# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1521260'
_audit_update_record             
;
2016-12-07 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C81 H108 Fe12 O38, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C81 H112 Cl2 Fe12 O48'
_chemical_formula_weight         2594.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5327(5)
_cell_length_b                   17.2702(9)
_cell_length_c                   17.4391(9)
_cell_angle_alpha                60.820(5)
_cell_angle_beta                 71.422(4)
_cell_angle_gamma                72.941(4)
_cell_volume                     2834.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6213
_cell_measurement_theta_min      3.5000
_cell_measurement_theta_max      28.8620

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.616
_shelx_estimated_absorpt_T_min   0.749
_shelx_estimated_absorpt_T_max   0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63944
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Oxford Diffraction SuperNova with Atlas detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            24309
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.954
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             11121
_reflns_number_gt                7495
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
 The structure exhibits substitutional disorder in the methoxo O11-C15
 and the hydroxo O11-H11 groups (50:50), bridging Fe3 and Fe4 atoms.
 Carefull refinement of the title compound reveals that the sites of the 
 O18W and O19W water molecules are partially occupied (50%).
;

_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990);
MERCURY (Bruno et al. 2002); DIAMOND (Brandenburg, 2014); 
X-SEED (Barbour, 2001)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1082P)²+8.3726P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11121
_refine_ls_number_parameters     674
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.2242
_refine_ls_wR_factor_gt          0.1903
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.68104(9) 0.63531(6) 0.56348(5) 0.0322(2) Uani 1 1 d . . . . .
Fe2 Fe 0.67224(8) 0.72588(6) 0.35426(5) 0.0303(2) Uani 1 1 d . . . . .
Fe3 Fe 0.44628(9) 0.57067(6) 0.70579(5) 0.0332(2) Uani 1 1 d . . . . .
Fe4 Fe 0.44333(8) 0.65690(5) 0.50485(5) 0.0275(2) Uani 1 1 d . . . . .
Fe5 Fe 0.41680(8) 0.76115(5) 0.30685(5) 0.0295(2) Uani 1 1 d . . . . .
Fe6 Fe 0.51198(8) 0.44851(5) 0.60760(5) 0.0265(2) Uani 1 1 d . . . . .
C1A C 0.3092(7) 0.5399(5) 0.8901(4) 0.0436(16) Uani 1 1 d . . . . .
C1B C 0.8803(6) 0.5731(5) 0.6612(4) 0.0377(14) Uani 1 1 d . . . . .
C1C C 0.8791(6) 0.7561(4) 0.1949(4) 0.0357(14) Uani 1 1 d . . . . .
C1D C 0.2790(6) 0.9210(4) 0.1776(4) 0.0352(14) Uani 1 1 d . . . . .
C2A C 0.4018(7) 0.4711(5) 0.9346(4) 0.0452(17) Uani 1 1 d . . . . .
C2B C 0.9019(7) 0.6593(5) 0.6363(4) 0.0428(16) Uani 1 1 d . . . . .
C2C C 0.9214(6) 0.8210(5) 0.2021(4) 0.0387(15) Uani 1 1 d . . . . .
C2D C 0.3497(6) 0.9107(4) 0.0999(4) 0.0386(15) Uani 1 1 d . . . . .
C3A C 0.3712(8) 0.4217(6) 1.0301(5) 0.064(2) Uani 1 1 d . . . . .
H3A H 0.4303 0.3769 1.0605 0.076 Uiso 1 1 calc R U . . .
C3B C 0.9830(7) 0.6679(5) 0.6777(4) 0.0469(17) Uani 1 1 d . . . . .
H3B H 0.9946 0.7248 0.6637 0.056 Uiso 1 1 calc R U . . .
C3C C 1.0251(7) 0.8600(6) 0.1360(5) 0.0549(19) Uani 1 1 d . . . . .
H3C H 1.0525 0.9035 0.1395 0.066 Uiso 1 1 calc R U . . .
C3D C 0.3170(8) 0.9755(5) 0.0162(5) 0.055(2) Uani 1 1 d . . . . .
H3D H 0.3601 0.9682 -0.0355 0.065 Uiso 1 1 calc R U . . .
C4A C 0.2534(9) 0.4406(8) 1.0772(5) 0.084(3) Uani 1 1 d . . . . .
H4A H 0.2337 0.4073 1.1392 0.101 Uiso 1 1 calc R U . . .
C4B C 1.0441(7) 0.5934(5) 0.7377(5) 0.0488(18) Uani 1 1 d . . . . .
H4B H 1.0990 0.5993 0.7629 0.059 Uiso 1 1 calc R U . . .
C4C C 1.0846(7) 0.8354(6) 0.0682(5) 0.059(2) Uani 1 1 d . . . . .
H4C H 1.1531 0.8606 0.0269 0.070 Uiso 1 1 calc R U . . .
C4D C 0.2264(9) 1.0463(5) 0.0095(5) 0.063(2) Uani 1 1 d . . . . .
H4D H 0.2055 1.0858 -0.0458 0.075 Uiso 1 1 calc R U . . .
C5A C 0.1634(9) 0.5089(8) 1.0333(5) 0.085(3) Uani 1 1 d . . . . .
H5A H 0.0844 0.5204 1.0658 0.102 Uiso 1 1 calc R U . . .
C5B C 1.0232(7) 0.5089(5) 0.7606(5) 0.0485(17) Uani 1 1 d . . . . .
H5B H 1.0643 0.4585 0.8019 0.058 Uiso 1 1 calc R U . . .
C5C C 1.0419(7) 0.7724(5) 0.0613(5) 0.0490(17) Uani 1 1 d . . . . .
H5C H 1.0816 0.7560 0.0146 0.059 Uiso 1 1 calc R U . . .
C5D C 0.1627(8) 1.0611(5) 0.0857(5) 0.057(2) Uani 1 1 d . . . . .
H5D H 0.1035 1.1124 0.0802 0.068 Uiso 1 1 calc R U . . .
C6A C 0.1926(8) 0.5585(6) 0.9422(5) 0.063(2) Uani 1 1 d . . . . .
H6A H 0.1339 0.6058 0.9139 0.075 Uiso 1 1 calc R U . . .
C6B C 0.9444(6) 0.4973(5) 0.7245(4) 0.0406(15) Uani 1 1 d . . . . .
H6B H 0.9325 0.4397 0.7413 0.049 Uiso 1 1 calc R U . . .
C6C C 0.9426(6) 0.7342(5) 0.1220(4) 0.0423(15) Uani 1 1 d . . . . .
H6C H 0.9156 0.6924 0.1154 0.051 Uiso 1 1 calc R U . . .
C6D C 0.1882(6) 0.9993(4) 0.1685(5) 0.0426(16) Uani 1 1 d . . . . .
H6D H 0.1455 1.0090 0.2191 0.051 Uiso 1 1 calc R U . . .
C7A C 0.5234(7) 0.4477(4) 0.8861(4) 0.0402(15) Uani 1 1 d . . . . .
C7B C 0.8411(8) 0.7396(5) 0.5721(5) 0.0529(19) Uani 1 1 d . . . . .
C7C C 0.8580(7) 0.8531(5) 0.2714(4) 0.0448(16) Uani 1 1 d . . . . .
C7D C 0.4524(7) 0.8376(4) 0.1034(4) 0.0389(15) Uani 1 1 d . . . . .
C8A C 0.6231(8) 0.3831(6) 0.9341(5) 0.061(2) Uani 1 1 d . . . . .
H8A1 H 0.5988 0.3248 0.9697 0.091 Uiso 1 1 calc R U . . .
H8A2 H 0.6363 0.4035 0.9725 0.091 Uiso 1 1 calc R U . . .
H8A3 H 0.6985 0.3793 0.8911 0.091 Uiso 1 1 calc R U . . .
C8B C 0.8702(11) 0.8306(6) 0.5432(7) 0.085(3) Uani 1 1 d . . . . .
H8B1 H 0.8213 0.8759 0.5007 0.128 Uiso 1 1 calc R U . . .
H8B2 H 0.9567 0.8315 0.5158 0.128 Uiso 1 1 calc R U . . .
H8B3 H 0.8512 0.8424 0.5947 0.128 Uiso 1 1 calc R U . . .
C8C C 0.9049(9) 0.9217(7) 0.2778(6) 0.076(3) Uani 1 1 d . . . . .
H8C1 H 0.8557 0.9312 0.3294 0.115 Uiso 1 1 calc R U . . .
H8C2 H 0.8990 0.9773 0.2245 0.115 Uiso 1 1 calc R U . . .
H8C3 H 0.9898 0.9005 0.2836 0.115 Uiso 1 1 calc R U . . .
C8D C 0.5300(8) 0.8304(5) 0.0195(4) 0.0528(19) Uani 1 1 d . . . . .
H8D1 H 0.5859 0.7740 0.0349 0.079 Uiso 1 1 calc R U . . .
H8D2 H 0.5767 0.8789 -0.0152 0.079 Uiso 1 1 calc R U . . .
H8D3 H 0.4772 0.8335 -0.0152 0.079 Uiso 1 1 calc R U . . .
C9 C 0.5726(8) 0.6872(5) 0.7231(5) 0.0512(19) Uani 1 1 d . . . . .
H9A H 0.4998 0.6818 0.7704 0.077 Uiso 1 1 calc R U . . .
H9B H 0.5820 0.7493 0.6887 0.077 Uiso 1 1 calc R U . . .
H9C H 0.6442 0.6530 0.7487 0.077 Uiso 1 1 calc R U . . .
C10 C 0.9065(6) 0.6184(5) 0.4234(5) 0.0465(17) Uani 1 1 d . . . . .
H10A H 0.9322 0.5957 0.3790 0.070 Uiso 1 1 calc R U . . .
H10B H 0.9362 0.5740 0.4766 0.070 Uiso 1 1 calc R U . . .
H10C H 0.9402 0.6722 0.4002 0.070 Uiso 1 1 calc R U . . .
C11 C 0.5233(7) 0.8223(5) 0.4758(5) 0.0507(18) Uani 1 1 d . . . . .
H11A H 0.4617 0.8558 0.4398 0.076 Uiso 1 1 calc R U . . .
H11B H 0.5916 0.8543 0.4518 0.076 Uiso 1 1 calc R U . . .
H11C H 0.4874 0.8146 0.5364 0.076 Uiso 1 1 calc R U . . .
C12 C 0.5633(8) 0.9125(4) 0.2265(5) 0.055(2) Uani 1 1 d . . . . .
H12A H 0.6310 0.9101 0.1780 0.083 Uiso 1 1 calc R U . . .
H12B H 0.5816 0.9427 0.2541 0.083 Uiso 1 1 calc R U . . .
H12C H 0.4891 0.9446 0.2038 0.083 Uiso 1 1 calc R U . . .
C13 C 0.2013(11) 0.7777(9) 0.4535(7) 0.110(4) Uani 1 1 d . . . . .
H13A H 0.1579 0.7627 0.4250 0.164 Uiso 1 1 calc R U . . .
H13B H 0.1847 0.8415 0.4340 0.164 Uiso 1 1 calc R U . . .
H13C H 0.1736 0.7480 0.5175 0.164 Uiso 1 1 calc R U . . .
C14 C 0.2583(6) 0.5441(4) 0.5478(4) 0.0401(15) Uani 1 1 d . . . . .
H14A H 0.2231 0.5649 0.5937 0.060 Uiso 1 1 calc R U . . .
H14B H 0.2442 0.4837 0.5711 0.060 Uiso 1 1 calc R U . . .
H14C H 0.2199 0.5826 0.4972 0.060 Uiso 1 1 calc R U . . .
C16 C 0.3338(6) 0.4048(5) 0.7917(4) 0.0427(16) Uani 1 1 d . . . . .
H16A H 0.3021 0.3686 0.7778 0.064 Uiso 1 1 calc R U . . .
H16B H 0.2661 0.4374 0.8191 0.064 Uiso 1 1 calc R U . . .
H16C H 0.3886 0.3668 0.8323 0.064 Uiso 1 1 calc R U . . .
C17 C 0.7325(6) 0.3484(4) 0.7049(5) 0.0416(16) Uani 1 1 d . . . . .
H17A H 0.7429 0.4089 0.6850 0.062 Uiso 1 1 calc R U . . .
H17B H 0.8085 0.3160 0.6840 0.062 Uiso 1 1 calc R U . . .
H17C H 0.7114 0.3194 0.7693 0.062 Uiso 1 1 calc R U . . .
O1A O 0.3267(4) 0.5885(3) 0.8029(3) 0.0411(11) Uani 1 1 d . . . . .
O1B O 0.8079(4) 0.5565(3) 0.6272(3) 0.0409(11) Uani 1 1 d . . . . .
O1C O 0.7870(4) 0.7148(3) 0.2519(3) 0.0371(10) Uani 1 1 d . . . . .
O1D O 0.2923(4) 0.8630(3) 0.2594(3) 0.0393(10) Uani 1 1 d . . . . .
O2A O 0.5510(4) 0.4807(3) 0.8021(3) 0.0387(10) Uani 1 1 d . . . . .
O2B O 0.7621(5) 0.7392(3) 0.5381(3) 0.0461(12) Uani 1 1 d . . . . .
O2C O 0.7660(4) 0.8241(3) 0.3285(3) 0.0370(10) Uani 1 1 d . . . . .
O2D O 0.4847(4) 0.7794(3) 0.1748(3) 0.0387(10) Uani 1 1 d . . . . .
O3 O 0.5620(4) 0.5592(2) 0.5872(2) 0.0279(8) Uani 1 1 d . . . . .
O4 O 0.5449(4) 0.6545(2) 0.3834(2) 0.0267(8) Uani 1 1 d . . . . .
O5 O 0.5603(4) 0.6542(3) 0.6665(3) 0.0385(10) Uani 1 1 d . . . . .
O6 O 0.7735(4) 0.6384(3) 0.4448(3) 0.0333(9) Uani 1 1 d . . . . .
O7 O 0.5670(4) 0.7350(2) 0.4751(2) 0.0302(9) Uani 1 1 d . . . . .
O8 O 0.5458(4) 0.8242(3) 0.2909(3) 0.0344(10) Uani 1 1 d . . . . .
O9 O 0.3303(4) 0.7492(3) 0.4300(2) 0.0304(9) Uani 1 1 d . . . . .
O10 O 0.3924(4) 0.5455(3) 0.5196(2) 0.0282(8) Uani 1 1 d . . . . .
O12 O 0.3997(4) 0.4664(3) 0.7114(2) 0.0320(9) Uani 1 1 d . . . . .
O13 O 0.6359(4) 0.3497(3) 0.6697(3) 0.0320(9) Uani 1 1 d . . . . .
C15 C 0.2737(13) 0.7412(8) 0.6309(8) 0.033(3) Uani 0.5 1 d . . P . .
H15A H 0.2051 0.7244 0.6810 0.050 Uiso 0.5 1 calc R U P . .
H15B H 0.2432 0.7856 0.5780 0.050 Uiso 0.5 1 calc R U P . .
H15C H 0.3272 0.7655 0.6429 0.050 Uiso 0.5 1 calc R U P . .
O11 O 0.3438(4) 0.6611(3) 0.6166(3) 0.0334(9) Uani 1 1 d D . . . .
H11 H 0.299(14) 0.704(7) 0.629(11) 0.050 Uiso 0.5 1 d D U P . .
Cl Cl 0.3468(4) 0.8483(2) 0.82796(19) 0.1124(12) Uani 1 1 d . . . . .
O14 O 0.4681(11) 0.7974(7) 0.8567(6) 0.149(4) Uani 1 1 d . . . . .
O15 O 0.3782(11) 0.8974(6) 0.7339(5) 0.150(4) Uani 1 1 d . . . . .
O16 O 0.2959(11) 0.9091(7) 0.8683(6) 0.145(4) Uani 1 1 d . . . . .
O17 O 0.2712(13) 0.7897(9) 0.8509(9) 0.192(6) Uani 1 1 d . . . . .
O18W O -0.025(2) 1.0559(13) 0.3758(14) 0.150(7) Uani 0.5 1 d . U P . .
O19W O 0.684(2) 0.8648(16) 0.7542(16) 0.160(8) Uani 0.5 1 d . U P . .


