# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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/access/V1 
# 
# 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_i
_database_code_depnum_ccdc_archive 'CCDC 1059601'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H48 Br8 Fe2 N8 O'
_chemical_formula_weight         1984.32

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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   28.406(2)
_cell_length_b                   15.1613(11)
_cell_length_c                   19.2086(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.473(9)
_cell_angle_gamma                90.00
_cell_volume                     8160.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3153
_cell_measurement_theta_min      2.9238
_cell_measurement_theta_max      28.9132

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PURPLE
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3888
_exptl_absorpt_coefficient_mu    4.324
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.3475
_exptl_absorpt_correction_T_max  0.4362
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23088
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7168
_reflns_number_gt                3409
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
Highest peak    1.50  at  0.1416  0.4440  0.0426  [  1.24 A from BR4 ]
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0903P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7168
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.0808
_refine_ls_wR_factor_ref         0.2229
_refine_ls_wR_factor_gt          0.1855
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.46752(4) 0.56183(6) 0.32047(5) 0.0371(3) Uani 1 1 d . . .
N1 N 0.3977(2) 0.5274(4) 0.2769(3) 0.0406(15) Uani 1 1 d . . .
N2 N 0.4755(2) 0.4336(3) 0.3605(3) 0.0368(14) Uani 1 1 d . . .
N3 N 0.5174(2) 0.5985(4) 0.4066(3) 0.0379(14) Uani 1 1 d . . .
N4 N 0.4446(2) 0.6919(4) 0.3188(3) 0.0395(15) Uani 1 1 d . . .
O1 O 0.5000 0.5563(4) 0.2500 0.0486(18) Uani 1 2 d S . .
Br1 Br 0.21679(7) 0.89528(12) 0.04700(11) 0.1803(9) Uani 1 1 d . . .
Br2 Br 0.30676(5) 0.00802(8) 0.21261(10) 0.1380(7) Uani 1 1 d . . .
Br3 Br 0.73544(4) 0.27466(10) 0.59356(6) 0.1071(5) Uani 1 1 d . . .
Br4 Br 0.61139(7) 1.10494(9) 0.50758(8) 0.1533(8) Uani 1 1 d . . .
C1 C 0.3792(3) 0.4425(5) 0.2667(4) 0.0440(19) Uani 1 1 d . . .
C2 C 0.3328(3) 0.4481(5) 0.2273(4) 0.053(2) Uani 1 1 d . . .
H2 H 0.3123 0.4008 0.2147 0.064 Uiso 1 1 calc R . .
C3 C 0.3232(3) 0.5324(5) 0.2111(4) 0.057(2) Uani 1 1 d . . .
H3 H 0.2952 0.5544 0.1850 0.068 Uiso 1 1 calc R . .
C4 C 0.3637(3) 0.5821(5) 0.2409(4) 0.0423(18) Uani 1 1 d . . .
C5 C 0.3672(3) 0.6739(5) 0.2357(4) 0.0432(19) Uani 1 1 d . . .
C6 C 0.3292(3) 0.7224(5) 0.1903(4) 0.051(2) Uani 1 1 d . . .
C7 C 0.3361(4) 0.7512(9) 0.1256(5) 0.110(4) Uani 1 1 d . . .
H7 H 0.3644 0.7373 0.1097 0.132 Uiso 1 1 calc R . .
C9 C 0.2615(4) 0.8220(7) 0.1061(8) 0.089(3) Uani 1 1 d . . .
C10 C 0.2534(4) 0.7967(8) 0.1698(8) 0.097(4) Uani 1 1 d . . .
H10 H 0.2252 0.8117 0.1856 0.116 Uiso 1 1 calc R . .
C11 C 0.2882(4) 0.7475(7) 0.2113(6) 0.084(3) Uani 1 1 d . . .
H11 H 0.2831 0.7309 0.2561 0.101 Uiso 1 1 calc R . .
C12 C 0.4047(3) 0.7239(4) 0.2739(4) 0.0421(19) Uani 1 1 d . . .
C13 C 0.4056(3) 0.8185(5) 0.2763(4) 0.051(2) Uani 1 1 d . . .
H13 H 0.3831 0.8557 0.2507 0.062 Uiso 1 1 calc R . .
C14 C 0.4437(3) 0.8438(5) 0.3210(4) 0.053(2) Uani 1 1 d . . .
H14 H 0.4529 0.9016 0.3326 0.063 Uiso 1 1 calc R . .
C15 C 0.4688(3) 0.7634(5) 0.3485(4) 0.047(2) Uani 1 1 d . . .
C16 C 0.5095(3) 0.7611(5) 0.4001(4) 0.0427(19) Uani 1 1 d . . .
C17 C 0.5332(3) 0.8456(5) 0.4272(4) 0.052(2) Uani 1 1 d . . .
C18 C 0.5543(4) 0.8984(6) 0.3832(5) 0.091(4) Uani 1 1 d . . .
H18 H 0.5527 0.8820 0.3362 0.109 Uiso 1 1 calc R . .
C19 C 0.5779(5) 0.9758(6) 0.4069(6) 0.108(4) Uani 1 1 d . . .
H19 H 0.5921 1.0107 0.3763 0.130 Uiso 1 1 calc R . .
C20 C 0.5798(4) 0.9992(6) 0.4752(6) 0.085(3) Uani 1 1 d . . .
C21 C 0.5572(4) 0.9514(6) 0.5182(5) 0.082(3) Uani 1 1 d . . .
H21 H 0.5579 0.9692 0.5647 0.098 Uiso 1 1 calc R . .
C22 C 0.5327(3) 0.8758(5) 0.4939(4) 0.065(3) Uani 1 1 d . . .
H22 H 0.5157 0.8451 0.5234 0.078 Uiso 1 1 calc R . .
C23 C 0.5322(3) 0.6833(5) 0.4279(4) 0.046(2) Uani 1 1 d . . .
C24 C 0.5735(3) 0.6793(5) 0.4818(4) 0.052(2) Uani 1 1 d . . .
H24 H 0.5891 0.7270 0.5059 0.062 Uiso 1 1 calc R . .
C25 C 0.5857(3) 0.5934(5) 0.4913(4) 0.050(2) Uani 1 1 d . . .
H25 H 0.6116 0.5710 0.5223 0.059 Uiso 1 1 calc R . .
