# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_pi28-rt
_database_code_depnum_ccdc_archive 'CCDC 1920840'
loop_
_audit_author_name
_audit_author_address
'Shane Telfer'
;Massey University
New Zealand
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_pi28-rt             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal diffracts weakly and although every effort was made to get better data this was the best result achieved
;
_vrf_PLAT234_pi28-rt             
;
PROBLEM: Large Hirshfeld Difference C1       --C2       .       0.32 Ang.
RESPONSE: This relates to the weak diffraction noted above
;
_vrf_PLAT090_pi28-rt             
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.96 Note
RESPONSE: Due to weak diffraction by the sample
;
_vrf_PLAT201_pi28-rt             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: As above
;
_vrf_PLAT213_pi28-rt             
;
PROBLEM: Atom C28             has ADP max/min Ratio .....        4.1 prolat
RESPONSE: As above
;
_vrf_PLAT234_pi28-rt_2           
;
PROBLEM: Large Hirshfeld Difference O1       --C16      .       0.26 Ang.
RESPONSE: As above
;
_vrf_PLAT341_pi28-rt             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02244 Ang.
RESPONSE: Due to weak diffraction by the sample
;
_vrf_PLAT431_pi28-rt             
;
PROBLEM: Short Inter HL..A Contact  Br2      ..O4       .       2.93 Ang.
RESPONSE: This is a strong halogen bond
;
_vrf_PLAT987_pi28-rt             
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: A twin refinement was attempted but did not give a better model
;
# Added during the CSD deposition process: Wednesday 05 June 2019 01:51 AM
# end Validation Reply Form

_audit_creation_date             2018-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H20 Br2 Fe N4 O2, C7 H7 O3 S, H2 O'
_chemical_formula_sum            'C39 H29 Br2 Fe N4 O6 S'
_chemical_formula_weight         897.39
_chemical_absolute_configuration ?
_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 0.0181 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'
Br Br -0.6763 1.2805 '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'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 '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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   12.4432(3)
_cell_length_b                   14.6561(4)
_cell_length_c                   19.1005(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3483.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8805
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.6
_shelx_estimated_absorpt_T_max   0.479
_shelx_estimated_absorpt_T_min   0.207
_exptl_absorpt_coefficient_mu    7.190
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19306
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        50.422
_diffrn_reflns_theta_max         50.422
_diffrn_reflns_theta_min         6.577
_diffrn_ambient_temperature      293
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 34
	           Slice: 22.0000 - 192.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 26
	           Slice: 42.0000 - 172.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 27
	           Slice: 20.0000 - 155.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 270.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 34
	           Slice: 23.0000 - 193.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.017985
_diffrn_orient_matrix_UB_12      -0.039011
_diffrn_orient_matrix_UB_13      -0.041325
_diffrn_orient_matrix_UB_21      -0.006619
_diffrn_orient_matrix_UB_22      -0.055817
_diffrn_orient_matrix_UB_23      0.029801
_diffrn_orient_matrix_UB_31      -0.078047
_diffrn_orient_matrix_UB_32      -0.004256
_diffrn_orient_matrix_UB_33      -0.012050
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Cu
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                2414
_reflns_number_total             3616
_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       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Flack x determined using 756 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.499(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0773
_refine_ls_restrained_S_all      1.096
_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)+(0.1147P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2198
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H6A-O5
 1.966 with sigma of 0.02
 H6B-O3_$1
 2.046 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C1(H1), C2(H2), C3(H3), C28(H28), C30(H30), C31(H31),
 C12(H12), C15(H15), C14(H14), C26(H26), C10(H10), C24(H24), C23(H23), C22(H22),
  C17(H17), C18(H18), C19(H19), C38(H38), C37(H37), C35(H35), C34(H34)
4.c Fitted hexagon refined as free rotating group:
 C32(C27,C28,C29,C30,C31), C13(C12,C11,C16,C15,C14), C38(C37,C36,C35,C34,C33)
4.d Naphthalene refined as free rotating group:
 C9(C8,C7,C6,C4,C5,N1,C1,C2,C3), C25(C24,C23,C22,C20,C21,N3,C17,C18,C19)
4.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.7420(2) 0.68708(15) 0.94802(14) 0.0783(10) Uani 1 1 d . . . . .
Br2 Br 0.2628(2) 0.68205(15) 0.41221(13) 0.0784(10) Uani 1 1 d . . . . .
Fe1 Fe 0.5043(3) 0.38575(17) 0.6809(3) 0.0661(10) Uani 1 1 d . . . . .
S1 S 0.6608(7) 0.1060(6) 0.3188(5) 0.111(3) Uani 1 1 d . . . . .
O1 O 0.4675(12) 0.4721(12) 0.7484(9) 0.081(5) Uani 1 1 d . . . . .
N2 N 0.6554(13) 0.3862(12) 0.7075(10) 0.060(5) Uani 1 1 d . . . . .
C9 C 0.7180(10) 0.3218(8) 0.6659(6) 0.068(8) Uani 1 1 d . . . . .
C8 C 0.8281(10) 0.3064(9) 0.6699(8) 0.065(7) Uani 1 1 d G . . . .
H8 H 0.8693 0.3382 0.7024 0.078 Uiso 1 1 calc R . . . .
C7 C 0.8765(8) 0.2435(10) 0.6255(9) 0.101(10) Uani 1 1 d G . . . .
H7 H 0.9501 0.2332 0.6283 0.122 Uiso 1 1 calc R . . . .
C6 C 0.8148(8) 0.1959(9) 0.5771(8) 0.083(8) Uani 1 1 d G . . . .
H6 H 0.8472 0.1538 0.5473 0.100 Uiso 1 1 calc R . . . .
C4 C 0.7048(8) 0.2113(6) 0.5730(5) 0.063(6) Uani 1 1 d G . . . .
C5 C 0.6564(8) 0.2742(6) 0.6174(5) 0.079(8) Uani 1 1 d G . . . .
N1 N 0.5463(8) 0.2895(8) 0.6133(6) 0.057(5) Uani 1 1 d G U . . .
C1 C 0.4846(8) 0.2420(9) 0.5648(7) 0.084(9) Uani 1 1 d G . . . .
H1 H 0.4110 0.2522 0.5621 0.101 Uiso 1 1 calc R . . . .
C2 C 0.5330(11) 0.1790(9) 0.5204(7) 0.087(9) Uani 1 1 d G . . . .
H2 H 0.4918 0.1472 0.4880 0.104 Uiso 1 1 calc R . . . .
C3 C 0.6431(11) 0.1637(8) 0.5245(6) 0.097(9) Uani 1 1 d G . . . .
H3 H 0.6755 0.1216 0.4948 0.116 Uiso 1 1 calc R . . . .
N4 N 0.3538(14) 0.3825(12) 0.6578(11) 0.067(5) Uani 1 1 d . . . . .
O2 O 0.5392(11) 0.4719(10) 0.6128(9) 0.070(4) Uani 1 1 d . . . . .
C32 C 0.4721(13) 0.5143(11) 0.5687(8) 0.075(8) Uani 1 1 d . . . . .
C27 C 0.3612(14) 0.5036(10) 0.5693(8) 0.069(8) Uani 1 1 d G . . . .
C28 C 0.2979(9) 0.5515(11) 0.5219(9) 0.068(8) Uani 1 1 d G . . . .
H28 H 0.2236 0.5443 0.5223 0.081 Uiso 1 1 calc R . . . .
C29 C 0.3456(12) 0.6101(9) 0.4739(8) 0.053(6) Uiso 1 1 d G . . . .
C30 C 0.4566(13) 0.6208(9) 0.4732(8) 0.091(8) Uiso 1 1 d G . . . .
H30 H 0.4885 0.6601 0.4411 0.110 Uiso 1 1 calc R . . . .
C31 C 0.5199(9) 0.5730(11) 0.5207(9) 0.074(8) Uani 1 1 d G . . . .
H31 H 0.5941 0.5802 0.5202 0.089 Uiso 1 1 calc R . . . .
C13 C 0.6589(12) 0.6173(10) 0.8840(8) 0.080(7) Uani 1 1 d . . . . .
C12 C 0.7070(9) 0.5559(11) 0.8383(9) 0.064(7) Uani 1 1 d G . . . .
H12 H 0.7813 0.5490 0.8381 0.077 Uiso 1 1 calc R . . . .
C11 C 0.6441(13) 0.5047(10) 0.7927(8) 0.061(7) Uani 1 1 d G U . . .
C16 C 0.5330(13) 0.5149(11) 0.7930(9) 0.071(7) Uani 1 1 d G . . . .
C15 C 0.4849(9) 0.5763(12) 0.8387(10) 0.088(9) Uani 1 1 d G . . . .
H15 H 0.4106 0.5832 0.8388 0.106 Uiso 1 1 calc R . . . .
C14 C 0.5478(13) 0.6276(10) 0.8842(8) 0.066(6) Uiso 1 1 d G . . . .
H14 H 0.5156 0.6687 0.9148 0.079 Uiso 1 1 calc R . . . .
C26 C 0.3060(17) 0.4384(16) 0.6158(14) 0.067(7) Uani 1 1 d . . . . .
H26 H 0.2313 0.4374 0.6149 0.080 Uiso 1 1 calc R . . . .
C10 C 0.6992(18) 0.4423(15) 0.7496(15) 0.068(7) Uani 1 1 d . . . . .
H10 H 0.7738 0.4421 0.7521 0.082 Uiso 1 1 calc R . . . .
C25 C 0.2880(10) 0.3191(8) 0.6962(6) 0.068(7) Uani 1 1 d . . . . .
C24 C 0.1782(9) 0.3015(10) 0.6942(8) 0.092(10) Uani 1 1 d G . . . .
H24 H 0.1344 0.3334 0.6633 0.110 Uiso 1 1 calc R . . . .
C23 C 0.1340(7) 0.2361(11) 0.7383(9) 0.082(9) Uani 1 1 d G . . . .
H23 H 0.0606 0.2243 0.7370 0.099 Uiso 1 1 calc R . . . .
C22 C 0.1995(8) 0.1883(9) 0.7845(8) 0.077(8) Uani 1 1 d G . . . .
H22 H 0.1699 0.1446 0.8141 0.092 Uiso 1 1 calc R . . . .
C20 C 0.3092(8) 0.2059(7) 0.7865(6) 0.082(8) Uani 1 1 d G . . . .
C21 C 0.3535(7) 0.2713(7) 0.7424(5) 0.060(6) Uani 1 1 d G . . . .
N3 N 0.4632(8) 0.2889(8) 0.7444(6) 0.080(6) Uani 1 1 d G . . . .
C17 C 0.5287(7) 0.2411(9) 0.7906(7) 0.075(7) Uani 1 1 d G . . . .
