# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_Br-018-d_CCDC-2014803_R1
_database_code_depnum_ccdc_archive 'CCDC 2014803'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-29
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br1.08 C18 Cl4.92 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br1.08 Cl4.92 Fe2 N2 O12'
_chemical_formula_weight         1153.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl4.92 Br1.08 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8043(10)
_cell_length_b                   20.7436(17)
_cell_length_c                   12.2725(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.419(9)
_cell_angle_gamma                90
_cell_volume                     2696.1(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6106
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.6480
_cell_measurement_theta_min      1.9420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.046
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20498
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.593
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0502831000
_diffrn_orient_matrix_UB_12      -0.0162392000
_diffrn_orient_matrix_UB_13      0.0177210000
_diffrn_orient_matrix_UB_21      -0.0006842000
_diffrn_orient_matrix_UB_22      0.0240481000
_diffrn_orient_matrix_UB_23      0.0409562000
_diffrn_orient_matrix_UB_31      -0.0441559000
_diffrn_orient_matrix_UB_32      0.0181797000
_diffrn_orient_matrix_UB_33      -0.0384785000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3842
_reflns_number_total             6142
_reflns_odcompleteness_completeness 90.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6142
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0796
_refine_ls_restrained_S_all      1.118
_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)+(0.0367P)²+13.6623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1734
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-Br2
 1.88 with sigma of 0.02
 C3-Br1
 1.88 with sigma of 0.02
 C8-Br3
 1.88 with sigma of 0.02
3. Rigid bond restraints
 Cl2, Cl1, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3, Br2, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl1 \\sim Cl3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Br3 \\sim Br2 \\sim Br1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
5. Others
 Fixed Sof: Cl2(0.815) Cl3(0.83) Cl1(0.815) Br2(0.185) Br3(0.17) Br1(0.185)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C16(H16A,H16B), C19(H19A,H19B), C10(H10A,H10B), C11(H11A,
 H11B), C13(H13A,H13B), C20(H20A,H20B), C14(H14A,H14B)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C21(H21A,H21B,
 H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Fe01 Fe 0.54118(8) 0.68918(4) -0.02794(7) 0.0274(2) Uani 1 1 d . . . . .
Cl2 Cl 0.9277(6) 0.8308(2) 0.0559(5) 0.0296(16) Uani 0.815 1 d . . P A 2
Cl3 Cl 0.7981(7) 0.4807(7) 0.0201(15) 0.0320(13) Uani 0.83 1 d . . P B 2
Cl1 Cl 0.6598(5) 0.6675(2) 0.3877(4) 0.0351(16) Uani 0.815 1 d . . P C 2
O6 O 0.5976(4) 0.38119(19) 0.0275(3) 0.0301(9) Uani 1 1 d . . . . .
O2 O 0.5761(3) 0.68763(19) 0.1377(3) 0.0288(9) Uani 1 1 d . . . . .
O3 O 0.9026(3) 0.74671(19) 0.4413(3) 0.0276(9) Uani 1 1 d . . . . .
O1 O 0.6918(4) 0.74601(19) 0.0017(3) 0.0286(9) Uani 1 1 d . . . . .
O4 O 1.0115(3) 0.81258(18) 0.3070(3) 0.0278(9) Uani 1 1 d . . . . .
O5 O 0.6425(4) 0.60353(19) -0.0243(3) 0.0309(9) Uani 1 1 d . . . . .
N00B N 0.3890(5) 0.8600(2) 0.2462(4) 0.0332(12) Uani 1 1 d . . . . .
C2 C 0.6810(5) 0.7153(3) 0.1829(5) 0.0255(12) Uani 1 1 d . . . . .
C5 C 0.9084(5) 0.7838(3) 0.2610(4) 0.0248(12) Uani 1 1 d . . . . .
C1 C 0.7457(5) 0.7502(3) 0.1061(4) 0.0256(12) Uani 1 1 d . . . . .
C9 C 0.5591(5) 0.4385(3) 0.0154(5) 0.0281(13) Uani 1 1 d . . . . .
C4 C 0.8459(5) 0.7463(3) 0.3369(4) 0.0258(12) Uani 1 1 d . . . . .
C7 C 0.5830(5) 0.5527(3) -0.0112(4) 0.0271(13) Uani 1 1 d . . . . .
C8 C 0.6345(5) 0.4919(3) 0.0069(5) 0.0297(13) Uani 1 1 d D . . . .
C17 C 0.2840(6) 0.7489(3) 0.2498(5) 0.0374(15) Uani 1 1 d . . . . .
H17A H 0.2014 0.7629 0.2059 0.045 Uiso 1 1 calc R U . . .
H17B H 0.2831 0.7557 0.3294 0.045 Uiso 1 1 calc R U . . .
C6 C 0.8539(5) 0.7853(3) 0.1479(4) 0.0265(12) Uani 1 1 d D . . . .
C3 C 0.7355(5) 0.7135(3) 0.2974(4) 0.0267(12) Uani 1 1 d D . . . .
C16 C 0.3882(6) 0.7887(3) 0.2174(5) 0.0354(14) Uani 1 1 d . . . . .
H16A H 0.3821 0.7847 0.1361 0.043 Uiso 1 1 calc R U . . .
H16B H 0.4703 0.7700 0.2539 0.043 Uiso 1 1 calc R U . . .
C19 C 0.2675(6) 0.8908(3) 0.1833(5) 0.0371(15) Uani 1 1 d . . . . .
H19A H 0.2579 0.8798 0.1036 0.045 Uiso 1 1 calc R U . . .
H19B H 0.1955 0.8713 0.2102 0.045 Uiso 1 1 calc R U . . .
C10 C 0.3955(6) 0.8709(3) 0.3686(5) 0.0369(15) Uani 1 1 d . . . . .
H10A H 0.3123 0.8597 0.3856 0.044 Uiso 1 1 calc R U . . .
H10B H 0.4092 0.9175 0.3837 0.044 Uiso 1 1 calc R U . . .
C11 C 0.4966(6) 0.8339(3) 0.4486(5) 0.0400(15) Uani 1 1 d . . . . .
H11A H 0.5811 0.8434 0.4329 0.048 Uiso 1 1 calc R U . . .
H11B H 0.4812 0.7869 0.4403 0.048 Uiso 1 1 calc R U . . .
C13 C 0.5051(6) 0.8908(3) 0.2144(5) 0.0404(16) Uani 1 1 d . . . . .
H13A H 0.5121 0.9355 0.2431 0.048 Uiso 1 1 calc R U . . .
H13B H 0.5807 0.8671 0.2531 0.048 Uiso 1 1 calc R U . . .
C18 C 0.3040(6) 0.6777(3) 0.2287(6) 0.0407(16) Uani 1 1 d . . . . .
H18A H 0.3009 0.6708 0.1493 0.061 Uiso 1 1 calc R U . . .
H18B H 0.2375 0.6524 0.2524 0.061 Uiso 1 1 calc R U . . .
H18C H 0.3866 0.6642 0.2710 0.061 Uiso 1 1 calc R U . . .
C12 C 0.4897(7) 0.8556(3) 0.5676(5) 0.0459(17) Uani 1 1 d . . . . .
H12A H 0.4024 0.8521 0.5784 0.069 Uiso 1 1 calc R U . . .
H12B H 0.5179 0.9004 0.5785 0.069 Uiso 1 1 calc R U . . .
H12C H 0.5443 0.8279 0.6216 0.069 Uiso 1 1 calc R U . . .
C20 C 0.2592(7) 0.9637(3) 0.1937(6) 0.0490(18) Uani 1 1 d . . . . .
H20A H 0.3299 0.9844 0.1665 0.059 Uiso 1 1 calc R U . . .
H20B H 0.2653 0.9758 0.2726 0.059 Uiso 1 1 calc R U . . .
C14 C 0.5087(8) 0.8929(4) 0.0917(6) 0.054(2) Uani 1 1 d . . . . .
H14A H 0.4327 0.9154 0.0507 0.064 Uiso 1 1 calc R U . . .
H14B H 0.5086 0.8485 0.0623 0.064 Uiso 1 1 calc R U . . .
C15 C 0.6266(8) 0.9282(4) 0.0745(8) 0.071(3) Uani 1 1 d . . . . .
H15A H 0.6317 0.9265 -0.0043 0.107 Uiso 1 1 calc R U . . .
H15B H 0.7013 0.9075 0.1190 0.107 Uiso 1 1 calc R U . . .
H15C H 0.6227 0.9732 0.0977 0.107 Uiso 1 1 calc R U . . .
C21 C 0.1336(8) 0.9868(4) 0.1251(8) 0.074(3) Uani 1 1 d . . . . .
H21A H 0.1284 0.9749 0.0471 0.110 Uiso 1 1 calc R U . . .
H21B H 0.1278 1.0337 0.1312 0.110 Uiso 1 1 calc R U . . .
H21C H 0.0640 0.9666 0.1530 0.110 Uiso 1 1 calc R U . . .
Br2 Br 0.9309(13) 0.8322(6) 0.0535(11) 0.054(4) Uani 0.185 1 d D . P A -2
Br3 Br 0.8072(17) 0.4803(17) 0.007(3) 0.044(6) Uani 0.17 1 d D . P B -2
Br1 Br 0.6608(9) 0.6662(6) 0.3895(8) 0.062(4) Uani 0.185 1 d D . P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 O6 2.093(4) 3_665 ?
Fe01 O2 1.992(4) . ?
Fe01 O3 1.982(4) 4_575 ?
Fe01 O1 1.984(4) . ?
Fe01 O4 1.988(4) 4_575 ?
Fe01 O5 2.082(4) . ?
Cl2 C6 1.777(8) . ?
Cl3 C8 1.758(11) . ?
Cl1 C3 1.780(7) . ?
O6 Fe01 2.093(4) 3_665 ?
O6 C9 1.258(7) . ?
O2 C2 1.294(6) . ?
O3 Fe01 1.982(4) 4_676 ?
O3 C4 1.305(6) . ?
O1 C1 1.302(6) . ?
O4 Fe01 1.988(4) 4_676 ?
O4 C5 1.291(6) . ?
O5 C7 1.262(7) . ?
N00B C16 1.519(8) . ?
N00B C19 1.525(7) . ?
N00B C10 1.507(8) . ?
N00B C13 1.526(8) . ?
C2 C1 1.470(8) . ?
C2 C3 1.412(7) . ?
C5 C4 1.477(8) . ?
C5 C6 1.396(7) . ?
C1 C6 1.387(8) . ?
C9 C7 1.537(8) 3_665 ?
C9 C8 1.390(8) . ?
C4 C3 1.376(8) . ?
C7 C9 1.537(8) 3_665 ?
C7 C8 1.379(8) . ?
C8 Br3 1.882(18) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C16 1.511(8) . ?
C17 C18 1.522(9) . ?
C6 Br2 1.834(12) . ?
C3 Br1 1.803(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.523(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.524(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.545(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.515(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.524(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.519(10) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
O2 Fe01 O6 88.68(15) . 3_665 ?
O2 Fe01 O5 88.40(16) . . ?
O3 Fe01 O6 87.37(16) 4_575 3_665 ?
O3 Fe01 O2 100.87(16) 4_575 . ?
O3 Fe01 O1 101.40(16) 4_575 . ?
O3 Fe01 O4 81.64(15) 4_575 4_575 ?
O3 Fe01 O5 161.87(16) 4_575 . ?
O1 Fe01 O6 167.37(15) . 3_665 ?
O1 Fe01 O2 80.80(15) . . ?
O1 Fe01 O4 99.12(16) . 4_575 ?
O1 Fe01 O5 95.42(16) . . ?
O4 Fe01 O6 91.09(16) 4_575 3_665 ?
O4 Fe01 O2 177.47(16) 4_575 . ?
O4 Fe01 O5 89.09(16) 4_575 . ?
O5 Fe01 O6 77.21(16) . 3_665 ?
C9 O6 Fe01 116.1(4) . 3_665 ?
C2 O2 Fe01 113.8(4) . . ?
C4 O3 Fe01 112.5(3) . 4_676 ?
C1 O1 Fe01 114.2(3) . . ?
C5 O4 Fe01 112.9(3) . 4_676 ?
C7 O5 Fe01 115.9(4) . . ?
C16 N00B C19 109.0(5) . . ?
C16 N00B C13 108.4(5) . . ?
C19 N00B C13 111.4(5) . . ?
C10 N00B C16 112.0(5) . . ?
C10 N00B C19 107.9(5) . . ?
C10 N00B C13 108.2(5) . . ?
O2 C2 C1 115.5(5) . . ?
O2 C2 C3 124.9(5) . . ?
C3 C2 C1 119.6(5) . . ?
O4 C5 C4 115.5(5) . . ?
O4 C5 C6 125.6(5) . . ?
C6 C5 C4 118.9(5) . . ?
O1 C1 C2 115.0(5) . . ?
O1 C1 C6 125.4(5) . . ?
C6 C1 C2 119.6(5) . . ?
O6 C9 C7 114.9(5) . 3_665 ?
O6 C9 C8 125.2(5) . . ?
C8 C9 C7 119.9(5) . 3_665 ?
O3 C4 C5 115.5(5) . . ?
O3 C4 C3 123.8(5) . . ?
C3 C4 C5 120.7(5) . . ?
O5 C7 C9 115.3(5) . 3_665 ?
O5 C7 C8 125.9(5) . . ?
C8 C7 C9 118.9(5) . 3_665 ?
Cl3 C8 Br3 5.2(18) . . ?
C9 C8 Cl3 118.8(7) . . ?
C9 C8 Br3 119.6(12) . . ?
C7 C8 Cl3 120.1(7) . . ?
C7 C8 C9 121.1(5) . . ?
C7 C8 Br3 119.0(12) . . ?
H17A C17 H17B 108.1 . . ?
C16 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C16 C17 C18 110.3(5) . . ?
C18 C17 H17A 109.6 . . ?
C18 C17 H17B 109.6 . . ?
Cl2 C6 Br2 0.3(7) . . ?
C5 C6 Cl2 119.3(5) . . ?
C5 C6 Br2 119.0(6) . . ?
C1 C6 Cl2 119.7(4) . . ?
C1 C6 C5 121.0(5) . . ?
C1 C6 Br2 119.9(6) . . ?
Cl1 C3 Br1 0.8(5) . . ?
C2 C3 Cl1 118.8(4) . . ?
C2 C3 Br1 119.2(5) . . ?
C4 C3 Cl1 121.2(4) . . ?
C4 C3 C2 120.0(5) . . ?
C4 C3 Br1 120.8(5) . . ?
N00B C16 H16A 108.3 . . ?
N00B C16 H16B 108.3 . . ?
C17 C16 N00B 116.1(5) . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
N00B C19 H19A 108.4 . . ?
N00B C19 H19B 108.4 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N00B 115.7(5) . . ?
C20 C19 H19A 108.4 . . ?
C20 C19 H19B 108.4 . . ?
N00B C10 H10A 108.1 . . ?
N00B C10 H10B 108.1 . . ?
N00B C10 C11 116.9(5) . . ?
H10A C10 H10B 107.3 . . ?
C11 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
C10 C11 H11A 110.2 . . ?
C10 C11 H11B 110.2 . . ?
C10 C11 C12 107.5(5) . . ?
H11A C11 H11B 108.5 . . ?
C12 C11 H11A 110.2 . . ?
C12 C11 H11B 110.2 . . ?
N00B C13 H13A 108.1 . . ?
N00B C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 N00B 116.7(6) . . ?
C14 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C19 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
C19 C20 C21 109.1(6) . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C13 C14 C15 109.8(7) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
Fe01 O6 C9 C7 4.1(6) 3_665 . . 3_665 ?
Fe01 O6 C9 C8 -176.5(5) 3_665 . . . ?
Fe01 O2 C2 C1 8.1(6) . . . . ?
Fe01 O2 C2 C3 -171.3(5) . . . . ?
Fe01 O3 C4 C5 10.3(6) 4_676 . . . ?
Fe01 O3 C4 C3 -169.9(5) 4_676 . . . ?
Fe01 O1 C1 C2 -3.4(6) . . . . ?
Fe01 O1 C1 C6 178.2(5) . . . . ?
Fe01 O4 C5 C4 -10.2(6) 4_676 . . . ?
Fe01 O4 C5 C6 170.2(5) 4_676 . . . ?
Fe01 O5 C7 C9 7.7(6) . . . 3_665 ?
Fe01 O5 C7 C8 -171.8(5) . . . . ?
O6 C9 C8 Cl3 -3.1(11) . . . . ?
O6 C9 C8 C7 177.1(5) . . . . ?
O6 C9 C8 Br3 2.9(16) . . . . ?
O2 C2 C1 O1 -3.2(7) . . . . ?
O2 C2 C1 C6 175.3(5) . . . . ?
O2 C2 C3 Cl1 2.6(8) . . . . ?
O2 C2 C3 C4 -178.2(5) . . . . ?
O2 C2 C3 Br1 3.4(9) . . . . ?
O3 C4 C3 Cl1 -0.4(8) . . . . ?
O3 C4 C3 C2 -179.6(5) . . . . ?
O3 C4 C3 Br1 -1.2(9) . . . . ?
O1 C1 C6 Cl2 1.5(8) . . . . ?
O1 C1 C6 C5 -176.4(5) . . . . ?
O1 C1 C6 Br2 1.3(10) . . . . ?
O4 C5 C4 O3 -0.1(7) . . . . ?
O4 C5 C4 C3 -179.9(5) . . . . ?
O4 C5 C6 Cl2 -0.9(8) . . . . ?
O4 C5 C6 C1 177.0(5) . . . . ?
O4 C5 C6 Br2 -0.7(10) . . . . ?
O5 C7 C8 Cl3 3.1(11) . . . . ?
O5 C7 C8 C9 -177.0(5) . . . . ?
O5 C7 C8 Br3 -2.8(16) . . . . ?
N00B C19 C20 C21 179.2(6) . . . . ?
N00B C10 C11 C12 177.0(5) . . . . ?
N00B C13 C14 C15 177.0(6) . . . . ?
C2 C1 C6 Cl2 -176.8(5) . . . . ?
C2 C1 C6 C5 5.3(8) . . . . ?
C2 C1 C6 Br2 -177.0(7) . . . . ?
C5 C4 C3 Cl1 179.5(4) . . . . ?
C5 C4 C3 C2 0.2(8) . . . . ?
C5 C4 C3 Br1 178.7(6) . . . . ?
C1 C2 C3 Cl1 -176.7(5) . . . . ?
C1 C2 C3 C4 2.5(8) . . . . ?
C1 C2 C3 Br1 -175.9(6) . . . . ?
C9 C7 C8 Cl3 -176.4(8) 3_665 . . . ?
C9 C7 C8 C9 3.5(9) 3_665 . . . ?
C9 C7 C8 Br3 177.7(14) 3_665 . . . ?
C4 C5 C6 Cl2 179.6(5) . . . . ?
C4 C5 C6 C1 -2.5(8) . . . . ?
C4 C5 C6 Br2 179.7(7) . . . . ?
C7 C9 C8 Cl3 176.4(8) 3_665 . . . ?
C7 C9 C8 C7 -3.5(9) 3_665 . . . ?
C7 C9 C8 Br3 -177.7(14) 3_665 . . . ?
C6 C5 C4 O3 179.5(5) . . . . ?
C6 C5 C4 C3 -0.3(8) . . . . ?
C3 C2 C1 O1 176.2(5) . . . . ?
C3 C2 C1 C6 -5.3(8) . . . . ?
C16 N00B C19 C20 -174.0(6) . . . . ?
C16 N00B C10 C11 49.2(7) . . . . ?
C16 N00B C13 C14 66.0(7) . . . . ?
C19 N00B C16 C17 -62.4(7) . . . . ?
C19 N00B C10 C11 169.2(5) . . . . ?
C19 N00B C13 C14 -53.9(7) . . . . ?
C10 N00B C16 C17 56.9(7) . . . . ?
C10 N00B C19 C20 64.1(7) . . . . ?
C10 N00B C13 C14 -172.3(6) . . . . ?
C13 N00B C16 C17 176.2(5) . . . . ?
C13 N00B C19 C20 -54.4(7) . . . . ?
C13 N00B C10 C11 -70.3(7) . . . . ?
C18 C17 C16 N00B -173.2(5) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.801
####################################################################### 
# 
# 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_Br-018_CCDC-2014808_R1
_database_code_depnum_ccdc_archive 'CCDC 2014808'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-29
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br1.08 C18 Cl4.92 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Br1.08 Cl4.92 Fe2 N2 O15'
_chemical_formula_weight         1287.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl4.92 Br1.08 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.2837(8)
_cell_length_b                   21.7936(7)
_cell_length_c                   14.4042(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.042(4)
_cell_angle_gamma                90
_cell_volume                     6054.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8973
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.0610
_cell_measurement_theta_min      1.7500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2662
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.033
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_unetI/netI     0.1250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.366
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0149811000
_diffrn_orient_matrix_UB_12      -0.0019088000
_diffrn_orient_matrix_UB_13      -0.0514086000
_diffrn_orient_matrix_UB_21      -0.0335621000
_diffrn_orient_matrix_UB_22      0.0016711000
_diffrn_orient_matrix_UB_23      0.0053037000
_diffrn_orient_matrix_UB_31      0.0008406000
_diffrn_orient_matrix_UB_32      0.0324588000
_diffrn_orient_matrix_UB_33      -0.0033114000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6833
_reflns_number_total             13874
_reflns_odcompleteness_completeness 91.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.40
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         13874
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1758
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      1.015
_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)+(0.0774P)²+13.1458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.2207
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-Br5
 1.88 with sigma of 0.02
 Cl1-C3
 1.73 with sigma of 0.02
 C3-Br1
 1.88 with sigma of 0.02
 C6-Br2
 1.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(Cl1) = Uanis(Br1)
Uanis(Cl2) = Uanis(Br2)
Uanis(Cl6) = Uanis(Br6)
4. Others
 Fixed Sof: Cl5(0.815) Cl2(0.825) Cl3(0.82) Cl4(0.82) Cl6(0.815) Cl1(0.825)
 O15(0.5) O16(0.5) Br3(0.18) Br4(0.18) Br6(0.185) Br2(0.175) Br5(0.185)
 Br1(0.175)
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C38(H38A,H38B), C37(H37A,H37B), C19(H19A,H19B), C25(H25A,
 H25B), C22(H22A,H22B), C29(H29A,H29B), C41(H41A,H41B), C34(H34A,H34B),
 C31(H31A,H31B), C28(H28A,H28B), C20(H20A,H20B), C26(H26A,H26B), C35(H35A,H35B),
  C23(H23A,H23B), C32(H32A,H32B)
5.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C39(H39A,H39B,H39C), C21(H21A,H21B,H21C), C30(H30A,H30B,
 H30C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22019(5) 0.31959(4) 0.39456(6) 0.0227(2) Uani 1 1 d . . . . .
Fe2 Fe 0.24046(5) 0.68311(4) 0.40945(6) 0.0223(2) Uani 1 1 d . . . . .
Cl5 Cl 0.1030(3) 0.6729(4) 0.0551(8) 0.0209(11) Uani 0.815 1 d . . P A 2
Cl2 Cl 0.0798(6) 0.1799(4) 0.5327(9) 0.0261(12) Uani 0.825 1 d . . P B 2
Cl3 Cl 0.0947(10) 0.5077(7) 0.4741(15) 0.0271(19) Uani 0.82 1 d . . P C 2
Cl4 Cl 0.3797(3) 0.4981(4) 0.3705(6) 0.0239(10) Uani 0.82 1 d . . P D 2
Cl6 Cl 0.3837(8) 0.8160(4) 0.2605(10) 0.0320(15) Uani 0.815 1 d . . P E 2
Cl1 Cl 0.3648(3) 0.3143(2) 0.7467(5) 0.0312(10) Uani 0.825 1 d D . P F 2
O10 O 0.1868(2) 0.75697(17) -0.0378(3) 0.0232(9) Uani 1 1 d . . . . .
O4 O 0.1614(2) 0.17999(18) 0.7540(3) 0.0241(9) Uani 1 1 d . . . . .
O1 O 0.1650(2) 0.26176(18) 0.4485(3) 0.0253(10) Uani 1 1 d . . . . .
O6 O 0.1814(2) 0.61160(18) 0.4362(3) 0.0248(10) Uani 1 1 d . . . . .
O7 O 0.2983(2) 0.60701(18) 0.3966(3) 0.0248(10) Uani 1 1 d . . . . .
O12 O 0.2969(2) 0.73856(18) 0.3547(3) 0.0254(10) Uani 1 1 d . . . . .
O2 O 0.2813(2) 0.31483(18) 0.5341(3) 0.0260(10) Uani 1 1 d . . . . .
O5 O 0.1668(2) 0.39645(18) 0.4203(3) 0.0260(10) Uani 1 1 d . . . . .
O11 O 0.3021(2) 0.81365(18) 0.0484(3) 0.0267(10) Uani 1 1 d . . . . .
O3 O 0.2761(2) 0.23668(18) 0.8394(3) 0.0261(10) Uani 1 1 d . . . . .
O9 O 0.1832(2) 0.68047(17) 0.2699(3) 0.0237(9) Uani 1 1 d . . . . .
O8 O 0.2841(2) 0.39203(18) 0.3822(3) 0.0262(10) Uani 1 1 d . . . . .
N2 N 0.0479(3) 0.8521(2) 0.2283(4) 0.0310(13) Uani 1 1 d . . . . .
N1 N 0.5088(3) 0.7004(2) 0.5080(4) 0.0311(13) Uani 1 1 d . . . . .
C13 C 0.2086(3) 0.7111(3) 0.2117(4) 0.0224(13) Uani 1 1 d . . . . .
C15 C 0.2111(3) 0.7503(3) 0.0560(4) 0.0200(13) Uani 1 1 d . . . . .
C18 C 0.2739(3) 0.7442(3) 0.2605(4) 0.0238(14) Uani 1 1 d . . . . .
C10 C 0.2717(3) 0.5558(3) 0.4040(4) 0.0227(14) Uani 1 1 d . . . . .
C16 C 0.2760(3) 0.7832(3) 0.1047(4) 0.0232(14) Uani 1 1 d . . . . .
C5 C 0.1872(3) 0.2107(3) 0.6974(4) 0.0229(14) Uani 1 1 d . . . . .
C14 C 0.1810(3) 0.7142(3) 0.1107(4) 0.0225(14) Uani 1 1 d D . . . .
C6 C 0.1583(3) 0.2166(3) 0.5965(4) 0.0226(13) Uani 1 1 d D . . . .
C9 C 0.2023(3) 0.5584(3) 0.4270(4) 0.0239(14) Uani 1 1 d . . . . .
C2 C 0.2549(3) 0.2840(3) 0.5903(4) 0.0230(14) Uani 1 1 d . . . . .
C4 C 0.2529(3) 0.2432(3) 0.7452(4) 0.0252(14) Uani 1 1 d . . . . .
C17 C 0.3050(3) 0.7788(3) 0.2055(5) 0.0272(15) Uani 1 1 d . . . . .
C7 C 0.1952(3) 0.4473(3) 0.4197(4) 0.0257(14) Uani 1 1 d . . . . .
C12 C 0.2644(3) 0.4453(3) 0.3970(4) 0.0257(14) Uani 1 1 d . . . . .
C3 C 0.2846(3) 0.2782(3) 0.6908(4) 0.0271(15) Uani 1 1 d D . . . .
C11 C 0.2993(3) 0.4990(3) 0.3924(4) 0.0244(14) Uani 1 1 d . . . . .
C1 C 0.1892(3) 0.2528(3) 0.5413(4) 0.0239(14) Uani 1 1 d . . . . .
C8 C 0.1694(3) 0.5043(3) 0.4374(4) 0.0251(14) Uani 1 1 d . . . . .
C40 C 0.0594(3) 0.7838(3) 0.2498(5) 0.0316(16) Uani 1 1 d . . . . .
H40A H 0.0847 0.7668 0.2067 0.038 Uiso 1 1 calc R U . . .
H40B H 0.0898 0.7790 0.3179 0.038 Uiso 1 1 calc R U . . .
C38 C 0.0140(4) 0.8307(3) 0.0425(5) 0.0392(18) Uani 1 1 d . . . . .
H38A H 0.0144 0.7857 0.0522 0.047 Uiso 1 1 calc R U . . .
H38B H 0.0600 0.8432 0.0391 0.047 Uiso 1 1 calc R U . . .
C37 C -0.0011(4) 0.8627(3) 0.1264(5) 0.0370(17) Uani 1 1 d . . . . .
H37A H -0.0481 0.8504 0.1261 0.044 Uiso 1 1 calc R U . . .
H37B H -0.0025 0.9073 0.1134 0.044 Uiso 1 1 calc R U . . .
C19 C 0.5309(4) 0.6614(3) 0.6000(5) 0.0368(17) Uani 1 1 d . . . . .
H19A H 0.5738 0.6391 0.6015 0.044 Uiso 1 1 calc R U . . .
H19B H 0.5426 0.6891 0.6572 0.044 Uiso 1 1 calc R U . . .
C25 C 0.5712(3) 0.7395(3) 0.5097(5) 0.0357(17) Uani 1 1 d . . . . .
H25A H 0.5860 0.7621 0.5724 0.043 Uiso 1 1 calc R U . . .
H25B H 0.6096 0.7117 0.5089 0.043 Uiso 1 1 calc R U . . .
C42 C 0.0154(4) 0.6779(3) 0.2487(6) 0.0408(18) Uani 1 1 d . . . . .
H42A H 0.0395 0.6670 0.2018 0.061 Uiso 1 1 calc R U . . .
H42B H -0.0264 0.6527 0.2369 0.061 Uiso 1 1 calc R U . . .
H42C H 0.0461 0.6707 0.3152 0.061 Uiso 1 1 calc R U . . .
C22 C 0.4468(3) 0.7397(3) 0.5068(5) 0.0346(17) Uani 1 1 d . . . . .
H22A H 0.4308 0.7614 0.4433 0.042 Uiso 1 1 calc R U . . .
H22B H 0.4088 0.7122 0.5103 0.042 Uiso 1 1 calc R U . . .
C29 C 0.5407(4) 0.6154(3) 0.4069(5) 0.0406(18) Uani 1 1 d . . . . .
H29A H 0.5480 0.5832 0.4575 0.049 Uiso 1 1 calc R U . . .
H29B H 0.5853 0.6368 0.4160 0.049 Uiso 1 1 calc R U . . .
C41 C -0.0050(3) 0.7456(3) 0.2368(5) 0.0342(16) Uani 1 1 d . . . . .
H41A H -0.0384 0.7528 0.1712 0.041 Uiso 1 1 calc R U . . .
H41B H -0.0275 0.7575 0.2862 0.041 Uiso 1 1 calc R U . . .
C34 C 0.0156(4) 0.8797(3) 0.2999(5) 0.0366(17) Uani 1 1 d . . . . .
H34A H 0.0460 0.8708 0.3669 0.044 Uiso 1 1 calc R U . . .
H34B H -0.0294 0.8594 0.2916 0.044 Uiso 1 1 calc R U . . .
C39 C -0.0416(4) 0.8478(3) -0.0513(5) 0.0446(19) Uani 1 1 d . . . . .
H39A H -0.0401 0.8192 -0.1031 0.067 Uiso 1 1 calc R U . . .
H39B H -0.0336 0.8896 -0.0700 0.067 Uiso 1 1 calc R U . . .
H39C H -0.0873 0.8455 -0.0414 0.067 Uiso 1 1 calc R U . . .
C31 C 0.1178(4) 0.8811(3) 0.2365(6) 0.0437(19) Uani 1 1 d . . . . .
H31A H 0.1391 0.8579 0.1941 0.052 Uiso 1 1 calc R U . . .
H31B H 0.1096 0.9235 0.2107 0.052 Uiso 1 1 calc R U . . .
C28 C 0.4868(4) 0.6608(3) 0.4170(5) 0.0361(17) Uani 1 1 d . . . . .
H28A H 0.4446 0.6378 0.4166 0.043 Uiso 1 1 calc R U . . .
H28B H 0.4741 0.6880 0.3591 0.043 Uiso 1 1 calc R U . . .
C20 C 0.4781(4) 0.6149(3) 0.6110(5) 0.0395(18) Uani 1 1 d . . . . .
H20A H 0.4732 0.5814 0.5630 0.047 Uiso 1 1 calc R U . . .
H20B H 0.4324 0.6349 0.5986 0.047 Uiso 1 1 calc R U . . .
C26 C 0.5614(4) 0.7856(4) 0.4278(6) 0.046(2) Uani 1 1 d . . . . .
H26A H 0.5558 0.7637 0.3656 0.056 Uiso 1 1 calc R U . . .
H26B H 0.5189 0.8100 0.4206 0.056 Uiso 1 1 calc R U . . .
C21 C 0.5026(4) 0.5889(3) 0.7149(5) 0.048(2) Uani 1 1 d . . . . .
H21A H 0.4693 0.5581 0.7222 0.071 Uiso 1 1 calc R U . . .
H21B H 0.5059 0.6221 0.7619 0.071 Uiso 1 1 calc R U . . .
H21C H 0.5482 0.5697 0.7269 0.071 Uiso 1 1 calc R U . . .
C35 C 0.0038(5) 0.9487(3) 0.2899(6) 0.049(2) Uani 1 1 d . . . . .
H35A H 0.0477 0.9696 0.2925 0.059 Uiso 1 1 calc R U . . .
H35B H -0.0309 0.9581 0.2261 0.059 Uiso 1 1 calc R U . . .
O14 O 0.1321(4) 1.0350(3) 0.2748(8) 0.126(3) Uani 1 1 d . U . . .
C30 C 0.5157(4) 0.5861(4) 0.3048(5) 0.054(2) Uani 1 1 d . . . . .
H30A H 0.5140 0.6174 0.2553 0.082 Uiso 1 1 calc R U . . .
H30B H 0.4693 0.5687 0.2936 0.082 Uiso 1 1 calc R U . . .
H30C H 0.5479 0.5535 0.3005 0.082 Uiso 1 1 calc R U . . .
C23 C 0.4583(4) 0.7862(4) 0.5861(6) 0.055(2) Uani 1 1 d . . . . .
H23A H 0.5000 0.8109 0.5898 0.066 Uiso 1 1 calc R U . . .
H23B H 0.4660 0.7653 0.6496 0.066 Uiso 1 1 calc R U . . .
C32 C 0.1691(4) 0.8836(4) 0.3381(6) 0.059(3) Uani 1 1 d . . . . .
H32A H 0.1752 0.8421 0.3674 0.071 Uiso 1 1 calc R U . . .
H32B H 0.1513 0.9110 0.3797 0.071 Uiso 1 1 calc R U . . .
C24 C 0.3939(4) 0.8288(3) 0.5647(6) 0.053(2) Uani 1 1 d . . . . .
H24A H 0.3879 0.8508 0.5034 0.079 Uiso 1 1 calc R U . . .
H24B H 0.4006 0.8583 0.6181 0.079 Uiso 1 1 calc R U . . .
H24C H 0.3525 0.8040 0.5592 0.079 Uiso 1 1 calc R U . . .
C27 C 0.6234(4) 0.8279(3) 0.4495(7) 0.056(2) Uani 1 1 d . . . . .
H27A H 0.6201 0.8533 0.3920 0.085 Uiso 1 1 calc R U . . .
H27B H 0.6660 0.8035 0.4657 0.085 Uiso 1 1 calc R U . . .
H27C H 0.6244 0.8545 0.5049 0.085 Uiso 1 1 calc R U . . .
C33 C 0.2383(4) 0.9074(4) 0.3336(7) 0.072(3) Uani 1 1 d . . . . .
H33A H 0.2517 0.8849 0.2833 0.108 Uiso 1 1 calc R U . . .
H33B H 0.2736 0.9014 0.3971 0.108 Uiso 1 1 calc R U . . .
H33C H 0.2343 0.9512 0.3175 0.108 Uiso 1 1 calc R U . . .
O13 O 0.3329(6) 0.4957(4) 0.0820(9) 0.160(5) Uani 1 1 d . . . . .
C46 C 0.1752(5) 1.0743(4) 0.2699(8) 0.073(3) Uani 1 1 d . . . . .
C36 C -0.0217(6) 0.9719(4) 0.3715(7) 0.089(4) Uani 1 1 d . . . . .
H36A H 0.0058 0.9533 0.4334 0.133 Uiso 1 1 calc R U . . .
H36B H -0.0706 0.9607 0.3582 0.133 Uiso 1 1 calc R U . . .
H36C H -0.0169 1.0166 0.3760 0.133 Uiso 1 1 calc R U . . .
C43 C 0.2795(7) 0.4974(5) 0.1035(9) 0.090(4) Uani 1 1 d . . . . .
C48 C 0.2158(6) 1.0685(5) 0.1977(7) 0.089(3) Uani 1 1 d . . . . .
H48A H 0.2038 1.0298 0.1619 0.133 Uiso 1 1 calc R U . . .
H48B H 0.2656 1.0692 0.2330 0.133 Uiso 1 1 calc R U . . .
H48C H 0.2041 1.1029 0.1515 0.133 Uiso 1 1 calc R U . . .
C45 C 0.2522(6) 0.5580(5) 0.1252(8) 0.099(4) Uani 1 1 d . . . . .
H45A H 0.2739 0.5683 0.1942 0.148 Uiso 1 1 calc R U . . .
H45B H 0.2018 0.5553 0.1113 0.148 Uiso 1 1 calc R U . . .
H45C H 0.2631 0.5899 0.0843 0.148 Uiso 1 1 calc R U . . .
C47 C 0.1859(6) 1.1289(5) 0.3363(8) 0.102(4) Uani 1 1 d . . . . .
H47A H 0.1639 1.1650 0.2987 0.152 Uiso 1 1 calc R U . . .
H47B H 0.2357 1.1365 0.3655 0.152 Uiso 1 1 calc R U . . .
H47C H 0.1651 1.1209 0.3881 0.152 Uiso 1 1 calc R U . . .
C44 C 0.2397(7) 0.4422(5) 0.1164(10) 0.122(5) Uani 1 1 d . . . . .
H44A H 0.2673 0.4053 0.1170 0.183 Uiso 1 1 calc R U . . .
H44B H 0.1962 0.4398 0.0624 0.183 Uiso 1 1 calc R U . . .
H44C H 0.2294 0.4454 0.1784 0.183 Uiso 1 1 calc R U . . .
O15 O 0.442(2) 0.5035(13) -0.068(2) 0.242(16) Uani 0.5 1 d . U P G 3
O16 O 0.4881(14) 0.439(2) -0.012(3) 0.279(18) Uani 0.5 1 d . U P G -3
Br3 Br 0.0845(19) 0.5134(15) 0.464(3) 0.033(5) Uani 0.18 1 d . . P C -2
Br4 Br 0.3809(9) 0.4934(9) 0.3623(15) 0.061(5) Uani 0.18 1 d . . P D -2
Br6 Br 0.3790(15) 0.8290(9) 0.267(2) 0.0320(15) Uani 0.185 1 d . . P E -2
Br2 Br 0.0801(13) 0.1686(10) 0.539(2) 0.0261(12) Uani 0.175 1 d D . P B -2
Br5 Br 0.1040(9) 0.6703(9) 0.0441(17) 0.048(5) Uani 0.185 1 d D . P A -2
Br1 Br 0.3562(7) 0.3294(6) 0.7554(11) 0.0312(10) Uani 0.175 1 d D . P F -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O4 2.006(4) 4_565 ?
Fe1 O1 1.996(4) . ?
Fe1 O2 2.011(4) . ?
Fe1 O5 2.089(4) . ?
Fe1 O3 1.994(4) 4_565 ?
Fe1 O8 2.085(4) . ?
Fe2 O10 1.994(4) 4_576 ?
Fe2 O6 2.072(4) . ?
Fe2 O7 2.073(4) . ?
Fe2 O12 1.988(4) . ?
Fe2 O11 2.006(4) 4_576 ?
Fe2 O9 1.987(4) . ?
Cl5 C14 1.781(9) . ?
Cl2 C6 1.764(11) . ?
Cl3 C8 1.75(2) . ?
Cl4 C11 1.756(9) . ?
Cl6 C17 1.745(15) . ?
Cl1 C3 1.762(8) . ?
O10 Fe2 1.994(4) 4_575 ?
O10 C15 1.296(6) . ?
O4 Fe1 2.006(4) 4_566 ?
O4 C5 1.286(7) . ?
O1 C1 1.288(7) . ?
O6 C9 1.256(7) . ?
O7 C10 1.258(7) . ?
O12 C18 1.296(7) . ?
O2 C2 1.289(7) . ?
O5 C7 1.252(7) . ?
O11 Fe2 2.006(4) 4_575 ?
O11 C16 1.284(7) . ?
O3 Fe1 1.994(4) 4_566 ?
O3 C4 1.299(7) . ?
O9 C13 1.297(7) . ?
O8 C12 1.266(7) . ?
N2 C40 1.525(8) . ?
N2 C37 1.513(8) . ?
N2 C34 1.507(8) . ?
N2 C31 1.523(8) . ?
N1 C19 1.521(8) . ?
N1 C25 1.519(8) . ?
N1 C22 1.517(8) . ?
N1 C28 1.517(8) . ?
C13 C18 1.480(8) . ?
C13 C14 1.388(8) . ?
C15 C16 1.471(8) . ?
C15 C14 1.383(8) . ?
C18 C17 1.380(8) . ?
C10 C9 1.542(8) . ?
C10 C11 1.391(8) . ?
C16 C17 1.391(8) . ?
C5 C6 1.394(8) . ?
C5 C4 1.478(8) . ?
C14 Br5 1.831(15) . ?
C6 C1 1.399(8) . ?
C6 Br2 1.867(17) . ?
C9 C8 1.386(8) . ?
C2 C3 1.390(8) . ?
C2 C1 1.468(8) . ?
C4 C3 1.386(8) . ?
C17 Br6 1.85(3) . ?
C7 C12 1.536(9) . ?
C7 C8 1.401(8) . ?
C12 C11 1.380(8) . ?
C3 Br1 1.840(13) . ?
C11 Br4 1.84(2) . ?
C8 Br3 1.89(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.511(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.506(9) . ?
C38 C39 1.514(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.518(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.515(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 C41 1.527(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.490(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C28 1.514(9) . ?
C29 C30 1.538(9) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.523(9) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.512(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.532(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.513(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.510(10) . ?
O14 C46 1.242(11) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.553(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.515(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O13 C43 1.216(12) . ?
C46 C48 1.518(13) . ?
C46 C47 1.499(13) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C43 C45 1.503(13) . ?
C43 C44 1.491(15) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O15 O16 1.74(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Fe1 O2 176.90(17) 4_565 . ?
O4 Fe1 O5 89.81(16) 4_565 . ?
O4 Fe1 O8 95.80(17) 4_565 . ?
O1 Fe1 O4 99.55(17) . 4_565 ?
O1 Fe1 O2 79.91(16) . . ?
O1 Fe1 O5 93.04(16) . . ?
O1 Fe1 O8 161.77(17) . . ?
O2 Fe1 O5 93.27(17) . . ?
O2 Fe1 O8 85.27(16) . . ?
O3 Fe1 O4 80.47(16) 4_565 4_565 ?
O3 Fe1 O1 102.90(17) 4_565 . ?
O3 Fe1 O2 96.64(17) 4_565 . ?
O3 Fe1 O5 162.47(17) 4_565 . ?
O3 Fe1 O8 89.23(16) 4_565 . ?
O8 Fe1 O5 77.19(16) . . ?
O10 Fe2 O6 90.41(16) 4_576 . ?
O10 Fe2 O7 161.56(17) 4_576 . ?
O10 Fe2 O11 80.91(16) 4_576 4_576 ?
O6 Fe2 O7 77.91(16) . . ?
O12 Fe2 O10 101.64(17) . 4_576 ?
O12 Fe2 O6 165.35(16) . . ?
O12 Fe2 O7 92.27(16) . . ?
O12 Fe2 O11 96.72(17) . 4_576 ?
O11 Fe2 O6 93.36(17) 4_576 . ?
O11 Fe2 O7 85.54(16) 4_576 . ?
O9 Fe2 O10 100.81(16) . 4_576 ?
O9 Fe2 O6 88.62(16) . . ?
O9 Fe2 O7 93.21(16) . . ?
O9 Fe2 O12 81.02(16) . . ?
O9 Fe2 O11 177.38(18) . 4_576 ?
C15 O10 Fe2 113.3(4) . 4_575 ?
C5 O4 Fe1 114.0(4) . 4_566 ?
C1 O1 Fe1 114.9(4) . . ?
C9 O6 Fe2 116.2(4) . . ?
C10 O7 Fe2 115.6(4) . . ?
C18 O12 Fe2 114.1(4) . . ?
C2 O2 Fe1 114.0(4) . . ?
C7 O5 Fe1 116.3(4) . . ?
C16 O11 Fe2 113.4(4) . 4_575 ?
C4 O3 Fe1 114.7(4) . 4_566 ?
C13 O9 Fe2 114.5(4) . . ?
C12 O8 Fe1 116.3(4) . . ?
C37 N2 C40 111.0(5) . . ?
C37 N2 C31 109.1(5) . . ?
C34 N2 C40 108.9(5) . . ?
C34 N2 C37 108.0(5) . . ?
C34 N2 C31 111.8(5) . . ?
C31 N2 C40 108.0(5) . . ?
C25 N1 C19 106.3(5) . . ?
C22 N1 C19 110.2(5) . . ?
C22 N1 C25 111.5(5) . . ?
C28 N1 C19 111.2(5) . . ?
C28 N1 C25 110.8(5) . . ?
C28 N1 C22 106.8(5) . . ?
O9 C13 C18 114.8(5) . . ?
O9 C13 C14 126.1(5) . . ?
C14 C13 C18 119.1(5) . . ?
O10 C15 C16 116.0(5) . . ?
O10 C15 C14 124.5(5) . . ?
C14 C15 C16 119.5(5) . . ?
O12 C18 C13 115.5(5) . . ?
O12 C18 C17 124.9(6) . . ?
C17 C18 C13 119.6(5) . . ?
O7 C10 C9 115.5(5) . . ?
O7 C10 C11 125.5(6) . . ?
C11 C10 C9 119.0(5) . . ?
O11 C16 C15 115.7(5) . . ?
O11 C16 C17 124.8(6) . . ?
C17 C16 C15 119.5(5) . . ?
O4 C5 C6 125.9(5) . . ?
O4 C5 C4 116.1(5) . . ?
C6 C5 C4 118.0(5) . . ?
Cl5 C14 Br5 5.3(12) . . ?
C13 C14 Cl5 117.5(6) . . ?
C13 C14 Br5 121.7(9) . . ?
C15 C14 Cl5 121.2(6) . . ?
C15 C14 C13 121.2(5) . . ?
C15 C14 Br5 117.0(9) . . ?
Cl2 C6 Br2 7.6(10) . . ?
C5 C6 Cl2 121.5(6) . . ?
C5 C6 C1 121.7(5) . . ?
C5 C6 Br2 116.0(9) . . ?
C1 C6 Cl2 116.8(6) . . ?
C1 C6 Br2 122.1(9) . . ?
O6 C9 C10 114.6(5) . . ?
O6 C9 C8 125.8(6) . . ?
C8 C9 C10 119.6(5) . . ?
O2 C2 C3 124.8(6) . . ?
O2 C2 C1 115.6(5) . . ?
C3 C2 C1 119.6(5) . . ?
O3 C4 C5 114.6(5) . . ?
O3 C4 C3 124.8(6) . . ?
C3 C4 C5 120.6(5) . . ?
Cl6 C17 Br6 9.7(9) . . ?
C18 C17 Cl6 120.7(7) . . ?
C18 C17 C16 121.0(6) . . ?
C18 C17 Br6 119.9(10) . . ?
C16 C17 Cl6 118.3(7) . . ?
C16 C17 Br6 118.5(10) . . ?
O5 C7 C12 115.4(5) . . ?
O5 C7 C8 125.7(6) . . ?
C8 C7 C12 118.9(5) . . ?
O8 C12 C7 114.8(5) . . ?
O8 C12 C11 125.2(6) . . ?
C11 C12 C7 120.0(5) . . ?
Cl1 C3 Br1 12.8(4) . . ?
C2 C3 Cl1 118.5(5) . . ?
C2 C3 Br1 119.5(7) . . ?
C4 C3 Cl1 120.7(5) . . ?
C4 C3 C2 120.8(5) . . ?
C4 C3 Br1 118.6(7) . . ?
Cl4 C11 Br4 4.4(9) . . ?
C10 C11 Cl4 117.5(5) . . ?
C10 C11 Br4 120.8(7) . . ?
C12 C11 Cl4 121.2(5) . . ?
C12 C11 C10 121.3(6) . . ?
C12 C11 Br4 117.8(7) . . ?
O1 C1 C6 125.6(6) . . ?
O1 C1 C2 115.2(5) . . ?
C6 C1 C2 119.2(5) . . ?
Cl3 C8 Br3 6.7(18) . . ?
C9 C8 Cl3 119.1(7) . . ?
C9 C8 C7 120.9(6) . . ?
C9 C8 Br3 115.6(11) . . ?
C7 C8 Cl3 120.0(7) . . ?
C7 C8 Br3 123.2(11) . . ?
N2 C40 H40A 108.3 . . ?
N2 C40 H40B 108.3 . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 N2 116.1(5) . . ?
C41 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
H38A C38 H38B 108.3 . . ?
C37 C38 H38A 109.9 . . ?
C37 C38 H38B 109.9 . . ?
C37 C38 C39 108.8(6) . . ?
C39 C38 H38A 109.9 . . ?
C39 C38 H38B 109.9 . . ?
N2 C37 H37A 107.8 . . ?
N2 C37 H37B 107.8 . . ?
C38 C37 N2 118.2(6) . . ?
C38 C37 H37A 107.8 . . ?
C38 C37 H37B 107.8 . . ?
H37A C37 H37B 107.1 . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N1 115.9(6) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
N1 C25 H25A 108.1 . . ?
N1 C25 H25B 108.1 . . ?
H25A C25 H25B 107.3 . . ?
C26 C25 N1 116.8(5) . . ?
C26 C25 H25A 108.1 . . ?
C26 C25 H25B 108.1 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
N1 C22 H22A 108.2 . . ?
N1 C22 H22B 108.2 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N1 116.2(6) . . ?
C23 C22 H22A 108.2 . . ?
C23 C22 H22B 108.2 . . ?
H29A C29 H29B 108.3 . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
C28 C29 C30 109.2(6) . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
C40 C41 C42 108.9(5) . . ?
C40 C41 H41A 109.9 . . ?
C40 C41 H41B 109.9 . . ?
C42 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
N2 C34 H34A 108.6 . . ?
N2 C34 H34B 108.6 . . ?
N2 C34 C35 114.8(6) . . ?
H34A C34 H34B 107.6 . . ?
C35 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C31 H31A 108.3 . . ?
N2 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 N2 115.9(6) . . ?
C32 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
N1 C28 H28A 108.5 . . ?
N1 C28 H28B 108.5 . . ?
C29 C28 N1 115.2(6) . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C19 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
C19 C20 C21 108.9(6) . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
C25 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
H26A C26 H26B 108.2 . . ?
C27 C26 C25 110.1(6) . . ?
C27 C26 H26A 109.6 . . ?
C27 C26 H26B 109.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C34 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 C34 109.8(6) . . ?
C36 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C22 C23 C24 109.4(6) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C31 C32 C33 109.9(7) . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O14 C46 C48 121.5(10) . . ?
O14 C46 C47 118.4(11) . . ?
C47 C46 C48 120.1(9) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O13 C43 C45 119.6(12) . . ?
O13 C43 C44 124.5(11) . . ?
C44 C43 C45 115.7(11) . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 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 O4 C5 C6 178.2(5) 4_566 . . . ?
Fe1 O4 C5 C4 -3.0(6) 4_566 . . . ?
Fe1 O1 C1 C6 177.0(5) . . . . ?
Fe1 O1 C1 C2 -3.1(6) . . . . ?
Fe1 O2 C2 C3 -174.6(5) . . . . ?
Fe1 O2 C2 C1 6.1(6) . . . . ?
Fe1 O5 C7 C12 1.7(7) . . . . ?
Fe1 O5 C7 C8 -178.4(5) . . . . ?
Fe1 O3 C4 C5 3.6(6) 4_566 . . . ?
Fe1 O3 C4 C3 -177.7(5) 4_566 . . . ?
Fe1 O8 C12 C7 -1.3(6) . . . . ?
Fe1 O8 C12 C11 179.9(5) . . . . ?
Fe2 O10 C15 C16 -5.1(6) 4_575 . . . ?
Fe2 O10 C15 C14 176.1(5) 4_575 . . . ?
Fe2 O6 C9 C10 3.9(6) . . . . ?
Fe2 O6 C9 C8 -177.2(5) . . . . ?
Fe2 O7 C10 C9 -3.2(6) . . . . ?
Fe2 O7 C10 C11 176.3(5) . . . . ?
Fe2 O12 C18 C13 2.8(6) . . . . ?
Fe2 O12 C18 C17 -178.2(5) . . . . ?
Fe2 O11 C16 C15 7.4(6) 4_575 . . . ?
Fe2 O11 C16 C17 -173.7(5) 4_575 . . . ?
Fe2 O9 C13 C18 -2.3(6) . . . . ?
Fe2 O9 C13 C14 176.5(5) . . . . ?
Cl2 C6 C1 O1 0.6(10) . . . . ?
Cl2 C6 C1 C2 -179.4(7) . . . . ?
O10 C15 C16 O11 -1.5(8) . . . . ?
O10 C15 C16 C17 179.4(5) . . . . ?
O10 C15 C14 Cl5 -0.7(9) . . . . ?
O10 C15 C14 C13 -177.6(5) . . . . ?
O10 C15 C14 Br5 3.1(11) . . . . ?
O4 C5 C6 Cl2 -0.9(10) . . . . ?
O4 C5 C6 C1 177.9(6) . . . . ?
O4 C5 C6 Br2 -6.8(14) . . . . ?
O4 C5 C4 O3 -0.4(8) . . . . ?
O4 C5 C4 C3 -179.2(6) . . . . ?
O6 C9 C8 Cl3 -4.4(11) . . . . ?
O6 C9 C8 C7 176.1(6) . . . . ?
O6 C9 C8 Br3 2.1(16) . . . . ?
O7 C10 C9 O6 -0.5(8) . . . . ?
O7 C10 C9 C8 -179.4(5) . . . . ?
O7 C10 C11 Cl4 2.7(9) . . . . ?
O7 C10 C11 C12 -176.6(6) . . . . ?
O7 C10 C11 Br4 -0.8(12) . . . . ?
O12 C18 C17 Cl6 3.5(10) . . . . ?
O12 C18 C17 C16 -178.8(6) . . . . ?
O12 C18 C17 Br6 -7.8(12) . . . . ?
O2 C2 C3 Cl1 -1.2(9) . . . . ?
O2 C2 C3 C4 -179.0(6) . . . . ?
O2 C2 C3 Br1 13.4(10) . . . . ?
O2 C2 C1 O1 -2.0(8) . . . . ?
O2 C2 C1 C6 177.9(5) . . . . ?
O5 C7 C12 O8 -0.3(8) . . . . ?
O5 C7 C12 C11 178.6(6) . . . . ?
O5 C7 C8 Cl3 5.8(12) . . . . ?
O5 C7 C8 C9 -174.7(6) . . . . ?
O5 C7 C8 Br3 -1.1(17) . . . . ?
O11 C16 C17 Cl6 -1.3(9) . . . . ?
O11 C16 C17 C18 -179.1(6) . . . . ?
O11 C16 C17 Br6 9.8(11) . . . . ?
O3 C4 C3 Cl1 4.1(9) . . . . ?
O3 C4 C3 C2 -178.2(6) . . . . ?
O3 C4 C3 Br1 -10.5(10) . . . . ?
O9 C13 C18 O12 -0.3(7) . . . . ?
O9 C13 C18 C17 -179.4(5) . . . . ?
O9 C13 C14 Cl5 0.5(9) . . . . ?
O9 C13 C14 C15 177.6(6) . . . . ?
O9 C13 C14 Br5 -3.1(12) . . . . ?
O8 C12 C11 Cl4 -3.3(10) . . . . ?
O8 C12 C11 C10 176.0(6) . . . . ?
O8 C12 C11 Br4 0.1(11) . . . . ?
N2 C40 C41 C42 173.0(5) . . . . ?
N2 C34 C35 C36 -174.3(7) . . . . ?
N2 C31 C32 C33 174.2(6) . . . . ?
N1 C19 C20 C21 -169.1(6) . . . . ?
N1 C25 C26 C27 170.1(6) . . . . ?
N1 C22 C23 C24 171.1(6) . . . . ?
C13 C18 C17 Cl6 -177.6(5) . . . . ?
C13 C18 C17 C16 0.2(9) . . . . ?
C13 C18 C17 Br6 171.2(9) . . . . ?
C15 C16 C17 Cl6 177.6(5) . . . . ?
C15 C16 C17 C18 -0.1(9) . . . . ?
C15 C16 C17 Br6 -171.3(9) . . . . ?
C18 C13 C14 Cl5 179.3(5) . . . . ?
C18 C13 C14 C15 -3.7(9) . . . . ?
C18 C13 C14 Br5 175.6(9) . . . . ?
C10 C9 C8 Cl3 174.4(8) . . . . ?
C10 C9 C8 C7 -5.1(9) . . . . ?
C10 C9 C8 Br3 -179.1(14) . . . . ?
C16 C15 C14 Cl5 -179.4(6) . . . . ?
C16 C15 C14 C13 3.7(9) . . . . ?
C16 C15 C14 Br5 -175.6(9) . . . . ?
C5 C6 C1 O1 -178.3(6) . . . . ?
C5 C6 C1 C2 1.8(9) . . . . ?
C5 C4 C3 Cl1 -177.2(5) . . . . ?
C5 C4 C3 C2 0.5(9) . . . . ?
C5 C4 C3 Br1 168.2(6) . . . . ?
C14 C13 C18 O12 -179.2(5) . . . . ?
C14 C13 C18 C17 1.7(9) . . . . ?
C14 C15 C16 O11 177.3(5) . . . . ?
C14 C15 C16 C17 -1.8(8) . . . . ?
C6 C5 C4 O3 178.6(5) . . . . ?
C6 C5 C4 C3 -0.2(9) . . . . ?
C9 C10 C11 Cl4 -177.8(5) . . . . ?
C9 C10 C11 C12 2.9(9) . . . . ?
C9 C10 C11 Br4 178.7(9) . . . . ?
C4 C5 C6 Cl2 -179.7(7) . . . . ?
C4 C5 C6 C1 -0.9(9) . . . . ?
C4 C5 C6 Br2 174.3(12) . . . . ?
C7 C12 C11 Cl4 178.0(5) . . . . ?
C7 C12 C11 C10 -2.8(9) . . . . ?
C7 C12 C11 Br4 -178.7(8) . . . . ?
C12 C7 C8 Cl3 -174.3(9) . . . . ?
C12 C7 C8 C9 5.2(9) . . . . ?
C12 C7 C8 Br3 178.8(15) . . . . ?
C3 C2 C1 O1 178.6(5) . . . . ?
C3 C2 C1 C6 -1.5(9) . . . . ?
C11 C10 C9 O6 180.0(5) . . . . ?
C11 C10 C9 C8 1.1(8) . . . . ?
C1 C2 C3 Cl1 178.1(5) . . . . ?
C1 C2 C3 C4 0.3(9) . . . . ?
C1 C2 C3 Br1 -167.3(6) . . . . ?
C8 C7 C12 O8 179.8(5) . . . . ?
C8 C7 C12 C11 -1.3(9) . . . . ?
C40 N2 C37 C38 -51.1(8) . . . . ?
C40 N2 C34 C35 177.6(6) . . . . ?
C40 N2 C31 C32 -68.7(8) . . . . ?
C37 N2 C40 C41 -55.4(7) . . . . ?
C37 N2 C34 C35 -61.8(8) . . . . ?
C37 N2 C31 C32 170.6(6) . . . . ?
C19 N1 C25 C26 -176.8(6) . . . . ?
C19 N1 C22 C23 63.6(8) . . . . ?
C19 N1 C28 C29 -56.7(8) . . . . ?
C25 N1 C19 C20 -176.0(6) . . . . ?
C25 N1 C22 C23 -54.2(8) . . . . ?
C25 N1 C28 C29 61.3(7) . . . . ?
C22 N1 C19 C20 63.0(7) . . . . ?
C22 N1 C25 C26 -56.6(8) . . . . ?
C22 N1 C28 C29 -177.0(6) . . . . ?
C34 N2 C40 C41 63.4(7) . . . . ?
C34 N2 C37 C38 -170.4(6) . . . . ?
C34 N2 C31 C32 51.1(8) . . . . ?
C39 C38 C37 N2 179.7(6) . . . . ?
C31 N2 C40 C41 -175.0(6) . . . . ?
C31 N2 C37 C38 67.8(8) . . . . ?
C31 N2 C34 C35 58.4(8) . . . . ?
C28 N1 C19 C20 -55.3(8) . . . . ?
C28 N1 C25 C26 62.3(8) . . . . ?
C28 N1 C22 C23 -175.4(6) . . . . ?
C30 C29 C28 N1 -171.2(6) . . . . ?
Br2 C6 C1 O1 6.7(14) . . . . ?
Br2 C6 C1 C2 -173.2(12) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.222
_oxdiff_exptl_absorpt_empirical_full_min 0.887
####################################################################### 
# 
# 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_Br-035-d_CCDC-2014804_R1
_database_code_depnum_ccdc_archive 'CCDC 2014804'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-28
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br2.118 C18 Cl3.882 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br2.12 Cl3.88 Fe2 N2 O12'
_chemical_formula_weight         1199.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl3.88 Br2.12 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8837(10)
_cell_length_b                   20.7386(13)
_cell_length_c                   12.3417(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.410(9)
_cell_angle_gamma                90
_cell_volume                     2730.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5392
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.0470
_cell_measurement_theta_min      1.9260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.043
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20720
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.587
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120634000
_diffrn_orient_matrix_UB_12      -0.0241848000
_diffrn_orient_matrix_UB_13      -0.0371304000
_diffrn_orient_matrix_UB_21      0.0451747000
_diffrn_orient_matrix_UB_22      0.0202554000
_diffrn_orient_matrix_UB_23      -0.0169638000
_diffrn_orient_matrix_UB_31      0.0473002000
_diffrn_orient_matrix_UB_32      -0.0131585000
_diffrn_orient_matrix_UB_33      0.0421442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3929
_reflns_number_total             6116
_reflns_odcompleteness_completeness 88.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.1010
_refine_ls_restrained_S_all      1.169
_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)+48.9236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2303
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-Br2
 1.88 with sigma of 0.02
 C6-Cl2
 1.73 with sigma of 0.02
 Cl3-C8
 1.73 with sigma of 0.02
3. Rigid bond restraints
 Br1, Br3, Cl3, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Br1 \\sim Br3 \\sim Cl3 \\sim Cl1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Uanis(Cl2) = Uanis(Br2)
5. Rigid body (RIGU) restrains
 Cl2, Br2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: Br1(0.35834) Cl3(0.65768) Cl2(0.64166) Br3(0.34232) Cl1(0.64166)
 Br2(0.35834)
7.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C19(H19A,H19B), C14(H14A,H14B), C13(H13A,
 H13B), C16(H16A,H16B), C11(H11A,H11B), C17(H17A,H17B)
7.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C12(H12A,H12B,
 H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.03958(13) 0.68948(6) 0.46913(11) 0.0247(3) Uani 1 1 d . . . . .
Br1 Br 0.9297(7) 0.6668(4) 0.0506(4) 0.0289(19) Uani 0.3583 1 d . U P A -2
Cl3 Cl 1.2999(9) 0.4803(6) 0.5166(9) 0.036(4) Uani 0.6577 1 d D U P B 2
Cl2 Cl 0.663(5) 0.829(2) 0.386(3) 0.038(3) Uani 0.6417 1 d D . P C 2
O5 O 1.0976(6) 0.3810(3) 0.5297(5) 0.0269(14) Uani 1 1 d . . . . .
O3 O 0.6895(6) 0.7533(3) -0.0003(5) 0.0282(14) Uani 1 1 d . . . . .
O4 O 0.5741(6) 0.8120(3) 0.1352(5) 0.0289(14) Uani 1 1 d . . . . .
O1 O 0.9011(6) 0.7536(3) 0.4384(5) 0.0266(14) Uani 1 1 d . . . . .
O2 O 1.0094(6) 0.6871(3) 0.3029(5) 0.0291(14) Uani 1 1 d . . . . .
O6 O 1.1420(6) 0.6041(3) 0.4741(5) 0.0292(15) Uani 1 1 d . . . . .
N1 N 0.3875(7) 0.6399(4) 0.2443(7) 0.0312(18) Uani 1 1 d . . . . .
C2 C 0.9067(8) 0.7160(4) 0.2589(7) 0.0237(19) Uani 1 1 d . . . . .
C5 C 0.6796(9) 0.7841(4) 0.1796(8) 0.027(2) Uani 1 1 d . . . . .
C4 C 0.7430(8) 0.7487(4) 0.1039(7) 0.0235(19) Uani 1 1 d . . . . .
C7 C 1.0605(9) 0.4382(4) 0.5157(7) 0.027(2) Uani 1 1 d . . . . .
C3 C 0.8515(9) 0.7139(4) 0.1456(7) 0.026(2) Uani 1 1 d . . . . .
C1 C 0.8441(9) 0.7538(4) 0.3343(7) 0.0254(19) Uani 1 1 d . . . . .
C6 C 0.7325(8) 0.7871(4) 0.2943(7) 0.0261(19) Uani 1 1 d D . . . .
C8 C 1.1357(8) 0.4920(4) 0.5081(8) 0.029(2) Uani 1 1 d D . . . .
C20 C 0.2818(9) 0.7519(5) 0.2463(9) 0.036(2) Uani 1 1 d . . . . .
H20A H 0.2805 0.7457 0.3256 0.043 Uiso 1 1 calc R U . . .
H20B H 0.1999 0.7378 0.2028 0.043 Uiso 1 1 calc R U . . .
C9 C 1.0818(9) 0.5531(5) 0.4880(7) 0.027(2) Uani 1 1 d . . . . .
C10 C 0.2675(10) 0.6089(5) 0.1830(8) 0.036(2) Uani 1 1 d . . . . .
H10A H 0.2574 0.6199 0.1037 0.044 Uiso 1 1 calc R U . . .
H10B H 0.1963 0.6286 0.2101 0.044 Uiso 1 1 calc R U . . .
C19 C 0.3847(9) 0.7113(5) 0.2156(8) 0.032(2) Uani 1 1 d . . . . .
H19A H 0.4660 0.7302 0.2518 0.038 Uiso 1 1 calc R U . . .
H19B H 0.3791 0.7151 0.1348 0.038 Uiso 1 1 calc R U . . .
C14 C 0.4949(9) 0.6668(5) 0.4464(8) 0.034(2) Uani 1 1 d . . . . .
H14A H 0.4805 0.7138 0.4377 0.040 Uiso 1 1 calc R U . . .
H14B H 0.5784 0.6569 0.4301 0.040 Uiso 1 1 calc R U . . .
C13 C 0.3936(9) 0.6302(5) 0.3675(8) 0.033(2) Uani 1 1 d . . . . .
H13A H 0.4054 0.5836 0.3836 0.040 Uiso 1 1 calc R U . . .
H13B H 0.3113 0.6424 0.3840 0.040 Uiso 1 1 calc R U . . .
C16 C 0.5030(10) 0.6089(5) 0.2129(9) 0.038(2) Uani 1 1 d . . . . .
H16A H 0.5780 0.6326 0.2516 0.045 Uiso 1 1 calc R U . . .
H16B H 0.5097 0.5642 0.2415 0.045 Uiso 1 1 calc R U . . .
C21 C 0.3013(10) 0.8225(5) 0.2243(9) 0.041(3) Uani 1 1 d . . . . .
H21A H 0.3040 0.8285 0.1461 0.061 Uiso 1 1 calc R U . . .
H21B H 0.3805 0.8370 0.2700 0.061 Uiso 1 1 calc R U . . .
H21C H 0.2320 0.8477 0.2426 0.061 Uiso 1 1 calc R U . . .
C11 C 0.2581(11) 0.5362(5) 0.1929(10) 0.049(3) Uani 1 1 d . . . . .
H11A H 0.2645 0.5242 0.2714 0.058 Uiso 1 1 calc R U . . .
H11B H 0.3283 0.5155 0.1659 0.058 Uiso 1 1 calc R U . . .
C15 C 0.4897(11) 0.6461(6) 0.5650(8) 0.047(3) Uani 1 1 d . . . . .
H15A H 0.4033 0.6492 0.5762 0.071 Uiso 1 1 calc R U . . .
H15B H 0.5436 0.6744 0.6176 0.071 Uiso 1 1 calc R U . . .
H15C H 0.5190 0.6015 0.5768 0.071 Uiso 1 1 calc R U . . .
C17 C 0.5070(13) 0.6067(5) 0.0901(10) 0.054(3) Uani 1 1 d . . . . .
H17A H 0.4315 0.5844 0.0492 0.065 Uiso 1 1 calc R U . . .
H17B H 0.5073 0.6511 0.0608 0.065 Uiso 1 1 calc R U . . .
C18 C 0.6242(14) 0.5712(6) 0.0732(13) 0.071(4) Uani 1 1 d . . . . .
H18A H 0.6286 0.5719 -0.0053 0.107 Uiso 1 1 calc R U . . .
H18B H 0.6210 0.5264 0.0979 0.107 Uiso 1 1 calc R U . . .
H18C H 0.6986 0.5924 0.1163 0.107 Uiso 1 1 calc R U . . .
C12 C 0.1331(13) 0.5120(6) 0.1251(12) 0.072(4) Uani 1 1 d . . . . .
H12A H 0.1260 0.5248 0.0477 0.107 Uiso 1 1 calc R U . . .
H12B H 0.0637 0.5309 0.1543 0.107 Uiso 1 1 calc R U . . .
H12C H 0.1296 0.4649 0.1299 0.107 Uiso 1 1 calc R U . . .
Br3 Br 1.3052(7) 0.4810(4) 0.5179(7) 0.040(3) Uani 0.3423 1 d . U P B -2
Cl1 Cl 0.9213(12) 0.6668(4) 0.0532(10) 0.050(4) Uani 0.6417 1 d . U P A 2
Br2 Br 0.655(4) 0.8386(17) 0.386(3) 0.038(3) Uani 0.3583 1 d D . P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O5 2.092(6) 3_766 ?
Fe1 O3 1.992(6) 4_676 ?
Fe1 O4 2.010(6) 4_676 ?
Fe1 O1 1.990(6) . ?
Fe1 O2 2.014(6) . ?
Fe1 O6 2.087(6) . ?
Br1 C3 1.858(11) . ?
Cl3 C8 1.786(11) . ?
Cl2 C6 1.721(17) . ?
O5 Fe1 2.092(6) 3_766 ?
O5 C7 1.254(10) . ?
O3 Fe1 1.992(6) 4_575 ?
O3 C4 1.306(10) . ?
O4 Fe1 2.010(6) 4_575 ?
O4 C5 1.305(11) . ?
O1 C1 1.312(10) . ?
O2 C2 1.289(10) . ?
O6 C9 1.272(11) . ?
N1 C10 1.517(12) . ?
N1 C19 1.520(12) . ?
N1 C13 1.522(12) . ?
N1 C16 1.529(12) . ?
C2 C3 1.409(12) . ?
C2 C1 1.482(12) . ?
C5 C4 1.464(12) . ?
C5 C6 1.420(12) . ?
C4 C3 1.392(12) . ?
C7 C8 1.398(13) . ?
C7 C9 1.552(13) 3_766 ?
C3 Cl1 1.782(14) . ?
C1 C6 1.399(12) . ?
C6 Br2 1.868(14) . ?
C8 C9 1.398(12) . ?
C8 Br3 1.839(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C19 1.508(13) . ?
C20 C21 1.511(14) . ?
C9 C7 1.552(13) 3_766 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.519(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.523(13) . ?
C14 C15 1.537(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.526(15) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.534(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.523(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
O3 Fe1 O5 166.9(2) 4_676 3_766 ?
O3 Fe1 O4 80.5(3) 4_676 4_676 ?
O3 Fe1 O2 99.8(3) 4_676 . ?
O3 Fe1 O6 95.0(3) 4_676 . ?
O4 Fe1 O5 88.4(3) 4_676 3_766 ?
O4 Fe1 O2 177.3(3) 4_676 . ?
O4 Fe1 O6 88.0(3) 4_676 . ?
O1 Fe1 O5 87.3(2) . 3_766 ?
O1 Fe1 O3 101.5(3) . 4_676 ?
O1 Fe1 O4 100.7(3) . 4_676 ?
O1 Fe1 O2 81.8(3) . . ?
O1 Fe1 O6 162.3(3) . . ?
O2 Fe1 O5 91.0(3) . 3_766 ?
O2 Fe1 O6 89.3(3) . . ?
O6 Fe1 O5 77.5(2) . 3_766 ?
C7 O5 Fe1 116.9(6) . 3_766 ?
C4 O3 Fe1 114.8(6) . 4_575 ?
C5 O4 Fe1 113.1(6) . 4_575 ?
C1 O1 Fe1 112.4(5) . . ?
C2 O2 Fe1 111.8(6) . . ?
C9 O6 Fe1 115.0(6) . . ?
C10 N1 C19 108.7(7) . . ?
C10 N1 C13 107.7(7) . . ?
C10 N1 C16 111.4(8) . . ?
C19 N1 C13 110.9(7) . . ?
C19 N1 C16 109.3(7) . . ?
C13 N1 C16 108.7(8) . . ?
O2 C2 C3 124.6(8) . . ?
O2 C2 C1 116.7(8) . . ?
C3 C2 C1 118.7(8) . . ?
O4 C5 C4 116.2(8) . . ?
O4 C5 C6 123.3(8) . . ?
C6 C5 C4 120.5(8) . . ?
O3 C4 C5 114.6(8) . . ?
O3 C4 C3 125.6(8) . . ?
C3 C4 C5 119.8(8) . . ?
O5 C7 C8 126.0(9) . . ?
O5 C7 C9 113.9(8) . 3_766 ?
C8 C7 C9 120.0(8) . 3_766 ?
C2 C3 Br1 118.9(7) . . ?
C2 C3 Cl1 120.0(8) . . ?
C4 C3 Br1 120.0(7) . . ?
C4 C3 C2 121.0(8) . . ?
C4 C3 Cl1 119.0(8) . . ?
Cl1 C3 Br1 2.2(6) . . ?
O1 C1 C2 115.3(8) . . ?
O1 C1 C6 123.7(8) . . ?
C6 C1 C2 121.0(8) . . ?
Cl2 C6 Br2 5(3) . . ?
C5 C6 Cl2 122.4(19) . . ?
C5 C6 Br2 118.9(13) . . ?
C1 C6 Cl2 118.7(19) . . ?
C1 C6 C5 118.9(8) . . ?
C1 C6 Br2 122.1(14) . . ?
Cl3 C8 Br3 0.8(7) . . ?
C7 C8 Cl3 118.6(8) . . ?
C7 C8 Br3 119.3(7) . . ?
C9 C8 Cl3 120.9(8) . . ?
C9 C8 C7 120.3(8) . . ?
C9 C8 Br3 120.3(8) . . ?
H20A C20 H20B 108.0 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C19 C20 C21 111.0(8) . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
O6 C9 C7 115.9(8) . 3_766 ?
O6 C9 C8 124.6(9) . . ?
C8 C9 C7 119.4(8) . 3_766 ?
N1 C10 H10A 108.2 . . ?
N1 C10 H10B 108.2 . . ?
N1 C10 C11 116.5(8) . . ?
H10A C10 H10B 107.3 . . ?
C11 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
N1 C19 H19A 107.9 . . ?
N1 C19 H19B 107.9 . . ?
C20 C19 N1 117.8(8) . . ?
C20 C19 H19A 107.9 . . ?
C20 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
H14A C14 H14B 108.4 . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C13 C14 C15 108.1(8) . . ?
C15 C14 H14A 110.1 . . ?
C15 C14 H14B 110.1 . . ?
N1 C13 C14 117.1(8) . . ?
N1 C13 H13A 108.0 . . ?
N1 C13 H13B 108.0 . . ?
C14 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
N1 C16 H16A 108.1 . . ?
N1 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N1 116.8(9) . . ?
C17 C16 H16A 108.1 . . ?
C17 C16 H16B 108.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C10 C11 C12 110.3(9) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 C16 109.8(11) . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 O5 C7 C8 -177.4(7) 3_766 . . . ?
Fe1 O5 C7 C9 5.2(10) 3_766 . . 3_766 ?
Fe1 O3 C4 C5 2.5(9) 4_575 . . . ?
Fe1 O3 C4 C3 -177.2(7) 4_575 . . . ?