C26 C 0.5511(3) 0.5437(5) 0.4444(4) 0.0413(18) Uani 1 1 d . . .
C27 C 0.5533(2) 0.4523(5) 0.4367(4) 0.0395(17) Uani 1 1 d . . .
C28 C 0.5967(3) 0.4076(4) 0.4728(4) 0.0418(19) Uani 1 1 d . . .
C29 C 0.6413(3) 0.4216(5) 0.4533(4) 0.054(2) Uani 1 1 d . . .
H29 H 0.6434 0.4577 0.4147 0.065 Uiso 1 1 calc R . .
C30 C 0.6816(3) 0.3845(6) 0.4886(5) 0.062(2) Uani 1 1 d . . .
H30 H 0.7110 0.3969 0.4757 0.074 Uiso 1 1 calc R . .
C31 C 0.6785(3) 0.3270(6) 0.5450(5) 0.058(2) Uani 1 1 d . . .
C32 C 0.6367(3) 0.3121(5) 0.5652(5) 0.060(2) Uani 1 1 d . . .
H32 H 0.6351 0.2764 0.6041 0.072 Uiso 1 1 calc R . .
C33 C 0.5956(3) 0.3494(5) 0.5289(4) 0.052(2) Uani 1 1 d . . .
H33 H 0.5664 0.3354 0.5420 0.063 Uiso 1 1 calc R . .
C34 C 0.5182(3) 0.4014(5) 0.3962(4) 0.0416(18) Uani 1 1 d . . .
C36 C 0.4772(3) 0.2841(5) 0.3497(4) 0.053(2) Uani 1 1 d . . .
H36 H 0.4674 0.2271 0.3365 0.064 Uiso 1 1 calc R . .
C37 C 0.4501(3) 0.3628(5) 0.3312(4) 0.0456(19) Uani 1 1 d . . .
C39 C 0.3796(3) 0.2781(5) 0.2708(4) 0.049(2) Uani 1 1 d . . .
C40 C 0.3671(3) 0.2254(6) 0.3237(5) 0.074(3) Uani 1 1 d . . .
H40 H 0.3731 0.2433 0.3707 0.089 Uiso 1 1 calc R . .
C42 C 0.3368(4) 0.1187(6) 0.2369(7) 0.076(3) Uani 1 1 d . . .
C43 C 0.3495(3) 0.1707(6) 0.1846(5) 0.072(3) Uani 1 1 d . . .
H43 H 0.3431 0.1525 0.1378 0.086 Uiso 1 1 calc R . .
C44 C 0.3720(3) 0.2513(5) 0.2026(5) 0.067(3) Uani 1 1 d . . .
H44 H 0.3817 0.2864 0.1679 0.080 Uiso 1 1 calc R . .
C8 C 0.3022(5) 0.8005(10) 0.0834(6) 0.138(6) Uani 1 1 d . . .
H8 H 0.3075 0.8190 0.0391 0.166 Uiso 1 1 calc R . .
C35 C 0.5190(3) 0.3063(5) 0.3893(4) 0.052(2) Uani 1 1 d . . .
H35 H 0.5435 0.2684 0.4084 0.062 Uiso 1 1 calc R . .
C38 C 0.4034(3) 0.3655(5) 0.2912(4) 0.046(2) Uani 1 1 d . . .
C41 C 0.3452(4) 0.1448(6) 0.3046(7) 0.094(4) Uani 1 1 d . . .
H41 H 0.3363 0.1085 0.3392 0.113 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe O1 1.7611(10) . ?
Fe N3 2.070(6) . ?
Fe N4 2.076(6) . ?
Fe N1 2.089(6) . ?
Fe N2 2.090(5) . ?
N1 C4 1.372(9) . ?
N1 C1 1.392(9) . ?
N2 C37 1.362(9) . ?
N2 C34 1.381(9) . ?
N3 C26 1.379(9) . ?
N3 C23 1.393(8) . ?
N4 C15 1.357(9) . ?
N4 C12 1.394(9) . ?
O1 Fe 1.7611(10) 2_655 ?
Br1 C9 1.913(11) . ?
Br2 C42 1.905(8) . ?
Br3 C31 1.901(8) . ?
Br4 C20 1.891(9) . ?
C1 C38 1.397(10) . ?
C1 C2 1.409(11) . ?
C2 C3 1.333(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.414(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(9) . ?
C5 C12 1.411(10) . ?
C5 C6 1.468(10) . ?
C6 C11 1.348(11) . ?
C6 C7 1.362(12) . ?
C7 C8 1.374(14) . ?
C7 H7 0.9300 . ?
C9 C10 1.339(15) . ?
C9 C8 1.341(16) . ?
C10 C11 1.383(14) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.435(10) . ?
C13 C14 1.324(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.465(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.395(11) . ?
C16 C23 1.406(10) . ?
C16 C17 1.500(10) . ?
C17 C22 1.362(10) . ?
C17 C18 1.370(11) . ?
C18 C19 1.390(12) . ?
C18 H18 0.9300 . ?
C19 C20 1.352(13) . ?
C19 H19 0.9300 . ?
C20 C21 1.341(13) . ?
C21 C22 1.380(11) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.432(11) . ?
C24 C25 1.352(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.434(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.396(9) . ?
C27 C34 1.392(10) . ?
C27 C28 1.477(10) . ?
C28 C29 1.396(10) . ?
C28 C33 1.396(10) . ?
C29 C30 1.354(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.404(11) . ?
C30 H30 0.9300 . ?
C31 C32 1.330(12) . ?
C32 C33 1.378(11) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.447(9) . ?
C36 C35 1.345(11) . ?
C36 C37 1.431(10) . ?
C36 H36 0.9300 . ?
C37 C38 1.421(11) . ?
C39 C44 1.354(11) . ?
C39 C40 1.386(11) . ?
C39 C38 1.510(10) . ?
C40 C41 1.392(13) . ?
C40 H40 0.9300 . ?
C42 C41 1.343(14) . ?
C42 C43 1.370(13) . ?
C43 C44 1.396(12) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C8 H8 0.9300 . ?
C35 H35 0.9300 . ?
C41 H41 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe N3 104.49(17) . . ?
O1 Fe N4 103.6(3) . . ?
N3 Fe N4 85.9(2) . . ?