H17 H 0.6021 0.2529 0.7919 0.090 Uiso 1 1 calc R . . . .
C18 C 0.4845(10) 0.1758(9) 0.8347(7) 0.074(7) Uani 1 1 d G U . . .
H18 H 0.5283 0.1438 0.8656 0.089 Uiso 1 1 calc R . . . .
C19 C 0.3747(11) 0.1582(8) 0.8327(7) 0.081(8) Uani 1 1 d G . . . .
H19 H 0.3451 0.1145 0.8623 0.098 Uiso 1 1 calc R . . . .
O6 O 0.9091(15) -0.008(2) 0.4317(17) 0.171(8) Uani 1 1 d . . . . .
H6A H 0.8479 0.0167 0.4253 0.256 Uiso 1 1 d DG . . . .
H6B H 0.9398 -0.0156 0.3924 0.256 Uiso 1 1 d DG . . . .
O5 O 0.7274(18) 0.0661(14) 0.3708(11) 0.155(8) Uani 1 1 d D . . . .
C38 C 0.6224(16) 0.0074(15) 0.1993(14) 0.118(11) Uani 1 1 d . . . . .
H38 H 0.5506 0.0113 0.2127 0.141 Uiso 1 1 calc R . . . .
C37 C 0.650(2) -0.0381(14) 0.1381(13) 0.148(14) Uani 1 1 d G . . . .
H37 H 0.5972 -0.0648 0.1105 0.177 Uiso 1 1 calc R . . . .
C36 C 0.757(3) -0.0439(13) 0.1180(13) 0.118(13) Uani 1 1 d G . . . .
C35 C 0.8367(17) -0.0040(16) 0.1592(18) 0.123(12) Uani 1 1 d G . . . .
H35 H 0.9084 -0.0079 0.1457 0.148 Uiso 1 1 calc R . . . .
C34 C 0.809(2) 0.0415(14) 0.2203(15) 0.116(11) Uani 1 1 d G . . . .
H34 H 0.8619 0.0682 0.2479 0.139 Uiso 1 1 calc R . . . .
C33 C 0.702(3) 0.0473(13) 0.2404(10) 0.093(9) Uani 1 1 d G . . . .
O3 O 0.550(2) 0.0825(14) 0.3309(14) 0.175(9) Uani 1 1 d D . . . .
C39 C 0.799(3) -0.0936(16) 0.0528(18) 0.174(18) Uani 1 1 d . . . . .
H39A H 0.7779 -0.1565 0.0548 0.261 Uiso 1 1 calc GR . . . .
H39B H 0.8759 -0.0895 0.0512 0.261 Uiso 1 1 calc GR . . . .
H39C H 0.7691 -0.0658 0.0117 0.261 Uiso 1 1 calc GR . . . .
O4 O 0.669(3) 0.2003(13) 0.3042(12) 0.192(12) 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 C13 1.901(12) . ?
Br2 C29 1.887(13) . ?
Fe1 O1 1.864(18) . ?
Fe1 N2 1.948(17) . ?
Fe1 N1 1.981(12) . ?
Fe1 N4 1.924(17) . ?
Fe1 O2 1.863(15) . ?
Fe1 N3 1.936(12) . ?
S1 O5 1.419(19) . ?
S1 C33 1.80(2) . ?
S1 O3 1.44(2) . ?
S1 O4 1.414(18) . ?
O1 C16 1.33(2) . ?
N2 C9 1.46(2) . ?
N2 C10 1.27(3) . ?
C9 C8 1.3900 . ?
C9 C5 1.3900 . ?
C8 H8 0.9300 . ?
C8 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C5 N1 1.3900 . ?
N1 C1 1.3900 . ?
C1 H1 0.9300 . ?
C1 C2 1.3900 . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
N4 C26 1.29(3) . ?
N4 C25 1.44(2) . ?
O2 C32 1.339(19) . ?
C32 C27 1.3900 . ?
C32 C31 1.3900 . ?
C27 C28 1.3900 . ?
C27 C26 1.47(3) . ?
C28 H28 0.9300 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C30 H30 0.9300 . ?
C30 C31 1.3900 . ?
C31 H31 0.9300 . ?
C13 C12 1.3900 . ?
C13 C14 1.3900 . ?
C12 H12 0.9300 . ?
C12 C11 1.3900 . ?
C11 C16 1.3900 . ?
C11 C10 1.41(3) . ?
C16 C15 1.3900 . ?
C15 H15 0.9300 . ?
C15 C14 1.3900 . ?
C14 H14 0.9300 . ?
C26 H26 0.9300 . ?
C10 H10 0.9300 . ?
C25 C24 1.3900 . ?
C25 C21 1.3900 . ?
C24 H24 0.9300 . ?
C24 C23 1.3900 . ?
C23 H23 0.9300 . ?
C23 C22 1.3900 . ?
C22 H22 0.9300 . ?
C22 C20 1.3900 . ?
C20 C21 1.3900 . ?
C20 C19 1.3900 . ?
C21 N3 1.3900 . ?
N3 C17 1.3900 . ?
C17 H17 0.9300 . ?
C17 C18 1.3900 . ?
C18 H18 0.9300 . ?
C18 C19 1.3900 . ?
C19 H19 0.9300 . ?
O6 H6A 0.8496 . ?
O6 H6B 0.8504 . ?
C38 H38 0.9300 . ?
C38 C37 1.3900 . ?
C38 C33 1.3900 . ?
C37 H37 0.9300 . ?
C37 C36 1.3900 . ?
C36 C35 1.3900 . ?
C36 C39 1.53(4) . ?
C35 H35 0.9300 . ?
C35 C34 1.3900 . ?
C34 H34 0.9300 . ?
C34 C33 1.3900 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N2 93.1(8) . . ?
O1 Fe1 N1 176.8(7) . . ?
O1 Fe1 N4 86.3(7) . . ?
O1 Fe1 N3 89.9(7) . . ?
N2 Fe1 N1 85.3(7) . . ?
N4 Fe1 N2 177.7(10) . . ?
N4 Fe1 N1 95.2(6) . . ?
N4 Fe1 N3 82.4(7) . . ?
O2 Fe1 O1 94.6(5) . . ?
O2 Fe1 N2 87.4(7) . . ?
O2 Fe1 N1 88.1(7) . . ?
O2 Fe1 N4 94.8(8) . . ?
O2 Fe1 N3 174.5(7) . . ?
N3 Fe1 N2 95.4(6) . . ?
N3 Fe1 N1 87.5(4) . . ?
O5 S1 C33 102.7(11) . . ?
O5 S1 O3 110.5(16) . . ?
O3 S1 C33 106.8(13) . . ?
O4 S1 O5 119.9(15) . . ?
O4 S1 C33 106.4(13) . . ?
O4 S1 O3 109.5(17) . . ?
C16 O1 Fe1 127.6(13) . . ?
C9 N2 Fe1 111.7(13) . . ?
C10 N2 Fe1 125.5(16) . . ?
C10 N2 C9 122.3(18) . . ?
C8 C9 N2 126.8(10) . . ?
C8 C9 C5 120.0 . . ?
C5 C9 N2 113.2(10) . . ?
C9 C8 H8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C4 C6 C7 120.0 . . ?
C4 C6 H6 120.0 . . ?
C6 C4 C5 120.0 . . ?
C6 C4 C3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C5 C9 120.0 . . ?
N1 C5 C9 120.0 . . ?
N1 C5 C4 120.0 . . ?
C5 N1 Fe1 109.8(5) . . ?
C5 N1 C1 120.0 . . ?
C1 N1 Fe1 130.2(5) . . ?
N1 C1 H1 120.0 . . ?
C2 C1 N1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C26 N4 Fe1 125.0(16) . . ?
C26 N4 C25 117.6(17) . . ?
C25 N4 Fe1 117.0(12) . . ?
C32 O2 Fe1 127.5(12) . . ?
O2 C32 C27 124.1(14) . . ?
O2 C32 C31 115.9(14) . . ?
C27 C32 C31 120.0 . . ?
C32 C27 C26 122.7(15) . . ?
C28 C27 C32 120.0 . . ?
C28 C27 C26 117.2(16) . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 Br2 121.6(10) . . ?
C28 C29 C30 120.0 . . ?
C30 C29 Br2 118.3(10) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 C29 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 C32 120.0 . . ?
C30 C31 H31 120.0 . . ?
C12 C13 Br1 121.2(10) . . ?
C12 C13 C14 120.0 . . ?
C14 C13 Br1 118.8(10) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C10 116.2(15) . . ?
C16 C11 C10 123.7(15) . . ?
O1 C16 C11 123.7(14) . . ?
O1 C16 C15 116.2(14) . . ?
C15 C16 C11 120.0 . . ?
C16 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C14 C15 H15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
N4 C26 C27 125(2) . . ?
N4 C26 H26 117.6 . . ?
C27 C26 H26 117.6 . . ?
N2 C10 C11 126(2) . . ?
N2 C10 H10 117.2 . . ?
C11 C10 H10 117.2 . . ?
C24 C25 N4 131.7(9) . . ?
C24 C25 C21 120.0 . . ?
C21 C25 N4 108.3(9) . . ?
C25 C24 H24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C22 H22 120.0 . . ?
C23 C22 C20 120.0 . . ?
C20 C22 H22 120.0 . . ?
C22 C20 C19 120.0 . . ?
C21 C20 C22 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C25 120.0 . . ?
N3 C21 C25 120.0 . . ?
N3 C21 C20 120.0 . . ?
C21 N3 Fe1 112.2(5) . . ?
C21 N3 C17 120.0 . . ?
C17 N3 Fe1 127.7(5) . . ?
N3 C17 H17 120.0 . . ?
C18 C17 N3 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
H6A O6 H6B 109.4 . . ?
C37 C38 H38 120.0 . . ?
C37 C38 C33 120.0 . . ?
C33 C38 H38 120.0 . . ?
C38 C37 H37 120.0 . . ?
C38 C37 C36 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C36 C39 125(3) . . ?
C35 C36 C37 120.0 . . ?
C35 C36 C39 115(3) . . ?
C36 C35 H35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C38 C33 S1 118(2) . . ?
C34 C33 S1 122(2) . . ?
C34 C33 C38 120.0 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

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 C13 C12 C11 179.0(11) . . . . ?
Br1 C13 C14 C15 -179.0(11) . . . . ?
Br2 C29 C30 C31 176.3(9) . . . . ?
Fe1 O1 C16 C11 4(2) . . . . ?
Fe1 O1 C16 C15 -179.7(10) . . . . ?
Fe1 N2 C9 C8 178.3(5) . . . . ?