_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 O1B 1.903(4) . ?
Fe1 O6 1.985(4) . ?
Fe1 O3 1.987(4) . ?
Fe1 O5 1.996(4) . ?
Fe1 O2B 2.058(4) . ?
Fe1 O7 2.108(4) . ?
Fe2 O1C 1.912(4) . ?
Fe2 O4 1.977(4) . ?
Fe2 O6 1.989(4) . ?
Fe2 O8 1.994(4) . ?
Fe2 O2C 2.066(4) . ?
Fe2 O7 2.127(4) . ?
Fe3 O1A 1.906(4) . ?
Fe3 O5 1.963(4) . ?
Fe3 O12 1.974(4) . ?
Fe3 O11 1.994(4) . ?
Fe3 O2A 2.083(4) . ?
Fe3 O3 2.141(4) . ?
Fe4 O9 1.944(4) . ?
Fe4 O11 1.945(4) . ?
Fe4 O7 2.024(4) . ?
Fe4 O10 2.048(4) . ?
Fe4 O3 2.078(4) . ?
Fe4 O4 2.083(4) . ?
Fe5 O1D 1.922(4) . ?
Fe5 O8 1.967(4) . ?
Fe5 O13 1.991(4) 2_666 ?
Fe5 O9 1.993(4) . ?
Fe5 O2D 2.075(4) . ?
Fe5 O4 2.149(4) . ?
Fe6 O12 1.967(4) . ?
Fe6 O13 1.969(4) . ?
Fe6 O3 1.992(4) . ?
Fe6 O4 1.992(4) 2_666 ?
Fe6 O10 2.106(4) 2_666 ?
Fe6 O10 2.133(4) . ?
C1A O1A 1.311(7) . ?
C1A C6A 1.411(10) . ?
C1A C2A 1.428(10) . ?
C1B O1B 1.323(7) . ?
C1B C2B 1.409(9) . ?
C1B C6B 1.422(9) . ?
C1C O1C 1.306(7) . ?
C1C C2C 1.416(9) . ?
C1C C6C 1.418(9) . ?
C1D O1D 1.311(7) . ?
C1D C2D 1.405(9) . ?
C1D C6D 1.421(9) . ?
C2A C3A 1.429(9) . ?
C2A C7A 1.446(10) . ?
C2B C3B 1.426(9) . ?
C2B C7B 1.443(10) . ?
C2C C3C 1.431(10) . ?
C2C C7C 1.469(9) . ?
C2D C3D 1.427(9) . ?
C2D C7D 1.448(10) . ?
C3A C4A 1.384(12) . ?
C3A H3A 0.9300 . ?
C3B C4B 1.369(10) . ?
C3B H3B 0.9300 . ?
C3C C4C 1.361(11) . ?
C3C H3C 0.9300 . ?
C3D C4D 1.338(11) . ?
C3D H3D 0.9300 . ?
C4A C5A 1.401(13) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.388(10) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.386(11) . ?
C4C H4C 0.9300 . ?
C4D C5D 1.403(11) . ?
C4D H4D 0.9300 . ?
C5A C6A 1.369(11) . ?
C5A H5A 0.9300 . ?
C5B C6B 1.362(9) . ?
C5B H5B 0.9300 . ?
C5C C6C 1.364(10) . ?
C5C H5C 0.9300 . ?
C5D C6D 1.377(9) . ?
C5D H5D 0.9300 . ?
C6A H6A 0.9300 . ?
C6B H6B 0.9300 . ?
C6C H6C 0.9300 . ?
C6D H6D 0.9300 . ?
C7A O2A 1.252(7) . ?
C7A C8A 1.489(10) . ?
C7B O2B 1.238(8) . ?
C7B C8B 1.505(10) . ?
C7C O2C 1.233(8) . ?
C7C C8C 1.499(10) . ?
C7D O2D 1.246(7) . ?
C7D C8D 1.495(9) . ?
C8A H8A1 0.9600 . ?
C8A H8A2 0.9600 . ?
C8A H8A3 0.9600 . ?
C8B H8B1 0.9600 . ?
C8B H8B2 0.9600 . ?
C8B H8B3 0.9600 . ?
C8C H8C1 0.9600 . ?
C8C H8C2 0.9600 . ?
C8C H8C3 0.9600 . ?
C8D H8D1 0.9600 . ?
C8D H8D2 0.9600 . ?
C8D H8D3 0.9600 . ?
C9 O5 1.417(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O6 1.436(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 O7 1.448(8) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O8 1.411(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O9 1.416(11) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 O10 1.470(8) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C16 O12 1.419(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O13 1.424(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O4 Fe6 1.992(4) 2_666 ?
O10 Fe6 2.105(4) 2_666 ?
O13 Fe5 1.991(4) 2_666 ?
C15 O11 1.476(12) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 H11 0.63(4) . ?
O11 H11 0.850(10) . ?
Cl O17 1.358(10) . ?
Cl O15 1.409(8) . ?
Cl O16 1.427(8) . ?
Cl O14 1.509(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Fe1 O6 96.09(19) . . ?
O1B Fe1 O3 106.22(17) . . ?
O6 Fe1 O3 96.41(16) . . ?
O1B Fe1 O5 96.93(19) . . ?
O6 Fe1 O5 166.86(17) . . ?
O3 Fe1 O5 81.62(16) . . ?
O1B Fe1 O2B 86.74(18) . . ?
O6 Fe1 O2B 90.07(18) . . ?
O3 Fe1 O2B 164.72(19) . . ?
O5 Fe1 O2B 88.92(18) . . ?
O1B Fe1 O7 169.53(18) . . ?
O6 Fe1 O7 76.71(16) . . ?
O3 Fe1 O7 82.39(15) . . ?
O5 Fe1 O7 90.14(17) . . ?
O2B Fe1 O7 85.68(16) . . ?
O1C Fe2 O4 104.31(17) . . ?
O1C Fe2 O6 97.08(18) . . ?
O4 Fe2 O6 100.19(16) . . ?
O1C Fe2 O8 98.30(18) . . ?
O4 Fe2 O8 80.54(16) . . ?
O6 Fe2 O8 163.91(17) . . ?
O1C Fe2 O2C 86.12(17) . . ?
O4 Fe2 O2C 165.31(18) . . ?
O6 Fe2 O2C 88.54(17) . . ?
O8 Fe2 O2C 87.82(17) . . ?
O1C Fe2 O7 171.95(17) . . ?
O4 Fe2 O7 81.52(15) . . ?
O6 Fe2 O7 76.22(16) . . ?
O8 Fe2 O7 88.06(16) . . ?
O2C Fe2 O7 89.22(16) . . ?
O1A Fe3 O5 103.84(19) . . ?
O1A Fe3 O12 101.83(18) . . ?
O5 Fe3 O12 153.28(19) . . ?
O1A Fe3 O11 92.42(18) . . ?
O5 Fe3 O11 92.08(18) . . ?
O12 Fe3 O11 94.12(17) . . ?
O1A Fe3 O2A 85.37(18) . . ?
O5 Fe3 O2A 86.53(18) . . ?
O12 Fe3 O2A 88.29(17) . . ?
O11 Fe3 O2A 177.02(16) . . ?
O1A Fe3 O3 172.64(17) . . ?
O5 Fe3 O3 78.63(16) . . ?
O12 Fe3 O3 76.82(15) . . ?
O11 Fe3 O3 80.51(16) . . ?
O2A Fe3 O3 101.76(16) . . ?
O9 Fe4 O11 95.48(17) . . ?
O9 Fe4 O7 97.59(16) . . ?
O11 Fe4 O7 99.27(17) . . ?
O9 Fe4 O10 98.87(16) . . ?
O11 Fe4 O10 98.76(17) . . ?
O7 Fe4 O10 154.21(17) . . ?
O9 Fe4 O3 178.67(15) . . ?
O11 Fe4 O3 83.24(16) . . ?
O7 Fe4 O3 82.27(15) . . ?
O10 Fe4 O3 81.71(15) . . ?
O9 Fe4 O4 82.77(15) . . ?
O11 Fe4 O4 178.17(17) . . ?
O7 Fe4 O4 81.51(15) . . ?
O10 Fe4 O4 81.03(15) . . ?
O3 Fe4 O4 98.51(15) . . ?
O1D Fe5 O8 99.52(18) . . ?
O1D Fe5 O13 108.97(18) . 2_666 ?
O8 Fe5 O13 150.50(18) . 2_666 ?
O1D Fe5 O9 88.94(17) . . ?
O8 Fe5 O9 96.47(17) . . ?
O13 Fe5 O9 91.66(17) 2_666 . ?
O1D Fe5 O2D 84.93(18) . . ?
O8 Fe5 O2D 88.44(17) . . ?
O13 Fe5 O2D 86.63(17) 2_666 . ?
O9 Fe5 O2D 172.72(17) . . ?
O1D Fe5 O4 167.85(17) . . ?
O8 Fe5 O4 77.02(15) . . ?
O13 Fe5 O4 76.57(15) 2_666 . ?
O9 Fe5 O4 79.98(15) . . ?
O2D Fe5 O4 106.45(16) . . ?
O12 Fe6 O13 98.99(17) . . ?
O12 Fe6 O3 80.58(16) . . ?
O13 Fe6 O3 104.28(16) . . ?
O12 Fe6 O4 101.65(16) . 2_666 ?
O13 Fe6 O4 80.80(16) . 2_666 ?
O3 Fe6 O4 174.15(14) . 2_666 ?
O12 Fe6 O10 167.59(16) . 2_666 ?
O13 Fe6 O10 93.33(16) . 2_666 ?
O3 Fe6 O10 94.94(15) . 2_666 ?
O4 Fe6 O10 81.77(15) 2_666 2_666 ?
O12 Fe6 O10 92.06(16) . . ?
O13 Fe6 O10 168.14(15) . . ?
O3 Fe6 O10 81.65(15) . . ?
O4 Fe6 O10 92.83(15) 2_666 . ?
O10 Fe6 O10 75.78(17) 2_666 . ?
O1A C1A C6A 117.5(6) . . ?
O1A C1A C2A 123.7(6) . . ?
C6A C1A C2A 118.8(6) . . ?
O1B C1B C2B 124.8(6) . . ?
O1B C1B C6B 116.8(6) . . ?
C2B C1B C6B 118.4(6) . . ?
O1C C1C C2C 124.1(6) . . ?
O1C C1C C6C 118.5(6) . . ?
C2C C1C C6C 117.4(6) . . ?
O1D C1D C2D 124.2(6) . . ?
O1D C1D C6D 116.7(6) . . ?
C2D C1D C6D 119.1(6) . . ?
C1A C2A C3A 118.6(7) . . ?
C1A C2A C7A 122.3(6) . . ?
C3A C2A C7A 119.1(7) . . ?
C1B C2B C3B 119.2(6) . . ?
C1B C2B C7B 121.8(6) . . ?
C3B C2B C7B 118.9(6) . . ?
C1C C2C C3C 118.4(6) . . ?
C1C C2C C7C 122.2(6) . . ?
C3C C2C C7C 119.3(6) . . ?
C1D C2D C3D 117.6(6) . . ?
C1D C2D C7D 122.0(5) . . ?
C3D C2D C7D 120.4(6) . . ?
C4A C3A C2A 119.9(8) . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C4B C3B C2B 120.8(7) . . ?
C4B C3B H3B 119.6 . . ?
C2B C3B H3B 119.6 . . ?
C4C C3C C2C 122.0(7) . . ?
C4C C3C H3C 119.0 . . ?
C2C C3C H3C 119.0 . . ?
C4D C3D C2D 122.3(7) . . ?
C4D C3D H3D 118.8 . . ?
C2D C3D H3D 118.8 . . ?
C3A C4A C5A 121.2(8) . . ?
C3A C4A H4A 119.4 . . ?
C5A C4A H4A 119.4 . . ?
C3B C4B C5B 119.3(6) . . ?
C3B C4B H4B 120.4 . . ?
C5B C4B H4B 120.4 . . ?
C3C C4C C5C 119.2(7) . . ?
C3C C4C H4C 120.4 . . ?
C5C C4C H4C 120.4 . . ?
C3D C4D C5D 120.2(7) . . ?
C3D C4D H4D 119.9 . . ?
C5D C4D H4D 119.9 . . ?
C6A C5A C4A 119.4(8) . . ?
C6A C5A H5A 120.3 . . ?
C4A C5A H5A 120.3 . . ?
C6B C5B C4B 122.1(7) . . ?
C6B C5B H5B 118.9 . . ?
C4B C5B H5B 118.9 . . ?
C6C C5C C4C 120.9(7) . . ?
C6C C5C H5C 119.5 . . ?
C4C C5C H5C 119.5 . . ?
C6D C5D C4D 119.7(7) . . ?
C6D C5D H5D 120.1 . . ?
C4D C5D H5D 120.1 . . ?
C5A C6A C1A 121.9(8) . . ?
C5A C6A H6A 119.1 . . ?
C1A C6A H6A 119.1 . . ?
C5B C6B C1B 120.2(7) . . ?
C5B C6B H6B 119.9 . . ?
C1B C6B H6B 119.9 . . ?
C5C C6C C1C 122.0(7) . . ?
C5C C6C H6C 119.0 . . ?
C1C C6C H6C 119.0 . . ?
C5D C6D C1D 120.6(7) . . ?
C5D C6D H6D 119.7 . . ?
C1D C6D H6D 119.7 . . ?
O2A C7A C2A 122.2(6) . . ?
O2A C7A C8A 116.5(6) . . ?
C2A C7A C8A 121.3(6) . . ?
O2B C7B C2B 123.4(6) . . ?
O2B C7B C8B 115.7(7) . . ?
C2B C7B C8B 120.9(6) . . ?
O2C C7C C2C 122.3(6) . . ?
O2C C7C C8C 116.5(6) . . ?
C2C C7C C8C 121.2(6) . . ?
O2D C7D C2D 122.8(6) . . ?
O2D C7D C8D 116.1(6) . . ?
C2D C7D C8D 121.1(6) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7C C8C H8C1 109.5 . . ?
C7C C8C H8C2 109.5 . . ?
H8C1 C8C H8C2 109.5 . . ?
C7C C8C H8C3 109.5 . . ?
H8C1 C8C H8C3 109.5 . . ?
H8C2 C8C H8C3 109.5 . . ?
C7D C8D H8D1 109.5 . . ?
C7D C8D H8D2 109.5 . . ?
H8D1 C8D H8D2 109.5 . . ?
C7D C8D H8D3 109.5 . . ?
H8D1 C8D H8D3 109.5 . . ?
H8D2 C8D H8D3 109.5 . . ?
O5 C9 H9A 109.5 . . ?
O5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O6 C10 H10A 109.5 . . ?
O6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C11 H11A 109.5 . . ?
O7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O8 C12 H12A 109.5 . . ?
O8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O9 C13 H13A 109.5 . . ?
O9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O10 C14 H14A 109.5 . . ?
O10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O12 C16 H16A 109.5 . . ?
O12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O13 C17 H17A 109.5 . . ?
O13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1A O1A Fe3 132.1(4) . . ?
C1B O1B Fe1 129.9(4) . . ?
C1C O1C Fe2 133.1(4) . . ?
C1D O1D Fe5 133.2(4) . . ?
C7A O2A Fe3 131.3(5) . . ?
C7B O2B Fe1 130.3(5) . . ?
C7C O2C Fe2 132.1(4) . . ?
C7D O2D Fe5 132.1(4) . . ?
Fe1 O3 Fe6 155.4(2) . . ?
Fe1 O3 Fe4 98.69(16) . . ?
Fe6 O3 Fe4 100.07(17) . . ?
Fe1 O3 Fe3 96.72(15) . . ?
Fe6 O3 Fe3 97.85(16) . . ?
Fe4 O3 Fe3 93.59(16) . . ?
Fe2 O4 Fe6 153.5(2) . 2_666 ?
Fe2 O4 Fe4 99.91(15) . . ?
Fe6 O4 Fe4 99.75(16) 2_666 . ?
Fe2 O4 Fe5 98.22(15) . . ?
Fe6 O4 Fe5 98.00(16) 2_666 . ?
Fe4 O4 Fe5 93.78(16) . . ?
C9 O5 Fe3 122.6(4) . . ?
C9 O5 Fe1 130.7(4) . . ?
Fe3 O5 Fe1 102.43(18) . . ?
C10 O6 Fe1 121.9(4) . . ?
C10 O6 Fe2 123.3(4) . . ?
Fe1 O6 Fe2 108.1(2) . . ?
C11 O7 Fe4 119.8(4) . . ?
C11 O7 Fe1 119.9(4) . . ?
Fe4 O7 Fe1 96.56(16) . . ?
C11 O7 Fe2 119.6(4) . . ?
Fe4 O7 Fe2 96.97(15) . . ?
Fe1 O7 Fe2 98.86(17) . . ?
C12 O8 Fe5 126.5(4) . . ?
C12 O8 Fe2 126.8(4) . . ?
Fe5 O8 Fe2 103.99(18) . . ?
C13 O9 Fe4 129.7(5) . . ?
C13 O9 Fe5 123.0(5) . . ?
Fe4 O9 Fe5 103.38(19) . . ?
C14 O10 Fe4 115.1(3) . . ?
C14 O10 Fe6 119.8(3) . 2_666 ?
Fe4 O10 Fe6 97.23(16) . 2_666 ?
C14 O10 Fe6 119.5(3) . . ?
Fe4 O10 Fe6 96.51(16) . . ?
Fe6 O10 Fe6 104.22(17) 2_666 . ?
C16 O12 Fe6 129.6(4) . . ?
C16 O12 Fe3 122.1(3) . . ?
Fe6 O12 Fe3 104.54(19) . . ?
C17 O13 Fe6 131.8(4) . . ?
C17 O13 Fe5 123.3(4) . 2_666 ?
Fe6 O13 Fe5 104.32(18) . 2_666 ?
O11 C15 H15A 109.5 . . ?
O11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
H15A C15 H11 102.3 . . ?
H15B C15 H11 113.3 . . ?
H15C C15 H11 112.5 . . ?
C15 O11 Fe4 127.8(5) . . ?
C15 O11 Fe3 116.8(5) . . ?
Fe4 O11 Fe3 102.6(2) . . ?
Fe4 O11 H11 133(10) . . ?
Fe3 O11 H11 115(10) . . ?
O17 Cl O15 110.7(8) . . ?
O17 Cl O16 113.6(8) . . ?
O15 Cl O16 109.5(6) . . ?
O17 Cl O14 110.0(8) . . ?
O15 Cl O14 105.5(7) . . ?
O16 Cl O14 107.2(7) . . ?

_refine_diff_density_max         1.360
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.138

# start Validation Reply Form

_vrf_PLAT420_2                   
;
RESPONSE:The O11-H11 hydroxo group is involved in substitutional disorder with 
O11-C15 methoxo group in a 50:50 domain ratio. No suitable acceptor has been 
located for this hydroxo group.
;
_vrf_PLAT430_2                   
;
RESPONSE: This short distance assumes a strong hydrogen bond between
the O14 atom of the perchlorate counterion and the O19W water molecule. 
No hydrogen atoms have been located for the latter O19W molecule.
;
_vrf_PLAT041_2                   
;
RESPONSE:The missing (not located by a difference synthesis) hydrogen atoms 
of the crystallization water molecules (O18W and O19W) have been included in 
the sum and moiety formula and the Mr, Dx and F(000) have been modified 
accordingly. These modifications account for the differences detected in the 
relevant data items.  
;
_vrf_CELLZ01_2                   
; 
RESPONSE:See comment above.
;

_vrf_PLAT311_2                   
; 
RESPONSE:See comment above.
;
# end Validation Reply Form


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
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# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1521256'
_audit_update_record             
;
2016-12-07 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H92 Fe10 O32, 2(N O3), 3(C H4 O)'
_chemical_formula_sum            'C67 H104 Fe10 N2 O41'
_chemical_formula_weight         2152.02

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0455(11)
_cell_length_b                   13.9295(11)
_cell_length_c                   16.0391(14)
_cell_angle_alpha                96.034(7)
_cell_angle_beta                 108.589(8)
_cell_angle_gamma                108.143(8)
_cell_volume                     2164.7(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3171
_cell_measurement_theta_min      3.3900
_cell_measurement_theta_max      27.6320

