# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_1-chcl3
_database_code_depnum_ccdc_archive 'CCDC 2258378'
loop_
_audit_author_name
_audit_author_address
'ryo tsunashima'
;yamaguchi university
Japan
;
_audit_update_record             
;
2023-07-13 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H72 Fe4 O60, 2(C H Cl3), 0.5(H8 N2)'
_chemical_formula_sum            'C74 H78 Cl6 Fe4 N O60'
_chemical_formula_weight         2377.47
_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'
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   27.4286(8)
_cell_length_b                   17.9342(2)
_cell_length_c                   15.0384(4)
_cell_angle_alpha                90
_cell_angle_beta                 133.511(5)
_cell_angle_gamma                90
_cell_volume                     5365.0(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17902
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      77.8360
_cell_measurement_theta_min      3.3280
_shelx_estimated_absorpt_T_max   0.617
_shelx_estimated_absorpt_T_min   0.492
_exptl_absorpt_coefficient_mu    6.507
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2430
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 2 7 0.0643
-9 9 1 0.0598
16 3 -8 0.0524
7 -10 0 0.0301
8 8 0 0.0192
-9 -8 0 0.0612
14 1 -10 0.0503
-9 3 9 0.0411
-15 -5 8 0.0621

_exptl_crystal_preparation       'local laboratory'
_exptl_crystal_recrystallization_method 'vaper diffusion with hexane'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.082
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27983
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.195
_diffrn_reflns_theta_min         3.318
_diffrn_ambient_temperature      223.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -14.00   0.50    1.16    --  -43.03  95.00  95.00  108
  2  ω    -11.00  25.00   0.50    1.16    --  -43.03  95.00  95.00   72
  3  ω      9.00  67.00   0.50    1.16    --   43.03 -95.00 -14.00  116
  4  ω    -25.00   3.00   0.50    1.16    --   43.03 -95.00 -14.00   56
  5  ω    -67.00 -40.00   0.50    4.64    -- -103.00  95.00  95.00   54
  6  ω     92.00 178.00   0.50    4.64    --  113.50  95.00  95.00  172
  7  ω     21.00 115.00   0.50    1.16    --   43.03  57.00  30.00  188
  8  ω     26.00  64.00   0.50    1.16    --   43.03 -38.00 -30.00   76
  9  ω    -32.00  22.00   0.50    1.16    --   43.03 -38.00 -30.00  108
 10  ω     22.00 116.00   0.50    1.16    --   43.03  57.00  90.00  188
 11  ω     23.00 116.00   0.50    1.16    --   43.03  57.00 -90.00  186
 12  ω   -153.00-128.00   0.50    4.64    -- -103.00 -95.00 -14.00   50
 13  ω     39.00 105.00   0.50    4.64    --  113.50 -95.00  90.00  132
 14  ω     98.00 135.00   0.50    4.64    --  113.50 -45.00-180.00   74
 15  ω     85.00 178.00   0.50    4.64    --  113.50  77.00-120.00  186
 16  ω     38.00  90.00   0.50    4.64    --  113.50 -45.00-180.00  104
 17  ω     90.00 172.00   0.50    4.64    --  113.50  61.00  60.00  164
 18  ω     38.00  82.00   0.50    4.64    --  113.50 -45.00 -60.00   88
 19  ω     89.00 134.00   0.50    4.64    --  113.50 -45.00 -60.00   90
 20  ω     90.00 174.00   0.50    4.64    --  113.50  61.00 -60.00  168
 21  ω     39.00 105.00   0.50    4.64    --  113.50 -95.00 120.00  132
 22  ω     85.00 173.00   0.50    4.64    --  113.50  77.00  30.00  176
 23  ω     90.00 178.00   0.50    4.64    --  113.50  61.00-150.00  176
 24  ω     91.00 177.00   0.50    4.64    --  113.50  45.00-180.00  172
 25  ω     41.00 105.00   0.50    4.64    --  113.50 -95.00 -90.00  128
 26  ω     39.00 103.00   0.50    4.64    --  113.50 -95.00  30.00  128
 27  ω     43.00 103.00   0.50    4.64    --  113.50 -95.00 -60.00  120
 28  ω     57.00 105.00   0.50    4.64    --  113.50 -95.00 -14.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                10290
_reflns_number_total             11080
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.022(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11080
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1001P)²+9.8214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1643
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.978(5)
 0.022(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1a
 1.07 with sigma of 0.02
 N1-H1b
 1.07 with sigma of 0.02
 N1-H1c
 1.07 with sigma of 0.02
 N1-H1d
 1.07 with sigma of 0.02
 H1a-H1b
 1.75 with sigma of 0.04
 H1a-H1c
 1.75 with sigma of 0.04
 H1a-H1d
 1.75 with sigma of 0.04
 H1b-H1c
 1.75 with sigma of 0.04
 H1b-H1d
 1.75 with sigma of 0.04
 H1c-H1d
 1.75 with sigma of 0.04
4. Others
 Fixed Sof: H1a(0.5) H1b(0.5) H1c(0.5) H1d(0.5)
5.a Ternary CH refined with riding coordinates:
 C99(H99)
5.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C14(H14a,
 H14b,H14c), C15(H15a,H15b,H15c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c),
 C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C32(H32a,H32b,H32c), C33(H33a,H33b,
 H33c)
;
_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
Fe1 Fe 0.66218(4) 0.42225(5) 0.72176(8) 0.0254(2) Uani 1 1 d . . . . .
Fe2 Fe 0.50927(4) 0.67081(5) 0.29850(8) 0.0243(2) Uani 1 1 d . . . . .
O1 O 0.6767(2) 0.3322(2) 0.6646(4) 0.0327(9) Uani 1 1 d . . . . .
O2 O 0.6569(3) 0.2469(4) 0.5376(6) 0.0547(15) Uani 1 1 d . . . . .
O3 O 0.5533(3) 0.1573(3) 0.4518(7) 0.068(2) Uani 1 1 d . . . . .
O4 O 0.4625(3) 0.2306(4) 0.3316(5) 0.0592(16) Uani 1 1 d . . . . .
O5 O 0.5670(2) 0.3888(2) 0.6081(4) 0.0322(9) Uani 1 1 d . . . . .
O6 O 0.7557(2) 0.4669(2) 0.8322(4) 0.0327(9) Uani 1 1 d . . . . .
O7 O 0.8233(2) 0.5656(3) 0.9244(4) 0.0413(11) Uani 1 1 d . . . . .
O8 O 0.8181(3) 0.6565(5) 0.7826(7) 0.085(3) Uani 1 1 d . . . . .
O9 O 0.7131(3) 0.6983(3) 0.6426(7) 0.0647(17) Uani 1 1 d . . . . .
O10 O 0.6432(2) 0.4848(2) 0.5953(4) 0.0312(9) Uani 1 1 d . . . . .
O11 O 0.5543(2) 0.6379(3) 0.2402(4) 0.0320(9) Uani 1 1 d . . . . .
O12 O 0.6389(3) 0.6078(3) 0.2562(5) 0.0449(12) Uani 1 1 d . . . . .
O13 O 0.7649(3) 0.5998(4) 0.5142(7) 0.069(2) Uani 1 1 d . . . . .
O14 O 0.7338(3) 0.4858(4) 0.5103(8) 0.076(2) Uani 1 1 d . . . . .
O15 O 0.5770(2) 0.6091(3) 0.4439(4) 0.0304(8) Uani 1 1 d . . . . .
O16 O 0.5658(2) 0.7615(2) 0.3579(4) 0.0348(9) Uani 1 1 d . . . . .
O17 O 0.6353(3) 0.8524(3) 0.4845(6) 0.0498(13) Uani 1 1 d . . . . .
O18 O 0.6032(3) 0.8448(4) 0.6899(5) 0.0558(15) Uani 1 1 d . . . . .
O19 O 0.5914(4) 0.9355(3) 0.5761(7) 0.0626(16) Uani 1 1 d . . . . .
O20 O 0.4849(2) 0.7081(2) 0.3867(4) 0.0287(8) Uani 1 1 d . . . . .
O21 O 0.4347(2) 0.7182(2) 0.1347(4) 0.0304(8) Uani 1 1 d . . . . .
O22 O 0.3314(2) 0.7458(3) -0.0420(4) 0.0399(11) Uani 1 1 d . . . . .
O23 O 0.2496(3) 0.6270(4) -0.1678(5) 0.0559(15) Uani 1 1 d . . . . .
O24 O 0.2385(3) 0.5909(3) -0.0404(6) 0.0525(14) Uani 1 1 d . . . . .
O25 O 0.4480(2) 0.5855(2) 0.2332(4) 0.0305(9) Uani 1 1 d . . . . .
O26 O 0.3097(2) 0.3630(2) 0.1345(4) 0.0353(9) Uani 1 1 d . . . . .
O27 O 0.3058(4) 0.3272(3) -0.0102(6) 0.0554(15) Uani 1 1 d . . . . .
O28 O 0.2730(3) 0.4476(4) -0.1577(5) 0.0511(14) Uani 1 1 d . . . . .
O29 O 0.3794(3) 0.4865(4) -0.0332(5) 0.0494(13) Uani 1 1 d . . . . .
O30 O 0.3638(2) 0.5020(2) 0.2286(4) 0.0286(8) Uani 1 1 d . . . . .
C1 C 0.6357(3) 0.2886(4) 0.5772(6) 0.0322(12) Uani 1 1 d . . . . .
C2 C 0.7272(5) 0.2545(7) 0.6025(13) 0.080(4) Uani 1 1 d . . . . .
H2A H 0.738381 0.218888 0.570224 0.120 Uiso 1 1 calc R U . . .
H2B H 0.754741 0.244973 0.689046 0.120 Uiso 1 1 calc R U . . .
H2C H 0.735566 0.304653 0.591579 0.120 Uiso 1 1 calc R U . . .
C3 C 0.5129(6) 0.0937(7) 0.3723(13) 0.091(4) Uani 1 1 d . . . . .
H3A H 0.498743 0.101113 0.293401 0.137 Uiso 1 1 calc R U . . .
H3B H 0.473655 0.089254 0.360858 0.137 Uiso 1 1 calc R U . . .
H3C H 0.539516 0.048491 0.409775 0.137 Uiso 1 1 calc R U . . .
C4 C 0.5225(3) 0.2218(4) 0.4220(7) 0.0435(16) Uani 1 1 d . . . . .
C5 C 0.5665(3) 0.2818(4) 0.5139(6) 0.0319(12) Uani 1 1 d . . . . .
C6 C 0.5375(3) 0.3330(3) 0.5357(6) 0.0287(11) Uani 1 1 d . . . . .
C7 C 0.7703(3) 0.5321(3) 0.8258(6) 0.0302(12) Uani 1 1 d . . . . .
C8 C 0.8645(4) 0.5249(5) 1.0385(7) 0.0503(18) Uani 1 1 d . . . . .
H8A H 0.878925 0.478392 1.029739 0.075 Uiso 1 1 calc R U . . .
H8B H 0.838725 0.514430 1.059381 0.075 Uiso 1 1 calc R U . . .
H8C H 0.903611 0.554547 1.102928 0.075 Uiso 1 1 calc R U . . .
C9 C 0.8412(8) 0.7318(10) 0.7877(14) 0.132(8) Uani 1 1 d . . . . .
H9A H 0.824803 0.744534 0.708341 0.198 Uiso 1 1 calc R U . . .
H9B H 0.889916 0.733160 0.849202 0.198 Uiso 1 1 calc R U . . .
H9C H 0.823985 0.767449 0.809033 0.198 Uiso 1 1 calc R U . . .
C10 C 0.7519(4) 0.6502(4) 0.7096(7) 0.0459(16) Uani 1 1 d . . . . .
C11 C 0.7320(3) 0.5744(4) 0.7140(6) 0.0342(13) Uani 1 1 d . . . . .
C12 C 0.6732(3) 0.5451(3) 0.6075(5) 0.0277(11) Uani 1 1 d . . . . .
C13 C 0.6127(3) 0.6126(4) 0.3036(6) 0.0311(12) Uani 1 1 d . . . . .
C14 C 0.5987(5) 0.6330(6) 0.1324(8) 0.057(2) Uani 1 1 d . . . . .
H14A H 0.558021 0.603270 0.077817 0.086 Uiso 1 1 calc R U . . .
H14B H 0.623974 0.627715 0.109317 0.086 Uiso 1 1 calc R U . . .
H14C H 0.586893 0.684948 0.126235 0.086 Uiso 1 1 calc R U . . .
C15 C 0.8318(5) 0.5711(8) 0.5745(12) 0.081(4) Uani 1 1 d . . . . .
H15A H 0.827177 0.531639 0.525033 0.122 Uiso 1 1 calc R U . . .
H15B H 0.853661 0.551605 0.654729 0.122 Uiso 1 1 calc R U . . .
H15C H 0.858706 0.611171 0.583580 0.122 Uiso 1 1 calc R U . . .
C16 C 0.7209(3) 0.5509(4) 0.4858(7) 0.0407(15) Uani 1 1 d . . . . .
C17 C 0.6544(3) 0.5857(4) 0.4256(6) 0.0350(13) Uani 1 1 d . . . . .
C18 C 0.6328(3) 0.5838(3) 0.4842(5) 0.0286(11) Uani 1 1 d . . . . .
C19 C 0.5856(3) 0.8070(4) 0.4408(6) 0.0350(13) Uani 1 1 d . . . . .
C20 C 0.6672(6) 0.8423(6) 0.4375(11) 0.067(3) Uani 1 1 d . . . . .
H20A H 0.635370 0.854957 0.351102 0.100 Uiso 1 1 calc R U . . .
H20B H 0.680966 0.790718 0.448208 0.100 Uiso 1 1 calc R U . . .
H20C H 0.706203 0.874466 0.482174 0.100 Uiso 1 1 calc R U . . .
C21 C 0.6237(7) 0.8983(7) 0.7803(11) 0.081(4) Uani 1 1 d . . . . .
H21A H 0.584440 0.923761 0.754385 0.122 Uiso 1 1 calc R U . . .
H21B H 0.653510 0.934411 0.790271 0.122 Uiso 1 1 calc R U . . .
H21C H 0.647053 0.873272 0.857696 0.122 Uiso 1 1 calc R U . . .
C22 C 0.5863(4) 0.8712(4) 0.5894(7) 0.0407(15) Uani 1 1 d . . . . .
C23 C 0.5602(3) 0.8109(4) 0.4979(6) 0.0327(12) Uani 1 1 d . . . . .
C24 C 0.5123(3) 0.7609(3) 0.4674(5) 0.0278(11) Uani 1 1 d . . . . .
C25 C 0.3739(3) 0.6996(3) 0.0495(5) 0.0290(11) Uani 1 1 d . . . . .
C26 C 0.3582(4) 0.8140(4) -0.0451(8) 0.0511(19) Uani 1 1 d . . . . .
H26A H 0.376038 0.804322 -0.081575 0.077 Uiso 1 1 calc R U . . .
H26B H 0.393755 0.832502 0.037709 0.077 Uiso 1 1 calc R U . . .
H26C H 0.322661 0.850910 -0.093625 0.077 Uiso 1 1 calc R U . . .
C27 C 0.1783(4) 0.6135(6) -0.2694(8) 0.075(3) Uani 1 1 d . . . . .
H27A H 0.166082 0.623815 -0.345999 0.113 Uiso 1 1 calc R U . . .
H27B H 0.152890 0.645830 -0.262062 0.113 Uiso 1 1 calc R U . . .
H27C H 0.168316 0.561858 -0.268184 0.113 Uiso 1 1 calc R U . . .
C28 C 0.2725(3) 0.6143(4) -0.0573(6) 0.0363(13) Uani 1 1 d . . . . .
C29 C 0.3451(3) 0.6312(3) 0.0439(6) 0.0296(11) Uani 1 1 d . . . . .
C30 C 0.3854(3) 0.5790(3) 0.1366(5) 0.0260(11) Uani 1 1 d . . . . .
C31 C 0.3157(3) 0.3789(4) 0.0624(6) 0.0340(13) Uani 1 1 d . . . . .
C32 C 0.2912(7) 0.2515(5) 0.0020(12) 0.078(3) Uani 1 1 d . . . . .
H32A H 0.288940 0.218188 -0.051664 0.117 Uiso 1 1 calc R U . . .
H32B H 0.248553 0.250993 -0.020466 0.117 Uiso 1 1 calc R U . . .
H32C H 0.326584 0.234976 0.086239 0.117 Uiso 1 1 calc R U . . .
C33 C 0.2663(5) 0.4562(7) -0.2618(8) 0.067(3) Uani 1 1 d . . . . .
H33A H 0.281974 0.505269 -0.259503 0.101 Uiso 1 1 calc R U . . .
H33B H 0.219441 0.450590 -0.337329 0.101 Uiso 1 1 calc R U . . .
H33C H 0.292929 0.418408 -0.258165 0.101 Uiso 1 1 calc R U . . .
C34 C 0.3329(4) 0.4631(4) -0.0490(6) 0.0373(14) Uani 1 1 d . . . . .
C35 C 0.3348(3) 0.4499(3) 0.0516(6) 0.0308(12) Uani 1 1 d . . . . .
C36 C 0.3582(3) 0.5057(3) 0.1371(5) 0.0255(11) Uani 1 1 d . . . . .
Cl1 Cl 0.5714(3) 0.4244(4) 0.1685(5) 0.1359(18) Uani 1 1 d . . . . .
Cl2 Cl 0.5449(3) 0.4191(2) 0.3220(4) 0.1196(15) Uani 1 1 d . . . . .
Cl3 Cl 0.4934(4) 0.3034(3) 0.1417(6) 0.154(2) Uani 1 1 d . . . . .
C99 C 0.5150(6) 0.3970(8) 0.1794(10) 0.076(3) Uani 1 1 d . . . . .
H99 H 0.473413 0.426279 0.117961 0.092 Uiso 1 1 calc R U . . .
N1 N 0.500000 0.5436(5) 0.500000 0.0406(18) Uani 1 2 d DS T P . .
H1A H 0.498(7) 0.486(2) 0.481(12) 0.049 Uiso 0.5 1 d D U P A -1
H1B H 0.544(5) 0.553(7) 0.595(4) 0.049 Uiso 0.5 1 d D U P B -1
H1C H 0.458(5) 0.557(7) 0.489(14) 0.049 Uiso 0.5 1 d D U P C -1
H1D H 0.500(7) 0.577(6) 0.442(10) 0.049 Uiso 0.5 1 d D U P D -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.993(4) . ?
Fe1 O5 1.987(4) . ?
Fe1 O6 2.027(4) . ?
Fe1 O10 1.945(4) . ?
Fe1 O26 2.025(5) 2_656 ?
Fe1 O30 1.959(4) 2_656 ?
Fe2 O11 2.033(4) . ?
Fe2 O15 1.966(4) . ?
Fe2 O16 1.985(4) . ?
Fe2 O20 1.969(4) . ?
Fe2 O21 2.008(4) . ?
Fe2 O25 1.964(4) . ?
O1 C1 1.252(8) . ?
O2 C1 1.318(8) . ?
