# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_290
_database_code_depnum_ccdc_archive 'CCDC 1027572'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H14 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.213(10)
_cell_length_b                   24.04(3)
_cell_length_c                   8.220(14)
_cell_angle_alpha                90
_cell_angle_beta                 119.528(17)
_cell_angle_gamma                90
_cell_volume                     1412(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1843
_cell_measurement_temperature    290
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.061
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1483 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.4232.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1190
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9966
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         0.847
_diffrn_ambient_temperature      290.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1631
_reflns_number_total             2794
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2794
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1472
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Shared sites
{H4B, H4C}
2. Others
 Fixed Sof: O1A(0.5) O1B(0.5) O2B(0.5) H4A(0.5) H4B(0.5) H4C(0.5) H4D(0.5)
 C5A(0.5) O2A(0.5) O3A(0.5) O3B(0.5) C5C(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5)
 H7BC(0.5) N3B(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5)
 C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) N1B(0.5) N2A(0.5) N2B(0.5) N1A(0.5)
 N3A(0.5)
 Fixed U12: Fe1(0)
 Fixed U23: Fe1(0)
 Fixed Uiso: H4A(0.066) H4B(0.066) H4C(0.066) H4D(0.066) C5A(0.08) C5C(0.08)
 C7B(0.08) H7BA(0.12) H7BB(0.12) H7BC(0.12) C6B(0.08) H6BA(0.096) H6BB(0.096)
 C6A(0.08) H6AA(0.096) H6AB(0.096) C7A(0.08) H7AA(0.12) H7AB(0.12) H7AC(0.12)
 Fixed X: H4A(0.3051) H4B(0.417) H4C(0.4156) H4D(0.1982) H7BA(-0.0958) H7BB(-
 0.1715) H7BC(-0.0911) H6BA(0.207) H6BB(0.1263) H6AA(0.2865) H6AB(0.4834)
 H7AA(0.3196) H7AB(0.3539) H7AC(0.1572)
 Fixed Y: H4A(-0.0441) H4B(-0.0426) H4C(-0.0429) H4D(-0.0442) Fe1(-0.25)
 H7BA(0.0713) H7BB(0.0179) H7BC(0.0138) H6BA(0.0353) H6BB(0.0394) H6AA(0.0466)
 H6AB(0.0308) H7AA(0.0835) H7AB(0.0239) H7AC(0.0397)
 Fixed Z: H4A(-0.3062) H4B(-0.0887) H4C(-0.0865) H4D(-0.1916) H7BA(-0.1952)
 H7BB(-0.3197) H7BC(-0.1031) H6BA(-0.0539) H6BB(-0.2713) H6AA(-0.321) H6AB(-
 0.2945) H7AA(-0.5641) H7AB(-0.6181) H7AC(-0.6446)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br3 Br 0.82287(15) -0.17701(6) -0.1832(2) 0.0596(4) Uani 1 1 d . . . . .
Br2 Br 0.31695(19) -0.17695(6) 0.32308(17) 0.0597(4) Uani 1 1 d . . . . .
B1 B 0.3154(16) -0.1237(6) -0.1865(19) 0.048(3) Uani 1 1 d . . . . .
O1A O 0.177(2) -0.1455(8) -0.379(2) 0.037(4) Uani 0.5 1 d . . . A 1
O1B O 0.1175(19) -0.1480(9) -0.329(2) 0.040(5) Uani 0.5 1 d . . . A 2
O2B O 0.372(2) -0.1453(7) 0.0019(17) 0.035(4) Uani 0.5 1 d . . . A 2
C2 C 0.3126(12) -0.2205(4) 0.1359(12) 0.033(3) Uani 1 1 d . U . . .
C1 C -0.0117(11) -0.2208(4) -0.5102(12) 0.037(3) Uani 1 1 d . . . . .
C3 C 0.6364(10) -0.2201(5) -0.1858(13) 0.043(4) Uani 1 1 d . . . . .
C4 C 0.3072(16) -0.0572(4) -0.1948(18) 0.055(3) Uani 1 1 d D . . . .
H4A H 0.3051 -0.0441 -0.3062 0.066 Uiso 0.5 1 d R . . . .
H4B H 0.4170 -0.0426 -0.0887 0.066 Uiso 0.5 1 d R . . . .
H4C H 0.4156 -0.0429 -0.0865 0.066 Uiso 0.5 1 d R . . . .
H4D H 0.1982 -0.0442 -0.1916 0.066 Uiso 0.5 1 d R . . . .
C5A C 0.307(4) -0.0358(11) -0.368(3) 0.080 Uiso 0.5 1 d D . . . .
O2A O 0.253(2) -0.1469(8) -0.0487(19) 0.039(4) Uani 0.5 1 d . . . A 1
O3A O 0.5004(18) -0.1453(8) -0.129(2) 0.038(4) Uani 0.5 1 d . . . A 1
Fe1 Fe 0.3122(2) -0.2500 -0.1878(2) 0.0242(4) Uani 1 2 d S T P . .
O3B O 0.4479(18) -0.1460(7) -0.251(2) 0.033(4) Uani 0.5 1 d . . . A 2
Br1 Br -0.19498(15) -0.17689(5) -0.69517(17) 0.0532(4) Uani 1 1 d . . . . .
C5C C 0.136(3) -0.0405(11) -0.183(4) 0.080 Uiso 0.5 1 d D . . . .
C7B C -0.079(3) 0.0320(13) -0.200(4) 0.080 Uiso 0.5 1 d D . . B -2
H7BA H -0.0958 0.0713 -0.1952 0.120 Uiso 0.5 1 calc R . . B -2
H7BB H -0.1715 0.0179 -0.3197 0.120 Uiso 0.5 1 calc R . . B -2
H7BC H -0.0911 0.0138 -0.1031 0.120 Uiso 0.5 1 calc R . . B -2
N3B N 0.470(2) -0.1995(10) -0.232(3) 0.034(5) Uiso 0.5 1 d . . . A 2
C6B C 0.112(3) 0.0210(11) -0.174(4) 0.080 Uiso 0.5 1 d D . . B -2
H6BA H 0.2070 0.0353 -0.0539 0.096 Uiso 0.5 1 calc R . . B -2
H6BB H 0.1263 0.0394 -0.2713 0.096 Uiso 0.5 1 calc R . . B -2
C6A C 0.350(4) 0.0249(10) -0.372(3) 0.080 Uiso 0.5 1 d D . . C 2
H6AA H 0.2865 0.0466 -0.3210 0.096 Uiso 0.5 1 calc R . . C 2
H6AB H 0.4834 0.0308 -0.2945 0.096 Uiso 0.5 1 calc R . . C 2
C7A C 0.290(3) 0.0448(10) -0.567(3) 0.080 Uiso 0.5 1 d D . . C 2
H7AA H 0.3196 0.0835 -0.5641 0.120 Uiso 0.5 1 calc R . . C 2
H7AB H 0.3539 0.0239 -0.6181 0.120 Uiso 0.5 1 calc R . . C 2
H7AC H 0.1572 0.0397 -0.6446 0.120 Uiso 0.5 1 calc R . . C 2
N1B N 0.111(2) -0.2029(8) -0.350(2) 0.019(4) Uiso 0.5 1 d . . . A 2
N2A N 0.269(2) -0.2012(9) -0.027(2) 0.026(4) Uiso 0.5 1 d . . . A 1
N2B N 0.352(2) -0.2007(8) 0.009(2) 0.025(4) Uiso 0.5 1 d . . . A 2
N1A N 0.158(2) -0.2012(9) -0.386(2) 0.031(5) Uiso 0.5 1 d . . . A 1
N3A N 0.506(2) -0.1986(9) -0.153(3) 0.022(4) Uiso 0.5 1 d . . . A 1


_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
Br3 C3 1.841(10) . ?
Br2 C2 1.847(10) . ?
B1 O1A 1.51(2) . ?
B1 O1B 1.575(19) . ?
B1 O2B 1.474(19) . ?
B1 C4 1.602(16) . ?
B1 O2A 1.56(2) . ?
B1 O3A 1.446(18) . ?
B1 O3B 1.52(2) . ?
O1A N1A 1.35(3) . ?
O1B N1B 1.33(3) . ?
O2B N2B 1.35(2) . ?
C2 C2 1.42(2) 4 ?
C2 N2A 1.291(18) . ?
C2 N2B 1.324(19) . ?
C1 C1 1.40(2) 4 ?
C1 Br1 1.854(9) . ?
C1 N1B 1.274(17) . ?
C1 N1A 1.344(19) . ?
C3 C3 1.44(2) 4 ?
C3 N3B 1.32(2) . ?
C3 N3A 1.335(19) . ?
C4 C5A 1.510(10) . ?
C4 C5C 1.515(10) . ?
C5A C6A 1.505(10) . ?
O2A N2A 1.31(2) . ?
O3A N3A 1.30(2) . ?
Fe1 N3B 1.94(2) 4 ?
Fe1 N3B 1.94(2) . ?
Fe1 N1B 1.901(16) 4 ?
Fe1 N1B 1.901(16) . ?
Fe1 N2A 1.925(19) . ?
Fe1 N2A 1.925(19) 4 ?
Fe1 N2B 1.899(18) . ?
Fe1 N2B 1.899(18) 4 ?
Fe1 N1A 1.899(19) 4 ?
Fe1 N1A 1.899(19) . ?
Fe1 N3A 1.919(18) . ?
Fe1 N3A 1.919(18) 4 ?
O3B N3B 1.30(3) . ?
C5C C6B 1.497(10) . ?
C7B C6B 1.497(10) . ?
C6A C7A 1.504(10) . ?

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
O1A B1 C4 107.8(11) . . ?
O1A B1 O2A 106.9(11) . . ?
O1B B1 C4 109.4(11) . . ?
O2B B1 O1B 109.2(12) . . ?
O2B B1 C4 112.4(12) . . ?
O2B B1 O3B 109.3(11) . . ?
O2A B1 C4 111.5(12) . . ?
O3A B1 O1A 110.1(13) . . ?
O3A B1 C4 112.8(11) . . ?
O3A B1 O2A 107.5(12) . . ?
O3B B1 O1B 105.3(12) . . ?
O3B B1 C4 111.0(11) . . ?
N1A O1A B1 113.7(14) . . ?
N1B O1B B1 115.1(13) . . ?
N2B O2B B1 114.3(13) . . ?
C2 C2 Br2 124.6(3) 4 . ?
N2A C2 Br2 122.8(12) . . ?
N2A C2 C2 111.1(10) . 4 ?
N2B C2 Br2 122.7(11) . . ?
N2B C2 C2 111.1(10) . 4 ?
C1 C1 Br1 124.7(3) 4 . ?
N1B C1 C1 109.7(10) . 4 ?
N1B C1 Br1 124.4(11) . . ?
N1A C1 C1 110.6(10) . 4 ?
N1A C1 Br1 122.8(12) . . ?
C3 C3 Br3 124.3(3) 4 . ?
N3B C3 Br3 121.9(13) . . ?
N3B C3 C3 112.1(11) . 4 ?
N3A C3 Br3 121.8(12) . . ?
N3A C3 C3 112.8(10) . 4 ?
C5A C4 B1 111.2(13) . . ?
C5A C4 C5C 113.7(17) . . ?
C5C C4 B1 106.4(14) . . ?
C6A C5A C4 117.6(19) . . ?
N2A O2A B1 114.1(13) . . ?
N3A O3A B1 114.3(13) . . ?
N3B Fe1 N3B 77.6(13) 4 . ?
N1B Fe1 N3B 85.7(8) . . ?
N1B Fe1 N3B 132.1(9) 4 . ?
N1B Fe1 N3B 85.7(8) 4 4 ?
N1B Fe1 N3B 132.1(9) . 4 ?
N1B Fe1 N1B 73.0(11) 4 . ?
N2A Fe1 N2A 75.2(12) . 4 ?
N2B Fe1 N3B 85.3(8) . . ?
N2B Fe1 N3B 134.5(8) . 4 ?
N2B Fe1 N3B 134.5(8) 4 . ?
N2B Fe1 N3B 85.3(8) 4 4 ?
N2B Fe1 N1B 134.1(8) . 4 ?
N2B Fe1 N1B 87.3(8) 4 4 ?
N2B Fe1 N1B 87.3(8) . . ?
N2B Fe1 N1B 134.1(8) 4 . ?
N2B Fe1 N2B 77.3(11) 4 . ?
N1A Fe1 N2A 86.7(8) 4 4 ?
N1A Fe1 N2A 134.2(8) 4 . ?
N1A Fe1 N2A 134.2(8) . 4 ?
N1A Fe1 N2A 86.7(8) . . ?
N1A Fe1 N1A 76.4(12) . 4 ?
N1A Fe1 N3A 132.8(8) 4 . ?
N1A Fe1 N3A 83.3(8) 4 4 ?
N1A Fe1 N3A 132.8(8) . 4 ?
N1A Fe1 N3A 83.3(8) . . ?
N3A Fe1 N2A 85.5(8) . . ?
N3A Fe1 N2A 85.5(8) 4 4 ?
N3A Fe1 N2A 135.0(7) . 4 ?
N3A Fe1 N2A 135.0(7) 4 . ?
N3A Fe1 N3A 80.1(11) . 4 ?
N3B O3B B1 113.0(14) . . ?
C6B C5C C4 114.2(18) . . ?
C3 N3B Fe1 113.9(16) . . ?
O3B N3B C3 118.2(17) . . ?
O3B N3B Fe1 125.0(13) . . ?
C7B C6B C5C 108.5(19) . . ?
C7A C6A C5A 112.3(10) . . ?
O1B N1B Fe1 122.4(11) . . ?
C1 N1B O1B 115.4(15) . . ?
C1 N1B Fe1 119.8(14) . . ?
C2 N2A O2A 117.1(16) . . ?
C2 N2A Fe1 116.3(14) . . ?
O2A N2A Fe1 123.5(12) . . ?
O2B N2B Fe1 123.6(12) . . ?
C2 N2B O2B 118.3(15) . . ?
C2 N2B Fe1 116.1(14) . . ?
O1A N1A Fe1 124.2(13) . . ?
C1 N1A O1A 116.0(15) . . ?
C1 N1A Fe1 115.9(15) . . ?
C3 N3A Fe1 114.2(14) . . ?
O3A N3A C3 120.2(15) . . ?
O3A N3A Fe1 124.8(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3A_a B1 O1A_a N1A_a 62(2) . . . . ?
Br3 C3 N3B Fe1 -171.2(6) . . . . ?
Br3 C3 N3B O3B -9(3) . . . . ?
Br3 C3 N3A O3A 4(2) . . . . ?
Br3 C3 N3A Fe1 174.0(6) . . . . ?
Br2 C2 N2A O2A 9(2) . . . . ?
Br2 C2 N2A Fe1 170.3(6) . . . . ?
Br2 C2 N2B O2B -9(2) . . . . ?
Br2 C2 N2B Fe1 -173.2(5) . . . . ?
B1 O1A N1A C1 148.4(15) . . . . ?
B1 O1A N1A Fe1 -9(2) . . . . ?
B1 O1B N1B C1 -150.8(14) . . . . ?
B1 O1B N1B Fe1 11(2) . . . . ?
B1 O2B N2B C2 -148.7(13) . . . . ?
B1 O2B N2B Fe1 15(2) . . . . ?
B1 C4 C5A C6A -164.5(19) . . . . ?
B1 C4 C5C C6B 176(2) . . . . ?
B1 O2A N2A C2 146.4(14) . . . . ?
B1 O2A N2A Fe1 -13(2) . . . . ?
B1 O3A N3A C3 150.4(15) . . . . ?
B1 O3A N3A Fe1 -18(2) . . . . ?
B1 O3B N3B C3 -144.9(16) . . . . ?
B1 O3B N3B Fe1 15(2) . . . . ?
O1A B1 O1B N1B 81(3) . . . . ?
O1A B1 O2B N2B 26(2) . . . . ?
O1A B1 C4 C5A -45.0(17) . . . . ?
O1A B1 C4 C5C 79.4(17) . . . . ?
O1A B1 O2A N2A 66.7(17) . . . . ?
O1A B1 O3A N3A -48(2) . . . . ?
O1A B1 O3B N3B -80.2(16) . . . . ?
O1B B1 O1A N1A -76(2) . . . . ?
O1B B1 O2B N2B 48.1(18) . . . . ?
O1B B1 C4 C5A -75.7(17) . . . . ?
O1B B1 C4 C5C 48.6(18) . . . . ?
O1B B1 O2A N2A 77.4(15) . . . . ?
O1B B1 O3A N3A -23(3) . . . . ?
O1B B1 O3B N3B -67.0(18) . . . . ?
O2B B1 O1A N1A -29(3) . . . . ?
O2B B1 O1B N1B -63.7(19) . . . . ?
O2B B1 C4 C5A 162.8(15) . . . . ?
O2B B1 C4 C5C -72.9(17) . . . . ?
O2B B1 O2A N2A -77.4(19) . . . . ?
O2B B1 O3A N3A 82.3(18) . . . . ?
O2B B1 O3B N3B 50.2(18) . . . . ?
C2 C2 N2A O2A 176.0(12) 4 . . . ?
C2 C2 N2A Fe1 -23.1(13) 4 . . . ?
C2 C2 N2B O2B -174.7(11) 4 . . . ?
C2 C2 N2B Fe1 20.8(12) 4 . . . ?
C1 C1 N1B O1B -176.2(13) 4 . . . ?
C1 C1 N1B Fe1 21.0(14) 4 . . . ?
C1 C1 N1A O1A 177.5(14) 4 . . . ?
C1 C1 N1A Fe1 -23.5(14) 4 . . . ?
C3 C3 N3B Fe1 23.3(15) 4 . . . ?
C3 C3 N3B O3B -174.9(15) 4 . . . ?
C3 C3 N3A O3A 172.8(14) 4 . . . ?
C3 C3 N3A Fe1 -17.5(13) 4 . . . ?
C4 B1 O1A N1A -174.2(15) . . . . ?
C4 B1 O1B N1B 172.9(15) . . . . ?
C4 B1 O2B N2B 169.8(13) . . . . ?
C4 B1 O2A N2A -175.7(13) . . . . ?
C4 B1 O3A N3A -168.3(15) . . . . ?
C4 B1 O3B N3B 174.7(14) . . . . ?
C4 C5A C6A C7A -163(2) . . . . ?
C4 C5C C6B C7B 169(2) . . . . ?
C5A C4 C5C C6B -62(3) . . . . ?
O2A B1 O1A N1A -54(2) . . . . ?
O2A B1 O1B N1B -77.7(17) . . . . ?
O2A B1 O2B N2B 74.5(18) . . . . ?
O2A B1 C4 C5A -162.1(15) . . . . ?
O2A B1 C4 C5C -37.7(17) . . . . ?
O2A B1 O3A N3A 68.4(19) . . . . ?
O2A B1 O3B N3B 23(2) . . . . ?
O3A B1 O1B N1B 27(3) . . . . ?
O3A B1 O2B N2B -80.4(15) . . . . ?
O3A B1 C4 C5A 76.9(18) . . . . ?
O3A B1 C4 C5C -158.8(17) . . . . ?
O3A B1 O2A N2A -51.6(17) . . . . ?
O3A B1 O3B N3B 74.8(19) . . . . ?
O3B B1 O1A N1A 77.0(17) . . . . ?
O3B B1 O1B N1B 54(2) . . . . ?
O3B B1 O2B N2B -66.5(17) . . . . ?
O3B B1 C4 C5A 40.0(17) . . . . ?
O3B B1 C4 C5C 164.3(15) . . . . ?
O3B B1 O2A N2A -24(2) . . . . ?
O3B B1 O3A N3A -74.0(19) . . . . ?
Br1 C1 N1B O1B -8(2) . . . . ?
Br1 C1 N1B Fe1 -171.0(7) . . . . ?
Br1 C1 N1A O1A 13(2) . . . . ?
Br1 C1 N1A Fe1 171.6(7) . . . . ?
C5C C4 C5A C6A 75(3) . . . . ?
N3B C3 N3A O3A -94(4) . . . . ?
N3B C3 N3A Fe1 76(4) . . . . ?
N3B Fe1 N2B O2B 33.6(15) . . . . ?
N3B Fe1 N2B O2B 101.1(16) 4 . . . ?
N3B Fe1 N2B C2 -95.3(15) 4 . . . ?
N3B Fe1 N2B C2 -162.8(14) . . . . ?
N3B Fe1 N1A O1A -114.3(18) 4 . . . ?
N3B Fe1 N1A O1A -49.6(18) . . . . ?
N3B Fe1 N1A C1 153.4(16) . . . . ?
N3B Fe1 N1A C1 88.7(16) 4 . . . ?
N1B C1 N1A O1A -90(3) . . . . ?
N1B C1 N1A Fe1 69(3) . . . . ?
N1B Fe1 N2B O2B -52.3(15) . . . . ?
N1B Fe1 N2B O2B -115.4(16) 4 . . . ?
N1B Fe1 N2B C2 111.3(12) . . . . ?
N1B Fe1 N2B C2 48.2(17) 4 . . . ?
N1B Fe1 N1A O1A 94(3) . . . . ?
N1B Fe1 N1A O1A 167.1(17) 4 . . . ?
N1B Fe1 N1A C1 10.1(15) 4 . . . ?
N1B Fe1 N1A C1 -63(3) . . . . ?
N2A C2 N2B O2B 90(3) . . . . ?
N2A C2 N2B Fe1 -74(3) . . . . ?
N2A Fe1 N2B O2B -170.7(14) 4 . . . ?
N2A Fe1 N2B O2B -95(3) . . . . ?
N2A Fe1 N2B C2 -7.1(13) 4 . . . ?
N2A Fe1 N2B C2 69(3) . . . . ?
N2A Fe1 N1A O1A 48.3(18) . . . . ?
N2A Fe1 N1A O1A 113.9(19) 4 . . . ?
N2A Fe1 N1A C1 -108.7(14) . . . . ?
N2A Fe1 N1A C1 -43(2) 4 . . . ?
N2B C2 N2A O2A -89(3) . . . . ?
N2B C2 N2A Fe1 72(3) . . . . ?
N2B Fe1 N2B O2B 171.3(11) 4 . . . ?
N2B Fe1 N2B C2 -25.1(15) 4 . . . ?
N2B Fe1 N1A O1A 108(2) 4 . . . ?
N2B Fe1 N1A O1A 33.3(19) . . . . ?
N2B Fe1 N1A C1 -49(2) 4 . . . ?
N2B Fe1 N1A C1 -123.7(14) . . . . ?
N1A C1 N1B O1B 87(3) . . . . ?
N1A C1 N1B Fe1 -76(3) . . . . ?
N1A Fe1 N2B O2B -36.8(16) . . . . ?
N1A Fe1 N2B O2B -109(2) 4 . . . ?
N1A Fe1 N2B C2 54(2) 4 . . . ?
N1A Fe1 N2B C2 126.8(13) . . . . ?
N1A Fe1 N1A O1A -174.6(14) 4 . . . ?
N1A Fe1 N1A C1 28.4(17) 4 . . . ?
N3A C3 N3B Fe1 -73(4) . . . . ?
N3A C3 N3B O3B 88(4) . . . . ?
N3A Fe1 N2B O2B 110.9(15) 4 . . . ?
N3A Fe1 N2B O2B 44.0(14) . . . . ?
N3A Fe1 N2B C2 -152.3(14) . . . . ?
N3A Fe1 N2B C2 -85.5(14) 4 . . . ?
N3A Fe1 N1A O1A -107.4(18) 4 . . . ?
N3A Fe1 N1A O1A -37.5(18) . . . . ?
N3A Fe1 N1A C1 95.6(16) 4 . . . ?
N3A Fe1 N1A C1 165.4(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_270
_database_code_depnum_ccdc_archive 'CCDC 1027573'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H14 B2 Br6 Fe N6 O6'
_chemical_formula_weight         919.24
_chemical_melting_point          ?
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.2075(16)
_cell_length_b                   24.257(5)
_cell_length_c                   8.2107(16)
_cell_angle_alpha                90
_cell_angle_beta                 119.427(3)
_cell_angle_gamma                90
_cell_volume                     1423.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    270
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.988
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1623 before and 0.0696 after correction.
The Ratio of minimum to maximum transmission is 0.4194.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.1308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13486
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.727
_diffrn_reflns_theta_min         2.519
_diffrn_ambient_temperature      270
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1995
_reflns_number_total             4052
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.987
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.0606
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1473
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N2A \\sim N2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N1B \\sim N1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3B \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C1) \\sim Ueq, Uanis(O1A) \\sim Ueq, : with sigma of 0.008 and sigma for
terminal atoms of 0.008
3. Others
 Fixed Sof: N1B(0.5) N2A(0.5) N3B(0.5) H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5)
 O1A(0.5) O2A(0.5) O3A(0.5) O1B(0.5) O2B(0.5) O3B(0.5) C5B(0.5) H5BA(0.5)
 H5BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) N2B(0.5) N1A(0.5) N3A(0.5)
 Fixed Uiso: C7A(0.09) C7B(0.09) C6A(0.08) C6B(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C5B(H5BA,H5BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB)
4.b Me refined with riding coordinates:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3345(2) -0.2500 -0.16562(18) 0.0200(3) Uani 1 2 d S T P . .
Br1 Br -0.17075(13) -0.17727(4) -0.67077(12) 0.0445(3) Uani 1 1 d . . . . .
Br3 Br 0.84825(13) -0.17753(4) -0.15977(15) 0.0519(3) Uani 1 1 d . . . . .
Br2 Br 0.34029(16) -0.17756(4) 0.34839(12) 0.0521(3) Uani 1 1 d . . . . .
B1 B 0.3329(13) -0.1248(4) -0.1659(13) 0.034(2) Uani 1 1 d . . . . .
N1B N 0.1342(18) -0.2010(7) -0.3230(18) 0.024(3) Uiso 0.5 1 d . U . A 2
N2A N 0.2899(19) -0.2022(6) -0.0033(16) 0.020(3) Uiso 0.5 1 d . U . A 1
N3B N 0.4954(18) -0.2038(6) -0.2081(19) 0.023(3) Uiso 0.5 1 d . . . A 2
C2 C 0.3364(11) -0.2205(4) 0.1630(9) 0.035(2) Uani 1 1 d . . . . .
C1 C 0.0161(10) -0.2200(3) -0.4837(9) 0.0262(18) Uani 1 1 d . U . . .
C3 C 0.6622(10) -0.2210(4) -0.1629(10) 0.0298(19) Uani 1 1 d . . . . .
C4 C 0.3326(13) -0.0595(3) -0.1688(13) 0.046(2) Uani 1 1 d . . . . .
H4BC H 0.3504 -0.0462 -0.2704 0.055 Uiso 0.5 1 calc R . . B 2
H4BD H 0.4331 -0.0453 -0.0521 0.055 Uiso 0.5 1 calc R . . B 2
H4AA H 0.4488 -0.0457 -0.0663 0.055 Uiso 0.5 1 calc R . . C 1
H4AB H 0.2301 -0.0457 -0.1533 0.055 Uiso 0.5 1 calc R . . C 1
O1A O 0.1997(17) -0.1451(7) -0.3551(16) 0.031(3) Uani 0.5 1 d . U . A 1
O2A O 0.2694(17) -0.1474(5) -0.0272(15) 0.029(3) Uani 0.5 1 d . . . A 1
O3A O 0.5235(14) -0.1444(5) -0.1043(17) 0.030(3) Uani 0.5 1 d . . . A 1
O1B O 0.1440(15) -0.1461(6) -0.3018(16) 0.026(3) Uani 0.5 1 d . . . A 2
O2B O 0.3984(19) -0.1450(5) 0.0242(14) 0.033(3) Uani 0.5 1 d . . . A 2
O3B O 0.4745(15) -0.1475(6) -0.2291(15) 0.032(3) Uani 0.5 1 d . . . A 2
C5B C 0.128(3) -0.0389(11) -0.198(3) 0.072(6) Uiso 0.5 1 d . . . D 2
H5BA H 0.0305 -0.0532 -0.3159 0.086 Uiso 0.5 1 calc R . . D 2
H5BB H 0.1105 -0.0546 -0.0992 0.086 Uiso 0.5 1 calc R . . D 2
C5A C 0.309(3) -0.0375(10) -0.372(3) 0.066(6) Uiso 0.5 1 d . . . D 1
H5AA H 0.4130 -0.0512 -0.3854 0.079 Uiso 0.5 1 calc R . . D 1
H5AB H 0.1948 -0.0526 -0.4737 0.079 Uiso 0.5 1 calc R . . D 1
C7A C 0.274(3) 0.0405(12) -0.576(3) 0.090 Uiso 0.5 1 d . . . D 1
H7AA H 0.2695 0.0800 -0.5862 0.135 Uiso 0.5 1 calc R . . D 1
H7AB H 0.3746 0.0266 -0.5913 0.135 Uiso 0.5 1 calc R . . D 1
H7AC H 0.1575 0.0253 -0.6712 0.135 Uiso 0.5 1 calc R . . D 1
C7B C -0.077(3) 0.0397(12) -0.218(3) 0.090 Uiso 0.5 1 d . . . D 2
H7BA H -0.0818 0.0792 -0.2164 0.135 Uiso 0.5 1 calc R . . D 2
H7BB H -0.1760 0.0262 -0.3344 0.135 Uiso 0.5 1 calc R . . D 2
H7BC H -0.0898 0.0250 -0.1165 0.135 Uiso 0.5 1 calc R . . D 2
C6A C 0.303(4) 0.0244(11) -0.388(3) 0.080 Uiso 0.5 1 d . . . D 1
H6AA H 0.2017 0.0386 -0.3710 0.096 Uiso 0.5 1 calc R . . D 1
H6AB H 0.4194 0.0399 -0.2910 0.096 Uiso 0.5 1 calc R . . D 1
C6B C 0.107(3) 0.0221(11) -0.197(3) 0.080 Uiso 0.5 1 d . . . D 2
H6BA H 0.1211 0.0378 -0.2983 0.096 Uiso 0.5 1 calc R . . D 2
H6BB H 0.2072 0.0367 -0.0806 0.096 Uiso 0.5 1 calc R . . D 2
N2B N 0.3774(19) -0.1986(6) 0.0321(16) 0.018(3) Uiso 0.5 1 d . . . A 2
N1A N 0.1759(17) -0.2000(6) -0.3605(16) 0.017(3) Uiso 0.5 1 d . . . A 1
N3A N 0.5322(17) -0.1987(6) -0.1257(18) 0.022(3) Uiso 0.5 1 d . . . A 1