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             1108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.714
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Oxford Diffraction SuperNova with Atlas detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            13401
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.047
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7586
_reflns_number_gt                4905
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990);
MERCURY (Bruno et al. 2002); DIAMOND (Brandenburg, 2014); 
X-SEED (Barbour, 2001)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1269P)²+3.8940P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7586
_refine_ls_number_parameters     568
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.2355
_refine_ls_wR_factor_gt          0.1905
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.15546(10) 0.28942(7) 0.48087(6) 0.0262(3) Uani 1 1 d . . . . .
Fe2 Fe 0.20895(10) 0.44972(7) 0.65890(6) 0.0252(3) Uani 1 1 d . . . . .
Fe3 Fe -0.12163(10) 0.21906(7) 0.32170(7) 0.0277(3) Uani 1 1 d . . . . .
Fe4 Fe -0.06687(9) 0.38400(7) 0.48988(6) 0.0216(3) Uani 1 1 d . . . . .
Fe5 Fe -0.00971(10) 0.54053(7) 0.66286(6) 0.0252(3) Uani 1 1 d . . . . .
C1A C -0.3321(8) 0.0334(5) 0.1793(4) 0.0318(17) Uani 1 1 d . . . . .
C1B C 0.2929(8) 0.1943(6) 0.3917(5) 0.0380(18) Uani 1 1 d . . . . .
C1C C 0.4716(7) 0.5801(6) 0.8060(5) 0.0341(17) Uani 1 1 d . . . . .
C2A C -0.2510(8) 0.0298(5) 0.1270(5) 0.0329(17) Uani 1 1 d . . . . .
C2B C 0.3135(8) 0.1270(6) 0.4507(6) 0.0408(19) Uani 1 1 d . . . . .
C2C C 0.4944(7) 0.4975(6) 0.8473(5) 0.0324(16) Uani 1 1 d . . . . .
C3A C -0.3128(8) -0.0457(6) 0.0440(5) 0.0402(19) Uani 1 1 d . . . . .
H3A H -0.2621 -0.0488 0.0080 0.048 Uiso 1 1 calc R U . . .
C3B C 0.3348(8) 0.0358(6) 0.4201(6) 0.048(2) Uani 1 1 d . . . . .
H3B H 0.3495 -0.0082 0.4586 0.057 Uiso 1 1 calc R U . . .
C3C C 0.6126(8) 0.5211(6) 0.9250(5) 0.0394(18) Uani 1 1 d . . . . .
H3C H 0.6292 0.4679 0.9515 0.047 Uiso 1 1 calc R U . . .
C4A C -0.4461(9) -0.1144(6) 0.0160(5) 0.044(2) Uani 1 1 d . . . . .
H4A H -0.4852 -0.1632 -0.0385 0.052 Uiso 1 1 calc R U . . .
C4B C 0.3338(9) 0.0127(7) 0.3361(7) 0.059(3) Uani 1 1 d . . . . .
H4B H 0.3485 -0.0467 0.3174 0.071 Uiso 1 1 calc R U . . .
C4C C 0.7049(8) 0.6220(7) 0.9627(5) 0.044(2) Uani 1 1 d . . . . .
H4C H 0.7827 0.6359 1.0140 0.052 Uiso 1 1 calc R U . . .
C5A C -0.5221(8) -0.1101(5) 0.0703(5) 0.0402(19) Uani 1 1 d . . . . .
H5A H -0.6119 -0.1570 0.0515 0.048 Uiso 1 1 calc R U . . .
C5B C 0.3107(9) 0.0777(6) 0.2767(6) 0.052(2) Uani 1 1 d . . . . .
H5B H 0.3050 0.0591 0.2178 0.063 Uiso 1 1 calc R U . . .
C5C C 0.6818(8) 0.7026(6) 0.9240(5) 0.0401(19) Uani 1 1 d . . . . .
H5C H 0.7432 0.7704 0.9499 0.048 Uiso 1 1 calc R U . . .
C6A C -0.4671(8) -0.0381(5) 0.1509(5) 0.0353(17) Uani 1 1 d . . . . .
H6A H -0.5191 -0.0367 0.1863 0.042 Uiso 1 1 calc R U . . .
C6B C 0.2961(8) 0.1707(7) 0.3054(6) 0.048(2) Uani 1 1 d . . . . .
H6B H 0.2886 0.2165 0.2675 0.057 Uiso 1 1 calc R U . . .
C6C C 0.5687(7) 0.6817(6) 0.8480(5) 0.0361(18) Uani 1 1 d . . . . .
H6C H 0.5549 0.7364 0.8227 0.043 Uiso 1 1 calc R U . . .
C7A C -0.1095(9) 0.1004(6) 0.1542(5) 0.0386(18) Uani 1 1 d . . . . .
C7B C 0.3036(8) 0.1450(6) 0.5377(6) 0.046(2) Uani 1 1 d . . . . .
C7C C 0.3994(8) 0.3910(6) 0.8088(5) 0.0331(17) Uani 1 1 d . . . . .
C8A C -0.0298(9) 0.0969(6) 0.0946(5) 0.044(2) Uani 1 1 d . . . . .
H8A1 H -0.0768 0.1080 0.0370 0.065 Uiso 1 1 calc R U . . .
H8A2 H -0.0213 0.0303 0.0864 0.065 Uiso 1 1 calc R U . . .
H8A3 H 0.0600 0.1502 0.1222 0.065 Uiso 1 1 calc R U . . .
C8B C 0.3643(12) 0.0926(9) 0.6101(7) 0.078(3) Uani 1 1 d . . . . .
H8B1 H 0.4592 0.1075 0.6195 0.118 Uiso 1 1 calc R U . . .
H8B2 H 0.3151 0.0190 0.5911 0.118 Uiso 1 1 calc R U . . .
H8B3 H 0.3570 0.1184 0.6655 0.118 Uiso 1 1 calc R U . . .
C8C C 0.4306(9) 0.3053(6) 0.8501(6) 0.046(2) Uani 1 1 d . . . . .
H8C1 H 0.5163 0.3042 0.8485 0.069 Uiso 1 1 calc R U . . .
H8C2 H 0.3587 0.2400 0.8166 0.069 Uiso 1 1 calc R U . . .
H8C3 H 0.4367 0.3170 0.9116 0.069 Uiso 1 1 calc R U . . .
C9 C -0.0211(9) 0.0539(6) 0.3839(5) 0.0434(19) Uani 1 1 d . . . . .
H9A H 0.0233 0.0340 0.4375 0.065 Uiso 1 1 calc R U . . .
H9B H 0.0211 0.0462 0.3410 0.065 Uiso 1 1 calc R U . . .
H9C H -0.1166 0.0104 0.3581 0.065 Uiso 1 1 calc R U . . .
C10 C 0.4363(8) 0.4444(7) 0.5963(6) 0.054(2) Uani 1 1 d . . . . .
H10A H 0.4781 0.5187 0.6120 0.080 Uiso 1 1 calc R U . . .
H10B H 0.4540 0.4177 0.5456 0.080 Uiso 1 1 calc R U . . .
H10C H 0.4740 0.4171 0.6468 0.080 Uiso 1 1 calc R U . . .
C11 C 0.0867(9) 0.4269(6) 0.8085(6) 0.046(2) Uani 1 1 d . . . . .
H11A H 0.1772 0.4322 0.8451 0.070 Uiso 1 1 calc R U . . .
H11B H 0.0244 0.3565 0.7947 0.070 Uiso 1 1 calc R U . . .
H11C H 0.0573 0.4714 0.8407 0.070 Uiso 1 1 calc R U . . .
C12 C -0.0160(7) 0.2263(5) 0.6017(5) 0.0323(16) Uani 1 1 d . . . . .
H12A H 0.0506 0.2030 0.6397 0.048 Uiso 1 1 calc R U . . .
H12B H -0.0807 0.1704 0.5514 0.048 Uiso 1 1 calc R U . . .
H12C H -0.0635 0.2489 0.6358 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2199(8) 0.6897(6) 0.8361(5) 0.0395(18) Uani 1 1 d . . . . .
H13A H 0.2609 0.6380 0.8414 0.059 Uiso 1 1 calc R U . . .
H13B H 0.1691 0.6858 0.8751 0.059 Uiso 1 1 calc R U . . .
H13C H 0.2905 0.7572 0.8531 0.059 Uiso 1 1 calc R U . . .
C14 C -0.1804(9) 0.6033(6) 0.7651(6) 0.051(2) Uani 1 1 d . . . . .
H14A H -0.2178 0.5820 0.8095 0.076 Uiso 1 1 calc R U . . .
H14B H -0.2497 0.6116 0.7153 0.076 Uiso 1 1 calc R U . . .
H14C H -0.1042 0.6681 0.7917 0.076 Uiso 1 1 calc R U . . .
C15 C -0.3006(9) 0.4071(7) 0.5360(6) 0.056(2) Uani 1 1 d . . . . .
H15A H -0.3069 0.4698 0.5619 0.083 Uiso 1 1 calc R U . . .
H15B H -0.3549 0.3494 0.5525 0.083 Uiso 1 1 calc R U . . .
H15C H -0.3339 0.3967 0.4714 0.083 Uiso 1 1 calc R U . . .
C16 C -0.3408(9) 0.2037(7) 0.4032(8) 0.077(4) Uani 1 1 d . . . . .
H16A H -0.3760 0.1344 0.3673 0.116 Uiso 1 1 calc R U . . .
H16B H -0.3983 0.2402 0.3760 0.116 Uiso 1 1 calc R U . . .
H16C H -0.3400 0.2011 0.4629 0.116 Uiso 1 1 calc R U . . .
O1A O -0.2865(5) 0.1030(4) 0.2564(3) 0.0352(12) Uani 1 1 d . . . . .
O1B O 0.2690(5) 0.2794(4) 0.4134(3) 0.0334(12) Uani 1 1 d . . . . .
O1C O 0.3670(5) 0.5682(3) 0.7330(3) 0.0297(11) Uani 1 1 d . . . . .
O2A O -0.0490(5) 0.1663(4) 0.2271(3) 0.0337(11) Uani 1 1 d . . . . .
O2B O 0.2441(5) 0.2011(4) 0.5598(3) 0.0363(12) Uani 1 1 d . . . . .
O2C O 0.2893(5) 0.3648(3) 0.7425(3) 0.0298(11) Uani 1 1 d . . . . .
O3 O 0.0397(5) 0.3557(3) 0.4086(3) 0.0259(10) Uani 1 1 d . . . . .
O4 O 0.0931(5) 0.5134(3) 0.5824(3) 0.0229(10) Uani 1 1 d . . . . .
O5 O -0.0078(5) 0.1599(3) 0.4065(3) 0.0289(11) Uani 1 1 d . . . . .
O6 O 0.2920(5) 0.4143(4) 0.5733(3) 0.0287(11) Uani 1 1 d . . . . .
O7 O 0.0882(5) 0.4566(3) 0.7288(3) 0.0299(11) Uani 1 1 d . . . . .
O8 O 0.0522(4) 0.3111(3) 0.5691(3) 0.0236(10) Uani 1 1 d . . . . .
O9 O 0.1307(5) 0.6720(3) 0.7461(3) 0.0300(11) Uani 1 1 d . . . . .
O10 O -0.1351(5) 0.5266(4) 0.7337(4) 0.0359(12) Uani 1 1 d D . . . .
H10 H -0.161(9) 0.476(4) 0.756(5) 0.054 Uiso 1 1 d D U . . .
O11 O -0.1590(5) 0.4151(3) 0.5693(3) 0.0260(10) Uani 1 1 d . . . . .
O12 O -0.2053(5) 0.2560(3) 0.4080(3) 0.0260(10) Uani 1 1 d . . . . .
N1 N 0.7031(13) 0.2798(8) 0.7491(9) 0.110(4) Uani 1 1 d D U . . .
O13 O 0.6960(16) 0.2602(9) 0.6691(11) 0.180(5) Uani 1 1 d . U . . .
O14 O 0.7324(11) 0.3697(6) 0.7830(8) 0.123(3) Uani 1 1 d D U . . .
O15 O 0.6859(12) 0.2110(6) 0.7915(8) 0.129(3) Uani 1 1 d . U . . .
C17 C 0.0293(11) 0.1433(7) 0.8233(6) 0.063(3) Uani 1 1 d . . . . .
H17A H 0.0804 0.2123 0.8215 0.095 Uiso 1 1 calc R U . . .
H17B H -0.0600 0.1187 0.7761 0.095 Uiso 1 1 calc R U . . .
H17C H 0.0770 0.0984 0.8146 0.095 Uiso 1 1 calc R U . . .
O16 O 0.0157(8) 0.1441(6) 0.9062(5) 0.083(2) Uani 1 1 d D . . . .
H16 H -0.037(6) 0.173(7) 0.910(7) 0.125 Uiso 1 1 d D U . . .
O17 O -0.1229(14) 0.2672(11) 0.9467(9) 0.070(4) Uani 0.5 1 d D U P . .
C18 C -0.068(2) 0.3703(15) 0.9904(14) 0.087(7) Uani 0.5 1 d D U P . .
H18A H -0.0500 0.3759 1.0536 0.130 Uiso 0.5 1 calc R U P . .
H18B H -0.1312 0.4033 0.9657 0.130 Uiso 0.5 1 calc R U P . .
H18C H 0.0167 0.4035 0.9822 0.130 Uiso 0.5 1 calc R U P . .


_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 O1B 1.925(5) . ?
Fe1 O3 1.961(4) . ?
Fe1 O6 1.974(5) . ?
Fe1 O5 2.020(5) . ?
Fe1 O2B 2.089(5) . ?
Fe1 O8 2.133(4) . ?
Fe2 O1C 1.912(5) . ?
Fe2 O4 1.966(4) . ?
Fe2 O6 1.978(4) . ?
Fe2 O7 2.014(5) . ?
Fe2 O2C 2.052(5) . ?
Fe2 O8 2.132(5) . ?
Fe3 O1A 1.903(5) . ?
Fe3 O9 1.967(5) 2_566 ?
Fe3 O5 1.975(5) . ?
Fe3 O12 1.998(4) . ?
Fe3 O2A 2.096(5) . ?
Fe3 O3 2.118(5) . ?
Fe4 O12 1.942(5) . ?
Fe4 O11 1.957(4) . ?
Fe4 O4 1.965(4) 2_566 ?
Fe4 O4 2.088(5) . ?
Fe4 O3 2.097(4) . ?
Fe4 O8 2.101(4) . ?
Fe5 O3 1.980(4) 2_566 ?
Fe5 O9 1.984(5) . ?
Fe5 O7 1.993(4) . ?
Fe5 O11 2.025(5) . ?
Fe5 O10 2.032(5) . ?
Fe5 O4 2.048(4) . ?
C1A O1A 1.330(8) . ?
C1A C6A 1.404(10) . ?
C1A C2A 1.417(10) . ?
C1B O1B 1.328(8) . ?
C1B C6B 1.402(11) . ?
C1B C2B 1.417(11) . ?
C1C O1C 1.308(8) . ?
C1C C6C 1.414(10) . ?
C1C C2C 1.435(10) . ?
C2A C3A 1.422(10) . ?
C2A C7A 1.456(11) . ?
C2B C3B 1.427(10) . ?
C2B C7B 1.437(11) . ?
C2C C3C 1.405(10) . ?
C2C C7C 1.453(10) . ?
C3A C4A 1.377(11) . ?
C3A H3A 0.9300 . ?
C3B C4B 1.347(12) . ?
C3B H3B 0.9300 . ?
C3C C4C 1.385(11) . ?
C3C H3C 0.9300 . ?
C4A C5A 1.397(11) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.401(13) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.391(11) . ?
C4C H4C 0.9300 . ?
C5A C6A 1.376(10) . ?
C5A H5A 0.9300 . ?
C5B C6B 1.403(11) . ?
C5B H5B 0.9300 . ?
C5C C6C 1.364(10) . ?
C5C H5C 0.9300 . ?
C6A H6A 0.9300 . ?
C6B H6B 0.9300 . ?
C6C H6C 0.9300 . ?
C7A O2A 1.246(8) . ?
C7A C8A 1.499(10) . ?
C7B O2B 1.256(9) . ?
C7B C8B 1.523(12) . ?
C7C O2C 1.250(8) . ?
C7C C8C 1.502(10) . ?
C8A H8A1 0.9600 . ?
C8A H8A2 0.9600 . ?
C8A H8A3 0.9600 . ?
C8B H8B1 0.9600 . ?
C8B H8B2 0.9600 . ?
C8B H8B3 0.9600 . ?
C8C H8C1 0.9600 . ?
C8C H8C2 0.9600 . ?
C8C H8C3 0.9600 . ?
C9 O5 1.433(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O6 1.424(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 O7 1.388(9) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O8 1.436(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O9 1.408(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 O10 1.424(8) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O11 1.445(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O12 1.419(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O3 Fe5 1.980(4) 2_566 ?
O4 Fe4 1.965(4) 2_566 ?
O9 Fe3 1.967(5) 2_566 ?
O10 H10 0.839(10) . ?
N1 O14 1.209(7) . ?
N1 O15 1.234(14) . ?
N1 O13 1.255(15) . ?
C17 O16 1.384(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O16 H16 0.821(7) . ?
O17 C18 1.376(16) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Fe1 O3 102.0(2) . . ?
O1B Fe1 O6 96.4(2) . . ?
O3 Fe1 O6 98.21(19) . . ?
O1B Fe1 O5 96.8(2) . . ?
O3 Fe1 O5 81.77(19) . . ?
O6 Fe1 O5 166.53(19) . . ?
O1B Fe1 O2B 86.23(19) . . ?
O3 Fe1 O2B 169.0(2) . . ?
O6 Fe1 O2B 87.9(2) . . ?
O5 Fe1 O2B 90.17(19) . . ?
O1B Fe1 O8 173.1(2) . . ?
O3 Fe1 O8 81.75(18) . . ?
O6 Fe1 O8 77.20(18) . . ?
O5 Fe1 O8 89.50(18) . . ?
O2B Fe1 O8 90.81(18) . . ?
O1C Fe2 O4 102.01(19) . . ?
O1C Fe2 O6 95.0(2) . . ?
O4 Fe2 O6 97.62(19) . . ?
O1C Fe2 O7 97.9(2) . . ?
O4 Fe2 O7 80.28(18) . . ?
O6 Fe2 O7 167.0(2) . . ?
O1C Fe2 O2C 86.93(19) . . ?
O4 Fe2 O2C 166.91(19) . . ?
O6 Fe2 O2C 91.02(19) . . ?
O7 Fe2 O2C 89.10(18) . . ?
O1C Fe2 O8 171.76(18) . . ?
O4 Fe2 O8 81.80(18) . . ?
O6 Fe2 O8 77.14(18) . . ?
O7 Fe2 O8 89.91(18) . . ?
O2C Fe2 O8 90.61(18) . . ?
O1A Fe3 O9 105.6(2) . 2_566 ?
O1A Fe3 O5 103.3(2) . . ?
O9 Fe3 O5 148.4(2) 2_566 . ?
O1A Fe3 O12 89.8(2) . . ?
O9 Fe3 O12 99.02(19) 2_566 . ?
O5 Fe3 O12 93.64(19) . . ?
O1A Fe3 O2A 85.0(2) . . ?
O9 Fe3 O2A 83.88(19) 2_566 . ?
O5 Fe3 O2A 86.14(19) . . ?
O12 Fe3 O2A 174.51(19) . . ?
O1A Fe3 O3 168.83(19) . . ?
O9 Fe3 O3 75.13(18) 2_566 . ?
O5 Fe3 O3 79.00(18) . . ?
O12 Fe3 O3 79.16(18) . . ?
O2A Fe3 O3 106.15(18) . . ?
O12 Fe4 O11 101.48(19) . . ?
O12 Fe4 O4 101.61(19) . 2_566 ?
O11 Fe4 O4 96.99(18) . 2_566 ?
O12 Fe4 O4 174.63(18) . . ?
O11 Fe4 O4 80.67(18) . . ?
O4 Fe4 O4 82.92(19) 2_566 . ?
O12 Fe4 O3 80.94(18) . . ?
O11 Fe4 O3 177.54(19) . . ?
O4 Fe4 O3 82.89(17) 2_566 . ?
O4 Fe4 O3 96.89(18) . . ?
O12 Fe4 O8 94.98(18) . . ?
O11 Fe4 O8 99.85(18) . . ?
O4 Fe4 O8 153.46(19) 2_566 . ?
O4 Fe4 O8 79.77(17) . . ?
O3 Fe4 O8 79.41(17) . . ?
O3 Fe5 O9 77.96(19) 2_566 . ?
O3 Fe5 O7 158.2(2) 2_566 . ?
O9 Fe5 O7 91.8(2) . . ?
O3 Fe5 O11 96.29(19) 2_566 . ?
O9 Fe5 O11 174.25(19) . . ?
O7 Fe5 O11 93.67(19) . . ?
O3 Fe5 O10 105.9(2) 2_566 . ?
O9 Fe5 O10 93.8(2) . . ?
O7 Fe5 O10 93.8(2) . . ?
O11 Fe5 O10 87.5(2) . . ?
O3 Fe5 O4 83.82(18) 2_566 . ?
O9 Fe5 O4 99.36(19) . . ?
O7 Fe5 O4 78.84(18) . . ?
O11 Fe5 O4 80.05(17) . . ?
O10 Fe5 O4 165.07(19) . . ?
O1A C1A C6A 116.6(7) . . ?
O1A C1A C2A 122.9(7) . . ?
C6A C1A C2A 120.4(6) . . ?
O1B C1B C6B 117.4(7) . . ?
O1B C1B C2B 123.2(7) . . ?
C6B C1B C2B 119.4(7) . . ?
O1C C1C C6C 117.8(7) . . ?
O1C C1C C2C 124.8(7) . . ?
C6C C1C C2C 117.5(7) . . ?
C1A C2A C3A 117.8(7) . . ?
C1A C2A C7A 122.8(6) . . ?
C3A C2A C7A 119.4(7) . . ?
C1B C2B C3B 119.0(7) . . ?
C1B C2B C7B 121.3(7) . . ?
C3B C2B C7B 119.6(7) . . ?
C3C C2C C1C 118.8(7) . . ?
C3C C2C C7C 120.2(7) . . ?
C1C C2C C7C 121.0(7) . . ?
C4A C3A C2A 121.3(8) . . ?
C4A C3A H3A 119.3 . . ?
C2A C3A H3A 119.3 . . ?
C4B C3B C2B 121.0(8) . . ?
C4B C3B H3B 119.5 . . ?
C2B C3B H3B 119.5 . . ?
C4C C3C C2C 121.2(7) . . ?
C4C C3C H3C 119.4 . . ?
C2C C3C H3C 119.4 . . ?
C3A C4A C5A 119.4(7) . . ?
C3A C4A H4A 120.3 . . ?
C5A C4A H4A 120.3 . . ?
C3B C4B C5B 120.4(8) . . ?
C3B C4B H4B 119.8 . . ?
C5B C4B H4B 119.8 . . ?
C3C C4C C5C 120.2(7) . . ?
C3C C4C H4C 119.9 . . ?
C5C C4C H4C 119.9 . . ?
C6A C5A C4A 121.4(7) . . ?
C6A C5A H5A 119.3 . . ?
C4A C5A H5A 119.3 . . ?
C4B C5B C6B 120.5(9) . . ?
C4B C5B H5B 119.7 . . ?
C6B C5B H5B 119.7 . . ?
C6C C5C C4C 119.8(7) . . ?
C6C C5C H5C 120.1 . . ?
C4C C5C H5C 120.1 . . ?
C5A C6A C1A 119.6(7) . . ?
C5A C6A H6A 120.2 . . ?
C1A C6A H6A 120.2 . . ?
C1B C6B C5B 119.6(8) . . ?
C1B C6B H6B 120.2 . . ?
C5B C6B H6B 120.2 . . ?
C5C C6C C1C 122.5(7) . . ?
C5C C6C H6C 118.7 . . ?
C1C C6C H6C 118.7 . . ?
O2A C7A C2A 122.2(7) . . ?
O2A C7A C8A 116.8(7) . . ?
C2A C7A C8A 120.9(6) . . ?
O2B C7B C2B 124.5(7) . . ?
O2B C7B C8B 115.1(8) . . ?
C2B C7B C8B 120.4(7) . . ?
O2C C7C C2C 123.7(6) . . ?
O2C C7C C8C 116.5(7) . . ?
C2C C7C C8C 119.8(7) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7C C8C H8C1 109.5 . . ?
C7C C8C H8C2 109.5 . . ?
H8C1 C8C H8C2 109.5 . . ?
C7C C8C H8C3 109.5 . . ?
H8C1 C8C H8C3 109.5 . . ?
H8C2 C8C H8C3 109.5 . . ?
O5 C9 H9A 109.5 . . ?
O5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O6 C10 H10A 109.5 . . ?
O6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C11 H11A 109.5 . . ?
O7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O8 C12 H12A 109.5 . . ?
O8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O9 C13 H13A 109.5 . . ?
O9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O10 C14 H14A 109.5 . . ?
O10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O11 C15 H15A 109.5 . . ?
O11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O12 C16 H16A 109.5 . . ?
O12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1A O1A Fe3 134.4(5) . . ?
C1B O1B Fe1 124.3(5) . . ?
C1C O1C Fe2 132.3(4) . . ?
C7A O2A Fe3 131.5(5) . . ?
C7B O2B Fe1 126.2(5) . . ?
C7C O2C Fe2 131.0(5) . . ?
Fe1 O3 Fe5 152.9(3) . 2_566 ?
Fe1 O3 Fe4 102.26(19) . . ?
Fe5 O3 Fe4 95.62(18) 2_566 . ?
Fe1 O3 Fe3 97.88(18) . . ?
Fe5 O3 Fe3 100.61(19) 2_566 . ?
Fe4 O3 Fe3 95.34(19) . . ?
Fe4 O4 Fe2 152.2(3) 2_566 . ?
Fe4 O4 Fe5 97.67(18) 2_566 . ?
Fe2 O4 Fe5 99.74(19) . . ?
Fe4 O4 Fe4 97.08(19) 2_566 . ?
Fe2 O4 Fe4 102.11(19) . . ?
Fe5 O4 Fe4 97.08(19) . . ?
C9 O5 Fe3 121.3(4) . . ?
C9 O5 Fe1 131.9(5) . . ?
Fe3 O5 Fe1 100.77(19) . . ?
C10 O6 Fe1 123.6(4) . . ?
C10 O6 Fe2 123.2(5) . . ?
Fe1 O6 Fe2 108.2(2) . . ?
C11 O7 Fe5 128.4(4) . . ?
C11 O7 Fe2 130.9(4) . . ?
Fe5 O7 Fe2 100.0(2) . . ?
C12 O8 Fe4 118.0(4) . . ?
C12 O8 Fe2 121.8(4) . . ?
Fe4 O8 Fe2 96.32(17) . . ?
C12 O8 Fe1 121.1(4) . . ?
Fe4 O8 Fe1 96.56(18) . . ?
Fe2 O8 Fe1 97.32(17) . . ?
C13 O9 Fe3 124.4(4) . 2_566 ?
C13 O9 Fe5 129.6(4) . . ?
Fe3 O9 Fe5 106.0(2) 2_566 . ?
C14 O10 Fe5 127.8(5) . . ?
C14 O10 H10 107(6) . . ?
Fe5 O10 H10 125(6) . . ?
C15 O11 Fe4 123.0(5) . . ?
C15 O11 Fe5 121.3(4) . . ?
Fe4 O11 Fe5 102.2(2) . . ?
C16 O12 Fe4 128.9(4) . . ?
C16 O12 Fe3 126.3(5) . . ?
Fe4 O12 Fe3 104.5(2) . . ?
O14 N1 O15 122.1(13) . . ?
O14 N1 O13 116.5(13) . . ?
O15 N1 O13 121.4(11) . . ?
O16 C17 H17A 109.5 . . ?
O16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C17 O16 H16 110(9) . . ?
O17 C18 H18A 109.5 . . ?
O17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_refine_diff_density_max         1.485
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.159