O2 C2 1.448(10) . ?
O3 C3 1.461(11) . ?
O3 C4 1.316(9) . ?
O4 C4 1.224(9) . ?
O5 C6 1.277(7) . ?
O6 C7 1.261(8) . ?
O7 C7 1.306(8) . ?
O7 C8 1.443(9) . ?
O8 C9 1.471(14) . ?
O8 C10 1.331(10) . ?
O9 C10 1.189(10) . ?
O10 C12 1.293(8) . ?
O11 C13 1.256(8) . ?
O12 C13 1.318(8) . ?
O12 C14 1.435(9) . ?
O13 C15 1.471(10) . ?
O13 C16 1.303(10) . ?
O14 C16 1.202(10) . ?
O15 C18 1.282(7) . ?
O16 C19 1.258(8) . ?
O17 C19 1.312(8) . ?
O17 C20 1.464(10) . ?
O18 C21 1.426(11) . ?
O18 C22 1.325(10) . ?
O19 C22 1.196(10) . ?
O20 C24 1.296(7) . ?
O21 C25 1.263(7) . ?
O22 C25 1.315(7) . ?
O22 C26 1.444(9) . ?
O23 C27 1.449(9) . ?
O23 C28 1.330(9) . ?
O24 C28 1.197(9) . ?
O25 C30 1.280(7) . ?
O26 C31 1.237(8) . ?
O27 C31 1.311(8) . ?
O27 C32 1.463(11) . ?
O28 C33 1.454(10) . ?
O28 C34 1.323(9) . ?
O29 C34 1.201(9) . ?
O30 C36 1.277(7) . ?
C1 C5 1.426(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 C5 1.492(9) . ?
C5 C6 1.392(8) . ?
C6 C6 1.533(11) 2_656 ?
C7 C11 1.441(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.483(10) . ?
C11 C12 1.373(9) . ?
C12 C18 1.522(8) . ?
C13 C17 1.421(9) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.503(9) . ?
C17 C18 1.359(9) . ?
C19 C23 1.432(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 C23 1.489(9) . ?
C23 C24 1.383(8) . ?
C24 C24 1.524(12) 2_656 ?
C25 C29 1.429(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 C29 1.483(8) . ?
C29 C30 1.385(8) . ?
C30 C36 1.515(8) . ?
C31 C35 1.427(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 C35 1.496(9) . ?
C35 C36 1.389(8) . ?
Cl1 C99 1.734(12) . ?
Cl2 C99 1.734(13) . ?
Cl3 C99 1.739(14) . ?
C99 H99 0.9900 . ?
N1 H1A 1.07(3) . ?
N1 H1B 1.07(3) . ?
N1 H1C 1.07(3) . ?
N1 H1D 1.06(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O6 99.08(18) . . ?
O1 Fe1 O26 89.58(19) . 2_656 ?
O5 Fe1 O1 85.32(18) . . ?
O5 Fe1 O6 174.30(19) . . ?
O5 Fe1 O26 94.0(2) . 2_656 ?
O10 Fe1 O1 92.5(2) . . ?
O10 Fe1 O5 91.40(19) . . ?
O10 Fe1 O6 84.81(18) . . ?
O10 Fe1 O26 174.4(2) . 2_656 ?
O10 Fe1 O30 91.65(19) . 2_656 ?
O26 Fe1 O6 89.68(19) 2_656 . ?
O30 Fe1 O1 171.03(18) 2_656 . ?
O30 Fe1 O5 86.65(18) 2_656 . ?
O30 Fe1 O6 89.20(18) 2_656 . ?
O30 Fe1 O26 86.99(18) 2_656 2_656 ?
O15 Fe2 O11 85.84(18) . . ?
O15 Fe2 O16 96.5(2) . . ?
O15 Fe2 O20 86.58(18) . . ?
O15 Fe2 O21 170.65(19) . . ?
O16 Fe2 O11 85.1(2) . . ?
O16 Fe2 O21 91.49(19) . . ?
O20 Fe2 O11 168.02(18) . . ?
O20 Fe2 O16 86.58(18) . . ?
O20 Fe2 O21 98.72(18) . . ?
O21 Fe2 O11 90.09(18) . . ?
O25 Fe2 O11 97.09(19) . . ?
O25 Fe2 O15 86.87(18) . . ?
O25 Fe2 O16 176.1(2) . . ?
O25 Fe2 O20 91.74(18) . . ?
O25 Fe2 O21 85.29(17) . . ?
C1 O1 Fe1 131.0(4) . . ?
C1 O2 C2 116.1(6) . . ?
C4 O3 C3 117.3(7) . . ?
C6 O5 Fe1 131.0(4) . . ?
C7 O6 Fe1 126.3(4) . . ?
C7 O7 C8 117.7(6) . . ?
C10 O8 C9 114.4(10) . . ?
C12 O10 Fe1 128.9(4) . . ?
C13 O11 Fe2 127.8(4) . . ?
C13 O12 C14 117.6(5) . . ?
C16 O13 C15 116.7(8) . . ?
C18 O15 Fe2 129.2(4) . . ?
C19 O16 Fe2 130.4(4) . . ?
C19 O17 C20 116.2(6) . . ?
C22 O18 C21 116.5(8) . . ?
C24 O20 Fe2 129.3(4) . . ?
C25 O21 Fe2 130.7(4) . . ?
C25 O22 C26 117.6(5) . . ?
C28 O23 C27 115.0(7) . . ?
C30 O25 Fe2 131.0(4) . . ?
C31 O26 Fe1 129.2(4) . 2_656 ?
C31 O27 C32 118.0(7) . . ?
C34 O28 C33 115.9(6) . . ?
C36 O30 Fe1 130.0(4) . 2_656 ?
O1 C1 O2 118.2(6) . . ?
O1 C1 C5 125.1(6) . . ?
O2 C1 C5 116.7(6) . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 C5 113.4(6) . . ?
O4 C4 O3 123.3(7) . . ?
O4 C4 C5 123.2(7) . . ?
C1 C5 C4 122.5(6) . . ?
C6 C5 C1 119.9(6) . . ?
C6 C5 C4 117.7(5) . . ?
O5 C6 C5 126.1(5) . . ?
O5 C6 C6 110.7(4) . 2_656 ?
C5 C6 C6 123.0(5) . 2_656 ?
O6 C7 O7 120.3(6) . . ?
O6 C7 C11 124.3(6) . . ?
O7 C7 C11 115.4(6) . . ?
O7 C8 H8A 109.5 . . ?
O7 C8 H8B 109.5 . . ?
O7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O8 C9 H9A 109.5 . . ?
O8 C9 H9B 109.5 . . ?
O8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O8 C10 C11 112.0(7) . . ?
O9 C10 O8 123.7(8) . . ?
O9 C10 C11 124.1(7) . . ?
C7 C11 C10 122.7(6) . . ?
C12 C11 C7 119.1(6) . . ?
C12 C11 C10 118.1(6) . . ?
O10 C12 C11 127.4(6) . . ?
O10 C12 C18 110.5(5) . . ?
C11 C12 C18 122.1(5) . . ?
O11 C13 O12 119.9(6) . . ?
O11 C13 C17 125.2(6) . . ?
O12 C13 C17 115.0(5) . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
O12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O13 C15 H15A 109.5 . . ?
O13 C15 H15B 109.5 . . ?
O13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C16 C17 112.6(6) . . ?
O14 C16 O13 122.7(7) . . ?
O14 C16 C17 124.6(7) . . ?
C13 C17 C16 118.9(6) . . ?
C18 C17 C13 121.5(6) . . ?
C18 C17 C16 119.2(6) . . ?
O15 C18 C12 111.5(5) . . ?
O15 C18 C17 126.6(6) . . ?
C17 C18 C12 121.8(5) . . ?
O16 C19 O17 119.3(6) . . ?
O16 C19 C23 124.7(6) . . ?
O17 C19 C23 115.9(6) . . ?
O17 C20 H20A 109.5 . . ?
O17 C20 H20B 109.5 . . ?
O17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O18 C21 H21A 109.5 . . ?
O18 C21 H21B 109.5 . . ?
O18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O18 C22 C23 111.3(6) . . ?
O19 C22 O18 123.1(7) . . ?
O19 C22 C23 125.6(7) . . ?
C19 C23 C22 117.9(6) . . ?
C24 C23 C19 120.8(6) . . ?
C24 C23 C22 121.3(6) . . ?
O20 C24 C23 126.2(5) . . ?
O20 C24 C24 112.0(4) . 2_656 ?
C23 C24 C24 121.8(5) . 2_656 ?
O21 C25 O22 119.7(5) . . ?
O21 C25 C29 125.3(5) . . ?
O22 C25 C29 115.0(5) . . ?
O22 C26 H26A 109.5 . . ?
O22 C26 H26B 109.5 . . ?
O22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O23 C27 H27A 109.5 . . ?
O23 C27 H27B 109.5 . . ?
O23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O23 C28 C29 113.1(6) . . ?
O24 C28 O23 123.9(6) . . ?
O24 C28 C29 123.0(7) . . ?
C25 C29 C28 122.2(5) . . ?
C30 C29 C25 119.6(5) . . ?
C30 C29 C28 118.2(5) . . ?
O25 C30 C29 126.8(5) . . ?
O25 C30 C36 110.7(5) . . ?
C29 C30 C36 122.5(5) . . ?
O26 C31 O27 119.4(6) . . ?
O26 C31 C35 125.8(6) . . ?
O27 C31 C35 114.7(6) . . ?
O27 C32 H32A 109.5 . . ?
O27 C32 H32B 109.5 . . ?
O27 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O28 C33 H33A 109.5 . . ?
O28 C33 H33B 109.5 . . ?
O28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O28 C34 C35 111.4(6) . . ?
O29 C34 O28 124.3(7) . . ?
O29 C34 C35 124.2(6) . . ?
C31 C35 C34 119.7(6) . . ?
C36 C35 C31 120.6(6) . . ?
C36 C35 C34 119.6(5) . . ?
O30 C36 C30 110.9(5) . . ?
O30 C36 C35 126.5(5) . . ?
C35 C36 C30 122.4(5) . . ?
Cl1 C99 Cl2 111.0(7) . . ?
Cl1 C99 Cl3 111.7(8) . . ?
Cl1 C99 H99 107.0 . . ?
Cl2 C99 Cl3 112.8(7) . . ?
Cl2 C99 H99 107.0 . . ?
Cl3 C99 H99 107.0 . . ?
H1A N1 H1B 108(5) . . ?
H1A N1 H1C 109(5) . . ?
H1A N1 H1D 111(5) . . ?
H1B N1 H1C 106(5) . . ?
H1B N1 H1D 111(5) . . ?
H1C N1 H1D 111(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
Fe1 O1 C1 O2 160.6(5) . . . . ?
Fe1 O1 C1 C5 -17.5(10) . . . . ?
Fe1 O5 C6 C5 -3.8(10) . . . . ?
Fe1 O5 C6 C6 -178.4(4) . . . 2_656 ?
Fe1 O6 C7 O7 150.4(5) . . . . ?
Fe1 O6 C7 C11 -30.1(9) . . . . ?
Fe1 O10 C12 C11 10.0(9) . . . . ?
Fe1 O10 C12 C18 -168.5(4) . . . . ?
Fe1 O26 C31 O27 167.2(5) 2_656 . . . ?
Fe1 O26 C31 C35 -11.0(10) 2_656 . . . ?
Fe1 O30 C36 C30 179.9(4) 2_656 . . . ?
Fe1 O30 C36 C35 -4.0(9) 2_656 . . . ?
Fe2 O11 C13 O12 -166.5(5) . . . . ?
Fe2 O11 C13 C17 15.3(9) . . . . ?
Fe2 O15 C18 C12 174.0(4) . . . . ?
Fe2 O15 C18 C17 -9.5(10) . . . . ?
Fe2 O16 C19 O17 163.7(5) . . . . ?
Fe2 O16 C19 C23 -12.7(10) . . . . ?
Fe2 O20 C24 C23 9.8(9) . . . . ?
Fe2 O20 C24 C24 -167.8(4) . . . 2_656 ?
Fe2 O21 C25 O22 169.1(4) . . . . ?
Fe2 O21 C25 C29 -9.2(9) . . . . ?
Fe2 O25 C30 C29 6.8(9) . . . . ?
Fe2 O25 C30 C36 -170.7(4) . . . . ?
O1 C1 C5 C4 -171.4(7) . . . . ?
O1 C1 C5 C6 9.5(10) . . . . ?
O2 C1 C5 C4 10.4(10) . . . . ?
O2 C1 C5 C6 -168.6(7) . . . . ?
O3 C4 C5 C1 37.6(11) . . . . ?
O3 C4 C5 C6 -143.3(7) . . . . ?
O4 C4 C5 C1 -146.5(8) . . . . ?
O4 C4 C5 C6 32.6(12) . . . . ?
O6 C7 C11 C10 -178.2(6) . . . . ?
O6 C7 C11 C12 4.7(10) . . . . ?
O7 C7 C11 C10 1.4(10) . . . . ?
O7 C7 C11 C12 -175.7(6) . . . . ?
O8 C10 C11 C7 39.2(11) . . . . ?
O8 C10 C11 C12 -143.7(7) . . . . ?
O9 C10 C11 C7 -145.6(8) . . . . ?
O9 C10 C11 C12 31.5(12) . . . . ?
O10 C12 C18 O15 67.4(7) . . . . ?
O10 C12 C18 C17 -109.3(7) . . . . ?
O11 C13 C17 C16 174.7(6) . . . . ?
O11 C13 C17 C18 1.6(11) . . . . ?
O12 C13 C17 C16 -3.7(9) . . . . ?
O12 C13 C17 C18 -176.8(6) . . . . ?
O13 C16 C17 C13 72.0(9) . . . . ?
O13 C16 C17 C18 -114.7(8) . . . . ?
O14 C16 C17 C13 -110.8(10) . . . . ?
O14 C16 C17 C18 62.5(11) . . . . ?
O16 C19 C23 C22 -176.4(7) . . . . ?
O16 C19 C23 C24 2.7(11) . . . . ?
O17 C19 C23 C22 7.1(10) . . . . ?
O17 C19 C23 C24 -173.8(6) . . . . ?
O18 C22 C23 C19 -133.2(7) . . . . ?
O18 C22 C23 C24 47.7(9) . . . . ?
O19 C22 C23 C19 47.4(11) . . . . ?
O19 C22 C23 C24 -131.7(8) . . . . ?
O21 C25 C29 C28 177.8(6) . . . . ?
O21 C25 C29 C30 -0.9(9) . . . . ?
O22 C25 C29 C28 -0.6(9) . . . . ?
O22 C25 C29 C30 -179.3(6) . . . . ?
O23 C28 C29 C25 48.6(9) . . . . ?
O23 C28 C29 C30 -132.7(6) . . . . ?
O24 C28 C29 C25 -132.3(7) . . . . ?
O24 C28 C29 C30 46.4(10) . . . . ?
O25 C30 C36 O30 61.5(6) . . . . ?
O25 C30 C36 C35 -114.8(6) . . . . ?
O26 C31 C35 C34 -173.5(6) . . . . ?
O26 C31 C35 C36 9.7(10) . . . . ?
O27 C31 C35 C34 8.2(9) . . . . ?
O27 C31 C35 C36 -168.6(6) . . . . ?
O28 C34 C35 C31 54.7(9) . . . . ?
O28 C34 C35 C36 -128.5(6) . . . . ?
O29 C34 C35 C31 -127.1(8) . . . . ?
O29 C34 C35 C36 49.8(10) . . . . ?
C1 C5 C6 O5 1.2(10) . . . . ?
C1 C5 C6 C6 175.2(6) . . . 2_656 ?
C2 O2 C1 O1 1.6(12) . . . . ?
C2 O2 C1 C5 179.9(9) . . . . ?
C3 O3 C4 O4 -0.6(15) . . . . ?
C3 O3 C4 C5 175.3(10) . . . . ?
C4 C5 C6 O5 -177.9(6) . . . . ?
C4 C5 C6 C6 -3.9(10) . . . 2_656 ?
C7 C11 C12 O10 6.4(10) . . . . ?
C7 C11 C12 C18 -175.2(6) . . . . ?
C8 O7 C7 O6 1.4(10) . . . . ?
C8 O7 C7 C11 -178.2(6) . . . . ?
C9 O8 C10 O9 8.3(17) . . . . ?
C9 O8 C10 C11 -176.5(11) . . . . ?
C10 C11 C12 O10 -170.8(6) . . . . ?
C10 C11 C12 C18 7.6(9) . . . . ?
C11 C12 C18 O15 -111.2(6) . . . . ?
C11 C12 C18 C17 72.1(8) . . . . ?
C13 C17 C18 O15 -5.0(11) . . . . ?
C13 C17 C18 C12 171.2(6) . . . . ?
C14 O12 C13 O11 0.6(10) . . . . ?
C14 O12 C13 C17 179.0(7) . . . . ?
C15 O13 C16 O14 2.3(14) . . . . ?
C15 O13 C16 C17 179.5(8) . . . . ?
C16 C17 C18 O15 -178.1(6) . . . . ?
C16 C17 C18 C12 -1.9(10) . . . . ?
C19 C23 C24 O20 -1.3(10) . . . . ?
C19 C23 C24 C24 176.1(6) . . . 2_656 ?
C20 O17 C19 O16 -4.1(12) . . . . ?
C20 O17 C19 C23 172.6(8) . . . . ?
C21 O18 C22 O19 4.5(13) . . . . ?
C21 O18 C22 C23 -175.0(8) . . . . ?
C22 C23 C24 O20 177.8(6) . . . . ?
C22 C23 C24 C24 -4.8(9) . . . 2_656 ?
C25 C29 C30 O25 2.2(10) . . . . ?
C25 C29 C30 C36 179.5(5) . . . . ?
C26 O22 C25 O21 4.9(9) . . . . ?
C26 O22 C25 C29 -176.6(6) . . . . ?
C27 O23 C28 O24 2.7(12) . . . . ?
C27 O23 C28 C29 -178.2(7) . . . . ?
C28 C29 C30 O25 -176.5(6) . . . . ?
C28 C29 C30 C36 0.8(9) . . . . ?
C29 C30 C36 O30 -116.2(6) . . . . ?
C29 C30 C36 C35 67.5(8) . . . . ?
C31 C35 C36 O30 -1.8(9) . . . . ?
C31 C35 C36 C30 173.8(5) . . . . ?
C32 O27 C31 O26 -3.0(12) . . . . ?
C32 O27 C31 C35 175.4(8) . . . . ?
C33 O28 C34 O29 3.7(12) . . . . ?
C33 O28 C34 C35 -178.1(7) . . . . ?
C34 C35 C36 O30 -178.7(6) . . . . ?