O1 Fe N1 105.28(16) . . ?
N3 Fe N1 150.2(2) . . ?
N4 Fe N1 87.5(2) . . ?
O1 Fe N2 101.5(3) . . ?
N3 Fe N2 86.4(2) . . ?
N4 Fe N2 154.8(2) . . ?
N1 Fe N2 87.3(2) . . ?
C4 N1 C1 105.7(6) . . ?
C4 N1 Fe 126.5(5) . . ?
C1 N1 Fe 126.8(5) . . ?
C37 N2 C34 106.7(6) . . ?
C37 N2 Fe 124.3(5) . . ?
C34 N2 Fe 123.0(5) . . ?
C26 N3 C23 104.6(6) . . ?
C26 N3 Fe 125.7(4) . . ?
C23 N3 Fe 128.1(5) . . ?
C15 N4 C12 106.6(6) . . ?
C15 N4 Fe 128.1(5) . . ?
C12 N4 Fe 124.1(5) . . ?
Fe O1 Fe 174.5(4) . 2_655 ?
N1 C1 C38 124.9(7) . . ?
N1 C1 C2 108.5(7) . . ?
C38 C1 C2 126.6(7) . . ?
C3 C2 C1 108.8(8) . . ?
C3 C2 H2 125.6 . . ?
C1 C2 H2 125.6 . . ?
C2 C3 C4 107.1(7) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
N1 C4 C5 125.8(7) . . ?
N1 C4 C3 109.9(6) . . ?
C5 C4 C3 124.3(7) . . ?
C4 C5 C12 123.6(7) . . ?
C4 C5 C6 119.1(7) . . ?
C12 C5 C6 117.3(6) . . ?
C11 C6 C7 116.3(9) . . ?
C11 C6 C5 123.3(8) . . ?
C7 C6 C5 120.1(8) . . ?
C6 C7 C8 121.4(11) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C10 C9 C8 121.0(11) . . ?
C10 C9 Br1 120.7(10) . . ?
C8 C9 Br1 118.2(11) . . ?
C9 C10 C11 117.8(11) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C6 C11 C10 123.5(10) . . ?
C6 C11 H11 118.3 . . ?
C10 C11 H11 118.3 . . ?
N4 C12 C5 127.1(6) . . ?
N4 C12 C13 108.6(7) . . ?
C5 C12 C13 124.2(7) . . ?
C14 C13 C12 108.6(8) . . ?
C14 C13 H13 125.7 . . ?
C12 C13 H13 125.7 . . ?
C13 C14 C15 106.8(7) . . ?
C13 C14 H14 126.6 . . ?
C15 C14 H14 126.6 . . ?
N4 C15 C16 125.5(7) . . ?
N4 C15 C14 109.3(7) . . ?
C16 C15 C14 125.1(8) . . ?
C15 C16 C23 124.5(7) . . ?
C15 C16 C17 119.8(7) . . ?
C23 C16 C17 115.6(7) . . ?
C22 C17 C18 117.1(7) . . ?
C22 C17 C16 122.7(7) . . ?
C18 C17 C16 120.1(7) . . ?
C17 C18 C19 121.8(9) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C20 C19 C18 118.7(9) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
C21 C20 C19 120.5(9) . . ?
C21 C20 Br4 120.4(7) . . ?
C19 C20 Br4 118.9(8) . . ?
C20 C21 C22 120.4(8) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 121.0(8) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N3 C23 C16 124.4(7) . . ?
N3 C23 C24 110.2(7) . . ?
C16 C23 C24 125.5(7) . . ?
C25 C24 C23 107.4(7) . . ?
C25 C24 H24 126.3 . . ?
C23 C24 H24 126.3 . . ?
C24 C25 C26 106.7(7) . . ?
C24 C25 H25 126.7 . . ?
C26 C25 H25 126.7 . . ?
N3 C26 C27 125.5(6) . . ?
N3 C26 C25 111.0(6) . . ?
C27 C26 C25 123.4(7) . . ?
C34 C27 C26 124.8(6) . . ?
C34 C27 C28 118.2(6) . . ?
C26 C27 C28 117.0(6) . . ?
C29 C28 C33 116.0(8) . . ?
C29 C28 C27 121.9(7) . . ?
C33 C28 C27 122.0(7) . . ?
C30 C29 C28 122.2(8) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 H29 118.9 . . ?
C29 C30 C31 119.4(8) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C32 C31 C30 120.1(8) . . ?
C32 C31 Br3 121.0(7) . . ?
C30 C31 Br3 118.8(7) . . ?
C31 C32 C33 120.4(8) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C32 C33 C28 121.8(8) . . ?
C32 C33 H33 119.1 . . ?
C28 C33 H33 119.1 . . ?
N2 C34 C27 124.7(6) . . ?
N2 C34 C35 109.4(7) . . ?
C27 C34 C35 125.7(7) . . ?
C35 C36 C37 108.6(7) . . ?
C35 C36 H36 125.7 . . ?
C37 C36 H36 125.7 . . ?
N2 C37 C38 125.8(7) . . ?
N2 C37 C36 109.2(7) . . ?
C38 C37 C36 125.0(7) . . ?
C44 C39 C40 121.2(8) . . ?
C44 C39 C38 120.6(7) . . ?
C40 C39 C38 118.2(7) . . ?
C39 C40 C41 118.0(9) . . ?
C39 C40 H40 121.0 . . ?
C41 C40 H40 121.0 . . ?
C41 C42 C43 120.9(8) . . ?
C41 C42 Br2 119.9(9) . . ?
C43 C42 Br2 119.2(8) . . ?
C42 C43 C44 119.1(8) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
C39 C44 C43 119.7(9) . . ?
C39 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C9 C8 C7 119.9(11) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C36 C35 C34 106.0(7) . . ?
C36 C35 H35 127.0 . . ?
C34 C35 H35 127.0 . . ?
C1 C38 C37 124.8(7) . . ?
C1 C38 C39 118.1(7) . . ?
C37 C38 C39 117.0(7) . . ?