# start Validation Reply Form

_vrf_PLAT430_1                   
;
RESPONSE: This short distance assumes a strong hydrogen bond between
the O15 atom of the nitrate counterion and the O17 hydroxyl group of 
the crystallization methanol (whose H atom has not been located from 
a difference map).
;

_vrf_PLAT041_1                   
;
RESPONSE:The missing (not located by a difference synthesis) H-atom 
of the crystallization methanol molecule C18-O17 has been included in 
the sum and moiety formula and the Mr, Dx and F(000) have been modified 
accordingly. These modifications account for the differences detected in the 
relevant data items.  
;

_vrf_PLAT341_1                   
;
RESPONSE:Several crystals of the title compound were carefully
tested on the X-rays at 100 K. 
The diffraction quality of the crystals has proven to be moderate
and structure determination was eventually carried out by means of the
best data set collected. 
;

_vrf_CELLZ01_1                   
; 
RESPONSE:See comment above.
;

_vrf_PLAT003_1                   
;
RESPONSE: The structure is disordered, especially one solvent methanol 
molecule and the nitrate counter ion. Soft restraints were used to 
handle the disorder of these molecules. 
;
_vrf_PLAT300_1                   
;
RESPONSE: Carefull refinement of the title compound reveals 
that the site of the C18-O17 methanol molecule is partially occupied (50%).
;

_vrf_PLAT309_1                   
; 
RESPONSE:See comment above.
;

# end Validation Reply Form


####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1521259'
_audit_update_record             
;
2016-12-07 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H70 Fe6 O24'
_chemical_formula_sum            'C68 H70 Fe6 O24'
_chemical_formula_weight         1606.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4235(6)
_cell_length_b                   13.8876(9)
_cell_length_c                   14.4700(7)
_cell_angle_alpha                75.758(5)
_cell_angle_beta                 71.129(5)
_cell_angle_gamma                69.329(6)
_cell_volume                     2009.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5419
_cell_measurement_theta_min      4.1700
_cell_measurement_theta_max      27.9120

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_F_000             826
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.122
_shelx_estimated_absorpt_T_min   0.841
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.32633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Oxford Diffraction SuperNova with Atlas detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            20526
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.084
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7862
_reflns_number_gt                5682
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990);
MERCURY (Bruno et al. 2002); DIAMOND (Brandenburg, 2014); 
X-SEED (Barbour, 2001)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0753P)²+3.1859P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7862
_refine_ls_number_parameters     502
_refine_ls_number_restraints     431
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1701
_refine_ls_wR_factor_gt          0.1501
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.01771(6) 0.33250(5) 0.41705(5) 0.02387(18) Uani 1 1 d . . . . .
Fe2 Fe 0.09542(6) 0.26824(5) 0.60239(5) 0.03045(19) Uani 1 1 d . . . . .
Fe3 Fe 0.14619(5) 0.47358(5) 0.48866(4) 0.01918(17) Uani 1 1 d . . . . .
C1A C 0.1855(5) 0.2717(4) 0.2309(4) 0.0369(12) Uani 1 1 d . U . . .
C2A C 0.2807(4) 0.3208(4) 0.2221(4) 0.0364(12) Uani 1 1 d . U . . .
C3A C 0.4070(5) 0.2831(5) 0.1598(4) 0.0521(15) Uani 1 1 d . U . . .
H3A H 0.4710 0.3124 0.1546 0.063 Uiso 1 1 calc R U . . .
C4A C 0.4359(6) 0.2030(5) 0.1067(4) 0.0608(17) Uani 1 1 d . U . . .
H4A H 0.5194 0.1782 0.0675 0.073 Uiso 1 1 calc R U . . .
C5A C 0.3416(6) 0.1601(5) 0.1118(4) 0.0605(17) Uani 1 1 d . U . . .
H5A H 0.3611 0.1088 0.0736 0.073 Uiso 1 1 calc R U . . .
C6A C 0.2177(5) 0.1929(4) 0.1735(4) 0.0467(14) Uani 1 1 d . U . . .
H6A H 0.1555 0.1625 0.1769 0.056 Uiso 1 1 calc R U . . .
C7A C 0.2537(4) 0.4051(4) 0.2765(3) 0.0303(11) Uani 1 1 d . U . . .
C8A C 0.3235(4) 0.4822(4) 0.2423(3) 0.0341(11) Uani 1 1 d . U . . .
C9A C 0.3397(4) 0.5329(4) 0.3102(3) 0.0340(11) Uani 1 1 d . U . . .
C10A C 0.4125(4) 0.6030(5) 0.2724(4) 0.0417(12) Uani 1 1 d . U . . .
H10A H 0.4287 0.6332 0.3158 0.050 Uiso 1 1 calc R U . . .
C11A C 0.4607(5) 0.6283(5) 0.1725(4) 0.0521(14) Uani 1 1 d . U . . .
H11A H 0.5085 0.6755 0.1491 0.062 Uiso 1 1 calc R U . . .
C12A C 0.4382(5) 0.5836(5) 0.1062(4) 0.0548(15) Uani 1 1 d . U . . .
H12A H 0.4683 0.6027 0.0386 0.066 Uiso 1 1 calc R U . . .
C13A C 0.3733(5) 0.5130(5) 0.1397(4) 0.0459(13) Uani 1 1 d . U . . .
H13A H 0.3603 0.4831 0.0944 0.055 Uiso 1 1 calc R U . . .
O1A O 0.0680(3) 0.2982(3) 0.2878(2) 0.0342(8) Uani 1 1 d . . . . .
O2A O 0.1641(2) 0.4122(2) 0.3576(2) 0.0254(7) Uani 1 1 d . . . . .
O3A O 0.2936(3) 0.5143(3) 0.4068(2) 0.0345(8) Uani 1 1 d . . . . .
C1B C 0.2556(6) 0.1465(4) 0.7319(5) 0.0531(16) Uani 1 1 d . U . . .
C2B C 0.2036(6) 0.2201(4) 0.7999(4) 0.0454(14) Uani 1 1 d . U . . .
C3B C 0.2807(6) 0.2190(4) 0.8597(4) 0.0491(15) Uani 1 1 d . U . . .
H3B H 0.2474 0.2656 0.9049 0.059 Uiso 1 1 calc R U . . .
C4B C 0.4043(7) 0.1504(5) 0.8529(5) 0.0664(19) Uani 1 1 d . U . . .
H4B H 0.4552 0.1530 0.8904 0.080 Uiso 1 1 calc R U . . .
C5B C 0.4504(8) 0.0781(5) 0.7893(6) 0.077(2) Uani 1 1 d . U . . .
H5B H 0.5320 0.0300 0.7861 0.092 Uiso 1 1 calc R U . . .
C6B C 0.3774(7) 0.0754(5) 0.7296(6) 0.070(2) Uani 1 1 d . U . . .
H6B H 0.4107 0.0254 0.6878 0.084 Uiso 1 1 calc R U . . .
C7B C 0.0747(5) 0.2963(4) 0.8069(4) 0.0380(12) Uani 1 1 d D . . . .
C8B C -0.0139(7) 0.3597(5) 0.8976(4) 0.0313(12) Uani 0.5 1 d DG U P A 1
C9B C -0.0344(7) 0.3092(4) 0.9944(5) 0.0345(11) Uani 0.5 1 d G U P A 1
C10B C -0.1061(7) 0.3661(5) 1.0717(3) 0.0343(12) Uani 0.5 1 d G U P A 1
H10B H -0.1198 0.3323 1.1366 0.041 Uiso 0.5 1 calc R U P A 1
C11B C -0.1571(6) 0.4736(5) 1.0522(4) 0.0335(13) Uani 0.5 1 d G U P A 1
H11B H -0.2051 0.5116 1.1039 0.040 Uiso 0.5 1 calc R U P A 1
C12B C -0.1366(7) 0.5241(4) 0.9553(4) 0.0314(12) Uani 0.5 1 d G U P A 1
H12B H -0.1708 0.5960 0.9422 0.038 Uiso 0.5 1 calc R U P A 1
C13B C -0.0650(8) 0.4672(5) 0.8780(3) 0.0316(12) Uani 0.5 1 d G U P A 1
H13B H -0.0512 0.5010 0.8132 0.038 Uiso 0.5 1 calc R U P A 1
O3B O 0.0121(8) 0.2061(6) 1.0157(5) 0.0359(15) Uani 0.5 1 d . U P A 1
C8C C 0.0125(7) 0.3303(5) 0.8975(4) 0.0318(12) Uani 0.5 1 d DG U P A 2
C9C C 0.0091(7) 0.2690(4) 0.9896(5) 0.0355(12) Uani 0.5 1 d DG U P A 2
C10C C -0.0682(7) 0.3117(5) 1.0746(3) 0.0379(13) Uani 0.5 1 d G U P A 2
H10C H -0.0705 0.2707 1.1362 0.045 Uiso 0.5 1 calc R U P A 2
C11C C -0.1421(6) 0.4157(5) 1.0676(4) 0.0359(12) Uani 0.5 1 d G U P A 2
H11C H -0.1938 0.4443 1.1245 0.043 Uiso 0.5 1 calc R U P A 2
C12C C -0.1386(7) 0.4770(4) 0.9756(4) 0.0345(12) Uani 0.5 1 d G U P A 2
H12C H -0.1881 0.5466 0.9709 0.041 Uiso 0.5 1 calc R U P A 2
C13C C -0.0613(7) 0.4343(5) 0.8905(3) 0.0315(12) Uani 0.5 1 d G U P A 2
H13C H -0.0591 0.4753 0.8290 0.038 Uiso 0.5 1 calc R U P A 2
O3C O 0.0755(7) 0.1640(5) 0.9919(5) 0.0399(18) Uani 0.5 1 d D . P A 2
O1B O 0.1922(4) 0.1437(3) 0.6714(3) 0.0519(11) Uani 1 1 d . U . . .
O2B O 0.0239(3) 0.3239(3) 0.7362(2) 0.0337(8) Uani 1 1 d . U . . .
C14 C -0.1224(5) 0.2090(4) 0.5812(4) 0.0440(13) Uani 1 1 d . . . . .
C15 C -0.2145(6) 0.1455(5) 0.6233(5) 0.0594(17) Uani 1 1 d . . . . .
H15A H -0.2641 0.1552 0.5776 0.089 Uiso 1 1 calc R U . . .
H15B H -0.2719 0.1671 0.6845 0.089 Uiso 1 1 calc R U . . .
H15C H -0.1667 0.0733 0.6348 0.089 Uiso 1 1 calc R U . . .
C16 C -0.1962(4) 0.4878(4) 0.3277(3) 0.0270(10) Uani 1 1 d . . . . .
H16A H -0.1402 0.4710 0.2636 0.032 Uiso 1 1 calc R U . . .
H16B H -0.2400 0.5621 0.3204 0.032 Uiso 1 1 calc R U . . .
C17 C -0.2950(5) 0.4300(4) 0.3613(4) 0.0411(13) Uani 1 1 d . . . . .
H17A H -0.2518 0.3566 0.3647 0.062 Uiso 1 1 calc R U . . .
H17B H -0.3472 0.4513 0.3153 0.062 Uiso 1 1 calc R U . . .
H17C H -0.3493 0.4452 0.4255 0.062 Uiso 1 1 calc R U . . .
C18 C 0.3701(4) 0.2791(4) 0.5103(4) 0.0432(14) Uani 1 1 d . . . . .
H18A H 0.3909 0.2978 0.4391 0.052 Uiso 1 1 calc R U . . .
H18B H 0.3813 0.2048 0.5258 0.052 Uiso 1 1 calc R U . . .
C19 C 0.4600(4) 0.3045(5) 0.5505(5) 0.0504(16) Uani 1 1 d . . . . .
H19A H 0.4470 0.3782 0.5368 0.076 Uiso 1 1 calc R U . . .
H19B H 0.5482 0.2690 0.5198 0.076 Uiso 1 1 calc R U . . .
H19C H 0.4424 0.2824 0.6206 0.076 Uiso 1 1 calc R U . . .
C20A C 0.1735(9) 0.1098(5) 0.4631(8) 0.0405(18) Uani 0.75 1 d D U P B 1
H20A H 0.1382 0.1074 0.4114 0.049 Uiso 0.75 1 calc R U P B 1
H20B H 0.1329 0.0732 0.5245 0.049 Uiso 0.75 1 calc R U P B 1
C21A C 0.3178(9) 0.0607(12) 0.4374(10) 0.062(4) Uani 0.75 1 d D U P B 1
H21A H 0.3375 -0.0106 0.4299 0.093 Uiso 0.75 1 calc R U P B 1
H21B H 0.3567 0.0976 0.3765 0.093 Uiso 0.75 1 calc R U P B 1
H21C H 0.3514 0.0636 0.4891 0.093 Uiso 0.75 1 calc R U P B 1
C20B C 0.204(2) 0.1155(13) 0.441(2) 0.038(5) Uani 0.25 1 d D U P B 2
H20C H 0.1660 0.1184 0.3888 0.045 Uiso 0.25 1 calc R U P B 2
H20D H 0.1754 0.0655 0.4956 0.045 Uiso 0.25 1 calc R U P B 2
C21B C 0.349(2) 0.072(4) 0.403(3) 0.048(6) Uani 0.25 1 d D U P B 2
H21D H 0.3690 0.0051 0.3844 0.072 Uiso 0.25 1 calc R U P B 2
H21E H 0.3798 0.1183 0.3465 0.072 Uiso 0.25 1 calc R U P B 2
H21F H 0.3893 0.0651 0.4538 0.072 Uiso 0.25 1 calc R U P B 2
O4 O 0.0047(2) 0.4009(2) 0.5305(2) 0.0195(6) Uani 1 1 d . . . . .
O5 O -0.1095(3) 0.2514(3) 0.4923(3) 0.0372(8) Uani 1 1 d . . . . .
O6 O -0.0623(4) 0.2149(3) 0.6388(3) 0.0432(9) Uani 1 1 d . . . . .
O7 O -0.1185(2) 0.4622(2) 0.3962(2) 0.0208(6) Uani 1 1 d . . . . .
O8 O 0.2371(3) 0.3353(2) 0.5529(2) 0.0273(7) Uani 1 1 d . . . . .
O9 O 0.1498(3) 0.2162(2) 0.4733(3) 0.0375(8) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1A 1.899(3) . ?
Fe1 O7 1.953(3) . ?
Fe1 O9 1.994(3) . ?
Fe1 O5 2.024(3) . ?
Fe1 O4 2.033(3) . ?
Fe1 O2A 2.161(3) . ?
Fe1 Fe2 2.9290(9) . ?
Fe2 O1B 1.930(3) . ?
Fe2 O4 1.989(3) . ?
Fe2 O8 1.997(3) . ?
Fe2 O9 1.999(3) . ?
Fe2 O6 2.051(3) . ?
Fe2 O2B 2.070(3) . ?
Fe3 O3A 1.901(3) . ?
Fe3 O7 1.966(3) 2_566 ?
Fe3 O8 1.992(3) . ?
Fe3 O4 2.010(3) 2_566 ?
Fe3 O4 2.053(3) . ?
Fe3 O2A 2.187(3) . ?
C1A O1A 1.303(6) . ?
C1A C6A 1.411(7) . ?
C1A C2A 1.434(7) . ?
C2A C3A 1.423(7) . ?
C2A C7A 1.459(7) . ?
C3A C4A 1.391(8) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.378(9) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.391(8) . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?
C7A O2A 1.282(5) . ?
C7A C8A 1.454(7) . ?
C8A C13A 1.423(7) . ?
C8A C9A 1.430(7) . ?
C9A O3A 1.318(5) . ?
C9A C10A 1.398(7) . ?
C10A C11A 1.374(7) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.391(8) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.339(8) . ?
C12A H12A 0.9300 . ?
C13A H13A 0.9300 . ?
C1B O1B 1.319(6) . ?
C1B C6B 1.388(8) . ?
C1B C2B 1.432(8) . ?
C2B C3B 1.415(7) . ?
C2B C7B 1.468(8) . ?
C3B C4B 1.384(8) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.379(9) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.394(8) . ?
C5B H5B 0.9300 . ?
C6B H6B 0.9300 . ?
C7B O2B 1.250(5) . ?
C7B C8C 1.383(7) . ?
C7B C8B 1.613(7) . ?
C8B C9B 1.3900 . ?
C8B C13B 1.3900 . ?
C9B O3B 1.334(9) . ?
C9B C10B 1.3900 . ?
C10B C11B 1.3900 . ?
C10B H10B 0.9300 . ?
C11B C12B 1.3900 . ?
C11B H11B 0.9300 . ?
C12B C13B 1.3900 . ?
C12B H12B 0.9300 . ?
C13B H13B 0.9300 . ?
C8C C9C 1.3900 . ?
C8C C13C 1.3900 . ?
C9C O3C 1.383(7) . ?
C9C C10C 1.3900 . ?
C10C C11C 1.3900 . ?
C10C H10C 0.9300 . ?
C11C C12C 1.3900 . ?
C11C H11C 0.9300 . ?
C12C C13C 1.3900 . ?
C12C H12C 0.9300 . ?
C13C H13C 0.9300 . ?
C14 O5 1.261(6) . ?
C14 O6 1.271(6) . ?
C14 C15 1.495(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O7 1.438(5) . ?
C16 C17 1.500(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O8 1.446(5) . ?
C18 C19 1.504(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20A O9 1.441(6) . ?
C20A C21A 1.502(10) . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
C20B O9 1.444(10) . ?
C20B C21B 1.503(12) . ?
C20B H20C 0.9700 . ?
C20B H20D 0.9700 . ?
C21B H21D 0.9600 . ?
C21B H21E 0.9600 . ?
C21B H21F 0.9600 . ?
O4 Fe3 2.010(3) 2_566 ?
O7 Fe3 1.966(3) 2_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1A Fe1 O7 97.26(13) . . ?
O1A Fe1 O9 98.82(14) . . ?
O7 Fe1 O9 163.47(13) . . ?
O1A Fe1 O5 102.72(14) . . ?
O7 Fe1 O5 93.49(13) . . ?
O9 Fe1 O5 86.71(14) . . ?
O1A Fe1 O4 159.98(14) . . ?
O7 Fe1 O4 80.22(11) . . ?
O9 Fe1 O4 83.36(12) . . ?
O5 Fe1 O4 97.27(13) . . ?
O1A Fe1 O2A 84.33(13) . . ?
O7 Fe1 O2A 91.19(12) . . ?
O9 Fe1 O2A 86.60(13) . . ?
O5 Fe1 O2A 170.95(12) . . ?
O4 Fe1 O2A 75.90(11) . . ?
O1A Fe1 Fe2 141.51(10) . . ?
O7 Fe1 Fe2 120.76(8) . . ?
O9 Fe1 Fe2 42.87(10) . . ?
O5 Fe1 Fe2 82.16(9) . . ?
O4 Fe1 Fe2 42.66(8) . . ?
O2A Fe1 Fe2 88.80(8) . . ?
O1B Fe2 O4 176.15(14) . . ?
O1B Fe2 O8 95.37(15) . . ?
O4 Fe2 O8 80.89(12) . . ?
O1B Fe2 O9 96.55(15) . . ?
O4 Fe2 O9 84.37(12) . . ?
O8 Fe2 O9 89.46(14) . . ?
O1B Fe2 O6 92.52(15) . . ?
O4 Fe2 O6 91.25(12) . . ?
O8 Fe2 O6 171.86(13) . . ?
O9 Fe2 O6 87.63(15) . . ?
O1B Fe2 O2B 85.85(15) . . ?
O4 Fe2 O2B 93.49(12) . . ?
O8 Fe2 O2B 94.20(12) . . ?
O9 Fe2 O2B 175.42(13) . . ?
O6 Fe2 O2B 88.37(14) . . ?
O1B Fe2 Fe1 137.96(11) . . ?
O4 Fe2 Fe1 43.84(8) . . ?
O8 Fe2 Fe1 94.30(9) . . ?
O9 Fe2 Fe1 42.74(9) . . ?
O6 Fe2 Fe1 78.43(9) . . ?
O2B Fe2 Fe1 133.99(9) . . ?
O3A Fe3 O7 98.20(13) . 2_566 ?
O3A Fe3 O8 98.74(14) . . ?
O7 Fe3 O8 91.01(12) 2_566 . ?
O3A Fe3 O4 104.14(14) . 2_566 ?
O7 Fe3 O4 80.49(11) 2_566 2_566 ?
O8 Fe3 O4 156.47(12) . 2_566 ?
O3A Fe3 O4 157.54(13) . . ?
O7 Fe3 O4 104.20(11) 2_566 . ?
O8 Fe3 O4 79.45(11) . . ?
O4 Fe3 O4 81.44(12) 2_566 . ?
O3A Fe3 O2A 82.86(12) . . ?
O7 Fe3 O2A 175.48(11) 2_566 . ?
O8 Fe3 O2A 93.17(12) . . ?
O4 Fe3 O2A 95.00(11) 2_566 . ?
O4 Fe3 O2A 74.93(11) . . ?
O1A C1A C6A 117.6(5) . . ?
O1A C1A C2A 123.2(4) . . ?
C6A C1A C2A 119.1(5) . . ?
C3A C2A C1A 118.2(5) . . ?
C3A C2A C7A 119.3(5) . . ?
C1A C2A C7A 122.5(4) . . ?
C4A C3A C2A 120.8(6) . . ?
C4A C3A H3A 119.6 . . ?
C2A C3A H3A 119.6 . . ?
C5A C4A C3A 120.5(5) . . ?
C5A C4A H4A 119.7 . . ?
C3A C4A H4A 119.7 . . ?
C4A C5A C6A 120.6(6) . . ?
C4A C5A H5A 119.7 . . ?
C6A C5A H5A 119.7 . . ?
C5A C6A C1A 120.7(6) . . ?
C5A C6A H6A 119.6 . . ?
C1A C6A H6A 119.6 . . ?
O2A C7A C8A 118.4(4) . . ?
O2A C7A C2A 118.8(4) . . ?
C8A C7A C2A 122.8(4) . . ?
C13A C8A C9A 117.7(5) . . ?
C13A C8A C7A 120.9(5) . . ?
C9A C8A C7A 121.3(4) . . ?
O3A C9A C10A 118.2(4) . . ?
O3A C9A C8A 123.6(4) . . ?
C10A C9A C8A 118.1(4) . . ?
C11A C10A C9A 121.5(5) . . ?
C11A C10A H10A 119.2 . . ?
C9A C10A H10A 119.2 . . ?
C10A C11A C12A 120.1(5) . . ?
C10A C11A H11A 119.9 . . ?
C12A C11A H11A 119.9 . . ?
C13A C12A C11A 120.1(5) . . ?
C13A C12A H12A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
C12A C13A C8A 122.2(5) . . ?
C12A C13A H13A 118.9 . . ?
C8A C13A H13A 118.9 . . ?
C1A O1A Fe1 126.9(3) . . ?
C7A O2A Fe1 128.8(3) . . ?
C7A O2A Fe3 129.7(3) . . ?
Fe1 O2A Fe3 99.88(11) . . ?
C9A O3A Fe3 133.1(3) . . ?
O1B C1B C6B 118.7(6) . . ?
O1B C1B C2B 122.5(5) . . ?
C6B C1B C2B 118.8(5) . . ?
C3B C2B C1B 118.3(5) . . ?
C3B C2B C7B 120.3(5) . . ?
C1B C2B C7B 121.4(4) . . ?
C4B C3B C2B 121.8(5) . . ?
C4B C3B H3B 119.1 . . ?
C2B C3B H3B 119.1 . . ?
C5B C4B C3B 118.7(5) . . ?
C5B C4B H4B 120.6 . . ?
C3B C4B H4B 120.6 . . ?
C4B C5B C6B 121.5(6) . . ?
C4B C5B H5B 119.3 . . ?
C6B C5B H5B 119.3 . . ?
C1B C6B C5B 120.8(6) . . ?
C1B C6B H6B 119.6 . . ?
C5B C6B H6B 119.6 . . ?
O2B C7B C8C 123.2(5) . . ?
O2B C7B C2B 121.2(5) . . ?
C8C C7B C2B 115.5(5) . . ?
O2B C7B C8B 111.6(5) . . ?
C2B C7B C8B 127.0(5) . . ?
C9B C8B C13B 120.0 . . ?
C9B C8B C7B 121.0(4) . . ?
C13B C8B C7B 118.9(4) . . ?
O3B C9B C10B 118.5(5) . . ?
O3B C9B C8B 121.5(5) . . ?
C10B C9B C8B 120.0 . . ?
C11B C10B C9B 120.0 . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C10B C11B C12B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C12B C11B H11B 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C13B C12B H12B 120.0 . . ?
C11B C12B H12B 120.0 . . ?
C12B C13B C8B 120.0 . . ?
C12B C13B H13B 120.0 . . ?
C8B C13B H13B 120.0 . . ?
C7B C8C C9C 126.3(5) . . ?
C7B C8C C13C 113.5(5) . . ?
C9C C8C C13C 120.0 . . ?
O3C C9C C10C 122.2(5) . . ?
O3C C9C C8C 117.6(5) . . ?
C10C C9C C8C 120.0 . . ?
C9C C10C C11C 120.0 . . ?
C9C C10C H10C 120.0 . . ?
C11C C10C H10C 120.0 . . ?
C12C C11C C10C 120.0 . . ?
C12C C11C H11C 120.0 . . ?
C10C C11C H11C 120.0 . . ?
C11C C12C C13C 120.0 . . ?
C11C C12C H12C 120.0 . . ?
C13C C12C H12C 120.0 . . ?
C12C C13C C8C 120.0 . . ?
C12C C13C H13C 120.0 . . ?
C8C C13C H13C 120.0 . . ?
C1B O1B Fe2 122.5(3) . . ?
C7B O2B Fe2 127.7(4) . . ?
O5 C14 O6 125.4(5) . . ?
O5 C14 C15 118.1(5) . . ?
O6 C14 C15 116.5(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 C17 111.9(4) . . ?
O7 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
O7 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O8 C18 C19 110.1(4) . . ?
O8 C18 H18A 109.6 . . ?
C19 C18 H18A 109.6 . . ?
O8 C18 H18B 109.6 . . ?
C19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O9 C20A C21A 107.0(9) . . ?
O9 C20A H20A 110.3 . . ?
C21A C20A H20A 110.3 . . ?
O9 C20A H20B 110.3 . . ?
C21A C20A H20B 110.3 . . ?
H20A C20A H20B 108.6 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
O9 C20B C21B 120(3) . . ?
O9 C20B H20C 107.4 . . ?
C21B C20B H20C 107.4 . . ?
O9 C20B H20D 107.4 . . ?
C21B C20B H20D 107.4 . . ?
H20C C20B H20D 106.9 . . ?
C20B C21B H21D 109.5 . . ?
C20B C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
C20B C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
Fe2 O4 Fe3 155.24(16) . 2_566 ?
Fe2 O4 Fe1 93.49(12) . . ?
Fe3 O4 Fe1 97.35(11) 2_566 . ?
Fe2 O4 Fe3 98.80(11) . . ?
Fe3 O4 Fe3 98.56(12) 2_566 . ?
Fe1 O4 Fe3 109.11(13) . . ?
C14 O5 Fe1 125.1(3) . . ?
C14 O6 Fe2 127.9(4) . . ?
C16 O7 Fe1 126.8(3) . . ?
C16 O7 Fe3 130.1(2) . 2_566 ?
Fe1 O7 Fe3 101.56(12) . 2_566 ?
C18 O8 Fe3 122.6(3) . . ?
C18 O8 Fe2 122.4(3) . . ?
Fe3 O8 Fe2 100.59(12) . . ?
C20A O9 Fe1 121.4(5) . . ?
C20B O9 Fe1 122.7(17) . . ?
C20A O9 Fe2 124.5(5) . . ?
C20B O9 Fe2 135.8(14) . . ?
Fe1 O9 Fe2 94.38(13) . . ?