C34 C35 C36 C30 -3.0(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.472 0.000 252.2 106.8 '2 chloroform'
2 0.500 0.972 1.000 252.2 106.8 '2 chloroform'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.978(5)
2 0.022(5)
####################################################################### 
# 
# 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_1-ch2cl2
_database_code_depnum_ccdc_archive 'CCDC 2279856'
loop_
_audit_author_name
_audit_author_address
'ryo tsunashima' 'yamaguchi university'
_audit_update_record             
;
2023-07-24 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_audit_creation_date             2023-07-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        C74H76Cl4Fe4NO60
_chemical_formula_moiety         'C72 H72 Fe4 O60, 0.5(H8 N2), 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H80 Cl4 Fe4 N O60'
_chemical_formula_weight         2308.59
_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'
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   27.2657(8)
_cell_length_b                   17.98779(19)
_cell_length_c                   15.0294(4)
_cell_angle_alpha                90
_cell_angle_beta                 133.512(5)
_cell_angle_gamma                90
_cell_volume                     5345.8(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    38132
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      30.6240
_cell_measurement_theta_min      1.7890
_shelx_estimated_absorpt_T_max   0.636
_shelx_estimated_absorpt_T_min   0.513
_exptl_absorpt_coefficient_mu    6.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.42.47a(Rigaku Oxford Diffraction, 2022)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2366
_exptl_crystal_preparation       'rocal laboratory'
_exptl_crystal_recrystallization_method 'vapor diffusion with poor solbent'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.082
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43615
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.490
_diffrn_reflns_theta_min         3.873
_diffrn_ambient_temperature      223.15
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                10626
_reflns_number_total             10810
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.437(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10810
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0823P)²+20.8647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1392
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.563(5)
 0.437(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1A
 1.07 with sigma of 0.02
 N1-H1B
 1.07 with sigma of 0.02
 N1-H1C
 1.07 with sigma of 0.02
 N1-H1D
 1.07 with sigma of 0.02
 C99-Cl1
 1.78 with sigma of 0.02
 C99-Cl2
 1.78 with sigma of 0.02
 C99A-Cl1A
 1.78 with sigma of 0.02
 C99A-Cl2A
 1.78 with sigma of 0.02
 H1A-H1B
 1.75 with sigma of 0.04
 H1A-H1C
 1.75 with sigma of 0.04
 H1A-H1D
 1.75 with sigma of 0.04
 H1B-H1C
 1.75 with sigma of 0.04
 H1B-H1D
 1.75 with sigma of 0.04
 H1C-H1D
 1.75 with sigma of 0.04
 Cl1-Cl2
 3.2 with sigma of 0.04
 C99-Cl1 \\sim C99A-Cl1A
 with sigma of 0.02
 C99-Cl2 \\sim C99A-Cl2A
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl2A
 with sigma of 0.04
 O8-C9 \\sim O8-C9A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C99 \\sim C99: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Uanis(O8) = Uanis(C9) = Uanis(C9A)
Uanis(C99) = Uanis(Cl1) = Uanis(Cl2)
Uanis(C99A) = Uanis(Cl1A) = Uanis(Cl2A)
5. Rigid body (RIGU) restrains
 Cl1, Cl2, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl2A)=Sof(Cl1A)=Sof(C99A)=Sof(H99C)=Sof(H99D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C99)=Sof(H99A)=Sof(H99B)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C99(H99A,H99B), C99A(H99C,H99D)
7.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C20(H20A,H20B,
 H20C), C2(H2A,H2B,H2C), C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C27(H27A,H27B,
 H27C), C32(H32A,H32B,H32C), C3(H3A,H3B,H3C), C15(H15A,H15B,H15C), C9(H9A,H9B,
 H9C), C9A(H9AA,H9AB,H9AC)
;
_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
Fe1 Fe 0.66337(4) 0.44024(4) 0.72177(7) 0.01525(17) Uani 1 1 d . . . . .
Fe2 Fe 0.50903(4) 0.68851(4) 0.29878(7) 0.01433(17) Uani 1 1 d . . . . .
O2 O 0.6580(3) 0.2615(3) 0.5417(5) 0.0419(12) Uani 1 1 d . . . . .
O27 O 0.3115(3) 0.3414(3) -0.0006(6) 0.0473(14) Uani 1 1 d . . . . .
O17 O 0.6361(3) 0.8683(3) 0.4837(5) 0.0455(13) Uani 1 1 d . . . . .
O9 O 0.7095(3) 0.7148(3) 0.6361(6) 0.0609(18) Uani 1 1 d . . . . .
O10 O 0.6444(2) 0.5019(2) 0.5951(4) 0.0254(8) Uani 1 1 d . . . . .
O6 O 0.7577(2) 0.4844(2) 0.8323(4) 0.0258(8) Uani 1 1 d . . . . .
O28 O 0.2814(3) 0.4580(3) -0.1496(5) 0.0526(15) Uani 1 1 d . . . . .
O5 O 0.5674(2) 0.4067(2) 0.6086(4) 0.0266(9) Uani 1 1 d . . . . .
O19 O 0.5933(4) 0.9525(3) 0.5765(6) 0.0597(16) Uani 1 1 d . . . . .
O13 O 0.7656(3) 0.6151(4) 0.5142(7) 0.067(2) Uani 1 1 d . . . . .
O8 O 0.8156(3) 0.6805(5) 0.7853(7) 0.098(3) Uani 1 1 d D . . . .
O25 O 0.44871(19) 0.6020(2) 0.2356(4) 0.0238(8) Uani 1 1 d . . . . .
O4 O 0.4636(3) 0.2489(4) 0.3299(5) 0.0559(16) Uani 1 1 d . . . . .
O29 O 0.3866(3) 0.5049(4) -0.0191(5) 0.0492(13) Uani 1 1 d . . . . .
O22 O 0.3292(2) 0.7606(2) -0.0420(4) 0.0321(10) Uani 1 1 d . . . . .
O3 O 0.5523(3) 0.1749(3) 0.4568(6) 0.0590(17) Uani 1 1 d . . . . .
O12 O 0.6383(3) 0.6236(3) 0.2553(5) 0.0412(12) Uani 1 1 d . . . . .
O1 O 0.6778(2) 0.3500(2) 0.6653(4) 0.0257(8) Uani 1 1 d . . . . .
O23 O 0.2510(3) 0.6403(3) -0.1678(4) 0.0474(14) Uani 1 1 d . . . . .
O16 O 0.5666(2) 0.7778(2) 0.3596(4) 0.0304(9) Uani 1 1 d . . . . .
O14 O 0.7331(4) 0.5027(4) 0.5069(9) 0.076(2) Uani 1 1 d . . . . .
O21 O 0.4330(2) 0.7353(2) 0.1349(4) 0.0256(8) Uani 1 1 d . . . . .
O20 O 0.4852(2) 0.7258(2) 0.3875(4) 0.0242(8) Uani 1 1 d . . . . .
O11 O 0.5536(2) 0.6547(2) 0.2397(4) 0.0260(8) Uani 1 1 d . . . . .
O18 O 0.6040(3) 0.8627(3) 0.6900(5) 0.0513(15) Uani 1 1 d . . . . .
O26 O 0.3082(2) 0.3802(2) 0.1352(4) 0.0279(9) Uani 1 1 d . . . . .
O7 O 0.8250(2) 0.5833(3) 0.9241(4) 0.0348(10) Uani 1 1 d . . . . .
O24 O 0.2372(3) 0.6039(3) -0.0443(5) 0.0480(13) Uani 1 1 d . . . . .
O15 O 0.57659(19) 0.6263(2) 0.4439(4) 0.0245(8) Uani 1 1 d . . . . .
O30 O 0.3625(2) 0.5193(2) 0.2286(4) 0.0244(8) Uani 1 1 d . . . . .
C26 C 0.3545(4) 0.8304(4) -0.0458(7) 0.0392(16) Uani 1 1 d . . . . .
H26A H 0.389241 0.849875 0.036775 0.059 Uiso 1 1 calc R U . . .
H26B H 0.317709 0.865881 -0.095974 0.059 Uiso 1 1 calc R U . . .
H26C H 0.373527 0.822053 -0.080688 0.059 Uiso 1 1 calc R U . . .
C21 C 0.6256(7) 0.9164(7) 0.7808(10) 0.076(3) Uani 1 1 d . . . . .
H21A H 0.658215 0.949638 0.794527 0.114 Uiso 1 1 calc R U . . .
H21B H 0.646237 0.891204 0.856821 0.114 Uiso 1 1 calc R U . . .
H21C H 0.586823 0.944760 0.752798 0.114 Uiso 1 1 calc R U . . .
C14 C 0.5972(5) 0.6457(6) 0.1297(8) 0.058(2) Uani 1 1 d . . . . .
H14A H 0.554166 0.619984 0.078447 0.087 Uiso 1 1 calc R U . . .
H14B H 0.620170 0.633226 0.103307 0.087 Uiso 1 1 calc R U . . .
H14C H 0.589588 0.698967 0.122536 0.087 Uiso 1 1 calc R U . . .
C18 C 0.6330(3) 0.6006(3) 0.4850(5) 0.0240(11) Uani 1 1 d . . . . .
C35 C 0.3380(3) 0.4649(3) 0.0573(6) 0.0276(12) Uani 1 1 d . . . . .
C24 C 0.5127(3) 0.7792(3) 0.4675(5) 0.0215(11) Uani 1 1 d . . . . .
C20 C 0.6686(6) 0.8563(6) 0.4371(11) 0.065(3) Uani 1 1 d . . . . .
H20A H 0.635677 0.864140 0.349063 0.097 Uiso 1 1 calc R U . . .
H20B H 0.685619 0.805779 0.455166 0.097 Uiso 1 1 calc R U . . .
H20C H 0.705717 0.890961 0.476372 0.097 Uiso 1 1 calc R U . . .
C2 C 0.7296(5) 0.2671(6) 0.6087(11) 0.070(3) Uani 1 1 d . . . . .
H2A H 0.755772 0.274780 0.695146 0.105 Uiso 1 1 calc R U . . .
H2B H 0.736536 0.308625 0.577170 0.105 Uiso 1 1 calc R U . . .
H2C H 0.744186 0.221491 0.598166 0.105 Uiso 1 1 calc R U . . .
C16 C 0.7206(4) 0.5672(4) 0.4849(7) 0.0348(15) Uani 1 1 d . . . . .
C36 C 0.3584(3) 0.5210(3) 0.1383(5) 0.0208(11) Uani 1 1 d . . . . .
C7 C 0.7718(3) 0.5497(4) 0.8258(6) 0.0263(12) Uani 1 1 d . . . . .
C28 C 0.2721(3) 0.6284(4) -0.0595(6) 0.0311(13) Uani 1 1 d . . . . .
C33 C 0.2794(7) 0.4668(6) -0.2496(9) 0.077(4) Uani 1 1 d . . . . .
H33A H 0.280241 0.519280 -0.263339 0.115 Uiso 1 1 calc R U . . .
H33B H 0.238239 0.444605 -0.323953 0.115 Uiso 1 1 calc R U . . .
H33C H 0.318282 0.442368 -0.227202 0.115 Uiso 1 1 calc R U . . .
C8 C 0.8667(4) 0.5431(5) 1.0393(6) 0.0409(16) Uani 1 1 d . . . . .
H8A H 0.881576 0.496716 1.031390 0.061 Uiso 1 1 calc R U . . .
H8B H 0.840722 0.532730 1.060114 0.061 Uiso 1 1 calc R U . . .
H8C H 0.905844 0.573027 1.103496 0.061 Uiso 1 1 calc R U . . .
C25 C 0.3725(3) 0.7161(3) 0.0498(5) 0.0235(11) Uani 1 1 d . . . . .
C10 C 0.7508(4) 0.6687(4) 0.7085(7) 0.0410(17) Uani 1 1 d . . . . .
C4 C 0.5220(3) 0.2407(4) 0.4220(6) 0.0366(15) Uani 1 1 d . . . . .
C5 C 0.5662(3) 0.3006(3) 0.5146(6) 0.0271(12) Uani 1 1 d . . . . .
C27 C 0.1789(5) 0.6251(6) -0.2721(7) 0.068(3) Uani 1 1 d . . . . .
H27A H 0.171380 0.571818 -0.282131 0.102 Uiso 1 1 calc R U . . .
H27B H 0.164775 0.646231 -0.346064 0.102 Uiso 1 1 calc R U . . .
H27C H 0.152750 0.647265 -0.256892 0.102 Uiso 1 1 calc R U . . .
C11 C 0.7319(3) 0.5922(4) 0.7139(6) 0.0288(12) Uani 1 1 d . . . . .
C22 C 0.5869(4) 0.8896(4) 0.5888(7) 0.0345(14) Uani 1 1 d . . . . .
C23 C 0.5600(3) 0.8287(3) 0.4966(6) 0.0274(12) Uani 1 1 d . . . . .
C19 C 0.5864(3) 0.8230(4) 0.4408(6) 0.0312(13) Uani 1 1 d . . . . .
C6 C 0.5377(3) 0.3515(3) 0.5358(5) 0.0236(11) Uani 1 1 d . . . . .
C13 C 0.6121(3) 0.6289(3) 0.3023(6) 0.0262(12) Uani 1 1 d . . . . .
C32 C 0.2965(7) 0.2669(4) 0.0133(11) 0.066(3) Uani 1 1 d . . . . .
H32A H 0.296370 0.232249 -0.036371 0.099 Uiso 1 1 calc R U . . .
H32B H 0.252451 0.266661 -0.013302 0.099 Uiso 1 1 calc R U . . .
H32C H 0.330695 0.252048 0.098736 0.099 Uiso 1 1 calc R U . . .
C31 C 0.3181(3) 0.3944(3) 0.0669(6) 0.0277(12) Uani 1 1 d . . . . .
C34 C 0.3395(4) 0.4772(4) -0.0393(7) 0.0352(14) Uani 1 1 d . . . . .
C3 C 0.5110(5) 0.1144(5) 0.3712(11) 0.082(4) Uani 1 1 d . . . . .
H3A H 0.535754 0.068020 0.407343 0.123 Uiso 1 1 calc R U . . .
H3B H 0.500412 0.123557 0.295912 0.123 Uiso 1 1 calc R U . . .
H3C H 0.469474 0.111226 0.353358 0.123 Uiso 1 1 calc R U . . .
C12 C 0.6732(3) 0.5618(3) 0.6070(6) 0.0246(11) Uani 1 1 d . . . . .
C17 C 0.6546(3) 0.6018(3) 0.4252(6) 0.0269(12) Uani 1 1 d . . . . .
C29 C 0.3447(3) 0.6463(3) 0.0442(5) 0.0224(11) Uani 1 1 d . . . . .
C30 C 0.3858(3) 0.5953(3) 0.1381(5) 0.0211(11) Uani 1 1 d . . . . .
C15 C 0.8316(5) 0.5864(8) 0.5747(13) 0.087(4) Uani 1 1 d . . . . .
H15A H 0.851132 0.562867 0.651202 0.130 Uiso 1 1 calc R U . . .
H15B H 0.860486 0.626803 0.591464 0.130 Uiso 1 1 calc R U . . .
H15C H 0.827428 0.550100 0.522087 0.130 Uiso 1 1 calc R U . . .
C1 C 0.6364(3) 0.3060(3) 0.5785(6) 0.0252(12) Uani 1 1 d . . . . .
C9 C 0.8271(14) 0.7630(12) 0.788(2) 0.098(3) Uani 0.62(5) 1 d D . P A 2
H9A H 0.799154 0.781226 0.704687 0.147 Uiso 0.62(5) 1 calc R U P A 2
H9B H 0.874357 0.771999 0.833209 0.147 Uiso 0.62(5) 1 calc R U P A 2
H9C H 0.815249 0.788704 0.827646 0.147 Uiso 0.62(5) 1 calc R U P A 2
N1 N 0.500000 0.5620(4) 0.500000 0.0330(16) Uani 1 2 d DS T P . .
H1A H 0.526(6) 0.550(6) 0.593(4) 0.040 Uiso 0.5 1 d D U P B -1
H1B H 0.478(5) 0.616(3) 0.478(10) 0.040 Uiso 0.5 1 d D U P C -1
H1C H 0.462(4) 0.522(5) 0.439(9) 0.040 Uiso 0.5 1 d D U P D -1
H1D H 0.536(5) 0.564(6) 0.493(12) 0.040 Uiso 0.5 1 d D U P E -1
Cl1 Cl 0.4991(9) 0.3725(11) 0.2344(18) 0.257(7) Uani 0.691(13) 1 d D . P F 1
Cl2 Cl 0.5608(9) 0.4432(11) 0.1621(17) 0.257(7) Uani 0.691(13) 1 d D . P F 1
C99 C 0.5791(17) 0.404(4) 0.291(3) 0.257(7) Uani 0.691(13) 1 d D . P F 1
H99A H 0.599146 0.441295 0.355757 0.309 Uiso 0.691(13) 1 calc R U P F 1
H99B H 0.610722 0.362247 0.324869 0.309 Uiso 0.691(13) 1 calc R U P F 1
Cl2A Cl 0.5953(11) 0.4159(14) 0.3218(17) 0.145(7) Uani 0.309(13) 1 d D . P F 2
Cl1A Cl 0.4866(9) 0.3262(11) 0.1362(16) 0.145(7) Uani 0.309(13) 1 d D . P F 2
C99A C 0.5099(19) 0.4218(17) 0.182(5) 0.145(7) Uani 0.309(13) 1 d D . P F 2
H99C H 0.505159 0.450522 0.121090 0.174 Uiso 0.309(13) 1 calc R U P F 2
H99D H 0.482131 0.444847 0.193915 0.174 Uiso 0.309(13) 1 calc R U P F 2
C9A C 0.850(2) 0.743(3) 0.785(4) 0.098(3) Uani 0.38(5) 1 d D . P A 3
H9AA H 0.826262 0.756404 0.701104 0.147 Uiso 0.38(5) 1 calc R U P A 3
H9AB H 0.896191 0.728988 0.828030 0.147 Uiso 0.38(5) 1 calc R U P A 3
H9AC H 0.850821 0.785500 0.825861 0.147 Uiso 0.38(5) 1 calc R U P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O10 1.940(4) . ?
Fe1 O6 2.032(4) . ?
Fe1 O5 1.994(4) . ?
Fe1 O1 1.992(4) . ?
Fe1 O26 2.024(4) 2_656 ?
Fe1 O30 1.948(4) 2_656 ?
Fe2 O25 1.969(4) . ?
Fe2 O16 1.975(4) . ?
Fe2 O21 2.010(4) . ?
Fe2 O20 1.962(4) . ?
Fe2 O11 2.031(4) . ?
Fe2 O15 1.968(4) . ?
O2 C2 1.460(9) . ?
O2 C1 1.320(8) . ?
O27 C32 1.458(9) . ?
O27 C31 1.311(8) . ?
O17 C20 1.473(10) . ?
O17 C19 1.310(8) . ?
O9 C10 1.205(9) . ?
O10 C12 1.272(8) . ?
O6 C7 1.259(8) . ?
O28 C33 1.472(10) . ?
O28 C34 1.326(9) . ?
O5 C6 1.273(7) . ?
O19 C22 1.177(10) . ?
O13 C16 1.304(9) . ?
O13 C15 1.441(10) . ?
O8 C10 1.300(10) . ?
O8 C9 1.512(18) . ?
O8 C9A 1.47(2) . ?
O25 C30 1.281(7) . ?