Fe1 O4 C5 C4 -9.1(9) 4_575 . . . ?
Fe1 O4 C5 C6 170.8(7) 4_575 . . . ?
Fe1 O1 C1 C2 -10.3(9) . . . . ?
Fe1 O1 C1 C6 170.0(7) . . . . ?
Fe1 O2 C2 C3 -170.1(7) . . . . ?
Fe1 O2 C2 C1 10.1(9) . . . . ?
Fe1 O6 C9 C7 7.4(10) . . . 3_766 ?
Fe1 O6 C9 C8 -171.3(7) . . . . ?
Cl3 C8 C9 O6 0.3(14) . . . . ?
Cl3 C8 C9 C7 -178.4(7) . . . 3_766 ?
O5 C7 C8 Cl3 1.0(14) . . . . ?
O5 C7 C8 C9 177.5(9) . . . . ?
O5 C7 C8 Br3 0.5(14) . . . . ?
O3 C4 C3 Br1 -2.1(13) . . . . ?
O3 C4 C3 C2 175.2(8) . . . . ?
O3 C4 C3 Cl1 -4.3(13) . . . . ?
O4 C5 C4 O3 4.5(11) . . . . ?
O4 C5 C4 C3 -175.7(8) . . . . ?
O4 C5 C6 Cl2 -1(3) . . . . ?
O4 C5 C6 C1 178.0(8) . . . . ?
O4 C5 C6 Br2 -5(2) . . . . ?
O1 C1 C6 Cl2 -1(3) . . . . ?
O1 C1 C6 C5 179.6(8) . . . . ?
O1 C1 C6 Br2 3(2) . . . . ?
O2 C2 C3 Br1 0.0(13) . . . . ?
O2 C2 C3 C4 -177.4(8) . . . . ?
O2 C2 C3 Cl1 2.2(13) . . . . ?
O2 C2 C1 O1 0.0(11) . . . . ?
O2 C2 C1 C6 179.7(8) . . . . ?
N1 C10 C11 C12 -179.0(10) . . . . ?
N1 C16 C17 C18 -176.9(9) . . . . ?
C2 C1 C6 Cl2 179(2) . . . . ?
C2 C1 C6 C5 0.0(13) . . . . ?
C2 C1 C6 Br2 -176.9(17) . . . . ?
C5 C4 C3 Br1 178.1(7) . . . . ?
C5 C4 C3 C2 -4.5(13) . . . . ?
C5 C4 C3 Cl1 175.9(8) . . . . ?
C4 C5 C6 Cl2 179(3) . . . . ?
C4 C5 C6 C1 -2.0(13) . . . . ?
C4 C5 C6 Br2 174.9(17) . . . . ?
C7 C8 C9 O6 -176.1(9) . . . . ?
C7 C8 C9 C7 5.2(15) . . . 3_766 ?
C3 C2 C1 O1 -179.8(8) . . . . ?
C3 C2 C1 C6 -0.1(13) . . . . ?
C1 C2 C3 Br1 179.8(7) . . . . ?
C1 C2 C3 C4 2.5(13) . . . . ?
C1 C2 C3 Cl1 -178.0(8) . . . . ?
C6 C5 C4 O3 -175.4(8) . . . . ?
C6 C5 C4 C3 4.4(13) . . . . ?
C9 C7 C8 Cl3 178.3(7) 3_766 . . . ?
C9 C7 C8 C9 -5.3(15) 3_766 . . . ?
C9 C7 C8 Br3 177.8(7) 3_766 . . . ?
C10 N1 C19 C20 61.7(11) . . . . ?
C10 N1 C13 C14 -170.1(8) . . . . ?
C10 N1 C16 C17 54.5(11) . . . . ?
C19 N1 C10 C11 174.5(9) . . . . ?
C19 N1 C13 C14 -51.2(11) . . . . ?
C19 N1 C16 C17 -65.7(11) . . . . ?
C13 N1 C10 C11 -65.2(12) . . . . ?
C13 N1 C19 C20 -56.6(11) . . . . ?
C13 N1 C16 C17 173.1(9) . . . . ?
C16 N1 C10 C11 54.0(12) . . . . ?
C16 N1 C19 C20 -176.5(9) . . . . ?
C16 N1 C13 C14 69.0(10) . . . . ?
C21 C20 C19 N1 173.4(8) . . . . ?
C15 C14 C13 N1 -176.0(8) . . . . ?
Br3 C8 C9 O6 0.8(14) . . . . ?
Br3 C8 C9 C7 -177.8(7) . . . 3_766 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.666
####################################################################### 
# 
# 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_Br-065-d_CCDC-2014807_R1
_database_code_depnum_ccdc_archive 'CCDC 2014807'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-29
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3.88 C18 Cl2.12 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br3.88 Cl2.12 Fe2 N2 O12'
_chemical_formula_weight         1277.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl2.12 Br3.88 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9142(5)
_cell_length_b                   20.5604(9)
_cell_length_c                   12.3173(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.617(4)
_cell_angle_gamma                90
_cell_volume                     2707.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7380
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.7870
_cell_measurement_theta_min      1.9470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21279
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.603
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0225074000
_diffrn_orient_matrix_UB_12      0.0104746000
_diffrn_orient_matrix_UB_13      -0.0472399000
_diffrn_orient_matrix_UB_21      0.0523143000
_diffrn_orient_matrix_UB_22      -0.0209706000
_diffrn_orient_matrix_UB_23      0.0146849000
_diffrn_orient_matrix_UB_31      -0.0340506000
_diffrn_orient_matrix_UB_32      -0.0253211000
_diffrn_orient_matrix_UB_33      -0.0317330000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4246
_reflns_number_total             6175
_reflns_odcompleteness_completeness 90.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6175
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0548
_refine_ls_restrained_S_all      1.071
_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)+(0.0261P)²+8.3762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1056
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C6
 1.73 with sigma of 0.02
 C3-Cl1
 1.73 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br3) = Uanis(Cl3)
4. Others
 Fixed Sof: Br3(0.676) Br1(0.632) Cl2(0.368) Br2(0.632) Cl1(0.368) Cl3(0.324)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C10(H10A,H10B), C14(H14A,H14B), C19(H19A,
 H19B), C11(H11A,H11B), C20(H20A,H20B), C17(H17A,H17B)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C18(H18A,H18B,
 H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br3 Br 0.1926(4) 0.5198(3) 0.9784(4) 0.0277(4) Uani 0.676 1 d . . P A -2
Br1 Br 0.0766(2) 0.16296(15) 0.95383(18) 0.0225(6) Uani 0.632 1 d . . P B -2
Fe1 Fe 0.46272(6) 0.30958(3) 1.03556(5) 0.01788(15) Uani 1 1 d . . . . .
Cl2 Cl 0.3397(11) 0.3362(7) 0.6219(10) 0.063(4) Uani 0.368 1 d D . P C 2
O5 O 0.4011(3) 0.61938(14) 0.9662(2) 0.0193(7) Uani 1 1 d . . . . .
O4 O 0.1011(3) 0.25461(14) 0.5676(2) 0.0189(7) Uani 1 1 d . . . . .
O3 O -0.0069(3) 0.18744(14) 0.7008(2) 0.0194(7) Uani 1 1 d . . . . .
O1 O 0.4279(3) 0.31151(14) 0.8702(2) 0.0197(7) Uani 1 1 d . . . . .
O6 O 0.3613(3) 0.39584(15) 1.0305(2) 0.0211(7) Uani 1 1 d . . . . .
O2 O 0.3139(3) 0.25187(14) 1.0050(2) 0.0201(7) Uani 1 1 d . . . . .
N1 N 0.6152(3) 0.13964(18) 0.7578(3) 0.0232(8) Uani 1 1 d . . . . .
C1 C 0.3235(4) 0.2842(2) 0.8241(3) 0.0168(9) Uani 1 1 d . . . . .
C4 C 0.0970(4) 0.2157(2) 0.7455(3) 0.0171(9) Uani 1 1 d . . . . .
C2 C 0.2598(4) 0.2479(2) 0.9006(3) 0.0170(9) Uani 1 1 d . . . . .
C3 C 0.1517(4) 0.2124(2) 0.8585(3) 0.0180(9) Uani 1 1 d D . . . .
C9 C 0.4181(4) 0.4470(2) 1.0131(3) 0.0191(9) Uani 1 1 d . . . . .
C6 C 0.2685(4) 0.2873(2) 0.7112(3) 0.0187(9) Uani 1 1 d D . . . .
C5 C 0.1578(4) 0.2542(2) 0.6703(3) 0.0183(9) Uani 1 1 d . . . . .
C7 C 0.4406(4) 0.5620(2) 0.9806(3) 0.0197(10) Uani 1 1 d . . . . .
C8 C 0.3675(4) 0.5080(2) 0.9922(4) 0.0212(10) Uani 1 1 d . . . . .
C13 C 0.6163(5) 0.2116(2) 0.7886(4) 0.0269(11) Uani 1 1 d . . . . .
H13A H 0.5349 0.2307 0.7531 0.032 Uiso 1 1 calc R U . . .
H13B H 0.6234 0.2149 0.8698 0.032 Uiso 1 1 calc R U . . .
C16 C 0.4995(5) 0.1086(2) 0.7878(4) 0.0305(11) Uani 1 1 d . . . . .
H16A H 0.4250 0.1332 0.7500 0.037 Uiso 1 1 calc R U . . .
H16B H 0.4916 0.0638 0.7580 0.037 Uiso 1 1 calc R U . . .
C10 C 0.6081(4) 0.1308(2) 0.6343(4) 0.0249(10) Uani 1 1 d . . . . .
H10A H 0.6902 0.1431 0.6178 0.030 Uiso 1 1 calc R U . . .
H10B H 0.5955 0.0840 0.6169 0.030 Uiso 1 1 calc R U . . .
C14 C 0.7198(4) 0.2521(2) 0.7565(4) 0.0285(11) Uani 1 1 d . . . . .
H14A H 0.7182 0.2471 0.6763 0.034 Uiso 1 1 calc R U . . .
H14B H 0.8021 0.2370 0.7980 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5128(5) 0.1492(3) 0.4374(4) 0.0331(12) Uani 1 1 d . . . . .
H12A H 0.4626 0.1797 0.3856 0.050 Uiso 1 1 calc R U . . .
H12B H 0.4792 0.1051 0.4226 0.050 Uiso 1 1 calc R U . . .
H12C H 0.5997 0.1503 0.4277 0.050 Uiso 1 1 calc R U . . .
C19 C 0.7357(4) 0.1081(2) 0.8193(4) 0.0271(11) Uani 1 1 d . . . . .
H19A H 0.8069 0.1281 0.7931 0.033 Uiso 1 1 calc R U . . .
H19B H 0.7458 0.1182 0.8992 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5077(5) 0.1685(2) 0.5564(4) 0.0319(12) Uani 1 1 d . . . . .
H11A H 0.5223 0.2158 0.5668 0.038 Uiso 1 1 calc R U . . .
H11B H 0.4244 0.1582 0.5721 0.038 Uiso 1 1 calc R U . . .
C15 C 0.7011(4) 0.3236(2) 0.7830(4) 0.0316(12) Uani 1 1 d . . . . .
H15A H 0.6188 0.3381 0.7429 0.047 Uiso 1 1 calc R U . . .
H15B H 0.7664 0.3499 0.7602 0.047 Uiso 1 1 calc R U . . .
H15C H 0.7059 0.3286 0.8629 0.047 Uiso 1 1 calc R U . . .
C20 C 0.7433(5) 0.0348(2) 0.8064(4) 0.0367(13) Uani 1 1 d . . . . .
H20A H 0.7369 0.0235 0.7273 0.044 Uiso 1 1 calc R U . . .
H20B H 0.6731 0.0136 0.8327 0.044 Uiso 1 1 calc R U . . .
C17 C 0.4973(6) 0.1056(3) 0.9105(5) 0.0416(14) Uani 1 1 d . . . . .
H17A H 0.4971 0.1502 0.9409 0.050 Uiso 1 1 calc R U . . .
H17B H 0.5728 0.0828 0.9508 0.050 Uiso 1 1 calc R U . . .
C21 C 0.8677(6) 0.0105(3) 0.8741(5) 0.0558(18) Uani 1 1 d . . . . .
H21A H 0.9368 0.0319 0.8483 0.084 Uiso 1 1 calc R U . . .
H21B H 0.8738 -0.0367 0.8648 0.084 Uiso 1 1 calc R U . . .
H21C H 0.8724 0.0205 0.9526 0.084 Uiso 1 1 calc R U . . .
C18 C 0.3798(6) 0.0692(3) 0.9257(6) 0.0533(17) Uani 1 1 d . . . . .
H18A H 0.3059 0.0903 0.8814 0.080 Uiso 1 1 calc R U . . .
H18B H 0.3742 0.0700 1.0041 0.080 Uiso 1 1 calc R U . . .
H18C H 0.3841 0.0241 0.9013 0.080 Uiso 1 1 calc R U . . .
Br2 Br 0.3444(2) 0.33721(10) 0.61758(16) 0.0277(6) Uani 0.632 1 d . . P C -2
Cl1 Cl 0.0804(13) 0.1671(8) 0.9509(10) 0.053(4) Uani 0.368 1 d D . P B 2
Cl3 Cl 0.206(2) 0.5167(14) 0.991(2) 0.0277(4) Uani 0.324 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br3 C8 1.897(6) . ?
Br1 C3 1.863(5) . ?
Fe1 O5 2.087(3) 3_667 ?
Fe1 O4 1.984(3) 4_666 ?
Fe1 O3 1.996(3) 4_666 ?
Fe1 O1 1.995(3) . ?
Fe1 O6 2.085(3) . ?
Fe1 O2 1.985(3) . ?
Cl2 C6 1.781(11) . ?
O5 Fe1 2.087(3) 3_667 ?
O5 C7 1.256(5) . ?
O4 Fe1 1.984(3) 4_565 ?
O4 C5 1.292(5) . ?
O3 Fe1 1.996(3) 4_565 ?
O3 C4 1.294(5) . ?
O1 C1 1.294(5) . ?
O6 C9 1.260(5) . ?
O2 C2 1.306(5) . ?
N1 C13 1.526(6) . ?
N1 C16 1.525(6) . ?
N1 C10 1.519(5) . ?
N1 C19 1.524(6) . ?
C1 C2 1.481(6) . ?
C1 C6 1.401(5) . ?
C4 C3 1.401(5) . ?
C4 C5 1.474(6) . ?
C2 C3 1.395(6) . ?
C3 Cl1 1.767(12) . ?
C9 C7 1.540(6) 3_667 ?
C9 C8 1.375(6) . ?
C6 C5 1.389(6) . ?
C6 Br2 1.859(5) . ?
C7 C9 1.540(6) 3_667 ?
C7 C8 1.391(6) . ?
C8 Cl3 1.77(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.519(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.518(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.515(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.527(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 C11 1.531(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.520(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.527(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.528(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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
O4 Fe1 O5 87.29(12) 4_666 3_667 ?
O4 Fe1 O3 81.62(12) 4_666 4_666 ?
O4 Fe1 O1 101.35(12) 4_666 . ?
O4 Fe1 O6 161.79(12) 4_666 . ?
O4 Fe1 O2 101.59(12) 4_666 . ?
O3 Fe1 O5 90.94(12) 4_666 3_667 ?
O3 Fe1 O6 89.00(12) 4_666 . ?
O1 Fe1 O5 88.01(12) . 3_667 ?
O1 Fe1 O3 176.79(13) . 4_666 ?
O1 Fe1 O6 87.81(12) . . ?
O6 Fe1 O5 77.25(12) . 3_667 ?
O2 Fe1 O5 166.77(12) . 3_667 ?
O2 Fe1 O3 99.97(12) . 4_666 ?
O2 Fe1 O1 80.69(12) . . ?
O2 Fe1 O6 95.36(12) . . ?
C7 O5 Fe1 115.7(3) . 3_667 ?
C5 O4 Fe1 112.7(3) . 4_565 ?
C4 O3 Fe1 111.9(3) . 4_565 ?
C1 O1 Fe1 114.2(3) . . ?
C9 O6 Fe1 116.0(3) . . ?
C2 O2 Fe1 114.5(3) . . ?
C16 N1 C13 108.1(3) . . ?
C10 N1 C13 111.2(3) . . ?
C10 N1 C16 108.4(3) . . ?
C10 N1 C19 108.2(3) . . ?
C19 N1 C13 109.0(3) . . ?
C19 N1 C16 112.0(4) . . ?
O1 C1 C2 115.1(3) . . ?
O1 C1 C6 125.5(4) . . ?
C6 C1 C2 119.4(4) . . ?
O3 C4 C3 124.3(4) . . ?
O3 C4 C5 116.1(4) . . ?
C3 C4 C5 119.6(4) . . ?
O2 C2 C1 114.7(4) . . ?
O2 C2 C3 125.4(4) . . ?
C3 C2 C1 119.9(4) . . ?
C4 C3 Br1 119.9(3) . . ?
C4 C3 Cl1 120.7(6) . . ?
C2 C3 Br1 119.9(3) . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 Cl1 119.0(5) . . ?
Cl1 C3 Br1 1.3(6) . . ?
O6 C9 C7 114.5(4) . 3_667 ?
O6 C9 C8 126.9(4) . . ?
C8 C9 C7 118.7(4) . 3_667 ?
Cl2 C6 Br2 0.9(5) . . ?
C1 C6 Cl2 119.0(5) . . ?
C1 C6 Br2 119.0(3) . . ?
C5 C6 Cl2 120.6(5) . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 Br2 120.6(3) . . ?
O4 C5 C4 115.5(4) . . ?
O4 C5 C6 124.2(4) . . ?
C6 C5 C4 120.2(4) . . ?
O5 C7 C9 115.5(4) . 3_667 ?
O5 C7 C8 125.2(4) . . ?
C8 C7 C9 119.2(4) . 3_667 ?
C9 C8 Br3 119.5(4) . . ?
C9 C8 C7 122.0(4) . . ?
C9 C8 Cl3 117.2(10) . . ?
C7 C8 Br3 118.5(4) . . ?
C7 C8 Cl3 120.6(10) . . ?
Cl3 C8 Br3 4.7(9) . . ?
N1 C13 H13A 108.3 . . ?
N1 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 N1 115.9(4) . . ?
C14 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
N1 C16 H16A 108.3 . . ?
N1 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C17 C16 N1 116.0(4) . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
N1 C10 H10A 108.0 . . ?
N1 C10 H10B 108.0 . . ?
H10A C10 H10B 107.2 . . ?
C11 C10 N1 117.2(4) . . ?
C11 C10 H10A 108.0 . . ?
C11 C10 H10B 108.0 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C13 C14 C15 109.5(4) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
N1 C19 H19A 108.4 . . ?
N1 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 N1 115.5(4) . . ?
C20 C19 H19A 108.4 . . ?
C20 C19 H19B 108.4 . . ?
C10 C11 C12 108.2(4) . . ?
C10 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
C19 C20 C21 109.2(4) . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
C16 C17 H17A 109.9 . . ?
C16 C17 H17B 109.9 . . ?
C16 C17 C18 108.9(5) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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 O5 C7 C9 -3.9(4) 3_667 . . 3_667 ?
Fe1 O5 C7 C8 175.3(3) 3_667 . . . ?
Fe1 O4 C5 C4 -10.0(4) 4_565 . . . ?
Fe1 O4 C5 C6 170.2(3) 4_565 . . . ?
Fe1 O3 C4 C3 -169.8(3) 4_565 . . . ?
Fe1 O3 C4 C5 11.3(4) 4_565 . . . ?
Fe1 O1 C1 C2 -9.3(4) . . . . ?
Fe1 O1 C1 C6 170.1(3) . . . . ?
Fe1 O6 C9 C7 -10.4(4) . . . 3_667 ?
Fe1 O6 C9 C8 171.1(4) . . . . ?
Fe1 O2 C2 C1 3.1(4) . . . . ?
Fe1 O2 C2 C3 -177.7(3) . . . . ?
Cl2 C6 C5 O4 1.9(8) . . . . ?
Cl2 C6 C5 C4 -177.9(6) . . . . ?
O5 C7 C8 Br3 3.2(6) . . . . ?
O5 C7 C8 C9 -176.8(4) . . . . ?
O5 C7 C8 Cl3 -1.6(12) . . . . ?
O3 C4 C3 Br1 1.8(6) . . . . ?
O3 C4 C3 C2 -175.9(4) . . . . ?
O3 C4 C3 Cl1 0.6(9) . . . . ?
O3 C4 C5 O4 -1.0(6) . . . . ?
O3 C4 C5 C6 178.8(4) . . . . ?
O1 C1 C2 O2 4.2(5) . . . . ?
O1 C1 C2 C3 -175.0(4) . . . . ?
O1 C1 C6 Cl2 -4.0(8) . . . . ?
O1 C1 C6 C5 177.9(4) . . . . ?
O1 C1 C6 Br2 -3.0(6) . . . . ?
O6 C9 C8 Br3 -4.0(6) . . . . ?
O6 C9 C8 C7 176.1(4) . . . . ?
O6 C9 C8 Cl3 0.7(12) . . . . ?
O2 C2 C3 Br1 -2.5(6) . . . . ?
O2 C2 C3 C4 175.2(4) . . . . ?
O2 C2 C3 Cl1 -1.3(8) . . . . ?
N1 C13 C14 C15 174.8(4) . . . . ?
N1 C16 C17 C18 -176.2(4) . . . . ?
N1 C10 C11 C12 -176.6(4) . . . . ?
N1 C19 C20 C21 -179.0(5) . . . . ?
C1 C2 C3 Br1 176.6(3) . . . . ?
C1 C2 C3 C4 -5.6(6) . . . . ?
C1 C2 C3 Cl1 177.8(6) . . . . ?
C1 C6 C5 O4 179.9(4) . . . . ?
C1 C6 C5 C4 0.2(6) . . . . ?
C2 C1 C6 Cl2 175.3(6) . . . . ?
C2 C1 C6 C5 -2.7(6) . . . . ?
C2 C1 C6 Br2 176.3(3) . . . . ?
C3 C4 C5 O4 -180.0(4) . . . . ?
C3 C4 C5 C6 -0.2(6) . . . . ?
C9 C7 C8 Br3 -177.6(3) 3_667 . . . ?
C9 C7 C8 C9 2.4(7) 3_667 . . . ?
C9 C7 C8 Cl3 177.7(10) 3_667 . . . ?
C6 C1 C2 O2 -175.2(4) . . . . ?
C6 C1 C2 C3 5.5(6) . . . . ?
C5 C4 C3 Br1 -179.2(3) . . . . ?
C5 C4 C3 C2 3.0(6) . . . . ?
C5 C4 C3 Cl1 179.5(7) . . . . ?
C7 C9 C8 Br3 177.6(3) 3_667 . . . ?
C7 C9 C8 C7 -2.4(7) 3_667 . . . ?
C7 C9 C8 Cl3 -177.8(10) 3_667 . . . ?
C13 N1 C16 C17 -66.3(5) . . . . ?
C13 N1 C10 C11 -49.9(5) . . . . ?
C13 N1 C19 C20 174.1(4) . . . . ?
C16 N1 C13 C14 -175.4(4) . . . . ?
C16 N1 C10 C11 68.7(5) . . . . ?
C16 N1 C19 C20 54.5(5) . . . . ?
C10 N1 C13 C14 -56.5(5) . . . . ?
C10 N1 C16 C17 173.1(4) . . . . ?
C10 N1 C19 C20 -64.9(5) . . . . ?
C19 N1 C13 C14 62.6(5) . . . . ?
C19 N1 C16 C17 53.8(5) . . . . ?
C19 N1 C10 C11 -169.6(4) . . . . ?
Br2 C6 C5 O4 0.8(6) . . . . ?
Br2 C6 C5 C4 -178.9(3) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.828
####################################################################### 
# 
# 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_Br-035_CCDC-2014806_R1
_database_code_depnum_ccdc_archive 'CCDC 2014806'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-08-01
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br2.12 C18 Cl3.88 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Br2.12 Cl3.88 Fe2 N2 O15'
_chemical_formula_weight         1333.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl3.88 Br2.12 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.3278(4)
_cell_length_b                   21.7798(3)
_cell_length_c                   14.4219(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.935(2)
_cell_angle_gamma                90
_cell_volume                     6074.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24741
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.3920
_cell_measurement_theta_min      1.7410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2737
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41976
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.754
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0313101000
_diffrn_orient_matrix_UB_12      0.0162833000
_diffrn_orient_matrix_UB_13      -0.0207428000
_diffrn_orient_matrix_UB_21      -0.0190729000
_diffrn_orient_matrix_UB_22      -0.0269691000
_diffrn_orient_matrix_UB_23      0.0019508000
_diffrn_orient_matrix_UB_31      -0.0005982000
_diffrn_orient_matrix_UB_32      0.0082328000
_diffrn_orient_matrix_UB_33      0.0473322000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8830
_reflns_number_total             11085
_reflns_odcompleteness_completeness 90.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.37
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         11085
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.054
_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)+(0.0553P)²+5.4512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1071
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C3
 1.73 with sigma of 0.02
 C17-Cl6
 1.73 with sigma of 0.02
 Cl3-C8
 1.73 with sigma of 0.02
 Cl2-C6
 1.73 with sigma of 0.02
 C11-Br4
 1.88 with sigma of 0.02
 Cl5-C14
 1.73 with sigma of 0.02
 C17-Br6
 1.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O15) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(Cl1) = Uanis(Br1)
4. Others
 Fixed Sof: Cl6(0.642) Cl1(0.656) Cl3(0.642) Cl4(0.642) Cl5(0.642) Cl2(0.656)
 O16(0.5) O15(0.5) Br2(0.344) Br5(0.358) Br6(0.358) Br3(0.358) Br1(0.344)
 Br4(0.358)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C22(H22A,H22B), C34(H34A,H34B), C41(H41A,H41B), C40(H40A,
 H40B), C20(H20A,H20B), C29(H29A,H29B), C19(H19A,H19B), C31(H31A,H31B),
 C28(H28A,H28B), C35(H35A,H35B), C26(H26A,H26B), C37(H37A,H37B), C23(H23A,H23B),
  C32(H32A,H32B), C38(H38A,H38B)
5.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C33(H33A,H33B,H33C), C44(H44A,H44B,H44C),
 C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe2 Fe 0.22105(2) 0.31958(2) 0.39562(3) 0.01493(10) Uani 1 1 d . . . . .
Fe1 Fe 0.23943(2) 0.68349(2) 0.41099(3) 0.01591(10) Uani 1 1 d . . . . .
Cl6 Cl 0.0811(6) 0.3195(5) 0.0382(9) 0.0202(11) Uani 0.642 1 d D . P A 2
Cl1 Cl 0.1042(8) 0.8261(8) 0.5519(13) 0.0224(8) Uani 0.656 1 d D . P B 2
Cl3 Cl 0.3792(4) 0.4973(3) 0.3670(5) 0.045(2) Uani 0.642 1 d D . P C 2
Cl4 Cl 0.0896(6) 0.5087(6) 0.4647(11) 0.0235(15) Uani 0.642 1 d . . P D 2
Cl5 Cl 0.3569(5) 0.1781(4) 0.2521(7) 0.042(2) Uani 0.642 1 d D . P E 2
Cl2 Cl 0.3781(7) 0.6747(7) 0.7644(9) 0.033(2) Uani 0.656 1 d D . P F 2
O12 O 0.16253(9) 0.32004(8) 0.25524(13) 0.0175(4) Uani 1 1 d . . . . .
O9 O 0.27668(9) 0.26373(8) 0.33995(12) 0.0178(4) Uani 1 1 d . . . . .
O2 O 0.18606(9) 0.74323(8) 0.46346(12) 0.0175(4) Uani 1 1 d . . . . .
O11 O 0.16569(9) 0.23807(8) -0.05073(12) 0.0178(4) Uani 1 1 d . . . . .
O8 O 0.18084(9) 0.61145(8) 0.43761(13) 0.0188(4) Uani 1 1 d . . . . .
O3 O 0.18226(9) 0.81924(8) 0.77128(13) 0.0183(4) Uani 1 1 d . . . . .
O4 O 0.29520(9) 0.76101(9) 0.85580(12) 0.0195(4) Uani 1 1 d . . . . .
O7 O 0.16728(9) 0.39601(8) 0.42205(13) 0.0186(4) Uani 1 1 d . . . . .
O10 O 0.28176(9) 0.18509(8) 0.03496(13) 0.0187(4) Uani 1 1 d . . . . .
O1 O 0.30063(9) 0.68661(8) 0.54886(13) 0.0189(4) Uani 1 1 d . . . . .
O6 O 0.28435(9) 0.39268(8) 0.38383(13) 0.0187(4) Uani 1 1 d . . . . .
O5 O 0.29748(9) 0.60744(8) 0.39752(13) 0.0188(4) Uani 1 1 d . . . . .
N1 N 0.50877(12) 0.79985(11) 1.00771(16) 0.0231(5) Uani 1 1 d . . . . .
N2 N 0.04718(12) 0.64770(11) 0.72822(17) 0.0245(5) Uani 1 1 d . . . . .
C16 C 0.19005(13) 0.24763(12) 0.04209(19) 0.0163(5) Uani 1 1 d . . . . .
C2 C 0.20980(13) 0.75000(12) 0.55729(18) 0.0161(6) Uani 1 1 d . . . . .
C4 C 0.20823(13) 0.78912(12) 0.71389(19) 0.0162(6) Uani 1 1 d . . . . .
C18 C 0.18851(13) 0.28920(11) 0.19776(19) 0.0157(5) Uani 1 1 d . . . . .
C15 C 0.25574(13) 0.21623(12) 0.09101(19) 0.0169(6) Uani 1 1 d . . . . .
C5 C 0.27248(14) 0.75530(12) 0.76214(19) 0.0174(6) Uani 1 1 d . . . . .
C1 C 0.27432(13) 0.71681(12) 0.60559(19) 0.0174(6) Uani 1 1 d . . . . .
C13 C 0.25361(13) 0.25695(12) 0.24664(19) 0.0170(6) Uani 1 1 d . . . . .
C3 C 0.17965(13) 0.78612(12) 0.61271(19) 0.0167(6) Uani 1 1 d D . . . .
C9 C 0.26419(14) 0.44555(12) 0.39806(19) 0.0176(6) Uani 1 1 d . . . . .
C7 C 0.27110(14) 0.55608(12) 0.40501(19) 0.0181(6) Uani 1 1 d . . . . .
C10 C 0.19529(13) 0.44757(12) 0.42108(18) 0.0166(6) Uani 1 1 d . . . . .
C6 C 0.30363(14) 0.72064(13) 0.7065(2) 0.0208(6) Uani 1 1 d D . . . .
C17 C 0.15959(13) 0.28438(12) 0.09664(19) 0.0177(6) Uani 1 1 d D . . . .
C14 C 0.28487(14) 0.22195(12) 0.19163(19) 0.0192(6) Uani 1 1 d D . . . .
C12 C 0.20230(14) 0.55857(12) 0.42858(18) 0.0177(6) Uani 1 1 d . . . . .
C8 C 0.29898(14) 0.49967(12) 0.3942(2) 0.0196(6) Uani 1 1 d D . . . .
C25 C 0.57063(14) 0.76075(13) 1.0089(2) 0.0259(7) Uani 1 1 d . . . . .
H25A H 0.6089 0.7885 1.0077 0.031 Uiso 1 1 calc R U . . .
H25B H 0.5856 0.7381 1.0714 0.031 Uiso 1 1 calc R U . . .
C22 C 0.44658(14) 0.76041(14) 1.0058(2) 0.0266(7) Uani 1 1 d . . . . .
H22A H 0.4083 0.7880 1.0078 0.032 Uiso 1 1 calc R U . . .
H22B H 0.4315 0.7382 0.9429 0.032 Uiso 1 1 calc R U . . .
C11 C 0.16931(14) 0.50406(12) 0.4387(2) 0.0194(6) Uani 1 1 d D . . . .
C34 C -0.00112(16) 0.63750(14) 0.6262(2) 0.0289(7) Uani 1 1 d . . . . .
H34A H -0.0021 0.5929 0.6125 0.035 Uiso 1 1 calc R U . . .
H34B H -0.0482 0.6493 0.6257 0.035 Uiso 1 1 calc R U . . .
C41 C -0.00599(16) 0.75445(13) 0.7369(2) 0.0300(7) Uani 1 1 d . . . . .
H41A H -0.0289 0.7424 0.7856 0.036 Uiso 1 1 calc R U . . .
H41B H -0.0389 0.7475 0.6711 0.036 Uiso 1 1 calc R U . . .
C40 C 0.05805(16) 0.71599(14) 0.7503(2) 0.0298(7) Uani 1 1 d . . . . .
H40A H 0.0878 0.7205 0.8187 0.036 Uiso 1 1 calc R U . . .
H40B H 0.0838 0.7332 0.7081 0.036 Uiso 1 1 calc R U . . .
C20 C 0.47863(17) 0.88514(14) 1.1114(2) 0.0305(7) Uani 1 1 d . . . . .
H20A H 0.4329 0.8652 1.0986 0.037 Uiso 1 1 calc R U . . .
H20B H 0.4739 0.9189 1.0638 0.037 Uiso 1 1 calc R U . . .
C29 C 0.53951(18) 0.88544(14) 0.9055(2) 0.0341(8) Uani 1 1 d . . . . .
H29A H 0.5845 0.8647 0.9154 0.041 Uiso 1 1 calc R U . . .
H29B H 0.5460 0.9182 0.9551 0.041 Uiso 1 1 calc R U . . .
C19 C 0.53068(16) 0.83899(14) 1.0995(2) 0.0271(7) Uani 1 1 d . . . . .
H19A H 0.5425 0.8112 1.1566 0.033 Uiso 1 1 calc R U . . .
H19B H 0.5734 0.8613 1.1008 0.033 Uiso 1 1 calc R U . . .
C31 C 0.01432(17) 0.61932(14) 0.7991(2) 0.0306(7) Uani 1 1 d . . . . .
H31A H 0.0443 0.6281 0.8662 0.037 Uiso 1 1 calc R U . . .
H31B H -0.0306 0.6398 0.7906 0.037 Uiso 1 1 calc R U . . .
C28 C 0.48641(16) 0.83951(14) 0.9166(2) 0.0272(7) Uani 1 1 d . . . . .
H28A H 0.4739 0.8122 0.8589 0.033 Uiso 1 1 calc R U . . .
H28B H 0.4442 0.8622 0.9163 0.033 Uiso 1 1 calc R U . . .
C42 C 0.01403(18) 0.82194(15) 0.7494(3) 0.0380(8) Uani 1 1 d . . . . .
H42A H -0.0275 0.8469 0.7412 0.057 Uiso 1 1 calc R U . . .
H42B H 0.0360 0.8338 0.7004 0.057 Uiso 1 1 calc R U . . .
H42C H 0.0465 0.8286 0.8147 0.057 Uiso 1 1 calc R U . . .
C35 C 0.01402(19) 0.67026(15) 0.5438(2) 0.0366(8) Uani 1 1 d . . . . .
H35A H 0.0599 0.6577 0.5397 0.044 Uiso 1 1 calc R U . . .
H35B H 0.0146 0.7152 0.5545 0.044 Uiso 1 1 calc R U . . .
C26 C 0.56058(17) 0.71503(16) 0.9277(3) 0.0410(9) Uani 1 1 d . . . . .
H26A H 0.5547 0.7369 0.8654 0.049 Uiso 1 1 calc R U . . .
H26B H 0.5184 0.6905 0.9211 0.049 Uiso 1 1 calc R U . . .
C27 C 0.62326(17) 0.67270(15) 0.9495(3) 0.0431(9) Uani 1 1 d . . . . .
H27A H 0.6175 0.6441 0.8951 0.065 Uiso 1 1 calc R U . . .
H27B H 0.6274 0.6495 1.0092 0.065 Uiso 1 1 calc R U . . .
H27C H 0.6651 0.6973 0.9581 0.065 Uiso 1 1 calc R U . . .
C37 C 0.11682(16) 0.61893(15) 0.7368(2) 0.0341(8) Uani 1 1 d . . . . .
H37A H 0.1088 0.5767 0.7105 0.041 Uiso 1 1 calc R U . . .
H37B H 0.1384 0.6424 0.6950 0.041 Uiso 1 1 calc R U . . .
C23 C 0.45733(17) 0.71395(17) 1.0869(3) 0.0421(9) Uani 1 1 d . . . . .
H23A H 0.4638 0.7353 1.1497 0.051 Uiso 1 1 calc R U . . .
H23B H 0.4993 0.6894 1.0924 0.051 Uiso 1 1 calc R U . . .
C24 C 0.39424(17) 0.67182(15) 1.0648(3) 0.0420(9) Uani 1 1 d . . . . .
H24A H 0.3900 0.6486 1.0051 0.063 Uiso 1 1 calc R U . . .
H24B H 0.3525 0.6966 1.0561 0.063 Uiso 1 1 calc R U . . .
H24C H 0.3997 0.6432 1.1192 0.063 Uiso 1 1 calc R U . . .
O13 O 0.1338(2) 0.46449(16) 0.7765(4) 0.1114(15) Uani 1 1 d . . . . .
C30 C 0.5147(2) 0.91348(17) 0.8037(3) 0.0464(10) Uani 1 1 d . . . . .
H30A H 0.5088 0.8809 0.7549 0.070 Uiso 1 1 calc R U . . .
H30B H 0.5490 0.9432 0.7964 0.070 Uiso 1 1 calc R U . . .
H30C H 0.4704 0.9343 0.7945 0.070 Uiso 1 1 calc R U . . .
C32 C 0.00210(19) 0.55118(15) 0.7897(2) 0.0382(8) Uani 1 1 d . . . . .
H32A H 0.0460 0.5302 0.7933 0.046 Uiso 1 1 calc R U . . .
H32B H -0.0316 0.5420 0.7253 0.046 Uiso 1 1 calc R U . . .
C21 C 0.50187(19) 0.91114(16) 1.2147(2) 0.0425(9) Uani 1 1 d . . . . .
H21A H 0.4684 0.9419 1.2213 0.064 Uiso 1 1 calc R U . . .
H21B H 0.5474 0.9303 1.2276 0.064 Uiso 1 1 calc R U . . .
H21C H 0.5047 0.8779 1.2616 0.064 Uiso 1 1 calc R U . . .
C36 C -0.0419(2) 0.65379(16) 0.4501(2) 0.0434(9) Uani 1 1 d . . . . .
H36A H -0.0392 0.6816 0.3980 0.065 Uiso 1 1 calc R U . . .
H36B H -0.0874 0.6578 0.4598 0.065 Uiso 1 1 calc R U . . .
H36C H -0.0353 0.6114 0.4320 0.065 Uiso 1 1 calc R U . . .
C38 C 0.16765(18) 0.61589(18) 0.8381(3) 0.0521(10) Uani 1 1 d . . . . .
H38A H 0.1497 0.5880 0.8789 0.063 Uiso 1 1 calc R U . . .
H38B H 0.1732 0.6572 0.8680 0.063 Uiso 1 1 calc R U . . .
C39 C 0.23700(19) 0.59284(18) 0.8344(3) 0.0602(12) Uani 1 1 d . . . . .
H39A H 0.2315 0.5518 0.8052 0.090 Uiso 1 1 calc R U . . .
H39B H 0.2694 0.5909 0.9007 0.090 Uiso 1 1 calc R U . . .
H39C H 0.2551 0.6209 0.7950 0.090 Uiso 1 1 calc R U . . .
C43 C 0.1736(2) 0.42536(18) 0.7700(4) 0.0597(12) Uani 1 1 d . . . . .
O14 O 0.3355(3) 1.00418(19) 0.5853(5) 0.134(2) Uani 1 1 d . . . . .
C45 C 0.2135(3) 0.4314(2) 0.6985(3) 0.0731(14) Uani 1 1 d . . . . .
H45A H 0.2026 0.4709 0.6645 0.110 Uiso 1 1 calc R U . . .
H45B H 0.2009 0.3979 0.6509 0.110 Uiso 1 1 calc R U . . .
H45C H 0.2632 0.4295 0.7333 0.110 Uiso 1 1 calc R U . . .
C46 C 0.2813(3) 1.0016(2) 0.6054(4) 0.0717(14) Uani 1 1 d . . . . .
C48 C 0.2548(3) 0.9417(2) 0.6258(4) 0.0782(15) Uani 1 1 d . . . . .
H48A H 0.2775 0.9087 0.6007 0.117 Uiso 1 1 calc R U . . .
H48B H 0.2048 0.9398 0.5939 0.117 Uiso 1 1 calc R U . . .
H48C H 0.2647 0.9368 0.6963 0.117 Uiso 1 1 calc R U . . .
C33 C -0.0249(3) 0.5268(2) 0.8689(4) 0.0798(16) Uani 1 1 d . . . . .
H33A H -0.0337 0.4826 0.8594 0.120 Uiso 1 1 calc R U . . .
H33B H -0.0681 0.5479 0.8661 0.120 Uiso 1 1 calc R U . . .
H33C H 0.0094 0.5340 0.9326 0.120 Uiso 1 1 calc R U . . .
C44 C 0.1858(3) 0.3706(2) 0.8348(4) 0.0917(18) Uani 1 1 d . . . . .
H44A H 0.1612 0.3757 0.8830 0.138 Uiso 1 1 calc R U . . .
H44B H 0.2354 0.3663 0.8683 0.138 Uiso 1 1 calc R U . . .
H44C H 0.1688 0.3338 0.7956 0.138 Uiso 1 1 calc R U . . .
C47 C 0.2436(3) 1.0579(2) 0.6173(5) 0.0928(18) Uani 1 1 d . . . . .
H47A H 0.2399 1.0592 0.6835 0.139 Uiso 1 1 calc R U . . .
H47B H 0.1972 1.0575 0.5700 0.139 Uiso 1 1 calc R U . . .
H47C H 0.2688 1.0942 0.6064 0.139 Uiso 1 1 calc R U . . .
O16 O 0.4361(12) 0.9987(6) 0.4272(11) 0.236(10) Uani 0.5 1 d . U P G 3
O15 O 0.4859(7) 1.0678(12) 0.4826(14) 0.296(11) Uani 0.5 1 d . U P H -3
Br2 Br 0.3844(6) 0.6801(6) 0.7652(7) 0.0318(12) Uani 0.344 1 d . . P F -2
Br5 Br 0.3679(4) 0.1803(2) 0.2510(4) 0.0246(5) Uani 0.358 1 d . . P E -2
Br6 Br 0.0795(5) 0.3298(4) 0.0310(7) 0.0219(10) Uani 0.358 1 d D . P A -2
Br3 Br 0.3818(2) 0.49812(17) 0.3703(2) 0.0164(8) Uani 0.358 1 d . . P C -2
Br1 Br 0.1003(6) 0.8330(6) 0.5539(10) 0.0224(8) Uani 0.344 1 d . . P B -2
Br4 Br 0.0900(4) 0.5102(5) 0.4793(8) 0.0224(10) Uani 0.358 1 d D . P D -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe2 O12 2.0077(18) . ?
Fe2 O9 1.9904(18) . ?
Fe2 O11 1.9945(18) 4_566 ?
Fe2 O7 2.0899(18) . ?
Fe2 O10 2.0110(18) 4_566 ?
Fe2 O6 2.0867(18) . ?
Fe1 O2 1.9872(18) . ?
Fe1 O8 2.0759(18) . ?
Fe1 O3 1.9929(18) 4_575 ?
Fe1 O4 1.9838(18) 4_575 ?
Fe1 O1 1.9957(18) . ?
Fe1 O5 2.0772(19) . ?
Cl6 C17 1.736(10) . ?
Cl1 C3 1.746(13) . ?
Cl3 C8 1.792(8) . ?
Cl4 C11 1.775(13) . ?
Cl5 C14 1.741(8) . ?
Cl2 C6 1.793(11) . ?
O12 C18 1.299(3) . ?
O9 C13 1.290(3) . ?
O2 C2 1.298(3) . ?
O11 Fe2 1.9945(18) 4_565 ?
O11 C16 1.293(3) . ?
O8 C12 1.252(3) . ?
O3 Fe1 1.9929(18) 4_576 ?
O3 C4 1.290(3) . ?
O4 Fe1 1.9837(18) 4_576 ?
O4 C5 1.292(3) . ?
O7 C10 1.261(3) . ?
O10 Fe2 2.0111(18) 4_565 ?
O10 C15 1.287(3) . ?
O1 C1 1.288(3) . ?
O6 C9 1.260(3) . ?
O5 C7 1.259(3) . ?
N1 C25 1.514(3) . ?
N1 C22 1.522(3) . ?
N1 C19 1.521(4) . ?
N1 C28 1.521(4) . ?
N2 C34 1.513(4) . ?
N2 C40 1.523(4) . ?
N2 C31 1.515(4) . ?
N2 C37 1.518(4) . ?
C16 C15 1.472(4) . ?
C16 C17 1.394(4) . ?
C2 C1 1.471(4) . ?
C2 C3 1.391(4) . ?
C4 C5 1.474(4) . ?
C4 C3 1.396(4) . ?
C18 C13 1.472(4) . ?
C18 C17 1.398(4) . ?
C15 C14 1.394(4) . ?
C5 C6 1.389(4) . ?
C1 C6 1.395(4) . ?
C13 C14 1.387(4) . ?
C3 Br1 1.876(11) . ?
C9 C10 1.536(4) . ?
C9 C8 1.385(4) . ?
C7 C12 1.538(4) . ?
C7 C8 1.382(4) . ?
C10 C11 1.393(4) . ?
C6 Br2 1.826(9) . ?
C17 Br6 1.891(8) . ?
C14 Br5 1.875(7) . ?
C12 C11 1.393(4) . ?
C8 Br3 1.820(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.502(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.511(4) . ?
C11 Br4 1.881(10) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.497(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C40 1.510(4) . ?
C41 C42 1.521(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C19 1.507(4) . ?
C20 C21 1.526(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C28 1.516(4) . ?
C29 C30 1.525(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.504(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.517(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.525(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.509(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.529(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O13 C43 1.199(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.507(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.513(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C43 C45 1.502(6) . ?
C43 C44 1.488(6) . ?
O14 C46 1.224(6) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.475(6) . ?
C46 C47 1.483(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 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
O12 Fe2 O7 89.95(7) . . ?
O12 Fe2 O10 177.01(8) . 4_566 ?
O12 Fe2 O6 95.90(7) . . ?
O9 Fe2 O12 80.22(7) . . ?
O9 Fe2 O11 103.31(8) . 4_566 ?
O9 Fe2 O7 162.62(7) . . ?
O9 Fe2 O10 97.01(7) . 4_566 ?
O9 Fe2 O6 89.56(7) . . ?
O11 Fe2 O12 99.47(7) 4_566 . ?
O11 Fe2 O7 92.37(7) 4_566 . ?
O11 Fe2 O10 80.00(7) 4_566 4_566 ?
O11 Fe2 O6 161.38(7) 4_566 . ?
O10 Fe2 O7 93.01(7) 4_566 . ?
O10 Fe2 O6 85.18(7) 4_566 . ?
O6 Fe2 O7 77.14(7) . . ?
O2 Fe1 O8 90.73(7) . . ?
O2 Fe1 O3 100.82(7) . 4_575 ?
O2 Fe1 O1 81.04(7) . . ?
O2 Fe1 O5 161.85(7) . . ?
O8 Fe1 O5 77.84(7) . . ?
O3 Fe1 O8 88.58(7) 4_575 . ?
O3 Fe1 O1 177.31(8) 4_575 . ?
O3 Fe1 O5 93.03(7) 4_575 . ?
O4 Fe1 O2 101.55(8) 4_575 . ?
O4 Fe1 O8 165.02(7) 4_575 . ?
O4 Fe1 O3 80.79(7) 4_575 4_575 ?
O4 Fe1 O1 96.96(7) 4_575 . ?
O4 Fe1 O5 92.13(7) 4_575 . ?
O1 Fe1 O8 93.36(7) . . ?
O1 Fe1 O5 85.56(7) . . ?
C18 O12 Fe2 114.20(16) . . ?
C13 O9 Fe2 114.93(16) . . ?
C2 O2 Fe1 113.58(16) . . ?
C16 O11 Fe2 114.90(16) . 4_565 ?
C12 O8 Fe1 115.96(17) . . ?
C4 O3 Fe1 114.03(16) . 4_576 ?
C5 O4 Fe1 114.43(16) . 4_576 ?
C10 O7 Fe2 116.36(16) . . ?
C15 O10 Fe2 114.20(16) . 4_565 ?
C1 O1 Fe1 113.39(16) . . ?
C9 O6 Fe2 116.38(16) . . ?
C7 O5 Fe1 115.54(17) . . ?
C25 N1 C22 111.4(2) . . ?
C25 N1 C19 106.6(2) . . ?
C25 N1 C28 110.8(2) . . ?
C19 N1 C22 110.5(2) . . ?
C28 N1 C22 106.2(2) . . ?
C28 N1 C19 111.3(2) . . ?
C34 N2 C40 110.8(2) . . ?
C34 N2 C31 107.9(2) . . ?
C34 N2 C37 109.2(2) . . ?
C31 N2 C40 108.8(2) . . ?
C31 N2 C37 111.8(2) . . ?
C37 N2 C40 108.3(2) . . ?
O11 C16 C15 115.0(2) . . ?
O11 C16 C17 125.6(2) . . ?
C17 C16 C15 119.4(2) . . ?
O2 C2 C1 115.4(2) . . ?
O2 C2 C3 125.1(2) . . ?
C3 C2 C1 119.5(2) . . ?
O3 C4 C5 115.4(2) . . ?
O3 C4 C3 125.0(2) . . ?
C3 C4 C5 119.5(2) . . ?
O12 C18 C13 115.0(2) . . ?
O12 C18 C17 125.6(2) . . ?
C17 C18 C13 119.4(2) . . ?
O10 C15 C16 115.5(2) . . ?
O10 C15 C14 125.2(2) . . ?
C14 C15 C16 119.3(2) . . ?
O4 C5 C4 115.1(2) . . ?
O4 C5 C6 125.2(2) . . ?
C6 C5 C4 119.6(2) . . ?
O1 C1 C2 115.7(2) . . ?
O1 C1 C6 124.5(2) . . ?
C6 C1 C2 119.8(2) . . ?
O9 C13 C18 115.4(2) . . ?
O9 C13 C14 125.2(2) . . ?
C14 C13 C18 119.4(2) . . ?
Cl1 C3 Br1 3.8(10) . . ?
C2 C3 Cl1 117.9(6) . . ?
C2 C3 C4 120.8(2) . . ?
C2 C3 Br1 121.2(5) . . ?
C4 C3 Cl1 121.3(6) . . ?
C4 C3 Br1 118.0(5) . . ?
O6 C9 C10 115.2(2) . . ?
O6 C9 C8 125.2(2) . . ?
C8 C9 C10 119.7(2) . . ?
O5 C7 C12 115.3(2) . . ?
O5 C7 C8 125.4(2) . . ?
C8 C7 C12 119.3(2) . . ?
O7 C10 C9 114.9(2) . . ?
O7 C10 C11 125.9(2) . . ?
C11 C10 C9 119.1(2) . . ?
Cl2 C6 Br2 5.3(11) . . ?
C5 C6 Cl2 120.3(5) . . ?
C5 C6 C1 120.7(2) . . ?
C5 C6 Br2 120.0(4) . . ?
C1 C6 Cl2 118.7(5) . . ?
C1 C6 Br2 119.3(4) . . ?
Cl6 C17 Br6 6.0(7) . . ?
C16 C17 Cl6 118.8(5) . . ?
C16 C17 C18 121.0(2) . . ?
C16 C17 Br6 118.8(4) . . ?
C18 C17 Cl6 120.1(5) . . ?
C18 C17 Br6 120.2(4) . . ?
Cl5 C14 Br5 6.1(6) . . ?
C15 C14 Cl5 119.7(4) . . ?
C15 C14 Br5 117.8(3) . . ?
C13 C14 Cl5 118.5(4) . . ?
C13 C14 C15 121.5(2) . . ?
C13 C14 Br5 120.8(3) . . ?
O8 C12 C7 115.1(2) . . ?
O8 C12 C11 125.3(2) . . ?
C11 C12 C7 119.5(2) . . ?
Cl3 C8 Br3 1.7(3) . . ?
C9 C8 Cl3 119.7(3) . . ?
C9 C8 Br3 120.4(2) . . ?
C7 C8 Cl3 118.9(3) . . ?
C7 C8 C9 121.3(3) . . ?
C7 C8 Br3 118.3(2) . . ?
N1 C25 H25A 108.1 . . ?
N1 C25 H25B 108.1 . . ?
H25A C25 H25B 107.3 . . ?
C26 C25 N1 116.8(2) . . ?
C26 C25 H25A 108.1 . . ?
C26 C25 H25B 108.1 . . ?
N1 C22 H22A 108.2 . . ?
N1 C22 H22B 108.2 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N1 116.3(2) . . ?
C23 C22 H22A 108.2 . . ?
C23 C22 H22B 108.2 . . ?
Cl4 C11 Br4 5.7(8) . . ?
C10 C11 Cl4 120.7(5) . . ?
C10 C11 C12 120.8(2) . . ?
C10 C11 Br4 121.9(4) . . ?
C12 C11 Cl4 118.3(5) . . ?
C12 C11 Br4 117.3(4) . . ?
N2 C34 H34A 107.8 . . ?
N2 C34 H34B 107.8 . . ?
H34A C34 H34B 107.1 . . ?
C35 C34 N2 118.1(3) . . ?
C35 C34 H34A 107.8 . . ?
C35 C34 H34B 107.8 . . ?
H41A C41 H41B 108.2 . . ?
C40 C41 H41A 109.8 . . ?
C40 C41 H41B 109.8 . . ?
C40 C41 C42 109.4(3) . . ?
C42 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
N2 C40 H40A 108.1 . . ?
N2 C40 H40B 108.1 . . ?
C41 C40 N2 116.8(2) . . ?
C41 C40 H40A 108.1 . . ?
C41 C40 H40B 108.1 . . ?
H40A C40 H40B 107.3 . . ?
H20A C20 H20B 108.2 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 110.0(3) . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
H29A C29 H29B 108.3 . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
C28 C29 C30 109.3(3) . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
N1 C19 H19A 108.2 . . ?
N1 C19 H19B 108.2 . . ?
C20 C19 N1 116.5(2) . . ?
C20 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
H19A C19 H19B 107.3 . . ?
N2 C31 H31A 108.3 . . ?
N2 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 N2 115.9(3) . . ?
C32 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
N1 C28 H28A 108.4 . . ?
N1 C28 H28B 108.4 . . ?
C29 C28 N1 115.7(2) . . ?
C29 C28 H28A 108.4 . . ?
C29 C28 H28B 108.4 . . ?
H28A C28 H28B 107.4 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C34 C35 H35A 110.0 . . ?
C34 C35 H35B 110.0 . . ?
C34 C35 C36 108.3(3) . . ?
H35A C35 H35B 108.4 . . ?
C36 C35 H35A 110.0 . . ?
C36 C35 H35B 110.0 . . ?
C25 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
C25 C26 C27 109.6(3) . . ?
H26A C26 H26B 108.2 . . ?
C27 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C37 H37A 108.3 . . ?
N2 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 N2 116.1(3) . . ?
C38 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C22 C23 C24 109.2(3) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C31 C32 C33 111.6(3) . . ?
H32A C32 H32B 108.0 . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C37 C38 H38A 109.6 . . ?
C37 C38 H38B 109.6 . . ?
C37 C38 C39 110.4(3) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.6 . . ?
C39 C38 H38B 109.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O13 C43 C45 120.8(4) . . ?
O13 C43 C44 120.4(5) . . ?
C44 C43 C45 118.8(4) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O14 C46 C48 119.8(5) . . ?
O14 C46 C47 121.6(5) . . ?
C48 C46 C47 118.4(5) . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 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
Fe2 O12 C18 C13 3.3(3) . . . . ?
Fe2 O12 C18 C17 -177.2(2) . . . . ?
Fe2 O9 C13 C18 -2.7(3) . . . . ?
Fe2 O9 C13 C14 177.9(2) . . . . ?
Fe2 O11 C16 C15 2.3(3) 4_565 . . . ?
Fe2 O11 C16 C17 -177.9(2) 4_565 . . . ?
Fe2 O7 C10 C9 1.3(3) . . . . ?
Fe2 O7 C10 C11 -178.6(2) . . . . ?
Fe2 O10 C15 C16 -5.7(3) 4_565 . . . ?
Fe2 O10 C15 C14 174.4(2) 4_565 . . . ?
Fe2 O6 C9 C10 -0.5(3) . . . . ?
Fe2 O6 C9 C8 179.6(2) . . . . ?
Fe1 O2 C2 C1 5.0(3) . . . . ?
Fe1 O2 C2 C3 -176.0(2) . . . . ?
Fe1 O8 C12 C7 3.4(3) . . . . ?
Fe1 O8 C12 C11 -177.0(2) . . . . ?
Fe1 O3 C4 C5 3.7(3) 4_576 . . . ?
Fe1 O3 C4 C3 -177.2(2) 4_576 . . . ?
Fe1 O4 C5 C4 -2.1(3) 4_576 . . . ?
Fe1 O4 C5 C6 178.0(2) 4_576 . . . ?
Fe1 O1 C1 C2 -8.0(3) . . . . ?
Fe1 O1 C1 C6 173.5(2) . . . . ?
Fe1 O5 C7 C12 -3.3(3) . . . . ?
Fe1 O5 C7 C8 177.0(2) . . . . ?
O12 C18 C13 O9 -0.4(3) . . . . ?
O12 C18 C13 C14 179.0(2) . . . . ?
O12 C18 C17 Cl6 -2.1(6) . . . . ?
O12 C18 C17 C16 -176.9(2) . . . . ?
O12 C18 C17 Br6 4.9(5) . . . . ?
O9 C13 C14 Cl5 5.7(5) . . . . ?
O9 C13 C14 C15 178.9(2) . . . . ?
O9 C13 C14 Br5 -0.8(5) . . . . ?
O2 C2 C1 O1 2.0(3) . . . . ?
O2 C2 C1 C6 -179.4(2) . . . . ?
O2 C2 C3 Cl1 -0.4(8) . . . . ?
O2 C2 C3 C4 178.3(2) . . . . ?
O2 C2 C3 Br1 -2.5(7) . . . . ?
O11 C16 C15 O10 2.3(3) . . . . ?
O11 C16 C15 C14 -177.8(2) . . . . ?
O11 C16 C17 Cl6 1.8(6) . . . . ?
O11 C16 C17 C18 176.8(2) . . . . ?
O11 C16 C17 Br6 -5.0(5) . . . . ?
O8 C12 C11 Cl4 1.0(7) . . . . ?
O8 C12 C11 C10 175.9(2) . . . . ?
O8 C12 C11 Br4 -5.3(5) . . . . ?
O3 C4 C5 O4 -1.1(3) . . . . ?
O3 C4 C5 C6 178.9(2) . . . . ?
O3 C4 C3 Cl1 1.7(9) . . . . ?
O3 C4 C3 C2 -177.0(2) . . . . ?
O3 C4 C3 Br1 3.8(6) . . . . ?
O4 C5 C6 Cl2 4.6(8) . . . . ?
O4 C5 C6 C1 179.1(3) . . . . ?
O4 C5 C6 Br2 -1.5(7) . . . . ?
O7 C10 C11 Cl4 -0.5(7) . . . . ?
O7 C10 C11 C12 -175.2(2) . . . . ?
O7 C10 C11 Br4 6.0(5) . . . . ?
O10 C15 C14 Cl5 -7.5(6) . . . . ?
O10 C15 C14 C13 179.5(3) . . . . ?
O10 C15 C14 Br5 -0.9(4) . . . . ?
O1 C1 C6 Cl2 -6.7(8) . . . . ?
O1 C1 C6 C5 178.7(3) . . . . ?
O1 C1 C6 Br2 -0.7(7) . . . . ?
O6 C9 C10 O7 -0.5(3) . . . . ?
O6 C9 C10 C11 179.4(2) . . . . ?
O6 C9 C8 Cl3 0.1(5) . . . . ?
O6 C9 C8 C7 176.1(3) . . . . ?
O6 C9 C8 Br3 -1.8(4) . . . . ?
O5 C7 C12 O8 -0.1(3) . . . . ?
O5 C7 C12 C11 -179.7(2) . . . . ?
O5 C7 C8 Cl3 -0.1(5) . . . . ?
O5 C7 C8 C9 -176.1(3) . . . . ?
O5 C7 C8 Br3 1.7(4) . . . . ?
N1 C25 C26 C27 -170.4(3) . . . . ?
N1 C22 C23 C24 -170.9(3) . . . . ?
N2 C34 C35 C36 -178.9(3) . . . . ?
N2 C31 C32 C33 175.1(3) . . . . ?
N2 C37 C38 C39 -173.7(3) . . . . ?
C16 C15 C14 Cl5 172.6(4) . . . . ?
C16 C15 C14 C13 -0.5(4) . . . . ?
C16 C15 C14 Br5 179.2(3) . . . . ?
C2 C1 C6 Cl2 174.8(7) . . . . ?
C2 C1 C6 C5 0.2(4) . . . . ?
C2 C1 C6 Br2 -179.2(6) . . . . ?
C4 C5 C6 Cl2 -175.4(7) . . . . ?
C4 C5 C6 C1 -0.9(4) . . . . ?
C4 C5 C6 Br2 178.5(6) . . . . ?
C18 C13 C14 Cl5 -173.6(4) . . . . ?
C18 C13 C14 C15 -0.5(4) . . . . ?
C18 C13 C14 Br5 179.9(3) . . . . ?
C15 C16 C17 Cl6 -178.4(5) . . . . ?
C15 C16 C17 C18 -3.5(4) . . . . ?
C15 C16 C17 Br6 174.7(4) . . . . ?
C5 C4 C3 Cl1 -179.2(8) . . . . ?
C5 C4 C3 C2 2.1(4) . . . . ?
C5 C4 C3 Br1 -177.1(6) . . . . ?
C1 C2 C3 Cl1 178.5(8) . . . . ?
C1 C2 C3 C4 -2.8(4) . . . . ?
C1 C2 C3 Br1 176.4(6) . . . . ?
C13 C18 C17 Cl6 177.4(5) . . . . ?
C13 C18 C17 C16 2.5(4) . . . . ?
C13 C18 C17 Br6 -175.7(4) . . . . ?
C3 C2 C1 O1 -177.0(2) . . . . ?
C3 C2 C1 C6 1.6(4) . . . . ?
C3 C4 C5 O4 179.7(2) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C9 C10 C11 Cl4 179.5(6) . . . . ?
C9 C10 C11 C12 4.8(4) . . . . ?
C9 C10 C11 Br4 -173.9(4) . . . . ?
C7 C12 C11 Cl4 -179.4(6) . . . . ?
C7 C12 C11 C10 -4.5(4) . . . . ?
C7 C12 C11 Br4 174.3(4) . . . . ?
C10 C9 C8 Cl3 -179.8(3) . . . . ?
C10 C9 C8 C7 -3.9(4) . . . . ?
C10 C9 C8 Br3 178.3(2) . . . . ?
C17 C16 C15 O10 -177.5(2) . . . . ?
C17 C16 C15 C14 2.5(4) . . . . ?
C17 C18 C13 O9 -179.9(2) . . . . ?
C17 C18 C13 C14 -0.5(4) . . . . ?
C12 C7 C8 Cl3 -179.9(3) . . . . ?
C12 C7 C8 C9 4.1(4) . . . . ?
C12 C7 C8 Br3 -178.0(2) . . . . ?
C8 C9 C10 O7 179.4(2) . . . . ?
C8 C9 C10 C11 -0.6(4) . . . . ?
C8 C7 C12 O8 179.7(2) . . . . ?
C8 C7 C12 C11 0.1(4) . . . . ?
C25 N1 C22 C23 55.8(3) . . . . ?
C25 N1 C19 C20 176.2(2) . . . . ?
C25 N1 C28 C29 -61.9(3) . . . . ?
C22 N1 C25 C26 55.9(3) . . . . ?
C22 N1 C19 C20 -62.6(3) . . . . ?
C22 N1 C28 C29 177.0(2) . . . . ?
C34 N2 C40 C41 54.9(3) . . . . ?
C34 N2 C31 C32 61.6(3) . . . . ?
C34 N2 C37 C38 -170.6(3) . . . . ?
C40 N2 C34 C35 50.9(4) . . . . ?
C40 N2 C31 C32 -178.0(3) . . . . ?
C40 N2 C37 C38 68.7(4) . . . . ?
C19 N1 C25 C26 176.6(3) . . . . ?
C19 N1 C22 C23 -62.5(3) . . . . ?
C19 N1 C28 C29 56.6(3) . . . . ?
C31 N2 C34 C35 170.0(3) . . . . ?
C31 N2 C40 C41 -63.6(3) . . . . ?
C31 N2 C37 C38 -51.3(4) . . . . ?
C28 N1 C25 C26 -62.1(3) . . . . ?
C28 N1 C22 C23 176.6(3) . . . . ?
C28 N1 C19 C20 55.3(3) . . . . ?
C42 C41 C40 N2 -172.7(3) . . . . ?
C37 N2 C34 C35 -68.3(3) . . . . ?
C37 N2 C40 C41 174.7(3) . . . . ?
C37 N2 C31 C32 -58.4(3) . . . . ?
C30 C29 C28 N1 170.3(2) . . . . ?
C21 C20 C19 N1 168.5(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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.103
_oxdiff_exptl_absorpt_empirical_full_min 0.914
####################################################################### 
# 
# 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_Br-065_CCDC-2014809_R1
_database_code_depnum_ccdc_archive 'CCDC 2014809'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-31
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br3.91 C18 Cl2.09 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Br3.91 Cl2.09 Fe2 N2 O15'
_chemical_formula_weight         1413.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl2.09 Br3.91 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.4745(6)
_cell_length_b                   21.8256(5)
_cell_length_c                   14.4440(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.895(3)
_cell_angle_gamma                90
_cell_volume                     6142.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15180
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.4120
_cell_measurement_theta_min      1.7390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.166
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2866
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.049
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42253
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.751
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0208726000
_diffrn_orient_matrix_UB_12      -0.0138444000
_diffrn_orient_matrix_UB_13      -0.0252733000
_diffrn_orient_matrix_UB_21      0.0298149000
_diffrn_orient_matrix_UB_22      0.0097778000
_diffrn_orient_matrix_UB_23      0.0369469000
_diffrn_orient_matrix_UB_31      0.0000915000
_diffrn_orient_matrix_UB_32      -0.0277331000
_diffrn_orient_matrix_UB_33      0.0256740000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8393
_reflns_number_total             11244
_reflns_odcompleteness_completeness 90.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.52
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11244
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.062
_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)+(0.0535P)²+14.1021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1273
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-Cl6
 1.73 with sigma of 0.02
 C11-Cl4
 1.73 with sigma of 0.015
 C8-Cl3
 1.73 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
4. Others
 Fixed Sof: Br6(0.6517) Br1(0.6317) Br4(0.6717) Br3(0.6717) Br5(0.6517)
 Br2(0.6317) Cl5(0.3483) Cl2(0.3683) Cl6(0.3483) Cl1(0.3683) Cl3(0.3283)
 Cl4(0.3283) O16(0.5) O15(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C31(H31A,H31B), C25(H25A,H25B), C22(H22A,H22B), C40(H40A,
 H40B), C38(H38A,H38B), C19(H19A,H19B), C23(H23A,H23B), C34(H34A,H34B),
 C20(H20A,H20B), C28(H28A,H28B), C32(H32A,H32B), C41(H41A,H41B), C29(H29A,H29B),
  C35(H35A,H35B), C26(H26A,H26B)
5.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C39(H39A,H39B,
 H39C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C27(H27A,H27B,H27C), C30(H30A,
 H30B,H30C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br6 Br 0.0792(2) 0.67260(14) 0.0310(4) 0.0257(6) Uani 0.6517 1 d . . P A -2
Fe2 Fe 0.22034(3) 0.68030(3) 0.39554(4) 0.01649(16) Uani 1 1 d . . . . .
Br1 Br 0.10145(10) 0.33094(9) 0.05298(18) 0.0211(4) Uani 0.6317 1 d . . P B -2
Br4 Br 0.08864(8) 0.48951(10) 0.4752(2) 0.0227(4) Uani 0.6717 1 d . . P C -2
Fe1 Fe 0.23946(3) 0.31646(3) 0.41203(4) 0.01723(16) Uani 1 1 d . . . . .
Br3 Br 0.38109(6) 0.50196(6) 0.36902(9) 0.0232(3) Uani 0.6717 1 d . . P D -2
Br5 Br 0.36436(9) 0.82161(8) 0.25167(13) 0.0309(3) Uani 0.6517 1 d . . P E -2
Br2 Br 0.38279(15) 0.17660(16) 0.2657(2) 0.0315(6) Uani 0.6317 1 d . . P F -2
O11 O 0.16573(14) 0.76165(13) -0.05048(19) 0.0184(6) Uani 1 1 d . . . . .
O12 O 0.16245(15) 0.67955(13) 0.2545(2) 0.0197(7) Uani 1 1 d . . . . .
O3 O 0.18662(14) 0.24356(13) -0.03517(19) 0.0177(6) Uani 1 1 d . . . . .
O7 O 0.16671(15) 0.60352(13) 0.4218(2) 0.0196(6) Uani 1 1 d . . . . .
O2 O 0.18251(15) 0.31893(13) 0.2726(2) 0.0192(6) Uani 1 1 d . . . . .
O1 O 0.29499(15) 0.26114(13) 0.3565(2) 0.0204(7) Uani 1 1 d . . . . .
O9 O 0.27550(15) 0.73630(13) 0.3397(2) 0.0204(7) Uani 1 1 d . . . . .
O10 O 0.28059(14) 0.81510(13) 0.0351(2) 0.0200(7) Uani 1 1 d . . . . .
O4 O 0.30036(15) 0.18651(13) 0.0498(2) 0.0202(7) Uani 1 1 d . . . . .
O8 O 0.18099(15) 0.38827(13) 0.4391(2) 0.0203(7) Uani 1 1 d . . . . .
O5 O 0.29669(14) 0.39269(13) 0.3980(2) 0.0197(7) Uani 1 1 d . . . . .
O6 O 0.28327(15) 0.60720(13) 0.3843(2) 0.0215(7) Uani 1 1 d . . . . .
N1 N 0.04755(19) 0.14769(17) 0.2286(3) 0.0262(9) Uani 1 1 d . . . . .
N2 N 0.50884(19) 0.30044(18) 0.5082(3) 0.0268(9) Uani 1 1 d . . . . .
C2 C 0.2084(2) 0.28921(19) 0.2146(3) 0.0171(9) Uani 1 1 d . . . . .
C16 C 0.1900(2) 0.75214(18) 0.0422(3) 0.0171(9) Uani 1 1 d . . . . .
C9 C 0.2631(2) 0.55447(19) 0.3984(3) 0.0192(9) Uani 1 1 d . . . . .
C10 C 0.1950(2) 0.5523(2) 0.4213(3) 0.0188(9) Uani 1 1 d . . . . .
C7 C 0.2704(2) 0.44372(19) 0.4056(3) 0.0180(9) Uani 1 1 d . . . . .
C5 C 0.2742(2) 0.21716(19) 0.1067(3) 0.0192(9) Uani 1 1 d . . . . .
C4 C 0.2100(2) 0.25045(18) 0.0583(3) 0.0167(9) Uani 1 1 d . . . . .
C18 C 0.1881(2) 0.71037(19) 0.1975(3) 0.0175(9) Uani 1 1 d . . . . .
C6 C 0.3033(2) 0.2204(2) 0.2073(3) 0.0225(10) Uani 1 1 d . . . . .
C17 C 0.1599(2) 0.71504(19) 0.0968(3) 0.0194(9) Uani 1 1 d D . . . .
C1 C 0.2727(2) 0.25573(19) 0.2633(3) 0.0180(9) Uani 1 1 d . . . . .
C15 C 0.2552(2) 0.7838(2) 0.0914(3) 0.0193(9) Uani 1 1 d . . . . .
C3 C 0.1803(2) 0.28608(19) 0.1136(3) 0.0179(9) Uani 1 1 d . . . . .
C13 C 0.2528(2) 0.74301(19) 0.2464(3) 0.0191(9) Uani 1 1 d . . . . .
C12 C 0.2021(2) 0.4413(2) 0.4299(3) 0.0193(9) Uani 1 1 d . . . . .
C11 C 0.1691(2) 0.49582(19) 0.4394(3) 0.0193(9) Uani 1 1 d D . . . .
C14 C 0.2841(2) 0.7782(2) 0.1912(3) 0.0219(10) Uani 1 1 d . . . . .
C8 C 0.2983(2) 0.5003(2) 0.3943(3) 0.0217(10) Uani 1 1 d D . . . .
C37 C 0.5308(2) 0.3394(2) 0.6001(3) 0.0294(11) Uani 1 1 d . . . . .
H37A H 0.5424 0.3116 0.6570 0.035 Uiso 1 1 calc R U . . .
H37B H 0.5733 0.3616 0.6015 0.035 Uiso 1 1 calc R U . . .
C31 C 0.5705(2) 0.2614(2) 0.5093(4) 0.0282(11) Uani 1 1 d . . . . .
H31A H 0.6085 0.2892 0.5085 0.034 Uiso 1 1 calc R U . . .
H31B H 0.5852 0.2387 0.5717 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1166(3) 0.1192(2) 0.2359(4) 0.0373(13) Uani 1 1 d . . . . .
H25A H 0.1085 0.0771 0.2094 0.045 Uiso 1 1 calc R U . . .
H25B H 0.1374 0.1428 0.1935 0.045 Uiso 1 1 calc R U . . .
C22 C 0.0586(3) 0.2159(2) 0.2516(4) 0.0316(11) Uani 1 1 d . . . . .
H22A H 0.0883 0.2201 0.3198 0.038 Uiso 1 1 calc R U . . .
H22B H 0.0840 0.2333 0.2095 0.038 Uiso 1 1 calc R U . . .
C40 C 0.4470(2) 0.2610(2) 0.5065(4) 0.0292(11) Uani 1 1 d . . . . .
H40A H 0.4093 0.2885 0.5097 0.035 Uiso 1 1 calc R U . . .
H40B H 0.4315 0.2394 0.4433 0.035 Uiso 1 1 calc R U . . .
C38 C 0.4791(3) 0.3856(2) 0.6118(4) 0.0342(12) Uani 1 1 d . . . . .
H38A H 0.4337 0.3658 0.5993 0.041 Uiso 1 1 calc R U . . .
H38B H 0.4745 0.4193 0.5644 0.041 Uiso 1 1 calc R U . . .
C19 C -0.0009(3) 0.1378(2) 0.1264(3) 0.0305(11) Uani 1 1 d . . . . .
H19A H -0.0014 0.0934 0.1120 0.037 Uiso 1 1 calc R U . . .
H19B H -0.0477 0.1490 0.1266 0.037 Uiso 1 1 calc R U . . .
C23 C -0.0052(3) 0.2541(2) 0.2391(4) 0.0316(11) Uani 1 1 d . . . . .
H23A H -0.0280 0.2416 0.2874 0.038 Uiso 1 1 calc R U . . .
H23B H -0.0378 0.2477 0.1732 0.038 Uiso 1 1 calc R U . . .
C24 C 0.0151(3) 0.3212(2) 0.2531(4) 0.0405(13) Uani 1 1 d . . . . .
H24A H 0.0396 0.3327 0.2072 0.061 Uiso 1 1 calc R U . . .
H24B H 0.0449 0.3277 0.3198 0.061 Uiso 1 1 calc R U . . .
H24C H -0.0263 0.3465 0.2414 0.061 Uiso 1 1 calc R U . . .
C34 C 0.4864(3) 0.3401(2) 0.4172(3) 0.0321(12) Uani 1 1 d . . . . .
H34A H 0.4737 0.3128 0.3596 0.038 Uiso 1 1 calc R U . . .
H34B H 0.4446 0.3628 0.4174 0.038 Uiso 1 1 calc R U . . .
C42 C 0.3950(3) 0.1727(2) 0.5656(5) 0.0448(14) Uani 1 1 d . . . . .
H42A H 0.3879 0.1518 0.5033 0.067 Uiso 1 1 calc R U . . .
H42B H 0.3545 0.1976 0.5627 0.067 Uiso 1 1 calc R U . . .
H42C H 0.4020 0.1422 0.6176 0.067 Uiso 1 1 calc R U . . .
C20 C 0.0132(3) 0.1712(2) 0.0448(4) 0.0376(13) Uani 1 1 d . . . . .
H20A H 0.0587 0.1592 0.0400 0.045 Uiso 1 1 calc R U . . .
H20B H 0.0136 0.2159 0.0565 0.045 Uiso 1 1 calc R U . . .