_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 N1B 1.922(14) 4 ?
Fe1 N1B 1.922(14) . ?
Fe1 N2A 1.932(13) . ?
Fe1 N2A 1.932(13) 4 ?
Fe1 N3B 1.890(14) . ?
Fe1 N3B 1.890(14) 4 ?
Fe1 N2B 1.937(12) . ?
Fe1 N2B 1.937(12) 4 ?
Fe1 N1A 1.918(13) 4 ?
Fe1 N1A 1.918(13) . ?
Fe1 N3A 1.941(13) 4 ?
Fe1 N3A 1.941(13) . ?
Br1 C1 1.863(7) . ?
Br3 C3 1.846(7) . ?
Br2 C2 1.831(7) . ?
B1 C4 1.584(11) . ?
B1 O1A 1.478(15) . ?
B1 O2A 1.566(15) . ?
B1 O3A 1.467(14) . ?
B1 O1B 1.489(14) . ?
B1 O2B 1.464(14) . ?
B1 O3B 1.586(15) . ?
N1B C1 1.278(14) . ?
N1B O1B 1.34(2) . ?
N2A C2 1.301(13) . ?
N2A O2A 1.344(18) . ?
N3B C3 1.298(14) . ?
N3B O3B 1.379(18) . ?
C2 C2 1.432(18) 4 ?
C2 N2B 1.381(14) . ?
C1 C1 1.456(15) 4 ?
C1 N1A 1.294(14) . ?
C3 C3 1.407(17) 4 ?
C3 N3A 1.358(15) . ?
C4 C5B 1.65(2) . ?
C4 C5A 1.67(2) . ?
O1A N1A 1.34(2) . ?
O3A N3A 1.334(18) . ?
O2B N2B 1.316(18) . ?
C5B C6B 1.49(3) . ?
C5A C6A 1.50(3) . ?
C7A C6A 1.49(3) . ?
C7B C6B 1.50(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1B Fe1 N1B 76.3(9) 4 . ?
N1B Fe1 N2B 84.8(6) . . ?
N1B Fe1 N2B 134.8(6) . 4 ?
N1B Fe1 N2B 134.8(6) 4 . ?
N1B Fe1 N2B 84.8(6) 4 4 ?
N2A Fe1 N2A 73.7(8) . 4 ?
N2A Fe1 N3A 134.0(5) 4 . ?
N2A Fe1 N3A 85.7(6) . . ?
N2A Fe1 N3A 134.0(5) . 4 ?
N2A Fe1 N3A 85.7(6) 4 4 ?
N3B Fe1 N1B 87.4(6) . . ?
N3B Fe1 N1B 133.3(6) 4 . ?
N3B Fe1 N1B 133.3(6) . 4 ?
N3B Fe1 N1B 87.4(6) 4 4 ?
N3B Fe1 N3B 72.6(9) . 4 ?
N3B Fe1 N2B 132.9(6) . 4 ?
N3B Fe1 N2B 85.3(6) 4 4 ?
N3B Fe1 N2B 132.9(6) 4 . ?
N3B Fe1 N2B 85.3(6) . . ?
N2B Fe1 N2B 80.2(8) 4 . ?
N1A Fe1 N2A 85.2(5) . . ?
N1A Fe1 N2A 132.4(6) 4 . ?
N1A Fe1 N2A 132.4(6) . 4 ?
N1A Fe1 N2A 85.2(5) 4 4 ?
N1A Fe1 N1A 78.4(8) 4 . ?
N1A Fe1 N3A 84.5(6) 4 4 ?
N1A Fe1 N3A 135.6(5) 4 . ?
N1A Fe1 N3A 135.6(5) . 4 ?
N1A Fe1 N3A 84.5(6) . . ?
N3A Fe1 N3A 79.8(8) 4 . ?
C4 B1 O3B 109.7(9) . . ?
O1A B1 C4 108.8(9) . . ?
O1A B1 O2A 108.0(9) . . ?
O2A B1 C4 111.3(9) . . ?
O3A B1 C4 108.9(8) . . ?
O3A B1 O1A 111.5(10) . . ?
O3A B1 O2A 108.4(8) . . ?
O1B B1 C4 110.1(8) . . ?
O1B B1 O3B 107.1(9) . . ?
O2B B1 C4 110.4(8) . . ?
O2B B1 O1B 112.6(10) . . ?
O2B B1 O3B 106.8(8) . . ?
C1 N1B Fe1 115.9(11) . . ?
C1 N1B O1B 117.3(12) . . ?
O1B N1B Fe1 123.3(9) . . ?
C2 N2A Fe1 117.6(10) . . ?
C2 N2A O2A 116.2(11) . . ?
O2A N2A Fe1 123.1(9) . . ?
C3 N3B Fe1 119.5(10) . . ?
C3 N3B O3B 113.8(11) . . ?
O3B N3B Fe1 123.7(10) . . ?
N2A C2 Br2 123.7(9) . . ?
N2A C2 C2 109.9(7) . 4 ?
C2 C2 Br2 124.7(3) 4 . ?
N2B C2 Br2 121.1(8) . . ?
N2B C2 C2 112.6(7) . 4 ?
N1B C1 Br1 123.4(9) . . ?
N1B C1 C1 111.1(8) . 4 ?
C1 C1 Br1 123.8(2) 4 . ?
N1A C1 Br1 123.0(8) . . ?
N1A C1 C1 112.0(7) . 4 ?
N3B C3 Br3 124.7(9) . . ?
N3B C3 C3 108.7(7) . 4 ?
C3 C3 Br3 124.8(3) 4 . ?
N3A C3 Br3 120.4(8) . . ?
N3A C3 C3 113.5(7) . 4 ?
B1 C4 C5B 107.4(11) . . ?
B1 C4 C5A 109.5(11) . . ?
N1A O1A B1 112.7(10) . . ?
N2A O2A B1 113.0(10) . . ?
N3A O3A B1 113.1(10) . . ?
N1B O1B B1 114.6(10) . . ?
N2B O2B B1 113.3(10) . . ?
N3B O3B B1 111.7(10) . . ?
C6B C5B C4 114.3(18) . . ?
C6A C5A C4 112.7(17) . . ?
C7A C6A C5A 109(2) . . ?
C5B C6B C7B 113(2) . . ?
C2 N2B Fe1 113.0(9) . . ?
O2B N2B Fe1 124.7(9) . . ?
O2B N2B C2 120.4(11) . . ?
C1 N1A Fe1 115.3(10) . . ?
C1 N1A O1A 118.1(11) . . ?
O1A N1A Fe1 124.8(9) . . ?
C3 N3A Fe1 113.0(10) . . ?
O3A N3A Fe1 124.1(9) . . ?
O3A N3A C3 121.4(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3B_b Fe1 N3B_b C3 -29.3(13) 4 . . . ?
Fe1 N1B C1 Br1 -171.8(5) . . . . ?
Fe1 N1B C1 C1 22.7(11) . . . 4 ?
Fe1 N1B C1 N1A -74(3) . . . . ?
Fe1 N1B O1B B1 9.2(19) . . . . ?
Fe1 N2A C2 Br2 169.7(5) . . . . ?
Fe1 N2A C2 C2 -24.8(11) . . . 4 ?
Fe1 N2A C2 N2B 76(2) . . . . ?
Fe1 N2A O2A B1 -14.0(16) . . . . ?
Fe1 N3B C3 Br3 -169.8(5) . . . . ?
Fe1 N3B C3 C3 24.6(11) . . . 4 ?
Fe1 N3B C3 N3A -81(2) . . . . ?
Fe1 N3B O3B B1 13.7(15) . . . . ?
Br1 C1 N1A Fe1 173.3(5) . . . . ?
Br1 C1 N1A O1A 7.6(17) . . . . ?
Br3 C3 N3A Fe1 173.2(4) . . . . ?
Br3 C3 N3A O3A 6.7(16) . . . . ?
Br2 C2 N2B Fe1 -173.0(4) . . . . ?
Br2 C2 N2B O2B -8.1(17) . . . . ?
B1 C4 C5B C6B 177.9(17) . . . . ?
B1 C4 C5A C6A 178.6(16) . . . . ?
B1 O1A N1A Fe1 -14.0(18) . . . . ?
B1 O1A N1A C1 150.3(11) . . . . ?
B1 O3A N3A Fe1 -16.4(16) . . . . ?
B1 O3A N3A C3 148.6(11) . . . . ?
B1 O2B N2B Fe1 17.0(18) . . . . ?
B1 O2B N2B C2 -146.0(11) . . . . ?
N1B Fe1 N3B C3 -98.2(12) 4 . . . ?
N1B Fe1 N3B C3 -166.5(12) . . . . ?
N1B Fe1 N3B O3B 34.5(12) . . . . ?
N1B Fe1 N3B O3B 102.9(13) 4 . . . ?
N1B C1 N1A Fe1 74(3) . . . . ?
N1B C1 N1A O1A -92(3) . . . . ?
N2A Fe1 N3B C3 121.4(11) . . . . ?
N2A Fe1 N3B C3 48.4(19) 4 . . . ?
N2A Fe1 N3B O3B -37.6(12) . . . . ?
N2A Fe1 N3B O3B -110.6(15) 4 . . . ?
N2A C2 N2B Fe1 -69(2) . . . . ?
N2A C2 N2B O2B 96(2) . . . . ?
N3B Fe1 N3B O3B 171.7(9) 4 . . . ?
N3B C3 N3A Fe1 65(2) . . . . ?
N3B C3 N3A O3A -101(2) . . . . ?
C2 N2A O2A B1 145.3(11) . . . . ?
C2 C2 N2B Fe1 20.8(9) 4 . . . ?
C2 C2 N2B O2B -174.4(10) 4 . . . ?
C1 N1B O1B B1 -148.6(12) . . . . ?
C1 C1 N1A Fe1 -19.2(10) 4 . . . ?
C1 C1 N1A O1A 175.1(10) 4 . . . ?
C3 N3B O3B B1 -146.4(10) . . . . ?
C3 C3 N3A Fe1 -19.3(9) 4 . . . ?
C3 C3 N3A O3A 174.2(10) 4 . . . ?
C4 B1 O1A N1A -173.2(12) . . . . ?
C4 B1 O2A N2A -172.3(10) . . . . ?
C4 B1 O3A N3A -170.0(10) . . . . ?
C4 B1 O1B N1B 173.9(12) . . . . ?
C4 B1 O2B N2B 171.1(11) . . . . ?
C4 B1 O3B N3B 173.0(10) . . . . ?
C4 C5B C6B C7B -178.3(17) . . . . ?
C4 C5A C6A C7A -177.6(17) . . . . ?
O1A B1 C4 C5B 69.1(13) . . . . ?
O1A B1 C4 C5A -36.8(14) . . . . ?
O1A B1 O2A N2A 68.3(13) . . . . ?
O1A B1 O3A N3A -49.9(15) . . . . ?
O1A B1 O1B N1B 81(2) . . . . ?
O1A B1 O2B N2B 22(2) . . . . ?
O1A B1 O3B N3B -80.5(12) . . . . ?
O2A B1 C4 C5B -49.8(13) . . . . ?
O2A B1 C4 C5A -155.8(11) . . . . ?
O2A B1 O1A N1A -52.2(15) . . . . ?
O2A B1 O3A N3A 68.9(13) . . . . ?
O2A B1 O1B N1B -77.0(13) . . . . ?
O2A B1 O2B N2B 72.8(14) . . . . ?
O2A B1 O3B N3B 24.7(16) . . . . ?
O2A N2A C2 Br2 9.3(18) . . . . ?
O2A N2A C2 C2 174.8(10) . . . 4 ?
O2A N2A C2 N2B -84(2) . . . . ?
O3A B1 C4 C5B -169.1(12) . . . . ?
O3A B1 C4 C5A 84.9(13) . . . . ?
O3A B1 O1A N1A 66.7(14) . . . . ?
O3A B1 O2A N2A -52.6(13) . . . . ?
O3A B1 O1B N1B 29(2) . . . . ?
O3A B1 O2B N2B -83.7(12) . . . . ?
O3A B1 O3B N3B 78.3(13) . . . . ?
O1B B1 C4 C5B 37.1(14) . . . . ?
O1B B1 C4 C5A -68.9(13) . . . . ?
O1B B1 O1A N1A -75.4(19) . . . . ?
O1B B1 O2A N2A 79.9(12) . . . . ?
O1B B1 O3A N3A -24.8(19) . . . . ?
O1B B1 O2B N2B 47.6(15) . . . . ?
O1B B1 O3B N3B -67.5(12) . . . . ?
O1B N1B C1 Br1 -12.3(19) . . . . ?
O1B N1B C1 C1 -177.8(11) . . . 4 ?
O1B N1B C1 N1A 85(3) . . . . ?
O2B B1 C4 C5B -87.9(13) . . . . ?
O2B B1 C4 C5A 166.2(12) . . . . ?
O2B B1 O1A N1A -24(2) . . . . ?
O2B B1 O2A N2A -76.6(14) . . . . ?
O2B B1 O3A N3A 83.0(12) . . . . ?
O2B B1 O1B N1B -62.5(15) . . . . ?
O2B B1 O3B N3B 53.4(13) . . . . ?
O3B B1 C4 C5B 154.7(11) . . . . ?
O3B B1 C4 C5A 48.8(12) . . . . ?
O3B B1 O1A N1A 79.3(13) . . . . ?
O3B B1 O2A N2A -24.2(17) . . . . ?
O3B B1 O3A N3A -72.4(14) . . . . ?
O3B B1 O1B N1B 54.6(15) . . . . ?
O3B B1 O2B N2B -69.7(14) . . . . ?
O3B N3B C3 Br3 -8.8(17) . . . . ?
O3B N3B C3 C3 -174.4(9) . . . 4 ?
O3B N3B C3 N3A 80(2) . . . . ?
C5B C4 C5A C6A 67(2) . . . . ?
C5A C4 C5B C6B -69(2) . . . . ?
N2B Fe1 N3B C3 36.6(15) 4 . . . ?
N2B Fe1 N3B C3 108.5(11) . . . . ?
N2B Fe1 N3B O3B -50.4(12) . . . . ?
N2B Fe1 N3B O3B -122.3(12) 4 . . . ?
N1A Fe1 N3B C3 -89.5(12) 4 . . . ?
N1A Fe1 N3B C3 -156.4(12) . . . . ?
N1A Fe1 N3B O3B 44.6(11) . . . . ?
N1A Fe1 N3B O3B 111.6(12) 4 . . . ?
N3A Fe1 N3B C3 -11.8(12) 4 . . . ?
N3A Fe1 N3B C3 79(2) . . . . ?
N3A Fe1 N3B O3B -80(2) . . . . ?
N3A Fe1 N3B O3B -170.8(12) 4 . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_260
_database_code_depnum_ccdc_archive 'CCDC 1027574'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.1967(17)
_cell_length_b                   24.248(5)
_cell_length_c                   8.1999(18)
_cell_angle_alpha                90
_cell_angle_beta                 119.392(3)
_cell_angle_gamma                90
_cell_volume                     1420.0(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2222
_cell_measurement_temperature    260
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.013
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.1147
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12344
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.659
_diffrn_reflns_theta_min         2.520
_diffrn_ambient_temperature      260
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1926
_reflns_number_total             3613
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0579
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1507
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim N1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2 \\sim N2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3 \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
: with sigma of 0.008 and sigma for terminal atoms of 0.008
3. Others
 Fixed Sof: N1(0.5) N2(0.5) N3(0.5) H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5)
 O1A(0.5) O2A(0.5) O3A(0.5) O1B(0.5) O2B(0.5) O3B(0.5) C5B(0.5) H5BA(0.5)
 H5BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) N1A(0.5) N2A(0.5) N3A(0.5)
 Fixed Uiso: C7A(0.09) C7B(0.09) C6A(0.08) C6B(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C5B(H5BA,H5BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB)
4.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3364(2) -0.2500 -0.16384(19) 0.0196(3) Uani 1 2 d S T P . .
Br1 Br -0.16923(13) -0.17726(4) -0.66935(12) 0.0427(3) Uani 1 1 d . . . . .
Br3 Br 0.85017(14) -0.17758(5) -0.15819(16) 0.0506(3) Uani 1 1 d . . . . .
Br2 Br 0.34175(17) -0.17758(5) 0.35033(12) 0.0507(3) Uani 1 1 d . . . . .
B1 B 0.3330(13) -0.1244(4) -0.1658(13) 0.033(2) Uani 1 1 d . . . . .
N1 N 0.1371(18) -0.2001(7) -0.3219(18) 0.020(3) Uiso 0.5 1 d . . . A 2
N2 N 0.293(2) -0.2024(6) -0.0017(17) 0.019(3) Uiso 0.5 1 d . U . A 1
N3 N 0.4993(18) -0.2029(6) -0.2057(19) 0.021(3) Uiso 0.5 1 d . . . A 2
C2 C 0.3373(12) -0.2206(4) 0.1645(9) 0.034(2) Uani 1 1 d . . . . .
C1 C 0.0160(10) -0.2199(3) -0.4826(9) 0.0267(19) Uani 1 1 d . . . . .
C3 C 0.6643(10) -0.2207(4) -0.1611(10) 0.028(2) Uani 1 1 d . . . . .
C4 C 0.3322(14) -0.0595(3) -0.1680(13) 0.045(2) Uani 1 1 d . . . . .
H4BC H 0.3498 -0.0462 -0.2698 0.054 Uiso 0.5 1 calc R . . B 2
H4BD H 0.4335 -0.0455 -0.0513 0.054 Uiso 0.5 1 calc R . . B 2
H4AA H 0.4478 -0.0456 -0.0649 0.054 Uiso 0.5 1 calc R . . C 1
H4AB H 0.2286 -0.0458 -0.1540 0.054 Uiso 0.5 1 calc R . . C 1
O1A O 0.1988(15) -0.1454(5) -0.3520(14) 0.024(3) Uani 0.5 1 d . . . A 1
O2A O 0.2734(15) -0.1478(5) -0.0237(13) 0.025(2) Uiso 0.5 1 d . . . A 1
O3A O 0.5257(15) -0.1443(5) -0.1007(15) 0.033(3) Uiso 0.5 1 d . . . A 1
O1B O 0.1453(16) -0.1454(6) -0.2978(16) 0.028(3) Uiso 0.5 1 d . . . A 2
O2B O 0.4009(16) -0.1451(5) 0.0264(14) 0.029(3) Uiso 0.5 1 d . . . A 2
O3B O 0.4768(14) -0.1469(5) -0.2271(14) 0.027(2) Uiso 0.5 1 d . . . A 2
C5B C 0.130(3) -0.0380(11) -0.196(3) 0.064(6) Uiso 0.5 1 d . . . D 2
H5BA H 0.0310 -0.0525 -0.3131 0.077 Uiso 0.5 1 calc R . . D 2
H5BB H 0.1123 -0.0536 -0.0962 0.077 Uiso 0.5 1 calc R . . D 2
C5A C 0.311(3) -0.0384(10) -0.369(3) 0.062(6) Uiso 0.5 1 d . . . D 1
H5AA H 0.4148 -0.0528 -0.3811 0.075 Uiso 0.5 1 calc R . . D 1
H5AB H 0.1965 -0.0537 -0.4704 0.075 Uiso 0.5 1 calc R . . D 1
C7A C 0.272(4) 0.0391(13) -0.581(3) 0.090 Uiso 0.5 1 d . . . D 1
H7AA H 0.2034 0.0104 -0.6691 0.135 Uiso 0.5 1 calc GR . . D 1
H7AB H 0.3906 0.0442 -0.5773 0.135 Uiso 0.5 1 calc GR . . D 1
H7AC H 0.2022 0.0728 -0.6197 0.135 Uiso 0.5 1 calc GR . . D 1
C7B C -0.077(3) 0.0393(13) -0.222(4) 0.090 Uiso 0.5 1 d . . . D 2
H7BA H -0.1431 0.0593 -0.3369 0.135 Uiso 0.5 1 calc GR . . D 2
H7BB H -0.0584 0.0626 -0.1193 0.135 Uiso 0.5 1 calc GR . . D 2
H7BC H -0.1483 0.0074 -0.2252 0.135 Uiso 0.5 1 calc GR . . D 2
C6A C 0.306(4) 0.0232(11) -0.391(3) 0.080 Uiso 0.5 1 d . . . D 1
H6AA H 0.2066 0.0383 -0.3718 0.096 Uiso 0.5 1 calc R . . D 1
H6AB H 0.4235 0.0387 -0.2964 0.096 Uiso 0.5 1 calc R . . D 1
C6B C 0.107(3) 0.0215(12) -0.196(4) 0.080 Uiso 0.5 1 d . . . D 2
H6BA H 0.1237 0.0374 -0.2947 0.096 Uiso 0.5 1 calc R . . D 2
H6BB H 0.2041 0.0362 -0.0777 0.096 Uiso 0.5 1 calc R . . D 2
N1A N 0.1769(19) -0.2005(7) -0.3598(17) 0.019(3) Uiso 0.5 1 d . . . A 1
N2A N 0.380(2) -0.1987(6) 0.0356(17) 0.021(3) Uiso 0.5 1 d . . . A 2
N3A N 0.5332(19) -0.1985(6) -0.1226(19) 0.025(3) Uiso 0.5 1 d . . . A 1