_refine_diff_density_max         0.564
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.108

# start Validation Reply Form

_vrf_PLAT041_5                   
;
RESPONSE:The missing (not located by a difference synthesis) H-atoms 
of the disordered hydroxyl groups O3B/O3C of the ligand 
(2,2'-dihydroxybenzophenone) have been included in the sum and moiety 
formula and the Mr, Dx and F(000) have been modified accordingly. 
These modifications account for the differences detected in the 
relevant data items.  
;

_vrf_PLAT309_5                   
; 
RESPONSE:See comment below (PLAT041).
;

_vrf_PLAT341_5                   
;
RESPONSE:Several crystals of the title compound were carefully
tested on the X-rays at 100 K. 
The diffraction quality of the crystals has proven to be moderate
and structure determination was eventually carried out by means of the
best data set collected. 
;

_vrf_CELLZ01_5                   
; 
RESPONSE:See comment below (PLAT041).
;

_vrf_PLAT003_5                   
;
RESPONSE: The structure is disordered and soft restraints were used to 
handle the disordered atoms. 
;

_vrf_PLAT606_5                   
;
RESPONSE: The structure contains an area of disordered 
solvent molecules; attempts to model it with a chemically reasonable 
geometry were unsuccessful. Therefore, the SQUEEZE procedure of PLATON 
(A.L.Spek (2015) Acta Cryst. C71, 9-18) was employed to remove the 
contribution of the electron density associated with those solvent 
molecules from the intensity data. The solvent-free model and intensity 
data were used for the final results reported here.  
;

_vrf_PLAT869_5                   
; 
RESPONSE:See comment above.
;

# end Validation Reply Form




#===END
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1521258'
_audit_update_record             
;
2016-12-07 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H86 Cl4 Fe10 O28'
_chemical_formula_sum            'C68 H86 Cl4 Fe10 O28'
_chemical_formula_weight         2051.66

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4131(9)
_cell_length_b                   15.8853(14)
_cell_length_c                   15.9163(14)
_cell_angle_alpha                72.941(8)
_cell_angle_beta                 79.233(8)
_cell_angle_gamma                71.106(9)
_cell_volume                     2369.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3388
_cell_measurement_theta_min      3.5710
_cell_measurement_theta_max      29.0700

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_F_000             1046
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.661
_shelx_estimated_absorpt_T_min   0.801
_shelx_estimated_absorpt_T_max   0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Oxford Diffraction SuperNova with Atlas detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            16535
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.971
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8313
_reflns_number_gt                5206
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990);
MERCURY (Bruno et al. 2002); DIAMOND (Brandenburg, 2014); 
X-SEED (Barbour, 2001)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'