C28 C 0.0156(3) 0.1185(2) 0.2991(3) 0.0334(12) Uani 1 1 d . . . . .
H28A H -0.0290 0.1388 0.2916 0.040 Uiso 1 1 calc R U . . .
H28B H 0.0456 0.1269 0.3660 0.040 Uiso 1 1 calc R U . . .
C33 C 0.6225(3) 0.1738(2) 0.4483(5) 0.0472(15) Uani 1 1 d . . . . .
H33A H 0.6179 0.1469 0.3923 0.071 Uiso 1 1 calc R U . . .
H33B H 0.6254 0.1489 0.5058 0.071 Uiso 1 1 calc R U . . .
H33C H 0.6642 0.1986 0.4603 0.071 Uiso 1 1 calc R U . . .
C32 C 0.5608(3) 0.2155(3) 0.4275(4) 0.0436(14) Uani 1 1 d . . . . .
H32A H 0.5190 0.1908 0.4208 0.052 Uiso 1 1 calc R U . . .
H32B H 0.5548 0.2374 0.3654 0.052 Uiso 1 1 calc R U . . .
C41 C 0.4583(3) 0.2142(3) 0.5865(4) 0.0477(15) Uani 1 1 d . . . . .
H41A H 0.4661 0.2351 0.6498 0.057 Uiso 1 1 calc R U . . .
H41B H 0.4994 0.1893 0.5900 0.057 Uiso 1 1 calc R U . . .
C29 C 0.0036(3) 0.0499(2) 0.2886(4) 0.0407(13) Uani 1 1 d . . . . .
H29A H -0.0312 0.0412 0.2251 0.049 Uiso 1 1 calc R U . . .
H29B H 0.0468 0.0292 0.2893 0.049 Uiso 1 1 calc R U . . .
C35 C 0.5391(3) 0.3858(2) 0.4057(4) 0.0374(13) Uani 1 1 d . . . . .
H35A H 0.5837 0.3650 0.4156 0.045 Uiso 1 1 calc R U . . .
H35B H 0.5456 0.4185 0.4551 0.045 Uiso 1 1 calc R U . . .
C39 C 0.5030(3) 0.4111(3) 0.7150(4) 0.0467(15) Uani 1 1 d . . . . .
H39A H 0.4684 0.4394 0.7242 0.070 Uiso 1 1 calc R U . . .
H39B H 0.5465 0.4329 0.7255 0.070 Uiso 1 1 calc R U . . .
H39C H 0.5096 0.3773 0.7617 0.070 Uiso 1 1 calc R U . . .
C21 C -0.0432(3) 0.1550(3) -0.0500(4) 0.0452(15) Uani 1 1 d . . . . .
H21A H -0.0425 0.1847 -0.1006 0.068 Uiso 1 1 calc R U . . .
H21B H -0.0880 0.1563 -0.0388 0.068 Uiso 1 1 calc R U . . .
H21C H -0.0351 0.1138 -0.0709 0.068 Uiso 1 1 calc R U . . .
C26 C 0.1680(3) 0.1159(3) 0.3358(5) 0.0573(18) Uani 1 1 d . . . . .
H26A H 0.1741 0.1571 0.3658 0.069 Uiso 1 1 calc R U . . .
H26B H 0.1506 0.0882 0.3772 0.069 Uiso 1 1 calc R U . . .
C36 C 0.5141(3) 0.4137(3) 0.3034(4) 0.0526(17) Uani 1 1 d . . . . .
H36A H 0.5123 0.3818 0.2550 0.079 Uiso 1 1 calc R U . . .
H36B H 0.5459 0.4460 0.2977 0.079 Uiso 1 1 calc R U . . .
H36C H 0.4683 0.4312 0.2921 0.079 Uiso 1 1 calc R U . . .
O14 O 0.1338(3) -0.0353(3) 0.2784(6) 0.129(3) Uani 1 1 d . . . . .
C27 C 0.2357(3) 0.0927(3) 0.3311(6) 0.069(2) Uani 1 1 d . . . . .
H27A H 0.2506 0.1173 0.2845 0.103 Uiso 1 1 calc R U . . .
H27B H 0.2311 0.0498 0.3102 0.103 Uiso 1 1 calc R U . . .
H27C H 0.2699 0.0958 0.3956 0.103 Uiso 1 1 calc R U . . .
C46 C 0.1736(4) -0.0751(3) 0.2710(6) 0.068(2) Uani 1 1 d . . . . .
O13 O 0.3361(4) 0.5047(3) 0.0859(6) 0.134(3) Uani 1 1 d . . . . .
C30 C -0.0209(5) 0.0244(3) 0.3697(5) 0.085(3) Uani 1 1 d . . . . .
H30A H -0.0272 -0.0200 0.3616 0.127 Uiso 1 1 calc R U . . .
H30B H -0.0647 0.0435 0.3674 0.127 Uiso 1 1 calc R U . . .
H30C H 0.0133 0.0331 0.4325 0.127 Uiso 1 1 calc R U . . .
C48 C 0.2128(4) -0.0691(4) 0.1978(6) 0.083(2) Uani 1 1 d . . . . .
H48A H 0.2009 -0.1033 0.1518 0.124 Uiso 1 1 calc R U . . .
H48B H 0.2622 -0.0697 0.2320 0.124 Uiso 1 1 calc R U . . .
H48C H 0.2006 -0.0303 0.1625 0.124 Uiso 1 1 calc R U . . .
C43 C 0.2816(5) 0.5017(4) 0.1047(6) 0.080(2) Uani 1 1 d . . . . .
C45 C 0.2558(4) 0.4414(4) 0.1240(6) 0.087(3) Uani 1 1 d . . . . .
H45A H 0.2651 0.4108 0.0800 0.130 Uiso 1 1 calc R U . . .
H45B H 0.2062 0.4439 0.1133 0.130 Uiso 1 1 calc R U . . .
H45C H 0.2790 0.4294 0.1916 0.130 Uiso 1 1 calc R U . . .
C47 C 0.1858(5) -0.1298(4) 0.3354(7) 0.106(3) Uani 1 1 d . . . . .
H47A H 0.1577 -0.1269 0.3793 0.159 Uiso 1 1 calc R U . . .
H47B H 0.2344 -0.1317 0.3738 0.159 Uiso 1 1 calc R U . . .
H47C H 0.1733 -0.1669 0.2956 0.159 Uiso 1 1 calc R U . . .
C44 C 0.2428(5) 0.5567(4) 0.1166(8) 0.108(3) Uani 1 1 d . . . . .
H44A H 0.2706 0.5809 0.1718 0.162 Uiso 1 1 calc R U . . .
H44B H 0.2001 0.5441 0.1287 0.162 Uiso 1 1 calc R U . . .
H44C H 0.2318 0.5815 0.0572 0.162 Uiso 1 1 calc R U . . .
Cl5 Cl 0.3505(7) 0.8247(7) 0.2542(11) 0.110(6) Uani 0.3483 1 d . . P E 2
Cl2 Cl 0.3782(9) 0.1801(9) 0.2675(13) 0.072(6) Uani 0.3683 1 d . . P F 2
Cl6 Cl 0.0843(10) 0.6736(9) 0.043(2) 0.037(5) Uani 0.3483 1 d D . P A 2
Cl1 Cl 0.1051(7) 0.3308(7) 0.0581(11) 0.072(5) Uani 0.3683 1 d . . P B 2
Cl3 Cl 0.3773(7) 0.5046(7) 0.3651(13) 0.120(6) Uani 0.3283 1 d D . P D 2
Cl4 Cl 0.0917(7) 0.4925(8) 0.4705(14) 0.069(5) Uani 0.3283 1 d D . P C 2
O16 O 0.4418(15) 0.4971(9) -0.0696(15) 0.220(11) Uani 0.5 1 d . U P G 3
O15 O 0.4851(11) 0.5642(15) -0.020(2) 0.255(11) Uani 0.5 1 d . U P G -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
Br6 C17 1.877(6) . ?
Fe2 O11 2.000(3) 4_576 ?
Fe2 O12 2.017(3) . ?
Fe2 O7 2.101(3) . ?
Fe2 O9 1.995(3) . ?
Fe2 O10 2.017(3) 4_576 ?
Fe2 O6 2.088(3) . ?
Br1 C3 1.861(5) . ?
Br4 C11 1.877(5) . ?
Fe1 O3 1.994(3) 4_566 ?
Fe1 O2 1.993(3) . ?
Fe1 O1 1.988(3) . ?
Fe1 O4 1.999(3) 4_566 ?
Fe1 O8 2.081(3) . ?
Fe1 O5 2.080(3) . ?
Br3 C8 1.841(5) . ?
Br5 C14 1.865(4) . ?
Br2 C6 1.853(5) . ?
O11 Fe2 2.000(3) 4_575 ?
O11 C16 1.294(5) . ?
O12 C18 1.293(5) . ?
O3 Fe1 1.994(3) 4_565 ?
O3 C4 1.295(5) . ?
O7 C10 1.261(5) . ?
O2 C2 1.295(5) . ?
O1 C1 1.288(5) . ?
O9 C13 1.292(5) . ?
O10 Fe2 2.017(3) 4_575 ?
O10 C15 1.287(5) . ?
O4 Fe1 1.999(3) 4_565 ?
O4 C5 1.296(5) . ?
O8 C12 1.257(5) . ?
O5 C7 1.257(5) . ?
O6 C9 1.260(5) . ?
N1 C25 1.518(6) . ?
N1 C22 1.527(6) . ?
N1 C19 1.520(6) . ?
N1 C28 1.510(6) . ?
N2 C37 1.524(6) . ?
N2 C31 1.518(6) . ?
N2 C40 1.524(6) . ?
N2 C34 1.521(6) . ?
C2 C1 1.480(6) . ?
C2 C3 1.396(6) . ?
C16 C17 1.399(6) . ?
C16 C15 1.478(6) . ?
C9 C10 1.529(6) . ?
C9 C8 1.395(6) . ?
C10 C11 1.398(6) . ?
C7 C12 1.542(6) . ?
C7 C8 1.391(6) . ?
C5 C4 1.477(6) . ?
C5 C6 1.392(6) . ?
C4 C3 1.383(6) . ?
C18 C17 1.394(6) . ?
C18 C13 1.479(6) . ?
C6 C1 1.397(6) . ?
C6 Cl2 1.750(18) . ?
C17 Cl6 1.754(17) . ?
C15 C14 1.385(6) . ?
C3 Cl1 1.791(15) . ?
C13 C14 1.396(6) . ?
C12 C11 1.397(6) . ?
C11 Cl4 1.776(12) . ?
C14 Cl5 1.717(15) . ?
C8 Cl3 1.796(13) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.510(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.516(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.514(7) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.506(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.524(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.488(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.518(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.516(7) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 C41 1.534(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.537(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.518(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C32 1.510(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.515(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.534(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.496(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O14 C46 1.217(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C46 C48 1.517(10) . ?
C46 C47 1.487(10) . ?
O13 C43 1.229(10) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C43 C45 1.476(10) . ?
C43 C44 1.479(11) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O16 O15 1.75(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
O11 Fe2 O12 99.98(12) 4_576 . ?
O11 Fe2 O7 92.83(11) 4_576 . ?
O11 Fe2 O10 79.77(11) 4_576 4_576 ?
O11 Fe2 O6 161.22(11) 4_576 . ?
O12 Fe2 O7 89.90(11) . . ?
O12 Fe2 O6 95.76(12) . . ?
O9 Fe2 O11 102.90(12) . 4_576 ?
O9 Fe2 O12 80.02(11) . . ?
O9 Fe2 O7 162.53(12) . . ?
O9 Fe2 O10 97.19(12) . 4_576 ?
O9 Fe2 O6 89.83(12) . . ?
O10 Fe2 O12 177.08(12) 4_576 . ?
O10 Fe2 O7 93.02(12) 4_576 . ?
O10 Fe2 O6 85.03(11) 4_576 . ?
O6 Fe2 O7 76.93(11) . . ?
O3 Fe1 O4 81.01(11) 4_566 4_566 ?
O3 Fe1 O8 90.70(12) 4_566 . ?
O3 Fe1 O5 161.93(11) 4_566 . ?
O2 Fe1 O3 100.75(12) . 4_566 ?
O2 Fe1 O4 177.38(12) . 4_566 ?
O2 Fe1 O8 88.70(11) . . ?
O2 Fe1 O5 93.00(11) . . ?
O1 Fe1 O3 101.54(12) . 4_566 ?
O1 Fe1 O2 80.71(11) . . ?
O1 Fe1 O4 97.05(12) . 4_566 ?
O1 Fe1 O8 165.08(12) . . ?
O1 Fe1 O5 92.15(12) . . ?
O4 Fe1 O8 93.24(12) 4_566 . ?
O4 Fe1 O5 85.69(11) 4_566 . ?
O5 Fe1 O8 77.85(11) . . ?
C16 O11 Fe2 115.0(3) . 4_575 ?
C18 O12 Fe2 114.3(3) . . ?
C4 O3 Fe1 113.9(3) . 4_565 ?
C10 O7 Fe2 116.1(3) . . ?
C2 O2 Fe1 114.3(3) . . ?
C1 O1 Fe1 114.5(3) . . ?
C13 O9 Fe2 115.1(3) . . ?
C15 O10 Fe2 114.6(3) . 4_575 ?
C5 O4 Fe1 113.3(3) . 4_565 ?
C12 O8 Fe1 115.9(3) . . ?
C7 O5 Fe1 115.5(3) . . ?
C9 O6 Fe2 116.4(3) . . ?
C25 N1 C22 108.1(4) . . ?
C25 N1 C19 109.0(4) . . ?
C19 N1 C22 111.1(4) . . ?
C28 N1 C25 111.5(4) . . ?
C28 N1 C22 109.3(4) . . ?
C28 N1 C19 107.8(3) . . ?
C37 N2 C40 110.5(4) . . ?
C31 N2 C37 106.3(3) . . ?
C31 N2 C40 111.5(4) . . ?
C31 N2 C34 111.0(4) . . ?
C34 N2 C37 111.4(4) . . ?
C34 N2 C40 106.1(4) . . ?
O2 C2 C1 114.9(4) . . ?
O2 C2 C3 125.5(4) . . ?
C3 C2 C1 119.6(4) . . ?
O11 C16 C17 125.5(4) . . ?
O11 C16 C15 115.2(4) . . ?
C17 C16 C15 119.3(4) . . ?
O6 C9 C10 115.4(4) . . ?
O6 C9 C8 124.6(4) . . ?
C8 C9 C10 119.9(4) . . ?
O7 C10 C9 115.1(4) . . ?
O7 C10 C11 125.4(4) . . ?
C11 C10 C9 119.5(4) . . ?
O5 C7 C12 115.6(4) . . ?
O5 C7 C8 125.0(4) . . ?
C8 C7 C12 119.4(4) . . ?
O4 C5 C4 115.8(4) . . ?
O4 C5 C6 124.1(4) . . ?
C6 C5 C4 120.2(4) . . ?
O3 C4 C5 115.2(4) . . ?
O3 C4 C3 125.5(4) . . ?
C3 C4 C5 119.2(4) . . ?
O12 C18 C17 125.7(4) . . ?
O12 C18 C13 115.2(4) . . ?
C17 C18 C13 119.1(4) . . ?
C5 C6 Br2 118.9(3) . . ?
C5 C6 C1 120.5(4) . . ?
C5 C6 Cl2 121.5(7) . . ?
C1 C6 Br2 120.6(3) . . ?
C1 C6 Cl2 118.0(7) . . ?
Cl2 C6 Br2 2.6(7) . . ?
C16 C17 Br6 118.1(4) . . ?
C16 C17 Cl6 122.1(10) . . ?
C18 C17 Br6 120.7(4) . . ?
C18 C17 C16 121.2(4) . . ?
C18 C17 Cl6 116.8(10) . . ?
Cl6 C17 Br6 3.9(11) . . ?
O1 C1 C2 115.4(4) . . ?
O1 C1 C6 125.3(4) . . ?
C6 C1 C2 119.3(4) . . ?
O10 C15 C16 115.2(4) . . ?
O10 C15 C14 125.4(4) . . ?
C14 C15 C16 119.5(4) . . ?
C2 C3 Br1 119.1(3) . . ?
C2 C3 Cl1 117.6(6) . . ?
C4 C3 Br1 119.7(3) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 Cl1 121.2(6) . . ?
Cl1 C3 Br1 1.6(6) . . ?
O9 C13 C18 115.2(4) . . ?
O9 C13 C14 125.2(4) . . ?
C14 C13 C18 119.6(4) . . ?
O8 C12 C7 114.9(4) . . ?
O8 C12 C11 125.5(4) . . ?
C11 C12 C7 119.5(4) . . ?
C10 C11 Br4 122.2(3) . . ?
C10 C11 Cl4 120.2(6) . . ?
C12 C11 Br4 117.2(3) . . ?
C12 C11 C10 120.6(4) . . ?
C12 C11 Cl4 119.1(6) . . ?
Cl4 C11 Br4 2.3(7) . . ?
C15 C14 Br5 118.4(3) . . ?
C15 C14 C13 121.3(4) . . ?
C15 C14 Cl5 120.9(6) . . ?
C13 C14 Br5 120.3(3) . . ?
C13 C14 Cl5 116.8(6) . . ?
Cl5 C14 Br5 8.5(6) . . ?
C9 C8 Br3 120.7(3) . . ?
C9 C8 Cl3 118.6(6) . . ?
C7 C8 Br3 118.5(3) . . ?
C7 C8 C9 120.8(4) . . ?
C7 C8 Cl3 120.4(6) . . ?
Cl3 C8 Br3 2.8(6) . . ?
N2 C37 H37A 108.2 . . ?
N2 C37 H37B 108.2 . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 N2 116.2(4) . . ?
C38 C37 H37A 108.2 . . ?
C38 C37 H37B 108.2 . . ?
N2 C31 H31A 108.1 . . ?
N2 C31 H31B 108.1 . . ?
H31A C31 H31B 107.3 . . ?
C32 C31 N2 117.0(4) . . ?
C32 C31 H31A 108.1 . . ?
C32 C31 H31B 108.1 . . ?
N1 C25 H25A 108.1 . . ?
N1 C25 H25B 108.1 . . ?
H25A C25 H25B 107.3 . . ?
C26 C25 N1 116.7(4) . . ?
C26 C25 H25A 108.1 . . ?
C26 C25 H25B 108.1 . . ?
N1 C22 H22A 108.2 . . ?
N1 C22 H22B 108.2 . . ?
H22A C22 H22B 107.3 . . ?
C23 C22 N1 116.5(4) . . ?
C23 C22 H22A 108.2 . . ?
C23 C22 H22B 108.2 . . ?
N2 C40 H40A 108.3 . . ?
N2 C40 H40B 108.3 . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 N2 116.1(4) . . ?
C41 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
C37 C38 H38A 109.9 . . ?
C37 C38 H38B 109.9 . . ?
C37 C38 C39 109.1(4) . . ?
H38A C38 H38B 108.3 . . ?
C39 C38 H38A 109.9 . . ?
C39 C38 H38B 109.9 . . ?
N1 C19 H19A 107.8 . . ?
N1 C19 H19B 107.8 . . ?
H19A C19 H19B 107.1 . . ?
C20 C19 N1 118.1(4) . . ?
C20 C19 H19A 107.8 . . ?
C20 C19 H19B 107.8 . . ?
C22 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
C22 C23 C24 109.0(4) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C34 H34A 108.4 . . ?
N2 C34 H34B 108.4 . . ?
H34A C34 H34B 107.4 . . ?
C35 C34 N2 115.6(4) . . ?
C35 C34 H34A 108.4 . . ?
C35 C34 H34B 108.4 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
C19 C20 H20A 110.0 . . ?
C19 C20 H20B 110.0 . . ?
C19 C20 C21 108.5(4) . . ?
H20A C20 H20B 108.4 . . ?
C21 C20 H20A 110.0 . . ?
C21 C20 H20B 110.0 . . ?
N1 C28 H28A 108.3 . . ?
N1 C28 H28B 108.3 . . ?
N1 C28 C29 116.1(4) . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 H28A 108.3 . . ?
C29 C28 H28B 108.3 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C33 C32 C31 110.0(4) . . ?
C33 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C40 C41 C42 109.2(5) . . ?
C40 C41 H41A 109.8 . . ?
C40 C41 H41B 109.8 . . ?
C42 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
H41A C41 H41B 108.3 . . ?
C28 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 C28 111.5(5) . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C34 C35 H35A 109.8 . . ?
C34 C35 H35B 109.8 . . ?
C34 C35 C36 109.3(5) . . ?
H35A C35 H35B 108.3 . . ?
C36 C35 H35A 109.8 . . ?
C36 C35 H35B 109.8 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C27 C26 C25 111.0(6) . . ?
C27 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O14 C46 C48 120.7(7) . . ?
O14 C46 C47 120.4(8) . . ?
C47 C46 C48 118.8(6) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O13 C43 C45 119.4(9) . . ?
O13 C43 C44 122.6(8) . . ?
C45 C43 C44 117.8(8) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 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
Fe2 O11 C16 C17 177.9(3) 4_575 . . . ?
Fe2 O11 C16 C15 -2.3(4) 4_575 . . . ?
Fe2 O12 C18 C17 177.2(3) . . . . ?
Fe2 O12 C18 C13 -3.1(4) . . . . ?
Fe2 O7 C10 C9 -1.8(4) . . . . ?
Fe2 O7 C10 C11 178.4(3) . . . . ?
Fe2 O9 C13 C18 2.8(5) . . . . ?
Fe2 O9 C13 C14 -177.8(4) . . . . ?
Fe2 O10 C15 C16 5.6(5) 4_575 . . . ?
Fe2 O10 C15 C14 -174.4(4) 4_575 . . . ?
Fe2 O6 C9 C10 0.3(5) . . . . ?
Fe2 O6 C9 C8 -179.8(3) . . . . ?
Fe1 O3 C4 C5 5.1(4) 4_565 . . . ?
Fe1 O3 C4 C3 -175.5(3) 4_565 . . . ?
Fe1 O2 C2 C1 4.0(4) . . . . ?
Fe1 O2 C2 C3 -177.1(3) . . . . ?
Fe1 O1 C1 C2 -2.5(4) . . . . ?
Fe1 O1 C1 C6 178.9(4) . . . . ?
Fe1 O4 C5 C4 -7.7(5) 4_565 . . . ?
Fe1 O4 C5 C6 173.0(3) 4_565 . . . ?
Fe1 O8 C12 C7 -3.2(4) . . . . ?
Fe1 O8 C12 C11 176.4(3) . . . . ?
Fe1 O5 C7 C12 3.4(4) . . . . ?
Fe1 O5 C7 C8 -176.9(3) . . . . ?
Br2 C6 C1 O1 -0.3(6) . . . . ?
Br2 C6 C1 C2 -178.8(3) . . . . ?
O11 C16 C17 Br6 2.5(6) . . . . ?
O11 C16 C17 C18 -176.4(4) . . . . ?
O11 C16 C17 Cl6 2.2(11) . . . . ?
O11 C16 C15 O10 -2.3(6) . . . . ?
O11 C16 C15 C14 177.7(4) . . . . ?
O12 C18 C17 Br6 -2.1(6) . . . . ?
O12 C18 C17 C16 176.8(4) . . . . ?
O12 C18 C17 Cl6 -1.9(10) . . . . ?
O12 C18 C13 O9 0.3(5) . . . . ?
O12 C18 C13 C14 -179.2(4) . . . . ?
O3 C4 C3 Br1 -1.9(6) . . . . ?
O3 C4 C3 C2 178.2(4) . . . . ?
O3 C4 C3 Cl1 -2.8(8) . . . . ?
O7 C10 C11 Br4 -3.9(6) . . . . ?
O7 C10 C11 C12 175.2(4) . . . . ?
O7 C10 C11 Cl4 -2.5(10) . . . . ?
O2 C2 C1 O1 -1.0(5) . . . . ?
O2 C2 C1 C6 177.7(4) . . . . ?
O2 C2 C3 Br1 3.6(6) . . . . ?
O2 C2 C3 C4 -176.6(4) . . . . ?
O2 C2 C3 Cl1 4.4(8) . . . . ?
O9 C13 C14 Br5 -1.1(6) . . . . ?
O9 C13 C14 C15 -178.6(4) . . . . ?
O9 C13 C14 Cl5 -9.9(9) . . . . ?
O10 C15 C14 Br5 2.7(6) . . . . ?
O10 C15 C14 C13 -179.8(4) . . . . ?
O10 C15 C14 Cl5 12.0(9) . . . . ?
O4 C5 C4 O3 1.8(5) . . . . ?
O4 C5 C4 C3 -177.6(4) . . . . ?
O4 C5 C6 Br2 -2.1(6) . . . . ?
O4 C5 C6 C1 178.5(4) . . . . ?
O4 C5 C6 Cl2 -2.3(10) . . . . ?
O8 C12 C11 Br4 3.4(6) . . . . ?
O8 C12 C11 C10 -175.7(4) . . . . ?
O8 C12 C11 Cl4 2.0(10) . . . . ?
O5 C7 C12 O8 -0.1(5) . . . . ?
O5 C7 C12 C11 -179.8(4) . . . . ?
O5 C7 C8 Br3 -1.5(6) . . . . ?
O5 C7 C8 C9 176.2(4) . . . . ?
O5 C7 C8 Cl3 0.8(9) . . . . ?
O6 C9 C10 O7 1.0(5) . . . . ?
O6 C9 C10 C11 -179.1(4) . . . . ?
O6 C9 C8 Br3 1.2(6) . . . . ?
O6 C9 C8 C7 -176.4(4) . . . . ?
O6 C9 C8 Cl3 -1.0(9) . . . . ?
N1 C25 C26 C27 -174.3(5) . . . . ?
N1 C22 C23 C24 -173.2(4) . . . . ?
N1 C19 C20 C21 -178.7(4) . . . . ?
N1 C28 C29 C30 173.5(5) . . . . ?
N2 C37 C38 C39 168.8(4) . . . . ?
N2 C31 C32 C33 -170.8(4) . . . . ?
N2 C40 C41 C42 -171.8(4) . . . . ?
N2 C34 C35 C36 170.0(4) . . . . ?
C16 C15 C14 Br5 -177.3(3) . . . . ?
C16 C15 C14 C13 0.2(7) . . . . ?
C16 C15 C14 Cl5 -168.0(7) . . . . ?
C9 C10 C11 Br4 176.3(3) . . . . ?
C9 C10 C11 C12 -4.6(6) . . . . ?
C9 C10 C11 Cl4 177.7(8) . . . . ?
C10 C9 C8 Br3 -178.9(3) . . . . ?
C10 C9 C8 C7 3.5(6) . . . . ?
C10 C9 C8 Cl3 178.9(7) . . . . ?
C7 C12 C11 Br4 -177.0(3) . . . . ?
C7 C12 C11 C10 3.9(6) . . . . ?
C7 C12 C11 Cl4 -178.3(8) . . . . ?
C5 C4 C3 Br1 177.4(3) . . . . ?
C5 C4 C3 C2 -2.5(6) . . . . ?
C5 C4 C3 Cl1 176.5(6) . . . . ?
C5 C6 C1 O1 179.1(4) . . . . ?
C5 C6 C1 C2 0.6(7) . . . . ?
C4 C5 C6 Br2 178.6(3) . . . . ?
C4 C5 C6 C1 -0.8(7) . . . . ?
C4 C5 C6 Cl2 178.4(8) . . . . ?
C18 C13 C14 Br5 178.2(3) . . . . ?
C18 C13 C14 C15 0.7(7) . . . . ?
C18 C13 C14 Cl5 169.4(7) . . . . ?
C6 C5 C4 O3 -178.9(4) . . . . ?
C6 C5 C4 C3 1.8(6) . . . . ?
C17 C16 C15 O10 177.5(4) . . . . ?
C17 C16 C15 C14 -2.5(6) . . . . ?
C17 C18 C13 O9 -180.0(4) . . . . ?
C17 C18 C13 C14 0.6(6) . . . . ?
C1 C2 C3 Br1 -177.5(3) . . . . ?
C1 C2 C3 C4 2.3(6) . . . . ?
C1 C2 C3 Cl1 -176.7(6) . . . . ?
C15 C16 C17 Br6 -177.2(3) . . . . ?
C15 C16 C17 C18 3.9(6) . . . . ?
C15 C16 C17 Cl6 -177.6(9) . . . . ?
C3 C2 C1 O1 -180.0(4) . . . . ?
C3 C2 C1 C6 -1.4(6) . . . . ?
C13 C18 C17 Br6 178.2(3) . . . . ?
C13 C18 C17 C16 -2.9(6) . . . . ?
C13 C18 C17 Cl6 178.4(9) . . . . ?
C12 C7 C8 Br3 178.2(3) . . . . ?
C12 C7 C8 C9 -4.2(6) . . . . ?
C12 C7 C8 Cl3 -179.5(7) . . . . ?
C8 C9 C10 O7 -178.9(4) . . . . ?
C8 C9 C10 C11 0.9(6) . . . . ?
C8 C7 C12 O8 -179.8(4) . . . . ?
C8 C7 C12 C11 0.5(6) . . . . ?
C37 N2 C31 C32 176.8(4) . . . . ?
C37 N2 C40 C41 -63.3(5) . . . . ?
C37 N2 C34 C35 56.8(5) . . . . ?
C31 N2 C37 C38 176.0(4) . . . . ?
C31 N2 C40 C41 54.8(6) . . . . ?
C31 N2 C34 C35 -61.5(5) . . . . ?
C25 N1 C22 C23 174.4(4) . . . . ?
C25 N1 C19 C20 -68.8(5) . . . . ?
C25 N1 C28 C29 -58.3(6) . . . . ?
C22 N1 C25 C26 68.2(6) . . . . ?
C22 N1 C19 C20 50.2(6) . . . . ?
C22 N1 C28 C29 -177.8(4) . . . . ?
C40 N2 C37 C38 -62.9(5) . . . . ?
C40 N2 C31 C32 56.3(6) . . . . ?
C40 N2 C34 C35 177.1(4) . . . . ?
C19 N1 C25 C26 -170.9(5) . . . . ?
C19 N1 C22 C23 54.9(5) . . . . ?
C19 N1 C28 C29 61.3(5) . . . . ?
C34 N2 C37 C38 54.9(5) . . . . ?
C34 N2 C31 C32 -61.8(6) . . . . ?
C34 N2 C40 C41 175.8(4) . . . . ?
C28 N1 C25 C26 -52.0(6) . . . . ?
C28 N1 C22 C23 -64.0(5) . . . . ?
C28 N1 C19 C20 169.9(4) . . . . ?
Cl2 C6 C1 O1 -0.2(10) . . . . ?
Cl2 C6 C1 C2 -178.6(8) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.918
####################################################################### 
# 
# 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_Br-010-d_CCDC-2014805_R1
_database_code_depnum_ccdc_archive 'CCDC 2014805'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Br0.96 C36 Cl11.04 Fe4 O24), 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br0.48 Cl5.52 Fe2 N2 O12'
_chemical_formula_weight         1126.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl5.4 Br0.6 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.7693(7)
_cell_length_b                   20.6834(12)
_cell_length_c                   12.2409(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.308(6)
_cell_angle_gamma                90
_cell_volume                     2673.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4654
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.1930
_cell_measurement_theta_min      1.9590
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1161
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22556
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.113
_diffrn_reflns_theta_min         1.962
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0570106000
_diffrn_orient_matrix_UB_12      -0.0070019000
_diffrn_orient_matrix_UB_13      -0.0183653000
_diffrn_orient_matrix_UB_21      -0.0285033000
_diffrn_orient_matrix_UB_22      0.0098059000
_diffrn_orient_matrix_UB_23      -0.0546885000
_diffrn_orient_matrix_UB_31      0.0211468000
_diffrn_orient_matrix_UB_32      0.0321321000
_diffrn_orient_matrix_UB_33      0.0126884000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3951
_reflns_number_total             7609
_reflns_odcompleteness_completeness 88.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         7609
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.2150
_refine_ls_R_factor_gt           0.1294
_refine_ls_restrained_S_all      1.032
_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)+(0.0394P)²+49.4766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.3004
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C9 \\sim Cl3-C3 \\sim Cl1-C6
 with sigma of 0.02
 Br1-C6 \\sim Br2-C9 \\sim Br3-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim C9 \\sim Br2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Cl1 \\sim C6 \\sim Br1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Cl3 \\sim Br3 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
4. Rigid body (RIGU) restrains
 Cl2, C9, Br2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, C6, Br1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, C3, Br3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Br1)=Sof(Br2)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl1)=FVAR(1)
 Sof(Br3)=1-FVAR(2)
 Sof(Cl3)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C7(H7A,H7B), C14(H14A,H14B), C10(H10A,H10B), C13(H13A,H13B),
 C16(H16A,H16B), C11(H11A,H11B), C12(H12A,H12B)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C1A(H1AA,H1AB,
 H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.04276(12) 0.31076(6) 0.52616(11) 0.0334(4) Uani 1 1 d . . . . .
Cl2 Cl 0.0661(7) 0.3290(5) 0.9414(7) 0.0350(12) Uani 0.919(6) 1 d D U P A 1
Cl3 Cl -0.2993(6) 0.5191(5) 0.4807(5) 0.0380(12) Uani 0.923(8) 1 d D U P B 3
Cl1 Cl 0.3395(9) 0.1703(3) 0.6093(7) 0.0387(14) Uani 0.919(6) 1 d D U P A 1
O3 O 0.4221(5) 0.1877(3) 0.8601(5) 0.0351(14) Uani 1 1 d . . . . .
O4 O 0.3061(5) 0.2457(3) 0.9963(5) 0.0333(14) Uani 1 1 d . . . . .
O2 O 0.0957(5) 0.2466(3) 0.5570(5) 0.0329(14) Uani 1 1 d . . . . .
O6 O -0.0976(6) 0.6191(3) 0.4740(5) 0.0382(15) Uani 1 1 d . . . . .
O1 O -0.0131(5) 0.3129(3) 0.6925(5) 0.0344(14) Uani 1 1 d . . . . .
O5 O -0.1435(6) 0.3963(3) 0.5227(5) 0.0391(15) Uani 1 1 d . . . . .
N1 N 0.6094(7) 0.3606(4) 0.7539(6) 0.0365(17) Uani 1 1 d . . . . .
C4 C 0.3170(8) 0.2142(4) 0.8142(7) 0.0309(18) Uani 1 1 d . . . . .
C2 C 0.1517(8) 0.2461(4) 0.6604(7) 0.0314(18) Uani 1 1 d . . . . .
C8 C -0.0841(8) 0.4473(4) 0.5104(7) 0.0324(19) Uani 1 1 d . . . . .
C1 C 0.0892(8) 0.2842(4) 0.7373(7) 0.0305(18) Uani 1 1 d . . . . .
C3 C -0.1345(7) 0.5092(4) 0.4929(7) 0.0335(18) Uani 1 1 d D U . . .
C5 C 0.2530(8) 0.2508(4) 0.8939(7) 0.0320(19) Uani 1 1 d . . . . .
C6 C 0.2626(8) 0.2127(4) 0.7001(6) 0.0329(18) Uani 1 1 d D U . . .
C17 C 0.7145(10) 0.2489(5) 0.7489(8) 0.043(2) Uani 1 1 d . . . . .
H17A H 0.797316 0.262647 0.793226 0.052 Uiso 1 1 calc R . . . .
H17B H 0.716283 0.255909 0.669202 0.052 Uiso 1 1 calc R . . . .
C7 C 0.7311(9) 0.3909(5) 0.8155(8) 0.042(2) Uani 1 1 d . . . . .
H7A H 0.802633 0.371327 0.787271 0.051 Uiso 1 1 calc R . . . .
H7B H 0.741784 0.379479 0.895310 0.051 Uiso 1 1 calc R . . . .
C C -0.0591(8) 0.5624(5) 0.4854(7) 0.036(2) Uani 1 1 d . . . . .
C9 C 0.1430(8) 0.2854(4) 0.8506(7) 0.0331(18) Uani 1 1 d D U . . .
C14 C 0.5022(9) 0.3346(5) 0.5498(8) 0.043(2) Uani 1 1 d . . . . .
H14A H 0.417149 0.343907 0.565342 0.052 Uiso 1 1 calc R . . . .
H14B H 0.518042 0.287560 0.558595 0.052 Uiso 1 1 calc R . . . .
C10 C 0.7403(11) 0.4640(5) 0.8062(9) 0.053(3) Uani 1 1 d . . . . .
H10A H 0.736064 0.476312 0.727393 0.063 Uiso 1 1 calc R . . . .
H10B H 0.668247 0.484580 0.832097 0.063 Uiso 1 1 calc R . . . .
C13 C 0.6021(9) 0.3719(5) 0.6295(8) 0.039(2) Uani 1 1 d . . . . .
H13A H 0.587425 0.418545 0.614482 0.047 Uiso 1 1 calc R . . . .
H13B H 0.685711 0.361168 0.612142 0.047 Uiso 1 1 calc R . . . .
C16 C 0.6105(9) 0.2896(5) 0.7809(8) 0.042(2) Uani 1 1 d . . . . .
H16A H 0.528203 0.271107 0.743680 0.050 Uiso 1 1 calc R . . . .
H16B H 0.615793 0.285087 0.862170 0.050 Uiso 1 1 calc R . . . .
C18 C 0.6943(9) 0.1774(5) 0.7690(9) 0.045(2) Uani 1 1 d . . . . .
H18A H 0.612044 0.163886 0.725664 0.067 Uiso 1 1 calc GR . . . .
H18B H 0.696143 0.170189 0.848407 0.067 Uiso 1 1 calc GR . . . .
H18C H 0.761705 0.152196 0.745837 0.067 Uiso 1 1 calc GR . . . .
C11 C 0.4919(10) 0.3911(5) 0.7839(9) 0.047(2) Uani 1 1 d . . . . .
H11A H 0.484004 0.435696 0.754119 0.057 Uiso 1 1 calc R . . . .
H11B H 0.416978 0.366605 0.745399 0.057 Uiso 1 1 calc R . . . .
C15 C 0.5090(10) 0.3558(6) 0.4312(8) 0.051(3) Uani 1 1 d . . . . .
H15A H 0.456332 0.327030 0.377505 0.077 Uiso 1 1 calc GR . . . .
H15B H 0.596934 0.353537 0.421077 0.077 Uiso 1 1 calc GR . . . .
H15C H 0.478058 0.400253 0.419104 0.077 Uiso 1 1 calc GR . . . .
C12 C 0.4875(12) 0.3939(6) 0.9051(10) 0.059(3) Uani 1 1 d . . . . .
H12A H 0.563371 0.416849 0.945735 0.071 Uiso 1 1 calc R . . . .
H12B H 0.488371 0.349503 0.935310 0.071 Uiso 1 1 calc R . . . .
C19 C 0.8632(12) 0.4873(6) 0.8760(12) 0.077(4) Uani 1 1 d . . . . .
H19A H 0.934048 0.471964 0.843400 0.116 Uiso 1 1 calc GR . . . .
H19B H 0.871916 0.470353 0.951893 0.116 Uiso 1 1 calc GR . . . .
H19C H 0.863670 0.534638 0.878066 0.116 Uiso 1 1 calc GR . . . .
C1A C 0.3694(14) 0.4287(6) 0.9229(12) 0.077(4) Uani 1 1 d . . . . .
H1AA H 0.294320 0.404962 0.885428 0.115 Uiso 1 1 calc GR . . . .
H1AB H 0.367962 0.472488 0.892027 0.115 Uiso 1 1 calc GR . . . .
H1AC H 0.369432 0.431245 1.002888 0.115 Uiso 1 1 calc GR . . . .
Br1 Br 0.330(4) 0.1555(16) 0.615(4) 0.038(4) Uani 0.081(6) 1 d D U P A 2
Br2 Br 0.086(4) 0.337(3) 0.951(4) 0.037(4) Uani 0.081(6) 1 d D U P A 2
Br3 Br -0.297(3) 0.523(3) 0.506(3) 0.037(4) Uani 0.077(8) 1 d D U P B 4


_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 O3 1.993(6) 4_565 ?
Fe1 O4 1.978(6) 4_565 ?
Fe1 O2 1.976(6) . ?
Fe1 O6 2.095(7) 3_566 ?
Fe1 O1 1.999(6) . ?
Fe1 O5 2.071(7) . ?
Cl2 C9 1.760(10) . ?
Cl3 C3 1.763(10) . ?
Cl1 C6 1.747(10) . ?
O3 C4 1.284(10) . ?
O4 C5 1.277(10) . ?
O2 C2 1.291(9) . ?
O6 C 1.242(11) . ?
O1 C1 1.277(10) . ?
O5 C8 1.258(11) . ?
N1 C7 1.513(11) . ?
N1 C13 1.527(11) . ?
N1 C16 1.506(12) . ?
N1 C11 1.522(12) . ?
C4 C5 1.505(11) . ?
C4 C6 1.404(11) . ?
C2 C1 1.486(12) . ?
C2 C6 1.383(12) . ?
C8 C3 1.391(12) . ?
C8 C 1.545(12) 3_566 ?
C1 C9 1.394(11) . ?
C3 C 1.382(13) . ?
C3 Br3 1.81(3) . ?
C5 C9 1.396(12) . ?
C6 Br1 1.82(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C16 1.513(13) . ?
C17 C18 1.522(14) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C10 1.521(15) . ?
C9 Br2 1.82(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.514(13) . ?
C14 C15 1.532(14) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C19 1.507(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.494(14) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C1A 1.514(16) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 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
O3 Fe1 O6 88.9(2) 4_565 3_566 ?
O3 Fe1 O1 177.2(3) 4_565 . ?
O3 Fe1 O5 88.3(3) 4_565 . ?
O4 Fe1 O3 80.6(2) 4_565 4_565 ?
O4 Fe1 O6 167.4(3) 4_565 3_566 ?
O4 Fe1 O1 99.4(2) 4_565 . ?
O4 Fe1 O5 95.2(3) 4_565 . ?
O2 Fe1 O3 101.0(2) . 4_565 ?
O2 Fe1 O4 101.7(3) . 4_565 ?
O2 Fe1 O6 87.0(3) . 3_566 ?
O2 Fe1 O1 81.8(2) . . ?
O2 Fe1 O5 161.8(3) . . ?
O1 Fe1 O6 90.8(3) . 3_566 ?
O1 Fe1 O5 88.9(3) . . ?
O5 Fe1 O6 77.5(3) . 3_566 ?
C4 O3 Fe1 114.5(5) . 4_666 ?
C5 O4 Fe1 115.1(5) . 4_666 ?
C2 O2 Fe1 112.5(5) . . ?
C O6 Fe1 115.4(6) . 3_566 ?
C1 O1 Fe1 112.3(5) . . ?
C8 O5 Fe1 116.2(6) . . ?
C7 N1 C13 107.7(7) . . ?
C7 N1 C11 112.9(8) . . ?
C16 N1 C7 109.0(7) . . ?
C16 N1 C13 111.3(7) . . ?
C16 N1 C11 108.8(7) . . ?
C11 N1 C13 107.2(7) . . ?
O3 C4 C5 114.0(7) . . ?
O3 C4 C6 125.9(8) . . ?
C6 C4 C5 120.1(8) . . ?
O2 C2 C1 115.7(7) . . ?
O2 C2 C6 123.6(8) . . ?
C6 C2 C1 120.6(7) . . ?
O5 C8 C3 126.7(8) . . ?
O5 C8 C 114.5(8) . 3_566 ?
C3 C8 C 118.7(8) . 3_566 ?
O1 C1 C2 115.8(7) . . ?
O1 C1 C9 125.0(8) . . ?
C9 C1 C2 119.2(7) . . ?
C8 C3 Cl3 118.5(7) . . ?
C8 C3 Br3 119.0(19) . . ?
C C3 Cl3 119.7(8) . . ?
C C3 C8 121.8(7) . . ?
C C3 Br3 118.2(19) . . ?
O4 C5 C4 114.9(8) . . ?
O4 C5 C9 126.8(8) . . ?
C9 C5 C4 118.3(7) . . ?
C4 C6 Cl1 119.1(7) . . ?
C4 C6 Br1 116.5(17) . . ?
C2 C6 Cl1 120.8(7) . . ?
C2 C6 C4 120.1(7) . . ?
C2 C6 Br1 122.6(18) . . ?
H17A C17 H17B 108.0 . . ?
C16 C17 H17A 109.4 . . ?
C16 C17 H17B 109.4 . . ?
C16 C17 C18 111.2(8) . . ?
C18 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
N1 C7 H7A 108.3 . . ?
N1 C7 H7B 108.3 . . ?
N1 C7 C10 115.9(8) . . ?
H7A C7 H7B 107.4 . . ?
C10 C7 H7A 108.3 . . ?
C10 C7 H7B 108.3 . . ?
O6 C C8 115.7(8) . 3_566 ?
O6 C C3 124.9(8) . . ?
C3 C C8 119.4(8) . 3_566 ?
C1 C9 Cl2 118.8(7) . . ?
C1 C9 C5 121.6(7) . . ?
C1 C9 Br2 123.5(17) . . ?
C5 C9 Cl2 119.5(7) . . ?
C5 C9 Br2 114.7(17) . . ?
H14A C14 H14B 108.5 . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C13 C14 C15 107.8(8) . . ?
C15 C14 H14A 110.1 . . ?
C15 C14 H14B 110.1 . . ?
C7 C10 H10A 109.7 . . ?
C7 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C19 C10 C7 109.7(9) . . ?
C19 C10 H10A 109.7 . . ?
C19 C10 H10B 109.7 . . ?
N1 C13 H13A 108.0 . . ?
N1 C13 H13B 108.0 . . ?
C14 C13 N1 117.2(8) . . ?
C14 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
N1 C16 C17 117.4(8) . . ?
N1 C16 H16A 108.0 . . ?
N1 C16 H16B 108.0 . . ?
C17 C16 H16A 108.0 . . ?
C17 C16 H16B 108.0 . . ?
H16A C16 H16B 107.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C11 H11A 108.2 . . ?
N1 C11 H11B 108.2 . . ?
H11A C11 H11B 107.3 . . ?
C12 C11 N1 116.5(9) . . ?
C12 C11 H11A 108.2 . . ?
C12 C11 H11B 108.2 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 C1A 110.7(11) . . ?
H12A C12 H12B 108.1 . . ?
C1A C12 H12A 109.5 . . ?
C1A C12 H12B 109.5 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C1A H1AA 109.5 . . ?
C12 C1A H1AB 109.5 . . ?
C12 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 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 O3 C4 C5 9.9(9) 4_666 . . . ?
Fe1 O3 C4 C6 -171.8(7) 4_666 . . . ?
Fe1 O4 C5 C4 -1.4(9) 4_666 . . . ?
Fe1 O4 C5 C9 177.5(7) 4_666 . . . ?
Fe1 O2 C2 C1 9.9(9) . . . . ?
Fe1 O2 C2 C6 -170.1(7) . . . . ?
Fe1 O6 C C8 -4.0(9) 3_566 . . 3_566 ?
Fe1 O6 C C3 176.9(7) 3_566 . . . ?
Fe1 O1 C1 C2 -10.2(9) . . . . ?
Fe1 O1 C1 C9 170.8(7) . . . . ?
Fe1 O5 C8 C3 172.1(7) . . . . ?
Fe1 O5 C8 C -7.2(9) . . . 3_566 ?
Cl3 C3 C O6 2.5(13) . . . . ?
Cl3 C3 C C8 -176.6(6) . . . 3_566 ?
O3 C4 C5 O4 -5.8(11) . . . . ?
O3 C4 C5 C9 175.2(8) . . . . ?
O3 C4 C6 Cl1 1.4(13) . . . . ?
O3 C4 C6 C2 -176.7(8) . . . . ?
O3 C4 C6 Br1 12.9(19) . . . . ?
O4 C5 C9 Cl2 1.3(14) . . . . ?
O4 C5 C9 C1 -175.8(8) . . . . ?
O4 C5 C9 Br2 9(2) . . . . ?
O2 C2 C1 O1 0.3(11) . . . . ?
O2 C2 C1 C9 179.3(8) . . . . ?
O2 C2 C6 Cl1 2.4(13) . . . . ?
O2 C2 C6 C4 -179.5(8) . . . . ?
O2 C2 C6 Br1 -9.8(19) . . . . ?
O1 C1 C9 Cl2 0.5(13) . . . . ?
O1 C1 C9 C5 177.7(8) . . . . ?
O1 C1 C9 Br2 -8(2) . . . . ?
O5 C8 C3 Cl3 -2.6(13) . . . . ?
O5 C8 C3 C 177.0(9) . . . . ?
O5 C8 C3 Br3 8.9(17) . . . . ?
N1 C7 C10 C19 177.2(10) . . . . ?
N1 C11 C12 C1A 176.7(10) . . . . ?
C4 C5 C9 Cl2 -179.8(7) . . . . ?
C4 C5 C9 C1 3.0(13) . . . . ?
C4 C5 C9 Br2 -172(2) . . . . ?
C2 C1 C9 Cl2 -178.4(7) . . . . ?
C2 C1 C9 C5 -1.2(13) . . . . ?
C2 C1 C9 Br2 173(2) . . . . ?
C8 C3 C O6 -177.2(8) . . . . ?
C8 C3 C C8 3.7(14) . . . 3_566 ?
C1 C2 C6 Cl1 -177.6(7) . . . . ?
C1 C2 C6 C4 0.4(13) . . . . ?
C1 C2 C6 Br1 170.2(16) . . . . ?
C5 C4 C6 Cl1 179.6(7) . . . . ?
C5 C4 C6 C2 1.4(13) . . . . ?
C5 C4 C6 Br1 -168.9(15) . . . . ?
C6 C4 C5 O4 175.8(8) . . . . ?
C6 C4 C5 C9 -3.2(13) . . . . ?
C6 C2 C1 O1 -179.7(8) . . . . ?
C6 C2 C1 C9 -0.6(13) . . . . ?
C7 N1 C13 C14 168.1(8) . . . . ?
C7 N1 C16 C17 -61.2(11) . . . . ?
C7 N1 C11 C12 -53.5(12) . . . . ?
C C8 C3 Cl3 176.6(6) 3_566 . . . ?
C C8 C3 C -3.7(14) 3_566 . . . ?
C C8 C3 Br3 -171.8(13) 3_566 . . . ?
C13 N1 C7 C10 64.7(11) . . . . ?
C13 N1 C16 C17 57.5(11) . . . . ?
C13 N1 C11 C12 -171.9(9) . . . . ?
C16 N1 C7 C10 -174.4(8) . . . . ?
C16 N1 C13 C14 48.6(11) . . . . ?
C16 N1 C11 C12 67.7(11) . . . . ?
C18 C17 C16 N1 -173.4(8) . . . . ?
C11 N1 C7 C10 -53.4(11) . . . . ?
C11 N1 C13 C14 -70.2(10) . . . . ?
C11 N1 C16 C17 175.3(8) . . . . ?
C15 C14 C13 N1 177.6(8) . . . . ?
Br3 C3 C O6 -9.0(17) . . . . ?
Br3 C3 C C8 171.9(13) . . . 3_566 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.703
####################################################################### 
# 
# 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_Br-010-CCDC-2014810_R1
_database_code_depnum_ccdc_archive 'CCDC 2014810'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-31
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br0.6 C18 Cl5.4 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Br0.60 Cl5.40 Fe2 N2 O15'
_chemical_formula_weight         1266.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl5.40 Br0.60 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.2076(7)
_cell_length_b                   21.8087(7)
_cell_length_c                   14.3967(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.080(4)
_cell_angle_gamma                90
_cell_volume                     6031.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15682
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.4930
_cell_measurement_theta_min      1.7470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2627
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.027
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.388
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0215527000
_diffrn_orient_matrix_UB_12      -0.0191622000
_diffrn_orient_matrix_UB_13      0.0181457000
_diffrn_orient_matrix_UB_21      0.0298298000
_diffrn_orient_matrix_UB_22      -0.0114946000
_diffrn_orient_matrix_UB_23      0.0362312000
_diffrn_orient_matrix_UB_31      -0.0029846000
_diffrn_orient_matrix_UB_32      0.0236382000
_diffrn_orient_matrix_UB_33      0.0322971000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8584
_reflns_number_total             13837
_reflns_odcompleteness_completeness 91.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.40
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         13837
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      1.019
_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)+(0.0602P)²+2.8263P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1399
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-Br2
 1.88 with sigma of 0.02
 C3-Br1
 1.88 with sigma of 0.02
 C11-Br4
 1.88 with sigma of 0.02
 C8-Br3
 1.88 with sigma of 0.02
 C17-Br6
 1.88 with sigma of 0.02
 C14-Br5
 1.88 with sigma of 0.02
3. Rigid bond restraints
 Cl1, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl5, Cl1, Cl3, Cl6, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Br1 \\sim Cl1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Cl5 \\sim Cl1 \\sim Cl3 \\sim Cl6 \\sim Cl4: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(O15) \\sim Ueq: with sigma of 0.08 and sigma for terminal atoms of 0.08
Uanis(O16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl2) = Uanis(Br2)
5. Others
 Fixed Sof: Cl5(0.902) Cl2(0.9) Cl4(0.898) Cl3(0.898) Cl1(0.9) Cl6(0.902)
 Br4(0.102) Br6(0.098) Br1(0.1) Br5(0.098) Br3(0.102) O15(0.5) O16(0.5) Br2(0.1)
6.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C40(H40A,H40B), C19(H19A,H19B), C31(H31A,H31B), C34(H34A,
 H34B), C22(H22A,H22B), C38(H38A,H38B), C20(H20A,H20B), C23(H23A,H23B),
 C25(H25A,H25B), C28(H28A,H28B), C29(H29A,H29B), C37(H37A,H37B), C26(H26A,H26B),
  C32(H32A,H32B), C41(H41A,H41B)
6.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C21(H21A,H21B,
 H21C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C27(H27A,H27B,H27C), C24(H24A,
 H24B,H24C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.72119(2) 0.31962(2) 0.39480(3) 0.01390(12) Uani 1 1 d . . . . .
Fe2 Fe 0.74004(2) 0.68282(2) 0.40914(3) 0.01453(12) Uani 1 1 d . . . . .
Cl5 Cl 0.60382(16) 0.82597(16) 0.5521(3) 0.0169(6) Uani 0.902 1 d . . P A 2
Cl2 Cl 0.5805(3) 0.18018(19) 0.5354(4) 0.0215(6) Uani 0.9 1 d . . P B 2
Cl4 Cl 0.87981(13) 0.49746(11) 0.37004(18) 0.0185(5) Uani 0.898 1 d . . P C 2
Cl3 Cl 0.5924(3) 0.5092(4) 0.4660(7) 0.0227(10) Uani 0.898 1 d . . P D 2
Cl1 Cl 0.8635(2) 0.3151(4) 0.7480(5) 0.0259(7) Uani 0.9 1 d . U P E 2
Cl6 Cl 0.8814(3) 0.6828(4) 0.7618(5) 0.0263(8) Uani 0.902 1 d . . P F 2
O6 O 0.68099(11) 0.61116(9) 0.43578(15) 0.0162(5) Uani 1 1 d . . . . .
O3 O 0.77720(11) 0.23592(9) 0.83918(15) 0.0158(5) Uani 1 1 d . . . . .
O1 O 0.66517(11) 0.26250(9) 0.44828(15) 0.0158(5) Uani 1 1 d . . . . .
O5 O 0.66746(11) 0.39604(10) 0.42089(15) 0.0180(5) Uani 1 1 d . . . . .
O9 O 0.68620(11) 0.74230(9) 0.46154(14) 0.0158(5) Uani 1 1 d . . . . .
O11 O 0.79620(11) 0.76168(10) 0.85421(14) 0.0163(5) Uani 1 1 d . . . . .
O8 O 0.78539(11) 0.39243(9) 0.38321(15) 0.0169(5) Uani 1 1 d . . . . .
O12 O 0.80147(11) 0.68602(10) 0.54765(15) 0.0165(5) Uani 1 1 d . . . . .
O7 O 0.79850(11) 0.60680(10) 0.39596(15) 0.0166(5) Uani 1 1 d . . . . .
O2 O 0.78251(11) 0.31478(10) 0.53394(15) 0.0173(5) Uani 1 1 d . . . . .
O10 O 0.68274(11) 0.81971(9) 0.76890(15) 0.0158(5) Uani 1 1 d . . . . .
O4 O 0.66217(11) 0.18023(9) 0.75422(15) 0.0165(5) Uani 1 1 d . . . . .
N1 N 0.45253(14) 0.35187(13) 0.2717(2) 0.0213(6) Uani 1 1 d . . . . .
N2 N 1.00879(14) 0.79928(13) 1.00796(19) 0.0203(6) Uani 1 1 d . . . . .
C10 C 0.77234(16) 0.55568(15) 0.4043(2) 0.0160(7) Uani 1 1 d . . . . .
C7 C 0.69554(16) 0.44756(14) 0.4198(2) 0.0152(7) Uani 1 1 d . . . . .
C12 C 0.76534(16) 0.44532(14) 0.3971(2) 0.0146(7) Uani 1 1 d . . . . .
C18 C 0.77549(15) 0.71663(14) 0.6046(2) 0.0141(7) Uani 1 1 d . . . . .
C9 C 0.70271(16) 0.55821(15) 0.4271(2) 0.0158(7) Uani 1 1 d . . . . .
C14 C 0.67993(15) 0.78562(14) 0.6107(2) 0.0154(7) Uani 1 1 d D . . . .
C15 C 0.70852(16) 0.78924(14) 0.7116(2) 0.0148(7) Uani 1 1 d . . . . .
C16 C 0.77330(16) 0.75581(14) 0.7603(2) 0.0143(7) Uani 1 1 d . . . . .
C1 C 0.68966(16) 0.25281(14) 0.5414(2) 0.0151(7) Uani 1 1 d . . . . .
C5 C 0.68802(16) 0.21102(14) 0.6967(2) 0.0144(7) Uani 1 1 d . . . . .
C13 C 0.70997(16) 0.74936(14) 0.5557(2) 0.0154(7) Uani 1 1 d . . . . .
C2 C 0.75629(16) 0.28353(14) 0.5906(2) 0.0145(7) Uani 1 1 d . . . . .
C4 C 0.75405(16) 0.24251(14) 0.7455(2) 0.0159(7) Uani 1 1 d . . . . .
C8 C 0.66968(16) 0.50393(14) 0.4372(2) 0.0169(7) Uani 1 1 d D . . . .
C11 C 0.80014(16) 0.49906(14) 0.3931(2) 0.0171(7) Uani 1 1 d D . . . .
C6 C 0.65882(16) 0.21636(14) 0.5956(2) 0.0156(7) Uani 1 1 d D . . . .
C17 C 0.80475(16) 0.72090(15) 0.7054(2) 0.0179(7) Uani 1 1 d D . . . .
C35 C 0.97871(19) 0.88482(16) 1.1107(2) 0.0263(8) Uani 1 1 d . . . . .
H35A H 0.9325 0.8652 1.0973 0.032 Uiso 1 1 calc R U . . .
H35B H 0.9745 0.9183 1.0627 0.032 Uiso 1 1 calc R U . . .
C3 C 0.78564(16) 0.27744(15) 0.6913(2) 0.0179(7) Uani 1 1 d D . . . .
C40 C 1.07135(16) 0.76026(16) 1.0098(2) 0.0220(8) Uani 1 1 d . . . . .
H40A H 1.1098 0.7880 1.0082 0.026 Uiso 1 1 calc R U . . .
H40B H 1.0866 0.7379 1.0728 0.026 Uiso 1 1 calc R U . . .
C19 C 0.50132(18) 0.36300(16) 0.3736(2) 0.0228(8) Uani 1 1 d . . . . .
H19A H 0.5487 0.3507 0.3747 0.027 Uiso 1 1 calc R U . . .
H19B H 0.5025 0.4077 0.3863 0.027 Uiso 1 1 calc R U . . .
C31 C 0.94638(17) 0.76016(16) 1.0051(2) 0.0240(8) Uani 1 1 d . . . . .
H31A H 0.9312 0.7383 0.9417 0.029 Uiso 1 1 calc R U . . .
H31B H 0.9079 0.7876 1.0073 0.029 Uiso 1 1 calc R U . . .
C34 C 1.03104(18) 0.83817(16) 1.0998(2) 0.0229(8) Uani 1 1 d . . . . .
H34A H 1.0424 0.8104 1.1570 0.027 Uiso 1 1 calc R U . . .
H34B H 1.0743 0.8601 1.1016 0.027 Uiso 1 1 calc R U . . .
C22 C 0.48538(19) 0.37942(16) 0.2004(2) 0.0267(8) Uani 1 1 d . . . . .
H22A H 0.5305 0.3587 0.2091 0.032 Uiso 1 1 calc R U . . .
H22B H 0.4551 0.3704 0.1333 0.032 Uiso 1 1 calc R U . . .
C38 C 1.0397(2) 0.88477(16) 0.9064(3) 0.0295(9) Uani 1 1 d . . . . .
H38A H 1.0850 0.8641 0.9166 0.035 Uiso 1 1 calc R U . . .
H38B H 1.0461 0.9173 0.9565 0.035 Uiso 1 1 calc R U . . .
O13 O 0.3664(2) 0.53513(16) 0.2257(3) 0.0891(14) Uani 1 1 d . . . . .
C20 C 0.4851(2) 0.33087(17) 0.4567(3) 0.0278(8) Uani 1 1 d . . . . .
H20A H 0.4844 0.2859 0.4469 0.033 Uiso 1 1 calc R U . . .
H20B H 0.4389 0.3438 0.4599 0.033 Uiso 1 1 calc R U . . .
C23 C 0.4979(2) 0.44767(16) 0.2091(3) 0.0313(9) Uani 1 1 d . . . . .
H23A H 0.5322 0.4571 0.2734 0.038 Uiso 1 1 calc R U . . .
H23B H 0.4539 0.4690 0.2052 0.038 Uiso 1 1 calc R U . . .
C25 C 0.38253(17) 0.38101(16) 0.2631(3) 0.0270(8) Uani 1 1 d . . . . .
H25A H 0.3607 0.3578 0.3050 0.032 Uiso 1 1 calc R U . . .
H25B H 0.3907 0.4233 0.2891 0.032 Uiso 1 1 calc R U . . .
C28 C 0.44118(18) 0.28355(15) 0.2504(3) 0.0241(8) Uani 1 1 d . . . . .
H28A H 0.4154 0.2668 0.2930 0.029 Uiso 1 1 calc R U . . .
H28B H 0.4110 0.2787 0.1820 0.029 Uiso 1 1 calc R U . . .
C29 C 0.50597(17) 0.24498(15) 0.2643(3) 0.0243(8) Uani 1 1 d . . . . .
H29A H 0.5394 0.2525 0.3300 0.029 Uiso 1 1 calc R U . . .
H29B H 0.5286 0.2563 0.2149 0.029 Uiso 1 1 calc R U . . .
C37 C 0.98665(18) 0.83899(16) 0.9169(2) 0.0242(8) Uani 1 1 d . . . . .
H37A H 0.9743 0.8118 0.8590 0.029 Uiso 1 1 calc R U . . .
H37B H 0.9440 0.8616 0.9163 0.029 Uiso 1 1 calc R U . . .
C30 C 0.48585(19) 0.17768(16) 0.2538(3) 0.0300(9) Uani 1 1 d . . . . .
H30A H 0.4530 0.1704 0.1886 0.045 Uiso 1 1 calc R U . . .
H30B H 0.4640 0.1666 0.3034 0.045 Uiso 1 1 calc R U . . .
H30C H 0.5276 0.1526 0.2625 0.045 Uiso 1 1 calc R U . . .
C39 C 1.0152(2) 0.91333(18) 0.8045(3) 0.0380(10) Uani 1 1 d . . . . .
H39A H 1.0100 0.8812 0.7552 0.057 Uiso 1 1 calc R U . . .
H39B H 1.0495 0.9435 0.7983 0.057 Uiso 1 1 calc R U . . .
H39C H 0.9702 0.9336 0.7947 0.057 Uiso 1 1 calc R U . . .
C36 C 1.0018(2) 0.91102(18) 1.2137(3) 0.0366(10) Uani 1 1 d . . . . .
H36A H 0.9692 0.9431 1.2190 0.055 Uiso 1 1 calc R U . . .
H36B H 1.0485 0.9285 1.2279 0.055 Uiso 1 1 calc R U . . .
H36C H 1.0025 0.8783 1.2607 0.055 Uiso 1 1 calc R U . . .
C21 C 0.5416(2) 0.34806(18) 0.5512(3) 0.0341(9) Uani 1 1 d . . . . .
H21A H 0.5874 0.3449 0.5414 0.051 Uiso 1 1 calc R U . . .
H21B H 0.5396 0.3201 0.6035 0.051 Uiso 1 1 calc R U . . .
H21C H 0.5342 0.3902 0.5692 0.051 Uiso 1 1 calc R U . . .
C42 C 1.12374(19) 0.67185(17) 0.9509(3) 0.0378(10) Uani 1 1 d . . . . .
H42A H 1.1179 0.6433 0.8964 0.057 Uiso 1 1 calc R U . . .
H42B H 1.1278 0.6487 1.0108 0.057 Uiso 1 1 calc R U . . .
H42C H 1.1659 0.6963 0.9598 0.057 Uiso 1 1 calc R U . . .
C26 C 0.3318(2) 0.38353(19) 0.1605(3) 0.0391(10) Uani 1 1 d . . . . .
H26A H 0.3263 0.3421 0.1308 0.047 Uiso 1 1 calc R U . . .
H26B H 0.3498 0.4113 0.1196 0.047 Uiso 1 1 calc R U . . .
C32 C 0.9576(2) 0.71337(18) 1.0862(3) 0.0364(10) Uani 1 1 d . . . . .
H32A H 0.9643 0.7345 1.1494 0.044 Uiso 1 1 calc R U . . .
H32B H 0.9998 0.6888 1.0913 0.044 Uiso 1 1 calc R U . . .
C41 C 1.0606(2) 0.71437(18) 0.9288(3) 0.0359(10) Uani 1 1 d . . . . .
H41A H 1.0545 0.7359 0.8661 0.043 Uiso 1 1 calc R U . . .
H41B H 1.0181 0.6901 0.9225 0.043 Uiso 1 1 calc R U . . .
C33 C 0.89396(19) 0.67134(17) 1.0635(3) 0.0373(10) Uani 1 1 d . . . . .
H33A H 0.8893 0.6488 1.0030 0.056 Uiso 1 1 calc R U . . .
H33B H 0.8521 0.6961 1.0558 0.056 Uiso 1 1 calc R U . . .
H33C H 0.8997 0.6422 1.1174 0.056 Uiso 1 1 calc R U . . .
C27 C 0.2614(2) 0.40678(19) 0.1647(3) 0.0452(11) Uani 1 1 d . . . . .
H27A H 0.2293 0.4107 0.0981 0.068 Uiso 1 1 calc R U . . .
H27B H 0.2675 0.4469 0.1970 0.068 Uiso 1 1 calc R U . . .
H27C H 0.2423 0.3777 0.2015 0.068 Uiso 1 1 calc R U . . .
O14 O 0.8329(3) 1.0042(2) 0.5828(5) 0.134(2) Uani 1 1 d . . . . .
C43 C 0.3256(2) 0.5741(2) 0.2307(4) 0.0491(12) Uani 1 1 d . . . . .
C46 C 0.7792(3) 1.0015(3) 0.6044(4) 0.0659(16) Uani 1 1 d . . . . .
C24 C 0.5249(3) 0.4704(2) 0.1285(4) 0.0673(17) Uani 1 1 d . . . . .
H24A H 0.4908 0.4613 0.0650 0.101 Uiso 1 1 calc R U . . .
H24B H 0.5690 0.4499 0.1333 0.101 Uiso 1 1 calc R U . . .
H24C H 0.5325 0.5148 0.1350 0.101 Uiso 1 1 calc R U . . .
C44 C 0.2853(3) 0.5687(2) 0.3026(3) 0.0596(14) Uani 1 1 d . . . . .
H44A H 0.2978 0.6028 0.3492 0.089 Uiso 1 1 calc R U . . .
H44B H 0.2968 0.5298 0.3379 0.089 Uiso 1 1 calc R U . . .
H44C H 0.2353 0.5701 0.2675 0.089 Uiso 1 1 calc R U . . .
C47 C 0.7526(3) 0.9421(2) 0.6266(4) 0.0715(16) Uani 1 1 d . . . . .
H47A H 0.7683 0.9093 0.5919 0.107 Uiso 1 1 calc R U . . .
H47B H 0.7016 0.9430 0.6056 0.107 Uiso 1 1 calc R U . . .
H47C H 0.7703 0.9345 0.6972 0.107 Uiso 1 1 calc R U . . .
C45 C 0.3138(3) 0.6292(2) 0.1663(4) 0.0765(18) Uani 1 1 d . . . . .
H45A H 0.2637 0.6360 0.1371 0.115 Uiso 1 1 calc R U . . .
H45B H 0.3350 0.6226 0.1144 0.115 Uiso 1 1 calc R U . . .
H45C H 0.3350 0.6651 0.2051 0.115 Uiso 1 1 calc R U . . .
C48 C 0.7413(3) 1.0582(3) 0.6167(5) 0.0856(19) Uani 1 1 d . . . . .
H48A H 0.7464 1.0640 0.6861 0.128 Uiso 1 1 calc R U . . .
H48B H 0.6919 1.0541 0.5796 0.128 Uiso 1 1 calc R U . . .
H48C H 0.7609 1.0936 0.5925 0.128 Uiso 1 1 calc R U . . .
Br4 Br 0.8826(7) 0.4952(7) 0.3677(13) 0.067(4) Uani 0.102 1 d D . P C -2
Br6 Br 0.8821(13) 0.6723(17) 0.764(2) 0.032(5) Uani 0.098 1 d D . P F -2
Br1 Br 0.8632(10) 0.3244(14) 0.753(2) 0.039(5) Uani 0.1 1 d D U P E -2
Br5 Br 0.6007(8) 0.8314(8) 0.5509(14) 0.044(4) Uani 0.098 1 d D . P A -2
Br3 Br 0.5920(12) 0.5068(14) 0.481(2) 0.020(3) Uani 0.102 1 d D . P D -2
O15 O 0.9882(8) 1.0660(12) 1.4845(15) 0.270(10) Uani 0.5 1 d . U P G -3
O16 O 0.9405(11) 0.9984(7) 1.4303(11) 0.212(8) Uani 0.5 1 d . U P G 3
Br2 Br 0.5799(11) 0.1698(9) 0.5369(18) 0.0215(6) Uani 0.1 1 d D . P B -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 1.988(2) 4_565 ?
Fe1 O1 1.992(2) . ?
Fe1 O5 2.086(2) . ?
Fe1 O8 2.090(2) . ?
Fe1 O2 2.005(2) . ?
Fe1 O4 2.005(2) 4_565 ?
Fe2 O6 2.073(2) . ?
Fe2 O9 1.986(2) . ?
Fe2 O11 1.984(2) 4_575 ?
Fe2 O12 1.997(2) . ?
Fe2 O7 2.078(2) . ?
Fe2 O10 1.992(2) 4_575 ?
Cl5 C14 1.745(5) . ?
Cl2 C6 1.740(5) . ?
Cl4 C11 1.742(4) . ?
Cl3 C8 1.739(6) . ?
Cl1 C3 1.738(5) . ?
Cl6 C17 1.723(6) . ?
O6 C9 1.255(4) . ?
O3 Fe1 1.988(2) 4_566 ?
O3 C4 1.291(4) . ?
O1 C1 1.294(4) . ?
O5 C7 1.261(4) . ?
O9 C13 1.299(4) . ?
O11 Fe2 1.984(2) 4_576 ?
O11 C16 1.293(4) . ?
O8 C12 1.259(4) . ?
O12 C18 1.288(4) . ?
O7 C10 1.255(4) . ?
O2 C2 1.295(4) . ?
O10 Fe2 1.992(2) 4_576 ?
O10 C15 1.288(4) . ?
O4 Fe1 2.005(2) 4_566 ?
O4 C5 1.295(4) . ?
N1 C19 1.511(4) . ?
N1 C22 1.510(4) . ?
N1 C25 1.520(4) . ?
N1 C28 1.524(4) . ?
N2 C40 1.517(4) . ?
N2 C31 1.512(4) . ?
N2 C34 1.517(4) . ?
N2 C37 1.518(4) . ?
C10 C9 1.542(4) . ?
C10 C11 1.386(4) . ?
C7 C12 1.545(4) . ?
C7 C8 1.388(4) . ?
C12 C11 1.377(4) . ?
C18 C13 1.476(4) . ?
C18 C17 1.390(4) . ?
C9 C8 1.389(4) . ?
C14 C15 1.389(4) . ?
C14 C13 1.386(4) . ?
C14 Br5 1.856(15) . ?
C15 C16 1.472(4) . ?
C16 C17 1.385(4) . ?
C1 C2 1.474(4) . ?
C1 C6 1.390(4) . ?
C5 C4 1.471(4) . ?
C5 C6 1.395(4) . ?
C2 C3 1.393(4) . ?
C4 C3 1.380(4) . ?
C8 Br3 1.867(17) . ?
C11 Br4 1.815(13) . ?
C6 Br2 1.858(15) . ?
C17 Br6 1.859(18) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.510(5) . ?
C35 C36 1.522(5) . ?
C3 Br1 1.853(17) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.502(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.508(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.514(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.509(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.507(5) . ?
C38 C39 1.528(5) . ?
O13 C43 1.202(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.526(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.511(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.516(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.516(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.518(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 C41 1.528(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.528(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O14 C46 1.218(7) . ?
C43 C44 1.506(6) . ?
C43 C45 1.491(6) . ?
C46 C47 1.476(7) . ?
C46 C48 1.493(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O15 O16 1.80(2) . ?

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
O3 Fe1 O1 103.74(9) 4_565 . ?
O3 Fe1 O5 162.30(9) 4_565 . ?
O3 Fe1 O8 89.18(9) 4_565 . ?
O3 Fe1 O2 96.76(9) 4_565 . ?
O3 Fe1 O4 80.16(8) 4_565 4_565 ?
O1 Fe1 O5 92.30(9) . . ?
O1 Fe1 O8 161.36(8) . . ?
O1 Fe1 O2 80.21(8) . . ?
O1 Fe1 O4 99.20(9) . 4_565 ?
O5 Fe1 O8 77.17(8) . . ?
O2 Fe1 O5 93.26(9) . . ?
O2 Fe1 O8 85.02(8) . . ?
O2 Fe1 O4 176.66(9) . 4_565 ?
O4 Fe1 O5 90.04(8) 4_565 . ?
O4 Fe1 O8 96.18(9) 4_565 . ?
O6 Fe2 O7 77.97(8) . . ?
O9 Fe2 O6 90.43(9) . . ?
O9 Fe2 O12 80.90(8) . . ?
O9 Fe2 O7 161.72(9) . . ?
O9 Fe2 O10 100.86(9) . 4_575 ?
O11 Fe2 O6 165.26(9) 4_575 . ?
O11 Fe2 O9 101.62(9) 4_575 . ?
O11 Fe2 O12 96.98(9) 4_575 . ?
O11 Fe2 O7 92.22(9) 4_575 . ?
O11 Fe2 O10 80.64(8) 4_575 4_575 ?
O12 Fe2 O6 93.25(9) . . ?
O12 Fe2 O7 85.66(8) . . ?
O10 Fe2 O6 88.84(8) 4_575 . ?
O10 Fe2 O12 177.26(9) 4_575 . ?
O10 Fe2 O7 93.06(8) 4_575 . ?
C9 O6 Fe2 115.8(2) . . ?
C4 O3 Fe1 114.93(19) . 4_566 ?
C1 O1 Fe1 114.97(19) . . ?
C7 O5 Fe1 116.6(2) . . ?
C13 O9 Fe2 113.89(19) . . ?
C16 O11 Fe2 114.47(18) . 4_576 ?
C12 O8 Fe1 116.4(2) . . ?
C18 O12 Fe2 113.81(19) . . ?
C10 O7 Fe2 115.6(2) . . ?
C2 O2 Fe1 114.21(19) . . ?
C15 O10 Fe2 114.27(19) . 4_576 ?
C5 O4 Fe1 114.39(19) . 4_566 ?
C19 N1 C25 108.8(3) . . ?
C19 N1 C28 111.4(3) . . ?
C22 N1 C19 107.7(3) . . ?
C22 N1 C25 111.9(3) . . ?
C22 N1 C28 108.8(3) . . ?
C25 N1 C28 108.3(2) . . ?
C40 N2 C37 110.9(3) . . ?
C31 N2 C40 111.5(3) . . ?
C31 N2 C34 111.0(3) . . ?
C31 N2 C37 106.2(2) . . ?
C34 N2 C40 106.2(2) . . ?
C34 N2 C37 111.2(3) . . ?
O7 C10 C9 115.3(3) . . ?
O7 C10 C11 125.6(3) . . ?