_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 N1 1.932(14) 4 ?
Fe1 N1 1.932(14) . ?
Fe1 N2 1.921(13) . ?
Fe1 N2 1.921(13) 4 ?
Fe1 N3 1.912(14) . ?
Fe1 N3 1.912(14) 4 ?
Fe1 N1A 1.915(14) 4 ?
Fe1 N1A 1.915(14) . ?
Fe1 N2A 1.943(13) . ?
Fe1 N2A 1.944(13) 4 ?
Fe1 N3A 1.934(14) . ?
Fe1 N3A 1.934(14) 4 ?
Br1 C1 1.854(7) . ?
Br3 C3 1.839(8) . ?
Br2 C2 1.833(8) . ?
B1 C4 1.573(12) . ?
B1 O1A 1.468(13) . ?
B1 O2A 1.573(15) . ?
B1 O3A 1.478(15) . ?
B1 O1B 1.471(15) . ?
B1 O2B 1.478(14) . ?
B1 O3B 1.589(15) . ?
N1 C1 1.292(14) . ?
N1 O1B 1.34(2) . ?
N2 C2 1.303(14) . ?
N2 O2A 1.337(18) . ?
N3 C3 1.290(15) . ?
N3 O3B 1.369(18) . ?
C2 C2 1.424(19) 4 ?
C2 N2A 1.371(15) . ?
C1 C1 1.458(17) 4 ?
C1 N1A 1.293(15) . ?
C3 C3 1.420(18) 4 ?
C3 N3A 1.370(16) . ?
C4 C5B 1.65(2) . ?
C4 C5A 1.65(2) . ?
O1A N1A 1.35(2) . ?
O3A N3A 1.333(19) . ?
O2B N2A 1.318(18) . ?
C5B C6B 1.46(3) . ?
C5A C6A 1.50(3) . ?
C7A C6A 1.50(3) . ?
C7B C6B 1.47(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 77.5(9) . 4 ?
N1 Fe1 N2A 84.8(6) . . ?
N1 Fe1 N2A 135.2(6) 4 . ?
N1 Fe1 N2A 84.8(6) 4 4 ?
N1 Fe1 N2A 135.2(6) . 4 ?
N2 Fe1 N2 73.8(8) . 4 ?
N2 Fe1 N3A 133.5(6) 4 . ?
N2 Fe1 N3A 133.5(6) . 4 ?
N2 Fe1 N3A 85.1(6) . . ?
N2 Fe1 N3A 85.1(6) 4 4 ?
N3 Fe1 N1 86.6(6) . . ?
N3 Fe1 N1 133.5(6) 4 . ?
N3 Fe1 N1 133.5(6) . 4 ?
N3 Fe1 N1 86.6(6) 4 4 ?
N3 Fe1 N3 73.4(9) . 4 ?
N3 Fe1 N2A 85.0(6) . . ?
N3 Fe1 N2A 132.7(6) 4 . ?
N3 Fe1 N2A 85.0(6) 4 4 ?
N3 Fe1 N2A 132.7(6) . 4 ?
N1A Fe1 N2 85.6(6) 4 4 ?
N1A Fe1 N2 132.4(6) . 4 ?
N1A Fe1 N2 85.6(6) . . ?
N1A Fe1 N2 132.4(6) 4 . ?
N1A Fe1 N1A 77.5(9) . 4 ?
N1A Fe1 N3A 135.9(6) 4 . ?
N1A Fe1 N3A 135.9(6) . 4 ?
N1A Fe1 N3A 84.8(6) . . ?
N1A Fe1 N3A 84.8(6) 4 4 ?
N2A Fe1 N2A 79.6(8) . 4 ?
N3A Fe1 N3A 80.4(9) 4 . ?
C4 B1 O2A 111.6(9) . . ?
C4 B1 O3B 109.9(9) . . ?
O1A B1 C4 109.8(8) . . ?
O1A B1 O2A 107.4(8) . . ?
O1A B1 O3A 112.6(10) . . ?
O3A B1 C4 109.2(9) . . ?
O3A B1 O2A 106.3(8) . . ?
O1B B1 C4 109.9(9) . . ?
O1B B1 O2B 112.1(10) . . ?
O1B B1 O3B 108.6(9) . . ?
O2B B1 C4 110.5(8) . . ?
O2B B1 O3B 105.7(8) . . ?
C1 N1 Fe1 115.1(11) . . ?
C1 N1 O1B 118.5(12) . . ?
O1B N1 Fe1 123.8(9) . . ?
C2 N2 Fe1 118.0(10) . . ?
C2 N2 O2A 115.5(11) . . ?
O2A N2 Fe1 123.5(9) . . ?
C3 N3 Fe1 118.5(10) . . ?
C3 N3 O3B 115.1(12) . . ?
O3B N3 Fe1 123.6(10) . . ?
N2 C2 Br2 123.9(9) . . ?
N2 C2 C2 109.8(7) . 4 ?
C2 C2 Br2 124.7(3) 4 . ?
N2A C2 Br2 120.7(8) . . ?
N2A C2 C2 112.8(7) . 4 ?
N1 C1 Br1 122.9(9) . . ?
N1 C1 C1 111.8(8) . 4 ?
C1 C1 Br1 123.9(2) 4 . ?
N1A C1 Br1 123.3(9) . . ?
N1A C1 C1 111.3(8) . 4 ?
N3 C3 Br3 124.1(9) . . ?
N3 C3 C3 109.6(8) . 4 ?
C3 C3 Br3 124.7(3) 4 . ?
N3A C3 Br3 120.8(9) . . ?
N3A C3 C3 113.1(7) . 4 ?
B1 C4 C5B 108.5(12) . . ?
B1 C4 C5A 108.6(11) . . ?
N1A O1A B1 114.2(10) . . ?
N2 O2A B1 113.4(10) . . ?
N3A O3A B1 112.7(10) . . ?
N1 O1B B1 114.2(11) . . ?
N2A O2B B1 113.9(10) . . ?
N3 O3B B1 112.0(10) . . ?
C6B C5B C4 115.9(19) . . ?
C6A C5A C4 114.2(18) . . ?
C7A C6A C5A 111(2) . . ?
C5B C6B C7B 114(2) . . ?
C1 N1A Fe1 116.2(11) . . ?
C1 N1A O1A 117.4(12) . . ?
O1A N1A Fe1 124.2(9) . . ?
C2 N2A Fe1 112.9(10) . . ?
O2B N2A Fe1 123.9(9) . . ?
O2B N2A C2 121.1(11) . . ?
C3 N3A Fe1 112.8(10) . . ?
O3A N3A Fe1 124.8(10) . . ?
O3A N3A C3 120.8(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2A_a N2_a C2 N2A_b -84(2) . . . . ?
Fe1 N1 C1 Br1 -171.9(5) . . . . ?
Fe1 N1 C1 C1 21.1(11) . . . 4 ?
Fe1 N1 C1 N1A -73(3) . . . . ?
Fe1 N1 O1B B1 12.2(19) . . . . ?
Fe1 N2 C2 Br2 169.7(5) . . . . ?
Fe1 N2 C2 C2 -24.0(11) . . . 4 ?
Fe1 N2 C2 N2A 78(2) . . . . ?
Fe1 N2 O2A B1 -12.7(16) . . . . ?
Fe1 N3 C3 Br3 -170.3(5) . . . . ?
Fe1 N3 C3 C3 23.9(11) . . . 4 ?
Fe1 N3 C3 N3A -79(2) . . . . ?
Fe1 N3 O3B B1 13.6(15) . . . . ?
Br1 C1 N1A Fe1 173.5(5) . . . . ?
Br1 C1 N1A O1A 9.9(18) . . . . ?
Br3 C3 N3A Fe1 173.0(5) . . . . ?
Br3 C3 N3A O3A 6.8(17) . . . . ?
Br2 C2 N2A Fe1 -173.1(5) . . . . ?
Br2 C2 N2A O2B -8.9(17) . . . . ?
B1 C4 C5B C6B 178.3(18) . . . . ?
B1 C4 C5A C6A 179.3(18) . . . . ?
B1 O1A N1A Fe1 -11.5(19) . . . . ?
B1 O1A N1A C1 150.6(11) . . . . ?
B1 O3A N3A Fe1 -17.1(16) . . . . ?
B1 O3A N3A C3 147.4(11) . . . . ?
B1 O2B N2A Fe1 17.7(17) . . . . ?
B1 O2B N2A C2 -144.7(11) . . . . ?
N1 C1 N1A Fe1 76(3) . . . . ?
N1 C1 N1A O1A -87(3) . . . . ?
N2 C2 N2A Fe1 -68(2) . . . . ?
N2 C2 N2A O2B 96(2) . . . . ?
N3 C3 N3A Fe1 68(2) . . . . ?
N3 C3 N3A O3A -99(3) . . . . ?
C2 N2 O2A B1 147.2(11) . . . . ?
C2 C2 N2A Fe1 21.3(10) 4 . . . ?
C2 C2 N2A O2B -174.5(10) 4 . . . ?
C1 N1 O1B B1 -148.9(12) . . . . ?
C1 C1 N1A Fe1 -19.8(11) 4 . . . ?
C1 C1 N1A O1A 176.7(10) 4 . . . ?
C3 N3 O3B B1 -147.0(10) . . . . ?
C3 C3 N3A Fe1 -19.8(10) 4 . . . ?
C3 C3 N3A O3A 174.0(10) 4 . . . ?
C4 B1 O1A N1A -174.2(12) . . . . ?
C4 B1 O2A N2 -172.8(10) . . . . ?
C4 B1 O3A N3A -170.2(10) . . . . ?
C4 B1 O1B N1 172.6(12) . . . . ?
C4 B1 O2B N2A 170.5(11) . . . . ?
C4 B1 O3B N3 172.6(9) . . . . ?
C4 C5B C6B C7B 179.7(19) . . . . ?
C4 C5A C6A C7A -176.0(19) . . . . ?
O1A B1 C4 C5B 68.2(14) . . . . ?
O1A B1 C4 C5A -38.6(14) . . . . ?
O1A B1 O2A N2 66.9(13) . . . . ?
O1A B1 O3A N3A -47.9(14) . . . . ?
O1A B1 O1B N1 77.3(18) . . . . ?
O1A B1 O2B N2A 21.9(19) . . . . ?
O1A B1 O3B N3 -79.4(11) . . . . ?
O2A B1 C4 C5B -50.7(13) . . . . ?
O2A B1 C4 C5A -157.5(12) . . . . ?
O2A B1 O1A N1A -52.8(15) . . . . ?
O2A B1 O3A N3A 69.4(12) . . . . ?
O2A B1 O1B N1 -77.9(13) . . . . ?
O2A B1 O2B N2A 71.9(13) . . . . ?
O2A B1 O3B N3 25.9(15) . . . . ?
O2A N2 C2 Br2 8.5(18) . . . . ?
O2A N2 C2 C2 174.9(10) . . . 4 ?
O3A B1 C4 C5B -167.8(11) . . . . ?
O3A B1 C4 C5A 85.4(13) . . . . ?
O3A B1 O1A N1A 63.9(15) . . . . ?
O3A B1 O2A N2 -53.9(13) . . . . ?
O3A B1 O1B N1 25(2) . . . . ?
O3A B1 O2B N2A -84.5(12) . . . . ?
O3A B1 O3B N3 77.5(13) . . . . ?
O1B B1 C4 C5B 36.2(14) . . . . ?
O1B B1 C4 C5A -70.6(14) . . . . ?
O1B B1 O1A N1A -78.4(18) . . . . ?
O1B B1 O2A N2 79.6(12) . . . . ?
O1B B1 O3A N3A -22.5(19) . . . . ?
O1B B1 O2B N2A 47.5(15) . . . . ?
O1B B1 O3B N3 -67.1(12) . . . . ?
O1B N1 C1 Br1 -9.2(19) . . . . ?
O1B N1 C1 C1 -176.2(11) . . . 4 ?
O1B N1 C1 N1A 90(3) . . . . ?
O2B B1 C4 C5B -88.1(13) . . . . ?
O2B B1 C4 C5A 165.1(12) . . . . ?
O2B B1 O1A N1A -25.5(19) . . . . ?
O2B B1 O2A N2 -77.6(13) . . . . ?
O2B B1 O3A N3A 83.2(12) . . . . ?
O2B B1 O1B N1 -64.0(15) . . . . ?
O2B B1 O3B N3 53.4(12) . . . . ?
O3B B1 C4 C5B 155.7(11) . . . . ?
O3B B1 C4 C5A 48.9(13) . . . . ?
O3B B1 O1A N1A 77.7(13) . . . . ?
O3B B1 O2A N2 -26.4(15) . . . . ?
O3B B1 O3A N3A -72.7(13) . . . . ?
O3B B1 O1B N1 52.4(15) . . . . ?
O3B B1 O2B N2A -70.6(13) . . . . ?
O3B N3 C3 Br3 -8.6(17) . . . . ?
O3B N3 C3 C3 -174.3(9) . . . 4 ?
O3B N3 C3 N3A 83(2) . . . . ?
C5B C4 C5A C6A 66(2) . . . . ?
C5A C4 C5B C6B -68(2) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_250
_database_code_depnum_ccdc_archive 'CCDC 1027575'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   8.2708(18)
_cell_length_b                   24.252(5)
_cell_length_c                   16.382(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.32
_cell_angle_gamma                90.00
_cell_volume                     2836.5(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2537
_cell_measurement_temperature    250
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.85
_exptl_absorpt_coefficient_mu    9.024
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.1190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2174
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7822
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         1.67
_diffrn_ambient_temperature      250
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_number_gt                2731
_reflns_number_total             7823
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.437
_refine_diff_density_rms         0.242
_refine_ls_extinction_coef       0.00098(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         7823
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.2435
_refine_ls_R_factor_gt           0.0834
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.2019
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H8AA(0.5) H8AB(0.5) H8BC(0.5) H8BD(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C10A(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C13A(0.5) H13C(0.5)
 H13D(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
 Fixed Uiso: H7A(0.041) H7B(0.041) H8AA(0.077) H8AB(0.077) H8BC(0.077)
 H8BD(0.077) H9A(0.112) H9B(0.112) H10A(0.112) H10B(0.112) H10C(0.112)
 H11A(0.043) H11B(0.043) H12A(0.071) H12B(0.071) H12C(0.071) H12D(0.071)
 H13A(0.13) H13B(0.13) H14A(0.131) H14B(0.131) H14C(0.131) H10D(0.112)
 H10E(0.112) H10F(0.112) H9AA(0.112) H9AB(0.112) H13C(0.13) H13D(0.13)
 H14D(0.131) H14E(0.131) H14F(0.131)
 Fixed X: H7A(0.7543) H7B(0.9714) H8AA(0.6978) H8AB(0.9152) H8BC(0.8888)
 H8BD(0.6789) H9A(0.6743) H9B(0.8921) H10A(0.6259) H10B(0.8429) H10C(0.721)
 H11A(0.8432) H11B(0.9221) H12A(0.6133) H12B(0.5365) H12C(0.6088) H12D(0.531)
 H13A(0.6593) H13B(0.6498) H14A(0.3226) H14B(0.4256) H14C(0.4076) H10D(0.7295)
 H10E(0.7969) H10F(0.9457) H9AA(0.9688) H9AB(0.7562) H13C(0.7441) H13D(0.6376)
 H14D(0.4336) H14E(0.3695) H14F(0.3272)
 Fixed Y: H7A(0.0426) H7B(0.0454) H8AA(0.058) H8AB(0.0499) H8BC(0.0603)
 H8BD(0.0474) H9A(-0.0364) H9B(-0.0444) H10A(-0.0166) H10B(-0.0236) H10C(-
 0.0753) H11A(0.4544) H11B(0.4547) H12A(0.4434) H12B(0.4444) H12C(0.4463)
 H12D(0.4472) H13A(0.5292) H13B(0.535) H14A(0.5182) H14B(0.5668) H14C(0.5683)
 H10D(-0.073) H10E(-0.0178) H10F(-0.0626) H9AA(-0.0264) H9AB(-0.0385)
 H13C(0.5374) H13D(0.5386) H14D(0.5236) H14E(0.5675) H14F(0.5041)
 Fixed Z: H7A(0.4513) H7B(0.5263) H8AA(0.5805) H8AB(0.6501) H8BC(0.6461)
 H8BD(0.5685) H9A(0.5274) H9B(0.5999) H10A(0.6523) H10B(0.7249) H10C(0.668)
 H11A(0.5514) H11B(0.481) H12A(0.3523) H12B(0.4227) H12C(0.3497) H12D(0.4209)
 H13A(0.3612) H13B(0.4536) H14A(0.314) H14B(0.2938) H14C(0.3855) H10D(0.6611)
 H10E(0.7207) H10F(0.7314) H9AA(0.6233) H9AB(0.5529) H13C(0.4077) H13D(0.467)
 H14D(0.25) H14E(0.2995) H14F(0.3026)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Br1 Br 0.32817(16) 0.17728(7) 0.49618(9) 0.0408(4) Uani 1 d . . . .
Br2 Br 0.33540(16) 0.32274(7) 0.50357(9) 0.0414(4) Uani 1 d . . . .
Br3 Br 1.34434(15) 0.18017(7) 0.76032(9) 0.0423(4) Uani 1 d . . . .
Br4 Br 1.35865(15) 0.32473(7) 0.74860(9) 0.0407(4) Uani 1 d . . . .
Br5 Br 0.86193(18) 0.17523(7) 0.25147(9) 0.0408(4) Uani 1 d . . . .
Br6 Br 0.82324(18) 0.31991(7) 0.23941(9) 0.0420(4) Uani 1 d . . . .
Fe1 Fe 0.83681(18) 0.25004(9) 0.49961(10) 0.0181(3) Uani 1 d . . . .
O1 O 0.6500(9) 0.1457(4) 0.4743(5) 0.031(2) Uani 1 d B . . .
O2 O 0.7020(9) 0.3554(4) 0.5259(5) 0.030(2) Uani 1 d D . . .
O3 O 0.9759(10) 0.1471(4) 0.6016(5) 0.031(2) Uani 1 d B . . .
O4 O 1.0271(9) 0.3549(4) 0.5625(5) 0.037(2) Uani 1 d D . . .
O5 O 0.8994(10) 0.1448(4) 0.4375(5) 0.032(2) Uani 1 d B . . .
O6 O 0.7741(10) 0.3529(4) 0.3982(5) 0.031(2) Uani 1 d D . . .
N1 N 0.6406(11) 0.2007(5) 0.4810(6) 0.023(3) Uani 1 d . . . .
N2 N 0.6779(12) 0.2992(5) 0.5181(6) 0.026(3) Uani 1 d . . . .
N3 N 1.0001(12) 0.2018(5) 0.6008(7) 0.028(3) Uani 1 d . . . .
N4 N 1.0355(11) 0.3003(5) 0.5798(6) 0.025(2) Uani 1 d . . . .
N5 N 0.8775(12) 0.1999(5) 0.4212(6) 0.026(2) Uani 1 d . . . .
N6 N 0.7991(12) 0.2995(5) 0.3983(6) 0.025(2) Uani 1 d . . . .
C1 C 0.5108(14) 0.2196(6) 0.4938(8) 0.024(3) Uani 1 d . . . U
C2 C 0.5241(14) 0.2799(6) 0.5062(8) 0.026(3) Uani 1 d . . . U
C3 C 1.1567(14) 0.2227(5) 0.6678(7) 0.022(3) Uani 1 d . . . U
C4 C 1.1717(13) 0.2801(5) 0.6577(7) 0.022(3) Uani 1 d . . . U
C5 C 0.8555(13) 0.2198(5) 0.3410(7) 0.020(3) Uani 1 d . . . U
C6 C 0.8228(14) 0.2770(6) 0.3322(7) 0.024(3) Uani 1 d . . . U
C7 C 0.8477(18) 0.0585(6) 0.5120(8) 0.034(3) Uani 1 d B . . .
H7A H 0.7543 0.0426 0.4513 0.041 Uiso 1 calc . . R .
H7B H 0.9714 0.0454 0.5263 0.041 Uiso 1 calc . . R .
C8 C 0.810(2) 0.0391(7) 0.5884(12) 0.064(5) Uani 1 d . . . .
H8AA H 0.6978 0.0580 0.5805 0.077 Uiso 0.50 calc A 1 R .
H8AB H 0.9152 0.0499 0.6501 0.077 Uiso 0.50 calc A 1 R .
H8BC H 0.8888 0.0603 0.6461 0.077 Uiso 0.50 calc A 2 R .
H8BD H 0.6789 0.0474 0.5685 0.077 Uiso 0.50 calc A 2 R .
C9 C 0.779(7) -0.025(3) 0.589(4) 0.093(11) Uiso 0.50 d B 1 . .
H9A H 0.6743 -0.0364 0.5274 0.112 Uiso 0.50 calc B 1 R .
H9B H 0.8921 -0.0444 0.5999 0.112 Uiso 0.50 calc B 1 R .
C10 C 0.739(5) -0.0360(18) 0.665(3) 0.074(9) Uiso 0.50 d B 1 . .
H10A H 0.6259 -0.0166 0.6523 0.112 Uiso 0.50 calc B 1 GR .
H10B H 0.8429 -0.0236 0.7249 0.112 Uiso 0.50 calc B 1 GR .
H10C H 0.7210 -0.0753 0.6680 0.112 Uiso 0.50 calc B 1 GR .
C11 C 0.8225(16) 0.4403(6) 0.4909(9) 0.036(3) Uani 1 d D . . .
H11A H 0.8432 0.4544 0.5514 0.043 Uiso 1 calc . . R .
H11B H 0.9221 0.4547 0.4810 0.043 Uiso 1 calc . . R .
C12 C 0.632(2) 0.4602(6) 0.4108(11) 0.059(5) Uani 1 d . . D .
H12A H 0.6133 0.4434 0.3523 0.071 Uiso 0.50 calc C 1 R .
H12B H 0.5365 0.4444 0.4227 0.071 Uiso 0.50 calc C 1 R .
H12C H 0.6088 0.4463 0.3497 0.071 Uiso 0.50 calc C 2 R .
H12D H 0.5310 0.4472 0.4209 0.071 Uiso 0.50 calc C 2 R .
C13 C 0.59(3) 0.518(2) 0.391(13) 0.108(9) Uiso 0.50 d D 1 . .
H13A H 0.6593 0.5292 0.3612 0.130 Uiso 0.50 calc D 1 R .
H13B H 0.6498 0.5350 0.4536 0.130 Uiso 0.50 calc D 1 R .
C14 C 0.425(6) 0.545(2) 0.343(3) 0.087(9) Uiso 0.50 d D 1 . .
H14A H 0.3226 0.5182 0.3140 0.131 Uiso 0.50 calc D 1 GR .
H14B H 0.4256 0.5668 0.2938 0.131 Uiso 0.50 calc D 1 GR .
H14C H 0.4076 0.5683 0.3855 0.131 Uiso 0.50 calc D 1 GR .
B1 B 0.8408(18) 0.1242(7) 0.5037(9) 0.028(4) Uani 1 d . . . .
B2 B 0.8311(17) 0.3770(8) 0.4940(10) 0.032(4) Uani 1 d . . . .
C10A C 0.827(5) -0.0453(18) 0.688(3) 0.074(9) Uiso 0.50 d B 2 . .
H10D H 0.7295 -0.0730 0.6611 0.112 Uiso 0.50 calc B 2 GR .
H10E H 0.7969 -0.0178 0.7207 0.112 Uiso 0.50 calc B 2 GR .
H10F H 0.9457 -0.0626 0.7314 0.112 Uiso 0.50 calc B 2 GR .
C9A C 0.842(7) -0.019(3) 0.611(4) 0.093(11) Uiso 0.50 d B 2 . .
H9AA H 0.9688 -0.0264 0.6233 0.112 Uiso 0.50 calc B 2 R .
H9AB H 0.7562 -0.0385 0.5529 0.112 Uiso 0.50 calc B 2 R .
C13A C 0.64(3) 0.5227(10) 0.412(13) 0.108(9) Uiso 0.50 d D 2 D .
H13C H 0.7441 0.5374 0.4077 0.130 Uiso 0.50 calc D 2 R .
H13D H 0.6376 0.5386 0.4670 0.130 Uiso 0.50 calc D 2 R .
C14A C 0.416(6) 0.530(2) 0.303(3) 0.087(9) Uiso 0.50 d D 2 . .
H14D H 0.4336 0.5236 0.2500 0.131 Uiso 0.50 calc D 2 GR .
H14E H 0.3695 0.5675 0.2995 0.131 Uiso 0.50 calc D 2 GR .
H14F H 0.3272 0.5041 0.3026 0.131 Uiso 0.50 calc D 2 GR .


_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 C1 1.843(12) . ?
Br2 C2 1.858(12) . ?
Br3 C3 1.842(11) . ?
Br4 C4 1.858(11) . ?
Br5 C5 1.846(11) . ?
Br6 C6 1.844(11) . ?
Fe1 N1 1.912(10) . ?
Fe1 N2 1.909(10) . ?
Fe1 N3 1.918(10) . ?
Fe1 N4 1.932(10) . ?
Fe1 N5 1.919(10) . ?
Fe1 N6 1.940(10) . ?
O1 N1 1.346(13) . ?
O1 B1 1.492(14) . ?
O2 N2 1.372(13) . ?
O2 B2 1.501(16) . ?
O3 N3 1.343(13) . ?
O3 B1 1.523(16) . ?
O4 N4 1.347(13) . ?
O4 B2 1.529(16) . ?
O5 N5 1.355(13) . ?
O5 B1 1.481(15) . ?
O6 N6 1.312(13) . ?
O6 B2 1.510(16) . ?
N1 C1 1.278(13) . ?
N2 C2 1.275(13) . ?
N3 C3 1.305(13) . ?
N4 C4 1.298(13) . ?
N5 C5 1.322(13) . ?
N6 C6 1.312(14) . ?
C1 C2 1.473(16) . ?
C3 C4 1.417(16) . ?
C5 C6 1.405(16) . ?
C7 C8 1.512(19) . ?
C7 B1 1.60(2) . ?
C8 C9 1.56(6) . ?
C8 C9A 1.44(6) . ?
C9 C10 1.48(6) . ?
C11 C12 1.535(18) . ?
C11 B2 1.54(2) . ?
C12 C13 1.43(6) . ?
C12 C13A 1.52(3) . ?
C13 C14 1.34(16) . ?
C10A C9A 1.47(7) . ?
C13A C14A 1.81(18) . ?

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
N1 Fe1 N3 85.8(4) . . ?
N1 Fe1 N4 149.9(4) . . ?
N1 Fe1 N5 85.3(4) . . ?
N1 Fe1 N6 119.5(4) . . ?
N2 Fe1 N1 79.6(4) . . ?
N2 Fe1 N3 119.0(4) . . ?
N2 Fe1 N4 85.1(4) . . ?
N2 Fe1 N5 150.5(4) . . ?
N2 Fe1 N6 85.6(4) . . ?
N3 Fe1 N4 79.1(4) . . ?
N3 Fe1 N5 84.7(4) . . ?
N3 Fe1 N6 148.7(4) . . ?
N4 Fe1 N6 84.6(4) . . ?
N5 Fe1 N4 118.6(4) . . ?
N5 Fe1 N6 79.9(4) . . ?
N1 O1 B1 114.5(9) . . ?
N2 O2 B2 114.2(10) . . ?
N3 O3 B1 112.6(9) . . ?
N4 O4 B2 115.0(10) . . ?
N5 O5 B1 114.6(9) . . ?
N6 O6 B2 114.5(10) . . ?
O1 N1 Fe1 123.7(7) . . ?
C1 N1 Fe1 117.7(10) . . ?
C1 N1 O1 117.2(10) . . ?
O2 N2 Fe1 123.8(7) . . ?
C2 N2 Fe1 117.3(10) . . ?
C2 N2 O2 117.8(10) . . ?
O3 N3 Fe1 124.6(7) . . ?
C3 N3 Fe1 117.2(9) . . ?
C3 N3 O3 117.7(10) . . ?
O4 N4 Fe1 122.7(7) . . ?
C4 N4 Fe1 116.7(9) . . ?
C4 N4 O4 120.3(10) . . ?
O5 N5 Fe1 122.9(7) . . ?
C5 N5 Fe1 116.7(9) . . ?
C5 N5 O5 119.6(10) . . ?
O6 N6 Fe1 124.6(7) . . ?
C6 N6 Fe1 115.0(9) . . ?
C6 N6 O6 119.9(10) . . ?
N1 C1 Br1 124.7(11) . . ?
N1 C1 C2 111.6(11) . . ?
C2 C1 Br1 123.7(8) . . ?
N2 C2 Br2 124.0(11) . . ?
N2 C2 C1 112.7(11) . . ?
C1 C2 Br2 123.3(8) . . ?
N3 C3 Br3 122.8(10) . . ?
N3 C3 C4 113.0(10) . . ?
C4 C3 Br3 124.0(8) . . ?
N4 C4 Br4 121.8(10) . . ?
N4 C4 C3 113.7(10) . . ?
C3 C4 Br4 124.4(8) . . ?
N5 C5 Br5 122.0(10) . . ?
N5 C5 C6 112.7(10) . . ?
C6 C5 Br5 125.3(8) . . ?
N6 C6 Br6 120.6(10) . . ?
N6 C6 C5 115.2(10) . . ?
C5 C6 Br6 124.1(9) . . ?
C8 C7 B1 111.6(11) . . ?
C7 C8 C9 114(2) . . ?
C9A C8 C7 115(3) . . ?
C9A C8 C9 18(3) . . ?
C10 C9 C8 107(4) . . ?
C12 C11 B2 110.7(11) . . ?
C13 C12 C11 122(7) . . ?
C13 C12 C13A 15(10) . . ?
C13A C12 C11 107(7) . . ?
C12 C13 C14 132(10) . . ?
O1 B1 O3 107.9(10) . . ?
O1 B1 C7 111.2(11) . . ?
O3 B1 C7 107.3(10) . . ?
O5 B1 O1 109.3(10) . . ?
O5 B1 O3 108.1(11) . . ?
O5 B1 C7 112.9(11) . . ?
O2 B2 O4 107.3(11) . . ?
O2 B2 O6 108.9(10) . . ?
O2 B2 C11 109.4(11) . . ?
O4 B2 C11 112.9(11) . . ?
O6 B2 O4 106.6(10) . . ?
O6 B2 C11 111.6(12) . . ?
C8 C9A C10A 124(5) . . ?
C12 C13A C14A 94(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 -11.7(14) . . . . ?
Br1 C1 C2 N2 168.7(8) . . . . ?
Br3 C3 C4 Br4 -13.5(15) . . . . ?
Br3 C3 C4 N4 170.0(8) . . . . ?
Br5 C5 C6 Br6 -11.7(14) . . . . ?
Br5 C5 C6 N6 171.2(7) . . . . ?
Fe1 N1 C1 Br1 -170.9(5) . . . . ?
Fe1 N1 C1 C2 9.3(12) . . . . ?
Fe1 N2 C2 Br2 -170.8(5) . . . . ?
Fe1 N2 C2 C1 8.8(13) . . . . ?
Fe1 N3 C3 Br3 -170.7(5) . . . . ?
Fe1 N3 C3 C4 5.0(13) . . . . ?
Fe1 N4 C4 Br4 -172.8(5) . . . . ?
Fe1 N4 C4 C3 3.8(13) . . . . ?
Fe1 N5 C5 Br5 -172.6(5) . . . . ?
Fe1 N5 C5 C6 5.8(11) . . . . ?
Fe1 N6 C6 Br6 -171.9(5) . . . . ?
Fe1 N6 C6 C5 5.3(12) . . . . ?
O1 N1 C1 Br1 -4.0(13) . . . . ?
O1 N1 C1 C2 176.2(8) . . . . ?
O2 N2 C2 Br2 -2.6(14) . . . . ?
O2 N2 C2 C1 177.0(9) . . . . ?
O3 N3 C3 Br3 1.3(15) . . . . ?
O3 N3 C3 C4 177.0(9) . . . . ?
O4 N4 C4 Br4 0.5(15) . . . . ?
O4 N4 C4 C3 177.1(9) . . . . ?
O5 N5 C5 Br5 -2.2(13) . . . . ?
O5 N5 C5 C6 176.2(9) . . . . ?
O6 N6 C6 Br6 0.5(14) . . . . ?
O6 N6 C6 C5 177.7(9) . . . . ?
N1 Fe1 N2 O2 -170.7(8) . . . . ?
N1 Fe1 N2 C2 -3.2(9) . . . . ?
N1 Fe1 N3 O3 32.4(9) . . . . ?
N1 Fe1 N3 C3 -156.2(9) . . . . ?
N1 Fe1 N4 O4 -112.7(11) . . . . ?
N1 Fe1 N4 C4 60.4(14) . . . . ?
N1 Fe1 N5 O5 -51.4(8) . . . . ?
N1 Fe1 N5 C5 118.6(8) . . . . ?
N1 Fe1 N6 O6 107.7(9) . . . . ?
N1 Fe1 N6 C6 -80.4(9) . . . . ?
N1 O1 B1 O3 52.0(13) . . . . ?
N1 O1 B1 O5 -65.3(13) . . . . ?
N1 O1 B1 C7 169.4(9) . . . . ?
N1 C1 C2 Br2 168.0(8) . . . . ?
N1 C1 C2 N2 -11.5(14) . . . . ?
N2 Fe1 N1 O1 -170.0(8) . . . . ?
N2 Fe1 N1 C1 -4.0(8) . . . . ?
N2 Fe1 N3 O3 108.1(9) . . . . ?
N2 Fe1 N3 C3 -80.6(9) . . . . ?
N2 Fe1 N4 O4 -53.3(8) . . . . ?
N2 Fe1 N4 C4 119.8(9) . . . . ?
N2 Fe1 N5 O5 -110.6(11) . . . . ?
N2 Fe1 N5 C5 59.5(13) . . . . ?
N2 Fe1 N6 O6 32.2(8) . . . . ?
N2 Fe1 N6 C6 -155.8(8) . . . . ?
N2 O2 B2 O4 -66.2(12) . . . . ?
N2 O2 B2 O6 48.8(13) . . . . ?
N2 O2 B2 C11 171.0(9) . . . . ?
N3 Fe1 N1 O1 -49.5(8) . . . . ?
N3 Fe1 N1 C1 116.5(8) . . . . ?
N3 Fe1 N2 O2 110.0(8) . . . . ?
N3 Fe1 N2 C2 -82.5(9) . . . . ?
N3 Fe1 N4 O4 -174.1(9) . . . . ?
N3 Fe1 N4 C4 -0.9(9) . . . . ?
N3 Fe1 N5 O5 34.8(8) . . . . ?
N3 Fe1 N5 C5 -155.1(8) . . . . ?
N3 Fe1 N6 O6 -111.9(10) . . . . ?
N3 Fe1 N6 C6 60.1(13) . . . . ?
N3 O3 B1 O1 -68.1(12) . . . . ?
N3 O3 B1 O5 49.9(13) . . . . ?
N3 O3 B1 C7 171.9(9) . . . . ?
N3 C3 C4 Br4 170.9(8) . . . . ?
N3 C3 C4 N4 -5.7(15) . . . . ?
N4 Fe1 N1 O1 -109.3(11) . . . . ?
N4 Fe1 N1 C1 56.7(13) . . . . ?
N4 Fe1 N2 O2 35.3(8) . . . . ?
N4 Fe1 N2 C2 -157.2(9) . . . . ?
N4 Fe1 N3 O3 -173.8(9) . . . . ?
N4 Fe1 N3 C3 -2.4(9) . . . . ?
N4 Fe1 N5 O5 109.3(8) . . . . ?
N4 Fe1 N5 C5 -80.6(8) . . . . ?
N4 Fe1 N6 O6 -53.3(8) . . . . ?
N4 Fe1 N6 C6 118.7(8) . . . . ?
N4 O4 B2 O2 48.6(13) . . . . ?
N4 O4 B2 O6 -67.9(13) . . . . ?
N4 O4 B2 C11 169.2(10) . . . . ?
N5 Fe1 N1 O1 35.5(8) . . . . ?
N5 Fe1 N1 C1 -158.5(8) . . . . ?
N5 Fe1 N2 O2 -110.2(11) . . . . ?
N5 Fe1 N2 C2 57.2(14) . . . . ?
N5 Fe1 N3 O3 -53.3(9) . . . . ?
N5 Fe1 N3 C3 118.1(9) . . . . ?
N5 Fe1 N4 O4 108.2(9) . . . . ?
N5 Fe1 N4 C4 -78.7(10) . . . . ?
N5 Fe1 N6 O6 -173.6(8) . . . . ?
N5 Fe1 N6 C6 -1.7(8) . . . . ?
N5 O5 B1 O1 49.4(14) . . . . ?
N5 O5 B1 O3 -67.8(12) . . . . ?
N5 O5 B1 C7 173.6(9) . . . . ?
N5 C5 C6 Br6 169.9(7) . . . . ?
N5 C5 C6 N6 -7.2(14) . . . . ?
N6 Fe1 N1 O1 111.1(8) . . . . ?
N6 Fe1 N1 C1 -82.9(9) . . . . ?
N6 Fe1 N2 O2 -49.6(8) . . . . ?
N6 Fe1 N2 C2 117.9(9) . . . . ?
N6 Fe1 N3 O3 -113.9(10) . . . . ?
N6 Fe1 N3 C3 57.5(15) . . . . ?
N6 Fe1 N4 O4 32.8(8) . . . . ?
N6 Fe1 N4 C4 -154.1(9) . . . . ?
N6 Fe1 N5 O5 -172.5(8) . . . . ?
N6 Fe1 N5 C5 -2.5(8) . . . . ?
N6 O6 B2 O2 -66.7(12) . . . . ?
N6 O6 B2 O4 48.8(13) . . . . ?
N6 O6 B2 C11 172.5(9) . . . . ?
C7 C8 C9 C10 -178(3) . . . . ?
C7 C8 C9A C10A 175(4) . . . . ?
C8 C7 B1 O1 -63.6(14) . . . . ?
C8 C7 B1 O3 54.2(14) . . . . ?
C8 C7 B1 O5 173.2(11) . . . . ?
C9 C8 C9A C10A -94(14) . . . . ?
C11 C12 C13 C14 -162(15) . . . . ?
C11 C12 C13A C14A 172(6) . . . . ?
C12 C11 B2 O2 -69.1(14) . . . . ?
C12 C11 B2 O4 171.5(11) . . . . ?
C12 C11 B2 O6 51.4(14) . . . . ?
C13 C12 C13A C14A -7(56) . . . . ?
B1 O1 N1 Fe1 13.0(12) . . . . ?
B1 O1 N1 C1 -153.1(9) . . . . ?
B1 O3 N3 Fe1 16.8(12) . . . . ?
B1 O3 N3 C3 -154.5(10) . . . . ?
B1 O5 N5 Fe1 15.4(12) . . . . ?
B1 O5 N5 C5 -154.4(9) . . . . ?
B1 C7 C8 C9 170(2) . . . . ?
B1 C7 C8 C9A -171(3) . . . . ?
B2 O2 N2 Fe1 15.2(12) . . . . ?
B2 O2 N2 C2 -152.2(10) . . . . ?
B2 O4 N4 Fe1 17.2(12) . . . . ?
B2 O4 N4 C4 -155.7(10) . . . . ?
B2 O6 N6 Fe1 16.9(12) . . . . ?
B2 O6 N6 C6 -154.7(10) . . . . ?
B2 C11 C12 C13 -179(11) . . . . ?
B2 C11 C12 C13A -179(9) . . . . ?
C9A C8 C9 C10 84(13) . . . . ?
C13A C12 C13 C14 -161(83) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT112_250                 
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem...
RESPONSE: see Alert PLAT113. 
;
_vrf_PLAT113_250                 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group.       Pbcn
RESPONSE: The crystal is twin, that simulates orthorhombic cell below 250 K,
and hexagonal cell at room temperature. At T = 250 the twin components were 
separated and refined using HKLF 5 instruction and two additional BASF factors.
;
_vrf_REFLT01_250                 
;
PROBLEM: The number of symmetry-independent reflections cannot
exceed the total number of reflections measured
RESPONSE: see Alert PLAT113. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_220
_database_code_depnum_ccdc_archive 'CCDC 1027576'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   8.261(2)
_cell_length_b                   24.238(7)
_cell_length_c                   16.354(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.34(1)
_cell_angle_gamma                90.00
_cell_volume                     2826.1(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2586
_cell_measurement_temperature    220
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.86
_exptl_absorpt_coefficient_mu    9.057
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.1190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1647 before and 0.0798 after correction.
The Ratio of minimum to maximum transmission is 0.4277.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.170
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1812
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7654
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.44
_diffrn_reflns_theta_min         1.67
_diffrn_ambient_temperature      220
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_special_details          ?
_reflns_number_gt                3147
_reflns_number_total             7654
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.369
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.250
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7654
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.0811
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0500P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.2026
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) H8AA(0.5) H8AB(0.5)
 H8BC(0.5) H8BD(0.5) C9(0.5) H9A(0.5) H9B(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 C9A(0.5) H9AA(0.5) H9AB(0.5) C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C13A(0.5)
 H13C(0.5) H13D(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
 Fixed Uiso: H11A(0.038) H11B(0.038) H7A(0.037) H7B(0.037) H12A(0.066)
 H12B(0.066) H12C(0.066) H12D(0.066) H8AA(0.063) H8AB(0.063) H8BC(0.063)
 H8BD(0.063) H9A(0.085) H9B(0.085) H13A(0.081) H13B(0.081) H10A(0.108)
 H10B(0.108) H10C(0.108) H14A(0.128) H14B(0.128) H14C(0.128) H9AA(0.085)
 H9AB(0.085) H10D(0.108) H10E(0.108) H10F(0.108) H13C(0.081) H13D(0.081)
 H14D(0.128) H14E(0.128) H14F(0.128)
 Fixed X: H11A(0.9192) H11B(0.8487) H7A(0.9692) H7B(0.7513) H12A(0.5411)
 H12B(0.5976) H12C(0.5342) H12D(0.6126) H8AA(0.6955) H8AB(0.9136) H8BC(0.6799)
 H8BD(0.8928) H9A(0.9005) H9B(0.685) H13A(0.6371) H13B(0.6989) H10A(0.6226)
 H10B(0.7066) H10C(0.8366) H14A(0.4043) H14B(0.3282) H14C(0.3791) H9AA(0.9594)
 H9AB(0.7434) H10D(0.786) H10E(0.9256) H10F(0.7075) H13C(0.6357) H13D(0.7162)
 H14D(0.4447) H14E(0.3405) H14F(0.3864)
 Fixed Y: H11A(0.546) H11B(0.5453) H7A(0.9537) H7B(0.9555) H12A(0.5485)
 H12B(0.5599) H12C(0.5565) H12D(0.5499) H8AA(0.9423) H8AB(0.9494) H8BC(0.9506)
 H8BD(0.9408) H9A(1.0401) H9B(1.0335) H13A(0.4569) H13B(0.4682) H10A(1.0197)
 H10B(1.079) H10C(1.0321) H14A(0.475) H14B(0.4931) H14C(0.4305) H9AA(1.0314)
 H9AB(1.0406) H10D(1.082) H10E(1.0361) H10F(1.0239) H13C(0.4671) H13D(0.4604)
 H14D(0.4388) H14E(0.4854) H14F(0.4279)
 Fixed Z: H11A(-0.0237) H11B(0.0502) H7A(0.0249) H7B(-0.0496) H12A(-0.0685)
 H12B(-0.1457) H12C(-0.0797) H12D(-0.1499) H8AA(0.0799) H8AB(0.15) H8BC(0.07)
 H8BD(0.147) H9A(0.1017) H9B(0.0252) H13A(-0.0568) H13B(-0.1329) H10A(0.1501)
 H10B(0.1536) H10C(0.2233) H14A(-0.2515) H14B(-0.184) H14C(-0.1878)
 H9AA(0.1209) H9AB(0.0499) H10D(0.1794) H10E(0.2473) H10F(0.1875) H13C(-0.0224)
 H13D(-0.0915) H14D(-0.21) H14E(-0.1861) H14F(-0.1329)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.83919(17) 0.75000(8) -0.00015(10) 0.0168(3) Uani 1 d . . . .
Br1 Br 0.33012(15) 0.82286(7) -0.00409(9) 0.0361(3) Uani 1 d . . . .
Br3 Br 0.86572(17) 0.82482(6) -0.24851(9) 0.0357(3) Uani 1 d . . . .
Br5 Br 1.34727(14) 0.81983(7) 0.26114(8) 0.0373(4) Uani 1 d . . . .
Br6 Br 1.36277(15) 0.67520(6) 0.24874(8) 0.0357(3) Uani 1 d . . . .
Br4 Br 0.82511(17) 0.68017(6) -0.26119(8) 0.0371(4) Uani 1 d . . . .
Br2 Br 0.33790(15) 0.67715(7) 0.00392(9) 0.0366(3) Uani 1 d . . . .
O5 O 0.9793(9) 0.8527(4) 0.1025(5) 0.0244(19) Uani 1 d . . . .
O4 O 0.7764(9) 0.6473(4) -0.1010(5) 0.0249(18) Uani 1 d . . . .
N2 N 0.6826(11) 0.7007(5) 0.0192(6) 0.021(2) Uani 1 d . . . .
N1 N 0.6433(11) 0.7993(4) -0.0198(5) 0.018(2) Uani 1 d . . . U
O6 O 1.0303(9) 0.6450(4) 0.0628(5) 0.028(2) Uani 1 d . . . .
O2 O 0.7044(9) 0.6454(4) 0.0264(5) 0.0248(19) Uani 1 d . . . .
O1 O 0.6515(9) 0.8540(4) -0.0269(5) 0.026(2) Uani 1 d . . . .
O3 O 0.9027(10) 0.8552(4) -0.0632(5) 0.0269(19) Uani 1 d . . . .
N5 N 1.0018(10) 0.7981(4) 0.1021(6) 0.020(2) Uani 1 d . . . .
N4 N 0.7993(11) 0.7016(4) -0.1010(6) 0.021(2) Uani 1 d . . . .
N6 N 1.0386(10) 0.6994(4) 0.0795(6) 0.018(2) Uani 1 d . . . .
N3 N 0.8810(11) 0.7999(4) -0.0780(6) 0.022(2) Uani 1 d . . . .
C5 C 1.1597(13) 0.7767(5) 0.1682(6) 0.021(3) Uani 1 d . . . .
C1 C 0.5134(13) 0.7797(5) -0.0063(7) 0.019(2) Uani 1 d . . . U
C4 C 0.8239(13) 0.7231(6) -0.1682(6) 0.021(3) Uani 1 d . . . .
C2 C 0.5263(13) 0.7196(5) 0.0070(7) 0.020(2) Uani 1 d . . . U
C3 C 0.8594(12) 0.7804(5) -0.1584(6) 0.021(3) Uani 1 d . . . .
C6 C 1.1747(13) 0.7197(5) 0.1575(7) 0.022(3) Uani 1 d . . . .
B2 B 0.8339(18) 0.6239(7) -0.0056(9) 0.031(4) Uani 1 d . . . .
B1 B 0.8433(18) 0.8759(7) 0.0046(10) 0.032(4) Uani 1 d . . . .
C11 C 0.8224(16) 0.5600(5) -0.0112(9) 0.031(3) Uani 1 d D . . .
H11A H 0.9192 0.5460 -0.0237 0.038 Uiso 1 calc . . R .
H11B H 0.8487 0.5453 0.0502 0.038 Uiso 1 calc . . R .
C7 C 0.8464(17) 0.9402(5) 0.0115(8) 0.031(3) Uani 1 d C . . .
H7A H 0.9692 0.9537 0.0249 0.037 Uiso 1 calc . . R .
H7B H 0.7513 0.9555 -0.0496 0.037 Uiso 1 calc . . R .
C12 C 0.6325(18) 0.5391(6) -0.0877(11) 0.055(4) Uani 1 d . . D .
H12A H 0.5411 0.5485 -0.0685 0.066 Uiso 0.50 calc A 1 R .
H12B H 0.5976 0.5599 -0.1457 0.066 Uiso 0.50 calc A 1 R .
H12C H 0.5342 0.5565 -0.0797 0.066 Uiso 0.50 calc A 2 R .
H12D H 0.6126 0.5499 -0.1499 0.066 Uiso 0.50 calc A 2 R .
C8 C 0.809(2) 0.9605(6) 0.0881(11) 0.053(4) Uani 1 d . . D .
H8AA H 0.6955 0.9423 0.0799 0.063 Uiso 0.50 calc B 1 R .
H8AB H 0.9136 0.9494 0.1500 0.063 Uiso 0.50 calc B 1 R .
H8BC H 0.6799 0.9506 0.0700 0.063 Uiso 0.50 calc B 2 R .
H8BD H 0.8928 0.9408 0.1470 0.063 Uiso 0.50 calc B 2 R .
C9 C 0.784(7) 1.0218(7) 0.088(3) 0.071(8) Uiso 0.50 d C 1 D .
H9A H 0.9005 1.0401 0.1017 0.085 Uiso 0.50 calc C 1 R .
H9B H 0.6850 1.0335 0.0252 0.085 Uiso 0.50 calc C 1 R .
C13 C 0.610(5) 0.4789(7) -0.112(3) 0.068(7) Uiso 0.50 d D 1 D .
H13A H 0.6371 0.4569 -0.0568 0.081 Uiso 0.50 calc D 1 R .
H13B H 0.6989 0.4682 -0.1329 0.081 Uiso 0.50 calc D 1 R .
C10 C 0.733(5) 1.0397(19) 0.160(2) 0.072(8) Uiso 0.50 d C 1 D .
H10A H 0.6226 1.0197 0.1501 0.108 Uiso 0.50 calc C 1 GR .
H10B H 0.7066 1.0790 0.1536 0.108 Uiso 0.50 calc C 1 GR .
H10C H 0.8366 1.0321 0.2233 0.108 Uiso 0.50 calc C 1 GR .
C14 C 0.413(5) 0.468(2) -0.191(3) 0.085(9) Uiso 0.50 d D 1 D .
H14A H 0.4043 0.4750 -0.2515 0.128 Uiso 0.50 calc D 1 GR .
H14B H 0.3282 0.4931 -0.1840 0.128 Uiso 0.50 calc D 1 GR .
H14C H 0.3791 0.4305 -0.1878 0.128 Uiso 0.50 calc D 1 GR .
C9A C 0.834(7) 1.0213(7) 0.108(3) 0.071(8) Uiso 0.50 d C 2 D .
H9AA H 0.9594 1.0314 0.1209 0.085 Uiso 0.50 calc C 2 R .
H9AB H 0.7434 1.0406 0.0499 0.085 Uiso 0.50 calc C 2 R .
C10A C 0.811(5) 1.0427(19) 0.188(2) 0.072(8) Uiso 0.50 d C 2 D .
H10D H 0.7860 1.0820 0.1794 0.108 Uiso 0.50 calc C 2 GR .
H10E H 0.9256 1.0361 0.2473 0.108 Uiso 0.50 calc C 2 GR .
H10F H 0.7075 1.0239 0.1875 0.108 Uiso 0.50 calc C 2 GR .
C13A C 0.616(5) 0.4776(7) -0.085(3) 0.068(7) Uiso 0.50 d D 2 D .
H13C H 0.6357 0.4671 -0.0224 0.081 Uiso 0.50 calc D 2 R .
H13D H 0.7162 0.4604 -0.0915 0.081 Uiso 0.50 calc D 2 R .
C14A C 0.431(5) 0.455(2) -0.160(3) 0.085(9) Uiso 0.50 d D 2 D .
H14D H 0.4447 0.4388 -0.2100 0.128 Uiso 0.50 calc D 2 GR .
H14E H 0.3405 0.4854 -0.1861 0.128 Uiso 0.50 calc D 2 GR .
H14F H 0.3864 0.4279 -0.1329 0.128 Uiso 0.50 calc D 2 GR .