C42 C41 C40 121.0(10) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.104

####################################################################### 
# 
# 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/access/V1 
# 
# 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_q
_database_code_depnum_ccdc_archive 'CCDC 1059602'
_audit_update_record             
;
2015-05-13 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46.50 H29.50 Br4 Cl Fe N4.75 O0.75'
_chemical_formula_weight         1077.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   14.2862(11)
_cell_length_b                   15.307(3)
_cell_length_c                   19.102(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.637(8)
_cell_angle_gamma                90.00
_cell_volume                     4163.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1755
_cell_measurement_theta_min      3.1009
_cell_measurement_theta_max      66.7631

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2123
_exptl_absorpt_coefficient_mu    8.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1890
_exptl_absorpt_correction_T_max  0.2299
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1396
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         24.98
_reflns_number_total             717
_reflns_number_gt                655
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

B Alert

CHEMW03_ALERT_2_B WARNING: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.95 <> 1.05
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          1077.69
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   44.00  528.48
           H         1.01   24.00   24.19
           N        14.01    4.00   56.03
           Cl       35.45    1.00   35.45
           Fe       55.85    1.00   55.85
           Br       79.90    4.00  319.62
           O        16.00    0.00    0.00
           Calculated formula weight             1019.62
Explain

Due to the removed disordered solvent by the SQUEEZE, the chemical formula weight is different from the calculated formula weight.

To limit the intense vibration of some atoms induced by the temperature, we added the restraints command simu 0.02 0.04 3.8 $c $n

TITL Q in P2(1)/c 
CELL 1.54178  14.2862  15.3074  19.1019  90.000  94.637  90.000 
ZERR    4.00   0.0011   0.0027   0.0029   0.000   0.008   0.000 
LATT 1 
SYMM -X, 0.5+Y, 0.5-Z 
SFAC C  H  N  Cl Fe Br O  
UNIT 186 118 19 4 4 16 3 
OMIT   0.00  50.00
L.S. 20
ACTA
BOND 
FMAP 2
PLAN 10
size 0.30 0.27 0.25 
simu 0.02 0.04 3.8 $c $n 
FREE C23  C25 
FREE C15  C13 
FREE C3   C1  
FREE C9   C43 
WGHT  0.071300  0.000000 
FVAR  0.408080
MOLE 1
N4     3   0.179585  0.464135  0.218140 11.000000  0.030930  0.023360 = 
           0.028720 -0.002300 -0.000290  0.004300
N3     3   0.029491  0.549418  0.140584 11.000000  0.032520  0.022540 = 
           0.029420  0.005050 -0.016160 -0.000240
C23    1  -0.052085  0.579567  0.105023 11.000000  0.033890  0.023370 = 
           0.036330  0.005650 -0.011990  0.001140
N2     3  -0.043008  0.384707  0.096620 11.000000  0.037520  0.024600 = 
           0.034520  0.006880 -0.014560  0.005900
C3     1   0.099220  0.148582  0.183113 11.000000  0.034850  0.024560 = 
           0.032470 -0.001560 -0.009020  0.005130
AFIX 43
H3     2   0.082871  0.090681  0.173821 11.000000 -1.200000
AFIX 0
C26    1   0.076727  0.622783  0.167062 11.000000  0.036050  0.023880 = 
           0.029860  0.007770 -0.007840  0.000700
C25    1   0.021310  0.698428  0.148309 11.000000  0.038190  0.023650 = 
           0.032340 -0.001980 -0.015580 -0.000420
AFIX 43
H25    2   0.037698  0.755772  0.159764 11.000000 -1.200000
AFIX 0
C9     1  -0.142696 -0.016265  0.019025 11.000000  0.046730  0.027870 = 
           0.036880 -0.006370  0.000260 -0.003230
N1     3   0.099948  0.295987  0.180602 11.000000  0.034470  0.022380 = 
           0.028570 -0.004070 -0.016660  0.006060
C4     1   0.050922  0.224036  0.151798 11.000000  0.036510  0.022530 = 
           0.026430  0.001490 -0.004910  0.005210
C6     1  -0.060359  0.136820  0.074124 11.000000  0.041380  0.024090 = 
           0.026000  0.000720 -0.003640 -0.002920
C14    1  -0.173876  0.384646  0.016047 11.000000  0.042030  0.026770 = 
           0.042270  0.001670 -0.016970  0.004270
AFIX 43
H14    2  -0.223091  0.405541 -0.014205 11.000000 -1.200000
AFIX 0
C10    1  -0.106388  0.045195 -0.024082 11.000000  0.051810  0.029340 = 
           0.032310  0.001790  0.000220 -0.004010
AFIX 43
H10    2  -0.109658  0.034980 -0.072211 11.000000 -1.200000
AFIX 0
C34    1   0.214819  0.547893  0.222701 11.000000  0.036250  0.023950 = 
           0.035710  0.003680 -0.015480 -0.000170
C20    1  -0.361302  0.627098 -0.049532 11.000000  0.028730  0.047210 = 
           0.036280  0.019870 -0.013690  0.007190
C39    1   0.328934  0.273696  0.295090 11.000000  0.037520  0.037650 = 
           0.038230 -0.004520 -0.009750  0.006270
C17    1  -0.199618  0.566838  0.029351 11.000000  0.033090  0.030150 = 
           0.031600  0.005360 -0.009460  0.002810
C5     1  -0.024864  0.222312  0.101228 11.000000  0.038320  0.022430 = 
           0.027700 -0.000130 -0.004550  0.002630
C28    1   0.209740  0.705252  0.216986 11.000000  0.041530  0.029210 = 
           0.035970  0.004590 -0.005400 -0.009650
C7     1  -0.095722  0.075332  0.119094 11.000000  0.041980  0.020490 = 
           0.029540 -0.002290 -0.003410  0.003320
AFIX 43
H7     2  -0.092608  0.085725  0.167194 11.000000 -1.200000
AFIX 0
C15    1  -0.110428  0.435784  0.060860 11.000000  0.037010  0.027450 = 
           0.034600  0.004400 -0.020210  0.003770
C1     1   0.174229  0.269026  0.224688 11.000000  0.038050  0.026810 = 
           0.030340 -0.001100 -0.009380  0.008520
C38    1   0.248639  0.316116  0.255806 11.000000  0.033550  0.031090 = 
           0.032100  0.004450 -0.009420  0.005490
C8     1  -0.135828 -0.001912  0.091563 11.000000  0.044600  0.024890 = 
           0.022590  0.006840 -0.007040 -0.011550
AFIX 43
H8     2  -0.157928 -0.043731  0.121467 11.000000 -1.200000
AFIX 0
C24    1  -0.058530  0.673063  0.111331 11.000000  0.031650  0.027480 = 