C11 C10 C9 119.1(3) . . ?
O5 C7 C12 114.7(3) . . ?
O5 C7 C8 126.2(3) . . ?
C8 C7 C12 119.1(3) . . ?
O8 C12 C7 115.0(3) . . ?
O8 C12 C11 125.4(3) . . ?
C11 C12 C7 119.6(3) . . ?
O12 C18 C13 115.4(3) . . ?
O12 C18 C17 125.0(3) . . ?
C17 C18 C13 119.6(3) . . ?
O6 C9 C10 115.1(3) . . ?
O6 C9 C8 125.4(3) . . ?
C8 C9 C10 119.5(3) . . ?
Cl5 C14 Br5 2.3(7) . . ?
C15 C14 Cl5 119.7(3) . . ?
C15 C14 Br5 118.3(7) . . ?
C13 C14 Cl5 119.2(3) . . ?
C13 C14 C15 121.1(3) . . ?
C13 C14 Br5 120.6(7) . . ?
O10 C15 C14 125.4(3) . . ?
O10 C15 C16 115.3(3) . . ?
C14 C15 C16 119.3(3) . . ?
O11 C16 C15 115.2(3) . . ?
O11 C16 C17 124.9(3) . . ?
C17 C16 C15 119.9(3) . . ?
O1 C1 C2 115.0(3) . . ?
O1 C1 C6 125.5(3) . . ?
C6 C1 C2 119.5(3) . . ?
O4 C5 C4 115.0(3) . . ?
O4 C5 C6 125.9(3) . . ?
C6 C5 C4 119.1(3) . . ?
O9 C13 C18 115.3(3) . . ?
O9 C13 C14 125.4(3) . . ?
C14 C13 C18 119.3(3) . . ?
O2 C2 C1 115.3(3) . . ?
O2 C2 C3 125.5(3) . . ?
C3 C2 C1 119.2(3) . . ?
O3 C4 C5 115.3(3) . . ?
O3 C4 C3 124.8(3) . . ?
C3 C4 C5 119.9(3) . . ?
Cl3 C8 Br3 6.0(13) . . ?
C7 C8 Cl3 121.1(4) . . ?
C7 C8 C9 121.1(3) . . ?
C7 C8 Br3 119.6(10) . . ?
C9 C8 Cl3 117.7(4) . . ?
C9 C8 Br3 119.3(10) . . ?
Cl4 C11 Br4 1.6(6) . . ?
C10 C11 Cl4 118.1(3) . . ?
C10 C11 Br4 119.7(5) . . ?
C12 C11 Cl4 120.3(3) . . ?
C12 C11 C10 121.5(3) . . ?
C12 C11 Br4 118.8(5) . . ?
Cl2 C6 Br2 6.2(8) . . ?
C1 C6 Cl2 118.5(3) . . ?
C1 C6 C5 121.0(3) . . ?
C1 C6 Br2 121.9(8) . . ?
C5 C6 Cl2 120.5(3) . . ?
C5 C6 Br2 117.0(8) . . ?
Cl6 C17 Br6 5.9(16) . . ?
C18 C17 Cl6 119.3(3) . . ?
C18 C17 Br6 117.3(10) . . ?
C16 C17 Cl6 120.0(3) . . ?
C16 C17 C18 120.7(3) . . ?
C16 C17 Br6 121.7(9) . . ?
H35A C35 H35B 108.2 . . ?
C34 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
C34 C35 C36 110.0(3) . . ?
C36 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
Cl1 C3 Br1 5.9(12) . . ?
C2 C3 Cl1 118.3(3) . . ?
C2 C3 Br1 118.2(10) . . ?
C4 C3 Cl1 120.4(3) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 Br1 120.2(10) . . ?
N2 C40 H40A 108.2 . . ?
N2 C40 H40B 108.2 . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 N2 116.2(3) . . ?
C41 C40 H40A 108.2 . . ?
C41 C40 H40B 108.2 . . ?
N1 C19 H19A 108.0 . . ?
N1 C19 H19B 108.0 . . ?
H19A C19 H19B 107.2 . . ?
C20 C19 N1 117.3(3) . . ?
C20 C19 H19A 108.0 . . ?
C20 C19 H19B 108.0 . . ?
N2 C31 H31A 108.3 . . ?
N2 C31 H31B 108.3 . . ?
N2 C31 C32 115.8(3) . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
N2 C34 H34A 108.3 . . ?
N2 C34 H34B 108.3 . . ?
C35 C34 N2 116.1(3) . . ?
C35 C34 H34A 108.3 . . ?
C35 C34 H34B 108.3 . . ?
H34A C34 H34B 107.4 . . ?
N1 C22 H22A 108.4 . . ?
N1 C22 H22B 108.4 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N1 115.7(3) . . ?
C23 C22 H22A 108.4 . . ?
C23 C22 H22B 108.4 . . ?
H38A C38 H38B 108.2 . . ?
C37 C38 H38A 109.7 . . ?
C37 C38 H38B 109.7 . . ?
C37 C38 C39 109.7(3) . . ?
C39 C38 H38A 109.7 . . ?
C39 C38 H38B 109.7 . . ?
C19 C20 H20A 110.1 . . ?
C19 C20 H20B 110.1 . . ?
C19 C20 C21 107.8(3) . . ?
H20A C20 H20B 108.5 . . ?
C21 C20 H20A 110.1 . . ?
C21 C20 H20B 110.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 C24 110.6(3) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
N1 C25 H25A 108.5 . . ?
N1 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 N1 115.2(3) . . ?
C26 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
N1 C28 H28A 108.2 . . ?
N1 C28 H28B 108.2 . . ?
H28A C28 H28B 107.3 . . ?
C29 C28 N1 116.5(3) . . ?
C29 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
C28 C29 C30 109.3(3) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
N2 C37 H37A 108.3 . . ?
N2 C37 H37B 108.3 . . ?
C38 C37 N2 115.9(3) . . ?
C38 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
C25 C26 C27 109.3(3) . . ?
H26A C26 H26B 108.3 . . ?
C27 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
C31 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C31 C32 C33 108.9(3) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.9 . . ?
C33 C32 H32B 109.9 . . ?
C40 C41 C42 109.4(3) . . ?
C40 C41 H41A 109.8 . . ?
C40 C41 H41B 109.8 . . ?
C42 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
H41A C41 H41B 108.2 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O13 C43 C44 120.9(5) . . ?
O13 C43 C45 120.8(5) . . ?
C45 C43 C44 118.3(4) . . ?
O14 C46 C47 120.7(6) . . ?
O14 C46 C48 121.4(5) . . ?
C47 C46 C48 117.8(5) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 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 O3 C4 C5 3.7(3) 4_566 . . . ?
Fe1 O3 C4 C3 -178.1(3) 4_566 . . . ?
Fe1 O1 C1 C2 -2.6(3) . . . . ?
Fe1 O1 C1 C6 178.0(3) . . . . ?
Fe1 O5 C7 C12 1.1(3) . . . . ?
Fe1 O5 C7 C8 -178.6(2) . . . . ?
Fe1 O8 C12 C7 -0.5(3) . . . . ?
Fe1 O8 C12 C11 179.8(2) . . . . ?
Fe1 O2 C2 C1 5.2(3) . . . . ?
Fe1 O2 C2 C3 -174.5(3) . . . . ?
Fe1 O4 C5 C4 -2.6(3) 4_566 . . . ?
Fe1 O4 C5 C6 177.5(3) 4_566 . . . ?
Fe2 O6 C9 C10 3.7(3) . . . . ?
Fe2 O6 C9 C8 -177.0(2) . . . . ?
Fe2 O9 C13 C18 5.3(3) . . . . ?
Fe2 O9 C13 C14 -176.5(3) . . . . ?
Fe2 O11 C16 C15 -2.3(3) 4_576 . . . ?
Fe2 O11 C16 C17 178.2(3) 4_576 . . . ?
Fe2 O12 C18 C13 -6.9(3) . . . . ?
Fe2 O12 C18 C17 173.7(3) . . . . ?
Fe2 O7 C10 C9 -2.4(3) . . . . ?
Fe2 O7 C10 C11 176.4(3) . . . . ?
Fe2 O10 C15 C14 -177.6(3) 4_576 . . . ?
Fe2 O10 C15 C16 2.9(3) 4_576 . . . ?
Cl5 C14 C15 O10 1.4(5) . . . . ?
Cl5 C14 C15 C16 -179.1(2) . . . . ?
Cl5 C14 C13 O9 0.0(5) . . . . ?
Cl5 C14 C13 C18 178.2(2) . . . . ?
O6 C9 C8 Cl3 -1.0(6) . . . . ?
O6 C9 C8 C7 175.7(3) . . . . ?
O6 C9 C8 Br3 -7.5(13) . . . . ?
O3 C4 C3 Cl1 1.7(6) . . . . ?
O3 C4 C3 C2 -178.3(3) . . . . ?
O3 C4 C3 Br1 -5.2(12) . . . . ?
O1 C1 C2 O2 -1.8(4) . . . . ?
O1 C1 C2 C3 178.0(3) . . . . ?
O1 C1 C6 Cl2 -0.1(5) . . . . ?
O1 C1 C6 C5 -177.2(3) . . . . ?
O1 C1 C6 Br2 5.8(10) . . . . ?
O5 C7 C12 O8 -0.5(4) . . . . ?
O5 C7 C12 C11 179.3(3) . . . . ?
O5 C7 C8 Cl3 1.3(6) . . . . ?
O5 C7 C8 C9 -175.3(3) . . . . ?
O5 C7 C8 Br3 8.0(13) . . . . ?
O11 C16 C17 Cl6 -1.7(6) . . . . ?
O11 C16 C17 C18 178.9(3) . . . . ?
O11 C16 C17 Br6 5.0(15) . . . . ?
O8 C12 C11 Cl4 -1.6(5) . . . . ?
O8 C12 C11 C10 176.5(3) . . . . ?
O8 C12 C11 Br4 -1.0(8) . . . . ?
O12 C18 C13 O9 1.1(4) . . . . ?
O12 C18 C13 C14 -177.2(3) . . . . ?
O12 C18 C17 Cl6 -0.4(6) . . . . ?
O12 C18 C17 C16 179.0(3) . . . . ?
O12 C18 C17 Br6 -6.8(14) . . . . ?
O7 C10 C9 O6 -0.8(4) . . . . ?
O7 C10 C9 C8 179.7(3) . . . . ?
O7 C10 C11 Cl4 2.6(5) . . . . ?
O7 C10 C11 C12 -175.6(3) . . . . ?
O7 C10 C11 Br4 1.9(8) . . . . ?
O2 C2 C3 Cl1 0.8(5) . . . . ?
O2 C2 C3 C4 -179.3(3) . . . . ?
O2 C2 C3 Br1 7.5(12) . . . . ?
O10 C15 C16 O11 -0.4(4) . . . . ?
O10 C15 C16 C17 179.1(3) . . . . ?
O4 C5 C4 O3 -0.7(4) . . . . ?
O4 C5 C4 C3 -179.0(3) . . . . ?
O4 C5 C6 Cl2 0.3(5) . . . . ?
O4 C5 C6 C1 177.3(3) . . . . ?
O4 C5 C6 Br2 -5.6(10) . . . . ?
N1 C19 C20 C21 179.1(3) . . . . ?
N1 C22 C23 C24 -175.0(4) . . . . ?
N1 C25 C26 C27 173.4(3) . . . . ?
N1 C28 C29 C30 172.2(3) . . . . ?
N2 C40 C41 C42 -170.3(3) . . . . ?
N2 C31 C32 C33 -171.1(3) . . . . ?
C10 C9 C8 Cl3 178.4(4) . . . . ?
C10 C9 C8 C7 -4.9(5) . . . . ?
C10 C9 C8 Br3 171.8(12) . . . . ?
C7 C12 C11 Cl4 178.7(2) . . . . ?
C7 C12 C11 C10 -3.2(5) . . . . ?
C7 C12 C11 Br4 179.3(7) . . . . ?
C12 C7 C8 Cl3 -178.5(4) . . . . ?
C12 C7 C8 C9 5.0(5) . . . . ?
C12 C7 C8 Br3 -171.8(12) . . . . ?
C9 C10 C11 Cl4 -178.6(2) . . . . ?
C9 C10 C11 C12 3.3(5) . . . . ?
C9 C10 C11 Br4 -179.3(7) . . . . ?
C14 C15 C16 O11 -179.9(3) . . . . ?
C14 C15 C16 C17 -0.5(5) . . . . ?
C15 C14 C13 O9 178.6(3) . . . . ?
C15 C14 C13 C18 -3.3(5) . . . . ?
C15 C16 C17 Cl6 178.9(4) . . . . ?
C15 C16 C17 C18 -0.5(5) . . . . ?
C15 C16 C17 Br6 -174.5(15) . . . . ?
C1 C2 C3 Cl1 -178.9(4) . . . . ?
C1 C2 C3 C4 1.0(5) . . . . ?
C1 C2 C3 Br1 -172.2(11) . . . . ?
C5 C4 C3 Cl1 179.8(4) . . . . ?
C5 C4 C3 C2 -0.1(5) . . . . ?
C5 C4 C3 Br1 172.9(12) . . . . ?
C13 C18 C17 Cl6 -179.8(4) . . . . ?
C13 C18 C17 C16 -0.4(5) . . . . ?
C13 C18 C17 Br6 173.8(14) . . . . ?
C13 C14 C15 O10 -177.1(3) . . . . ?
C13 C14 C15 C16 2.4(5) . . . . ?
C2 C1 C6 Cl2 -179.5(3) . . . . ?
C2 C1 C6 C5 3.5(5) . . . . ?
C2 C1 C6 Br2 -173.5(10) . . . . ?
C4 C5 C6 Cl2 -179.6(3) . . . . ?
C4 C5 C6 C1 -2.6(5) . . . . ?
C4 C5 C6 Br2 174.5(9) . . . . ?
C8 C7 C12 O8 179.3(3) . . . . ?
C8 C7 C12 C11 -0.9(4) . . . . ?
C11 C10 C9 O6 -179.8(3) . . . . ?
C11 C10 C9 C8 0.8(4) . . . . ?
C6 C1 C2 O2 177.6(3) . . . . ?
C6 C1 C2 C3 -2.6(5) . . . . ?
C6 C5 C4 O3 179.2(3) . . . . ?
C6 C5 C4 C3 0.9(5) . . . . ?
C17 C18 C13 O9 -179.4(3) . . . . ?
C17 C18 C13 C14 2.2(5) . . . . ?
C40 N2 C31 C32 55.3(4) . . . . ?
C40 N2 C34 C35 175.5(3) . . . . ?
C40 N2 C37 C38 -61.8(4) . . . . ?
C19 N1 C22 C23 -61.2(4) . . . . ?
C19 N1 C25 C26 169.9(3) . . . . ?
C19 N1 C28 C29 -55.0(4) . . . . ?
C31 N2 C40 C41 55.1(4) . . . . ?
C31 N2 C34 C35 -63.1(4) . . . . ?
C31 N2 C37 C38 176.9(3) . . . . ?
C34 N2 C40 C41 176.2(3) . . . . ?
C34 N2 C31 C32 -62.8(4) . . . . ?
C34 N2 C37 C38 56.0(4) . . . . ?
C22 N1 C19 C20 -170.5(3) . . . . ?
C22 N1 C25 C26 51.0(4) . . . . ?
C22 N1 C28 C29 63.6(4) . . . . ?
C25 N1 C19 C20 68.0(4) . . . . ?
C25 N1 C22 C23 58.3(4) . . . . ?
C25 N1 C28 C29 -174.6(3) . . . . ?
C28 N1 C19 C20 -51.3(4) . . . . ?
C28 N1 C22 C23 177.9(3) . . . . ?
C28 N1 C25 C26 -69.0(4) . . . . ?
C37 N2 C40 C41 -62.9(4) . . . . ?
C37 N2 C31 C32 176.2(3) . . . . ?
C37 N2 C34 C35 54.8(4) . . . . ?
C39 C38 C37 N2 170.5(3) . . . . ?
C36 C35 C34 N2 168.7(3) . . . . ?
Br5 C14 C15 O10 3.5(7) . . . . ?
Br5 C14 C15 C16 -177.0(6) . . . . ?
Br5 C14 C13 O9 -2.1(8) . . . . ?
Br5 C14 C13 C18 176.1(7) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.066
_oxdiff_exptl_absorpt_empirical_full_min 0.909
####################################################################### 
# 
# 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_F-006-d_CCDC-2014811_R1
_database_code_depnum_ccdc_archive 'CCDC 2014811'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-08-02
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl5.66 F0.34 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl5.66 F0.34 Fe2 N2 O12'
_chemical_formula_weight         1099.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl5.66 F0.34 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.7147(3)
_cell_length_b                   20.7638(7)
_cell_length_c                   12.2126(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.108(3)
_cell_angle_gamma                90
_cell_volume                     2666.13(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10151
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1260
_cell_measurement_theta_min      2.1670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1139
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.061
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20643
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.517
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0604650000
_diffrn_orient_matrix_UB_12      -0.0075781000
_diffrn_orient_matrix_UB_13      0.0120787000
_diffrn_orient_matrix_UB_21      0.0189278000
_diffrn_orient_matrix_UB_22      0.0132158000
_diffrn_orient_matrix_UB_23      0.0542242000
_diffrn_orient_matrix_UB_31      -0.0231853000
_diffrn_orient_matrix_UB_32      0.0305741000
_diffrn_orient_matrix_UB_33      -0.0204162000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4888
_reflns_number_total             6013
_reflns_odcompleteness_completeness 89.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.99
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6013
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.103
_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)+(0.0302P)²+6.5523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1144
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-F2
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(Cl1)
Uanis(Cl2) = Uanis(F2)
Uanis(F3) = Uanis(Cl3)
4. Others
 Fixed Sof: Cl1(0.938) Cl2(0.938) Cl3(0.954) F1(0.062) F2(0.062) F3(0.046)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C13(H13A,H13B), C20(H20A,H20B), C14(H14A,H14B), C10(H10A,
 H10B), C16(H16A,H16B), C11(H11A,H11B), C17(H17A,H17B)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C12(H12A,H12B,
 H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.04356(4) 0.68857(2) 0.47750(3) 0.02025(11) Uani 1 1 d . . . . .
Cl1 Cl 0.93296(10) 0.67236(6) 0.06184(9) 0.0244(2) Uani 0.938 1 d . . P A 2
Cl2 Cl 0.66228(9) 0.82973(5) 0.39298(7) 0.0265(2) Uani 0.938 1 d . . P B 2
Cl3 Cl 1.29746(7) 0.48039(5) 0.51446(9) 0.0292(2) Uani 0.954 1 d . . P C 2
O3 O 0.69573(19) 0.75506(10) 0.00668(16) 0.0213(4) Uani 1 1 d . . . . .
O1 O 0.90412(19) 0.75245(10) 0.44692(16) 0.0215(4) Uani 1 1 d . . . . .
O4 O 0.57819(18) 0.81311(10) 0.14356(16) 0.0217(4) Uani 1 1 d . . . . .
O6 O 1.14488(19) 0.60328(10) 0.47992(17) 0.0237(4) Uani 1 1 d . . . . .
O2 O 1.01485(18) 0.68727(10) 0.31144(16) 0.0208(4) Uani 1 1 d . . . . .
O5 O 1.09683(19) 0.38114(10) 0.52226(17) 0.0232(4) Uani 1 1 d . . . . .
N1 N 0.3918(2) 0.63991(13) 0.2490(2) 0.0262(6) Uani 1 1 d . . . . .
C5 C 0.6838(3) 0.78538(14) 0.1886(2) 0.0190(6) Uani 1 1 d . . . . .
C1 C 0.8485(3) 0.75350(14) 0.3430(2) 0.0191(6) Uani 1 1 d . . . . .
C4 C 0.7486(3) 0.75030(14) 0.1107(2) 0.0199(6) Uani 1 1 d . . . . .
C2 C 0.9112(3) 0.71640(14) 0.2661(2) 0.0186(6) Uani 1 1 d . . . . .
C9 C 1.0841(3) 0.55266(15) 0.4912(2) 0.0211(6) Uani 1 1 d . . . . .
C6 C 0.7369(3) 0.78662(14) 0.3027(2) 0.0202(6) Uani 1 1 d D . . . .
C7 C 1.0591(3) 0.43808(15) 0.5129(2) 0.0217(6) Uani 1 1 d . . . . .
C3 C 0.8582(3) 0.71559(14) 0.1522(2) 0.0207(6) Uani 1 1 d . . . . .
C8 C 1.1354(3) 0.49137(15) 0.5064(2) 0.0225(6) Uani 1 1 d . . . . .
C19 C 0.3915(3) 0.71136(16) 0.2214(3) 0.0285(7) Uani 1 1 d . . . . .
H19A H 0.4741 0.7299 0.2584 0.034 Uiso 1 1 calc R U . . .
H19B H 0.3856 0.7160 0.1399 0.034 Uiso 1 1 calc R U . . .
C13 C 0.3978(3) 0.62883(16) 0.3725(3) 0.0285(7) Uani 1 1 d . . . . .
H13A H 0.3141 0.6406 0.3898 0.034 Uiso 1 1 calc R U . . .
H13B H 0.4102 0.5822 0.3873 0.034 Uiso 1 1 calc R U . . .
C20 C 0.2859(3) 0.75080(17) 0.2550(3) 0.0307(7) Uani 1 1 d . . . . .
H20A H 0.2845 0.7434 0.3349 0.037 Uiso 1 1 calc R U . . .
H20B H 0.2028 0.7373 0.2106 0.037 Uiso 1 1 calc R U . . .
C14 C 0.4995(3) 0.66477(17) 0.4527(3) 0.0335(7) Uani 1 1 d . . . . .
H14A H 0.4849 0.7118 0.4450 0.040 Uiso 1 1 calc R U . . .
H14B H 0.5845 0.6551 0.4362 0.040 Uiso 1 1 calc R U . . .
C10 C 0.2694(3) 0.61016(17) 0.1858(3) 0.0311(7) Uani 1 1 d . . . . .
H10A H 0.1972 0.6297 0.2135 0.037 Uiso 1 1 calc R U . . .
H10B H 0.2601 0.6217 0.1060 0.037 Uiso 1 1 calc R U . . .
C16 C 0.5085(3) 0.60942(17) 0.2168(3) 0.0335(7) Uani 1 1 d . . . . .
H16A H 0.5846 0.6330 0.2557 0.040 Uiso 1 1 calc R U . . .
H16B H 0.5155 0.5646 0.2451 0.040 Uiso 1 1 calc R U . . .
C15 C 0.4930(3) 0.64309(18) 0.5710(3) 0.0373(8) Uani 1 1 d . . . . .
H15A H 0.4049 0.6456 0.5819 0.056 Uiso 1 1 calc R U . . .
H15B H 0.5468 0.6712 0.6250 0.056 Uiso 1 1 calc R U . . .
H15C H 0.5232 0.5986 0.5820 0.056 Uiso 1 1 calc R U . . .
C21 C 0.3076(3) 0.82209(17) 0.2354(3) 0.0346(8) Uani 1 1 d . . . . .
H21A H 0.3042 0.8296 0.1556 0.052 Uiso 1 1 calc R U . . .
H21B H 0.3912 0.8349 0.2775 0.052 Uiso 1 1 calc R U . . .
H21C H 0.2414 0.8476 0.2604 0.052 Uiso 1 1 calc R U . . .
C11 C 0.2597(4) 0.53747(18) 0.1946(3) 0.0405(9) Uani 1 1 d . . . . .
H11A H 0.2639 0.5249 0.2734 0.049 Uiso 1 1 calc R U . . .
H11B H 0.3314 0.5168 0.1678 0.049 Uiso 1 1 calc R U . . .
C17 C 0.5119(4) 0.6079(2) 0.0934(3) 0.0453(10) Uani 1 1 d . . . . .
H17A H 0.5122 0.6524 0.0644 0.054 Uiso 1 1 calc R U . . .
H17B H 0.4353 0.5857 0.0522 0.054 Uiso 1 1 calc R U . . .
C18 C 0.6307(5) 0.5726(2) 0.0756(4) 0.0581(12) Uani 1 1 d . . . . .
H18A H 0.6360 0.5743 -0.0036 0.087 Uiso 1 1 calc R U . . .
H18B H 0.6266 0.5276 0.0987 0.087 Uiso 1 1 calc R U . . .
H18C H 0.7060 0.5932 0.1201 0.087 Uiso 1 1 calc R U . . .
C12 C 0.1340(4) 0.5153(2) 0.1240(4) 0.0649(14) Uani 1 1 d . . . . .
H12A H 0.1308 0.5275 0.0460 0.097 Uiso 1 1 calc R U . . .
H12B H 0.0634 0.5357 0.1513 0.097 Uiso 1 1 calc R U . . .
H12C H 0.1270 0.4684 0.1294 0.097 Uiso 1 1 calc R U . . .
F1 F 0.913(5) 0.682(3) 0.076(4) 0.0244(2) Uani 0.062 1 d . . P A -2
F2 F 0.681(4) 0.826(2) 0.367(3) 0.0265(2) Uani 0.062 1 d D . P B -2
F3 F 1.259(5) 0.487(3) 0.506(5) 0.0292(2) Uani 0.046 1 d . . P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 1.983(2) 4_676 ?
Fe1 O1 1.979(2) . ?
Fe1 O4 1.990(2) 4_676 ?
Fe1 O6 2.074(2) . ?
Fe1 O2 1.992(2) . ?
Fe1 O5 2.088(2) 3_766 ?
Cl1 C3 1.734(3) . ?
Cl2 C6 1.731(3) . ?
Cl3 C8 1.735(3) . ?
O3 Fe1 1.983(2) 4_575 ?
O3 C4 1.291(3) . ?
O1 C1 1.294(3) . ?
O4 Fe1 1.990(2) 4_575 ?
O4 C5 1.294(3) . ?
O6 C9 1.258(4) . ?
O2 C2 1.292(3) . ?
O5 Fe1 2.088(2) 3_766 ?
O5 C7 1.248(4) . ?
N1 C19 1.521(4) . ?
N1 C13 1.515(4) . ?
N1 C10 1.519(4) . ?
N1 C16 1.519(4) . ?
C5 C4 1.474(4) . ?
C5 C6 1.400(4) . ?
C1 C2 1.473(4) . ?
C1 C6 1.385(4) . ?
C4 C3 1.388(4) . ?
C2 C3 1.397(4) . ?
C9 C7 1.538(4) 3_766 ?
C9 C8 1.384(4) . ?
C6 F2 1.353(18) . ?
C7 C9 1.538(4) 3_766 ?
C7 C8 1.387(4) . ?
C3 F1 1.38(4) . ?
C8 F3 1.33(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.516(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.514(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.524(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.528(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.518(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.515(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.523(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.519(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
O3 Fe1 O4 80.90(8) 4_676 4_676 ?
O3 Fe1 O6 95.24(8) 4_676 . ?
O3 Fe1 O2 98.71(8) 4_676 . ?
O3 Fe1 O5 167.60(8) 4_676 3_766 ?
O1 Fe1 O3 101.72(9) . 4_676 ?
O1 Fe1 O4 100.94(8) . 4_676 ?
O1 Fe1 O6 161.61(8) . . ?
O1 Fe1 O2 81.61(8) . . ?
O1 Fe1 O5 86.96(8) . 3_766 ?
O4 Fe1 O6 88.63(9) 4_676 . ?
O4 Fe1 O2 177.45(9) 4_676 . ?
O4 Fe1 O5 88.81(8) 4_676 3_766 ?
O6 Fe1 O5 77.49(8) . 3_766 ?
O2 Fe1 O6 88.89(8) . . ?
O2 Fe1 O5 91.26(8) . 3_766 ?
C4 O3 Fe1 114.30(18) . 4_575 ?
C1 O1 Fe1 112.61(18) . . ?
C5 O4 Fe1 113.66(18) . 4_575 ?
C9 O6 Fe1 115.76(19) . . ?
C2 O2 Fe1 112.43(18) . . ?
C7 O5 Fe1 115.86(19) . 3_766 ?
C13 N1 C19 111.5(2) . . ?
C13 N1 C10 108.1(2) . . ?
C13 N1 C16 108.4(2) . . ?
C10 N1 C19 108.6(2) . . ?
C10 N1 C16 111.9(3) . . ?
C16 N1 C19 108.4(2) . . ?
O4 C5 C4 115.3(2) . . ?
O4 C5 C6 124.7(3) . . ?
C6 C5 C4 119.9(3) . . ?
O1 C1 C2 115.9(2) . . ?
O1 C1 C6 124.1(3) . . ?
C6 C1 C2 120.1(2) . . ?
O3 C4 C5 115.2(2) . . ?
O3 C4 C3 125.4(3) . . ?
C3 C4 C5 119.5(2) . . ?
O2 C2 C1 115.5(2) . . ?
O2 C2 C3 124.9(3) . . ?
C3 C2 C1 119.6(2) . . ?
O6 C9 C7 115.2(3) . 3_766 ?
O6 C9 C8 125.6(3) . . ?
C8 C9 C7 119.1(3) . 3_766 ?
C5 C6 Cl2 119.6(2) . . ?
C1 C6 Cl2 120.2(2) . . ?
C1 C6 C5 120.2(3) . . ?
F2 C6 Cl2 6(2) . . ?
F2 C6 C5 116.4(19) . . ?
F2 C6 C1 123.1(19) . . ?
O5 C7 C9 115.2(3) . 3_766 ?
O5 C7 C8 125.2(3) . . ?
C8 C7 C9 119.6(3) . 3_766 ?
C4 C3 Cl1 119.9(2) . . ?
C4 C3 C2 120.7(3) . . ?
C2 C3 Cl1 119.4(2) . . ?
F1 C3 Cl1 3(2) . . ?
F1 C3 C4 117(2) . . ?
F1 C3 C2 122(2) . . ?
C9 C8 Cl3 119.7(2) . . ?
C9 C8 C7 121.2(3) . . ?
C7 C8 Cl3 119.1(2) . . ?
F3 C8 Cl3 5(3) . . ?
F3 C8 C9 115(3) . . ?
F3 C8 C7 123(3) . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N1 115.9(3) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
N1 C13 H13A 108.0 . . ?
N1 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 N1 117.1(3) . . ?
C14 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.7(3) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C13 C14 C15 107.9(3) . . ?
H14A C14 H14B 108.4 . . ?
C15 C14 H14A 110.1 . . ?
C15 C14 H14B 110.1 . . ?
N1 C10 H10A 108.4 . . ?
N1 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N1 115.7(3) . . ?
C11 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
N1 C16 H16A 108.2 . . ?
N1 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N1 116.4(3) . . ?
C17 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
C10 C11 C12 109.0(3) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C16 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
C16 C17 C18 109.5(4) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 O3 C4 C5 2.2(3) 4_575 . . . ?
Fe1 O3 C4 C3 -177.8(2) 4_575 . . . ?
Fe1 O1 C1 C2 -9.9(3) . . . . ?
Fe1 O1 C1 C6 170.0(2) . . . . ?
Fe1 O4 C5 C4 -8.2(3) 4_575 . . . ?
Fe1 O4 C5 C6 172.2(2) 4_575 . . . ?
Fe1 O6 C9 C7 7.0(3) . . . 3_766 ?
Fe1 O6 C9 C8 -173.0(2) . . . . ?
Fe1 O2 C2 C1 10.1(3) . . . . ?
Fe1 O2 C2 C3 -170.9(2) . . . . ?
Fe1 O5 C7 C9 2.9(3) 3_766 . . 3_766 ?
Fe1 O5 C7 C8 -177.3(2) 3_766 . . . ?
O3 C4 C3 Cl1 -1.7(4) . . . . ?
O3 C4 C3 C2 176.6(3) . . . . ?
O3 C4 C3 F1 -2(3) . . . . ?
O1 C1 C2 O2 -0.2(4) . . . . ?
O1 C1 C2 C3 -179.3(3) . . . . ?
O1 C1 C6 Cl2 -0.4(4) . . . . ?
O1 C1 C6 C5 179.6(3) . . . . ?
O1 C1 C6 F2 6(3) . . . . ?
O4 C5 C4 O3 4.1(4) . . . . ?
O4 C5 C4 C3 -175.9(3) . . . . ?
O4 C5 C6 Cl2 -2.1(4) . . . . ?
O4 C5 C6 C1 177.8(3) . . . . ?
O4 C5 C6 F2 -8(2) . . . . ?
O6 C9 C8 Cl3 1.6(4) . . . . ?
O6 C9 C8 C7 -177.0(3) . . . . ?
O6 C9 C8 F3 -1(3) . . . . ?
O2 C2 C3 Cl1 0.6(4) . . . . ?
O2 C2 C3 C4 -177.7(3) . . . . ?
O2 C2 C3 F1 1(3) . . . . ?
O5 C7 C8 Cl3 -1.4(4) . . . . ?
O5 C7 C8 C9 177.2(3) . . . . ?
O5 C7 C8 F3 2(3) . . . . ?
N1 C19 C20 C21 173.0(3) . . . . ?
N1 C13 C14 C15 -176.5(3) . . . . ?
N1 C10 C11 C12 -178.2(4) . . . . ?
N1 C16 C17 C18 -176.8(3) . . . . ?
C5 C4 C3 Cl1 178.3(2) . . . . ?
C5 C4 C3 C2 -3.4(4) . . . . ?
C5 C4 C3 F1 178(3) . . . . ?
C1 C2 C3 Cl1 179.5(2) . . . . ?
C1 C2 C3 C4 1.2(4) . . . . ?
C1 C2 C3 F1 180(3) . . . . ?
C4 C5 C6 Cl2 178.3(2) . . . . ?
C4 C5 C6 C1 -1.8(4) . . . . ?
C4 C5 C6 F2 172(2) . . . . ?
C2 C1 C6 Cl2 179.5(2) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
C2 C1 C6 F2 -174(2) . . . . ?
C9 C7 C8 Cl3 178.4(2) 3_766 . . . ?
C9 C7 C8 C9 -3.0(5) 3_766 . . . ?
C9 C7 C8 F3 -178(3) 3_766 . . . ?
C6 C5 C4 O3 -176.3(3) . . . . ?
C6 C5 C4 C3 3.7(4) . . . . ?
C6 C1 C2 O2 179.9(3) . . . . ?
C6 C1 C2 C3 0.8(4) . . . . ?
C7 C9 C8 Cl3 -178.5(2) 3_766 . . . ?
C7 C9 C8 C7 3.0(5) 3_766 . . . ?
C7 C9 C8 F3 178(3) 3_766 . . . ?
C19 N1 C13 C14 -49.8(4) . . . . ?
C19 N1 C10 C11 174.1(3) . . . . ?
C19 N1 C16 C17 -66.4(4) . . . . ?
C13 N1 C19 C20 -56.9(3) . . . . ?
C13 N1 C10 C11 -64.7(4) . . . . ?
C13 N1 C16 C17 172.5(3) . . . . ?
C10 N1 C19 C20 62.2(3) . . . . ?
C10 N1 C13 C14 -169.2(3) . . . . ?
C10 N1 C16 C17 53.4(4) . . . . ?
C16 N1 C19 C20 -176.1(3) . . . . ?
C16 N1 C13 C14 69.4(4) . . . . ?
C16 N1 C10 C11 54.5(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.788
####################################################################### 
# 
# 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_F-006_CCDC-2014812_R1
_database_code_depnum_ccdc_archive 'CCDC 2014812'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-08-04
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 Cl5.66 F0.34 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl5.66 F0.34 Fe2 N2 O15'
_chemical_formula_weight         1233.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl5.66 F0.34 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.1787(5)
_cell_length_b                   21.8982(6)
_cell_length_c                   14.4000(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.000(3)
_cell_angle_gamma                90
_cell_volume                     6051.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    35349
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1850
_cell_measurement_theta_min      1.7600
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2573
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.067
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42133
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         1.796
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0219250000
_diffrn_orient_matrix_UB_12      0.0138715000
_diffrn_orient_matrix_UB_13      -0.0240678000
_diffrn_orient_matrix_UB_21      0.0295510000
_diffrn_orient_matrix_UB_22      -0.0069165000
_diffrn_orient_matrix_UB_23      0.0404261000
_diffrn_orient_matrix_UB_31      0.0035033000
_diffrn_orient_matrix_UB_32      -0.0284706000
_diffrn_orient_matrix_UB_33      -0.0215645000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9736
_reflns_number_total             11040
_reflns_odcompleteness_completeness 89.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.07
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11040
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.033
_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)+(0.0598P)²+4.6914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1066
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-F4
 1.33 with sigma of 0.02
 C3-F1
 1.33 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C17-F6
 1.33 with sigma of 0.02
 C14-F5
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl6) = Uanis(F6)
Uanis(Cl4) = Uanis(F4)
Uanis(Cl5) = Uanis(F5)
Uanis(Cl2) = Uanis(F2)
Uanis(Cl3) = Uanis(F3)
Uanis(Cl1) = Uanis(F1)
4. Others
 Fixed Sof: Cl2(0.955) Cl5(0.955) Cl4(0.92) Cl3(0.92) Cl6(0.955) Cl1(0.955)
 F3(0.08) F2(0.045) F5(0.045) F1(0.045) F6(0.045) F4(0.08) O15(0.5) O16(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C31(H31A,H31B), C19(H19A,H19B), C37(H37A,H37B), C28(H28A,
 H28B), C22(H22A,H22B), C34(H34A,H34B), C38(H38A,H38B), C23(H23A,H23B),
 C25(H25A,H25B), C41(H41A,H41B), C32(H32A,H32B), C35(H35A,H35B), C20(H20A,H20B),
  C29(H29A,H29B), C26(H26A,H26B)
5.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C21(H21A,H21B,
 H21C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C27(H27A,H27B,H27C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C),
 C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Fe2 Fe 0.77870(2) 0.31986(2) 0.60476(2) 0.01429(8) Uani 1 1 d . . . . .
Fe1 Fe 0.76001(2) 0.68246(2) 0.59187(2) 0.01455(8) Uani 1 1 d . . . . .
Cl2 Cl 0.89646(3) 0.67463(3) 0.94868(4) 0.02065(13) Uani 0.955 1 d . . P A 2
Cl5 Cl 0.91951(3) 0.32006(3) 0.96277(4) 0.02270(14) Uani 0.955 1 d . . P B 2
Cl4 Cl 0.61982(3) 0.49699(4) 0.62965(7) 0.02297(15) Uani 0.92 1 d . . P C 2
Cl3 Cl 0.90733(3) 0.50848(3) 0.53264(5) 0.02240(14) Uani 0.92 1 d . . P D 2
Cl6 Cl 0.63648(3) 0.18440(3) 0.75145(4) 0.02739(15) Uani 0.955 1 d . . P E 2
Cl1 Cl 0.61872(3) 0.81802(3) 0.73937(4) 0.02817(15) Uani 0.955 1 d . . P F 2
O10 O 0.83522(7) 0.23699(6) 1.05133(9) 0.0171(3) Uani 1 1 d . . . . .
O12 O 0.72248(7) 0.26418(6) 0.66006(9) 0.0170(3) Uani 1 1 d . . . . .
O2 O 0.70355(7) 0.73799(6) 0.64672(9) 0.0180(3) Uani 1 1 d . . . . .
O4 O 0.81424(7) 0.75829(6) 1.03956(9) 0.0166(3) Uani 1 1 d . . . . .
O5 O 0.81936(7) 0.61079(6) 0.56581(9) 0.0183(3) Uani 1 1 d . . . . .
O6 O 0.83238(7) 0.39623(6) 0.57912(9) 0.0186(3) Uani 1 1 d . . . . .
O3 O 0.69839(7) 0.81424(6) 0.95313(9) 0.0180(3) Uani 1 1 d . . . . .
O9 O 0.83821(7) 0.31962(6) 0.74549(9) 0.0167(3) Uani 1 1 d . . . . .
O11 O 0.71729(7) 0.18516(6) 0.96532(9) 0.0181(3) Uani 1 1 d . . . . .
O1 O 0.81751(7) 0.68014(6) 0.73232(9) 0.0167(3) Uani 1 1 d . . . . .
O7 O 0.71424(7) 0.39242(6) 0.61660(9) 0.0184(3) Uani 1 1 d . . . . .
O8 O 0.70109(7) 0.60658(6) 0.60458(9) 0.0181(3) Uani 1 1 d . . . . .
N2 N 0.49120(8) 0.70110(8) 0.49280(11) 0.0209(4) Uani 1 1 d . . . . .
N1 N 0.95220(9) 0.85176(8) 0.77200(12) 0.0219(4) Uani 1 1 d . . . . .
C1 C 0.79162(9) 0.71075(8) 0.78955(13) 0.0148(4) Uani 1 1 d . . . . .
C5 C 0.79016(10) 0.75101(8) 0.94556(13) 0.0153(4) Uani 1 1 d . . . . .
C2 C 0.72666(10) 0.74404(9) 0.74057(13) 0.0158(4) Uani 1 1 d . . . . .
C15 C 0.81045(10) 0.24688(8) 0.95814(13) 0.0156(4) Uani 1 1 d . . . . .
C9 C 0.80434(10) 0.44753(9) 0.58053(13) 0.0169(4) Uani 1 1 d . . . . .
C4 C 0.72485(10) 0.78348(9) 0.89668(13) 0.0163(4) Uani 1 1 d . . . . .
C18 C 0.74580(9) 0.25735(8) 0.75366(13) 0.0154(4) Uani 1 1 d . . . . .
C7 C 0.79736(10) 0.55799(9) 0.57400(13) 0.0168(4) Uani 1 1 d . . . . .
C16 C 0.74386(9) 0.21639(9) 0.90920(13) 0.0161(4) Uani 1 1 d . . . . .
C13 C 0.81213(10) 0.28877(8) 0.80290(13) 0.0151(4) Uani 1 1 d . . . . .
C40 C 0.55403(10) 0.74039(10) 0.49522(15) 0.0249(4) Uani 1 1 d . . . . .
H40A H 0.5688 0.7627 0.5581 0.030 Uiso 1 1 calc R U . . .
H40B H 0.5928 0.7130 0.4940 0.030 Uiso 1 1 calc R U . . .
C31 C 0.42847(10) 0.74031(10) 0.49088(15) 0.0249(4) Uani 1 1 d . . . . .
H31A H 0.4137 0.7629 0.4283 0.030 Uiso 1 1 calc R U . . .
H31B H 0.3897 0.7129 0.4918 0.030 Uiso 1 1 calc R U . . .
C3 C 0.69536(10) 0.77897(9) 0.79589(13) 0.0188(4) Uani 1 1 d D . . . .
C10 C 0.73437(10) 0.44525(9) 0.60278(13) 0.0169(4) Uani 1 1 d . . . . .
C6 C 0.82089(9) 0.71478(9) 0.89085(13) 0.0155(4) Uani 1 1 d D . . . .
C17 C 0.71385(10) 0.22241(9) 0.80858(13) 0.0180(4) Uani 1 1 d D . . . .
C12 C 0.72756(10) 0.55548(9) 0.59662(13) 0.0168(4) Uani 1 1 d . . . . .
C8 C 0.83060(10) 0.50388(8) 0.56390(14) 0.0184(4) Uani 1 1 d . . . . .
C19 C 1.00090(11) 0.86310(10) 0.87408(14) 0.0250(4) Uani 1 1 d . . . . .
H19A H 1.0484 0.8509 0.8753 0.030 Uiso 1 1 calc R U . . .
H19B H 1.0019 0.9076 0.8865 0.030 Uiso 1 1 calc R U . . .
C14 C 0.84188(9) 0.28311(9) 0.90384(13) 0.0165(4) Uani 1 1 d D . . . .
C37 C 0.46876(11) 0.66211(10) 0.40086(14) 0.0241(4) Uani 1 1 d . . . . .
H37A H 0.4256 0.6400 0.3995 0.029 Uiso 1 1 calc R U . . .
H37B H 0.4571 0.6896 0.3435 0.029 Uiso 1 1 calc R U . . .
C28 C 0.98567(11) 0.87877(10) 0.70015(15) 0.0270(5) Uani 1 1 d . . . . .
H28A H 1.0310 0.8583 0.7096 0.032 Uiso 1 1 calc R U . . .
H28B H 0.9557 0.8693 0.6331 0.032 Uiso 1 1 calc R U . . .
C22 C 0.94112(11) 0.78342(10) 0.75172(16) 0.0254(5) Uani 1 1 d . . . . .
H22A H 0.9156 0.7669 0.7949 0.030 Uiso 1 1 calc R U . . .
H22B H 0.9107 0.7782 0.6836 0.030 Uiso 1 1 calc R U . . .
C11 C 0.69924(10) 0.49926(8) 0.60677(15) 0.0189(4) Uani 1 1 d D . . . .
C34 C 0.51343(11) 0.66146(10) 0.58386(14) 0.0247(4) Uani 1 1 d . . . . .
H34A H 0.5561 0.6389 0.5843 0.030 Uiso 1 1 calc R U . . .
H34B H 0.5258 0.6885 0.6417 0.030 Uiso 1 1 calc R U . . .
C38 C 0.52187(12) 0.61566(10) 0.38998(15) 0.0278(5) Uani 1 1 d . . . . .
H38A H 0.5266 0.5824 0.4381 0.033 Uiso 1 1 calc R U . . .
H38B H 0.5679 0.6355 0.4026 0.033 Uiso 1 1 calc R U . . .
C39 C 0.49801(14) 0.58934(11) 0.28640(17) 0.0377(6) Uani 1 1 d . . . . .
H39A H 0.4954 0.6222 0.2392 0.057 Uiso 1 1 calc R U . . .
H39B H 0.4519 0.5706 0.2737 0.057 Uiso 1 1 calc R U . . .
H39C H 0.5314 0.5584 0.2800 0.057 Uiso 1 1 calc R U . . .
C23 C 1.00630(11) 0.74502(10) 0.76558(15) 0.0270(5) Uani 1 1 d . . . . .
H23A H 1.0400 0.7530 0.8308 0.032 Uiso 1 1 calc R U . . .
H23B H 1.0286 0.7560 0.7156 0.032 Uiso 1 1 calc R U . . .
C25 C 0.88167(11) 0.88081(10) 0.76220(16) 0.0290(5) Uani 1 1 d . . . . .
H25A H 0.8595 0.8578 0.8038 0.035 Uiso 1 1 calc R U . . .
H25B H 0.8897 0.9230 0.7880 0.035 Uiso 1 1 calc R U . . .
C24 C 0.98623(13) 0.67749(10) 0.75626(18) 0.0333(5) Uani 1 1 d . . . . .
H24A H 0.9532 0.6698 0.6914 0.050 Uiso 1 1 calc R U . . .
H24B H 0.9646 0.6668 0.8063 0.050 Uiso 1 1 calc R U . . .
H24C H 1.0281 0.6526 0.7651 0.050 Uiso 1 1 calc R U . . .
C41 C 0.54343(12) 0.78638(12) 0.41352(19) 0.0384(6) Uani 1 1 d . . . . .
H41A H 0.5006 0.8104 0.4067 0.046 Uiso 1 1 calc R U . . .
H41B H 0.5380 0.7650 0.3511 0.046 Uiso 1 1 calc R U . . .
C32 C 0.43920(12) 0.78583(12) 0.57304(19) 0.0378(6) Uani 1 1 d . . . . .
H32A H 0.4820 0.8099 0.5801 0.045 Uiso 1 1 calc R U . . .
H32B H 0.4446 0.7641 0.6352 0.045 Uiso 1 1 calc R U . . .
C35 C 0.45982(12) 0.61557(10) 0.59449(16) 0.0299(5) Uani 1 1 d . . . . .
H35A H 0.4530 0.5835 0.5440 0.036 Uiso 1 1 calc R U . . .
H35B H 0.4146 0.6363 0.5850 0.036 Uiso 1 1 calc R U . . .
C20 C 0.98476(13) 0.83127(11) 0.95779(16) 0.0322(5) Uani 1 1 d . . . . .
H20A H 0.9845 0.7864 0.9487 0.039 Uiso 1 1 calc R U . . .
H20B H 0.9384 0.8439 0.9608 0.039 Uiso 1 1 calc R U . . .
C36 C 0.48465(14) 0.58654(12) 0.69612(18) 0.0410(6) Uani 1 1 d . . . . .
H36A H 0.4510 0.5555 0.7015 0.061 Uiso 1 1 calc R U . . .
H36B H 0.4886 0.6181 0.7458 0.061 Uiso 1 1 calc R U . . .
H36C H 0.5302 0.5674 0.7061 0.061 Uiso 1 1 calc R U . . .
C21 C 1.04114(14) 0.84931(12) 1.05176(16) 0.0378(6) Uani 1 1 d . . . . .
H21A H 1.0871 0.8448 1.0428 0.057 Uiso 1 1 calc R U . . .
H21B H 1.0382 0.8228 1.1052 0.057 Uiso 1 1 calc R U . . .
H21C H 1.0343 0.8919 1.0677 0.057 Uiso 1 1 calc R U . . .
O14 O 0.86599(14) 1.03513(11) 0.7252(3) 0.0945(10) Uani 1 1 d . . . . .
C29 C 0.99781(13) 0.94724(11) 0.70827(17) 0.0344(5) Uani 1 1 d . . . . .
H29A H 0.9534 0.9684 0.7025 0.041 Uiso 1 1 calc R U . . .
H29B H 1.0312 0.9571 0.7729 0.041 Uiso 1 1 calc R U . . .
C42 C 0.60663(12) 0.82895(11) 0.4371(2) 0.0409(6) Uani 1 1 d . . . . .
H42A H 0.6013 0.8575 0.3828 0.061 Uiso 1 1 calc R U . . .
H42B H 0.6491 0.8047 0.4468 0.061 Uiso 1 1 calc R U . . .
H42C H 0.6099 0.8519 0.4968 0.061 Uiso 1 1 calc R U . . .
C33 C 0.37596(13) 0.82837(11) 0.5500(2) 0.0413(6) Uani 1 1 d . . . . .
H33A H 0.3730 0.8521 0.4911 0.062 Uiso 1 1 calc R U . . .
H33B H 0.3809 0.8562 0.6050 0.062 Uiso 1 1 calc R U . . .
H33C H 0.3335 0.8040 0.5390 0.062 Uiso 1 1 calc R U . . .
C26 C 0.83106(13) 0.88333(12) 0.65957(19) 0.0416(6) Uani 1 1 d . . . . .
H26A H 0.8258 0.8421 0.6298 0.050 Uiso 1 1 calc R U . . .
H26B H 0.8492 0.9111 0.6189 0.050 Uiso 1 1 calc R U . . .
C27 C 0.76057(13) 0.90622(13) 0.6632(2) 0.0475(7) Uani 1 1 d . . . . .
H27A H 0.7288 0.9106 0.5965 0.071 Uiso 1 1 calc R U . . .
H27B H 0.7665 0.9459 0.6962 0.071 Uiso 1 1 calc R U . . .
H27C H 0.7411 0.8769 0.6991 0.071 Uiso 1 1 calc R U . . .
O13 O 0.6669(2) 0.49627(14) 0.9181(4) 0.1381(17) Uani 1 1 d . . . . .
C46 C 0.82517(15) 1.07375(13) 0.7300(2) 0.0513(7) Uani 1 1 d . . . . .
C43 C 0.7209(2) 0.49826(15) 0.8958(3) 0.0674(10) Uani 1 1 d . . . . .
C45 C 0.7481(2) 0.55780(15) 0.8741(3) 0.0671(9) Uani 1 1 d . . . . .
H45A H 0.7365 0.5628 0.8032 0.101 Uiso 1 1 calc R U . . .
H45B H 0.7988 0.5589 0.9039 0.101 Uiso 1 1 calc R U . . .
H45C H 0.7268 0.5910 0.9008 0.101 Uiso 1 1 calc R U . . .
C48 C 0.78564(18) 1.06807(15) 0.8022(2) 0.0621(8) Uani 1 1 d . . . . .
H48A H 0.7985 1.0298 0.8387 0.093 Uiso 1 1 calc R U . . .
H48B H 0.7355 1.0681 0.7676 0.093 Uiso 1 1 calc R U . . .
H48C H 0.7971 1.1026 0.8477 0.093 Uiso 1 1 calc R U . . .
C30 C 1.0263(2) 0.96913(15) 0.6289(3) 0.0736(11) Uani 1 1 d . . . . .
H30A H 0.9922 0.9611 0.5650 0.110 Uiso 1 1 calc R U . . .
H30B H 1.0697 0.9474 0.6338 0.110 Uiso 1 1 calc R U . . .
H30C H 1.0355 1.0131 0.6363 0.110 Uiso 1 1 calc R U . . .
C44 C 0.7589(2) 0.44115(17) 0.8835(3) 0.0785(11) Uani 1 1 d . . . . .
H44A H 0.7364 0.4056 0.9021 0.118 Uiso 1 1 calc R U . . .
H44B H 0.8074 0.4435 0.9252 0.118 Uiso 1 1 calc R U . . .
H44C H 0.7575 0.4372 0.8151 0.118 Uiso 1 1 calc R U . . .
C47 C 0.8137(2) 1.12906(17) 0.6667(3) 0.0748(10) Uani 1 1 d . . . . .
H47A H 0.8296 1.1653 0.7074 0.112 Uiso 1 1 calc R U . . .
H47B H 0.7640 1.1331 0.6311 0.112 Uiso 1 1 calc R U . . .
H47C H 0.8400 1.1251 0.6201 0.112 Uiso 1 1 calc R U . . .
F3 F 0.8912(11) 0.5031(9) 0.5485(16) 0.02240(14) Uani 0.08 1 d . . P D -2
F2 F 0.8805(13) 0.6902(17) 0.938(2) 0.02065(13) Uani 0.045 1 d D . P A -2
F5 F 0.9033(13) 0.3067(18) 0.946(3) 0.02270(14) Uani 0.045 1 d D . P B -2
F1 F 0.6318(12) 0.7986(18) 0.751(2) 0.02817(15) Uani 0.045 1 d D . P F -2
F6 F 0.6514(13) 0.2002(19) 0.765(3) 0.02739(15) Uani 0.045 1 d D . P E -2
F4 F 0.6371(11) 0.4945(13) 0.629(2) 0.02297(15) Uani 0.08 1 d D . P C -2
O15 O 0.4390(9) 1.0023(5) 0.4292(10) 0.250(8) Uani 0.5 1 d . . P G -3
O16 O 0.4841(5) 0.9268(9) 0.4766(10) 0.256(7) Uani 0.5 1 d . . P H 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
Fe2 O10 1.9963(13) 4_565 ?
Fe2 O12 1.9916(13) . ?
Fe2 O6 2.0866(13) . ?
Fe2 O9 2.0111(13) . ?
Fe2 O11 2.0105(13) 4_565 ?
Fe2 O7 2.0934(13) . ?
Fe1 O2 1.9892(13) . ?
Fe1 O4 1.9894(13) 4_575 ?
Fe1 O5 2.0774(13) . ?
Fe1 O3 2.0019(13) 4_575 ?
Fe1 O1 1.9973(13) . ?
Fe1 O8 2.0840(13) . ?
Cl2 C6 1.7341(18) . ?
Cl5 C14 1.7340(18) . ?
Cl4 C11 1.7337(19) . ?
Cl3 C8 1.744(2) . ?
Cl6 C17 1.7357(19) . ?
Cl1 C3 1.7342(19) . ?
Cl1 F1 0.50(3) . ?
O10 Fe2 1.9963(13) 4_566 ?
O10 C15 1.297(2) . ?
O12 C18 1.292(2) . ?
O2 C2 1.293(2) . ?
O4 Fe1 1.9895(13) 4_576 ?
O4 C5 1.299(2) . ?
O5 C7 1.257(2) . ?
O6 C9 1.261(2) . ?
O3 Fe1 2.0020(13) 4_576 ?
O3 C4 1.291(2) . ?
O9 C13 1.298(2) . ?
O11 Fe2 2.0104(13) 4_566 ?
O11 C16 1.295(2) . ?
O1 C1 1.291(2) . ?
O7 C10 1.262(2) . ?
O8 C12 1.260(2) . ?
N2 C40 1.524(3) . ?
N2 C31 1.523(3) . ?
N2 C37 1.522(2) . ?
N2 C34 1.520(3) . ?
N1 C19 1.515(3) . ?
N1 C28 1.519(3) . ?
N1 C22 1.528(3) . ?
N1 C25 1.525(3) . ?
C1 C2 1.475(3) . ?
C1 C6 1.397(3) . ?
C5 C4 1.471(3) . ?
C5 C6 1.392(3) . ?
C2 C3 1.389(3) . ?
C15 C16 1.471(3) . ?
C15 C14 1.396(3) . ?
C9 C10 1.542(3) . ?
C9 C8 1.393(3) . ?
C4 C3 1.392(3) . ?
C18 C13 1.477(3) . ?
C18 C17 1.394(3) . ?
C7 C12 1.542(3) . ?
C7 C8 1.391(3) . ?
C16 C17 1.393(3) . ?
C13 C14 1.396(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.513(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.511(3) . ?
C3 F1 1.317(18) . ?
C10 C11 1.389(3) . ?
C6 F2 1.302(18) . ?
C17 F6 1.314(18) . ?
C12 C11 1.384(3) . ?
C8 F3 1.310(19) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.512(3) . ?
C14 F5 1.305(18) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.520(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.518(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.521(3) . ?
C11 F4 1.390(16) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.518(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.531(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.528(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.516(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.531(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.531(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.531(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.526(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
O14 C46 1.197(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.507(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.524(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O13 C43 1.229(5) . ?
C46 C48 1.499(4) . ?
C46 C47 1.490(4) . ?
C43 C45 1.485(4) . ?
C43 C44 1.505(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 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
O10 Fe2 O6 92.40(5) 4_565 . ?
O10 Fe2 O9 98.77(5) 4_565 . ?
O10 Fe2 O11 80.22(5) 4_565 4_565 ?
O10 Fe2 O7 161.46(5) 4_565 . ?
O12 Fe2 O10 103.66(6) . 4_565 ?
O12 Fe2 O6 162.27(5) . . ?
O12 Fe2 O9 80.33(5) . . ?
O12 Fe2 O11 96.57(5) . 4_565 ?
O12 Fe2 O7 89.26(5) . . ?
O6 Fe2 O7 77.04(5) . . ?
O9 Fe2 O6 89.97(5) . . ?
O9 Fe2 O7 96.46(5) . . ?
O11 Fe2 O6 93.47(5) 4_565 . ?
O11 Fe2 O9 176.45(5) 4_565 . ?
O11 Fe2 O7 85.19(5) 4_565 . ?
O2 Fe1 O4 101.61(6) . 4_575 ?
O2 Fe1 O5 165.12(5) . . ?
O2 Fe1 O3 96.82(5) . 4_575 ?
O2 Fe1 O1 80.69(5) . . ?
O2 Fe1 O8 92.31(5) . . ?
O4 Fe1 O5 90.52(5) 4_575 . ?
O4 Fe1 O3 80.98(5) 4_575 4_575 ?
O4 Fe1 O1 100.64(5) 4_575 . ?
O4 Fe1 O8 161.59(5) 4_575 . ?
O5 Fe1 O8 77.87(5) . . ?
O3 Fe1 O5 93.55(5) 4_575 . ?
O3 Fe1 O8 85.48(5) 4_575 . ?
O1 Fe1 O5 88.67(5) . . ?
O1 Fe1 O3 177.24(5) . 4_575 ?
O1 Fe1 O8 93.41(5) . . ?
F1 Cl1 C3 29(4) . . ?
C15 O10 Fe2 114.80(12) . 4_566 ?
C18 O12 Fe2 114.78(11) . . ?
C2 O2 Fe1 114.32(12) . . ?
C5 O4 Fe1 113.71(11) . 4_576 ?
C7 O5 Fe1 115.97(12) . . ?
C9 O6 Fe2 116.81(12) . . ?
C4 O3 Fe1 113.38(12) . 4_576 ?
C13 O9 Fe2 114.19(11) . . ?
C16 O11 Fe2 113.95(12) . 4_566 ?
C1 O1 Fe1 114.21(11) . . ?
C10 O7 Fe2 116.39(11) . . ?
C12 O8 Fe1 115.51(12) . . ?
C31 N2 C40 111.29(16) . . ?
C37 N2 C40 111.01(15) . . ?
C37 N2 C31 106.16(15) . . ?
C34 N2 C40 106.32(15) . . ?
C34 N2 C31 111.09(15) . . ?
C34 N2 C37 111.05(17) . . ?
C19 N1 C28 107.78(15) . . ?
C19 N1 C22 111.02(16) . . ?
C19 N1 C25 109.17(15) . . ?
C28 N1 C22 108.71(15) . . ?
C28 N1 C25 111.91(16) . . ?
C25 N1 C22 108.28(15) . . ?
O1 C1 C2 115.23(15) . . ?
O1 C1 C6 125.12(17) . . ?
C6 C1 C2 119.64(16) . . ?
O4 C5 C4 115.51(16) . . ?
O4 C5 C6 124.83(17) . . ?
C6 C5 C4 119.65(16) . . ?
O2 C2 C1 115.43(16) . . ?
O2 C2 C3 125.08(17) . . ?
C3 C2 C1 119.49(16) . . ?
O10 C15 C16 115.01(16) . . ?
O10 C15 C14 125.29(17) . . ?
C14 C15 C16 119.70(16) . . ?
O6 C9 C10 114.76(16) . . ?
O6 C9 C8 126.17(17) . . ?
C8 C9 C10 119.07(16) . . ?
O3 C4 C5 115.75(16) . . ?
O3 C4 C3 124.52(17) . . ?
C3 C4 C5 119.72(16) . . ?
O12 C18 C13 115.54(16) . . ?
O12 C18 C17 124.91(17) . . ?
C17 C18 C13 119.54(16) . . ?
O5 C7 C12 115.14(16) . . ?
O5 C7 C8 125.31(17) . . ?
C8 C7 C12 119.55(17) . . ?
O11 C16 C15 115.73(16) . . ?
O11 C16 C17 124.63(17) . . ?
C17 C16 C15 119.64(16) . . ?
O9 C13 C18 114.97(16) . . ?
O9 C13 C14 125.50(17) . . ?
C14 C13 C18 119.53(16) . . ?
N2 C40 H40A 108.2 . . ?
N2 C40 H40B 108.2 . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 N2 116.20(17) . . ?
C41 C40 H40A 108.2 . . ?
C41 C40 H40B 108.2 . . ?
N2 C31 H31A 108.2 . . ?
N2 C31 H31B 108.2 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 N2 116.15(17) . . ?
C32 C31 H31A 108.2 . . ?
C32 C31 H31B 108.2 . . ?
C2 C3 Cl1 120.00(14) . . ?
C2 C3 C4 120.90(17) . . ?
C4 C3 Cl1 119.10(15) . . ?
F1 C3 Cl1 10.6(18) . . ?
F1 C3 C2 116.6(16) . . ?
F1 C3 C4 121.5(16) . . ?
O7 C10 C9 114.98(16) . . ?
O7 C10 C11 125.51(17) . . ?
C11 C10 C9 119.51(17) . . ?
C1 C6 Cl2 119.64(14) . . ?
C5 C6 Cl2 119.79(14) . . ?
C5 C6 C1 120.57(17) . . ?
F2 C6 Cl2 6.2(18) . . ?
F2 C6 C1 123.2(16) . . ?
F2 C6 C5 116.0(17) . . ?
C18 C17 Cl6 120.03(14) . . ?
C16 C17 Cl6 119.07(14) . . ?
C16 C17 C18 120.89(17) . . ?
F6 C17 Cl6 7(2) . . ?
F6 C17 C18 118.5(17) . . ?
F6 C17 C16 120.3(17) . . ?
O8 C12 C7 115.35(16) . . ?
O8 C12 C11 125.44(17) . . ?
C11 C12 C7 119.21(17) . . ?
C9 C8 Cl3 120.73(14) . . ?
C7 C8 Cl3 118.23(14) . . ?
C7 C8 C9 121.02(18) . . ?
F3 C8 Cl3 6.4(9) . . ?
F3 C8 C9 116.3(9) . . ?
F3 C8 C7 122.4(9) . . ?
N1 C19 H19A 107.9 . . ?
N1 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C20 C19 N1 117.57(18) . . ?
C20 C19 H19A 107.9 . . ?
C20 C19 H19B 107.9 . . ?
C15 C14 Cl5 119.27(14) . . ?
C13 C14 Cl5 120.06(14) . . ?
C13 C14 C15 120.66(17) . . ?
F5 C14 Cl5 5.4(19) . . ?
F5 C14 C15 119.8(17) . . ?
F5 C14 C13 119.1(17) . . ?
N2 C37 H37A 108.3 . . ?
N2 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 N2 115.81(17) . . ?
C38 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
N1 C28 H28A 108.5 . . ?
N1 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 N1 115.29(17) . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
N1 C22 H22A 108.2 . . ?
N1 C22 H22B 108.2 . . ?
H22A C22 H22B 107.3 . . ?
C23 C22 N1 116.54(16) . . ?
C23 C22 H22A 108.2 . . ?
C23 C22 H22B 108.2 . . ?
C10 C11 Cl4 119.79(15) . . ?
C10 C11 F4 117.0(12) . . ?
C12 C11 Cl4 118.80(14) . . ?
C12 C11 C10 121.37(18) . . ?
C12 C11 F4 121.4(12) . . ?
F4 C11 Cl4 3.4(13) . . ?
N2 C34 H34A 108.3 . . ?
N2 C34 H34B 108.3 . . ?
H34A C34 H34B 107.4 . . ?
C35 C34 N2 115.81(17) . . ?
C35 C34 H34A 108.3 . . ?
C35 C34 H34B 108.3 . . ?
C37 C38 H38A 109.8 . . ?
C37 C38 H38B 109.8 . . ?
C37 C38 C39 109.44(19) . . ?
H38A C38 H38B 108.2 . . ?
C39 C38 H38A 109.8 . . ?
C39 C38 H38B 109.8 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C22 C23 C24 109.17(17) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
N1 C25 H25A 108.4 . . ?
N1 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 N1 115.70(18) . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C40 C41 H41A 109.9 . . ?
C40 C41 H41B 109.9 . . ?
C40 C41 C42 109.0(2) . . ?
H41A C41 H41B 108.3 . . ?
C42 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
C31 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C31 C32 C33 108.9(2) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.9 . . ?
C33 C32 H32B 109.9 . . ?
C34 C35 H35A 109.7 . . ?
C34 C35 H35B 109.7 . . ?
C34 C35 C36 109.8(2) . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
C19 C20 H20A 110.2 . . ?
C19 C20 H20B 110.2 . . ?
C19 C20 C21 107.59(19) . . ?
H20A C20 H20B 108.5 . . ?
C21 C20 H20A 110.2 . . ?
C21 C20 H20B 110.2 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C28 C29 H29A 109.6 . . ?
C28 C29 H29B 109.6 . . ?
H29A C29 H29B 108.1 . . ?
C30 C29 C28 110.2(2) . . ?
C30 C29 H29A 109.6 . . ?
C30 C29 H29B 109.6 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
C25 C26 C27 109.5(2) . . ?
H26A C26 H26B 108.2 . . ?
C27 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O14 C46 C48 120.3(3) . . ?
O14 C46 C47 121.2(3) . . ?
C47 C46 C48 118.5(3) . . ?
O13 C43 C45 120.1(4) . . ?
O13 C43 C44 121.7(3) . . ?
C45 C43 C44 118.1(3) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Cl1 F1 C3 141(6) . . ?

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
Fe2 O10 C15 C16 2.3(2) 4_566 . . . ?
Fe2 O10 C15 C14 -177.68(15) 4_566 . . . ?
Fe2 O12 C18 C13 -3.6(2) . . . . ?
Fe2 O12 C18 C17 177.67(15) . . . . ?
Fe2 O6 C9 C10 0.8(2) . . . . ?
Fe2 O6 C9 C8 -178.97(15) . . . . ?
Fe2 O9 C13 C18 2.86(19) . . . . ?
Fe2 O9 C13 C14 -177.81(15) . . . . ?
Fe2 O11 C16 C15 -5.2(2) 4_566 . . . ?
Fe2 O11 C16 C17 174.76(15) 4_566 . . . ?
Fe2 O7 C10 C9 -0.8(2) . . . . ?
Fe2 O7 C10 C11 179.67(15) . . . . ?
Fe1 O2 C2 C1 2.1(2) . . . . ?
Fe1 O2 C2 C3 -178.28(15) . . . . ?
Fe1 O4 C5 C4 -4.81(19) 4_576 . . . ?
Fe1 O4 C5 C6 176.31(15) 4_576 . . . ?
Fe1 O5 C7 C12 3.21(19) . . . . ?
Fe1 O5 C7 C8 -177.09(15) . . . . ?
Fe1 O3 C4 C5 6.9(2) 4_576 . . . ?
Fe1 O3 C4 C3 -173.97(16) 4_576 . . . ?
Fe1 O1 C1 C2 -2.88(19) . . . . ?
Fe1 O1 C1 C6 178.12(15) . . . . ?
Fe1 O8 C12 C7 -2.77(19) . . . . ?
Fe1 O8 C12 C11 177.03(15) . . . . ?
O10 C15 C16 O11 2.0(2) . . . . ?
O10 C15 C16 C17 -177.94(17) . . . . ?
O10 C15 C14 Cl5 -1.4(3) . . . . ?
O10 C15 C14 C13 177.39(17) . . . . ?
O10 C15 C14 F5 5(2) . . . . ?
O12 C18 C13 O9 0.4(2) . . . . ?
O12 C18 C13 C14 -178.93(16) . . . . ?
O12 C18 C17 Cl6 -0.4(3) . . . . ?
O12 C18 C17 C16 178.29(18) . . . . ?
O12 C18 C17 F6 -8(2) . . . . ?
O2 C2 C3 Cl1 0.7(3) . . . . ?
O2 C2 C3 C4 -178.93(18) . . . . ?
O2 C2 C3 F1 12(2) . . . . ?
O4 C5 C4 O3 -1.5(2) . . . . ?
O4 C5 C4 C3 179.36(17) . . . . ?
O4 C5 C6 Cl2 0.8(3) . . . . ?
O4 C5 C6 C1 -178.83(17) . . . . ?
O4 C5 C6 F2 -5(2) . . . . ?
O5 C7 C12 O8 -0.3(2) . . . . ?
O5 C7 C12 C11 179.91(17) . . . . ?
O5 C7 C8 Cl3 -2.7(3) . . . . ?
O5 C7 C8 C9 175.82(17) . . . . ?
O5 C7 C8 F3 3.0(12) . . . . ?
O6 C9 C10 O7 -0.1(2) . . . . ?
O6 C9 C10 C11 179.56(17) . . . . ?
O6 C9 C8 Cl3 2.9(3) . . . . ?
O6 C9 C8 C7 -175.52(18) . . . . ?
O6 C9 C8 F3 -2.3(12) . . . . ?
O3 C4 C3 Cl1 1.4(3) . . . . ?
O3 C4 C3 C2 -178.93(18) . . . . ?
O3 C4 C3 F1 -11(2) . . . . ?
O9 C13 C14 Cl5 1.0(3) . . . . ?
O9 C13 C14 C15 -177.70(17) . . . . ?
O9 C13 C14 F5 -5(2) . . . . ?
O11 C16 C17 Cl6 -1.7(3) . . . . ?
O11 C16 C17 C18 179.53(18) . . . . ?
O11 C16 C17 F6 6(2) . . . . ?
O1 C1 C2 O2 0.5(2) . . . . ?
O1 C1 C2 C3 -179.11(17) . . . . ?
O1 C1 C6 Cl2 -2.1(3) . . . . ?
O1 C1 C6 C5 177.48(17) . . . . ?
O1 C1 C6 F2 4(2) . . . . ?
O7 C10 C11 Cl4 -1.5(3) . . . . ?
O7 C10 C11 C12 175.88(18) . . . . ?
O7 C10 C11 F4 0.7(15) . . . . ?
O8 C12 C11 Cl4 1.6(3) . . . . ?
O8 C12 C11 C10 -175.90(17) . . . . ?
O8 C12 C11 F4 -0.9(16) . . . . ?
N2 C40 C41 C42 170.05(19) . . . . ?
N2 C31 C32 C33 170.14(19) . . . . ?
N2 C37 C38 C39 -168.89(17) . . . . ?
N2 C34 C35 C36 -170.96(17) . . . . ?
N1 C19 C20 C21 179.41(18) . . . . ?
N1 C28 C29 C30 -175.9(2) . . . . ?
N1 C22 C23 C24 172.12(17) . . . . ?
N1 C25 C26 C27 173.2(2) . . . . ?
C1 C2 C3 Cl1 -179.65(14) . . . . ?
C1 C2 C3 C4 0.7(3) . . . . ?
C1 C2 C3 F1 -168(2) . . . . ?
C5 C4 C3 Cl1 -179.51(14) . . . . ?
C5 C4 C3 C2 0.2(3) . . . . ?
C5 C4 C3 F1 169(2) . . . . ?
C2 C1 C6 Cl2 178.92(14) . . . . ?
C2 C1 C6 C5 -1.5(3) . . . . ?
C2 C1 C6 F2 -175(2) . . . . ?
C2 C3 F1 Cl1 -111(8) . . . . ?
C15 C16 C17 Cl6 178.22(14) . . . . ?
C15 C16 C17 C18 -0.5(3) . . . . ?
C15 C16 C17 F6 -174(2) . . . . ?
C9 C10 C11 Cl4 178.89(14) . . . . ?
C9 C10 C11 C12 -3.7(3) . . . . ?
C9 C10 C11 F4 -178.9(15) . . . . ?
C4 C5 C6 Cl2 -178.07(14) . . . . ?
C4 C5 C6 C1 2.3(3) . . . . ?
C4 C5 C6 F2 176(2) . . . . ?
C4 C3 F1 Cl1 80(9) . . . . ?
C18 C13 C14 Cl5 -179.66(14) . . . . ?
C18 C13 C14 C15 1.6(3) . . . . ?
C18 C13 C14 F5 174(2) . . . . ?
C7 C12 C11 Cl4 -178.66(13) . . . . ?
C7 C12 C11 C10 3.9(3) . . . . ?
C7 C12 C11 F4 178.9(15) . . . . ?
C16 C15 C14 Cl5 178.72(14) . . . . ?
C16 C15 C14 C13 -2.5(3) . . . . ?
C16 C15 C14 F5 -175(2) . . . . ?
C13 C18 C17 Cl6 -179.14(14) . . . . ?
C13 C18 C17 C16 -0.4(3) . . . . ?
C13 C18 C17 F6 173(2) . . . . ?
C40 N2 C31 C32 -56.0(2) . . . . ?
C40 N2 C37 C38 62.8(2) . . . . ?
C40 N2 C34 C35 -176.88(17) . . . . ?
C31 N2 C40 C41 -56.1(2) . . . . ?
C31 N2 C37 C38 -176.10(17) . . . . ?
C31 N2 C34 C35 61.9(2) . . . . ?
C10 C9 C8 Cl3 -176.87(13) . . . . ?
C10 C9 C8 C7 4.7(3) . . . . ?
C10 C9 C8 F3 177.9(11) . . . . ?
C6 C1 C2 O2 179.59(16) . . . . ?
C6 C1 C2 C3 -0.1(3) . . . . ?
C6 C5 C4 O3 177.48(17) . . . . ?
C6 C5 C4 C3 -1.7(3) . . . . ?
C17 C18 C13 O9 179.28(17) . . . . ?
C17 C18 C13 C14 -0.1(3) . . . . ?
C12 C7 C8 Cl3 177.02(13) . . . . ?
C12 C7 C8 C9 -4.5(3) . . . . ?
C12 C7 C8 F3 -177.3(12) . . . . ?
C8 C9 C10 O7 179.77(16) . . . . ?
C8 C9 C10 C11 -0.6(3) . . . . ?
C8 C7 C12 O8 180.00(17) . . . . ?
C8 C7 C12 C11 0.2(3) . . . . ?
C19 N1 C28 C29 -61.7(2) . . . . ?
C19 N1 C22 C23 -55.6(2) . . . . ?
C19 N1 C25 C26 169.64(19) . . . . ?
C14 C15 C16 O11 -178.04(17) . . . . ?
C14 C15 C16 C17 2.0(3) . . . . ?
C37 N2 C40 C41 62.0(2) . . . . ?
C37 N2 C31 C32 -176.92(19) . . . . ?
C37 N2 C34 C35 -56.0(2) . . . . ?
C28 N1 C19 C20 -170.03(19) . . . . ?
C28 N1 C22 C23 62.8(2) . . . . ?
C28 N1 C25 C26 50.4(2) . . . . ?
C22 N1 C19 C20 -51.1(2) . . . . ?
C22 N1 C28 C29 177.87(18) . . . . ?
C22 N1 C25 C26 -69.4(2) . . . . ?
C34 N2 C40 C41 -177.15(19) . . . . ?
C34 N2 C31 C32 62.2(2) . . . . ?
C34 N2 C37 C38 -55.2(2) . . . . ?