_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1531P)²+3.2142P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8313
_refine_ls_number_parameters     515
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0828
_refine_ls_wR_factor_ref         0.2639
_refine_ls_wR_factor_gt          0.2211
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.13174(12) 0.67933(7) 0.31459(7) 0.0322(3) Uani 1 1 d . . . . .
Fe2 Fe 0.07128(11) 0.66900(7) 0.52088(7) 0.0288(3) Uani 1 1 d . . . . .
Fe3 Fe 0.21481(11) 0.49755(7) 0.25558(7) 0.0304(3) Uani 1 1 d . . . . .
Fe4 Fe 0.14318(10) 0.48966(6) 0.45453(6) 0.0233(3) Uani 1 1 d . . . . .
Fe5 Fe -0.08310(11) 0.51641(7) 0.34366(7) 0.0290(3) Uani 1 1 d . . . . .
C1A C 0.3606(8) 0.3943(6) 0.1252(5) 0.0379(19) Uani 1 1 d . . . . .
C1B C -0.0704(9) 0.8202(5) 0.6087(5) 0.040(2) Uani 1 1 d . . . . .
C2A C 0.2883(8) 0.4536(5) 0.0517(5) 0.0328(18) Uani 1 1 d . . . . .
C2B C 0.0390(8) 0.8619(5) 0.5882(5) 0.0322(18) Uani 1 1 d . . . . .
C3A C 0.2916(9) 0.4210(5) -0.0216(5) 0.041(2) Uani 1 1 d . . . . .
H3A H 0.2436 0.4600 -0.0688 0.049 Uiso 1 1 calc R U . . .
C3B C 0.0156(9) 0.9464(5) 0.6094(5) 0.040(2) Uani 1 1 d . . . . .
H3B H 0.0825 0.9769 0.5920 0.048 Uiso 1 1 calc R U . . .
C4A C 0.3633(9) 0.3338(6) -0.0255(6) 0.047(2) Uani 1 1 d . . . . .
H4A H 0.3633 0.3131 -0.0744 0.057 Uiso 1 1 calc R U . . .
C4B C -0.1027(9) 0.9836(5) 0.6546(5) 0.043(2) Uani 1 1 d . . . . .
H4B H -0.1154 1.0387 0.6688 0.052 Uiso 1 1 calc R U . . .
C5A C 0.4383(9) 0.2747(6) 0.0457(6) 0.045(2) Uani 1 1 d . . . . .
H5A H 0.4886 0.2150 0.0437 0.054 Uiso 1 1 calc R U . . .
C5B C -0.2050(9) 0.9405(6) 0.6799(6) 0.046(2) Uani 1 1 d . . . . .
H5B H -0.2858 0.9664 0.7112 0.055 Uiso 1 1 calc R U . . .
C6A C 0.4359(8) 0.3063(5) 0.1174(5) 0.040(2) Uani 1 1 d . . . . .
H6A H 0.4871 0.2671 0.1631 0.048 Uiso 1 1 calc R U . . .
C6B C -0.1871(8) 0.8599(5) 0.6587(5) 0.0376(19) Uani 1 1 d . . . . .
H6B H -0.2550 0.8304 0.6784 0.045 Uiso 1 1 calc R U . . .
C7A C 0.1999(9) 0.5457(6) 0.0562(5) 0.040(2) Uani 1 1 d . . . . .
C7B C 0.1695(8) 0.8190(5) 0.5429(5) 0.0333(18) Uani 1 1 d . . . . .
C8A C 0.1533(9) 0.6167(5) -0.0239(5) 0.040(2) Uani 1 1 d . . . . .
C8B C 0.2939(8) 0.8488(5) 0.5370(5) 0.0349(19) Uani 1 1 d . . . . .
C9A C 0.0194(9) 0.6699(6) -0.0224(6) 0.045(2) Uani 1 1 d . . . . .
H9A H -0.0418 0.6571 0.0268 0.054 Uiso 1 1 calc R U . . .
C9B C 0.3793(9) 0.8529(5) 0.4581(5) 0.038(2) Uani 1 1 d . . . . .
H9B H 0.3555 0.8409 0.4102 0.045 Uiso 1 1 calc R U . . .
C10A C -0.0253(11) 0.7437(6) -0.0952(6) 0.052(2) Uani 1 1 d . . . . .
H10A H -0.1165 0.7782 -0.0959 0.062 Uiso 1 1 calc R U . . .
C10B C 0.5018(9) 0.8752(5) 0.4514(5) 0.039(2) Uani 1 1 d . . . . .
H10B H 0.5593 0.8783 0.3990 0.046 Uiso 1 1 calc R U . . .
C11A C 0.0701(11) 0.7637(6) -0.1657(6) 0.050(2) Uani 1 1 d . . . . .
H11A H 0.0428 0.8131 -0.2137 0.060 Uiso 1 1 calc R U . . .
C11B C 0.5362(9) 0.8928(5) 0.5247(6) 0.044(2) Uani 1 1 d . . . . .
H11B H 0.6160 0.9087 0.5209 0.053 Uiso 1 1 calc R U . . .
C12A C 0.2016(11) 0.7126(6) -0.1658(6) 0.055(3) Uani 1 1 d . . . . .
H12A H 0.2637 0.7276 -0.2138 0.066 Uiso 1 1 calc R U . . .
C12B C 0.4496(9) 0.8863(5) 0.6032(5) 0.039(2) Uani 1 1 d . . . . .
H12B H 0.4741 0.8949 0.6528 0.047 Uiso 1 1 calc R U . . .
C13A C 0.2461(9) 0.6383(6) -0.0958(5) 0.045(2) Uani 1 1 d . . . . .
H13A H 0.3370 0.6032 -0.0969 0.054 Uiso 1 1 calc R U . . .
C13B C 0.3288(8) 0.8675(5) 0.6077(5) 0.0355(19) Uani 1 1 d . . . . .
H13B H 0.2693 0.8674 0.6592 0.043 Uiso 1 1 calc R U . . .
C14 C 0.3941(9) 0.6221(6) 0.1857(6) 0.050(2) Uani 1 1 d . . . . .
H14A H 0.4598 0.5647 0.1810 0.074 Uiso 1 1 calc R U . . .
H14B H 0.4348 0.6568 0.2075 0.074 Uiso 1 1 calc R U . . .
H14C H 0.3649 0.6564 0.1285 0.074 Uiso 1 1 calc R U . . .
C15 C 0.0207(15) 0.7965(8) 0.1302(8) 0.097(4) Uani 1 1 d . U . . .
H15A H 0.0544 0.8448 0.1338 0.145 Uiso 1 1 calc R U . . .
H15B H -0.0626 0.8228 0.1025 0.145 Uiso 1 1 calc R U . . .
H15C H 0.0873 0.7587 0.0958 0.145 Uiso 1 1 calc R U . . .
C16 C 0.3611(7) 0.5881(5) 0.4334(5) 0.0356(18) Uani 1 1 d . . . . .
H16A H 0.4124 0.5570 0.3890 0.053 Uiso 1 1 calc R U . . .
H16B H 0.3870 0.5510 0.4906 0.053 Uiso 1 1 calc R U . . .
H16C H 0.3794 0.6460 0.4223 0.053 Uiso 1 1 calc R U . . .
C17 C -0.0991(9) 0.8195(6) 0.3853(6) 0.057(3) Uani 1 1 d . . . . .
H17A H -0.0585 0.8640 0.3445 0.085 Uiso 1 1 calc R U . . .
H17B H -0.1360 0.8391 0.4386 0.085 Uiso 1 1 calc R U . . .
H17C H -0.1710 0.8137 0.3593 0.085 Uiso 1 1 calc R U . . .
C18 C -0.2816(9) 0.4130(6) 0.3369(6) 0.045(2) Uani 1 1 d . . . . .
H18A H -0.3666 0.4302 0.3721 0.068 Uiso 1 1 calc R U . . .
H18B H -0.2646 0.3515 0.3319 0.068 Uiso 1 1 calc R U . . .
H18C H -0.2859 0.4544 0.2791 0.068 Uiso 1 1 calc R U . . .
C19 C 0.3493(13) 0.3306(6) 0.3900(6) 0.076(3) Uani 1 1 d . U . . .
H19A H 0.3098 0.2990 0.4447 0.114 Uiso 1 1 calc R U . . .
H19B H 0.4448 0.3191 0.3932 0.114 Uiso 1 1 calc R U . . .
H19C H 0.3375 0.3089 0.3425 0.114 Uiso 1 1 calc R U . . .
C20 C 0.0458(8) 0.3918(5) 0.2185(5) 0.0364(19) Uani 1 1 d . . . . .
H20A H 0.0057 0.4325 0.1663 0.055 Uiso 1 1 calc R U . . .
H20B H -0.0138 0.3557 0.2516 0.055 Uiso 1 1 calc R U . . .
H20C H 0.1322 0.3518 0.2019 0.055 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2299(2) 0.79864(14) 0.27156(15) 0.0499(6) Uani 1 1 d . . . . .
Cl2 Cl -0.1915(2) 0.61657(14) 0.22099(13) 0.0444(5) Uani 1 1 d . . . . .
O1A O 0.3602(5) 0.4201(4) 0.1959(3) 0.0366(13) Uani 1 1 d . . . . .
O1B O -0.0648(5) 0.7455(3) 0.5872(3) 0.0337(12) Uani 1 1 d . . . . .
O2A O 0.1576(6) 0.5680(3) 0.1289(3) 0.0382(13) Uani 1 1 d . . . . .
O2B O 0.1868(5) 0.7562(3) 0.5066(4) 0.0359(13) Uani 1 1 d . . . . .
O3 O 0.0648(5) 0.5710(3) 0.3375(3) 0.0266(11) Uani 1 1 d . . . . .
O4 O 0.0033(5) 0.5643(3) 0.5365(3) 0.0212(10) Uani 1 1 d . . . . .
O5 O 0.2794(5) 0.6049(3) 0.2450(3) 0.0342(12) Uani 1 1 d . . . . .
O6 O -0.0010(5) 0.7352(3) 0.4046(3) 0.0330(12) Uani 1 1 d . . . . .
O7 O -0.1751(5) 0.4174(3) 0.3772(3) 0.0316(12) Uani 1 1 d . . . . .
O8 O 0.2194(5) 0.6031(3) 0.4309(3) 0.0237(10) Uani 1 1 d . . . . .
O9 O 0.0653(5) 0.4441(3) 0.2712(3) 0.0305(12) Uani 1 1 d . . . . .
O10 O -0.0049(7) 0.7407(4) 0.2187(4) 0.0511(16) Uani 1 1 d D . . . .
H10 H -0.073(7) 0.723(7) 0.220(8) 0.077 Uiso 1 1 d D U . . .
O11 O -0.2164(5) 0.5813(3) 0.4318(3) 0.0276(11) Uani 1 1 d D . . . .
O12 O 0.2822(5) 0.4288(3) 0.3745(3) 0.0252(11) Uani 1 1 d . . . . .
C21A C -0.288(2) 0.6752(8) 0.4082(16) 0.042(5) Uani 0.35 1 d D U P A 1
H21A H -0.3113 0.6916 0.3488 0.063 Uiso 0.35 1 calc R U P A 1
H21B H -0.3693 0.6872 0.4478 0.063 Uiso 0.35 1 calc R U P A 1
H21C H -0.2311 0.7110 0.4119 0.063 Uiso 0.35 1 calc R U P A 1
C21B C -0.3481(13) 0.6381(10) 0.4140(8) 0.041(3) Uani 0.65 1 d . U P A 2
H21D H -0.3506 0.6628 0.3513 0.062 Uiso 0.65 1 calc R U P A 2
H21E H -0.4123 0.6029 0.4362 0.062 Uiso 0.65 1 calc R U P A 2
H21F H -0.3717 0.6876 0.4423 0.062 Uiso 0.65 1 calc R U 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 1.973(5) . ?
Fe1 O5 1.985(5) . ?
Fe1 O6 1.991(5) . ?
Fe1 O8 2.080(5) . ?
Fe1 O10 2.084(6) . ?
Fe1 Cl1 2.310(2) . ?
Fe2 O1B 1.918(5) . ?
Fe2 O4 1.945(5) . ?
Fe2 O6 1.991(5) . ?
Fe2 O7 2.018(5) 2_566 ?
Fe2 O2B 2.051(5) . ?
Fe2 O8 2.129(5) . ?
Fe3 O1A 1.910(5) . ?
Fe3 O9 1.948(5) . ?
Fe3 O5 1.981(5) . ?
Fe3 O12 2.014(5) . ?
Fe3 O2A 2.089(5) . ?
Fe3 O3 2.110(5) . ?
Fe4 O4 1.943(5) 2_566 ?
Fe4 O12 1.944(5) . ?
Fe4 O11 1.972(5) 2_566 ?
Fe4 O3 2.069(4) . ?
Fe4 O4 2.075(5) . ?
Fe4 O8 2.107(4) . ?
Fe5 O3 1.973(5) . ?
Fe5 O7 1.991(5) . ?
Fe5 O9 2.000(5) . ?
Fe5 O11 2.037(5) . ?
Fe5 O4 2.107(4) 2_566 ?
Fe5 Cl2 2.336(2) . ?
C1A O1A 1.305(9) . ?
C1A C6A 1.394(11) . ?
C1A C2A 1.430(10) . ?
C1B O1B 1.309(9) . ?
C1B C6B 1.394(11) . ?
C1B C2B 1.438(11) . ?
C2A C3A 1.400(11) . ?
C2A C7A 1.469(11) . ?
C2B C3B 1.413(11) . ?
C2B C7B 1.467(11) . ?
C3A C4A 1.357(11) . ?
C3A H3A 0.9300 . ?
C3B C4B 1.353(12) . ?
C3B H3B 0.9300 . ?
C4A C5A 1.416(11) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.384(12) . ?
C4B H4B 0.9300 . ?
C5A C6A 1.369(11) . ?
C5A H5A 0.9300 . ?
C5B C6B 1.364(12) . ?
C5B H5B 0.9300 . ?
C6A H6A 0.9300 . ?
C6B H6B 0.9300 . ?
C7A O2A 1.268(9) . ?
C7A C8A 1.471(11) . ?
C7B O2B 1.244(9) . ?
C7B C8B 1.496(11) . ?
C8A C9A 1.377(11) . ?
C8A C13A 1.391(12) . ?
C8B C13B 1.381(11) . ?
C8B C9B 1.394(11) . ?
C9A C10A 1.408(11) . ?
C9A H9A 0.9300 . ?
C9B C10B 1.408(11) . ?
C9B H9B 0.9300 . ?
C10A C11A 1.389(13) . ?
C10A H10A 0.9300 . ?
C10B C11B 1.409(12) . ?
C10B H10B 0.9300 . ?
C11A C12A 1.347(13) . ?
C11A H11A 0.9300 . ?
C11B C12B 1.396(12) . ?
C11B H11B 0.9300 . ?
C12A C13A 1.385(11) . ?
C12A H12A 0.9300 . ?
C12B C13B 1.368(11) . ?
C12B H12B 0.9300 . ?
C13A H13A 0.9300 . ?
C13B H13B 0.9300 . ?
C14 O5 1.425(10) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O10 1.457(12) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O8 1.422(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O6 1.386(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O7 1.411(9) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 O12 1.454(10) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O9 1.421(9) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O4 Fe4 1.943(5) 2_566 ?
O4 Fe5 2.107(4) 2_566 ?
O7 Fe2 2.018(5) 2_566 ?
O10 H10 0.841(10) . ?
O11 C21B 1.404(12) . ?
O11 C21A 1.406(10) . ?
O11 Fe4 1.972(5) 2_566 ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
C21B H21D 0.9600 . ?
C21B H21E 0.9600 . ?
C21B H21F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Fe1 O5 80.5(2) . . ?
O3 Fe1 O6 95.6(2) . . ?
O5 Fe1 O6 168.8(2) . . ?
O3 Fe1 O8 81.01(18) . . ?
O5 Fe1 O8 91.0(2) . . ?
O6 Fe1 O8 78.0(2) . . ?
O3 Fe1 O10 85.7(2) . . ?
O5 Fe1 O10 97.7(2) . . ?
O6 Fe1 O10 92.4(2) . . ?
O8 Fe1 O10 162.7(2) . . ?
O3 Fe1 Cl1 171.92(16) . . ?
O5 Fe1 Cl1 91.79(16) . . ?
O6 Fe1 Cl1 92.45(16) . . ?
O8 Fe1 Cl1 101.51(14) . . ?
O10 Fe1 Cl1 93.14(19) . . ?
O1B Fe2 O4 104.0(2) . . ?
O1B Fe2 O6 95.7(2) . . ?
O4 Fe2 O6 94.8(2) . . ?
O1B Fe2 O7 97.4(2) . 2_566 ?
O4 Fe2 O7 81.22(19) . 2_566 ?
O6 Fe2 O7 166.9(2) . 2_566 ?
O1B Fe2 O2B 86.8(2) . . ?
O4 Fe2 O2B 166.4(2) . . ?
O6 Fe2 O2B 92.2(2) . . ?
O7 Fe2 O2B 89.3(2) 2_566 . ?
O1B Fe2 O8 171.00(19) . . ?
O4 Fe2 O8 81.88(18) . . ?
O6 Fe2 O8 76.87(19) . . ?
O7 Fe2 O8 90.17(19) 2_566 . ?
O2B Fe2 O8 88.44(19) . . ?
O1A Fe3 O9 103.2(2) . . ?
O1A Fe3 O5 104.3(2) . . ?
O9 Fe3 O5 149.8(2) . . ?
O1A Fe3 O12 92.6(2) . . ?
O9 Fe3 O12 95.92(19) . . ?
O5 Fe3 O12 94.9(2) . . ?
O1A Fe3 O2A 84.6(2) . . ?
O9 Fe3 O2A 87.0(2) . . ?
O5 Fe3 O2A 83.6(2) . . ?
O12 Fe3 O2A 176.4(2) . . ?
O1A Fe3 O3 172.25(19) . . ?
O9 Fe3 O3 77.1(2) . . ?
O5 Fe3 O3 77.3(2) . . ?
O12 Fe3 O3 79.66(18) . . ?
O2A Fe3 O3 103.12(19) . . ?
O4 Fe4 O12 102.3(2) 2_566 . ?
O4 Fe4 O11 98.88(19) 2_566 2_566 ?
O12 Fe4 O11 100.0(2) . 2_566 ?
O4 Fe4 O3 82.97(19) 2_566 . ?
O12 Fe4 O3 82.29(19) . . ?
O11 Fe4 O3 176.66(19) 2_566 . ?
O4 Fe4 O4 82.6(2) 2_566 . ?
O12 Fe4 O4 174.75(18) . . ?
O11 Fe4 O4 81.13(19) 2_566 . ?
O3 Fe4 O4 96.40(19) . . ?
O4 Fe4 O8 152.2(2) 2_566 . ?
O12 Fe4 O8 95.28(19) . . ?
O11 Fe4 O8 99.07(19) 2_566 . ?
O3 Fe4 O8 78.21(18) . . ?
O4 Fe4 O8 79.47(18) . . ?
O3 Fe5 O7 156.1(2) . . ?
O3 Fe5 O9 79.2(2) . . ?
O7 Fe5 O9 90.1(2) . . ?
O3 Fe5 O11 97.2(2) . . ?
O7 Fe5 O11 90.4(2) . . ?
O9 Fe5 O11 171.72(19) . . ?
O3 Fe5 O4 81.29(18) . 2_566 ?
O7 Fe5 O4 77.98(19) . 2_566 ?
O9 Fe5 O4 93.15(19) . 2_566 ?
O11 Fe5 O4 78.89(19) . 2_566 ?
O3 Fe5 Cl2 99.66(14) . . ?
O7 Fe5 Cl2 102.36(15) . . ?
O9 Fe5 Cl2 93.75(14) . . ?
O11 Fe5 Cl2 94.20(14) . . ?
O4 Fe5 Cl2 173.09(15) 2_566 . ?
O1A C1A C6A 120.4(7) . . ?
O1A C1A C2A 123.0(7) . . ?
C6A C1A C2A 116.6(7) . . ?
O1B C1B C6B 118.4(8) . . ?
O1B C1B C2B 124.3(8) . . ?
C6B C1B C2B 117.2(7) . . ?
C3A C2A C1A 119.9(7) . . ?
C3A C2A C7A 119.6(7) . . ?
C1A C2A C7A 120.2(7) . . ?
C3B C2B C1B 118.4(7) . . ?
C3B C2B C7B 121.3(8) . . ?
C1B C2B C7B 120.2(7) . . ?
C4A C3A C2A 121.6(7) . . ?
C4A C3A H3A 119.2 . . ?
C2A C3A H3A 119.2 . . ?
C4B C3B C2B 121.0(8) . . ?
C4B C3B H3B 119.5 . . ?
C2B C3B H3B 119.5 . . ?
C3A C4A C5A 119.3(8) . . ?
C3A C4A H4A 120.3 . . ?
C5A C4A H4A 120.3 . . ?
C3B C4B C5B 120.8(8) . . ?
C3B C4B H4B 119.6 . . ?
C5B C4B H4B 119.6 . . ?
C6A C5A C4A 119.4(8) . . ?
C6A C5A H5A 120.3 . . ?
C4A C5A H5A 120.3 . . ?
C6B C5B C4B 119.8(8) . . ?
C6B C5B H5B 120.1 . . ?
C4B C5B H5B 120.1 . . ?
C5A C6A C1A 123.1(7) . . ?
C5A C6A H6A 118.4 . . ?
C1A C6A H6A 118.4 . . ?
C5B C6B C1B 122.4(8) . . ?
C5B C6B H6B 118.8 . . ?
C1B C6B H6B 118.8 . . ?
O2A C7A C2A 122.2(7) . . ?
O2A C7A C8A 116.4(7) . . ?
C2A C7A C8A 121.5(7) . . ?
O2B C7B C2B 123.9(7) . . ?
O2B C7B C8B 114.5(7) . . ?
C2B C7B C8B 121.5(7) . . ?
C9A C8A C13A 119.8(7) . . ?
C9A C8A C7A 119.0(8) . . ?
C13A C8A C7A 120.6(8) . . ?
C13B C8B C9B 120.0(8) . . ?
C13B C8B C7B 122.2(7) . . ?
C9B C8B C7B 117.7(7) . . ?
C8A C9A C10A 120.3(9) . . ?
C8A C9A H9A 119.9 . . ?
C10A C9A H9A 119.9 . . ?
C8B C9B C10B 119.6(8) . . ?
C8B C9B H9B 120.2 . . ?
C10B C9B H9B 120.2 . . ?
C11A C10A C9A 118.3(9) . . ?
C11A C10A H10A 120.8 . . ?
C9A C10A H10A 120.8 . . ?
C9B C10B C11B 119.3(8) . . ?
C9B C10B H10B 120.3 . . ?
C11B C10B H10B 120.3 . . ?
C12A C11A C10A 121.1(8) . . ?
C12A C11A H11A 119.5 . . ?
C10A C11A H11A 119.5 . . ?
C12B C11B C10B 119.5(8) . . ?
C12B C11B H11B 120.3 . . ?
C10B C11B H11B 120.3 . . ?
C11A C12A C13A 121.1(9) . . ?
C11A C12A H12A 119.4 . . ?
C13A C12A H12A 119.4 . . ?
C13B C12B C11B 120.4(8) . . ?
C13B C12B H12B 119.8 . . ?
C11B C12B H12B 119.8 . . ?
C12A C13A C8A 119.3(9) . . ?
C12A C13A H13A 120.4 . . ?
C8A C13A H13A 120.4 . . ?
C12B C13B C8B 121.0(8) . . ?
C12B C13B H13B 119.5 . . ?
C8B C13B H13B 119.5 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O10 C15 H15A 109.5 . . ?
O10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C17 H17A 109.5 . . ?
O6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O7 C18 H18A 109.5 . . ?
O7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O12 C19 H19A 109.5 . . ?
O12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O9 C20 H20A 109.5 . . ?
O9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1A O1A Fe3 129.3(5) . . ?
C1B O1B Fe2 132.8(6) . . ?
C7A O2A Fe3 129.8(5) . . ?
C7B O2B Fe2 130.2(5) . . ?
Fe5 O3 Fe1 150.7(3) . . ?
Fe5 O3 Fe4 98.03(19) . . ?
Fe1 O3 Fe4 102.8(2) . . ?
Fe5 O3 Fe3 99.4(2) . . ?
Fe1 O3 Fe3 98.9(2) . . ?
Fe4 O3 Fe3 95.34(19) . . ?
Fe4 O4 Fe2 152.0(3) 2_566 . ?
Fe4 O4 Fe4 97.5(2) 2_566 . ?
Fe2 O4 Fe4 102.8(2) . . ?
Fe4 O4 Fe5 97.70(19) 2_566 2_566 ?
Fe2 O4 Fe5 98.79(19) . 2_566 ?
Fe4 O4 Fe5 97.09(18) . 2_566 ?
C14 O5 Fe3 122.2(5) . . ?
C14 O5 Fe1 133.8(5) . . ?
Fe3 O5 Fe1 103.0(2) . . ?
C17 O6 Fe2 126.7(5) . . ?
C17 O6 Fe1 124.3(5) . . ?
Fe2 O6 Fe1 106.5(2) . . ?
C18 O7 Fe5 127.4(5) . . ?
C18 O7 Fe2 132.3(5) . 2_566 ?
Fe5 O7 Fe2 100.3(2) . 2_566 ?
C16 O8 Fe1 119.0(4) . . ?
C16 O8 Fe4 119.5(4) . . ?
Fe1 O8 Fe4 97.96(19) . . ?
C16 O8 Fe2 120.9(4) . . ?
Fe1 O8 Fe2 98.58(19) . . ?
Fe4 O8 Fe2 95.80(19) . . ?
C20 O9 Fe3 127.1(5) . . ?
C20 O9 Fe5 125.1(5) . . ?
Fe3 O9 Fe5 104.2(2) . . ?
C15 O10 Fe1 126.6(7) . . ?
C15 O10 H10 109(8) . . ?
Fe1 O10 H10 122(8) . . ?
C21B O11 Fe4 130.1(6) . 2_566 ?
C21A O11 Fe4 127.2(10) . 2_566 ?
C21B O11 Fe5 123.4(6) . . ?
C21A O11 Fe5 122.2(11) . . ?
Fe4 O11 Fe5 102.9(2) 2_566 . ?
C19 O12 Fe4 126.2(5) . . ?
C19 O12 Fe3 118.4(5) . . ?
Fe4 O12 Fe3 102.6(2) . . ?
O11 C21A H21A 109.5 . . ?
O11 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
O11 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
O11 C21B H21D 109.5 . . ?
O11 C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
O11 C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?