           0.038450 -0.001240 -0.013020  0.001610
AFIX 43
H24    2  -0.107615  0.708641  0.093575 11.000000 -1.200000
AFIX 0
C29    1   0.232385  0.762953  0.165161 11.000000  0.051820  0.028660 = 
           0.037570  0.006020 -0.012210 -0.012710
AFIX 43
H29    2   0.215910  0.746756  0.118877 11.000000 -1.200000
AFIX 0
C12    1  -0.066581  0.301067  0.075720 11.000000  0.038850  0.025620 = 
           0.029870 -0.001320 -0.015010  0.002660
C18    1  -0.290345  0.542622  0.045977 11.000000  0.034940  0.035780 = 
           0.039980  0.008500 -0.016050  0.000440
AFIX 43
H18    2  -0.297095  0.506862  0.084605 11.000000 -1.200000
AFIX 0
C30    1   0.277602  0.843085  0.175958 11.000000  0.051070  0.041760 = 
           0.048860  0.003910 -0.007630 -0.029200
AFIX 43
H30    2   0.292740  0.877739  0.138508 11.000000 -1.200000
AFIX 0
C35    1   0.307161  0.544795  0.255385 11.000000  0.040960  0.024970 = 
           0.050780  0.003470 -0.014320 -0.000650
AFIX 43
H35    2   0.345877  0.592934  0.264745 11.000000 -1.200000
AFIX 0
C37    1   0.250322  0.408565  0.247812 11.000000  0.034060  0.027500 = 
           0.030810 -0.002720 -0.014750  0.007050
C2     1   0.171164  0.175117  0.227583 11.000000  0.037580  0.030450 = 
           0.028280 -0.001740 -0.006340  0.007230
AFIX 43
H2     2   0.211675  0.139323  0.255242 11.000000 -1.200000
AFIX 0
C32    1   0.278357  0.819205  0.301383 11.000000  0.059090  0.043600 = 
           0.042380  0.000320 -0.007420 -0.026410
AFIX 43
H32    2   0.292188  0.837114  0.347585 11.000000 -1.200000
AFIX 0
C16    1  -0.117935  0.526307  0.068254 11.000000  0.033770  0.025900 = 
           0.028860  0.005120 -0.012030  0.005410
C36    1   0.330180  0.461990  0.270739 11.000000  0.040880  0.027740 = 
           0.045840  0.011040 -0.013350  0.005420
AFIX 43
H36    2   0.387089  0.442433  0.292209 11.000000 -1.200000
AFIX 0
C22    1  -0.197528  0.624755 -0.026319 11.000000  0.033970  0.030410 = 
           0.040000  0.005710 -0.018800  0.007600
AFIX 43
H22    2  -0.138954  0.644347 -0.037521 11.000000 -1.200000
AFIX 0
C27    1   0.162846  0.620811  0.202109 11.000000  0.037820  0.025040 = 
           0.034060  0.000410 -0.008130 -0.006090
C31    1   0.299112  0.868972  0.245272 11.000000  0.055190  0.033590 = 
           0.038870  0.016050 -0.009990 -0.023890
C21    1  -0.274763  0.655624 -0.066321 11.000000  0.042280  0.046040 = 
           0.038280  0.014470 -0.022700  0.006370
AFIX 43
H21    2  -0.268680  0.694256 -0.103254 11.000000 -1.200000
AFIX 0
C19    1  -0.369941  0.571101  0.005812 11.000000  0.030240  0.030250 = 
           0.033870  0.014590 -0.010640  0.009640
AFIX 43
H19    2  -0.429065  0.552267  0.016382 11.000000 -1.200000
AFIX 0
C13    1  -0.148620  0.299590  0.026038 11.000000  0.043860  0.027090 = 
           0.039130  0.002740 -0.016070  0.005560
AFIX 43
H13    2  -0.177927  0.250729  0.005293 11.000000 -1.200000
AFIX 0
C33    1   0.235177  0.740084  0.284336 11.000000  0.047040  0.029930 = 
           0.038640  0.006800 -0.007690 -0.019200
AFIX 43
H33    2   0.221138  0.705461  0.322101 11.000000 -1.200000
AFIX 0
C40    1   0.351509  0.288065  0.365298 11.000000  0.036450  0.044070 = 
           0.038640  0.001930 -0.011630  0.011130
AFIX 43
H40    2   0.314527  0.324661  0.390454 11.000000 -1.200000
AFIX 0
C11    1  -0.065508  0.121093  0.001858 11.000000  0.043410  0.024250 = 
           0.030150 -0.003340 -0.004700 -0.003070
AFIX 43
H11    2  -0.041549  0.161517 -0.028348 11.000000 -1.200000
AFIX 0
C44    1   0.383281  0.219064  0.256220 11.000000  0.042340  0.048800 = 
           0.039330 -0.004620 -0.018040  0.018920
AFIX 43
H44    2   0.368020  0.209446  0.208590 11.000000 -1.200000
AFIX 0
Fe1    5   0.047680  0.422716  0.178958 11.000000  0.045650  0.037150 = 
           0.039890 -0.001420 -0.004650  0.001820
Cl1    4  -0.040636  0.421511  0.269638 11.000000  0.062000  0.051420 = 
           0.048280 -0.002720  0.016170 -0.004250
Br6    6  -0.200734 -0.119737 -0.015157 11.000000  0.095730  0.064520 = 
           0.082260 -0.032130  0.015150 -0.033270
Br7    6   0.359586  0.978003  0.261005 11.000000  0.100480  0.049080 = 
           0.112110 -0.000390 -0.002060 -0.025510
Br5    6  -0.470276  0.660505 -0.104837 11.000000  0.065100  0.166040 = 
           0.096350  0.022110 -0.026340  0.024100
C42    1   0.484439  0.193800  0.361161 11.000000  0.031850  0.047550 = 
           0.038210  0.000390 -0.009820  0.005220
C41    1   0.431061  0.247032  0.399040 11.000000  0.046340  0.051630 = 
           0.039230 -0.000970 -0.012900  0.014340
AFIX 43
H41    2   0.447008  0.256152  0.446647 11.000000 -1.200000
AFIX 0
C43    1   0.460982  0.179617  0.291332 11.000000  0.039870  0.053090 = 
           0.044310 -0.003600 -0.014090  0.013250
AFIX 43
H43    2   0.498063  0.142547  0.266669 11.000000 -1.200000
AFIX 0
Br8    6   0.586665  0.136352  0.410402 11.000000  0.055370  0.123890 = 
           0.110190  0.053450 -0.011490  0.017210
HKLF 4 
END  

Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.500  0.500  0.500       253        63 ' '
   2  0.500  1.000  1.000       253        63 ' '

In this compound, the unit cell includes a large region of disordered solvent molecules, which could not be modeled as discrete atomic sites. We employed PLATON/SQUEEZE to calculate the diffraction contribution of the solvent molecules and, thereby, to produce a set of solvent-free diffraction intensities. The SQUEEZE calculations showed a total solvent accessible area volume of 506 A³ in this compound and the residual electron density amounted to 126 electron per unit cell, corresponding to nearly 3 molecules of DMF 
(about 0.75 DMF molecules per asymmetric unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0713P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         717
_refine_ls_number_parameters     487
_refine_ls_number_restraints     1344
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0556
_refine_ls_wR_factor_gt          0.0541
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      0.431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N4 N 0.1796(7) 0.4641(7) 0.2181(4) 0.028(2) Uani 1 1 d U . .