_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(9) . ?
Fe1 N1 1.903(9) . ?
Fe1 N5 1.922(9) . ?
Fe1 N4 1.913(9) . ?
Fe1 N6 1.935(9) . ?
Fe1 N3 1.910(9) . ?
Br1 C1 1.856(11) . ?
Br3 C3 1.846(11) . ?
Br5 C5 1.851(11) . ?
Br6 C6 1.861(11) . ?
Br4 C4 1.847(10) . ?
Br2 C2 1.846(11) . ?
O5 N5 1.335(12) . ?
O5 B1 1.525(15) . ?
O4 N4 1.329(12) . ?
O4 B2 1.495(15) . ?
N2 O2 1.349(12) . ?
N2 C2 1.287(12) . ?
N1 O1 1.335(12) . ?
N1 C1 1.291(12) . ?
O6 N6 1.341(12) . ?
O6 B2 1.521(15) . ?
O2 B2 1.502(15) . ?
O1 B1 1.494(14) . ?
O3 N3 1.358(12) . ?
O3 B1 1.507(15) . ?
N5 C5 1.310(12) . ?
N4 C4 1.321(13) . ?
N6 C6 1.298(12) . ?
N3 C3 1.322(13) . ?
C5 C6 1.405(16) . ?
C1 C2 1.467(15) . ?
C4 C3 1.412(16) . ?
B2 C11 1.55(2) . ?
B1 C7 1.56(2) . ?
C11 C12 1.516(17) . ?
C7 C8 1.517(17) . ?
C12 C13 1.501(10) . ?
C12 C13A 1.501(10) . ?
C8 C9 1.502(10) . ?
C8 C9A 1.500(10) . ?
C9 C10 1.499(10) . ?
C13 C14 1.501(10) . ?
C9A C10A 1.499(10) . ?
C13A C14A 1.502(10) . ?

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 N1 80.3(4) . . ?
N2 Fe1 N5 118.1(4) . . ?
N2 Fe1 N4 85.6(4) . . ?
N2 Fe1 N6 84.8(4) . . ?
N2 Fe1 N3 151.2(3) . . ?
N1 Fe1 N5 85.8(4) . . ?
N1 Fe1 N4 118.5(4) . . ?
N1 Fe1 N6 150.9(3) . . ?
N1 Fe1 N3 85.1(4) . . ?
N5 Fe1 N6 79.4(4) . . ?
N4 Fe1 N5 149.7(3) . . ?
N4 Fe1 N6 84.8(4) . . ?
N3 Fe1 N5 85.0(4) . . ?
N3 Fe1 N4 79.8(4) . . ?
N3 Fe1 N6 118.1(4) . . ?
N5 O5 B1 113.0(9) . . ?
N4 O4 B2 114.0(9) . . ?
O2 N2 Fe1 124.5(7) . . ?
C2 N2 Fe1 117.6(9) . . ?
C2 N2 O2 116.6(9) . . ?
O1 N1 Fe1 124.2(7) . . ?
C1 N1 Fe1 116.7(9) . . ?
C1 N1 O1 117.6(9) . . ?
N6 O6 B2 114.0(9) . . ?
N2 O2 B2 113.7(9) . . ?
N1 O1 B1 114.5(9) . . ?
N3 O3 B1 113.4(9) . . ?
O5 N5 Fe1 124.6(6) . . ?
C5 N5 Fe1 116.3(8) . . ?
C5 N5 O5 118.2(9) . . ?
O4 N4 Fe1 124.7(7) . . ?
C4 N4 Fe1 116.3(9) . . ?
C4 N4 O4 118.2(9) . . ?
O6 N6 Fe1 123.2(6) . . ?
C6 N6 Fe1 116.2(8) . . ?
C6 N6 O6 120.2(9) . . ?
O3 N3 Fe1 123.9(7) . . ?
C3 N3 Fe1 117.3(8) . . ?
C3 N3 O3 118.0(10) . . ?
N5 C5 Br5 121.6(10) . . ?
N5 C5 C6 113.6(10) . . ?
C6 C5 Br5 124.6(8) . . ?
N1 C1 Br1 123.5(10) . . ?
N1 C1 C2 112.7(10) . . ?
C2 C1 Br1 123.8(7) . . ?
N4 C4 Br4 122.0(10) . . ?
N4 C4 C3 113.9(9) . . ?
C3 C4 Br4 124.1(8) . . ?
N2 C2 Br2 124.8(10) . . ?
N2 C2 C1 111.7(10) . . ?
C1 C2 Br2 123.5(8) . . ?
N3 C3 Br3 122.8(10) . . ?
N3 C3 C4 112.3(10) . . ?
C4 C3 Br3 124.8(7) . . ?
N6 C6 Br6 121.7(10) . . ?
N6 C6 C5 114.1(10) . . ?
C5 C6 Br6 124.0(7) . . ?
O4 B2 O6 107.3(10) . . ?
O4 B2 O2 109.0(10) . . ?
O4 B2 C11 109.9(11) . . ?
O6 B2 C11 113.0(10) . . ?
O2 B2 O6 108.1(10) . . ?
O2 B2 C11 109.6(10) . . ?
O5 B1 C7 108.4(11) . . ?
O1 B1 O5 108.8(10) . . ?
O1 B1 O3 108.1(10) . . ?
O1 B1 C7 110.9(11) . . ?
O3 B1 O5 108.0(10) . . ?
O3 B1 C7 112.6(10) . . ?
C12 C11 B2 112.9(11) . . ?
C8 C7 B1 112.3(11) . . ?
C13 C12 C11 118.8(16) . . ?
C13A C12 C11 112.1(17) . . ?
C13A C12 C13 17(3) . . ?
C9 C8 C7 114.1(17) . . ?
C9A C8 C7 115.7(17) . . ?
C9A C8 C9 14(3) . . ?
C10 C9 C8 112(3) . . ?
C12 C13 C14 109(3) . . ?
C10A C9A C8 118(3) . . ?
C12 C13A C14A 113(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 O2 B2 -14.1(11) . . . . ?
Fe1 N2 C2 Br2 170.2(5) . . . . ?
Fe1 N2 C2 C1 -8.7(11) . . . . ?
Fe1 N1 O1 B1 -14.1(11) . . . . ?
Fe1 N1 C1 Br1 170.6(5) . . . . ?
Fe1 N1 C1 C2 -9.5(11) . . . . ?
Fe1 N5 C5 Br5 170.3(5) . . . . ?
Fe1 N5 C5 C6 -6.0(12) . . . . ?
Fe1 N4 C4 Br4 171.0(4) . . . . ?
Fe1 N4 C4 C3 -5.5(11) . . . . ?
Fe1 N6 C6 Br6 172.6(5) . . . . ?
Fe1 N6 C6 C5 -3.7(12) . . . . ?
Fe1 N3 C3 Br3 172.3(5) . . . . ?
Fe1 N3 C3 C4 -5.3(11) . . . . ?
Br1 C1 C2 Br2 12.6(12) . . . . ?
Br1 C1 C2 N2 -168.5(7) . . . . ?
Br5 C5 C6 Br6 13.8(13) . . . . ?
Br5 C5 C6 N6 -169.9(7) . . . . ?
Br4 C4 C3 Br3 13.0(12) . . . . ?
Br4 C4 C3 N3 -169.6(7) . . . . ?
O5 N5 C5 Br5 0.7(13) . . . . ?
O5 N5 C5 C6 -175.6(9) . . . . ?
O5 B1 C7 C8 -53.8(13) . . . . ?
O4 N4 C4 Br4 0.5(12) . . . . ?
O4 N4 C4 C3 -176.0(8) . . . . ?
O4 B2 C11 C12 -53.4(14) . . . . ?
N2 Fe1 N1 O1 169.5(7) . . . . ?
N2 Fe1 N1 C1 4.0(8) . . . . ?
N2 Fe1 N5 O5 -109.8(8) . . . . ?
N2 Fe1 N5 C5 81.4(8) . . . . ?
N2 Fe1 N4 O4 -33.0(8) . . . . ?
N2 Fe1 N4 C4 157.2(8) . . . . ?
N2 Fe1 N6 O6 52.9(8) . . . . ?
N2 Fe1 N6 C6 -119.5(8) . . . . ?
N2 Fe1 N3 O3 110.7(10) . . . . ?
N2 Fe1 N3 C3 -58.9(13) . . . . ?
N2 O2 B2 O4 -50.0(13) . . . . ?
N2 O2 B2 O6 66.3(11) . . . . ?
N2 O2 B2 C11 -170.2(9) . . . . ?
N1 Fe1 N2 O2 169.4(8) . . . . ?
N1 Fe1 N2 C2 3.2(8) . . . . ?
N1 Fe1 N5 O5 -33.2(8) . . . . ?
N1 Fe1 N5 C5 158.0(8) . . . . ?
N1 Fe1 N4 O4 -109.4(8) . . . . ?
N1 Fe1 N4 C4 80.8(8) . . . . ?
N1 Fe1 N6 O6 112.0(10) . . . . ?
N1 Fe1 N6 C6 -60.3(13) . . . . ?
N1 Fe1 N3 O3 51.3(7) . . . . ?
N1 Fe1 N3 C3 -118.3(8) . . . . ?
N1 O1 B1 O5 -50.5(13) . . . . ?
N1 O1 B1 O3 66.5(12) . . . . ?
N1 O1 B1 C7 -169.6(9) . . . . ?
N1 C1 C2 Br2 -167.3(7) . . . . ?
N1 C1 C2 N2 11.7(12) . . . . ?
O6 N6 C6 Br6 0.0(14) . . . . ?
O6 N6 C6 C5 -176.3(8) . . . . ?
O6 B2 C11 C12 -173.2(10) . . . . ?
O2 N2 C2 Br2 2.8(13) . . . . ?
O2 N2 C2 C1 -176.1(8) . . . . ?
O2 B2 C11 C12 66.3(14) . . . . ?
O1 N1 C1 Br1 4.1(12) . . . . ?
O1 N1 C1 C2 -176.0(8) . . . . ?
O1 B1 C7 C8 65.5(14) . . . . ?
O3 N3 C3 Br3 2.1(12) . . . . ?
O3 N3 C3 C4 -175.4(8) . . . . ?
O3 B1 C7 C8 -173.2(10) . . . . ?
N5 Fe1 N2 O2 -110.7(8) . . . . ?
N5 Fe1 N2 C2 83.1(8) . . . . ?
N5 Fe1 N1 O1 50.1(7) . . . . ?
N5 Fe1 N1 C1 -115.4(8) . . . . ?
N5 Fe1 N4 O4 110.6(10) . . . . ?
N5 Fe1 N4 C4 -59.1(13) . . . . ?
N5 Fe1 N6 O6 172.8(8) . . . . ?
N5 Fe1 N6 C6 0.5(8) . . . . ?
N5 Fe1 N3 O3 -34.9(7) . . . . ?
N5 Fe1 N3 C3 155.5(8) . . . . ?
N5 O5 B1 O1 66.0(12) . . . . ?
N5 O5 B1 O3 -51.0(12) . . . . ?
N5 O5 B1 C7 -173.3(8) . . . . ?
N5 C5 C6 Br6 -170.0(7) . . . . ?
N5 C5 C6 N6 6.3(14) . . . . ?
N4 Fe1 N2 O2 49.5(8) . . . . ?
N4 Fe1 N2 C2 -116.8(8) . . . . ?
N4 Fe1 N1 O1 -110.9(8) . . . . ?
N4 Fe1 N1 C1 83.5(8) . . . . ?
N4 Fe1 N5 O5 112.3(10) . . . . ?
N4 Fe1 N5 C5 -56.5(13) . . . . ?
N4 Fe1 N6 O6 -33.1(8) . . . . ?
N4 Fe1 N6 C6 154.5(8) . . . . ?
N4 Fe1 N3 O3 171.5(8) . . . . ?
N4 Fe1 N3 C3 1.9(7) . . . . ?
N4 O4 B2 O6 -50.6(12) . . . . ?
N4 O4 B2 O2 66.2(12) . . . . ?
N4 O4 B2 C11 -173.8(8) . . . . ?
N4 C4 C3 Br3 -170.6(7) . . . . ?
N4 C4 C3 N3 6.9(12) . . . . ?
N6 Fe1 N2 O2 -35.7(7) . . . . ?
N6 Fe1 N2 C2 158.1(8) . . . . ?
N6 Fe1 N1 O1 109.4(10) . . . . ?
N6 Fe1 N1 C1 -56.1(12) . . . . ?
N6 Fe1 N5 O5 172.1(8) . . . . ?
N6 Fe1 N5 C5 3.2(8) . . . . ?
N6 Fe1 N4 O4 52.1(7) . . . . ?
N6 Fe1 N4 C4 -117.6(8) . . . . ?
N6 Fe1 N3 O3 -110.1(8) . . . . ?
N6 Fe1 N3 C3 80.4(8) . . . . ?
N6 O6 B2 O4 68.1(12) . . . . ?
N6 O6 B2 O2 -49.2(12) . . . . ?
N6 O6 B2 C11 -170.6(9) . . . . ?
N3 Fe1 N2 O2 109.0(10) . . . . ?
N3 Fe1 N2 C2 -57.2(13) . . . . ?
N3 Fe1 N1 O1 -35.3(7) . . . . ?
N3 Fe1 N1 C1 159.2(8) . . . . ?
N3 Fe1 N5 O5 52.3(8) . . . . ?
N3 Fe1 N5 C5 -116.6(8) . . . . ?
N3 Fe1 N4 O4 171.9(8) . . . . ?
N3 Fe1 N4 C4 2.2(7) . . . . ?
N3 Fe1 N6 O6 -108.7(8) . . . . ?
N3 Fe1 N6 C6 79.0(9) . . . . ?
N3 O3 B1 O5 67.2(11) . . . . ?
N3 O3 B1 O1 -50.3(12) . . . . ?
N3 O3 B1 C7 -173.1(9) . . . . ?
C1 N1 O1 B1 151.3(9) . . . . ?
C2 N2 O2 B2 152.3(9) . . . . ?
B2 O4 N4 Fe1 -15.4(11) . . . . ?
B2 O4 N4 C4 154.2(9) . . . . ?
B2 O6 N6 Fe1 -16.5(11) . . . . ?
B2 O6 N6 C6 155.5(9) . . . . ?
B2 C11 C12 C13 170(2) . . . . ?
B2 C11 C12 C13A -173(2) . . . . ?
B1 O5 N5 Fe1 -15.0(11) . . . . ?
B1 O5 N5 C5 153.6(9) . . . . ?
B1 O3 N3 Fe1 -14.5(11) . . . . ?
B1 O3 N3 C3 154.9(9) . . . . ?
B1 C7 C8 C9 -172(2) . . . . ?
B1 C7 C8 C9A 172(2) . . . . ?
C11 C12 C13 C14 -179(3) . . . . ?
C11 C12 C13A C14A -179(3) . . . . ?
C7 C8 C9 C10 176(3) . . . . ?
C7 C8 C9A C10A -176(3) . . . . ?
C9 C8 C9A C10A 97(11) . . . . ?
C13 C12 C13A C14A -62(8) . . . . ?
C9A C8 C9 C10 -85(10) . . . . ?
C13A C12 C13 C14 111(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT112_220                 
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem...
RESPONSE: see Alert PLAT113. 
;
_vrf_PLAT113_220                 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group.       Pbcn
RESPONSE: The crystal is twin, that simulates orthorhombic cell below 250 K,
and hexagonal cell at room temperature. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Fe245
_database_code_depnum_ccdc_archive 'CCDC 1027577'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_vrf_RINTA01_Fe245               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The crystal is twin, that simulates orthorhombic cell below 250 K,
and hexagonal cell at room temperature. High Rint is caused by the three-
component twinning.
;
_vrf_PLAT020_Fe245               
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: see above.
;
_vrf_PLAT341_Fe245               
;
PROBLEM: Low Bond Precision on C-C Bonds
RESPONSE: The presence of twinning, poor crystal quality and disorder
could be the reason of the low bond precision.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.215(2)
_cell_length_b                   24.337(6)
_cell_length_c                   8.219(2)
_cell_angle_alpha                90
_cell_angle_beta                 119.347(3)
_cell_angle_gamma                90
_cell_volume                     1432.2(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1868
_cell_measurement_temperature    245
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.936
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.1190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.141
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3067
_diffrn_reflns_av_unetI/netI     0.2157
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13420
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.483
_diffrn_reflns_theta_min         2.511
_diffrn_ambient_temperature      245
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1800
_reflns_number_total             4004
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4004
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1811
_refine_ls_R_factor_gt           0.0842
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2263
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1B \\sim N1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2A \\sim N2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3B \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C1) \\sim Ueq, : with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(O3B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: N1B(0.5) N2A(0.5) N3B(0.5) H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5)
 O1A(0.5) O2A(0.5) O3A(0.5) O1B(0.5) O2B(0.5) O3B(0.5) C5B(0.5) H5BA(0.5)
 H5BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) N1A(0.5) N2B(0.5) N3A(0.5)
 Fixed Uiso: C7A(0.09) C7B(0.09) C6A(0.08) C6B(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C5B(H5BA,H5BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB)
4.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3377(3) -0.2500 -0.1621(3) 0.0239(4) Uani 1 2 d S T P . .
Br2 Br -0.16767(18) -0.17732(5) -0.66768(18) 0.0456(4) Uani 1 1 d . . . . .
Br3 Br 0.85262(19) -0.17757(6) -0.1561(2) 0.0545(4) Uani 1 1 d . . . . .
Br4 Br 0.3435(2) -0.17766(6) 0.35267(18) 0.0544(4) Uani 1 1 d . . . . .
B1 B 0.3375(19) -0.1202(6) -0.1622(19) 0.041(3) Uani 1 1 d . . . . .
N1B N 0.142(3) -0.1999(11) -0.316(3) 0.036(5) Uiso 0.5 1 d . U . A 2
N2A N 0.297(3) -0.2007(8) 0.001(3) 0.026(4) Uiso 0.5 1 d . . . A 1
N3B N 0.492(3) -0.2021(8) -0.208(3) 0.030(4) Uiso 0.5 1 d . . . A 2
C2 C 0.3372(16) -0.2221(5) 0.1630(12) 0.036(3) Uani 1 1 d . . . . .
C1 C 0.0177(15) -0.2215(5) -0.4806(13) 0.034(2) Uani 1 1 d . U . . .
C3 C 0.6636(15) -0.2210(5) -0.1615(16) 0.040(3) Uani 1 1 d . . . . .
C4 C 0.333(2) -0.0589(5) -0.170(2) 0.058(3) Uani 1 1 d . . . . .
H4BC H 0.3458 -0.0462 -0.2764 0.070 Uiso 0.5 1 calc R . . B 2
H4BD H 0.4379 -0.0439 -0.0556 0.070 Uiso 0.5 1 calc R . . B 2
H4AA H 0.4495 -0.0447 -0.0658 0.070 Uiso 0.5 1 calc R . . C 1
H4AB H 0.2297 -0.0457 -0.1533 0.070 Uiso 0.5 1 calc R . . C 1
O1A O 0.204(3) -0.1474(10) -0.354(2) 0.039(5) Uani 0.5 1 d . . . A 1
O2A O 0.273(3) -0.1507(8) -0.021(2) 0.042(4) Uani 0.5 1 d . . . A 1
O3A O 0.528(2) -0.1457(8) -0.097(2) 0.039(4) Uani 0.5 1 d . . . A 1
O1B O 0.149(2) -0.1460(8) -0.298(3) 0.035(4) Uani 0.5 1 d . . . A 2
O2B O 0.402(3) -0.1483(8) 0.030(2) 0.041(4) Uani 0.5 1 d . . . A 2
O3B O 0.477(2) -0.1494(6) -0.225(2) 0.027(3) Uani 0.5 1 d . U . A 2
C5B C 0.133(4) -0.0372(13) -0.191(5) 0.071(9) Uiso 0.5 1 d . . . D 2
H5BA H 0.0325 -0.0554 -0.3003 0.085 Uiso 0.5 1 calc R . . D 2
H5BB H 0.1265 -0.0503 -0.0815 0.085 Uiso 0.5 1 calc R . . D 2
C5A C 0.310(5) -0.0346(13) -0.362(5) 0.074(9) Uiso 0.5 1 d . . . D 1
H5AA H 0.4123 -0.0497 -0.3773 0.089 Uiso 0.5 1 calc R . . D 1
H5AB H 0.1939 -0.0496 -0.4629 0.089 Uiso 0.5 1 calc R . . D 1
C7A C 0.271(5) 0.0399(16) -0.586(5) 0.090 Uiso 0.5 1 d . . . D 1
H7AA H 0.2059 0.0107 -0.6753 0.135 Uiso 0.5 1 calc GR . . D 1
H7AB H 0.3887 0.0474 -0.5819 0.135 Uiso 0.5 1 calc GR . . D 1
H7AC H 0.1943 0.0728 -0.6244 0.135 Uiso 0.5 1 calc GR . . D 1
C7B C -0.077(5) 0.0392(15) -0.224(5) 0.090 Uiso 0.5 1 d . . . D 2
H7BA H -0.1513 0.0556 -0.3461 0.135 Uiso 0.5 1 calc GR . . D 2
H7BB H -0.0481 0.0668 -0.1284 0.135 Uiso 0.5 1 calc GR . . D 2
H7BC H -0.1462 0.0094 -0.2079 0.135 Uiso 0.5 1 calc GR . . D 2
C6A C 0.307(5) 0.0219(13) -0.390(5) 0.080 Uiso 0.5 1 d . . . D 1
H6AA H 0.4272 0.0373 -0.2961 0.096 Uiso 0.5 1 calc R . . D 1
H6AB H 0.2101 0.0381 -0.3681 0.096 Uiso 0.5 1 calc R . . D 1
C6B C 0.096(5) 0.0179(13) -0.208(5) 0.080 Uiso 0.5 1 d . . . D 2
H6BA H 0.1024 0.0306 -0.3177 0.096 Uiso 0.5 1 calc R . . D 2
H6BB H 0.1992 0.0358 -0.0992 0.096 Uiso 0.5 1 calc R . . D 2
N1A N 0.178(3) -0.1993(9) -0.357(2) 0.022(4) Uiso 0.5 1 d . . . A 1
N2B N 0.386(3) -0.1974(8) 0.038(3) 0.026(4) Uiso 0.5 1 d . . . A 2
N3A N 0.538(2) -0.1976(7) -0.121(2) 0.019(4) Uiso 0.5 1 d . . . A 1


_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 N1B 1.92(2) . ?
Fe1 N1B 1.92(2) 4 ?
Fe1 N2A 1.946(19) . ?
Fe1 N2A 1.946(19) 4 ?
Fe1 N3B 1.89(2) 4 ?
Fe1 N3B 1.89(2) . ?
Fe1 N1A 1.93(2) 4 ?
Fe1 N1A 1.93(2) . ?
Fe1 N2B 1.965(19) . ?
Fe1 N2B 1.965(19) 4 ?
Fe1 N3A 1.976(17) 4 ?
Fe1 N3A 1.976(17) . ?
Br2 C1 1.883(11) . ?
Br3 C3 1.860(11) . ?
Br4 C2 1.877(10) . ?
B1 C4 1.493(18) . ?
B1 O1A 1.56(2) . ?
B1 O2A 1.67(2) . ?
B1 O3A 1.52(2) . ?
B1 O1B 1.53(2) . ?
B1 O2B 1.55(2) . ?
B1 O3B 1.64(2) . ?
N1B C1 1.34(2) . ?
N1B O1B 1.32(3) . ?
N2A C2 1.31(2) . ?
N2A O2A 1.23(3) . ?
N3B C3 1.35(2) . ?
N3B O3B 1.29(3) . ?
C2 C2 1.36(2) 4 ?
C2 N2B 1.41(2) . ?
C1 C1 1.39(2) 4 ?
C1 N1A 1.32(2) . ?
C3 C3 1.41(2) 4 ?
C3 N3A 1.356(19) . ?
C4 C5B 1.65(3) . ?
C4 C5A 1.60(4) . ?
O1A N1A 1.28(3) . ?
O3A N3A 1.29(2) . ?
O2B N2B 1.21(3) . ?
C5B C6B 1.37(4) . ?
C5A C6A 1.39(4) . ?
C7A C6A 1.55(5) . ?
C7B C6B 1.46(4) . ?