O4 C4 1.199(9) . ?
O29 C34 1.205(9) . ?
O22 C26 1.453(7) . ?
O22 C25 1.303(7) . ?
O3 C4 1.327(9) . ?
O3 C3 1.453(10) . ?
O12 C14 1.437(9) . ?
O12 C13 1.309(7) . ?
O1 C1 1.255(7) . ?
O23 C28 1.317(9) . ?
O23 C27 1.467(9) . ?
O16 C19 1.240(8) . ?
O14 C16 1.191(10) . ?
O21 C25 1.253(7) . ?
O20 C24 1.299(7) . ?
O11 C13 1.257(8) . ?
O18 C21 1.427(10) . ?
O18 C22 1.337(9) . ?
O26 C31 1.254(8) . ?
O7 C7 1.304(8) . ?
O7 C8 1.449(8) . ?
O24 C28 1.206(9) . ?
O15 C18 1.284(7) . ?
O30 C36 1.285(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C18 C12 1.510(8) . ?
C18 C17 1.373(9) . ?
C35 C36 1.370(8) . ?
C35 C31 1.424(8) . ?
C35 C34 1.497(9) . ?
C24 C24 1.540(11) 2_656 ?
C24 C23 1.368(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C16 C17 1.485(8) . ?
C36 C30 1.531(7) . ?
C7 C11 1.441(8) . ?
C28 C29 1.484(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C25 C29 1.437(8) . ?
C10 C11 1.492(9) . ?
C4 C5 1.497(9) . ?
C5 C6 1.372(8) . ?
C5 C1 1.435(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C11 C12 1.379(9) . ?
C22 C23 1.503(9) . ?
C23 C19 1.434(9) . ?
C6 C6 1.529(12) 2_656 ?
C13 C17 1.430(8) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C29 C30 1.384(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
N1 H1A 1.07(3) . ?
N1 H1B 1.07(3) . ?
N1 H1C 1.06(3) . ?
N1 H1D 1.08(3) . ?
Cl1 C99 1.80(2) . ?
Cl2 C99 1.78(2) . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
Cl2A C99A 1.76(2) . ?
Cl1A C99A 1.80(2) . ?
C99A H99C 0.9800 . ?
C99A H99D 0.9800 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A H9AC 0.9700 . ?

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
O10 Fe1 O6 84.89(17) . . ?
O10 Fe1 O5 91.65(18) . . ?
O10 Fe1 O1 92.56(18) . . ?
O10 Fe1 O26 174.72(19) . 2_656 ?
O10 Fe1 O30 92.08(18) . 2_656 ?
O5 Fe1 O6 174.57(18) . . ?
O5 Fe1 O26 93.59(18) . 2_656 ?
O1 Fe1 O6 99.01(17) . . ?
O1 Fe1 O5 85.30(17) . . ?
O1 Fe1 O26 88.55(17) . 2_656 ?
O26 Fe1 O6 89.84(18) 2_656 . ?
O30 Fe1 O6 89.44(18) 2_656 . ?
O30 Fe1 O5 86.50(17) 2_656 . ?
O30 Fe1 O1 170.69(18) 2_656 . ?
O30 Fe1 O26 87.56(17) 2_656 2_656 ?
O25 Fe2 O16 177.80(19) . . ?
O25 Fe2 O21 85.71(16) . . ?
O25 Fe2 O11 96.07(18) . . ?
O16 Fe2 O21 92.73(18) . . ?
O16 Fe2 O11 85.50(18) . . ?
O21 Fe2 O11 90.70(17) . . ?
O20 Fe2 O25 92.29(17) . . ?
O20 Fe2 O16 86.39(17) . . ?
O20 Fe2 O21 98.32(18) . . ?
O20 Fe2 O11 168.13(17) . . ?
O20 Fe2 O15 86.36(17) . . ?
O15 Fe2 O25 85.31(17) . . ?
O15 Fe2 O16 96.35(19) . . ?
O15 Fe2 O21 170.03(18) . . ?
O15 Fe2 O11 85.95(17) . . ?
C1 O2 C2 116.2(6) . . ?
C31 O27 C32 117.5(6) . . ?
C19 O17 C20 115.7(6) . . ?
C12 O10 Fe1 128.6(4) . . ?
C7 O6 Fe1 125.7(4) . . ?
C34 O28 C33 114.9(7) . . ?
C6 O5 Fe1 130.9(4) . . ?
C16 O13 C15 116.9(8) . . ?
C10 O8 C9 108.2(13) . . ?
C10 O8 C9A 127.1(19) . . ?
C30 O25 Fe2 129.9(4) . . ?
C25 O22 C26 117.7(5) . . ?
C4 O3 C3 115.3(6) . . ?
C13 O12 C14 117.8(5) . . ?
C1 O1 Fe1 131.0(4) . . ?
C28 O23 C27 114.5(7) . . ?
C19 O16 Fe2 131.1(4) . . ?
C25 O21 Fe2 131.1(4) . . ?
C24 O20 Fe2 129.1(4) . . ?
C13 O11 Fe2 128.1(4) . . ?
C22 O18 C21 115.7(7) . . ?
C31 O26 Fe1 128.3(4) . 2_656 ?
C7 O7 C8 118.0(5) . . ?
C18 O15 Fe2 129.4(4) . . ?
C36 O30 Fe1 129.2(4) . 2_656 ?
O22 C26 H26A 109.5 . . ?
O22 C26 H26B 109.5 . . ?
O22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O18 C21 H21A 109.5 . . ?
O18 C21 H21B 109.5 . . ?
O18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
O12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O15 C18 C12 112.2(5) . . ?
O15 C18 C17 126.2(5) . . ?
C17 C18 C12 121.5(5) . . ?
C36 C35 C31 121.1(6) . . ?
C36 C35 C34 119.1(5) . . ?
C31 C35 C34 119.7(5) . . ?
O20 C24 C24 111.1(4) . 2_656 ?
O20 C24 C23 126.5(5) . . ?
C23 C24 C24 122.3(5) . 2_656 ?
O17 C20 H20A 109.5 . . ?
O17 C20 H20B 109.5 . . ?
O17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O13 C16 C17 113.2(6) . . ?
O14 C16 O13 121.8(7) . . ?
O14 C16 C17 125.0(7) . . ?
O30 C36 C35 127.4(5) . . ?
O30 C36 C30 109.6(5) . . ?
C35 C36 C30 122.8(5) . . ?
O6 C7 O7 120.2(5) . . ?
O6 C7 C11 124.1(6) . . ?
O7 C7 C11 115.7(6) . . ?
O23 C28 C29 113.3(6) . . ?
O24 C28 O23 124.2(6) . . ?
O24 C28 C29 122.5(6) . . ?
O28 C33 H33A 109.5 . . ?
O28 C33 H33B 109.5 . . ?
O28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O7 C8 H8A 109.5 . . ?
O7 C8 H8B 109.5 . . ?
O7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O22 C25 C29 114.7(5) . . ?
O21 C25 O22 120.5(5) . . ?
O21 C25 C29 124.8(5) . . ?
O9 C10 O8 123.0(7) . . ?
O9 C10 C11 122.7(7) . . ?
O8 C10 C11 114.3(7) . . ?
O4 C4 O3 122.4(7) . . ?
O4 C4 C5 124.4(7) . . ?
O3 C4 C5 113.0(6) . . ?
C6 C5 C4 118.2(6) . . ?
C6 C5 C1 120.5(6) . . ?
C1 C5 C4 121.3(5) . . ?
O23 C27 H27A 109.5 . . ?
O23 C27 H27B 109.5 . . ?
O23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C7 C11 C10 122.8(6) . . ?
C12 C11 C7 119.1(6) . . ?
C12 C11 C10 118.0(6) . . ?
O19 C22 O18 123.6(7) . . ?
O19 C22 C23 125.8(7) . . ?
O18 C22 C23 110.6(6) . . ?
C24 C23 C22 121.5(6) . . ?
C24 C23 C19 120.5(6) . . ?
C19 C23 C22 118.0(6) . . ?
O17 C19 C23 115.8(6) . . ?
O16 C19 O17 119.5(6) . . ?
O16 C19 C23 124.7(6) . . ?
O5 C6 C5 126.4(6) . . ?
O5 C6 C6 110.9(4) . 2_656 ?
C5 C6 C6 122.6(5) . 2_656 ?
O12 C13 C17 114.5(5) . . ?
O11 C13 O12 120.4(5) . . ?
O11 C13 C17 125.1(5) . . ?
O27 C32 H32A 109.5 . . ?
O27 C32 H32B 109.5 . . ?
O27 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O27 C31 C35 115.4(6) . . ?
O26 C31 O27 119.5(6) . . ?
O26 C31 C35 125.1(5) . . ?
O28 C34 C35 111.6(6) . . ?
O29 C34 O28 124.7(6) . . ?
O29 C34 C35 123.5(7) . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O10 C12 C18 111.0(5) . . ?
O10 C12 C11 127.5(6) . . ?
C11 C12 C18 121.4(5) . . ?
C18 C17 C16 119.0(5) . . ?
C18 C17 C13 121.4(6) . . ?
C13 C17 C16 119.3(6) . . ?
C25 C29 C28 121.3(5) . . ?
C30 C29 C28 119.0(5) . . ?
C30 C29 C25 119.7(5) . . ?
O25 C30 C36 110.5(5) . . ?
O25 C30 C29 127.6(5) . . ?
C29 C30 C36 121.8(5) . . ?
O13 C15 H15A 109.5 . . ?
O13 C15 H15B 109.5 . . ?
O13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 C1 C5 116.9(5) . . ?
O1 C1 O2 118.4(5) . . ?
O1 C1 C5 124.7(5) . . ?
O8 C9 H9A 109.5 . . ?
O8 C9 H9B 109.5 . . ?
O8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H1A N1 H1B 109(5) . . ?
H1A N1 H1C 112(5) . . ?
H1A N1 H1D 108(5) . . ?
H1B N1 H1C 110(5) . . ?
H1B N1 H1D 108(5) . . ?
H1C N1 H1D 110(5) . . ?
Cl1 C99 H99A 110.6 . . ?
Cl1 C99 H99B 110.6 . . ?
Cl2 C99 Cl1 105.5(17) . . ?
Cl2 C99 H99A 110.6 . . ?
Cl2 C99 H99B 110.6 . . ?
H99A C99 H99B 108.8 . . ?
Cl2A C99A Cl1A 103.1(17) . . ?
Cl2A C99A H99C 111.1 . . ?
Cl2A C99A H99D 111.1 . . ?
Cl1A C99A H99C 111.1 . . ?
Cl1A C99A H99D 111.1 . . ?
H99C C99A H99D 109.1 . . ?
O8 C9A H9AA 109.5 . . ?
O8 C9A H9AB 109.5 . . ?
O8 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 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
Fe1 O10 C12 C18 -167.2(4) . . . . ?
Fe1 O10 C12 C11 10.7(9) . . . . ?
Fe1 O6 C7 O7 150.0(5) . . . . ?
Fe1 O6 C7 C11 -29.4(9) . . . . ?
Fe1 O5 C6 C5 -2.2(9) . . . . ?
Fe1 O5 C6 C6 -177.7(4) . . . 2_656 ?
Fe1 O1 C1 O2 163.4(4) . . . . ?
Fe1 O1 C1 C5 -15.9(9) . . . . ?
Fe1 O26 C31 O27 163.0(5) 2_656 . . . ?
Fe1 O26 C31 C35 -15.6(9) 2_656 . . . ?
Fe1 O30 C36 C35 -4.1(9) 2_656 . . . ?
Fe1 O30 C36 C30 -179.5(3) 2_656 . . . ?
Fe2 O25 C30 C36 -171.3(4) . . . . ?
Fe2 O25 C30 C29 6.6(9) . . . . ?
Fe2 O16 C19 O17 164.8(5) . . . . ?
Fe2 O16 C19 C23 -13.0(10) . . . . ?
Fe2 O21 C25 O22 170.1(4) . . . . ?
Fe2 O21 C25 C29 -9.2(9) . . . . ?
Fe2 O20 C24 C24 -168.6(4) . . . 2_656 ?
Fe2 O20 C24 C23 9.2(9) . . . . ?
Fe2 O11 C13 O12 -166.2(5) . . . . ?
Fe2 O11 C13 C17 15.2(9) . . . . ?
Fe2 O15 C18 C12 174.0(4) . . . . ?
Fe2 O15 C18 C17 -10.6(9) . . . . ?
O9 C10 C11 C7 -149.8(8) . . . . ?
O9 C10 C11 C12 29.6(11) . . . . ?
O6 C7 C11 C10 -178.3(6) . . . . ?
O6 C7 C11 C12 2.4(10) . . . . ?
O19 C22 C23 C24 -133.7(8) . . . . ?
O19 C22 C23 C19 47.3(11) . . . . ?
O13 C16 C17 C18 -114.0(7) . . . . ?
O13 C16 C17 C13 72.2(9) . . . . ?
O8 C10 C11 C7 32.5(11) . . . . ?
O8 C10 C11 C12 -148.1(8) . . . . ?
O4 C4 C5 C6 35.1(11) . . . . ?
O4 C4 C5 C1 -143.8(8) . . . . ?
O22 C25 C29 C28 -0.1(8) . . . . ?
O22 C25 C29 C30 -178.7(5) . . . . ?
O3 C4 C5 C6 -139.5(7) . . . . ?
O3 C4 C5 C1 41.5(10) . . . . ?
O12 C13 C17 C18 -177.1(6) . . . . ?
O12 C13 C17 C16 -3.4(9) . . . . ?
O23 C28 C29 C25 49.7(8) . . . . ?
O23 C28 C29 C30 -131.8(6) . . . . ?
O14 C16 C17 C18 64.8(11) . . . . ?
O14 C16 C17 C13 -109.0(9) . . . . ?
O21 C25 C29 C28 179.3(6) . . . . ?
O21 C25 C29 C30 0.7(9) . . . . ?
O20 C24 C23 C22 178.4(6) . . . . ?
O20 C24 C23 C19 -2.6(10) . . . . ?
O11 C13 C17 C18 1.5(10) . . . . ?
O11 C13 C17 C16 175.2(6) . . . . ?
O18 C22 C23 C24 47.3(9) . . . . ?
O18 C22 C23 C19 -131.7(7) . . . . ?
O7 C7 C11 C10 2.3(10) . . . . ?
O7 C7 C11 C12 -177.1(6) . . . . ?
O24 C28 C29 C25 -131.9(7) . . . . ?
O24 C28 C29 C30 46.7(9) . . . . ?
O15 C18 C12 O10 68.5(6) . . . . ?
O15 C18 C12 C11 -109.6(6) . . . . ?
O15 C18 C17 C16 -178.0(6) . . . . ?
O15 C18 C17 C13 -4.3(10) . . . . ?
O30 C36 C30 O25 63.1(6) . . . . ?
O30 C36 C30 C29 -115.0(6) . . . . ?
C26 O22 C25 O21 4.0(9) . . . . ?
C26 O22 C25 C29 -176.6(6) . . . . ?
C21 O18 C22 O19 5.4(12) . . . . ?
C21 O18 C22 C23 -175.5(8) . . . . ?
C14 O12 C13 O11 -2.1(10) . . . . ?
C14 O12 C13 C17 176.6(7) . . . . ?
C35 C36 C30 O25 -112.5(6) . . . . ?
C35 C36 C30 C29 69.4(8) . . . . ?
C24 C24 C23 C22 -4.0(10) 2_656 . . . ?
C24 C24 C23 C19 174.9(6) 2_656 . . . ?
C24 C23 C19 O17 -173.5(6) . . . . ?
C24 C23 C19 O16 4.5(11) . . . . ?
C20 O17 C19 O16 -5.2(11) . . . . ?
C20 O17 C19 C23 172.9(8) . . . . ?
C2 O2 C1 O1 1.3(10) . . . . ?
C2 O2 C1 C5 -179.3(8) . . . . ?
C36 C35 C31 O27 -168.1(6) . . . . ?
C36 C35 C31 O26 10.5(10) . . . . ?
C36 C35 C34 O28 -130.6(7) . . . . ?
C36 C35 C34 O29 45.6(10) . . . . ?
C7 C11 C12 O10 8.3(10) . . . . ?
C7 C11 C12 C18 -174.0(6) . . . . ?
C28 C29 C30 O25 -178.0(6) . . . . ?
C28 C29 C30 C36 -0.2(8) . . . . ?
C33 O28 C34 O29 5.3(12) . . . . ?
C33 O28 C34 C35 -178.7(7) . . . . ?
C8 O7 C7 O6 0.2(9) . . . . ?
C8 O7 C7 C11 179.7(6) . . . . ?
C25 C29 C30 O25 0.6(9) . . . . ?
C25 C29 C30 C36 178.4(5) . . . . ?
C10 C11 C12 O10 -171.1(6) . . . . ?
C10 C11 C12 C18 6.6(9) . . . . ?
C4 C5 C6 O5 -178.1(6) . . . . ?
C4 C5 C6 C6 -3.1(9) . . . 2_656 ?
C4 C5 C1 O2 7.9(9) . . . . ?
C4 C5 C1 O1 -172.8(6) . . . . ?
C27 O23 C28 O24 3.3(11) . . . . ?
C27 O23 C28 C29 -178.3(7) . . . . ?
C22 C23 C19 O17 5.5(9) . . . . ?
C22 C23 C19 O16 -176.5(7) . . . . ?
C6 C5 C1 O2 -171.1(6) . . . . ?
C6 C5 C1 O1 8.2(9) . . . . ?
C32 O27 C31 O26 -3.5(11) . . . . ?
C32 O27 C31 C35 175.2(8) . . . . ?
C31 C35 C36 O30 -0.2(10) . . . . ?
C31 C35 C36 C30 174.7(5) . . . . ?
C31 C35 C34 O28 52.0(9) . . . . ?
C31 C35 C34 O29 -131.8(8) . . . . ?
C34 C35 C36 O30 -177.5(6) . . . . ?
C34 C35 C36 C30 -2.7(9) . . . . ?
C34 C35 C31 O27 9.2(9) . . . . ?
C34 C35 C31 O26 -172.1(6) . . . . ?
C3 O3 C4 O4 4.1(14) . . . . ?
C3 O3 C4 C5 178.8(9) . . . . ?
C12 C18 C17 C16 -2.9(9) . . . . ?
C12 C18 C17 C13 170.7(5) . . . . ?
C17 C18 C12 O10 -107.2(6) . . . . ?
C17 C18 C12 C11 74.7(8) . . . . ?
C15 O13 C16 O14 0.0(14) . . . . ?
C15 O13 C16 C17 178.9(9) . . . . ?
C1 C5 C6 O5 0.9(10) . . . . ?
C1 C5 C6 C6 175.8(6) . . . 2_656 ?
C9 O8 C10 O9 14(2) . . . . ?
C9 O8 C10 C11 -168.6(16) . . . . ?
C9A O8 C10 O9 -12(4) . . . . ?
C9A O8 C10 C11 166(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.531 0.000 359.7 159.8 '4 CH2Cl2'
2 0.158 0.196 0.756 17.9 0.0 ?