N3 N 0.0295(7) 0.5494(7) 0.1406(4) 0.029(2) Uani 1 1 d U . .
C23 C -0.0521(10) 0.5796(10) 0.1050(6) 0.032(2) Uani 1 1 d U . .
N2 N -0.0430(6) 0.3847(7) 0.0966(4) 0.033(2) Uani 1 1 d U . .
C3 C 0.0992(6) 0.1486(6) 0.1831(4) 0.031(2) Uani 1 1 d U . .
H3 H 0.0829 0.0907 0.1738 0.038 Uiso 1 1 calc R . .
C26 C 0.0767(11) 0.6228(10) 0.1671(6) 0.030(2) Uani 1 1 d U . .
C25 C 0.0213(7) 0.6984(6) 0.1483(4) 0.032(2) Uani 1 1 d U . .
H25 H 0.0377 0.7558 0.1598 0.039 Uiso 1 1 calc R . .
C9 C -0.1427(7) -0.0163(8) 0.0190(7) 0.037(3) Uani 1 1 d U . .
N1 N 0.0999(7) 0.2960(6) 0.1806(4) 0.030(2) Uani 1 1 d U . .
C4 C 0.0509(9) 0.2240(10) 0.1518(6) 0.029(2) Uani 1 1 d U . .
C6 C -0.0604(7) 0.1368(9) 0.0741(7) 0.031(2) Uani 1 1 d U . .
C14 C -0.1739(7) 0.3846(6) 0.0160(4) 0.038(2) Uani 1 1 d U . .
H14 H -0.2231 0.4055 -0.0142 0.046 Uiso 1 1 calc R . .
C10 C -0.1064(6) 0.0452(7) -0.0241(5) 0.038(3) Uani 1 1 d U . .
H10 H -0.1097 0.0350 -0.0722 0.046 Uiso 1 1 calc R . .
C34 C 0.2148(10) 0.5479(11) 0.2227(5) 0.033(2) Uani 1 1 d U . .
C20 C -0.3613(10) 0.6271(7) -0.0495(6) 0.038(3) Uani 1 1 d U . .
C39 C 0.3289(10) 0.2737(7) 0.2951(7) 0.038(2) Uani 1 1 d U . .
C17 C -0.1996(11) 0.5668(7) 0.0294(6) 0.032(2) Uani 1 1 d U . .
C5 C -0.0249(9) 0.2223(11) 0.1012(6) 0.030(2) Uani 1 1 d U . .
C28 C 0.2097(7) 0.7053(9) 0.2170(7) 0.036(2) Uani 1 1 d U . .
C7 C -0.0957(6) 0.0753(7) 0.1191(5) 0.031(2) Uani 1 1 d U . .
H7 H -0.0926 0.0857 0.1672 0.037 Uiso 1 1 calc R . .
C15 C -0.1104(9) 0.4358(10) 0.0609(6) 0.034(2) Uani 1 1 d U . .
C1 C 0.1742(10) 0.2690(10) 0.2247(6) 0.032(2) Uani 1 1 d U . .
C38 C 0.2486(11) 0.3161(10) 0.2558(6) 0.033(2) Uani 1 1 d U . .
C8 C -0.1358(5) -0.0019(7) 0.0916(5) 0.031(3) Uani 1 1 d U . .
H8 H -0.1579 -0.0437 0.1215 0.037 Uiso 1 1 calc R . .
C24 C -0.0585(6) 0.6731(6) 0.1113(4) 0.033(2) Uani 1 1 d U . .
H24 H -0.1076 0.7086 0.0936 0.040 Uiso 1 1 calc R . .
C29 C 0.2324(6) 0.7630(7) 0.1652(5) 0.040(2) Uani 1 1 d U . .
H29 H 0.2159 0.7468 0.1189 0.048 Uiso 1 1 calc R . .
C12 C -0.0666(9) 0.3011(11) 0.0757(6) 0.032(2) Uani 1 1 d U . .
C18 C -0.2903(8) 0.5426(5) 0.0460(5) 0.038(2) Uani 1 1 d U . .
H18 H -0.2971 0.5069 0.0846 0.046 Uiso 1 1 calc R . .
C30 C 0.2776(6) 0.8431(7) 0.1760(5) 0.048(3) Uani 1 1 d U . .
H30 H 0.2927 0.8777 0.1385 0.057 Uiso 1 1 calc R . .
C35 C 0.3072(7) 0.5448(7) 0.2554(4) 0.040(2) Uani 1 1 d U . .
H35 H 0.3459 0.5929 0.2647 0.048 Uiso 1 1 calc R . .
C37 C 0.2503(10) 0.4086(9) 0.2478(5) 0.032(2) Uani 1 1 d U . .
C2 C 0.1712(6) 0.1751(7) 0.2276(4) 0.033(2) Uani 1 1 d U . .
H2 H 0.2117 0.1393 0.2552 0.039 Uiso 1 1 calc R . .