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
N1B Fe1 N1B 79.0(15) . 4 ?
N1B Fe1 N2B 84.2(9) 4 4 ?
N1B Fe1 N2B 84.2(9) . . ?
N1B Fe1 N2B 136.7(9) . 4 ?
N1B Fe1 N2B 136.7(9) 4 . ?
N2A Fe1 N2A 76.2(12) 4 . ?
N2A Fe1 N3A 133.8(8) 4 . ?
N2A Fe1 N3A 133.8(8) . 4 ?
N2A Fe1 N3A 83.9(8) 4 4 ?
N2A Fe1 N3A 83.9(8) . . ?
N3B Fe1 N1B 84.4(9) . . ?
N3B Fe1 N1B 133.3(10) . 4 ?
N3B Fe1 N1B 133.3(10) 4 . ?
N3B Fe1 N1B 84.4(9) 4 4 ?
N3B Fe1 N3B 76.0(12) . 4 ?
N3B Fe1 N2B 83.4(9) 4 4 ?
N3B Fe1 N2B 133.4(8) 4 . ?
N3B Fe1 N2B 83.4(9) . . ?
N3B Fe1 N2B 133.4(8) . 4 ?
N1A Fe1 N2A 84.2(8) . . ?
N1A Fe1 N2A 133.3(9) 4 . ?
N1A Fe1 N2A 84.2(8) 4 4 ?
N1A Fe1 N2A 133.3(9) . 4 ?
N1A Fe1 N1A 79.2(12) . 4 ?
N1A Fe1 N3A 136.4(8) . 4 ?
N1A Fe1 N3A 136.4(8) 4 . ?
N1A Fe1 N3A 84.3(8) 4 4 ?
N1A Fe1 N3A 84.3(8) . . ?
N2B Fe1 N2B 81.2(11) . 4 ?
N3A Fe1 N3A 80.5(10) . 4 ?
C4 B1 O1A 113.1(14) . . ?
C4 B1 O2A 117.7(14) . . ?
C4 B1 O3A 114.9(13) . . ?
C4 B1 O1B 112.7(13) . . ?
C4 B1 O2B 118.2(14) . . ?
C4 B1 O3B 115.2(13) . . ?
O1A B1 O2A 101.9(12) . . ?
O3A B1 O1A 106.2(14) . . ?
O3A B1 O2A 101.3(12) . . ?
O1B B1 O2B 106.2(14) . . ?
O1B B1 O3B 102.0(12) . . ?
O2B B1 O3B 100.7(11) . . ?
C1 N1B Fe1 113.3(17) . . ?
O1B N1B Fe1 125.8(16) . . ?
O1B N1B C1 118.3(19) . . ?
C2 N2A Fe1 114.2(14) . . ?
O2A N2A Fe1 125.3(15) . . ?
O2A N2A C2 118.9(18) . . ?
C3 N3B Fe1 116.4(14) . . ?
O3B N3B Fe1 126.8(15) . . ?
O3B N3B C3 113.5(17) . . ?
N2A C2 Br4 120.3(12) . . ?
N2A C2 C2 113.4(10) . 4 ?
C2 C2 Br4 125.2(3) 4 . ?
C2 C2 N2B 115.2(9) 4 . ?
N2B C2 Br4 117.3(11) . . ?
N1B C1 Br2 120.8(13) . . ?
N1B C1 C1 113.1(12) . 4 ?
C1 C1 Br2 124.8(3) 4 . ?
N1A C1 Br2 119.8(12) . . ?
N1A C1 C1 114.1(10) . 4 ?
N3B C3 Br3 123.9(12) . . ?
N3B C3 C3 109.9(10) . 4 ?
C3 C3 Br3 124.6(4) 4 . ?
N3A C3 Br3 118.9(11) . . ?
N3A C3 C3 114.8(9) . 4 ?
B1 C4 C5B 108.9(16) . . ?
B1 C4 C5A 113.4(17) . . ?
N1A O1A B1 117.8(17) . . ?
N2A O2A B1 117.3(16) . . ?
N3A O3A B1 118.5(15) . . ?
N1B O1B B1 117.4(17) . . ?
N2B O2B B1 120.2(17) . . ?
N3B O3B B1 116.1(14) . . ?
C6B C5B C4 119(3) . . ?
C6A C5A C4 121(3) . . ?
C5A C6A C7A 115(3) . . ?
C5B C6B C7B 121(3) . . ?
C1 N1A Fe1 113.1(15) . . ?
O1A N1A Fe1 125.1(15) . . ?
O1A N1A C1 120.7(17) . . ?
C2 N2B Fe1 108.7(13) . . ?
O2B N2B Fe1 125.3(15) . . ?
O2B N2B C2 122.9(17) . . ?
C3 N3A Fe1 110.9(12) . . ?
O3A N3A Fe1 123.4(13) . . ?
O3A N3A C3 124.3(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3B_b Fe1 N3B_b O3B_b 172.6(16) 4 . . . ?
Fe1 N1B C1 Br2 -171.7(7) . . . . ?
Fe1 N1B C1 C1 20.4(17) . . . 4 ?
Fe1 N1B C1 N1A -77(4) . . . . ?
Fe1 N1B O1B B1 10(3) . . . . ?
Fe1 N2A C2 Br4 170.2(7) . . . . ?
Fe1 N2A C2 C2 -21.4(16) . . . 4 ?
Fe1 N2A C2 N2B 79(3) . . . . ?
Fe1 N2A O2A B1 -18(3) . . . . ?
Fe1 N3B C3 Br3 -169.3(7) . . . . ?
Fe1 N3B C3 C3 24.4(16) . . . 4 ?
Fe1 N3B C3 N3A -81(3) . . . . ?
Fe1 N3B O3B B1 13(3) . . . . ?
Br2 C1 N1A Fe1 173.9(7) . . . . ?
Br2 C1 N1A O1A 5(3) . . . . ?
Br3 C3 N3A Fe1 174.0(6) . . . . ?
Br3 C3 N3A O3A 7(2) . . . . ?
Br4 C2 N2B Fe1 -173.0(6) . . . . ?
Br4 C2 N2B O2B -12(3) . . . . ?
B1 C4 C5B C6B -177(3) . . . . ?
B1 C4 C5A C6A -179(3) . . . . ?
B1 O1A N1A Fe1 -18(3) . . . . ?
B1 O1A N1A C1 149.6(16) . . . . ?
B1 O3A N3A Fe1 -20(2) . . . . ?
B1 O3A N3A C3 144.8(16) . . . . ?
B1 O2B N2B Fe1 15(3) . . . . ?
B1 O2B N2B C2 -142.7(17) . . . . ?
N1B Fe1 N3B C3 -166.8(17) . . . . ?
N1B Fe1 N3B C3 -97.6(18) 4 . . . ?
N1B Fe1 N3B O3B 104(2) 4 . . . ?
N1B Fe1 N3B O3B 35(2) . . . . ?
N1B C1 N1A Fe1 75(4) . . . . ?
N1B C1 N1A O1A -94(5) . . . . ?
N2A Fe1 N3B C3 122.1(16) . . . . ?
N2A Fe1 N3B C3 49(3) 4 . . . ?
N2A Fe1 N3B O3B -36(2) . . . . ?
N2A Fe1 N3B O3B -109(2) 4 . . . ?
N2A C2 N2B Fe1 -69(3) . . . . ?
N2A C2 N2B O2B 92(3) . . . . ?
N3B Fe1 N3B C3 -29.5(19) 4 . . . ?
N3B C3 N3A Fe1 65(3) . . . . ?
N3B C3 N3A O3A -102(3) . . . . ?
C2 N2A O2A B1 146.9(16) . . . . ?
C2 C2 N2B Fe1 23.2(13) 4 . . . ?
C2 C2 N2B O2B -175.9(18) 4 . . . ?
C1 N1B O1B B1 -150.1(17) . . . . ?
C1 C1 N1A Fe1 -18.2(14) 4 . . . ?
C1 C1 N1A O1A 172.9(17) 4 . . . ?
C3 N3B O3B B1 -145.9(15) . . . . ?
C3 C3 N3A Fe1 -20.1(12) 4 . . . ?
C3 C3 N3A O3A 173.1(15) 4 . . . ?
C4 B1 O1A N1A -170.6(19) . . . . ?
C4 B1 O2A N2A -171.9(18) . . . . ?
C4 B1 O3A N3A -166.4(17) . . . . ?
C4 B1 O1B N1B 173(2) . . . . ?
C4 B1 O2B N2B 171.0(19) . . . . ?
C4 B1 O3B N3B 175.5(17) . . . . ?
C4 C5B C6B C7B -179(3) . . . . ?
C4 C5A C6A C7A -176(3) . . . . ?
O1A B1 C4 C5B 72(2) . . . . ?
O1A B1 C4 C5A -37(2) . . . . ?
O1A B1 O2A N2A 64(2) . . . . ?
O1A B1 O3A N3A -41(2) . . . . ?
O1A B1 O1B N1B 76(3) . . . . ?
O1A B1 O2B N2B 17(3) . . . . ?
O1A B1 O3B N3B -75.4(18) . . . . ?
O2A B1 C4 C5B -47(2) . . . . ?
O2A B1 C4 C5A -155.0(19) . . . . ?
O2A B1 O1A N1A -43(2) . . . . ?
O2A B1 O3A N3A 66(2) . . . . ?
O2A B1 O1B N1B -72(2) . . . . ?
O2A B1 O2B N2B 73(2) . . . . ?
O2A B1 O3B N3B 20(2) . . . . ?
O2A N2A C2 Br4 4(3) . . . . ?
O2A N2A C2 C2 172.2(17) . . . 4 ?
O2A N2A C2 N2B -88(3) . . . . ?
O3A B1 C4 C5B -165.8(18) . . . . ?
O3A B1 C4 C5A 86(2) . . . . ?
O3A B1 O1A N1A 62(2) . . . . ?
O3A B1 O2A N2A -46(2) . . . . ?
O3A B1 O1B N1B 22(3) . . . . ?
O3A B1 O2B N2B -80(2) . . . . ?
O3A B1 O3B N3B 78(2) . . . . ?
O1B B1 C4 C5B 40(2) . . . . ?
O1B B1 C4 C5A -69(2) . . . . ?
O1B B1 O1A N1A -75(3) . . . . ?
O1B B1 O2A N2A 79(2) . . . . ?
O1B B1 O3A N3A -16(3) . . . . ?
O1B B1 O2B N2B 43(2) . . . . ?
O1B B1 O3B N3B -62.1(19) . . . . ?
O1B N1B C1 Br2 -9(3) . . . . ?
O1B N1B C1 C1 -177.1(18) . . . 4 ?
O1B N1B C1 N1A 85(5) . . . . ?
O2B B1 C4 C5B -85(2) . . . . ?
O2B B1 C4 C5A 166.9(19) . . . . ?
O2B B1 O1A N1A -16(3) . . . . ?
O2B B1 O2A N2A -72(2) . . . . ?
O2B B1 O3A N3A 80.5(19) . . . . ?
O2B B1 O1B N1B -56(2) . . . . ?
O2B B1 O3B N3B 47(2) . . . . ?
O3B B1 C4 C5B 156.4(18) . . . . ?
O3B B1 C4 C5A 48(2) . . . . ?
O3B B1 O1A N1A 78(2) . . . . ?
O3B B1 O2A N2A -17(3) . . . . ?
O3B B1 O3A N3A -67.7(18) . . . . ?
O3B B1 O1B N1B 49(2) . . . . ?
O3B B1 O2B N2B -63(2) . . . . ?
O3B N3B C3 Br3 -8(3) . . . . ?
O3B N3B C3 C3 -174.8(14) . . . 4 ?
O3B N3B C3 N3A 79(3) . . . . ?
C5B C4 C5A C6A 66(4) . . . . ?
C5A C4 C5B C6B -59(4) . . . . ?
N1A Fe1 N3B C3 -156.2(18) . . . . ?
N1A Fe1 N3B C3 -89.7(17) 4 . . . ?
N1A Fe1 N3B O3B 45.9(19) . . . . ?
N1A Fe1 N3B O3B 112(2) 4 . . . ?
N2B Fe1 N3B C3 108.4(17) . . . . ?
N2B Fe1 N3B C3 37(2) 4 . . . ?
N2B Fe1 N3B O3B -120.9(19) 4 . . . ?
N2B Fe1 N3B O3B -50(2) . . . . ?
N3A Fe1 N3B C3 -11.2(17) 4 . . . ?
N3A Fe1 N3B C3 75(3) . . . . ?
N3A Fe1 N3B O3B -83(3) . . . . ?
N3A Fe1 N3B O3B -169(2) 4 . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_265
_database_code_depnum_ccdc_archive 'CCDC 1027578'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.216(2)
_cell_length_b                   24.294(6)
_cell_length_c                   8.219(3)
_cell_angle_alpha                90
_cell_angle_beta                 119.409(3)
_cell_angle_gamma                90
_cell_volume                     1429.0(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    265
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.955
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_av_unetI/netI     0.1690
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13686
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.824
_diffrn_reflns_theta_min         2.515
_diffrn_ambient_temperature      265
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1727
_reflns_number_total             4147
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1843
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1337
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim N2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N1 \\sim N1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3 \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O1A) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
: with sigma of 0.008 and sigma for terminal atoms of 0.008
3. Others
 Fixed Sof: N1(0.5) N2(0.5) N3(0.5) H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5)
 O1A(0.5) O2A(0.5) O3A(0.5) O1B(0.5) O2B(0.5) O3B(0.5) C5B(0.5) H5BA(0.5)
 H5BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) N2A(0.5) N1A(0.5) N3A(0.5)
 Fixed Uiso: C7A(0.09) C7B(0.09) C6A(0.08) C6B(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C5B(H5BA,H5BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB)
4.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3355(2) -0.2500 -0.1646(2) 0.0219(4) Uani 1 2 d S T P . .
Br1 Br -0.17000(13) -0.17730(4) -0.66992(12) 0.0458(3) Uani 1 1 d . . . . .
Br3 Br 0.84922(14) -0.17759(5) -0.15896(15) 0.0539(3) Uani 1 1 d . . . . .
Br2 Br 0.34108(16) -0.17754(5) 0.34930(12) 0.0538(3) Uani 1 1 d . . . . .
B1 B 0.3333(14) -0.1241(4) -0.1672(13) 0.033(2) Uani 1 1 d . . . . .
N1 N 0.135(2) -0.2012(8) -0.324(2) 0.027(4) Uiso 0.5 1 d . U . A 2
N2 N 0.289(2) -0.2014(6) -0.0043(17) 0.018(3) Uiso 0.5 1 d . U . A 1
N3 N 0.498(2) -0.2030(7) -0.203(2) 0.023(3) Uiso 0.5 1 d . . . A 2
C2 C 0.3367(13) -0.2209(4) 0.1631(10) 0.037(2) Uani 1 1 d . . . . .
C1 C 0.0157(11) -0.2198(3) -0.4831(10) 0.029(2) Uani 1 1 d . U . . .
C3 C 0.6620(11) -0.2208(3) -0.1618(11) 0.030(2) Uani 1 1 d . . . . .
C4 C 0.3320(14) -0.0591(3) -0.1698(13) 0.050(2) Uani 1 1 d . . . . .
H4BC H 0.3433 -0.0455 -0.2748 0.060 Uiso 0.5 1 calc R . . B 2
H4BD H 0.4349 -0.0447 -0.0554 0.060 Uiso 0.5 1 calc R . . B 2
H4AA H 0.4477 -0.0451 -0.0676 0.060 Uiso 0.5 1 calc R . . C 1
H4AB H 0.2290 -0.0454 -0.1554 0.060 Uiso 0.5 1 calc R . . C 1
O1A O 0.201(2) -0.1465(7) -0.3531(18) 0.035(4) Uani 0.5 1 d . U . A 1
O2A O 0.2694(19) -0.1472(5) -0.0274(16) 0.029(3) Uani 0.5 1 d . . . A 1
O3A O 0.5229(15) -0.1442(6) -0.1032(17) 0.032(3) Uani 0.5 1 d . . . A 1
O1B O 0.1438(17) -0.1449(6) -0.3014(17) 0.028(3) Uani 0.5 1 d . . . A 2
O2B O 0.399(2) -0.1450(6) 0.0243(15) 0.035(3) Uani 0.5 1 d . . . A 2
O3B O 0.4734(15) -0.1467(6) -0.2286(15) 0.030(3) Uani 0.5 1 d . . . A 2
C5B C 0.130(3) -0.0406(11) -0.189(3) 0.072(7) Uiso 0.5 1 d . . . D 2
H5BA H 0.0289 -0.0561 -0.3026 0.086 Uiso 0.5 1 calc R . . D 2
H5BB H 0.1205 -0.0548 -0.0840 0.086 Uiso 0.5 1 calc R . . D 2
C5A C 0.309(3) -0.0385(10) -0.370(3) 0.065(6) Uiso 0.5 1 d . . . D 1
H5AA H 0.4095 -0.0545 -0.3851 0.077 Uiso 0.5 1 calc R . . D 1
H5AB H 0.1923 -0.0526 -0.4702 0.077 Uiso 0.5 1 calc R . . D 1
C7A C 0.273(3) 0.0377(11) -0.576(3) 0.090 Uiso 0.5 1 d . . . D 1
H7AA H 0.1945 0.0103 -0.6641 0.135 Uiso 0.5 1 calc GR . . D 1
H7AB H 0.3883 0.0402 -0.5797 0.135 Uiso 0.5 1 calc GR . . D 1
H7AC H 0.2112 0.0727 -0.6088 0.135 Uiso 0.5 1 calc GR . . D 1
C7B C -0.080(3) 0.0406(12) -0.221(3) 0.090 Uiso 0.5 1 d . . . D 2
H7BA H -0.1376 0.0656 -0.3243 0.135 Uiso 0.5 1 calc GR . . D 2
H7BB H -0.0617 0.0588 -0.1093 0.135 Uiso 0.5 1 calc GR . . D 2
H7BC H -0.1592 0.0091 -0.2445 0.135 Uiso 0.5 1 calc GR . . D 2
C6A C 0.313(3) 0.0224(11) -0.391(3) 0.080 Uiso 0.5 1 d . . . D 1
H6AA H 0.2206 0.0391 -0.3649 0.096 Uiso 0.5 1 calc R . . D 1
H6AB H 0.4346 0.0364 -0.3003 0.096 Uiso 0.5 1 calc R . . D 1
C6B C 0.113(3) 0.0216(11) -0.195(3) 0.080 Uiso 0.5 1 d . . . D 2
H6BA H 0.1280 0.0357 -0.2972 0.096 Uiso 0.5 1 calc R . . D 2
H6BB H 0.2122 0.0368 -0.0796 0.096 Uiso 0.5 1 calc R . . D 2
N2A N 0.381(2) -0.1984(6) 0.0348(17) 0.020(3) Uiso 0.5 1 d . . . A 2
N1A N 0.1762(19) -0.1997(7) -0.3595(18) 0.018(3) Uiso 0.5 1 d . . . A 1
N3A N 0.533(2) -0.1980(7) -0.122(2) 0.029(4) Uiso 0.5 1 d . . . A 1