3 0.500 0.031 0.000 359.7 159.8 '4 CH2Cl2'
4 0.342 0.696 0.244 17.9 0.0 ?
5 0.658 0.696 0.756 17.9 0.0 ?
6 0.842 0.196 0.244 17.9 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.563(5)
2 0.437(5)
####################################################################### 
# 
# 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_1-ch2br2
_database_code_depnum_ccdc_archive 'CCDC 2281391'
loop_
_audit_author_name
_audit_author_address
'ryo tsunashima' 'yamaguchi university'
_audit_update_record             
;
2023-07-24 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_audit_creation_date             2023-07-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[NH4<C72H72O60Fe4](CH2Br2)2'
_chemical_formula_moiety         
'C72 H72 Fe4 O60, 0.5(H8 N2), 2(C H2 Br2), [+ solvents]1.8[CH2Br2]'
_chemical_formula_sum            'C74 H80 Br4 Fe4 N O60'
_chemical_formula_weight         2486.43
_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 0.0033 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   27.2902(13)
_cell_length_b                   17.9198(3)
_cell_length_c                   15.0346(7)
_cell_angle_alpha                90
_cell_angle_beta                 133.441(9)
_cell_angle_gamma                90
_cell_volume                     5338.5(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17632
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      30.7100
_cell_measurement_theta_min      2.0630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2510
_exptl_crystal_preparation       'local laboratory'
_exptl_crystal_recrystallization_method 
'vapor difusion from dibromomethane and hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25043
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.694
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.491
_diffrn_reflns_theta_min         1.786
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00  29.00   0.50  317.14    --   -9.35  96.00  68.00  152
  2  ω    -28.00  29.00   0.50  317.14    --   10.05  96.00  68.00  114
  3  ω    -16.00  48.00   0.50  317.14    --   10.05 -96.00 -40.00  128
  4  ω    -17.00  47.00   0.50  317.14    --   10.05 -99.00 -90.00  128
  5  ω    -13.00  48.00   0.50  317.14    --   10.05 -99.00-150.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_diffrn_special_details          'Dibromomethane was disordered'
_reflns_Friedel_coverage         0.671
_reflns_Friedel_fraction_full    0.800
_reflns_Friedel_fraction_max     0.574
_reflns_number_gt                10442
_reflns_number_total             11309
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.526
_refine_diff_density_min         -2.297
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11309
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0709
_refine_ls_restrained_S_all      1.063
_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)+(0.1676P)²+6.0761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2038
_refine_ls_wR_factor_ref         0.2077
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.61(2)
 0.39(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1A
 1.065 with sigma of 0.02
 N1-H1D
 1.065 with sigma of 0.02
 N1-H1B
 1.065 with sigma of 0.02
 N1-H1C
 1.065 with sigma of 0.02
 C99-Br1
 1.96 with sigma of 0.02
 C99-Br2
 1.96 with sigma of 0.02
 H1A-H1D
 1.75 with sigma of 0.04
 H1A-H1B
 1.75 with sigma of 0.04
 H1A-H1C
 1.75 with sigma of 0.04
 H1D-H1B
 1.75 with sigma of 0.04
 H1D-H1C
 1.75 with sigma of 0.04
 H1B-H1C
 1.75 with sigma of 0.04
 Br1-Br2
 3.52 with sigma of 0.04
 O13-C15 \\sim O13-C15A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C99) = Uanis(Br1) = Uanis(Br2)
Uiso(H1A) = Uiso(H1B) = Uiso(H1D) = Uiso(H1C)
Uanis(C9) = Uanis(O8)
Uanis(O13) = Uanis(C15) = Uanis(C15A)
5. Others
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C99(H99A,H99B)
6.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C3(H3A,H3B,H3C), C33(H33A,H33B,
 H33C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C8(H8A,
 H8B,H8C), C32(H32A,H32B,H32C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C15(H15A,H15B,
 H15C), C15A(H15D,H15E,H15F)
;
_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
Fe1 Fe 0.66308(4) 0.53255(4) 0.72161(7) 0.01870(19) Uani 1 1 d . . . . .
Fe2 Fe 0.50906(4) 0.78217(4) 0.29894(7) 0.01773(19) Uani 1 1 d . . . . .
O17 O 0.6379(3) 0.9611(3) 0.4871(5) 0.0394(13) Uani 1 1 d . . . . .
O25 O 0.4487(2) 0.6961(2) 0.2355(4) 0.0242(9) Uani 1 1 d . . . . .
O21 O 0.4329(2) 0.8291(3) 0.1347(4) 0.0253(9) Uani 1 1 d . . . . .
O16 O 0.5666(3) 0.8729(3) 0.3599(4) 0.0268(9) Uani 1 1 d . . . . .
O30 O 0.3618(2) 0.6121(2) 0.2271(4) 0.0212(8) Uani 1 1 d . . . . .
O24 O 0.2381(3) 0.6964(4) -0.0411(6) 0.0500(16) Uani 1 1 d . . . . .
O19 O 0.5944(5) 1.0476(4) 0.5774(8) 0.064(2) Uani 1 1 d . . . . .
O20 O 0.4847(2) 0.8207(2) 0.3872(4) 0.0216(8) Uani 1 1 d . . . . .
O23 O 0.2503(3) 0.7348(4) -0.1675(5) 0.0473(16) Uani 1 1 d . . . . .
O1 O 0.6776(2) 0.4434(2) 0.6650(4) 0.0237(8) Uani 1 1 d . . . . .
O28 O 0.2813(4) 0.5515(4) -0.1501(5) 0.0538(18) Uani 1 1 d . . . . .
O29 O 0.3861(4) 0.5989(4) -0.0208(6) 0.0489(15) Uani 1 1 d . . . . .
O15 O 0.5769(2) 0.7196(3) 0.4446(4) 0.0241(9) Uani 1 1 d . . . . .
O2 O 0.6583(3) 0.3541(3) 0.5419(5) 0.0387(12) Uani 1 1 d . . . . .
O7 O 0.8243(3) 0.6769(3) 0.9210(4) 0.0339(11) Uani 1 1 d . . . . .
O18 O 0.6027(4) 0.9572(4) 0.6893(6) 0.0530(18) Uani 1 1 d . . . . .
O9 O 0.7098(4) 0.8077(4) 0.6362(7) 0.0555(18) Uani 1 1 d . . . . .
O3 O 0.5522(3) 0.2669(3) 0.4580(7) 0.0539(18) Uani 1 1 d . . . . .
O10 O 0.6432(2) 0.5949(3) 0.5946(4) 0.0227(8) Uani 1 1 d . . . . .
O22 O 0.3303(2) 0.8553(3) -0.0420(4) 0.0311(11) Uani 1 1 d . . . . .
O11 O 0.5538(2) 0.7493(3) 0.2396(4) 0.0259(9) Uani 1 1 d . . . . .
O4 O 0.4637(3) 0.3417(4) 0.3307(6) 0.058(2) Uani 1 1 d . . . . .
O12 O 0.6378(3) 0.7175(4) 0.2539(5) 0.0398(13) Uani 1 1 d . . . . .
O26 O 0.3087(3) 0.4729(3) 0.1353(4) 0.0280(9) Uani 1 1 d . . . . .
O13 O 0.7646(3) 0.7099(5) 0.5136(9) 0.073(2) Uani 1 1 d D . . . .
O5 O 0.5674(2) 0.4997(3) 0.6095(4) 0.0239(8) Uani 1 1 d . . . . .
O14 O 0.7329(4) 0.5949(5) 0.5058(10) 0.072(2) Uani 1 1 d . . . . .
O8 O 0.8164(5) 0.7686(7) 0.7796(9) 0.106(4) Uani 1 1 d . . . . .
O6 O 0.7566(2) 0.5779(3) 0.8312(4) 0.0259(9) Uani 1 1 d . . . . .
O27 O 0.3111(4) 0.4351(3) -0.0012(6) 0.0453(15) Uani 1 1 d . . . . .
C5 C 0.5668(4) 0.3929(4) 0.5150(6) 0.0286(13) Uani 1 1 d . . . . .
C21 C 0.6235(8) 1.0150(7) 0.7774(11) 0.075(4) Uani 1 1 d . . . . .
H21A H 0.669000 1.031065 0.819847 0.113 Uiso 1 1 calc R U . . .
H21B H 0.622495 0.995341 0.836171 0.113 Uiso 1 1 calc R U . . .
H21C H 0.592978 1.057122 0.734798 0.113 Uiso 1 1 calc R U . . .
C29 C 0.3462(3) 0.7401(3) 0.0470(5) 0.0222(11) Uani 1 1 d . . . . .
C14 C 0.5956(6) 0.7419(7) 0.1271(9) 0.054(3) Uani 1 1 d . . . . .
H14A H 0.553570 0.714140 0.075090 0.081 Uiso 1 1 calc R U . . .
H14B H 0.619083 0.733024 0.100838 0.081 Uiso 1 1 calc R U . . .
H14C H 0.586069 0.794765 0.121209 0.081 Uiso 1 1 calc R U . . .
C3 C 0.5111(5) 0.2062(7) 0.3740(12) 0.074(4) Uani 1 1 d . . . . .
H3A H 0.511115 0.206721 0.309510 0.110 Uiso 1 1 calc R U . . .
H3B H 0.465286 0.212094 0.338395 0.110 Uiso 1 1 calc R U . . .
H3C H 0.529330 0.159197 0.417774 0.110 Uiso 1 1 calc R U . . .
C19 C 0.5866(4) 0.9162(4) 0.4410(6) 0.0287(13) Uani 1 1 d . . . . .
C17 C 0.6536(4) 0.6948(4) 0.4235(6) 0.0285(13) Uani 1 1 d . . . . .
C13 C 0.6109(3) 0.7233(3) 0.3012(6) 0.0246(12) Uani 1 1 d . . . . .
C4 C 0.5216(4) 0.3342(5) 0.4208(7) 0.0358(16) Uani 1 1 d . . . . .
C16 C 0.7198(4) 0.6601(5) 0.4821(8) 0.0381(17) Uani 1 1 d . . . . .
C33 C 0.2822(9) 0.5608(9) -0.2458(11) 0.081(5) Uani 1 1 d . . . . .
H33A H 0.242801 0.536896 -0.320531 0.121 Uiso 1 1 calc R U . . .
H33B H 0.322726 0.538117 -0.219312 0.121 Uiso 1 1 calc R U . . .
H33C H 0.281704 0.613558 -0.260925 0.121 Uiso 1 1 calc R U . . .
C18 C 0.6325(3) 0.6949(3) 0.4839(5) 0.0206(11) Uani 1 1 d . . . . .
C25 C 0.3741(3) 0.8094(3) 0.0523(5) 0.0181(10) Uani 1 1 d . . . . .
C20 C 0.6673(6) 0.9509(7) 0.4372(12) 0.060(3) Uani 1 1 d . . . . .
H20A H 0.632349 0.954288 0.348541 0.089 Uiso 1 1 calc R U . . .
H20B H 0.688588 0.902225 0.460634 0.089 Uiso 1 1 calc R U . . .
H20C H 0.700876 0.989353 0.468662 0.089 Uiso 1 1 calc R U . . .
C23 C 0.5610(4) 0.9234(4) 0.4986(6) 0.0255(12) Uani 1 1 d . . . . .
C1 C 0.6359(4) 0.3988(4) 0.5782(6) 0.0255(12) Uani 1 1 d . . . . .
C7 C 0.7708(3) 0.6431(4) 0.8250(6) 0.0238(11) Uani 1 1 d . . . . .
C26 C 0.3562(5) 0.9234(4) -0.0456(7) 0.0404(18) Uani 1 1 d . . . . .
H26A H 0.378917 0.913247 -0.073081 0.061 Uiso 1 1 calc R U . . .
H26B H 0.387920 0.945317 0.035615 0.061 Uiso 1 1 calc R U . . .
H26C H 0.319273 0.957958 -0.101907 0.061 Uiso 1 1 calc R U . . .
C27 C 0.1797(5) 0.7184(6) -0.2709(8) 0.060(3) Uani 1 1 d . . . . .
H27A H 0.158310 0.705358 -0.241746 0.090 Uiso 1 1 calc R U . . .
H27B H 0.175860 0.676923 -0.316880 0.090 Uiso 1 1 calc R U . . .
H27C H 0.157697 0.761939 -0.323452 0.090 Uiso 1 1 calc R U . . .
C28 C 0.2730(4) 0.7228(4) -0.0570(7) 0.0335(15) Uani 1 1 d . . . . .
C8 C 0.8666(4) 0.6375(5) 1.0349(7) 0.0419(18) Uani 1 1 d . . . . .
H8A H 0.887664 0.595722 1.030928 0.063 Uiso 1 1 calc R U . . .
H8B H 0.839664 0.619258 1.050463 0.063 Uiso 1 1 calc R U . . .
H8C H 0.901270 0.670860 1.100428 0.063 Uiso 1 1 calc R U . . .
C30 C 0.3866(3) 0.6883(3) 0.1394(5) 0.0190(10) Uani 1 1 d . . . . .
C31 C 0.3173(4) 0.4870(4) 0.0660(6) 0.0292(13) Uani 1 1 d . . . . .
C32 C 0.2940(9) 0.3610(5) 0.0087(13) 0.072(4) Uani 1 1 d . . . . .
H32A H 0.246733 0.359686 -0.033400 0.108 Uiso 1 1 calc R U . . .
H32B H 0.321664 0.348730 0.094430 0.108 Uiso 1 1 calc R U . . .
H32C H 0.302067 0.325058 -0.028197 0.108 Uiso 1 1 calc R U . . .
C10 C 0.7494(4) 0.7632(4) 0.7053(7) 0.0381(17) Uani 1 1 d . . . . .
C34 C 0.3408(4) 0.5707(4) -0.0386(7) 0.0344(15) Uani 1 1 d . . . . .
C35 C 0.3387(4) 0.5592(4) 0.0575(6) 0.0261(12) Uani 1 1 d . . . . .
C36 C 0.3585(3) 0.6144(3) 0.1389(5) 0.0198(10) Uani 1 1 d . . . . .
C11 C 0.7310(3) 0.6854(4) 0.7109(6) 0.0269(12) Uani 1 1 d . . . . .
C12 C 0.6725(3) 0.6547(3) 0.6059(5) 0.0216(11) Uani 1 1 d . . . . .
C22 C 0.5866(4) 0.9825(4) 0.5894(7) 0.0340(15) Uani 1 1 d . . . . .
C24 C 0.5127(3) 0.8730(3) 0.4675(5) 0.0206(11) Uani 1 1 d . . . . .
C2 C 0.7294(5) 0.3615(6) 0.6083(12) 0.059(3) Uani 1 1 d . . . . .
H2A H 0.737706 0.339144 0.560878 0.088 Uiso 1 1 calc R U . . .
H2B H 0.756512 0.336373 0.686697 0.088 Uiso 1 1 calc R U . . .
H2C H 0.741477 0.413953 0.621486 0.088 Uiso 1 1 calc R U . . .
C6 C 0.5376(4) 0.4446(3) 0.5365(6) 0.0247(12) Uani 1 1 d . . . . .
C9 C 0.8348(7) 0.8515(10) 0.7870(13) 0.106(4) Uani 1 1 d . . . . .
H9A H 0.840631 0.860335 0.731097 0.159 Uiso 1 1 calc R U . . .
H9B H 0.876484 0.863023 0.869958 0.159 Uiso 1 1 calc R U . . .
H9C H 0.798868 0.882963 0.764662 0.159 Uiso 1 1 calc R U . . .
C15 C 0.8368(13) 0.726(3) 0.617(4) 0.073(2) Uani 0.25(2) 1 d D . P A 1
H15A H 0.841772 0.765606 0.666761 0.109 Uiso 0.25(2) 1 calc R U P A 1
H15B H 0.856347 0.742703 0.585023 0.109 Uiso 0.25(2) 1 calc R U P A 1
H15C H 0.859905 0.681838 0.665722 0.109 Uiso 0.25(2) 1 calc R U P A 1
C15A C 0.8289(7) 0.6785(11) 0.563(2) 0.073(2) Uani 0.75(2) 1 d D . P A 2
H15D H 0.841000 0.636135 0.615067 0.109 Uiso 0.75(2) 1 calc R U P A 2
H15E H 0.863918 0.716174 0.610703 0.109 Uiso 0.75(2) 1 calc R U P A 2
H15F H 0.824399 0.662275 0.496108 0.109 Uiso 0.75(2) 1 calc R U P A 2
N1 N 0.500000 0.6560(5) 0.500000 0.0330(18) Uani 1 2 d DS T P . .
H1A H 0.517(6) 0.599(3) 0.516(13) 0.04(2) Uiso 0.5 1 d D . P B -1
H1B H 0.488(8) 0.675(8) 0.420(8) 0.04(2) Uiso 0.5 1 d D . P C -1
H1C H 0.539(5) 0.687(7) 0.580(8) 0.04(2) Uiso 0.5 1 d D . P D -1
H1D H 0.455(4) 0.657(7) 0.481(14) 0.04(2) Uiso 0.5 1 d D . P E -1
Br2 Br 0.49446(19) 0.3694(2) 0.1382(3) 0.1561(9) Uani 1 1 d D . . F 3
Br1 Br 0.59104(19) 0.5051(2) 0.3180(3) 0.1561(9) Uani 1 1 d D . . F 3
C99 C 0.4994(12) 0.4602(15) 0.217(2) 0.1561(9) Uani 1 1 d D . . F 3
H99A H 0.490820 0.448121 0.268391 0.187 Uiso 1 1 calc R U . F 3
H99B H 0.465035 0.495880 0.153933 0.187 Uiso 1 1 calc R U . F 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O30 1.951(4) 2_656 ?
Fe1 O1 1.974(4) . ?
Fe1 O10 1.940(4) . ?
Fe1 O26 2.022(5) 2_656 ?
Fe1 O5 1.989(4) . ?
Fe1 O6 2.027(5) . ?
Fe2 O25 1.959(4) . ?
Fe2 O21 2.016(4) . ?
Fe2 O16 1.993(4) . ?
Fe2 O20 1.972(4) . ?
Fe2 O15 1.976(4) . ?
Fe2 O11 2.032(4) . ?
O17 C19 1.323(8) . ?
O17 C20 1.440(10) . ?
O25 C30 1.270(8) . ?
O21 C25 1.224(8) . ?
O16 C19 1.214(9) . ?
O30 C36 1.268(7) . ?
O24 C28 1.226(10) . ?
O19 C22 1.220(10) . ?
O20 C24 1.286(7) . ?
O23 C27 1.447(10) . ?
O23 C28 1.332(10) . ?
O1 C1 1.263(8) . ?
O28 C33 1.466(11) . ?
O28 C34 1.350(10) . ?
O29 C34 1.182(10) . ?
O15 C18 1.271(8) . ?
O2 C1 1.330(8) . ?
O2 C2 1.455(11) . ?
O7 C7 1.297(8) . ?
O7 C8 1.430(9) . ?
O18 C21 1.455(11) . ?
O18 C22 1.322(10) . ?