C32 C 0.2784(6) 0.8192(7) 0.3014(5) 0.049(3) Uani 1 1 d U . .
H32 H 0.2922 0.8371 0.3476 0.059 Uiso 1 1 calc R . .
C16 C -0.1179(11) 0.5263(10) 0.0683(6) 0.030(2) Uani 1 1 d U . .
C36 C 0.3302(7) 0.4620(7) 0.2707(4) 0.039(2) Uani 1 1 d U . .
H36 H 0.3871 0.4424 0.2922 0.047 Uiso 1 1 calc R . .
C22 C -0.1975(7) 0.6248(5) -0.0263(5) 0.036(2) Uani 1 1 d U . .
H22 H -0.1390 0.6443 -0.0375 0.043 Uiso 1 1 calc R . .
C27 C 0.1628(11) 0.6208(10) 0.2021(6) 0.033(2) Uani 1 1 d U . .
C31 C 0.2991(7) 0.8690(8) 0.2453(7) 0.043(3) Uani 1 1 d U . .
C21 C -0.2748(9) 0.6556(6) -0.0663(5) 0.044(3) Uani 1 1 d U . .
H21 H -0.2687 0.6943 -0.1033 0.052 Uiso 1 1 calc R . .
C19 C -0.3699(8) 0.5711(5) 0.0058(5) 0.032(3) Uani 1 1 d U . .
H19 H -0.4291 0.5523 0.0164 0.039 Uiso 1 1 calc R . .
C13 C -0.1486(7) 0.2996(6) 0.0260(4) 0.038(2) Uani 1 1 d U . .
H13 H -0.1779 0.2507 0.0053 0.045 Uiso 1 1 calc R . .
C33 C 0.2352(6) 0.7401(7) 0.2843(5) 0.039(2) Uani 1 1 d U . .
H33 H 0.2211 0.7055 0.3221 0.047 Uiso 1 1 calc R . .
C40 C 0.3515(7) 0.2881(5) 0.3653(5) 0.041(2) Uani 1 1 d U . .
H40 H 0.3145 0.3247 0.3905 0.049 Uiso 1 1 calc R . .
C11 C -0.0655(6) 0.1211(7) 0.0019(5) 0.033(2) Uani 1 1 d U . .
H11 H -0.0415 0.1615 -0.0283 0.040 Uiso 1 1 calc R . .
C44 C 0.3833(7) 0.2191(6) 0.2562(5) 0.045(2) Uani 1 1 d U . .
H44 H 0.3680 0.2094 0.2086 0.054 Uiso 1 1 calc R . .
Fe1 Fe 0.04768(11) 0.42272(9) 0.17896(7) 0.0413(8) Uani 1 1 d . . .
Cl1 Cl -0.04064(14) 0.42151(12) 0.26964(11) 0.0533(10) Uani 1 1 d . . .
Br6 Br -0.20073(7) -0.11974(7) -0.01516(5) 0.0804(7) Uani 1 1 d . . .
Br7 Br 0.35959(7) 0.97800(7) 0.26100(5) 0.0878(7) Uani 1 1 d . . .
Br5 Br -0.47028(9) 0.66051(7) -0.10484(6) 0.1109(7) Uani 1 1 d . . .
C42 C 0.4844(8) 0.1938(7) 0.3612(7) 0.040(3) Uani 1 1 d U . .
C41 C 0.4311(8) 0.2470(6) 0.3990(5) 0.047(3) Uani 1 1 d U . .
H41 H 0.4470 0.2562 0.4466 0.056 Uiso 1 1 calc R . .
C43 C 0.4610(7) 0.1796(6) 0.2913(6) 0.047(3) Uani 1 1 d U . .
H43 H 0.4981 0.1425 0.2667 0.056 Uiso 1 1 calc R . .
Br8 Br 0.58667(8) 0.13635(7) 0.41040(6) 0.0975(7) 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
N4 C34 1.378(10) . ?
N4 C37 1.405(10) . ?
N4 Fe1 2.070(10) . ?
N3 C23 1.380(10) . ?
N3 C26 1.385(11) . ?
N3 Fe1 2.082(10) . ?
C23 C16 1.391(11) . ?
C23 C24 1.440(10) . ?
N2 C12 1.375(10) . ?
N2 C15 1.378(10) . ?
N2 Fe1 2.040(10) . ?
C3 C2 1.342(8) . ?
C3 C4 1.450(10) . ?
C26 C27 1.353(11) . ?
C26 C25 1.432(10) . ?
C25 C24 1.349(8) . ?
C9 C10 1.379(10) . ?
C9 C8 1.399(9) . ?
C9 Br6 1.880(12) . ?
N1 C1 1.364(10) . ?
N1 C4 1.394(10) . ?
N1 Fe1 2.078(9) . ?
C4 C5 1.392(10) . ?
C6 C7 1.396(10) . ?
C6 C11 1.397(10) . ?
C6 C5 1.482(11) . ?
C14 C13 1.360(7) . ?
C14 C15 1.429(10) . ?
C10 C11 1.375(8) . ?
C34 C27 1.380(11) . ?
C34 C35 1.414(10) . ?
C20 C21 1.373(10) . ?
C20 C19 1.374(9) . ?
C20 Br5 1.880(13) . ?
C39 C40 1.372(10) . ?
C39 C44 1.395(10) . ?
C39 C38 1.470(11) . ?
C17 C22 1.387(10) . ?
C17 C18 1.409(10) . ?
C17 C16 1.469(11) . ?
C5 C12 1.414(11) . ?
C28 C29 1.384(10) . ?
C28 C33 1.413(10) . ?
C28 C27 1.473(11) . ?
C7 C8 1.398(9) . ?
C15 C16 1.398(10) . ?
C1 C38 1.379(11) . ?
C1 C2 1.439(10) . ?
C38 C37 1.424(11) . ?
C29 C30 1.394(8) . ?
C12 C13 1.447(10) . ?
C18 C19 1.389(8) . ?
C30 C31 1.392(10) . ?
C35 C36 1.336(8) . ?
C37 C36 1.443(10) . ?
C32 C31 1.367(10) . ?
C32 C33 1.386(8) . ?
C22 C21 1.374(9) . ?
C31 Br7 1.892(12) . ?
C40 C41 1.408(9) . ?
C44 C43 1.388(9) . ?