Fe1 N2 C9 C5 -0.6(13) . . . . ?
Fe1 N2 C10 C11 11(3) . . . . ?
Fe1 N1 C1 C2 177.5(8) . . . . ?
Fe1 N4 C26 C27 11(3) . . . . ?
Fe1 N4 C25 C24 177.9(6) . . . . ?
Fe1 N4 C25 C21 -1.3(14) . . . . ?
Fe1 O2 C32 C27 3(2) . . . . ?
Fe1 O2 C32 C31 -177.3(10) . . . . ?
Fe1 N3 C17 C18 177.3(8) . . . . ?
O1 Fe1 O2 C32 -84.0(17) . . . . ?
O1 C16 C15 C14 -176.5(16) . . . . ?
N2 Fe1 O1 C16 2.4(17) . . . . ?
N2 Fe1 O2 C32 -176.9(17) . . . . ?
N2 C9 C8 C7 -178.8(13) . . . . ?
N2 C9 C5 C4 179.0(11) . . . . ?
N2 C9 C5 N1 -1.0(11) . . . . ?
C9 N2 C10 C11 -178.2(17) . . . . ?
C9 C8 C7 C6 0.0 . . . . ?
C9 C5 N1 Fe1 2.1(7) . . . . ?
C9 C5 N1 C1 180.0 . . . . ?
C8 C9 C5 C4 0.0 . . . . ?
C8 C9 C5 N1 180.0 . . . . ?
C8 C7 C6 C4 0.0 . . . . ?
C7 C6 C4 C5 0.0 . . . . ?
C7 C6 C4 C3 180.0 . . . . ?
C6 C4 C5 C9 0.0 . . . . ?
C6 C4 C5 N1 180.0 . . . . ?
C6 C4 C3 C2 180.0 . . . . ?
C4 C5 N1 Fe1 -177.9(7) . . . . ?
C4 C5 N1 C1 0.0 . . . . ?
C5 C9 C8 C7 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 N1 C1 C2 0.0 . . . . ?
N1 Fe1 O2 C32 97.7(16) . . . . ?
N1 C1 C2 C3 0.0 . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C3 C4 C5 C9 180.0 . . . . ?
C3 C4 C5 N1 0.0 . . . . ?
N4 Fe1 O1 C16 -179.9(17) . . . . ?
N4 Fe1 O2 C32 2.7(16) . . . . ?
N4 C25 C24 C23 -179.1(14) . . . . ?
N4 C25 C21 C20 179.3(11) . . . . ?
N4 C25 C21 N3 -0.7(11) . . . . ?
O2 Fe1 O1 C16 -85.3(17) . . . . ?
O2 C32 C27 C28 179.2(16) . . . . ?
O2 C32 C27 C26 -4.6(19) . . . . ?
O2 C32 C31 C30 -179.3(15) . . . . ?
C32 C27 C28 C29 0.0 . . . . ?
C32 C27 C26 N4 -3(3) . . . . ?
C27 C32 C31 C30 0.0 . . . . ?
C27 C28 C29 Br2 -176.2(10) . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C27 C26 N4 173.0(17) . . . . ?
C28 C29 C30 C31 0.0 . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C31 C32 C27 C28 0.0 . . . . ?
C31 C32 C27 C26 176.1(15) . . . . ?
C13 C12 C11 C16 0.0 . . . . ?
C13 C12 C11 C10 -178.3(16) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C11 C16 O1 176.2(17) . . . . ?
C12 C11 C16 C15 0.0 . . . . ?
C12 C11 C10 N2 176.0(19) . . . . ?
C11 C16 C15 C14 0.0 . . . . ?
C16 C11 C10 N2 -2(3) . . . . ?
C16 C15 C14 C13 0.0 . . . . ?
C14 C13 C12 C11 0.0 . . . . ?
C26 N4 C25 C24 4(2) . . . . ?
C26 N4 C25 C21 -174.8(15) . . . . ?
C26 C27 C28 C29 -176.3(14) . . . . ?
C10 N2 C9 C8 6(2) . . . . ?
C10 N2 C9 C5 -172.8(17) . . . . ?
C10 C11 C16 O1 -6(2) . . . . ?
C10 C11 C16 C15 178.2(18) . . . . ?
C25 N4 C26 C27 -175.9(16) . . . . ?
C25 C24 C23 C22 0.0 . . . . ?
C25 C21 N3 Fe1 2.3(7) . . . . ?
C25 C21 N3 C17 180.0 . . . . ?
C24 C25 C21 C20 0.0 . . . . ?
C24 C25 C21 N3 180.0 . . . . ?
C24 C23 C22 C20 0.0 . . . . ?
C23 C22 C20 C21 0.0 . . . . ?
C23 C22 C20 C19 180.0 . . . . ?
C22 C20 C21 C25 0.0 . . . . ?
C22 C20 C21 N3 180.0 . . . . ?
C22 C20 C19 C18 180.0 . . . . ?
C20 C21 N3 Fe1 -177.7(7) . . . . ?
C20 C21 N3 C17 0.0 . . . . ?
C21 C25 C24 C23 0.0 . . . . ?
C21 C20 C19 C18 0.0 . . . . ?
C21 N3 C17 C18 0.0 . . . . ?
N3 Fe1 O1 C16 97.8(16) . . . . ?
N3 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C19 C20 C21 C25 180.0 . . . . ?
C19 C20 C21 N3 0.0 . . . . ?
O5 S1 C33 C38 128.3(14) . . . . ?
O5 S1 C33 C34 -52.1(15) . . . . ?
C38 C37 C36 C35 0.0 . . . . ?
C38 C37 C36 C39 179(2) . . . . ?
C37 C38 C33 S1 179.6(12) . . . . ?
C37 C38 C33 C34 0.0 . . . . ?
C37 C36 C35 C34 0.0 . . . . ?
C36 C35 C34 C33 0.0 . . . . ?
C35 C34 C33 S1 -179.6(13) . . . . ?
C35 C34 C33 C38 0.0 . . . . ?
C33 C38 C37 C36 0.0 . . . . ?
O3 S1 C33 C38 12.0(16) . . . . ?
O3 S1 C33 C34 -168.3(13) . . . . ?
C39 C36 C35 C34 -178.8(18) . . . . ?
O4 S1 C33 C38 -104.9(16) . . . . ?
O4 S1 C33 C34 74.7(16) . . . . ?

_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/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_pi28-lt
_database_code_depnum_ccdc_archive 'CCDC 1920841'
loop_
_audit_author_name
_audit_author_address
'Shane Telfer'
;Massey University
New Zealand
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_pi28-lt             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal diffracts weakly and although every effort was made to get better data this was the best result achieved
;
_vrf_PLAT090_pi28-lt             
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.98 Note
RESPONSE: This relates to the weak diffraction noted above
;
_vrf_PLAT431_pi28-lt             
;
PROBLEM: Short Inter HL..A Contact  Br2      ..O3       .       2.84 Ang.
RESPONSE: This is a strong halogen bond
;
_vrf_REFNR01_pi28-lt             
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: Due to weak diffraction by the sample
;
_vrf_PLAT341_pi28-lt             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03615 Ang.
RESPONSE: As above
;
_vrf_PLAT987_pi28-lt             
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: A twin refinement was attempted but did not give a better model
;
# Added during the CSD deposition process: Wednesday 05 June 2019 01:51 AM
# end Validation Reply Form

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H20 Br2 Fe N4 O2, C7 H7 O3 S, H2 O'
_chemical_formula_sum            'C39 H29 Br2 Fe N4 O6 S'
_chemical_formula_weight         897.39
_chemical_absolute_configuration ad
_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 0.0181 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'
Br Br -0.6763 1.2805 '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'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 '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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   12.3433(8)
_cell_length_b                   14.3546(8)
_cell_length_c                   19.2425(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3409.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2928
_cell_measurement_temperature    123
_cell_measurement_theta_max      70.5
_cell_measurement_theta_min      6.6
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.346
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1804
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1447
_diffrn_reflns_av_unetI/netI     0.1465
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18081
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        50.421
_diffrn_reflns_theta_max         50.421
_diffrn_reflns_theta_min         6.598
_diffrn_ambient_temperature      123
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
scan:
	Number of images: 24
	           Slice: 20.0000 - 140.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 30
	           Slice: 20.0000 - 170.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 31
	           Slice: 21.0000 - 176.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 270.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 32
	           Slice: 22.0000 - 182.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
;
_diffrn_measurement_device       
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       ω-scans
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.016906
_diffrn_orient_matrix_UB_12      -0.010153
_diffrn_orient_matrix_UB_13      0.050257
_diffrn_orient_matrix_UB_21      -0.008367
_diffrn_orient_matrix_UB_22      0.068730
_diffrn_orient_matrix_UB_23      0.006569
_diffrn_orient_matrix_UB_31      -0.078789
_diffrn_orient_matrix_UB_32      -0.005120
_diffrn_orient_matrix_UB_33      -0.011481
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2318
_reflns_number_total             3505
_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       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         3505
_refine_ls_number_restraints     235
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0859
_refine_ls_restrained_S_all      1.074
_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)+(0.1137P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2225
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C26)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) = Uanis(N1)
3.a Free rotating group:
 O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C31(H31), C6(H6), C7(H7), C19(H19), C12(H12), C8(H8), C30(H30),
 C2(H2), C14(H14), C24(H24), C28(H28), C17(H17), C1(H1), C18(H18), C34(H34),
 C35(H35), C37(H37), C38(H38), C22(H22), C23(H23), C3(H3), C15(H15), C26(H26)
3.c Fitted hexagon refined as free rotating group:
 C33(C34,C35,C36,C37,C38)
3.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_atom_sites_solution_hydrogens   mixed
_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
Br2 Br 0.2650(2) 0.68371(17) 0.40997(15) 0.0610(10) Uani 1 1 d . . . . .
Br1 Br 0.7414(2) 0.69227(16) 0.94738(17) 0.0627(10) Uani 1 1 d . . . . .
Fe1 Fe 0.5066(3) 0.3850(2) 0.6799(3) 0.0565(11) Uani 1 1 d . . . . .
S1 S 0.1558(7) 0.8929(6) 0.3165(5) 0.078(2) Uani 1 1 d . . . . .
N2 N 0.6565(15) 0.3871(13) 0.7037(12) 0.053(6) Uani 1 1 d . . . . .
O2 O 0.5466(14) 0.4753(12) 0.6120(9) 0.056(4) Uani 1 1 d . . . . .
C4 C 0.708(2) 0.2105(19) 0.5711(14) 0.054(7) Uani 1 1 d . U . . .
C13 C 0.662(2) 0.6193(16) 0.8836(14) 0.056(7) Uani 1 1 d . U . . .