C25 N1 C19 C20 68.2(2) . . . . ?
C25 N1 C28 C29 58.3(2) . . . . ?
C25 N1 C22 C23 -175.39(17) . . . . ?
F1 Cl1 C3 C2 74(9) . . . . ?
F1 Cl1 C3 C4 -106(9) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.507
_oxdiff_exptl_absorpt_empirical_full_min 0.566
####################################################################### 
# 
# 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_F-024-d_CCDC-2014815_R1
_database_code_depnum_ccdc_archive 'CCDC 2014815'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-28
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl4.55 F1.45 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl4.55 F1.45 Fe2 N2 O12'
_chemical_formula_weight         1081.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl4.55 F1.45 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.5632(6)
_cell_length_b                   21.1362(10)
_cell_length_c                   12.2412(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.998(6)
_cell_angle_gamma                90
_cell_volume                     2682.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8645
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.6900
_cell_measurement_theta_min      2.1880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1121
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.067
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21209
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.528
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0613208000
_diffrn_orient_matrix_UB_12      0.0134784000
_diffrn_orient_matrix_UB_13      0.0008995000
_diffrn_orient_matrix_UB_21      -0.0079579000
_diffrn_orient_matrix_UB_22      -0.0209376000
_diffrn_orient_matrix_UB_23      0.0434071000
_diffrn_orient_matrix_UB_31      0.0293273000
_diffrn_orient_matrix_UB_32      0.0224759000
_diffrn_orient_matrix_UB_33      0.0399934000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4476
_reflns_number_total             6006
_reflns_odcompleteness_completeness 86.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.90
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6006
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0588
_refine_ls_restrained_S_all      1.089
_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)+(0.0619P)²+4.3107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1597
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-F1
 1.33 with sigma of 0.02
 C6-F2
 1.4 with sigma of 0.02
3. Rigid bond restraints
 F2, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F2 \\sim Cl2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5. Others
 Fixed Sof: Cl1(0.76583) Cl2(0.76583) Cl3(0.74324) F2(0.23417) F3(0.25676)
 F1(0.23417)
6.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C10(H10A,H10B), C20(H20A,H20B), C16(H16A,H16B), C13(H13A,
 H13B), C17(H17A,H17B), C11(H11A,H11B), C14(H14A,H14B)
6.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.04539(5) 0.31408(2) 0.49000(4) 0.03585(16) Uani 1 1 d . . . . .
Cl1 Cl 0.6658(3) 0.17036(14) 0.4049(2) 0.0454(5) Uani 0.7658 1 d . . P A 2
Cl2 Cl 0.9386(3) 0.32474(10) 0.07323(19) 0.0439(4) Uani 0.7658 1 d . U P B 2
Cl3 Cl 1.3015(2) 0.51881(12) 0.5141(2) 0.0472(5) Uani 0.7432 1 d . . P C 2
O5 O 1.1483(2) 0.39782(11) 0.4886(2) 0.0395(6) Uani 1 1 d . . . . .
O4 O 0.7006(2) 0.24123(11) 0.01908(18) 0.0385(6) Uani 1 1 d . . . . .
O1 O 1.0170(2) 0.31393(10) 0.32380(19) 0.0354(5) Uani 1 1 d . . . . .
O3 O 0.5817(2) 0.18422(11) 0.15613(19) 0.0379(5) Uani 1 1 d . . . . .
O6 O 1.0978(2) 0.61737(11) 0.5103(2) 0.0395(6) Uani 1 1 d . . . . .
O2 O 0.9041(2) 0.25060(11) 0.46042(19) 0.0377(5) Uani 1 1 d . . . . .
N00B N 0.3975(3) 0.35856(15) 0.2577(3) 0.0465(8) Uani 1 1 d . . . . .
C4 C 0.6866(3) 0.21256(15) 0.2013(3) 0.0332(7) Uani 1 1 d . . . . .
C9 C 1.0593(3) 0.56096(16) 0.5063(3) 0.0363(7) Uani 1 1 d . . . . .
C3 C 0.7393(3) 0.21322(15) 0.3152(3) 0.0347(7) Uani 1 1 d D . . . .
C5 C 0.7538(3) 0.24691(15) 0.1236(3) 0.0343(7) Uani 1 1 d . . . . .
C7 C 1.0857(3) 0.44761(16) 0.4954(3) 0.0359(7) Uani 1 1 d . . . . .
C2 C 0.8501(3) 0.24732(15) 0.3562(3) 0.0331(7) Uani 1 1 d . . . . .
C1 C 0.9149(3) 0.28334(15) 0.2781(3) 0.0336(7) Uani 1 1 d . . . . .
C6 C 0.8637(3) 0.28182(16) 0.1645(3) 0.0347(7) Uani 1 1 d D . . . .
C8 C 1.1367(3) 0.50832(17) 0.5040(3) 0.0394(8) Uani 1 1 d . . . . .
C19 C 0.3975(4) 0.28829(19) 0.2337(4) 0.0504(9) Uani 1 1 d . . . . .
H19A H 0.4809 0.2705 0.2721 0.060 Uiso 1 1 calc R U . . .
H19B H 0.3928 0.2825 0.1528 0.060 Uiso 1 1 calc R U . . .
C10 C 0.2718(4) 0.3873(2) 0.1949(4) 0.0587(11) Uani 1 1 d . . . . .
H10A H 0.2608 0.3745 0.1158 0.070 Uiso 1 1 calc R U . . .
H10B H 0.1995 0.3687 0.2248 0.070 Uiso 1 1 calc R U . . .
C20 C 0.2898(4) 0.2500(2) 0.2678(3) 0.0518(10) Uani 1 1 d . . . . .
H20A H 0.2062 0.2626 0.2216 0.062 Uiso 1 1 calc R U . . .
H20B H 0.2864 0.2591 0.3465 0.062 Uiso 1 1 calc R U . . .
C16 C 0.4034(4) 0.3710(2) 0.3816(3) 0.0526(10) Uani 1 1 d . . . . .
H16A H 0.4155 0.4170 0.3947 0.063 Uiso 1 1 calc R U . . .
H16B H 0.3188 0.3596 0.3994 0.063 Uiso 1 1 calc R U . . .
C13 C 0.5152(5) 0.3882(2) 0.2237(4) 0.0621(12) Uani 1 1 d . . . . .
H13A H 0.5927 0.3653 0.2623 0.075 Uiso 1 1 calc R U . . .
H13B H 0.5224 0.4325 0.2506 0.075 Uiso 1 1 calc R U . . .
C17 C 0.5073(5) 0.3365(2) 0.4626(4) 0.0614(12) Uani 1 1 d . . . . .
H17A H 0.5933 0.3459 0.4456 0.074 Uiso 1 1 calc R U . . .
H17B H 0.4929 0.2903 0.4568 0.074 Uiso 1 1 calc R U . . .
C21 C 0.3110(4) 0.1796(2) 0.2540(4) 0.0628(12) Uani 1 1 d . . . . .
H21A H 0.3072 0.1700 0.1751 0.094 Uiso 1 1 calc R U . . .
H21B H 0.2438 0.1557 0.2812 0.094 Uiso 1 1 calc R U . . .
H21C H 0.3958 0.1675 0.2966 0.094 Uiso 1 1 calc R U . . .
C11 C 0.2613(5) 0.4588(2) 0.1998(4) 0.0737(14) Uani 1 1 d . . . . .
H11A H 0.3316 0.4785 0.1685 0.088 Uiso 1 1 calc R U . . .
H11B H 0.2701 0.4726 0.2782 0.088 Uiso 1 1 calc R U . . .
C18 C 0.5004(5) 0.3595(2) 0.5808(4) 0.0712(14) Uani 1 1 d . . . . .
H18A H 0.4110 0.3574 0.5917 0.107 Uiso 1 1 calc R U . . .
H18B H 0.5313 0.4032 0.5903 0.107 Uiso 1 1 calc R U . . .
H18C H 0.5546 0.3324 0.6357 0.107 Uiso 1 1 calc R U . . .
C14 C 0.5166(6) 0.3886(2) 0.0994(5) 0.0789(16) Uani 1 1 d . . . . .
H14A H 0.4387 0.4103 0.0587 0.095 Uiso 1 1 calc R U . . .
H14B H 0.5160 0.3446 0.0715 0.095 Uiso 1 1 calc R U . . .
C15 C 0.6379(7) 0.4228(3) 0.0789(6) 0.105(2) Uani 1 1 d . . . . .
H15A H 0.6472 0.4164 0.0015 0.158 Uiso 1 1 calc R U . . .
H15B H 0.7137 0.4058 0.1290 0.158 Uiso 1 1 calc R U . . .
H15C H 0.6302 0.4682 0.0931 0.158 Uiso 1 1 calc R U . . .
C12 C 0.1309(7) 0.4800(3) 0.1335(7) 0.121(3) Uani 1 1 d . . . . .
H12A H 0.1236 0.4674 0.0555 0.181 Uiso 1 1 calc R U . . .
H12B H 0.1236 0.5261 0.1380 0.181 Uiso 1 1 calc R U . . .
H12C H 0.0616 0.4600 0.1643 0.181 Uiso 1 1 calc R U . . .
F2 F 0.926(2) 0.3059(8) 0.0917(15) 0.054(5) Uani 0.2342 1 d D U P B -2
F3 F 1.2627(17) 0.5138(10) 0.4866(17) 0.077(6) Uani 0.2568 1 d . . P C -2
F1 F 0.671(3) 0.1864(11) 0.389(2) 0.081(8) Uani 0.2342 1 d D . P A -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O5 2.079(2) . ?
Fe1 O4 1.990(2) 4_666 ?
Fe1 O1 1.999(2) . ?
Fe1 O3 1.997(2) 4_666 ?
Fe1 O6 2.094(2) 3_766 ?
Fe1 O2 1.988(2) . ?
Cl1 C3 1.719(4) . ?
Cl2 C6 1.742(4) . ?
Cl3 C8 1.735(4) . ?
O5 C7 1.254(4) . ?
O4 Fe1 1.990(2) 4_565 ?
O4 C5 1.301(4) . ?
O1 C1 1.290(4) . ?
O3 Fe1 1.997(2) 4_565 ?
O3 C4 1.287(4) . ?
O6 Fe1 2.094(2) 3_766 ?
O6 C9 1.258(4) . ?
O2 C2 1.296(4) . ?
N00B C19 1.514(5) . ?
N00B C10 1.527(5) . ?
N00B C16 1.528(5) . ?
N00B C13 1.520(5) . ?
C4 C3 1.399(5) . ?
C4 C5 1.481(5) . ?
C9 C7 1.538(5) 3_766 ?
C9 C8 1.384(5) . ?
C3 C2 1.385(5) . ?
C3 F1 1.377(15) . ?
C5 C6 1.386(5) . ?
C7 C9 1.538(5) 3_766 ?
C7 C8 1.388(5) . ?
C2 C1 1.487(5) . ?
C1 C6 1.393(5) . ?
C6 F2 1.306(12) . ?
C8 F3 1.39(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.518(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.517(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.520(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.518(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.525(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.541(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.527(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.533(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
O5 Fe1 O6 77.87(9) . 3_766 ?
O4 Fe1 O5 94.99(10) 4_666 . ?
O4 Fe1 O1 98.03(9) 4_666 . ?
O4 Fe1 O3 80.59(9) 4_666 4_666 ?
O4 Fe1 O6 167.73(10) 4_666 3_766 ?
O1 Fe1 O5 88.28(9) . . ?
O1 Fe1 O6 91.77(10) . 3_766 ?
O3 Fe1 O5 89.65(10) 4_666 . ?
O3 Fe1 O1 177.41(10) 4_666 . ?
O3 Fe1 O6 89.32(10) 4_666 3_766 ?
O2 Fe1 O5 161.56(10) . . ?
O2 Fe1 O4 101.57(10) . 4_666 ?
O2 Fe1 O1 81.48(9) . . ?
O2 Fe1 O3 100.92(10) . 4_666 ?
O2 Fe1 O6 87.11(10) . 3_766 ?
C7 O5 Fe1 115.5(2) . . ?
C5 O4 Fe1 114.6(2) . 4_565 ?
C1 O1 Fe1 113.1(2) . . ?
C4 O3 Fe1 114.3(2) . 4_565 ?
C9 O6 Fe1 115.3(2) . 3_766 ?
C2 O2 Fe1 112.9(2) . . ?
C19 N00B C10 108.9(3) . . ?
C19 N00B C16 111.1(3) . . ?
C19 N00B C13 108.7(3) . . ?
C10 N00B C16 107.4(3) . . ?
C13 N00B C10 112.1(3) . . ?
C13 N00B C16 108.7(3) . . ?
O3 C4 C3 125.4(3) . . ?
O3 C4 C5 115.5(3) . . ?
C3 C4 C5 119.1(3) . . ?
O6 C9 C7 115.2(3) . 3_766 ?
O6 C9 C8 125.1(3) . . ?
C8 C9 C7 119.7(3) . 3_766 ?
C4 C3 Cl1 119.3(3) . . ?
C2 C3 Cl1 119.7(3) . . ?
C2 C3 C4 121.0(3) . . ?
F1 C3 Cl1 7.9(11) . . ?
F1 C3 C4 119.3(12) . . ?
F1 C3 C2 119.1(12) . . ?
O4 C5 C4 114.6(3) . . ?
O4 C5 C6 125.4(3) . . ?
C6 C5 C4 120.0(3) . . ?
O5 C7 C9 115.9(3) . 3_766 ?
O5 C7 C8 125.3(3) . . ?
C8 C7 C9 118.8(3) . 3_766 ?
O2 C2 C3 124.6(3) . . ?
O2 C2 C1 115.8(3) . . ?
C3 C2 C1 119.6(3) . . ?
O1 C1 C2 115.3(3) . . ?
O1 C1 C6 125.3(3) . . ?
C6 C1 C2 119.4(3) . . ?
C5 C6 Cl2 119.8(3) . . ?
C5 C6 C1 120.8(3) . . ?
C1 C6 Cl2 119.4(3) . . ?
F2 C6 Cl2 8.5(9) . . ?
F2 C6 C5 117.0(9) . . ?
F2 C6 C1 121.5(10) . . ?
C9 C8 Cl3 119.0(3) . . ?
C9 C8 C7 121.5(3) . . ?
C9 C8 F3 121.5(10) . . ?
C7 C8 Cl3 119.6(3) . . ?
C7 C8 F3 115.7(9) . . ?
F3 C8 Cl3 12.9(8) . . ?
N00B C19 H19A 108.2 . . ?
N00B C19 H19B 108.2 . . ?
N00B C19 C20 116.2(3) . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
N00B C10 H10A 108.3 . . ?
N00B C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N00B 116.1(4) . . ?
C11 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 C21 110.9(3) . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
N00B C16 H16A 108.0 . . ?
N00B C16 H16B 108.0 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N00B 117.0(3) . . ?
C17 C16 H16A 108.0 . . ?
C17 C16 H16B 108.0 . . ?
N00B C13 H13A 108.3 . . ?
N00B C13 H13B 108.3 . . ?
N00B C13 C14 116.1(4) . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
C16 C17 H17A 110.2 . . ?
C16 C17 H17B 110.2 . . ?
C16 C17 C18 107.8(4) . . ?
H17A C17 H17B 108.5 . . ?
C18 C17 H17A 110.2 . . ?
C18 C17 H17B 110.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
C10 C11 C12 109.7(5) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C13 C14 C15 109.4(5) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 O5 C7 C9 -5.0(4) . . . 3_766 ?
Fe1 O5 C7 C8 175.1(3) . . . . ?
Fe1 O4 C5 C4 -1.6(4) 4_565 . . . ?
Fe1 O4 C5 C6 178.9(3) 4_565 . . . ?
Fe1 O1 C1 C2 -8.2(3) . . . . ?
Fe1 O1 C1 C6 172.0(3) . . . . ?
Fe1 O3 C4 C3 -174.0(3) 4_565 . . . ?
Fe1 O3 C4 C5 6.2(3) 4_565 . . . ?
Fe1 O6 C9 C7 -1.3(4) 3_766 . . 3_766 ?
Fe1 O6 C9 C8 179.0(3) 3_766 . . . ?
Fe1 O2 C2 C3 -171.3(3) . . . . ?
Fe1 O2 C2 C1 8.8(3) . . . . ?
Cl1 C3 C2 O2 -1.1(5) . . . . ?
Cl1 C3 C2 C1 178.8(3) . . . . ?
O5 C7 C8 Cl3 -3.8(5) . . . . ?
O5 C7 C8 C9 177.1(3) . . . . ?
O5 C7 C8 F3 10.1(11) . . . . ?
O4 C5 C6 Cl2 2.1(5) . . . . ?
O4 C5 C6 C1 -178.2(3) . . . . ?
O4 C5 C6 F2 -7.0(11) . . . . ?
O1 C1 C6 Cl2 -0.9(5) . . . . ?
O1 C1 C6 C5 179.4(3) . . . . ?
O1 C1 C6 F2 8.6(11) . . . . ?
O3 C4 C3 Cl1 3.2(5) . . . . ?
O3 C4 C3 C2 -177.3(3) . . . . ?
O3 C4 C3 F1 -5.8(13) . . . . ?
O3 C4 C5 O4 -3.1(4) . . . . ?
O3 C4 C5 C6 176.5(3) . . . . ?
O6 C9 C8 Cl3 3.4(5) . . . . ?
O6 C9 C8 C7 -177.6(3) . . . . ?
O6 C9 C8 F3 -11.3(11) . . . . ?
O2 C2 C1 O1 -0.4(4) . . . . ?
O2 C2 C1 C6 179.4(3) . . . . ?
N00B C19 C20 C21 -172.2(4) . . . . ?
N00B C10 C11 C12 -179.9(5) . . . . ?
N00B C16 C17 C18 176.4(4) . . . . ?
N00B C13 C14 C15 177.2(4) . . . . ?
C4 C3 C2 O2 179.5(3) . . . . ?
C4 C3 C2 C1 -0.6(5) . . . . ?
C4 C5 C6 Cl2 -177.4(3) . . . . ?
C4 C5 C6 C1 2.3(5) . . . . ?
C4 C5 C6 F2 173.5(10) . . . . ?
C9 C7 C8 Cl3 176.4(3) 3_766 . . . ?
C9 C7 C8 C9 -2.7(6) 3_766 . . . ?
C9 C7 C8 F3 -169.7(9) 3_766 . . . ?
C3 C4 C5 O4 177.1(3) . . . . ?
C3 C4 C5 C6 -3.4(5) . . . . ?
C3 C2 C1 O1 179.7(3) . . . . ?
C3 C2 C1 C6 -0.5(5) . . . . ?
C5 C4 C3 Cl1 -176.9(3) . . . . ?
C5 C4 C3 C2 2.5(5) . . . . ?
C5 C4 C3 F1 174.0(13) . . . . ?
C7 C9 C8 Cl3 -176.4(3) 3_766 . . . ?
C7 C9 C8 C7 2.7(6) 3_766 . . . ?
C7 C9 C8 F3 169.0(10) 3_766 . . . ?
C2 C1 C6 Cl2 179.3(3) . . . . ?
C2 C1 C6 C5 -0.4(5) . . . . ?
C2 C1 C6 F2 -171.2(11) . . . . ?
C19 N00B C10 C11 -173.9(4) . . . . ?
C19 N00B C16 C17 50.1(5) . . . . ?
C19 N00B C13 C14 67.1(5) . . . . ?
C10 N00B C19 C20 -60.5(5) . . . . ?
C10 N00B C16 C17 169.1(4) . . . . ?
C10 N00B C13 C14 -53.4(5) . . . . ?
C16 N00B C19 C20 57.5(5) . . . . ?
C16 N00B C10 C11 65.8(5) . . . . ?
C16 N00B C13 C14 -171.9(4) . . . . ?
C13 N00B C19 C20 177.1(4) . . . . ?
C13 N00B C10 C11 -53.5(5) . . . . ?
C13 N00B C16 C17 -69.5(5) . . . . ?
F1 C3 C2 O2 7.9(13) . . . . ?
F1 C3 C2 C1 -172.1(12) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.768
_oxdiff_exptl_absorpt_empirical_full_min 0.406
####################################################################### 
# 
# 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_F-042-d_CCDC-2014820_R1
_database_code_depnum_ccdc_archive 'CCDC 2014820'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-28
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl3.49 F2.51 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl3.49 F2.51 Fe2 N2 O12'
_chemical_formula_weight         1064.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl3.49 F2.51 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.4272(5)
_cell_length_b                   21.1795(9)
_cell_length_c                   12.1426(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.168(4)
_cell_angle_gamma                90
_cell_volume                     2630.83(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8989
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1220
_cell_measurement_theta_min      1.9590
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.037
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21256
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.548
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0164912000
_diffrn_orient_matrix_UB_12      0.0137674000
_diffrn_orient_matrix_UB_13      0.0486555000
_diffrn_orient_matrix_UB_21      -0.0602989000
_diffrn_orient_matrix_UB_22      -0.0165126000
_diffrn_orient_matrix_UB_23      -0.0102803000
_diffrn_orient_matrix_UB_31      0.0299516000
_diffrn_orient_matrix_UB_32      -0.0256920000
_diffrn_orient_matrix_UB_33      0.0327323000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3889
_reflns_number_total             5916
_reflns_odcompleteness_completeness 88.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.06
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5916
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0642
_refine_ls_restrained_S_all      1.036
_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)+(0.1040P)²+1.2802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1925
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-F1
 1.33 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C8-F3
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F2)
4. Others
 Fixed Sof: Cl1(0.60666) Cl2(0.60666) Cl3(0.53178) F2(0.39334) F1(0.39334)
 F3(0.46822)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C16(H16A,H16B), C13(H13A,H13B), C20(H20A,H20B), C10(H10A,
 H10B), C17(H17A,H17B), C11(H11A,H11B), C14(H14A,H14B)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.04708(5) 0.31520(3) 0.49494(4) 0.0420(2) Uani 1 1 d . . . . .
Cl1 Cl 0.6663(5) 0.1696(3) 0.4110(4) 0.0460(7) Uani 0.6067 1 d . . P A 2
Cl2 Cl 0.9419(4) 0.32448(19) 0.0759(3) 0.0439(6) Uani 0.6067 1 d . . P B 2
Cl3 Cl 1.3088(5) 0.5191(5) 0.5135(7) 0.0436(8) Uani 0.5318 1 d . . P C 2
O1 O 1.0188(2) 0.31430(11) 0.32860(19) 0.0413(6) Uani 1 1 d . . . . .
O3 O 0.5837(2) 0.18318(11) 0.16124(19) 0.0426(6) Uani 1 1 d . . . . .
O5 O 1.1498(2) 0.39837(12) 0.4922(2) 0.0456(6) Uani 1 1 d . . . . .
O2 O 0.9054(2) 0.25195(11) 0.46579(18) 0.0424(6) Uani 1 1 d . . . . .
O6 O 1.0967(2) 0.61691(12) 0.50608(19) 0.0438(6) Uani 1 1 d . . . . .
O4 O 0.7033(3) 0.23970(12) 0.02346(18) 0.0449(6) Uani 1 1 d . . . . .
N1 N 0.3999(3) 0.35775(17) 0.2616(3) 0.0548(9) Uani 1 1 d . . . . .
C7 C 1.0872(4) 0.44814(19) 0.4977(3) 0.0418(8) Uani 1 1 d . . . . .
C9 C 1.0601(4) 0.56067(19) 0.5040(3) 0.0419(9) Uani 1 1 d . . . . .
C4 C 0.6890(3) 0.21186(17) 0.2063(3) 0.0385(8) Uani 1 1 d . . . . .
C2 C 0.8519(3) 0.24773(16) 0.3608(3) 0.0370(8) Uani 1 1 d . . . . .
C1 C 0.9165(4) 0.28333(17) 0.2835(3) 0.0392(8) Uani 1 1 d . . . . .
C3 C 0.7409(3) 0.21309(17) 0.3200(3) 0.0392(8) Uani 1 1 d D . . . .
C5 C 0.7563(4) 0.24598(16) 0.1286(3) 0.0396(8) Uani 1 1 d . . . . .
C8 C 1.1379(3) 0.50854(19) 0.5041(3) 0.0438(8) Uani 1 1 d D . . . .
C6 C 0.8658(4) 0.28111(17) 0.1690(3) 0.0415(8) Uani 1 1 d D . . . .
C19 C 0.3999(4) 0.2878(2) 0.2376(3) 0.0569(11) Uani 1 1 d . . . . .
H19A H 0.3944 0.2820 0.1559 0.068 Uiso 1 1 calc R U . . .
H19B H 0.4847 0.2701 0.2761 0.068 Uiso 1 1 calc R U . . .
C16 C 0.4063(5) 0.3713(2) 0.3847(3) 0.0599(11) Uani 1 1 d . . . . .
H16A H 0.4202 0.4173 0.3969 0.072 Uiso 1 1 calc R U . . .
H16B H 0.3202 0.3610 0.4030 0.072 Uiso 1 1 calc R U . . .
C13 C 0.5181(5) 0.3875(2) 0.2270(4) 0.0671(13) Uani 1 1 d . . . . .
H13A H 0.5240 0.4320 0.2528 0.081 Uiso 1 1 calc R U . . .
H13B H 0.5972 0.3655 0.2670 0.081 Uiso 1 1 calc R U . . .
C20 C 0.2917(4) 0.2501(2) 0.2725(3) 0.0589(11) Uani 1 1 d . . . . .
H20A H 0.2068 0.2620 0.2252 0.071 Uiso 1 1 calc R U . . .
H20B H 0.2879 0.2598 0.3516 0.071 Uiso 1 1 calc R U . . .
C10 C 0.2735(5) 0.3862(2) 0.1971(4) 0.0685(13) Uani 1 1 d . . . . .
H10A H 0.2633 0.3736 0.1174 0.082 Uiso 1 1 calc R U . . .
H10B H 0.1997 0.3676 0.2263 0.082 Uiso 1 1 calc R U . . .
C17 C 0.5100(5) 0.3369(2) 0.4661(4) 0.0688(12) Uani 1 1 d . . . . .
H17A H 0.5975 0.3457 0.4493 0.083 Uiso 1 1 calc R U . . .
H17B H 0.4945 0.2908 0.4606 0.083 Uiso 1 1 calc R U . . .
C21 C 0.3148(5) 0.1801(2) 0.2605(4) 0.0715(13) Uani 1 1 d . . . . .
H21A H 0.3088 0.1697 0.1810 0.107 Uiso 1 1 calc R U . . .
H21B H 0.2486 0.1562 0.2903 0.107 Uiso 1 1 calc R U . . .
H21C H 0.4019 0.1690 0.3023 0.107 Uiso 1 1 calc R U . . .
C11 C 0.2632(6) 0.4568(3) 0.2022(4) 0.0827(16) Uani 1 1 d . . . . .
H11A H 0.3338 0.4765 0.1700 0.099 Uiso 1 1 calc R U . . .
H11B H 0.2732 0.4706 0.2813 0.099 Uiso 1 1 calc R U . . .
C18 C 0.5028(5) 0.3604(3) 0.5847(4) 0.0820(15) Uani 1 1 d . . . . .
H18A H 0.4126 0.3570 0.5963 0.123 Uiso 1 1 calc R U . . .
H18B H 0.5310 0.4046 0.5926 0.123 Uiso 1 1 calc R U . . .
H18C H 0.5602 0.3345 0.6406 0.123 Uiso 1 1 calc R U . . .
C14 C 0.5202(6) 0.3868(3) 0.1029(4) 0.0891(18) Uani 1 1 d . . . . .
H14A H 0.5211 0.3426 0.0763 0.107 Uiso 1 1 calc R U . . .
H14B H 0.4407 0.4076 0.0608 0.107 Uiso 1 1 calc R U . . .
C15 C 0.6400(7) 0.4209(3) 0.0823(6) 0.114(2) Uani 1 1 d . . . . .
H15A H 0.6518 0.4125 0.0055 0.171 Uiso 1 1 calc R U . . .
H15B H 0.7168 0.4060 0.1357 0.171 Uiso 1 1 calc R U . . .
H15C H 0.6292 0.4664 0.0922 0.171 Uiso 1 1 calc R U . . .
C12 C 0.1304(7) 0.4779(3) 0.1362(7) 0.131(3) Uani 1 1 d . . . . .
H12A H 0.1218 0.4649 0.0576 0.197 Uiso 1 1 calc R U . . .
H12B H 0.1234 0.5239 0.1403 0.197 Uiso 1 1 calc R U . . .
H12C H 0.0609 0.4582 0.1683 0.197 Uiso 1 1 calc R U . . .
F2 F 0.9328(14) 0.3098(6) 0.0959(10) 0.043(2) Uani 0.3933 1 d D . P B -2
F1 F 0.6753(18) 0.1826(8) 0.3965(13) 0.043(2) Uani 0.3933 1 d D . P A -2
F3 F 1.2737(9) 0.5163(10) 0.5038(16) 0.040(3) Uani 0.4682 1 d D . P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.984(2) . ?
Fe1 O3 1.981(2) 4_666 ?
Fe1 O5 2.065(3) . ?
Fe1 O2 1.975(3) . ?
Fe1 O6 2.076(3) 3_766 ?
Fe1 O4 1.977(3) 4_666 ?
Cl1 C3 1.734(5) . ?
Cl2 C6 1.761(4) . ?
Cl3 C8 1.777(6) . ?
O1 C1 1.281(4) . ?
O3 Fe1 1.981(2) 4_565 ?
O3 C4 1.281(4) . ?
O5 C7 1.249(4) . ?
O2 C2 1.292(4) . ?
O6 Fe1 2.076(3) 3_766 ?
O6 C9 1.250(4) . ?
O4 Fe1 1.977(3) 4_565 ?
O4 C5 1.296(4) . ?
N1 C19 1.510(6) . ?
N1 C16 1.511(5) . ?
N1 C13 1.514(5) . ?
N1 C10 1.521(6) . ?
C7 C9 1.543(5) 3_766 ?
C7 C8 1.381(5) . ?
C9 C7 1.543(5) 3_766 ?
C9 C8 1.370(6) . ?
C4 C3 1.382(4) . ?
C4 C5 1.469(5) . ?
C2 C1 1.465(5) . ?
C2 C3 1.379(5) . ?
C1 C6 1.389(4) . ?
C3 F1 1.412(11) . ?
C5 C6 1.372(5) . ?
C8 F3 1.427(10) . ?
C6 F2 1.373(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.510(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.506(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.511(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.513(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.502(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.538(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.526(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.506(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
O1 Fe1 O5 88.13(10) . . ?
O1 Fe1 O6 92.05(10) . 3_766 ?
O3 Fe1 O1 177.46(11) 4_666 . ?
O3 Fe1 O5 90.20(10) 4_666 . ?
O3 Fe1 O6 89.45(10) 4_666 3_766 ?
O5 Fe1 O6 77.62(10) . 3_766 ?
O2 Fe1 O1 81.50(10) . . ?
O2 Fe1 O3 100.61(10) . 4_666 ?
O2 Fe1 O5 161.46(10) . . ?
O2 Fe1 O6 87.39(10) . 3_766 ?
O2 Fe1 O4 101.23(11) . 4_666 ?
O4 Fe1 O1 97.34(10) 4_666 . ?
O4 Fe1 O3 80.91(10) 4_666 4_666 ?
O4 Fe1 O5 95.28(11) 4_666 . ?
O4 Fe1 O6 168.07(10) 4_666 3_766 ?
C1 O1 Fe1 112.8(2) . . ?
C4 O3 Fe1 114.0(2) . 4_565 ?
C7 O5 Fe1 116.2(2) . . ?
C2 O2 Fe1 112.9(2) . . ?
C9 O6 Fe1 116.2(2) . 3_766 ?
C5 O4 Fe1 114.4(2) . 4_565 ?
C19 N1 C16 112.1(3) . . ?
C19 N1 C13 109.0(3) . . ?
C19 N1 C10 108.8(3) . . ?
C16 N1 C13 108.2(3) . . ?
C16 N1 C10 107.5(3) . . ?
C13 N1 C10 111.2(3) . . ?
O5 C7 C9 115.3(3) . 3_766 ?
O5 C7 C8 125.9(4) . . ?
C8 C7 C9 118.8(3) . 3_766 ?
O6 C9 C7 114.5(3) . 3_766 ?
O6 C9 C8 126.1(4) . . ?
C8 C9 C7 119.3(4) . 3_766 ?
O3 C4 C3 124.9(3) . . ?
O3 C4 C5 115.8(3) . . ?
C3 C4 C5 119.3(3) . . ?
O2 C2 C1 115.6(3) . . ?
O2 C2 C3 124.3(3) . . ?
C3 C2 C1 120.1(3) . . ?
O1 C1 C2 115.9(3) . . ?
O1 C1 C6 124.7(3) . . ?
C6 C1 C2 119.4(3) . . ?
C4 C3 Cl1 119.3(3) . . ?
C4 C3 F1 120.2(8) . . ?
C2 C3 Cl1 120.2(3) . . ?
C2 C3 C4 120.5(3) . . ?
C2 C3 F1 119.1(8) . . ?
F1 C3 Cl1 5.0(10) . . ?
O4 C5 C4 114.6(3) . . ?
O4 C5 C6 125.1(3) . . ?
C6 C5 C4 120.3(3) . . ?
C7 C8 Cl3 119.2(4) . . ?
C7 C8 F3 118.5(9) . . ?
C9 C8 Cl3 119.0(4) . . ?
C9 C8 C7 121.8(3) . . ?
C9 C8 F3 119.7(9) . . ?
F3 C8 Cl3 3.8(10) . . ?
C1 C6 Cl2 119.6(3) . . ?
C5 C6 Cl2 120.1(3) . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 F2 120.1(7) . . ?
F2 C6 Cl2 5.6(8) . . ?
F2 C6 C1 119.3(7) . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N1 115.9(3) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
N1 C16 H16A 108.2 . . ?
N1 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N1 116.5(4) . . ?
C17 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
N1 C13 H13A 108.2 . . ?
N1 C13 H13B 108.2 . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 N1 116.2(4) . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
C19 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
C19 C20 C21 110.5(4) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
N1 C10 H10A 108.3 . . ?
N1 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N1 115.8(4) . . ?
C11 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C16 C17 H17A 110.2 . . ?
C16 C17 H17B 110.2 . . ?
C16 C17 C18 107.4(4) . . ?
H17A C17 H17B 108.5 . . ?
C18 C17 H17A 110.2 . . ?
C18 C17 H17B 110.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
C10 C11 C12 109.5(5) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 C13 109.5(5) . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 O1 C1 C2 -8.3(4) . . . . ?
Fe1 O1 C1 C6 172.4(3) . . . . ?
Fe1 O3 C4 C3 -174.7(3) 4_565 . . . ?
Fe1 O3 C4 C5 6.0(4) 4_565 . . . ?
Fe1 O5 C7 C9 -4.8(4) . . . 3_766 ?
Fe1 O5 C7 C8 175.8(3) . . . . ?
Fe1 O2 C2 C1 7.9(4) . . . . ?
Fe1 O2 C2 C3 -171.6(3) . . . . ?
Fe1 O6 C9 C7 -0.6(3) 3_766 . . 3_766 ?
Fe1 O6 C9 C8 180.0(3) 3_766 . . . ?
Fe1 O4 C5 C4 -0.8(4) 4_565 . . . ?
Fe1 O4 C5 C6 179.4(3) 4_565 . . . ?
O1 C1 C6 Cl2 -1.4(5) . . . . ?
O1 C1 C6 C5 179.3(3) . . . . ?
O1 C1 C6 F2 5.0(9) . . . . ?
O3 C4 C3 Cl1 3.9(6) . . . . ?
O3 C4 C3 C2 -177.1(3) . . . . ?
O3 C4 C3 F1 -1.7(11) . . . . ?
O3 C4 C5 O4 -3.5(5) . . . . ?
O3 C4 C5 C6 176.3(3) . . . . ?
O5 C7 C8 Cl3 -3.8(6) . . . . ?
O5 C7 C8 C9 176.5(3) . . . . ?
O5 C7 C8 F3 0.5(10) . . . . ?
O2 C2 C1 O1 0.3(5) . . . . ?
O2 C2 C1 C6 179.6(3) . . . . ?
O2 C2 C3 Cl1 -1.9(6) . . . . ?
O2 C2 C3 C4 179.1(3) . . . . ?
O2 C2 C3 F1 3.7(11) . . . . ?
O6 C9 C8 Cl3 2.6(6) . . . . ?
O6 C9 C8 C7 -177.7(3) . . . . ?
O6 C9 C8 F3 -1.7(10) . . . . ?
O4 C5 C6 Cl2 2.4(6) . . . . ?
O4 C5 C6 C1 -178.3(3) . . . . ?
O4 C5 C6 F2 -4.1(9) . . . . ?
N1 C19 C20 C21 -171.3(4) . . . . ?
N1 C16 C17 C18 177.2(4) . . . . ?
N1 C13 C14 C15 177.1(4) . . . . ?
N1 C10 C11 C12 -178.6(5) . . . . ?
C7 C9 C8 Cl3 -176.8(4) 3_766 . . . ?
C7 C9 C8 C7 2.9(5) 3_766 . . . ?
C7 C9 C8 F3 178.9(9) 3_766 . . . ?
C9 C7 C8 Cl3 176.8(4) 3_766 . . . ?
C9 C7 C8 C9 -2.9(5) 3_766 . . . ?
C9 C7 C8 F3 -178.9(9) 3_766 . . . ?
C4 C5 C6 Cl2 -177.4(3) . . . . ?
C4 C5 C6 C1 1.9(5) . . . . ?
C4 C5 C6 F2 176.1(8) . . . . ?
C2 C1 C6 Cl2 179.3(3) . . . . ?
C2 C1 C6 C5 0.1(5) . . . . ?
C2 C1 C6 F2 -174.3(8) . . . . ?
C1 C2 C3 Cl1 178.6(4) . . . . ?
C1 C2 C3 C4 -0.4(5) . . . . ?
C1 C2 C3 F1 -175.8(10) . . . . ?
C3 C4 C5 O4 177.1(3) . . . . ?
C3 C4 C5 C6 -3.1(5) . . . . ?
C3 C2 C1 O1 179.8(3) . . . . ?
C3 C2 C1 C6 -0.9(5) . . . . ?
C5 C4 C3 Cl1 -176.7(4) . . . . ?
C5 C4 C3 C2 2.3(5) . . . . ?
C5 C4 C3 F1 177.6(10) . . . . ?
C19 N1 C16 C17 49.1(5) . . . . ?
C19 N1 C13 C14 65.9(5) . . . . ?
C19 N1 C10 C11 -174.1(4) . . . . ?
C16 N1 C19 C20 57.3(5) . . . . ?
C16 N1 C13 C14 -172.0(4) . . . . ?
C16 N1 C10 C11 64.3(5) . . . . ?
C13 N1 C19 C20 177.1(4) . . . . ?
C13 N1 C16 C17 -71.1(5) . . . . ?
C13 N1 C10 C11 -54.0(5) . . . . ?
C10 N1 C19 C20 -61.5(4) . . . . ?
C10 N1 C16 C17 168.6(4) . . . . ?
C10 N1 C13 C14 -54.1(5) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.047
_oxdiff_exptl_absorpt_empirical_full_min 0.416
####################################################################### 
# 
# 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_F-031_CCDC-2014821_R1
_database_code_depnum_ccdc_archive 'CCDC 2014821'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-31
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 Cl4.16 F1.84 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl4.16 F1.84 Fe2 N2 O15'
_chemical_formula_weight         1209.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl4.16 F1.84 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.8524(7)
_cell_length_b                   21.9805(8)
_cell_length_c                   14.2863(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.662(4)
_cell_angle_gamma                90
_cell_volume                     5940.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18131
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1380
_cell_measurement_theta_min      1.8050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2525
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.036
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41974
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.760
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0316566000
_diffrn_orient_matrix_UB_12      0.0095922000
_diffrn_orient_matrix_UB_13      -0.0088041000
_diffrn_orient_matrix_UB_21      0.0199360000
_diffrn_orient_matrix_UB_22      -0.0116107000
_diffrn_orient_matrix_UB_23      0.0464607000
_diffrn_orient_matrix_UB_31      0.0025302000
_diffrn_orient_matrix_UB_32      -0.0285669000
_diffrn_orient_matrix_UB_33      -0.0217909000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7441
_reflns_number_total             10791
_reflns_odcompleteness_completeness 87.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.11
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         10791
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0591
_refine_ls_restrained_S_all      1.033
_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)+(0.1038P)²+5.0787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1874
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-F2
 1.33 with sigma of 0.02
 C11-F4
 1.33 with sigma of 0.02
 C17-F6
 1.33 with sigma of 0.02
 C14-F5
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl6) = Uanis(F6)
Uanis(Cl4) = Uanis(F4)
4. Others
 Fixed Sof: Cl5(0.7133) Cl4(0.6733) Cl6(0.7133) Cl2(0.6933) Cl3(0.6733)
 Cl1(0.6933) O16(0.5) O15(0.5) F3(0.3267) F2(0.3067) F5(0.2867) F6(0.2867)
 F1(0.3067) F4(0.3267)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C34(H34A,H34B), C31(H31A,H31B), C32(H32A,H32B), C40(H40A,
 H40B), C41(H41A,H41B), C28(H28A,H28B), C38(H38A,H38B), C22(H22A,H22B),
 C25(H25A,H25B), C23(H23A,H23B), C19(H19A,H19B), C35(H35A,H35B), C20(H20A,H20B),
  C29(H29A,H29B), C26(H26A,H26B)
5.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C39(H39A,H39B,H39C), C36(H36A,H36B,
 H36C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C),
 C01T(H01D,H01E,H01F), C01X(H01G,H01H,H01I), C01Y(H01A,H01B,H01C), C30(H30A,
 H30B,H30C), C020(H02A,H02B,H02C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Fe2 Fe 0.22173(3) 0.32093(2) 0.39898(3) 0.02795(16) Uani 1 1 d . . . . .
Fe1 Fe 0.23886(3) 0.68079(2) 0.40491(3) 0.02926(17) Uani 1 1 d . . . . .
Cl5 Cl 0.0794(3) 0.3193(3) 0.0395(3) 0.0358(6) Uani 0.7133 1 d . . P A 2
Cl4 Cl 0.38184(12) 0.49792(14) 0.3701(2) 0.0361(4) Uani 0.6733 1 d . . P B 2
Cl6 Cl 0.36363(10) 0.18224(9) 0.25353(15) 0.0435(5) Uani 0.7133 1 d . . P C 2
Cl2 Cl 0.10257(18) 0.6736(2) 0.0478(3) 0.0363(7) Uani 0.6933 1 d . . P D 2
Cl3 Cl 0.09089(16) 0.50981(16) 0.4689(2) 0.0361(6) Uani 0.6733 1 d . . P E 2
Cl1 Cl 0.3805(3) 0.8185(3) 0.2589(4) 0.0441(8) Uani 0.6933 1 d . . P F 2
O10 O 0.16389(12) 0.23539(11) -0.04743(16) 0.0292(5) Uani 1 1 d . . . . .
O12 O 0.27833(12) 0.26466(11) 0.34427(16) 0.0308(6) Uani 1 1 d . . . . .
O9 O 0.16160(12) 0.31998(10) 0.25829(16) 0.0295(5) Uani 1 1 d . . . . .
O4 O 0.18386(12) 0.75984(11) -0.04295(16) 0.0300(5) Uani 1 1 d . . . . .
O5 O 0.17868(12) 0.60951(11) 0.43147(17) 0.0316(6) Uani 1 1 d . . . . .
O7 O 0.28754(12) 0.39272(11) 0.38559(17) 0.0313(6) Uani 1 1 d . . . . .
O2 O 0.29652(13) 0.73607(11) 0.35016(16) 0.0328(6) Uani 1 1 d . . . . .
O6 O 0.16703(12) 0.39686(11) 0.42313(17) 0.0323(6) Uani 1 1 d . . . . .
O1 O 0.18126(13) 0.67855(10) 0.26400(16) 0.0301(6) Uani 1 1 d . . . . .
O11 O 0.28315(13) 0.18356(11) 0.03891(17) 0.0315(6) Uani 1 1 d . . . . .
O14 O 0.29919(13) 0.60546(11) 0.39280(17) 0.0320(6) Uani 1 1 d . . . . .
O3 O 0.30094(13) 0.81564(11) 0.04428(17) 0.0320(6) Uani 1 1 d . . . . .
N2 N 0.49164(16) 0.29826(16) 0.4955(2) 0.0382(8) Uani 1 1 d . . . . .
N1 N 0.04921(17) 0.85204(16) 0.2252(2) 0.0446(8) Uani 1 1 d . . . . .
C18 C 0.25441(17) 0.25714(16) 0.2505(2) 0.0267(7) Uani 1 1 d . . . . .
C13 C 0.18746(17) 0.28828(15) 0.2011(2) 0.0264(7) Uani 1 1 d . . . . .
C2 C 0.27290(18) 0.74280(16) 0.2559(2) 0.0288(8) Uani 1 1 d . . . . .
C5 C 0.20832(17) 0.75174(16) 0.0511(2) 0.0270(7) Uani 1 1 d . . . . .
C4 C 0.27454(18) 0.78398(16) 0.1009(2) 0.0279(8) Uani 1 1 d . . . . .
C1 C 0.20722(18) 0.70969(15) 0.2069(2) 0.0273(7) Uani 1 1 d . . . . .
C16 C 0.25637(18) 0.21502(16) 0.0955(2) 0.0288(8) Uani 1 1 d . . . . .
C7 C 0.20145(18) 0.55751(17) 0.4242(2) 0.0296(8) Uani 1 1 d . . . . .
C15 C 0.18898(18) 0.24537(16) 0.0462(2) 0.0276(8) Uani 1 1 d . . . . .
C10 C 0.26650(18) 0.44536(17) 0.3977(2) 0.0295(8) Uani 1 1 d . . . . .
C6 C 0.17793(18) 0.71503(15) 0.1057(2) 0.0268(7) Uani 1 1 d D . . . .
C9 C 0.19527(18) 0.44786(17) 0.4202(2) 0.0307(8) Uani 1 1 d . . . . .
C12 C 0.27237(18) 0.55463(17) 0.4014(2) 0.0312(8) Uani 1 1 d . . . . .
C3 C 0.30444(19) 0.77841(17) 0.2015(2) 0.0317(8) Uani 1 1 d . . . . .
C14 C 0.15719(17) 0.28151(15) 0.1004(2) 0.0279(8) Uani 1 1 d D . . . .
C8 C 0.16866(19) 0.50372(16) 0.4352(3) 0.0312(8) Uani 1 1 d . . . . .
C11 C 0.30164(18) 0.49854(16) 0.3928(3) 0.0305(8) Uani 1 1 d D . . . .
C17 C 0.28640(18) 0.22187(16) 0.1955(2) 0.0305(8) Uani 1 1 d D . . . .
C37 C 0.4282(2) 0.25930(19) 0.4937(3) 0.0449(10) Uani 1 1 d . . . . .
H37A H 0.3883 0.2866 0.4926 0.054 Uiso 1 1 calc R U . . .
H37B H 0.4144 0.2357 0.4318 0.054 Uiso 1 1 calc R U . . .
C34 C 0.5551(2) 0.25868(19) 0.4980(3) 0.0439(10) Uani 1 1 d . . . . .
H34A H 0.5952 0.2857 0.4991 0.053 Uiso 1 1 calc R U . . .
H34B H 0.5686 0.2354 0.5602 0.053 Uiso 1 1 calc R U . . .
C31 C 0.4696(2) 0.33703(18) 0.4030(3) 0.0410(9) Uani 1 1 d . . . . .
H31A H 0.4584 0.3096 0.3454 0.049 Uiso 1 1 calc R U . . .
H31B H 0.4257 0.3589 0.4012 0.049 Uiso 1 1 calc R U . . .
C32 C 0.5235(2) 0.38316(19) 0.3927(3) 0.0466(10) Uani 1 1 d . . . . .
H32A H 0.5702 0.3634 0.4050 0.056 Uiso 1 1 calc R U . . .
H32B H 0.5282 0.4161 0.4416 0.056 Uiso 1 1 calc R U . . .
C40 C 0.5141(2) 0.33800(19) 0.5867(3) 0.0437(10) Uani 1 1 d . . . . .
H40A H 0.5264 0.3112 0.6452 0.052 Uiso 1 1 calc R U . . .
H40B H 0.5574 0.3603 0.5869 0.052 Uiso 1 1 calc R U . . .
C41 C 0.4596(2) 0.38384(19) 0.5968(3) 0.0477(10) Uani 1 1 d . . . . .
H41A H 0.4138 0.3632 0.5883 0.057 Uiso 1 1 calc R U . . .
H41B H 0.4526 0.4154 0.5453 0.057 Uiso 1 1 calc R U . . .
C28 C 0.0148(3) 0.8776(2) 0.2977(3) 0.0595(13) Uani 1 1 d . . . . .
H28A H 0.0442 0.8665 0.3648 0.071 Uiso 1 1 calc R U . . .
H28B H -0.0318 0.8578 0.2862 0.071 Uiso 1 1 calc R U . . .
C38 C 0.4385(2) 0.2156(2) 0.5779(4) 0.0624(13) Uani 1 1 d . . . . .
H38A H 0.4422 0.2382 0.6391 0.075 Uiso 1 1 calc R U . . .
H38B H 0.4827 0.1922 0.5874 0.075 Uiso 1 1 calc R U . . .
C22 C 0.0590(2) 0.7837(2) 0.2430(3) 0.0533(11) Uani 1 1 d . . . . .
H22A H 0.0839 0.7676 0.1977 0.064 Uiso 1 1 calc R U . . .
H22B H 0.0907 0.7776 0.3107 0.064 Uiso 1 1 calc R U . . .
C25 C 0.1195(2) 0.8806(2) 0.2360(4) 0.0604(13) Uani 1 1 d . . . . .
H25A H 0.1114 0.9229 0.2115 0.072 Uiso 1 1 calc R U . . .
H25B H 0.1419 0.8584 0.1929 0.072 Uiso 1 1 calc R U . . .
C23 C -0.0058(2) 0.74577(19) 0.2307(3) 0.0533(12) Uani 1 1 d . . . . .
H23A H -0.0413 0.7555 0.1671 0.064 Uiso 1 1 calc R U . . .
H23B H -0.0267 0.7556 0.2837 0.064 Uiso 1 1 calc R U . . .
C33 C 0.4997(3) 0.4095(2) 0.2898(3) 0.0675(15) Uani 1 1 d . . . . .
H33A H 0.4960 0.3769 0.2418 0.101 Uiso 1 1 calc R U . . .
H33B H 0.5342 0.4397 0.2829 0.101 Uiso 1 1 calc R U . . .
H33C H 0.4534 0.4290 0.2780 0.101 Uiso 1 1 calc R U . . .
C19 C 0.0007(2) 0.8640(2) 0.1228(3) 0.0550(12) Uani 1 1 d . . . . .
H19A H -0.0477 0.8521 0.1213 0.066 Uiso 1 1 calc R U . . .
H19B H 0.0001 0.9085 0.1115 0.066 Uiso 1 1 calc R U . . .
C35 C 0.5449(2) 0.2143(2) 0.4141(4) 0.0632(14) Uani 1 1 d . . . . .
H35A H 0.5419 0.2366 0.3527 0.076 Uiso 1 1 calc R U . . .
H35B H 0.5004 0.1913 0.4042 0.076 Uiso 1 1 calc R U . . .
C42 C 0.4848(3) 0.4133(2) 0.6977(3) 0.0684(15) Uani 1 1 d . . . . .
H42A H 0.4516 0.4454 0.7021 0.103 Uiso 1 1 calc R U . . .
H42B H 0.5317 0.4310 0.7078 0.103 Uiso 1 1 calc R U . . .
H42C H 0.4872 0.3825 0.7483 0.103 Uiso 1 1 calc R U . . .
C39 C 0.3754(2) 0.1724(2) 0.5546(4) 0.0687(15) Uani 1 1 d . . . . .
H39A H 0.3757 0.1465 0.4989 0.103 Uiso 1 1 calc R U . . .
H39B H 0.3315 0.1960 0.5378 0.103 Uiso 1 1 calc R U . . .
H39C H 0.3786 0.1469 0.6120 0.103 Uiso 1 1 calc R U . . .
C20 C 0.0164(3) 0.8338(2) 0.0387(4) 0.0651(14) Uani 1 1 d . . . . .
H20A H 0.0157 0.7891 0.0468 0.078 Uiso 1 1 calc R U . . .
H20B H 0.0640 0.8458 0.0370 0.078 Uiso 1 1 calc R U . . .
C36 C 0.6080(2) 0.1703(2) 0.4391(5) 0.0698(16) Uani 1 1 d . . . . .
H36A H 0.6046 0.1439 0.3826 0.105 Uiso 1 1 calc R U . . .
H36B H 0.6076 0.1453 0.4957 0.105 Uiso 1 1 calc R U . . .
H36C H 0.6522 0.1936 0.4550 0.105 Uiso 1 1 calc R U . . .
C24 C 0.0117(3) 0.6785(2) 0.2342(4) 0.0715(15) Uani 1 1 d . . . . .
H24A H 0.0337 0.6690 0.1831 0.107 Uiso 1 1 calc R U . . .
H24B H -0.0318 0.6547 0.2229 0.107 Uiso 1 1 calc R U . . .
H24C H 0.0444 0.6683 0.2987 0.107 Uiso 1 1 calc R U . . .
C29 C 0.0043(3) 0.9457(2) 0.2932(4) 0.0695(14) Uani 1 1 d . . . . .
H29A H -0.0276 0.9572 0.2277 0.083 Uiso 1 1 calc R U . . .
H29B H 0.0503 0.9661 0.3026 0.083 Uiso 1 1 calc R U . . .
O8 O 0.1386(3) 1.0344(2) 0.2878(6) 0.177(3) Uani 1 1 d . . . . .
C26 C 0.1708(3) 0.8820(3) 0.3380(4) 0.0797(17) Uani 1 1 d . . . . .
H26A H 0.1520 0.9087 0.3801 0.096 Uiso 1 1 calc R U . . .
H26B H 0.1759 0.8405 0.3662 0.096 Uiso 1 1 calc R U . . .
C21 C -0.0377(4) 0.8519(3) -0.0555(4) 0.0876(19) Uani 1 1 d . . . . .
H21A H -0.0317 0.8272 -0.1094 0.131 Uiso 1 1 calc R U . . .
H21B H -0.0317 0.8950 -0.0686 0.131 Uiso 1 1 calc R U . . .
H21C H -0.0852 0.8454 -0.0499 0.131 Uiso 1 1 calc R U . . .
C27 C 0.2416(3) 0.9049(3) 0.3376(5) 0.090(2) Uani 1 1 d . . . . .
H27A H 0.2625 0.8762 0.3019 0.135 Uiso 1 1 calc R U . . .
H27B H 0.2725 0.9087 0.4054 0.135 Uiso 1 1 calc R U . . .
H27C H 0.2362 0.9447 0.3053 0.135 Uiso 1 1 calc R U . . .
C01T C 0.2485(4) 0.5575(3) 0.1243(5) 0.102(2) Uani 1 1 d . . . . .
H01D H 0.2848 0.5787 0.1760 0.153 Uiso 1 1 calc R U . . .
H01E H 0.2067 0.5507 0.1460 0.153 Uiso 1 1 calc R U . . .
H01F H 0.2354 0.5822 0.0645 0.153 Uiso 1 1 calc R U . . .
O13 O 0.3338(4) 0.4968(3) 0.0834(7) 0.185(4) Uani 1 1 d . . . . .
C01V C 0.1777(4) 1.0741(3) 0.2780(6) 0.099(2) Uani 1 1 d . . . . .
C01W C 0.2767(5) 0.4978(3) 0.1039(5) 0.104(3) Uani 1 1 d . . . . .
C01X C 0.2398(4) 0.4414(3) 0.1186(5) 0.108(2) Uani 1 1 d . . . . .
H01G H 0.2063 0.4511 0.1546 0.163 Uiso 1 1 calc R U . . .
H01H H 0.2746 0.4119 0.1562 0.163 Uiso 1 1 calc R U . . .
H01I H 0.2142 0.4239 0.0545 0.163 Uiso 1 1 calc R U . . .
C01Y C 0.2165(5) 1.0671(3) 0.1997(5) 0.124(3) Uani 1 1 d . . . . .
H01A H 0.2052 1.0273 0.1677 0.187 Uiso 1 1 calc R U . . .
H01B H 0.2676 1.0701 0.2313 0.187 Uiso 1 1 calc R U . . .
H01C H 0.2013 1.0993 0.1504 0.187 Uiso 1 1 calc R U . . .
C30 C -0.0272(5) 0.9666(3) 0.3717(6) 0.131(3) Uani 1 1 d . . . . .
H30A H -0.0748 0.9495 0.3586 0.197 Uiso 1 1 calc R U . . .
H30B H -0.0300 1.0111 0.3711 0.197 Uiso 1 1 calc R U . . .
H30C H 0.0026 0.9528 0.4361 0.197 Uiso 1 1 calc R U . . .
C020 C 0.1908(4) 1.1273(3) 0.3398(6) 0.112(2) Uani 1 1 d . . . . .
H02A H 0.1616 1.1256 0.3841 0.168 Uiso 1 1 calc R U . . .
H02B H 0.1789 1.1639 0.2989 0.168 Uiso 1 1 calc R U . . .
H02C H 0.2409 1.1286 0.3786 0.168 Uiso 1 1 calc R U . . .
O16 O 0.4368(15) 0.5030(8) -0.0741(14) 0.260(13) Uani 0.5 1 d . . P G -3
O15 O 0.4836(8) 0.4338(15) -0.0206(13) 0.283(13) Uani 0.5 1 d . . P H 3
F3 F 0.1019(9) 0.5008(7) 0.4456(11) 0.051(4) Uani 0.3267 1 d . . P E -2
F2 F 0.1140(9) 0.6887(9) 0.0585(17) 0.047(6) Uani 0.3067 1 d D . P D -2
F5 F 0.0925(11) 0.3075(12) 0.0599(15) 0.035(5) Uani 0.2867 1 d D . P A -2
F6 F 0.3515(7) 0.1987(7) 0.2430(10) 0.0435(5) Uani 0.2867 1 d D . P C -2
F1 F 0.3698(15) 0.8030(12) 0.2450(18) 0.046(6) Uani 0.3067 1 d . . P F -2
F4 F 0.3665(7) 0.4927(7) 0.3733(13) 0.0361(4) Uani 0.3267 1 d D . P B -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe2 O10 1.993(2) 4_566 ?
Fe2 O12 1.984(2) . ?
Fe2 O9 2.002(2) . ?
Fe2 O7 2.094(2) . ?
Fe2 O6 2.076(2) . ?
Fe2 O11 2.003(2) 4_566 ?
Fe1 O4 1.986(2) 4_576 ?
Fe1 O5 2.074(2) . ?
Fe1 O2 1.985(2) . ?
Fe1 O1 1.991(2) . ?
Fe1 O14 2.081(2) . ?
Fe1 O3 2.000(2) 4_576 ?
Cl5 C14 1.737(5) . ?
Cl4 C11 1.718(4) . ?
Cl6 C17 1.739(3) . ?
Cl2 C6 1.732(4) . ?
Cl3 C8 1.757(4) . ?
Cl1 C3 1.726(5) . ?
O10 Fe2 1.993(2) 4_565 ?
O10 C15 1.296(4) . ?
O12 C18 1.289(4) . ?
O9 C13 1.293(4) . ?
O4 Fe1 1.986(2) 4_575 ?
O4 C5 1.296(4) . ?
O5 C7 1.245(4) . ?
O7 C10 1.260(4) . ?
O2 C2 1.293(4) . ?
O6 C9 1.260(4) . ?
O1 C1 1.287(4) . ?
O11 Fe2 2.003(2) 4_565 ?
O11 C16 1.294(4) . ?
O14 C12 1.260(4) . ?
O3 Fe1 2.000(2) 4_575 ?
O3 C4 1.293(4) . ?
N2 C37 1.516(5) . ?
N2 C34 1.522(5) . ?
N2 C31 1.520(5) . ?
N2 C40 1.520(5) . ?
N1 C28 1.510(5) . ?
N1 C22 1.526(6) . ?
N1 C25 1.494(5) . ?
N1 C19 1.510(5) . ?
C18 C13 1.471(5) . ?
C18 C17 1.387(5) . ?
C13 C14 1.389(5) . ?
C2 C1 1.472(5) . ?
C2 C3 1.380(5) . ?
C5 C4 1.473(5) . ?
C5 C6 1.381(5) . ?
C4 C3 1.383(5) . ?
C1 C6 1.389(5) . ?
C16 C15 1.469(5) . ?
C16 C17 1.379(5) . ?
C7 C12 1.540(5) . ?
C7 C8 1.381(5) . ?
C15 C14 1.387(5) . ?
C10 C9 1.544(5) . ?
C10 C11 1.374(5) . ?
C6 F2 1.371(14) . ?
C9 C8 1.379(5) . ?
C12 C11 1.384(5) . ?
C3 F1 1.37(2) . ?
C14 F5 1.364(15) . ?
C8 F3 1.380(16) . ?
C11 F4 1.402(11) . ?
C17 F6 1.363(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.504(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.510(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.513(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.517(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.517(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.520(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.510(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.525(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.499(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.517(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.485(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.538(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.499(7) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.511(7) . ?
O8 C01V 1.204(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.494(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C01T H01D 0.9800 . ?
C01T H01E 0.9800 . ?
C01T H01F 0.9800 . ?
C01T C01W 1.489(8) . ?
O13 C01W 1.254(9) . ?
C01V C01Y 1.547(10) . ?
C01V C020 1.440(9) . ?
C01W C01X 1.487(9) . ?
C01X H01G 0.9800 . ?
C01X H01H 0.9800 . ?
C01X H01I 0.9800 . ?
C01Y H01A 0.9800 . ?
C01Y H01B 0.9800 . ?
C01Y H01C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C020 H02A 0.9800 . ?
C020 H02B 0.9800 . ?
C020 H02C 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
O10 Fe2 O9 98.13(9) 4_566 . ?
O10 Fe2 O7 162.08(9) 4_566 . ?
O10 Fe2 O6 92.53(9) 4_566 . ?
O10 Fe2 O11 80.40(9) 4_566 4_566 ?
O12 Fe2 O10 103.02(10) . 4_566 ?
O12 Fe2 O9 80.47(9) . . ?
O12 Fe2 O7 89.44(10) . . ?
O12 Fe2 O6 162.53(10) . . ?
O12 Fe2 O11 96.68(10) . 4_566 ?
O9 Fe2 O7 96.59(9) . . ?
O9 Fe2 O6 89.58(9) . . ?
O9 Fe2 O11 176.46(10) . 4_566 ?
O6 Fe2 O7 77.40(9) . . ?
O11 Fe2 O7 85.45(9) 4_566 . ?
O11 Fe2 O6 93.70(10) 4_566 . ?
O4 Fe1 O5 90.86(10) 4_576 . ?
O4 Fe1 O1 100.55(9) 4_576 . ?
O4 Fe1 O14 161.76(9) 4_576 . ?
O4 Fe1 O3 81.01(9) 4_576 4_576 ?
O5 Fe1 O14 78.00(10) . . ?
O2 Fe1 O4 101.18(10) . 4_576 ?
O2 Fe1 O5 165.34(10) . . ?
O2 Fe1 O1 80.78(9) . . ?
O2 Fe1 O14 92.24(10) . . ?
O2 Fe1 O3 96.51(10) . 4_576 ?
O1 Fe1 O5 88.88(9) . . ?
O1 Fe1 O14 93.71(9) . . ?
O1 Fe1 O3 177.07(10) . 4_576 ?
O3 Fe1 O5 93.59(10) 4_576 . ?
O3 Fe1 O14 85.27(9) 4_576 . ?
C15 O10 Fe2 114.6(2) . 4_565 ?
C18 O12 Fe2 114.5(2) . . ?
C13 O9 Fe2 114.2(2) . . ?
C5 O4 Fe1 113.8(2) . 4_575 ?
C7 O5 Fe1 115.8(2) . . ?
C10 O7 Fe2 116.0(2) . . ?
C2 O2 Fe1 114.2(2) . . ?
C9 O6 Fe2 116.7(2) . . ?
C1 O1 Fe1 114.2(2) . . ?
C16 O11 Fe2 114.1(2) . 4_565 ?
C12 O14 Fe1 115.3(2) . . ?
C4 O3 Fe1 113.6(2) . 4_575 ?
C37 N2 C34 110.7(3) . . ?
C37 N2 C31 106.5(3) . . ?
C37 N2 C40 111.4(3) . . ?
C31 N2 C34 111.0(3) . . ?
C40 N2 C34 106.5(3) . . ?
C40 N2 C31 110.8(3) . . ?
C28 N1 C22 108.3(3) . . ?
C28 N1 C19 108.2(3) . . ?
C25 N1 C28 112.1(3) . . ?
C25 N1 C22 109.1(3) . . ?
C25 N1 C19 109.1(3) . . ?
C19 N1 C22 110.1(3) . . ?
O12 C18 C13 115.7(3) . . ?
O12 C18 C17 124.9(3) . . ?
C17 C18 C13 119.4(3) . . ?
O9 C13 C18 115.0(3) . . ?
O9 C13 C14 125.6(3) . . ?
C14 C13 C18 119.4(3) . . ?
O2 C2 C1 115.3(3) . . ?
O2 C2 C3 124.6(3) . . ?
C3 C2 C1 120.0(3) . . ?
O4 C5 C4 115.7(3) . . ?
O4 C5 C6 125.1(3) . . ?
C6 C5 C4 119.1(3) . . ?
O3 C4 C5 115.4(3) . . ?
O3 C4 C3 124.7(3) . . ?
C3 C4 C5 119.9(3) . . ?
O1 C1 C2 115.4(3) . . ?
O1 C1 C6 125.7(3) . . ?
C6 C1 C2 118.9(3) . . ?
O11 C16 C15 115.5(3) . . ?
O11 C16 C17 125.1(3) . . ?
C17 C16 C15 119.4(3) . . ?
O5 C7 C12 115.7(3) . . ?
O5 C7 C8 125.5(3) . . ?
C8 C7 C12 118.8(3) . . ?
O10 C15 C16 115.2(3) . . ?
O10 C15 C14 125.1(3) . . ?
C14 C15 C16 119.7(3) . . ?
O7 C10 C9 115.1(3) . . ?
O7 C10 C11 125.4(3) . . ?
C11 C10 C9 119.5(3) . . ?
C5 C6 Cl2 119.9(3) . . ?
C5 C6 C1 121.3(3) . . ?
C1 C6 Cl2 118.7(3) . . ?
F2 C6 Cl2 6.8(11) . . ?
F2 C6 C5 117.8(11) . . ?
F2 C6 C1 120.6(11) . . ?
O6 C9 C10 114.9(3) . . ?
O6 C9 C8 126.3(3) . . ?
C8 C9 C10 118.8(3) . . ?
O14 C12 C7 115.1(3) . . ?
O14 C12 C11 125.4(3) . . ?
C11 C12 C7 119.4(3) . . ?
C2 C3 Cl1 120.2(3) . . ?
C2 C3 C4 120.7(3) . . ?
C4 C3 Cl1 119.1(3) . . ?
F1 C3 Cl1 8.1(15) . . ?
F1 C3 C2 119.8(12) . . ?
F1 C3 C4 119.1(12) . . ?
C13 C14 Cl5 120.5(3) . . ?
C15 C14 Cl5 118.7(3) . . ?
C15 C14 C13 120.8(3) . . ?
F5 C14 Cl5 6.9(13) . . ?
F5 C14 C13 116.7(11) . . ?
F5 C14 C15 122.2(11) . . ?
C7 C8 Cl3 116.7(3) . . ?
C9 C8 Cl3 121.4(3) . . ?
C9 C8 C7 121.9(3) . . ?
F3 C8 Cl3 11.7(6) . . ?
F3 C8 C7 123.6(7) . . ?
F3 C8 C9 113.7(7) . . ?
C10 C11 Cl4 121.1(3) . . ?
C10 C11 C12 121.3(3) . . ?
C10 C11 F4 116.3(7) . . ?
C12 C11 Cl4 117.5(3) . . ?
F4 C11 Cl4 4.8(7) . . ?
F4 C11 C12 122.3(7) . . ?
C18 C17 Cl6 119.9(3) . . ?
C16 C17 Cl6 118.7(3) . . ?
C16 C17 C18 121.3(3) . . ?
F6 C17 Cl6 8.2(8) . . ?
F6 C17 C18 117.0(7) . . ?
F6 C17 C16 121.4(7) . . ?
N2 C37 H37A 108.3 . . ?
N2 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 N2 116.0(3) . . ?
C38 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
N2 C34 H34A 108.3 . . ?
N2 C34 H34B 108.3 . . ?
H34A C34 H34B 107.4 . . ?
C35 C34 N2 116.1(3) . . ?
C35 C34 H34A 108.3 . . ?
C35 C34 H34B 108.3 . . ?
N2 C31 H31A 108.3 . . ?
N2 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 N2 115.8(3) . . ?
C32 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
C31 C32 C33 109.2(4) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.8 . . ?
C33 C32 H32B 109.8 . . ?
N2 C40 H40A 108.4 . . ?
N2 C40 H40B 108.4 . . ?
H40A C40 H40B 107.5 . . ?
C41 C40 N2 115.6(3) . . ?
C41 C40 H40A 108.4 . . ?
C41 C40 H40B 108.4 . . ?
C40 C41 H41A 109.8 . . ?
C40 C41 H41B 109.8 . . ?
C40 C41 C42 109.5(4) . . ?
H41A C41 H41B 108.2 . . ?
C42 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
N1 C28 H28A 108.5 . . ?
N1 C28 H28B 108.5 . . ?
N1 C28 C29 115.2(4) . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C37 C38 H38A 110.0 . . ?
C37 C38 H38B 110.0 . . ?
C37 C38 C39 108.7(4) . . ?
H38A C38 H38B 108.3 . . ?
C39 C38 H38A 110.0 . . ?
C39 C38 H38B 110.0 . . ?
N1 C22 H22A 107.9 . . ?
N1 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C23 C22 N1 117.8(3) . . ?
C23 C22 H22A 107.9 . . ?
C23 C22 H22B 107.9 . . ?
N1 C25 H25A 108.2 . . ?
N1 C25 H25B 108.2 . . ?
N1 C25 C26 116.4(4) . . ?
H25A C25 H25B 107.3 . . ?
C26 C25 H25A 108.2 . . ?
C26 C25 H25B 108.2 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C22 C23 C24 111.0(4) . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C19 H19A 107.7 . . ?
N1 C19 H19B 107.7 . . ?
H19A C19 H19B 107.1 . . ?
C20 C19 N1 118.5(4) . . ?
C20 C19 H19A 107.7 . . ?
C20 C19 H19B 107.7 . . ?
C34 C35 H35A 110.0 . . ?
C34 C35 H35B 110.0 . . ?
C34 C35 C36 108.5(4) . . ?
H35A C35 H35B 108.4 . . ?
C36 C35 H35A 110.0 . . ?
C36 C35 H35B 110.0 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.8(4) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 C30 110.7(5) . . ?
H29A C29 H29B 108.1 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C25 C26 H26A 109.4 . . ?
C25 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C27 C26 C25 111.4(5) . . ?
C27 C26 H26A 109.3 . . ?
C27 C26 H26B 109.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
H01D C01T H01E 109.5 . . ?
H01D C01T H01F 109.5 . . ?
H01E C01T H01F 109.5 . . ?
C01W C01T H01D 109.5 . . ?
C01W C01T H01E 109.5 . . ?
C01W C01T H01F 109.5 . . ?
O8 C01V C01Y 119.4(7) . . ?
O8 C01V C020 121.3(8) . . ?
C020 C01V C01Y 119.2(6) . . ?
O13 C01W C01T 118.8(7) . . ?
O13 C01W C01X 122.5(7) . . ?
C01X C01W C01T 118.5(7) . . ?
C01W C01X H01G 109.5 . . ?
C01W C01X H01H 109.5 . . ?
C01W C01X H01I 109.5 . . ?
H01G C01X H01H 109.5 . . ?
H01G C01X H01I 109.5 . . ?
H01H C01X H01I 109.5 . . ?
C01V C01Y H01A 109.5 . . ?
C01V C01Y H01B 109.5 . . ?
C01V C01Y H01C 109.5 . . ?
H01A C01Y H01B 109.5 . . ?
H01A C01Y H01C 109.5 . . ?
H01B C01Y H01C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C01V C020 H02A 109.5 . . ?
C01V C020 H02B 109.5 . . ?
C01V C020 H02C 109.5 . . ?
H02A C020 H02B 109.5 . . ?
H02A C020 H02C 109.5 . . ?
H02B C020 H02C 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
Fe2 O10 C15 C16 1.7(4) 4_565 . . . ?
Fe2 O10 C15 C14 -178.2(3) 4_565 . . . ?
Fe2 O12 C18 C13 -3.6(4) . . . . ?
Fe2 O12 C18 C17 177.5(3) . . . . ?
Fe2 O9 C13 C18 2.3(4) . . . . ?
Fe2 O9 C13 C14 -178.3(3) . . . . ?
Fe2 O7 C10 C9 -0.1(4) . . . . ?
Fe2 O7 C10 C11 179.5(3) . . . . ?
Fe2 O6 C9 C10 0.7(4) . . . . ?
Fe2 O6 C9 C8 -179.2(3) . . . . ?
Fe2 O11 C16 C15 -4.4(4) 4_565 . . . ?
Fe2 O11 C16 C17 176.0(3) 4_565 . . . ?
Fe1 O4 C5 C4 -4.3(4) 4_575 . . . ?
Fe1 O4 C5 C6 177.0(3) 4_575 . . . ?
Fe1 O5 C7 C12 2.7(4) . . . . ?
Fe1 O5 C7 C8 -177.5(3) . . . . ?
Fe1 O2 C2 C1 1.3(4) . . . . ?
Fe1 O2 C2 C3 -179.3(3) . . . . ?
Fe1 O1 C1 C2 -2.0(4) . . . . ?
Fe1 O1 C1 C6 179.2(3) . . . . ?
Fe1 O14 C12 C7 -2.8(4) . . . . ?
Fe1 O14 C12 C11 177.7(3) . . . . ?
Fe1 O3 C4 C5 6.0(4) 4_575 . . . ?
Fe1 O3 C4 C3 -174.8(3) 4_575 . . . ?
O10 C15 C14 Cl5 -2.6(5) . . . . ?
O10 C15 C14 C13 178.5(3) . . . . ?
O10 C15 C14 F5 4.3(15) . . . . ?
O12 C18 C13 O9 0.9(4) . . . . ?
O12 C18 C13 C14 -178.6(3) . . . . ?
O12 C18 C17 Cl6 1.6(5) . . . . ?
O12 C18 C17 C16 178.4(3) . . . . ?
O12 C18 C17 F6 -7.1(10) . . . . ?
O9 C13 C14 Cl5 2.3(6) . . . . ?
O9 C13 C14 C15 -178.8(3) . . . . ?
O9 C13 C14 F5 -4.4(15) . . . . ?
O4 C5 C4 O3 -1.2(4) . . . . ?
O4 C5 C4 C3 179.6(3) . . . . ?
O4 C5 C6 Cl2 2.0(5) . . . . ?
O4 C5 C6 C1 -179.0(3) . . . . ?
O4 C5 C6 F2 -5.4(12) . . . . ?
O5 C7 C12 O14 0.1(4) . . . . ?
O5 C7 C12 C11 179.6(3) . . . . ?
O5 C7 C8 Cl3 -3.8(5) . . . . ?
O5 C7 C8 C9 176.1(3) . . . . ?
O5 C7 C8 F3 7.1(9) . . . . ?
O7 C10 C9 O6 -0.4(4) . . . . ?
O7 C10 C9 C8 179.5(3) . . . . ?
O7 C10 C11 Cl4 -0.8(5) . . . . ?
O7 C10 C11 C12 176.2(3) . . . . ?
O7 C10 C11 F4 -0.5(10) . . . . ?
O2 C2 C1 O1 0.5(4) . . . . ?
O2 C2 C1 C6 179.3(3) . . . . ?
O2 C2 C3 Cl1 -0.6(6) . . . . ?
O2 C2 C3 C4 -178.6(3) . . . . ?
O2 C2 C3 F1 8.8(16) . . . . ?
O6 C9 C8 Cl3 4.1(5) . . . . ?
O6 C9 C8 C7 -175.8(3) . . . . ?
O6 C9 C8 F3 -5.8(9) . . . . ?
O1 C1 C6 Cl2 -3.8(5) . . . . ?
O1 C1 C6 C5 177.2(3) . . . . ?
O1 C1 C6 F2 3.8(12) . . . . ?
O11 C16 C15 O10 1.8(4) . . . . ?
O11 C16 C15 C14 -178.2(3) . . . . ?