Fe1 Cl1 2.224(2) . ?
C42 C41 1.363(10) . ?
C42 C43 1.366(9) . ?
C42 Br8 1.889(13) . ?

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
C34 N4 C37 106.9(13) . . ?
C34 N4 Fe1 128.7(11) . . ?
C37 N4 Fe1 124.4(10) . . ?
C23 N3 C26 106.0(14) . . ?
C23 N3 Fe1 124.1(10) . . ?
C26 N3 Fe1 125.7(10) . . ?
N3 C23 C16 124.2(17) . . ?
N3 C23 C24 110.4(14) . . ?
C16 C23 C24 125.4(16) . . ?
C12 N2 C15 103.9(13) . . ?
C12 N2 Fe1 127.9(11) . . ?
C15 N2 Fe1 126.5(10) . . ?
C2 C3 C4 109.6(11) . . ?
C27 C26 N3 124.0(17) . . ?
C27 C26 C25 127.2(18) . . ?
N3 C26 C25 108.7(14) . . ?
C24 C25 C26 109.0(12) . . ?
C10 C9 C8 119.0(14) . . ?
C10 C9 Br6 123.0(11) . . ?
C8 C9 Br6 118.0(11) . . ?
C1 N1 C4 110.2(13) . . ?
C1 N1 Fe1 123.5(11) . . ?
C4 N1 Fe1 124.3(10) . . ?
C5 C4 N1 128.8(18) . . ?
C5 C4 C3 126.1(18) . . ?
N1 C4 C3 105.0(13) . . ?
C7 C6 C11 119.9(15) . . ?
C7 C6 C5 120.7(13) . . ?
C11 C6 C5 119.1(14) . . ?
C13 C14 C15 107.0(11) . . ?
C11 C10 C9 122.1(12) . . ?
N4 C34 C27 123.3(17) . . ?
N4 C34 C35 108.7(14) . . ?
C27 C34 C35 127.9(18) . . ?
C21 C20 C19 121.1(14) . . ?
C21 C20 Br5 120.2(12) . . ?
C19 C20 Br5 118.7(11) . . ?
C40 C39 C44 121.3(15) . . ?
C40 C39 C38 122.7(14) . . ?
C44 C39 C38 116.0(14) . . ?
C22 C17 C18 114.7(14) . . ?
C22 C17 C16 126.3(14) . . ?
C18 C17 C16 118.8(14) . . ?
C4 C5 C12 120.4(18) . . ?
C4 C5 C6 119.0(17) . . ?
C12 C5 C6 120.7(16) . . ?
C29 C28 C33 110.6(13) . . ?
C29 C28 C27 123.4(14) . . ?
C33 C28 C27 125.9(14) . . ?
C6 C7 C8 119.8(12) . . ?
N2 C15 C16 124.7(17) . . ?
N2 C15 C14 111.7(13) . . ?
C16 C15 C14 123.6(17) . . ?
N1 C1 C38 130.0(18) . . ?
N1 C1 C2 107.5(14) . . ?
C38 C1 C2 122.0(17) . . ?
C1 C38 C37 119.5(18) . . ?
C1 C38 C39 122.1(16) . . ?
C37 C38 C39 118.3(16) . . ?
C7 C8 C9 120.0(12) . . ?
C25 C24 C23 105.8(11) . . ?
C28 C29 C30 126.0(12) . . ?
N2 C12 C5 127.4(17) . . ?
N2 C12 C13 111.8(14) . . ?
C5 C12 C13 120.6(16) . . ?
C19 C18 C17 121.3(12) . . ?
C31 C30 C29 117.1(13) . . ?
C36 C35 C34 109.5(12) . . ?
N4 C37 C38 128.9(17) . . ?
N4 C37 C36 107.7(12) . . ?
C38 C37 C36 123.4(17) . . ?
C3 C2 C1 107.6(11) . . ?
C31 C32 C33 115.0(12) . . ?
C23 C16 C15 125.3(18) . . ?
C23 C16 C17 119.0(15) . . ?
C15 C16 C17 115.6(17) . . ?
C35 C36 C37 107.3(11) . . ?
C21 C22 C17 125.5(13) . . ?
C26 C27 C34 127.3(19) . . ?
C26 C27 C28 117.2(17) . . ?
C34 C27 C28 115.4(17) . . ?
C32 C31 C30 122.8(14) . . ?
C32 C31 Br7 119.5(11) . . ?
C30 C31 Br7 117.7(11) . . ?
C20 C21 C22 117.3(12) . . ?
C20 C19 C18 120.0(12) . . ?
C14 C13 C12 105.6(12) . . ?
C32 C33 C28 128.4(12) . . ?
C39 C40 C41 119.6(12) . . ?
C10 C11 C6 119.2(13) . . ?
C43 C44 C39 117.5(12) . . ?
N2 Fe1 N4 150.3(2) . . ?
N2 Fe1 N1 87.2(4) . . ?
N4 Fe1 N1 88.0(4) . . ?
N2 Fe1 N3 86.6(4) . . ?
N4 Fe1 N3 85.8(4) . . ?
N1 Fe1 N3 155.4(2) . . ?
N2 Fe1 Cl1 103.49(19) . . ?
N4 Fe1 Cl1 106.15(17) . . ?
N1 Fe1 Cl1 101.91(17) . . ?
N3 Fe1 Cl1 102.67(18) . . ?
C41 C42 C43 120.6(14) . . ?
C41 C42 Br8 117.2(11) . . ?
C43 C42 Br8 122.1(11) . . ?
C42 C41 C40 119.3(12) . . ?
C42 C43 C44 121.7(12) . . ?

# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 253 63 ' '
2 0.500 1.000 1.000 253 63 ' '
_platon_squeeze_details          
;
In this compound, the unit cell includes a large region of disordered 
solvent molecules, which could not be modeled as discrete atomic 
sites. We employed PLATON/SQUEEZE to calculate the diffraction 
contribution of the solvent molecules and, thereby, to produce 
a set of solvent-free diffraction intensities. The SQUEEZE calculations 
showed a total solvent accessible area volume of 506 A³ in 
this compound and the residual electron density amounted to 
126 electron per unit cell, corresponding to nearly 3 molecules of DMF 
(about 0.75 DMF molecules per asymmetric unit).
;

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.044