N3 N 0.4647(18) 0.2858(14) 0.7442(11) 0.057(3) Uani 1 1 d . . . . .
C10 C 0.703(2) 0.4411(16) 0.7463(13) 0.044(7) Uani 1 1 d . U . . .
H10 H 0.7797 0.4391 0.7493 0.053 Uiso 1 1 calc R . . . .
O1 O 0.4702(15) 0.4721(13) 0.7468(9) 0.059(5) Uani 1 1 d . . . . .
C31 C 0.521(2) 0.5748(19) 0.5186(13) 0.057(7) Uani 1 1 d . U . . .
H31 H 0.5973 0.5843 0.5196 0.068 Uiso 1 1 calc R . . . .
C11 C 0.646(2) 0.5052(15) 0.7902(12) 0.052(7) Uani 1 1 d . U . . .
C6 C 0.818(2) 0.1961(18) 0.5740(15) 0.061(8) Uani 1 1 d . U . . .
H6 H 0.8515 0.1547 0.5420 0.073 Uiso 1 1 calc R . . . .
C7 C 0.880(2) 0.2421(17) 0.6237(14) 0.063(8) Uani 1 1 d . U . . .
H7 H 0.9559 0.2303 0.6271 0.075 Uiso 1 1 calc R . . . .
C19 C 0.377(2) 0.1502(17) 0.8349(14) 0.065(8) Uani 1 1 d . U . . .
H19 H 0.3488 0.1043 0.8656 0.078 Uiso 1 1 calc R . . . .
C25 C 0.293(2) 0.3183(16) 0.6965(18) 0.057(8) Uani 1 1 d . U . . .
O6 O -0.0898(15) 0.9938(18) 0.4321(12) 0.100(6) Uani 1 1 d . . . . .
H6A H -0.0371 0.9968 0.4022 0.149 Uiso 1 1 d G . . . .
H6B H -0.1507 1.0064 0.4115 0.149 Uiso 1 1 d G . . . .
C12 C 0.704(2) 0.557(2) 0.8409(16) 0.067(8) Uani 1 1 d . U . . .
H12 H 0.7802 0.5464 0.8442 0.081 Uiso 1 1 calc R . . . .
C32 C 0.479(2) 0.513(2) 0.5665(16) 0.062(9) Uani 1 1 d . U . . .
C8 C 0.832(2) 0.3042(16) 0.6674(16) 0.061(8) Uani 1 1 d . U . . .
H8 H 0.8746 0.3360 0.7009 0.073 Uiso 1 1 calc R . . . .
C30 C 0.4667(19) 0.6207(16) 0.4724(13) 0.046(7) Uani 1 1 d . U . . .
H30 H 0.5018 0.6590 0.4391 0.055 Uiso 1 1 calc R . . . .
C5 C 0.659(2) 0.2735(17) 0.6144(16) 0.055(7) Uani 1 1 d . U . . .
C2 C 0.534(2) 0.1818(17) 0.5207(14) 0.065(8) Uani 1 1 d . U . . .
H2 H 0.4879 0.1519 0.4880 0.078 Uiso 1 1 calc R . . . .
N1 N 0.5526(18) 0.2903(13) 0.6149(12) 0.057(3) Uani 1 1 d . . . . .
C14 C 0.551(2) 0.6330(16) 0.8835(13) 0.056(7) Uani 1 1 d . U . . .
H14 H 0.5182 0.6769 0.9139 0.067 Uiso 1 1 calc R . . . .
N4 N 0.3547(17) 0.3820(15) 0.6569(12) 0.060(6) Uani 1 1 d . . . . .
O4 O 0.0427(16) 0.9144(14) 0.3288(10) 0.098(6) Uani 1 1 d . . . . .
C21 C 0.354(2) 0.2658(17) 0.7433(14) 0.050(7) Uani 1 1 d . U . . .
C24 C 0.182(2) 0.3039(15) 0.6910(17) 0.061(8) Uani 1 1 d . U . . .
H24 H 0.1390 0.3381 0.6591 0.073 Uiso 1 1 calc R . . . .
C16 C 0.529(3) 0.519(2) 0.7894(15) 0.056(7) Uani 1 1 d . U . . .
C28 C 0.3038(19) 0.5541(17) 0.5216(14) 0.048(7) Uani 1 1 d . U . . .
H28 H 0.2273 0.5476 0.5225 0.058 Uiso 1 1 calc R . . . .
C17 C 0.525(2) 0.2380(18) 0.7892(12) 0.056(8) Uani 1 1 d . U . . .
H17 H 0.6002 0.2500 0.7902 0.067 Uiso 1 1 calc R . . . .
C1 C 0.4915(19) 0.247(2) 0.5700(13) 0.062(9) Uani 1 1 d . U . . .
H1 H 0.4159 0.2598 0.5699 0.075 Uiso 1 1 calc R . . . .
C9 C 0.722(2) 0.3219(17) 0.6641(18) 0.055(8) Uani 1 1 d . U . . .
O3 O 0.174(2) 0.7955(13) 0.3029(10) 0.111(8) Uani 1 1 d . . . . .
C20 C 0.310(3) 0.1978(16) 0.7885(16) 0.061(8) Uani 1 1 d . U . . .
C18 C 0.484(2) 0.1725(19) 0.8344(14) 0.066(9) Uani 1 1 d . U . . .
H18 H 0.5320 0.1423 0.8659 0.079 Uiso 1 1 calc R . . . .
C33 C 0.1922(17) 0.9511(11) 0.2394(8) 0.067(7) Uani 1 1 d . U . . .
C34 C 0.1124(12) 0.9929(12) 0.1992(11) 0.090(9) Uani 1 1 d G U . . .
H34 H 0.0387 0.9899 0.2133 0.108 Uiso 1 1 calc R . . . .
C35 C 0.1403(16) 1.0393(12) 0.1383(11) 0.096(10) Uani 1 1 d G U . . .
H35 H 0.0857 1.0679 0.1109 0.115 Uiso 1 1 calc R . . . .
C36 C 0.2481(19) 1.0437(12) 0.1177(9) 0.072(8) Uani 1 1 d G U . . .
C37 C 0.3280(13) 1.0019(13) 0.1579(11) 0.084(9) Uani 1 1 d G U . . .
H37 H 0.4016 1.0049 0.1438 0.101 Uiso 1 1 calc R . . . .
C38 C 0.3000(15) 0.9555(12) 0.2188(9) 0.073(8) Uani 1 1 d G U . . .
H38 H 0.3546 0.9269 0.2463 0.087 Uiso 1 1 calc R . . . .
C22 C 0.192(2) 0.1848(16) 0.7835(15) 0.058(8) Uani 1 1 d . U . . .
H22 H 0.1566 0.1419 0.8135 0.070 Uiso 1 1 calc R . . . .
C23 C 0.135(2) 0.2330(18) 0.7371(15) 0.071(8) Uani 1 1 d . U . . .
H23 H 0.0590 0.2210 0.7336 0.085 Uiso 1 1 calc R . . . .
C39 C 0.287(3) 1.0968(18) 0.0497(16) 0.099(10) Uani 1 1 d . U . . .
H39A H 0.2520 1.0691 0.0089 0.148 Uiso 1 1 calc GR . . . .
H39B H 0.3657 1.0915 0.0453 0.148 Uiso 1 1 calc GR . . . .
H39C H 0.2666 1.1627 0.0530 0.148 Uiso 1 1 calc GR . . . .
C27 C 0.362(2) 0.5063(16) 0.5682(12) 0.053(7) Uani 1 1 d . U . . .
C3 C 0.641(2) 0.1637(17) 0.5219(13) 0.060(8) Uani 1 1 d . U . . .
H3 H 0.6717 0.1202 0.4903 0.072 Uiso 1 1 calc R . . . .
C15 C 0.487(2) 0.579(2) 0.8359(14) 0.068(8) Uani 1 1 d . U . . .
H15 H 0.4100 0.5854 0.8375 0.082 Uiso 1 1 calc R . . . .
C29 C 0.347(2) 0.6109(16) 0.4738(13) 0.056(7) Uani 1 1 d . U . . .
C26 C 0.307(2) 0.4414(18) 0.6128(16) 0.061(8) Uani 1 1 d . U . . .
H26 H 0.2303 0.4405 0.6108 0.073 Uiso 1 1 calc R . . . .
O5 O 0.2247(14) 0.9324(13) 0.3715(10) 0.083(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
Br2 C29 1.91(2) . ?
Br1 C13 1.89(3) . ?
Fe1 N2 1.91(2) . ?
Fe1 O2 1.905(18) . ?
Fe1 N3 1.96(2) . ?
Fe1 O1 1.849(19) . ?
Fe1 N1 1.93(2) . ?
Fe1 N4 1.93(2) . ?
S1 O4 1.450(19) . ?
S1 O3 1.439(18) . ?
S1 C33 1.761(16) . ?
S1 O5 1.471(18) . ?
N2 C10 1.26(3) . ?
N2 C9 1.45(3) . ?
O2 C32 1.33(3) . ?
C4 C6 1.37(3) . ?
C4 C5 1.37(3) . ?
C4 C3 1.43(3) . ?
C13 C12 1.32(3) . ?
C13 C14 1.38(3) . ?
N3 C21 1.40(3) . ?
N3 C17 1.33(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.44(3) . ?
O1 C16 1.28(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.38(4) . ?
C31 C30 1.29(3) . ?
C11 C12 1.43(4) . ?
C11 C16 1.46(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.40(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.36(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.39(3) . ?
C19 C18 1.36(3) . ?
C25 N4 1.41(3) . ?
C25 C21 1.39(4) . ?
C25 C24 1.39(3) . ?
O6 H6A 0.8696 . ?
O6 H6B 0.8695 . ?
C12 H12 0.9500 . ?
C32 C27 1.44(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.39(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.48(3) . ?
C5 N1 1.34(3) . ?
C5 C9 1.41(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.44(3) . ?
C2 C3 1.35(3) . ?
N1 C1 1.30(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.44(4) . ?
N4 C26 1.34(3) . ?
C21 C20 1.41(3) . ?
C24 H24 0.9500 . ?
C24 C23 1.47(3) . ?
C16 C15 1.34(4) . ?
C28 H28 0.9500 . ?
C28 C27 1.34(3) . ?
C28 C29 1.34(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.37(3) . ?
C1 H1 0.9500 . ?
C20 C22 1.47(3) . ?
C18 H18 0.9500 . ?
C33 C34 1.3900 . ?
C33 C38 1.3900 . ?
C34 H34 0.9500 . ?
C34 C35 1.3900 . ?
C35 H35 0.9500 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C36 C39 1.59(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.3900 . ?
C38 H38 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.33(3) . ?