O11 C16 C17 Cl6 -3.9(5) . . . . ?
O11 C16 C17 C18 179.2(3) . . . . ?
O11 C16 C17 F6 5.0(10) . . . . ?
O14 C12 C11 Cl4 1.0(5) . . . . ?
O14 C12 C11 C10 -176.2(3) . . . . ?
O14 C12 C11 F4 0.3(10) . . . . ?
O3 C4 C3 Cl1 2.9(6) . . . . ?
O3 C4 C3 C2 -179.0(3) . . . . ?
O3 C4 C3 F1 -6.4(16) . . . . ?
N2 C37 C38 C39 -169.4(4) . . . . ?
N2 C34 C35 C36 -169.0(4) . . . . ?
N2 C31 C32 C33 169.6(3) . . . . ?
N2 C40 C41 C42 171.5(3) . . . . ?
N1 C28 C29 C30 -177.4(5) . . . . ?
N1 C22 C23 C24 170.5(4) . . . . ?
N1 C25 C26 C27 173.4(4) . . . . ?
N1 C19 C20 C21 -179.9(4) . . . . ?
C18 C13 C14 Cl5 -178.3(3) . . . . ?
C18 C13 C14 C15 0.6(5) . . . . ?
C18 C13 C14 F5 175.0(14) . . . . ?
C13 C18 C17 Cl6 -177.3(3) . . . . ?
C13 C18 C17 C16 -0.5(5) . . . . ?
C13 C18 C17 F6 174.0(9) . . . . ?
C2 C1 C6 Cl2 177.5(3) . . . . ?
C2 C1 C6 C5 -1.5(5) . . . . ?
C2 C1 C6 F2 -174.9(11) . . . . ?
C5 C4 C3 Cl1 -178.0(4) . . . . ?
C5 C4 C3 C2 0.1(5) . . . . ?
C5 C4 C3 F1 172.7(15) . . . . ?
C4 C5 C6 Cl2 -176.7(3) . . . . ?
C4 C5 C6 C1 2.3(5) . . . . ?
C4 C5 C6 F2 175.9(11) . . . . ?
C1 C2 C3 Cl1 178.8(4) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C1 C2 C3 F1 -171.9(15) . . . . ?
C16 C15 C14 Cl5 177.4(3) . . . . ?
C16 C15 C14 C13 -1.5(5) . . . . ?
C16 C15 C14 F5 -175.6(15) . . . . ?
C7 C12 C11 Cl4 -178.5(3) . . . . ?
C7 C12 C11 C10 4.4(5) . . . . ?
C7 C12 C11 F4 -179.2(9) . . . . ?
C15 C16 C17 Cl6 176.5(3) . . . . ?
C15 C16 C17 C18 -0.3(5) . . . . ?
C15 C16 C17 F6 -174.6(9) . . . . ?
C10 C9 C8 Cl3 -175.8(3) . . . . ?
C10 C9 C8 C7 4.3(5) . . . . ?
C10 C9 C8 F3 174.3(8) . . . . ?
C6 C5 C4 O3 177.6(3) . . . . ?
C6 C5 C4 C3 -1.6(5) . . . . ?
C9 C10 C11 Cl4 178.8(3) . . . . ?
C9 C10 C11 C12 -4.2(5) . . . . ?
C9 C10 C11 F4 179.1(9) . . . . ?
C12 C7 C8 Cl3 176.0(3) . . . . ?
C12 C7 C8 C9 -4.1(5) . . . . ?
C12 C7 C8 F3 -173.1(8) . . . . ?
C3 C2 C1 O1 -178.9(3) . . . . ?
C3 C2 C1 C6 -0.1(5) . . . . ?
C8 C7 C12 O14 -179.8(3) . . . . ?
C8 C7 C12 C11 -0.2(5) . . . . ?
C11 C10 C9 O6 180.0(3) . . . . ?
C11 C10 C9 C8 -0.1(5) . . . . ?
C17 C18 C13 O9 179.9(3) . . . . ?
C17 C18 C13 C14 0.4(5) . . . . ?
C17 C16 C15 O10 -178.6(3) . . . . ?
C17 C16 C15 C14 1.4(5) . . . . ?
C37 N2 C34 C35 58.1(5) . . . . ?
C37 N2 C31 C32 175.8(3) . . . . ?
C37 N2 C40 C41 -62.1(4) . . . . ?
C34 N2 C37 C38 57.7(5) . . . . ?
C34 N2 C31 C32 -63.5(4) . . . . ?
C34 N2 C40 C41 177.1(3) . . . . ?
C31 N2 C37 C38 178.5(4) . . . . ?
C31 N2 C34 C35 -60.0(5) . . . . ?
C31 N2 C40 C41 56.2(4) . . . . ?
C40 N2 C37 C38 -60.6(5) . . . . ?
C40 N2 C34 C35 179.3(4) . . . . ?
C40 N2 C31 C32 54.6(4) . . . . ?
C28 N1 C22 C23 60.8(5) . . . . ?
C28 N1 C25 C26 50.7(5) . . . . ?
C28 N1 C19 C20 -169.3(4) . . . . ?
C22 N1 C28 C29 177.3(4) . . . . ?
C22 N1 C25 C26 -69.2(5) . . . . ?
C22 N1 C19 C20 -51.1(5) . . . . ?
C25 N1 C28 C29 56.9(5) . . . . ?
C25 N1 C22 C23 -177.0(4) . . . . ?
C25 N1 C19 C20 68.6(5) . . . . ?
C19 N1 C28 C29 -63.3(5) . . . . ?
C19 N1 C22 C23 -57.3(5) . . . . ?
C19 N1 C25 C26 170.5(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.579
####################################################################### 
# 
# 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_F-024_CCDC-2014816_R1
_database_code_depnum_ccdc_archive 'CCDC 2014816'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-31
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 Cl4.55 F1.45 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl4.55 F1.45 Fe2 N2 O15'
_chemical_formula_weight         1215.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl4.55 F1.45 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.8773(6)
_cell_length_b                   21.9737(7)
_cell_length_c                   14.2912(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.608(4)
_cell_angle_gamma                90
_cell_volume                     5949.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15655
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.4920
_cell_measurement_theta_min      1.7500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2538
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40793
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.759
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   15.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   15.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0231446000
_diffrn_orient_matrix_UB_12      0.0151266000
_diffrn_orient_matrix_UB_13      -0.0409855000
_diffrn_orient_matrix_UB_21      -0.0293084000
_diffrn_orient_matrix_UB_22      -0.0096163000
_diffrn_orient_matrix_UB_23      0.0149400000
_diffrn_orient_matrix_UB_31      0.0026529000
_diffrn_orient_matrix_UB_32      0.0268278000
_diffrn_orient_matrix_UB_33      0.0284110000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7675
_reflns_number_total             10874
_reflns_odcompleteness_completeness 90.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.35
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10874
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.043
_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)+(0.1133P)²+4.5906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2026
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-F5
 1.33 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C11-F4
 1.33 with sigma of 0.02
 C8-F3
 1.33 with sigma of 0.02
3. Others
 Fixed Sof: Cl2(0.7849) Cl4(0.745) Cl3(0.745) Cl1(0.7849) Cl5(0.745)
 Cl6(0.745) O16(0.5) O15(0.5) F3(0.255) F2(0.2151) F5(0.255) F4(0.255)
 F1(0.2151) F6(0.255)
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C35(H35A,H35B), C40(H40A,H40B), C38(H38A,H38B), C34(H34A,
 H34B), C37(H37A,H37B), C22(H22A,H22B), C19(H19A,H19B), C29(H29A,H29B),
 C25(H25A,H25B), C23(H23A,H23B), C28(H28A,H28B), C32(H32A,H32B), C41(H41A,H41B),
  C20(H20A,H20B), C26(H26A,H26B)
4.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C33(H33A,H33B,
 H33C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.77824(3) 0.67877(2) 0.60061(3) 0.03010(17) Uani 1 1 d . . . . .
Fe2 Fe 0.76143(3) 0.31915(2) 0.59484(4) 0.03233(17) Uani 1 1 d . . . . .
Cl2 Cl 0.91939(10) 0.68018(11) 0.95938(19) 0.0377(5) Uani 0.7849 1 d . . P A 2
Cl4 Cl 0.61828(19) 0.50230(18) 0.6294(3) 0.0393(5) Uani 0.745 1 d . . P B 2
Cl3 Cl 0.90903(10) 0.49076(12) 0.53093(17) 0.0409(5) Uani 0.745 1 d . . P C 2
Cl1 Cl 0.6368(2) 0.81782(14) 0.7461(3) 0.0473(7) Uani 0.7849 1 d . . P D 2
Cl5 Cl 0.89719(12) 0.32578(15) 0.9521(2) 0.0401(5) Uani 0.745 1 d . . P E 2
Cl6 Cl 0.6201(2) 0.18214(17) 0.7411(3) 0.0481(7) Uani 0.745 1 d . . P F 2
O4 O 0.83584(12) 0.76478(11) 1.04706(16) 0.0322(5) Uani 1 1 d . . . . .
O1 O 0.83823(12) 0.67965(10) 0.74142(16) 0.0309(5) Uani 1 1 d . . . . .
O5 O 0.83300(12) 0.60289(11) 0.57624(17) 0.0343(6) Uani 1 1 d . . . . .
O3 O 0.71696(13) 0.81678(11) 0.96036(17) 0.0336(6) Uani 1 1 d . . . . .
O10 O 0.81623(12) 0.24000(11) 1.04258(16) 0.0332(5) Uani 1 1 d . . . . .
O7 O 0.70122(12) 0.39438(11) 0.60711(17) 0.0349(6) Uani 1 1 d . . . . .
O8 O 0.71272(12) 0.60690(11) 0.61394(17) 0.0349(6) Uani 1 1 d . . . . .
O6 O 0.82134(12) 0.39025(11) 0.56799(17) 0.0349(6) Uani 1 1 d . . . . .
O11 O 0.69932(13) 0.18455(11) 0.95557(17) 0.0346(6) Uani 1 1 d . . . . .
O2 O 0.72170(12) 0.73496(11) 0.65551(16) 0.0335(5) Uani 1 1 d . . . . .
O9 O 0.81910(13) 0.32141(10) 0.73574(17) 0.0334(6) Uani 1 1 d . . . . .
O12 O 0.70373(13) 0.26416(11) 0.64989(16) 0.0360(6) Uani 1 1 d . . . . .
N2 N 0.50804(15) 0.70134(16) 0.5042(2) 0.0404(8) Uani 1 1 d . . . . .
N1 N 0.95069(17) 0.14788(16) 0.7751(2) 0.0472(8) Uani 1 1 d . . . . .
C8 C 0.83161(19) 0.49615(16) 0.5644(3) 0.0355(8) Uani 1 1 d D . . . .
C10 C 0.72784(18) 0.44477(17) 0.5981(2) 0.0333(8) Uani 1 1 d . . . . .
C7 C 0.80476(18) 0.55218(16) 0.5793(2) 0.0328(8) Uani 1 1 d . . . . .
C9 C 0.79879(18) 0.44247(17) 0.5753(2) 0.0327(8) Uani 1 1 d . . . . .
C12 C 0.73380(18) 0.55445(16) 0.6017(2) 0.0323(8) Uani 1 1 d . . . . .
C1 C 0.81240(17) 0.71146(15) 0.7986(2) 0.0289(7) Uani 1 1 d . . . . .
C11 C 0.69854(19) 0.50114(15) 0.6068(3) 0.0341(8) Uani 1 1 d D . . . .
C4 C 0.74358(18) 0.78508(16) 0.9038(2) 0.0314(8) Uani 1 1 d . . . . .
C15 C 0.79177(18) 0.24856(15) 0.9489(2) 0.0306(7) Uani 1 1 d . . . . .
C5 C 0.81105(18) 0.75459(15) 0.9537(2) 0.0298(7) Uani 1 1 d . . . . .
C2 C 0.74546(17) 0.74283(16) 0.7486(2) 0.0302(7) Uani 1 1 d . . . . .
C13 C 0.79309(18) 0.29043(15) 0.7932(2) 0.0319(8) Uani 1 1 d . . . . .
C14 C 0.82239(18) 0.28527(16) 0.8939(2) 0.0311(8) Uani 1 1 d D . . . .
C6 C 0.84256(17) 0.71851(15) 0.8991(2) 0.0305(8) Uani 1 1 d D . . . .
C16 C 0.72568(18) 0.21600(16) 0.8991(2) 0.0326(8) Uani 1 1 d . . . . .
C18 C 0.72727(18) 0.25730(16) 0.7436(2) 0.0324(8) Uani 1 1 d . . . . .
C3 C 0.71349(18) 0.77847(16) 0.8042(2) 0.0336(8) Uani 1 1 d . . . . .
C17 C 0.69611(19) 0.22169(17) 0.7994(3) 0.0372(8) Uani 1 1 d . . . . .
C31 C 0.4450(2) 0.74100(18) 0.5018(3) 0.0466(10) Uani 1 1 d . . . . .
H31A H 0.4316 0.7643 0.4397 0.056 Uiso 1 1 calc R U . . .
H31B H 0.4049 0.7140 0.5007 0.056 Uiso 1 1 calc R U . . .
C35 C 0.4764(2) 0.61669(19) 0.6072(3) 0.0494(10) Uani 1 1 d . . . . .
H35A H 0.4719 0.5836 0.5586 0.059 Uiso 1 1 calc R U . . .
H35B H 0.4297 0.6365 0.5945 0.059 Uiso 1 1 calc R U . . .
C40 C 0.57151(19) 0.74019(18) 0.5062(3) 0.0459(10) Uani 1 1 d . . . . .
H40A H 0.5852 0.7638 0.5681 0.055 Uiso 1 1 calc R U . . .
H40B H 0.6113 0.7128 0.5075 0.055 Uiso 1 1 calc R U . . .
C38 C 0.5401(2) 0.61621(19) 0.4025(3) 0.0509(10) Uani 1 1 d . . . . .
H38A H 0.5473 0.5846 0.4540 0.061 Uiso 1 1 calc R U . . .
H38B H 0.5857 0.6371 0.4110 0.061 Uiso 1 1 calc R U . . .
C39 C 0.5149(3) 0.5868(2) 0.3014(3) 0.0715(15) Uani 1 1 d . . . . .
H39A H 0.5126 0.6176 0.2510 0.107 Uiso 1 1 calc R U . . .
H39B H 0.4679 0.5692 0.2913 0.107 Uiso 1 1 calc R U . . .
H39C H 0.5479 0.5546 0.2969 0.107 Uiso 1 1 calc R U . . .
C34 C 0.5300(2) 0.66268(18) 0.5968(3) 0.0441(9) Uani 1 1 d . . . . .
H34A H 0.5740 0.6408 0.5987 0.053 Uiso 1 1 calc R U . . .
H34B H 0.5412 0.6902 0.6543 0.053 Uiso 1 1 calc R U . . .
C37 C 0.4854(2) 0.66170(18) 0.4127(3) 0.0463(10) Uani 1 1 d . . . . .
H37A H 0.4423 0.6392 0.4127 0.056 Uiso 1 1 calc R U . . .
H37B H 0.4729 0.6885 0.3544 0.056 Uiso 1 1 calc R U . . .
C36 C 0.4998(3) 0.5905(2) 0.7104(3) 0.0699(14) Uani 1 1 d . . . . .
H36A H 0.4662 0.5592 0.7163 0.105 Uiso 1 1 calc R U . . .
H36B H 0.5015 0.6230 0.7580 0.105 Uiso 1 1 calc R U . . .
H36C H 0.5468 0.5723 0.7235 0.105 Uiso 1 1 calc R U . . .
C22 C 0.9853(3) 0.1221(2) 0.7035(3) 0.0644(13) Uani 1 1 d . . . . .
H22A H 1.0320 0.1417 0.7156 0.077 Uiso 1 1 calc R U . . .
H22B H 0.9563 0.1333 0.6363 0.077 Uiso 1 1 calc R U . . .
C19 C 0.9988(2) 0.1357(2) 0.8775(3) 0.0566(11) Uani 1 1 d . . . . .
H19A H 0.9988 0.0913 0.8890 0.068 Uiso 1 1 calc R U . . .
H19B H 1.0473 0.1470 0.8789 0.068 Uiso 1 1 calc R U . . .
C29 C 1.0058(2) 0.2540(2) 0.7690(3) 0.0573(12) Uani 1 1 d . . . . .
H29A H 1.0270 0.2439 0.7166 0.069 Uiso 1 1 calc R U . . .
H29B H 1.0409 0.2445 0.8330 0.069 Uiso 1 1 calc R U . . .
C25 C 0.8805(2) 0.1198(2) 0.7643(4) 0.0644(13) Uani 1 1 d . . . . .
H25A H 0.8584 0.1421 0.8076 0.077 Uiso 1 1 calc R U . . .
H25B H 0.8885 0.0774 0.7890 0.077 Uiso 1 1 calc R U . . .
C23 C 0.9956(3) 0.0538(2) 0.7074(4) 0.0719(14) Uani 1 1 d . . . . .
H23A H 1.0276 0.0421 0.7727 0.086 Uiso 1 1 calc R U . . .
H23B H 0.9496 0.0334 0.6984 0.086 Uiso 1 1 calc R U . . .
C28 C 0.9411(2) 0.2164(2) 0.7566(3) 0.0556(11) Uani 1 1 d . . . . .
H28A H 0.9098 0.2223 0.6887 0.067 Uiso 1 1 calc R U . . .
H28B H 0.9159 0.2328 0.8013 0.067 Uiso 1 1 calc R U . . .
C32 C 0.4551(2) 0.7852(2) 0.5854(4) 0.0667(14) Uani 1 1 d . . . . .
H32A H 0.4996 0.8082 0.5952 0.080 Uiso 1 1 calc R U . . .
H32B H 0.4581 0.7630 0.6468 0.080 Uiso 1 1 calc R U . . .
C41 C 0.5616(2) 0.7842(2) 0.4217(4) 0.0661(13) Uani 1 1 d . . . . .
H41A H 0.5175 0.8076 0.4120 0.079 Uiso 1 1 calc R U . . .
H41B H 0.5580 0.7614 0.3605 0.079 Uiso 1 1 calc R U . . .
C42 C 0.6242(2) 0.8272(2) 0.4445(4) 0.0707(15) Uani 1 1 d . . . . .
H42A H 0.6234 0.8499 0.3851 0.106 Uiso 1 1 calc R U . . .
H42B H 0.6681 0.8037 0.4672 0.106 Uiso 1 1 calc R U . . .
H42C H 0.6215 0.8558 0.4959 0.106 Uiso 1 1 calc R U . . .
C33 C 0.3923(2) 0.8292(2) 0.5608(4) 0.0706(15) Uani 1 1 d . . . . .
H33A H 0.3951 0.8568 0.5082 0.106 Uiso 1 1 calc R U . . .
H33B H 0.3934 0.8530 0.6193 0.106 Uiso 1 1 calc R U . . .
H33C H 0.3482 0.8060 0.5392 0.106 Uiso 1 1 calc R U . . .
C20 C 0.9837(3) 0.1664(2) 0.9613(4) 0.0684(14) Uani 1 1 d . . . . .
H20A H 0.9361 0.1547 0.9636 0.082 Uiso 1 1 calc R U . . .
H20B H 0.9845 0.2111 0.9529 0.082 Uiso 1 1 calc R U . . .
C30 C 0.9880(3) 0.3215(2) 0.7645(4) 0.0743(15) Uani 1 1 d . . . . .
H30A H 0.9561 0.3314 0.6993 0.112 Uiso 1 1 calc R U . . .
H30B H 1.0314 0.3454 0.7769 0.112 Uiso 1 1 calc R U . . .
H30C H 0.9650 0.3311 0.8144 0.112 Uiso 1 1 calc R U . . .
O14 O 0.8607(3) -0.0343(2) 0.7101(6) 0.187(3) Uani 1 1 d . . . . .
C26 C 0.8287(3) 0.1181(3) 0.6631(4) 0.0840(18) Uani 1 1 d . . . . .
H26A H 0.8234 0.1596 0.6348 0.101 Uiso 1 1 calc R U . . .
H26B H 0.8474 0.0916 0.6208 0.101 Uiso 1 1 calc R U . . .
C21 C 1.0378(4) 0.1484(3) 1.0551(4) 0.0898(19) Uani 1 1 d . . . . .
H21A H 1.0850 0.1520 1.0476 0.135 Uiso 1 1 calc R U . . .
H21B H 1.0296 0.1062 1.0709 0.135 Uiso 1 1 calc R U . . .
H21C H 1.0341 0.1751 1.1082 0.135 Uiso 1 1 calc R U . . .
O13 O 0.6658(4) 0.5034(3) 0.9160(7) 0.186(4) Uani 1 1 d . . . . .
C43 C 0.7230(5) 0.5017(3) 0.8958(5) 0.109(3) Uani 1 1 d . . . . .
C27 C 0.7582(3) 0.0951(3) 0.6631(5) 0.098(2) Uani 1 1 d . . . . .
H27A H 0.7284 0.0891 0.5952 0.146 Uiso 1 1 calc R U . . .
H27B H 0.7360 0.1248 0.6955 0.146 Uiso 1 1 calc R U . . .
H27C H 0.7639 0.0563 0.6984 0.146 Uiso 1 1 calc R U . . .
C44 C 0.7519(4) 0.4424(3) 0.8769(5) 0.112(2) Uani 1 1 d . . . . .
H44A H 0.7145 0.4186 0.8312 0.168 Uiso 1 1 calc R U . . .
H44B H 0.7701 0.4201 0.9388 0.168 Uiso 1 1 calc R U . . .
H44C H 0.7903 0.4493 0.8483 0.168 Uiso 1 1 calc R U . . .
C46 C 0.8224(4) -0.0742(3) 0.7215(6) 0.101(2) Uani 1 1 d . . . . .
C45 C 0.7601(4) 0.5584(3) 0.8818(6) 0.113(2) Uani 1 1 d . . . . .
H45A H 0.7954 0.5485 0.8489 0.170 Uiso 1 1 calc R U . . .
H45B H 0.7836 0.5768 0.9459 0.170 Uiso 1 1 calc R U . . .
H45C H 0.7258 0.5872 0.8415 0.170 Uiso 1 1 calc R U . . .
C24 C 1.0266(5) 0.0328(3) 0.6284(6) 0.137(3) Uani 1 1 d . . . . .
H24A H 0.9955 0.0452 0.5640 0.206 Uiso 1 1 calc R U . . .
H24B H 1.0312 -0.0116 0.6307 0.206 Uiso 1 1 calc R U . . .
H24C H 1.0732 0.0513 0.6394 0.206 Uiso 1 1 calc R U . . .
C47 C 0.7832(5) -0.0668(4) 0.7999(5) 0.135(3) Uani 1 1 d . . . . .
H47A H 0.7948 -0.0271 0.8321 0.202 Uiso 1 1 calc R U . . .
H47B H 0.7980 -0.0992 0.8491 0.202 Uiso 1 1 calc R U . . .
H47C H 0.7322 -0.0694 0.7682 0.202 Uiso 1 1 calc R U . . .
C48 C 0.8092(4) -0.1275(3) 0.6591(6) 0.118(3) Uani 1 1 d . . . . .
H48A H 0.7586 -0.1305 0.6244 0.177 Uiso 1 1 calc R U . . .
H48B H 0.8246 -0.1639 0.6994 0.177 Uiso 1 1 calc R U . . .
H48C H 0.8355 -0.1241 0.6113 0.177 Uiso 1 1 calc R U . . .
O16 O 0.5165(8) 0.5661(16) 1.0219(14) 0.290(14) Uani 0.5 1 d . . P G -3
O15 O 0.5619(15) 0.4974(8) 1.0737(15) 0.257(13) Uani 0.5 1 d . . P G 3
F3 F 0.8986(9) 0.4977(9) 0.5573(14) 0.079(7) Uani 0.255 1 d D . P C -2
F2 F 0.9103(9) 0.6975(8) 0.9398(16) 0.054(7) Uani 0.2151 1 d D . P A -2
F5 F 0.8865(10) 0.3116(10) 0.9375(17) 0.078(8) Uani 0.255 1 d D . P E -2
F4 F 0.6356(11) 0.5075(12) 0.626(2) 0.048(7) Uani 0.255 1 d D . P B -2
F1 F 0.6465(14) 0.7988(9) 0.758(2) 0.033(5) Uani 0.2151 1 d . . P D -2
F6 F 0.6293(15) 0.1989(11) 0.7581(18) 0.064(7) Uani 0.255 1 d . . P F -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O4 1.991(2) 4_575 ?
Fe1 O1 2.005(2) . ?
Fe1 O5 2.077(2) . ?
Fe1 O3 2.008(2) 4_575 ?
Fe1 O8 2.092(2) . ?
Fe1 O2 1.984(2) . ?
Fe2 O10 1.981(2) 4_565 ?
Fe2 O7 2.079(2) . ?
Fe2 O6 2.069(2) . ?
Fe2 O11 2.001(2) 4_565 ?
Fe2 O9 1.994(2) . ?
Fe2 O12 1.985(2) . ?
Cl2 C6 1.729(3) . ?
Cl4 C11 1.721(5) . ?
Cl3 C8 1.748(4) . ?
Cl3 F3 0.505(14) . ?
Cl1 C3 1.731(4) . ?
Cl5 C14 1.717(4) . ?
Cl6 C17 1.723(4) . ?
O4 Fe1 1.991(2) 4_576 ?
O4 C5 1.294(4) . ?
O1 C1 1.294(4) . ?
O5 C7 1.254(4) . ?
O3 Fe1 2.008(2) 4_576 ?
O3 C4 1.295(4) . ?
O10 Fe2 1.981(2) 4_566 ?
O10 C15 1.292(4) . ?
O7 C10 1.250(4) . ?
O8 C12 1.256(4) . ?
O6 C9 1.248(4) . ?
O11 Fe2 2.001(2) 4_566 ?
O11 C16 1.288(4) . ?
O2 C2 1.282(4) . ?
O9 C13 1.289(4) . ?
O12 C18 1.288(4) . ?
N2 C31 1.518(5) . ?
N2 C40 1.516(5) . ?
N2 C34 1.521(5) . ?
N2 C37 1.521(5) . ?
N1 C22 1.505(5) . ?
N1 C19 1.510(5) . ?
N1 C25 1.490(5) . ?
N1 C28 1.530(5) . ?
C8 C7 1.383(5) . ?
C8 C9 1.380(5) . ?
C8 F3 1.367(15) . ?
C10 C9 1.541(5) . ?
C10 C11 1.390(5) . ?
C7 C12 1.539(5) . ?
C12 C11 1.378(5) . ?
C1 C2 1.477(4) . ?
C1 C6 1.388(5) . ?
C11 F4 1.363(15) . ?
C4 C5 1.476(5) . ?
C4 C3 1.375(5) . ?
C15 C14 1.389(5) . ?
C15 C16 1.476(5) . ?
C5 C6 1.388(5) . ?
C2 C3 1.398(5) . ?
C13 C14 1.385(5) . ?
C13 C18 1.477(5) . ?
C14 F5 1.366(15) . ?
C6 F2 1.374(15) . ?
C16 C17 1.373(5) . ?
C18 C17 1.389(5) . ?
C3 F1 1.37(2) . ?
C17 F6 1.37(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.505(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.509(6) . ?
C35 C36 1.520(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.513(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.523(6) . ?
C38 C37 1.515(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.514(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.484(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C28 1.495(6) . ?
C29 C30 1.522(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.502(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.513(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.534(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.517(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.496(8) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O14 C46 1.205(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.489(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
O13 C43 1.256(9) . ?
C43 C44 1.481(9) . ?
C43 C45 1.492(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C46 C47 1.554(10) . ?
C46 C48 1.446(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O16 O15 1.80(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
O4 Fe1 O1 98.24(9) 4_575 . ?
O4 Fe1 O5 92.54(9) 4_575 . ?
O4 Fe1 O3 80.32(9) 4_575 4_575 ?
O4 Fe1 O8 162.06(9) 4_575 . ?
O1 Fe1 O5 89.61(9) . . ?
O1 Fe1 O3 176.56(10) . 4_575 ?
O1 Fe1 O8 96.51(9) . . ?
O5 Fe1 O8 77.38(9) . . ?
O3 Fe1 O5 93.57(10) 4_575 . ?
O3 Fe1 O8 85.48(9) 4_575 . ?
O2 Fe1 O4 102.98(10) . 4_575 ?
O2 Fe1 O1 80.39(9) . . ?
O2 Fe1 O5 162.54(10) . . ?
O2 Fe1 O3 96.85(10) . 4_575 ?
O2 Fe1 O8 89.48(10) . . ?
O10 Fe2 O7 161.71(9) 4_565 . ?
O10 Fe2 O6 90.72(10) 4_565 . ?
O10 Fe2 O11 80.94(9) 4_565 4_565 ?
O10 Fe2 O9 100.56(10) 4_565 . ?
O10 Fe2 O12 101.51(10) 4_565 . ?
O6 Fe2 O7 78.09(9) . . ?
O11 Fe2 O7 85.33(9) 4_565 . ?
O11 Fe2 O6 93.60(10) 4_565 . ?
O9 Fe2 O7 93.72(9) . . ?
O9 Fe2 O6 88.92(9) . . ?
O9 Fe2 O11 177.06(10) . 4_565 ?
O12 Fe2 O7 91.96(10) . . ?
O12 Fe2 O6 165.22(10) . . ?
O12 Fe2 O11 96.48(10) . 4_565 ?
O12 Fe2 O9 80.76(9) . . ?
F3 Cl3 C8 35(2) . . ?
C5 O4 Fe1 114.8(2) . 4_576 ?
C1 O1 Fe1 114.2(2) . . ?
C7 O5 Fe1 116.4(2) . . ?
C4 O3 Fe1 114.2(2) . 4_576 ?
C15 O10 Fe2 114.1(2) . 4_566 ?
C10 O7 Fe2 115.0(2) . . ?
C12 O8 Fe1 115.9(2) . . ?
C9 O6 Fe2 115.9(2) . . ?
C16 O11 Fe2 113.5(2) . 4_566 ?
C2 O2 Fe1 114.8(2) . . ?
C13 O9 Fe2 114.3(2) . . ?
C18 O12 Fe2 114.3(2) . . ?
C31 N2 C34 111.0(3) . . ?
C31 N2 C37 106.4(3) . . ?
C40 N2 C31 110.7(3) . . ?
C40 N2 C34 106.2(3) . . ?
C40 N2 C37 111.5(3) . . ?
C37 N2 C34 111.1(3) . . ?
C22 N1 C19 107.8(3) . . ?
C22 N1 C28 108.2(3) . . ?
C19 N1 C28 110.6(3) . . ?
C25 N1 C22 112.3(4) . . ?
C25 N1 C19 109.0(3) . . ?
C25 N1 C28 109.0(3) . . ?
C7 C8 Cl3 121.0(3) . . ?
C9 C8 Cl3 117.3(3) . . ?
C9 C8 C7 121.7(3) . . ?
F3 C8 Cl3 12.3(7) . . ?
F3 C8 C7 114.8(8) . . ?
F3 C8 C9 122.3(9) . . ?
O7 C10 C9 115.8(3) . . ?
O7 C10 C11 125.3(3) . . ?
C11 C10 C9 118.9(3) . . ?
O5 C7 C8 126.0(3) . . ?
O5 C7 C12 115.2(3) . . ?
C8 C7 C12 118.8(3) . . ?
O6 C9 C8 125.6(3) . . ?
O6 C9 C10 115.0(3) . . ?
C8 C9 C10 119.3(3) . . ?
O8 C12 C7 115.1(3) . . ?
O8 C12 C11 125.2(3) . . ?
C11 C12 C7 119.7(3) . . ?
O1 C1 C2 114.7(3) . . ?
O1 C1 C6 125.8(3) . . ?
C6 C1 C2 119.5(3) . . ?
C10 C11 Cl4 117.8(3) . . ?
C12 C11 Cl4 120.8(3) . . ?
C12 C11 C10 121.3(3) . . ?
F4 C11 Cl4 5.1(12) . . ?
F4 C11 C10 122.9(11) . . ?
F4 C11 C12 115.7(11) . . ?
O3 C4 C5 115.2(3) . . ?
O3 C4 C3 124.8(3) . . ?
C3 C4 C5 120.0(3) . . ?
O10 C15 C14 125.4(3) . . ?
O10 C15 C16 115.5(3) . . ?
C14 C15 C16 119.1(3) . . ?
O4 C5 C4 115.2(3) . . ?
O4 C5 C6 125.7(3) . . ?
C6 C5 C4 119.1(3) . . ?
O2 C2 C1 115.7(3) . . ?
O2 C2 C3 125.3(3) . . ?
C3 C2 C1 119.0(3) . . ?
O9 C13 C14 125.6(3) . . ?
O9 C13 C18 115.0(3) . . ?
C14 C13 C18 119.4(3) . . ?
C15 C14 Cl5 119.4(3) . . ?
C13 C14 Cl5 119.5(3) . . ?
C13 C14 C15 121.2(3) . . ?
F5 C14 Cl5 7.1(11) . . ?
F5 C14 C15 119.7(11) . . ?
F5 C14 C13 118.7(11) . . ?
C1 C6 Cl2 120.1(3) . . ?
C1 C6 C5 121.3(3) . . ?
C5 C6 Cl2 118.6(3) . . ?
F2 C6 Cl2 11.8(8) . . ?
F2 C6 C1 117.5(10) . . ?
F2 C6 C5 120.3(11) . . ?
O11 C16 C15 115.4(3) . . ?
O11 C16 C17 124.8(3) . . ?
C17 C16 C15 119.7(3) . . ?
O12 C18 C13 115.5(3) . . ?
O12 C18 C17 125.3(3) . . ?
C17 C18 C13 119.1(3) . . ?
C4 C3 Cl1 119.2(3) . . ?
C4 C3 C2 121.2(3) . . ?
C2 C3 Cl1 119.5(3) . . ?
F1 C3 Cl1 11.2(11) . . ?
F1 C3 C4 121.3(12) . . ?
F1 C3 C2 116.8(12) . . ?
C16 C17 Cl6 119.6(3) . . ?
C16 C17 C18 121.4(3) . . ?
C16 C17 F6 117.9(12) . . ?
C18 C17 Cl6 118.9(3) . . ?
F6 C17 Cl6 10.5(13) . . ?
F6 C17 C18 119.9(12) . . ?
N2 C31 H31A 108.2 . . ?
N2 C31 H31B 108.2 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 N2 116.2(3) . . ?
C32 C31 H31A 108.2 . . ?
C32 C31 H31B 108.2 . . ?
H35A C35 H35B 108.3 . . ?
C34 C35 H35A 109.8 . . ?
C34 C35 H35B 109.8 . . ?
C34 C35 C36 109.3(4) . . ?
C36 C35 H35A 109.8 . . ?
C36 C35 H35B 109.8 . . ?
N2 C40 H40A 108.3 . . ?
N2 C40 H40B 108.3 . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 N2 116.0(3) . . ?
C41 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
H38A C38 H38B 108.3 . . ?
C39 C38 H38A 109.8 . . ?
C39 C38 H38B 109.8 . . ?
C37 C38 H38A 109.8 . . ?
C37 C38 H38B 109.8 . . ?
C37 C38 C39 109.4(4) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C34 H34A 108.4 . . ?
N2 C34 H34B 108.4 . . ?
C35 C34 N2 115.7(3) . . ?
C35 C34 H34A 108.4 . . ?
C35 C34 H34B 108.4 . . ?
H34A C34 H34B 107.4 . . ?
N2 C37 H37A 108.5 . . ?
N2 C37 H37B 108.5 . . ?
C38 C37 N2 115.2(3) . . ?
C38 C37 H37A 108.5 . . ?
C38 C37 H37B 108.5 . . ?
H37A C37 H37B 107.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N1 C22 H22A 108.4 . . ?
N1 C22 H22B 108.4 . . ?
N1 C22 C23 115.7(4) . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 H22A 108.4 . . ?
C23 C22 H22B 108.4 . . ?
N1 C19 H19A 107.7 . . ?
N1 C19 H19B 107.7 . . ?
H19A C19 H19B 107.1 . . ?
C20 C19 N1 118.6(4) . . ?
C20 C19 H19A 107.7 . . ?
C20 C19 H19B 107.7 . . ?
H29A C29 H29B 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 C30 110.6(4) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
N1 C25 H25A 108.0 . . ?
N1 C25 H25B 108.0 . . ?
N1 C25 C26 117.2(4) . . ?
H25A C25 H25B 107.2 . . ?
C26 C25 H25A 108.0 . . ?
C26 C25 H25B 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 C22 110.8(5) . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
N1 C28 H28A 107.9 . . ?
N1 C28 H28B 107.9 . . ?
C29 C28 N1 117.7(3) . . ?
C29 C28 H28A 107.9 . . ?
C29 C28 H28B 107.9 . . ?
H28A C28 H28B 107.2 . . ?
C31 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C31 C32 C33 108.7(4) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.9 . . ?
C33 C32 H32B 109.9 . . ?
C40 C41 H41A 109.9 . . ?
C40 C41 H41B 109.9 . . ?
C40 C41 C42 109.0(4) . . ?
H41A C41 H41B 108.3 . . ?
C42 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.7(4) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C25 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 C25 112.3(5) . . ?
C27 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O13 C43 C44 119.7(8) . . ?
O13 C43 C45 121.7(7) . . ?
C44 C43 C45 118.4(7) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O14 C46 C47 119.8(7) . . ?
O14 C46 C48 120.6(8) . . ?
C48 C46 C47 119.5(6) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Cl3 F3 C8 133(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 O4 C5 C4 -1.7(4) 4_576 . . . ?
Fe1 O4 C5 C6 178.0(3) 4_576 . . . ?
Fe1 O1 C1 C2 -2.3(3) . . . . ?
Fe1 O1 C1 C6 178.6(3) . . . . ?
Fe1 O5 C7 C8 179.4(3) . . . . ?
Fe1 O5 C7 C12 -0.6(4) . . . . ?
Fe1 O3 C4 C5 4.2(4) 4_576 . . . ?
Fe1 O3 C4 C3 -176.0(3) 4_576 . . . ?
Fe1 O8 C12 C7 0.2(4) . . . . ?
Fe1 O8 C12 C11 -179.6(3) . . . . ?
Fe1 O2 C2 C1 2.9(4) . . . . ?
Fe1 O2 C2 C3 -177.6(3) . . . . ?
Fe2 O10 C15 C14 -176.6(3) 4_566 . . . ?
Fe2 O10 C15 C16 3.6(4) 4_566 . . . ?
Fe2 O7 C10 C9 2.4(4) . . . . ?
Fe2 O7 C10 C11 -177.7(3) . . . . ?
Fe2 O6 C9 C8 177.3(3) . . . . ?
Fe2 O6 C9 C10 -3.0(4) . . . . ?
Fe2 O11 C16 C15 -6.5(4) 4_566 . . . ?
Fe2 O11 C16 C17 174.8(3) 4_566 . . . ?
Fe2 O9 C13 C14 -179.2(3) . . . . ?
Fe2 O9 C13 C18 2.3(4) . . . . ?
Fe2 O12 C18 C13 -1.0(4) . . . . ?
Fe2 O12 C18 C17 179.4(3) . . . . ?
Cl3 C8 C7 O5 -4.1(5) . . . . ?
Cl3 C8 C7 C12 175.9(3) . . . . ?
Cl3 C8 C9 O6 3.6(5) . . . . ?
Cl3 C8 C9 C10 -176.0(3) . . . . ?
O4 C5 C6 Cl2 3.4(5) . . . . ?
O4 C5 C6 C1 -178.6(3) . . . . ?
O4 C5 C6 F2 -10.0(10) . . . . ?
O1 C1 C2 O2 -0.4(4) . . . . ?
O1 C1 C2 C3 -179.9(3) . . . . ?
O1 C1 C6 Cl2 -3.1(5) . . . . ?
O1 C1 C6 C5 178.9(3) . . . . ?
O1 C1 C6 F2 10.0(10) . . . . ?
O5 C7 C12 O8 0.3(5) . . . . ?
O5 C7 C12 C11 -179.9(3) . . . . ?
O3 C4 C5 O4 -1.8(4) . . . . ?
O3 C4 C5 C6 178.6(3) . . . . ?
O3 C4 C3 Cl1 3.6(5) . . . . ?
O3 C4 C3 C2 -179.4(3) . . . . ?
O3 C4 C3 F1 -9.1(13) . . . . ?
O10 C15 C14 Cl5 -2.5(5) . . . . ?
O10 C15 C14 C13 178.4(3) . . . . ?
O10 C15 C14 F5 5.7(12) . . . . ?
O10 C15 C16 O11 2.1(4) . . . . ?
O10 C15 C16 C17 -179.2(3) . . . . ?
O7 C10 C9 O6 0.4(4) . . . . ?
O7 C10 C9 C8 -179.9(3) . . . . ?
O7 C10 C11 Cl4 -1.3(5) . . . . ?
O7 C10 C11 C12 175.9(3) . . . . ?
O7 C10 C11 F4 -0.7(17) . . . . ?
O8 C12 C11 Cl4 1.1(6) . . . . ?
O8 C12 C11 C10 -176.1(3) . . . . ?
O8 C12 C11 F4 0.8(16) . . . . ?
O11 C16 C17 Cl6 -3.0(6) . . . . ?
O11 C16 C17 C18 179.0(3) . . . . ?
O11 C16 C17 F6 8.8(14) . . . . ?
O2 C2 C3 Cl1 -1.9(5) . . . . ?
O2 C2 C3 C4 -178.9(3) . . . . ?
O2 C2 C3 F1 10.5(13) . . . . ?
O9 C13 C14 Cl5 3.7(5) . . . . ?
O9 C13 C14 C15 -177.2(3) . . . . ?
O9 C13 C14 F5 -4.4(12) . . . . ?
O9 C13 C18 O12 -0.9(5) . . . . ?
O9 C13 C18 C17 178.7(3) . . . . ?
O12 C18 C17 Cl6 0.7(6) . . . . ?
O12 C18 C17 C16 178.7(3) . . . . ?
O12 C18 C17 F6 -11.4(14) . . . . ?
N2 C31 C32 C33 169.1(4) . . . . ?
N2 C40 C41 C42 169.4(4) . . . . ?
N1 C22 C23 C24 176.6(5) . . . . ?
N1 C19 C20 C21 -179.6(4) . . . . ?
N1 C25 C26 C27 -173.9(4) . . . . ?
C8 C7 C12 O8 -179.7(3) . . . . ?
C8 C7 C12 C11 0.1(5) . . . . ?
C7 C8 C9 O6 -176.3(3) . . . . ?
C7 C8 C9 C10 4.0(5) . . . . ?
C7 C8 F3 Cl3 -123(4) . . . . ?
C7 C12 C11 Cl4 -178.7(3) . . . . ?
C7 C12 C11 C10 4.1(6) . . . . ?
C7 C12 C11 F4 -179.0(16) . . . . ?
C9 C8 C7 O5 175.8(3) . . . . ?
C9 C8 C7 C12 -4.1(5) . . . . ?
C9 C8 F3 Cl3 69(5) . . . . ?
C9 C10 C11 Cl4 178.5(3) . . . . ?
C9 C10 C11 C12 -4.2(5) . . . . ?
C9 C10 C11 F4 179.1(17) . . . . ?
C1 C2 C3 Cl1 177.6(3) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C1 C2 C3 F1 -170.1(12) . . . . ?
C11 C10 C9 O6 -179.5(3) . . . . ?
C11 C10 C9 C8 0.2(5) . . . . ?
C4 C5 C6 Cl2 -177.0(3) . . . . ?
C4 C5 C6 C1 1.0(5) . . . . ?
C4 C5 C6 F2 169.6(9) . . . . ?
C15 C16 C17 Cl6 178.4(3) . . . . ?
C15 C16 C17 C18 0.4(6) . . . . ?
C15 C16 C17 F6 -169.8(14) . . . . ?
C5 C4 C3 Cl1 -176.6(3) . . . . ?
C5 C4 C3 C2 0.4(5) . . . . ?
C5 C4 C3 F1 170.6(12) . . . . ?
C2 C1 C6 Cl2 177.9(3) . . . . ?
C2 C1 C6 C5 -0.1(5) . . . . ?
C2 C1 C6 F2 -168.9(9) . . . . ?
C13 C18 C17 Cl6 -178.9(3) . . . . ?
C13 C18 C17 C16 -0.9(5) . . . . ?
C13 C18 C17 F6 169.0(14) . . . . ?
C14 C15 C16 O11 -177.8(3) . . . . ?
C14 C15 C16 C17 1.0(5) . . . . ?
C14 C13 C18 O12 -179.5(3) . . . . ?
C14 C13 C18 C17 0.1(5) . . . . ?
C6 C1 C2 O2 178.7(3) . . . . ?
C6 C1 C2 C3 -0.8(5) . . . . ?
C16 C15 C14 Cl5 177.3(3) . . . . ?
C16 C15 C14 C13 -1.8(5) . . . . ?
C16 C15 C14 F5 -174.5(12) . . . . ?
C18 C13 C14 Cl5 -177.8(3) . . . . ?
C18 C13 C14 C15 1.3(5) . . . . ?
C18 C13 C14 F5 174.1(12) . . . . ?
C3 C4 C5 O4 178.4(3) . . . . ?
C3 C4 C5 C6 -1.2(5) . . . . ?
C31 N2 C40 C41 -57.9(5) . . . . ?
C31 N2 C34 C35 63.8(4) . . . . ?
C31 N2 C37 C38 -177.5(3) . . . . ?
C40 N2 C31 C32 -57.9(5) . . . . ?
C40 N2 C34 C35 -175.8(3) . . . . ?
C40 N2 C37 C38 61.7(4) . . . . ?
C39 C38 C37 N2 -171.5(3) . . . . ?
C34 N2 C31 C32 59.8(5) . . . . ?
C34 N2 C40 C41 -178.5(4) . . . . ?
C34 N2 C37 C38 -56.6(4) . . . . ?
C37 N2 C31 C32 -179.2(4) . . . . ?
C37 N2 C40 C41 60.3(5) . . . . ?
C37 N2 C34 C35 -54.4(4) . . . . ?
C36 C35 C34 N2 -169.4(3) . . . . ?
C22 N1 C19 C20 168.8(4) . . . . ?
C22 N1 C25 C26 -51.1(6) . . . . ?
C22 N1 C28 C29 -60.8(5) . . . . ?
C19 N1 C22 C23 63.5(5) . . . . ?
C19 N1 C25 C26 -170.5(4) . . . . ?
C19 N1 C28 C29 57.0(5) . . . . ?
C25 N1 C22 C23 -56.6(5) . . . . ?
C25 N1 C19 C20 -69.1(5) . . . . ?
C25 N1 C28 C29 176.8(4) . . . . ?
C28 N1 C22 C23 -176.9(4) . . . . ?
C28 N1 C19 C20 50.7(5) . . . . ?
C28 N1 C25 C26 68.7(5) . . . . ?
C30 C29 C28 N1 -170.6(4) . . . . ?
F3 Cl3 C8 C7 63(5) . . . . ?
F3 Cl3 C8 C9 -117(5) . . . . ?
F3 C8 C7 O5 7.9(11) . . . . ?
F3 C8 C7 C12 -172.1(10) . . . . ?
F3 C8 C9 O6 -9.3(11) . . . . ?
F3 C8 C9 C10 171.1(10) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.615
####################################################################### 
# 
# 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_F-031-d_CCDC-2014819_R1
_database_code_depnum_ccdc_archive 'CCDC 2014819'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-27
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl4.16 F1.84 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl4.16 F1.84 Fe2 N2 O12'
_chemical_formula_weight         1075.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl4.16 F1.84 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.4941(6)
_cell_length_b                   21.1640(13)
_cell_length_c                   12.1914(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.118(6)
_cell_angle_gamma                90
_cell_volume                     2656.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7129
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1600
_cell_measurement_theta_min      1.9490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1115
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.027
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21412
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.537
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0663520000
_diffrn_orient_matrix_UB_12      -0.0020584000
_diffrn_orient_matrix_UB_13      -0.0042041000
_diffrn_orient_matrix_UB_21      -0.0181369000
_diffrn_orient_matrix_UB_22      -0.0011840000
_diffrn_orient_matrix_UB_23      -0.0590983000
_diffrn_orient_matrix_UB_31      0.0034309000
_diffrn_orient_matrix_UB_32      0.0334312000
_diffrn_orient_matrix_UB_33      -0.0023461000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4158
_reflns_number_total             6103
_reflns_odcompleteness_completeness 91.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0534
_refine_ls_restrained_S_all      1.024
_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)+(0.0594P)²+2.5538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1418
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-F1
 1.33 with sigma of 0.02
 C8-F3
 1.33 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(Cl1)
4. Others
 Fixed Sof: Cl1(0.7233) Cl2(0.7233) Cl3(0.6333) F2(0.2767) F3(0.3667) F1(0.2767)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C13(H13A,H13B), C10(H10A,H10B), C16(H16A,H16B), C20(H20A,
 H20B), C17(H17A,H17B), C11(H11A,H11B), C14(H14A,H14B)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.04732(4) 0.31465(2) 0.49420(3) 0.03660(15) Uani 1 1 d . . . . .
Cl1 Cl 0.6670(2) 0.17030(9) 0.40921(15) 0.0469(4) Uani 0.7233 1 d . . P A 2
Cl2 Cl 0.9414(3) 0.32390(13) 0.0771(2) 0.0446(5) Uani 0.7233 1 d . . P B 2
Cl3 Cl 1.3039(3) 0.5191(2) 0.5139(3) 0.0437(5) Uani 0.6333 1 d . . P C 2
O3 O 0.58374(19) 0.18384(10) 0.16037(16) 0.0368(5) Uani 1 1 d . . . . .
O1 O 1.01947(19) 0.31393(10) 0.32790(16) 0.0356(5) Uani 1 1 d . . . . .
O2 O 0.9060(2) 0.25108(10) 0.46523(16) 0.0369(5) Uani 1 1 d . . . . .
O5 O 1.14969(19) 0.39819(10) 0.49173(17) 0.0394(5) Uani 1 1 d . . . . .
O4 O 0.7034(2) 0.24052(10) 0.02307(16) 0.0387(5) Uani 1 1 d . . . . .
O6 O 1.09639(19) 0.61707(10) 0.50665(17) 0.0381(5) Uani 1 1 d . . . . .
N1 N 0.3996(3) 0.35819(14) 0.2608(2) 0.0476(7) Uani 1 1 d . . . . .
C4 C 0.6893(3) 0.21212(14) 0.2055(2) 0.0325(6) Uani 1 1 d . . . . .
C7 C 1.0868(3) 0.44796(16) 0.4970(2) 0.0368(7) Uani 1 1 d . . . . .
C9 C 1.0597(3) 0.56093(16) 0.5046(2) 0.0371(7) Uani 1 1 d . . . . .
C1 C 0.9169(3) 0.28310(14) 0.2826(2) 0.0337(6) Uani 1 1 d . . . . .
C2 C 0.8522(3) 0.24760(14) 0.3601(2) 0.0330(6) Uani 1 1 d . . . . .
C5 C 0.7564(3) 0.24630(14) 0.1276(2) 0.0342(6) Uani 1 1 d . . . . .
C8 C 1.1371(3) 0.50849(16) 0.5040(3) 0.0385(7) Uani 1 1 d D . . . .
C3 C 0.7411(3) 0.21324(15) 0.3192(2) 0.0350(7) Uani 1 1 d D . . . .
C6 C 0.8661(3) 0.28120(15) 0.1688(2) 0.0357(7) Uani 1 1 d D . . . .
C19 C 0.3997(3) 0.28805(18) 0.2368(3) 0.0518(9) Uani 1 1 d . . . . .
H19A H 0.4839 0.2704 0.2750 0.062 Uiso 1 1 calc R U . . .
H19B H 0.3941 0.2822 0.1555 0.062 Uiso 1 1 calc R U . . .
C13 C 0.5172(4) 0.3882(2) 0.2266(3) 0.0613(10) Uani 1 1 d . . . . .
H13A H 0.5229 0.4326 0.2523 0.074 Uiso 1 1 calc R U . . .
H13B H 0.5958 0.3662 0.2665 0.074 Uiso 1 1 calc R U . . .
C10 C 0.2736(4) 0.3864(2) 0.1969(3) 0.0605(10) Uani 1 1 d . . . . .
H10A H 0.2632 0.3735 0.1176 0.073 Uiso 1 1 calc R U . . .
H10B H 0.2006 0.3676 0.2265 0.073 Uiso 1 1 calc R U . . .
C16 C 0.4054(4) 0.37131(19) 0.3839(3) 0.0528(9) Uani 1 1 d . . . . .
H16A H 0.4181 0.4173 0.3963 0.063 Uiso 1 1 calc R U . . .
H16B H 0.3199 0.3604 0.4017 0.063 Uiso 1 1 calc R U . . .
C20 C 0.2916(3) 0.24995(19) 0.2721(3) 0.0524(9) Uani 1 1 d . . . . .
H20A H 0.2886 0.2593 0.3511 0.063 Uiso 1 1 calc R U . . .
H20B H 0.2071 0.2622 0.2257 0.063 Uiso 1 1 calc R U . . .
C17 C 0.5091(4) 0.3371(2) 0.4658(3) 0.0614(10) Uani 1 1 d . . . . .
H17A H 0.5958 0.3460 0.4488 0.074 Uiso 1 1 calc R U . . .
H17B H 0.4940 0.2910 0.4606 0.074 Uiso 1 1 calc R U . . .
C11 C 0.2623(5) 0.4578(2) 0.2015(4) 0.0739(13) Uani 1 1 d . . . . .
H11A H 0.3329 0.4776 0.1701 0.089 Uiso 1 1 calc R U . . .
H11B H 0.2709 0.4717 0.2801 0.089 Uiso 1 1 calc R U . . .
C21 C 0.3140(4) 0.17999(19) 0.2587(4) 0.0644(11) Uani 1 1 d . . . . .
H21A H 0.3114 0.1704 0.1796 0.097 Uiso 1 1 calc R U . . .
H21B H 0.2460 0.1560 0.2852 0.097 Uiso 1 1 calc R U . . .
H21C H 0.3991 0.1683 0.3025 0.097 Uiso 1 1 calc R U . . .
C14 C 0.5196(5) 0.3875(2) 0.1028(4) 0.0784(14) Uani 1 1 d . . . . .
H14A H 0.4409 0.4086 0.0608 0.094 Uiso 1 1 calc R U . . .
H14B H 0.5200 0.3433 0.0761 0.094 Uiso 1 1 calc R U . . .
C18 C 0.5027(4) 0.3605(2) 0.5836(3) 0.0719(12) Uani 1 1 d . . . . .
H18A H 0.4130 0.3577 0.5952 0.108 Uiso 1 1 calc R U . . .
H18B H 0.5321 0.4045 0.5918 0.108 Uiso 1 1 calc R U . . .
H18C H 0.5589 0.3342 0.6390 0.108 Uiso 1 1 calc R U . . .
C15 C 0.6401(6) 0.4216(2) 0.0821(5) 0.1042(19) Uani 1 1 d . . . . .
H15A H 0.6487 0.4154 0.0042 0.156 Uiso 1 1 calc R U . . .
H15B H 0.7169 0.4045 0.1320 0.156 Uiso 1 1 calc R U . . .
H15C H 0.6324 0.4668 0.0968 0.156 Uiso 1 1 calc R U . . .
C12 C 0.1308(6) 0.4785(3) 0.1343(6) 0.119(2) Uani 1 1 d . . . . .
H12A H 0.1236 0.4655 0.0562 0.178 Uiso 1 1 calc R U . . .
H12B H 0.1231 0.5245 0.1382 0.178 Uiso 1 1 calc R U . . .
H12C H 0.0613 0.4586 0.1655 0.178 Uiso 1 1 calc R U . . .
F2 F 0.9297(17) 0.3064(8) 0.0979(13) 0.055(4) Uani 0.2767 1 d D . P B -2
F3 F 1.2666(8) 0.5160(8) 0.4966(14) 0.053(3) Uani 0.3667 1 d D . P C -2
F1 F 0.6761(14) 0.1854(7) 0.3937(11) 0.0469(4) Uani 0.2767 1 d D . P A -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 1.988(2) 4_666 ?
Fe1 O1 1.992(2) . ?
Fe1 O2 1.983(2) . ?
Fe1 O5 2.072(2) . ?
Fe1 O4 1.987(2) 4_666 ?
Fe1 O6 2.087(2) 3_766 ?
Cl1 C3 1.722(3) . ?
Cl2 C6 1.741(3) . ?
Cl3 C8 1.746(4) . ?
O3 Fe1 1.988(2) 4_565 ?
O3 C4 1.286(3) . ?
O1 C1 1.288(3) . ?
O2 C2 1.299(3) . ?
O5 C7 1.251(4) . ?
O4 Fe1 1.987(2) 4_565 ?
O4 C5 1.294(3) . ?
O6 Fe1 2.087(2) 3_766 ?
O6 C9 1.248(4) . ?
N1 C19 1.513(5) . ?
N1 C13 1.516(5) . ?
N1 C10 1.521(4) . ?
N1 C16 1.516(4) . ?
C4 C5 1.477(4) . ?
C4 C3 1.388(4) . ?
C7 C9 1.545(4) 3_766 ?
C7 C8 1.382(4) . ?
C9 C7 1.545(4) 3_766 ?
C9 C8 1.376(4) . ?
C1 C2 1.472(4) . ?
C1 C6 1.388(4) . ?
C2 C3 1.383(4) . ?
C5 C6 1.378(4) . ?
C8 F3 1.389(10) . ?
C3 F1 1.370(10) . ?
C6 F2 1.304(11) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.519(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.514(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.519(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.513(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.513(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.532(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.527(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.518(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
O3 Fe1 O1 177.36(8) 4_666 . ?
O3 Fe1 O5 90.16(9) 4_666 . ?
O3 Fe1 O6 89.47(8) 4_666 3_766 ?
O1 Fe1 O5 88.08(8) . . ?
O1 Fe1 O6 92.07(8) . 3_766 ?
O2 Fe1 O3 100.53(8) . 4_666 ?
O2 Fe1 O1 81.69(8) . . ?
O2 Fe1 O5 161.51(8) . . ?
O2 Fe1 O4 101.28(9) . 4_666 ?
O2 Fe1 O6 87.36(9) . 3_766 ?
O5 Fe1 O6 77.60(8) . 3_766 ?
O4 Fe1 O3 80.74(8) 4_666 4_666 ?
O4 Fe1 O1 97.47(8) 4_666 . ?
O4 Fe1 O5 95.27(9) 4_666 . ?
O4 Fe1 O6 167.93(8) 4_666 3_766 ?
C4 O3 Fe1 114.16(18) . 4_565 ?
C1 O1 Fe1 112.76(18) . . ?
C2 O2 Fe1 112.47(18) . . ?
C7 O5 Fe1 115.93(19) . . ?
C5 O4 Fe1 114.40(19) . 4_565 ?
C9 O6 Fe1 116.07(19) . 3_766 ?
C19 N1 C13 109.1(3) . . ?
C19 N1 C10 108.6(3) . . ?
C19 N1 C16 111.7(3) . . ?
C13 N1 C10 111.6(3) . . ?
C13 N1 C16 108.4(3) . . ?
C16 N1 C10 107.4(3) . . ?
O3 C4 C5 115.5(2) . . ?
O3 C4 C3 125.1(3) . . ?
C3 C4 C5 119.4(3) . . ?
O5 C7 C9 115.5(3) . 3_766 ?
O5 C7 C8 125.8(3) . . ?
C8 C7 C9 118.7(3) . 3_766 ?
O6 C9 C7 114.7(3) . 3_766 ?
O6 C9 C8 126.0(3) . . ?
C8 C9 C7 119.2(3) . 3_766 ?
O1 C1 C2 115.7(2) . . ?
O1 C1 C6 124.9(3) . . ?
C6 C1 C2 119.4(3) . . ?
O2 C2 C1 116.0(3) . . ?
O2 C2 C3 124.2(3) . . ?
C3 C2 C1 119.9(2) . . ?
O4 C5 C4 114.8(2) . . ?
O4 C5 C6 125.5(3) . . ?
C6 C5 C4 119.7(2) . . ?
C7 C8 Cl3 119.3(3) . . ?
C7 C8 F3 118.0(8) . . ?
C9 C8 Cl3 118.7(3) . . ?
C9 C8 C7 122.0(3) . . ?
C9 C8 F3 119.6(8) . . ?
F3 C8 Cl3 7.6(8) . . ?
C4 C3 Cl1 119.3(2) . . ?
C2 C3 Cl1 120.0(2) . . ?
C2 C3 C4 120.7(3) . . ?
F1 C3 Cl1 6.5(8) . . ?
F1 C3 C4 120.3(7) . . ?
F1 C3 C2 118.7(7) . . ?
C1 C6 Cl2 119.5(2) . . ?
C5 C6 Cl2 119.6(2) . . ?
C5 C6 C1 120.9(3) . . ?
F2 C6 Cl2 7.3(9) . . ?
F2 C6 C1 120.3(8) . . ?
F2 C6 C5 118.4(8) . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
N1 C19 C20 116.0(3) . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
N1 C13 H13A 108.3 . . ?
N1 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 N1 116.1(3) . . ?
C14 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
N1 C10 H10A 108.3 . . ?
N1 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N1 116.0(3) . . ?
C11 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
N1 C16 H16A 108.1 . . ?
N1 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N1 116.9(3) . . ?
C17 C16 H16A 108.1 . . ?
C17 C16 H16B 108.1 . . ?
C19 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 C19 110.4(3) . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C16 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
C16 C17 C18 108.0(3) . . ?
H17A C17 H17B 108.4 . . ?
C18 C17 H17A 110.1 . . ?
C18 C17 H17B 110.1 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
C10 C11 C12 109.5(4) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C13 C14 C15 109.6(4) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 O3 C4 C5 6.4(3) 4_565 . . . ?
Fe1 O3 C4 C3 -174.6(2) 4_565 . . . ?
Fe1 O1 C1 C2 -8.3(3) . . . . ?
Fe1 O1 C1 C6 172.1(2) . . . . ?
Fe1 O2 C2 C1 8.8(3) . . . . ?
Fe1 O2 C2 C3 -171.3(2) . . . . ?
Fe1 O5 C7 C9 -4.5(3) . . . 3_766 ?
Fe1 O5 C7 C8 175.5(2) . . . . ?
Fe1 O4 C5 C4 -1.4(3) 4_565 . . . ?
Fe1 O4 C5 C6 179.2(2) 4_565 . . . ?
Fe1 O6 C9 C7 -0.6(3) 3_766 . . 3_766 ?
Fe1 O6 C9 C8 179.6(2) 3_766 . . . ?
O3 C4 C5 O4 -3.4(4) . . . . ?
O3 C4 C5 C6 176.1(3) . . . . ?
O3 C4 C3 Cl1 4.1(4) . . . . ?
O3 C4 C3 C2 -176.9(3) . . . . ?
O3 C4 C3 F1 -3.3(9) . . . . ?
O1 C1 C2 O2 -0.3(4) . . . . ?
O1 C1 C2 C3 179.8(3) . . . . ?
O1 C1 C6 Cl2 -1.1(5) . . . . ?
O1 C1 C6 C5 179.3(3) . . . . ?
O1 C1 C6 F2 7.3(11) . . . . ?
O2 C2 C3 Cl1 -1.2(4) . . . . ?
O2 C2 C3 C4 179.7(3) . . . . ?
O2 C2 C3 F1 6.0(9) . . . . ?
O5 C7 C8 Cl3 -3.5(5) . . . . ?
O5 C7 C8 C9 177.1(3) . . . . ?
O5 C7 C8 F3 5.0(9) . . . . ?
O4 C5 C6 Cl2 1.9(5) . . . . ?
O4 C5 C6 C1 -178.5(3) . . . . ?
O4 C5 C6 F2 -6.3(11) . . . . ?
O6 C9 C8 Cl3 3.4(5) . . . . ?
O6 C9 C8 C7 -177.2(3) . . . . ?
O6 C9 C8 F3 -5.2(9) . . . . ?
N1 C19 C20 C21 -171.9(3) . . . . ?
N1 C13 C14 C15 177.6(4) . . . . ?
N1 C10 C11 C12 -179.6(4) . . . . ?
N1 C16 C17 C18 176.4(3) . . . . ?
C4 C5 C6 Cl2 -177.5(3) . . . . ?
C4 C5 C6 C1 2.1(5) . . . . ?
C4 C5 C6 F2 174.2(10) . . . . ?
C7 C9 C8 Cl3 -176.4(3) 3_766 . . . ?
C7 C9 C8 C7 3.0(5) 3_766 . . . ?
C7 C9 C8 F3 175.0(8) 3_766 . . . ?
C9 C7 C8 Cl3 176.4(3) 3_766 . . . ?
C9 C7 C8 C9 -2.9(5) 3_766 . . . ?
C9 C7 C8 F3 -175.1(8) 3_766 . . . ?
C1 C2 C3 Cl1 178.6(2) . . . . ?
C1 C2 C3 C4 -0.4(4) . . . . ?
C1 C2 C3 F1 -174.1(8) . . . . ?
C2 C1 C6 Cl2 179.2(3) . . . . ?
C2 C1 C6 C5 -0.3(4) . . . . ?
C2 C1 C6 F2 -172.4(10) . . . . ?
C5 C4 C3 Cl1 -176.9(2) . . . . ?
C5 C4 C3 C2 2.1(4) . . . . ?
C5 C4 C3 F1 175.7(8) . . . . ?
C3 C4 C5 O4 177.5(3) . . . . ?
C3 C4 C5 C6 -3.0(4) . . . . ?
C6 C1 C2 O2 179.3(3) . . . . ?
C6 C1 C2 C3 -0.6(4) . . . . ?
C19 N1 C13 C14 65.9(4) . . . . ?
C19 N1 C10 C11 -174.0(3) . . . . ?
C19 N1 C16 C17 49.7(4) . . . . ?
C13 N1 C19 C20 176.8(3) . . . . ?
C13 N1 C10 C11 -53.7(4) . . . . ?
C13 N1 C16 C17 -70.5(4) . . . . ?
C10 N1 C19 C20 -61.3(4) . . . . ?
C10 N1 C13 C14 -54.1(4) . . . . ?
C10 N1 C16 C17 168.6(3) . . . . ?
C16 N1 C19 C20 57.0(4) . . . . ?
C16 N1 C13 C14 -172.3(3) . . . . ?
C16 N1 C10 C11 65.1(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.571
####################################################################### 
# 
# 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_F-012_CCDC-2014814_R1
_database_code_depnum_ccdc_archive 'CCDC 2014814'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-08-01
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 Cl5.31 F0.69 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl5.31 F0.69 Fe2 N2 O15'
_chemical_formula_weight         1228.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl5.31 F0.69 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.1163(7)
_cell_length_b                   21.8555(5)
_cell_length_c                   14.3929(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.051(4)
_cell_angle_gamma                90
_cell_volume                     6016.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19507
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1080
_cell_measurement_theta_min      1.7950
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2562
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42236
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.756
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_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   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0261935000
_diffrn_orient_matrix_UB_12      0.0174994000
_diffrn_orient_matrix_UB_13      -0.0339602000
_diffrn_orient_matrix_UB_21      -0.0261013000
_diffrn_orient_matrix_UB_22      -0.0192819000
_diffrn_orient_matrix_UB_23      0.0077423000
_diffrn_orient_matrix_UB_31      -0.0024089000
_diffrn_orient_matrix_UB_32      0.0193645000
_diffrn_orient_matrix_UB_33      0.0384380000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8114
_reflns_number_total             10859
_reflns_odcompleteness_completeness 85.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.05
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         10859
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.024
_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)+(0.0785P)²+8.0394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1492
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-F3
 1.33 with sigma of 0.011
 C17-F6
 1.33 with sigma of 0.02
 C3-F1
 1.33 with sigma of 0.02
 C14-F5
 1.33 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C11-F4
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F3) = Uanis(Cl3)
Uanis(F5) = Uanis(Cl5)
Uanis(F2) = Uanis(Cl2)
Uanis(Cl6) = Uanis(F6)
Uanis(F1) = Uanis(Cl1)
Uanis(F4) = Uanis(Cl4)
4. Others
 Fixed Sof: Cl1(0.915) Cl6(0.88) Cl3(0.86) Cl4(0.86) Cl2(0.915) Cl5(0.88)
 O15(0.5) O16(0.5) F4(0.14) F1(0.085) F5(0.12) F3(0.14) F6(0.12) F2(0.085)
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C28(H28A,H28B), C37(H37A,H37B), C31(H31A,H31B), C19(H19A,
 H19B), C22(H22A,H22B), C34(H34A,H34B), C29(H29A,H29B), C25(H25A,H25B),
 C32(H32A,H32B), C20(H20A,H20B), C35(H35A,H35B), C38(H38A,H38B), C41(H41A,H41B),
  C23(H23A,H23B), C26(H26A,H26B)
5.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C39(H39A,H39B,H39C), C42(H42A,H42B,
 H42C), C36(H36A,H36B,H36C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C),
 C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.72157(2) 0.67984(2) 0.39556(3) 0.01581(13) Uani 1 1 d . . . . .
Fe2 Fe 0.73990(2) 0.31798(2) 0.40770(3) 0.01616(13) Uani 1 1 d . . . . .
Cl1 Cl 0.58052(6) 0.82034(5) 0.53682(8) 0.0209(2) Uani 0.915 1 d . . P A 2
Cl6 Cl 0.60307(6) 0.17442(6) 0.55017(10) 0.0173(2) Uani 0.88 1 d . . P B 2
Cl3 Cl 0.88073(5) 0.50295(7) 0.37054(12) 0.0190(2) Uani 0.86 1 d . . P C 2
Cl4 Cl 0.59255(6) 0.49121(5) 0.46782(9) 0.0205(3) Uani 0.86 1 d . . P D 2
Cl2 Cl 0.86355(6) 0.68384(5) 0.74956(9) 0.0263(3) Uani 0.915 1 d . . P E 2
Cl5 Cl 0.88147(7) 0.31848(6) 0.76116(10) 0.0245(3) Uani 0.88 1 d . . P F 2
O12 O 0.68561(11) 0.25836(9) 0.45996(15) 0.0155(5) Uani 1 1 d . . . . .
O2 O 0.66489(11) 0.73695(10) 0.44886(15) 0.0158(5) Uani 1 1 d . . . . .
O4 O 0.77770(11) 0.76411(9) 0.84051(15) 0.0157(5) Uani 1 1 d . . . . .
O10 O 0.79647(11) 0.23802(10) 0.85332(15) 0.0160(5) Uani 1 1 d . . . . .
O1 O 0.78292(11) 0.68495(10) 0.53543(16) 0.0169(5) Uani 1 1 d . . . . .
O5 O 0.78616(11) 0.60762(9) 0.38364(15) 0.0160(5) Uani 1 1 d . . . . .
O9 O 0.80163(11) 0.31449(10) 0.54671(15) 0.0168(5) Uani 1 1 d . . . . .
O7 O 0.68061(11) 0.38928(10) 0.43411(16) 0.0168(5) Uani 1 1 d . . . . .
O6 O 0.79906(11) 0.39355(9) 0.39497(15) 0.0157(5) Uani 1 1 d . . . . .
O8 O 0.66778(11) 0.60378(9) 0.42118(16) 0.0169(5) Uani 1 1 d . . . . .
O3 O 0.66177(11) 0.81976(9) 0.75437(15) 0.0156(5) Uani 1 1 d . . . . .
O11 O 0.68244(11) 0.17977(9) 0.76687(15) 0.0151(5) Uani 1 1 d . . . . .
N1 N 0.45218(14) 0.64834(13) 0.2722(2) 0.0211(6) Uani 1 1 d . . . . .
N2 N 1.00874(14) 0.20063(13) 1.00707(19) 0.0197(6) Uani 1 1 d . . . . .
C13 C 0.77521(16) 0.28391(14) 0.6033(2) 0.0139(7) Uani 1 1 d . . . . .
C15 C 0.77335(16) 0.24398(14) 0.7592(2) 0.0140(7) Uani 1 1 d . . . . .
C16 C 0.70793(16) 0.21060(13) 0.7095(2) 0.0128(6) Uani 1 1 d . . . . .
C5 C 0.75432(16) 0.75732(14) 0.7466(2) 0.0141(7) Uani 1 1 d . . . . .
C18 C 0.70970(16) 0.25114(14) 0.5540(2) 0.0141(7) Uani 1 1 d . . . . .
C2 C 0.68967(16) 0.74693(14) 0.5422(2) 0.0134(6) Uani 1 1 d . . . . .
C1 C 0.75662(16) 0.71614(14) 0.5915(2) 0.0140(7) Uani 1 1 d . . . . .
C9 C 0.77296(16) 0.44466(14) 0.4037(2) 0.0148(7) Uani 1 1 d . . . . .
C4 C 0.68770(16) 0.78910(13) 0.6970(2) 0.0130(6) Uani 1 1 d . . . . .
C17 C 0.67876(16) 0.21446(14) 0.6087(2) 0.0155(7) Uani 1 1 d D . . . .
C3 C 0.65810(15) 0.78306(14) 0.5962(2) 0.0148(7) Uani 1 1 d D . . . .
C14 C 0.80484(16) 0.27915(15) 0.7043(2) 0.0178(7) Uani 1 1 d D . . . .
C10 C 0.70271(16) 0.44216(14) 0.4254(2) 0.0157(7) Uani 1 1 d . . . . .
C12 C 0.69575(16) 0.55223(14) 0.4194(2) 0.0152(7) Uani 1 1 d . . . . .
C7 C 0.76605(16) 0.55503(14) 0.3975(2) 0.0159(7) Uani 1 1 d . . . . .
C40 C 0.94594(17) 0.23995(15) 1.0048(3) 0.0234(8) Uani 1 1 d . . . . .
H40A H 0.9313 0.2625 0.9420 0.028 Uiso 1 1 calc R U . . .
H40B H 0.9070 0.2125 1.0055 0.028 Uiso 1 1 calc R U . . .
C6 C 0.78637(16) 0.72230(14) 0.6922(2) 0.0177(7) Uani 1 1 d D . . . .
C28 C 0.44082(18) 0.71659(15) 0.2523(3) 0.0240(8) Uani 1 1 d . . . . .
H28A H 0.4102 0.7219 0.1842 0.029 Uiso 1 1 calc R U . . .
H28B H 0.4154 0.7330 0.2958 0.029 Uiso 1 1 calc R U . . .
C37 C 1.07147(17) 0.24009(16) 1.0088(3) 0.0244(8) Uani 1 1 d . . . . .
H37A H 1.0858 0.2632 1.0710 0.029 Uiso 1 1 calc R U . . .
H37B H 1.1107 0.2126 1.0090 0.029 Uiso 1 1 calc R U . . .
C8 C 0.80109(17) 0.50105(14) 0.3932(2) 0.0177(7) Uani 1 1 d D . . . .
C11 C 0.66954(17) 0.49610(14) 0.4362(2) 0.0189(7) Uani 1 1 d D . . . .
C31 C 1.03139(18) 0.16174(15) 1.0993(2) 0.0222(8) Uani 1 1 d . . . . .
H31A H 1.0746 0.1395 1.1007 0.027 Uiso 1 1 calc R U . . .
H31B H 1.0432 0.1894 1.1566 0.027 Uiso 1 1 calc R U . . .
C19 C 0.50107(19) 0.63685(16) 0.3742(2) 0.0239(8) Uani 1 1 d . . . . .
H19A H 0.5021 0.5922 0.3865 0.029 Uiso 1 1 calc R U . . .
H19B H 0.5487 0.6490 0.3754 0.029 Uiso 1 1 calc R U . . .
C22 C 0.48578(19) 0.62140(16) 0.2004(3) 0.0245(8) Uani 1 1 d . . . . .
H22A H 0.4557 0.6309 0.1333 0.029 Uiso 1 1 calc R U . . .
H22B H 0.5313 0.6419 0.2101 0.029 Uiso 1 1 calc R U . . .
C34 C 0.98644(19) 0.16101(16) 0.9157(3) 0.0247(8) Uani 1 1 d . . . . .
H34A H 0.9438 0.1382 0.9151 0.030 Uiso 1 1 calc R U . . .
H34B H 0.9739 0.1882 0.8578 0.030 Uiso 1 1 calc R U . . .
C29 C 0.50627(18) 0.75494(16) 0.2662(3) 0.0251(8) Uani 1 1 d . . . . .
H29A H 0.5401 0.7468 0.3314 0.030 Uiso 1 1 calc R U . . .
H29B H 0.5286 0.7440 0.2161 0.030 Uiso 1 1 calc R U . . .
C25 C 0.38199(18) 0.61934(16) 0.2624(3) 0.0278(8) Uani 1 1 d . . . . .
H25A H 0.3599 0.6422 0.3044 0.033 Uiso 1 1 calc R U . . .