_refine_diff_density_max         2.755
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.172

_vrf_PLAT606_3                   
;
RESPONSE: The structure contains an area of disordered 
solvent involving two methanol molecules with partial occupancies; attempts 
to model it with a chemically reasonable geometry were unsuccessful. 
Therefore, the SQUEEZE procedure of PLATON (A.L.Spek (2015) Acta Cryst. C71, 
9-18) was employed to remove the contribution of the electron 
density associated with those solvent molecules from the intensity 
data. The solvent-free model and intensity data were used for the 
final results reported here.  
;

_vrf_PLAT084_3                   
;
RESPONSE: The rather high value of wR2 is attributed to the moderate 
quality of the diffraction data of the crystal.
;

_vrf_PLAT097_3                   
;
RESPONSE: The diffraction quality of the crystals has proven to be 
moderate and structure determination was eventually carried out by means 
of the best data set collected. 
The highest residual electron density maxima are located 
close to the Fe2 ion of the complex.
;

_vrf_PLAT869_3                   
; 
RESPONSE:See comment above.
;

# end Validation Reply Form




#===END
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1521257'
_audit_update_record             
;
2016-12-07 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C102 H106 Fe10 N2 O30, 2(Cl O4), C H4 O'
_chemical_formula_sum            'C103 H110 Cl2 Fe10 N2 O39'
_chemical_formula_weight         2629.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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

_cell_length_a                   27.692(3)
_cell_length_b                   17.496(2)
_cell_length_c                   27.706(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.695(11)
_cell_angle_gamma                90
_cell_volume                     11993(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6192
_cell_measurement_theta_min      3.7110
_cell_measurement_theta_max      28.4820

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_F_000             5392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.295
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Oxford Diffraction SuperNova with Atlas detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            29340
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.155
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10500
_reflns_number_gt                8100
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990);
MERCURY (Bruno et al. 2002); DIAMOND (Brandenburg, 2014); 
X-SEED (Barbour, 2001)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1113P)²+62.2471P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10500
_refine_ls_number_parameters     743
_refine_ls_number_restraints     141
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.2220
_refine_ls_wR_factor_gt          0.2048
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.42639(3) 0.81089(4) 0.48857(3) 0.0281(2) Uani 1 1 d . . . . .
Fe2 Fe 0.37394(3) 0.97190(5) 0.44152(3) 0.0299(2) Uani 1 1 d . . . . .
Fe3 Fe 0.46216(4) 1.22702(4) 0.50683(4) 0.0320(2) Uani 1 1 d . . . . .
Fe4 Fe 0.49182(3) 0.93694(4) 0.46068(3) 0.0248(2) Uani 1 1 d . . . . .
Fe5 Fe 0.44124(3) 1.09642(4) 0.42019(3) 0.0270(2) Uani 1 1 d . . . . .
C1A C 0.2571(3) 0.9773(4) 0.3796(3) 0.0468(18) Uani 1 1 d . . . . .
C1B C 0.3894(3) 0.7210(3) 0.5536(2) 0.0310(13) Uani 1 1 d . . . . .
C1C C 0.4209(3) 1.3564(3) 0.5461(3) 0.0373(14) Uani 1 1 d . . . . .
C2A C 0.2512(3) 1.0442(4) 0.4059(3) 0.0455(17) Uani 1 1 d . . . . .
C2B C 0.3384(2) 0.7033(3) 0.5112(2) 0.0324(13) Uani 1 1 d . . . . .
C2C C 0.4181(3) 1.4114(3) 0.5071(3) 0.0354(14) Uani 1 1 d . . . . .
C3A C 0.2033(3) 1.0863(6) 0.3808(3) 0.069(3) Uani 1 1 d . . . . .
H3A H 0.1990 1.1305 0.3972 0.083 Uiso 1 1 calc R U . . .
C3B C 0.2969(3) 0.6775(3) 0.5236(3) 0.0383(15) Uani 1 1 d . . . . .
H3B H 0.2627 0.6677 0.4957 0.046 Uiso 1 1 calc R U . . .
C3C C 0.4121(3) 1.4890(4) 0.5168(3) 0.0443(16) Uani 1 1 d . . . . .
H3C H 0.4097 1.5254 0.4914 0.053 Uiso 1 1 calc R U . . .
C4A C 0.1625(3) 1.0628(7) 0.3322(4) 0.079(3) Uani 1 1 d . . . . .
H4A H 0.1316 1.0928 0.3149 0.095 Uiso 1 1 calc R U . . .
C4B C 0.3060(3) 0.6666(4) 0.5756(3) 0.0449(16) Uani 1 1 d . . . . .
H4B H 0.2782 0.6497 0.5830 0.054 Uiso 1 1 calc R U . . .
C4C C 0.4096(3) 1.5118(4) 0.5626(3) 0.0486(18) Uani 1 1 d . . . . .
H4C H 0.4054 1.5633 0.5682 0.058 Uiso 1 1 calc R U . . .
C5A C 0.1667(3) 0.9968(7) 0.3092(3) 0.077(3) Uani 1 1 d . . . . .
H5A H 0.1377 0.9798 0.2777 0.092 Uiso 1 1 calc R U . . .
C5B C 0.3568(3) 0.6808(4) 0.6176(3) 0.0478(17) Uani 1 1 d . . . . .
H5B H 0.3631 0.6724 0.6531 0.057 Uiso 1 1 calc R U . . .
C5C C 0.4134(3) 1.4585(4) 0.6005(3) 0.0474(17) Uani 1 1 d . . . . .
H5C H 0.4128 1.4744 0.6323 0.057 Uiso 1 1 calc R U . . .
C6A C 0.2134(3) 0.9545(5) 0.3317(3) 0.060(2) Uani 1 1 d . . . . .
H6A H 0.2160 0.9099 0.3147 0.072 Uiso 1 1 calc R U . . .
C6B C 0.3981(3) 0.7073(3) 0.6071(3) 0.0399(15) Uani 1 1 d . . . . .
H6B H 0.4321 0.7163 0.6356 0.048 Uiso 1 1 calc R U . . .
C6C C 0.4180(3) 1.3828(4) 0.5923(3) 0.0444(16) Uani 1 1 d . . . . .
H6C H 0.4191 1.3477 0.6180 0.053 Uiso 1 1 calc R U . . .
C7A C 0.2938(3) 1.0656(4) 0.4581(3) 0.0411(16) Uani 1 1 d . . . . .
C7B C 0.3275(2) 0.7120(3) 0.4551(2) 0.0298(13) Uani 1 1 d . . . . .
C7C C 0.4259(3) 1.3885(3) 0.4607(3) 0.0364(14) Uani 1 1 d . . . . .
C8A C 0.2826(3) 1.1115(4) 0.4973(3) 0.0453(17) Uani 1 1 d . . . . .
C8B C 0.2831(3) 0.6693(3) 0.4112(2) 0.0356(14) Uani 1 1 d . . . . .
C8C C 0.4118(3) 1.4420(4) 0.4144(3) 0.0427(16) Uani 1 1 d . . . . .
C9A C 0.3220(3) 1.1600(4) 0.5321(3) 0.0525(18) Uani 1 1 d . . . . .
H9A H 0.3543 1.1651 0.5298 0.063 Uiso 1 1 calc R U . . .
C9B C 0.2563(3) 0.7026(4) 0.3607(3) 0.0477(17) Uani 1 1 d . . . . .
H9B H 0.2657 0.7515 0.3549 0.057 Uiso 1 1 calc R U . . .
C9C C 0.4483(4) 1.4513(4) 0.3934(3) 0.0515(19) Uani 1 1 d . . . . .
H9C H 0.4805 1.4239 0.4076 0.062 Uiso 1 1 calc R U . . .
C10A C 0.3142(4) 1.2009(5) 0.5702(4) 0.065(2) Uani 1 1 d . . . . .
H10A H 0.3406 1.2347 0.5927 0.078 Uiso 1 1 calc R U . . .
C10B C 0.2156(4) 0.6632(5) 0.3189(3) 0.068(2) Uani 1 1 d . . . . .
H10B H 0.1976 0.6856 0.2850 0.082 Uiso 1 1 calc R U . . .
C10C C 0.4362(5) 1.5017(5) 0.3510(4) 0.070(3) Uani 1 1 d . . . . .
H10C H 0.4609 1.5100 0.3372 0.084 Uiso 1 1 calc R U . . .
C11A C 0.2674(4) 1.1919(5) 0.5753(4) 0.065(2) Uani 1 1 d . . . . .
H11A H 0.2625 1.2192 0.6016 0.078 Uiso 1 1 calc R U . . .
C11B C 0.2021(4) 0.5925(5) 0.3275(3) 0.072(3) Uani 1 1 d . . . . .
H11B H 0.1740 0.5671 0.2994 0.087 Uiso 1 1 calc R U . . .
C11C C 0.3867(6) 1.5402(5) 0.3292(3) 0.080(4) Uani 1 1 d . . . . .
H11C H 0.3782 1.5733 0.3003 0.096 Uiso 1 1 calc R U . . .
C12A C 0.2280(4) 1.1431(5) 0.5418(4) 0.065(2) Uani 1 1 d . . . . .
H12A H 0.1966 1.1371 0.5457 0.078 Uiso 1 1 calc R U . . .
C12B C 0.2287(3) 0.5570(4) 0.3763(3) 0.061(2) Uani 1 1 d . . . . .
H12B H 0.2196 0.5074 0.3811 0.073 Uiso 1 1 calc R U . . .
C12C C 0.3516(4) 1.5300(4) 0.3493(3) 0.070(3) Uani 1 1 d . . . . .
H12C H 0.3189 1.5560 0.3340 0.084 Uiso 1 1 calc R U . . .
C13A C 0.2345(3) 1.1025(4) 0.5021(3) 0.0512(19) Uani 1 1 d . . . . .
H13A H 0.2075 1.0698 0.4790 0.061 Uiso 1 1 calc R U . . .
C13B C 0.2694(3) 0.5957(4) 0.4185(3) 0.0416(15) Uani 1 1 d . . . . .
H13B H 0.2877 0.5721 0.4519 0.050 Uiso 1 1 calc R U . . .
C13C C 0.3629(3) 1.4818(4) 0.3920(3) 0.0538(19) Uani 1 1 d . . . . .
H13C H 0.3382 1.4757 0.4059 0.065 Uiso 1 1 calc R U . . .
C14 C 0.4345(3) 1.1212(5) 0.3083(3) 0.0561(19) Uani 1 1 d . . . . .
H14 H 0.4315 1.0682 0.3068 0.067 Uiso 1 1 calc R U . . .
C15 C 0.4352(4) 1.1591(6) 0.2648(3) 0.069(2) Uani 1 1 d . . . . .
H15 H 0.4316 1.1322 0.2344 0.083 Uiso 1 1 calc R U . . .
C16 C 0.4415(4) 1.2378(5) 0.2673(3) 0.065(2) Uani 1 1 d . . . . .
H16 H 0.4427 1.2649 0.2389 0.078 Uiso 1 1 calc R U . . .
C17 C 0.4460(4) 1.2742(5) 0.3128(4) 0.069(2) Uani 1 1 d . . . . .
H17 H 0.4498 1.3271 0.3154 0.083 Uiso 1 1 calc R U . . .
C18 C 0.4449(3) 1.2341(4) 0.3542(3) 0.0529(19) Uani 1 1 d . . . . .
H18 H 0.4491 1.2605 0.3850 0.063 Uiso 1 1 calc R U . . .
C19 C 0.3341(3) 1.0443(5) 0.3264(3) 0.057(2) Uani 1 1 d . . . . .
H19A H 0.3470 1.0796 0.3083 0.086 Uiso 1 1 calc R U . . .
H19B H 0.2995 1.0609 0.3225 0.086 Uiso 1 1 calc R U . . .
H19C H 0.3308 0.9944 0.3108 0.086 Uiso 1 1 calc R U . . .
C20 C 0.3534(3) 0.8963(4) 0.5269(3) 0.0541(19) Uani 1 1 d . . . . .
H20A H 0.3167 0.8871 0.5007 0.081 Uiso 1 1 calc R U . . .
H20B H 0.3556 0.9444 0.5444 0.081 Uiso 1 1 calc R U . . .
H20C H 0.3650 0.8561 0.5534 0.081 Uiso 1 1 calc R U . . .
C21 C 0.3917(3) 0.8594(4) 0.3683(2) 0.0443(16) Uani 1 1 d . . . . .
H21A H 0.3534 0.8531 0.3543 0.066 Uiso 1 1 calc R U . . .
H21B H 0.4079 0.8111 0.3676 0.066 Uiso 1 1 calc R U . . .
H21C H 0.3992 0.8956 0.3464 0.066 Uiso 1 1 calc R U . . .
C22 C 0.4452(3) 0.6652(4) 0.4366(4) 0.061(2) Uani 1 1 d . . . . .
H22A H 0.4700 0.6448 0.4244 0.091 Uiso 1 1 calc R U . . .
H22B H 0.4099 0.6692 0.4066 0.091 Uiso 1 1 calc R U . . .
H22C H 0.4436 0.6318 0.4634 0.091 Uiso 1 1 calc R U . . .
C23 C 0.3519(3) 1.2082(4) 0.4124(3) 0.0456(17) Uani 1 1 d . . . . .
H23A H 0.3399 1.2290 0.4373 0.068 Uiso 1 1 calc R U . . .
H23B H 0.3285 1.1669 0.3927 0.068 Uiso 1 1 calc R U . . .
H23C H 0.3508 1.2473 0.3877 0.068 Uiso 1 1 calc R U . . .
C24 C 0.5235(4) 0.8447(5) 0.3870(3) 0.063(2) Uani 1 1 d . . . . .
H24A H 0.4968 0.8782 0.3615 0.094 Uiso 1 1 calc R U . . .
H24B H 0.5136 0.7926 0.3762 0.094 Uiso 1 1 calc R U . . .
H24C H 0.5580 0.8553 0.3883 0.094 Uiso 1 1 calc R U . . .
C25 C 0.5267(3) 1.0259(5) 0.3913(3) 0.057(2) Uani 1 1 d . . . . .
H25A H 0.5579 0.9975 0.4153 0.086 Uiso 1 1 calc R U . . .
H25B H 0.5352 1.0794 0.3943 0.086 Uiso 1 1 calc R U . . .
H25C H 0.5157 1.0094 0.3548 0.086 Uiso 1 1 calc R U . . .
N N 0.4379(2) 1.1574(3) 0.35282(19) 0.0353(12) Uani 1 1 d . . . . .
O1A O 0.30132(17) 0.9356(3) 0.39858(19) 0.0449(11) Uani 1 1 d . . . . .
O1B O 0.43023(16) 0.7486(2) 0.54674(16) 0.0334(9) Uani 1 1 d . . . . .
O1C O 0.4261(2) 1.2829(2) 0.54033(19) 0.0429(11) Uani 1 1 d . . . . .
O2A O 0.34192(17) 1.0475(2) 0.47400(19) 0.0385(10) Uani 1 1 d . . . . .
O2C O 0.44596(19) 1.3260(2) 0.45796(18) 0.0399(10) Uani 1 1 d . . . . .
O2B O 0.35524(17) 0.7551(2) 0.44130(16) 0.0352(10) Uani 1 1 d . . . . .
O3 O 0.50228(15) 1.1434(2) 0.48113(14) 0.0254(8) Uani 1 1 d . . . . .
O4 O 0.44693(15) 1.0174(2) 0.47735(15) 0.0247(8) Uani 1 1 d . . . . .
O5 O 0.46287(18) 0.7384(2) 0.45938(17) 0.0345(10) Uani 1 1 d . . . . .
O6 O 0.38739(16) 0.8979(2) 0.50052(16) 0.0293(9) Uani 1 1 d . . . . .
O7 O 0.37177(16) 1.0414(2) 0.38280(16) 0.0334(9) Uani 1 1 d . . . . .
O8 O 0.41392(16) 0.8870(2) 0.42313(15) 0.0279(8) Uani 1 1 d . . . . .
O9 O 0.40537(16) 1.1808(2) 0.44128(16) 0.0330(9) Uani 1 1 d . . . . .
O11 O 0.48368(16) 1.0131(2) 0.40536(15) 0.0281(8) Uani 1 1 d . . . . .
O12 O 0.52642(17) 0.8564(2) 0.43951(16) 0.0317(9) Uani 1 1 d . . . . .
Cl1 Cl 0.5000 0.55744(17) 0.7500 0.0579(7) Uani 1 2 d DS T P . .
O13A O 0.5349(7) 0.5967(9) 0.7905(7) 0.177(5) Uani 0.5 1 d D U P A 1
O14A O 0.5267(8) 0.5094(8) 0.7334(8) 0.177(5) Uani 0.5 1 d D U P A 1
O13B O 0.5144(9) 0.5988(9) 0.7970(7) 0.177(5) Uani 0.5 1 d D U P A 2
O14B O 0.5425(7) 0.5066(8) 0.7572(8) 0.177(5) Uani 0.5 1 d D U P A 2
Cl2 Cl 0.4268(3) 0.9372(4) 0.2225(3) 0.104(2) Uani 0.5 1 d D . P B -1
O15 O 0.4075(7) 0.9477(8) 0.2561(6) 0.129(6) Uani 0.5 1 d D U P B -1
O16 O 0.3893(6) 0.9374(11) 0.1738(5) 0.166(7) Uani 0.5 1 d D U P B -1
O17 O 0.4536(8) 0.8741(8) 0.2316(8) 0.204(9) Uani 0.5 1 d D U P B -1
O18 O 0.4594(7) 0.9933(9) 0.2269(9) 0.213(9) Uani 0.5 1 d D U P B -1
C26 C 0.2610(8) 0.7894(11) 0.2339(8) 0.089(6) Uani 0.5 1 d D U P . .
H26A H 0.2663 0.7900 0.2706 0.134 Uiso 0.5 1 calc R U P . .
H26B H 0.2386 0.7467 0.2152 0.134 Uiso 0.5 1 calc R U P . .
H26C H 0.2438 0.8360 0.2163 0.134 Uiso 0.5 1 calc R U P . .
O10 O 0.3136(9) 0.7824(15) 0.2332(7) 0.159(8) Uani 0.5 1 d D U P . .