C23 H23 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C27 C26 1.44(3) . ?
C3 H3 0.9500 . ?
C15 H15 0.9500 . ?
C26 H26 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N3 96.6(9) . . ?
N2 Fe1 N1 83.2(9) . . ?
N2 Fe1 N4 179.2(11) . . ?
O2 Fe1 N2 84.4(8) . . ?
O2 Fe1 N3 175.9(8) . . ?
O2 Fe1 N1 87.6(9) . . ?
O2 Fe1 N4 96.3(9) . . ?
O1 Fe1 N2 93.3(9) . . ?
O1 Fe1 O2 94.6(6) . . ?
O1 Fe1 N3 89.3(9) . . ?
O1 Fe1 N1 175.6(9) . . ?
O1 Fe1 N4 86.5(8) . . ?
N1 Fe1 N3 88.5(7) . . ?
N4 Fe1 N3 82.6(10) . . ?
N4 Fe1 N1 97.0(9) . . ?
O4 S1 C33 106.4(11) . . ?
O4 S1 O5 110.9(12) . . ?
O3 S1 O4 112.7(15) . . ?
O3 S1 C33 105.6(11) . . ?
O3 S1 O5 114.6(12) . . ?
O5 S1 C33 106.0(10) . . ?
C10 N2 Fe1 127.2(17) . . ?
C10 N2 C9 119(2) . . ?
C9 N2 Fe1 113.6(17) . . ?
C32 O2 Fe1 124.5(18) . . ?
C6 C4 C5 121(3) . . ?
C6 C4 C3 122(2) . . ?
C5 C4 C3 117(3) . . ?
C12 C13 Br1 125(2) . . ?
C12 C13 C14 119(2) . . ?
C14 C13 Br1 116(2) . . ?
C21 N3 Fe1 113.6(17) . . ?
C17 N3 Fe1 130(2) . . ?
C17 N3 C21 116(3) . . ?
N2 C10 H10 118.2 . . ?
N2 C10 C11 124(2) . . ?
C11 C10 H10 118.2 . . ?
C16 O1 Fe1 132(2) . . ?
C32 C31 H31 117.1 . . ?
C30 C31 H31 117.1 . . ?
C30 C31 C32 126(3) . . ?
C10 C11 C16 125(2) . . ?
C12 C11 C10 119(3) . . ?
C12 C11 C16 116(3) . . ?
C4 C6 H6 120.0 . . ?
C4 C6 C7 120(3) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119(3) . . ?
C8 C7 H7 120.3 . . ?
C20 C19 H19 121.5 . . ?
C18 C19 H19 121.5 . . ?
C18 C19 C20 117(3) . . ?
C21 C25 N4 114(3) . . ?
C21 C25 C24 120(3) . . ?
C24 C25 N4 126(3) . . ?
H6A O6 H6B 109.5 . . ?
C13 C12 C11 125(3) . . ?
C13 C12 H12 117.5 . . ?
C11 C12 H12 117.5 . . ?
O2 C32 C31 118(3) . . ?
O2 C32 C27 126(3) . . ?
C31 C32 C27 116(3) . . ?
C7 C8 H8 119.2 . . ?
C7 C8 C9 122(3) . . ?
C9 C8 H8 119.2 . . ?
C31 C30 H30 121.4 . . ?
C31 C30 C29 117(2) . . ?
C29 C30 H30 121.4 . . ?
C4 C5 C9 119(3) . . ?
N1 C5 C4 124(3) . . ?
N1 C5 C9 116(3) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C3 C2 C1 118(3) . . ?
C5 N1 Fe1 115.0(18) . . ?
C1 N1 Fe1 126.3(19) . . ?
C1 N1 C5 119(2) . . ?
C13 C14 H14 121.0 . . ?
C13 C14 C15 118(2) . . ?
C15 C14 H14 121.0 . . ?
C25 N4 Fe1 114.5(19) . . ?
C26 N4 Fe1 123.9(19) . . ?
C26 N4 C25 121(2) . . ?
N3 C21 C20 120(2) . . ?
C25 C21 N3 115(2) . . ?
C25 C21 C20 125(3) . . ?
C25 C24 H24 121.6 . . ?
C25 C24 C23 117(3) . . ?
C23 C24 H24 121.6 . . ?
O1 C16 C11 119(3) . . ?
O1 C16 C15 123(3) . . ?
C15 C16 C11 117(3) . . ?
C27 C28 H28 118.1 . . ?
C27 C28 C29 124(2) . . ?
C29 C28 H28 118.1 . . ?
N3 C17 H17 117.8 . . ?
N3 C17 C18 124(3) . . ?
C18 C17 H17 117.8 . . ?
C2 C1 H1 118.8 . . ?
N1 C1 C2 122(3) . . ?
N1 C1 H1 118.8 . . ?
C8 C9 N2 130(3) . . ?
C8 C9 C5 119(3) . . ?
C5 C9 N2 112(2) . . ?
C19 C20 C21 121(3) . . ?
C19 C20 C22 124(2) . . ?
C21 C20 C22 115(2) . . ?
C19 C18 C17 121(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C34 C33 S1 119.6(13) . . ?
C34 C33 C38 120.0 . . ?
C38 C33 S1 120.4(13) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C37 120.0 . . ?
C35 C36 C39 123.1(18) . . ?
C37 C36 C39 116.9(18) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 C36 120.0 . . ?
C38 C37 H37 120.0 . . ?
C33 C38 H38 120.0 . . ?
C37 C38 C33 120.0 . . ?
C37 C38 H38 120.0 . . ?
C20 C22 H22 119.9 . . ?
C23 C22 C20 120(2) . . ?
C23 C22 H22 119.9 . . ?
C24 C23 H23 118.3 . . ?
C22 C23 C24 123(3) . . ?
C22 C23 H23 118.3 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C28 C27 C32 119(3) . . ?
C28 C27 C26 119(3) . . ?
C26 C27 C32 122(2) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 C4 120(3) . . ?
C2 C3 H3 120.2 . . ?
C14 C15 H15 118.1 . . ?
C16 C15 C14 124(3) . . ?
C16 C15 H15 118.1 . . ?
C30 C29 Br2 117.9(18) . . ?
C28 C29 Br2 124(2) . . ?
C28 C29 C30 118(2) . . ?
N4 C26 C27 126(2) . . ?
N4 C26 H26 117.0 . . ?
C27 C26 H26 117.0 . . ?

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 C13 C12 C11 -176.7(19) . . . . ?
Br1 C13 C14 C15 -179.8(19) . . . . ?
Fe1 N2 C10 C11 7(3) . . . . ?
Fe1 N2 C9 C8 -180(2) . . . . ?
Fe1 N2 C9 C5 2(3) . . . . ?
Fe1 O2 C32 C31 -177.2(17) . . . . ?
Fe1 O2 C32 C27 12(4) . . . . ?
Fe1 N3 C21 C25 1(3) . . . . ?
Fe1 N3 C21 C20 -178.0(18) . . . . ?
Fe1 N3 C17 C18 176.6(19) . . . . ?
Fe1 O1 C16 C11 -1(4) . . . . ?
Fe1 O1 C16 C15 -178.6(18) . . . . ?
Fe1 N1 C1 C2 176.1(17) . . . . ?
Fe1 N4 C26 C27 10(4) . . . . ?
S1 C33 C34 C35 179.8(12) . . . . ?
S1 C33 C38 C37 -179.8(12) . . . . ?
N2 Fe1 O1 C16 4(2) . . . . ?
N2 C10 C11 C12 174(2) . . . . ?
N2 C10 C11 C16 -3(4) . . . . ?
O2 Fe1 O1 C16 -81(2) . . . . ?
O2 C32 C27 C28 175(2) . . . . ?
O2 C32 C27 C26 -12(4) . . . . ?
C4 C6 C7 C8 -3(4) . . . . ?
C4 C5 N1 Fe1 -179(2) . . . . ?
C4 C5 N1 C1 -3(4) . . . . ?
C4 C5 C9 N2 178(2) . . . . ?
C4 C5 C9 C8 0(4) . . . . ?
C13 C14 C15 C16 -3(4) . . . . ?
N3 Fe1 O1 C16 100(2) . . . . ?
N3 C21 C20 C19 1(4) . . . . ?
N3 C21 C20 C22 179(2) . . . . ?
N3 C17 C18 C19 1(4) . . . . ?
C10 N2 C9 C8 4(4) . . . . ?
C10 N2 C9 C5 -174(2) . . . . ?
C10 C11 C12 C13 179(2) . . . . ?
C10 C11 C16 O1 0(4) . . . . ?
C10 C11 C16 C15 177(2) . . . . ?
O1 C16 C15 C14 -179(2) . . . . ?
C31 C32 C27 C28 4(3) . . . . ?
C31 C32 C27 C26 177(2) . . . . ?
C31 C30 C29 Br2 176.2(19) . . . . ?
C31 C30 C29 C28 -1(3) . . . . ?
C11 C16 C15 C14 4(4) . . . . ?
C6 C4 C5 N1 -179(2) . . . . ?
C6 C4 C5 C9 -2(4) . . . . ?
C6 C4 C3 C2 -179(2) . . . . ?
C6 C7 C8 C9 1(4) . . . . ?
C7 C8 C9 N2 -177(3) . . . . ?
C7 C8 C9 C5 0(4) . . . . ?
C19 C20 C22 C23 -180(3) . . . . ?
C25 N4 C26 C27 -177(2) . . . . ?
C25 C21 C20 C19 -178(2) . . . . ?
C25 C21 C20 C22 0(4) . . . . ?
C25 C24 C23 C22 1(4) . . . . ?
C12 C13 C14 C15 0(4) . . . . ?
C12 C11 C16 O1 -178(2) . . . . ?
C12 C11 C16 C15 0(3) . . . . ?
C32 C31 C30 C29 4(4) . . . . ?
C32 C27 C26 N4 0(4) . . . . ?
C30 C31 C32 O2 -177(2) . . . . ?
C30 C31 C32 C27 -5(4) . . . . ?
C5 C4 C6 C7 3(4) . . . . ?
C5 C4 C3 C2 -1(4) . . . . ?
C5 N1 C1 C2 1(4) . . . . ?
N1 C5 C9 N2 -4(3) . . . . ?
N1 C5 C9 C8 178(2) . . . . ?
C14 C13 C12 C11 4(4) . . . . ?
N4 Fe1 O1 C16 -177(2) . . . . ?
N4 C25 C21 N3 1(3) . . . . ?
N4 C25 C21 C20 -180(2) . . . . ?
N4 C25 C24 C23 179(2) . . . . ?
O4 S1 C33 C34 -9.3(14) . . . . ?