H25B H 0.3901 0.5770 0.2879 0.033 Uiso 1 1 calc R U . . .
C32 C 0.9779(2) 0.11552(16) 1.1099(3) 0.0267(8) Uani 1 1 d . . . . .
H32A H 0.9728 0.0823 1.0615 0.032 Uiso 1 1 calc R U . . .
H32B H 0.9319 0.1356 1.0976 0.032 Uiso 1 1 calc R U . . .
C20 C 0.4851(2) 0.66852(17) 0.4581(3) 0.0300(9) Uani 1 1 d . . . . .
H20A H 0.4384 0.6561 0.4608 0.036 Uiso 1 1 calc R U . . .
H20B H 0.4852 0.7134 0.4493 0.036 Uiso 1 1 calc R U . . .
C35 C 1.0405(2) 0.11549(17) 0.9054(3) 0.0287(8) Uani 1 1 d . . . . .
H35A H 1.0477 0.0834 0.9562 0.034 Uiso 1 1 calc R U . . .
H35B H 1.0856 0.1366 0.9145 0.034 Uiso 1 1 calc R U . . .
C30 C 0.4865(2) 0.82210(17) 0.2573(3) 0.0323(9) Uani 1 1 d . . . . .
H30A H 0.4524 0.8297 0.1931 0.048 Uiso 1 1 calc R U . . .
H30B H 0.5284 0.8469 0.2645 0.048 Uiso 1 1 calc R U . . .
H30C H 0.4660 0.8331 0.3086 0.048 Uiso 1 1 calc R U . . .
C38 C 1.0612(2) 0.28502(19) 0.9261(3) 0.0380(10) Uani 1 1 d . . . . .
H38A H 1.0179 0.3090 0.9178 0.046 Uiso 1 1 calc R U . . .
H38B H 1.0565 0.2628 0.8645 0.046 Uiso 1 1 calc R U . . .
C33 C 1.0021(2) 0.08902(18) 1.2134(3) 0.0375(10) Uani 1 1 d . . . . .
H33A H 0.9687 0.0578 1.2197 0.056 Uiso 1 1 calc R U . . .
H33B H 1.0046 0.1218 1.2608 0.056 Uiso 1 1 calc R U . . .
H33C H 1.0484 0.0705 1.2260 0.056 Uiso 1 1 calc R U . . .
O13 O 0.3659(2) 0.46517(17) 0.2250(4) 0.0910(15) Uani 1 1 d . . . . .
C41 C 0.9563(2) 0.28563(19) 1.0865(3) 0.0382(10) Uani 1 1 d . . . . .
H41A H 0.9995 0.3095 1.0942 0.046 Uiso 1 1 calc R U . . .
H41B H 0.9611 0.2640 1.1487 0.046 Uiso 1 1 calc R U . . .
C39 C 1.1244(2) 0.32801(18) 0.9497(4) 0.0407(11) Uani 1 1 d . . . . .
H39A H 1.1210 0.3541 0.8931 0.061 Uiso 1 1 calc R U . . .
H39B H 1.1674 0.3038 0.9653 0.061 Uiso 1 1 calc R U . . .
H39C H 1.1251 0.3536 1.0059 0.061 Uiso 1 1 calc R U . . .
C42 C 0.8932(2) 0.32870(18) 1.0626(4) 0.0415(11) Uani 1 1 d . . . . .
H42A H 0.8924 0.3541 1.0061 0.062 Uiso 1 1 calc R U . . .
H42B H 0.8967 0.3551 1.1190 0.062 Uiso 1 1 calc R U . . .
H42C H 0.8501 0.3045 1.0473 0.062 Uiso 1 1 calc R U . . .
C36 C 1.0154(2) 0.08625(19) 0.8040(3) 0.0410(11) Uani 1 1 d . . . . .
H36A H 1.0114 0.1178 0.7542 0.061 Uiso 1 1 calc R U . . .
H36B H 0.9697 0.0671 0.7942 0.061 Uiso 1 1 calc R U . . .
H36C H 1.0491 0.0551 0.7987 0.061 Uiso 1 1 calc R U . . .
C23 C 0.4978(2) 0.55311(17) 0.2084(3) 0.0324(9) Uani 1 1 d . . . . .
H23A H 0.4532 0.5319 0.2022 0.039 Uiso 1 1 calc R U . . .
H23B H 0.5312 0.5430 0.2731 0.039 Uiso 1 1 calc R U . . .
C21 C 0.5412(2) 0.65028(18) 0.5522(3) 0.0364(10) Uani 1 1 d . . . . .
H21A H 0.5359 0.6069 0.5656 0.055 Uiso 1 1 calc R U . . .
H21B H 0.5362 0.6751 0.6064 0.055 Uiso 1 1 calc R U . . .
H21C H 0.5875 0.6571 0.5451 0.055 Uiso 1 1 calc R U . . .
C26 C 0.3309(2) 0.61700(19) 0.1596(3) 0.0407(11) Uani 1 1 d . . . . .
H26A H 0.3490 0.5893 0.1186 0.049 Uiso 1 1 calc R U . . .
H26B H 0.3255 0.6583 0.1301 0.049 Uiso 1 1 calc R U . . .
C27 C 0.2600(2) 0.59391(19) 0.1631(3) 0.0439(11) Uani 1 1 d . . . . .
H27A H 0.2287 0.5881 0.0964 0.066 Uiso 1 1 calc R U . . .
H27B H 0.2397 0.6239 0.1970 0.066 Uiso 1 1 calc R U . . .
H27C H 0.2662 0.5548 0.1982 0.066 Uiso 1 1 calc R U . . .
C43 C 0.3247(2) 0.4265(2) 0.2296(4) 0.0489(12) Uani 1 1 d . . . . .
C45 C 0.2856(3) 0.4323(2) 0.3021(4) 0.0584(14) Uani 1 1 d . . . . .
H45A H 0.2974 0.3977 0.3477 0.088 Uiso 1 1 calc R U . . .
H45B H 0.2352 0.4321 0.2678 0.088 Uiso 1 1 calc R U . . .
H45C H 0.2985 0.4706 0.3384 0.088 Uiso 1 1 calc R U . . .
C48 C 0.7518(3) 0.0577(2) 0.6254(4) 0.0644(15) Uani 1 1 d . . . . .
H48A H 0.7649 0.0631 0.6964 0.097 Uiso 1 1 calc R U . . .
H48B H 0.7007 0.0583 0.5976 0.097 Uiso 1 1 calc R U . . .
H48C H 0.7717 0.0911 0.5970 0.097 Uiso 1 1 calc R U . . .
C46 C 0.7790(3) -0.0016(2) 0.6029(4) 0.0671(17) Uani 1 1 d . . . . .
O14 O 0.8328(3) -0.0038(2) 0.5813(5) 0.135(3) Uani 1 1 d . . . . .
C24 C 0.5268(4) 0.5316(2) 0.1284(4) 0.0708(17) Uani 1 1 d . . . . .
H24A H 0.4925 0.5397 0.0644 0.106 Uiso 1 1 calc R U . . .
H24B H 0.5363 0.4876 0.1355 0.106 Uiso 1 1 calc R U . . .
H24C H 0.5702 0.5537 0.1335 0.106 Uiso 1 1 calc R U . . .
C47 C 0.7416(3) -0.0586(3) 0.6160(5) 0.0754(17) Uani 1 1 d . . . . .
H47A H 0.7492 -0.0655 0.6858 0.113 Uiso 1 1 calc R U . . .
H47B H 0.7598 -0.0935 0.5887 0.113 Uiso 1 1 calc R U . . .
H47C H 0.6915 -0.0540 0.5822 0.113 Uiso 1 1 calc R U . . .
C44 C 0.3132(3) 0.3713(3) 0.1663(4) 0.0729(17) Uani 1 1 d . . . . .
H44A H 0.3398 0.3753 0.1199 0.109 Uiso 1 1 calc R U . . .
H44B H 0.2634 0.3674 0.1303 0.109 Uiso 1 1 calc R U . . .
H44C H 0.3290 0.3349 0.2069 0.109 Uiso 1 1 calc R U . . .
O15 O 1.0604(13) 0.5027(8) 1.0691(14) 0.228(11) Uani 0.5 1 d . . P G -3
O16 O 1.0158(8) 0.4328(13) 1.0208(14) 0.257(11) Uani 0.5 1 d . . P G 3
F4 F 0.6046(9) 0.4977(10) 0.4494(17) 0.0205(3) Uani 0.14 1 d D . P D -2
F1 F 0.5935(12) 0.8052(15) 0.554(2) 0.0209(2) Uani 0.085 1 d D . P A -2
F5 F 0.8683(12) 0.3058(14) 0.749(2) 0.0245(3) Uani 0.12 1 d D . P F -2
F3 F 0.8629(9) 0.5041(12) 0.372(2) 0.0190(2) Uani 0.14 1 d D . P C -2
F6 F 0.6189(11) 0.1835(13) 0.563(2) 0.0173(2) Uani 0.12 1 d D . P B -2
F2 F 0.8490(14) 0.6979(18) 0.739(3) 0.0263(3) Uani 0.085 1 d D . P E -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.997(2) . ?
Fe1 O4 1.989(2) 4_575 ?
Fe1 O1 2.012(2) . ?
Fe1 O5 2.085(2) . ?
Fe1 O8 2.078(2) . ?
Fe1 O3 2.015(2) 4_575 ?
Fe2 O12 1.991(2) . ?
Fe2 O10 1.990(2) 4_565 ?
Fe2 O9 2.003(2) . ?
Fe2 O7 2.068(2) . ?
Fe2 O6 2.077(2) . ?
Fe2 O11 1.999(2) 4_565 ?
Cl1 C3 1.733(3) . ?
Cl6 C17 1.732(3) . ?
Cl3 C8 1.732(3) . ?
Cl4 C11 1.748(3) . ?
Cl2 C6 1.733(3) . ?
Cl5 C14 1.733(3) . ?
O12 C18 1.298(4) . ?
O2 C2 1.299(4) . ?
O4 Fe1 1.989(2) 4_576 ?
O4 C5 1.295(4) . ?
O10 Fe2 1.989(2) 4_566 ?
O10 C15 1.296(4) . ?
O1 C1 1.289(4) . ?
O5 C7 1.255(4) . ?
O9 C13 1.289(4) . ?
O7 C10 1.258(4) . ?
O6 C9 1.257(4) . ?
O8 C12 1.263(4) . ?
O3 Fe1 2.015(2) 4_576 ?
O3 C4 1.292(4) . ?
O11 Fe2 1.999(2) 4_566 ?
O11 C16 1.289(4) . ?
N1 C28 1.523(4) . ?
N1 C19 1.514(4) . ?
N1 C22 1.518(4) . ?
N1 C25 1.514(4) . ?
N2 C40 1.520(4) . ?
N2 C37 1.522(4) . ?
N2 C31 1.522(4) . ?
N2 C34 1.521(4) . ?
C13 C18 1.474(4) . ?
C13 C14 1.393(4) . ?
C15 C16 1.481(4) . ?
C15 C14 1.388(4) . ?
C16 C17 1.388(4) . ?
C5 C4 1.481(4) . ?
C5 C6 1.389(4) . ?
C18 C17 1.398(4) . ?
C2 C1 1.476(4) . ?
C2 C3 1.391(4) . ?
C1 C6 1.392(5) . ?
C9 C10 1.541(4) . ?
C9 C8 1.383(4) . ?
C4 C3 1.394(4) . ?
C17 F6 1.361(15) . ?
C3 F1 1.343(17) . ?
C14 F5 1.368(16) . ?
C10 C11 1.387(4) . ?
C12 C7 1.543(4) . ?
C12 C11 1.386(4) . ?
C7 C8 1.385(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.508(5) . ?
C6 F2 1.343(18) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.521(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.507(5) . ?
C8 F3 1.369(10) . ?
C11 F4 1.377(15) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.518(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.510(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.511(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.515(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.516(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.518(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.522(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.528(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.532(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O13 C43 1.200(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.531(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.517(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.527(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C43 C45 1.493(7) . ?
C43 C44 1.486(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C46 1.482(7) . ?
C46 O14 1.217(7) . ?
C46 C47 1.496(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O15 O16 1.80(2) . ?

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
O2 Fe1 O1 80.05(9) . . ?
O2 Fe1 O5 161.67(9) . . ?
O2 Fe1 O8 92.35(9) . . ?
O2 Fe1 O3 98.70(9) . 4_575 ?
O4 Fe1 O2 103.31(9) 4_575 . ?
O4 Fe1 O1 96.69(9) 4_575 . ?
O4 Fe1 O5 89.33(9) 4_575 . ?
O4 Fe1 O8 162.62(9) 4_575 . ?
O4 Fe1 O3 80.26(9) 4_575 4_575 ?
O1 Fe1 O5 85.39(8) . . ?
O1 Fe1 O8 93.36(9) . . ?
O1 Fe1 O3 176.38(9) . 4_575 ?
O8 Fe1 O5 77.35(8) . . ?
O3 Fe1 O5 96.47(9) 4_575 . ?
O3 Fe1 O8 90.08(8) 4_575 . ?
O12 Fe2 O9 80.82(9) . . ?
O12 Fe2 O7 90.49(9) . . ?
O12 Fe2 O6 161.82(9) . . ?
O12 Fe2 O11 100.76(9) . 4_565 ?
O10 Fe2 O12 101.16(9) 4_565 . ?
O10 Fe2 O9 96.68(9) 4_565 . ?
O10 Fe2 O7 165.64(9) 4_565 . ?
O10 Fe2 O6 92.36(9) 4_565 . ?
O10 Fe2 O11 80.66(8) 4_565 4_565 ?
O9 Fe2 O7 93.41(9) . . ?
O9 Fe2 O6 85.62(8) . . ?
O7 Fe2 O6 78.22(8) . . ?
O11 Fe2 O9 177.11(9) 4_565 . ?
O11 Fe2 O7 89.01(8) 4_565 . ?
O11 Fe2 O6 93.33(9) 4_565 . ?
C18 O12 Fe2 113.71(19) . . ?
C2 O2 Fe1 114.88(19) . . ?
C5 O4 Fe1 114.77(19) . 4_576 ?
C15 O10 Fe2 114.18(19) . 4_566 ?
C1 O1 Fe1 114.37(19) . . ?
C7 O5 Fe1 116.14(19) . . ?
C13 O9 Fe2 113.69(19) . . ?
C10 O7 Fe2 115.61(19) . . ?
C9 O6 Fe2 115.4(2) . . ?
C12 O8 Fe1 116.8(2) . . ?
C4 O3 Fe1 114.41(19) . 4_576 ?
C16 O11 Fe2 114.64(19) . 4_566 ?
C19 N1 C28 111.1(3) . . ?
C19 N1 C22 107.7(3) . . ?
C22 N1 C28 108.9(2) . . ?
C25 N1 C28 108.1(2) . . ?
C25 N1 C19 109.1(3) . . ?
C25 N1 C22 111.9(3) . . ?
C40 N2 C37 111.1(3) . . ?
C40 N2 C31 110.9(3) . . ?
C40 N2 C34 106.4(2) . . ?
C37 N2 C31 106.2(2) . . ?
C34 N2 C37 111.0(3) . . ?
C34 N2 C31 111.4(3) . . ?
O9 C13 C18 115.4(3) . . ?
O9 C13 C14 124.8(3) . . ?
C14 C13 C18 119.7(3) . . ?
O10 C15 C16 115.6(3) . . ?
O10 C15 C14 124.9(3) . . ?
C14 C15 C16 119.5(3) . . ?
O11 C16 C15 114.8(3) . . ?
O11 C16 C17 125.3(3) . . ?
C17 C16 C15 119.9(3) . . ?
O4 C5 C4 115.5(3) . . ?
O4 C5 C6 124.8(3) . . ?
C6 C5 C4 119.7(3) . . ?
O12 C18 C13 115.6(3) . . ?
O12 C18 C17 124.7(3) . . ?
C17 C18 C13 119.7(3) . . ?
O2 C2 C1 114.9(3) . . ?
O2 C2 C3 125.3(3) . . ?
C3 C2 C1 119.8(3) . . ?
O1 C1 C2 115.5(3) . . ?
O1 C1 C6 125.1(3) . . ?
C6 C1 C2 119.4(3) . . ?
O6 C9 C10 115.2(3) . . ?
O6 C9 C8 125.7(3) . . ?
C8 C9 C10 119.0(3) . . ?
O3 C4 C5 114.8(3) . . ?
O3 C4 C3 126.0(3) . . ?
C3 C4 C5 119.2(3) . . ?
C16 C17 Cl6 120.1(2) . . ?
C16 C17 C18 120.4(3) . . ?
C18 C17 Cl6 119.6(2) . . ?
F6 C17 Cl6 0.6(14) . . ?
F6 C17 C16 120.2(13) . . ?
F6 C17 C18 119.4(13) . . ?
C2 C3 Cl1 119.3(2) . . ?
C2 C3 C4 120.9(3) . . ?
C4 C3 Cl1 119.9(2) . . ?
F1 C3 Cl1 8.1(15) . . ?
F1 C3 C2 119.9(16) . . ?
F1 C3 C4 118.5(16) . . ?
C13 C14 Cl5 119.1(2) . . ?
C15 C14 Cl5 120.1(2) . . ?
C15 C14 C13 120.8(3) . . ?
F5 C14 Cl5 4.8(14) . . ?
F5 C14 C13 119.5(13) . . ?
F5 C14 C15 119.5(13) . . ?
O7 C10 C9 115.3(3) . . ?
O7 C10 C11 124.9(3) . . ?
C11 C10 C9 119.7(3) . . ?
O8 C12 C7 114.3(3) . . ?
O8 C12 C11 126.2(3) . . ?
C11 C12 C7 119.6(3) . . ?
O5 C7 C12 115.5(3) . . ?
O5 C7 C8 125.4(3) . . ?
C8 C7 C12 119.1(3) . . ?
N2 C40 H40A 108.2 . . ?
N2 C40 H40B 108.2 . . ?
H40A C40 H40B 107.3 . . ?
C41 C40 N2 116.4(3) . . ?
C41 C40 H40A 108.2 . . ?
C41 C40 H40B 108.2 . . ?
C5 C6 Cl2 120.2(2) . . ?
C5 C6 C1 121.0(3) . . ?
C1 C6 Cl2 118.8(2) . . ?
F2 C6 Cl2 5.6(18) . . ?
F2 C6 C5 117.5(17) . . ?
F2 C6 C1 121.4(17) . . ?
N1 C28 H28A 108.2 . . ?
N1 C28 H28B 108.2 . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 N1 116.2(3) . . ?
C29 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
N2 C37 H37A 108.2 . . ?
N2 C37 H37B 108.2 . . ?
H37A C37 H37B 107.3 . . ?
C38 C37 N2 116.5(3) . . ?
C38 C37 H37A 108.2 . . ?
C38 C37 H37B 108.2 . . ?
C9 C8 Cl3 118.4(2) . . ?
C9 C8 C7 121.5(3) . . ?
C7 C8 Cl3 120.1(2) . . ?
F3 C8 Cl3 2.2(12) . . ?
F3 C8 C9 119.8(11) . . ?
F3 C8 C7 118.5(11) . . ?
C10 C11 Cl4 118.2(2) . . ?
C12 C11 Cl4 121.0(2) . . ?
C12 C11 C10 120.7(3) . . ?
F4 C11 Cl4 8.4(9) . . ?
F4 C11 C10 123.2(9) . . ?
F4 C11 C12 115.4(9) . . ?
N2 C31 H31A 108.4 . . ?
N2 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 N2 115.4(3) . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
N1 C19 H19A 107.9 . . ?
N1 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C20 C19 N1 117.7(3) . . ?
C20 C19 H19A 107.9 . . ?
C20 C19 H19B 107.9 . . ?
N1 C22 H22A 108.5 . . ?
N1 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
C23 C22 N1 115.2(3) . . ?
C23 C22 H22A 108.5 . . ?
C23 C22 H22B 108.5 . . ?
N2 C34 H34A 108.4 . . ?
N2 C34 H34B 108.4 . . ?
H34A C34 H34B 107.5 . . ?
C35 C34 N2 115.5(3) . . ?
C35 C34 H34A 108.4 . . ?
C35 C34 H34B 108.4 . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 C28 109.2(3) . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
N1 C25 H25A 108.3 . . ?
N1 C25 H25B 108.3 . . ?
N1 C25 C26 115.8(3) . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
C31 C32 C33 109.2(3) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.8 . . ?
C33 C32 H32B 109.8 . . ?
C19 C20 H20A 110.1 . . ?
C19 C20 H20B 110.1 . . ?
C19 C20 C21 108.0(3) . . ?
H20A C20 H20B 108.4 . . ?
C21 C20 H20A 110.1 . . ?
C21 C20 H20B 110.1 . . ?
C34 C35 H35A 109.8 . . ?
C34 C35 H35B 109.8 . . ?
C34 C35 C36 109.5(3) . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 H35A 109.8 . . ?
C36 C35 H35B 109.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C37 C38 H38A 109.9 . . ?
C37 C38 H38B 109.9 . . ?
C37 C38 C39 108.9(3) . . ?
H38A C38 H38B 108.3 . . ?
C39 C38 H38A 109.9 . . ?
C39 C38 H38B 109.9 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C40 C41 H41A 109.9 . . ?
C40 C41 H41B 109.9 . . ?
C40 C41 C42 109.1(3) . . ?
H41A C41 H41B 108.3 . . ?
C42 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C22 C23 H23A 109.7 . . ?
C22 C23 H23B 109.7 . . ?
C22 C23 C24 109.8(3) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.7 . . ?
C24 C23 H23B 109.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
C25 C26 C27 109.7(3) . . ?
H26A C26 H26B 108.2 . . ?
C27 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O13 C43 C45 120.2(5) . . ?
O13 C43 C44 121.0(5) . . ?
C44 C43 C45 118.8(4) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
C48 C46 C47 117.8(5) . . ?
O14 C46 C48 120.6(6) . . ?
O14 C46 C47 121.4(5) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 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 O2 C2 C1 2.2(3) . . . . ?
Fe1 O2 C2 C3 -177.5(2) . . . . ?
Fe1 O4 C5 C4 -3.7(3) 4_576 . . . ?
Fe1 O4 C5 C6 177.5(2) 4_576 . . . ?
Fe1 O1 C1 C2 -5.2(3) . . . . ?
Fe1 O1 C1 C6 174.7(3) . . . . ?
Fe1 O5 C7 C12 1.1(3) . . . . ?
Fe1 O5 C7 C8 -179.9(3) . . . . ?
Fe1 O8 C12 C7 -0.3(3) . . . . ?
Fe1 O8 C12 C11 178.8(3) . . . . ?
Fe1 O3 C4 C5 3.2(3) 4_576 . . . ?
Fe1 O3 C4 C3 -178.0(2) 4_576 . . . ?
Fe2 O12 C18 C13 -4.8(3) . . . . ?
Fe2 O12 C18 C17 176.4(2) . . . . ?
Fe2 O10 C15 C16 2.5(3) 4_566 . . . ?
Fe2 O10 C15 C14 -178.2(3) 4_566 . . . ?
Fe2 O9 C13 C18 7.4(3) . . . . ?
Fe2 O9 C13 C14 -174.2(3) . . . . ?
Fe2 O7 C10 C9 -4.1(3) . . . . ?
Fe2 O7 C10 C11 177.4(3) . . . . ?
Fe2 O6 C9 C10 1.8(3) . . . . ?
Fe2 O6 C9 C8 -176.7(3) . . . . ?
Fe2 O11 C16 C15 -2.5(3) 4_566 . . . ?
Fe2 O11 C16 C17 177.9(2) 4_566 . . . ?
O12 C18 C17 Cl6 0.5(4) . . . . ?
O12 C18 C17 C16 -178.8(3) . . . . ?
O12 C18 C17 F6 -0.2(16) . . . . ?
O2 C2 C1 O1 2.0(4) . . . . ?
O2 C2 C1 C6 -177.9(3) . . . . ?
O2 C2 C3 Cl1 -1.8(4) . . . . ?
O2 C2 C3 C4 177.6(3) . . . . ?
O2 C2 C3 F1 7.5(18) . . . . ?
O4 C5 C4 O3 0.3(4) . . . . ?
O4 C5 C4 C3 -178.6(3) . . . . ?
O4 C5 C6 Cl2 -0.2(4) . . . . ?
O4 C5 C6 C1 178.3(3) . . . . ?
O4 C5 C6 F2 -6(2) . . . . ?
O10 C15 C16 O11 0.0(4) . . . . ?
O10 C15 C16 C17 179.6(3) . . . . ?
O10 C15 C14 Cl5 0.8(5) . . . . ?
O10 C15 C14 C13 -178.5(3) . . . . ?
O10 C15 C14 F5 6.3(17) . . . . ?
O1 C1 C6 Cl2 -2.0(5) . . . . ?
O1 C1 C6 C5 179.5(3) . . . . ?
O1 C1 C6 F2 4(2) . . . . ?
O5 C7 C8 Cl3 1.9(5) . . . . ?
O5 C7 C8 C9 -176.0(3) . . . . ?
O5 C7 C8 F3 0.0(15) . . . . ?
O9 C13 C18 O12 -1.8(4) . . . . ?
O9 C13 C18 C17 177.1(3) . . . . ?
O9 C13 C14 Cl5 2.1(5) . . . . ?
O9 C13 C14 C15 -178.5(3) . . . . ?
O9 C13 C14 F5 -3.3(17) . . . . ?
O7 C10 C11 Cl4 2.1(5) . . . . ?
O7 C10 C11 C12 -176.0(3) . . . . ?
O7 C10 C11 F4 -5.9(13) . . . . ?
O6 C9 C10 O7 1.5(4) . . . . ?
O6 C9 C10 C11 -179.9(3) . . . . ?
O6 C9 C8 Cl3 -2.5(5) . . . . ?
O6 C9 C8 C7 175.5(3) . . . . ?
O6 C9 C8 F3 -0.5(15) . . . . ?
O8 C12 C7 O5 -0.5(4) . . . . ?
O8 C12 C7 C8 -179.6(3) . . . . ?
O8 C12 C11 Cl4 -2.6(5) . . . . ?
O8 C12 C11 C10 175.5(3) . . . . ?
O8 C12 C11 F4 4.6(12) . . . . ?
O3 C4 C3 Cl1 1.7(4) . . . . ?
O3 C4 C3 C2 -177.7(3) . . . . ?
O3 C4 C3 F1 -7.4(18) . . . . ?
O11 C16 C17 Cl6 -1.5(4) . . . . ?
O11 C16 C17 C18 177.7(3) . . . . ?
O11 C16 C17 F6 -0.9(16) . . . . ?
N1 C28 C29 C30 -172.2(3) . . . . ?
N1 C19 C20 C21 -179.8(3) . . . . ?
N1 C22 C23 C24 176.1(4) . . . . ?
N1 C25 C26 C27 -173.1(3) . . . . ?
N2 C40 C41 C42 169.6(3) . . . . ?
N2 C37 C38 C39 169.9(3) . . . . ?
N2 C31 C32 C33 -169.2(3) . . . . ?
N2 C34 C35 C36 -171.4(3) . . . . ?
C13 C18 C17 Cl6 -178.3(2) . . . . ?
C13 C18 C17 C16 2.4(4) . . . . ?
C13 C18 C17 F6 -178.9(15) . . . . ?
C15 C16 C17 Cl6 178.9(2) . . . . ?
C15 C16 C17 C18 -1.9(4) . . . . ?
C15 C16 C17 F6 179.5(16) . . . . ?
C16 C15 C14 Cl5 -179.9(2) . . . . ?
C16 C15 C14 C13 0.7(5) . . . . ?
C16 C15 C14 F5 -174.5(16) . . . . ?
C5 C4 C3 Cl1 -179.5(2) . . . . ?
C5 C4 C3 C2 1.1(4) . . . . ?
C5 C4 C3 F1 171.3(18) . . . . ?
C18 C13 C14 Cl5 -179.5(2) . . . . ?
C18 C13 C14 C15 -0.1(5) . . . . ?
C18 C13 C14 F5 175.1(16) . . . . ?
C2 C1 C6 Cl2 177.9(2) . . . . ?
C2 C1 C6 C5 -0.5(5) . . . . ?
C2 C1 C6 F2 -176(2) . . . . ?
C1 C2 C3 Cl1 178.5(2) . . . . ?
C1 C2 C3 C4 -2.1(4) . . . . ?
C1 C2 C3 F1 -172.2(18) . . . . ?
C9 C10 C11 Cl4 -176.4(2) . . . . ?
C9 C10 C11 C12 5.5(5) . . . . ?
C9 C10 C11 F4 175.7(12) . . . . ?
C4 C5 C6 Cl2 -178.9(2) . . . . ?
C4 C5 C6 C1 -0.5(5) . . . . ?
C4 C5 C6 F2 175(2) . . . . ?
C3 C2 C1 O1 -178.3(3) . . . . ?
C3 C2 C1 C6 1.8(4) . . . . ?
C14 C13 C18 O12 179.7(3) . . . . ?
C14 C13 C18 C17 -1.5(4) . . . . ?
C14 C15 C16 O11 -179.4(3) . . . . ?
C14 C15 C16 C17 0.3(4) . . . . ?
C10 C9 C8 Cl3 179.1(2) . . . . ?
C10 C9 C8 C7 -3.0(5) . . . . ?
C10 C9 C8 F3 -179.0(14) . . . . ?
C12 C7 C8 Cl3 -179.1(2) . . . . ?
C12 C7 C8 C9 3.0(5) . . . . ?
C12 C7 C8 F3 179.0(14) . . . . ?
C7 C12 C11 Cl4 176.5(2) . . . . ?
C7 C12 C11 C10 -5.5(5) . . . . ?
C7 C12 C11 F4 -176.4(12) . . . . ?
C40 N2 C37 C38 -56.9(4) . . . . ?
C40 N2 C31 C32 62.8(4) . . . . ?
C40 N2 C34 C35 -177.1(3) . . . . ?
C6 C5 C4 O3 179.1(3) . . . . ?
C6 C5 C4 C3 0.2(4) . . . . ?
C28 N1 C19 C20 50.8(4) . . . . ?
C28 N1 C22 C23 -177.7(3) . . . . ?
C28 N1 C25 C26 69.3(4) . . . . ?
C37 N2 C40 C41 -56.5(4) . . . . ?
C37 N2 C31 C32 -176.4(3) . . . . ?
C37 N2 C34 C35 61.9(4) . . . . ?
C8 C9 C10 O7 -179.9(3) . . . . ?
C8 C9 C10 C11 -1.3(4) . . . . ?
C11 C12 C7 O5 -179.7(3) . . . . ?
C11 C12 C7 C8 1.2(4) . . . . ?
C31 N2 C40 C41 61.4(4) . . . . ?
C31 N2 C37 C38 -177.6(3) . . . . ?
C31 N2 C34 C35 -56.2(4) . . . . ?
C19 N1 C28 C29 55.8(4) . . . . ?
C19 N1 C22 C23 61.8(4) . . . . ?
C19 N1 C25 C26 -169.8(3) . . . . ?
C22 N1 C28 C29 -62.6(4) . . . . ?
C22 N1 C19 C20 170.0(3) . . . . ?
C22 N1 C25 C26 -50.7(4) . . . . ?
C34 N2 C40 C41 -177.4(3) . . . . ?
C34 N2 C37 C38 61.2(4) . . . . ?
C34 N2 C31 C32 -55.5(4) . . . . ?
C25 N1 C28 C29 175.5(3) . . . . ?
C25 N1 C19 C20 -68.3(4) . . . . ?
C25 N1 C22 C23 -58.1(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.667
_oxdiff_exptl_absorpt_empirical_full_min 0.636
####################################################################### 
# 
# 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_F-017_CCDC-2014813_R1
_database_code_depnum_ccdc_archive 'CCDC 2014813'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-08-01
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 Cl4.98 F1.02 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl4.98 F1.02 Fe2 N2 O15'
_chemical_formula_weight         1222.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl4.98 F1.02 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.0262(4)
_cell_length_b                   21.8928(4)
_cell_length_c                   14.3496(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.832(2)
_cell_angle_gamma                90
_cell_volume                     5989.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29417
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.2810
_cell_measurement_theta_min      1.7860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2551
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.062
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41330
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.804
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0252162000
_diffrn_orient_matrix_UB_12      0.0078495000
_diffrn_orient_matrix_UB_13      0.0451000000
_diffrn_orient_matrix_UB_21      0.0272854000
_diffrn_orient_matrix_UB_22      -0.0093038000
_diffrn_orient_matrix_UB_23      -0.0187891000
_diffrn_orient_matrix_UB_31      0.0018860000
_diffrn_orient_matrix_UB_32      0.0300216000
_diffrn_orient_matrix_UB_33      -0.0176099000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9405
_reflns_number_total             10938
_reflns_odcompleteness_completeness 90.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.15
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         10938
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0427
_refine_ls_restrained_S_all      1.048
_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)+(0.0713P)²+5.5297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1294
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-F3
 1.33 with sigma of 0.01
 C11-F4
 1.33 with sigma of 0.02
 C17-F6
 1.33 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C14-F5
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(F1)
Uanis(F5) = Uanis(Cl5)
Uanis(F3) = Uanis(Cl3)
Uanis(F2) = Uanis(Cl2)
4. Others
 Fixed Sof: Cl6(0.86) Cl3(0.8) Cl1(0.83) Cl4(0.8) Cl5(0.86) Cl2(0.83) O16(0.5)
 O15(0.5) F4(0.2) F6(0.14) F3(0.2) F1(0.17) F2(0.17) F5(0.14)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C19(H19A,H19B), C28(H28A,H28B), C20(H20A,
 H20B), C29(H29A,H29B), C34(H34A,H34B), C37(H37A,H37B), C31(H31A,H31B),
 C40(H40A,H40B), C32(H32A,H32B), C35(H35A,H35B), C23(H23A,H23B), C38(H38A,H38B),
  C26(H26A,H26B), C41(H41A,H41B)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C27(H27A,H27B,
 H27C), C24(H24A,H24B,H24C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C48(H48A,
 H48B,H48C), C45(H45A,H45B,H45C), C36(H36A,H36B,H36C), C47(H47A,H47B,H47C),
 C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe2 Fe 0.77850(2) 0.32043(2) 1.10311(2) 0.01904(10) Uani 1 1 d . . . . .
Fe1 Fe 0.76053(2) 0.68160(2) 1.09287(2) 0.01980(10) Uani 1 1 d . . . . .
Cl6 Cl 0.91967(7) 0.18011(8) 0.96163(13) 0.0262(3) Uani 0.86 1 d . . P A 2
Cl3 Cl 0.61920(4) 0.49729(5) 1.12978(10) 0.02568(19) Uani 0.8 1 d . . P B 2
Cl1 Cl 0.89720(4) 0.82574(4) 0.95016(7) 0.02460(19) Uani 0.83 1 d . . P C 2
Cl4 Cl 0.90838(9) 0.50894(9) 1.03182(13) 0.0258(3) Uani 0.8 1 d . . P D 2
Cl5 Cl 0.63639(4) 0.31620(4) 0.74930(7) 0.0324(2) Uani 0.86 1 d . . P E 2
Cl2 Cl 0.61882(5) 0.68177(5) 0.73966(8) 0.0320(2) Uani 0.83 1 d . . P F 2
O7 O 0.83268(8) 0.39650(7) 1.07815(11) 0.0228(3) Uani 1 1 d . . . . .
O8 O 0.82023(8) 0.61018(7) 1.06661(11) 0.0229(3) Uani 1 1 d . . . . .
O12 O 0.83544(8) 0.26372(7) 1.04953(10) 0.0212(3) Uani 1 1 d . . . . .
O2 O 0.81500(8) 0.74099(7) 1.04042(10) 0.0209(3) Uani 1 1 d . . . . .
O1 O 0.69879(8) 0.68497(7) 0.95384(11) 0.0222(3) Uani 1 1 d . . . . .
O11 O 0.83830(8) 0.18015(7) 0.74380(11) 0.0203(3) Uani 1 1 d . . . . .
O9 O 0.71719(8) 0.31554(7) 0.96353(11) 0.0222(3) Uani 1 1 d . . . . .
O5 O 0.70119(8) 0.60611(7) 1.10554(11) 0.0218(3) Uani 1 1 d . . . . .
O10 O 0.72215(8) 0.23552(7) 0.65822(10) 0.0216(3) Uani 1 1 d . . . . .
O3 O 0.81801(8) 0.82056(7) 0.73350(11) 0.0208(3) Uani 1 1 d . . . . .
O6 O 0.71354(8) 0.39256(7) 1.11561(11) 0.0223(3) Uani 1 1 d . . . . .
O4 O 0.70361(8) 0.76285(7) 0.64749(10) 0.0223(3) Uani 1 1 d . . . . .
N1 N 0.49135(10) 0.79890(10) 0.49378(14) 0.0262(4) Uani 1 1 d . . . . .
N2 N 0.95166(11) 0.64813(10) 0.77314(15) 0.0292(5) Uani 1 1 d . . . . .
C7 C 0.72766(11) 0.55518(10) 1.09698(15) 0.0209(5) Uani 1 1 d . . . . .
C9 C 0.73413(11) 0.44521(10) 1.10248(15) 0.0214(5) Uani 1 1 d . . . . .
C16 C 0.81233(11) 0.21127(9) 0.80101(15) 0.0180(4) Uani 1 1 d . . . . .
C10 C 0.80443(11) 0.44757(10) 1.08015(15) 0.0211(5) Uani 1 1 d . . . . .
C4 C 0.79215(11) 0.78982(10) 0.79082(15) 0.0187(4) Uani 1 1 d . . . . .
C12 C 0.79784(11) 0.55776(10) 1.07445(15) 0.0209(5) Uani 1 1 d . . . . .
C8 C 0.69876(12) 0.49892(10) 1.10693(17) 0.0226(5) Uani 1 1 d D . . . .
C5 C 0.72692(11) 0.75633(10) 0.74161(15) 0.0198(4) Uani 1 1 d . . . . .
C3 C 0.82139(11) 0.78514(10) 0.89185(15) 0.0192(4) Uani 1 1 d . . . . .
C1 C 0.72520(11) 0.71608(10) 0.89743(15) 0.0197(5) Uani 1 1 d . . . . .
C11 C 0.83121(12) 0.50372(10) 1.06421(17) 0.0230(5) Uani 1 1 d D . . . .
C15 C 0.74576(11) 0.24280(10) 0.75179(15) 0.0191(4) Uani 1 1 d . . . . .
C17 C 0.84227(11) 0.21765(10) 0.90198(16) 0.0201(4) Uani 1 1 d D . . . .
C2 C 0.79078(11) 0.74877(10) 0.94670(15) 0.0186(4) Uani 1 1 d . . . . .
C13 C 0.74358(11) 0.28430(10) 0.90710(15) 0.0200(5) Uani 1 1 d . . . . .
C18 C 0.81067(11) 0.25372(10) 0.95642(15) 0.0186(4) Uani 1 1 d . . . . .
C22 C 0.55441(12) 0.75952(11) 0.49625(19) 0.0305(5) Uani 1 1 d . . . . .
H22A H 0.5937 0.7868 0.4959 0.037 Uiso 1 1 calc R U . . .
H22B H 0.5687 0.7368 0.5589 0.037 Uiso 1 1 calc R U . . .
C6 C 0.69534(12) 0.72109(11) 0.79656(16) 0.0232(5) Uani 1 1 d D . . . .
C25 C 0.42851(12) 0.75957(12) 0.49205(19) 0.0312(5) Uani 1 1 d . . . . .
H25A H 0.3892 0.7869 0.4921 0.037 Uiso 1 1 calc R U . . .
H25B H 0.4142 0.7365 0.4297 0.037 Uiso 1 1 calc R U . . .
C19 C 0.46918(13) 0.83752(11) 0.40179(17) 0.0298(5) Uani 1 1 d . . . . .
H19A H 0.4578 0.8099 0.3445 0.036 Uiso 1 1 calc R U . . .
H19B H 0.4256 0.8595 0.4000 0.036 Uiso 1 1 calc R U . . .
C14 C 0.71365(11) 0.27792(10) 0.80674(16) 0.0223(5) Uani 1 1 d D . . . .
C28 C 0.51357(13) 0.83831(12) 0.58489(18) 0.0302(5) Uani 1 1 d . . . . .
H28A H 0.5566 0.8608 0.5855 0.036 Uiso 1 1 calc R U . . .
H28B H 0.5259 0.8112 0.6428 0.036 Uiso 1 1 calc R U . . .
C20 C 0.52220(15) 0.88391(12) 0.39067(19) 0.0346(6) Uani 1 1 d . . . . .
H20A H 0.5685 0.8641 0.4029 0.042 Uiso 1 1 calc R U . . .
H20B H 0.5270 0.9170 0.4392 0.042 Uiso 1 1 calc R U . . .
C29 C 0.45973(15) 0.88422(12) 0.59556(19) 0.0360(6) Uani 1 1 d . . . . .
H29A H 0.4143 0.8635 0.5865 0.043 Uiso 1 1 calc R U . . .
H29B H 0.4528 0.9162 0.5446 0.043 Uiso 1 1 calc R U . . .
C34 C 0.98573(14) 0.62145(13) 0.70128(19) 0.0371(6) Uani 1 1 d . . . . .
H34A H 0.9561 0.6316 0.6341 0.044 Uiso 1 1 calc R U . . .
H34B H 1.0317 0.6416 0.7118 0.044 Uiso 1 1 calc R U . . .
C37 C 1.00017(14) 0.63645(12) 0.87545(18) 0.0347(6) Uani 1 1 d . . . . .
H37A H 1.0006 0.5919 0.8876 0.042 Uiso 1 1 calc R U . . .
H37B H 1.0482 0.6482 0.8768 0.042 Uiso 1 1 calc R U . . .
C31 C 0.94113(14) 0.71669(12) 0.7536(2) 0.0343(6) Uani 1 1 d . . . . .
H31A H 0.9104 0.7223 0.6855 0.041 Uiso 1 1 calc R U . . .
H31B H 0.9157 0.7332 0.7974 0.041 Uiso 1 1 calc R U . . .
C21 C 0.49839(18) 0.91048(14) 0.2876(2) 0.0479(8) Uani 1 1 d . . . . .
H21A H 0.4955 0.8778 0.2399 0.072 Uiso 1 1 calc R U . . .
H21B H 0.5322 0.9413 0.2813 0.072 Uiso 1 1 calc R U . . .
H21C H 0.4522 0.9294 0.2754 0.072 Uiso 1 1 calc R U . . .
C30 C 0.48463(18) 0.91348(15) 0.6967(2) 0.0514(8) Uani 1 1 d . . . . .
H30A H 0.4509 0.9447 0.7019 0.077 Uiso 1 1 calc R U . . .
H30B H 0.5306 0.9324 0.7065 0.077 Uiso 1 1 calc R U . . .
H30C H 0.4884 0.8821 0.7468 0.077 Uiso 1 1 calc R U . . .
C40 C 0.88094(14) 0.61947(13) 0.7629(2) 0.0395(6) Uani 1 1 d . . . . .
H40A H 0.8888 0.5771 0.7882 0.047 Uiso 1 1 calc R U . . .
H40B H 0.8587 0.6423 0.8050 0.047 Uiso 1 1 calc R U . . .
C32 C 1.00640(14) 0.75466(12) 0.76717(19) 0.0359(6) Uani 1 1 d . . . . .
H32A H 1.0284 0.7440 0.7162 0.043 Uiso 1 1 calc R U . . .
H32B H 1.0406 0.7461 0.8320 0.043 Uiso 1 1 calc R U . . .
C35 C 0.99709(17) 0.55338(13) 0.7076(2) 0.0450(7) Uani 1 1 d . . . . .
H35A H 0.9519 0.5325 0.6999 0.054 Uiso 1 1 calc R U . . .
H35B H 1.0296 0.5427 0.7728 0.054 Uiso 1 1 calc R U . . .
C33 C 0.98709(17) 0.82192(13) 0.7598(2) 0.0456(7) Uani 1 1 d . . . . .
H33A H 0.9538 0.8303 0.6951 0.068 Uiso 1 1 calc R U . . .
H33B H 1.0295 0.8466 0.7690 0.068 Uiso 1 1 calc R U . . .
H33C H 0.9655 0.8323 0.8105 0.068 Uiso 1 1 calc R U . . .
C23 C 0.54388(15) 0.71416(14) 0.4137(2) 0.0470(7) Uani 1 1 d . . . . .
H23A H 0.5393 0.7360 0.3516 0.056 Uiso 1 1 calc R U . . .
H23B H 0.5004 0.6904 0.4058 0.056 Uiso 1 1 calc R U . . .
O13 O 0.86435(19) 0.46520(14) 0.7199(4) 0.1227(15) Uani 1 1 d . . . . .
C38 C 0.98438(18) 0.66808(14) 0.9590(2) 0.0442(7) Uani 1 1 d . . . . .
H38A H 0.9374 0.6560 0.9616 0.053 Uiso 1 1 calc R U . . .
H38B H 0.9847 0.7129 0.9501 0.053 Uiso 1 1 calc R U . . .
C26 C 0.43912(15) 0.71469(14) 0.5750(2) 0.0472(8) Uani 1 1 d . . . . .
H26A H 0.4442 0.7368 0.6369 0.057 Uiso 1 1 calc R U . . .
H26B H 0.4824 0.6907 0.5826 0.057 Uiso 1 1 calc R U . . .
C27 C 0.37578(15) 0.67219(14) 0.5521(3) 0.0508(8) Uani 1 1 d . . . . .
H27A H 0.3733 0.6481 0.4935 0.076 Uiso 1 1 calc R U . . .
H27B H 0.3329 0.6965 0.5404 0.076 Uiso 1 1 calc R U . . .
H27C H 0.3805 0.6447 0.6076 0.076 Uiso 1 1 calc R U . . .
C24 C 0.60725(15) 0.67116(13) 0.4378(3) 0.0495(8) Uani 1 1 d . . . . .
H24A H 0.6033 0.6440 0.3821 0.074 Uiso 1 1 calc R U . . .
H24B H 0.6086 0.6467 0.4956 0.074 Uiso 1 1 calc R U . . .
H24C H 0.6504 0.6952 0.4513 0.074 Uiso 1 1 calc R U . . .
C39 C 1.03978(19) 0.65003(15) 1.0532(2) 0.0527(8) Uani 1 1 d . . . . .
H39A H 1.0863 0.6531 1.0445 0.079 Uiso 1 1 calc R U . . .
H39B H 1.0316 0.6079 1.0700 0.079 Uiso 1 1 calc R U . . .
H39C H 1.0373 0.6774 1.1060 0.079 Uiso 1 1 calc R U . . .
O14 O 0.6669(3) 1.00344(17) 0.9181(5) 0.150(2) Uani 1 1 d . . . . .
C41 C 0.83018(16) 0.61750(15) 0.6605(3) 0.0539(9) Uani 1 1 d . . . . .
H41A H 0.8248 0.6590 0.6317 0.065 Uiso 1 1 calc R U . . .
H41B H 0.8488 0.5904 0.6191 0.065 Uiso 1 1 calc R U . . .
C42 C 0.75985(16) 0.59424(16) 0.6625(3) 0.0608(9) Uani 1 1 d . . . . .
H42A H 0.7282 0.5911 0.5954 0.091 Uiso 1 1 calc R U . . .
H42B H 0.7400 0.6226 0.6998 0.091 Uiso 1 1 calc R U . . .
H42C H 0.7656 0.5539 0.6935 0.091 Uiso 1 1 calc R U . . .
C48 C 0.7492(3) 0.94243(18) 0.8746(3) 0.0776(12) Uani 1 1 d . . . . .
H48A H 0.8003 0.9418 0.9035 0.116 Uiso 1 1 calc R U . . .
H48B H 0.7370 0.9369 0.8035 0.116 Uiso 1 1 calc R U . . .
H48C H 0.7285 0.9093 0.9025 0.116 Uiso 1 1 calc R U . . .
C43 C 0.82419(19) 0.42641(16) 0.7276(3) 0.0674(11) Uani 1 1 d . . . . .
C45 C 0.7857(3) 0.43259(19) 0.8020(3) 0.0798(12) Uani 1 1 d . . . . .
H45A H 0.7993 0.3992 0.8496 0.120 Uiso 1 1 calc R U . . .
H45B H 0.7350 0.4308 0.7690 0.120 Uiso 1 1 calc R U . . .
H45C H 0.7975 0.4718 0.8360 0.120 Uiso 1 1 calc R U . . .
C46 C 0.7216(3) 1.00180(19) 0.8959(3) 0.0782(13) Uani 1 1 d . . . . .
C36 C 1.0273(3) 0.53192(19) 0.6288(3) 0.0900(15) Uani 1 1 d . . . . .
H36A H 0.9939 0.5404 0.5643 0.135 Uiso 1 1 calc R U . . .
H36B H 1.0363 0.4879 0.6357 0.135 Uiso 1 1 calc R U . . .
H36C H 1.0714 0.5535 0.6353 0.135 Uiso 1 1 calc R U . . .
C47 C 0.7591(3) 1.05883(19) 0.8827(4) 0.0830(13) Uani 1 1 d . . . . .
H47A H 0.7370 1.0943 0.9029 0.124 Uiso 1 1 calc R U . . .
H47B H 0.7566 1.0631 0.8138 0.124 Uiso 1 1 calc R U . . .
H47C H 0.8084 1.0564 0.9230 0.124 Uiso 1 1 calc R U . . .
C44 C 0.8119(2) 0.3718(2) 0.6642(4) 0.0871(14) Uani 1 1 d . . . . .
H44A H 0.7619 0.3688 0.6277 0.131 Uiso 1 1 calc R U . . .
H44B H 0.8266 0.3352 0.7046 0.131 Uiso 1 1 calc R U . . .
H44C H 0.8391 0.3752 0.6181 0.131 Uiso 1 1 calc R U . . .
O16 O 0.5160(6) 1.0752(9) 1.0246(12) 0.255(8) Uani 0.5 1 d . . P G -3
O15 O 0.5591(11) 1.0000(7) 1.0695(12) 0.264(10) Uani 0.5 1 d . . P H 3
F4 F 0.8953(8) 0.5017(8) 1.0519(13) 0.035(4) Uani 0.2 1 d D . P D -2
F6 F 0.9083(10) 0.1949(10) 0.9421(17) 0.032(6) Uani 0.14 1 d D . P A -2
F3 F 0.6356(5) 0.4943(6) 1.1264(12) 0.02568(19) Uani 0.2 1 d D . P B -2
F1 F 0.8824(7) 0.8135(6) 0.9376(10) 0.02460(19) Uani 0.17 1 d . . P C -2
F2 F 0.6318(7) 0.6945(7) 0.7518(11) 0.0320(2) Uani 0.17 1 d D . P F -2
F5 F 0.6506(7) 0.3018(8) 0.7626(11) 0.0324(2) Uani 0.14 1 d D . P E -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe2 O7 2.0777(16) . ?
Fe2 O12 1.9924(15) . ?
Fe2 O11 2.0073(15) 4_566 ?
Fe2 O9 2.0062(15) . ?
Fe2 O10 1.9864(15) 4_566 ?
Fe2 O6 2.0884(15) . ?
Fe1 O8 2.0717(16) . ?
Fe1 O2 1.9875(15) . ?
Fe1 O1 2.0009(15) . ?
Fe1 O5 2.0757(16) . ?
Fe1 O3 1.9942(15) 4_576 ?
Fe1 O4 1.9848(15) 4_576 ?
Cl6 C17 1.732(2) . ?
Cl3 C8 1.723(2) . ?
Cl1 C3 1.737(2) . ?
Cl4 C11 1.749(3) . ?
Cl5 C14 1.731(2) . ?
Cl2 C6 1.729(2) . ?
O7 C10 1.257(3) . ?
O8 C12 1.250(3) . ?
O12 C18 1.293(3) . ?
O2 C2 1.294(3) . ?
O1 C1 1.289(3) . ?
O11 Fe2 2.0072(15) 4_565 ?
O11 C16 1.292(3) . ?
O9 C13 1.290(3) . ?
O5 C7 1.257(3) . ?
O10 Fe2 1.9864(15) 4_565 ?
O10 C15 1.290(3) . ?
O3 Fe1 1.9943(15) 4_575 ?
O3 C4 1.288(3) . ?
O6 C9 1.258(3) . ?
O4 Fe1 1.9848(15) 4_575 ?
O4 C5 1.295(3) . ?
N1 C22 1.521(3) . ?
N1 C25 1.519(3) . ?
N1 C19 1.515(3) . ?
N1 C28 1.515(3) . ?
N2 C34 1.517(3) . ?
N2 C37 1.514(3) . ?
N2 C31 1.530(3) . ?
N2 C40 1.514(3) . ?
C7 C12 1.537(3) . ?
C7 C8 1.387(3) . ?
C9 C10 1.537(3) . ?
C9 C8 1.384(3) . ?
C16 C15 1.475(3) . ?
C16 C17 1.395(3) . ?
C10 C11 1.388(3) . ?
C4 C5 1.476(3) . ?
C4 C3 1.391(3) . ?
C12 C11 1.388(3) . ?
C8 F3 1.381(8) . ?
C5 C6 1.386(3) . ?
C3 C2 1.387(3) . ?
C3 F1 1.349(12) . ?
C1 C2 1.472(3) . ?
C1 C6 1.391(3) . ?
C11 F4 1.348(13) . ?
C15 C14 1.392(3) . ?
C17 C18 1.392(3) . ?
C17 F6 1.364(15) . ?
C13 C18 1.474(3) . ?
C13 C14 1.387(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.510(4) . ?
C6 F2 1.367(11) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.507(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.513(4) . ?
C14 F5 1.335(12) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.516(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.523(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.524(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.506(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.500(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.510(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.509(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.518(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.512(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.532(4) . ?
O13 C43 1.197(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.515(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.526(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
O14 C46 1.231(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.506(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C46 1.481(5) . ?
C43 C45 1.503(6) . ?
C43 C44 1.477(6) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.499(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
O7 Fe2 O6 77.33(6) . . ?
O12 Fe2 O7 92.42(6) . . ?
O12 Fe2 O11 98.54(6) . 4_566 ?
O12 Fe2 O9 80.16(6) . . ?
O12 Fe2 O6 161.72(6) . . ?
O11 Fe2 O7 89.79(6) 4_566 . ?
O11 Fe2 O6 96.54(6) 4_566 . ?
O9 Fe2 O7 93.61(6) . . ?
O9 Fe2 O11 176.41(6) . 4_566 ?
O9 Fe2 O6 85.36(6) . . ?
O10 Fe2 O7 162.41(6) 4_566 . ?
O10 Fe2 O12 103.38(7) 4_566 . ?
O10 Fe2 O11 80.35(6) 4_566 4_566 ?
O10 Fe2 O9 96.65(6) 4_566 . ?
O10 Fe2 O6 89.27(6) 4_566 . ?
O8 Fe1 O5 78.05(6) . . ?
O2 Fe1 O8 90.61(6) . . ?
O2 Fe1 O1 80.88(6) . . ?
O2 Fe1 O5 161.69(6) . . ?
O2 Fe1 O3 100.66(6) . 4_576 ?
O1 Fe1 O8 93.52(6) . . ?
O1 Fe1 O5 85.48(6) . . ?
O3 Fe1 O8 88.84(6) 4_576 . ?
O3 Fe1 O1 177.18(6) 4_576 . ?
O3 Fe1 O5 93.50(6) 4_576 . ?
O4 Fe1 O8 165.34(6) 4_576 . ?
O4 Fe1 O2 101.35(7) 4_576 . ?
O4 Fe1 O1 96.71(6) 4_576 . ?
O4 Fe1 O5 92.28(6) 4_576 . ?
O4 Fe1 O3 80.69(6) 4_576 4_576 ?
C10 O7 Fe2 116.51(14) . . ?
C12 O8 Fe1 115.70(14) . . ?
C18 O12 Fe2 114.85(13) . . ?
C2 O2 Fe1 113.90(13) . . ?
C1 O1 Fe1 113.49(13) . . ?
C16 O11 Fe2 114.20(13) . 4_565 ?
C13 O9 Fe2 114.31(13) . . ?
C7 O5 Fe1 115.33(14) . . ?
C15 O10 Fe2 114.76(13) . 4_565 ?
C4 O3 Fe1 114.42(13) . 4_575 ?
C9 O6 Fe2 116.02(14) . . ?
C5 O4 Fe1 114.35(14) . 4_575 ?
C25 N1 C22 110.92(19) . . ?
C19 N1 C22 110.88(18) . . ?
C19 N1 C25 106.38(18) . . ?
C19 N1 C28 111.4(2) . . ?
C28 N1 C22 106.28(18) . . ?
C28 N1 C25 111.10(18) . . ?
C34 N2 C31 108.59(19) . . ?
C37 N2 C34 107.80(19) . . ?
C37 N2 C31 110.8(2) . . ?
C37 N2 C40 109.1(2) . . ?
C40 N2 C34 112.1(2) . . ?
C40 N2 C31 108.44(19) . . ?
O5 C7 C12 115.36(19) . . ?
O5 C7 C8 125.2(2) . . ?
C8 C7 C12 119.45(19) . . ?
O6 C9 C10 115.16(19) . . ?
O6 C9 C8 125.2(2) . . ?
C8 C9 C10 119.7(2) . . ?
O11 C16 C15 115.03(18) . . ?
O11 C16 C17 125.7(2) . . ?
C17 C16 C15 119.25(19) . . ?
O7 C10 C9 114.97(19) . . ?
O7 C10 C11 125.8(2) . . ?
C11 C10 C9 119.26(19) . . ?
O3 C4 C5 115.10(18) . . ?
O3 C4 C3 125.5(2) . . ?
C3 C4 C5 119.38(19) . . ?
O8 C12 C7 115.42(19) . . ?
O8 C12 C11 125.1(2) . . ?
C11 C12 C7 119.5(2) . . ?
C7 C8 Cl3 118.52(17) . . ?
C9 C8 Cl3 120.49(17) . . ?
C9 C8 C7 120.9(2) . . ?
F3 C8 Cl3 3.1(6) . . ?
F3 C8 C7 121.6(6) . . ?
F3 C8 C9 117.4(6) . . ?
O4 C5 C4 115.34(19) . . ?
O4 C5 C6 125.0(2) . . ?
C6 C5 C4 119.70(19) . . ?
C4 C3 Cl1 119.42(17) . . ?
C2 C3 Cl1 119.56(16) . . ?
C2 C3 C4 121.02(19) . . ?
F1 C3 Cl1 3.4(7) . . ?
F1 C3 C4 120.2(6) . . ?
F1 C3 C2 118.7(6) . . ?
O1 C1 C2 115.63(18) . . ?
O1 C1 C6 124.5(2) . . ?
C6 C1 C2 119.8(2) . . ?
C10 C11 Cl4 121.28(18) . . ?
C10 C11 C12 121.0(2) . . ?
C12 C11 Cl4 117.76(18) . . ?
F4 C11 Cl4 9.4(7) . . ?
F4 C11 C10 115.1(7) . . ?
F4 C11 C12 123.4(8) . . ?
O10 C15 C16 115.48(19) . . ?
O10 C15 C14 124.9(2) . . ?
C14 C15 C16 119.60(19) . . ?
C16 C17 Cl6 120.07(18) . . ?
C18 C17 Cl6 118.94(18) . . ?
C18 C17 C16 120.99(19) . . ?
F6 C17 Cl6 9.3(10) . . ?
F6 C17 C16 117.0(11) . . ?
F6 C17 C18 121.2(11) . . ?
O2 C2 C3 125.1(2) . . ?
O2 C2 C1 115.51(19) . . ?
C3 C2 C1 119.38(19) . . ?
O9 C13 C18 115.33(18) . . ?
O9 C13 C14 125.1(2) . . ?
C14 C13 C18 119.57(19) . . ?
O12 C18 C17 125.4(2) . . ?
O12 C18 C13 115.09(18) . . ?
C17 C18 C13 119.51(19) . . ?
N1 C22 H22A 108.3 . . ?
N1 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N1 116.0(2) . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
C5 C6 Cl2 120.07(17) . . ?
C5 C6 C1 120.7(2) . . ?
C1 C6 Cl2 119.25(18) . . ?
F2 C6 Cl2 4.9(8) . . ?
F2 C6 C5 119.4(7) . . ?
F2 C6 C1 119.8(7) . . ?
N1 C25 H25A 108.2 . . ?
N1 C25 H25B 108.2 . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 N1 116.2(2) . . ?
C26 C25 H25A 108.2 . . ?
C26 C25 H25B 108.2 . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N1 116.0(2) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C15 C14 Cl5 119.90(17) . . ?
C13 C14 Cl5 119.01(17) . . ?
C13 C14 C15 121.1(2) . . ?
F5 C14 Cl5 6.1(8) . . ?
F5 C14 C15 118.8(7) . . ?
F5 C14 C13 119.9(7) . . ?
N1 C28 H28A 108.3 . . ?
N1 C28 H28B 108.3 . . ?
N1 C28 C29 115.8(2) . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 H28A 108.3 . . ?
C29 C28 H28B 108.3 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.7(2) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C28 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
C28 C29 C30 109.8(2) . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
N2 C34 H34A 108.4 . . ?
N2 C34 H34B 108.4 . . ?
H34A C34 H34B 107.5 . . ?
C35 C34 N2 115.5(2) . . ?
C35 C34 H34A 108.4 . . ?
C35 C34 H34B 108.4 . . ?
N2 C37 H37A 107.8 . . ?
N2 C37 H37B 107.8 . . ?
H37A C37 H37B 107.2 . . ?
C38 C37 N2 117.9(2) . . ?
C38 C37 H37A 107.8 . . ?
C38 C37 H37B 107.8 . . ?
N2 C31 H31A 108.1 . . ?
N2 C31 H31B 108.1 . . ?
H31A C31 H31B 107.3 . . ?
C32 C31 N2 116.8(2) . . ?
C32 C31 H31A 108.1 . . ?
C32 C31 H31B 108.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 C40 H40A 108.3 . . ?
N2 C40 H40B 108.3 . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 N2 116.0(2) . . ?
C41 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
C31 C32 C33 109.4(2) . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.8 . . ?
C33 C32 H32B 109.8 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
C34 C35 C36 110.5(3) . . ?
H35A C35 H35B 108.1 . . ?
C36 C35 H35A 109.6 . . ?
C36 C35 H35B 109.6 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C22 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
C22 C23 C24 108.6(2) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 110.0 . . ?
C24 C23 H23B 110.0 . . ?
C37 C38 H38A 110.0 . . ?
C37 C38 H38B 110.0 . . ?
C37 C38 C39 108.5(2) . . ?
H38A C38 H38B 108.4 . . ?
C39 C38 H38A 110.0 . . ?
C39 C38 H38B 110.0 . . ?
C25 C26 H26A 109.9 . . ?
C25 C26 H26B 109.9 . . ?
C25 C26 C27 108.7(2) . . ?
H26A C26 H26B 108.3 . . ?
C27 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C40 C41 H41A 109.6 . . ?
C40 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
C42 C41 C40 110.3(3) . . ?
C42 C41 H41A 109.6 . . ?
C42 C41 H41B 109.6 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
O13 C43 C45 120.4(4) . . ?
O13 C43 C44 120.5(4) . . ?
C44 C43 C45 119.1(3) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O14 C46 C48 119.8(4) . . ?
O14 C46 C47 121.9(4) . . ?
C48 C46 C47 118.2(4) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 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
Fe2 O7 C10 C9 0.8(2) . . . . ?
Fe2 O7 C10 C11 -179.13(18) . . . . ?
Fe2 O12 C18 C17 177.64(17) . . . . ?
Fe2 O12 C18 C13 -2.0(2) . . . . ?
Fe2 O11 C16 C15 -2.8(2) 4_565 . . . ?
Fe2 O11 C16 C17 178.18(17) 4_565 . . . ?
Fe2 O9 C13 C18 5.0(2) . . . . ?
Fe2 O9 C13 C14 -175.21(18) . . . . ?
Fe2 O10 C15 C16 3.3(2) 4_565 . . . ?
Fe2 O10 C15 C14 -177.48(18) 4_565 . . . ?
Fe2 O6 C9 C10 -0.5(2) . . . . ?
Fe2 O6 C9 C8 179.62(18) . . . . ?
Fe1 O8 C12 C7 3.1(2) . . . . ?
Fe1 O8 C12 C11 -177.06(18) . . . . ?
Fe1 O2 C2 C3 -176.38(17) . . . . ?
Fe1 O2 C2 C1 4.2(2) . . . . ?
Fe1 O1 C1 C2 -6.8(2) . . . . ?
Fe1 O1 C1 C6 174.50(18) . . . . ?
Fe1 O5 C7 C12 -2.4(2) . . . . ?
Fe1 O5 C7 C8 177.13(18) . . . . ?
Fe1 O3 C4 C5 2.9(2) 4_575 . . . ?
Fe1 O3 C4 C3 -178.64(17) 4_575 . . . ?
Fe1 O4 C5 C4 -1.5(2) 4_575 . . . ?
Fe1 O4 C5 C6 178.48(18) 4_575 . . . ?
Cl6 C17 C18 O12 2.4(3) . . . . ?
Cl6 C17 C18 C13 -178.00(17) . . . . ?
Cl1 C3 C2 O2 -1.5(3) . . . . ?
Cl1 C3 C2 C1 177.93(16) . . . . ?
O7 C10 C11 Cl4 3.6(3) . . . . ?
O7 C10 C11 C12 -175.8(2) . . . . ?
O7 C10 C11 F4 -4.4(9) . . . . ?
O8 C12 C11 Cl4 -3.4(3) . . . . ?
O8 C12 C11 C10 176.0(2) . . . . ?
O8 C12 C11 F4 5.4(10) . . . . ?
O1 C1 C2 O2 1.8(3) . . . . ?
O1 C1 C2 C3 -177.67(19) . . . . ?
O1 C1 C6 Cl2 -2.0(3) . . . . ?
O1 C1 C6 C5 179.1(2) . . . . ?
O1 C1 C6 F2 3.5(9) . . . . ?
O11 C16 C15 O10 -0.3(3) . . . . ?
O11 C16 C15 C14 -179.56(19) . . . . ?
O11 C16 C17 Cl6 -2.1(3) . . . . ?
O11 C16 C17 C18 178.3(2) . . . . ?
O11 C16 C17 F6 7.9(11) . . . . ?
O9 C13 C18 O12 -2.0(3) . . . . ?
O9 C13 C18 C17 178.3(2) . . . . ?
O9 C13 C14 Cl5 2.3(3) . . . . ?
O9 C13 C14 C15 -179.5(2) . . . . ?
O9 C13 C14 F5 -4.6(10) . . . . ?
O5 C7 C12 O8 -0.4(3) . . . . ?
O5 C7 C12 C11 179.7(2) . . . . ?
O5 C7 C8 Cl3 1.8(3) . . . . ?
O5 C7 C8 C9 -175.8(2) . . . . ?
O5 C7 C8 F3 1.0(9) . . . . ?
O10 C15 C14 Cl5 -0.4(3) . . . . ?
O10 C15 C14 C13 -178.6(2) . . . . ?
O10 C15 C14 F5 6.4(10) . . . . ?
O3 C4 C5 O4 -0.9(3) . . . . ?
O3 C4 C5 C6 179.1(2) . . . . ?
O3 C4 C3 Cl1 2.9(3) . . . . ?
O3 C4 C3 C2 -177.4(2) . . . . ?
O3 C4 C3 F1 -1.0(8) . . . . ?
O6 C9 C10 O7 -0.2(3) . . . . ?
O6 C9 C10 C11 179.7(2) . . . . ?
O6 C9 C8 Cl3 -1.2(3) . . . . ?
O6 C9 C8 C7 176.2(2) . . . . ?
O6 C9 C8 F3 -0.7(8) . . . . ?
O4 C5 C6 Cl2 -0.1(3) . . . . ?
O4 C5 C6 C1 178.8(2) . . . . ?
O4 C5 C6 F2 -5.6(9) . . . . ?
N1 C22 C23 C24 -169.8(2) . . . . ?
N1 C25 C26 C27 -170.3(2) . . . . ?
N1 C19 C20 C21 169.6(2) . . . . ?
N1 C28 C29 C30 171.4(2) . . . . ?
N2 C34 C35 C36 176.7(3) . . . . ?
N2 C37 C38 C39 -179.5(2) . . . . ?
N2 C31 C32 C33 -171.6(2) . . . . ?
N2 C40 C41 C42 -173.9(3) . . . . ?
C7 C12 C11 Cl4 176.49(17) . . . . ?
C7 C12 C11 C10 -4.1(3) . . . . ?
C7 C12 C11 F4 -174.7(9) . . . . ?
C9 C10 C11 Cl4 -176.39(17) . . . . ?
C9 C10 C11 C12 4.3(3) . . . . ?
C9 C10 C11 F4 175.6(9) . . . . ?
C16 C15 C14 Cl5 178.81(16) . . . . ?
C16 C15 C14 C13 0.7(3) . . . . ?
C16 C15 C14 F5 -174.3(10) . . . . ?
C16 C17 C18 O12 -178.0(2) . . . . ?
C16 C17 C18 C13 1.7(3) . . . . ?
C10 C9 C8 Cl3 178.90(16) . . . . ?
C10 C9 C8 C7 -3.6(3) . . . . ?
C10 C9 C8 F3 179.5(8) . . . . ?
C4 C5 C6 Cl2 179.90(17) . . . . ?
C4 C5 C6 C1 -1.2(3) . . . . ?
C4 C5 C6 F2 174.4(9) . . . . ?
C4 C3 C2 O2 178.8(2) . . . . ?
C4 C3 C2 C1 -1.8(3) . . . . ?
C12 C7 C8 Cl3 -178.73(16) . . . . ?
C12 C7 C8 C9 3.8(3) . . . . ?
C12 C7 C8 F3 -179.5(8) . . . . ?
C8 C7 C12 O8 180.0(2) . . . . ?
C8 C7 C12 C11 0.1(3) . . . . ?
C8 C9 C10 O7 179.7(2) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C5 C4 C3 Cl1 -178.72(16) . . . . ?
C5 C4 C3 C2 1.0(3) . . . . ?
C5 C4 C3 F1 177.4(8) . . . . ?
C3 C4 C5 O4 -179.50(19) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C15 C16 C17 Cl6 178.99(17) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
C15 C16 C17 F6 -171.0(11) . . . . ?
C17 C16 C15 O10 178.80(19) . . . . ?
C17 C16 C15 C14 -0.5(3) . . . . ?
C2 C1 C6 Cl2 179.32(17) . . . . ?
C2 C1 C6 C5 0.4(3) . . . . ?
C2 C1 C6 F2 -175.1(9) . . . . ?
C18 C13 C14 Cl5 -177.83(17) . . . . ?
C18 C13 C14 C15 0.3(3) . . . . ?
C18 C13 C14 F5 175.3(10) . . . . ?
C22 N1 C25 C26 56.7(3) . . . . ?
C22 N1 C19 C20 -63.2(3) . . . . ?
C22 N1 C28 C29 176.9(2) . . . . ?
C6 C1 C2 O2 -179.4(2) . . . . ?
C6 C1 C2 C3 1.1(3) . . . . ?
C25 N1 C22 C23 56.9(3) . . . . ?
C25 N1 C19 C20 176.1(2) . . . . ?
C25 N1 C28 C29 -62.3(3) . . . . ?
C19 N1 C22 C23 -61.1(3) . . . . ?
C19 N1 C25 C26 177.3(2) . . . . ?
C19 N1 C28 C29 56.1(3) . . . . ?
C14 C13 C18 O12 178.1(2) . . . . ?
C14 C13 C18 C17 -1.5(3) . . . . ?
C28 N1 C22 C23 177.8(2) . . . . ?
C28 N1 C25 C26 -61.3(3) . . . . ?
C28 N1 C19 C20 54.9(3) . . . . ?
C34 N2 C37 C38 169.4(2) . . . . ?
C34 N2 C31 C32 -62.1(3) . . . . ?
C34 N2 C40 C41 -50.7(3) . . . . ?
C37 N2 C34 C35 62.4(3) . . . . ?
C37 N2 C31 C32 56.1(3) . . . . ?
C37 N2 C40 C41 -170.0(2) . . . . ?
C31 N2 C34 C35 -177.5(2) . . . . ?
C31 N2 C37 C38 50.7(3) . . . . ?
C31 N2 C40 C41 69.2(3) . . . . ?
C40 N2 C34 C35 -57.7(3) . . . . ?
C40 N2 C37 C38 -68.7(3) . . . . ?
C40 N2 C31 C32 175.9(2) . . . . ?
F6 C17 C18 O12 -8.0(12) . . . . ?
F6 C17 C18 C13 171.6(11) . . . . ?
F1 C3 C2 O2 2.3(8) . . . . ?
F1 C3 C2 C1 -178.3(7) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.741
_oxdiff_exptl_absorpt_empirical_full_min 0.474
####################################################################### 
# 
# 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_F-042_CCDC-2014822_R1
_database_code_depnum_ccdc_archive 'CCDC 2014822'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 Cl3.49 F2.51 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl3.49 F2.51 Fe2 N2 O15'
_chemical_formula_weight         1198.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Cl5.66 F0.34 Fe2 N2 O15'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.6602(8)
_cell_length_b                   22.2123(10)
_cell_length_c                   14.2016(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.210(4)
_cell_angle_gamma                90
_cell_volume                     5924.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19055
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.2680
_cell_measurement_theta_min      2.0940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.061
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.818
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0282173000
_diffrn_orient_matrix_UB_12      0.0153442000
_diffrn_orient_matrix_UB_13      -0.0343966000
_diffrn_orient_matrix_UB_21      0.0250762000
_diffrn_orient_matrix_UB_22      0.0177252000
_diffrn_orient_matrix_UB_23      -0.0147493000
_diffrn_orient_matrix_UB_31      0.0005300000
_diffrn_orient_matrix_UB_32      -0.0216974000
_diffrn_orient_matrix_UB_33      -0.0364890000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7500
_reflns_number_total             10838
_reflns_odcompleteness_completeness 90.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.21
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10838
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0754
_refine_ls_restrained_S_all      1.016
_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)+(0.1574P)²+6.8083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2266
_refine_ls_wR_factor_ref         0.2567
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-C8
 1.73 with sigma of 0.02
 C44-O13
 1.22 with sigma of 0.02
 Cl2-C6
 1.73 with sigma of 0.02
 Cl1-C3
 1.73 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C3-F1
 1.33 with sigma of 0.02
 C12-F4
 1.33 with sigma of 0.02
3. Rigid bond restraints
 C45, C44, O13, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O14) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: Cl6(0.6117) Cl3(0.5317) Cl5(0.6117) Cl2(0.6017) Cl1(0.6017)
 Cl4(0.5317) O15(0.5) O14(0.5) F1(0.3983) F6(0.3883) F4(0.4683) F5(0.3883)
 F2(0.3983) F3(0.4683)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C19(H19A,H19B), C28(H28A,H28B), C20(H20A,
 H20B), C29(H29A,H29B), C41(H41A,H41B), C26(H26A,H26B), C23(H23A,H23B),
 C40(H40A,H40B), C34(H34A,H34B), C31(H31A,H31B), C35(H35A,H35B), C37(H37A,H37B),
  C38(H38A,H38B), C32(H32A,H32B)
6.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C24(H24A,H24B,
 H24C), C42(H42A,H42B,H42C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C48(H48A,
 H48B,H48C), C47(H47A,H47B,H47C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe2 Fe 0.77848(3) 0.32266(3) 0.59817(4) 0.0402(2) Uani 1 1 d . . . . .
Fe1 Fe 0.76234(3) 0.67866(3) 0.59976(4) 0.0418(2) Uani 1 1 d . . . . .
Cl6 Cl 0.9214(4) 0.3177(3) 0.9575(4) 0.0530(9) Uani 0.6117 1 d . . P A 2
Cl3 Cl 0.6169(4) 0.4975(3) 0.6303(6) 0.0490(9) Uani 0.5317 1 d D . P B 2
Cl5 Cl 0.6371(3) 0.1818(3) 0.7422(4) 0.0611(10) Uani 0.6117 1 d . . P C 2
Cl2 Cl 0.6211(3) 0.6833(3) 0.2448(5) 0.0646(13) Uani 0.6017 1 d D . P D 2
Cl1 Cl 0.8979(2) 0.8249(3) 0.4567(4) 0.0581(9) Uani 0.6017 1 d D . P E 2
Cl4 Cl 0.9113(3) 0.5101(3) 0.5316(4) 0.0531(9) Uani 0.5317 1 d . . P F 2
O12 O 0.83880(14) 0.32069(12) 0.7390(2) 0.0407(6) Uani 1 1 d . . . . .
O6 O 0.70023(15) 0.68284(13) 0.4603(2) 0.0444(7) Uani 1 1 d . . . . .
O9 O 0.72164(14) 0.26606(13) 0.65215(19) 0.0444(7) Uani 1 1 d . . . . .