_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 N1 1.926(16) 4 ?
Fe1 N1 1.926(16) . ?
Fe1 N2 1.940(14) 4 ?
Fe1 N2 1.940(14) . ?
Fe1 N3 1.896(15) . ?
Fe1 N3 1.896(15) 4 ?
Fe1 N2A 1.947(13) 4 ?
Fe1 N2A 1.947(13) . ?
Fe1 N1A 1.927(15) . ?
Fe1 N1A 1.926(15) 4 ?
Fe1 N3A 1.948(16) 4 ?
Fe1 N3A 1.948(16) . ?
Br1 C1 1.857(8) . ?
Br3 C3 1.852(8) . ?
Br2 C2 1.843(8) . ?
B1 C4 1.578(11) . ?
B1 O1A 1.478(16) . ?
B1 O2A 1.582(16) . ?
B1 O3A 1.462(15) . ?
B1 O1B 1.486(16) . ?
B1 O2B 1.481(15) . ?
B1 O3B 1.567(16) . ?
N1 C1 1.271(16) . ?
N1 O1B 1.38(2) . ?
N2 C2 1.320(14) . ?
N2 O2A 1.329(17) . ?
N3 C3 1.294(16) . ?
N3 O3B 1.383(18) . ?
C2 C2 1.415(17) 4 ?
C2 N2A 1.386(15) . ?
C1 C1 1.468(16) 4 ?
C1 N1A 1.301(15) . ?
C3 C3 1.421(16) 4 ?
C3 N3A 1.370(17) . ?
C4 C5B 1.65(2) . ?
C4 C5A 1.64(2) . ?
O1A N1A 1.31(2) . ?
O3A N3A 1.324(19) . ?
O2B N2A 1.313(18) . ?
C5B C6B 1.52(3) . ?
C5A C6A 1.49(3) . ?
C7A C6A 1.44(3) . ?
C7B C6B 1.56(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 75.9(10) 4 . ?
N1 Fe1 N2A 135.7(6) . 4 ?
N1 Fe1 N2A 85.6(6) . . ?
N1 Fe1 N2A 85.6(6) 4 4 ?
N1 Fe1 N2A 135.7(6) 4 . ?
N2 Fe1 N2 74.9(8) 4 . ?
N2 Fe1 N3A 84.7(6) . . ?
N2 Fe1 N3A 134.1(6) 4 . ?
N2 Fe1 N3A 84.7(6) 4 4 ?
N2 Fe1 N3A 134.1(6) . 4 ?
N3 Fe1 N1 133.7(6) 4 . ?
N3 Fe1 N1 87.2(7) . . ?
N3 Fe1 N1 87.2(7) 4 4 ?
N3 Fe1 N1 133.7(6) . 4 ?
N3 Fe1 N3 74.0(9) 4 . ?
N3 Fe1 N2A 131.9(6) 4 . ?
N3 Fe1 N2A 83.9(6) . . ?
N3 Fe1 N2A 131.9(6) . 4 ?
N3 Fe1 N2A 83.9(6) 4 4 ?
N2A Fe1 N2A 80.1(8) . 4 ?
N1A Fe1 N2 132.1(6) . 4 ?
N1A Fe1 N2 132.1(6) 4 . ?
N1A Fe1 N2 84.2(6) . . ?
N1A Fe1 N2 84.2(6) 4 4 ?
N1A Fe1 N1A 78.7(9) 4 . ?
N1A Fe1 N3A 136.6(6) 4 . ?
N1A Fe1 N3A 136.6(6) . 4 ?
N1A Fe1 N3A 84.5(6) 4 4 ?
N1A Fe1 N3A 84.5(6) . . ?
N3A Fe1 N3A 80.9(10) 4 . ?
C4 B1 O2A 111.3(9) . . ?
O1A B1 C4 111.0(9) . . ?
O1A B1 O2A 106.4(10) . . ?
O3A B1 C4 109.8(9) . . ?
O3A B1 O1A 111.2(11) . . ?
O3A B1 O2A 107.1(9) . . ?
O1B B1 C4 109.4(9) . . ?
O1B B1 O3B 108.0(9) . . ?
O2B B1 C4 110.8(9) . . ?
O2B B1 O1B 112.0(10) . . ?
O2B B1 O3B 106.2(9) . . ?
O3B B1 C4 110.3(9) . . ?
C1 N1 Fe1 116.9(13) . . ?
C1 N1 O1B 117.0(13) . . ?
O1B N1 Fe1 123.3(10) . . ?
C2 N2 Fe1 115.7(10) . . ?
C2 N2 O2A 117.2(11) . . ?
O2A N2 Fe1 123.8(9) . . ?
C3 N3 Fe1 119.0(11) . . ?
C3 N3 O3B 115.0(12) . . ?
O3B N3 Fe1 124.0(10) . . ?
N2 C2 Br2 122.4(9) . . ?
N2 C2 C2 111.0(7) . 4 ?
C2 C2 Br2 124.8(3) 4 . ?
N2A C2 Br2 120.1(8) . . ?
N2A C2 C2 113.2(7) . 4 ?
N1 C1 Br1 124.0(10) . . ?
N1 C1 C1 110.8(9) . 4 ?
C1 C1 Br1 123.8(2) 4 . ?
N1A C1 Br1 122.9(9) . . ?
N1A C1 C1 112.0(8) . 4 ?
N3 C3 Br3 124.6(9) . . ?
N3 C3 C3 109.4(8) . 4 ?
C3 C3 Br3 124.5(3) 4 . ?
N3A C3 Br3 120.3(9) . . ?
N3A C3 C3 113.8(8) . 4 ?
B1 C4 C5B 105.9(12) . . ?
B1 C4 C5A 108.4(11) . . ?
N1A O1A B1 115.3(12) . . ?
N2 O2A B1 113.3(10) . . ?
N3A O3A B1 113.9(11) . . ?
N1 O1B B1 113.8(11) . . ?
N2A O2B B1 114.5(11) . . ?
N3 O3B B1 111.9(10) . . ?
C6B C5B C4 110.4(17) . . ?
C6A C5A C4 114.6(17) . . ?
C7A C6A C5A 112(2) . . ?
C5B C6B C7B 112(2) . . ?
C2 N2A Fe1 111.9(10) . . ?
O2B N2A Fe1 124.2(10) . . ?
O2B N2A C2 121.3(12) . . ?
C1 N1A Fe1 115.2(12) . . ?
C1 N1A O1A 118.7(13) . . ?
O1A N1A Fe1 124.4(10) . . ?
C3 N3A Fe1 111.7(11) . . ?
O3A N3A Fe1 124.5(11) . . ?
O3A N3A C3 121.8(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3_b Fe1 N3_b C3 -26.7(14) 4 . . . ?
Fe1 N1 C1 Br1 -171.8(6) . . . . ?
Fe1 N1 C1 C1 21.6(13) . . . 4 ?
Fe1 N1 C1 N1A -76(3) . . . . ?
Fe1 N1 O1B B1 11(2) . . . . ?
Fe1 N2 C2 Br2 169.6(5) . . . . ?
Fe1 N2 C2 C2 -24.8(11) . . . 4 ?
Fe1 N2 C2 N2A 75(2) . . . . ?
Fe1 N2 O2A B1 -13.5(17) . . . . ?
Fe1 N3 C3 Br3 -171.0(5) . . . . ?
Fe1 N3 C3 C3 22.4(12) . . . 4 ?
Fe1 N3 C3 N3A -82(3) . . . . ?
Fe1 N3 O3B B1 15.9(16) . . . . ?
Br1 C1 N1A Fe1 173.8(5) . . . . ?
Br1 C1 N1A O1A 8(2) . . . . ?
Br3 C3 N3A Fe1 173.0(5) . . . . ?
Br3 C3 N3A O3A 8.4(19) . . . . ?
Br2 C2 N2A Fe1 -172.7(5) . . . . ?
Br2 C2 N2A O2B -10.4(19) . . . . ?
B1 C4 C5B C6B -179.5(15) . . . . ?
B1 C4 C5A C6A -177.9(17) . . . . ?
B1 O1A N1A Fe1 -14(2) . . . . ?
B1 O1A N1A C1 150.4(12) . . . . ?
B1 O3A N3A Fe1 -16.1(19) . . . . ?
B1 O3A N3A C3 146.5(12) . . . . ?
B1 O2B N2A Fe1 16(2) . . . . ?
B1 O2B N2A C2 -144.5(12) . . . . ?
N1 Fe1 N3 C3 -163.9(13) . . . . ?
N1 Fe1 N3 C3 -96.5(13) 4 . . . ?
N1 Fe1 N3 O3B 100.3(14) 4 . . . ?
N1 Fe1 N3 O3B 32.9(13) . . . . ?
N1 C1 N1A Fe1 73(3) . . . . ?
N1 C1 N1A O1A -93(3) . . . . ?
N2 Fe1 N3 C3 51(2) 4 . . . ?
N2 Fe1 N3 C3 124.0(12) . . . . ?
N2 Fe1 N3 O3B -39.1(13) . . . . ?
N2 Fe1 N3 O3B -112.3(15) 4 . . . ?
N2 C2 N2A Fe1 -69(2) . . . . ?
N2 C2 N2A O2B 93(2) . . . . ?
N3 Fe1 N3 O3B 170.2(10) 4 . . . ?
N3 C3 N3A Fe1 65(3) . . . . ?
N3 C3 N3A O3A -99(3) . . . . ?
C2 N2 O2A B1 145.0(12) . . . . ?
C2 C2 N2A Fe1 22.1(10) 4 . . . ?
C2 C2 N2A O2B -175.6(11) 4 . . . ?
C1 N1 O1B B1 -149.1(13) . . . . ?
C1 C1 N1A Fe1 -18.9(11) 4 . . . ?
C1 C1 N1A O1A 175.0(12) 4 . . . ?
C3 N3 O3B B1 -147.8(11) . . . . ?
C3 C3 N3A Fe1 -20.2(10) 4 . . . ?
C3 C3 N3A O3A 175.1(11) 4 . . . ?
C4 B1 O1A N1A -172.3(13) . . . . ?
C4 B1 O2A N2 -172.6(11) . . . . ?
C4 B1 O3A N3A -170.7(12) . . . . ?
C4 B1 O1B N1 173.4(13) . . . . ?
C4 B1 O2B N2A 171.4(12) . . . . ?
C4 B1 O3B N3 171.7(10) . . . . ?
C4 C5B C6B C7B 177.9(16) . . . . ?
C4 C5A C6A C7A -174.2(18) . . . . ?
O1A B1 C4 C5B 71.0(14) . . . . ?
O1A B1 C4 C5A -37.7(14) . . . . ?
O1A B1 O2A N2 66.4(14) . . . . ?
O1A B1 O3A N3A -47.5(17) . . . . ?
O1A B1 O1B N1 75(2) . . . . ?
O1A B1 O2B N2A 22(2) . . . . ?
O1A B1 O3B N3 -79.6(12) . . . . ?
O2A B1 C4 C5B -47.2(13) . . . . ?
O2A B1 C4 C5A -155.9(12) . . . . ?
O2A B1 O1A N1A -51.1(17) . . . . ?
O2A B1 O3A N3A 68.3(14) . . . . ?
O2A B1 O1B N1 -77.5(14) . . . . ?
O2A B1 O2B N2A 73.6(16) . . . . ?
O2A B1 O3B N3 23.1(17) . . . . ?
O2A N2 C2 Br2 9.3(19) . . . . ?
O2A N2 C2 C2 174.9(11) . . . 4 ?
O2A N2 C2 N2A -85(2) . . . . ?
O3A B1 C4 C5B -165.6(12) . . . . ?
O3A B1 C4 C5A 85.7(13) . . . . ?
O3A B1 O1A N1A 65.2(17) . . . . ?
O3A B1 O2A N2 -52.6(14) . . . . ?
O3A B1 O1B N1 26(2) . . . . ?
O3A B1 O2B N2A -82.9(14) . . . . ?
O3A B1 O3B N3 76.0(14) . . . . ?
O1B B1 C4 C5B 38.8(13) . . . . ?
O1B B1 C4 C5A -69.9(13) . . . . ?
O1B B1 O1A N1A -80(2) . . . . ?
O1B B1 O2A N2 80.5(13) . . . . ?
O1B B1 O3A N3A -24(2) . . . . ?
O1B B1 O2B N2A 49.0(17) . . . . ?
O1B B1 O3B N3 -68.8(13) . . . . ?
O1B N1 C1 Br1 -10(2) . . . . ?
O1B N1 C1 C1 -176.9(12) . . . 4 ?
O1B N1 C1 N1A 85(3) . . . . ?
O2B B1 C4 C5B -85.2(13) . . . . ?
O2B B1 C4 C5A 166.1(12) . . . . ?
O2B B1 O1A N1A -23(2) . . . . ?
O2B B1 O2A N2 -76.3(15) . . . . ?
O2B B1 O3A N3A 82.3(14) . . . . ?
O2B B1 O1B N1 -63.3(16) . . . . ?
O2B B1 O3B N3 51.5(13) . . . . ?
O3B B1 C4 C5B 157.5(11) . . . . ?
O3B B1 C4 C5A 48.8(12) . . . . ?
O3B B1 O1A N1A 79.7(15) . . . . ?
O3B B1 O2A N2 -24.3(18) . . . . ?
O3B B1 O3A N3A -73.3(15) . . . . ?
O3B B1 O1B N1 53.3(16) . . . . ?
O3B B1 O2B N2A -68.7(15) . . . . ?
O3B N3 C3 Br3 -6.4(18) . . . . ?
O3B N3 C3 C3 -173.0(10) . . . 4 ?
O3B N3 C3 N3A 82(3) . . . . ?
C5B C4 C5A C6A 71(2) . . . . ?
C5A C4 C5B C6B -66.2(19) . . . . ?
N2A Fe1 N3 C3 110.1(12) . . . . ?
N2A Fe1 N3 C3 39.3(16) 4 . . . ?
N2A Fe1 N3 O3B -123.8(12) 4 . . . ?
N2A Fe1 N3 O3B -53.0(13) . . . . ?
N1A Fe1 N3 C3 -154.3(13) . . . . ?
N1A Fe1 N3 C3 -87.5(13) 4 . . . ?
N1A Fe1 N3 O3B 109.4(13) 4 . . . ?
N1A Fe1 N3 O3B 42.6(12) . . . . ?
N3A Fe1 N3 C3 81(3) . . . . ?
N3A Fe1 N3 C3 -9.6(13) 4 . . . ?
N3A Fe1 N3 O3B -82(3) . . . . ?
N3A Fe1 N3 O3B -172.7(12) 4 . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_280
_database_code_depnum_ccdc_archive 'CCDC 1027579'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_melting_point          ?
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   8.209(2)
_cell_length_b                   24.227(6)
_cell_length_c                   8.210(2)
_cell_angle_alpha                90
_cell_angle_beta                 119.472(3)
_cell_angle_gamma                90
_cell_volume                     1421.4(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1755
_cell_measurement_temperature    280
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.003
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1449
_diffrn_reflns_av_unetI/netI     0.1573
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13435
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.519
_diffrn_reflns_theta_min         2.522
_diffrn_ambient_temperature      280
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1701
_reflns_number_total             3983
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.0582
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0250P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1236
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1B \\sim N1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3B \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2A \\sim N2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O1A) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
3. Others
 Fixed Sof: N1B(0.5) N2A(0.5) N3B(0.5) H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5)
 O1A(0.5) O2A(0.5) O3A(0.5) O1B(0.5) O2B(0.5) O3B(0.5) C5B(0.5) H5BA(0.5)
 H5BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) N1A(0.5) N3A(0.5) N2B(0.5)
 Fixed Uiso: C7A(0.095) C7B(0.095) C6A(0.085) C6B(0.085)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C5B(H5BA,H5BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB)
4.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3325(2) -0.2500 -0.1676(2) 0.0232(3) Uani 1 2 d S T P . .
Br1 Br -0.17301(13) -0.17726(4) -0.67322(12) 0.0488(3) Uani 1 1 d . . . . .
Br3 Br 0.84521(13) -0.17753(4) -0.16227(15) 0.0567(3) Uani 1 1 d . . . . .
Br2 Br 0.33775(16) -0.17758(4) 0.34546(12) 0.0562(3) Uani 1 1 d . . . . .
B1 B 0.3313(13) -0.1234(4) -0.1694(13) 0.038(2) Uani 1 1 d . . . . .
N1B N 0.132(2) -0.2009(7) -0.3272(19) 0.026(4) Uiso 0.5 1 d . U . A 2
N2A N 0.287(2) -0.2020(6) -0.0079(18) 0.024(3) Uiso 0.5 1 d . . . A 1
N3B N 0.4930(19) -0.2030(6) -0.2090(19) 0.024(3) Uiso 0.5 1 d . . . A 2
C2 C 0.3335(12) -0.2205(3) 0.1586(9) 0.037(2) Uani 1 1 d . . . . .
C1 C 0.0126(11) -0.2196(3) -0.4861(10) 0.032(2) Uani 1 1 d . U . . .
C3 C 0.6585(11) -0.2210(3) -0.1662(10) 0.034(2) Uani 1 1 d . . . . .
C4 C 0.3279(13) -0.0591(3) -0.1734(13) 0.051(2) Uani 1 1 d . . . . .
H4BC H 0.3412 -0.0457 -0.2775 0.061 Uiso 0.5 1 calc R . . B 2
H4BD H 0.4302 -0.0445 -0.0583 0.061 Uiso 0.5 1 calc R . . B 2
H4AA H 0.4422 -0.0448 -0.0693 0.061 Uiso 0.5 1 calc R . . C 1
H4AB H 0.2231 -0.0458 -0.1611 0.061 Uiso 0.5 1 calc R . . C 1
O1A O 0.1968(18) -0.1464(7) -0.3582(17) 0.034(4) Uani 0.5 1 d . U . A 1
O2A O 0.2688(18) -0.1467(6) -0.0320(17) 0.035(3) Uani 0.5 1 d . . . A 1
O3A O 0.5202(15) -0.1441(6) -0.1066(18) 0.036(3) Uani 0.5 1 d . . . A 1
O1B O 0.1413(17) -0.1449(7) -0.3044(18) 0.034(4) Uani 0.5 1 d . . . A 2
O2B O 0.395(2) -0.1454(5) 0.0220(15) 0.036(3) Uani 0.5 1 d . . . A 2
O3B O 0.4706(16) -0.1468(5) -0.2290(16) 0.031(3) Uani 0.5 1 d . . . A 2
C5B C 0.128(3) -0.0395(10) -0.196(3) 0.072(6) Uiso 0.5 1 d . . . D 2
H5BA H 0.0278 -0.0528 -0.3144 0.086 Uiso 0.5 1 calc R . . D 2
H5BB H 0.1124 -0.0558 -0.0967 0.086 Uiso 0.5 1 calc R . . D 2
C5A C 0.309(3) -0.0375(10) -0.370(3) 0.082(7) Uiso 0.5 1 d . . . D 1
H5AA H 0.4107 -0.0531 -0.3828 0.098 Uiso 0.5 1 calc R . . D 1
H5AB H 0.1929 -0.0517 -0.4717 0.098 Uiso 0.5 1 calc R . . D 1
C7A C 0.273(3) 0.0372(11) -0.582(3) 0.095 Uiso 0.5 1 d . . . D 1
H7AA H 0.1913 0.0102 -0.6700 0.143 Uiso 0.5 1 calc GR . . D 1
H7AB H 0.3890 0.0379 -0.5847 0.143 Uiso 0.5 1 calc GR . . D 1
H7AC H 0.2153 0.0729 -0.6159 0.143 Uiso 0.5 1 calc GR . . D 1
C7B C -0.077(3) 0.0405(11) -0.216(3) 0.095 Uiso 0.5 1 d . . . D 2
H7BA H -0.1411 0.0616 -0.3293 0.143 Uiso 0.5 1 calc GR . . D 2
H7BB H -0.0584 0.0629 -0.1118 0.143 Uiso 0.5 1 calc GR . . D 2
H7BC H -0.1508 0.0088 -0.2243 0.143 Uiso 0.5 1 calc GR . . D 2
C6A C 0.311(3) 0.0226(10) -0.391(3) 0.085 Uiso 0.5 1 d . . . D 1
H6AA H 0.4317 0.0371 -0.2992 0.102 Uiso 0.5 1 calc R . . D 1
H6AB H 0.2162 0.0392 -0.3683 0.102 Uiso 0.5 1 calc R . . D 1
C6B C 0.115(3) 0.0214(10) -0.189(3) 0.085 Uiso 0.5 1 d . . . D 2
H6BA H 0.1349 0.0378 -0.2851 0.102 Uiso 0.5 1 calc R . . D 2
H6BB H 0.2131 0.0346 -0.0685 0.102 Uiso 0.5 1 calc R . . D 2
N1A N 0.173(2) -0.1995(7) -0.3637(18) 0.023(4) Uiso 0.5 1 d . . . A 1
N3A N 0.5298(18) -0.1990(6) -0.1272(19) 0.026(3) Uiso 0.5 1 d . . . A 1
N2B N 0.377(2) -0.1990(6) 0.0317(16) 0.020(3) Uiso 0.5 1 d . . . A 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 N1B 1.927(15) . ?
Fe1 N1B 1.927(15) 4 ?
Fe1 N2A 1.923(14) 4 ?
Fe1 N2A 1.923(14) . ?
Fe1 N3B 1.895(14) 4 ?
Fe1 N3B 1.895(14) . ?
Fe1 N1A 1.932(15) . ?
Fe1 N1A 1.932(15) 4 ?
Fe1 N3A 1.931(14) 4 ?
Fe1 N3A 1.931(14) . ?
Fe1 N2B 1.936(13) 4 ?
Fe1 N2B 1.936(13) . ?
Br1 C1 1.852(7) . ?
Br3 C3 1.847(8) . ?
Br2 C2 1.840(7) . ?
B1 C4 1.558(11) . ?
B1 O1A 1.500(16) . ?
B1 O2A 1.556(16) . ?
B1 O3A 1.461(15) . ?
B1 O1B 1.494(15) . ?
B1 O2B 1.489(15) . ?
B1 O3B 1.556(15) . ?
N1B C1 1.269(15) . ?
N1B O1B 1.37(2) . ?
N2A C2 1.303(14) . ?
N2A O2A 1.354(18) . ?
N3B C3 1.300(15) . ?
N3B O3B 1.371(17) . ?
C2 C2 1.430(16) 4 ?
C2 N2B 1.360(14) . ?
C1 C1 1.474(14) 4 ?
C1 N1A 1.294(15) . ?
C3 C3 1.404(16) 4 ?
C3 N3A 1.356(15) . ?
C4 C5B 1.63(2) . ?
C4 C5A 1.63(2) . ?
O1A N1A 1.30(2) . ?
O3A N3A 1.348(18) . ?
O2B N2B 1.313(17) . ?
C5B C6B 1.48(3) . ?
C5A C6A 1.47(3) . ?
C7A C6A 1.49(3) . ?
C7B C6B 1.55(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1B Fe1 N1B 76.2(10) 4 . ?
N1B Fe1 N2B 135.4(6) 4 . ?
N1B Fe1 N2B 135.4(6) . 4 ?
N1B Fe1 N2B 85.6(6) . . ?
N1B Fe1 N2B 85.6(6) 4 4 ?
N2A Fe1 N2A 74.4(8) . 4 ?
N2A Fe1 N1A 84.5(6) . . ?
N2A Fe1 N1A 132.1(6) . 4 ?
N2A Fe1 N1A 84.5(6) 4 4 ?
N2A Fe1 N1A 132.1(6) 4 . ?
N2A Fe1 N3A 134.3(6) . 4 ?
N2A Fe1 N3A 134.3(6) 4 . ?
N2A Fe1 N3A 85.7(6) . . ?
N2A Fe1 N3A 85.7(6) 4 4 ?
N3B Fe1 N1B 133.2(6) 4 . ?
N3B Fe1 N1B 86.7(6) 4 4 ?
N3B Fe1 N1B 133.2(6) . 4 ?
N3B Fe1 N1B 86.7(6) . . ?
N3B Fe1 N3B 73.9(9) . 4 ?
N3B Fe1 N2B 84.8(6) . . ?
N3B Fe1 N2B 132.6(6) 4 . ?
N3B Fe1 N2B 84.8(6) 4 4 ?
N3B Fe1 N2B 132.6(6) . 4 ?
N1A Fe1 N1A 78.6(9) 4 . ?
N3A Fe1 N1A 84.6(6) 4 4 ?
N3A Fe1 N1A 135.7(6) . 4 ?
N3A Fe1 N1A 84.6(6) . . ?
N3A Fe1 N1A 135.7(6) 4 . ?
N3A Fe1 N3A 79.5(9) . 4 ?
N2B Fe1 N2B 79.4(8) . 4 ?
O1A B1 C4 110.7(9) . . ?
O1A B1 O2A 106.1(9) . . ?
O2A B1 C4 111.6(9) . . ?
O3A B1 C4 110.9(9) . . ?
O3A B1 O1A 110.5(10) . . ?
O3A B1 O2A 106.9(9) . . ?
O1B B1 C4 109.4(9) . . ?
O1B B1 O3B 107.5(9) . . ?
O2B B1 C4 111.9(8) . . ?
O2B B1 O1B 110.7(10) . . ?
O2B B1 O3B 105.7(9) . . ?
O3B B1 C4 111.5(9) . . ?
C1 N1B Fe1 116.7(12) . . ?
C1 N1B O1B 117.2(13) . . ?
O1B N1B Fe1 123.3(10) . . ?
C2 N2A Fe1 116.8(10) . . ?
C2 N2A O2A 116.7(12) . . ?
O2A N2A Fe1 122.9(10) . . ?
C3 N3B Fe1 118.4(10) . . ?
C3 N3B O3B 115.3(12) . . ?
O3B N3B Fe1 123.6(10) . . ?
N2A C2 Br2 123.7(8) . . ?
N2A C2 C2 110.1(7) . 4 ?
C2 C2 Br2 124.4(2) 4 . ?
N2B C2 Br2 121.2(8) . . ?
N2B C2 C2 112.6(7) . 4 ?
N1B C1 Br1 124.1(9) . . ?
N1B C1 C1 110.9(8) . 4 ?
C1 C1 Br1 123.6(2) 4 . ?
N1A C1 Br1 122.9(9) . . ?
N1A C1 C1 112.1(8) . 4 ?
N3B C3 Br3 124.1(8) . . ?
N3B C3 C3 109.7(7) . 4 ?
C3 C3 Br3 124.8(2) 4 . ?
N3A C3 Br3 120.5(8) . . ?
N3A C3 C3 113.2(7) . 4 ?
B1 C4 C5B 107.5(11) . . ?
B1 C4 C5A 109.5(11) . . ?
N1A O1A B1 115.3(12) . . ?
N2A O2A B1 114.5(11) . . ?
N3A O3A B1 114.3(10) . . ?
N1B O1B B1 114.4(11) . . ?
N2B O2B B1 115.2(10) . . ?
N3B O3B B1 113.6(10) . . ?
C6B C5B C4 112.1(17) . . ?
C6A C5A C4 115.8(18) . . ?
C5A C6A C7A 111(2) . . ?
C5B C6B C7B 112(2) . . ?
C1 N1A Fe1 115.0(11) . . ?
C1 N1A O1A 118.6(13) . . ?
O1A N1A Fe1 124.7(10) . . ?
C3 N3A Fe1 113.2(10) . . ?
O3A N3A Fe1 123.8(10) . . ?
O3A N3A C3 121.2(12) . . ?
C2 N2B Fe1 113.0(10) . . ?
O2B N2B Fe1 124.1(9) . . ?
O2B N2B C2 120.3(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3B_b Fe1 N3B_b C3 -27.7(13) 4 . . . ?
Fe1 N1B C1 Br1 -171.8(5) . . . . ?
Fe1 N1B C1 C1 21.4(12) . . . 4 ?
Fe1 N1B C1 N1A -76(3) . . . . ?
Fe1 N1B O1B B1 11(2) . . . . ?
Fe1 N2A C2 Br2 169.6(5) . . . . ?
Fe1 N2A C2 C2 -25.0(11) . . . 4 ?
Fe1 N2A C2 N2B 76(2) . . . . ?
Fe1 N2A O2A B1 -12.9(17) . . . . ?
Fe1 N3B C3 Br3 -170.1(5) . . . . ?
Fe1 N3B C3 C3 23.2(11) . . . 4 ?
Fe1 N3B C3 N3A -79(2) . . . . ?
Fe1 N3B O3B B1 13.4(17) . . . . ?
Br1 C1 N1A Fe1 173.8(5) . . . . ?
Br1 C1 N1A O1A 8(2) . . . . ?
Br3 C3 N3A Fe1 173.3(5) . . . . ?
Br3 C3 N3A O3A 8.0(17) . . . . ?
Br2 C2 N2B Fe1 -172.9(5) . . . . ?
Br2 C2 N2B O2B -10.5(18) . . . . ?
B1 C4 C5B C6B 176.2(15) . . . . ?
B1 C4 C5A C6A -177.8(17) . . . . ?
B1 O1A N1A Fe1 -14(2) . . . . ?
B1 O1A N1A C1 150.1(12) . . . . ?
B1 O3A N3A Fe1 -16.7(18) . . . . ?
B1 O3A N3A C3 147.0(11) . . . . ?
B1 O2B N2B Fe1 15.0(19) . . . . ?
B1 O2B N2B C2 -145.3(12) . . . . ?
N1B Fe1 N3B C3 -164.6(12) . . . . ?
N1B Fe1 N3B C3 -97.0(12) 4 . . . ?
N1B Fe1 N3B O3B 102.6(14) 4 . . . ?
N1B Fe1 N3B O3B 35.0(13) . . . . ?
N1B C1 N1A Fe1 73(3) . . . . ?
N1B C1 N1A O1A -93(3) . . . . ?
N2A Fe1 N3B C3 123.4(11) . . . . ?
N2A Fe1 N3B C3 50.5(19) 4 . . . ?
N2A Fe1 N3B O3B -109.9(16) 4 . . . ?
N2A Fe1 N3B O3B -37.0(13) . . . . ?
N2A C2 N2B Fe1 -69(2) . . . . ?
N2A C2 N2B O2B 94(2) . . . . ?
N3B Fe1 N3B O3B 171.9(9) 4 . . . ?
N3B C3 N3A Fe1 67(2) . . . . ?
N3B C3 N3A O3A -98(3) . . . . ?
C2 N2A O2A B1 144.9(12) . . . . ?
C2 C2 N2B Fe1 22.0(10) 4 . . . ?
C2 C2 N2B O2B -175.6(11) 4 . . . ?
C1 N1B O1B B1 -149.2(13) . . . . ?
C1 C1 N1A Fe1 -19.3(11) 4 . . . ?
C1 C1 N1A O1A 174.9(12) 4 . . . ?
C3 N3B O3B B1 -147.5(11) . . . . ?
C3 C3 N3A Fe1 -20.0(10) 4 . . . ?
C3 C3 N3A O3A 174.7(11) 4 . . . ?
C4 B1 O1A N1A -172.0(13) . . . . ?
C4 B1 O2A N2A -173.7(11) . . . . ?
C4 B1 O3A N3A -170.1(11) . . . . ?
C4 B1 O1B N1B 173.5(13) . . . . ?
C4 B1 O2B N2B 171.1(12) . . . . ?
C4 B1 O3B N3B 173.6(10) . . . . ?
C4 C5B C6B C7B 178.2(16) . . . . ?
C4 C5A C6A C7A -174.3(17) . . . . ?
O1A B1 C4 C5B 70.1(13) . . . . ?
O1A B1 C4 C5A -39.0(14) . . . . ?
O1A B1 O2A N2A 65.6(14) . . . . ?
O1A B1 O3A N3A -46.9(16) . . . . ?
O1A B1 O1B N1B 75(2) . . . . ?
O1A B1 O2B N2B 23(2) . . . . ?
O1A B1 O3B N3B -78.1(12) . . . . ?
O2A B1 C4 C5B -47.8(12) . . . . ?
O2A B1 C4 C5A -156.9(12) . . . . ?
O2A B1 O1A N1A -50.7(17) . . . . ?
O2A B1 O3A N3A 68.1(14) . . . . ?
O2A B1 O1B N1B -77.2(14) . . . . ?
O2A B1 O2B N2B 74.5(16) . . . . ?
O2A B1 O3B N3B 24.3(17) . . . . ?
O2A N2A C2 Br2 10.5(19) . . . . ?
O2A N2A C2 C2 175.8(11) . . . 4 ?
O2A N2A C2 N2B -84(2) . . . . ?
O3A B1 C4 C5B -166.9(12) . . . . ?
O3A B1 C4 C5A 84.1(13) . . . . ?
O3A B1 O1A N1A 64.8(16) . . . . ?
O3A B1 O2A N2A -52.3(14) . . . . ?
O3A B1 O1B N1B 26(2) . . . . ?
O3A B1 O2B N2B -82.0(14) . . . . ?
O3A B1 O3B N3B 77.9(15) . . . . ?
O1B B1 C4 C5B 38.1(13) . . . . ?
O1B B1 C4 C5A -71.0(14) . . . . ?
O1B B1 O1A N1A -79(2) . . . . ?
O1B B1 O2A N2A 79.6(13) . . . . ?
O1B B1 O3A N3A -23(2) . . . . ?
O1B B1 O2B N2B 48.8(16) . . . . ?
O1B B1 O3B N3B -66.6(13) . . . . ?
O1B N1B C1 Br1 -10(2) . . . . ?
O1B N1B C1 C1 -177.0(12) . . . 4 ?
O1B N1B C1 N1A 85(3) . . . . ?
O2B B1 C4 C5B -85.0(12) . . . . ?
O2B B1 C4 C5A 166.0(13) . . . . ?
O2B B1 O1A N1A -23(2) . . . . ?
O2B B1 O2A N2A -76.1(15) . . . . ?
O2B B1 O3A N3A 81.7(13) . . . . ?
O2B B1 O1B N1B -62.7(16) . . . . ?
O2B B1 O3B N3B 51.7(13) . . . . ?
O3B B1 C4 C5B 156.8(11) . . . . ?
O3B B1 C4 C5A 47.8(13) . . . . ?
O3B B1 O1A N1A 78.8(15) . . . . ?
O3B B1 O2A N2A -24.4(17) . . . . ?
O3B B1 O3A N3A -72.3(15) . . . . ?
O3B B1 O1B N1B 52.3(16) . . . . ?
O3B B1 O2B N2B -67.3(15) . . . . ?
O3B N3B C3 Br3 -8.1(17) . . . . ?
O3B N3B C3 C3 -174.8(10) . . . 4 ?
O3B N3B C3 N3A 83(2) . . . . ?
C5B C4 C5A C6A 69(2) . . . . ?
C5A C4 C5B C6B -69.0(19) . . . . ?
N1A Fe1 N3B C3 -88.2(12) 4 . . . ?
N1A Fe1 N3B C3 -154.8(13) . . . . ?
N1A Fe1 N3B O3B 111.4(12) 4 . . . ?
N1A Fe1 N3B O3B 44.8(12) . . . . ?
N3A Fe1 N3B C3 -10.3(12) 4 . . . ?
N3A Fe1 N3B C3 78(2) . . . . ?
N3A Fe1 N3B O3B -170.7(12) 4 . . . ?
N3A Fe1 N3B O3B -82(2) . . . . ?
N2B Fe1 N3B C3 109.5(11) . . . . ?
N2B Fe1 N3B C3 39.1(15) 4 . . . ?
N2B Fe1 N3B O3B -50.9(12) . . . . ?
N2B Fe1 N3B O3B -121.3(12) 4 . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co290
_database_code_depnum_ccdc_archive 'CCDC 1027580'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.687(3)
_cell_length_b                   8.4103(14)
_cell_length_c                   17.601(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.919(9)
_cell_angle_gamma                90
_cell_volume                     2616.7(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6181
_cell_measurement_temperature    290
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.243
_shelx_estimated_absorpt_T_min   0.130
_exptl_absorpt_coefficient_mu    9.861
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1109
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.813
_diffrn_reflns_theta_min         2.304
_diffrn_ambient_temperature      290
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1886
_reflns_number_total             3254
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0626
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.27657(2) -0.93476(5) 0.19879(2) 0.05889(16) Uani 1 1 d . . . . .
Br2 Br 0.39713(2) -0.94300(5) 0.04863(2) 0.05895(17) Uani 1 1 d . . . . .
Br3 Br 0.43958(2) -0.14708(4) 0.32707(2) 0.05325(16) Uani 1 1 d . . . . .
Co1 Co 0.5000 -0.65111(7) 0.2500 0.03059(19) Uani 1 2 d S T P . .
O1 O 0.35349(12) -0.7357(3) 0.32252(11) 0.0366(6) Uani 1 1 d . . . . .
O2 O 0.53341(12) -0.7524(2) 0.09347(11) 0.0342(6) Uani 1 1 d . . . . .
O3 O 0.41536(12) -0.4882(2) 0.36697(11) 0.0325(6) Uani 1 1 d . . . . .
N1 N 0.39500(15) -0.7461(3) 0.25842(15) 0.0309(7) Uani 1 1 d . . . . .
N2 N 0.48173(16) -0.7560(3) 0.14945(13) 0.0298(7) Uani 1 1 d . . . . .
N3 N 0.46071(15) -0.4715(3) 0.30656(13) 0.0263(7) Uani 1 1 d . . . . .
C1 C 0.36863(18) -0.8280(4) 0.20218(18) 0.0289(8) Uani 1 1 d . . . . .
C2 C 0.4203(2) -0.8316(4) 0.13783(17) 0.0300(9) Uani 1 1 d . . . . .
C3 C 0.47554(18) -0.3299(4) 0.28275(16) 0.0257(8) Uani 1 1 d . . . . .
C4 C 0.34647(18) -0.6523(4) 0.46044(15) 0.0293(9) Uani 1 1 d . . . . .
H4A H 0.3013 -0.5904 0.4487 0.035 Uiso 1 1 calc R . . . .
H4B H 0.3305 -0.7596 0.4723 0.035 Uiso 1 1 calc R . . . .
C5 C 0.3867(2) -0.5812(4) 0.53090(17) 0.0444(10) Uani 1 1 d . . . . .
H5A H 0.4315 -0.6440 0.5430 0.053 Uiso 1 1 calc R . . . .
H5B H 0.4033 -0.4745 0.5188 0.053 Uiso 1 1 calc R . . . .
C6 C 0.3385(2) -0.5734(4) 0.60113(19) 0.0477(11) Uani 1 1 d . . . . .
H6A H 0.3203 -0.6791 0.6127 0.057 Uiso 1 1 calc R . . . .
H6B H 0.3696 -0.5371 0.6442 0.057 Uiso 1 1 calc R . . . .
C7 C 0.2724(2) -0.4633(4) 0.5896(2) 0.0636(13) Uani 1 1 d . . . . .
H7A H 0.2388 -0.5048 0.5505 0.095 Uiso 1 1 calc GR . . . .
H7B H 0.2901 -0.3603 0.5749 0.095 Uiso 1 1 calc GR . . . .
H7C H 0.2459 -0.4543 0.6362 0.095 Uiso 1 1 calc GR . . . .
B1 B 0.3958(2) -0.6580(5) 0.3882(2) 0.0268(10) 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
Br1 C1 1.858(3) . ?
Br2 C2 1.862(3) . ?
Br3 C3 1.847(3) . ?
Co1 N1 2.031(3) 2_655 ?
Co1 N1 2.031(3) . ?
Co1 N2 1.994(2) 2_655 ?
Co1 N2 1.994(2) . ?
Co1 N3 1.950(2) . ?
Co1 N3 1.950(2) 2_655 ?
O1 N1 1.369(3) . ?
O1 B1 1.505(4) . ?
O2 N2 1.367(3) . ?
O2 B1 1.508(4) 2_655 ?
O3 N3 1.360(3) . ?
O3 B1 1.519(4) . ?
N1 C1 1.281(4) . ?
N2 C2 1.269(4) . ?
N3 C3 1.292(3) . ?
C1 C2 1.479(4) . ?
C3 C3 1.464(5) 2_655 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.531(4) . ?
C4 B1 1.567(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.526(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.500(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
B1 O2 1.508(4) 2_655 ?