O4 S1 C33 C38 170.6(11) . . . . ?
C21 N3 C17 C18 -1(3) . . . . ?
C21 C25 N4 Fe1 -3(3) . . . . ?
C21 C25 N4 C26 -176(2) . . . . ?
C21 C25 C24 C23 1(3) . . . . ?
C21 C20 C22 C23 2(3) . . . . ?
C24 C25 N4 Fe1 178.8(19) . . . . ?
C24 C25 N4 C26 6(4) . . . . ?
C24 C25 C21 N3 180(2) . . . . ?
C24 C25 C21 C20 -1(4) . . . . ?
C16 C11 C12 C13 -4(4) . . . . ?
C28 C27 C26 N4 173(2) . . . . ?
C17 N3 C21 C25 179(2) . . . . ?
C17 N3 C21 C20 0(3) . . . . ?
C1 C2 C3 C4 -1(4) . . . . ?
C9 N2 C10 C11 -177(2) . . . . ?
C9 C5 N1 Fe1 4(3) . . . . ?
C9 C5 N1 C1 180(2) . . . . ?
O3 S1 C33 C34 110.7(14) . . . . ?
O3 S1 C33 C38 -69.5(15) . . . . ?
C20 C19 C18 C17 -1(4) . . . . ?
C20 C22 C23 C24 -3(4) . . . . ?
C18 C19 C20 C21 0(4) . . . . ?
C18 C19 C20 C22 -178(2) . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C33 C38 C37 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C34 C35 C36 C39 -178.9(19) . . . . ?
C35 C36 C37 C38 0.0 . . . . ?
C36 C37 C38 C33 0.0 . . . . ?
C38 C33 C34 C35 0.0 . . . . ?
C39 C36 C37 C38 178.9(18) . . . . ?
C27 C28 C29 Br2 -177.0(17) . . . . ?
C27 C28 C29 C30 0(4) . . . . ?
C3 C4 C6 C7 -179(2) . . . . ?
C3 C4 C5 N1 3(4) . . . . ?
C3 C4 C5 C9 -180(2) . . . . ?
C3 C2 C1 N1 1(4) . . . . ?
C29 C28 C27 C32 -2(4) . . . . ?
C29 C28 C27 C26 -174(2) . . . . ?
O5 S1 C33 C34 -127.4(11) . . . . ?
O5 S1 C33 C38 52.4(13) . . . . ?

_shelx_SHELXL_version_number     2014/7
_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/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_pi24-lt
_database_code_depnum_ccdc_archive 'CCDC 1920842'
loop_
_audit_author_name
_audit_author_address
'Shane Telfer'
;Massey University
New Zealand
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_pi24-lt             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The crystal diffracts weakly and although every effort was made to get better data this was the best result achieved
;
_vrf_PLAT090_pi24-lt             
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.57 Note
RESPONSE: Due to weak diffraction
;
_vrf_PLAT987_pi24-lt             
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The space group is chiral but it is evident that the sample contains a mixture of both enantiomers.
;
# Added during the CSD deposition process: Wednesday 05 June 2019 01:51 AM
# end Validation Reply Form

_audit_creation_date             2018-05-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H20 Fe I2 N4 O2, C7 H7 O3 S, 2(H2 O)'
_chemical_formula_sum            'C39 H31 Fe I2 N4 O7 S'
_chemical_formula_weight         1010.39
_chemical_absolute_configuration ?
_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 0.0181 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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   12.7045(3)
_cell_length_b                   14.1173(3)
_cell_length_c                   20.3416(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3648.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5211
_cell_measurement_temperature    103
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      7.0
_shelx_estimated_absorpt_T_max   0.300
_shelx_estimated_absorpt_T_min   0.144
_exptl_absorpt_coefficient_mu    17.621
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.1070
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17087
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        58.925
_diffrn_reflns_theta_max         58.925
_diffrn_reflns_theta_min         6.970
_diffrn_ambient_temperature      103
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 36
	           Slice: 20.0000 - 200.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 27
	           Slice: 53.0000 - 188.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 24
	           Slice: 76.0000 - 196.0000
	     Image width: 5.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
;
_diffrn_measurement_device       
;
Crystal Goniometer
;
_diffrn_measurement_device_type  
;
Rigaku Spider
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.047543
_diffrn_orient_matrix_UB_12      -0.029083
_diffrn_orient_matrix_UB_13      -0.033580
_diffrn_orient_matrix_UB_21      0.001623
_diffrn_orient_matrix_UB_22      -0.060121
_diffrn_orient_matrix_UB_23      0.025976
_diffrn_orient_matrix_UB_31      -0.062711
_diffrn_orient_matrix_UB_32      -0.023605
_diffrn_orient_matrix_UB_33      -0.024786
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                3957
_reflns_number_total             5002
_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       
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_refine_diff_density_max         1.695
_refine_diff_density_min         -2.059
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 
;
 Flack x determined using 1254 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.071(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      1.050
_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)+(0.0709P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1516
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C29 \\sim C28 \\sim C27 \\sim C32 \\sim C31 \\sim C30: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12 \\sim C11: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C29) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed X: H7A(0.60614) H7B(0.4938)
 Fixed Y: H7A(0.03725) H7B(0.05494)
 Fixed Z: H7A(0.047569) H7B(0.046599)
4.a Free rotating group:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C12(H12), C30(H30), C18(H18), C19(H19), C15(H15), C8(H8), C6(H6),
 C10(H10), C24(H24), C17(H17), C14(H14), C3(H3), C22(H22), C31(H31), C7(H7),
 C26(H26), C2(H2), C23(H23), C1(H1), C37(H37), C34(H34), C38(H38), C35(H35)
4.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_atom_sites_solution_hydrogens   mixed
_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
I2 I 0.72940(9) 0.69072(9) 0.60164(5) 0.0349(4) Uani 1 1 d . . . . .
I1 I 0.26766(9) 0.70906(9) 0.06378(5) 0.0364(4) Uani 1 1 d . . . . .
Fe1 Fe 0.4858(2) 0.39217(17) 0.33265(15) 0.0315(7) Uani 1 1 d . . . . .
S4 S 0.6065(4) -0.1126(4) 0.1813(3) 0.0428(13) Uani 1 1 d . . . . .
O1 O 0.5286(8) 0.4788(8) 0.2686(6) 0.029(3) Uani 1 1 d . . . . .
O2 O 0.4482(10) 0.4865(8) 0.3954(5) 0.032(3) Uani 1 1 d . . . . .
O4 O 0.6673(9) -0.0639(8) 0.1289(6) 0.042(3) Uani 1 1 d . . . . .
O3 O 0.6354(11) -0.2092(8) 0.1895(7) 0.056(4) Uani 1 1 d . . . . .
N4 N 0.6328(10) 0.3887(10) 0.3571(7) 0.028(3) Uani 1 1 d . . . . .
N3 N 0.5262(11) 0.2895(9) 0.2738(7) 0.028(4) Uani 1 1 d . . . . .
N2 N 0.3392(10) 0.3929(10) 0.3058(7) 0.028(3) Uani 1 1 d . . . . .
N1 N 0.4368(12) 0.2959(9) 0.3941(7) 0.028(4) Uani 1 1 d . . . . .
O5 O 0.4917(9) -0.0986(10) 0.1717(7) 0.059(4) Uani 1 1 d . . . . .
C28 C 0.6810(13) 0.5558(12) 0.4906(9) 0.028(4) Uani 1 1 d . U . . .
H28 H 0.7550 0.5464 0.4926 0.033 Uiso 1 1 calc R . . . .
C12 C 0.3006(13) 0.5679(13) 0.1733(9) 0.034(5) Uani 1 1 d . U . . .
H12 H 0.2260 0.5643 0.1719 0.041 Uiso 1 1 calc R . . . .
C29 C 0.6344(14) 0.6144(13) 0.5349(10) 0.038(5) Uani 1 1 d . U . . .
C30 C 0.5245(14) 0.6296(14) 0.5330(9) 0.037(5) Uani 1 1 d . U . . .
H30 H 0.4909 0.6708 0.5634 0.045 Uiso 1 1 calc R . . . .
C9 C 0.2774(12) 0.3274(13) 0.3423(9) 0.022(4) Uani 1 1 d . . . . .
C11 C 0.3561(14) 0.5129(12) 0.2201(8) 0.029(4) Uani 1 1 d . U . . .
C18 C 0.5075(14) 0.1759(13) 0.1874(9) 0.038(5) Uani 1 1 d . . . . .
H18 H 0.4631 0.1431 0.1575 0.046 Uiso 1 1 calc R . . . .
C16 C 0.4666(14) 0.5223(13) 0.2246(9) 0.032(4) Uani 1 1 d . U . . .
C5 C 0.3298(14) 0.2773(12) 0.3908(9) 0.025(4) Uani 1 1 d . . . . .
C19 C 0.6120(14) 0.1578(12) 0.1890(8) 0.031(4) Uani 1 1 d . . . . .
H19 H 0.6406 0.1121 0.1597 0.037 Uiso 1 1 calc R . . . .
C25 C 0.6916(15) 0.3245(13) 0.3200(12) 0.041(5) Uani 1 1 d . . . . .
C15 C 0.5162(13) 0.5838(12) 0.1798(8) 0.030(4) Uani 1 1 d . U . . .
H15 H 0.5906 0.5905 0.1810 0.036 Uiso 1 1 calc R . . . .
C13 C 0.3523(13) 0.6265(13) 0.1299(8) 0.031(4) Uani 1 1 d . U . . .
C8 C 0.1693(15) 0.3125(11) 0.3362(9) 0.026(5) Uani 1 1 d . . . . .
H8 H 0.1309 0.3464 0.3039 0.031 Uiso 1 1 calc R . . . .
C6 C 0.1717(16) 0.1972(14) 0.4257(10) 0.041(6) Uani 1 1 d . . . . .
H6 H 0.1356 0.1538 0.4534 0.049 Uiso 1 1 calc R . . . .
C32 C 0.5115(15) 0.5246(14) 0.4392(10) 0.034(5) Uani 1 1 d . U . . .
C10 C 0.2993(14) 0.4497(14) 0.2637(9) 0.032(5) Uani 1 1 d . . . . .
H10 H 0.2247 0.4505 0.2607 0.038 Uiso 1 1 calc R . . . .
C24 C 0.7993(16) 0.3078(12) 0.3206(11) 0.033(5) Uani 1 1 d . . . . .
H24 H 0.8418 0.3429 0.3503 0.040 Uiso 1 1 calc R . . . .
C17 C 0.4659(15) 0.2430(13) 0.2302(9) 0.038(5) Uani 1 1 d . . . . .
H17 H 0.3927 0.2564 0.2285 0.046 Uiso 1 1 calc R . . . .