O11 O 0.83735(14) 0.23288(13) 1.04449(19) 0.0423(6) Uani 1 1 d . . . . .
O4 O 0.81984(15) 0.82270(12) 0.2416(2) 0.0432(7) Uani 1 1 d . . . . .
O5 O 0.70117(14) 0.60396(13) 0.6117(2) 0.0453(7) Uani 1 1 d . . . . .
O2 O 0.81790(14) 0.73816(13) 0.54793(19) 0.0430(7) Uani 1 1 d . . . . .
O3 O 0.70352(15) 0.76659(14) 0.1545(2) 0.0468(7) Uani 1 1 d . . . . .
O10 O 0.71738(15) 0.18150(13) 0.9576(2) 0.0437(7) Uani 1 1 d . . . . .
O7 O 0.83413(14) 0.39793(13) 0.5759(2) 0.0459(7) Uani 1 1 d . . . . .
O1 O 0.71193(15) 0.39339(13) 0.6130(2) 0.0452(7) Uani 1 1 d . . . . .
O8 O 0.82331(14) 0.60835(13) 0.5732(2) 0.0450(7) Uani 1 1 d . . . . .
N1 N 0.49208(18) 0.7977(2) -0.0014(3) 0.0551(10) Uani 1 1 d . . . . .
C2 C 0.7930(2) 0.74755(18) 0.4537(3) 0.0392(9) Uani 1 1 d . . . . .
C18 C 0.8135(2) 0.28812(18) 0.7960(3) 0.0380(9) Uani 1 1 d . . . . .
C13 C 0.7457(2) 0.25715(19) 0.7459(3) 0.0397(9) Uani 1 1 d . . . . .
C17 C 0.8442(2) 0.27970(19) 0.8962(3) 0.0409(9) Uani 1 1 d . . . . .
C1 C 0.7263(2) 0.71552(19) 0.4039(3) 0.0411(9) Uani 1 1 d . . . . .
C4 C 0.7939(2) 0.79110(18) 0.2982(3) 0.0390(9) Uani 1 1 d . . . . .
C5 C 0.7275(2) 0.75901(19) 0.2487(3) 0.0401(9) Uani 1 1 d . . . . .
C15 C 0.7441(2) 0.21351(19) 0.9005(3) 0.0405(9) Uani 1 1 d . . . . .
C9 C 0.7334(2) 0.4457(2) 0.6024(3) 0.0417(9) Uani 1 1 d . . . . .
C16 C 0.8123(2) 0.24364(18) 0.9508(3) 0.0396(9) Uani 1 1 d . . . . .
C7 C 0.7277(2) 0.5536(2) 0.6011(3) 0.0425(9) Uani 1 1 d . . . . .
C14 C 0.7135(2) 0.2213(2) 0.8008(3) 0.0435(10) Uani 1 1 d . . . . .
C6 C 0.6960(2) 0.7227(2) 0.3040(3) 0.0435(10) Uani 1 1 d D . . . .
C3 C 0.8234(2) 0.78452(19) 0.4002(3) 0.0415(9) Uani 1 1 d D . . . .
C10 C 0.8057(2) 0.4481(2) 0.5811(3) 0.0433(10) Uani 1 1 d . . . . .
N2 N 0.9488(2) 0.6480(2) 0.2790(3) 0.0732(13) Uani 1 1 d . . . . .
C11 C 0.8000(2) 0.5565(2) 0.5793(3) 0.0416(9) Uani 1 1 d . . . . .
C12 C 0.8334(2) 0.50365(19) 0.5677(3) 0.0456(10) Uani 1 1 d D . . . .
C22 C 0.4280(2) 0.7593(2) -0.0029(4) 0.0623(13) Uani 1 1 d . . . . .
H22A H 0.387644 0.786448 -0.004854 0.075 Uiso 1 1 calc R . . . .
H22B H 0.414645 0.735554 -0.064598 0.075 Uiso 1 1 calc R . . . .
C25 C 0.5563(2) 0.7583(2) 0.0014(4) 0.0635(13) Uani 1 1 d . . . . .
H25A H 0.596893 0.784929 0.002489 0.076 Uiso 1 1 calc R . . . .
H25B H 0.569402 0.735254 0.063869 0.076 Uiso 1 1 calc R . . . .
C8 C 0.6983(2) 0.49851(18) 0.6088(3) 0.0447(10) Uani 1 1 d D . . . .
C19 C 0.5151(3) 0.8373(2) 0.0897(4) 0.0620(13) Uani 1 1 d . . . . .
H19A H 0.558716 0.859330 0.088997 0.074 Uiso 1 1 calc R . . . .
H19B H 0.527507 0.811130 0.148727 0.074 Uiso 1 1 calc R . . . .
C28 C 0.4705(3) 0.8364(2) -0.0942(4) 0.0606(13) Uani 1 1 d . . . . .
H28A H 0.459778 0.809363 -0.152227 0.073 Uiso 1 1 calc R . . . .
H28B H 0.425993 0.857892 -0.096245 0.073 Uiso 1 1 calc R . . . .
C20 C 0.4597(3) 0.8830(3) 0.0996(4) 0.0684(14) Uani 1 1 d . . . . .
H20A H 0.413746 0.862467 0.092450 0.082 Uiso 1 1 calc R . . . .
H20B H 0.452249 0.913704 0.046982 0.082 Uiso 1 1 calc R . . . .
C29 C 0.5248(3) 0.8820(2) -0.1037(4) 0.0638(13) Uani 1 1 d . . . . .
H29A H 0.571952 0.862578 -0.091293 0.077 Uiso 1 1 calc R . . . .
H29B H 0.529031 0.914494 -0.054482 0.077 Uiso 1 1 calc R . . . .
C30 C 0.5012(4) 0.9084(3) -0.2076(5) 0.097(2) Uani 1 1 d . . . . .
H30A H 0.492537 0.875700 -0.256007 0.145 Uiso 1 1 calc GR . . . .
H30B H 0.538513 0.934946 -0.216804 0.145 Uiso 1 1 calc GR . . . .
H30C H 0.457220 0.931544 -0.216732 0.145 Uiso 1 1 calc GR . . . .
C41 C 1.0051(3) 0.7537(3) 0.2732(5) 0.0843(19) Uani 1 1 d . . . . .
H41A H 1.023265 0.745632 0.216463 0.101 Uiso 1 1 calc R . . . .
H41B H 1.042594 0.741866 0.333949 0.101 Uiso 1 1 calc R . . . .
C26 C 0.5457(3) 0.7143(3) -0.0835(5) 0.089(2) Uani 1 1 d . . . . .
H26A H 0.543331 0.736304 -0.145052 0.106 Uiso 1 1 calc R . . . .
H26B H 0.500586 0.691918 -0.093502 0.106 Uiso 1 1 calc R . . . .
C21 C 0.4857(4) 0.9133(3) 0.2008(5) 0.102(2) Uani 1 1 d . . . . .
H21A H 0.452716 0.945642 0.204777 0.154 Uiso 1 1 calc GR . . . .
H21B H 0.533261 0.930179 0.210039 0.154 Uiso 1 1 calc GR . . . .
H21C H 0.487666 0.883488 0.252438 0.154 Uiso 1 1 calc GR . . . .
C23 C 0.4374(3) 0.7170(3) 0.0817(5) 0.0876(19) Uani 1 1 d . . . . .
H23A H 0.439846 0.739878 0.142415 0.105 Uiso 1 1 calc R . . . .
H23B H 0.482393 0.694262 0.092640 0.105 Uiso 1 1 calc R . . . .
C40 C 0.9396(3) 0.7158(3) 0.2634(5) 0.0869(19) Uani 1 1 d . . . . .
H40A H 0.906602 0.722506 0.196595 0.104 Uiso 1 1 calc R . . . .
H40B H 0.915899 0.731305 0.311010 0.104 Uiso 1 1 calc R . . . .
C34 C 0.9969(4) 0.6338(3) 0.3810(4) 0.091(2) Uani 1 1 d . . . . .
H34A H 0.995926 0.589682 0.389963 0.109 Uiso 1 1 calc R . . . .
H34B H 1.046023 0.644570 0.382353 0.109 Uiso 1 1 calc R . . . .
C27 C 0.6087(3) 0.6704(3) -0.0586(6) 0.094(2) Uani 1 1 d . . . . .
H27A H 0.610939 0.650069 -0.118885 0.142 Uiso 1 1 calc GR . . . .
H27B H 0.602374 0.640389 -0.011304 0.142 Uiso 1 1 calc GR . . . .
H27C H 0.653019 0.692634 -0.029748 0.142 Uiso 1 1 calc GR . . . .
C31 C 0.8787(4) 0.6204(3) 0.2671(6) 0.100(2) Uani 1 1 d . . . . .
H31A H 0.856912 0.641055 0.312805 0.120 Uiso 1 1 calc R . . . .
H31B H 0.886740 0.577988 0.289112 0.120 Uiso 1 1 calc R . . . .
C24 C 0.3745(3) 0.6736(3) 0.0584(6) 0.094(2) Uani 1 1 d . . . . .
H24A H 0.377686 0.645833 0.006217 0.141 Uiso 1 1 calc GR . . . .
H24B H 0.329960 0.696401 0.036262 0.141 Uiso 1 1 calc GR . . . .
H24C H 0.375557 0.650661 0.117743 0.141 Uiso 1 1 calc GR . . . .
C35 C 0.9834(4) 0.6618(4) 0.4669(5) 0.099(2) Uani 1 1 d . . . . .
H35A H 0.934485 0.651616 0.467440 0.119 Uiso 1 1 calc R . . . .
H35B H 0.986230 0.706076 0.461248 0.119 Uiso 1 1 calc R . . . .
C37 C 0.9838(4) 0.6242(4) 0.2047(5) 0.102(2) Uani 1 1 d . . . . .
H37A H 0.955538 0.637426 0.138035 0.123 Uiso 1 1 calc R . . . .
H37B H 1.031736 0.642433 0.218626 0.123 Uiso 1 1 calc R . . . .
C38 C 0.9914(5) 0.5567(3) 0.2041(6) 0.113(3) Uani 1 1 d . . . . .
H38A H 0.943836 0.537852 0.190553 0.136 Uiso 1 1 calc R . . . .
H38B H 1.020905 0.542966 0.269818 0.136 Uiso 1 1 calc R . . . .
C42 C 0.9905(4) 0.8209(4) 0.2774(6) 0.113(3) Uani 1 1 d . . . . .
H42A H 0.961783 0.834777 0.212286 0.170 Uiso 1 1 calc GR . . . .
H42B H 1.035801 0.842882 0.296983 0.170 Uiso 1 1 calc GR . . . .
H42C H 0.964703 0.828310 0.325648 0.170 Uiso 1 1 calc GR . . . .
C36 C 1.0344(5) 0.6423(4) 0.5613(5) 0.139(4) Uani 1 1 d . . . . .
H36A H 1.083095 0.650803 0.560350 0.208 Uiso 1 1 calc GR . . . .
H36B H 1.029083 0.598922 0.570042 0.208 Uiso 1 1 calc GR . . . .
H36C H 1.024759 0.664110 0.615917 0.208 Uiso 1 1 calc GR . . . .
C33 C 0.7550(4) 0.5975(4) 0.1652(9) 0.153(4) Uani 1 1 d . . . . .
H33A H 0.726720 0.589924 0.096852 0.230 Uiso 1 1 calc GR . . . .
H33B H 0.730682 0.627227 0.194739 0.230 Uiso 1 1 calc GR . . . .
H33C H 0.760687 0.559848 0.202786 0.230 Uiso 1 1 calc GR . . . .
C32 C 0.8255(4) 0.6206(4) 0.1671(7) 0.131(3) Uani 1 1 d . . . . .
H32A H 0.820012 0.662327 0.141466 0.157 Uiso 1 1 calc R . . . .
H32B H 0.844132 0.595887 0.122208 0.157 Uiso 1 1 calc R . . . .
C48 C 0.8061(6) 0.3741(4) 0.1564(9) 0.158(4) Uani 1 1 d . U . . .
H48A H 0.819070 0.338649 0.198979 0.237 Uiso 1 1 calc GR . . . .
H48B H 0.834463 0.374892 0.110045 0.237 Uiso 1 1 calc GR . . . .
H48C H 0.755413 0.372269 0.119547 0.237 Uiso 1 1 calc GR . . . .
C47 C 0.7809(9) 0.4333(6) 0.2989(10) 0.221(7) Uani 1 1 d . U . . .
H47A H 0.729203 0.429676 0.270002 0.331 Uiso 1 1 calc GR . . . .
H47B H 0.792303 0.473101 0.329353 0.331 Uiso 1 1 calc GR . . . .
H47C H 0.797878 0.402069 0.348991 0.331 Uiso 1 1 calc GR . . . .
C46 C 0.8193(6) 0.4254(5) 0.2132(12) 0.174(5) Uani 1 1 d . U . . .
O16 O 0.8531(6) 0.4667(4) 0.1926(12) 0.302(7) Uani 1 1 d . U . . .
C39 C 1.0265(8) 0.5362(6) 0.1246(9) 0.222(7) Uani 1 1 d . . . . .
H39A H 0.999807 0.552936 0.060464 0.334 Uiso 1 1 calc GR . . . .
H39B H 1.026098 0.492177 0.120817 0.334 Uiso 1 1 calc GR . . . .
H39C H 1.075787 0.550701 0.142487 0.334 Uiso 1 1 calc GR . . . .
O15 O 0.4852(9) 0.5763(17) -0.0186(17) 0.285(14) Uani 0.5 1 d . U P G 3
O14 O 0.445(2) 0.4998(10) -0.0710(17) 0.290(14) Uani 0.5 1 d . U P H -3
F1 F 0.8885(9) 0.8083(8) 0.4475(15) 0.085(7) Uani 0.3983 1 d D . P E -2
F6 F 0.9087(12) 0.3042(10) 0.9387(15) 0.060(5) Uani 0.3883 1 d . . P A -2
F4 F 0.8990(7) 0.5031(6) 0.5559(10) 0.062(3) Uani 0.4683 1 d D . P F -2
F5 F 0.6489(11) 0.2000(8) 0.7576(14) 0.061(4) Uani 0.3883 1 d . . P C -2
F2 F 0.6308(10) 0.6988(10) 0.2618(17) 0.073(6) Uani 0.3983 1 d D . P D -2
F3 F 0.6349(8) 0.4938(8) 0.6289(17) 0.062(5) Uani 0.4683 1 d . . P B -2
C43 C 0.7540(6) 0.5572(4) -0.1223(7) 0.152(4) Uani 1 1 d . U . . .
H43A H 0.797560 0.551635 -0.141436 0.229 Uiso 1 1 calc GR . . . .
H43B H 0.764128 0.582798 -0.063652 0.229 Uiso 1 1 calc GR . . . .
H43C H 0.717521 0.576319 -0.176535 0.229 Uiso 1 1 calc GR . . . .
C45 C 0.7624(6) 0.4417(4) -0.1200(7) 0.141(3) Uani 1 1 d . U . . .
H45A H 0.729333 0.419745 -0.174483 0.212 Uiso 1 1 calc GR . . . .
H45B H 0.774902 0.416398 -0.060740 0.212 Uiso 1 1 calc GR . . . .
H45C H 0.805554 0.451757 -0.137609 0.212 Uiso 1 1 calc GR . . . .
C44 C 0.7279(8) 0.4979(4) -0.1003(10) 0.176(6) Uani 1 1 d D U . . .
O13 O 0.6679(7) 0.4972(4) -0.0814(12) 0.264(6) Uani 1 1 d D U . . .


_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
Fe2 O12 2.001(3) . ?
Fe2 O9 1.981(3) . ?
Fe2 O11 1.991(3) 4_565 ?
Fe2 O10 2.005(3) 4_565 ?
Fe2 O7 2.073(3) . ?
Fe2 O1 2.095(3) . ?
Fe1 O6 1.998(3) . ?
Fe1 O4 1.998(3) 4_576 ?
Fe1 O5 2.085(3) . ?
Fe1 O2 1.989(3) . ?
Fe1 O3 1.988(3) 4_576 ?
Fe1 O8 2.070(3) . ?
Cl6 C17 1.731(6) . ?
Cl3 C8 1.714(7) . ?
Cl5 C14 1.726(5) . ?
Cl2 C6 1.706(6) . ?
Cl1 C3 1.702(5) . ?
Cl4 C12 1.759(5) . ?
Cl4 F4 0.501(9) . ?
O12 C18 1.291(5) . ?
O6 C1 1.293(5) . ?
O9 C13 1.289(5) . ?
O11 C16 1.298(5) . ?
O4 C4 1.281(5) . ?
O5 C7 1.262(5) . ?
O2 C2 1.298(5) . ?
O3 C5 1.291(5) . ?
O10 C15 1.299(5) . ?
O7 C10 1.259(5) . ?
O1 C9 1.260(5) . ?
O8 C11 1.253(5) . ?
N1 C22 1.516(6) . ?
N1 C25 1.526(6) . ?
N1 C19 1.519(6) . ?
N1 C28 1.523(6) . ?
C2 C1 1.476(5) . ?
C2 C3 1.371(6) . ?
C18 C13 1.480(5) . ?
C18 C17 1.384(5) . ?
C13 C14 1.392(6) . ?
C17 C16 1.386(6) . ?
C17 F6 1.348(18) . ?
C1 C6 1.376(6) . ?
C4 C5 1.470(5) . ?
C4 C3 1.400(6) . ?
C5 C6 1.392(6) . ?
C15 C16 1.480(5) . ?
C15 C14 1.376(6) . ?
C9 C10 1.538(5) . ?
C9 C8 1.379(6) . ?
C7 C11 1.543(5) . ?
C7 C8 1.371(6) . ?
C14 F5 1.324(15) . ?
C6 F2 1.353(15) . ?
C3 F1 1.365(14) . ?
C10 C12 1.384(6) . ?
N2 C40 1.525(8) . ?
N2 C34 1.510(7) . ?
N2 C31 1.471(8) . ?
N2 C37 1.517(7) . ?
C11 C12 1.378(6) . ?
C12 F4 1.350(11) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.493(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.520(8) . ?
C8 F3 1.362(15) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.524(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.508(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.532(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.527(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C40 1.510(8) . ?
C41 C42 1.524(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.533(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.525(7) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.461(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.495(10) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.481(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.507(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.555(12) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C32 1.470(11) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C46 1.376(15) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C47 C46 1.620(17) . ?
C46 O16 1.218(12) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C44 1.479(12) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C45 C44 1.487(13) . ?
C44 O13 1.284(12) . ?

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
O12 Fe2 O10 176.08(12) . 4_565 ?
O12 Fe2 O7 89.25(11) . . ?
O12 Fe2 O1 96.82(11) . . ?
O9 Fe2 O12 80.49(11) . . ?
O9 Fe2 O11 102.32(12) . 4_565 ?
O9 Fe2 O10 96.65(11) . 4_565 ?
O9 Fe2 O7 162.68(12) . . ?
O9 Fe2 O1 89.78(12) . . ?
O11 Fe2 O12 97.44(11) 4_565 . ?
O11 Fe2 O10 80.50(11) 4_565 4_565 ?
O11 Fe2 O7 92.77(11) 4_565 . ?
O11 Fe2 O1 162.63(11) 4_565 . ?
O10 Fe2 O7 94.17(12) 4_565 . ?
O10 Fe2 O1 85.81(11) 4_565 . ?
O7 Fe2 O1 77.53(11) . . ?
O6 Fe1 O4 176.46(12) . 4_576 ?
O6 Fe1 O5 85.37(11) . . ?
O6 Fe1 O8 94.09(12) . . ?
O4 Fe1 O5 94.25(12) 4_576 . ?
O4 Fe1 O8 89.27(11) 4_576 . ?
O2 Fe1 O6 81.01(11) . . ?
O2 Fe1 O4 100.05(11) . 4_576 ?
O2 Fe1 O5 162.11(11) . . ?
O2 Fe1 O8 91.30(11) . . ?
O3 Fe1 O6 95.94(12) 4_576 . ?
O3 Fe1 O4 80.56(11) 4_576 4_576 ?
O3 Fe1 O5 92.23(12) 4_576 . ?
O3 Fe1 O2 100.64(12) 4_576 . ?
O3 Fe1 O8 165.45(12) 4_576 . ?
O8 Fe1 O5 78.09(11) . . ?
F4 Cl4 C12 30(2) . . ?
C18 O12 Fe2 114.5(2) . . ?
C1 O6 Fe1 113.7(2) . . ?
C13 O9 Fe2 114.8(2) . . ?
C16 O11 Fe2 114.8(2) . 4_566 ?
C4 O4 Fe1 114.3(2) . 4_575 ?
C7 O5 Fe1 115.3(3) . . ?
C2 O2 Fe1 114.0(2) . . ?
C5 O3 Fe1 114.1(2) . 4_575 ?
C15 O10 Fe2 114.4(2) . 4_566 ?
C10 O7 Fe2 116.2(2) . . ?
C9 O1 Fe2 115.9(2) . . ?
C11 O8 Fe1 116.0(2) . . ?
C22 N1 C25 110.8(4) . . ?
C22 N1 C19 112.0(4) . . ?
C22 N1 C28 106.7(4) . . ?
C19 N1 C25 105.9(4) . . ?
C19 N1 C28 110.3(4) . . ?
C28 N1 C25 111.3(4) . . ?
O2 C2 C1 115.3(3) . . ?
O2 C2 C3 125.0(4) . . ?
C3 C2 C1 119.6(4) . . ?
O12 C18 C13 114.7(3) . . ?
O12 C18 C17 126.1(4) . . ?
C17 C18 C13 119.2(3) . . ?
O9 C13 C18 115.4(3) . . ?
O9 C13 C14 125.2(4) . . ?
C14 C13 C18 119.4(3) . . ?
C18 C17 Cl6 120.1(4) . . ?
C18 C17 C16 121.4(4) . . ?
C16 C17 Cl6 118.3(4) . . ?
F6 C17 Cl6 7.3(14) . . ?
F6 C17 C18 118.2(11) . . ?
F6 C17 C16 120.2(11) . . ?
O6 C1 C2 115.6(3) . . ?
O6 C1 C6 125.1(4) . . ?
C6 C1 C2 119.3(4) . . ?
O4 C4 C5 115.4(3) . . ?
O4 C4 C3 125.8(4) . . ?
C3 C4 C5 118.8(4) . . ?
O3 C5 C4 115.6(3) . . ?
O3 C5 C6 125.0(4) . . ?
C6 C5 C4 119.4(3) . . ?
O10 C15 C16 115.0(3) . . ?
O10 C15 C14 125.2(4) . . ?
C14 C15 C16 119.8(4) . . ?
O1 C9 C10 114.7(4) . . ?
O1 C9 C8 125.7(4) . . ?
C8 C9 C10 119.6(4) . . ?
O11 C16 C17 125.7(3) . . ?
O11 C16 C15 115.2(3) . . ?
C17 C16 C15 119.1(3) . . ?
O5 C7 C11 115.1(4) . . ?
O5 C7 C8 125.7(4) . . ?
C8 C7 C11 119.2(4) . . ?
C13 C14 Cl5 119.7(4) . . ?
C15 C14 Cl5 119.1(4) . . ?
C15 C14 C13 121.0(4) . . ?
F5 C14 Cl5 10.4(12) . . ?
F5 C14 C13 118.6(9) . . ?
F5 C14 C15 120.0(9) . . ?
C1 C6 Cl2 119.7(4) . . ?
C1 C6 C5 121.4(4) . . ?
C5 C6 Cl2 118.8(4) . . ?
F2 C6 Cl2 9.4(13) . . ?
F2 C6 C1 118.3(11) . . ?
F2 C6 C5 119.9(11) . . ?
C2 C3 Cl1 120.6(4) . . ?
C2 C3 C4 121.4(4) . . ?
C4 C3 Cl1 118.0(4) . . ?
F1 C3 Cl1 9.1(10) . . ?
F1 C3 C2 117.3(10) . . ?
F1 C3 C4 120.7(10) . . ?
O7 C10 C9 115.7(4) . . ?
O7 C10 C12 125.5(4) . . ?
C12 C10 C9 118.8(4) . . ?
C34 N2 C40 111.0(5) . . ?
C34 N2 C37 108.1(5) . . ?
C31 N2 C40 109.2(4) . . ?
C31 N2 C34 108.8(5) . . ?
C31 N2 C37 112.2(5) . . ?
C37 N2 C40 107.5(5) . . ?
O8 C11 C7 115.5(4) . . ?
O8 C11 C12 125.3(4) . . ?
C12 C11 C7 119.2(4) . . ?
C10 C12 Cl4 121.7(4) . . ?
C11 C12 Cl4 116.8(4) . . ?
C11 C12 C10 121.5(4) . . ?
F4 C12 Cl4 10.8(7) . . ?
F4 C12 C10 116.0(7) . . ?
F4 C12 C11 122.0(7) . . ?
N1 C22 H22A 108.3 . . ?
N1 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N1 116.0(4) . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
N1 C25 H25A 108.4 . . ?
N1 C25 H25B 108.4 . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 N1 115.5(4) . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C9 C8 Cl3 120.9(4) . . ?
C7 C8 Cl3 117.6(4) . . ?
C7 C8 C9 121.5(4) . . ?
F3 C8 Cl3 4.1(10) . . ?
F3 C8 C9 117.1(8) . . ?
F3 C8 C7 121.3(8) . . ?
N1 C19 H19A 108.5 . . ?
N1 C19 H19B 108.5 . . ?
N1 C19 C20 115.0(4) . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
N1 C28 H28A 108.4 . . ?
N1 C28 H28B 108.4 . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 N1 115.6(4) . . ?
C29 C28 H28A 108.4 . . ?
C29 C28 H28B 108.4 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
C19 C20 C21 109.3(5) . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
C28 C29 H29A 109.9 . . ?
C28 C29 H29B 109.9 . . ?
C28 C29 C30 108.9(5) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 109.9 . . ?
C30 C29 H29B 109.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H41A C41 H41B 107.8 . . ?
C40 C41 H41A 109.1 . . ?
C40 C41 H41B 109.1 . . ?
C40 C41 C42 112.7(5) . . ?
C42 C41 H41A 109.1 . . ?
C42 C41 H41B 109.1 . . ?
C25 C26 H26A 110.0 . . ?
C25 C26 H26B 110.0 . . ?
C25 C26 C27 108.4(5) . . ?
H26A C26 H26B 108.4 . . ?
C27 C26 H26A 110.0 . . ?
C27 C26 H26B 110.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
C22 C23 C24 108.9(5) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
N2 C40 H40A 107.7 . . ?
N2 C40 H40B 107.7 . . ?
C41 C40 N2 118.5(5) . . ?
C41 C40 H40A 107.7 . . ?
C41 C40 H40B 107.7 . . ?
H40A C40 H40B 107.1 . . ?
N2 C34 H34A 107.4 . . ?
N2 C34 H34B 107.4 . . ?
H34A C34 H34B 106.9 . . ?
C35 C34 N2 119.7(5) . . ?
C35 C34 H34A 107.4 . . ?
C35 C34 H34B 107.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C31 H31A 107.7 . . ?
N2 C31 H31B 107.7 . . ?
N2 C31 C32 118.5(6) . . ?
H31A C31 H31B 107.1 . . ?
C32 C31 H31A 107.7 . . ?
C32 C31 H31B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C34 C35 H35A 109.0 . . ?
C34 C35 H35B 109.0 . . ?
C34 C35 C36 112.9(7) . . ?
H35A C35 H35B 107.8 . . ?
C36 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
N2 C37 H37A 108.6 . . ?
N2 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 N2 114.6(6) . . ?
C38 C37 H37A 108.6 . . ?
C38 C37 H37B 108.6 . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
C37 C38 C39 111.1(9) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
C31 C32 H32A 108.7 . . ?
C31 C32 H32B 108.7 . . ?
C33 C32 C31 114.0(9) . . ?
C33 C32 H32A 108.7 . . ?
C33 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
C48 C46 C47 118.8(10) . . ?
O16 C46 C48 120.3(16) . . ?
O16 C46 C47 120.5(13) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Cl4 F4 C12 139(3) . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
C43 C44 C45 120.1(10) . . ?
O13 C44 C43 116.9(11) . . ?
O13 C44 C45 121.8(10) . . ?

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
Fe2 O12 C18 C13 1.6(4) . . . . ?
Fe2 O12 C18 C17 -179.3(3) . . . . ?
Fe2 O9 C13 C18 -3.0(4) . . . . ?
Fe2 O9 C13 C14 177.3(3) . . . . ?
Fe2 O11 C16 C17 -178.7(3) 4_566 . . . ?
Fe2 O11 C16 C15 0.8(4) 4_566 . . . ?
Fe2 O10 C15 C16 -3.3(4) 4_566 . . . ?
Fe2 O10 C15 C14 177.5(3) 4_566 . . . ?
Fe2 O7 C10 C9 -0.6(5) . . . . ?
Fe2 O7 C10 C12 -179.4(4) . . . . ?
Fe2 O1 C9 C10 -0.6(4) . . . . ?
Fe2 O1 C9 C8 179.9(3) . . . . ?
Fe1 O6 C1 C2 -5.0(4) . . . . ?
Fe1 O6 C1 C6 176.0(3) . . . . ?
Fe1 O4 C4 C5 0.9(4) 4_575 . . . ?
Fe1 O4 C4 C3 -179.8(3) 4_575 . . . ?
Fe1 O5 C7 C11 -1.2(4) . . . . ?
Fe1 O5 C7 C8 177.9(4) . . . . ?
Fe1 O2 C2 C1 3.5(4) . . . . ?
Fe1 O2 C2 C3 -177.2(3) . . . . ?
Fe1 O3 C5 C4 -0.9(4) 4_575 . . . ?
Fe1 O3 C5 C6 -179.7(3) 4_575 . . . ?
Fe1 O8 C11 C7 2.6(4) . . . . ?
Fe1 O8 C11 C12 -177.6(3) . . . . ?
Cl6 C17 C16 O11 -3.9(7) . . . . ?
Cl6 C17 C16 C15 176.6(4) . . . . ?
O12 C18 C13 O9 0.9(5) . . . . ?
O12 C18 C13 C14 -179.4(4) . . . . ?
O12 C18 C17 Cl6 3.5(7) . . . . ?
O12 C18 C17 C16 180.0(4) . . . . ?
O12 C18 C17 F6 -4.5(14) . . . . ?
O6 C1 C6 Cl2 -3.9(7) . . . . ?
O6 C1 C6 C5 179.8(4) . . . . ?
O6 C1 C6 F2 6.7(14) . . . . ?
O9 C13 C14 Cl5 3.1(7) . . . . ?
O9 C13 C14 C15 178.7(4) . . . . ?
O9 C13 C14 F5 -8.7(13) . . . . ?
O4 C4 C5 O3 0.0(5) . . . . ?
O4 C4 C5 C6 178.9(4) . . . . ?
O4 C4 C3 Cl1 3.8(6) . . . . ?
O4 C4 C3 C2 -177.3(4) . . . . ?
O4 C4 C3 F1 -6.1(12) . . . . ?
O5 C7 C11 O8 -1.0(5) . . . . ?
O5 C7 C11 C12 179.3(4) . . . . ?
O5 C7 C8 Cl3 2.5(7) . . . . ?
O5 C7 C8 C9 -175.8(4) . . . . ?
O5 C7 C8 F3 0.4(13) . . . . ?
O2 C2 C1 O6 1.0(5) . . . . ?
O2 C2 C1 C6 -179.9(4) . . . . ?
O2 C2 C3 Cl1 -2.6(6) . . . . ?
O2 C2 C3 C4 178.5(4) . . . . ?
O2 C2 C3 F1 7.1(11) . . . . ?
O3 C5 C6 Cl2 1.5(7) . . . . ?
O3 C5 C6 C1 177.9(4) . . . . ?
O3 C5 C6 F2 -9.2(14) . . . . ?
O10 C15 C16 O11 1.6(5) . . . . ?
O10 C15 C16 C17 -178.8(4) . . . . ?
O10 C15 C14 Cl5 -5.2(7) . . . . ?
O10 C15 C14 C13 179.2(4) . . . . ?
O10 C15 C14 F5 6.7(13) . . . . ?
O7 C10 C12 Cl4 4.9(7) . . . . ?
O7 C10 C12 C11 -177.0(4) . . . . ?
O7 C10 C12 F4 -5.5(10) . . . . ?
O1 C9 C10 O7 0.8(5) . . . . ?
O1 C9 C10 C12 179.6(4) . . . . ?
O1 C9 C8 Cl3 -1.6(7) . . . . ?
O1 C9 C8 C7 176.5(4) . . . . ?
O1 C9 C8 F3 0.3(13) . . . . ?
O8 C11 C12 Cl4 -5.5(6) . . . . ?
O8 C11 C12 C10 176.4(4) . . . . ?
O8 C11 C12 F4 5.4(10) . . . . ?
N1 C22 C23 C24 -168.6(5) . . . . ?
N1 C25 C26 C27 -168.8(5) . . . . ?
N1 C19 C20 C21 172.1(4) . . . . ?
N1 C28 C29 C30 169.7(4) . . . . ?
C2 C1 C6 Cl2 177.1(4) . . . . ?
C2 C1 C6 C5 0.8(6) . . . . ?
C2 C1 C6 F2 -172.3(13) . . . . ?
C18 C13 C14 Cl5 -176.5(4) . . . . ?
C18 C13 C14 C15 -1.0(6) . . . . ?
C18 C13 C14 F5 171.7(12) . . . . ?
C18 C17 C16 O11 179.6(4) . . . . ?
C18 C17 C16 C15 0.1(6) . . . . ?
C13 C18 C17 Cl6 -177.4(4) . . . . ?
C13 C18 C17 C16 -1.0(6) . . . . ?
C13 C18 C17 F6 174.5(13) . . . . ?
C17 C18 C13 O9 -178.2(4) . . . . ?
C17 C18 C13 C14 1.4(6) . . . . ?
C1 C2 C3 Cl1 176.7(4) . . . . ?
C1 C2 C3 C4 -2.2(6) . . . . ?
C1 C2 C3 F1 -173.7(10) . . . . ?
C4 C5 C6 Cl2 -177.3(4) . . . . ?
C4 C5 C6 C1 -0.9(6) . . . . ?
C4 C5 C6 F2 172.0(13) . . . . ?
C5 C4 C3 Cl1 -176.9(4) . . . . ?
C5 C4 C3 C2 2.0(6) . . . . ?
C5 C4 C3 F1 173.2(10) . . . . ?
C9 C10 C12 Cl4 -173.8(4) . . . . ?
C9 C10 C12 C11 4.2(7) . . . . ?
C9 C10 C12 F4 175.7(8) . . . . ?
C16 C15 C14 Cl5 175.6(4) . . . . ?
C16 C15 C14 C13 0.0(6) . . . . ?
C16 C15 C14 F5 -172.5(12) . . . . ?
C7 C11 C12 Cl4 174.2(4) . . . . ?
C7 C11 C12 C10 -3.9(7) . . . . ?
C7 C11 C12 F4 -174.9(8) . . . . ?
C14 C15 C16 O11 -179.1(4) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C3 C2 C1 O6 -178.3(4) . . . . ?
C3 C2 C1 C6 0.8(6) . . . . ?
C3 C4 C5 O3 -179.4(4) . . . . ?
C3 C4 C5 C6 -0.4(6) . . . . ?
C10 C9 C8 Cl3 178.8(4) . . . . ?
C10 C9 C8 C7 -3.0(7) . . . . ?
C10 C9 C8 F3 -179.3(11) . . . . ?
C10 C12 F4 Cl4 124(4) . . . . ?
N2 C34 C35 C36 178.8(7) . . . . ?
N2 C31 C32 C33 -174.2(7) . . . . ?
N2 C37 C38 C39 179.0(8) . . . . ?
C11 C7 C8 Cl3 -178.5(4) . . . . ?
C11 C7 C8 C9 3.3(7) . . . . ?
C11 C7 C8 F3 179.4(12) . . . . ?
C11 C12 F4 Cl4 -64(5) . . . . ?
C22 N1 C25 C26 58.3(6) . . . . ?
C22 N1 C19 C20 -61.9(6) . . . . ?
C22 N1 C28 C29 175.2(4) . . . . ?
C25 N1 C22 C23 58.2(6) . . . . ?
C25 N1 C19 C20 177.3(4) . . . . ?
C25 N1 C28 C29 -63.8(5) . . . . ?
C8 C9 C10 O7 -179.7(4) . . . . ?
C8 C9 C10 C12 -0.8(6) . . . . ?
C8 C7 C11 O8 179.9(4) . . . . ?
C8 C7 C11 C12 0.1(6) . . . . ?
C19 N1 C22 C23 -59.8(6) . . . . ?
C19 N1 C25 C26 179.9(5) . . . . ?
C19 N1 C28 C29 53.4(5) . . . . ?
C28 N1 C22 C23 179.4(5) . . . . ?
C28 N1 C25 C26 -60.2(6) . . . . ?
C28 N1 C19 C20 56.8(5) . . . . ?
C40 N2 C34 C35 50.3(8) . . . . ?
C40 N2 C31 C32 67.6(8) . . . . ?
C40 N2 C37 C38 -175.2(6) . . . . ?
C34 N2 C40 C41 59.4(7) . . . . ?
C34 N2 C31 C32 -171.2(6) . . . . ?
C34 N2 C37 C38 64.9(8) . . . . ?
C31 N2 C40 C41 179.3(6) . . . . ?
C31 N2 C34 C35 -69.9(8) . . . . ?
C31 N2 C37 C38 -55.1(8) . . . . ?
C37 N2 C40 C41 -58.7(7) . . . . ?
C37 N2 C34 C35 168.0(7) . . . . ?
C37 N2 C31 C32 -51.6(8) . . . . ?
C42 C41 C40 N2 -167.9(6) . . . . ?
F6 C17 C16 O11 4.2(15) . . . . ?
F6 C17 C16 C15 -175.3(14) . . . . ?
F4 Cl4 C12 C10 -61(5) . . . . ?
F4 Cl4 C12 C11 121(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.600
_oxdiff_exptl_absorpt_empirical_full_min 0.631
####################################################################### 
# 
# 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_F-017-d_CCDC-2014817_R1
_database_code_depnum_ccdc_archive 'CCDC 2014817'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-27
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl4.98 F1.02 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl4.98 F1.02 Fe2 N2 O12'
_chemical_formula_weight         1088.51
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl4.98 F1.02 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.6203(4)
_cell_length_b                   20.9025(5)
_cell_length_c                   12.2015(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.021(4)
_cell_angle_gamma                90
_cell_volume                     2658.67(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13305
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.1030
_cell_measurement_theta_min      2.5220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.137
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21062
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.528
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0129223000
_diffrn_orient_matrix_UB_12      -0.0141219000
_diffrn_orient_matrix_UB_13      -0.0495534000
_diffrn_orient_matrix_UB_21      0.0582309000
_diffrn_orient_matrix_UB_22      0.0174138000
_diffrn_orient_matrix_UB_23      0.0063617000
_diffrn_orient_matrix_UB_31      0.0327633000
_diffrn_orient_matrix_UB_32      -0.0254580000
_diffrn_orient_matrix_UB_33      0.0318340000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5211
_reflns_number_total             5996
_reflns_odcompleteness_completeness 88.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.99
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.105
_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)+(0.0395P)²+2.3181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0978
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-F1
 1.33 with sigma of 0.02
3. Others
 Fixed Sof: Cl2(0.835) Cl1(0.835) Cl3(0.82) F2(0.165) F1(0.165) F3(0.18)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C13(H13A,H13B), C16(H16A,H16B), C20(H20A,H20B), C10(H10A,
 H10B), C17(H17A,H17B), C11(H11A,H11B), C14(H14A,H14B)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe -0.04437(3) 0.31267(2) 0.51700(2) 0.02424(9) Uani 1 1 d . . . . .
Cl2 Cl 0.06432(13) 0.32623(6) 0.93315(10) 0.0309(2) Uani 0.835 1 d . . P A 2
Cl1 Cl 0.33593(18) 0.17004(9) 0.60176(15) 0.0330(2) Uani 0.835 1 d . . P B 2
Cl3 Cl -0.29945(10) 0.51924(6) 0.48547(11) 0.0337(2) Uani 0.82 1 d . . P C 2
O4 O 0.30189(13) 0.24307(7) 0.98804(11) 0.0266(3) Uani 1 1 d . . . . .
O2 O 0.09593(13) 0.24899(7) 0.54705(11) 0.0261(3) Uani 1 1 d . . . . .
O3 O 0.42007(13) 0.18554(7) 0.85063(11) 0.0265(3) Uani 1 1 d . . . . .
O1 O -0.01588(13) 0.31322(7) 0.68338(11) 0.0259(3) Uani 1 1 d . . . . .
O5 O -0.14643(13) 0.39716(7) 0.51671(12) 0.0284(3) Uani 1 1 d . . . . .
O6 O -0.09752(13) 0.61827(7) 0.48330(12) 0.0279(3) Uani 1 1 d . . . . .
N00B N 0.60552(18) 0.35954(9) 0.74748(15) 0.0332(4) Uani 1 1 d . . . . .
C4 C 0.31477(18) 0.21343(9) 0.80574(16) 0.0236(4) Uani 1 1 d . . . . .
C2 C 0.15074(18) 0.24681(9) 0.65085(15) 0.0225(4) Uani 1 1 d . . . . .
C5 C 0.24902(18) 0.24824(9) 0.88345(15) 0.0236(4) Uani 1 1 d . . . . .
C3 C 0.26221(19) 0.21321(10) 0.69213(16) 0.0250(4) Uani 1 1 d D . . . .
C1 C 0.08702(18) 0.28345(9) 0.72841(16) 0.0229(4) Uani 1 1 d . . . . .
C6 C 0.13922(19) 0.28325(9) 0.84228(16) 0.0250(4) Uani 1 1 d . . . . .
C9 C -0.05922(19) 0.56150(10) 0.49031(16) 0.0252(4) Uani 1 1 d . . . . .
C7 C -0.08499(19) 0.44746(10) 0.50704(16) 0.0252(4) Uani 1 1 d . . . . .
C19 C 0.6056(2) 0.28849(11) 0.7735(2) 0.0350(5) Uani 1 1 d . . . . .
H19A H 0.6115 0.2833 0.8550 0.042 Uiso 1 1 calc R U . . .
H19B H 0.5224 0.2703 0.7362 0.042 Uiso 1 1 calc R U . . .
C13 C 0.4885(2) 0.38977(12) 0.7809(2) 0.0420(5) Uani 1 1 d . . . . .
H13A H 0.4817 0.4345 0.7535 0.050 Uiso 1 1 calc R U . . .
H13B H 0.4114 0.3667 0.7420 0.050 Uiso 1 1 calc R U . . .
C8 C -0.13626(18) 0.50853(10) 0.49521(17) 0.0271(4) Uani 1 1 d . . . . .
C16 C 0.5994(2) 0.37129(12) 0.62387(18) 0.0365(5) Uani 1 1 d . . . . .
H16A H 0.5864 0.4177 0.6098 0.044 Uiso 1 1 calc R U . . .
H16B H 0.6839 0.3600 0.6062 0.044 Uiso 1 1 calc R U . . .
C20 C 0.7121(2) 0.24964(12) 0.7389(2) 0.0370(5) Uani 1 1 d . . . . .
H20A H 0.7958 0.2627 0.7840 0.044 Uiso 1 1 calc R U . . .
H20B H 0.7141 0.2579 0.6594 0.044 Uiso 1 1 calc R U . . .
C10 C 0.7297(2) 0.38866(12) 0.8103(2) 0.0412(5) Uani 1 1 d . . . . .
H10A H 0.7399 0.3765 0.8900 0.049 Uiso 1 1 calc R U . . .
H10B H 0.8020 0.3694 0.7813 0.049 Uiso 1 1 calc R U . . .
C17 C 0.4971(3) 0.33571(12) 0.5432(2) 0.0433(6) Uani 1 1 d . . . . .
H17A H 0.4114 0.3449 0.5601 0.052 Uiso 1 1 calc R U . . .
H17B H 0.5125 0.2890 0.5500 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6902(2) 0.17882(12) 0.7561(2) 0.0450(6) Uani 1 1 d . . . . .
H21A H 0.6063 0.1663 0.7129 0.068 Uiso 1 1 calc R U . . .
H21B H 0.6927 0.1705 0.8355 0.068 Uiso 1 1 calc R U . . .
H21C H 0.7575 0.1540 0.7308 0.068 Uiso 1 1 calc R U . . .
C11 C 0.7399(3) 0.46088(13) 0.8033(2) 0.0522(7) Uani 1 1 d . . . . .
H11A H 0.6684 0.4812 0.8320 0.063 Uiso 1 1 calc R U . . .
H11B H 0.7338 0.4740 0.7245 0.063 Uiso 1 1 calc R U . . .
C14 C 0.4859(3) 0.39057(14) 0.9044(3) 0.0580(8) Uani 1 1 d . . . . .
H14A H 0.5632 0.4126 0.9455 0.070 Uiso 1 1 calc R U . . .
H14B H 0.4861 0.3462 0.9328 0.070 Uiso 1 1 calc R U . . .
C18 C 0.5032(3) 0.35809(14) 0.4247(2) 0.0506(6) Uani 1 1 d . . . . .
H18A H 0.4493 0.3303 0.3703 0.076 Uiso 1 1 calc R U . . .
H18B H 0.5921 0.3561 0.4135 0.076 Uiso 1 1 calc R U . . .
H18C H 0.4721 0.4022 0.4145 0.076 Uiso 1 1 calc R U . . .
C15 C 0.3660(4) 0.42516(16) 0.9232(3) 0.0758(11) Uani 1 1 d . . . . .
H15A H 0.2903 0.4057 0.8765 0.114 Uiso 1 1 calc R U . . .
H15B H 0.3711 0.4704 0.9032 0.114 Uiso 1 1 calc R U . . .
H15C H 0.3592 0.4217 1.0019 0.114 Uiso 1 1 calc R U . . .
C12 C 0.8675(4) 0.48270(17) 0.8721(4) 0.0864(13) Uani 1 1 d . . . . .
H12A H 0.9379 0.4640 0.8413 0.130 Uiso 1 1 calc R U . . .
H12B H 0.8739 0.4687 0.9496 0.130 Uiso 1 1 calc R U . . .
H12C H 0.8729 0.5295 0.8696 0.130 Uiso 1 1 calc R U . . .
F2 F 0.0764(18) 0.3084(7) 0.9147(15) 0.045(4) Uani 0.165 1 d . . P A -2
F1 F 0.329(2) 0.1848(11) 0.6191(18) 0.050(6) Uani 0.165 1 d D . P B -2
F3 F -0.2608(13) 0.5144(8) 0.5116(13) 0.053(4) Uani 0.18 1 d . . P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 O4 1.9818(14) 4_565 ?
Fe01 O2 1.9793(14) . ?
Fe01 O3 1.9928(14) 4_565 ?
Fe01 O1 1.9945(14) . ?
Fe01 O5 2.0716(14) . ?
Fe01 O6 2.0872(14) 3_566 ?
Cl2 C6 1.734(2) . ?
Cl2 F2 0.467(11) . ?
Cl1 C3 1.724(2) . ?
Cl3 C8 1.729(2) . ?
O4 Fe01 1.9818(14) 4_666 ?
O4 C5 1.297(2) . ?
O2 C2 1.290(2) . ?
O3 Fe01 1.9928(14) 4_666 ?
O3 C4 1.287(2) . ?
O1 C1 1.286(2) . ?
O5 C7 1.255(2) . ?
O6 Fe01 2.0873(14) 3_566 ?
O6 C9 1.252(2) . ?
N00B C19 1.519(3) . ?
N00B C13 1.518(3) . ?
N00B C16 1.517(3) . ?
N00B C10 1.520(3) . ?
C4 C5 1.473(3) . ?
C4 C3 1.392(3) . ?
C2 C3 1.386(3) . ?
C2 C1 1.478(3) . ?
C5 C6 1.387(3) . ?
C3 F1 1.377(14) . ?
C1 C6 1.394(3) . ?
C6 F2 1.314(14) . ?
C9 C7 1.537(3) 3_566 ?
C9 C8 1.385(3) . ?
C7 C9 1.537(3) 3_566 ?
C7 C8 1.384(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.516(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.512(4) . ?
C8 F3 1.381(16) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.514(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.519(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.517(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.533(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.521(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.520(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
O4 Fe01 O3 80.80(5) 4_565 4_565 ?
O4 Fe01 O1 98.30(6) 4_565 . ?
O4 Fe01 O5 95.04(6) 4_565 . ?
O4 Fe01 O6 167.62(6) 4_565 3_566 ?
O2 Fe01 O4 101.71(6) . 4_565 ?
O2 Fe01 O3 100.99(6) . 4_565 ?
O2 Fe01 O1 81.54(6) . . ?
O2 Fe01 O5 161.57(6) . . ?
O2 Fe01 O6 86.97(6) . 3_566 ?
O3 Fe01 O1 177.43(6) 4_565 . ?
O3 Fe01 O5 89.15(6) 4_565 . ?
O3 Fe01 O6 88.95(6) 4_565 3_566 ?
O1 Fe01 O5 88.54(6) . . ?
O1 Fe01 O6 91.65(6) . 3_566 ?
O5 Fe01 O6 77.77(5) . 3_566 ?
F2 Cl2 C6 22(3) . . ?
C5 O4 Fe01 114.30(12) . 4_666 ?
C2 O2 Fe01 112.83(12) . . ?
C4 O3 Fe01 113.90(12) . 4_666 ?
C1 O1 Fe01 112.54(12) . . ?
C7 O5 Fe01 115.67(13) . . ?
C9 O6 Fe01 115.49(13) . 3_566 ?
C19 N00B C10 108.67(18) . . ?
C13 N00B C19 108.59(17) . . ?
C13 N00B C10 111.93(19) . . ?
C16 N00B C19 111.38(17) . . ?
C16 N00B C13 108.57(18) . . ?
C16 N00B C10 107.74(17) . . ?
O3 C4 C5 115.48(17) . . ?
O3 C4 C3 124.94(18) . . ?
C3 C4 C5 119.58(17) . . ?
O2 C2 C3 124.65(17) . . ?
O2 C2 C1 115.76(17) . . ?
C3 C2 C1 119.59(16) . . ?
O4 C5 C4 115.02(17) . . ?
O4 C5 C6 125.19(18) . . ?
C6 C5 C4 119.79(17) . . ?
C4 C3 Cl1 119.60(17) . . ?
C2 C3 Cl1 119.58(16) . . ?
C2 C3 C4 120.82(17) . . ?
F1 C3 Cl1 6.5(11) . . ?
F1 C3 C4 119.1(11) . . ?
F1 C3 C2 119.7(11) . . ?
O1 C1 C2 115.64(16) . . ?
O1 C1 C6 124.82(18) . . ?
C6 C1 C2 119.54(17) . . ?
C5 C6 Cl2 119.90(15) . . ?
C5 C6 C1 120.61(17) . . ?
C1 C6 Cl2 119.48(16) . . ?
F2 C6 Cl2 7.7(8) . . ?
F2 C6 C5 117.9(8) . . ?
F2 C6 C1 120.8(8) . . ?
O6 C9 C7 115.23(17) . 3_566 ?
O6 C9 C8 125.02(18) . . ?
C8 C9 C7 119.75(17) . 3_566 ?
O5 C7 C9 115.46(17) . 3_566 ?
O5 C7 C8 125.54(18) . . ?
C8 C7 C9 119.00(17) . 3_566 ?
N00B C19 H19A 108.3 . . ?
N00B C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N00B 115.87(18) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
N00B C13 H13A 108.2 . . ?
N00B C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 N00B 116.4(2) . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
C9 C8 Cl3 119.09(16) . . ?
C7 C8 Cl3 119.71(16) . . ?
C7 C8 C9 121.19(17) . . ?
F3 C8 Cl3 12.3(6) . . ?
F3 C8 C9 121.7(7) . . ?
F3 C8 C7 115.8(7) . . ?
N00B C16 H16A 108.0 . . ?
N00B C16 H16B 108.0 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N00B 117.10(19) . . ?
C17 C16 H16A 108.0 . . ?
C17 C16 H16B 108.0 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.97(19) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
N00B C10 H10A 108.3 . . ?
N00B C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N00B 115.7(2) . . ?
C11 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C16 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
C16 C17 C18 108.0(2) . . ?
H17A C17 H17B 108.4 . . ?
C18 C17 H17A 110.1 . . ?
C18 C17 H17B 110.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
C10 C11 C12 109.4(2) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C13 C14 C15 109.3(3) . . ?
H14A C14 H14B 108.3 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Cl2 F2 C6 150(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
Fe01 O4 C5 C4 -1.7(2) 4_666 . . . ?
Fe01 O4 C5 C6 178.53(16) 4_666 . . . ?
Fe01 O2 C2 C3 -170.64(16) . . . . ?
Fe01 O2 C2 C1 9.3(2) . . . . ?
Fe01 O3 C4 C5 7.5(2) 4_666 . . . ?
Fe01 O3 C4 C3 -173.28(16) 4_666 . . . ?
Fe01 O1 C1 C2 -9.4(2) . . . . ?
Fe01 O1 C1 C6 171.34(16) . . . . ?
Fe01 O5 C7 C9 -6.3(2) . . . 3_566 ?
Fe01 O5 C7 C8 174.11(16) . . . . ?
Fe01 O6 C9 C7 -2.2(2) 3_566 . . 3_566 ?
Fe01 O6 C9 C8 178.00(16) 3_566 . . . ?
O4 C5 C6 Cl2 1.7(3) . . . . ?
O4 C5 C6 C1 -177.24(18) . . . . ?
O4 C5 C6 F2 -6.8(10) . . . . ?
O2 C2 C3 Cl1 -0.5(3) . . . . ?
O2 C2 C3 C4 -179.92(18) . . . . ?
O2 C2 C3 F1 7.0(12) . . . . ?
O2 C2 C1 O1 0.1(2) . . . . ?
O2 C2 C1 C6 179.43(17) . . . . ?
O3 C4 C5 O4 -3.9(3) . . . . ?
O3 C4 C5 C6 175.88(17) . . . . ?
O3 C4 C3 Cl1 3.2(3) . . . . ?
O3 C4 C3 C2 -177.39(18) . . . . ?
O3 C4 C3 F1 -4.3(12) . . . . ?
O1 C1 C6 Cl2 -0.7(3) . . . . ?
O1 C1 C6 C5 178.27(18) . . . . ?
O1 C1 C6 F2 8.1(10) . . . . ?
O5 C7 C8 Cl3 -3.4(3) . . . . ?
O5 C7 C8 C9 176.96(19) . . . . ?
O5 C7 C8 F3 9.7(8) . . . . ?
O6 C9 C8 Cl3 2.8(3) . . . . ?
O6 C9 C8 C7 -177.60(19) . . . . ?
O6 C9 C8 F3 -11.1(8) . . . . ?
N00B C19 C20 C21 -172.6(2) . . . . ?
N00B C13 C14 C15 177.3(2) . . . . ?
N00B C16 C17 C18 176.3(2) . . . . ?
N00B C10 C11 C12 178.8(3) . . . . ?
C4 C5 C6 Cl2 -178.06(15) . . . . ?
C4 C5 C6 C1 3.0(3) . . . . ?
C4 C5 C6 F2 173.4(9) . . . . ?
C2 C1 C6 Cl2 -179.97(15) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
C2 C1 C6 F2 -171.2(9) . . . . ?
C5 C4 C3 Cl1 -177.61(16) . . . . ?
C5 C4 C3 C2 1.8(3) . . . . ?
C5 C4 C3 F1 175.0(12) . . . . ?
C5 C6 F2 Cl2 107(6) . . . . ?
C3 C4 C5 O4 176.76(17) . . . . ?
C3 C4 C5 C6 -3.4(3) . . . . ?
C3 C2 C1 O1 -179.95(17) . . . . ?
C3 C2 C1 C6 -0.6(3) . . . . ?
C1 C2 C3 Cl1 179.57(16) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C1 C2 C3 F1 -173.0(12) . . . . ?
C1 C6 F2 Cl2 -82(6) . . . . ?
C9 C7 C8 Cl3 176.98(15) 3_566 . . . ?
C9 C7 C8 C9 -2.6(3) 3_566 . . . ?
C9 C7 C8 F3 -169.9(7) 3_566 . . . ?
C7 C9 C8 Cl3 -176.96(15) 3_566 . . . ?
C7 C9 C8 C7 2.6(3) 3_566 . . . ?
C7 C9 C8 F3 169.1(7) 3_566 . . . ?
C19 N00B C13 C14 66.4(3) . . . . ?
C19 N00B C16 C17 49.5(3) . . . . ?
C19 N00B C10 C11 -174.0(2) . . . . ?
C13 N00B C19 C20 176.5(2) . . . . ?
C13 N00B C16 C17 -70.0(3) . . . . ?
C13 N00B C10 C11 -54.1(3) . . . . ?
C16 N00B C19 C20 57.0(3) . . . . ?
C16 N00B C13 C14 -172.4(2) . . . . ?
C16 N00B C10 C11 65.2(3) . . . . ?
C10 N00B C19 C20 -61.6(3) . . . . ?
C10 N00B C13 C14 -53.6(3) . . . . ?
C10 N00B C16 C17 168.6(2) . . . . ?
F2 Cl2 C6 C5 -77(6) . . . . ?
F2 Cl2 C6 C1 102(6) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.632
_oxdiff_exptl_absorpt_empirical_full_min 0.677
####################################################################### 
# 
# 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_F-012-d_CCDC-2014818_R1
_database_code_depnum_ccdc_archive 'CCDC 2014818'
loop_
_audit_author_name
_audit_author_address
'Hitoshi Miyasaka'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-07-29
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl5.31 F0.69 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl5.31 F0.69 Fe2 N2 O12'
_chemical_formula_weight         1093.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H56 Cl5.31 F0.69 Fe2 N2 O12'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.6805(6)
_cell_length_b                   20.8987(11)
_cell_length_c                   12.2445(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.108(5)
_cell_angle_gamma                90
_cell_volume                     2681.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11290
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.0980
_cell_measurement_theta_min      2.5110
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.748
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1133
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20637
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.516
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0642547000
_diffrn_orient_matrix_UB_12      -0.0025760000
_diffrn_orient_matrix_UB_13      -0.0068597000
_diffrn_orient_matrix_UB_21      -0.0211622000
_diffrn_orient_matrix_UB_22      -0.0043002000
_diffrn_orient_matrix_UB_23      -0.0580938000
_diffrn_orient_matrix_UB_31      0.0022376000
_diffrn_orient_matrix_UB_32      0.0335662000
_diffrn_orient_matrix_UB_33      -0.0079312000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5270
_reflns_number_total             6140
_reflns_odcompleteness_completeness 91.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.88
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.106
_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)+(0.0357P)²+6.4450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1246
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-F3
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F2) = Uanis(Cl2)
Uanis(F1) = Uanis(Cl1)
Uanis(F3) = Uanis(Cl3)
4. Others
 Fixed Sof: Cl1(0.8875) Cl2(0.8875) Cl3(0.88) F2(0.1125) F1(0.1125) F3(0.12)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C14(H14A,H14B), C13(H13A,H13B), C20(H20A,H20B), C16(H16A,
 H16B), C10(H10A,H10B), C11(H11A,H11B), C17(H17A,H17B)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C18(H18A,H18B,
 H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.04348(4) 0.68773(2) 0.48013(3) 0.02407(11) Uani 1 1 d . . . . .
Cl1 Cl 0.93394(10) 0.67300(5) 0.06431(8) 0.0299(2) Uani 0.8875 1 d . . P A 2
Cl2 Cl 0.66255(12) 0.82994(7) 0.39558(9) 0.0329(2) Uani 0.8875 1 d . . P B 2
Cl3 Cl 1.29931(8) 0.48081(5) 0.51440(9) 0.0343(2) Uani 0.88 1 d . . P C 2
O3 O 0.69654(19) 0.75609(10) 0.00934(15) 0.0255(4) Uani 1 1 d . . . . .
O4 O 0.57874(18) 0.81393(10) 0.14641(16) 0.0259(4) Uani 1 1 d . . . . .
O6 O 1.14554(19) 0.60297(10) 0.48123(17) 0.0283(4) Uani 1 1 d . . . . .
O5 O 1.09788(19) 0.38156(10) 0.51950(17) 0.0276(4) Uani 1 1 d . . . . .
O2 O 1.01470(19) 0.68686(10) 0.31400(16) 0.0257(4) Uani 1 1 d . . . . .
O1 O 0.90366(19) 0.75151(10) 0.44972(15) 0.0256(4) Uani 1 1 d . . . . .
N1 N 0.3931(2) 0.64023(13) 0.2506(2) 0.0317(6) Uani 1 1 d . . . . .
C5 C 0.6841(3) 0.78615(13) 0.1910(2) 0.0225(5) Uani 1 1 d . . . . .
C4 C 0.7496(3) 0.75114(13) 0.1135(2) 0.0231(5) Uani 1 1 d . . . . .
C1 C 0.8482(3) 0.75330(13) 0.3458(2) 0.0223(5) Uani 1 1 d . . . . .
C6 C 0.7369(3) 0.78689(14) 0.3047(2) 0.0240(5) Uani 1 1 d . . . . .
C7 C 1.0593(3) 0.43831(14) 0.5111(2) 0.0255(6) Uani 1 1 d . . . . .
C2 C 0.9120(3) 0.71640(13) 0.2687(2) 0.0230(5) Uani 1 1 d . . . . .
C3 C 0.8590(3) 0.71629(14) 0.1549(2) 0.0244(6) Uani 1 1 d . . . . .
C9 C 1.0844(3) 0.55255(14) 0.4921(2) 0.0255(6) Uani 1 1 d . . . . .
C8 C 1.1361(3) 0.49156(14) 0.5055(2) 0.0269(6) Uani 1 1 d D . . . .
C19 C 0.3927(3) 0.71151(16) 0.2240(3) 0.0335(7) Uani 1 1 d . . . . .
H19A H 0.4756 0.7298 0.2610 0.040 Uiso 1 1 calc R U . . .
H19B H 0.3867 0.7165 0.1427 0.040 Uiso 1 1 calc R U . . .
C14 C 0.5014(3) 0.66466(18) 0.4545(3) 0.0411(8) Uani 1 1 d . . . . .
H14A H 0.4862 0.7113 0.4473 0.049 Uiso 1 1 calc R U . . .
H14B H 0.5867 0.6554 0.4382 0.049 Uiso 1 1 calc R U . . .
C13 C 0.3995(3) 0.62879(17) 0.3739(3) 0.0352(7) Uani 1 1 d . . . . .
H13A H 0.4126 0.5824 0.3882 0.042 Uiso 1 1 calc R U . . .
H13B H 0.3155 0.6400 0.3913 0.042 Uiso 1 1 calc R U . . .
C20 C 0.2867(3) 0.75048(17) 0.2583(3) 0.0360(7) Uani 1 1 d . . . . .
H20A H 0.2854 0.7428 0.3378 0.043 Uiso 1 1 calc R U . . .
H20B H 0.2032 0.7372 0.2139 0.043 Uiso 1 1 calc R U . . .
C15 C 0.4948(4) 0.6426(2) 0.5729(3) 0.0485(9) Uani 1 1 d . . . . .
H15A H 0.4060 0.6440 0.5831 0.073 Uiso 1 1 calc R U . . .
H15B H 0.5469 0.6710 0.6270 0.073 Uiso 1 1 calc R U . . .
H15C H 0.5271 0.5987 0.5841 0.073 Uiso 1 1 calc R U . . .
C21 C 0.3084(3) 0.82151(17) 0.2394(3) 0.0426(8) Uani 1 1 d . . . . .
H21A H 0.3044 0.8293 0.1599 0.064 Uiso 1 1 calc R U . . .
H21B H 0.3925 0.8341 0.2812 0.064 Uiso 1 1 calc R U . . .
H21C H 0.2423 0.8467 0.2651 0.064 Uiso 1 1 calc R U . . .
C16 C 0.5099(3) 0.60995(17) 0.2177(3) 0.0408(8) Uani 1 1 d . . . . .
H16A H 0.5863 0.6332 0.2566 0.049 Uiso 1 1 calc R U . . .
H16B H 0.5167 0.5653 0.2454 0.049 Uiso 1 1 calc R U . . .
C10 C 0.2693(3) 0.61078(17) 0.1877(3) 0.0395(8) Uani 1 1 d . . . . .
H10A H 0.1972 0.6299 0.2163 0.047 Uiso 1 1 calc R U . . .
H10B H 0.2591 0.6227 0.1082 0.047 Uiso 1 1 calc R U . . .
C11 C 0.2601(4) 0.53826(19) 0.1955(3) 0.0492(9) Uani 1 1 d . . . . .
H11A H 0.2660 0.5253 0.2741 0.059 Uiso 1 1 calc R U . . .
H11B H 0.3313 0.5180 0.1672 0.059 Uiso 1 1 calc R U . . .
C17 C 0.5132(5) 0.6087(2) 0.0946(4) 0.0570(11) Uani 1 1 d . . . . .
H17A H 0.5134 0.6531 0.0661 0.068 Uiso 1 1 calc R U . . .
H17B H 0.4362 0.5868 0.0535 0.068 Uiso 1 1 calc R U . . .
C12 C 0.1330(5) 0.5164(2) 0.1265(5) 0.0848(18) Uani 1 1 d . . . . .
H12A H 0.1264 0.5307 0.0494 0.127 Uiso 1 1 calc R U . . .
H12B H 0.0629 0.5348 0.1574 0.127 Uiso 1 1 calc R U . . .
H12C H 0.1280 0.4696 0.1284 0.127 Uiso 1 1 calc R U . . .
C18 C 0.6322(5) 0.5739(2) 0.0758(5) 0.0728(15) Uani 1 1 d . . . . .
H18A H 0.6391 0.5775 -0.0026 0.109 Uiso 1 1 calc R U . . .
H18B H 0.6265 0.5286 0.0953 0.109 Uiso 1 1 calc R U . . .
H18C H 0.7077 0.5930 0.1227 0.109 Uiso 1 1 calc R U . . .
F2 F 0.676(3) 0.8204(15) 0.376(2) 0.0329(2) Uani 0.1125 1 d . . P B -2
F1 F 0.921(2) 0.6903(11) 0.076(2) 0.0299(2) Uani 0.1125 1 d . . P A -2
F3 F 1.2599(14) 0.4844(11) 0.4942(19) 0.0343(2) Uani 0.12 1 d D . P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 1.988(2) 4_676 ?
Fe1 O4 1.9983(19) 4_676 ?
Fe1 O6 2.078(2) . ?
Fe1 O5 2.093(2) 3_766 ?
Fe1 O2 1.998(2) . ?
Fe1 O1 1.983(2) . ?
Cl1 C3 1.741(3) . ?
Cl2 C6 1.737(3) . ?
Cl3 C8 1.740(3) . ?
O3 Fe1 1.988(2) 4_575 ?
O3 C4 1.296(3) . ?
O4 Fe1 1.9983(19) 4_575 ?
O4 C5 1.290(3) . ?
O6 C9 1.260(4) . ?
O5 Fe1 2.093(2) 3_766 ?
O5 C7 1.253(4) . ?
O2 C2 1.288(3) . ?
O1 C1 1.296(3) . ?
N1 C19 1.525(4) . ?
N1 C13 1.516(4) . ?
N1 C16 1.521(4) . ?
N1 C10 1.525(4) . ?
C5 C4 1.477(4) . ?
C5 C6 1.398(4) . ?
C4 C3 1.387(4) . ?
C1 C6 1.388(4) . ?
C1 C2 1.483(4) . ?
C6 F2 1.38(2) . ?
C7 C9 1.540(4) 3_766 ?
C7 C8 1.392(4) . ?
C2 C3 1.399(4) . ?
C3 F1 1.38(2) . ?
C9 C7 1.540(4) 3_766 ?
C9 C8 1.386(4) . ?
C8 F3 1.364(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.519(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.519(5) . ?
C14 C15 1.535(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.527(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.515(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.523(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.524(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.521(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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
O3 Fe1 O4 80.79(8) 4_676 4_676 ?
O3 Fe1 O6 95.17(8) 4_676 . ?
O3 Fe1 O5 167.62(8) 4_676 3_766 ?
O3 Fe1 O2 98.53(8) 4_676 . ?
O4 Fe1 O6 89.02(8) 4_676 . ?
O4 Fe1 O5 88.87(8) 4_676 3_766 ?
O6 Fe1 O5 77.76(8) . 3_766 ?
O2 Fe1 O4 177.51(9) . 4_676 ?
O2 Fe1 O6 88.65(8) . . ?
O2 Fe1 O5 91.51(8) . 3_766 ?
O1 Fe1 O3 101.55(9) . 4_676 ?
O1 Fe1 O4 100.97(8) . 4_676 ?
O1 Fe1 O6 161.66(8) . . ?
O1 Fe1 O5 87.02(8) . 3_766 ?
O1 Fe1 O2 81.51(8) . . ?
C4 O3 Fe1 114.37(17) . 4_575 ?
C5 O4 Fe1 113.67(17) . 4_575 ?
C9 O6 Fe1 115.56(18) . . ?
C7 O5 Fe1 115.41(18) . 3_766 ?
C2 O2 Fe1 112.68(17) . . ?
C1 O1 Fe1 112.90(17) . . ?
C19 N1 C10 108.7(2) . . ?
C13 N1 C19 111.4(2) . . ?
C13 N1 C16 108.4(2) . . ?
C13 N1 C10 107.9(2) . . ?
C16 N1 C19 108.5(2) . . ?
C16 N1 C10 111.9(3) . . ?
O4 C5 C4 115.7(2) . . ?
O4 C5 C6 124.6(3) . . ?
C6 C5 C4 119.7(2) . . ?
O3 C4 C5 114.9(2) . . ?
O3 C4 C3 125.4(3) . . ?
C3 C4 C5 119.7(2) . . ?
O1 C1 C6 124.6(3) . . ?
O1 C1 C2 115.5(2) . . ?
C6 C1 C2 119.9(2) . . ?
C5 C6 Cl2 119.8(2) . . ?
C1 C6 Cl2 119.7(2) . . ?
C1 C6 C5 120.6(3) . . ?
F2 C6 Cl2 1.0(14) . . ?
F2 C6 C5 119.3(13) . . ?
F2 C6 C1 120.1(13) . . ?
O5 C7 C9 115.5(3) . 3_766 ?
O5 C7 C8 125.0(3) . . ?
C8 C7 C9 119.6(3) . 3_766 ?
O2 C2 C1 115.6(2) . . ?
O2 C2 C3 125.2(3) . . ?
C3 C2 C1 119.2(2) . . ?
C4 C3 Cl1 119.9(2) . . ?
C4 C3 C2 120.9(3) . . ?
C2 C3 Cl1 119.2(2) . . ?
F1 C3 Cl1 8.2(11) . . ?
F1 C3 C4 115.8(10) . . ?
F1 C3 C2 122.6(11) . . ?
O6 C9 C7 115.3(3) . 3_766 ?
O6 C9 C8 125.4(3) . . ?
C8 C9 C7 119.3(3) . 3_766 ?
C7 C8 Cl3 119.1(2) . . ?
C9 C8 Cl3 119.8(2) . . ?
C9 C8 C7 121.0(3) . . ?
F3 C8 Cl3 9.3(10) . . ?
F3 C8 C7 120.7(10) . . ?
F3 C8 C9 117.4(10) . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N1 115.8(3) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
H14A C14 H14B 108.4 . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C13 C14 C15 108.0(3) . . ?
C15 C14 H14A 110.1 . . ?
C15 C14 H14B 110.1 . . ?
N1 C13 C14 117.3(3) . . ?
N1 C13 H13A 108.0 . . ?
N1 C13 H13B 108.0 . . ?
C14 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C19 C20 C21 109.6(3) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N1 C16 H16A 108.1 . . ?
N1 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 N1 116.6(3) . . ?
C17 C16 H16A 108.1 . . ?
C17 C16 H16B 108.1 . . ?
N1 C10 H10A 108.4 . . ?
N1 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C11 C10 N1 115.5(3) . . ?
C11 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
C10 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
C10 C11 C12 109.0(3) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
C16 C17 C18 109.8(4) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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 O3 C4 C5 2.1(3) 4_575 . . . ?
Fe1 O3 C4 C3 -178.2(2) 4_575 . . . ?
Fe1 O4 C5 C4 -7.9(3) 4_575 . . . ?
Fe1 O4 C5 C6 172.7(2) 4_575 . . . ?
Fe1 O6 C9 C7 6.8(3) . . . 3_766 ?
Fe1 O6 C9 C8 -173.5(2) . . . . ?
Fe1 O5 C7 C9 2.7(3) 3_766 . . 3_766 ?
Fe1 O5 C7 C8 -177.8(2) 3_766 . . . ?
Fe1 O2 C2 C1 9.4(3) . . . . ?
Fe1 O2 C2 C3 -171.1(2) . . . . ?
Fe1 O1 C1 C6 170.6(2) . . . . ?
Fe1 O1 C1 C2 -9.7(3) . . . . ?
O3 C4 C3 Cl1 -1.6(4) . . . . ?
O3 C4 C3 C2 177.1(3) . . . . ?
O3 C4 C3 F1 6.5(13) . . . . ?
O4 C5 C4 O3 4.0(4) . . . . ?
O4 C5 C4 C3 -175.7(3) . . . . ?
O4 C5 C6 Cl2 -2.5(4) . . . . ?
O4 C5 C6 C1 177.3(3) . . . . ?
O4 C5 C6 F2 -1.6(17) . . . . ?
O6 C9 C8 Cl3 2.8(4) . . . . ?
O6 C9 C8 C7 -176.7(3) . . . . ?
O6 C9 C8 F3 -7.5(12) . . . . ?
O5 C7 C8 Cl3 -1.9(4) . . . . ?
O5 C7 C8 C9 177.5(3) . . . . ?
O5 C7 C8 F3 8.7(12) . . . . ?
O2 C2 C3 Cl1 0.5(4) . . . . ?
O2 C2 C3 C4 -178.2(3) . . . . ?
O2 C2 C3 F1 -8.2(14) . . . . ?
O1 C1 C6 Cl2 -0.4(4) . . . . ?
O1 C1 C6 C5 179.8(3) . . . . ?
O1 C1 C6 F2 -1.4(17) . . . . ?
O1 C1 C2 O2 0.1(4) . . . . ?
O1 C1 C2 C3 -179.4(2) . . . . ?
N1 C19 C20 C21 173.1(3) . . . . ?
N1 C16 C17 C18 -177.0(3) . . . . ?
N1 C10 C11 C12 -178.7(4) . . . . ?
C5 C4 C3 Cl1 178.1(2) . . . . ?
C5 C4 C3 C2 -3.3(4) . . . . ?
C5 C4 C3 F1 -173.9(12) . . . . ?
C4 C5 C6 Cl2 178.1(2) . . . . ?
C4 C5 C6 C1 -2.1(4) . . . . ?
C4 C5 C6 F2 179.1(16) . . . . ?
C1 C2 C3 Cl1 180.0(2) . . . . ?
C1 C2 C3 C4 1.3(4) . . . . ?
C1 C2 C3 F1 171.3(13) . . . . ?
C6 C5 C4 O3 -176.6(3) . . . . ?
C6 C5 C4 C3 3.7(4) . . . . ?
C6 C1 C2 O2 179.9(3) . . . . ?
C6 C1 C2 C3 0.3(4) . . . . ?
C7 C9 C8 Cl3 -177.6(2) 3_766 . . . ?
C7 C9 C8 C7 2.9(5) 3_766 . . . ?
C7 C9 C8 F3 172.1(11) 3_766 . . . ?
C2 C1 C6 Cl2 179.9(2) . . . . ?
C2 C1 C6 C5 0.1(4) . . . . ?
C2 C1 C6 F2 178.9(16) . . . . ?
C9 C7 C8 Cl3 177.6(2) 3_766 . . . ?
C9 C7 C8 C9 -2.9(5) 3_766 . . . ?
C9 C7 C8 F3 -171.8(11) 3_766 . . . ?
C19 N1 C13 C14 -49.4(4) . . . . ?
C19 N1 C16 C17 -66.4(4) . . . . ?
C19 N1 C10 C11 173.9(3) . . . . ?
C13 N1 C19 C20 -57.0(4) . . . . ?
C13 N1 C16 C17 172.5(3) . . . . ?
C13 N1 C10 C11 -65.2(4) . . . . ?
C15 C14 C13 N1 -176.7(3) . . . . ?
C16 N1 C19 C20 -176.3(3) . . . . ?
C16 N1 C13 C14 70.0(4) . . . . ?
C16 N1 C10 C11 54.1(4) . . . . ?
C10 N1 C19 C20 61.8(3) . . . . ?
C10 N1 C13 C14 -168.6(3) . . . . ?
C10 N1 C16 C17 53.6(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.804