O9 C10 1.157(11) . ?
O3 C3 1.444(11) . ?
O3 C4 1.351(10) . ?
O10 C12 1.276(8) . ?
O22 C25 1.336(7) . ?
O22 C26 1.431(8) . ?
O11 C13 1.232(9) . ?
O4 C4 1.185(10) . ?
O12 C14 1.460(10) . ?
O12 C13 1.333(8) . ?
O26 C31 1.242(8) . ?
O13 C16 1.312(12) . ?
O13 C15 1.47(3) . ?
O13 C15A 1.468(15) . ?
O5 C6 1.270(8) . ?
O14 C16 1.202(12) . ?
O8 C10 1.338(13) . ?
O8 C9 1.547(17) . ?
O6 C7 1.254(8) . ?
O27 C31 1.296(8) . ?
O27 C32 1.448(10) . ?
C5 C4 1.493(10) . ?
C5 C1 1.417(10) . ?
C5 C6 1.396(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C29 C25 1.431(8) . ?
C29 C28 1.496(9) . ?
C29 C30 1.379(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C19 C23 1.446(9) . ?
C17 C13 1.433(9) . ?
C17 C16 1.495(10) . ?
C17 C18 1.370(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C18 C12 1.524(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C23 C22 1.471(9) . ?
C23 C24 1.386(9) . ?
C7 C11 1.462(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C30 C36 1.526(8) . ?
C31 C35 1.460(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C10 C11 1.504(10) . ?
C34 C35 1.499(9) . ?
C35 C36 1.364(9) . ?
C11 C12 1.371(9) . ?
C24 C24 1.536(11) 2_656 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C6 C6 1.525(14) 2_656 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C15A H15D 0.9700 . ?
C15A H15E 0.9700 . ?
C15A H15F 0.9700 . ?
N1 H1A 1.07(3) . ?
N1 H1B 1.07(2) . ?
N1 H1C 1.06(3) . ?
N1 H1D 1.07(2) . ?
Br2 C99 1.96(2) . ?
Br1 C99 2.00(2) . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?

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
O30 Fe1 O1 171.5(2) 2_656 . ?
O30 Fe1 O26 86.99(18) 2_656 2_656 ?
O30 Fe1 O5 86.58(19) 2_656 . ?
O30 Fe1 O6 88.4(2) 2_656 . ?
O1 Fe1 O26 89.32(19) . 2_656 ?
O1 Fe1 O5 86.01(19) . . ?
O1 Fe1 O6 99.3(2) . . ?
O10 Fe1 O30 91.76(19) . 2_656 ?
O10 Fe1 O1 92.57(19) . . ?
O10 Fe1 O26 174.9(2) . 2_656 ?
O10 Fe1 O5 91.21(19) . . ?
O10 Fe1 O6 84.95(18) . . ?
O26 Fe1 O6 90.1(2) 2_656 . ?
O5 Fe1 O26 93.6(2) . 2_656 ?
O5 Fe1 O6 173.58(19) . . ?
O25 Fe2 O21 85.30(18) . . ?
O25 Fe2 O16 177.2(2) . . ?
O25 Fe2 O20 92.50(19) . . ?
O25 Fe2 O15 85.8(2) . . ?
O25 Fe2 O11 96.6(2) . . ?
O21 Fe2 O11 90.39(19) . . ?
O16 Fe2 O21 92.62(19) . . ?
O16 Fe2 O11 85.2(2) . . ?
O20 Fe2 O21 97.94(19) . . ?
O20 Fe2 O16 85.95(19) . . ?
O20 Fe2 O15 86.83(18) . . ?
O20 Fe2 O11 168.11(19) . . ?
O15 Fe2 O21 170.0(2) . . ?
O15 Fe2 O16 96.4(2) . . ?
O15 Fe2 O11 86.29(18) . . ?
C19 O17 C20 114.7(6) . . ?
C30 O25 Fe2 131.2(4) . . ?
C25 O21 Fe2 130.5(4) . . ?
C19 O16 Fe2 130.6(4) . . ?
C36 O30 Fe1 130.1(4) . 2_656 ?
C24 O20 Fe2 129.1(4) . . ?
C28 O23 C27 116.2(7) . . ?
C1 O1 Fe1 130.8(4) . . ?
C34 O28 C33 111.9(8) . . ?
C18 O15 Fe2 128.4(4) . . ?
C1 O2 C2 115.8(6) . . ?
C7 O7 C8 117.8(6) . . ?
C22 O18 C21 113.9(8) . . ?
C4 O3 C3 115.0(7) . . ?
C12 O10 Fe1 128.8(4) . . ?
C25 O22 C26 117.4(5) . . ?
C13 O11 Fe2 127.6(4) . . ?
C13 O12 C14 116.3(6) . . ?
C31 O26 Fe1 129.2(4) . 2_656 ?
C16 O13 C15 139.2(18) . . ?
C16 O13 C15A 114.6(11) . . ?
C6 O5 Fe1 130.5(4) . . ?
C10 O8 C9 108.6(11) . . ?
C7 O6 Fe1 126.5(4) . . ?
C31 O27 C32 117.1(6) . . ?
C1 C5 C4 122.6(6) . . ?
C6 C5 C4 117.2(6) . . ?
C6 C5 C1 120.2(6) . . ?
O18 C21 H21A 109.5 . . ?
O18 C21 H21B 109.5 . . ?
O18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C29 C28 121.1(5) . . ?
C30 C29 C25 120.1(5) . . ?
C30 C29 C28 118.8(5) . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
O12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O17 C19 C23 113.9(6) . . ?
O16 C19 O17 119.9(6) . . ?
O16 C19 C23 126.2(6) . . ?
C13 C17 C16 119.5(6) . . ?
C18 C17 C13 120.5(6) . . ?
C18 C17 C16 119.9(6) . . ?
O11 C13 O12 120.3(6) . . ?
O11 C13 C17 126.3(6) . . ?
O12 C13 C17 113.3(6) . . ?
O3 C4 C5 111.3(6) . . ?
O4 C4 O3 122.2(7) . . ?
O4 C4 C5 125.9(7) . . ?
O13 C16 C17 112.3(7) . . ?
O14 C16 O13 122.6(8) . . ?
O14 C16 C17 124.9(8) . . ?
O28 C33 H33A 109.5 . . ?
O28 C33 H33B 109.5 . . ?
O28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O15 C18 C17 127.2(6) . . ?
O15 C18 C12 111.3(5) . . ?
C17 C18 C12 121.1(6) . . ?
O21 C25 O22 119.4(5) . . ?
O21 C25 C29 125.7(5) . . ?
O22 C25 C29 114.8(5) . . ?
O17 C20 H20A 109.5 . . ?
O17 C20 H20B 109.5 . . ?
O17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C23 C22 120.1(6) . . ?
C24 C23 C19 118.7(6) . . ?
C24 C23 C22 121.2(6) . . ?
O1 C1 O2 117.7(6) . . ?
O1 C1 C5 125.3(6) . . ?
O2 C1 C5 117.0(6) . . ?
O7 C7 C11 115.0(6) . . ?
O6 C7 O7 121.4(6) . . ?
O6 C7 C11 123.5(6) . . ?
O22 C26 H26A 109.5 . . ?
O22 C26 H26B 109.5 . . ?
O22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O23 C27 H27A 109.5 . . ?
O23 C27 H27B 109.5 . . ?
O23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O24 C28 O23 123.3(7) . . ?
O24 C28 C29 122.3(7) . . ?
O23 C28 C29 114.3(6) . . ?
O7 C8 H8A 109.5 . . ?
O7 C8 H8B 109.5 . . ?
O7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O25 C30 C29 126.0(5) . . ?
O25 C30 C36 112.0(5) . . ?
C29 C30 C36 121.9(5) . . ?
O26 C31 O27 120.6(6) . . ?
O26 C31 C35 124.8(6) . . ?
O27 C31 C35 114.5(6) . . ?
O27 C32 H32A 109.5 . . ?
O27 C32 H32B 109.5 . . ?
O27 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O9 C10 O8 126.7(8) . . ?
O9 C10 C11 123.1(8) . . ?
O8 C10 C11 109.7(8) . . ?
O28 C34 C35 110.5(6) . . ?
O29 C34 O28 124.5(7) . . ?
O29 C34 C35 124.6(7) . . ?
C31 C35 C34 119.3(6) . . ?
C36 C35 C31 120.1(5) . . ?
C36 C35 C34 120.6(6) . . ?
O30 C36 C30 110.4(5) . . ?
O30 C36 C35 127.8(5) . . ?
C35 C36 C30 121.5(5) . . ?
C7 C11 C10 122.7(6) . . ?
C12 C11 C7 118.6(6) . . ?
C12 C11 C10 118.6(6) . . ?
O10 C12 C18 111.8(5) . . ?
O10 C12 C11 128.2(5) . . ?
C11 C12 C18 119.9(5) . . ?
O19 C22 O18 122.7(7) . . ?
O19 C22 C23 124.9(7) . . ?
O18 C22 C23 112.4(6) . . ?
O20 C24 C23 127.1(5) . . ?
O20 C24 C24 111.2(5) . 2_656 ?
C23 C24 C24 121.7(5) . 2_656 ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O5 C6 C5 126.1(6) . . ?
O5 C6 C6 111.5(5) . 2_656 ?
C5 C6 C6 122.2(6) . 2_656 ?
O8 C9 H9A 109.5 . . ?
O8 C9 H9B 109.5 . . ?
O8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O13 C15 H15A 109.5 . . ?
O13 C15 H15B 109.5 . . ?
O13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C15A H15D 109.5 . . ?
O13 C15A H15E 109.5 . . ?
O13 C15A H15F 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
H1A N1 H1B 108(5) . . ?
H1A N1 H1C 108(5) . . ?
H1A N1 H1D 109(5) . . ?
H1B N1 H1C 114(5) . . ?
H1B N1 H1D 108(5) . . ?
H1C N1 H1D 111(5) . . ?
Br2 C99 Br1 109.1(12) . . ?
Br2 C99 H99A 109.9 . . ?
Br2 C99 H99B 109.9 . . ?
Br1 C99 H99A 109.9 . . ?
Br1 C99 H99B 109.9 . . ?
H99A C99 H99B 108.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O30 C36 C30 -177.9(4) 2_656 . . . ?
Fe1 O30 C36 C35 -2.9(10) 2_656 . . . ?
Fe1 O1 C1 O2 164.2(5) . . . . ?
Fe1 O1 C1 C5 -15.2(10) . . . . ?
Fe1 O10 C12 C18 -168.1(4) . . . . ?
Fe1 O10 C12 C11 9.1(10) . . . . ?
Fe1 O26 C31 O27 162.9(6) 2_656 . . . ?
Fe1 O26 C31 C35 -13.2(11) 2_656 . . . ?
Fe1 O5 C6 C5 -1.9(10) . . . . ?
Fe1 O5 C6 C6 -176.7(4) . . . 2_656 ?
Fe1 O6 C7 O7 152.0(5) . . . . ?
Fe1 O6 C7 C11 -30.3(9) . . . . ?
Fe2 O25 C30 C29 5.8(10) . . . . ?
Fe2 O25 C30 C36 -170.9(4) . . . . ?
Fe2 O21 C25 O22 170.8(4) . . . . ?
Fe2 O21 C25 C29 -8.3(9) . . . . ?
Fe2 O16 C19 O17 162.5(5) . . . . ?
Fe2 O16 C19 C23 -15.3(11) . . . . ?
Fe2 O20 C24 C23 10.7(9) . . . . ?
Fe2 O20 C24 C24 -167.5(4) . . . 2_656 ?
Fe2 O15 C18 C17 -12.3(10) . . . . ?
Fe2 O15 C18 C12 174.8(4) . . . . ?
Fe2 O11 C13 O12 -167.3(5) . . . . ?
Fe2 O11 C13 C17 14.8(10) . . . . ?
O17 C19 C23 C22 6.8(10) . . . . ?
O17 C19 C23 C24 -172.5(6) . . . . ?
O25 C30 C36 O30 62.9(7) . . . . ?
O25 C30 C36 C35 -112.4(7) . . . . ?
O16 C19 C23 C22 -175.2(7) . . . . ?
O16 C19 C23 C24 5.5(11) . . . . ?
O28 C34 C35 C31 52.2(10) . . . . ?
O28 C34 C35 C36 -129.9(8) . . . . ?
O29 C34 C35 C31 -134.0(9) . . . . ?
O29 C34 C35 C36 43.9(12) . . . . ?
O15 C18 C12 O10 66.6(7) . . . . ?
O15 C18 C12 C11 -110.9(7) . . . . ?
O7 C7 C11 C10 -1.5(10) . . . . ?
O7 C7 C11 C12 -177.8(6) . . . . ?
O9 C10 C11 C7 -148.0(8) . . . . ?
O9 C10 C11 C12 28.3(12) . . . . ?
O26 C31 C35 C34 -174.2(7) . . . . ?
O26 C31 C35 C36 7.9(11) . . . . ?
O8 C10 C11 C7 39.6(11) . . . . ?
O8 C10 C11 C12 -144.1(9) . . . . ?
O6 C7 C11 C10 -179.3(7) . . . . ?
O6 C7 C11 C12 4.4(10) . . . . ?
O27 C31 C35 C34 9.5(11) . . . . ?
O27 C31 C35 C36 -168.4(7) . . . . ?
C21 O18 C22 O19 6.1(15) . . . . ?
C21 O18 C22 C23 -175.7(9) . . . . ?
C29 C30 C36 O30 -114.0(6) . . . . ?
C29 C30 C36 C35 70.7(8) . . . . ?
C14 O12 C13 O11 -1.2(11) . . . . ?
C14 O12 C13 C17 176.9(8) . . . . ?
C3 O3 C4 O4 5.7(15) . . . . ?
C3 O3 C4 C5 177.9(10) . . . . ?
C19 C23 C22 O19 45.7(12) . . . . ?
C19 C23 C22 O18 -132.5(8) . . . . ?
C19 C23 C24 O20 -3.2(10) . . . . ?
C19 C23 C24 C24 174.9(6) . . . 2_656 ?
C17 C18 C12 O10 -106.8(7) . . . . ?
C17 C18 C12 C11 75.7(8) . . . . ?
C13 C17 C16 O13 73.3(10) . . . . ?
C13 C17 C16 O14 -111.3(11) . . . . ?
C13 C17 C18 O15 -1.4(11) . . . . ?
C13 C17 C18 C12 170.9(6) . . . . ?
C4 C5 C1 O1 -174.2(7) . . . . ?
C4 C5 C1 O2 6.4(10) . . . . ?
C4 C5 C6 O5 -177.3(7) . . . . ?
C4 C5 C6 C6 -3.0(10) . . . 2_656 ?
C16 C17 C13 O11 175.6(7) . . . . ?
C16 C17 C13 O12 -2.4(10) . . . . ?
C16 C17 C18 O15 -177.2(7) . . . . ?
C16 C17 C18 C12 -5.0(10) . . . . ?
C33 O28 C34 O29 7.3(14) . . . . ?
C33 O28 C34 C35 -178.9(9) . . . . ?
C18 C17 C13 O11 -0.3(11) . . . . ?
C18 C17 C13 O12 -178.2(6) . . . . ?
C18 C17 C16 O13 -110.8(9) . . . . ?
C18 C17 C16 O14 64.6(13) . . . . ?
C25 C29 C28 O24 -134.2(8) . . . . ?
C25 C29 C28 O23 49.1(10) . . . . ?
C25 C29 C30 O25 2.1(10) . . . . ?
C25 C29 C30 C36 178.6(5) . . . . ?
C20 O17 C19 O16 -2.5(12) . . . . ?
C20 O17 C19 C23 175.6(8) . . . . ?
C1 C5 C4 O3 43.8(11) . . . . ?
C1 C5 C4 O4 -144.4(9) . . . . ?
C1 C5 C6 O5 0.5(10) . . . . ?
C1 C5 C6 C6 174.8(6) . . . 2_656 ?
C7 C11 C12 O10 7.3(11) . . . . ?
C7 C11 C12 C18 -175.7(6) . . . . ?
C26 O22 C25 O21 4.7(9) . . . . ?
C26 O22 C25 C29 -176.2(6) . . . . ?
C27 O23 C28 O24 3.1(13) . . . . ?
C27 O23 C28 C29 179.7(8) . . . . ?
C28 C29 C25 O21 178.5(6) . . . . ?
C28 C29 C25 O22 -0.6(9) . . . . ?
C28 C29 C30 O25 -177.1(6) . . . . ?
C28 C29 C30 C36 -0.7(9) . . . . ?
C8 O7 C7 O6 -0.1(10) . . . . ?
C8 O7 C7 C11 -178.0(7) . . . . ?
C30 C29 C25 O21 -0.8(10) . . . . ?
C30 C29 C25 O22 -179.8(6) . . . . ?
C30 C29 C28 O24 45.0(11) . . . . ?
C30 C29 C28 O23 -131.6(7) . . . . ?
C31 C35 C36 O30 0.5(11) . . . . ?
C31 C35 C36 C30 175.0(6) . . . . ?
C32 O27 C31 O26 -0.1(14) . . . . ?
C32 O27 C31 C35 176.4(10) . . . . ?
C10 C11 C12 O10 -169.1(7) . . . . ?
C10 C11 C12 C18 7.9(10) . . . . ?
C34 C35 C36 O30 -177.3(7) . . . . ?
C34 C35 C36 C30 -2.9(10) . . . . ?
C22 C23 C24 O20 177.6(6) . . . . ?
C22 C23 C24 C24 -4.4(10) . . . 2_656 ?
C24 C23 C22 O19 -135.1(10) . . . . ?
C24 C23 C22 O18 46.8(10) . . . . ?
C2 O2 C1 O1 0.5(11) . . . . ?
C2 O2 C1 C5 179.9(8) . . . . ?
C6 C5 C4 O3 -138.4(7) . . . . ?
C6 C5 C4 O4 33.3(13) . . . . ?
C6 C5 C1 O1 8.1(11) . . . . ?
C6 C5 C1 O2 -171.3(6) . . . . ?
C9 O8 C10 O9 16.3(18) . . . . ?
C9 O8 C10 C11 -171.7(11) . . . . ?
C15 O13 C16 O14 -38(4) . . . . ?
C15 O13 C16 C17 138(4) . . . . ?
C15A O13 C16 O14 8.8(18) . . . . ?
C15A O13 C16 C17 -175.6(12) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 282 electrons were 
found in a volume of 544Å³ in 3 voids per unit cell. 
This is consistent with the presence of 
[+ solvents]1.8[CH2Br2] per Formula Unit 
which account for 281 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.031 0.000 33.2 3.8 '1 ?'
2 0.000 0.560 0.000 216.9 136.9 '1.8 CH2Br2'
3 0.158 0.289 0.755 11.4 0.0 ?
4 0.500 0.060 0.000 216.9 136.9 '1.8 CH2Br2'
5 0.342 0.789 0.245 11.4 0.0 ?
6 0.500 0.531 0.000 33.2 3.8 '1 ?'
7 0.658 0.789 0.755 11.4 0.0 ?