C20 C 0.6802(14) 0.2055(13) 0.2333(10) 0.031(5) Uani 1 1 d . . . . .
C14 C 0.4591(14) 0.6344(13) 0.1343(9) 0.038(5) Uani 1 1 d . U . . .
H14 H 0.4950 0.6759 0.1051 0.046 Uiso 1 1 calc R . . . .
C4 C 0.2797(16) 0.2111(13) 0.4325(9) 0.032(5) Uani 1 1 d . . . . .
C3 C 0.3436(13) 0.1651(12) 0.4790(9) 0.033(4) Uani 1 1 d . . . . .
H3 H 0.3133 0.1199 0.5079 0.039 Uiso 1 1 calc R . . . .
C27 C 0.6225(14) 0.5086(11) 0.4421(8) 0.026(4) Uani 1 1 d . U . . .
C22 C 0.7919(16) 0.1921(13) 0.2367(11) 0.041(6) Uani 1 1 d . . . . .
H22 H 0.8260 0.1480 0.2086 0.050 Uiso 1 1 calc R . . . .
C31 C 0.4697(15) 0.5838(13) 0.4869(10) 0.041(5) Uani 1 1 d . U . . .
H31 H 0.3956 0.5926 0.4867 0.049 Uiso 1 1 calc R . . . .
C7 C 0.1165(17) 0.2483(14) 0.3770(9) 0.047(5) Uani 1 1 d . . . . .
H7 H 0.0429 0.2392 0.3719 0.056 Uiso 1 1 calc R . . . .
C26 C 0.6775(14) 0.4443(12) 0.4012(8) 0.029(4) Uani 1 1 d . . . . .
H26 H 0.7518 0.4408 0.4059 0.035 Uiso 1 1 calc R . . . .
C2 C 0.4496(14) 0.1848(12) 0.4829(9) 0.034(5) Uiso 1 1 d . . . . .
H2 H 0.4925 0.1538 0.5146 0.040 Uiso 1 1 calc R . . . .
C21 C 0.6331(15) 0.2702(14) 0.2729(10) 0.037(5) Uani 1 1 d . . . . .
C23 C 0.8472(13) 0.2429(13) 0.2802(8) 0.029(4) Uani 1 1 d . . . . .
H23 H 0.9212 0.2338 0.2831 0.035 Uiso 1 1 calc R . . . .
C1 C 0.4928(15) 0.2503(16) 0.4401(10) 0.046(6) Uani 1 1 d . . . . .
H1 H 0.5659 0.2636 0.4435 0.055 Uiso 1 1 calc R . . . .
C37 C 0.7701(17) -0.0065(14) 0.3331(11) 0.046(6) Uani 1 1 d . . . . .
H37 H 0.8421 -0.0044 0.3455 0.055 Uiso 1 1 calc R . . . .
C36 C 0.6969(18) 0.0344(13) 0.3746(9) 0.040(5) Uani 1 1 d . . . . .
C34 C 0.5616(16) -0.0172(14) 0.2948(9) 0.047(5) Uani 1 1 d . . . . .
H34 H 0.4895 -0.0206 0.2827 0.056 Uiso 1 1 calc R . . . .
C38 C 0.7440(17) -0.0504(16) 0.2743(11) 0.050(6) Uani 1 1 d . . . . .
H38 H 0.7977 -0.0766 0.2473 0.060 Uiso 1 1 calc R . . . .
C39 C 0.7296(16) 0.0850(16) 0.4360(11) 0.054(6) Uani 1 1 d . . . . .
H39A H 0.7253 0.1536 0.4289 0.081 Uiso 1 1 calc GR . . . .
H39B H 0.8021 0.0676 0.4471 0.081 Uiso 1 1 calc GR . . . .
H39C H 0.6827 0.0670 0.4721 0.081 Uiso 1 1 calc GR . . . .
C35 C 0.5922(17) 0.0273(14) 0.3539(8) 0.047(6) Uani 1 1 d . . . . .
H35 H 0.5390 0.0539 0.3811 0.057 Uiso 1 1 calc R . . . .
C33 C 0.6385(14) -0.0560(13) 0.2546(9) 0.038(5) Uani 1 1 d . . . . .
O6 O 0.3694(11) 0.0140(12) 0.0882(8) 0.072(4) Uani 1 1 d . . . . .
H6A H 0.3041 0.0213 0.0999 0.109 Uiso 1 1 d G . . . .
H6B H 0.3989 -0.0287 0.1129 0.109 Uiso 1 1 d G . . . .
O7 O 0.5557(13) 0.0676(15) 0.0279(9) 0.108(6) Uani 1 1 d . . . . .
H7A H 0.6061 0.0372 0.0476 0.162 Uiso 1 1 d R . . . .
H7B H 0.4938 0.0549 0.0466 0.162 Uiso 1 1 d 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
I2 C29 2.112(19) . ?
I1 C13 2.080(17) . ?
Fe1 O1 1.867(11) . ?
Fe1 O2 1.906(11) . ?
Fe1 N4 1.933(14) . ?
Fe1 N3 1.949(14) . ?
Fe1 N2 1.941(14) . ?
Fe1 N1 1.949(14) . ?
S4 O4 1.485(11) . ?
S4 O3 1.423(12) . ?
S4 O5 1.484(12) . ?
S4 C33 1.740(17) . ?
O1 C16 1.34(2) . ?
O2 C32 1.31(2) . ?
N4 C25 1.40(2) . ?
N4 C26 1.321(19) . ?
N3 C17 1.34(2) . ?
N3 C21 1.39(2) . ?
N2 C9 1.42(2) . ?
N2 C10 1.28(2) . ?
N1 C5 1.39(2) . ?
N1 C1 1.34(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.36(2) . ?
C28 C27 1.40(2) . ?
C12 H12 0.9500 . ?
C12 C11 1.42(2) . ?
C12 C13 1.38(2) . ?
C29 C30 1.41(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.33(2) . ?
C9 C5 1.39(2) . ?
C9 C8 1.39(3) . ?
C11 C16 1.41(2) . ?
C11 C10 1.45(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.35(2) . ?
C18 C17 1.39(2) . ?
C16 C15 1.41(2) . ?
C5 C4 1.41(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.42(2) . ?
C25 C24 1.39(2) . ?
C25 C21 1.43(3) . ?
C15 H15 0.9500 . ?
C15 C14 1.38(2) . ?
C13 C14 1.36(2) . ?
C8 H8 0.9500 . ?
C8 C7 1.40(2) . ?
C6 H6 0.9500 . ?
C6 C4 1.39(3) . ?
C6 C7 1.41(3) . ?
C32 C27 1.43(3) . ?
C32 C31 1.39(2) . ?
C10 H10 0.9500 . ?
C24 H24 0.9500 . ?
C24 C23 1.37(2) . ?
C17 H17 0.9500 . ?
C20 C22 1.43(2) . ?
C20 C21 1.36(2) . ?
C14 H14 0.9500 . ?
C4 C3 1.40(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.38(2) . ?
C27 C26 1.42(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.34(2) . ?
C31 H31 0.9500 . ?
C7 H7 0.9500 . ?
C26 H26 0.9500 . ?
C2 H2 0.9500 . ?
C2 C1 1.38(3) . ?
C23 H23 0.9500 . ?
C1 H1 0.9500 . ?
C37 H37 0.9500 . ?
C37 C36 1.38(3) . ?
C37 C38 1.39(3) . ?
C36 C39 1.50(3) . ?
C36 C35 1.40(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.41(2) . ?
C34 C33 1.39(2) . ?
C38 H38 0.9500 . ?
C38 C33 1.40(2) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C35 H35 0.9500 . ?
O6 H6A 0.8692 . ?
O6 H6B 0.8697 . ?
O7 H7A 0.868(18) . ?
O7 H7B 0.891(16) . ?

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 Fe1 O2 94.7(4) . . ?
O1 Fe1 N4 85.1(5) . . ?
O1 Fe1 N3 89.0(5) . . ?
O1 Fe1 N2 94.6(6) . . ?
O1 Fe1 N1 175.7(5) . . ?
O2 Fe1 N4 95.0(6) . . ?
O2 Fe1 N3 175.8(5) . . ?
O2 Fe1 N2 86.8(6) . . ?
O2 Fe1 N1 88.7(5) . . ?
N4 Fe1 N3 83.4(6) . . ?
N4 Fe1 N2 178.2(7) . . ?
N4 Fe1 N1 97.2(6) . . ?
N2 Fe1 N3 94.8(6) . . ?
N2 Fe1 N1 83.0(6) . . ?
N1 Fe1 N3 87.7(5) . . ?
O4 S4 C33 106.4(8) . . ?
O3 S4 O4 113.2(8) . . ?
O3 S4 O5 113.4(9) . . ?
O3 S4 C33 106.2(9) . . ?
O5 S4 O4 110.8(8) . . ?
O5 S4 C33 106.3(8) . . ?
C16 O1 Fe1 126.5(11) . . ?
C32 O2 Fe1 125.9(12) . . ?
C25 N4 Fe1 113.2(12) . . ?
C26 N4 Fe1 125.1(12) . . ?
C26 N4 C25 121.6(15) . . ?
C17 N3 Fe1 128.2(13) . . ?
C17 N3 C21 117.1(16) . . ?
C21 N3 Fe1 114.3(13) . . ?
C9 N2 Fe1 112.3(11) . . ?
C10 N2 Fe1 125.0(13) . . ?
C10 N2 C9 122.6(14) . . ?
C5 N1 Fe1 114.5(12) . . ?
C1 N1 Fe1 127.8(13) . . ?
C1 N1 C5 117.6(15) . . ?
C29 C28 H28 119.2 . . ?
C29 C28 C27 121.6(16) . . ?
C27 C28 H28 119.2 . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C13 C12 C11 121.5(16) . . ?
C28 C29 I2 119.2(13) . . ?
C28 C29 C30 120.3(18) . . ?
C30 C29 I2 120.3(13) . . ?
C29 C30 H30 121.3 . . ?
C31 C30 C29 117.5(18) . . ?
C31 C30 H30 121.3 . . ?
C5 C9 N2 116.0(14) . . ?
C5 C9 C8 117.3(16) . . ?
C8 C9 N2 126.6(16) . . ?
C12 C11 C10 120.1(17) . . ?
C16 C11 C12 119.2(16) . . ?
C16 C11 C10 120.8(17) . . ?
C19 C18 H18 120.4 . . ?
C19 C18 C17 119.1(18) . . ?
C17 C18 H18 120.4 . . ?
O1 C16 C11 125.7(17) . . ?
O1 C16 C15 116.9(15) . . ?