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
N1 Co1 N1 133.70(15) 2_655 . ?
N2 Co1 N1 83.26(11) 2_655 . ?
N2 Co1 N1 76.67(11) 2_655 2_655 ?
N2 Co1 N1 76.67(11) . . ?
N2 Co1 N1 83.26(11) . 2_655 ?
N2 Co1 N2 127.48(14) 2_655 . ?
N3 Co1 N1 133.17(11) 2_655 . ?
N3 Co1 N1 85.70(11) 2_655 2_655 ?
N3 Co1 N1 133.17(11) . 2_655 ?
N3 Co1 N1 85.70(11) . . ?
N3 Co1 N2 86.54(10) . 2_655 ?
N3 Co1 N2 138.24(10) 2_655 2_655 ?
N3 Co1 N2 138.24(10) . . ?
N3 Co1 N2 86.54(10) 2_655 . ?
N3 Co1 N3 78.45(15) . 2_655 ?
N1 O1 B1 113.2(2) . . ?
N2 O2 B1 115.3(2) . 2_655 ?
N3 O3 B1 115.8(2) . . ?
O1 N1 Co1 123.5(2) . . ?
C1 N1 Co1 117.7(2) . . ?
C1 N1 O1 118.6(3) . . ?
O2 N2 Co1 122.5(2) . . ?
C2 N2 Co1 118.5(2) . . ?
C2 N2 O2 119.0(3) . . ?
O3 N3 Co1 123.26(18) . . ?
C3 N3 Co1 117.9(2) . . ?
C3 N3 O3 118.7(2) . . ?
N1 C1 Br1 125.5(2) . . ?
N1 C1 C2 112.6(3) . . ?
C2 C1 Br1 121.9(2) . . ?
N2 C2 Br2 123.4(2) . . ?
N2 C2 C1 114.4(3) . . ?
C1 C2 Br2 122.1(3) . . ?
N3 C3 Br3 123.6(2) . . ?
N3 C3 C3 112.77(16) . 2_655 ?
C3 C3 Br3 123.61(9) 2_655 . ?
H4A C4 H4B 107.6 . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C5 C4 B1 114.4(3) . . ?
B1 C4 H4A 108.7 . . ?
B1 C4 H4B 108.7 . . ?
C4 C5 H5A 108.6 . . ?
C4 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C6 C5 C4 114.6(3) . . ?
C6 C5 H5A 108.6 . . ?
C6 C5 H5B 108.6 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 C5 111.8(3) . . ?
C7 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 B1 O2 108.9(3) . 2_655 ?
O1 B1 O3 109.3(3) . . ?
O1 B1 C4 111.1(3) . . ?
O2 B1 O3 110.7(3) 2_655 . ?
O2 B1 C4 108.8(3) 2_655 . ?
O3 B1 C4 108.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 0.0(4) . . . . ?
Br1 C1 C2 N2 -178.4(2) . . . . ?
Co1 N1 C1 Br1 176.63(15) . . . . ?
Co1 N1 C1 C2 -2.8(4) . . . . ?
Co1 N2 C2 Br2 -177.18(14) . . . . ?
Co1 N2 C2 C1 1.2(4) . . . . ?
Co1 N3 C3 Br3 177.40(15) . . . . ?
Co1 N3 C3 C3 -3.1(4) . . . 2_655 ?
O1 N1 C1 Br1 0.8(4) . . . . ?
O1 N1 C1 C2 -178.6(3) . . . . ?
O2 N2 C2 Br2 1.4(4) . . . . ?
O2 N2 C2 C1 179.9(3) . . . . ?
O3 N3 C3 Br3 0.9(4) . . . . ?
O3 N3 C3 C3 -179.6(3) . . . 2_655 ?
N1 O1 B1 O2 -59.0(3) . . . 2_655 ?
N1 O1 B1 O3 62.1(3) . . . . ?
N1 O1 B1 C4 -178.8(3) . . . . ?
N1 C1 C2 Br2 179.5(2) . . . . ?
N1 C1 C2 N2 1.0(4) . . . . ?
N3 O3 B1 O1 -61.3(3) . . . . ?
N3 O3 B1 O2 58.6(3) . . . 2_655 ?
N3 O3 B1 C4 177.7(2) . . . . ?
C4 C5 C6 C7 -64.6(4) . . . . ?
C5 C4 B1 O1 177.6(3) . . . . ?
C5 C4 B1 O2 57.7(4) . . . 2_655 ?
C5 C4 B1 O3 -62.5(4) . . . . ?
B1 O1 N1 Co1 -4.5(3) . . . . ?
B1 O1 N1 C1 171.1(3) . . . . ?
B1 O2 N2 Co1 -2.3(3) 2_655 . . . ?
B1 O2 N2 C2 179.2(3) 2_655 . . . ?
B1 O3 N3 Co1 -0.6(4) . . . . ?
B1 O3 N3 C3 175.7(3) . . . . ?
B1 C4 C5 C6 179.2(3) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co281
_database_code_depnum_ccdc_archive 'CCDC 1027581'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.6394(11)
_cell_length_b                   8.3798(6)
_cell_length_c                   17.5783(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.869(5)
_cell_angle_gamma                90
_cell_volume                     2596.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2308
_cell_measurement_temperature    281
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   0.241
_shelx_estimated_absorpt_T_min   0.129
_exptl_absorpt_coefficient_mu    9.936
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10402
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.127
_diffrn_reflns_theta_min         2.310
_diffrn_ambient_temperature      281
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1561
_reflns_number_total             3050
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3050
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0400
_refine_ls_restrained_S_all      0.948
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0080P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0638
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.27645(3) -0.93533(7) 0.19899(3) 0.0560(2) Uani 1 1 d . . . . .
Br2 Br 0.39725(3) -0.94360(7) 0.04871(3) 0.0559(2) Uani 1 1 d . . . . .
Br3 Br 0.43945(3) -0.14673(6) 0.32709(3) 0.0504(2) Uani 1 1 d . . . . .
Co1 Co 0.5000 -0.65073(10) 0.2500 0.0292(3) Uani 1 2 d S T P . .
O1 O 0.35332(17) -0.7349(3) 0.32234(18) 0.0353(8) Uani 1 1 d . . . . .
O2 O 0.53327(17) -0.7526(3) 0.09262(17) 0.0328(8) Uani 1 1 d . . . . .
O3 O 0.41557(16) -0.4891(3) 0.36749(17) 0.0318(8) Uani 1 1 d . . . . .
N1 N 0.3940(2) -0.7472(4) 0.2582(2) 0.0292(10) Uani 1 1 d . . . . .
N2 N 0.4816(2) -0.7575(4) 0.1492(2) 0.0268(9) Uani 1 1 d . . . . .
N3 N 0.4608(2) -0.4725(4) 0.3072(2) 0.0251(9) Uani 1 1 d . . . . .
C1 C 0.3685(2) -0.8272(5) 0.2016(3) 0.0253(11) Uani 1 1 d . . . . .
C2 C 0.4202(3) -0.8329(5) 0.1382(3) 0.0264(12) Uani 1 1 d . . . . .
C3 C 0.4757(2) -0.3298(5) 0.2824(3) 0.0272(12) Uani 1 1 d . . . . .
C4 C 0.3461(2) -0.6513(5) 0.4598(2) 0.0290(12) Uani 1 1 d . . . . .
H4A H 0.3015 -0.5872 0.4479 0.035 Uiso 1 1 calc R . . . .
H4B H 0.3291 -0.7585 0.4712 0.035 Uiso 1 1 calc R . . . .
C5 C 0.3871(3) -0.5818(6) 0.5312(3) 0.0428(14) Uani 1 1 d . . . . .
H5A H 0.4315 -0.6464 0.5433 0.051 Uiso 1 1 calc R . . . .
H5B H 0.4045 -0.4749 0.5196 0.051 Uiso 1 1 calc R . . . .
C6 C 0.3385(3) -0.5741(6) 0.6007(3) 0.0482(15) Uani 1 1 d . . . . .
H6A H 0.3198 -0.6802 0.6118 0.058 Uiso 1 1 calc R . . . .
H6B H 0.3695 -0.5391 0.6442 0.058 Uiso 1 1 calc R . . . .
C7 C 0.2719(3) -0.4614(6) 0.5896(3) 0.0561(16) Uani 1 1 d . . . . .
H7A H 0.2364 -0.5054 0.5527 0.084 Uiso 1 1 calc GR . . . .
H7B H 0.2896 -0.3601 0.5719 0.084 Uiso 1 1 calc GR . . . .
H7C H 0.2474 -0.4474 0.6371 0.084 Uiso 1 1 calc GR . . . .
B1 B 0.3964(3) -0.6576(6) 0.3884(3) 0.0257(14) 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
Br1 C1 1.859(4) . ?
Br2 C2 1.859(4) . ?
Br3 C3 1.848(4) . ?
Co1 N1 2.047(3) . ?
Co1 N1 2.047(3) 2_655 ?
Co1 N2 2.002(4) . ?
Co1 N2 2.002(4) 2_655 ?
Co1 N3 1.941(3) 2_655 ?
Co1 N3 1.941(3) . ?
O1 N1 1.359(4) . ?
O1 B1 1.512(6) . ?
O2 N2 1.370(4) . ?
O2 B1 1.503(6) 2_655 ?
O3 N3 1.354(4) . ?
O3 B1 1.500(6) . ?
N1 C1 1.270(5) . ?
N2 C2 1.265(5) . ?
N3 C3 1.303(4) . ?
C1 C2 1.464(5) . ?
C3 C3 1.447(8) 2_655 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.542(6) . ?
C4 B1 1.562(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.516(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.516(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
B1 O2 1.503(6) 2_655 ?

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
N1 Co1 N1 133.5(2) 2_655 . ?
N2 Co1 N1 83.27(15) 2_655 . ?
N2 Co1 N1 76.38(15) . . ?
N2 Co1 N1 83.27(15) . 2_655 ?
N2 Co1 N1 76.38(15) 2_655 2_655 ?
N2 Co1 N2 126.94(19) . 2_655 ?
N3 Co1 N1 133.02(15) . 2_655 ?
N3 Co1 N1 85.73(15) . . ?
N3 Co1 N1 133.02(15) 2_655 . ?
N3 Co1 N1 85.73(15) 2_655 2_655 ?
N3 Co1 N2 138.83(14) . . ?
N3 Co1 N2 86.26(15) . 2_655 ?
N3 Co1 N2 138.83(14) 2_655 2_655 ?
N3 Co1 N2 86.26(15) 2_655 . ?
N3 Co1 N3 79.4(2) . 2_655 ?
N1 O1 B1 113.8(3) . . ?
N2 O2 B1 114.7(3) . 2_655 ?
N3 O3 B1 115.6(3) . . ?
O1 N1 Co1 122.5(3) . . ?
C1 N1 Co1 117.0(3) . . ?
C1 N1 O1 120.5(4) . . ?
O2 N2 Co1 122.5(3) . . ?
C2 N2 Co1 118.2(3) . . ?
C2 N2 O2 119.4(4) . . ?
O3 N3 Co1 123.7(2) . . ?
C3 N3 Co1 116.9(3) . . ?
C3 N3 O3 119.2(3) . . ?
N1 C1 Br1 124.3(4) . . ?
N1 C1 C2 113.7(4) . . ?
C2 C1 Br1 122.0(3) . . ?
N2 C2 Br2 122.7(3) . . ?
N2 C2 C1 114.8(4) . . ?
C1 C2 Br2 122.5(3) . . ?
N3 C3 Br3 122.9(3) . . ?
N3 C3 C3 113.3(2) . 2_655 ?
C3 C3 Br3 123.84(13) 2_655 . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C5 C4 B1 113.8(4) . . ?
B1 C4 H4A 108.8 . . ?
B1 C4 H4B 108.8 . . ?
C4 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C6 C5 C4 114.1(4) . . ?
C6 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 C5 112.2(4) . . ?
C7 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 B1 C4 110.4(4) . . ?
O2 B1 O1 109.5(4) 2_655 . ?
O2 B1 C4 109.0(4) 2_655 . ?
O3 B1 O1 109.1(4) . . ?
O3 B1 O2 111.2(4) . 2_655 ?
O3 B1 C4 107.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 1.7(5) . . . . ?
Br1 C1 C2 N2 -177.9(3) . . . . ?
Co1 N1 C1 Br1 176.1(2) . . . . ?
Co1 N1 C1 C2 -1.5(5) . . . . ?
Co1 N2 C2 Br2 -177.71(19) . . . . ?
Co1 N2 C2 C1 1.9(5) . . . . ?
Co1 N3 C3 Br3 177.2(2) . . . . ?
Co1 N3 C3 C3 -4.0(6) . . . 2_655 ?
O1 N1 C1 Br1 -0.5(6) . . . . ?
O1 N1 C1 C2 -178.2(3) . . . . ?
O2 N2 C2 Br2 1.7(6) . . . . ?
O2 N2 C2 C1 -178.7(3) . . . . ?
O3 N3 C3 Br3 1.5(5) . . . . ?
O3 N3 C3 C3 -179.7(4) . . . 2_655 ?
N1 O1 B1 O2 -58.9(5) . . . 2_655 ?
N1 O1 B1 O3 63.0(5) . . . . ?
N1 O1 B1 C4 -178.9(4) . . . . ?
N1 C1 C2 Br2 179.4(3) . . . . ?
N1 C1 C2 N2 -0.2(6) . . . . ?
N3 O3 B1 O1 -61.7(5) . . . . ?
N3 O3 B1 O2 59.2(5) . . . 2_655 ?
N3 O3 B1 C4 178.5(3) . . . . ?
C4 C5 C6 C7 -64.3(6) . . . . ?
C5 C4 B1 O1 177.1(4) . . . . ?
C5 C4 B1 O2 56.8(5) . . . 2_655 ?
C5 C4 B1 O3 -63.9(5) . . . . ?
B1 O1 N1 Co1 -5.3(5) . . . . ?
B1 O1 N1 C1 171.1(4) . . . . ?
B1 O2 N2 Co1 -1.4(4) 2_655 . . . ?
B1 O2 N2 C2 179.1(4) 2_655 . . . ?
B1 O3 N3 Co1 -0.2(5) . . . . ?
B1 O3 N3 C3 175.2(4) . . . . ?
B1 C4 C5 C6 179.6(4) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co270
_database_code_depnum_ccdc_archive 'CCDC 1027582'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.6284(11)
_cell_length_b                   8.3742(6)
_cell_length_c                   17.5745(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.838(5)
_cell_angle_gamma                90
_cell_volume                     2593.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2352
_cell_measurement_temperature    273
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   0.241
_shelx_estimated_absorpt_T_min   0.128
_exptl_absorpt_coefficient_mu    9.951
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.373
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10296
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.961
_diffrn_reflns_theta_min         2.312
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1566
_reflns_number_total             3020
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3020
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      0.945
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0100P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0665
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.72352(3) -0.93582(7) 0.30090(3) 0.0532(2) Uani 1 1 d . . . . .
Br2 Br 0.60265(3) -0.94421(7) 0.45128(3) 0.0533(2) Uani 1 1 d . . . . .
Br3 Br 0.56058(3) -0.14657(6) 0.17282(3) 0.04850(19) Uani 1 1 d . . . . .
Co1 Co 0.5000 -0.65059(10) 0.2500 0.0278(3) Uani 1 2 d S T P . .
O1 O 0.64691(17) -0.7346(3) 0.17761(18) 0.0334(9) Uani 1 1 d . . . . .
O2 O 0.46638(17) -0.7538(3) 0.40687(17) 0.0298(8) Uani 1 1 d . . . . .
O3 O 0.58433(16) -0.4890(3) 0.13263(18) 0.0291(8) Uani 1 1 d . . . . .
N1 N 0.6066(2) -0.7466(4) 0.2420(2) 0.0275(10) Uani 1 1 d . . . . .
N2 N 0.5181(2) -0.7576(4) 0.3505(2) 0.0254(10) Uani 1 1 d . . . . .
N3 N 0.53897(19) -0.4720(4) 0.1926(2) 0.0244(10) Uani 1 1 d . . . . .
C1 C 0.6313(2) -0.8277(5) 0.2986(3) 0.0234(11) Uani 1 1 d . . . . .
C2 C 0.5801(3) -0.8335(5) 0.3621(3) 0.0262(12) Uani 1 1 d . . . . .
C3 C 0.5239(2) -0.3295(5) 0.2173(3) 0.0242(12) Uani 1 1 d . . . . .
C4 C 0.6539(2) -0.6511(5) 0.0397(3) 0.0266(12) Uani 1 1 d . . . . .
H4A H 0.6986 -0.5870 0.0513 0.032 Uiso 1 1 calc R . . . .
H4B H 0.6709 -0.7584 0.0281 0.032 Uiso 1 1 calc R . . . .
C5 C 0.6127(3) -0.5815(6) -0.0316(3) 0.0411(14) Uani 1 1 d . . . . .
H5A H 0.5683 -0.6464 -0.0437 0.049 Uiso 1 1 calc R . . . .
H5B H 0.5952 -0.4747 -0.0200 0.049 Uiso 1 1 calc R . . . .
C6 C 0.6613(3) -0.5735(6) -0.1010(3) 0.0455(15) Uani 1 1 d . . . . .
H6A H 0.6304 -0.5376 -0.1444 0.055 Uiso 1 1 calc R . . . .
H6B H 0.6798 -0.6797 -0.1124 0.055 Uiso 1 1 calc R . . . .
C7 C 0.7284(3) -0.4614(6) -0.0894(3) 0.0540(16) Uani 1 1 d . . . . .
H7A H 0.7541 -0.4499 -0.1365 0.081 Uiso 1 1 calc GR . . . .
H7B H 0.7628 -0.5046 -0.0513 0.081 Uiso 1 1 calc GR . . . .
H7C H 0.7107 -0.3589 -0.0732 0.081 Uiso 1 1 calc GR . . . .
B1 B 0.6041(3) -0.6577(7) 0.1118(3) 0.0249(14) 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
Br1 C1 1.861(4) . ?
Br2 C2 1.853(5) . ?
Br3 C3 1.846(4) . ?
Co1 N1 2.052(4) 2_655 ?
Co1 N1 2.052(4) . ?
Co1 N2 1.996(4) . ?
Co1 N2 1.997(4) 2_655 ?
Co1 N3 1.941(3) 2_655 ?
Co1 N3 1.941(3) . ?
O1 N1 1.360(4) . ?
O1 B1 1.506(6) . ?
O2 N2 1.369(4) . ?
O2 B1 1.508(6) 2_655 ?
O3 N3 1.351(4) . ?
O3 B1 1.504(6) . ?
N1 C1 1.270(5) . ?
N2 C2 1.275(5) . ?
N3 C3 1.300(5) . ?
C1 C2 1.458(6) . ?
C3 C3 1.447(8) 2_655 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.542(6) . ?
C4 B1 1.566(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.514(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.519(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
B1 O2 1.508(6) 2_655 ?

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
N1 Co1 N1 133.9(2) . 2_655 ?
N2 Co1 N1 76.35(16) 2_655 2_655 ?
N2 Co1 N1 83.35(15) . 2_655 ?
N2 Co1 N1 76.35(16) . . ?
N2 Co1 N1 83.35(15) 2_655 . ?
N2 Co1 N2 126.7(2) . 2_655 ?
N3 Co1 N1 85.78(15) . . ?
N3 Co1 N1 132.64(15) . 2_655 ?
N3 Co1 N1 85.78(15) 2_655 2_655 ?
N3 Co1 N1 132.64(15) 2_655 . ?
N3 Co1 N2 139.09(15) . . ?
N3 Co1 N2 86.30(15) . 2_655 ?
N3 Co1 N2 139.09(15) 2_655 2_655 ?
N3 Co1 N2 86.30(15) 2_655 . ?
N3 Co1 N3 79.3(2) . 2_655 ?
N1 O1 B1 114.1(3) . . ?
N2 O2 B1 114.7(3) . 2_655 ?
N3 O3 B1 115.9(3) . . ?
O1 N1 Co1 122.2(3) . . ?
C1 N1 Co1 116.6(3) . . ?
C1 N1 O1 121.1(4) . . ?
O2 N2 Co1 122.6(3) . . ?
C2 N2 Co1 118.5(3) . . ?
C2 N2 O2 118.9(4) . . ?
O3 N3 Co1 123.6(3) . . ?
C3 N3 Co1 117.0(3) . . ?
C3 N3 O3 119.3(3) . . ?
N1 C1 Br1 123.7(4) . . ?
N1 C1 C2 114.4(4) . . ?
C2 C1 Br1 121.9(4) . . ?
N2 C2 Br2 123.0(4) . . ?
N2 C2 C1 114.1(4) . . ?
C1 C2 Br2 122.9(3) . . ?
N3 C3 Br3 122.9(3) . . ?
N3 C3 C3 113.3(2) . 2_655 ?
C3 C3 Br3 123.85(14) 2_655 . ?
H4A C4 H4B 107.6 . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C5 C4 B1 114.2(4) . . ?
B1 C4 H4A 108.7 . . ?
B1 C4 H4B 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C6 C5 C4 114.0(4) . . ?
C6 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C5 C6 C7 112.2(5) . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 B1 O2 109.2(4) . 2_655 ?
O1 B1 C4 110.9(4) . . ?
O2 B1 C4 108.8(4) 2_655 . ?
O3 B1 O1 109.2(4) . . ?
O3 B1 O2 111.0(4) . 2_655 ?
O3 B1 C4 107.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 1.4(5) . . . . ?
Br1 C1 C2 N2 -177.6(3) . . . . ?
Co1 N1 C1 Br1 175.9(2) . . . . ?
Co1 N1 C1 C2 -2.4(5) . . . . ?
Co1 N2 C2 Br2 -177.7(2) . . . . ?
Co1 N2 C2 C1 1.4(5) . . . . ?
Co1 N3 C3 Br3 176.7(2) . . . . ?
Co1 N3 C3 C3 -3.2(6) . . . 2_655 ?
O1 N1 C1 Br1 0.4(6) . . . . ?
O1 N1 C1 C2 -177.9(4) . . . . ?
O2 N2 C2 Br2 1.7(6) . . . . ?
O2 N2 C2 C1 -179.2(3) . . . . ?
O3 N3 C3 Br3 1.1(6) . . . . ?
O3 N3 C3 C3 -178.8(4) . . . 2_655 ?
N1 O1 B1 O2 -59.1(5) . . . 2_655 ?
N1 O1 B1 O3 62.4(5) . . . . ?
N1 O1 B1 C4 -179.0(4) . . . . ?
N1 C1 C2 Br2 179.8(3) . . . . ?
N1 C1 C2 N2 0.7(6) . . . . ?
N3 O3 B1 O1 -61.6(5) . . . . ?
N3 O3 B1 O2 58.8(5) . . . 2_655 ?
N3 O3 B1 C4 177.8(3) . . . . ?
C4 C5 C6 C7 -63.8(6) . . . . ?
C5 C4 B1 O1 177.1(4) . . . . ?
C5 C4 B1 O2 57.0(5) . . . 2_655 ?
C5 C4 B1 O3 -63.4(5) . . . . ?
B1 O1 N1 Co1 -4.9(5) . . . . ?
B1 O1 N1 C1 170.4(4) . . . . ?
B1 O2 N2 Co1 -2.1(4) 2_655 . . . ?
B1 O2 N2 C2 178.5(4) 2_655 . . . ?
B1 O3 N3 Co1 -0.2(5) . . . . ?
B1 O3 N3 C3 175.1(4) . . . . ?
B1 C4 C5 C6 179.3(4) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co200
_database_code_depnum_ccdc_archive 'CCDC 1027583'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.5412(18)
_cell_length_b                   8.3247(9)
_cell_length_c                   17.5278(19)
_cell_angle_alpha                90
_cell_angle_beta                 91.682(7)
_cell_angle_gamma                90
_cell_volume                     2558.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2698
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.238
_shelx_estimated_absorpt_T_min   0.126
_exptl_absorpt_coefficient_mu    10.086
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10211
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.323
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1755
_reflns_number_total             2985
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2985
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0426
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0250P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0838
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.60133(3) -0.94814(7) 0.45077(3) 0.0376(2) Uani 1 1 d . . . . .
Br2 Br 0.72360(3) -0.94047(8) 0.30006(3) 0.03595(19) Uani 1 1 d . . . . .
Br3 Br 0.43870(3) -0.14507(6) 0.32780(3) 0.03439(19) Uani 1 1 d . . . . .
Co1 Co 0.5000 -0.64767(11) 0.2500 0.0228(3) Uani 1 2 d S T P . .
O1 O 0.46479(18) -0.7592(4) 0.40590(19) 0.0235(9) Uani 1 1 d . . . . .
O2 O 0.64893(18) -0.7304(4) 0.17815(18) 0.0237(9) Uani 1 1 d . . . . .
O3 O 0.41737(18) -0.4895(4) 0.36867(19) 0.0235(9) Uani 1 1 d . . . . .
N1 N 0.5171(2) -0.7615(4) 0.3489(2) 0.0187(10) Uani 1 1 d . . . . .
N2 N 0.6075(2) -0.7426(5) 0.2422(2) 0.0193(10) Uani 1 1 d . . . . .
N3 N 0.4626(2) -0.4724(5) 0.3082(2) 0.0184(10) Uani 1 1 d . . . . .
C1 C 0.5796(3) -0.8358(6) 0.3611(3) 0.0185(12) Uani 1 1 d . . . . .
C2 C 0.6315(3) -0.8278(6) 0.2977(3) 0.0159(11) Uani 1 1 d . . . . .
C3 C 0.4766(2) -0.3275(6) 0.2831(3) 0.0187(12) Uani 1 1 d . . . . .
C4 C 0.3449(3) -0.6500(6) 0.4609(3) 0.0201(12) Uani 1 1 d . . . . .
H4A H 0.3003 -0.5806 0.4493 0.024 Uiso 1 1 calc R . . . .
H4B H 0.3256 -0.7589 0.4724 0.024 Uiso 1 1 calc R . . . .
C5 C 0.3875(3) -0.5842(6) 0.5324(3) 0.0254(13) Uani 1 1 d . . . . .
H5A H 0.4315 -0.6549 0.5446 0.030 Uiso 1 1 calc R . . . .
H5B H 0.4076 -0.4762 0.5206 0.030 Uiso 1 1 calc R . . . .
C6 C 0.3386(3) -0.5720(6) 0.6021(3) 0.0285(14) Uani 1 1 d . . . . .
H6A H 0.3707 -0.5360 0.6462 0.034 Uiso 1 1 calc R . . . .
H6B H 0.3184 -0.6798 0.6142 0.034 Uiso 1 1 calc R . . . .
C7 C 0.2716(3) -0.4550(6) 0.5907(3) 0.0341(15) Uani 1 1 d . . . . .
H7A H 0.2359 -0.4972 0.5515 0.051 Uiso 1 1 calc GR . . . .
H7B H 0.2908 -0.3502 0.5745 0.051 Uiso 1 1 calc GR . . . .
H7C H 0.2452 -0.4428 0.6389 0.051 Uiso 1 1 calc GR . . . .
B1 B 0.3952(3) -0.6593(7) 0.3887(3) 0.0176(14) 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
Br1 C1 1.858(5) . ?
Br2 C2 1.867(5) . ?
Br3 C3 1.842(5) . ?
Co1 N1 1.991(4) . ?
Co1 N1 1.991(4) 2_655 ?
Co1 N2 2.053(4) . ?
Co1 N2 2.053(4) 2_655 ?
Co1 N3 1.908(4) 2_655 ?
Co1 N3 1.908(4) . ?
O1 N1 1.376(4) . ?
O1 B1 1.501(6) . ?
O2 N2 1.359(4) . ?
O2 B1 1.506(7) 2_655 ?
O3 N3 1.350(5) . ?
O3 B1 1.510(6) . ?
N1 C1 1.272(5) . ?
N2 C2 1.266(6) . ?
N3 C3 1.309(5) . ?
C1 C2 1.459(6) . ?
C3 C3 1.441(9) 2_655 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.539(7) . ?
C4 B1 1.566(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.516(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.535(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
B1 O2 1.506(7) 2_655 ?