8 0.842 0.289 0.245 11.4 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.0
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.61(2)
2 0.39(2)
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/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_1-chbr3
_database_code_depnum_ccdc_archive 'CCDC 2281393'
loop_
_audit_author_name
_audit_author_address
'ryo tsunashima'
;yamaguchi university
Japan
;
_audit_update_record             
;
2023-07-13 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        C72H72O60Fe4(CHBr3)2
_chemical_formula_moiety         '2(C H Br3), C72 H72 Fe4 O60, 0.5(H8 N2)'
_chemical_formula_sum            'C74 H78 Br6 Fe4 N O60'
_chemical_formula_weight         2644.23
_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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   27.5848(4)
_cell_length_b                   17.97775(10)
_cell_length_c                   15.1052(2)
_cell_angle_alpha                90
_cell_angle_beta                 133.527(3)
_cell_angle_gamma                90
_cell_volume                     5431.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20804
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.4000
_cell_measurement_theta_min      3.8980
_shelx_estimated_absorpt_T_max   0.572
_shelx_estimated_absorpt_T_min   0.443
_exptl_absorpt_coefficient_mu    7.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2646
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 2 7 0.0643
-9 9 1 0.0598
16 3 -8 0.0524
7 -10 0 0.0301
8 8 0 0.0192
-9 -8 0 0.0612
14 1 -10 0.0503
-9 3 9 0.0411
-15 -5 8 0.0621

_exptl_crystal_preparation       'local laboratory'
_exptl_crystal_recrystallization_method 'vaper diffusion with hexane'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.082
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.744
_diffrn_reflns_theta_min         3.305
_diffrn_ambient_temperature      223.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -14.00   0.50    1.16    --  -43.03  95.00  95.00  108
  2  ω    -11.00  25.00   0.50    1.16    --  -43.03  95.00  95.00   72
  3  ω      9.00  67.00   0.50    1.16    --   43.03 -95.00 -14.00  116
  4  ω    -25.00   3.00   0.50    1.16    --   43.03 -95.00 -14.00   56
  5  ω    -67.00 -40.00   0.50    4.64    -- -103.00  95.00  95.00   54
  6  ω     92.00 178.00   0.50    4.64    --  113.50  95.00  95.00  172
  7  ω     21.00 115.00   0.50    1.16    --   43.03  57.00  30.00  188
  8  ω     26.00  64.00   0.50    1.16    --   43.03 -38.00 -30.00   76
  9  ω    -32.00  22.00   0.50    1.16    --   43.03 -38.00 -30.00  108
 10  ω     22.00 116.00   0.50    1.16    --   43.03  57.00  90.00  188
 11  ω     23.00 116.00   0.50    1.16    --   43.03  57.00 -90.00  186
 12  ω   -153.00-128.00   0.50    4.64    -- -103.00 -95.00 -14.00   50
 13  ω     39.00 105.00   0.50    4.64    --  113.50 -95.00  90.00  132
 14  ω     98.00 135.00   0.50    4.64    --  113.50 -45.00-180.00   74
 15  ω     85.00 178.00   0.50    4.64    --  113.50  77.00-120.00  186
 16  ω     38.00  90.00   0.50    4.64    --  113.50 -45.00-180.00  104
 17  ω     90.00 172.00   0.50    4.64    --  113.50  61.00  60.00  164
 18  ω     38.00  82.00   0.50    4.64    --  113.50 -45.00 -60.00   88
 19  ω     89.00 134.00   0.50    4.64    --  113.50 -45.00 -60.00   90
 20  ω     90.00 174.00   0.50    4.64    --  113.50  61.00 -60.00  168
 21  ω     39.00 105.00   0.50    4.64    --  113.50 -95.00 120.00  132
 22  ω     85.00 173.00   0.50    4.64    --  113.50  77.00  30.00  176
 23  ω     90.00 178.00   0.50    4.64    --  113.50  61.00-150.00  176
 24  ω     91.00 177.00   0.50    4.64    --  113.50  45.00-180.00  172
 25  ω     41.00 105.00   0.50    4.64    --  113.50 -95.00 -90.00  128
 26  ω     39.00 103.00   0.50    4.64    --  113.50 -95.00  30.00  128
 27  ω     43.00 103.00   0.50    4.64    --  113.50 -95.00 -60.00  120
 28  ω     57.00 105.00   0.50    4.64    --  113.50 -95.00 -14.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_diffrn_special_details          nothing
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                10136
_reflns_number_total             10523
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.441(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10523
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0708
_refine_ls_restrained_S_all      1.020
_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)+(0.1438P)²+24.0166P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1947
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.559(7)
 0.441(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1A
 1.07 with sigma of 0.02
 N1-H1B
 1.07 with sigma of 0.02
 N1-H1C
 1.07 with sigma of 0.02
 N1-H1D
 1.07 with sigma of 0.02
 H1A-H1B
 1.75 with sigma of 0.04
 H1A-H1C
 1.75 with sigma of 0.04
 H1A-H1D
 1.75 with sigma of 0.04
 H1B-H1C
 1.75 with sigma of 0.04
 H1B-H1D
 1.75 with sigma of 0.04
 H1C-H1D
 1.75 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(O8)
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
6.a Ternary CH refined with riding coordinates:
 C99(H99)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C)
;
_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
Br1 Br 0.54160(15) 0.45255(12) 0.3214(2) 0.1013(8) Uani 1 1 d . . . . .
Br2 Br 0.57576(15) 0.45605(18) 0.1630(3) 0.1185(10) Uani 1 1 d . . . . .
Br3 Br 0.49331(16) 0.32099(15) 0.1362(3) 0.1136(9) Uani 1 1 d . . . . .
C99 C 0.5117(9) 0.4265(10) 0.1705(16) 0.069(4) Uani 1 1 d . . . . .
H99 H 0.469579 0.453755 0.106059 0.083 Uiso 1 1 calc R U . . .
Fe1 Fe 0.66061(6) 0.45646(7) 0.72002(10) 0.0197(3) Uani 1 1 d . . . . .
Fe2 Fe 0.50967(6) 0.70521(7) 0.29995(10) 0.0192(3) Uani 1 1 d . . . . .
O1 O 0.6755(3) 0.3666(3) 0.6640(6) 0.0264(12) Uani 1 1 d . . . . .
O2 O 0.6575(4) 0.2795(4) 0.5416(8) 0.0438(18) Uani 1 1 d . . . . .
O3 O 0.5546(4) 0.1905(4) 0.4560(8) 0.053(2) Uani 1 1 d . . . . .
O4 O 0.4640(3) 0.2634(5) 0.3345(7) 0.0480(19) Uani 1 1 d . . . . .
O5 O 0.5664(3) 0.4225(3) 0.6072(6) 0.0270(12) Uani 1 1 d . . . . .
O6 O 0.7537(3) 0.5014(4) 0.8313(6) 0.0301(13) Uani 1 1 d . . . . .
O7 O 0.8205(3) 0.6004(4) 0.9212(6) 0.0343(14) Uani 1 1 d . . . . .
O8 O 0.8152(5) 0.6904(7) 0.7783(10) 0.088(4) Uani 1 1 d . . . . .
O9 O 0.7090(5) 0.7319(4) 0.6400(8) 0.053(2) Uani 1 1 d . . . . .
O10 O 0.6420(3) 0.5187(3) 0.5935(5) 0.0260(12) Uani 1 1 d . . . . .
O11 O 0.5543(3) 0.6731(4) 0.2417(6) 0.0277(12) Uani 1 1 d . . . . .
O12 O 0.6382(4) 0.6452(5) 0.2576(6) 0.0381(16) Uani 1 1 d . . . . .
O13 O 0.7628(4) 0.6362(6) 0.5128(10) 0.063(3) Uani 1 1 d . . . . .
O14 O 0.7333(5) 0.5230(6) 0.5111(13) 0.077(3) Uani 1 1 d . . . . .
O15 O 0.5758(3) 0.6430(4) 0.4423(5) 0.0257(12) Uani 1 1 d . . . . .
O16 O 0.5681(3) 0.7952(3) 0.3640(6) 0.0285(13) Uani 1 1 d . . . . .
O17 O 0.6380(4) 0.8845(4) 0.4921(7) 0.0381(16) Uani 1 1 d . . . . .
O18 O 0.6026(5) 0.8794(5) 0.6904(8) 0.052(2) Uani 1 1 d . . . . .
O19 O 0.5916(5) 0.9696(4) 0.5775(9) 0.057(2) Uani 1 1 d . . . . .
O20 O 0.4855(3) 0.7426(3) 0.3881(5) 0.0241(11) Uani 1 1 d . . . . .
O21 O 0.4352(3) 0.7533(3) 0.1371(5) 0.0257(12) Uani 1 1 d . . . . .
O22 O 0.3322(3) 0.7811(4) -0.0379(6) 0.0373(15) Uani 1 1 d . . . . .
O23 O 0.2491(4) 0.6644(5) -0.1631(7) 0.051(2) Uani 1 1 d . . . . .
O24 O 0.2398(4) 0.6283(5) -0.0331(8) 0.0474(19) Uani 1 1 d . . . . .
O25 O 0.4484(3) 0.6212(3) 0.2352(5) 0.0246(11) Uani 1 1 d . . . . .
O26 O 0.3116(3) 0.3978(3) 0.1370(6) 0.0283(13) Uani 1 1 d . . . . .
O27 O 0.3060(5) 0.3641(4) -0.0104(8) 0.0468(19) Uani 1 1 d . . . . .
O28 O 0.2716(4) 0.4866(5) -0.1561(6) 0.0452(18) Uani 1 1 d . . . . .
O29 O 0.3773(4) 0.5239(5) -0.0334(7) 0.0422(17) Uani 1 1 d . . . . .
O30 O 0.3660(3) 0.5358(3) 0.2322(5) 0.0246(12) Uani 1 1 d . . . . .
C1 C 0.6362(4) 0.3224(5) 0.5789(8) 0.0235(16) Uani 1 1 d . . . . .
C2 C 0.7276(7) 0.2923(11) 0.6042(18) 0.081(6) Uani 1 1 d . . . . .
H2A H 0.729175 0.314401 0.547658 0.121 Uiso 1 1 calc R U . . .
H2B H 0.751361 0.245223 0.633482 0.121 Uiso 1 1 calc R U . . .
H2C H 0.748464 0.325551 0.672754 0.121 Uiso 1 1 calc R U . . .
C3 C 0.5155(8) 0.1289(9) 0.3771(17) 0.079(5) Uani 1 1 d . . . . .
H3A H 0.494349 0.141345 0.294623 0.118 Uiso 1 1 calc R U . . .
H3B H 0.481428 0.117583 0.377892 0.118 Uiso 1 1 calc R U . . .
H3C H 0.544173 0.085889 0.405120 0.118 Uiso 1 1 calc R U . . .
C4 C 0.5236(4) 0.2536(6) 0.4261(8) 0.0300(18) Uani 1 1 d . . . . .
C5 C 0.5659(4) 0.3156(5) 0.5152(8) 0.0252(16) Uani 1 1 d . . . . .
C6 C 0.5369(4) 0.3653(4) 0.5343(7) 0.0219(15) Uani 1 1 d . . . . .
C7 C 0.7684(4) 0.5667(5) 0.8248(7) 0.0244(16) Uani 1 1 d . . . . .
C8 C 0.8616(6) 0.5597(7) 1.0345(9) 0.045(3) Uani 1 1 d . . . . .
H8A H 0.890604 0.526113 1.038685 0.068 Uiso 1 1 calc R U . . .
H8B H 0.833255 0.531394 1.038605 0.068 Uiso 1 1 calc R U . . .
H8C H 0.888509 0.594333 1.102357 0.068 Uiso 1 1 calc R U . . .
C9 C 0.8382(7) 0.7661(11) 0.7851(14) 0.088(4) Uani 1 1 d . . . . .
H9A H 0.831326 0.775321 0.713882 0.132 Uiso 1 1 calc R U . . .
H9B H 0.885317 0.770784 0.858314 0.132 Uiso 1 1 calc R U . . .
H9C H 0.812894 0.802071 0.787589 0.132 Uiso 1 1 calc R U . . .
C10 C 0.7495(5) 0.6843(6) 0.7078(9) 0.035(2) Uani 1 1 d . . . . .
C11 C 0.7291(4) 0.6085(5) 0.7115(8) 0.0250(16) Uani 1 1 d . . . . .
C12 C 0.6720(4) 0.5786(5) 0.6067(8) 0.0226(15) Uani 1 1 d . . . . .
C13 C 0.6122(4) 0.6472(5) 0.3041(8) 0.0275(17) Uani 1 1 d . . . . .
C14 C 0.5992(7) 0.6695(9) 0.1346(11) 0.053(3) Uani 1 1 d . . . . .
H14A H 0.583590 0.719836 0.125382 0.080 Uiso 1 1 calc R U . . .
H14B H 0.561084 0.636713 0.079149 0.080 Uiso 1 1 calc R U . . .
H14C H 0.626450 0.668448 0.115761 0.080 Uiso 1 1 calc R U . . .
C15 C 0.8287(7) 0.6052(15) 0.5697(18) 0.094(7) Uani 1 1 d . . . . .
H15A H 0.855446 0.643791 0.575688 0.141 Uiso 1 1 calc R U . . .
H15B H 0.822193 0.564701 0.519815 0.141 Uiso 1 1 calc R U . . .
H15C H 0.851663 0.586685 0.650630 0.141 Uiso 1 1 calc R U . . .
C16 C 0.7201(5) 0.5862(6) 0.4853(9) 0.033(2) Uani 1 1 d . . . . .
C17 C 0.6537(4) 0.6210(5) 0.4261(8) 0.0259(16) Uani 1 1 d . . . . .
C18 C 0.6323(4) 0.6178(4) 0.4836(8) 0.0230(15) Uani 1 1 d . . . . .
C19 C 0.5871(4) 0.8405(5) 0.4454(8) 0.0272(17) Uani 1 1 d . . . . .
C20 C 0.6714(6) 0.8746(7) 0.4483(13) 0.050(3) Uani 1 1 d . . . . .
H20A H 0.676752 0.821893 0.443156 0.076 Uiso 1 1 calc R U . . .
H20B H 0.714917 0.898255 0.504696 0.076 Uiso 1 1 calc R U . . .
H20C H 0.644453 0.897000 0.368226 0.076 Uiso 1 1 calc R U . . .
C21 C 0.6236(10) 0.9336(12) 0.7811(15) 0.086(6) Uani 1 1 d . . . . .
H21A H 0.584651 0.958788 0.756042 0.129 Uiso 1 1 calc R U . . .
H21B H 0.652729 0.969719 0.789682 0.129 Uiso 1 1 calc R U . . .
H21C H 0.647474 0.908944 0.858677 0.129 Uiso 1 1 calc R U . . .
C22 C 0.5860(5) 0.9058(5) 0.5909(9) 0.033(2) Uani 1 1 d . . . . .
C23 C 0.5604(4) 0.8440(5) 0.4998(8) 0.0269(17) Uani 1 1 d . . . . .
C24 C 0.5132(4) 0.7952(5) 0.4692(7) 0.0231(16) Uani 1 1 d . . . . .
C25 C 0.3746(4) 0.7339(5) 0.0530(8) 0.0245(16) Uani 1 1 d . . . . .
C26 C 0.3587(6) 0.8482(6) -0.0435(11) 0.048(3) Uani 1 1 d . . . . .
H26A H 0.395315 0.835694 -0.036711 0.072 Uiso 1 1 calc R U . . .
H26B H 0.374697 0.880918 0.023116 0.072 Uiso 1 1 calc R U . . .
H26C H 0.323759 0.873117 -0.120706 0.072 Uiso 1 1 calc R U . . .
C27 C 0.1778(6) 0.6510(8) -0.2619(11) 0.062(4) Uani 1 1 d . . . . .
H27A H 0.164287 0.612193 -0.238096 0.093 Uiso 1 1 calc R U . . .
H27B H 0.168146 0.635564 -0.334222 0.093 Uiso 1 1 calc R U . . .
H27C H 0.153502 0.696348 -0.279243 0.093 Uiso 1 1 calc R U . . .
C28 C 0.2733(4) 0.6510(5) -0.0514(8) 0.0293(18) Uani 1 1 d . . . . .
C29 C 0.3461(4) 0.6663(5) 0.0472(7) 0.0246(16) Uani 1 1 d . . . . .
C30 C 0.3866(4) 0.6142(4) 0.1397(7) 0.0200(15) Uani 1 1 d . . . . .
C31 C 0.3167(5) 0.4149(5) 0.0634(8) 0.0256(16) Uani 1 1 d . . . . .
C32 C 0.2927(9) 0.2887(6) 0.0033(16) 0.064(4) Uani 1 1 d . . . . .
H32A H 0.246084 0.284381 -0.038526 0.097 Uiso 1 1 calc R U . . .
H32B H 0.320800 0.277713 0.089300 0.097 Uiso 1 1 calc R U . . .
H32C H 0.302428 0.253848 -0.031776 0.097 Uiso 1 1 calc R U . . .
C33 C 0.2626(8) 0.4969(9) -0.2608(11) 0.064(4) Uani 1 1 d . . . . .
H33A H 0.245437 0.451453 -0.308379 0.095 Uiso 1 1 calc R U . . .
H33B H 0.305206 0.509254 -0.234248 0.095 Uiso 1 1 calc R U . . .
H33C H 0.231151 0.537092 -0.310532 0.095 Uiso 1 1 calc R U . . .
C34 C 0.3317(5) 0.5002(5) -0.0476(8) 0.0305(18) Uani 1 1 d . . . . .
C35 C 0.3353(4) 0.4861(5) 0.0547(8) 0.0229(15) Uani 1 1 d . . . . .
C36 C 0.3588(4) 0.5411(4) 0.1397(7) 0.0203(15) Uani 1 1 d . . . . .
N1 N 0.500000 0.5781(7) 0.500000 0.035(2) Uani 1 2 d DS T P . .
H1A H 0.533(7) 0.605(10) 0.497(17) 0.041 Uiso 0.5 1 d D U P A -1
H1B H 0.496(9) 0.607(10) 0.556(14) 0.041 Uiso 0.5 1 d D U P B -1
H1C H 0.514(8) 0.521(3) 0.527(14) 0.041 Uiso 0.5 1 d D U P C -1
H1D H 0.451(4) 0.576(9) 0.408(7) 0.041 Uiso 0.5 1 d D U P D -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C99 1.872(17) . ?
Br2 C99 1.923(15) . ?
Br3 C99 1.939(18) . ?
C99 H99 0.9900 . ?
Fe1 O1 1.993(6) . ?
Fe1 O5 1.983(6) . ?
Fe1 O6 2.031(6) . ?
Fe1 O10 1.954(6) . ?
Fe1 O26 2.021(6) 2_656 ?
Fe1 O30 1.956(6) 2_656 ?
Fe2 O11 2.027(6) . ?
Fe2 O15 1.949(6) . ?
Fe2 O16 2.002(6) . ?
Fe2 O20 1.974(5) . ?
Fe2 O21 2.014(6) . ?
Fe2 O25 1.954(6) . ?