C15 C16 C11 117.4(16) . . ?
N1 C5 C4 122.5(16) . . ?
C9 C5 N1 114.1(16) . . ?
C9 C5 C4 123.3(17) . . ?
C18 C19 H19 119.2 . . ?
C18 C19 C20 121.6(18) . . ?
C20 C19 H19 119.2 . . ?
N4 C25 C21 115.5(16) . . ?
C24 C25 N4 129.2(19) . . ?
C24 C25 C21 115.2(18) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 C16 121.3(16) . . ?
C14 C15 H15 119.3 . . ?
C12 C13 I1 120.3(12) . . ?
C14 C13 I1 120.7(14) . . ?
C14 C13 C12 118.8(16) . . ?
C9 C8 H8 119.4 . . ?
C9 C8 C7 121.2(18) . . ?
C7 C8 H8 119.4 . . ?
C4 C6 H6 120.4 . . ?
C4 C6 C7 119.2(18) . . ?
C7 C6 H6 120.4 . . ?
O2 C32 C27 124.5(17) . . ?
O2 C32 C31 119.1(18) . . ?
C31 C32 C27 116.4(17) . . ?
N2 C10 C11 126.8(17) . . ?
N2 C10 H10 116.6 . . ?
C11 C10 H10 116.6 . . ?
C25 C24 H24 118.5 . . ?
C23 C24 C25 123.0(19) . . ?
C23 C24 H24 118.5 . . ?
N3 C17 C18 121.9(18) . . ?
N3 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C19 C20 C22 124.9(17) . . ?
C21 C20 C19 115.3(17) . . ?
C21 C20 C22 119.8(17) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 C15 121.7(18) . . ?
C13 C14 H14 119.2 . . ?
C6 C4 C5 118.4(17) . . ?
C6 C4 C3 124.9(17) . . ?
C3 C4 C5 116.7(18) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 C4 120.7(19) . . ?
C2 C3 H3 119.6 . . ?
C28 C27 C32 118.5(16) . . ?
C28 C27 C26 117.1(16) . . ?
C26 C27 C32 124.4(16) . . ?
C20 C22 H22 120.6 . . ?
C23 C22 C20 118.8(18) . . ?
C23 C22 H22 120.6 . . ?
C30 C31 C32 125.7(19) . . ?
C30 C31 H31 117.2 . . ?
C32 C31 H31 117.2 . . ?
C8 C7 C6 120.6(19) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
N4 C26 C27 124.6(16) . . ?
N4 C26 H26 117.7 . . ?
C27 C26 H26 117.7 . . ?
C3 C2 H2 120.5 . . ?
C3 C2 C1 119.0(18) . . ?
C1 C2 H2 120.5 . . ?
N3 C21 C25 113.3(17) . . ?
C20 C21 N3 124.9(18) . . ?
C20 C21 C25 121.9(17) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 C24 121.4(18) . . ?
C22 C23 H23 119.3 . . ?
N1 C1 C2 123.4(18) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C36 C37 H37 118.2 . . ?
C36 C37 C38 124(2) . . ?
C38 C37 H37 118.2 . . ?
C37 C36 C39 121(2) . . ?
C37 C36 C35 115.2(18) . . ?
C35 C36 C39 123(2) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
C33 C34 C35 118.9(19) . . ?
C37 C38 H38 120.0 . . ?
C37 C38 C33 120(2) . . ?
C33 C38 H38 120.0 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C35 C34 123.3(19) . . ?
C36 C35 H35 118.3 . . ?
C34 C35 H35 118.3 . . ?
C34 C33 S4 121.4(15) . . ?
C34 C33 C38 119.0(18) . . ?
C38 C33 S4 119.6(15) . . ?
H6A O6 H6B 109.5 . . ?
H7A O7 H7B 111(2) . . ?

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
I2 C29 C30 C31 175.8(14) . . . . ?
I1 C13 C14 C15 176.9(13) . . . . ?
Fe1 O1 C16 C11 2(3) . . . . ?
Fe1 O1 C16 C15 -178.7(11) . . . . ?
Fe1 O2 C32 C27 7(2) . . . . ?
Fe1 O2 C32 C31 -172.1(13) . . . . ?
Fe1 N4 C25 C24 175.1(16) . . . . ?
Fe1 N4 C25 C21 -3(2) . . . . ?
Fe1 N4 C26 C27 7(2) . . . . ?
Fe1 N3 C17 C18 174.7(13) . . . . ?
Fe1 N3 C21 C25 5(2) . . . . ?
Fe1 N3 C21 C20 -176.3(16) . . . . ?
Fe1 N2 C9 C5 1.8(19) . . . . ?
Fe1 N2 C9 C8 178.3(14) . . . . ?
Fe1 N2 C10 C11 11(3) . . . . ?
Fe1 N1 C5 C9 2.8(19) . . . . ?
Fe1 N1 C5 C4 -178.7(13) . . . . ?
Fe1 N1 C1 C2 178.0(14) . . . . ?
O1 C16 C15 C14 -177.7(15) . . . . ?
O2 Fe1 O1 C16 -85.0(13) . . . . ?
O2 C32 C27 C28 178.5(16) . . . . ?
O2 C32 C27 C26 -5(3) . . . . ?
O2 C32 C31 C30 -177.8(17) . . . . ?
O4 S4 C33 C34 124.2(16) . . . . ?
O4 S4 C33 C38 -56.7(18) . . . . ?
O3 S4 C33 C34 -115.0(16) . . . . ?
O3 S4 C33 C38 64.1(18) . . . . ?
N4 Fe1 O1 C16 -179.7(14) . . . . ?
N4 C25 C24 C23 -178.8(19) . . . . ?
N4 C25 C21 N3 -2(2) . . . . ?
N4 C25 C21 C20 179.7(18) . . . . ?
N3 Fe1 O1 C16 96.9(14) . . . . ?
N2 Fe1 O1 C16 2.1(14) . . . . ?
N2 C9 C5 N1 -3(2) . . . . ?
N2 C9 C5 C4 178.5(16) . . . . ?
N2 C9 C8 C7 -177.4(17) . . . . ?
N1 C5 C4 C6 179.9(17) . . . . ?
N1 C5 C4 C3 1(3) . . . . ?
O5 S4 C33 C34 6.1(19) . . . . ?
O5 S4 C33 C38 -174.8(16) . . . . ?
C28 C29 C30 C31 0(3) . . . . ?
C28 C27 C26 N4 174.1(15) . . . . ?
C12 C11 C16 O1 176.3(16) . . . . ?
C12 C11 C16 C15 -3(2) . . . . ?
C12 C11 C10 N2 176.4(17) . . . . ?
C12 C13 C14 C15 2(3) . . . . ?
C29 C28 C27 C32 1(3) . . . . ?
C29 C28 C27 C26 -175.9(17) . . . . ?
C29 C30 C31 C32 -2(3) . . . . ?
C9 N2 C10 C11 -174.2(16) . . . . ?
C9 C5 C4 C6 -2(3) . . . . ?
C9 C5 C4 C3 179.3(16) . . . . ?
C9 C8 C7 C6 0(3) . . . . ?
C11 C12 C13 I1 -178.2(13) . . . . ?
C11 C12 C13 C14 -3(3) . . . . ?
C11 C16 C15 C14 1(3) . . . . ?
C18 C19 C20 C22 -178.2(18) . . . . ?
C18 C19 C20 C21 -1(3) . . . . ?
C16 C11 C10 N2 -5(3) . . . . ?
C16 C15 C14 C13 -1(3) . . . . ?
C5 N1 C1 C2 1(3) . . . . ?
C5 C9 C8 C7 -1(3) . . . . ?
C5 C4 C3 C2 0(2) . . . . ?
C19 C18 C17 N3 -1(3) . . . . ?
C19 C20 C22 C23 178.9(18) . . . . ?
C19 C20 C21 N3 2(3) . . . . ?
C19 C20 C21 C25 -179.6(16) . . . . ?
C25 N4 C26 C27 -177.8(16) . . . . ?
C25 C24 C23 C22 1(3) . . . . ?
C13 C12 C11 C16 3(3) . . . . ?
C13 C12 C11 C10 -178.0(17) . . . . ?
C8 C9 C5 N1 -179.8(15) . . . . ?
C8 C9 C5 C4 2(3) . . . . ?
C6 C4 C3 C2 -178.7(18) . . . . ?
C32 C27 C26 N4 -2(3) . . . . ?
C10 N2 C9 C5 -173.6(16) . . . . ?
C10 N2 C9 C8 3(3) . . . . ?
C10 C11 C16 O1 -2(3) . . . . ?
C10 C11 C16 C15 178.9(16) . . . . ?
C24 C25 C21 N3 -179.7(17) . . . . ?
C24 C25 C21 C20 2(3) . . . . ?
C17 N3 C21 C25 178.7(16) . . . . ?
C17 N3 C21 C20 -3(3) . . . . ?
C17 C18 C19 C20 0(3) . . . . ?
C20 C22 C23 C24 -1(3) . . . . ?
C4 C6 C7 C8 0(3) . . . . ?
C4 C3 C2 C1 0(3) . . . . ?
C3 C2 C1 N1 0(3) . . . . ?
C27 C28 C29 I2 -175.3(12) . . . . ?
C27 C28 C29 C30 0(3) . . . . ?
C27 C32 C31 C30 3(3) . . . . ?
C22 C20 C21 N3 179.7(18) . . . . ?
C22 C20 C21 C25 -2(3) . . . . ?
C31 C32 C27 C28 -2(3) . . . . ?
C31 C32 C27 C26 174.4(17) . . . . ?
C7 C6 C4 C5 1(3) . . . . ?
C7 C6 C4 C3 179.8(17) . . . . ?
C26 N4 C25 C24 -1(3) . . . . ?
C26 N4 C25 C21 -178.6(16) . . . . ?
C21 N3 C17 C18 2(3) . . . . ?
C21 C25 C24 C23 -1(3) . . . . ?
C21 C20 C22 C23 1(3) . . . . ?
C1 N1 C5 C9 179.7(16) . . . . ?
C1 N1 C5 C4 -2(3) . . . . ?
C37 C36 C35 C34 -1(3) . . . . ?
C37 C38 C33 S4 -179.2(15) . . . . ?
C37 C38 C33 C34 0(3) . . . . ?
C36 C37 C38 C33 -1(3) . . . . ?
C38 C37 C36 C39 -177.1(18) . . . . ?
C38 C37 C36 C35 1(3) . . . . ?
C39 C36 C35 C34 177.5(19) . . . . ?
C35 C34 C33 S4 179.6(15) . . . . ?
C35 C34 C33 C38 0(3) . . . . ?
C33 C34 C35 C36 0(3) . . . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
