.2668 0.4240 0.5858 0.066 Uiso 1 1 calc R . .
H28B H 0.3636 0.3595 0.5135 0.066 Uiso 1 1 calc R . .
C29 C 0.2927(4) 0.4864(4) 0.4394(3) 0.0494(12) Uani 1 1 d . . .
H29A H 0.3723 0.5242 0.4262 0.059 Uiso 1 1 calc R . .
H29B H 0.2982 0.4600 0.3799 0.059 Uiso 1 1 calc R . .
C30 C 0.1912(5) 0.6493(4) 0.3787(4) 0.0537(12) Uani 1 1 d . . .
H30A H 0.2088 0.6271 0.3153 0.064 Uiso 1 1 calc R . .
H30B H 0.2621 0.6935 0.3738 0.064 Uiso 1 1 calc R . .
C31 C 0.6197(8) 0.6835(6) 0.2482(7) 0.120(3) Uani 1 1 d . . .
H31A H 0.6254 0.7311 0.2891 0.180 Uiso 1 1 calc R . .
H31B H 0.7045 0.6744 0.2025 0.180 Uiso 1 1 calc R . .
H31C H 0.5880 0.6178 0.2899 0.180 Uiso 1 1 calc R . .


_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 N4 1.884(3) . ?
Fe1 N3 1.894(3) . ?
Fe1 C2 1.982(4) . ?
Fe1 C1 1.985(4) . ?
Fe1 N6 2.005(3) . ?
Fe1 N5 2.007(3) . ?
Cu1 N8 2.016(3) . ?
Cu1 N8 2.016(3) 2_655 ?
Cu1 N7 2.018(3) . ?
Cu1 N7 2.018(3) 2_655 ?
Cu1 N1 2.578(3) . ?
Cu2 N10 2.006(3) 2_566 ?
Cu2 N10 2.006(3) . ?
Cu2 N9 2.025(3) . ?
Cu2 N9 2.025(3) 2_566 ?
Cu2 N2 2.523(3) . ?
Br1 C7 1.898(4) . ?
Br2 C6 1.897(4) . ?
Cl1 O4 1.314(5) . ?
Cl1 O3 1.370(6) . ?
Cl1 O6 1.406(5) . ?
Cl1 O5 1.415(6) . ?
O1 C15 1.228(4) . ?
O2 C9 1.235(5) . ?
O7 C31 1.293(7) . ?
O7 H7 0.8200 . ?
N1 C1 1.138(5) . ?
N2 C2 1.144(5) . ?
N3 C15 1.350(5) . ?
N3 C3 1.402(5) . ?
N4 C9 1.359(5) . ?
N4 C4 1.396(5) . ?
N5 C14 1.333(5) . ?
N5 C10 1.360(5) . ?
N6 C20 1.340(5) . ?
N6 C16 1.357(5) . ?
N7 C24 1.478(5) . ?
N7 C25 1.479(6) . ?
N7 H7A 0.9100 . ?
N8 C21 1.463(6) . ?
N8 C22 1.487(5) . ?
N8 H8 0.9100 . ?
N9 C27 1.477(5) . ?
N9 C26 1.478(6) . ?
N9 H9 0.9100 . ?
N10 C29 1.477(5) . ?
N10 C30 1.480(5) . ?
N10 H10 0.9100 . ?
C3 C8 1.392(5) . ?
C3 C4 1.414(5) . ?
C4 C5 1.382(5) . ?
C5 C6 1.375(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.406(6) . ?
C7 C8 1.376(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.485(6) . ?
C10 C11 1.378(6) . ?
C11 C12 1.383(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.366(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.505(5) . ?
C16 C17 1.381(5) . ?
C17 C18 1.382(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.382(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C25 1.506(7) 2_655 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.508(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.509(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C21 1.506(7) 2_655 ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C30 1.511(7) 2_566 ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.523(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.507(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C26 1.511(7) 2_566 ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?

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
N4 Fe1 N3 83.82(13) . . ?
N4 Fe1 C2 91.07(14) . . ?
N3 Fe1 C2 91.49(14) . . ?
N4 Fe1 C1 92.21(14) . . ?