O1 C1 1.242(11) . ?
O2 C1 1.309(10) . ?
O2 C2 1.471(14) . ?
O3 C3 1.428(15) . ?
O3 C4 1.301(12) . ?
O4 C4 1.231(12) . ?
O5 C6 1.303(10) . ?
O6 C7 1.268(11) . ?
O7 C7 1.293(11) . ?
O7 C8 1.440(12) . ?
O8 C9 1.474(17) . ?
O8 C10 1.332(14) . ?
O9 C10 1.206(14) . ?
O10 C12 1.287(11) . ?
O11 C13 1.260(11) . ?
O12 C13 1.304(11) . ?
O12 C14 1.432(13) . ?
O13 C15 1.484(18) . ?
O13 C16 1.303(14) . ?
O14 C16 1.174(15) . ?
O15 C18 1.298(10) . ?
O16 C19 1.250(11) . ?
O17 C19 1.314(11) . ?
O17 C20 1.467(11) . ?
O18 C21 1.439(15) . ?
O18 C22 1.321(13) . ?
O19 C22 1.193(14) . ?
O20 C24 1.301(10) . ?
O21 C25 1.267(10) . ?
O22 C25 1.328(10) . ?
O22 C26 1.442(12) . ?
O23 C27 1.452(13) . ?
O23 C28 1.342(13) . ?
O24 C28 1.203(13) . ?
O25 C30 1.272(10) . ?
O26 C31 1.251(10) . ?
O27 C31 1.308(11) . ?
O27 C32 1.454(13) . ?
O28 C33 1.433(13) . ?
O28 C34 1.324(12) . ?
O29 C34 1.199(12) . ?
O30 C36 1.271(10) . ?
C1 C5 1.461(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 C5 1.502(13) . ?
C5 C6 1.355(12) . ?
C6 C6 1.522(15) 2_656 ?
C7 C11 1.453(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.491(13) . ?
C11 C12 1.356(12) . ?
C12 C18 1.533(11) . ?
C13 C17 1.422(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.513(12) . ?
C17 C18 1.347(12) . ?
C19 C23 1.434(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 C23 1.512(12) . ?
C23 C24 1.360(12) . ?
C24 C24 1.526(15) 2_656 ?
C25 C29 1.418(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 C29 1.486(11) . ?
C29 C30 1.388(12) . ?
C30 C36 1.521(11) . ?
C31 C35 1.420(11) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 C35 1.499(11) . ?
C35 C36 1.379(11) . ?
N1 H1A 1.07(3) . ?
N1 H1B 1.07(3) . ?
N1 H1C 1.08(3) . ?
N1 H1D 1.09(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 C99 Br2 110.5(9) . . ?
Br1 C99 Br3 112.7(8) . . ?
Br1 C99 H99 107.9 . . ?
Br2 C99 Br3 109.6(9) . . ?
Br2 C99 H99 107.9 . . ?
Br3 C99 H99 107.9 . . ?
O1 Fe1 O6 99.2(3) . . ?
O1 Fe1 O26 89.6(3) . 2_656 ?
O5 Fe1 O1 85.3(2) . . ?
O5 Fe1 O6 174.5(3) . . ?
O5 Fe1 O26 93.8(3) . 2_656 ?
O10 Fe1 O1 92.4(3) . . ?
O10 Fe1 O5 91.7(3) . . ?
O10 Fe1 O6 85.0(3) . . ?
O10 Fe1 O26 174.3(3) . 2_656 ?
O10 Fe1 O30 91.8(3) . 2_656 ?
O26 Fe1 O6 89.4(3) 2_656 . ?
O30 Fe1 O1 170.9(3) 2_656 . ?
O30 Fe1 O5 86.5(3) 2_656 . ?
O30 Fe1 O6 89.2(3) 2_656 . ?
O30 Fe1 O26 87.0(2) 2_656 2_656 ?
O15 Fe2 O11 86.0(2) . . ?
O15 Fe2 O16 95.8(3) . . ?
O15 Fe2 O20 86.9(2) . . ?
O15 Fe2 O21 170.4(3) . . ?
O15 Fe2 O25 86.4(3) . . ?
O16 Fe2 O11 84.9(3) . . ?
O16 Fe2 O21 92.7(3) . . ?
O20 Fe2 O11 167.9(3) . . ?
O20 Fe2 O16 86.2(2) . . ?
O20 Fe2 O21 98.3(3) . . ?
O21 Fe2 O11 90.3(3) . . ?
O25 Fe2 O11 97.9(3) . . ?
O25 Fe2 O16 176.6(3) . . ?
O25 Fe2 O20 91.3(3) . . ?
O25 Fe2 O21 85.3(2) . . ?
C1 O1 Fe1 132.1(5) . . ?
C1 O2 C2 114.3(8) . . ?
C4 O3 C3 116.6(9) . . ?
C6 O5 Fe1 130.9(5) . . ?
C7 O6 Fe1 126.4(5) . . ?
C7 O7 C8 117.0(8) . . ?
C10 O8 C9 114.5(12) . . ?
C12 O10 Fe1 128.3(5) . . ?
C13 O11 Fe2 128.1(6) . . ?
C13 O12 C14 119.4(8) . . ?
C16 O13 C15 113.8(12) . . ?
C18 O15 Fe2 129.2(5) . . ?
C19 O16 Fe2 130.9(5) . . ?
C19 O17 C20 117.0(8) . . ?
C22 O18 C21 115.9(11) . . ?
C24 O20 Fe2 129.1(5) . . ?
C25 O21 Fe2 129.6(5) . . ?
C25 O22 C26 118.3(8) . . ?
C28 O23 C27 114.3(10) . . ?
C30 O25 Fe2 131.7(5) . . ?
C31 O26 Fe1 129.1(5) . 2_656 ?
C31 O27 C32 117.5(8) . . ?
C34 O28 C33 117.4(9) . . ?
C36 O30 Fe1 130.2(5) . 2_656 ?
O1 C1 O2 119.5(8) . . ?
O1 C1 C5 123.5(7) . . ?
O2 C1 C5 117.0(8) . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 C5 114.7(7) . . ?
O4 C4 O3 124.4(9) . . ?
O4 C4 C5 120.9(8) . . ?
C1 C5 C4 120.8(7) . . ?
C6 C5 C1 121.0(8) . . ?
C6 C5 C4 118.2(7) . . ?
O5 C6 C5 125.8(7) . . ?
O5 C6 C6 109.8(6) . 2_656 ?
C5 C6 C6 124.3(7) . 2_656 ?
O6 C7 O7 120.9(8) . . ?
O6 C7 C11 123.4(7) . . ?
O7 C7 C11 115.7(8) . . ?
O7 C8 H8A 109.5 . . ?
O7 C8 H8B 109.5 . . ?
O7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O8 C9 H9A 109.5 . . ?
O8 C9 H9B 109.5 . . ?
O8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O8 C10 C11 112.8(9) . . ?
O9 C10 O8 125.2(10) . . ?
O9 C10 C11 121.8(9) . . ?
C7 C11 C10 121.5(8) . . ?
C12 C11 C7 119.6(8) . . ?
C12 C11 C10 118.9(8) . . ?
O10 C12 C11 128.2(8) . . ?
O10 C12 C18 110.5(7) . . ?
C11 C12 C18 121.3(7) . . ?
O11 C13 O12 119.5(8) . . ?
O11 C13 C17 124.5(8) . . ?
O12 C13 C17 116.0(8) . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
O12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O13 C15 H15A 109.5 . . ?
O13 C15 H15B 109.5 . . ?
O13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C16 C17 111.3(8) . . ?
O14 C16 O13 123.8(10) . . ?
O14 C16 C17 124.7(10) . . ?
C13 C17 C16 118.0(8) . . ?
C18 C17 C13 122.1(8) . . ?
C18 C17 C16 119.4(8) . . ?
O15 C18 C12 111.3(7) . . ?
O15 C18 C17 126.2(8) . . ?
C17 C18 C12 122.5(7) . . ?
O16 C19 O17 119.3(8) . . ?
O16 C19 C23 124.0(8) . . ?
O17 C19 C23 116.5(8) . . ?
O17 C20 H20A 109.5 . . ?
O17 C20 H20B 109.5 . . ?
O17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O18 C21 H21A 109.5 . . ?
O18 C21 H21B 109.5 . . ?
O18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O18 C22 C23 110.5(8) . . ?
O19 C22 O18 123.7(9) . . ?
O19 C22 C23 125.8(9) . . ?
C19 C23 C22 116.9(8) . . ?
C24 C23 C19 121.8(8) . . ?
C24 C23 C22 121.3(8) . . ?
O20 C24 C23 126.4(7) . . ?
O20 C24 C24 110.8(7) . 2_656 ?
C23 C24 C24 122.7(7) . 2_656 ?
O21 C25 O22 118.4(8) . . ?
O21 C25 C29 126.2(8) . . ?
O22 C25 C29 115.3(7) . . ?
O22 C26 H26A 109.5 . . ?
O22 C26 H26B 109.5 . . ?
O22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O23 C27 H27A 109.5 . . ?
O23 C27 H27B 109.5 . . ?
O23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O23 C28 C29 112.6(8) . . ?
O24 C28 O23 123.7(8) . . ?
O24 C28 C29 123.7(9) . . ?
C25 C29 C28 122.0(7) . . ?
C30 C29 C25 119.3(7) . . ?
C30 C29 C28 118.6(8) . . ?
O25 C30 C29 126.5(8) . . ?
O25 C30 C36 111.6(7) . . ?
C29 C30 C36 121.8(7) . . ?
O26 C31 O27 119.2(8) . . ?
O26 C31 C35 125.0(8) . . ?
O27 C31 C35 115.8(7) . . ?
O27 C32 H32A 109.5 . . ?
O27 C32 H32B 109.5 . . ?
O27 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O28 C33 H33A 109.5 . . ?
O28 C33 H33B 109.5 . . ?
O28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O28 C34 C35 112.5(7) . . ?
O29 C34 O28 123.5(8) . . ?
O29 C34 C35 123.9(8) . . ?
C31 C35 C34 118.5(7) . . ?
C36 C35 C31 121.8(7) . . ?
C36 C35 C34 119.6(7) . . ?
O30 C36 C30 111.5(7) . . ?
O30 C36 C35 126.1(7) . . ?
C35 C36 C30 122.2(7) . . ?
H1A N1 H1B 113(5) . . ?
H1A N1 H1C 111(5) . . ?
H1A N1 H1D 108(5) . . ?
H1B N1 H1C 112(5) . . ?
H1B N1 H1D 108(5) . . ?
H1C N1 H1D 105(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
Fe1 O1 C1 O2 162.2(7) . . . . ?
Fe1 O1 C1 C5 -17.0(13) . . . . ?
Fe1 O5 C6 C5 -3.2(12) . . . . ?
Fe1 O5 C6 C6 -179.2(6) . . . 2_656 ?
Fe1 O6 C7 O7 151.1(7) . . . . ?
Fe1 O6 C7 C11 -28.7(12) . . . . ?
Fe1 O10 C12 C11 8.9(13) . . . . ?
Fe1 O10 C12 C18 -168.3(5) . . . . ?
Fe1 O26 C31 O27 168.6(7) 2_656 . . . ?
Fe1 O26 C31 C35 -9.6(14) 2_656 . . . ?
Fe1 O30 C36 C30 179.0(5) 2_656 . . . ?
Fe1 O30 C36 C35 -7.1(12) 2_656 . . . ?
Fe2 O11 C13 O12 -164.6(7) . . . . ?
Fe2 O11 C13 C17 13.6(13) . . . . ?
Fe2 O15 C18 C12 173.4(5) . . . . ?
Fe2 O15 C18 C17 -10.0(13) . . . . ?
Fe2 O16 C19 O17 163.5(7) . . . . ?
Fe2 O16 C19 C23 -11.1(14) . . . . ?
Fe2 O20 C24 C23 9.9(13) . . . . ?
Fe2 O20 C24 C24 -169.0(6) . . . 2_656 ?
Fe2 O21 C25 O22 169.0(6) . . . . ?
Fe2 O21 C25 C29 -8.9(13) . . . . ?
Fe2 O25 C30 C29 6.0(12) . . . . ?
Fe2 O25 C30 C36 -171.0(5) . . . . ?
O1 C1 C5 C4 -170.8(8) . . . . ?
O1 C1 C5 C6 9.6(13) . . . . ?
O2 C1 C5 C4 10.0(12) . . . . ?
O2 C1 C5 C6 -169.6(8) . . . . ?
O3 C4 C5 C1 36.5(12) . . . . ?
O3 C4 C5 C6 -143.9(9) . . . . ?
O4 C4 C5 C1 -145.2(9) . . . . ?
O4 C4 C5 C6 34.3(13) . . . . ?
O6 C7 C11 C10 -178.1(8) . . . . ?
O6 C7 C11 C12 2.6(13) . . . . ?
O7 C7 C11 C10 2.0(12) . . . . ?
O7 C7 C11 C12 -177.2(8) . . . . ?
O8 C10 C11 C7 40.0(13) . . . . ?
O8 C10 C11 C12 -140.7(10) . . . . ?
O9 C10 C11 C7 -145.2(10) . . . . ?
O9 C10 C11 C12 34.0(14) . . . . ?
O10 C12 C18 O15 66.9(9) . . . . ?
O10 C12 C18 C17 -109.9(9) . . . . ?
O11 C13 C17 C16 175.5(9) . . . . ?
O11 C13 C17 C18 4.0(14) . . . . ?
O12 C13 C17 C16 -6.3(13) . . . . ?
O12 C13 C17 C18 -177.8(9) . . . . ?
O13 C16 C17 C13 72.8(11) . . . . ?
O13 C16 C17 C18 -115.4(10) . . . . ?
O14 C16 C17 C13 -112.1(14) . . . . ?
O14 C16 C17 C18 59.7(16) . . . . ?
O16 C19 C23 C22 -175.9(9) . . . . ?
O16 C19 C23 C24 2.7(14) . . . . ?
O17 C19 C23 C22 9.3(13) . . . . ?
O17 C19 C23 C24 -172.1(9) . . . . ?
O18 C22 C23 C19 -132.6(9) . . . . ?
O18 C22 C23 C24 48.8(13) . . . . ?
O19 C22 C23 C19 46.6(15) . . . . ?
O19 C22 C23 C24 -132.0(12) . . . . ?
O21 C25 C29 C28 175.6(9) . . . . ?
O21 C25 C29 C30 -0.6(13) . . . . ?
O22 C25 C29 C28 -2.4(12) . . . . ?
O22 C25 C29 C30 -178.7(8) . . . . ?
O23 C28 C29 C25 49.7(12) . . . . ?
O23 C28 C29 C30 -134.0(9) . . . . ?
O24 C28 C29 C25 -131.1(10) . . . . ?
O24 C28 C29 C30 45.2(13) . . . . ?
O25 C30 C36 O30 59.0(9) . . . . ?
O25 C30 C36 C35 -115.1(8) . . . . ?
O26 C31 C35 C34 -173.2(9) . . . . ?
O26 C31 C35 C36 9.2(14) . . . . ?
O27 C31 C35 C34 8.6(13) . . . . ?
O27 C31 C35 C36 -169.0(9) . . . . ?
O28 C34 C35 C31 55.6(12) . . . . ?
O28 C34 C35 C36 -126.8(9) . . . . ?
O29 C34 C35 C31 -127.1(10) . . . . ?
O29 C34 C35 C36 50.5(14) . . . . ?
C1 C5 C6 O5 0.4(13) . . . . ?
C1 C5 C6 C6 175.8(8) . . . 2_656 ?
C2 O2 C1 O1 -2.9(16) . . . . ?
C2 O2 C1 C5 176.4(12) . . . . ?
C3 O3 C4 O4 -1.3(18) . . . . ?
C3 O3 C4 C5 176.9(13) . . . . ?
C4 C5 C6 O5 -179.2(8) . . . . ?
C4 C5 C6 C6 -3.8(13) . . . 2_656 ?
C7 C11 C12 O10 8.3(13) . . . . ?
C7 C11 C12 C18 -174.8(7) . . . . ?
C8 O7 C7 O6 1.8(13) . . . . ?
C8 O7 C7 C11 -178.3(8) . . . . ?
C9 O8 C10 O9 10(2) . . . . ?
C9 O8 C10 C11 -175.2(13) . . . . ?
C10 C11 C12 O10 -171.0(8) . . . . ?
C10 C11 C12 C18 5.9(12) . . . . ?
C11 C12 C18 O15 -110.5(9) . . . . ?
C11 C12 C18 C17 72.7(11) . . . . ?
C13 C17 C18 O15 -6.2(14) . . . . ?
C13 C17 C18 C12 170.1(8) . . . . ?
C14 O12 C13 O11 -2.6(15) . . . . ?
C14 O12 C13 C17 179.0(10) . . . . ?
C15 O13 C16 O14 5.7(19) . . . . ?
C15 O13 C16 C17 -179.2(12) . . . . ?
C16 C17 C18 O15 -177.6(8) . . . . ?
C16 C17 C18 C12 -1.3(13) . . . . ?
C19 C23 C24 O20 -2.1(14) . . . . ?
C19 C23 C24 C24 176.6(8) . . . 2_656 ?
C20 O17 C19 O16 -2.8(14) . . . . ?
C20 O17 C19 C23 172.2(10) . . . . ?
C21 O18 C22 O19 4.8(18) . . . . ?
C21 O18 C22 C23 -176.0(11) . . . . ?
C22 C23 C24 O20 176.4(8) . . . . ?
C22 C23 C24 C24 -4.9(14) . . . 2_656 ?
C25 C29 C30 O25 2.4(13) . . . . ?
C25 C29 C30 C36 179.1(7) . . . . ?
C26 O22 C25 O21 7.1(13) . . . . ?
C26 O22 C25 C29 -174.7(9) . . . . ?
C27 O23 C28 O24 1.5(16) . . . . ?
C27 O23 C28 C29 -179.3(10) . . . . ?
C28 C29 C30 O25 -174.0(8) . . . . ?
C28 C29 C30 C36 2.7(12) . . . . ?
C29 C30 C36 O30 -118.1(8) . . . . ?
C29 C30 C36 C35 67.8(11) . . . . ?
C31 C35 C36 O30 -0.6(14) . . . . ?
C31 C35 C36 C30 172.6(8) . . . . ?
C32 O27 C31 O26 -3.8(16) . . . . ?
C32 O27 C31 C35 174.6(11) . . . . ?
C33 O28 C34 O29 3.8(17) . . . . ?
C33 O28 C34 C35 -178.9(11) . . . . ?
C34 C35 C36 O30 -178.1(8) . . . . ?
C34 C35 C36 C30 -4.9(13) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.496 0.000 286.1 172.9 '1.5 CHBr3'
2 0.152 0.208 0.742 16.8 0.0 ?
3 0.500 0.996 1.000 286.1 172.3 '1.5 CHBr3'
4 0.348 0.708 0.258 16.8 0.0 ?
5 0.652 0.708 0.742 16.8 0.0 ?
6 0.848 0.208 0.258 16.8 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.559(7)
2 0.441(7)