_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 O1B 1.909(4) . ?
Fe1 O3 1.938(4) 5_676 ?
Fe1 O6 1.978(4) . ?
Fe1 O5 2.004(4) . ?
Fe1 O2B 2.057(4) . ?
Fe1 O8 2.148(4) . ?
Fe2 O1A 1.927(4) . ?
Fe2 O4 1.975(4) . ?
Fe2 O6 1.986(4) . ?
Fe2 O7 2.010(4) . ?
Fe2 O2A 2.016(4) . ?
Fe2 O8 2.050(4) . ?
Fe3 O1C 1.909(4) . ?
Fe3 O5 1.951(4) 5_676 ?
Fe3 O9 1.964(4) . ?
Fe3 O12 2.005(4) 5_676 ?
Fe3 O2C 2.118(4) . ?
Fe3 O3 2.143(4) . ?
Fe4 O12 1.937(4) . ?
Fe4 O4 1.961(4) 5_676 ?
Fe4 O11 1.966(4) . ?
Fe4 O4 2.063(4) . ?
Fe4 O3 2.090(4) 5_676 ?
Fe4 O8 2.118(4) . ?
Fe5 O3 1.955(4) . ?
Fe5 O7 1.978(4) . ?
Fe5 O9 2.007(4) . ?
Fe5 O11 2.027(4) . ?
Fe5 O4 2.054(4) . ?
Fe5 N 2.116(5) . ?
C1A O1A 1.315(8) . ?
C1A C6A 1.394(10) . ?
C1A C2A 1.427(11) . ?
C1B O1B 1.320(7) . ?
C1B C2B 1.406(9) . ?
C1B C6B 1.409(9) . ?
C1C O1C 1.312(7) . ?
C1C C6C 1.396(9) . ?
C1C C2C 1.424(9) . ?
C2A C3A 1.399(10) . ?
C2A C7A 1.446(10) . ?
C2B C3B 1.415(9) . ?
C2B C7B 1.454(8) . ?
C2C C3C 1.408(9) . ?
C2C C7C 1.451(9) . ?
C3A C4A 1.377(14) . ?
C3A H3A 0.9300 . ?
C3B C4B 1.358(9) . ?
C3B H3B 0.9300 . ?
C3C C4C 1.361(10) . ?
C3C H3C 0.9300 . ?
C4A C5A 1.349(15) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.388(10) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.374(10) . ?
C4C H4C 0.9300 . ?
C5A C6A 1.374(13) . ?
C5A H5A 0.9300 . ?
C5B C6B 1.381(10) . ?
C5B H5B 0.9300 . ?
C5C C6C 1.360(9) . ?
C5C H5C 0.9300 . ?
C6A H6A 0.9300 . ?
C6B H6B 0.9300 . ?
C6C H6C 0.9300 . ?
C7A O2A 1.243(7) . ?
C7A C8A 1.491(10) . ?
C7B O2B 1.251(7) . ?
C7B C8B 1.486(8) . ?
C7C O2C 1.245(7) . ?
C7C C8C 1.492(9) . ?
C8A C9A 1.377(11) . ?
C8A C13A 1.404(10) . ?
C8B C9B 1.382(9) . ?
C8B C13B 1.384(9) . ?
C8C C9C 1.381(10) . ?
C8C C13C 1.396(11) . ?
C9A C10A 1.369(11) . ?
C9A H9A 0.9300 . ?
C9B C10B 1.383(10) . ?
C9B H9B 0.9300 . ?
C9C C10C 1.386(11) . ?
C9C H9C 0.9300 . ?
C10A C11A 1.376(12) . ?
C10A H10A 0.9300 . ?
C10B C11B 1.344(12) . ?
C10B H10B 0.9300 . ?
C10C C11C 1.397(15) . ?
C10C H10C 0.9300 . ?
C11A C12A 1.367(13) . ?
C11A H11A 0.9300 . ?
C11B C12B 1.364(11) . ?
C11B H11B 0.9300 . ?
C11C C12C 1.332(15) . ?
C11C H11C 0.9300 . ?
C12A C13A 1.390(12) . ?
C12A H12A 0.9300 . ?
C12B C13B 1.382(10) . ?
C12B H12B 0.9300 . ?
C12C C13C 1.369(11) . ?
C12C H12C 0.9300 . ?
C13A H13A 0.9300 . ?
C13B H13B 0.9300 . ?
C13C H13C 0.9300 . ?
C14 N 1.353(9) . ?
C14 C15 1.383(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.385(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.358(11) . ?
C17 H17 0.9300 . ?
C18 N 1.353(9) . ?
C18 H18 0.9300 . ?
C19 O7 1.437(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O6 1.428(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O8 1.443(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.415(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O9 1.414(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 O12 1.434(8) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O11 1.427(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O3 Fe1 1.938(4) 5_676 ?
O3 Fe4 2.090(4) 5_676 ?
O4 Fe4 1.961(4) 5_676 ?
O5 Fe3 1.951(4) 5_676 ?
O12 Fe3 2.005(4) 5_676 ?
Cl1 O13A 1.30(2) . ?
Cl1 O13A 1.300(19) 2_656 ?
Cl1 O14A 1.331(19) 2_656 ?
Cl1 O14A 1.331(19) . ?
Cl1 O13B 1.382(19) . ?
Cl1 O13B 1.382(19) 2_656 ?
Cl1 O14B 1.416(19) 2_656 ?
Cl1 O14B 1.416(19) . ?
Cl2 O15 1.276(8) . ?
Cl2 O16 1.280(8) . ?
Cl2 O17 1.291(8) . ?
Cl2 O18 1.303(8) . ?
C26 O10 1.470(10) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Fe1 O3 102.16(17) . 5_676 ?
O1B Fe1 O6 97.21(17) . . ?
O3 Fe1 O6 97.89(16) 5_676 . ?
O1B Fe1 O5 97.59(18) . . ?
O3 Fe1 O5 80.52(16) 5_676 . ?
O6 Fe1 O5 165.11(17) . . ?
O1B Fe1 O2B 86.60(17) . . ?
O3 Fe1 O2B 165.89(17) 5_676 . ?
O6 Fe1 O2B 91.87(17) . . ?
O5 Fe1 O2B 87.42(17) . . ?
O1B Fe1 O8 173.37(17) . . ?
O3 Fe1 O8 81.73(15) 5_676 . ?
O6 Fe1 O8 76.82(15) . . ?
O5 Fe1 O8 88.31(16) . . ?
O2B Fe1 O8 90.67(15) . . ?
O1A Fe2 O4 172.55(18) . . ?
O1A Fe2 O6 92.93(18) . . ?
O4 Fe2 O6 94.47(16) . . ?
O1A Fe2 O7 93.22(18) . . ?
O4 Fe2 O7 79.33(16) . . ?
O6 Fe2 O7 170.86(17) . . ?
O1A Fe2 O2A 86.9(2) . . ?
O4 Fe2 O2A 93.86(17) . . ?
O6 Fe2 O2A 91.04(17) . . ?
O7 Fe2 O2A 96.04(18) . . ?
O1A Fe2 O8 97.94(18) . . ?
O4 Fe2 O8 82.64(15) . . ?
O6 Fe2 O8 78.99(15) . . ?
O7 Fe2 O8 93.46(16) . . ?
O2A Fe2 O8 169.10(17) . . ?
O1C Fe3 O5 106.49(19) . 5_676 ?
O1C Fe3 O9 106.5(2) . . ?
O5 Fe3 O9 143.96(18) 5_676 . ?
O1C Fe3 O12 87.42(17) . 5_676 ?
O5 Fe3 O12 95.20(18) 5_676 5_676 ?
O9 Fe3 O12 100.36(17) . 5_676 ?
O1C Fe3 O2C 83.42(17) . . ?
O5 Fe3 O2C 85.83(18) 5_676 . ?
O9 Fe3 O2C 83.91(17) . . ?
O12 Fe3 O2C 170.69(16) 5_676 . ?
O1C Fe3 O3 166.74(16) . . ?
O5 Fe3 O3 76.83(15) 5_676 . ?
O9 Fe3 O3 74.41(15) . . ?
O12 Fe3 O3 79.44(15) 5_676 . ?
O2C Fe3 O3 109.76(16) . . ?
O12 Fe4 O4 102.15(17) . 5_676 ?
O12 Fe4 O11 98.98(16) . . ?
O4 Fe4 O11 99.07(16) 5_676 . ?
O12 Fe4 O4 173.66(16) . . ?
O4 Fe4 O4 84.09(16) 5_676 . ?
O11 Fe4 O4 80.93(15) . . ?
O12 Fe4 O3 82.32(15) . 5_676 ?
O4 Fe4 O3 82.04(15) 5_676 5_676 ?
O11 Fe4 O3 178.04(15) . 5_676 ?
O4 Fe4 O3 97.62(15) . 5_676 ?
O12 Fe4 O8 94.84(16) . . ?
O4 Fe4 O8 152.59(16) 5_676 . ?
O11 Fe4 O8 99.33(15) . . ?
O4 Fe4 O8 78.96(15) . . ?
O3 Fe4 O8 79.07(14) 5_676 . ?
O3 Fe5 O7 156.59(17) . . ?
O3 Fe5 O9 77.76(16) . . ?
O7 Fe5 O9 91.07(17) . . ?
O3 Fe5 O11 97.04(16) . . ?
O7 Fe5 O11 93.43(17) . . ?
O9 Fe5 O11 174.70(17) . . ?
O3 Fe5 O4 83.12(15) . . ?
O7 Fe5 O4 78.21(15) . . ?
O9 Fe5 O4 98.47(16) . . ?
O11 Fe5 O4 79.73(15) . . ?
O3 Fe5 N 103.15(18) . . ?
O7 Fe5 N 97.89(18) . . ?
O9 Fe5 N 93.13(19) . . ?
O11 Fe5 N 89.04(18) . . ?
O4 Fe5 N 167.79(18) . . ?
O1A C1A C6A 118.4(8) . . ?
O1A C1A C2A 123.4(6) . . ?
C6A C1A C2A 118.2(7) . . ?
O1B C1B C2B 124.3(5) . . ?
O1B C1B C6B 117.4(6) . . ?
C2B C1B C6B 118.3(6) . . ?
O1C C1C C6C 119.4(6) . . ?
O1C C1C C2C 122.7(6) . . ?
C6C C1C C2C 117.8(5) . . ?
C3A C2A C1A 118.7(7) . . ?
C3A C2A C7A 121.7(8) . . ?
C1A C2A C7A 119.6(6) . . ?
C1B C2B C3B 119.2(6) . . ?
C1B C2B C7B 121.3(6) . . ?
C3B C2B C7B 119.5(6) . . ?
C3C C2C C1C 118.5(6) . . ?
C3C C2C C7C 120.9(6) . . ?
C1C C2C C7C 120.5(5) . . ?
C4A C3A C2A 120.5(10) . . ?
C4A C3A H3A 119.8 . . ?
C2A C3A H3A 119.8 . . ?
C4B C3B C2B 121.2(6) . . ?
C4B C3B H3B 119.4 . . ?
C2B C3B H3B 119.4 . . ?
C4C C3C C2C 121.4(7) . . ?
C4C C3C H3C 119.3 . . ?
C2C C3C H3C 119.3 . . ?
C5A C4A C3A 120.7(8) . . ?
C5A C4A H4A 119.6 . . ?
C3A C4A H4A 119.6 . . ?
C3B C4B C5B 120.0(7) . . ?
C3B C4B H4B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C3C C4C C5C 119.7(6) . . ?
C3C C4C H4C 120.2 . . ?
C5C C4C H4C 120.2 . . ?
C4A C5A C6A 120.7(9) . . ?
C4A C5A H5A 119.6 . . ?
C6A C5A H5A 119.6 . . ?
C6B C5B C4B 120.5(6) . . ?
C6B C5B H5B 119.8 . . ?
C4B C5B H5B 119.8 . . ?
C6C C5C C4C 120.9(7) . . ?
C6C C5C H5C 119.5 . . ?
C4C C5C H5C 119.5 . . ?
C5A C6A C1A 121.0(9) . . ?
C5A C6A H6A 119.5 . . ?
C1A C6A H6A 119.5 . . ?
C5B C6B C1B 120.7(6) . . ?
C5B C6B H6B 119.6 . . ?
C1B C6B H6B 119.6 . . ?
C5C C6C C1C 121.6(7) . . ?
C5C C6C H6C 119.2 . . ?
C1C C6C H6C 119.2 . . ?
O2A C7A C2A 123.4(6) . . ?
O2A C7A C8A 114.8(6) . . ?
C2A C7A C8A 121.8(6) . . ?
O2B C7B C2B 121.9(5) . . ?
O2B C7B C8B 116.7(5) . . ?
C2B C7B C8B 121.4(5) . . ?
O2C C7C C2C 123.0(6) . . ?
O2C C7C C8C 116.8(6) . . ?
C2C C7C C8C 120.2(5) . . ?
C9A C8A C13A 119.4(7) . . ?
C9A C8A C7A 119.0(6) . . ?
C13A C8A C7A 121.5(7) . . ?
C9B C8B C13B 118.8(6) . . ?
C9B C8B C7B 119.2(5) . . ?
C13B C8B C7B 121.9(6) . . ?
C9C C8C C13C 120.1(7) . . ?
C9C C8C C7C 118.5(7) . . ?
C13C C8C C7C 121.4(7) . . ?
C10A C9A C8A 120.7(7) . . ?
C10A C9A H9A 119.6 . . ?
C8A C9A H9A 119.6 . . ?
C8B C9B C10B 120.2(7) . . ?
C8B C9B H9B 119.9 . . ?
C10B C9B H9B 119.9 . . ?
C8C C9C C10C 119.3(8) . . ?
C8C C9C H9C 120.4 . . ?
C10C C9C H9C 120.4 . . ?
C9A C10A C11A 120.2(9) . . ?
C9A C10A H10A 119.9 . . ?
C11A C10A H10A 119.9 . . ?
C11B C10B C9B 119.8(7) . . ?
C11B C10B H10B 120.1 . . ?
C9B C10B H10B 120.1 . . ?
C9C C10C C11C 119.2(9) . . ?
C9C C10C H10C 120.4 . . ?
C11C C10C H10C 120.4 . . ?
C12A C11A C10A 120.1(8) . . ?
C12A C11A H11A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C10B C11B C12B 121.6(7) . . ?
C10B C11B H11B 119.2 . . ?
C12B C11B H11B 119.2 . . ?
C12C C11C C10C 120.9(8) . . ?
C12C C11C H11C 119.5 . . ?
C10C C11C H11C 119.5 . . ?
C11A C12A C13A 120.7(8) . . ?
C11A C12A H12A 119.7 . . ?
C13A C12A H12A 119.7 . . ?
C11B C12B C13B 119.2(7) . . ?
C11B C12B H12B 120.4 . . ?
C13B C12B H12B 120.4 . . ?
C11C C12C C13C 121.1(9) . . ?
C11C C12C H12C 119.4 . . ?
C13C C12C H12C 119.4 . . ?
C12A C13A C8A 118.8(8) . . ?
C12A C13A H13A 120.6 . . ?
C8A C13A H13A 120.6 . . ?
C12B C13B C8B 120.3(7) . . ?
C12B C13B H13B 119.8 . . ?
C8B C13B H13B 119.8 . . ?
C12C C13C C8C 119.3(9) . . ?
C12C C13C H13C 120.3 . . ?
C8C C13C H13C 120.3 . . ?
N C14 C15 123.2(8) . . ?
N C14 H14 118.4 . . ?
C15 C14 H14 118.4 . . ?
C14 C15 C16 119.0(8) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C17 C16 C15 117.7(7) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 121.1 . . ?
C18 C17 C16 120.8(8) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N C18 C17 123.0(7) . . ?
N C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
O7 C19 H19A 109.5 . . ?
O7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O6 C20 H20A 109.5 . . ?
O6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O8 C21 H21A 109.5 . . ?
O8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 H22A 109.5 . . ?
O5 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O5 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O9 C23 H23A 109.5 . . ?
O9 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O9 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O12 C24 H24A 109.5 . . ?
O12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O11 C25 H25A 109.5 . . ?
O11 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O11 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C18 N C14 116.2(6) . . ?
C18 N Fe5 121.7(4) . . ?
C14 N Fe5 121.8(5) . . ?
C1A O1A Fe2 126.2(4) . . ?
C1B O1B Fe1 127.2(4) . . ?
C1C O1C Fe3 132.2(4) . . ?
C7A O2A Fe2 128.8(5) . . ?
C7C O2C Fe3 130.7(4) . . ?
C7B O2B Fe1 129.4(4) . . ?
Fe1 O3 Fe5 149.9(2) 5_676 . ?
Fe1 O3 Fe4 103.42(16) 5_676 5_676 ?
Fe5 O3 Fe4 96.93(15) . 5_676 ?
Fe1 O3 Fe3 98.89(15) 5_676 . ?
Fe5 O3 Fe3 101.41(16) . . ?
Fe4 O3 Fe3 94.32(15) 5_676 . ?
Fe4 O4 Fe2 153.0(2) 5_676 . ?
Fe4 O4 Fe5 97.90(15) 5_676 . ?
Fe2 O4 Fe5 100.19(16) . . ?
Fe4 O4 Fe4 95.91(16) 5_676 . ?
Fe2 O4 Fe4 101.31(16) . . ?
Fe5 O4 Fe4 97.58(16) . . ?
C22 O5 Fe3 125.1(4) . 5_676 ?
C22 O5 Fe1 128.1(4) . . ?
Fe3 O5 Fe1 103.34(17) 5_676 . ?
C20 O6 Fe1 127.3(4) . . ?
C20 O6 Fe2 120.7(4) . . ?
Fe1 O6 Fe2 106.18(18) . . ?
C19 O7 Fe5 127.7(4) . . ?
C19 O7 Fe2 130.1(4) . . ?
Fe5 O7 Fe2 101.67(17) . . ?
C21 O8 Fe2 118.9(4) . . ?
C21 O8 Fe4 120.9(4) . . ?
Fe2 O8 Fe4 97.08(15) . . ?
C21 O8 Fe1 120.9(4) . . ?
Fe2 O8 Fe1 98.01(16) . . ?
Fe4 O8 Fe1 95.69(15) . . ?
C23 O9 Fe3 125.7(4) . . ?
C23 O9 Fe5 127.9(4) . . ?
Fe3 O9 Fe5 106.06(18) . . ?
C25 O11 Fe4 120.1(4) . . ?
C25 O11 Fe5 125.0(4) . . ?
Fe4 O11 Fe5 101.73(17) . . ?
C24 O12 Fe4 126.9(4) . . ?
C24 O12 Fe3 124.4(4) . 5_676 ?
Fe4 O12 Fe3 103.87(18) . 5_676 ?
O13A Cl1 O13A 116.2(10) . 2_656 ?
O13A Cl1 O14A 110.4(6) . 2_656 ?
O13A Cl1 O14A 108.6(6) 2_656 2_656 ?
O13A Cl1 O14A 108.6(6) . . ?
O13A Cl1 O14A 110.4(6) 2_656 . ?
O14A Cl1 O14A 101.8(10) 2_656 . ?
O13B Cl1 O13B 116.8(10) . 2_656 ?
O13B Cl1 O14B 109.3(6) . 2_656 ?
O13B Cl1 O14B 109.1(6) 2_656 2_656 ?
O13B Cl1 O14B 109.1(5) . . ?
O13B Cl1 O14B 109.3(6) 2_656 . ?
O14B Cl1 O14B 102.3(9) 2_656 . ?
O15 Cl2 O16 111.2(9) . . ?
O15 Cl2 O17 111.9(10) . . ?
O16 Cl2 O17 109.3(9) . . ?
O15 Cl2 O18 108.9(9) . . ?
O16 Cl2 O18 107.2(10) . . ?
O17 Cl2 O18 108.2(10) . . ?
O10 C26 H26A 109.5 . . ?
O10 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O10 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_refine_diff_density_max         1.698
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.135

# start Validation Reply Form

_vrf_PLAT041_4                   
;
RESPONSE:The missing (not located by a difference synthesis) H-atom 
of the crystallization methanol molecule C26-O10 has been included in 
the sum and moiety formula and the Mr and F(000) have been modified 
accordingly. These modifications account for the differences detected in the 
relevant data items.  
;

_vrf_PLAT341_4                   
;
RESPONSE:Several crystals of the title compound were carefully
tested on the X-rays at 100 K. 
The diffraction quality of the crystals has proven to be moderate
and structure determination was eventually carried out by means of the
best data set collected. 
;

_vrf_CELLZ01_4                   
; 
RESPONSE:See comment above.
;

_vrf_PLAT003_4                   
;
RESPONSE: The structure is disordered, especially the perchlorate counter ions. 
Soft restraints were used to handle the disorder of these molecules. 
;

# end Validation Reply Form