N3 Fe1 C1 92.03(14) . . ?
C2 Fe1 C1 175.43(15) . . ?
N4 Fe1 N6 165.29(13) . . ?
N3 Fe1 N6 81.72(13) . . ?
C2 Fe1 N6 86.61(13) . . ?
C1 Fe1 N6 91.01(14) . . ?
N4 Fe1 N5 81.91(13) . . ?
N3 Fe1 N5 165.66(13) . . ?
C2 Fe1 N5 87.39(13) . . ?
C1 Fe1 N5 89.92(14) . . ?
N6 Fe1 N5 112.46(13) . . ?
N8 Cu1 N8 180.0(3) . 2_655 ?
N8 Cu1 N7 94.65(14) . . ?
N8 Cu1 N7 85.35(14) 2_655 . ?
N8 Cu1 N7 85.35(14) . 2_655 ?
N8 Cu1 N7 94.65(14) 2_655 2_655 ?
N7 Cu1 N7 180.0(3) . 2_655 ?
N8 Cu1 N1 92.13(13) . . ?
N8 Cu1 N1 87.87(13) 2_655 . ?
N7 Cu1 N1 91.43(13) . . ?
N7 Cu1 N1 88.57(13) 2_655 . ?
N10 Cu2 N10 180.00(18) 2_566 . ?
N10 Cu2 N9 85.72(14) 2_566 . ?
N10 Cu2 N9 94.28(14) . . ?
N10 Cu2 N9 94.28(14) 2_566 2_566 ?
N10 Cu2 N9 85.72(14) . 2_566 ?
N9 Cu2 N9 180.00(17) . 2_566 ?
N10 Cu2 N2 86.45(12) 2_566 . ?
N10 Cu2 N2 93.55(12) . . ?
N9 Cu2 N2 92.88(12) . . ?
N9 Cu2 N2 87.12(12) 2_566 . ?
O4 Cl1 O3 111.3(5) . . ?
O4 Cl1 O6 113.6(4) . . ?
O3 Cl1 O6 110.1(4) . . ?
O4 Cl1 O5 109.3(5) . . ?
O3 Cl1 O5 103.6(5) . . ?
O6 Cl1 O5 108.5(3) . . ?
C31 O7 H7 109.5 . . ?
C1 N1 Cu1 145.7(3) . . ?
C2 N2 Cu2 150.5(3) . . ?
C15 N3 C3 126.1(3) . . ?
C15 N3 Fe1 119.6(2) . . ?
C3 N3 Fe1 114.2(2) . . ?
C9 N4 C4 126.3(3) . . ?
C9 N4 Fe1 118.9(3) . . ?
C4 N4 Fe1 114.6(2) . . ?
C14 N5 C10 118.3(3) . . ?
C14 N5 Fe1 130.1(3) . . ?
C10 N5 Fe1 111.5(2) . . ?
C20 N6 C16 117.5(3) . . ?
C20 N6 Fe1 130.3(3) . . ?
C16 N6 Fe1 112.2(2) . . ?
C24 N7 C25 112.4(4) . . ?
C24 N7 Cu1 116.8(3) . . ?
C25 N7 Cu1 106.9(3) . . ?
C24 N7 H7A 106.7 . . ?
C25 N7 H7A 106.7 . . ?
Cu1 N7 H7A 106.7 . . ?
C21 N8 C22 112.8(4) . . ?
C21 N8 Cu1 108.0(3) . . ?
C22 N8 Cu1 117.4(3) . . ?
C21 N8 H8 105.9 . . ?
C22 N8 H8 105.9 . . ?
Cu1 N8 H8 105.9 . . ?
C27 N9 C26 112.4(3) . . ?
C27 N9 Cu2 117.9(3) . . ?
C26 N9 Cu2 106.8(3) . . ?
C27 N9 H9 106.3 . . ?
C26 N9 H9 106.3 . . ?
Cu2 N9 H9 106.3 . . ?
C29 N10 C30 113.2(3) . . ?
C29 N10 Cu2 118.6(3) . . ?
C30 N10 Cu2 107.8(3) . . ?