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
N1 Co1 N1 123.1(2) 2_655 . ?
N1 Co1 N2 82.76(17) . 2_655 ?
N1 Co1 N2 76.09(16) . . ?
N1 Co1 N2 82.76(17) 2_655 . ?
N1 Co1 N2 76.09(16) 2_655 2_655 ?
N2 Co1 N2 134.7(2) 2_655 . ?
N3 Co1 N1 86.78(16) . . ?
N3 Co1 N1 141.67(16) 2_655 . ?
N3 Co1 N1 86.78(16) 2_655 2_655 ?
N3 Co1 N1 141.67(16) . 2_655 ?
N3 Co1 N2 85.87(16) 2_655 . ?
N3 Co1 N2 131.37(17) 2_655 2_655 ?
N3 Co1 N2 85.87(16) . 2_655 ?
N3 Co1 N2 131.37(17) . . ?
N3 Co1 N3 80.2(2) . 2_655 ?
N1 O1 B1 114.7(4) . . ?
N2 O2 B1 113.4(3) . 2_655 ?
N3 O3 B1 116.3(3) . . ?
O1 N1 Co1 122.6(3) . . ?
C1 N1 Co1 119.0(3) . . ?
C1 N1 O1 118.3(4) . . ?
O2 N2 Co1 122.7(3) . . ?
C2 N2 Co1 116.7(3) . . ?
C2 N2 O2 120.2(4) . . ?
O3 N3 Co1 123.9(3) . . ?
C3 N3 Co1 117.0(3) . . ?
C3 N3 O3 118.8(4) . . ?
N1 C1 Br1 122.8(4) . . ?
N1 C1 C2 113.8(4) . . ?
C2 C1 Br1 123.4(3) . . ?
N2 C2 Br2 124.5(4) . . ?
N2 C2 C1 114.2(4) . . ?
C1 C2 Br2 121.3(4) . . ?
N3 C3 Br3 122.9(3) . . ?
N3 C3 C3 112.8(3) . 2_655 ?
C3 C3 Br3 124.31(15) 2_655 . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C5 C4 B1 113.8(4) . . ?
B1 C4 H4A 108.8 . . ?
B1 C4 H4B 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.6 . . ?
C6 C5 C4 114.0(4) . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C5 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C5 C6 C7 112.8(5) . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 H6A 109.0 . . ?
C7 C6 H6B 109.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 B1 O2 109.6(4) . 2_655 ?
O1 B1 O3 110.6(4) . . ?
O1 B1 C4 109.8(4) . . ?
O2 B1 O3 108.5(4) 2_655 . ?
O2 B1 C4 111.1(4) 2_655 . ?
O3 B1 C4 107.3(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 3.0(6) . . . . ?
Br1 C1 C2 N2 -178.5(4) . . . . ?
Co1 N1 C1 Br1 -179.3(2) . . . . ?
Co1 N1 C1 C2 -0.7(6) . . . . ?
Co1 N2 C2 Br2 174.6(2) . . . . ?
Co1 N2 C2 C1 -3.8(6) . . . . ?
Co1 N3 C3 Br3 175.3(2) . . . . ?
Co1 N3 C3 C3 -4.1(7) . . . 2_655 ?
O1 N1 C1 Br1 2.7(6) . . . . ?
O1 N1 C1 C2 -178.8(4) . . . . ?
O2 N2 C2 Br2 1.1(7) . . . . ?
O2 N2 C2 C1 -177.3(4) . . . . ?
O3 N3 C3 Br3 1.3(6) . . . . ?
O3 N3 C3 C3 -178.1(5) . . . 2_655 ?
N1 O1 B1 O2 64.3(5) . . . 2_655 ?
N1 O1 B1 O3 -55.3(5) . . . . ?
N1 O1 B1 C4 -173.5(4) . . . . ?
N1 C1 C2 Br2 -175.5(4) . . . . ?
N1 C1 C2 N2 3.0(7) . . . . ?
N3 O3 B1 O1 58.9(5) . . . . ?
N3 O3 B1 O2 -61.2(5) . . . 2_655 ?
N3 O3 B1 C4 178.7(4) . . . . ?
C4 C5 C6 C7 -62.6(6) . . . . ?
C5 C4 B1 O1 56.5(6) . . . . ?
C5 C4 B1 O2 177.8(4) . . . 2_655 ?
C5 C4 B1 O3 -63.7(5) . . . . ?
B1 O1 N1 Co1 -2.1(5) . . . . ?
B1 O1 N1 C1 175.9(5) . . . . ?
B1 O2 N2 Co1 -7.1(5) 2_655 . . . ?
B1 O2 N2 C2 166.1(4) 2_655 . . . ?
B1 O3 N3 Co1 -1.1(5) . . . . ?
B1 O3 N3 C3 172.4(4) . . . . ?
B1 C4 C5 C6 178.9(4) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co100
_database_code_depnum_ccdc_archive 'CCDC 1027584'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.4640(15)
_cell_length_b                   8.2746(8)
_cell_length_c                   17.4676(15)
_cell_angle_alpha                90
_cell_angle_beta                 91.575(6)
_cell_angle_gamma                90
_cell_volume                     2523.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.234
_shelx_estimated_absorpt_T_min   0.124
_exptl_absorpt_coefficient_mu    10.226
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10962
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.631
_diffrn_reflns_theta_min         2.333
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2164
_reflns_number_total             3526
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.268
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.268
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1016
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.22368(3) -0.44394(7) -0.20024(3) 0.01840(15) Uani 1 1 d . . . . .
Br2 Br 0.10030(3) -0.45048(7) -0.04913(3) 0.02063(16) Uani 1 1 d . . . . .
Br3 Br 0.06197(3) 0.35758(6) -0.32830(3) 0.01901(15) Uani 1 1 d . . . . .
Co4 Co 0.0000 -0.14429(12) -0.2500 0.0159(3) Uani 1 2 d S T P . .
O1 O 0.15118(17) -0.2254(4) -0.32122(19) 0.0123(8) Uani 1 1 d . . . . .
O2 O -0.03782(18) -0.2647(4) -0.09572(19) 0.0118(8) Uani 1 1 d . . . . .
O3 O 0.08092(18) 0.0111(4) -0.37040(19) 0.0104(8) Uani 1 1 d . . . . .
N1 N 0.1086(2) -0.2375(5) -0.2565(2) 0.0100(9) Uani 1 1 d . . . . .
N2 N 0.0147(2) -0.2647(5) -0.1519(2) 0.0103(9) Uani 1 1 d . . . . .
N3 N 0.0359(2) 0.0280(5) -0.3093(2) 0.0102(9) Uani 1 1 d . . . . .
C1 C 0.1323(3) -0.3280(6) -0.2021(3) 0.0075(10) Uani 1 1 d . U . . .
C2 C 0.0790(3) -0.3382(6) -0.1397(3) 0.0122(11) Uani 1 1 d . . . . .
C3 C 0.0230(2) 0.1729(6) -0.2833(3) 0.0098(11) Uani 1 1 d . . . . .
C4 C 0.1557(3) -0.1493(6) -0.4618(3) 0.0123(11) Uani 1 1 d . . . . .
H4A H 0.2003 -0.0785 -0.4505 0.015 Uiso 1 1 calc R . . . .
H4B H 0.1755 -0.2585 -0.4733 0.015 Uiso 1 1 calc R . . . .
C5 C 0.1127(3) -0.0850(6) -0.5323(3) 0.0125(11) Uani 1 1 d . . . . .
H5A H 0.0918 0.0231 -0.5203 0.015 Uiso 1 1 calc R . . . .
H5B H 0.0688 -0.1573 -0.5443 0.015 Uiso 1 1 calc R . . . .
C6 C 0.1621(3) -0.0714(6) -0.6032(3) 0.0167(12) Uani 1 1 d . . . . .
H6A H 0.1296 -0.0364 -0.6474 0.020 Uiso 1 1 calc R . . . .
H6B H 0.1832 -0.1792 -0.6153 0.020 Uiso 1 1 calc R . . . .
C7 C 0.2286(3) 0.0493(6) -0.5915(3) 0.0195(13) Uani 1 1 d . . . . .
H7A H 0.2551 0.0632 -0.6398 0.029 Uiso 1 1 calc GR . . . .
H7B H 0.2648 0.0077 -0.5523 0.029 Uiso 1 1 calc GR . . . .
H7C H 0.2084 0.1536 -0.5749 0.029 Uiso 1 1 calc GR . . . .
B1 B 0.1054(3) -0.1593(7) -0.3888(3) 0.0112(13) 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
Br1 C1 1.862(4) . ?
Br2 C2 1.864(5) . ?
Br3 C3 1.857(5) . ?
Co4 N1 2.053(4) 2_554 ?
Co4 N1 2.053(4) . ?
Co4 N2 1.993(4) . ?
Co4 N2 1.993(4) 2_554 ?
Co4 N3 1.879(4) 2_554 ?
Co4 N3 1.879(4) . ?
O1 N1 1.373(5) . ?
O1 B1 1.511(7) . ?
O2 N2 1.362(4) . ?
O2 B1 1.486(6) 2_554 ?
O3 N3 1.351(5) . ?
O3 B1 1.511(7) . ?
N1 C1 1.272(6) . ?
N2 C2 1.290(6) . ?
N3 C3 1.304(6) . ?
C1 C2 1.454(6) . ?
C3 C3 1.430(9) 2_554 ?
C4 C5 1.521(7) . ?
C4 B1 1.570(7) . ?
C5 C6 1.533(6) . ?
C6 C7 1.541(7) . ?
B1 O2 1.486(6) 2_554 ?

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
N1 Co4 N1 135.9(2) . 2_554 ?
N2 Co4 N1 76.27(16) . . ?
N2 Co4 N1 82.06(16) . 2_554 ?
N2 Co4 N1 76.27(16) 2_554 2_554 ?
N2 Co4 N1 82.06(16) 2_554 . ?
N2 Co4 N2 120.0(2) . 2_554 ?
N3 Co4 N1 129.63(17) 2_554 . ?
N3 Co4 N1 129.63(17) . 2_554 ?
N3 Co4 N1 86.09(16) . . ?
N3 Co4 N1 86.09(16) 2_554 2_554 ?
N3 Co4 N2 86.70(17) . 2_554 ?
N3 Co4 N2 86.70(17) 2_554 . ?
N3 Co4 N2 144.67(17) 2_554 2_554 ?
N3 Co4 N2 144.68(17) . . ?
N3 Co4 N3 81.3(2) . 2_554 ?
N1 O1 B1 112.5(3) . . ?
N2 O2 B1 114.6(4) . 2_554 ?
N3 O3 B1 116.1(3) . . ?
O1 N1 Co4 122.7(3) . . ?
C1 N1 Co4 117.5(3) . . ?
C1 N1 O1 119.1(4) . . ?
O2 N2 Co4 123.1(3) . . ?
C2 N2 Co4 117.9(3) . . ?
C2 N2 O2 118.8(4) . . ?
O3 N3 Co4 124.6(3) . . ?
C3 N3 Co4 116.2(3) . . ?
C3 N3 O3 118.7(4) . . ?
N1 C1 Br1 125.3(4) . . ?
N1 C1 C2 113.1(4) . . ?
C2 C1 Br1 121.6(4) . . ?
N2 C2 Br2 121.8(4) . . ?
N2 C2 C1 114.9(4) . . ?
C1 C2 Br2 123.2(4) . . ?
N3 C3 Br3 122.7(3) . . ?
N3 C3 C3 112.9(3) . 2_554 ?
C3 C3 Br3 124.39(15) 2_554 . ?
C5 C4 B1 113.6(4) . . ?
C4 C5 C6 113.7(4) . . ?
C5 C6 C7 112.3(4) . . ?
O1 B1 C4 111.0(4) . . ?
O2 B1 O1 109.3(4) 2_554 . ?
O2 B1 O3 111.0(4) 2_554 . ?
O2 B1 C4 110.1(4) 2_554 . ?
O3 B1 O1 108.5(4) . . ?
O3 B1 C4 107.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 5.9(6) . . . . ?
Br1 C1 C2 N2 -173.4(4) . . . . ?
Co4 N1 C1 Br1 172.9(2) . . . . ?
Co4 N1 C1 C2 -5.2(6) . . . . ?
Co4 N2 C2 Br2 178.5(2) . . . . ?
Co4 N2 C2 C1 -2.2(6) . . . . ?
Co4 N3 C3 Br3 173.9(2) . . . . ?
Co4 N3 C3 C3 -5.4(7) . . . 2_554 ?
O1 N1 C1 Br1 2.3(7) . . . . ?
O1 N1 C1 C2 -175.9(4) . . . . ?
O2 N2 C2 Br2 2.3(6) . . . . ?
O2 N2 C2 C1 -178.4(4) . . . . ?
O3 N3 C3 Br3 1.6(6) . . . . ?
O3 N3 C3 C3 -177.7(5) . . . 2_554 ?
N1 Co4 N3 O3 -108.6(4) 2_554 . . . ?
N1 Co4 N3 O3 42.8(4) . . . . ?
N1 Co4 N3 C3 79.6(4) 2_554 . . . ?
N1 Co4 N3 C3 -129.0(4) . . . . ?
N1 O1 B1 O2 -57.8(5) . . . 2_554 ?
N1 O1 B1 O3 63.4(5) . . . . ?
N1 O1 B1 C4 -179.3(4) . . . . ?
N1 C1 C2 Br2 -175.9(4) . . . . ?
N1 C1 C2 N2 4.9(7) . . . . ?
N2 Co4 N3 O3 -39.5(4) 2_554 . . . ?
N2 Co4 N3 O3 102.3(4) . . . . ?
N2 Co4 N3 C3 -69.5(5) . . . . ?
N2 Co4 N3 C3 148.7(4) 2_554 . . . ?
N3 Co4 N3 O3 173.9(5) 2_554 . . . ?
N3 Co4 N3 C3 2.1(3) 2_554 . . . ?
N3 O3 B1 O1 -61.0(5) . . . . ?
N3 O3 B1 O2 59.1(5) . . . 2_554 ?
N3 O3 B1 C4 179.2(4) . . . . ?
C4 C5 C6 C7 -62.8(6) . . . . ?
C5 C4 B1 O1 179.5(4) . . . . ?
C5 C4 B1 O2 58.4(6) . . . 2_554 ?
C5 C4 B1 O3 -62.3(5) . . . . ?
B1 O1 N1 Co4 -8.3(5) . . . . ?
B1 O1 N1 C1 161.8(4) . . . . ?
B1 O2 N2 Co4 -3.6(5) 2_554 . . . ?
B1 O2 N2 C2 172.4(5) 2_554 . . . ?
B1 O3 N3 Co4 -2.4(5) . . . . ?
B1 O3 N3 C3 169.2(4) . . . . ?
B1 C4 C5 C6 178.7(4) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co70
_database_code_depnum_ccdc_archive 'CCDC 1027585'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '4(C14 H18 B2 Br6 Co N6 O6)'
_chemical_formula_sum            'C56 H72 B8 Br24 Co4 N24 O24'
_chemical_formula_weight         3705.41
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.4551(11)
_cell_length_b                   8.2748(5)
_cell_length_c                   17.4449(11)
_cell_angle_alpha                90
_cell_angle_beta                 91.634(5)
_cell_angle_gamma                90
_cell_volume                     2518.7(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3742
_cell_measurement_temperature    70(2)
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.245
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10730
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.328
_diffrn_reflns_theta_min         2.335
_diffrn_ambient_temperature      70(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2175
_reflns_number_total             3253
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0180P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0694
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.27642(2) 0.44464(5) 0.70031(2) 0.01741(12) Uani 1 1 d . . . . .
Br2 Br 0.39988(2) 0.45094(5) 0.54898(2) 0.02233(13) Uani 1 1 d . . . . .
Co1 Co 0.5000 0.14427(9) 0.7500 0.0154(2) Uani 1 2 d S T P . .
N1 N 0.39158(16) 0.2371(4) 0.75737(18) 0.0076(7) Uani 1 1 d . . . . .
O1 O 0.34891(14) 0.2249(3) 0.82104(14) 0.0103(6) Uani 1 1 d . . . . .
B1 B 0.3935(2) 0.1585(5) 0.8885(3) 0.0098(10) Uani 1 1 d . . . . .
C6 C 0.3372(2) 0.0687(5) 1.1028(2) 0.0150(9) Uani 1 1 d . . . . .
H6A H 0.3692 0.0339 1.1461 0.018 Uiso 1 1 calc R . . . .
H6B H 0.3169 0.1744 1.1149 0.018 Uiso 1 1 calc R . . . .
C7 C 0.2711(2) -0.0491(5) 1.0921(2) 0.0190(10) Uani 1 1 d . . . . .
H7A H 0.2355 -0.0080 1.0539 0.029 Uiso 1 1 calc GR . . . .
H7B H 0.2457 -0.0619 1.1397 0.029 Uiso 1 1 calc GR . . . .
H7C H 0.2904 -0.1518 1.0758 0.029 Uiso 1 1 calc GR . . . .
N2 N 0.48500(17) 0.2645(3) 0.65210(18) 0.0081(7) Uani 1 1 d . . . . .
C4 C 0.3439(2) 0.1505(4) 0.9619(2) 0.0083(8) Uani 1 1 d . . . . .
H4A H 0.3259 0.2584 0.9735 0.010 Uiso 1 1 calc R . . . .
H4B H 0.2993 0.0836 0.9509 0.010 Uiso 1 1 calc R . . . .
C2 C 0.4211(2) 0.3380(4) 0.6394(2) 0.0098(8) Uani 1 1 d . . . . .
C1 C 0.3679(2) 0.3283(4) 0.7020(2) 0.0101(8) Uani 1 1 d . . . . .
C5 C 0.3866(2) 0.0832(5) 1.0324(2) 0.0107(9) Uani 1 1 d . . . . .
H5A H 0.4066 -0.0227 1.0201 0.013 Uiso 1 1 calc R . . . .
H5B H 0.4299 0.1529 1.0448 0.013 Uiso 1 1 calc R . . . .
O3 O 0.41904(14) -0.0119(3) 0.87092(15) 0.0100(6) Uani 1 1 d . . . . .
Br3 Br 0.43793(2) -0.35809(4) 0.82837(3) 0.01895(12) Uani 1 1 d . . . . .
N3 N 0.46394(17) -0.0289(3) 0.80905(17) 0.0074(7) Uani 1 1 d . . . . .
C3 C 0.4769(2) -0.1738(4) 0.7833(2) 0.0065(8) Uani 1 1 d . . . . .
O2 O 0.53773(14) 0.2651(3) 0.59573(15) 0.0096(6) 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
Br1 C1 1.864(4) . ?
Br2 C2 1.862(4) . ?
Co1 N1 2.050(3) 2_656 ?
Co1 N1 2.050(3) . ?
Co1 N2 1.988(3) . ?
Co1 N2 1.988(3) 2_656 ?
Co1 N3 1.884(3) . ?
Co1 N3 1.884(3) 2_656 ?
N1 O1 1.359(4) . ?
N1 C1 1.284(5) . ?
O1 B1 1.496(5) . ?
B1 C4 1.566(6) . ?
B1 O3 1.513(5) . ?
B1 O2 1.509(5) 2_656 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.518(5) . ?
C6 C5 1.525(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
N2 C2 1.283(4) . ?
N2 O2 1.366(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.526(5) . ?
C2 C1 1.456(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
O3 N3 1.359(4) . ?
Br3 C3 1.854(3) . ?
N3 C3 1.303(4) . ?
C3 C3 1.434(7) 2_656 ?
O2 B1 1.509(5) 2_656 ?

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
N1 Co1 N1 136.00(17) . 2_656 ?
N2 Co1 N1 81.82(12) 2_656 . ?
N2 Co1 N1 81.83(12) . 2_656 ?
N2 Co1 N1 76.53(12) 2_656 2_656 ?
N2 Co1 N1 76.53(12) . . ?
N2 Co1 N2 119.91(17) . 2_656 ?
N3 Co1 N1 130.00(13) 2_656 . ?
N3 Co1 N1 85.83(12) 2_656 2_656 ?
N3 Co1 N1 85.83(12) . . ?
N3 Co1 N1 130.00(13) . 2_656 ?
N3 Co1 N2 87.07(12) . 2_656 ?
N3 Co1 N2 144.39(12) . . ?
N3 Co1 N2 144.39(12) 2_656 2_656 ?
N3 Co1 N2 87.07(12) 2_656 . ?
N3 Co1 N3 80.93(18) 2_656 . ?
O1 N1 Co1 123.5(2) . . ?
C1 N1 Co1 116.8(3) . . ?
C1 N1 O1 119.0(3) . . ?
N1 O1 B1 112.7(3) . . ?
O1 B1 C4 111.8(3) . . ?
O1 B1 O3 109.4(3) . . ?
O1 B1 O2 108.8(3) . 2_656 ?
O3 B1 C4 107.4(3) . . ?
O2 B1 C4 109.3(3) 2_656 . ?
O2 B1 O3 110.1(3) 2_656 . ?
H6A C6 H6B 107.7 . . ?
C7 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
C7 C6 C5 113.4(3) . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 N2 Co1 118.5(3) . . ?
C2 N2 O2 118.3(3) . . ?
O2 N2 Co1 123.1(2) . . ?
B1 C4 H4A 108.8 . . ?
B1 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 B1 114.0(3) . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
N2 C2 Br2 122.3(3) . . ?
N2 C2 C1 114.5(3) . . ?
C1 C2 Br2 123.2(3) . . ?
N1 C1 Br1 125.0(3) . . ?
N1 C1 C2 113.4(3) . . ?
C2 C1 Br1 121.6(3) . . ?
C6 C5 C4 113.8(3) . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N3 O3 B1 115.9(3) . . ?
O3 N3 Co1 124.4(2) . . ?
C3 N3 Co1 116.6(3) . . ?
C3 N3 O3 118.6(3) . . ?
N3 C3 Br3 122.8(3) . . ?
N3 C3 C3 112.7(2) . 2_656 ?
C3 C3 Br3 124.45(11) 2_656 . ?
N2 O2 B1 114.6(3) . 2_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br2 C2 C1 Br1 -5.5(4) . . . . ?
Br2 C2 C1 N1 176.3(3) . . . . ?
Co1 N1 O1 B1 8.4(4) . . . . ?
Co1 N1 C1 Br1 -172.98(18) . . . . ?
Co1 N1 C1 C2 5.2(4) . . . . ?
Co1 N2 C2 Br2 -178.75(16) . . . . ?
Co1 N2 C2 C1 2.5(4) . . . . ?
Co1 N2 O2 B1 3.6(4) . . . 2_656 ?
Co1 N3 C3 Br3 -174.08(17) . . . . ?
Co1 N3 C3 C3 5.2(5) . . . 2_656 ?
N1 Co1 N3 O3 -43.0(3) . . . . ?
N1 Co1 N3 O3 108.7(3) 2_656 . . . ?
N1 Co1 N3 C3 -78.7(3) 2_656 . . . ?
N1 Co1 N3 C3 129.6(3) . . . . ?
N1 O1 B1 C4 178.3(3) . . . . ?
N1 O1 B1 O3 -62.9(4) . . . . ?
N1 O1 B1 O2 57.5(4) . . . 2_656 ?
O1 N1 C1 Br1 -1.6(5) . . . . ?
O1 N1 C1 C2 176.5(3) . . . . ?
O1 B1 C4 C5 179.9(3) . . . . ?
O1 B1 O3 N3 59.3(4) . . . . ?
B1 C4 C5 C6 -177.5(3) . . . . ?
B1 O3 N3 Co1 4.1(4) . . . . ?
B1 O3 N3 C3 -168.4(3) . . . . ?
C7 C6 C5 C4 63.3(4) . . . . ?
N2 Co1 N3 O3 -102.8(3) . . . . ?
N2 Co1 N3 O3 39.0(3) 2_656 . . . ?
N2 Co1 N3 C3 69.8(3) . . . . ?
N2 Co1 N3 C3 -148.4(3) 2_656 . . . ?
N2 C2 C1 Br1 173.2(3) . . . . ?
N2 C2 C1 N1 -5.0(5) . . . . ?
C4 B1 O3 N3 -179.2(3) . . . . ?
C2 N2 O2 B1 -172.6(3) . . . 2_656 ?
C1 N1 O1 B1 -162.4(3) . . . . ?
O3 B1 C4 C5 59.8(4) . . . . ?
O3 N3 C3 Br3 -1.0(4) . . . . ?
O3 N3 C3 C3 178.3(3) . . . 2_656 ?
N3 Co1 N3 O3 -174.6(3) 2_656 . . . ?
N3 Co1 N3 C3 -2.02(19) 2_656 . . . ?
O2 B1 C4 C5 -59.6(4) 2_656 . . . ?
O2 B1 O3 N3 -60.3(4) 2_656 . . . ?
O2 N2 C2 Br2 -2.4(5) . . . . ?
O2 N2 C2 C1 178.8(3) . . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co60
_database_code_depnum_ccdc_archive 'CCDC 1027586'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_vrf_SYMMS02_Co60                
;
PROBLEM: The unit-cell lengths a and c should not be equal 
RESPONSE: These parameters in fact slightly differ from each other as
can be seen from crystal parameters at other temperatures.
;
_audit_creation_date             2014-11-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.455(4)
_cell_length_b                   8.2599(17)
_cell_length_c                   17.455(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.56(3)
_cell_angle_gamma                90
_cell_volume                     2515.8(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3751
_cell_measurement_temperature    60(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.257
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10951
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         32.280
_diffrn_reflns_theta_min         2.334
_diffrn_ambient_temperature      60(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.788
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2290
_reflns_number_total             3531
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'Apex II'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.231
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0902
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim
Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.64393(10) 0.2500 0.0152(2) Uani 1 2 d S T P . .
O1 O 0.34857(15) 0.7246(3) 0.17882(16) 0.0081(7) Uani 1 1 d . U . . .
N1 N 0.39159(19) 0.7374(4) 0.2433(2) 0.0087(8) Uani 1 1 d . . . . .
C1 C 0.3678(2) 0.8269(5) 0.2979(2) 0.0069(9) Uani 1 1 d . U . . .
Br1 Br 0.27645(2) 0.94489(6) 0.29969(3) 0.01638(13) Uani 1 1 d . . . . .
C2 C 0.4214(2) 0.8381(5) 0.3610(2) 0.0096(10) Uani 1 1 d . . . . .
Br2 Br 0.39990(3) 0.95108(6) 0.45102(3) 0.02203(15) Uani 1 1 d . . . . .
N2 N 0.48521(19) 0.7654(4) 0.3479(2) 0.0072(8) Uani 1 1 d . . . . .
O2 O 0.53778(16) 0.7644(3) 0.40447(16) 0.0091(7) Uani 1 1 d . U . . .
O3 O 0.41926(16) 0.4881(3) 0.12935(16) 0.0087(7) Uani 1 1 d . . . . .
N3 N 0.4643(2) 0.4716(4) 0.1905(2) 0.0081(8) Uani 1 1 d . . . . .
C3 C 0.4769(2) 0.3257(5) 0.2169(2) 0.0079(9) Uani 1 1 d . . . . .
Br3 Br 0.43790(3) 0.14165(6) 0.17160(3) 0.01904(14) Uani 1 1 d . . . . .
B1 B 0.3944(3) 0.6588(6) 0.1114(3) 0.0082(11) Uani 1 1 d . . . . .
C4 C 0.3440(2) 0.6490(5) 0.0382(2) 0.0081(9) Uani 1 1 d . . . . .
H4A H 0.3241 0.7560 0.0265 0.010 Uiso 1 1 calc R . . . .
H4B H 0.3007 0.5788 0.0476 0.010 Uiso 1 1 calc R . . . .
C5 C 0.3868(3) 0.5843(6) -0.0327(2) 0.0113(10) Uani 1 1 d . . . . .
H5A H 0.4292 0.6565 -0.0431 0.014 Uiso 1 1 calc R . . . .
H5B H 0.4082 0.4787 -0.0204 0.014 Uiso 1 1 calc R . . . .
C6 C 0.3374(2) 0.5701(6) -0.1031(3) 0.0135(10) Uani 1 1 d . U . . .
H6A H 0.3681 0.5338 -0.1453 0.016 Uiso 1 1 calc R . . . .
H6B H 0.3165 0.6756 -0.1164 0.016 Uiso 1 1 calc R . . . .
C7 C 0.2712(3) 0.4500(6) -0.0917(3) 0.0181(11) Uani 1 1 d . . . . .
H7A H 0.2447 0.4316 -0.1398 0.027 Uiso 1 1 calc GR . . . .
H7B H 0.2362 0.4942 -0.0557 0.027 Uiso 1 1 calc GR . . . .
H7C H 0.2914 0.3494 -0.0724 0.027 Uiso 1 1 calc GR . . . .


_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
Co1 N1 2.044(3) 2_655 ?
Co1 N1 2.044(3) . ?
Co1 N2 2.004(4) . ?
Co1 N2 2.004(4) 2_655 ?
Co1 N3 1.860(4) . ?
Co1 N3 1.860(4) 2_655 ?
O1 N1 1.341(4) . ?
O1 B1 1.540(6) . ?
N1 C1 1.283(5) . ?
C1 Br1 1.870(4) . ?
C1 C2 1.430(5) . ?
C2 Br2 1.874(4) . ?
C2 N2 1.291(5) . ?
N2 O2 1.330(4) . ?
O2 B1 1.502(6) 2_655 ?
O3 N3 1.315(4) . ?
O3 B1 1.505(6) . ?
N3 C3 1.306(5) . ?
C3 C3 1.392(8) 2_655 ?
C3 Br3 1.836(4) . ?
B1 O2 1.502(6) 2_655 ?
B1 C4 1.534(6) . ?
C4 C5 1.558(6) . ?
C5 C6 1.487(5) . ?
C6 C7 1.540(6) . ?

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
N1 Co1 N1 135.6(2) 2_655 . ?
N2 Co1 N1 73.67(14) 2_655 2_655 ?
N2 Co1 N1 84.43(14) 2_655 . ?
N2 Co1 N1 73.67(14) . . ?
N2 Co1 N1 84.43(14) . 2_655 ?
N2 Co1 N2 119.9(2) 2_655 . ?
N3 Co1 N1 87.79(15) 2_655 2_655 ?
N3 Co1 N1 128.08(15) 2_655 . ?
N3 Co1 N1 128.08(15) . 2_655 ?
N3 Co1 N1 87.79(15) . . ?
N3 Co1 N2 87.51(14) 2_655 . ?
N3 Co1 N2 144.12(15) . . ?
N3 Co1 N2 144.12(15) 2_655 2_655 ?
N3 Co1 N2 87.51(14) . 2_655 ?
N3 Co1 N3 80.1(2) . 2_655 ?
N1 O1 B1 112.3(3) . . ?
O1 N1 Co1 121.0(3) . . ?
C1 N1 Co1 119.5(3) . . ?
C1 N1 O1 118.9(3) . . ?
N1 C1 Br1 127.3(3) . . ?
N1 C1 C2 113.1(4) . . ?
C2 C1 Br1 119.6(3) . . ?
C1 C2 Br2 122.5(3) . . ?
N2 C2 C1 112.4(4) . . ?
N2 C2 Br2 125.1(3) . . ?
C2 N2 Co1 121.1(3) . . ?
C2 N2 O2 116.8(4) . . ?
O2 N2 Co1 121.9(3) . . ?
N2 O2 B1 113.4(3) . 2_655 ?
N3 O3 B1 115.4(3) . . ?
O3 N3 Co1 123.9(3) . . ?
C3 N3 Co1 117.3(3) . . ?
C3 N3 O3 118.2(3) . . ?
N3 C3 C3 112.4(2) . 2_655 ?
N3 C3 Br3 123.7(3) . . ?
C3 C3 Br3 123.87(13) 2_655 . ?
O2 B1 O1 111.4(4) 2_655 . ?
O2 B1 O3 111.0(4) 2_655 . ?
O2 B1 C4 108.3(4) 2_655 . ?
O3 B1 O1 108.9(4) . . ?
O3 B1 C4 106.2(4) . . ?
C4 B1 O1 110.9(4) . . ?
B1 C4 C5 113.8(3) . . ?
C6 C5 C4 113.8(4) . . ?
C5 C6 C7 111.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N1 C1 Br1 172.2(2) . . . . ?
Co1 N1 C1 C2 -4.8(5) . . . . ?
Co1 N2 O2 B1 -2.7(4) . . . 2_655 ?
Co1 N3 C3 C3 -6.3(6) . . . 2_655 ?
Co1 N3 C3 Br3 173.6(2) . . . . ?
O1 N1 C1 Br1 0.9(6) . . . . ?
O1 N1 C1 C2 -176.1(3) . . . . ?
O1 B1 C4 C5 179.6(4) . . . . ?
N1 Co1 N3 O3 -107.3(3) 2_655 . . . ?
N1 Co1 N3 O3 44.1(3) . . . . ?
N1 Co1 N3 C3 81.6(4) 2_655 . . . ?
N1 Co1 N3 C3 -126.9(3) . . . . ?
N1 O1 B1 O2 -58.1(4) . . . 2_655 ?
N1 O1 B1 O3 64.6(4) . . . . ?
N1 O1 B1 C4 -178.8(3) . . . . ?
N1 C1 C2 Br2 -176.5(3) . . . . ?
N1 C1 C2 N2 4.8(6) . . . . ?
C1 C2 N2 Co1 -2.9(5) . . . . ?
C1 C2 N2 O2 -177.7(3) . . . . ?
Br1 C1 C2 Br2 6.2(5) . . . . ?
Br1 C1 C2 N2 -172.5(3) . . . . ?
C2 N2 O2 B1 172.1(4) . . . 2_655 ?
Br2 C2 N2 Co1 178.5(2) . . . . ?
Br2 C2 N2 O2 3.7(6) . . . . ?
N2 Co1 N3 O3 101.9(4) . . . . ?
N2 Co1 N3 O3 -40.4(3) 2_655 . . . ?
N2 Co1 N3 C3 148.6(3) 2_655 . . . ?
N2 Co1 N3 C3 -69.1(4) . . . . ?
O2 B1 C4 C5 57.1(5) 2_655 . . . ?
O3 N3 C3 C3 -177.8(4) . . . 2_655 ?
O3 N3 C3 Br3 2.1(6) . . . . ?
O3 B1 C4 C5 -62.2(5) . . . . ?
N3 Co1 N3 O3 173.4(4) 2_655 . . . ?
N3 Co1 N3 C3 2.4(2) 2_655 . . . ?
N3 O3 B1 O1 -61.3(4) . . . . ?
N3 O3 B1 O2 61.7(5) . . . 2_655 ?
N3 O3 B1 C4 179.2(3) . . . . ?
B1 O1 N1 Co1 -8.8(4) . . . . ?
B1 O1 N1 C1 162.4(4) . . . . ?
B1 O3 N3 Co1 -2.7(5) . . . . ?
B1 O3 N3 C3 168.2(4) . . . . ?
B1 C4 C5 C6 178.2(4) . . . . ?
C4 C5 C6 C7 -61.4(5) . . . . ?