C29 N10 H10 105.3 . . ?
C30 N10 H10 105.3 . . ?
Cu2 N10 H10 105.3 . . ?
N1 C1 Fe1 175.3(4) . . ?
N2 C2 Fe1 173.7(3) . . ?
C8 C3 N3 127.1(3) . . ?
C8 C3 C4 119.6(3) . . ?
N3 C3 C4 113.2(3) . . ?
C5 C4 N4 126.5(4) . . ?
C5 C4 C3 120.1(3) . . ?
N4 C4 C3 113.5(3) . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.3(4) . . ?
C5 C6 Br2 117.5(3) . . ?
C7 C6 Br2 122.1(3) . . ?
C8 C7 C6 120.3(4) . . ?
C8 C7 Br1 118.5(3) . . ?
C6 C7 Br1 121.2(3) . . ?
C7 C8 C3 119.8(4) . . ?
C7 C8 H8A 120.1 . . ?
C3 C8 H8A 120.1 . . ?
O2 C9 N4 126.8(4) . . ?
O2 C9 C10 122.9(4) . . ?
N4 C9 C10 110.3(3) . . ?
N5 C10 C11 121.9(4) . . ?
N5 C10 C9 115.9(3) . . ?
C11 C10 C9 122.2(4) . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 118.5(4) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
N5 C14 C13 121.7(4) . . ?
N5 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
O1 C15 N3 127.9(4) . . ?
O1 C15 C16 122.1(4) . . ?
N3 C15 C16 109.9(3) . . ?
N6 C16 C17 122.8(4) . . ?
N6 C16 C15 115.7(3) . . ?
C17 C16 C15 121.4(4) . . ?
C16 C17 C18 118.9(4) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C19 C18 C17 118.5(4) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
C18 C19 C20 120.0(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
N6 C20 C19 122.3(4) . . ?
N6 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
N8 C21 C25 108.1(4) . 2_655 ?
N8 C21 H21A 110.1 . . ?
C25 C21 H21A 110.1 2_655 . ?
N8 C21 H21B 110.1 . . ?
C25 C21 H21B 110.1 2_655 . ?
H21A C21 H21B 108.4 . . ?
N8 C22 C23 111.8(4) . . ?
N8 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
N8 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
C22 C23 C24 115.0(4) . . ?
C22 C23 H23A 108.5 . . ?
C24 C23 H23A 108.5 . . ?
C22 C23 H23B 108.5 . . ?
C24 C23 H23B 108.5 . . ?
H23A C23 H23B 107.5 . . ?
N7 C24 C23 112.6(4) . . ?
N7 C24 H24A 109.1 . . ?
C23 C24 H24A 109.1 . . ?
N7 C24 H24B 109.1 . . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
N7 C25 C21 108.2(4) . 2_655 ?
N7 C25 H25A 110.1 . . ?
C21 C25 H25A 110.1 2_655 . ?
N7 C25 H25B 110.1 . . ?
C21 C25 H25B 110.1 2_655 . ?
H25A C25 H25B 108.4 . . ?
N9 C26 C30 108.0(4) . 2_566 ?
N9 C26 H26A 110.1 . . ?
C30 C26 H26A 110.1 2_566 . ?
N9 C26 H26B 110.1 . . ?
C30 C26 H26B 110.1 2_566 . ?
H26A C26 H26B 108.4 . . ?
N9 C27 C28 111.9(4) . . ?
N9 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
N9 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C29 C28 C27 115.2(4) . . ?
C29 C28 H28A 108.5 . . ?
C27 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C27 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
N10 C29 C28 111.9(4) . . ?
N10 C29 H29A 109.2 . . ?
C28 C29 H29A 109.2 . . ?
N10 C29 H29B 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
N10 C30 C26 108.0(4) . 2_566 ?
N10 C30 H30A 110.1 . . ?
C26 C30 H30A 110.1 2_566 . ?
N10 C30 H30B 110.1 . . ?
C26 C30 H30B 110.1 2_566 . ?
H30A C30 H30B 108.4 . . ?
O7 C31 H31A 109.5 . . ?
O7 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O7 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 1000036'
